#------------------------------------------------------------------------------
#$Date: 2023-12-23 03:56:48 +0100 (Sat, 23 Dec 2023) $
#$Revision: 288525 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022989.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2022989
loop_
_publ_author_name
'Neary, Michelle C.'
'Corfield, Peter W. R.'
'Parkin, Sean R.'
'Saba, Shahrokh'
_publ_section_title
;
Crystal structures of two formamidinium hexafluoridophosphate salts, one
with batch-dependent disorder
;
_journal_issue 1
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 88
_journal_page_last 93
_journal_paper_doi 10.1107/S2056989023010848
_journal_volume 80
_journal_year 2023
_chemical_formula_iupac 'C5 H11 N2 O +, P F6 -'
_chemical_formula_moiety 'C5 H11 N2 O +, F6 P -'
_chemical_formula_sum 'C5 H11 F6 N2 O P'
_chemical_formula_weight 260.13
_chemical_name_systematic
;
Morpholinoformamidinium hexafluorophosphate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 29
_space_group_name_Hall 'P 2c -2ac'
_space_group_name_H-M_alt 'P c a 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 10.4504(14)
_cell_length_b 13.7170(16)
_cell_length_c 13.4157(14)
_cell_measurement_reflns_used 9865
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 33.15
_cell_measurement_theta_min 3.38
_cell_volume 1923.1(4)
_computing_cell_refinement
;
SAINT (Bruker, 2022)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2022)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and WinGX (Farrugia,
2012)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0395
_diffrn_reflns_av_unetI/netI 0.0279
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 42268
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.130
_diffrn_reflns_theta_min 1.949
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.356
_exptl_absorpt_correction_T_max 0.9705
_exptl_absorpt_correction_T_min 0.8559
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.797
_exptl_crystal_description block
_exptl_crystal_F_000 1056
_exptl_crystal_size_max 0.240
_exptl_crystal_size_mid 0.230
_exptl_crystal_size_min 0.140
_refine_diff_density_max 0.275
_refine_diff_density_min -0.404
_refine_ls_abs_structure_details
;
Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack 0.5
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 364
_refine_ls_number_reflns 7300
_refine_ls_number_restraints 154
_refine_ls_restrained_S_all 1.008
_refine_ls_R_factor_all 0.0537
_refine_ls_R_factor_gt 0.0322
_refine_ls_shift/su_max 0.016
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0769
_refine_ls_wR_factor_ref 0.0881
_reflns_number_gt 5163
_reflns_number_total 7300
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5706sup1.cif
_cod_data_source_block 1recryst
_cod_database_code 2022989
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.919
_shelx_estimated_absorpt_t_max 0.952
_shelx_hkl_file
;
-1 0 0 0.54340 0.28905 4
-2 0 0 919.611 28.5571 1
-3 0 0 -0.2509 0.58363 4
-3 0 0 0.87553 0.70670 3
-3 0 0 0.37487 0.55509 5
3 0 0 0.27710 0.62278 4
-4 0 0 5160.20 125.790 1
-4 0 0 5234.09 126.119 1
-5 0 0 -0.3681 0.82045 5
-5 0 0 0.63698 1.05113 4
-5 0 0 -0.0606 0.68636 3
-5 0 0 1.05133 1.06061 6
5 0 0 0.75615 0.88310 4
-6 0 0 1963.68 44.0918 4
-6 0 0 2045.32 44.2255 6
-6 0 0 1877.34 42.8613 5
-7 0 0 0.53432 1.42374 3
-7 0 0 -0.7127 1.37678 4
-7 0 0 0.54873 1.35361 6
-8 0 0 717.177 20.8425 3
-8 0 0 734.555 21.6337 4
-8 0 0 756.853 21.6997 6
-9 0 0 1.52838 2.10252 4
-9 0 0 0.16689 1.77439 6
-9 0 0 6.23915 2.64946 3
-10 0 0 866.823 26.1957 4
-10 0 0 857.071 26.0419 6
-11 0 0 6.23741 2.83454 4
-11 0 0 2.86855 2.50696 6
-11 0 0 4.15527 2.44180 3
-12 0 0 15.5929 4.21697 4
-12 0 0 12.3670 4.06367 6
-12 0 0 8.96586 3.47343 3
-13 0 0 1.15894 2.94206 3
-13 0 0 -0.3479 2.55756 4
-13 0 0 3.54999 3.05688 6
-14 0 0 66.8547 7.96772 4
-14 0 0 59.3146 7.37016 6
-14 0 0 50.3719 7.00468 3
-15 0 0 -3.3758 3.72734 6
-15 0 0 10.2402 4.60024 4
-15 0 0 7.53906 3.88264 3
-16 0 0 29.0313 6.62697 6
-16 0 0 36.6085 6.91964 4
16 0 0 29.7759 6.31003 2
-16 1 0 -5.9847 4.16689 4
-16 1 0 -0.4943 3.43767 6
-16 1 0 -3.7155 4.03461 3
-15 1 0 -1.4240 2.99743 4
-15 1 0 -2.8774 3.14007 3
-15 1 0 -5.5561 3.19378 6
-14 1 0 1.16881 3.20221 3
-14 1 0 3.31840 3.56351 6
-14 1 0 1.32132 3.07785 4
-13 1 0 -0.1492 2.56127 4
-13 1 0 -2.2155 2.10372 6
-12 1 0 -3.7339 1.79149 4
-12 1 0 -0.3875 2.31849 6
-12 1 0 -1.7183 2.40556 3
-11 1 0 -0.6257 1.83654 6
-11 1 0 1.78681 2.37181 4
-11 1 0 0.49694 2.31186 3
-10 1 0 0.13990 2.10098 3
-10 1 0 0.21380 2.40050 6
-10 1 0 -0.9061 1.97785 4
-9 1 0 -1.6033 1.46310 3
-9 1 0 -1.7185 1.39514 6
-9 1 0 0.69969 2.15919 4
-8 1 0 0.88696 1.84079 4
-8 1 0 0.34849 1.86082 3
-8 1 0 -1.5552 1.37916 6
-7 1 0 1.81827 1.64135 4
-7 1 0 1.10115 1.07357 5
-7 1 0 1.01610 1.43403 6
-6 1 0 2.02588 1.14576 5
-6 1 0 0.31802 1.26615 4
-6 1 0 1.47966 1.34440 3
-6 1 0 0.73189 0.83935 6
5 -1 0 -0.4510 0.72252 4
5 -1 0 -0.2232 0.74002 5
5 -1 0 -0.1849 0.80058 3
-5 1 0 -0.3554 0.82292 4
-5 1 0 0.10683 0.77032 3
-5 1 0 -0.7780 0.69975 5
4 -1 0 1.41203 0.84885 3
4 -1 0 -0.0502 0.68344 5
4 -1 0 -0.0283 0.69401 4
-4 1 0 0.48843 0.60401 5
-4 1 0 0.18976 0.76900 4
-4 1 0 0.75868 0.71094 3
3 -1 0 0.42651 0.56522 3
3 -1 0 1.05593 0.67476 5
3 -1 0 -0.2424 0.47914 4
-3 1 0 -0.1052 0.64909 4
-3 1 0 0.18998 0.51897 5
-3 1 0 -0.0296 0.49815 3
2 -1 0 -0.1215 0.34638 5
2 -1 0 -0.0297 0.38219 4
2 -1 0 0.74784 0.59799 3
-2 1 0 -0.0219 0.38729 3
-2 1 0 -0.2550 0.40253 4
-2 1 0 0.40155 0.35279 5
1 -1 0 0.22475 0.21599 3
1 -1 0 -0.0585 0.19876 4
1 -1 0 0.07049 0.18277 5
-1 1 0 0.12208 0.17108 5
-1 1 0 0.12276 0.21445 4
-1 1 0 -0.0502 0.20917 3
-1 -1 0 0.19860 0.24823 6
-1 -1 0 0.09968 0.24624 4
-1 -1 0 -0.3671 0.25112 3
1 1 0 -0.4041 0.16470 4
1 1 0 0.04517 0.20362 6
1 1 0 0.00807 0.20065 2
-2 -1 0 0.42127 0.57087 4
-2 -1 0 -0.0076 0.51452 6
2 1 0 0.17156 0.46529 4
-3 -1 0 -0.5690 0.44383 5
-3 -1 0 0.23586 0.74061 4
-3 -1 0 -0.2419 0.58744 6
3 1 0 -0.0390 0.57386 4
-4 -1 0 -0.4321 0.67553 6
-4 -1 0 0.53872 0.97648 4
-4 -1 0 -0.9059 0.44175 5
4 1 0 -0.3370 0.62567 4
-5 -1 0 -0.1906 0.89209 6
-5 -1 0 -0.5485 0.76801 5
-5 -1 0 -0.0614 0.74841 3
-5 -1 0 -0.5807 0.84481 4
5 1 0 0.14924 0.58993 4
-6 -1 0 0.88282 1.32708 4
-6 -1 0 1.87209 1.07043 5
-6 -1 0 1.44923 1.42177 3
-6 -1 0 -0.4608 1.00679 6
-7 -1 0 -1.7767 0.98154 6
-7 -1 0 -0.4762 1.37582 4
-7 -1 0 -0.3937 1.20809 3
-8 -1 0 0.32170 1.62219 6
-8 -1 0 -1.3401 1.47261 4
-8 -1 0 0.55553 1.95907 3
-9 -1 0 0.49979 2.12506 3
-9 -1 0 2.60600 2.28597 4
-9 -1 0 2.60312 2.21656 6
-10 -1 0 0.24514 2.08106 4
-10 -1 0 0.90260 2.16640 3
-10 -1 0 0.85967 2.30334 6
-11 -1 0 0.87483 2.47063 3
-11 -1 0 -0.3385 1.84060 6
-11 -1 0 3.15984 2.42772 4
-12 -1 0 4.84931 2.82156 4
-12 -1 0 -0.8614 2.12110 3
-12 -1 0 -0.3569 2.55275 6
-13 -1 0 -0.0461 2.83730 3
-13 -1 0 2.34349 3.48269 4
-13 -1 0 1.52501 2.63451 6
-14 -1 0 2.87274 2.93164 6
-14 -1 0 1.23546 3.26867 3
-14 -1 0 -2.5971 3.00700 4
14 1 0 -3.9608 1.94455 2
-15 -1 0 2.13739 3.30018 6
-15 -1 0 4.93145 3.78067 4
-15 -1 0 3.99938 3.26727 3
15 1 0 1.83676 2.64636 2
-16 -1 0 -5.6756 3.28733 6
-16 -1 0 -0.8941 3.53757 4
16 1 0 -1.1231 3.73284 2
-16 2 0 27.8132 6.46671 6
-16 2 0 40.3212 7.87103 4
-15 2 0 5.40718 4.06487 6
-15 2 0 -2.2437 3.60726 4
-15 2 0 9.74023 4.23295 3
-14 2 0 45.9774 6.06401 3
-14 2 0 41.8644 6.33874 6
-14 2 0 44.7852 6.67069 4
-13 2 0 5.06434 3.28197 6
-13 2 0 3.02130 3.14243 4
-12 2 0 28.0761 4.93376 3
-12 2 0 26.6377 4.84015 6
-12 2 0 31.8714 5.16000 4
-11 2 0 2.24853 2.57860 4
-11 2 0 3.10709 2.60819 6
-11 2 0 3.89755 2.79864 3
-10 2 0 2375.40 56.5508 4
-10 2 0 2362.55 55.1010 3
-10 2 0 2346.80 56.2371 6
-9 2 0 285.352 12.1769 6
-9 2 0 287.586 11.8347 3
-9 2 0 283.614 12.2964 4
-8 2 0 75.0941 5.78442 4
-8 2 0 80.8390 5.82642 6
-7 2 0 56.0615 3.96868 5
-7 2 0 58.9328 4.59306 6
-7 2 0 57.8445 4.69199 4
6 -2 0 408.504 12.5325 3
6 -2 0 401.484 11.8166 5
-6 2 0 404.045 12.0889 3
-6 2 0 418.454 12.7781 5
-6 2 0 392.233 12.6459 6
-6 2 0 406.383 12.8353 4
5 -2 0 1165.56 27.1301 3
5 -2 0 1187.84 26.3865 5
5 -2 0 1129.36 27.1613 4
-5 2 0 1198.43 26.3605 5
-5 2 0 1157.23 27.3850 4
-4 2 0 8149.06 184.847 1
3 -2 0 61.2242 2.65631 5
3 -2 0 59.7798 2.96863 4
3 -2 0 57.2982 2.88457 3
-3 2 0 62.3907 3.06970 4
-3 2 0 62.2156 2.63261 5
-3 2 0 63.3666 2.84129 3
2 -2 0 3265.79 77.6212 1
-2 2 0 3288.15 77.5519 1
1 -2 0 -0.1697 0.37854 2
1 -2 0 0.24335 0.37740 3
1 -2 0 -0.1220 0.19608 4
1 -2 0 0.63908 0.33849 5
-1 2 0 0.38906 0.27410 4
-1 2 0 -0.0493 0.41004 2
-1 2 0 0.40205 0.29019 5
-1 -2 0 0.28371 0.33238 6
-1 -2 0 0.23754 0.34367 4
-1 -2 0 0.28784 0.34243 2
-1 -2 0 1.24566 0.52044 3
1 2 0 0.32619 0.30806 2
1 2 0 0.19772 0.37599 3
-2 -2 0 3314.01 77.8519 1
2 2 0 3257.57 77.7081 1
-3 -2 0 60.0943 3.40532 6
-3 -2 0 58.9754 3.49220 4
3 2 0 59.1451 3.01080 4
-5 -2 0 1163.50 27.0825 4
-5 -2 0 1140.31 26.7895 3
-5 -2 0 1117.29 26.6556 5
-5 -2 0 1150.22 26.9697 6
5 2 0 1114.58 26.6846 4
-6 -2 0 406.478 12.9954 4
-6 -2 0 391.341 12.6722 3
-6 -2 0 415.250 12.9699 6
-7 -2 0 55.4058 4.57450 6
-7 -2 0 57.9265 4.61065 3
-7 -2 0 54.6717 4.65281 4
-8 -2 0 83.4799 6.91799 4
-8 -2 0 86.0449 7.02585 6
-9 -2 0 265.735 11.8528 6
-9 -2 0 281.082 11.9479 3
-9 -2 0 256.441 11.7260 4
-10 -2 0 2394.53 56.2935 3
-10 -2 0 2370.33 56.8004 6
-10 -2 0 2376.59 57.0294 4
-11 -2 0 7.75557 3.22190 6
-11 -2 0 3.66172 2.91456 4
-11 -2 0 3.63432 2.70010 3
-12 -2 0 23.9898 5.20232 4
-12 -2 0 38.8215 5.80673 3
-12 -2 0 29.7176 5.16254 6
-13 -2 0 5.41492 3.63555 3
-13 -2 0 12.3660 4.63716 4
-13 -2 0 1.79690 2.84834 6
13 2 0 5.50484 2.89566 2
-14 -2 0 32.2518 6.25892 3
-14 -2 0 42.5247 6.70969 4
-14 -2 0 33.5689 6.58342 6
14 2 0 36.3615 5.37747 2
-15 -2 0 -1.1528 3.24470 3
-15 -2 0 1.96196 3.24661 6
-15 -2 0 1.25716 3.15309 4
15 2 0 -3.5294 3.12663 2
-16 -2 0 27.1939 6.81758 4
-16 -2 0 22.9152 6.49287 6
-15 3 0 0.20434 3.07289 6
-15 3 0 -2.1704 2.91566 4
-15 3 0 -1.5297 2.54315 3
-14 3 0 0.08282 3.47133 6
-14 3 0 1.01438 3.15710 4
-14 3 0 0.51334 3.22333 3
-13 3 0 3.02581 2.99668 6
-13 3 0 4.25641 3.15212 3
-13 3 0 0.09785 2.58760 4
-12 3 0 0.84382 2.49492 4
-12 3 0 -2.2001 1.81899 3
-12 3 0 -1.6380 2.09814 6
-11 3 0 2.51286 2.04031 3
-11 3 0 -2.5969 2.12894 4
-11 3 0 1.37784 2.51857 6
-10 3 0 1.34684 2.28304 6
-10 3 0 -1.4620 2.02454 4
-10 3 0 -1.2909 2.30206 3
-9 3 0 -1.6342 1.84373 3
-9 3 0 0.76788 1.96489 4
-9 3 0 3.48653 2.11831 6
-8 3 0 0.81587 2.27897 4
-8 3 0 1.50994 1.71278 6
7 -3 0 1.27946 1.51622 3
7 -3 0 -1.1979 0.87572 5
-7 3 0 0.89318 1.36123 6
-7 3 0 0.34478 1.40782 4
-7 3 0 1.09415 1.09361 5
6 -3 0 0.99240 1.08348 3
6 -3 0 -0.6502 0.78583 5
-6 3 0 -0.6700 0.70994 3
-6 3 0 0.72711 1.10084 4
-6 3 0 -0.0572 0.71943 5
5 -3 0 0.78694 0.89382 4
5 -3 0 -0.0266 0.75508 5
5 -3 0 -0.1816 0.70898 3
-5 3 0 -0.3039 0.73352 4
-5 3 0 -0.2750 0.59782 5
4 -3 0 0.94639 0.72881 4
4 -3 0 0.36875 0.66138 5
4 -3 0 0.12809 0.79659 3
-4 3 0 0.35269 0.59675 5
-4 3 0 1.26992 0.79350 3
-4 3 0 -0.3130 0.71313 4
3 -3 0 0.24302 0.39931 5
3 -3 0 -0.3571 0.43801 4
-3 3 0 0.83263 0.63389 3
-3 3 0 0.21701 0.58342 4
-3 3 0 0.00003 0.35151 5
2 -3 0 -0.5680 0.28644 4
2 -3 0 0.44042 0.41462 5
2 -3 0 0.37348 0.47000 3
2 -3 0 -0.3682 0.41607 2
-2 3 0 0.39248 0.37734 5
-2 3 0 0.00889 0.44556 3
1 -3 0 0.06126 0.32761 5
1 -3 0 -0.2527 0.48861 2
1 -3 0 -0.1778 0.41364 3
-1 3 0 -0.0517 0.27210 4
-1 3 0 0.44776 0.46978 3
-1 3 0 -0.2912 0.41397 2
0 -3 0 0.51106 0.53313 3
0 -3 0 0.34812 0.23330 6
0 3 0 0.09087 0.47727 3
0 3 0 -0.0878 0.21948 6
0 3 0 0.55528 0.40546 2
-1 -3 0 0.52092 0.71198 3
-1 -3 0 0.76004 0.41920 2
-1 -3 0 -0.2326 0.39780 6
1 3 0 0.11755 0.43931 3
1 3 0 0.13736 0.37261 4
1 3 0 0.01986 0.38009 2
1 3 0 0.06516 0.44322 6
-2 -3 0 0.27196 0.68786 3
-2 -3 0 0.35322 0.71772 4
-2 -3 0 0.19901 0.52286 2
-2 -3 0 0.05785 0.53069 6
2 3 0 0.19580 0.47098 6
2 3 0 -0.3231 0.34621 2
2 3 0 -0.3616 0.43409 4
-3 -3 0 0.92218 0.96628 3
3 3 0 0.02106 0.53670 4
3 3 0 0.49215 0.54468 2
-4 -3 0 -0.6330 0.73277 6
-4 -3 0 0.70159 0.93758 3
-4 -3 0 -0.8837 0.75685 4
4 3 0 1.11106 0.83878 2
4 3 0 -0.0308 0.66179 4
-5 -3 0 0.89647 0.95595 5
-5 -3 0 0.71994 1.09555 6
-5 -3 0 0.73771 1.27662 3
-5 -3 0 0.65434 1.08002 4
5 3 0 -0.5010 0.61215 2
5 3 0 -0.6842 0.74672 4
-6 -3 0 -0.0119 1.16914 6
-6 -3 0 -0.1884 1.09906 3
-6 -3 0 -0.1796 1.12171 4
6 3 0 0.69836 0.94891 2
-7 -3 0 0.22075 1.39686 3
-7 -3 0 0.70163 1.48953 6
-7 -3 0 -0.6340 1.29094 4
-8 -3 0 -0.5645 1.60790 3
-9 -3 0 0.66487 2.18935 4
-9 -3 0 -0.7932 1.66861 6
-9 -3 0 -2.7048 1.41712 3
-10 -3 0 1.31894 2.44327 3
-10 -3 0 -0.2994 2.14843 4
-10 -3 0 1.25229 2.28771 6
10 3 0 0.41997 2.15769 2
-11 -3 0 -0.4971 2.10455 4
-11 -3 0 1.11377 2.19760 3
-11 -3 0 -1.5713 1.97060 6
11 3 0 1.62511 1.88194 2
-12 -3 0 0.30773 2.14539 3
-12 -3 0 1.69006 2.67209 4
-12 -3 0 -0.8259 2.24033 6
-13 -3 0 1.32252 2.52206 3
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4 1 19 5.10060 4.11484 2
4 1 19 4.36125 3.92015 4
-5 -1 -19 17.0830 4.36217 5
-5 -1 -19 13.1960 4.90745 6
5 1 19 21.2895 5.41706 4
5 1 19 13.5240 4.88749 2
-6 -1 -19 -4.0685 2.76305 6
-6 -1 -19 6.17002 3.74277 5
6 1 19 2.13739 3.45904 2
6 -2 -19 18.9425 5.56099 5
-6 2 19 30.4264 6.94947 4
-6 2 19 14.2439 5.03051 2
5 -2 -19 5.04084 4.06154 5
-5 2 19 5.77918 3.93668 2
4 -2 -19 137.166 11.7427 5
-4 2 19 137.355 11.3945 4
-4 2 19 140.178 9.73351 2
3 -2 -19 29.3614 6.11151 5
-3 2 19 26.7944 5.53298 2
-3 2 19 21.3910 5.74473 4
2 -2 -19 38.1337 6.15290 5
-2 2 19 29.7568 5.60597 2
-2 2 19 32.2651 6.05051 4
1 -2 -19 21.1289 5.62848 5
-1 2 19 22.7052 4.34526 2
-1 2 19 12.9798 4.62246 4
0 -2 -19 3.70498 2.83815 5
0 2 19 -5.4792 2.59937 4
0 2 19 0.32063 2.91550 2
-1 -2 -19 17.4349 4.74941 5
1 2 19 17.2215 4.43890 2
1 2 19 15.9998 4.61839 4
-2 -2 -19 30.8156 5.86820 5
-2 -2 -19 29.2017 6.05379 6
2 2 19 31.8178 6.73840 4
2 2 19 42.9550 6.13390 2
-3 -2 -19 17.7683 4.77399 6
-3 -2 -19 22.5659 4.95390 5
3 2 19 24.6864 5.68341 4
3 2 19 22.1037 5.40834 2
-4 -2 -19 118.407 10.0673 6
-4 -2 -19 124.851 9.55401 5
4 2 19 130.925 10.9378 4
4 2 19 151.106 10.4288 2
-5 -2 -19 7.82929 4.22005 5
5 2 19 4.95400 3.76200 2
5 2 19 -0.4138 4.28644 4
-6 -2 -19 18.7099 5.20536 5
-6 -2 -19 26.8020 6.33625 6
-5 3 19 14.8385 4.44148 2
-5 3 19 14.4983 5.46394 4
4 -3 -19 -1.5382 3.39842 5
-4 3 19 -1.3102 3.34853 2
-4 3 19 -1.3089 3.16228 4
3 -3 -19 -0.2614 3.80355 5
-3 3 19 6.06912 3.53414 4
-3 3 19 -0.0124 3.27012 2
2 -3 -19 11.7306 4.06034 5
-2 3 19 9.18953 4.17786 4
-2 3 19 11.7682 4.11854 2
1 -3 -19 2.35076 3.09170 5
-1 3 19 -1.4942 2.68135 2
0 -3 -19 4.14941 3.74872 5
0 3 19 -1.7559 2.67346 2
0 3 19 3.41214 3.37479 4
-1 -3 -19 -0.1655 2.36691 5
1 3 19 1.47896 2.88480 4
1 3 19 0.23997 2.66898 2
-2 -3 -19 11.5748 3.72815 6
-2 -3 -19 8.52478 3.19599 5
2 3 19 2.61594 3.80434 2
2 3 19 10.1268 4.17778 4
-3 -3 -19 -1.2202 2.42865 6
-3 -3 -19 5.24163 3.37748 5
3 3 19 -1.6601 3.04985 4
3 3 19 2.38003 2.88247 2
-4 -3 -19 1.18497 3.34367 6
-4 -3 -19 3.23178 2.86274 5
4 3 19 -0.6590 3.05464 4
4 3 19 -0.0574 3.47079 2
-5 -3 -19 33.2615 6.21895 5
5 -4 -19 -0.6074 3.75312 5
-5 4 19 5.72332 4.38382 2
-5 4 19 13.9655 5.42355 4
4 -4 -19 50.0123 7.35355 5
-4 4 19 36.2679 5.89647 2
3 -4 -19 70.2977 8.47725 5
-3 4 19 89.5475 9.42612 4
-3 4 19 75.2754 7.98859 2
-2 4 19 130.482 9.65732 2
-2 4 19 122.665 10.9338 4
1 -4 -19 13.4254 4.61465 5
-1 4 19 9.88284 3.80241 2
-1 4 19 9.54599 4.06956 4
0 -4 -19 2.70783 3.24771 5
0 4 19 1.23963 2.60825 2
0 4 19 1.59146 3.93173 4
-1 -4 -19 8.60559 3.85428 5
1 4 19 18.7138 4.88265 2
1 4 19 14.9504 4.60594 4
-2 -4 -19 120.556 10.1647 6
-2 -4 -19 123.499 10.3258 5
2 4 19 123.043 9.82196 2
2 4 19 113.395 10.1180 4
-3 -4 -19 89.1769 8.75213 5
-3 -4 -19 65.0750 7.71027 6
3 4 19 80.5834 8.63466 4
-4 -4 -19 36.2431 6.43985 5
4 4 19 42.6042 6.20677 2
-5 -4 -19 24.3392 5.48711 5
-5 -4 -19 11.1002 4.33322 6
5 4 19 1.54548 4.06832 4
-4 5 19 0.45666 3.00650 2
-4 5 19 4.36850 3.99390 4
3 -5 -19 -1.8505 3.06648 5
-3 5 19 1.31118 3.55579 2
-2 5 19 6.09387 3.86093 4
-2 5 19 7.96415 4.16512 2
1 -5 -19 -2.0948 2.93502 5
-1 5 19 1.93847 3.12831 4
-1 5 19 2.72300 3.09008 2
0 -5 -19 3.24776 3.17390 5
0 5 19 -4.2451 2.70700 4
0 5 19 -2.4119 2.71039 2
-1 -5 -19 -3.5245 3.53692 5
1 5 19 3.67481 3.61930 2
1 5 19 -0.0758 3.14444 4
-2 -5 -19 3.67819 3.47167 6
-2 -5 -19 1.64769 2.79709 5
2 5 19 -2.1230 2.72800 2
2 5 19 -0.7326 3.13365 4
-3 -5 -19 0.15237 2.95725 5
3 5 19 5.84069 3.87780 2
-4 -5 -19 1.85637 3.50345 6
-4 -5 -19 2.21084 3.30932 5
4 5 19 1.14589 3.71676 4
4 5 19 4.50155 4.34691 2
4 -6 -19 16.5906 6.39957 5
-4 6 19 17.9561 5.75609 4
-4 6 19 7.38167 3.94679 2
-3 6 19 0.65219 3.24813 2
-3 6 19 5.99624 4.13040 4
2 -6 -19 46.1291 7.01212 5
-2 6 19 39.2026 6.18628 2
1 -6 -19 16.7500 5.00608 5
-1 6 19 20.3179 5.44026 2
0 -6 -19 1.10590 3.20065 5
0 6 19 -0.0816 3.30447 2
-1 -6 -19 15.0291 4.75406 5
1 6 19 7.05316 4.52783 2
-2 -6 -19 40.3756 6.96791 5
2 6 19 41.3808 6.78945 2
-3 -6 -19 2.07787 3.41350 5
-3 -6 -19 1.80867 3.31591 6
3 6 19 2.18640 3.18387 4
3 6 19 5.20214 3.72422 2
-4 -6 -19 7.16904 3.82918 5
-4 -6 -19 3.04065 4.04216 6
4 6 19 10.5635 5.06055 2
4 6 19 12.8314 4.88443 4
3 -7 -19 -1.6495 3.19773 5
-3 7 19 -7.1051 3.71745 2
-3 7 19 0.64505 3.28151 4
2 -7 -19 -1.1701 3.60290 5
-2 7 19 -3.0779 2.54654 2
-2 7 19 -2.3332 2.96786 4
-1 7 19 4.51437 3.84051 2
-1 7 19 -3.4279 3.94625 4
0 -7 -19 -5.3366 2.51264 5
0 7 19 -1.0910 3.32443 4
0 7 19 4.56519 4.24981 2
-1 -7 -19 3.16923 3.52043 5
1 7 19 0.31093 3.18206 4
1 7 19 3.75827 3.64179 2
-2 -7 -19 0.24689 2.91401 6
-2 -7 -19 -0.1898 2.92325 5
2 7 19 1.29691 4.07375 2
2 7 19 -0.4548 3.51592 4
-3 -7 -19 0.56429 3.99034 5
-3 -7 -19 5.39322 3.83780 6
3 7 19 -4.9256 2.90449 4
3 7 19 -4.3524 3.00171 2
1 -8 -19 8.72598 3.98666 5
-1 8 19 8.80407 4.64418 4
0 -8 -19 3.41139 3.41876 5
0 8 19 -0.4918 3.29496 4
-1 -8 -19 5.84280 3.68686 5
1 8 19 1.58442 3.68473 4
1 8 19 9.63601 4.70391 2
-1 -5 20 -0.6629 3.38118 4
0 5 -20 2.13948 3.93767 5
0 -5 20 0.95458 2.67256 4
1 -5 20 3.95626 3.10287 4
2 4 -20 11.0024 5.00590 5
-2 -4 20 7.01797 3.96672 4
1 4 -20 7.10696 3.56160 5
-1 -4 20 -0.8112 2.85302 4
0 4 -20 19.9964 5.04072 5
0 -4 20 23.6895 5.34642 4
-1 4 -20 4.74836 3.86732 5
1 -4 20 5.83837 3.94843 4
2 -4 20 9.72380 3.99087 4
2 -4 20 12.8793 3.41056 2
3 3 -20 17.2948 4.70674 5
-3 -3 20 5.44274 3.58274 4
2 3 -20 5.44215 4.63725 5
-2 -3 20 3.05920 3.66300 4
1 3 -20 2.49742 4.09048 5
-1 -3 20 4.58349 3.27145 4
0 3 -20 2.32889 3.60367 5
0 -3 20 0.34797 3.20364 4
0 -3 20 -0.1711 2.59406 2
-1 3 -20 0.39542 3.57466 5
1 -3 20 -0.8300 3.12709 4
2 -3 20 0.33127 3.07422 4
2 -3 20 2.92398 2.90247 2
3 -3 20 14.0064 4.98015 4
3 -3 20 6.12383 3.40171 2
3 2 -20 -2.8882 3.93512 5
-3 -2 20 0.15342 4.26831 4
2 2 -20 31.1580 6.38910 5
-2 -2 20 20.9842 5.49801 4
1 2 -20 1.66202 3.40009 5
-1 -2 20 6.80038 3.03651 2
-1 -2 20 3.38550 3.51622 4
0 2 -20 84.4614 8.47129 5
0 -2 20 75.0468 8.17862 4
-1 2 -20 7.21745 3.61028 5
1 -2 20 13.7587 4.25783 2
1 -2 20 14.5381 4.63597 4
-2 2 -20 39.9097 6.53720 5
2 -2 20 27.3431 6.01183 4
2 -2 20 32.0757 5.19413 2
3 -2 20 5.10143 3.54428 2
3 -2 20 6.15597 3.56825 4
3 1 -20 3.57923 3.79559 5
-3 -1 20 15.3360 5.06035 4
2 1 -20 -2.1793 3.07091 5
-2 -1 20 2.39533 2.79032 2
-2 -1 20 -0.4089 3.06695 4
1 1 -20 1.97262 2.95565 5
-1 -1 20 3.20743 3.41314 4
0 1 -20 8.36728 4.05626 5
0 -1 20 9.71979 3.95957 4
0 -1 20 4.54898 3.09046 2
-1 1 -20 3.17683 3.81727 5
1 -1 20 3.71776 3.65093 4
1 -1 20 -2.3214 2.97130 2
-2 1 -20 4.79754 3.90895 5
2 -1 20 4.49671 3.29386 2
2 -1 20 5.14335 3.34140 4
-3 1 -20 13.2042 4.49914 5
3 -1 20 11.1844 3.71412 2
3 -1 20 8.28453 4.01546 4
3 0 -20 0.25573 3.39114 5
-3 0 20 -1.1178 3.86407 4
2 0 -20 -2.4251 2.95586 5
-2 0 20 -6.0993 3.58736 4
-2 0 20 3.16432 2.85119 2
1 0 -20 -2.0398 2.62075 5
-1 0 20 -0.7555 2.53115 2
-1 0 20 0.24675 3.74563 4
0 0 -20 83.8752 8.45648 5
0 0 20 77.1718 8.40110 4
0 0 20 72.4419 7.12333 2
-1 0 -20 8.36189 3.54927 5
1 0 20 -1.6981 3.11446 4
1 0 20 2.39796 2.61956 2
-2 0 -20 -7.3891 3.62066 5
2 0 20 3.07789 3.43587 2
2 0 20 -2.5125 2.61449 4
-3 0 -20 -5.2393 2.77323 5
3 0 20 -1.9048 2.52466 2
3 0 20 -0.3402 3.00681 4
3 -1 -20 6.73253 4.04645 5
-3 1 20 6.48772 3.49474 2
2 -1 -20 2.49318 3.59233 5
-2 1 20 3.28882 4.24791 4
-2 1 20 2.22824 2.91091 2
1 -1 -20 -3.0836 3.75833 5
-1 1 20 -0.0478 2.55918 2
-1 1 20 7.28917 4.17628 4
0 -1 -20 3.70560 4.04965 5
0 1 20 2.47122 3.60958 4
0 1 20 8.48048 3.48172 2
-1 -1 -20 1.41553 3.71043 5
1 1 20 -2.6199 3.23339 2
1 1 20 4.98077 3.68834 4
-2 -1 -20 0.23443 3.09673 5
2 1 20 3.86497 3.08322 2
2 1 20 -0.8170 3.34798 4
-3 -1 -20 16.9435 4.83166 5
3 1 20 7.86276 3.65144 2
3 -2 -20 -1.6984 3.74058 5
-3 2 20 -0.7380 3.23908 2
-3 2 20 1.19935 3.35759 4
2 -2 -20 24.1548 5.49361 5
-2 2 20 26.7155 5.66719 2
1 -2 -20 13.0530 4.81027 5
-1 2 20 6.34569 3.27598 2
-1 2 20 17.3022 6.51239 4
0 -2 -20 74.7052 8.64160 5
0 2 20 63.3915 6.89120 2
0 2 20 85.0779 9.23010 4
-1 -2 -20 10.2338 4.52063 5
1 2 20 5.67024 3.59047 2
1 2 20 0.15783 5.22862 4
-2 -2 -20 21.2392 6.09667 5
2 2 20 34.6514 5.99685 2
-3 -2 -20 -1.0423 3.18479 5
-3 -2 -20 2.61529 3.35206 6
3 2 20 0.06814 2.92914 2
-3 3 20 10.3446 4.15823 2
-3 3 20 12.8335 4.72283 4
2 -3 -20 2.38819 3.80626 5
-2 3 20 -0.0256 3.50123 2
-2 3 20 2.30857 3.97868 4
1 -3 -20 2.62027 4.16430 5
-1 3 20 2.48873 3.25514 2
0 -3 -20 3.49370 3.12274 5
-1 -3 -20 1.85688 3.04815 5
1 3 20 -3.3541 2.73342 2
-2 -3 -20 -1.3035 2.84574 5
2 3 20 3.57417 3.38008 2
2 3 20 8.15811 5.41057 4
-3 -3 -20 5.50970 4.11195 6
-3 -3 -20 7.49602 3.84146 5
3 3 20 5.56551 4.40349 4
3 3 20 10.5201 4.61964 2
-2 4 20 8.48260 3.81815 2
-2 4 20 12.8208 5.28772 4
1 -4 -20 -4.4518 2.96976 5
-1 4 20 1.47568 3.21812 2
-1 4 20 4.33265 4.18942 4
0 -4 -20 17.3101 5.26197 5
0 4 20 21.4309 5.37085 4
0 4 20 15.6548 4.82056 2
-1 -4 -20 10.6907 4.79480 5
1 4 20 1.78883 3.07561 2
1 4 20 3.95141 3.91270 4
-2 -4 -20 1.70925 4.00520 5
2 4 20 4.72350 4.01096 4
2 4 20 12.0162 4.52194 2
-1 5 20 3.38134 3.56321 4
-1 5 20 -4.8372 3.50160 2
0 5 20 4.97150 3.24723 2
0 5 20 -2.4817 3.10887 4
-1 -5 -20 -1.6738 3.99829 5
1 5 20 4.46251 4.28760 4
1 5 20 -3.2932 2.78071 2
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.9705
_exptl_absorpt_correction_T_min 0.8559
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 0.71073 10.445 13.707 13.408 89.998 90.006 90.001
)
;
_shelx_hkl_checksum 2653
_shelx_res_file
;
TITL m23198 from Parkin, KY: SG Pca21(Saba3 from EtOH)
KY_low2.res
created by SHELXL-2018/3 at 16:44:11 on 21-Nov-2023
CELL 0.71073 10.4504 13.7170 13.4157 90.000 90.000 90.000
ZERR 8 0.0014 0.0016 0.0014 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 1/2+Z
SYMM 1/2+X, -Y, Z
SYMM 1/2-X, Y, 1/2+Z
SFAC C H F N O P
UNIT 40 88 48 16 8 8
TEMP -173
SIZE 0.24 0.23 0.14
REM COLR colourless
REM FORM cut block
REM Estimated minimum and maximum transmission: 0.8559 0.9705
REM OMIT -3 55
L.S. 15
REM TWIN 1 0 0 0 1 0 0 0 -1 leads to Checkcif errors; TWIN does not
TWIN
BOND $H
EQIV $1 x-1/2, -y+1, z
EQIV $2 -x+2, -y+1, z+1/2
EQIV $3 x+1/2, -y+1, z
EQIV $4 -x+3/2, y, z-1/2
EQIV $5 -x+1, -y, z+1/2
EQIV $6 x-1/2, -y, z
EQIV $7 -x+1/2, y, z-1/2
EQIV $8 -x+1/2, y, z+1/2
HTAB C2A F4_$1
HTAB C2A F3_$2
HTAB C6A F4B
HTAB C7A F2
HTAB N8A F4_$1
HTAB N8A F5A_$3
HTAB N8A F5B_$3
HTAB N8A O4A_$4
HTAB N8B F5_$6
HTAB N8B O4B_$7
HTAB N8B' F6_$5
HTAB N8B' O4B'_$8
HTAB
ACTA
CONF
FMAP -2
PLAN 20
REM BASF 0.40(9) not significantly different from 0.5
WGHT 0.039000 0.260000
EXTI 0.003440
FVAR 0.47800 0.63920 0.87555
N1A 4 0.828967 0.482388 0.575231 11.00000 0.01471 0.01196 =
0.01193 0.00007 0.00099 0.00171
C2A 1 0.800044 0.576010 0.622623 11.00000 0.01654 0.01318 =
0.01230 -0.00286 -0.00099 0.00024
AFIX 23
H2A1 2 0.824879 0.630306 0.578020 11.00000 -1.20000
H2A2 2 0.848505 0.582406 0.685693 11.00000 -1.20000
AFIX 0
C3A 1 0.656938 0.579709 0.643397 11.00000 0.01647 0.01393 =
0.01505 0.00031 0.00134 0.00127
AFIX 23
H3A1 2 0.635556 0.641635 0.677442 11.00000 -1.20000
H3A2 2 0.609306 0.577543 0.579648 11.00000 -1.20000
AFIX 0
O4A 5 0.619204 0.498976 0.704857 11.00000 0.02016 0.01962 =
0.01343 0.00047 0.00408 -0.00064
C5A 1 0.649986 0.406910 0.659783 11.00000 0.02320 0.01555 =
0.01924 0.00077 0.00537 -0.00440
AFIX 23
H5A1 2 0.601492 0.399677 0.596823 11.00000 -1.20000
H5A2 2 0.624178 0.353401 0.705039 11.00000 -1.20000
AFIX 0
C6A 1 0.792567 0.399331 0.638257 11.00000 0.02409 0.01429 =
0.01940 0.00612 0.00141 0.00233
AFIX 23
H6A1 2 0.841621 0.400702 0.701372 11.00000 -1.20000
H6A2 2 0.811463 0.337321 0.603486 11.00000 -1.20000
AFIX 0
C7A 1 0.851901 0.470146 0.479634 11.00000 0.00961 0.01439 =
0.01478 -0.00147 0.00039 0.00032
AFIX 43
H7A 2 0.858586 0.405015 0.456128 11.00000 -1.20000
AFIX 0
N8A 4 0.866370 0.540339 0.413800 11.00000 0.02194 0.01727 =
0.01227 -0.00044 0.00349 -0.00124
AFIX 94
H8A1 2 0.861165 0.598392 0.431579 11.00000 -1.20000
H8A2 2 0.880738 0.526744 0.354326 11.00000 -1.20000
AFIX 0
RIGU N1B > N8B
RIGU N1B' > N8B'
PART 1
SAME 0.02 N1A > N8A
N1B 4 0.331793 0.017252 0.572711 21.00000 0.01787 0.01271 =
0.01138 -0.00099 0.00106 -0.00116
C2B 1 0.293850 0.100842 0.634862 21.00000 0.02857 0.01167 =
0.01788 -0.00582 0.00317 -0.00323
AFIX 23
H2B1 2 0.311558 0.162540 0.599144 21.00000 -1.20000
H2B2 2 0.343451 0.100825 0.697733 21.00000 -1.20000
AFIX 0
C3B 1 0.151804 0.092814 0.657491 21.00000 0.02859 0.01918 =
0.01686 -0.00235 0.00237 0.00555
AFIX 23
H3B1 2 0.126171 0.146548 0.702529 21.00000 -1.20000
H3B2 2 0.102490 0.099394 0.594845 21.00000 -1.20000
AFIX 0
O4B 5 0.122242 0.001190 0.703380 21.00000 0.02429 0.02005 =
0.01289 0.00217 0.00560 0.00267
C5B 1 0.160402 -0.079622 0.643160 21.00000 0.01826 0.02002 =
0.01552 0.00058 0.00862 0.00005
AFIX 23
H5B1 2 0.112518 -0.078428 0.579499 21.00000 -1.20000
H5B2 2 0.139565 -0.141230 0.678005 21.00000 -1.20000
AFIX 0
C6B 1 0.303068 -0.075792 0.621944 21.00000 0.01794 0.01331 =
0.01168 0.00072 -0.00311 0.00082
AFIX 23
H6B1 2 0.351804 -0.081037 0.684996 21.00000 -1.20000
H6B2 2 0.327946 -0.130785 0.578259 21.00000 -1.20000
AFIX 0
C7B 1 0.353040 0.028737 0.477637 21.00000 0.01283 0.01659 =
0.01529 -0.00014 0.00091 -0.00005
AFIX 43
H7B 2 0.359065 0.093865 0.454013 21.00000 -1.20000
AFIX 0
N8B 4 0.366846 -0.040562 0.411719 21.00000 0.01988 0.01929 =
0.01845 -0.00122 0.00334 0.00093
AFIX 94
H8B1 2 0.362222 -0.099309 0.429379 21.00000 -1.20000
H8B2 2 0.380363 -0.026447 0.351605 21.00000 -1.20000
AFIX 0
PART 2
SAME 0.02 N1A > N8A
N1B' 4 0.168744 0.017648 0.693532 -21.00000 0.02356 0.01724 =
0.01890 0.00127 0.00280 -0.00313
C2B' 1 0.199041 -0.076943 0.644007 -21.00000 0.02761 0.01071 =
0.02385 -0.00138 0.00903 -0.00266
AFIX 23
H2C3 2 0.154138 -0.081905 0.579227 -21.00000 -1.20000
H2C4 2 0.172359 -0.132281 0.686577 -21.00000 -1.20000
AFIX 0
C3B' 1 0.342110 -0.077937 0.628784 -21.00000 0.02066 0.02372 =
0.02257 0.00247 0.00120 -0.00158
AFIX 23
H3C3 2 0.385858 -0.070707 0.693820 -21.00000 -1.20000
H3C4 2 0.368428 -0.140949 0.599215 -21.00000 -1.20000
AFIX 0
O4B' 5 0.378681 0.000814 0.563569 -21.00000 0.02752 0.02088 =
0.02357 -0.00439 0.00809 -0.00485
C5B' 1 0.344454 0.092319 0.606042 -21.00000 0.02952 0.02281 =
0.01989 0.00152 0.00590 -0.00151
AFIX 23
H5C3 2 0.367287 0.144961 0.558796 -21.00000 -1.20000
H5C4 2 0.394545 0.102477 0.667809 -21.00000 -1.20000
AFIX 0
C6B' 1 0.203593 0.099339 0.630275 -21.00000 0.02902 0.01447 =
0.02080 0.00152 0.01193 0.00201
AFIX 23
H6C3 2 0.185643 0.161482 0.665102 -21.00000 -1.20000
H6C4 2 0.152664 0.097779 0.568073 -21.00000 -1.20000
AFIX 0
C7B' 1 0.145267 0.028457 0.790534 -21.00000 0.01661 0.02014 =
0.01871 -0.00493 0.00098 -0.00251
AFIX 43
H7B' 2 0.133998 0.093460 0.813339 -21.00000 -1.20000
AFIX 0
N8B' 4 0.136199 -0.038045 0.856074 -21.00000 0.03332 0.02328 =
0.01437 -0.00130 0.00460 -0.00138
AFIX 93
H8C3 2 0.145814 -0.099558 0.839021 -21.00000 -1.20000
H8C4 2 0.120303 -0.022593 0.918522 -21.00000 -1.20000
AFIX 0
PART 0
REM Anions
P1 6 1.101737 0.251397 0.380951 11.00000 0.01200 0.01282 =
0.01519 -0.00023 0.00030 0.00034
F1 3 1.134452 0.137710 0.389141 11.00000 0.02642 0.01210 =
0.03228 0.00274 -0.00295 0.00195
F2 3 1.069412 0.365639 0.373237 11.00000 0.02988 0.01384 =
0.03597 0.00269 0.01048 0.00564
F3 3 1.205400 0.263353 0.294459 11.00000 0.03568 0.02336 =
0.02872 0.00247 0.01906 0.00246
F4 3 1.209328 0.274390 0.462915 11.00000 0.03340 0.02946 =
0.03282 -0.00477 -0.01625 -0.00750
F5 3 0.998161 0.240072 0.468084 11.00000 0.03063 0.03187 =
0.04078 0.00660 0.02090 0.00030
F6 3 0.994388 0.227330 0.299937 11.00000 0.03362 0.03114 =
0.04454 0.00292 -0.02455 -0.00293
REM Disordered PF6(2) by rotation about F7-P2-F8
EXYZ P1A P1B
EADP P1A P1B
EXYZ F1A F1B
EADP F1A F1B
EXYZ F2A F2B
EADP F2A F2B
PART 3
P1A 6 0.601695 0.248645 0.385723 31.00000 0.01151 0.01349 =
0.01931 0.00138 -0.00038 -0.00036
F1A 3 0.569761 0.135051 0.383541 31.00000 0.02908 0.01527 =
0.06204 -0.00048 0.00384 -0.00635
F2A 3 0.634150 0.362454 0.388914 31.00000 0.02395 0.01524 =
0.02968 -0.00015 0.00076 -0.00207
F3A 3 0.703340 0.232922 0.297745 31.00000 0.03291 0.02859 =
0.02901 -0.00420 0.01509 -0.00037
F4A 3 0.712165 0.227382 0.465814 31.00000 0.02582 0.03338 =
0.03325 0.00517 -0.01385 0.00552
F5A 3 0.500822 0.264452 0.475493 31.00000 0.02754 0.03491 =
0.02617 -0.00022 0.01276 -0.00248
F6A 3 0.491156 0.270848 0.306681 31.00000 0.02812 0.03531 =
0.03657 -0.00717 -0.01932 0.00687
PART 4
P1B 6 0.601695 0.248645 0.385723 -31.00000 0.01151 0.01349 =
0.01931 0.00138 -0.00038 -0.00036
F1B 3 0.569761 0.135051 0.383541 -31.00000 0.02908 0.01527 =
0.06204 -0.00048 0.00384 -0.00635
F2B 3 0.634150 0.362454 0.388914 -31.00000 0.02395 0.01524 =
0.02968 -0.00015 0.00076 -0.00207
F3B 3 0.723419 0.238427 0.321651 -31.00000 0.02156
F4B 3 0.689687 0.242789 0.484143 -31.00000 0.02179
F5B 3 0.476690 0.257122 0.448348 -31.00000 0.01343
F6B 3 0.517001 0.253059 0.287972 -31.00000 0.01753
PART 0
HKLF 4
REM m23198 from Parkin, KY: SG Pca21(Saba3 from EtOH)
REM wR2 = 0.0881, GooF = S = 1.016, Restrained GooF = 1.008 for all data
REM R1 = 0.0322 for 5163 Fo > 4sig(Fo) and 0.0537 for all 7300 data
REM 364 parameters refined using 154 restraints
END
WGHT 0.0387 0.2543
REM Instructions for potential hydrogen bonds
HTAB C2A F4_$1
HTAB C2A F3_$2
HTAB C3A F3_$2
EQIV $9 -x+1, -y+1, z+1/2
HTAB C3A F6A_$9
HTAB C3A F6B_$9
EQIV $10 -x+3/2, y, z+1/2
HTAB C5A F6_$10
HTAB C6A F2A_$10
HTAB C6A F4A
HTAB C6A F4B
HTAB C7A F2
HTAB N8A F4_$1
HTAB N8A F5A_$3
HTAB N8A F5B_$3
HTAB N8A O4A_$4
EQIV $11 x-1, y, z
HTAB C2B F4_$11
HTAB C2B F1_$10
HTAB C5B F6_$5
HTAB N8B F5_$6
HTAB N8B O4B_$7
HTAB C3B' F5_$6
HTAB C6B' F3_$10
HTAB C6B' F1_$11
HTAB N8B' F6_$5
HTAB N8B' O4B'_$8
REM Highest difference peak 0.275, deepest hole -0.404, 1-sigma level 0.047
Q1 1 1.0781 0.3121 0.3737 11.00000 0.05 0.28
Q2 1 0.3357 0.0216 0.5293 11.00000 0.05 0.26
Q3 1 1.1201 0.1932 0.3795 11.00000 0.05 0.26
Q4 1 0.6588 0.2466 0.3284 11.00000 0.05 0.24
Q5 1 0.6427 0.4871 0.7389 11.00000 0.05 0.23
Q6 1 0.6592 0.2483 0.4263 11.00000 0.05 0.23
Q7 1 0.8281 0.4796 0.5317 11.00000 0.05 0.22
Q8 1 0.8533 0.5017 0.4413 11.00000 0.05 0.22
Q9 1 0.3620 -0.0062 0.3193 11.00000 0.05 0.22
Q10 1 0.5837 0.1887 0.3865 11.00000 0.05 0.22
Q11 1 0.6333 0.3089 0.3908 11.00000 0.05 0.22
Q12 1 0.2009 0.0030 0.6340 11.00000 0.05 -0.22
Q13 1 0.9242 0.4870 0.4819 11.00000 0.05 -0.22
Q14 1 0.5598 0.2489 0.5007 11.00000 0.05 0.21
Q15 1 1.0505 0.2522 0.2671 11.00000 0.05 0.20
Q16 1 1.1584 0.2615 0.3416 11.00000 0.05 0.20
Q17 1 1.1438 0.2604 0.2766 11.00000 0.05 0.19
Q18 1 0.8733 0.5082 0.3149 11.00000 0.05 0.19
Q19 1 0.6901 0.1859 0.3204 11.00000 0.05 0.19
Q20 1 0.1358 0.0115 0.7422 11.00000 0.05 0.19
;
_shelx_res_checksum 69840
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1A 0.8290(2) 0.48239(16) 0.57523(16) 0.0129(4) Uani d 1 . .
C C2A 0.8000(2) 0.57601(18) 0.6226(2) 0.0140(5) Uani d 1 . .
H H2A1 0.824879 0.630306 0.578020 0.017 Uiso calc 1 . .
H H2A2 0.848505 0.582406 0.685693 0.017 Uiso calc 1 . .
C C3A 0.6569(2) 0.57971(19) 0.6434(2) 0.0151(5) Uani d 1 . .
H H3A1 0.635556 0.641635 0.677442 0.018 Uiso calc 1 . .
H H3A2 0.609306 0.577543 0.579648 0.018 Uiso calc 1 . .
O O4A 0.6192(2) 0.49898(12) 0.70486(17) 0.0177(4) Uani d 1 . .
C C5A 0.6500(2) 0.40691(18) 0.6598(2) 0.0193(5) Uani d 1 . .
H H5A1 0.601492 0.399677 0.596823 0.023 Uiso calc 1 . .
H H5A2 0.624178 0.353401 0.705039 0.023 Uiso calc 1 . .
C C6A 0.7926(3) 0.39933(17) 0.63826(19) 0.0193(5) Uani d 1 . .
H H6A1 0.841621 0.400702 0.701372 0.023 Uiso calc 1 . .
H H6A2 0.811463 0.337321 0.603486 0.023 Uiso calc 1 . .
C C7A 0.85190(19) 0.47015(19) 0.47963(18) 0.0129(4) Uani d 1 . .
H H7A 0.858586 0.405015 0.456128 0.016 Uiso calc 1 . .
N N8A 0.8664(2) 0.54034(17) 0.41380(18) 0.0172(4) Uani d 1 . .
H H8A1 0.8612(2) 0.5984(15) 0.4316(5) 0.021 Uiso calc 1 . .
H H8A2 0.8807(4) 0.5267(3) 0.3543(14) 0.021 Uiso calc 1 . .
N N1B 0.3318(4) 0.0173(3) 0.5727(3) 0.0140(6) Uani d 0.639(4) A 1
C C2B 0.2939(4) 0.1008(2) 0.6349(3) 0.0194(7) Uani d 0.639(4) A 1
H H2B1 0.311558 0.162540 0.599144 0.023 Uiso calc 0.639(4) A 1
H H2B2 0.343451 0.100825 0.697733 0.023 Uiso calc 0.639(4) A 1
C C3B 0.1518(4) 0.0928(3) 0.6575(3) 0.0215(7) Uani d 0.639(4) A 1
H H3B1 0.126171 0.146548 0.702529 0.026 Uiso calc 0.639(4) A 1
H H3B2 0.102490 0.099394 0.594845 0.026 Uiso calc 0.639(4) A 1
O O4B 0.1222(3) 0.0012(2) 0.7034(2) 0.0191(6) Uani d 0.639(4) A 1
C C5B 0.1604(5) -0.0796(6) 0.6432(6) 0.0179(10) Uani d 0.639(4) A 1
H H5B1 0.112518 -0.078428 0.579499 0.022 Uiso calc 0.639(4) A 1
H H5B2 0.139565 -0.141230 0.678005 0.022 Uiso calc 0.639(4) A 1
C C6B 0.3031(4) -0.0758(5) 0.6219(5) 0.0143(9) Uani d 0.639(4) A 1
H H6B1 0.351804 -0.081037 0.684996 0.017 Uiso calc 0.639(4) A 1
H H6B2 0.327946 -0.130785 0.578259 0.017 Uiso calc 0.639(4) A 1
C C7B 0.3530(3) 0.0287(2) 0.4776(2) 0.0149(6) Uani d 0.639(4) A 1
H H7B 0.359065 0.093865 0.454013 0.018 Uiso calc 0.639(4) A 1
N N8B 0.3668(3) -0.0406(2) 0.4117(3) 0.0192(6) Uani d 0.639(4) A 1
H H8B1 0.3622(3) -0.099(3) 0.4294(8) 0.023 Uiso calc 0.639(4) A 1
H H8B2 0.3804(7) -0.0264(6) 0.352(3) 0.023 Uiso calc 0.639(4) A 1
N N1B' 0.1687(8) 0.0176(6) 0.6935(6) 0.0199(15) Uani d 0.361(4) A 2
C C2B' 0.1990(10) -0.0769(9) 0.6440(12) 0.021(2) Uani d 0.361(4) A 2
H H2C3 0.154138 -0.081905 0.579227 0.025 Uiso calc 0.361(4) A 2
H H2C4 0.172359 -0.132281 0.686577 0.025 Uiso calc 0.361(4) A 2
C C3B' 0.3421(9) -0.0779(10) 0.6288(11) 0.022(2) Uani d 0.361(4) A 2
H H3C3 0.385858 -0.070707 0.693820 0.027 Uiso calc 0.361(4) A 2
H H3C4 0.368428 -0.140949 0.599215 0.027 Uiso calc 0.361(4) A 2
O O4B' 0.3787(8) 0.0008(5) 0.5636(6) 0.0240(15) Uani d 0.361(4) A 2
C C5B' 0.3445(8) 0.0923(6) 0.6060(7) 0.0241(17) Uani d 0.361(4) A 2
H H5C3 0.367287 0.144961 0.558796 0.029 Uiso calc 0.361(4) A 2
H H5C4 0.394545 0.102477 0.667809 0.029 Uiso calc 0.361(4) A 2
C C6B' 0.2036(8) 0.0993(5) 0.6303(6) 0.0214(16) Uani d 0.361(4) A 2
H H6C3 0.185643 0.161482 0.665102 0.026 Uiso calc 0.361(4) A 2
H H6C4 0.152664 0.097779 0.568073 0.026 Uiso calc 0.361(4) A 2
C C7B' 0.1453(6) 0.0285(6) 0.7905(5) 0.0185(14) Uani d 0.361(4) A 2
H H7B' 0.133998 0.093460 0.813339 0.022 Uiso calc 0.361(4) A 2
N N8B' 0.1362(7) -0.0380(5) 0.8561(6) 0.0237(14) Uani d 0.361(4) A 2
H H8C3 0.145814 -0.099558 0.839021 0.028 Uiso calc 0.361(4) A 2
H H8C4 0.120303 -0.022593 0.918522 0.028 Uiso calc 0.361(4) A 2
P P1 1.10174(10) 0.25140(7) 0.38095(4) 0.0133(2) Uani d 1 . .
F F1 1.1345(2) 0.13771(15) 0.38914(11) 0.0236(5) Uani d 1 . .
F F2 1.0694(2) 0.36564(14) 0.37324(14) 0.0266(4) Uani d 1 . .
F F3 1.2054(2) 0.26335(12) 0.29446(17) 0.0293(5) Uani d 1 . .
F F4 1.2093(2) 0.27439(14) 0.46292(18) 0.0319(5) Uani d 1 . .
F F5 0.9982(2) 0.24007(13) 0.46808(17) 0.0344(5) Uani d 1 . .
F F6 0.9944(2) 0.22733(15) 0.29994(19) 0.0364(5) Uani d 1 . .
P P1A 0.60169(10) 0.24864(7) 0.38572(4) 0.0148(2) Uani d 0.876(19) B 3
F F1A 0.5698(2) 0.13505(16) 0.38354(13) 0.0355(6) Uani d 0.876(19) B 3
F F2A 0.6341(2) 0.36245(16) 0.38891(11) 0.0230(5) Uani d 0.876(19) B 3
F F3A 0.7033(5) 0.2329(2) 0.2977(4) 0.0302(8) Uani d 0.876(19) B 3
F F4A 0.7122(4) 0.2274(3) 0.4658(4) 0.0308(7) Uani d 0.876(19) B 3
F F5A 0.5008(5) 0.2645(2) 0.4755(4) 0.0295(8) Uani d 0.876(19) B 3
F F6A 0.4912(5) 0.2708(3) 0.3067(4) 0.0333(8) Uani d 0.876(19) B 3
P P1B 0.60169(10) 0.24864(7) 0.38572(4) 0.0148(2) Uani d 0.124(19) B 4
F F1B 0.5698(2) 0.13505(16) 0.38354(13) 0.0355(6) Uani d 0.124(19) B 4
F F2B 0.6341(2) 0.36245(16) 0.38891(11) 0.0230(5) Uani d 0.124(19) B 4
F F3B 0.723(2) 0.2384(16) 0.3217(19) 0.022(4) Uiso d 0.124(19) B 4
F F4B 0.690(2) 0.2428(18) 0.4841(18) 0.022(4) Uiso d 0.124(19) B 4
F F5B 0.4767(16) 0.2571(11) 0.4483(16) 0.013(3) Uiso d 0.124(19) B 4
F F6B 0.517(2) 0.2531(16) 0.2880(14) 0.018(4) Uiso d 0.124(19) B 4
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1A 0.0147(9) 0.0120(9) 0.0119(9) 0.0017(8) 0.0010(8) 0.0001(8)
C2A 0.0165(12) 0.0132(10) 0.0123(10) 0.0002(9) -0.0010(10) -0.0029(8)
C3A 0.0165(12) 0.0139(11) 0.0150(11) 0.0013(8) 0.0013(9) 0.0003(9)
O4A 0.0202(9) 0.0196(10) 0.0134(8) -0.0006(7) 0.0041(9) 0.0005(6)
C5A 0.0232(14) 0.0156(12) 0.0192(13) -0.0044(9) 0.0054(9) 0.0008(10)
C6A 0.0241(14) 0.0143(11) 0.0194(13) 0.0023(10) 0.0014(10) 0.0061(8)
C7A 0.0096(9) 0.0144(11) 0.0148(10) 0.0003(7) 0.0004(7) -0.0015(9)
N8A 0.0219(10) 0.0173(10) 0.0123(10) -0.0012(8) 0.0035(9) -0.0004(9)
N1B 0.0179(17) 0.0127(13) 0.0114(12) -0.0012(12) 0.0011(13) -0.0010(10)
C2B 0.029(2) 0.0117(13) 0.0179(17) -0.0032(14) 0.0032(14) -0.0058(11)
C3B 0.029(2) 0.0192(16) 0.0169(16) 0.0056(14) 0.0024(14) -0.0024(12)
O4B 0.0243(17) 0.0200(14) 0.0129(11) 0.0027(12) 0.0056(12) 0.0022(9)
C5B 0.018(2) 0.0200(18) 0.0155(18) 0.000(2) 0.009(2) 0.0006(13)
C6B 0.018(2) 0.0133(15) 0.0117(15) 0.0008(19) -0.0031(19) 0.0007(11)
C7B 0.0128(13) 0.0166(13) 0.0153(13) 0.0000(10) 0.0009(10) -0.0001(10)
N8B 0.0199(14) 0.0193(14) 0.0185(14) 0.0009(11) 0.0033(12) -0.0012(11)
N1B' 0.024(4) 0.017(3) 0.019(3) -0.003(3) 0.003(3) 0.001(2)
C2B' 0.028(5) 0.011(3) 0.024(4) -0.003(4) 0.009(5) -0.001(3)
C3B' 0.021(5) 0.024(4) 0.023(5) -0.002(4) 0.001(4) 0.002(3)
O4B' 0.028(4) 0.021(3) 0.024(3) -0.005(3) 0.008(3) -0.004(2)
C5B' 0.030(4) 0.023(4) 0.020(4) -0.002(3) 0.006(3) 0.002(3)
C6B' 0.029(4) 0.014(3) 0.021(4) 0.002(3) 0.012(3) 0.002(3)
C7B' 0.017(3) 0.020(3) 0.019(3) -0.003(2) 0.001(2) -0.005(3)
N8B' 0.033(4) 0.023(3) 0.014(3) -0.001(3) 0.005(3) -0.001(3)
P1 0.0120(5) 0.0128(4) 0.0152(4) 0.0003(3) 0.00030(18) -0.00023(16)
F1 0.0264(12) 0.0121(10) 0.0323(13) 0.0020(9) -0.0029(6) 0.0027(5)
F2 0.0299(11) 0.0138(9) 0.0360(8) 0.0056(8) 0.0105(7) 0.0027(6)
F3 0.0357(12) 0.0234(8) 0.0287(11) 0.0025(7) 0.0191(9) 0.0025(8)
F4 0.0334(11) 0.0295(9) 0.0328(11) -0.0075(8) -0.0162(9) -0.0048(8)
F5 0.0306(11) 0.0319(10) 0.0408(14) 0.0003(9) 0.0209(11) 0.0066(9)
F6 0.0336(11) 0.0311(9) 0.0445(14) -0.0029(8) -0.0246(11) 0.0029(9)
P1A 0.0115(5) 0.0135(4) 0.0193(6) -0.0004(3) -0.00038(17) 0.00138(15)
F1A 0.0291(12) 0.0153(10) 0.0620(16) -0.0064(9) 0.0038(8) -0.0005(7)
F2A 0.0240(12) 0.0152(11) 0.0297(12) -0.0021(9) 0.0008(5) -0.0001(5)
F3A 0.0329(17) 0.0286(12) 0.0290(16) -0.0004(10) 0.0151(14) -0.0042(11)
F4A 0.0258(13) 0.0334(13) 0.0333(16) 0.0055(10) -0.0139(11) 0.0052(12)
F5A 0.0275(14) 0.0349(12) 0.0262(16) -0.0025(10) 0.0128(14) -0.0002(11)
F6A 0.0281(14) 0.0353(13) 0.0366(15) 0.0069(11) -0.0193(12) -0.0072(12)
P1B 0.0115(5) 0.0135(4) 0.0193(6) -0.0004(3) -0.00038(17) 0.00138(15)
F1B 0.0291(12) 0.0153(10) 0.0620(16) -0.0064(9) 0.0038(8) -0.0005(7)
F2B 0.0240(12) 0.0152(11) 0.0297(12) -0.0021(9) 0.0008(5) -0.0001(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C7A N1A C2A . . 124.9(2) ?
C7A N1A C6A . . 120.6(2) ?
C2A N1A C6A . . 112.1(2) ?
N1A C2A C3A . . 108.1(2) ?
N1A C2A H2A1 . . 110.1 ?
C3A C2A H2A1 . . 110.1 ?
N1A C2A H2A2 . . 110.1 ?
C3A C2A H2A2 . . 110.1 ?
H2A1 C2A H2A2 . . 108.4 ?
O4A C3A C2A . . 110.4(2) ?
O4A C3A H3A1 . . 109.6 ?
C2A C3A H3A1 . . 109.6 ?
O4A C3A H3A2 . . 109.6 ?
C2A C3A H3A2 . . 109.6 ?
H3A1 C3A H3A2 . . 108.1 ?
C3A O4A C5A . . 112.0(2) ?
O4A C5A C6A . . 111.1(2) ?
O4A C5A H5A1 . . 109.4 ?
C6A C5A H5A1 . . 109.4 ?
O4A C5A H5A2 . . 109.4 ?
C6A C5A H5A2 . . 109.4 ?
H5A1 C5A H5A2 . . 108.0 ?
N1A C6A C5A . . 108.1(2) ?
N1A C6A H6A1 . . 110.1 ?
C5A C6A H6A1 . . 110.1 ?
N1A C6A H6A2 . . 110.1 ?
C5A C6A H6A2 . . 110.1 ?
H6A1 C6A H6A2 . . 108.4 ?
N8A C7A N1A . . 125.6(2) ?
N8A C7A H7A . . 117.2 ?
N1A C7A H7A . . 117.2 ?
C7A N8A H8A1 . . 120.0 ?
C7A N8A H8A2 . . 120.0 ?
H8A1 N8A H8A2 . . 120.0 ?
C7B N1B C6B . . 125.4(4) ?
C7B N1B C2B . . 120.4(3) ?
C6B N1B C2B . . 111.5(4) ?
N1B C2B C3B . . 108.7(3) ?
N1B C2B H2B1 . . 110.0 ?
C3B C2B H2B1 . . 110.0 ?
N1B C2B H2B2 . . 110.0 ?
C3B C2B H2B2 . . 110.0 ?
H2B1 C2B H2B2 . . 108.3 ?
O4B C3B C2B . . 111.1(3) ?
O4B C3B H3B1 . . 109.4 ?
C2B C3B H3B1 . . 109.4 ?
O4B C3B H3B2 . . 109.4 ?
C2B C3B H3B2 . . 109.4 ?
H3B1 C3B H3B2 . . 108.0 ?
C5B O4B C3B . . 112.2(4) ?
O4B C5B C6B . . 110.7(5) ?
O4B C5B H5B1 . . 109.5 ?
C6B C5B H5B1 . . 109.5 ?
O4B C5B H5B2 . . 109.5 ?
C6B C5B H5B2 . . 109.5 ?
H5B1 C5B H5B2 . . 108.1 ?
N1B C6B C5B . . 108.4(4) ?
N1B C6B H6B1 . . 110.0 ?
C5B C6B H6B1 . . 110.0 ?
N1B C6B H6B2 . . 110.0 ?
C5B C6B H6B2 . . 110.0 ?
H6B1 C6B H6B2 . . 108.4 ?
N1B C7B N8B . . 126.4(3) ?
N1B C7B H7B . . 116.8 ?
N8B C7B H7B . . 116.8 ?
C7B N8B H8B1 . . 120.0 ?
C7B N8B H8B2 . . 120.0 ?
H8B1 N8B H8B2 . . 120.0 ?
C7B' N1B' C6B' . . 122.1(8) ?
C7B' N1B' C2B' . . 124.8(10) ?
C6B' N1B' C2B' . . 111.0(8) ?
N1B' C2B' C3B' . . 106.2(9) ?
N1B' C2B' H2C3 . . 110.5 ?
C3B' C2B' H2C3 . . 110.5 ?
N1B' C2B' H2C4 . . 110.5 ?
C3B' C2B' H2C4 . . 110.5 ?
H2C3 C2B' H2C4 . . 108.7 ?
O4B' C3B' C2B' . . 109.8(9) ?
O4B' C3B' H3C3 . . 109.7 ?
C2B' C3B' H3C3 . . 109.7 ?
O4B' C3B' H3C4 . . 109.7 ?
C2B' C3B' H3C4 . . 109.7 ?
H3C3 C3B' H3C4 . . 108.2 ?
C5B' O4B' C3B' . . 110.5(9) ?
O4B' C5B' C6B' . . 112.8(7) ?
O4B' C5B' H5C3 . . 109.0 ?
C6B' C5B' H5C3 . . 109.0 ?
O4B' C5B' H5C4 . . 109.0 ?
C6B' C5B' H5C4 . . 109.0 ?
H5C3 C5B' H5C4 . . 107.8 ?
N1B' C6B' C5B' . . 108.7(7) ?
N1B' C6B' H6C3 . . 109.9 ?
C5B' C6B' H6C3 . . 109.9 ?
N1B' C6B' H6C4 . . 109.9 ?
C5B' C6B' H6C4 . . 109.9 ?
H6C3 C6B' H6C4 . . 108.3 ?
N8B' C7B' N1B' . . 127.6(8) ?
N8B' C7B' H7B' . . 116.2 ?
N1B' C7B' H7B' . . 116.2 ?
C7B' N8B' H8C3 . . 120.0 ?
C7B' N8B' H8C4 . . 120.0 ?
H8C3 N8B' H8C4 . . 120.0 ?
F3 P1 F6 . . 90.19(14) ?
F3 P1 F1 . . 90.29(10) ?
F6 P1 F1 . . 89.73(11) ?
F3 P1 F5 . . 179.60(14) ?
F6 P1 F5 . . 90.11(17) ?
F1 P1 F5 . . 89.99(11) ?
F3 P1 F4 . . 90.14(15) ?
F6 P1 F4 . . 179.35(13) ?
F1 P1 F4 . . 89.70(11) ?
F5 P1 F4 . . 89.57(13) ?
F3 P1 F2 . . 89.75(10) ?
F6 P1 F2 . . 90.58(12) ?
F1 P1 F2 . . 179.68(14) ?
F5 P1 F2 . . 89.97(10) ?
F4 P1 F2 . . 89.99(12) ?
F6A P1A F1A . . 91.31(16) ?
F6A P1A F3A . . 90.92(18) ?
F1A P1A F3A . . 89.64(15) ?
F6A P1A F2A . . 89.14(15) ?
F1A P1A F2A . . 179.49(12) ?
F3A P1A F2A . . 90.60(15) ?
F6A P1A F4A . . 179.36(17) ?
F1A P1A F4A . . 89.15(16) ?
F3A P1A F4A . . 89.5(2) ?
F2A P1A F4A . . 90.40(16) ?
F6A P1A F5A . . 89.85(18) ?
F1A P1A F5A . . 90.47(15) ?
F3A P1A F5A . . 179.22(18) ?
F2A P1A F5A . . 89.28(15) ?
F4A P1A F5A . . 89.69(16) ?
F4B P1B F3B . . 88.9(10) ?
F4B P1B F5B . . 92.3(9) ?
F3B P1B F5B . . 178.4(8) ?
F4B P1B F6B . . 178.9(9) ?
F3B P1B F6B . . 90.2(9) ?
F5B P1B F6B . . 88.6(7) ?
F4B P1B F1B . . 94.9(9) ?
F3B P1B F1B . . 94.2(8) ?
F5B P1B F1B . . 84.7(6) ?
F6B P1B F1B . . 84.6(7) ?
F4B P1B F2B . . 84.6(8) ?
F3B P1B F2B . . 85.9(8) ?
F5B P1B F2B . . 95.2(6) ?
F6B P1B F2B . . 95.9(7) ?
F1B P1B F2B . . 179.49(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1A C7A . 1.315(3) ?
N1A C2A . 1.465(3) ?
N1A C6A . 1.469(3) ?
C2A C3A . 1.522(3) ?
C2A H2A1 . 0.9900 ?
C2A H2A2 . 0.9900 ?
C3A O4A . 1.436(3) ?
C3A H3A1 . 0.9900 ?
C3A H3A2 . 0.9900 ?
O4A C5A . 1.437(3) ?
C5A C6A . 1.521(3) ?
C5A H5A1 . 0.9900 ?
C5A H5A2 . 0.9900 ?
C6A H6A1 . 0.9900 ?
C6A H6A2 . 0.9900 ?
C7A N8A . 1.315(3) ?
C7A H7A . 0.9500 ?
N8A H8A1 . 0.83(2) ?
N8A H8A2 . 0.83(2) ?
N1B C7B . 1.304(5) ?
N1B C6B . 1.468(7) ?
N1B C2B . 1.472(5) ?
C2B C3B . 1.519(6) ?
C2B H2B1 . 0.9900 ?
C2B H2B2 . 0.9900 ?
C3B O4B . 1.433(5) ?
C3B H3B1 . 0.9900 ?
C3B H3B2 . 0.9900 ?
O4B C5B . 1.428(8) ?
C5B C6B . 1.519(7) ?
C5B H5B1 . 0.9900 ?
C5B H5B2 . 0.9900 ?
C6B H6B1 . 0.9900 ?
C6B H6B2 . 0.9900 ?
C7B N8B . 1.306(4) ?
C7B H7B . 0.9500 ?
N8B H8B1 . 0.84(4) ?
N8B H8B2 . 0.84(4) ?
N1B' C7B' . 1.333(10) ?
N1B' C6B' . 1.452(10) ?
N1B' C2B' . 1.492(14) ?
C2B' C3B' . 1.509(12) ?
C2B' H2C3 . 0.9900 ?
C2B' H2C4 . 0.9900 ?
C3B' O4B' . 1.442(13) ?
C3B' H3C3 . 0.9900 ?
C3B' H3C4 . 0.9900 ?
O4B' C5B' . 1.424(10) ?
C5B' C6B' . 1.511(10) ?
C5B' H5C3 . 0.9900 ?
C5B' H5C4 . 0.9900 ?
C6B' H6C3 . 0.9900 ?
C6B' H6C4 . 0.9900 ?
C7B' N8B' . 1.271(10) ?
C7B' H7B' . 0.9500 ?
N8B' H8C3 . 0.8800 ?
N8B' H8C4 . 0.8800 ?
P1 F3 . 1.596(2) ?
P1 F6 . 1.596(2) ?
P1 F1 . 1.600(2) ?
P1 F5 . 1.601(2) ?
P1 F4 . 1.604(2) ?
P1 F2 . 1.606(2) ?
P1A F6A . 1.597(3) ?
P1A F1A . 1.594(2) ?
P1A F3A . 1.602(3) ?
P1A F2A . 1.598(2) ?
P1A F4A . 1.604(3) ?
P1A F5A . 1.615(3) ?
P1B F4B . 1.61(2) ?
P1B F3B . 1.54(2) ?
P1B F5B . 1.558(15) ?
P1B F6B . 1.583(18) ?
P1B F1B . 1.594(2) ?
P1B F2B . 1.598(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2A H2A1 F4 3_465 0.99 2.36 3.115(3) 132.8 yes
C2A H2A2 F3 2_765 0.99 2.63 3.189(3) 115.8 yes
C6A H6A2 F4B . 0.99 2.42 3.17(2) 131.8 yes
C7A H7A F2 . 0.95 2.53 3.043(3) 114.3 yes
N8A H8A1 F4 3_465 0.83 2.40 3.096(3) 142.2 yes
N8A H8A1 F5A 3_565 0.83 2.45 3.135(4) 139.7 yes
N8A H8A1 F5B 3_565 0.83 2.33 3.043(15) 143.7 yes
N8A H8A2 O4A 4_654 0.83 2.04 2.864(3) 169.4 yes
N8B H8B1 F5 3_455 0.84 2.45 3.153(4) 141.3 yes
N8B H8B2 O4B 4_554 0.84 2.02 2.855(5) 169.2 yes
N8B' H8C3 F6 2_655 0.88 2.34 3.028(8) 134.7 yes
N8B' H8C4 O4B' 4 0.88 1.97 2.839(12) 167.8 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C7A N1A C2A C3A . . . . 103.6(3) ?
C6A N1A C2A C3A . . . . -59.2(3) ?
N1A C2A C3A O4A . . . . 57.4(3) ?
C2A C3A O4A C5A . . . . -58.2(3) ?
C3A O4A C5A C6A . . . . 57.9(3) ?
C7A N1A C6A C5A . . . . -105.2(3) ?
C2A N1A C6A C5A . . . . 58.4(3) ?
O4A C5A C6A N1A . . . . -56.3(3) ?
C2A N1A C7A N8A . . . . 7.9(4) ?
C6A N1A C7A N8A . . . . 169.3(2) ?
C7B N1B C2B C3B . . . . 104.8(4) ?
C6B N1B C2B C3B . . . . -57.8(4) ?
N1B C2B C3B O4B . . . . 55.8(4) ?
C2B C3B O4B C5B . . . . -57.4(5) ?
C3B O4B C5B C6B . . . . 58.3(7) ?
C7B N1B C6B C5B . . . . -102.8(6) ?
C2B N1B C6B C5B . . . . 58.6(6) ?
O4B C5B C6B N1B . . . . -57.7(7) ?
C6B N1B C7B N8B . . . . -8.3(6) ?
C2B N1B C7B N8B . . . . -168.2(3) ?
C7B' N1B' C2B' C3B' . . . . -101.5(12) ?
C6B' N1B' C2B' C3B' . . . . 62.1(13) ?
N1B' C2B' C3B' O4B' . . . . -62.4(14) ?
C2B' C3B' O4B' C5B' . . . . 60.8(13) ?
C3B' O4B' C5B' C6B' . . . . -56.5(10) ?
C7B' N1B' C6B' C5B' . . . . 106.4(9) ?
C2B' N1B' C6B' C5B' . . . . -57.7(10) ?
O4B' C5B' C6B' N1B' . . . . 54.5(10) ?
C6B' N1B' C7B' N8B' . . . . -166.6(8) ?
C2B' N1B' C7B' N8B' . . . . -4.9(14) ?
_cod_database_fobs_code 2022989