#------------------------------------------------------------------------------
#$Date: 2024-02-05 13:08:12 +0100 (Mon, 05 Feb 2024) $
#$Revision: 289691 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022991.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_2022991
loop_
_publ_author_name
'Mairath, Tristan'
'Schmidt, Annika'
'Strohmann, Carsten'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
2-picolyllithium·3thf.
;
_journal_coeditor_code HB8083
_journal_issue 'Pt 1'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 78
_journal_page_last 82
_journal_paper_doi 10.1107/S2056989023010873
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Li (C6 H6 N) (C4 H8 O)3]'
_chemical_formula_moiety 'C18 H30 Li N O3'
_chemical_formula_sum 'C18 H30 Li N O3'
_chemical_formula_weight 315.37
_chemical_name_systematic
(2-Methylidene-1,2-dihydropyridinium-\kN)tris(tetrahydrofuran-\kO)lithium
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha 90
_cell_angle_beta 94.437(6)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.267(3)
_cell_length_b 13.178(4)
_cell_length_c 15.053(5)
_cell_measurement_reflns_used 812
_cell_measurement_temperature 100.00
_cell_measurement_theta_max 17.21
_cell_measurement_theta_min 2.69
_cell_volume 1832.8(10)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2016)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0480
_diffrn_reflns_av_unetI/netI 0.0343
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 58129
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 40.229
_diffrn_reflns_theta_min 2.057
_diffrn_source_current 1.0
_diffrn_source_power 0.05
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.075
_exptl_absorpt_correction_T_max 0.5699
_exptl_absorpt_correction_T_min 0.4929
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.143
_exptl_crystal_description block
_exptl_crystal_F_000 688
_exptl_crystal_size_max 0.393
_exptl_crystal_size_mid 0.286
_exptl_crystal_size_min 0.212
_refine_diff_density_max 0.679
_refine_diff_density_min -0.394
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 226
_refine_ls_number_reflns 10326
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.0738
_refine_ls_R_factor_gt 0.0524
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.2483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1428
_refine_ls_wR_factor_ref 0.1585
_reflns_number_gt 7724
_reflns_number_total 10326
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8083sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022991.cif.'
_cod_original_cell_volume 1832.7(10)
_cod_database_code 2022991
_cod_database_fobs_code 2022991
_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 0.971
_shelx_estimated_absorpt_t_max 0.984
_shelx_hkl_file
;
1 0 0 0.32117 0.20427 4
1 0 0 0.05202 0.11232 6
-1 0 0 0.01860 0.14149 4
-1 0 0 -0.1853 0.21507 2
1 0 0 -0.2180 0.23475 1
1 0 0 0.30407 0.21895 2
-1 0 0 -0.1073 0.07802 6
1 0 0 0.11411 0.10299 8
-2 0 0 573.932 22.2935 1
-2 0 0 543.357 21.3134 8
2 0 0 549.988 22.0416 4
-2 0 0 549.950 21.6165 3
-2 0 0 562.918 22.9473 2
-2 0 0 547.668 21.8998 6
-2 0 0 551.057 22.0859 4
2 0 0 532.749 21.2999 8
2 0 0 619.369 22.0325 6
3 0 0 0.14637 0.49565 4
-3 0 0 1.41578 1.10420 2
3 0 0 0.54162 0.31596 8
-3 0 0 0.65972 0.31123 8
-3 0 0 0.27871 0.30254 3
3 0 0 -0.1465 0.34847 6
-3 0 0 0.30666 0.30375 6
-3 0 0 0.02735 0.42263 4
-3 0 0 -0.1230 0.13070 5
-3 0 0 1.15486 0.64188 1
-4 0 0 71.1808 3.56091 3
-4 0 0 64.7810 2.99871 8
4 0 0 66.3986 3.01483 8
-4 0 0 58.8930 4.20527 1
4 0 0 65.5874 4.19055 4
4 0 0 71.2389 4.11269 6
-4 0 0 58.2425 4.12355 4
-4 0 0 58.7207 2.92143 5
-4 0 0 63.3338 5.22246 2
-4 0 0 60.0353 3.81182 6
5 0 0 -0.0205 0.45272 8
-5 0 0 -1.9671 1.63136 2
-5 0 0 -0.1054 0.40947 6
-5 0 0 0.03001 0.40327 3
-5 0 0 0.00698 1.04927 1
-5 0 0 1.24130 0.99174 4
-5 0 0 0.95932 0.36591 5
5 0 0 0.78212 1.01647 4
5 0 0 0.38419 0.60679 6
6 0 0 167.541 8.82530 4
6 0 0 176.723 8.86206 6
-6 0 0 154.091 10.5580 2
-6 0 0 160.591 8.89346 1
6 0 0 155.929 6.83982 8
-6 0 0 160.412 7.75447 3
-6 0 0 156.975 8.98151 4
-6 0 0 153.023 6.76828 5
-6 0 0 154.850 8.34538 6
7 0 0 1.02052 0.80959 6
-7 0 0 1.17743 0.82946 6
-7 0 0 -1.4905 1.49162 1
-7 0 0 0.89525 0.41558 5
-7 0 0 2.18781 2.48416 2
7 0 0 -0.1606 0.57705 8
-7 0 0 1.36709 0.82922 3
-7 0 0 0.77989 1.23666 4
-8 0 0 28.3951 2.86984 3
-8 0 0 27.0663 1.13224 11
-8 0 0 25.5300 3.11167 6
-8 0 0 30.2465 1.83402 5
8 0 0 26.1656 3.49054 6
8 0 0 25.3914 2.11446 8
8 0 0 25.3512 3.68638 4
-9 0 0 -0.0211 0.09849 11
9 0 0 -0.9667 0.96348 6
-9 0 0 0.10779 0.71049 3
-9 0 0 1.36318 1.58678 4
9 0 0 0.13513 0.67766 8
-9 0 0 0.18878 0.35280 5
9 0 0 -1.1495 1.16678 4
10 0 0 96.6725 7.80891 4
-10 0 0 111.218 4.03717 11
-10 0 0 99.9716 4.04127 11
-10 0 0 106.204 6.66235 3
10 0 0 113.260 5.52316 8
10 0 0 97.9016 7.75748 6
-11 0 0 2.54089 1.32877 3
11 0 0 0.38226 2.04001 4
11 0 0 0.51673 0.83564 8
12 0 0 9.83151 1.94563 8
13 0 0 -0.1813 0.83477 8
14 0 0 0.63074 1.07055 8
-1 -1 0 129.076 5.67966 4
-1 -1 0 156.486 6.91514 1
1 -1 0 150.797 5.99693 4
-1 -1 0 145.103 6.03237 6
1 1 0 137.387 5.56506 10
1 1 0 139.447 5.50786 8
1 1 0 140.830 5.71421 4
1 1 0 131.867 5.98268 6
-1 1 0 138.664 6.71820 2
-2 -1 0 6814.31 251.716 1
-2 -1 0 6472.49 250.568 2
-2 1 0 6586.70 251.968 2
3 -1 0 250.876 10.2152 6
-3 -1 0 225.926 11.4548 1
-3 -1 0 222.893 10.3080 4
3 -1 0 237.078 9.31902 8
-3 -1 0 247.189 10.0557 3
-3 -1 0 232.114 9.43913 8
3 -1 0 233.065 10.4950 4
-3 -1 0 237.648 10.4249 6
-3 -1 0 241.001 11.0391 2
-3 1 0 238.920 12.0298 2
3 1 0 239.673 10.3207 4
-3 1 0 244.165 9.66019 3
-3 1 0 229.584 10.6209 4
3 1 0 251.753 10.6277 6
3 1 0 240.061 9.47267 8
-3 1 0 237.609 10.1292 6
-4 -1 0 91.2314 5.28325 4
-4 -1 0 89.7582 4.11318 8
4 -1 0 97.4214 5.03520 6
4 -1 0 94.3007 3.99802 8
-4 -1 0 93.2838 6.14938 2
-4 -1 0 93.4211 4.77548 3
-4 -1 0 93.5435 5.20443 6
4 -1 0 96.0719 5.42933 4
-4 -1 0 85.3777 4.25256 5
4 1 0 100.147 5.32712 4
4 1 0 89.8680 5.28000 6
-4 1 0 92.3851 5.49782 4
-4 1 0 87.7262 3.76739 5
-4 1 0 97.3706 4.45297 3
-4 1 0 87.3382 4.87785 6
-4 1 0 98.0500 6.96710 2
4 1 0 89.9216 4.12501 8
-5 -1 0 103.272 6.90931 1
5 -1 0 107.499 4.54534 8
5 -1 0 107.587 5.84099 6
5 -1 0 104.703 6.18050 4
-5 -1 0 102.469 5.43003 3
-5 -1 0 103.302 4.81355 5
-5 -1 0 95.6490 6.90703 2
-5 -1 0 102.647 4.65573 8
-5 -1 0 101.978 6.13477 4
5 1 0 89.1432 5.81181 4
-5 1 0 109.734 5.17443 3
-5 1 0 112.413 8.33550 2
-5 1 0 102.399 5.66682 6
5 1 0 108.829 6.21746 6
-5 1 0 96.7194 4.24040 5
5 1 0 110.479 4.72469 8
-5 1 0 93.1572 6.19542 4
6 -1 0 83.7347 3.80077 8
-6 -1 0 84.0939 5.74640 4
-6 -1 0 83.4215 4.82731 3
6 -1 0 87.9068 5.30905 6
-6 -1 0 75.2138 5.15053 6
-6 -1 0 80.1099 6.41535 1
6 -1 0 83.3489 5.63160 4
-6 -1 0 77.9342 6.72176 2
-6 -1 0 77.7260 3.98221 5
-6 1 0 73.0110 4.88869 6
6 1 0 85.2099 5.68862 6
-6 1 0 74.4374 3.04699 11
-6 1 0 76.8088 5.72841 4
6 1 0 82.4018 3.96719 8
6 1 0 83.1556 5.48444 4
-6 1 0 69.3685 7.42380 2
-6 1 0 85.3886 4.50462 3
-6 1 0 75.3815 3.42918 5
-6 1 0 79.3178 3.05033 11
-7 -1 0 25.6191 1.83731 5
7 -1 0 21.4982 3.22369 4
-7 -1 0 21.9882 3.60339 4
-7 -1 0 20.6160 3.94451 1
7 -1 0 23.9043 1.80875 8
-7 -1 0 27.2140 4.78436 2
-7 -1 0 21.8972 2.44185 3
7 -1 0 22.8112 2.86736 6
-7 -1 0 21.9259 2.72437 6
7 1 0 26.3191 3.17140 6
-7 1 0 21.0744 0.92100 11
7 1 0 27.2582 3.17339 4
-7 1 0 23.6010 0.92464 11
-7 1 0 24.9528 5.11792 2
7 1 0 23.5420 1.93365 8
-7 1 0 16.6713 3.23389 4
-7 1 0 26.6534 2.42818 3
8 -1 0 0.91833 1.36053 4
-8 -1 0 1.02796 1.16704 4
8 -1 0 1.21034 0.70493 8
8 -1 0 1.46942 1.05112 6
-8 -1 0 1.77848 1.07103 3
-8 -1 0 0.83395 0.99028 6
-8 -1 0 1.87616 0.58077 5
8 1 0 1.37861 0.78830 8
8 1 0 1.46453 1.34575 4
8 1 0 0.68451 1.08239 6
-8 1 0 1.30828 0.89904 3
-9 -1 0 14.3193 3.15377 4
9 -1 0 15.2437 1.71567 8
-9 -1 0 12.3811 2.80372 6
9 -1 0 9.80235 2.50727 4
-9 -1 0 12.0142 1.33654 5
-9 -1 0 9.49702 2.14217 3
-9 -1 0 14.5238 0.67162 11
9 1 0 11.7233 2.83770 6
-9 1 0 12.7076 2.15105 3
9 1 0 15.2623 1.80025 8
9 1 0 10.7293 2.84865 4
10 -1 0 4.43628 1.16559 8
-10 -1 0 4.29546 0.81273 5
-10 -1 0 4.74233 1.53249 3
-10 -1 0 3.44589 0.29742 11
10 -1 0 1.40113 1.50641 6
10 -1 0 0.26460 1.59416 4
10 1 0 3.34053 1.18459 8
-10 1 0 2.29488 1.28395 3
10 1 0 0.36767 1.47808 6
10 1 0 3.44771 2.19499 4
-11 -1 0 1.02699 0.41731 5
-11 -1 0 0.56544 0.14760 11
11 -1 0 -0.8798 0.67071 8
11 -1 0 -1.1190 1.40914 4
-11 1 0 1.37897 1.26383 3
11 1 0 1.09033 1.75399 4
11 1 0 0.03542 0.79343 8
12 -1 0 11.7910 1.92692 8
12 1 0 12.9247 2.15628 8
13 -1 0 1.00770 0.94486 8
13 1 0 -0.1730 1.17426 8
14 -1 0 2.38846 1.27892 8
14 1 0 4.21841 1.65537 8
0 -2 0 219.778 9.59963 1
0 -2 0 212.587 8.10380 3
0 -2 0 229.213 8.61546 6
0 -2 0 190.406 8.04987 7
0 -2 0 199.700 7.85901 8
0 2 0 197.572 7.86539 8
0 2 0 185.184 8.81476 2
-1 -2 0 802.227 31.4902 7
-1 -2 0 842.671 33.6147 1
1 -2 0 860.634 32.3945 1
1 -2 0 862.056 31.9451 4
-1 -2 0 779.213 31.1784 9
1 -2 0 792.804 31.1326 8
-1 -2 0 814.574 31.4592 4
-1 -2 0 863.251 32.1724 6
-1 -2 0 829.795 31.7255 3
-1 -2 0 774.998 31.3044 8
1 -2 0 874.049 31.3873 5
1 2 0 787.579 31.4543 10
1 2 0 795.546 31.3169 8
1 2 0 821.978 31.5013 4
-1 2 0 872.736 33.4201 2
-2 -2 0 617.590 24.5349 8
-2 -2 0 629.309 24.9768 4
2 -2 0 667.805 25.5018 4
-2 -2 0 678.049 27.4366 1
-2 -2 0 629.391 25.1168 3
-2 -2 0 645.431 25.6136 6
2 2 0 609.307 24.6673 10
2 2 0 607.038 24.4471 9
2 2 0 680.812 25.7779 6
2 2 0 615.332 24.9324 4
2 2 0 617.067 24.5430 8
-2 2 0 677.320 25.6417 4
-2 2 0 669.074 27.4184 2
3 -2 0 2118.93 79.5717 4
-3 -2 0 2111.19 81.7156 1
-3 -2 0 2102.62 79.0315 3
-3 -2 0 2038.07 79.2623 2
-3 -2 0 2049.74 79.5387 6
-3 -2 0 1988.48 79.0605 4
3 -2 0 2038.47 78.8670 6
-3 -2 0 2003.36 78.2693 8
-3 2 0 2183.20 82.2495 2
3 2 0 2172.59 79.8259 6
-3 2 0 2076.11 79.7392 4
-3 2 0 2167.22 78.2263 3
3 2 0 1897.01 78.3709 10
3 2 0 1948.35 78.2011 9
3 2 0 2084.16 79.0327 4
-4 -2 0 94.8334 6.04621 2
4 -2 0 105.447 5.95261 4
4 -2 0 106.086 4.36375 8
-4 -2 0 102.720 5.81032 6
-4 -2 0 92.3575 4.86065 5
-4 -2 0 105.277 7.35731 1
-4 -2 0 104.074 5.68489 4
-4 -2 0 102.277 4.60491 8
-4 -2 0 102.116 5.35897 3
4 -2 0 115.919 5.45610 6
-4 2 0 106.470 7.85814 2
-4 2 0 106.086 6.16075 4
4 2 0 101.391 4.62807 9
4 2 0 115.952 4.72783 8
-4 2 0 101.214 4.67553 3
4 2 0 104.686 5.62059 4
4 2 0 110.900 6.15278 6
4 2 0 98.7183 4.68831 10
5 -2 0 98.7919 4.10377 8
-5 -2 0 93.9473 6.18224 2
5 -2 0 102.064 5.38355 6
-5 -2 0 87.5070 4.59284 5
5 -2 0 98.0456 5.94769 4
-5 -2 0 96.8533 5.28545 3
-5 -2 0 93.6028 5.69121 6
-5 -2 0 93.1014 7.25606 1
-5 -2 0 88.6251 5.61196 4
5 2 0 90.4322 4.42224 10
5 2 0 91.6966 5.50764 4
5 2 0 98.9490 6.03694 6
-5 2 0 99.2857 4.57325 3
5 2 0 84.2170 4.32065 9
-5 2 0 82.5251 5.86176 4
5 2 0 90.2348 4.36428 8
-5 2 0 93.2192 8.18443 2
6 -2 0 15.6758 1.99933 6
6 -2 0 13.4883 1.22673 8
-6 -2 0 7.50219 2.61840 2
-6 -2 0 14.3862 1.92817 3
-6 -2 0 11.5349 2.28405 4
-6 -2 0 13.6647 2.07319 6
-6 -2 0 10.0640 2.82673 1
6 -2 0 10.1921 2.10908 4
-6 -2 0 11.8235 1.39489 5
-6 2 0 14.9529 1.56865 3
6 2 0 11.4968 1.46272 8
6 2 0 10.6572 2.14024 4
6 2 0 13.9038 2.98746 6
7 -2 0 0.27478 0.50218 8
-7 -2 0 -0.4780 0.58393 3
7 -2 0 1.19908 1.11245 4
-7 -2 0 0.06136 0.41712 5
-7 -2 0 2.26619 1.90755 2
-7 -2 0 -0.2802 2.06284 1
-7 -2 0 -1.7074 0.75348 4
7 -2 0 -0.2761 0.66760 6
-7 -2 0 0.73416 0.72387 6
-7 2 0 0.79641 0.63678 3
7 2 0 0.79491 0.98579 6
7 2 0 -0.3942 1.08819 4
-7 2 0 -1.1095 2.48633 2
-7 2 0 0.38470 1.03206 4
7 2 0 -0.2566 0.57474 8
8 -2 0 -0.0848 0.48014 8
8 -2 0 0.13600 0.79378 6
8 -2 0 1.45679 1.44125 4
-8 -2 0 1.05744 0.75365 3
-8 -2 0 0.50232 0.66926 6
-8 -2 0 1.89725 1.36895 4
-8 -2 0 -0.1743 0.49083 5
-8 2 0 -0.9919 1.30378 4
-8 2 0 1.49851 0.74200 3
8 2 0 0.14300 0.65735 8
8 2 0 -0.1025 1.07235 6
8 2 0 -0.4580 1.37463 4
-9 -2 0 0.21295 1.11087 3
-9 -2 0 1.06027 1.09649 6
-9 -2 0 2.61011 1.57811 4
9 -2 0 1.39176 0.78111 8
-9 -2 0 1.59887 0.63152 5
9 -2 0 -0.4932 0.78804 6
9 -2 0 -1.0842 1.48996 4
-9 2 0 0.55898 0.79557 3
9 2 0 1.02549 1.25613 6
9 2 0 0.70380 1.56523 4
9 2 0 0.82029 0.86042 8
-10 -2 0 14.2565 1.71626 5
-10 -2 0 14.0414 3.22427 6
10 -2 0 23.7406 3.35138 6
10 -2 0 17.3924 1.86322 8
-10 -2 0 18.0997 0.84365 11
10 -2 0 11.0027 3.03285 4
-10 -2 0 12.1001 2.50215 3
10 2 0 13.0763 3.38650 4
10 2 0 19.6082 2.22368 8
-10 2 0 14.4904 2.33150 3
11 -2 0 -0.8049 0.62094 8
-11 -2 0 0.16323 0.16444 11
11 -2 0 -2.1100 1.39247 4
11 2 0 0.00893 0.84785 8
11 2 0 -1.0093 1.76749 4
-11 2 0 -0.7760 0.89845 3
12 -2 0 -1.2632 0.65025 8
-12 -2 0 0.50763 0.17631 11
12 2 0 2.22095 1.17092 8
13 -2 0 23.9547 2.47371 8
13 2 0 21.5091 3.02533 8
14 -2 0 11.5778 2.02242 8
14 2 0 12.3255 2.30130 8
0 -3 0 0.74758 0.27891 8
0 -3 0 0.98942 0.66458 7
0 -3 0 0.79036 0.67443 1
0 -3 0 -0.0077 0.27339 3
0 -3 0 0.00140 0.39982 6
0 3 0 0.45315 0.25958 8
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0 0 -26 37.1505 2.37557 11
-1 0 -26 0.14795 0.60753 11
-2 0 -26 26.7262 1.95139 11
-3 0 -26 0.14250 0.53992 11
6 -1 -26 3.60361 0.76979 12
5 -1 -26 2.39368 0.79914 12
4 -1 -26 3.49304 0.80708 12
3 -1 -26 8.85074 1.23274 11
2 -1 -26 0.74807 0.63482 11
1 -1 -26 3.23148 0.84891 11
0 -1 -26 1.89454 0.80244 11
0 1 -26 3.73959 0.88747 11
-1 -1 -26 5.41068 0.96127 11
-1 1 -26 4.40679 0.94927 11
-2 -1 -26 3.02699 0.82503 11
-2 1 -26 2.10355 0.79287 11
-3 -1 -26 1.17669 0.70726 11
-3 1 -26 0.37880 0.63001 11
6 -2 -26 0.21557 0.59899 12
5 -2 -26 2.55704 0.83955 12
4 -2 -26 2.38779 0.76995 11
3 -2 -26 1.29351 0.68049 11
2 -2 -26 12.2891 1.37113 11
1 -2 -26 6.57409 1.05617 11
0 -2 -26 23.1183 1.83916 11
-1 -2 -26 0.42589 0.60802 11
-2 -2 -26 2.75885 0.79089 11
-3 -2 -26 0.37512 0.59410 11
5 -3 -26 -0.9375 0.48427 11
5 -3 -26 -0.1160 0.61183 12
4 -3 -26 0.32802 0.58193 11
3 -3 -26 0.99888 0.61041 11
2 -3 -26 9.27329 1.19396 11
1 -3 -26 1.81214 0.74365 11
0 -3 -26 6.85800 1.10177 11
-1 -3 -26 0.04495 0.56743 11
-2 -3 -26 1.07547 0.68566 11
-3 -3 -26 5.22545 0.94167 11
5 -4 -26 3.17964 0.83308 11
4 -4 -26 2.22407 0.71572 11
3 -4 -26 8.61165 1.13800 11
2 -4 -26 0.64916 0.61778 11
1 -4 -26 18.4176 1.65438 11
0 -4 -26 9.32404 1.19477 11
-1 -4 -26 -0.2467 0.56571 11
-2 -4 -26 7.50454 1.10450 11
-3 -4 -26 -0.0174 0.54845 11
4 -5 -26 3.71148 0.86641 11
3 -5 -26 2.41788 0.76256 11
2 -5 -26 1.19457 0.70219 11
1 -5 -26 -0.1437 0.54605 11
0 -5 -26 1.83218 0.75497 11
-1 -5 -26 0.13080 0.58252 11
-2 -5 -26 5.00396 0.95059 11
4 -6 -26 2.40883 0.75716 11
3 -6 -26 1.24154 0.69004 11
2 -6 -26 -0.4171 0.46827 11
1 -6 -26 0.58671 0.57208 11
0 -6 -26 1.81733 0.72397 11
-1 -6 -26 1.60214 0.68590 11
2 -7 -26 7.85870 1.11874 11
1 -7 -26 24.3333 1.89235 11
0 -7 -26 5.09856 0.93766 11
1 0 -27 0.51762 0.63791 11
0 0 -27 2.09533 0.80499 11
-1 0 -27 9.06034 1.26341 11
2 -1 -27 0.17938 0.64451 11
1 -1 -27 0.12882 0.60597 11
0 -1 -27 0.96795 0.67330 11
-1 -1 -27 0.42648 0.60047 11
-1 1 -27 0.86102 0.68552 11
3 -2 -27 0.75077 0.65601 11
2 -2 -27 1.27164 0.67546 11
1 -2 -27 8.50612 1.23698 11
0 -2 -27 0.17555 0.54022 11
2 -3 -27 4.30797 0.92336 11
1 -3 -27 -0.6106 0.50288 11
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 0.5699
_exptl_absorpt_correction_T_min 0.4929
_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 0.71076 9.258 13.179 15.009 90.012 94.400 90.018
)
;
_shelx_hkl_checksum 67824
_shelx_res_file
;
mo_b2506_0m.res created by SHELXL-2014/7
TITL mo_b2506_0m_a.res in P2(1)/n
REM Old TITL mo_B2506_0m in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.146, Rweak 0.007, Alpha 0.050
REM 0.584 for 33 systematic absences, Orientation as input
REM Formula found by SHELXT: C18 Li N O3
CELL 0.71073 9.2667 13.1782 15.0529 90 94.437 90
ZERR 4 0.0027 0.0041 0.0048 0 0.006 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Li N O
UNIT 72 120 4 4 12
EQIV $1 1-X,1-Y,1-Z
L.S. 4
PLAN 5
SIZE 0.393 0.286 0.212
TEMP -173.15
CONF
HTAB C15 O1_$1
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 6 3 0
OMIT 2 3 24
REM
REM
REM
WGHT 0.081600 0.248300
FVAR 0.53801 0.71709
O1 5 0.546881 0.405452 0.699897 11.00000 0.01819 0.01801 =
0.02364 0.00186 -0.00041 -0.00114
O2 5 0.254727 0.370198 0.591946 11.00000 0.02419 0.02005 =
0.01507 -0.00015 -0.00091 -0.00422
O3 5 0.406638 0.594994 0.604659 11.00000 0.03538 0.01497 =
0.01725 0.00046 0.00246 -0.00083
N1 4 0.275029 0.502084 0.783895 11.00000 0.01753 0.01931 =
0.01434 -0.00134 0.00059 0.00114
C1 1 0.052856 0.551192 0.701406 11.00000 0.02045 0.02269 =
0.01804 0.00067 -0.00094 0.00240
H1A 2 0.095824 0.539943 0.644366 11.00000 0.03145
H1B 2 -0.049216 0.575909 0.697931 11.00000 0.02575
C2 1 0.131839 0.536785 0.781984 11.00000 0.01762 0.01341 =
0.01626 -0.00071 0.00128 -0.00083
C3 1 0.071937 0.556630 0.866808 11.00000 0.01987 0.01643 =
0.01841 -0.00203 0.00408 -0.00072
AFIX 43
H3 2 -0.026158 0.577418 0.867314 11.00000 -1.20000
AFIX 0
C4 1 0.153719 0.546013 0.945765 11.00000 0.02426 0.02050 =
0.01644 -0.00353 0.00416 -0.00296
AFIX 43
H4 2 0.112812 0.560097 1.000390 11.00000 -1.20000
AFIX 0
C5 1 0.299963 0.513886 0.945962 11.00000 0.02408 0.02694 =
0.01462 -0.00386 -0.00067 -0.00082
AFIX 43
H5 2 0.359966 0.506991 0.999714 11.00000 -1.20000
AFIX 0
C6 1 0.350628 0.493111 0.863679 11.00000 0.01888 0.02438 =
0.01615 -0.00290 -0.00045 0.00100
AFIX 43
H6 2 0.447889 0.470381 0.863468 11.00000 -1.20000
AFIX 0
C7 1 0.550766 0.303051 0.734599 11.00000 0.02107 0.01718 =
0.02566 0.00067 -0.00021 -0.00136
AFIX 23
H7A 2 0.509071 0.254722 0.689250 11.00000 -1.20000
H7B 2 0.495599 0.298271 0.788198 11.00000 -1.20000
AFIX 0
C8 1 0.709867 0.280603 0.757807 11.00000 0.02218 0.02375 =
0.02814 0.00156 -0.00169 0.00285
AFIX 23
H8A 2 0.757682 0.256738 0.705060 11.00000 -1.20000
H8B 2 0.723102 0.229245 0.805744 11.00000 -1.20000
AFIX 0
C9 1 0.767663 0.384247 0.789259 11.00000 0.02385 0.03026 =
0.02465 0.00201 -0.00558 -0.00525
AFIX 23
H9A 2 0.748660 0.397025 0.852106 11.00000 -1.20000
H9B 2 0.872850 0.390151 0.782836 11.00000 -1.20000
AFIX 0
C10 1 0.681267 0.456391 0.726329 11.00000 0.02443 0.02222 =
0.02708 0.00159 -0.00266 -0.00641
AFIX 23
H10A 2 0.662505 0.520995 0.756963 11.00000 -1.20000
H10B 2 0.735141 0.471371 0.673577 11.00000 -1.20000
AFIX 0
C11 1 0.172408 0.298712 0.641949 11.00000 0.02779 0.01849 =
0.01734 0.00149 0.00069 -0.00295
AFIX 23
H11A 2 0.147557 0.329088 0.698952 11.00000 -1.20000
H11B 2 0.228844 0.235942 0.654928 11.00000 -1.20000
AFIX 0
C12 1 0.036466 0.275869 0.582609 11.00000 0.02442 0.02435 =
0.02976 0.00034 -0.00056 -0.00496
AFIX 23
H12A 2 -0.040975 0.325688 0.591731 11.00000 -1.20000
H12B 2 0.000153 0.206624 0.593279 11.00000 -1.20000
AFIX 0
C13 1 0.090692 0.285506 0.489280 11.00000 0.03622 0.02267 =
0.02127 -0.00160 -0.00756 -0.00473
AFIX 23
H13A 2 0.142853 0.223658 0.472563 11.00000 -1.20000
H13B 2 0.010091 0.299124 0.443776 11.00000 -1.20000
AFIX 0
C14 1 0.192068 0.375888 0.501123 11.00000 0.03513 0.02342 =
0.01561 0.00159 -0.00249 -0.00465
AFIX 23
H14A 2 0.268446 0.372159 0.458748 11.00000 -1.20000
H14B 2 0.138016 0.440173 0.490963 11.00000 -1.20000
AFIX 0
C15 1 0.372183 0.622907 0.513093 11.00000 0.05796 0.02112 =
0.01626 0.00007 0.00283 -0.00435
AFIX 23
H15A 2 0.271945 0.602533 0.493411 11.00000 -1.20000
H15B 2 0.439334 0.589595 0.474145 11.00000 -1.20000
AFIX 0
C16 1 0.388171 0.736876 0.509376 11.00000 0.10422 0.02296 =
0.02725 0.00737 0.00304 -0.01341
PART 1
AFIX 23
H16A 2 0.488514 0.756519 0.498768 21.00000 -1.20000
H16B 2 0.320872 0.766607 0.462105 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H16C 2 0.460405 0.755446 0.467039 -21.00000 -1.20000
H16D 2 0.294498 0.768409 0.488854 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C17 1 0.349858 0.769688 0.600763 21.00000 0.03223 0.01585 =
0.04085 -0.00442 -0.00157 0.00099
AFIX 23
H17A 2 0.399390 0.833852 0.618801 21.00000 -1.20000
H17B 2 0.244074 0.779204 0.602099 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C17A 1 0.433710 0.771812 0.595639 -21.00000 0.02847 0.01503 =
0.02509 0.00152 -0.00381 -0.00407
AFIX 23
H17C 2 0.380051 0.833903 0.609994 -21.00000 -1.20000
H17D 2 0.538528 0.787403 0.600018 -21.00000 -1.20000
AFIX 0
PART 0
C18 1 0.401281 0.685360 0.659442 11.00000 0.05971 0.01745 =
0.02015 -0.00303 0.00217 -0.00799
PART 1
AFIX 23
H18A 2 0.498658 0.700859 0.687939 21.00000 -1.20000
H18B 2 0.334403 0.674856 0.706814 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H18C 2 0.474993 0.682477 0.710621 -21.00000 -1.20000
H18D 2 0.304475 0.693754 0.682056 -21.00000 -1.20000
AFIX 0
PART 0
LI1 3 0.361318 0.470855 0.668283 11.00000 0.02231 0.01843 =
0.01595 -0.00008 0.00108 -0.00067
HKLF 4
REM mo_b2506_0m_a.res in P2(1)/n
REM R1 = 0.0524 for 7724 Fo > 4sig(Fo) and 0.0738 for all 10326 data
REM 226 parameters refined using 0 restraints
END
WGHT 0.0817 0.2485
REM Highest difference peak 0.679, deepest hole -0.394, 1-sigma level 0.060
Q1 1 0.3269 0.4999 0.9052 11.00000 0.05 0.68
Q2 1 0.1003 0.5448 0.8250 11.00000 0.05 0.63
Q3 1 0.1112 0.5486 0.9053 11.00000 0.05 0.57
Q4 1 0.0880 0.5379 0.7424 11.00000 0.05 0.53
Q5 1 0.2025 0.5168 0.7873 11.00000 0.05 0.50
;
_shelx_res_checksum 16947
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
O O1 0.54688(6) 0.40545(4) 0.69990(4) 0.02005(10) Uani d 1 . .
O O2 0.25473(6) 0.37020(4) 0.59195(3) 0.01990(10) Uani d 1 . .
O O3 0.40664(7) 0.59499(4) 0.60466(4) 0.02251(11) Uani d 1 . .
N N1 0.27503(7) 0.50208(5) 0.78389(4) 0.01709(10) Uani d 1 . .
C C1 0.05286(9) 0.55119(6) 0.70141(5) 0.02052(13) Uani d 1 . .
H H1A 0.0958(14) 0.5399(11) 0.6444(9) 0.031(3) Uiso d 1 . .
H H1B -0.0492(14) 0.5759(10) 0.6979(8) 0.026(3) Uiso d 1 . .
C C2 0.13184(8) 0.53679(5) 0.78198(4) 0.01576(11) Uani d 1 . .
C C3 0.07194(8) 0.55663(5) 0.86681(5) 0.01810(12) Uani d 1 . .
H H3 -0.0262 0.5774 0.8673 0.022 Uiso calc 1 . .
C C4 0.15372(9) 0.54601(6) 0.94577(5) 0.02027(13) Uani d 1 . .
H H4 0.1128 0.5601 1.0004 0.024 Uiso calc 1 . .
C C5 0.29996(9) 0.51389(6) 0.94596(5) 0.02199(14) Uani d 1 . .
H H5 0.3600 0.5070 0.9997 0.026 Uiso calc 1 . .
C C6 0.35063(8) 0.49311(6) 0.86368(5) 0.01989(13) Uani d 1 . .
H H6 0.4479 0.4704 0.8635 0.024 Uiso calc 1 . .
C C7 0.55077(9) 0.30305(6) 0.73460(5) 0.02141(13) Uani d 1 . .
H H7A 0.5091 0.2547 0.6892 0.026 Uiso calc 1 . .
H H7B 0.4956 0.2983 0.7882 0.026 Uiso calc 1 . .
C C8 0.70987(9) 0.28060(6) 0.75781(6) 0.02488(15) Uani d 1 . .
H H8A 0.7577 0.2567 0.7051 0.030 Uiso calc 1 . .
H H8B 0.7231 0.2292 0.8057 0.030 Uiso calc 1 . .
C C9 0.76766(10) 0.38425(7) 0.78926(6) 0.02664(16) Uani d 1 . .
H H9A 0.7487 0.3970 0.8521 0.032 Uiso calc 1 . .
H H9B 0.8729 0.3902 0.7828 0.032 Uiso calc 1 . .
C C10 0.68127(9) 0.45639(6) 0.72633(6) 0.02482(15) Uani d 1 . .
H H10A 0.6625 0.5210 0.7570 0.030 Uiso calc 1 . .
H H10B 0.7351 0.4714 0.6736 0.030 Uiso calc 1 . .
C C11 0.17241(9) 0.29871(6) 0.64195(5) 0.02126(13) Uani d 1 . .
H H11A 0.1476 0.3291 0.6990 0.026 Uiso calc 1 . .
H H11B 0.2288 0.2359 0.6549 0.026 Uiso calc 1 . .
C C12 0.03647(10) 0.27587(7) 0.58261(6) 0.02632(16) Uani d 1 . .
H H12A -0.0410 0.3257 0.5917 0.032 Uiso calc 1 . .
H H12B 0.0002 0.2066 0.5933 0.032 Uiso calc 1 . .
C C13 0.09069(11) 0.28551(6) 0.48928(6) 0.02723(16) Uani d 1 . .
H H13A 0.1429 0.2237 0.4726 0.033 Uiso calc 1 . .
H H13B 0.0101 0.2991 0.4438 0.033 Uiso calc 1 . .
C C14 0.19207(10) 0.37589(6) 0.50112(5) 0.02495(15) Uani d 1 . .
H H14A 0.2684 0.3722 0.4587 0.030 Uiso calc 1 . .
H H14B 0.1380 0.4402 0.4910 0.030 Uiso calc 1 . .
C C15 0.37218(13) 0.62291(7) 0.51309(5) 0.0318(2) Uani d 1 . .
H H15A 0.2719 0.6025 0.4934 0.038 Uiso calc 1 . .
H H15B 0.4393 0.5896 0.4741 0.038 Uiso calc 1 . .
C C16 0.3882(2) 0.73688(8) 0.50938(7) 0.0516(4) Uani d 1 . .
H H16A 0.4885 0.7565 0.4988 0.062 Uiso calc 0.717(5) A 1
H H16B 0.3209 0.7666 0.4621 0.062 Uiso calc 0.717(5) A 1
H H16C 0.4604 0.7554 0.4670 0.062 Uiso calc 0.283(5) A 2
H H16D 0.2945 0.7684 0.4889 0.062 Uiso calc 0.283(5) A 2
C C17 0.3499(2) 0.76969(9) 0.60076(10) 0.0299(4) Uani d 0.717(5) A 1
H H17A 0.3994 0.8339 0.6188 0.036 Uiso calc 0.717(5) A 1
H H17B 0.2441 0.7792 0.6021 0.036 Uiso calc 0.717(5) A 1
C C17A 0.4337(5) 0.7718(2) 0.59564(19) 0.0232(9) Uani d 0.283(5) A 2
H H17C 0.3801 0.8339 0.6100 0.028 Uiso calc 0.283(5) A 2
H H17D 0.5385 0.7874 0.6000 0.028 Uiso calc 0.283(5) A 2
C C18 0.40128(13) 0.68536(6) 0.65944(6) 0.0325(2) Uani d 1 . .
H H18A 0.4987 0.7009 0.6879 0.039 Uiso calc 0.717(5) A 1
H H18B 0.3344 0.6749 0.7068 0.039 Uiso calc 0.717(5) A 1
H H18C 0.4750 0.6825 0.7106 0.039 Uiso calc 0.283(5) A 2
H H18D 0.3045 0.6938 0.6821 0.039 Uiso calc 0.283(5) A 2
Li Li1 0.36132(16) 0.47086(10) 0.66828(9) 0.0189(2) Uani d 1 . .
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
O1 0.0182(2) 0.0180(2) 0.0236(2) -0.00114(17) -0.00041(18) 0.00186(17)
O2 0.0242(3) 0.0201(2) 0.01507(19) -0.00422(18) -0.00091(17) -0.00015(16)
O3 0.0354(3) 0.0150(2) 0.0172(2) -0.00083(19) 0.0025(2) 0.00046(16)
N1 0.0175(3) 0.0193(2) 0.0143(2) 0.00114(19) 0.00059(18) -0.00134(17)
C1 0.0204(3) 0.0227(3) 0.0180(3) 0.0024(2) -0.0009(2) 0.0007(2)
C2 0.0176(3) 0.0134(2) 0.0163(2) -0.00083(19) 0.0013(2) -0.00071(18)
C3 0.0199(3) 0.0164(2) 0.0184(3) -0.0007(2) 0.0041(2) -0.0020(2)
C4 0.0243(3) 0.0205(3) 0.0164(3) -0.0030(2) 0.0042(2) -0.0035(2)
C5 0.0241(3) 0.0269(3) 0.0146(2) -0.0008(3) -0.0007(2) -0.0039(2)
C6 0.0189(3) 0.0244(3) 0.0161(3) 0.0010(2) -0.0005(2) -0.0029(2)
C7 0.0211(3) 0.0172(3) 0.0257(3) -0.0014(2) -0.0002(2) 0.0007(2)
C8 0.0222(3) 0.0237(3) 0.0281(4) 0.0028(3) -0.0017(3) 0.0016(3)
C9 0.0239(4) 0.0303(4) 0.0247(3) -0.0053(3) -0.0056(3) 0.0020(3)
C10 0.0244(4) 0.0222(3) 0.0271(3) -0.0064(3) -0.0027(3) 0.0016(3)
C11 0.0278(4) 0.0185(3) 0.0173(3) -0.0030(2) 0.0007(2) 0.0015(2)
C12 0.0244(4) 0.0244(3) 0.0298(4) -0.0050(3) -0.0006(3) 0.0003(3)
C13 0.0362(4) 0.0227(3) 0.0213(3) -0.0047(3) -0.0076(3) -0.0016(2)
C14 0.0351(4) 0.0234(3) 0.0156(3) -0.0047(3) -0.0025(3) 0.0016(2)
C15 0.0580(6) 0.0211(3) 0.0163(3) -0.0044(3) 0.0028(3) 0.0001(2)
C16 0.1042(11) 0.0230(4) 0.0273(4) -0.0134(5) 0.0030(6) 0.0074(3)
C17 0.0322(10) 0.0159(4) 0.0408(7) 0.0010(4) -0.0016(5) -0.0044(4)
C17A 0.028(2) 0.0150(9) 0.0251(12) -0.0041(9) -0.0038(10) 0.0015(8)
C18 0.0597(6) 0.0175(3) 0.0201(3) -0.0080(3) 0.0022(3) -0.0030(2)
Li1 0.0223(6) 0.0184(5) 0.0159(5) -0.0007(5) 0.0011(4) -0.0001(4)
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'
Li Li -0.0003 0.0001 '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'
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 O1 Li1 . . 119.84(6) ?
C10 O1 C7 . . 109.73(6) ?
C10 O1 Li1 . . 125.99(7) ?
C11 O2 Li1 . . 113.13(6) ?
C14 O2 C11 . . 109.51(6) ?
C14 O2 Li1 . . 131.57(6) ?
C15 O3 C18 . . 108.65(6) ?
C15 O3 Li1 . . 129.97(7) ?
C18 O3 Li1 . . 112.93(7) ?
C2 N1 Li1 . . 119.19(6) ?
C6 N1 C2 . . 118.22(6) ?
C6 N1 Li1 . . 122.58(7) ?
H1A C1 H1B . . 116.7(11) ?
C2 C1 H1A . . 121.5(8) ?
C2 C1 H1B . . 121.8(7) ?
N1 C2 C3 . . 117.74(6) ?
C1 C2 N1 . . 119.98(6) ?
C1 C2 C3 . . 122.28(7) ?
C2 C3 H3 . . 119.3 ?
C4 C3 C2 . . 121.43(7) ?
C4 C3 H3 . . 119.3 ?
C3 C4 H4 . . 120.1 ?
C3 C4 C5 . . 119.83(7) ?
C5 C4 H4 . . 120.1 ?
C4 C5 H5 . . 121.7 ?
C6 C5 C4 . . 116.52(7) ?
C6 C5 H5 . . 121.7 ?
N1 C6 C5 . . 126.19(7) ?
N1 C6 H6 . . 116.9 ?
C5 C6 H6 . . 116.9 ?
O1 C7 H7A . . 110.7 ?
O1 C7 H7B . . 110.7 ?
O1 C7 C8 . . 105.16(6) ?
H7A C7 H7B . . 108.8 ?
C8 C7 H7A . . 110.7 ?
C8 C7 H7B . . 110.7 ?
C7 C8 H8A . . 111.4 ?
C7 C8 H8B . . 111.4 ?
C7 C8 C9 . . 102.00(7) ?
H8A C8 H8B . . 109.2 ?
C9 C8 H8A . . 111.4 ?
C9 C8 H8B . . 111.4 ?
C8 C9 H9A . . 111.3 ?
C8 C9 H9B . . 111.3 ?
H9A C9 H9B . . 109.2 ?
C10 C9 C8 . . 102.13(7) ?
C10 C9 H9A . . 111.3 ?
C10 C9 H9B . . 111.3 ?
O1 C10 C9 . . 106.36(7) ?
O1 C10 H10A . . 110.5 ?
O1 C10 H10B . . 110.5 ?
C9 C10 H10A . . 110.5 ?
C9 C10 H10B . . 110.5 ?
H10A C10 H10B . . 108.6 ?
O2 C11 H11A . . 110.6 ?
O2 C11 H11B . . 110.6 ?
O2 C11 C12 . . 105.55(6) ?
H11A C11 H11B . . 108.8 ?
C12 C11 H11A . . 110.6 ?
C12 C11 H11B . . 110.6 ?
C11 C12 H12A . . 111.4 ?
C11 C12 H12B . . 111.4 ?
C11 C12 C13 . . 101.94(7) ?
H12A C12 H12B . . 109.2 ?
C13 C12 H12A . . 111.4 ?
C13 C12 H12B . . 111.4 ?
C12 C13 H13A . . 111.5 ?
C12 C13 H13B . . 111.5 ?
H13A C13 H13B . . 109.3 ?
C14 C13 C12 . . 101.59(6) ?
C14 C13 H13A . . 111.5 ?
C14 C13 H13B . . 111.5 ?
O2 C14 C13 . . 105.66(6) ?
O2 C14 H14A . . 110.6 ?
O2 C14 H14B . . 110.6 ?
C13 C14 H14A . . 110.6 ?
C13 C14 H14B . . 110.6 ?
H14A C14 H14B . . 108.7 ?
O3 C15 H15A . . 110.5 ?
O3 C15 H15B . . 110.5 ?
O3 C15 C16 . . 105.94(7) ?
H15A C15 H15B . . 108.7 ?
C16 C15 H15A . . 110.5 ?
C16 C15 H15B . . 110.5 ?
C15 C16 H16A . . 111.2 ?
C15 C16 H16B . . 111.2 ?
C15 C16 H16C . . 110.0 ?
C15 C16 H16D . . 110.0 ?
H16A C16 H16B . . 109.1 ?
H16C C16 H16D . . 108.4 ?
C17 C16 C15 . . 102.72(9) ?
C17 C16 H16A . . 111.2 ?
C17 C16 H16B . . 111.2 ?
C17A C16 C15 . . 108.27(13) ?
C17A C16 H16C . . 110.0 ?
C17A C16 H16D . . 110.0 ?
C16 C17 H17A . . 111.0 ?
C16 C17 H17B . . 111.0 ?
H17A C17 H17B . . 109.0 ?
C18 C17 C16 . . 104.00(10) ?
C18 C17 H17A . . 111.0 ?
C18 C17 H17B . . 111.0 ?
C16 C17A H17C . . 110.5 ?
C16 C17A H17D . . 110.5 ?
C16 C17A C18 . . 105.94(18) ?
H17C C17A H17D . . 108.7 ?
C18 C17A H17C . . 110.5 ?
C18 C17A H17D . . 110.5 ?
O3 C18 C17 . . 107.55(8) ?
O3 C18 C17A . . 103.68(13) ?
O3 C18 H18A . . 110.2 ?
O3 C18 H18B . . 110.2 ?
O3 C18 H18C . . 111.0 ?
O3 C18 H18D . . 111.0 ?
C17 C18 H18A . . 110.2 ?
C17 C18 H18B . . 110.2 ?
C17A C18 H18C . . 111.0 ?
C17A C18 H18D . . 111.0 ?
H18A C18 H18B . . 108.5 ?
H18C C18 H18D . . 109.0 ?
O1 Li1 O2 . . 103.75(7) y
O1 Li1 O3 . . 105.69(7) y
O1 Li1 N1 . . 106.33(7) y
O2 Li1 N1 . . 115.29(7) y
O3 Li1 O2 . . 113.22(7) y
O3 Li1 N1 . . 111.51(7) y
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
Li1 O1 . 1.9493(16) y
Li1 O2 . 1.9698(15) y
Li1 O3 . 1.9576(15) y
Li1 N1 . 2.0131(16) y
O1 C7 . 1.4465(10) ?
O1 C10 . 1.4433(10) ?
O2 C11 . 1.4577(10) ?
O2 C14 . 1.4454(10) ?
O3 C15 . 1.4384(11) ?
O3 C18 . 1.4515(10) ?
N1 C2 . 1.4017(10) y
N1 C6 . 1.3479(10) y
C1 H1A . 0.985(14) ?
C1 H1B . 0.998(13) ?
C1 C2 . 1.3804(10) ?
C2 C3 . 1.4548(10) y
C3 H3 . 0.9500 ?
C3 C4 . 1.3664(11) y
C4 H4 . 0.9500 ?
C4 C5 . 1.4196(12) y
C5 H5 . 0.9500 ?
C5 C6 . 1.3855(11) y
C6 H6 . 0.9500 ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C8 . 1.5177(12) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C8 C9 . 1.5288(13) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 C10 . 1.5248(12) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C11 C12 . 1.5170(12) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C12 C13 . 1.5335(14) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C13 C14 . 1.5189(12) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C15 C16 . 1.5107(14) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C16 H16C . 0.9900 ?
C16 H16D . 0.9900 ?
C16 C17 . 1.510(2) ?
C16 C17A . 1.411(3) ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C17 C18 . 1.4755(16) ?
C17A H17C . 0.9900 ?
C17A H17D . 0.9900 ?
C17A C18 . 1.535(3) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C18 H18C . 0.9900 ?
C18 H18D . 0.9900 ?
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
C15 H15B O1 3_666 0.99 2.63 3.3695(14) 131.2
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
O1 C7 C8 C9 . . . . 34.54(8) ?
O2 C11 C12 C13 . . . . 31.49(8) ?
O3 C15 C16 C17 . . . . -30.31(15) ?
O3 C15 C16 C17A . . . . 1.4(2) ?
N1 C2 C3 C4 . . . . 2.67(10) ?
C1 C2 C3 C4 . . . . -177.20(7) ?
C2 N1 C6 C5 . . . . 0.86(12) ?
C2 C3 C4 C5 . . . . -0.71(11) ?
C3 C4 C5 C6 . . . . -1.14(11) ?
C4 C5 C6 N1 . . . . 1.12(13) ?
C6 N1 C2 C1 . . . . 177.20(7) ?
C6 N1 C2 C3 . . . . -2.67(9) ?
C7 O1 C10 C9 . . . . -5.96(9) ?
C7 C8 C9 C10 . . . . -37.15(9) ?
C8 C9 C10 O1 . . . . 27.22(9) ?
C10 O1 C7 C8 . . . . -18.19(8) ?
C11 O2 C14 C13 . . . . -14.18(9) ?
C11 C12 C13 C14 . . . . -39.06(8) ?
C12 C13 C14 O2 . . . . 33.23(9) ?
C14 O2 C11 C12 . . . . -11.21(8) ?
C15 O3 C18 C17 . . . . 4.90(13) ?
C15 O3 C18 C17A . . . . -26.28(19) ?
C15 C16 C17 C18 . . . . 32.73(16) ?
C15 C16 C17A C18 . . . . -17.3(3) ?
C16 C17 C18 O3 . . . . -23.87(15) ?
C16 C17A C18 O3 . . . . 26.7(3) ?
C18 O3 C15 C16 . . . . 16.25(13) ?
Li1 O1 C7 C8 . . . . -175.91(7) ?
Li1 O1 C10 C9 . . . . 150.06(8) ?
Li1 O2 C11 C12 . . . . 145.25(7) ?
Li1 O2 C14 C13 . . . . -164.78(8) ?
Li1 O3 C15 C16 . . . . 161.28(10) ?
Li1 O3 C18 C17 . . . . -146.62(11) ?
Li1 O3 C18 C17A . . . . -177.80(17) ?
Li1 N1 C2 C1 . . . . -1.37(10) ?
Li1 N1 C2 C3 . . . . 178.76(6) ?
Li1 N1 C6 C5 . . . . 179.37(8) ?