#------------------------------------------------------------------------------
#$Date: 2023-12-23 03:56:48 +0100 (Sat, 23 Dec 2023) $
#$Revision: 288525 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022988.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_2022988
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_coeditor_code WM5706
_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 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_primary dual
_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 10.4638(3)
_cell_length_b 13.4495(4)
_cell_length_c 13.7340(4)
_cell_measurement_reflns_used 9781
_cell_measurement_temperature 130(2)
_cell_measurement_theta_max 74.6
_cell_measurement_theta_min 4.23
_cell_volume 1932.83(10)
_computing_cell_refinement
;
SAINT (Bruker, 2022)
;
_computing_data_collection
;
APEX4 (Bruker, 2022)
;
_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 130(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker D8 with PHOTON III area detector'
_diffrn_measurement_method '\f and \w shutterless scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0338
_diffrn_reflns_av_unetI/netI 0.0209
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 36889
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 74.590
_diffrn_reflns_theta_min 6.253
_diffrn_source microfocus
_exptl_absorpt_coefficient_mu 3.301
_exptl_absorpt_correction_T_max 0.754
_exptl_absorpt_correction_T_min 0.570
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.788
_exptl_crystal_description block
_exptl_crystal_F_000 1056
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.291
_refine_diff_density_min -0.281
_refine_ls_extinction_coef 0.00052(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.116
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 165
_refine_ls_number_reflns 1969
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.116
_refine_ls_R_factor_all 0.0265
_refine_ls_R_factor_gt 0.0251
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0702
_refine_ls_wR_factor_ref 0.0705
_reflns_number_gt 1923
_reflns_number_total 1969
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5706sup1.cif
_cod_data_source_block 1
_cod_database_code 2022988
_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 0.448
_shelx_estimated_absorpt_t_max 0.827
_shelx_hkl_file
;
1 0 0 0.10 0.10
1 0 0 -0.70 1.40
1 0 0 0.10 0.10
-1 0 0 0.10 0.10
-2 0 0 360.96 13.00
2 0 0 373.36 15.60
3 0 0 0.00 0.10
-3 0 0 0.00 0.20
-3 0 0 -0.10 0.30
-3 0 0 0.00 0.10
3 0 0 0.10 2.80
3 0 0 0.00 0.10
3 0 0 0.00 0.10
3 0 0 0.00 0.20
4 0 0 2209.88 81.09
5 0 0 0.00 0.10
-5 0 0 -0.10 0.50
-5 0 0 0.20 0.30
5 0 0 -2.50 5.20
5 0 0 0.00 0.10
6 0 0 725.33 32.60
-6 0 0 737.73 26.70
6 0 0 760.12 26.80
7 0 0 0.00 0.10
-7 0 0 -0.40 0.50
-7 0 0 0.20 1.00
7 0 0 0.90 0.70
7 0 0 0.10 0.10
7 0 0 0.00 0.10
-8 0 0 205.18 7.30
8 0 0 220.18 26.20
-8 0 0 221.78 8.40
-8 0 0 193.58 7.40
8 0 0 214.38 7.30
8 0 0 198.88 7.30
-8 0 0 215.88 7.30
-8 0 0 180.48 7.30
-9 0 0 0.00 0.10
9 0 0 0.00 0.10
9 0 0 0.00 0.10
-9 0 0 0.00 0.10
-9 0 0 0.10 0.10
-10 0 0 309.67 11.30
10 0 0 319.57 11.30
-10 0 0 334.47 11.60
-10 0 0 301.67 11.50
10 0 0 329.77 11.30
-11 0 0 0.10 0.10
11 0 0 0.00 0.10
-12 0 0 0.70 0.20
-13 0 0 0.00 0.10
0 -1 0 0.10 0.10
0 1 0 -0.10 0.10
1 1 0 0.00 0.10
-1 1 0 0.00 0.10
1 1 0 -0.30 1.00
-1 -1 0 0.10 0.10
1 -1 0 0.10 0.10
1 1 0 0.10 0.10
-1 1 0 0.30 0.10
2 1 0 1306.07 48.70
-2 1 0 1364.46 47.30
2 -1 0 1348.27 49.10
3 -1 0 -4.20 3.90
3 1 0 0.00 0.10
-3 -1 0 -0.50 0.30
-3 -1 0 0.00 0.20
3 1 0 0.10 0.20
3 -1 0 0.00 0.10
3 -1 0 0.10 0.10
3 -1 0 0.00 0.20
3 1 0 0.00 0.10
-3 1 0 0.10 0.20
-3 1 0 0.00 0.10
3 1 0 0.30 2.80
3 1 0 0.00 0.10
-4 1 0 165.28 6.30
-4 -1 0 173.08 6.40
4 1 0 168.58 6.30
-4 -1 0 161.58 6.30
-4 1 0 178.98 6.50
4 -1 0 172.58 6.40
-5 -1 0 -0.10 0.30
5 -1 0 0.10 0.10
5 1 0 0.00 0.10
-5 -1 0 0.10 0.60
-5 1 0 0.30 0.30
-5 1 0 0.10 0.10
5 -1 0 0.00 0.10
-5 -1 0 0.00 0.10
-5 1 0 0.00 0.50
5 1 0 0.10 0.10
5 1 0 -4.00 4.40
5 -1 0 0.30 6.50
5 1 0 0.00 0.20
5 -1 0 -0.10 0.20
6 1 0 128.39 5.00
6 -1 0 133.79 5.10
6 -1 0 123.39 4.40
-6 -1 0 118.89 4.40
6 1 0 118.59 4.40
6 -1 0 118.99 4.40
-6 1 0 112.29 4.50
6 1 0 124.99 12.60
6 1 0 119.49 4.40
-6 -1 0 127.89 5.20
6 -1 0 142.49 15.00
-6 1 0 130.19 5.20
-6 -1 0 124.39 5.00
-6 1 0 123.09 5.00
-7 1 0 0.00 0.10
-7 1 0 0.10 0.10
7 -1 0 0.10 0.10
-7 -1 0 0.40 0.60
-7 1 0 0.90 0.90
7 1 0 0.00 0.10
-7 -1 0 0.00 1.00
7 1 0 0.10 0.10
7 -1 0 -0.10 0.20
-7 1 0 0.10 0.10
7 1 0 -2.40 8.60
7 -1 0 0.00 0.50
7 1 0 -0.20 0.30
-7 -1 0 0.00 0.10
-8 1 0 1233.78 40.80
8 -1 0 1156.88 53.79
-8 1 0 997.60 39.60
8 1 0 1124.59 51.39
9 1 0 0.10 0.10
-9 1 0 0.00 0.10
9 1 0 -1.70 24.70
9 -1 0 0.10 0.10
-9 -1 0 0.00 0.10
-9 -1 0 0.00 0.10
9 1 0 0.20 0.10
-9 -1 0 0.10 0.10
-9 1 0 0.00 0.10
9 -1 0 0.10 0.10
10 1 0 5.20 0.30
-10 -1 0 4.40 0.40
10 1 0 3.90 0.20
10 -1 0 4.00 0.30
-10 1 0 4.70 0.30
10 -1 0 4.90 0.30
-10 1 0 4.70 0.40
-11 -1 0 0.00 0.10
-11 1 0 0.00 0.10
11 -1 0 0.00 0.10
-11 1 0 0.10 0.10
-12 -1 0 69.69 2.50
-12 1 0 68.79 2.50
-13 1 0 0.00 0.10
-13 -1 0 0.10 0.10
-1 2 0 0.00 0.10
1 2 0 -0.40 1.50
-1 2 0 0.10 0.10
-1 2 0 0.10 0.10
1 2 0 0.00 0.10
1 -2 0 0.10 0.10
1 2 0 0.10 0.10
1 2 0 0.10 0.10
1 2 0 0.30 0.10
-1 2 0 0.20 0.20
1 -2 0 0.00 0.10
2 2 0 2608.44 95.29
2 -2 0 2743.73 95.99
-2 -2 0 2626.74 93.69
3 -2 0 0.00 0.20
3 2 0 0.10 0.10
-3 -2 0 0.20 0.10
-3 -2 0 0.00 0.40
3 -2 0 3.90 4.30
3 2 0 0.10 0.10
-3 -2 0 0.10 0.20
-3 2 0 0.10 0.10
3 2 0 0.10 0.20
3 2 0 0.20 0.10
-3 2 0 0.00 0.20
4 2 0 66.69 2.40
4 -2 0 69.19 2.40
-4 -2 0 60.29 2.70
4 -2 0 69.29 2.30
-4 2 0 63.59 2.40
4 2 0 72.09 2.40
4 2 0 62.09 2.70
-4 2 0 62.69 2.80
-4 2 0 67.09 2.80
4 2 0 47.40 6.50
-4 -2 0 69.69 2.40
-4 -2 0 64.69 2.80
4 -2 0 63.49 2.70
-5 2 0 -0.70 0.50
-5 2 0 0.50 0.40
-5 -2 0 0.10 0.10
5 2 0 2.40 4.70
5 2 0 0.10 0.20
5 -2 0 0.20 0.30
-5 -2 0 0.00 0.30
5 -2 0 0.20 0.10
-5 -2 0 -0.10 0.60
5 2 0 0.40 0.10
-6 2 0 595.64 22.10
6 2 0 626.64 21.90
-6 -2 0 602.44 22.10
-6 2 0 632.74 22.50
6 -2 0 577.24 21.20
-6 -2 0 591.74 21.80
6 2 0 584.14 27.80
-7 2 0 0.10 0.90
7 -2 0 0.10 0.10
-7 -2 0 0.00 0.10
-7 2 0 0.10 0.10
-7 -2 0 0.40 0.60
7 2 0 0.00 0.10
7 2 0 -3.90 8.90
-7 2 0 0.20 0.10
7 -2 0 12.90 13.90
7 2 0 0.10 0.10
-8 2 0 246.48 9.30
8 2 0 246.48 8.40
8 2 0 256.27 31.10
8 2 0 232.68 8.50
-8 -2 0 255.37 9.70
-8 2 0 228.68 8.60
8 2 0 232.88 8.40
-8 -2 0 242.88 8.50
-8 2 0 237.68 8.40
8 -2 0 227.68 8.50
-8 -2 0 235.48 8.50
-8 2 0 229.78 8.50
8 -2 0 241.58 8.50
-9 2 0 2.40 2.30
-9 2 0 1.50 0.30
9 2 0 24.00 21.00
10 -2 0 148.99 5.20
10 2 0 148.39 5.10
-10 -2 0 140.39 5.20
-10 2 0 131.99 5.30
-10 2 0 150.38 5.20
10 -2 0 136.99 5.10
-10 -2 0 132.89 5.30
-11 2 0 0.00 0.10
-11 -2 0 0.00 0.10
11 -2 0 0.10 0.10
-11 2 0 0.00 0.10
-11 2 0 0.00 0.10
-12 -2 0 2.20 0.20
-12 2 0 2.10 0.20
0 3 0 0.00 0.10
0 3 0 0.10 0.10
0 3 0 0.10 0.30
0 -3 0 0.10 0.20
0 3 0 0.00 0.10
0 -3 0 0.00 0.10
-1 3 0 0.70 0.30
-1 -3 0 0.10 0.20
-1 -3 0 0.00 0.10
1 3 0 0.20 0.10
1 -3 0 0.10 0.10
-1 3 0 0.30 0.20
-1 -3 0 -0.60 0.50
1 3 0 0.00 0.20
-1 3 0 0.10 0.10
1 3 0 0.40 1.70
-1 3 0 0.00 0.10
1 3 0 0.10 0.10
1 -3 0 0.20 0.20
2 3 0 5657.13 198.38
-2 -3 0 5495.75 196.28
3 3 0 0.20 0.20
-3 3 0 0.40 0.40
3 -3 0 -8.70 6.00
3 -3 0 1.10 0.30
3 3 0 9.40 3.10
3 3 0 0.10 0.10
-3 3 0 0.20 0.30
-3 -3 0 0.30 0.20
4 3 0 127.59 5.00
4 3 0 116.39 8.60
4 -3 0 126.69 4.90
-4 3 0 125.49 5.00
-4 -3 0 135.99 4.50
-4 -3 0 117.99 4.90
-4 3 0 124.99 4.90
-4 -3 0 130.09 4.90
5 3 0 0.00 0.10
5 3 0 0.10 0.10
5 3 0 0.20 0.30
-5 3 0 0.10 0.30
5 3 0 -2.20 4.70
5 -3 0 -0.20 0.30
5 -3 0 0.00 0.10
-5 -3 0 -0.10 0.30
-5 3 0 0.00 0.50
-5 3 0 0.00 0.10
-5 -3 0 0.00 0.10
5 3 0 0.10 0.10
-5 3 0 0.10 0.10
6 -3 0 429.46 16.20
6 -3 0 363.36 26.70
6 3 0 477.85 26.00
-6 -3 0 459.65 16.30
-6 3 0 427.86 15.90
7 3 0 7.80 9.20
-7 3 0 -0.30 0.80
-7 3 0 0.70 0.20
8 3 0 231.18 25.10
8 -3 0 244.98 8.90
-8 3 0 254.07 8.90
-8 -3 0 225.58 8.90
8 -3 0 265.47 9.00
8 3 0 248.28 8.90
8 3 0 244.68 8.90
8 3 0 266.07 8.90
-8 3 0 228.18 8.90
-8 3 0 277.27 9.10
-8 -3 0 248.88 8.90
9 -3 0 0.00 0.10
9 3 0 0.00 0.10
9 -3 0 0.00 0.10
-9 -3 0 0.10 0.10
-9 -3 0 0.10 0.10
-9 3 0 -2.40 2.20
9 3 0 0.10 0.10
-9 3 0 0.10 0.10
-9 3 0 0.00 0.10
10 3 0 4.80 0.30
10 -3 0 3.60 0.20
-10 -3 0 3.80 0.30
-11 3 0 0.00 0.10
11 3 0 -0.10 0.10
-11 3 0 0.10 0.10
11 -3 0 0.00 0.10
-12 3 0 37.40 1.40
-1 4 0 0.10 0.10
-1 4 0 -0.50 0.30
-1 4 0 0.00 0.10
-1 4 0 0.00 0.10
1 4 0 0.20 0.30
1 4 0 0.00 0.10
1 4 0 0.10 0.10
-1 4 0 0.00 0.20
1 -4 0 0.00 0.20
-1 -4 0 0.40 0.20
2 -4 0 77.89 2.70
-2 4 0 75.09 3.00
2 4 0 68.19 6.10
2 -4 0 78.49 3.00
2 -4 0 63.99 10.70
-2 4 0 71.49 2.70
-2 4 0 72.79 3.00
-2 4 0 75.49 2.70
2 4 0 72.79 3.00
2 4 0 74.79 2.70
-2 -4 0 74.29 2.70
2 4 0 75.39 2.70
-2 -4 0 80.79 2.90
3 4 0 2.80 3.40
-3 -4 0 0.20 0.20
-3 4 0 0.30 0.40
-3 4 0 0.10 0.10
-3 -4 0 0.20 0.70
3 -4 0 -0.10 0.20
-3 4 0 0.20 0.20
3 4 0 -0.10 0.20
4 4 0 2822.02 103.79
-4 4 0 2837.22 99.99
-5 -4 0 0.20 0.30
-5 4 0 0.10 0.10
5 -4 0 0.10 0.30
-5 -4 0 0.30 0.10
5 -4 0 0.20 0.10
-5 4 0 0.10 0.30
5 4 0 -6.80 8.40
5 4 0 0.90 0.40
5 4 0 0.10 0.10
-6 4 0 592.94 19.00
-6 4 0 518.25 19.70
-6 -4 0 529.65 20.00
6 -4 0 514.45 20.20
6 4 0 542.85 26.30
7 4 0 11.70 9.80
-7 4 0 -0.40 0.90
8 4 0 40.30 14.10
9 4 0 37.90 34.40
-10 -4 0 17.60 0.80
-10 4 0 18.00 0.80
10 -4 0 20.80 0.80
-11 -4 0 0.00 0.10
11 4 0 0.10 0.10
11 -4 0 0.20 0.10
-11 4 0 0.00 0.10
12 4 0 0.80 0.10
-12 -4 0 1.00 0.20
-12 4 0 1.00 0.10
-12 4 0 0.80 0.10
0 5 0 0.10 0.10
0 -5 0 0.20 0.20
0 5 0 0.50 0.40
0 -5 0 0.10 0.20
0 -5 0 0.20 0.10
-1 -5 0 0.30 0.20
-1 5 0 -0.10 0.40
-1 5 0 0.10 0.10
1 5 0 0.10 0.10
-1 -5 0 0.00 0.20
1 5 0 0.30 0.40
1 5 0 0.20 0.10
-1 5 0 0.10 0.10
1 5 0 0.10 0.10
-1 5 0 0.10 0.10
1 -5 0 0.10 0.10
-1 -5 0 0.10 0.10
-1 5 0 0.10 0.10
1 -5 0 -0.10 0.20
1 5 0 0.10 0.10
-1 5 0 0.10 0.20
-2 5 0 72.69 3.00
2 5 0 71.19 2.60
-2 5 0 73.99 3.10
-2 -5 0 77.79 2.60
2 5 0 65.09 6.70
2 -5 0 76.09 3.10
2 -5 0 102.39 14.50
2 -5 0 74.29 2.60
-2 5 0 72.79 2.70
2 5 0 74.19 2.70
-2 5 0 75.19 2.70
-2 5 0 73.59 2.60
2 5 0 74.49 2.60
3 5 0 4.40 3.70
3 5 0 1.20 0.30
3 -5 0 4.80 11.50
4 -5 0 2308.87 93.79
-4 5 0 2430.66 86.69
4 5 0 2616.24 95.99
5 -5 0 0.10 0.40
-5 -5 0 0.00 0.40
5 5 0 0.20 0.10
5 -5 0 0.10 0.10
-5 5 0 0.60 0.60
5 5 0 -0.10 0.30
5 5 0 1.50 5.80
-6 5 0 554.34 20.00
6 5 0 577.74 28.20
-6 5 0 575.14 20.00
6 5 0 574.84 20.10
-6 5 0 550.54 20.70
6 -5 0 609.14 20.30
6 5 0 541.05 20.10
-7 5 0 0.00 0.10
7 5 0 0.10 0.10
-7 5 0 0.90 1.00
7 5 0 0.00 0.10
7 5 0 0.20 0.10
-7 -5 0 0.10 0.10
7 -5 0 0.00 0.10
7 5 0 0.10 0.10
7 -5 0 0.20 0.10
7 5 0 -7.40 16.30
8 -5 0 104.49 3.80
8 5 0 114.09 3.80
8 5 0 101.79 3.80
-8 -5 0 102.09 3.80
8 -5 0 113.59 3.90
-8 5 0 109.29 3.80
-8 5 0 96.29 3.80
8 5 0 104.99 3.80
-8 5 0 104.59 3.80
8 5 0 115.39 23.10
9 5 0 -0.10 0.10
-9 -5 0 0.00 0.10
-9 5 0 0.00 0.10
-9 -5 0 0.20 0.20
-9 5 0 -0.20 1.50
9 -5 0 -0.10 0.10
-9 5 0 0.10 0.10
-9 5 0 0.00 0.10
9 -5 0 0.00 0.10
9 5 0 -4.30 20.00
9 5 0 0.10 0.10
10 5 0 0.30 0.10
-10 5 0 0.10 0.10
-10 -5 0 -0.10 0.10
10 -5 0 0.10 0.10
11 -5 0 0.00 0.10
-11 -5 0 -0.10 0.10
11 5 0 0.10 0.10
-11 5 0 0.30 0.10
-12 5 0 12.60 0.50
-12 -5 0 13.50 0.60
0 -6 0 161.68 6.20
0 -6 0 160.38 6.10
0 6 0 160.78 6.20
0 -6 0 177.68 18.60
-1 -6 0 0.30 0.10
-1 -6 0 4.80 11.60
1 -6 0 0.70 12.80
-1 -6 0 -0.20 0.20
-1 6 0 0.10 0.10
-1 6 0 0.20 0.10
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3 -6 -15 2.70 0.10
3 -6 -15 2.50 0.20
3 6 15 2.50 0.20
-4 -6 -15 3.60 0.20
-4 -6 -15 3.70 0.20
4 6 -15 3.60 0.20
4 -6 -15 3.70 0.20
4 -6 -15 3.60 0.20
4 -6 -15 4.00 0.20
4 6 15 3.50 0.20
0 -7 -15 0.00 0.10
0 -7 -15 0.00 0.10
0 -7 -15 0.00 0.10
0 7 15 0.10 0.10
-1 7 15 16.80 0.70
-1 -7 -15 17.10 0.60
-1 -7 -15 16.10 0.60
-1 -7 -15 17.40 0.70
-1 -7 -15 17.50 0.60
1 7 15 16.30 0.70
1 -7 -15 17.60 0.60
1 -7 -15 15.60 0.60
-2 -7 -15 0.20 0.10
-2 -7 -15 0.20 0.10
-2 7 15 0.20 0.10
-2 -7 -15 0.30 0.10
-2 -7 -15 0.10 0.10
2 -7 -15 0.20 0.10
2 7 15 0.10 0.10
2 -7 -15 0.20 0.10
-3 -7 -15 0.50 0.10
-3 -7 -15 0.70 0.10
3 -7 -15 0.80 0.20
3 -7 -15 0.70 0.10
3 7 15 0.70 0.10
0 8 15 23.00 0.90
0 -8 -15 23.30 0.80
-1 8 15 0.60 0.10
-1 -8 -15 0.60 0.10
1 8 15 0.70 0.10
1 -8 -15 0.60 0.10
0 0 -16 29.10 1.10
0 0 -16 29.40 1.10
0 0 -16 28.60 1.10
0 0 -16 29.70 1.10
0 0 -16 28.90 1.10
-1 0 -16 25.40 0.90
1 0 -16 26.20 0.90
-1 0 -16 25.00 1.00
-1 0 -16 25.20 0.90
-1 0 -16 25.10 0.90
1 0 -16 25.90 1.00
-1 0 -16 24.80 1.00
1 0 -16 25.70 0.90
1 0 -16 24.70 1.00
-1 0 -16 24.20 0.90
1 0 -16 25.90 0.90
2 0 -16 73.99 2.70
-2 0 -16 72.69 2.70
2 0 -16 74.59 2.70
2 0 -16 75.79 2.70
2 0 -16 74.49 2.70
-2 0 -16 75.99 2.70
-2 0 -16 73.89 2.70
-2 0 -16 76.09 2.70
-2 0 -16 75.89 2.70
2 0 -16 73.59 2.70
2 0 -16 74.89 2.70
3 0 -16 3.60 0.20
-3 0 -16 3.40 0.20
-3 0 -16 3.60 0.20
3 0 -16 4.00 0.20
-3 0 -16 3.80 0.20
3 0 -16 3.70 0.20
3 0 -16 3.40 0.20
-3 0 -16 4.10 0.20
-4 0 -16 54.89 2.00
4 0 -16 56.59 2.00
-4 0 -16 55.69 2.00
-4 0 -16 56.99 2.00
4 0 -16 59.99 2.10
4 0 -16 55.29 2.00
-4 0 -16 55.69 2.00
4 0 -16 55.59 2.00
0 1 -16 0.00 0.10
0 1 -16 0.10 0.10
0 -1 -16 0.00 0.10
0 1 -16 0.00 0.10
0 -1 -16 0.20 0.10
0 -1 -16 0.00 0.10
0 -1 -16 0.10 0.10
0 -1 -16 0.10 0.10
0 1 -16 -0.10 0.10
0 1 -16 0.00 0.10
-1 -1 -16 7.20 0.30
-1 -1 -16 6.50 0.30
-1 -1 -16 7.00 0.30
1 1 -16 6.30 0.30
1 1 -16 7.00 0.30
1 1 -16 7.20 0.30
-1 -1 -16 6.10 0.30
1 1 -16 6.20 0.30
-1 -1 -16 6.10 0.30
-1 1 -16 6.30 0.30
-1 1 -16 5.80 0.30
1 -1 -16 7.00 0.30
-1 1 -16 5.80 0.30
-1 1 -16 6.70 0.30
1 -1 -16 7.10 0.30
-1 1 -16 7.60 0.30
1 -1 -16 6.00 0.30
1 -1 -16 6.40 0.30
2 1 -16 198.48 7.10
-2 -1 -16 188.78 7.00
-2 -1 -16 198.78 7.00
-2 -1 -16 200.98 7.00
-2 -1 -16 193.58 7.00
2 1 -16 199.68 7.00
2 1 -16 203.48 7.00
-2 -1 -16 198.08 7.10
-2 -1 -16 195.48 7.10
2 1 -16 197.88 7.10
2 1 -16 198.08 7.00
2 1 -16 193.08 7.00
-2 1 -16 197.58 7.00
2 -1 -16 198.28 7.00
-2 1 -16 204.88 7.10
-2 1 -16 203.98 7.00
2 -1 -16 195.38 7.10
2 -1 -16 205.38 7.10
-2 1 -16 188.88 7.00
-2 1 -16 200.98 7.10
2 -1 -16 203.18 7.00
2 -1 -16 197.18 7.00
2 -1 -16 202.08 7.10
3 1 -16 48.60 1.70
-3 -1 -16 48.80 1.70
3 1 -16 49.70 1.80
-3 -1 -16 48.00 1.70
-3 -1 -16 48.70 1.80
3 1 -16 46.30 1.80
3 1 -16 49.30 1.70
3 1 -16 47.50 1.80
-3 -1 -16 49.70 1.80
3 -1 -16 50.39 1.80
-3 1 -16 48.10 1.70
-3 1 -16 48.70 1.80
3 -1 -16 47.90 1.70
3 -1 -16 49.30 1.70
-3 1 -16 44.80 1.70
-3 1 -16 49.10 1.70
-3 1 -16 46.50 1.70
3 -1 -16 45.70 1.80
-3 1 -16 47.10 1.80
3 -1 -16 49.70 1.70
-4 -1 -16 38.70 1.40
4 1 -16 37.80 1.40
4 1 -16 37.50 1.40
-4 -1 -16 38.10 1.40
4 1 -16 38.40 1.40
-4 -1 -16 37.50 1.40
-4 -1 -16 36.90 1.40
-4 -1 -16 38.50 1.40
4 1 -16 38.30 1.40
4 -1 -16 38.80 1.40
-4 1 -16 37.30 1.40
4 -1 -16 39.00 1.40
-4 1 -16 38.30 1.40
4 -1 -16 37.40 1.40
-4 1 -16 37.20 1.40
-4 1 -16 34.60 1.40
-4 1 -16 38.30 1.40
4 -1 -16 38.20 1.40
0 -2 -16 144.09 5.10
0 2 -16 144.69 5.10
0 2 -16 143.49 5.20
0 -2 -16 146.99 5.20
0 -2 -16 147.29 5.10
0 -2 -16 142.79 5.20
0 2 -16 145.49 5.10
0 2 -16 142.39 5.10
0 2 -16 142.89 5.10
0 -2 -16 146.39 5.10
1 2 -16 88.69 3.10
1 2 -16 84.09 3.20
-1 -2 -16 88.59 3.10
1 2 -16 90.69 3.20
-1 -2 -16 86.39 3.20
-1 -2 -16 89.09 3.10
-1 -2 -16 89.99 3.10
-1 -2 -16 88.79 3.20
1 2 -16 88.29 3.10
-1 -2 -16 86.09 3.20
1 2 -16 83.49 3.10
1 -2 -16 90.09 3.10
1 -2 -16 88.79 3.10
-1 2 -16 88.79 3.20
-1 2 -16 87.29 3.10
1 -2 -16 88.39 3.20
-1 2 -16 87.19 3.10
1 -2 -16 88.89 3.10
1 -2 -16 88.19 3.20
-1 2 -16 88.89 3.20
2 2 -16 7.90 0.40
-2 -2 -16 9.50 0.40
-2 -2 -16 8.80 0.40
-2 -2 -16 9.30 0.40
2 2 -16 9.10 0.40
2 2 -16 9.40 0.40
-2 -2 -16 8.90 0.40
-2 -2 -16 9.20 0.40
2 2 -16 9.30 0.40
-2 -2 -16 9.30 0.40
2 -2 -16 9.00 0.40
-2 2 -16 9.60 0.40
-2 2 -16 7.90 0.40
2 -2 -16 9.00 0.40
2 -2 -16 9.40 0.40
2 -2 -16 9.30 0.40
2 -2 -16 8.60 0.40
-2 2 -16 9.00 0.40
-2 2 -16 9.30 0.40
2 -2 -16 9.20 0.40
-2 2 -16 9.10 0.40
3 2 -16 1.40 0.20
-3 -2 -16 1.10 0.20
-3 -2 -16 1.40 0.10
3 2 -16 1.40 0.10
-3 -2 -16 1.00 0.10
3 2 -16 0.90 0.10
3 2 -16 1.30 0.10
-3 -2 -16 1.40 0.10
-3 2 -16 1.10 0.10
-3 2 -16 1.40 0.10
3 -2 -16 1.00 0.10
3 -2 -16 1.30 0.10
3 -2 -16 1.10 0.10
-3 2 -16 1.40 0.10
-3 2 -16 1.20 0.10
3 -2 -16 0.80 0.10
4 2 -16 43.50 1.50
-4 -2 -16 43.60 1.50
-4 -2 -16 40.40 1.60
-4 -2 -16 43.00 1.50
4 2 -16 40.70 1.60
4 2 -16 45.80 1.60
-4 -2 -16 43.40 1.60
-4 -2 -16 41.80 1.50
-4 2 -16 44.30 1.50
-4 2 -16 41.30 1.50
4 -2 -16 44.10 1.50
-4 2 -16 41.70 1.60
4 -2 -16 45.40 1.60
4 -2 -16 43.00 1.50
4 -2 -16 42.10 1.60
-4 2 -16 42.70 1.60
0 3 -16 0.10 0.10
0 3 -16 0.00 0.10
0 -3 -16 0.00 0.10
0 -3 -16 0.10 0.10
0 -3 -16 0.10 0.10
0 -3 -16 0.00 0.10
0 -3 -16 0.00 0.10
0 3 -16 0.00 0.10
1 3 -16 1.70 0.20
-1 -3 -16 1.60 0.10
1 3 -16 1.40 0.10
-1 -3 -16 1.40 0.20
-1 -3 -16 1.60 0.10
-1 -3 -16 1.60 0.10
1 3 -16 1.60 0.10
-1 -3 -16 1.80 0.20
1 3 -16 1.80 0.10
1 -3 -16 1.40 0.10
-1 3 -16 1.70 0.10
1 -3 -16 1.60 0.10
1 -3 -16 1.40 0.20
-1 3 -16 1.80 0.10
-1 3 -16 1.60 0.10
1 -3 -16 1.70 0.10
1 -3 -16 1.80 0.20
2 3 -16 167.18 6.20
-2 -3 -16 173.28 6.20
2 3 -16 179.68 6.20
2 3 -16 173.78 6.20
-2 -3 -16 168.58 6.20
-2 -3 -16 176.98 6.20
2 3 -16 170.68 6.20
-2 -3 -16 175.08 6.20
-2 -3 -16 188.78 6.20
-2 -3 -16 178.38 6.20
2 -3 -16 182.78 6.20
-2 3 -16 168.38 6.20
-2 3 -16 171.88 6.20
2 -3 -16 177.28 6.20
2 -3 -16 175.08 6.30
-2 3 -16 171.18 6.20
2 -3 -16 172.68 6.20
2 -3 -16 178.58 6.20
2 -3 -16 176.48 6.20
-3 -3 -16 22.90 0.90
3 3 -16 22.90 0.80
3 3 -16 22.40 0.90
-3 -3 -16 22.70 0.80
-3 -3 -16 21.70 0.80
3 3 -16 23.30 0.80
-3 -3 -16 22.90 0.80
-3 -3 -16 23.20 0.90
3 -3 -16 22.30 0.80
3 -3 -16 22.90 0.90
-3 3 -16 21.70 0.80
3 -3 -16 22.10 0.90
3 -3 -16 22.80 0.90
3 -3 -16 23.70 0.80
-3 3 -16 21.20 0.80
4 3 -16 64.89 2.20
-4 -3 -16 62.89 2.20
-4 -3 -16 62.09 2.30
-4 -3 -16 64.69 2.20
-4 -3 -16 63.09 2.20
-4 -3 -16 62.39 2.30
4 3 -16 63.19 2.30
4 3 -16 62.29 2.40
-4 3 -16 57.19 2.20
4 -3 -16 63.09 2.20
4 -3 -16 62.89 2.20
-4 3 -16 62.19 2.20
4 -3 -16 63.99 2.30
4 -3 -16 64.89 2.30
0 -4 -16 86.49 3.00
0 -4 -16 86.59 3.10
0 -4 -16 85.19 3.00
0 -4 -16 85.49 3.10
0 -4 -16 85.29 3.00
0 4 -16 81.59 3.00
1 4 -16 13.00 0.60
-1 -4 -16 13.60 0.60
1 4 -16 14.00 0.50
-1 -4 -16 14.30 0.60
-1 -4 -16 14.40 0.50
-1 -4 -16 13.40 0.50
-1 -4 -16 14.30 0.50
1 -4 -16 14.20 0.50
1 -4 -16 13.80 0.50
1 -4 -16 14.90 0.60
1 -4 -16 13.70 0.60
1 -4 -16 13.40 0.50
-2 -4 -16 32.10 1.20
2 4 -16 27.90 1.10
2 4 -16 31.00 1.10
-2 -4 -16 30.80 1.10
-2 -4 -16 30.90 1.10
-2 -4 -16 31.10 1.10
-2 -4 -16 30.40 1.10
2 -4 -16 31.00 1.20
2 -4 -16 29.60 1.10
2 -4 -16 29.40 1.10
2 -4 -16 30.10 1.10
3 4 -16 20.60 0.80
3 4 -16 22.90 0.80
-3 -4 -16 21.80 0.80
-3 -4 -16 20.50 0.80
-3 -4 -16 21.30 0.80
-3 -4 -16 21.40 0.80
-3 -4 -16 21.80 0.80
3 -4 -16 20.20 0.90
3 -4 -16 20.90 0.80
3 -4 -16 21.30 0.80
3 -4 -16 21.90 0.80
3 -4 -16 20.20 0.80
0 -5 -16 0.00 0.10
0 -5 -16 0.10 0.10
0 -5 -16 0.20 0.10
0 -5 -16 0.10 0.10
0 -5 -16 0.10 0.10
-1 -5 -16 2.60 0.20
-1 -5 -16 2.60 0.10
-1 -5 -16 2.60 0.20
-1 -5 -16 2.50 0.10
-1 -5 -16 2.40 0.10
1 -5 -16 2.60 0.20
1 -5 -16 2.50 0.10
1 -5 -16 2.60 0.10
1 -5 -16 2.60 0.20
1 -5 -16 2.40 0.10
-2 -5 -16 87.69 3.10
-2 -5 -16 85.39 3.00
-2 -5 -16 84.59 3.00
-2 -5 -16 85.99 3.10
2 -5 -16 84.99 3.10
2 -5 -16 88.19 3.00
2 -5 -16 83.29 3.00
0 -6 -16 275.37 9.70
0 0 -17 0.00 0.10
0 0 -17 0.00 0.10
0 0 -17 0.10 0.10
0 0 -17 0.00 0.10
-1 0 -17 0.00 0.10
1 0 -17 0.00 0.10
-1 0 -17 0.10 0.10
-1 0 -17 0.00 0.10
1 0 -17 0.00 0.10
1 0 -17 -0.10 0.10
1 0 -17 0.00 0.10
-1 0 -17 0.00 0.10
0 1 -17 0.00 0.10
0 1 -17 0.00 0.10
0 -1 -17 0.00 0.10
0 -1 -17 0.00 0.10
0 -1 -17 0.10 0.10
0 -1 -17 0.00 0.10
0 1 -17 0.00 0.10
1 1 -17 2.40 0.10
1 1 -17 2.60 0.10
-1 -1 -17 2.40 0.20
1 1 -17 2.40 0.10
-1 -1 -17 2.50 0.20
-1 -1 -17 2.40 0.10
-1 -1 -17 2.40 0.10
1 -1 -17 2.40 0.10
1 -1 -17 2.50 0.10
1 -1 -17 2.50 0.10
-1 1 -17 2.50 0.10
1 -1 -17 2.50 0.20
1 -1 -17 2.40 0.10
-1 1 -17 2.50 0.10
0 2 -17 16.10 0.60
0 -2 -17 15.90 0.60
0 -2 -17 16.40 0.60
0 -2 -17 16.30 0.60
0 -2 -17 16.50 0.60
0 -2 -17 16.20 0.60
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 51253
_shelx_res_file
;
TITL saba3 lowtemp data morpholinium Iminium disordered PF6
saba3lowT.res
created by SHELXL-2018/3 at 21:30:02 on 06-Sep-2023
CELL 1.54178 10.4638 13.4495 13.7340 90.000 90.000 90.000
ZERR 8.000 0.0003 0.0004 0.0004 0.000 0.000 0.000
LATT 1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC O N C H P F
UNIT 8 16 40 88 8 48
L.S. 20
ACTA
BOND $H
EQIV $1 1/2-x,1.0-y,1/2+z
EQIV $2 x,1.5-y,1/2+z
EQIV $3 x-1/2,3/2-y,1.0-z
EQIV $4 x-1/2,y,3/2-z
EQIV $5 1/2-x, 1/2+y,z
SIZE 0.06 0.09 0.29
TEMP -143.150
HTAB
HTAB C2 F4B_$1
HTAB C2 F3A_$2
HTAB C3 F6B_$2
HTAB C5 F4B
HTAB C7 F2A_$3
HTAB C7 F1A
HTAB N8 F3A_$2
HTAB N8 F5A_$4
HTAB N8 F3B_$2
HTAB N8 F5B_$4
HTAB N8 O4_$5
MPLA 5 C7 N8 N1 C2 C6 C3 C5 O4
MPLA 3 N1 N8 C7 H7 H8A H8B
MPLA 6 N1 C7 H7 N8 H8A H8B
MPLA 3 C2 N1 C6 C7 N8 C3 C5 O4
MPLA 4 C2 C6 C3 C5 N1 O4
MPLA 3 C3 C5 O4 C2 C6 N1
FMAP 2
PLAN 20
WGHT 0.037300 0.517000
EXTI 0.000525
FVAR 0.32266 0.87035
N1 2 0.172298 0.558594 0.732563 11.00000 0.02247 0.01780 =
0.01786 -0.00064 -0.00100 -0.00029
C2 3 0.201872 0.511752 0.826404 11.00000 0.02459 0.01768 =
0.01866 0.00302 0.00133 -0.00037
AFIX 23
H2A 4 0.152903 0.449208 0.833665 11.00000 -1.50000
H2B 4 0.178416 0.556828 0.880516 11.00000 -1.50000
AFIX 0
C3 3 0.344496 0.490227 0.828737 11.00000 0.02469 0.02015 =
0.02126 -0.00003 -0.00034 0.00141
AFIX 23
H3A 4 0.392565 0.553533 0.825341 11.00000 -1.50000
H3B 4 0.366643 0.456964 0.890787 11.00000 -1.50000
AFIX 0
O4 1 0.380477 0.427873 0.748774 11.00000 0.03169 0.01886 =
0.02541 0.00057 0.00320 0.00591
C5 3 0.348960 0.472364 0.656810 11.00000 0.03711 0.02498 =
0.02146 -0.00005 0.00641 0.00688
AFIX 23
H5A 4 0.373554 0.426656 0.603505 11.00000 -1.50000
H5B 4 0.398048 0.534754 0.648785 11.00000 -1.50000
AFIX 0
C6 3 0.206843 0.494848 0.649958 11.00000 0.03670 0.02305 =
0.01999 -0.00505 -0.00265 0.00155
AFIX 23
H6A 4 0.157068 0.432289 0.652136 11.00000 -1.50000
H6B 4 0.187731 0.529177 0.587877 11.00000 -1.50000
AFIX 0
C7 3 0.149034 0.653738 0.719863 11.00000 0.01691 0.02141 =
0.02122 0.00304 -0.00008 0.00027
H7 4 0.138724 0.677088 0.655388 11.00000 0.02317
N8 2 0.135760 0.719715 0.788455 11.00000 0.03300 0.01803 =
0.02457 0.00179 0.00196 0.00483
EADP H8A H8B
H8A 4 0.144212 0.705831 0.846778 11.00000 0.03482
H8B 4 0.120748 0.779953 0.773495 11.00000 0.03482
EXYZ P1A P1B
EADP P1A P1B
EXYZ F1A F1B
EADP F1A F1B
EXYZ F2A F2B
EADP F2A F2B
PART 1
P1A 5 0.399817 0.743600 0.498271 21.00000 0.01731 0.02057 =
0.01767 -0.00186 0.00018 -0.00065
F1A 6 0.367615 0.750616 0.611813 21.00000 0.03650 0.03499 =
0.01897 -0.00250 0.00226 0.00649
F2A 6 0.431719 0.735924 0.384606 21.00000 0.04087 0.04408 =
0.02015 -0.00295 0.00701 -0.00833
F3A 6 0.297131 0.828635 0.475419 21.00000 0.04628 0.03546 =
0.03287 0.00435 -0.00647 0.01838
F4A 6 0.290724 0.660659 0.485115 21.00000 0.03245 0.03998 =
0.03923 -0.01024 0.00662 -0.01872
F5A 6 0.501508 0.657035 0.522516 21.00000 0.03906 0.03888 =
0.03363 -0.00106 0.00173 0.01999
F6A 6 0.508094 0.824700 0.512966 21.00000 0.03849 0.04457 =
0.04231 -0.00698 -0.00002 -0.02294
PART 2
P1B 5 0.399817 0.743600 0.498271 -21.00000 0.01731 0.02057 =
0.01767 -0.00186 0.00018 -0.00065
F1B 6 0.367615 0.750616 0.611813 -21.00000 0.03650 0.03499 =
0.01897 -0.00250 0.00226 0.00649
F2B 6 0.431719 0.735924 0.384606 -21.00000 0.04087 0.04408 =
0.02015 -0.00295 0.00701 -0.00833
F3B 6 0.274262 0.807831 0.486552 -21.00000 0.02764
F4B 6 0.324924 0.648725 0.489790 -21.00000 0.02429
F5B 6 0.531363 0.689886 0.507746 -21.00000 0.02091
F6B 6 0.480880 0.850880 0.494555 -21.00000 0.02460
PART 0
HKLF 4
REM saba3 lowtemp data morpholinium Iminium disordered PF6
REM wR2 = 0.0705, GooF = S = 1.116, Restrained GooF = 1.116 for all data
REM R1 = 0.0251 for 1923 Fo > 4sig(Fo) and 0.0265 for all 1969 data
REM 165 parameters refined using 0 restraints
END
WGHT 0.0371 0.5211
REM Instructions for potential hydrogen bonds
HTAB C2 F4A_$1
HTAB C2 F4B_$1
HTAB C2 F3A_$2
HTAB C2 F3B_$2
HTAB C3 F4A_$1
EQIV $6 -x+1, y-1/2, -z+3/2
HTAB C3 F6A_$6
EQIV $7 -x+1, -y+1, -z+1
HTAB C5 F5A_$7
HTAB C5 F5B_$7
HTAB C5 F5A
EQIV $8 -x+1/2, y-1/2, z
HTAB C6 F1A_$8
HTAB C6 F4A
HTAB C6 F4B
HTAB C7 F2A_$3
HTAB N8 F3A_$2
HTAB N8 F5A_$4
HTAB N8 F3B_$2
HTAB N8 F5B_$4
HTAB N8 O4_$5
REM Highest difference peak 0.291, deepest hole -0.281, 1-sigma level 0.047
Q1 1 0.2740 0.4996 0.8274 11.00000 0.05 0.29
Q2 1 0.1775 0.5393 0.7818 11.00000 0.05 0.26
Q3 1 0.2778 0.4852 0.6547 11.00000 0.05 0.24
Q4 1 0.1833 0.5254 0.6935 11.00000 0.05 0.23
Q5 1 0.3600 0.4611 0.7844 11.00000 0.05 0.21
Q6 1 0.1875 0.5990 0.7307 11.00000 0.05 0.20
Q7 1 0.2669 0.7761 0.4568 11.00000 0.05 0.17
Q8 1 0.5622 0.7359 0.4997 11.00000 0.05 0.17
Q9 1 0.4549 0.6294 0.4919 11.00000 0.05 0.17
Q10 1 0.3619 0.4522 0.7079 11.00000 0.05 0.16
Q11 1 0.3569 0.7430 0.5668 11.00000 0.05 0.16
Q12 1 0.3292 0.7574 0.5710 11.00000 0.05 0.16
Q13 1 0.3525 0.8241 0.4872 11.00000 0.05 0.16
Q14 1 0.4257 0.7767 0.5982 11.00000 0.05 0.16
Q15 1 0.4494 0.4264 0.7487 11.00000 0.05 0.14
Q16 1 0.4622 0.8039 0.5039 11.00000 0.05 0.14
Q17 1 0.1768 0.5346 0.8728 11.00000 0.05 0.14
Q18 1 0.3391 0.3791 0.7551 11.00000 0.05 0.14
Q19 1 0.3300 0.6733 0.5185 11.00000 0.05 0.14
Q20 1 0.4476 0.8585 0.5155 11.00000 0.05 0.14
;
_shelx_res_checksum 42353
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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 N1 0.17230(9) 0.55859(6) 0.73256(6) 0.01938(19) Uani d 1 . .
C C2 0.20187(10) 0.51175(7) 0.82640(7) 0.0203(2) Uani d 1 . .
H H2A 0.152903 0.449208 0.833665 0.030 Uiso calc 1 . .
H H2B 0.178416 0.556828 0.880516 0.030 Uiso calc 1 . .
C C3 0.34450(10) 0.49023(8) 0.82874(8) 0.0220(2) Uani d 1 . .
H H3A 0.392565 0.553533 0.825341 0.033 Uiso calc 1 . .
H H3B 0.366643 0.456964 0.890787 0.033 Uiso calc 1 . .
O O4 0.38048(9) 0.42787(6) 0.74877(5) 0.02532(19) Uani d 1 . .
C C5 0.34896(11) 0.47236(9) 0.65681(8) 0.0279(3) Uani d 1 . .
H H5A 0.373554 0.426656 0.603505 0.042 Uiso calc 1 . .
H H5B 0.398048 0.534754 0.648785 0.042 Uiso calc 1 . .
C C6 0.20684(12) 0.49485(8) 0.64996(8) 0.0266(2) Uani d 1 . .
H H6A 0.157068 0.432289 0.652136 0.040 Uiso calc 1 . .
H H6B 0.187731 0.529177 0.587877 0.040 Uiso calc 1 . .
C C7 0.14903(9) 0.65374(8) 0.71986(8) 0.0198(2) Uani d 1 . .
H H7 0.1387(12) 0.6771(10) 0.6554(10) 0.023(3) Uiso d 1 . .
N N8 0.13576(10) 0.71972(7) 0.78845(7) 0.0252(2) Uani d 1 . .
H H8A 0.1442(14) 0.7058(12) 0.8468(13) 0.035(3) Uiso d 1 . .
H H8B 0.1207(16) 0.7800(13) 0.7735(12) 0.035(3) Uiso d 1 . .
P P1A 0.39982(2) 0.74360(2) 0.49827(2) 0.01852(12) Uani d 0.870(8) A 1
F F1A 0.36762(8) 0.75062(5) 0.61181(5) 0.03015(19) Uani d 0.870(8) A 1
F F2A 0.43172(8) 0.73592(6) 0.38461(5) 0.0350(2) Uani d 0.870(8) A 1
F F3A 0.2971(3) 0.82864(17) 0.47542(12) 0.0382(4) Uani d 0.870(8) A 1
F F4A 0.2907(2) 0.66066(17) 0.48512(12) 0.0372(4) Uani d 0.870(8) A 1
F F5A 0.5015(2) 0.65703(19) 0.52252(9) 0.0372(5) Uani d 0.870(8) A 1
F F6A 0.5081(2) 0.82470(19) 0.51297(13) 0.0418(5) Uani d 0.870(8) A 1
P P1B 0.39982(2) 0.74360(2) 0.49827(2) 0.01852(12) Uani d 0.130(8) A 2
F F1B 0.36762(8) 0.75062(5) 0.61181(5) 0.03015(19) Uani d 0.130(8) A 2
F F2B 0.43172(8) 0.73592(6) 0.38461(5) 0.0350(2) Uani d 0.130(8) A 2
F F3B 0.2743(11) 0.8078(9) 0.4866(8) 0.028(2) Uiso d 0.130(8) A 2
F F4B 0.3249(11) 0.6487(8) 0.4898(7) 0.024(2) Uiso d 0.130(8) A 2
F F5B 0.5314(7) 0.6899(8) 0.5077(6) 0.0209(18) Uiso d 0.130(8) A 2
F F6B 0.4809(8) 0.8509(7) 0.4946(6) 0.0246(19) Uiso d 0.130(8) A 2
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
N1 0.0225(4) 0.0178(4) 0.0179(4) -0.0003(3) -0.0010(3) -0.0006(3)
C2 0.0246(5) 0.0177(4) 0.0187(4) -0.0004(4) 0.0013(4) 0.0030(4)
C3 0.0247(5) 0.0201(5) 0.0213(5) 0.0014(4) -0.0003(4) 0.0000(4)
O4 0.0317(4) 0.0189(4) 0.0254(4) 0.0059(3) 0.0032(3) 0.0006(3)
C5 0.0371(6) 0.0250(5) 0.0215(5) 0.0069(4) 0.0064(4) 0.0000(4)
C6 0.0367(6) 0.0230(5) 0.0200(5) 0.0016(4) -0.0026(4) -0.0051(4)
C7 0.0169(5) 0.0214(5) 0.0212(5) 0.0003(4) -0.0001(4) 0.0030(4)
N8 0.0330(5) 0.0180(5) 0.0246(5) 0.0048(4) 0.0020(4) 0.0018(4)
P1A 0.01731(18) 0.02057(17) 0.01767(17) -0.00065(9) 0.00018(9) -0.00186(8)
F1A 0.0365(4) 0.0350(4) 0.0190(3) 0.0065(3) 0.0023(3) -0.0025(2)
F2A 0.0409(4) 0.0441(4) 0.0202(3) -0.0083(3) 0.0070(3) -0.0029(3)
F3A 0.0463(9) 0.0355(8) 0.0329(6) 0.0184(7) -0.0065(6) 0.0044(6)
F4A 0.0325(8) 0.0400(7) 0.0392(6) -0.0187(7) 0.0066(6) -0.0102(5)
F5A 0.0391(7) 0.0389(9) 0.0336(5) 0.0200(7) 0.0017(5) -0.0011(5)
F6A 0.0385(7) 0.0446(9) 0.0423(6) -0.0229(7) 0.0000(6) -0.0070(6)
P1B 0.01731(18) 0.02057(17) 0.01767(17) -0.00065(9) 0.00018(9) -0.00186(8)
F1B 0.0365(4) 0.0350(4) 0.0190(3) 0.0065(3) 0.0023(3) -0.0025(2)
F2B 0.0409(4) 0.0441(4) 0.0202(3) -0.0083(3) 0.0070(3) -0.0029(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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
C7 N1 C2 . . 125.00(9) ?
C7 N1 C6 . . 120.79(9) ?
C2 N1 C6 . . 112.10(8) ?
N1 C2 C3 . . 107.89(8) ?
N1 C2 H2A . . 110.1 ?
C3 C2 H2A . . 110.1 ?
N1 C2 H2B . . 110.1 ?
C3 C2 H2B . . 110.1 ?
H2A C2 H2B . . 108.4 ?
O4 C3 C2 . . 110.69(8) ?
O4 C3 H3A . . 109.5 ?
C2 C3 H3A . . 109.5 ?
O4 C3 H3B . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 108.1 ?
C5 O4 C3 . . 111.72(8) ?
O4 C5 C6 . . 111.22(9) ?
O4 C5 H5A . . 109.4 ?
C6 C5 H5A . . 109.4 ?
O4 C5 H5B . . 109.4 ?
C6 C5 H5B . . 109.4 ?
H5A C5 H5B . . 108.0 ?
C5 C6 N1 . . 108.02(9) ?
C5 C6 H6A . . 110.1 ?
N1 C6 H6A . . 110.1 ?
C5 C6 H6B . . 110.1 ?
N1 C6 H6B . . 110.1 ?
H6A C6 H6B . . 108.4 ?
N1 C7 N8 . . 125.98(10) ?
N1 C7 H7 . . 118.0(8) ?
N8 C7 H7 . . 116.0(8) ?
C7 N8 H8A . . 122.4(11) ?
C7 N8 H8B . . 119.6(11) ?
H8A N8 H8B . . 118.0(15) ?
F6A P1A F3A . . 90.75(9) ?
F6A P1A F4A . . 179.05(8) ?
F3A P1A F4A . . 89.83(10) ?
F6A P1A F5A . . 89.94(9) ?
F3A P1A F5A . . 179.02(8) ?
F4A P1A F5A . . 89.47(8) ?
F6A P1A F1A . . 89.19(6) ?
F3A P1A F1A . . 90.44(7) ?
F4A P1A F1A . . 90.05(6) ?
F5A P1A F1A . . 88.87(6) ?
F6A P1A F2A . . 91.12(6) ?
F3A P1A F2A . . 89.70(7) ?
F4A P1A F2A . . 89.64(6) ?
F5A P1A F2A . . 90.99(6) ?
F1A P1A F2A . . 179.66(4) ?
F4B P1B F3B . . 91.3(5) ?
F4B P1B F5B . . 94.2(4) ?
F3B P1B F5B . . 174.3(4) ?
F4B P1B F1B . . 90.9(4) ?
F3B P1B F1B . . 83.8(4) ?
F5B P1B F1B . . 97.6(3) ?
F4B P1B F2B . . 88.8(4) ?
F3B P1B F2B . . 96.3(4) ?
F5B P1B F2B . . 82.4(3) ?
F1B P1B F2B . . 179.66(4) ?
F4B P1B F6B . . 173.7(5) ?
F3B P1B F6B . . 87.0(4) ?
F5B P1B F6B . . 87.4(4) ?
F1B P1B F6B . . 94.9(3) ?
F2B P1B F6B . . 85.4(3) ?
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
N1 C7 . 1.3142(13) ?
N1 C2 . 1.4675(12) ?
N1 C6 . 1.4672(13) ?
C2 C3 . 1.5206(14) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 O4 . 1.4322(12) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
O4 C5 . 1.4360(13) ?
C5 C6 . 1.5204(16) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 N8 . 1.3016(15) ?
C7 H7 . 0.946(14) ?
N8 H8A . 0.827(18) ?
N8 H8B . 0.850(18) ?
P1A F6A . 1.5856(10) ?
P1A F3A . 1.6003(14) ?
P1A F4A . 1.6063(14) ?
P1A F5A . 1.6120(11) ?
P1A F1A . 1.5982(7) ?
P1A F2A . 1.5997(7) ?
P1B F4B . 1.502(12) ?
P1B F3B . 1.581(13) ?
P1B F5B . 1.560(6) ?
P1B F1B . 1.5982(7) ?
P1B F2B . 1.5997(7) ?
P1B F6B . 1.674(8) ?
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
C2 H2A F4A 2_565 0.99 2.62 3.183(2) 116.3 yes
C2 H2A F4B 2_565 0.99 2.53 3.126(11) 118.7 yes
C2 H2B F3A 7_576 0.99 2.37 3.1290(19) 132.9 yes
C7 H7 F2A 4_466 0.946(14) 2.522(13) 3.0711(12) 117.1(9) yes
N8 H8A F3A 7_576 0.827(18) 2.428(17) 3.141(2) 144.9(13) yes
N8 H8A F5A 6_557 0.827(18) 2.425(16) 3.0699(16) 135.4(13) yes
N8 H8A F3B 7_576 0.827(18) 2.36(2) 3.105(12) 150.1(14) yes
N8 H8A F5B 6_557 0.827(18) 2.331(18) 3.031(6) 142.8(13) yes
N8 H8B O4 8_665 0.850(18) 2.018(18) 2.8572(13) 168.8(16) yes
_cod_database_fobs_code 2022988