#------------------------------------------------------------------------------
#$Date: 2019-07-30 07:29:56 +0300 (Tue, 30 Jul 2019) $
#$Revision: 217306 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021735.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_2021735
loop_
_publ_author_name
'Bogdanov, Georgii'
'Tillotson, John P.'
'Khrustalev, Victor N.'
'Rigin, Sergei'
'Timofeeva, Tatiana V.'
_publ_section_title
;
Synthesis, crystal structure studies and solvatochromic behaviour of two
2-{5-[4-(dimethylamino)phenyl]penta-2,4-dien-1-ylidene}malononitrile
derivatives
;
_journal_coeditor_code JX3037
_journal_issue 8
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 1175
_journal_page_last 1181
_journal_paper_doi 10.1107/S2053229619010398
_journal_volume 75
_journal_year 2019
_chemical_formula_moiety 'C16 H15 N3'
_chemical_formula_sum 'C16 H15 N3'
_chemical_formula_weight 249.31
_chemical_name_systematic
;
2-{5-[4-(Dimethylamino)phenyl]penta-2,4-dien-1-ylidene}malononitrile
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary difmap
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2017/1
_cell_angle_alpha 90
_cell_angle_beta 104.9826(18)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 16.9417(3)
_cell_length_b 7.45114(13)
_cell_length_c 23.0287(4)
_cell_measurement_reflns_used 11249
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 73.5429
_cell_measurement_theta_min 3.7409
_cell_volume 2808.20(9)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
Mercury (Macrae et al., 2008)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2017 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Atlas detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0275
_diffrn_reflns_av_unetI/netI 0.0168
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 27221
_diffrn_reflns_theta_full 72.000
_diffrn_reflns_theta_max 73.705
_diffrn_reflns_theta_min 3.974
_diffrn_source 'sealed X-ray tube'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.560
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.58376
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.179
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1056
_exptl_crystal_size_max 0.350
_exptl_crystal_size_mid 0.140
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.246
_refine_diff_density_min -0.228
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 347
_refine_ls_number_reflns 5596
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.046
_refine_ls_R_factor_all 0.0436
_refine_ls_R_factor_gt 0.0380
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1015
_refine_ls_wR_factor_ref 0.1079
_reflns_number_gt 4914
_reflns_number_total 5596
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jx3037sup1.cif
_cod_data_source_block DCV3
_cod_database_code 2021735
_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 0.828
_shelx_estimated_absorpt_t_max 0.989
_shelx_hkl_file
;
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10 2 -17 1097.82 66.7223 3
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10 -2 -17 1071.55 107.672 7
10 -2 -17 1145.93 108.433 10
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10 -2 -16 2161.48 143.855 21
10 2 -16 2286.49 123.868 21
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10 -2 -16 2200.97 151.466 7
10 -2 -16 2371.32 153.399 10
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10 -2 -15 2861.68 162.023 21
10 2 -15 2678.54 129.339 21
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10 -2 -15 2870.86 169.613 7
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10 -2 -15 2891.49 164.620 10
10 -2 -15 2843.79 270.385 1
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10 2 -14 21.2309 18.5116 13
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10 -2 -14 68.9680 34.6364 7
10 -2 -14 17.2881 28.8964 10
10 -2 -14 15.5995 20.8099 21
10 -2 -14 59.8891 43.6422 1
-10 -2 13 4761.77 162.058 14
10 2 -13 5001.53 180.544 13
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10 -2 -13 4698.82 339.002 1
10 -2 -13 4713.50 207.915 7
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10 -2 -13 4968.54 205.831 10
10 -2 -13 4533.91 193.395 21
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10 -2 -12 59.5301 29.0224 21
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10 -2 -12 78.7247 30.6900 7
10 -2 -12 67.1258 54.0318 1
10 -2 -12 93.9382 36.9552 10
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10 -2 -11 2026.46 217.313 1
10 -2 -11 2117.10 125.680 21
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10 -2 -10 3149.81 264.996 1
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10 -2 -10 3637.87 168.658 7
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10 -2 -10 3692.36 166.541 10
10 -2 -10 3494.99 156.608 21
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10 -2 -9 794.161 132.498 1
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10 2 -8 156.991 55.5741 19
10 -2 -8 93.8110 47.2949 19
10 -2 -8 70.9478 50.9402 1
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10 -2 -7 373.222 93.9062 1
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10 -2 -7 545.645 105.712 19
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10 -2 -6 53.0568 47.4673 1
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10 -2 -6 174.331 61.9547 19
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10 -2 -5 390.686 90.7885 1
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10 -2 -4 180.526 61.4618 1
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10 -2 -3 300.298 79.1601 19
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10 -2 -2 10436.4 482.511 1
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10 -2 2 29.1075 27.1647 19
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10 -2 3 203.132 59.0069 19
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10 -3 -25 1126.71 70.1120 7
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10 -3 -24 211.741 36.0051 10
10 -3 -24 214.825 38.4841 7
10 -3 -24 148.996 21.6396 17
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10 -3 -23 1496.93 78.2756 17
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10 -3 -22 685.408 74.7128 7
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10 -3 -22 681.261 59.2603 17
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10 -3 -21 1061.64 92.8061 21
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10 -3 -21 1138.45 103.051 7
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10 -3 -21 1108.84 82.4966 17
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10 -3 -20 395.365 65.6772 21
10 3 -20 416.062 50.8419 21
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10 -3 -20 548.210 74.5529 10
10 -3 -20 453.844 69.1096 7
10 -3 -20 524.964 63.3536 17
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10 3 -19 363.822 51.1520 21
10 3 -19 324.802 36.0073 3
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10 -3 -19 331.634 62.4576 7
10 -3 -19 316.516 59.1932 21
10 -3 -19 390.450 64.4031 10
10 -3 -19 376.221 56.4104 17
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10 -3 -18-2.02866 30.2690 21
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10 -3 -18 42.7170 30.6847 7
10 -3 -18 47.2226 38.0617 10
10 -3 -18 4.06359 20.9669 17
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10 -3 -17 132.303 41.9477 21
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10 -3 -17 139.562 44.9918 7
10 -3 -17 150.392 46.4023 10
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10 -3 -16 2323.89 155.908 7
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10 -3 -16 2570.27 160.588 10
10 -3 -16 2470.34 156.629 21
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10 3 -15 2025.51 117.408 13
10 -3 -15 1880.45 136.932 7
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10 -3 -15 1895.45 137.502 10
10 -3 -15 1844.99 133.864 21
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10 -3 -14 818.494 90.3551 21
10 -3 -14 774.147 87.9221 7
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10 -3 -14 794.157 88.9278 10
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10 -3 -13 291.008 54.0642 21
10 3 -13 308.383 48.6937 13
10 -3 -13 275.948 94.6429 1
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10 -3 -13 309.497 57.1282 7
10 -3 -13 301.924 52.9543 10
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10 -3 -12 492.601 68.1448 7
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10 -3 -12 576.031 72.4226 10
10 -3 -12 547.884 116.969 1
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10 3 -11 2081.02 118.834 13
10 -3 -11 2039.84 224.547 1
10 -3 -11 1908.07 130.569 7
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10 -3 -10 53.7741 42.0435 1
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10 -3 -10 4.88753 22.7788 7
10 -3 -10 33.1350 28.5600 10
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10 -3 -9 307.045 53.7112 7
10 -3 -9 339.545 53.5971 10
10 -3 -9 284.134 84.8418 1
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10 3 -8 24.5991 24.1548 13
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10 -3 -8-16.0917 17.2126 7
10 -3 -8-38.2669 36.7899 1
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10 -3 -7 385.638 98.0774 1
10 -3 -7 379.978 55.8997 7
-10 -3 7 343.120 46.5599 6
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-10 3 7 374.485 36.4339 14
-10 -3 6 1715.75 87.8153 14
10 3 -6 2036.89 117.199 13
-10 -3 6 1849.22 161.303 12
10 -3 -6 1973.90 123.625 7
10 -3 -6 1784.92 203.276 1
-10 -3 6 1793.97 101.912 6
-10 3 6 1989.26 80.4354 14
10 3 -5 3402.61 151.051 13
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10 3 -5 3244.31 231.817 19
10 -3 -5 3616.06 163.833 7
10 -3 -5 3329.23 261.404 19
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10 -3 -5 3100.56 271.265 1
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-10 3 4 3.14501 13.5652 14
-10 3 4 31.7601 21.1270 2
10 3 -4-18.1196 26.8851 13
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10 3 -4 14.2616 17.4557 19
10 -3 -4-26.2983 32.3217 19
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10 3 -3 2324.89 128.356 13
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10 3 -3 2201.50 202.025 19
10 -3 -3 2496.81 220.676 19
-10 3 3 2200.40 150.656 2
10 -3 -3 1995.36 221.080 1
-10 -3 3 2394.19 113.636 6
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-10 3 2 23.2722 17.4937 14
-10 3 2 56.7139 34.2020 2
10 3 -2 27.3767 22.7615 13
-10 -3 2 20.9789 18.7161 12
10 3 -2 69.2921 40.6550 19
10 -3 -2 66.9537 47.0394 19
10 -3 -2 18.9621 41.0275 1
10 -3 -2 27.5454 20.7763 15
-10 -3 2-2.99308 17.2829 6
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10 3 -1 8571.02 420.077 19
10 -3 -1 8918.10 401.181 19
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10 -3 -1 8938.59 474.580 1
-10 -3 1 9209.17 219.187 6
10 -3 -1 9469.26 238.140 15
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-10 -3 0 1562.55 62.5159 8
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10 3 0 1270.36 171.063 19
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10 -3 0 1451.72 192.679 1
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10 -3 0 1499.97 97.9252 15
-10 3 0 1440.27 92.8936 9
-10 3 0 1395.91 70.4242 14
-10 -3 -1 1922.38 70.8017 8
10 3 1 1859.16 121.889 13
10 3 1 1967.60 215.054 19
10 -3 1 1933.34 180.439 19
-10 3 -1 1911.13 153.318 2
-10 -3 -1 1818.00 97.5262 6
10 -3 1 1953.24 114.327 15
-10 3 -1 1921.02 107.919 9
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-10 -3 -2 843.072 48.6979 8
-10 3 -2 782.243 100.019 2
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-10 3 -2 829.430 72.4399 9
-10 3 -2 779.604 54.0952 14
-10 -3 -3 1915.11 74.3572 8
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-10 3 -3 1773.72 151.874 2
-10 -3 -3 1853.65 99.7834 6
-10 -3 -3 1881.65 112.549 16
10 -3 3 1935.45 118.202 15
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-20 -2 4-11.9705 13.9310 16
20 -2 -4-5.39317 11.5230 15
-20 2 4 20.1826 11.1363 9
-20 -2 3 343.370 32.5015 16
20 -2 -3 386.310 36.4017 15
-20 2 3 371.993 34.3062 9
-20 -2 2 15.5575 9.54771 16
20 -2 -2 15.2442 12.8139 15
-20 2 2 15.6898 10.5364 9
-20 -2 1 914.993 47.7268 16
20 -2 -1 838.271 48.0779 15
-20 2 1 991.233 49.9825 9
21 0 -9-1.90599 8.37370 15
21 0 -8 267.216 28.0203 15
21 0 -7 11.2942 8.00980 15
21 0 -6 1038.90 52.8962 15
0 0 0 0.00 0.00 0
TITL tvt05 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 16.941692 7.451142 23.028692 90.0000 104.9826 90.0000
ZERR 8.00 0.000296 0.000129 0.000405 0.0000 0.0018 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N
UNIT 128.00 120.00 24.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 97125
_shelx_res_file
;
TITL
DCV3.res
created by SHELXL-2017/1 at 16:56:56 on 20-Sep-2018
CELL 1.54184 16.941692 7.451142 23.028692 90 104.9826 90
ZERR 8 0.000296 0.000129 0.000405 0 0.0018 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N
UNIT 128 120 24
L.S. 6
PLAN 20
TEMP -173
BOND $H
MPLA C1a c12a c13a c14a c16a c4a c9a c8a c6a c5a n4a
MPLA C1b c12b c13b c14b c16b c4b c9b c8b c6b c5b n4b
CONF
EQIV $1 x+1, -y+3/2, z+1/2
HTAB C10A N2A_$1
fmap 2
acta 144
REM
REM
REM
WGHT 0.056100 0.684400
FVAR 2.64562
N2A 3 0.062476 0.800318 0.486080 11.00000 0.02360 0.07474 =
0.06460 -0.01437 -0.00596 0.00709
N3A 3 0.285081 0.545909 0.460143 11.00000 0.03454 0.03475 =
0.03509 -0.00332 0.01035 -0.00299
N4A 3 0.827981 0.686289 0.882889 11.00000 0.01707 0.02983 =
0.02509 -0.00196 0.00255 0.00036
C1A 1 0.216004 0.735199 0.526993 11.00000 0.01713 0.02461 =
0.02944 0.00213 0.00258 -0.00045
C2A 1 0.130740 0.772098 0.504159 11.00000 0.02328 0.03926 =
0.03800 -0.00571 0.00044 0.00043
C3A 1 0.253802 0.631458 0.489271 11.00000 0.02169 0.02596 =
0.02701 0.00196 0.00173 -0.00422
C4A 1 0.750544 0.723073 0.849323 11.00000 0.01833 0.01863 =
0.02533 0.00082 0.00389 -0.00260
C5A 1 0.692073 0.799873 0.875962 11.00000 0.02084 0.02116 =
0.02175 -0.00112 0.00379 -0.00297
AFIX 43
H5A 2 0.706959 0.828252 0.917595 11.00000 -1.20000
AFIX 0
C6A 1 0.613685 0.833980 0.842130 11.00000 0.02041 0.01975 =
0.02586 -0.00057 0.00639 -0.00130
AFIX 43
H6A 2 0.575881 0.886870 0.861154 11.00000 -1.20000
AFIX 0
C7A 1 0.587661 0.793406 0.780568 11.00000 0.02013 0.01797 =
0.02423 0.00103 0.00326 -0.00227
C8A 1 0.646319 0.718542 0.753993 11.00000 0.02270 0.02254 =
0.02206 -0.00086 0.00374 -0.00242
AFIX 43
H8A 2 0.631024 0.690352 0.712348 11.00000 -1.20000
AFIX 0
C9A 1 0.725282 0.685165 0.786842 11.00000 0.02124 0.02236 =
0.02641 -0.00178 0.00640 -0.00151
AFIX 43
H9A 2 0.763399 0.636009 0.767350 11.00000 -1.20000
AFIX 0
C10A 1 0.854024 0.743299 0.945310 11.00000 0.02089 0.03789 =
0.02729 -0.00416 0.00099 -0.00009
AFIX 137
H10A 2 0.852240 0.874562 0.947330 11.00000 -1.50000
H10B 2 0.909967 0.701822 0.963037 11.00000 -1.50000
H10C 2 0.817418 0.691944 0.967642 11.00000 -1.50000
AFIX 0
C11A 1 0.890751 0.626950 0.854343 11.00000 0.02011 0.03439 =
0.03282 -0.00439 0.00432 0.00416
AFIX 137
H11A 2 0.871072 0.521883 0.829159 11.00000 -1.50000
H11B 2 0.940306 0.595055 0.885314 11.00000 -1.50000
H11C 2 0.903123 0.723971 0.829343 11.00000 -1.50000
AFIX 0
C12A 1 0.259133 0.795600 0.581908 11.00000 0.02078 0.02108 =
0.02853 0.00207 0.00571 0.00040
AFIX 43
H12A 2 0.230592 0.863249 0.604962 11.00000 -1.20000
AFIX 0
C13A 1 0.343458 0.764505 0.606938 11.00000 0.01962 0.02098 =
0.02660 0.00120 0.00439 -0.00012
AFIX 43
H13A 2 0.373680 0.704052 0.583396 11.00000 -1.20000
AFIX 0
C14A 1 0.382860 0.817984 0.663478 11.00000 0.02084 0.01992 =
0.02712 0.00172 0.00484 -0.00019
AFIX 43
H14A 2 0.352602 0.882770 0.686008 11.00000 -1.20000
AFIX 0
C15A 1 0.466954 0.782431 0.690890 11.00000 0.02045 0.02176 =
0.02596 0.00132 0.00396 0.00004
AFIX 43
H15A 2 0.498461 0.724196 0.667806 11.00000 -1.20000
AFIX 0
C16A 1 0.503817 0.828154 0.748432 11.00000 0.02097 0.01943 =
0.02649 0.00159 0.00571 -0.00068
AFIX 43
H16A 2 0.471131 0.889509 0.769931 11.00000 -1.20000
AFIX 0
N2B 3 0.726181 0.935409 0.540552 11.00000 0.02483 0.03554 =
0.03548 0.00292 0.00399 -0.00156
N3B 3 0.520139 0.621850 0.570394 11.00000 0.03140 0.03118 =
0.03293 0.00011 0.01205 0.00201
N4B 3 -0.051742 0.757281 0.159116 11.00000 0.02326 0.04127 =
0.02769 0.00425 0.00076 -0.00339
C1B 1 0.578675 0.819046 0.499068 11.00000 0.01972 0.02264 =
0.02801 -0.00259 0.00697 0.00049
C2B 1 0.660679 0.883482 0.521814 11.00000 0.02450 0.02565 =
0.02723 0.00098 0.00740 0.00263
C3B 1 0.547300 0.708747 0.539085 11.00000 0.02127 0.02573 =
0.02647 -0.00385 0.00483 0.00229
C4B 1 0.029015 0.773464 0.188583 11.00000 0.02296 0.02287 =
0.02439 -0.00173 0.00362 0.00042
C5B 1 0.084271 0.863700 0.162115 11.00000 0.02914 0.02622 =
0.02353 0.00326 0.00355 -0.00100
AFIX 43
H5B 2 0.065020 0.914725 0.123211 11.00000 -1.20000
AFIX 0
C6B 1 0.165701 0.878721 0.191949 11.00000 0.02746 0.02381 =
0.02638 0.00109 0.00820 -0.00341
AFIX 43
H6B 2 0.201216 0.939349 0.172628 11.00000 -1.20000
AFIX 0
C7B 1 0.198356 0.808336 0.249599 11.00000 0.02316 0.02005 =
0.02414 -0.00122 0.00580 0.00055
C8B 1 0.143447 0.716321 0.275665 11.00000 0.02407 0.02662 =
0.02300 0.00265 0.00472 0.00019
AFIX 43
H8B 2 0.163285 0.664412 0.314380 11.00000 -1.20000
AFIX 0
C9B 1 0.061734 0.699442 0.246596 11.00000 0.02437 0.02812 =
0.02469 0.00193 0.00681 -0.00245
AFIX 43
H9B 2 0.026616 0.636962 0.265806 11.00000 -1.20000
AFIX 0
C10B 1 -0.082231 0.835529 0.099978 11.00000 0.02988 0.06134 =
0.03433 0.01260 -0.00520 -0.00558
AFIX 137
H10D 2 -0.073492 0.965625 0.102372 11.00000 -1.50000
H10E 2 -0.140778 0.810377 0.085156 11.00000 -1.50000
H10F 2 -0.053054 0.783531 0.072392 11.00000 -1.50000
AFIX 0
C11B 1 -0.109120 0.671654 0.186113 11.00000 0.02465 0.06551 =
0.04091 0.01350 0.00157 -0.00922
AFIX 137
H11D 2 -0.088805 0.552333 0.200560 11.00000 -1.50000
H11E 2 -0.161843 0.659886 0.156271 11.00000 -1.50000
H11F 2 -0.115976 0.744148 0.219980 11.00000 -1.50000
AFIX 0
C12B 1 0.531959 0.862800 0.443239 11.00000 0.02276 0.02142 =
0.02777 -0.00219 0.00874 0.00156
AFIX 43
H12B 2 0.556126 0.935891 0.418722 11.00000 -1.20000
AFIX 0
C13B 1 0.449782 0.807120 0.419023 11.00000 0.02183 0.02218 =
0.02835 -0.00184 0.00771 0.00066
AFIX 43
H13B 2 0.423801 0.738391 0.443515 11.00000 -1.20000
AFIX 0
C14B 1 0.406946 0.848640 0.362039 11.00000 0.02305 0.02281 =
0.02868 -0.00149 0.00797 0.00020
AFIX 43
H14B 2 0.433744 0.916488 0.337859 11.00000 -1.20000
AFIX 0
C15B 1 0.324119 0.796385 0.336375 11.00000 0.02254 0.02417 =
0.02807 -0.00017 0.00687 -0.00033
AFIX 43
H15B 2 0.296749 0.727550 0.359934 11.00000 -1.20000
AFIX 0
C16B 1 0.283349 0.841614 0.279657 11.00000 0.02328 0.02177 =
0.02858 -0.00126 0.00809 -0.00092
AFIX 43
H16B 2 0.314240 0.902680 0.256732 11.00000 -1.20000
AFIX 0
HKLF 4
REM
REM R1 = 0.0380 for 4914 Fo > 4sig(Fo) and 0.0436 for all 5596 data
REM 347 parameters refined using 0 restraints
END
WGHT 0.0560 0.6838
REM Highest difference peak 0.246, deepest hole -0.228, 1-sigma level 0.040
Q1 1 -0.0946 0.6172 0.2287 11.00000 0.05 0.25
Q2 1 0.5481 0.7875 0.7672 11.00000 0.05 0.18
Q3 1 -0.0968 0.5605 0.1694 11.00000 0.05 0.17
Q4 1 0.4304 0.8000 0.6773 11.00000 0.05 0.17
Q5 1 0.7229 0.7763 0.8608 11.00000 0.05 0.17
Q6 1 0.6523 0.7744 0.8581 11.00000 0.05 0.16
Q7 1 0.2384 0.8329 0.2690 11.00000 0.05 0.16
Q8 1 0.6012 0.8000 0.8088 11.00000 0.05 0.15
Q9 1 0.7409 0.7118 0.8195 11.00000 0.05 0.15
Q10 1 -0.0478 0.8619 0.0692 11.00000 0.05 0.14
Q11 1 0.6750 0.6889 0.7744 11.00000 0.05 0.13
Q12 1 0.1213 0.8774 0.1793 11.00000 0.05 0.12
Q13 1 0.1776 0.7569 0.2584 11.00000 0.05 0.12
Q14 1 0.0509 0.8626 0.1826 11.00000 0.05 0.12
Q15 1 0.7893 0.6816 0.8683 11.00000 0.05 0.12
Q16 1 0.3008 0.7820 0.5912 11.00000 0.05 0.12
Q17 1 0.4675 0.8917 0.7896 11.00000 0.05 0.12
Q18 1 0.3665 0.8092 0.3489 11.00000 0.05 0.12
Q19 1 0.1792 0.8631 0.2291 11.00000 0.05 0.12
Q20 1 0.3118 0.9734 0.2569 11.00000 0.05 0.12
;
_shelx_res_checksum 65486
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
N N2A 0.06248(7) 0.8003(2) 0.48608(6) 0.0575(4) Uani d 1
N N3A 0.28508(6) 0.54591(15) 0.46014(5) 0.0345(2) Uani d 1
N N4A 0.82798(5) 0.68629(13) 0.88289(4) 0.0245(2) Uani d 1
C C1A 0.21600(6) 0.73520(15) 0.52699(5) 0.0244(2) Uani d 1
C C2A 0.13074(7) 0.77210(18) 0.50416(6) 0.0349(3) Uani d 1
C C3A 0.25380(6) 0.63146(15) 0.48927(5) 0.0257(2) Uani d 1
C C4A 0.75054(6) 0.72307(14) 0.84932(5) 0.0211(2) Uani d 1
C C5A 0.69207(6) 0.79987(14) 0.87596(5) 0.0216(2) Uani d 1
H H5A 0.706959 0.828252 0.917595 0.026 Uiso calc 1
C C6A 0.61369(6) 0.83398(14) 0.84213(5) 0.0219(2) Uani d 1
H H6A 0.575881 0.886870 0.861154 0.026 Uiso calc 1
C C7A 0.58766(6) 0.79341(14) 0.78057(5) 0.0212(2) Uani d 1
C C8A 0.64632(6) 0.71854(14) 0.75399(5) 0.0228(2) Uani d 1
H H8A 0.631024 0.690352 0.712348 0.027 Uiso calc 1
C C9A 0.72528(6) 0.68516(14) 0.78684(5) 0.0233(2) Uani d 1
H H9A 0.763399 0.636009 0.767350 0.028 Uiso calc 1
C C10A 0.85402(7) 0.74330(18) 0.94531(5) 0.0297(3) Uani d 1
H H10A 0.852240 0.874562 0.947330 0.044 Uiso calc 1
H H10B 0.909967 0.701822 0.963037 0.044 Uiso calc 1
H H10C 0.817418 0.691944 0.967642 0.044 Uiso calc 1
C C11A 0.89075(6) 0.62695(17) 0.85434(5) 0.0296(3) Uani d 1
H H11A 0.871072 0.521883 0.829159 0.044 Uiso calc 1
H H11B 0.940306 0.595055 0.885314 0.044 Uiso calc 1
H H11C 0.903123 0.723971 0.829343 0.044 Uiso calc 1
C C12A 0.25913(6) 0.79560(14) 0.58191(5) 0.0236(2) Uani d 1
H H12A 0.230592 0.863249 0.604962 0.028 Uiso calc 1
C C13A 0.34346(6) 0.76451(15) 0.60694(5) 0.0227(2) Uani d 1
H H13A 0.373680 0.704052 0.583396 0.027 Uiso calc 1
C C14A 0.38286(6) 0.81798(14) 0.66348(5) 0.0229(2) Uani d 1
H H14A 0.352602 0.882770 0.686008 0.027 Uiso calc 1
C C15A 0.46695(6) 0.78243(14) 0.69089(5) 0.0231(2) Uani d 1
H H15A 0.498461 0.724196 0.667806 0.028 Uiso calc 1
C C16A 0.50382(6) 0.82815(14) 0.74843(5) 0.0224(2) Uani d 1
H H16A 0.471131 0.889509 0.769931 0.027 Uiso calc 1
N N2B 0.72618(6) 0.93541(15) 0.54055(4) 0.0327(2) Uani d 1
N N3B 0.52014(6) 0.62185(14) 0.57039(4) 0.0311(2) Uani d 1
N N4B -0.05174(6) 0.75728(15) 0.15912(4) 0.0318(2) Uani d 1
C C1B 0.57868(6) 0.81905(15) 0.49907(5) 0.0233(2) Uani d 1
C C2B 0.66068(6) 0.88348(15) 0.52181(5) 0.0257(2) Uani d 1
C C3B 0.54730(6) 0.70875(15) 0.53908(5) 0.0247(2) Uani d 1
C C4B 0.02901(6) 0.77346(15) 0.18858(5) 0.0239(2) Uani d 1
C C5B 0.08427(7) 0.86370(16) 0.16212(5) 0.0269(2) Uani d 1
H H5B 0.065020 0.914725 0.123211 0.032 Uiso calc 1
C C6B 0.16570(7) 0.87872(15) 0.19195(5) 0.0257(2) Uani d 1
H H6B 0.201216 0.939349 0.172628 0.031 Uiso calc 1
C C7B 0.19836(6) 0.80834(14) 0.24960(5) 0.0225(2) Uani d 1
C C8B 0.14345(7) 0.71632(15) 0.27566(5) 0.0248(2) Uani d 1
H H8B 0.163285 0.664412 0.314380 0.030 Uiso calc 1
C C9B 0.06173(7) 0.69944(15) 0.24660(5) 0.0256(2) Uani d 1
H H9B 0.026616 0.636962 0.265806 0.031 Uiso calc 1
C C10B -0.08223(8) 0.8355(2) 0.09998(6) 0.0443(3) Uani d 1
H H10D -0.073492 0.965625 0.102372 0.067 Uiso calc 1
H H10E -0.140778 0.810377 0.085156 0.067 Uiso calc 1
H H10F -0.053054 0.783531 0.072392 0.067 Uiso calc 1
C C11B -0.10912(8) 0.6717(2) 0.18611(6) 0.0450(4) Uani d 1
H H11D -0.088805 0.552333 0.200560 0.067 Uiso calc 1
H H11E -0.161843 0.659886 0.156271 0.067 Uiso calc 1
H H11F -0.115976 0.744148 0.219980 0.067 Uiso calc 1
C C12B 0.53196(6) 0.86280(15) 0.44324(5) 0.0236(2) Uani d 1
H H12B 0.556126 0.935891 0.418722 0.028 Uiso calc 1
C C13B 0.44978(6) 0.80712(15) 0.41902(5) 0.0239(2) Uani d 1
H H13B 0.423801 0.738391 0.443515 0.029 Uiso calc 1
C C14B 0.40695(6) 0.84864(15) 0.36204(5) 0.0246(2) Uani d 1
H H14B 0.433744 0.916488 0.337859 0.030 Uiso calc 1
C C15B 0.32412(6) 0.79638(15) 0.33637(5) 0.0249(2) Uani d 1
H H15B 0.296749 0.727550 0.359934 0.030 Uiso calc 1
C C16B 0.28335(6) 0.84161(15) 0.27966(5) 0.0243(2) Uani d 1
H H16B 0.314240 0.902680 0.256732 0.029 Uiso calc 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
N2A 0.0236(6) 0.0747(10) 0.0646(8) 0.0071(6) -0.0060(5) -0.0144(7)
N3A 0.0345(5) 0.0348(6) 0.0351(5) -0.0030(4) 0.0104(4) -0.0033(5)
N4A 0.0171(4) 0.0298(5) 0.0251(4) 0.0004(4) 0.0025(3) -0.0020(4)
C1A 0.0171(5) 0.0246(6) 0.0294(5) -0.0005(4) 0.0026(4) 0.0021(4)
C2A 0.0233(6) 0.0393(7) 0.0380(6) 0.0004(5) 0.0004(5) -0.0057(5)
C3A 0.0217(5) 0.0260(6) 0.0270(5) -0.0042(4) 0.0017(4) 0.0020(4)
C4A 0.0183(5) 0.0186(5) 0.0253(5) -0.0026(4) 0.0039(4) 0.0008(4)
C5A 0.0208(5) 0.0212(5) 0.0218(5) -0.0030(4) 0.0038(4) -0.0011(4)
C6A 0.0204(5) 0.0197(5) 0.0259(5) -0.0013(4) 0.0064(4) -0.0006(4)
C7A 0.0201(5) 0.0180(5) 0.0242(5) -0.0023(4) 0.0033(4) 0.0010(4)
C8A 0.0227(5) 0.0225(5) 0.0221(5) -0.0024(4) 0.0037(4) -0.0009(4)
C9A 0.0212(5) 0.0224(5) 0.0264(5) -0.0015(4) 0.0064(4) -0.0018(4)
C10A 0.0209(5) 0.0379(7) 0.0273(5) -0.0001(5) 0.0010(4) -0.0042(5)
C11A 0.0201(5) 0.0344(6) 0.0328(6) 0.0042(5) 0.0043(4) -0.0044(5)
C12A 0.0208(5) 0.0211(5) 0.0285(5) 0.0004(4) 0.0057(4) 0.0021(4)
C13A 0.0196(5) 0.0210(5) 0.0266(5) -0.0001(4) 0.0044(4) 0.0012(4)
C14A 0.0208(5) 0.0199(5) 0.0271(5) -0.0002(4) 0.0048(4) 0.0017(4)
C15A 0.0205(5) 0.0218(5) 0.0260(5) 0.0000(4) 0.0040(4) 0.0013(4)
C16A 0.0210(5) 0.0194(5) 0.0265(5) -0.0007(4) 0.0057(4) 0.0016(4)
N2B 0.0248(5) 0.0355(6) 0.0355(5) -0.0016(4) 0.0040(4) 0.0029(4)
N3B 0.0314(5) 0.0312(5) 0.0329(5) 0.0020(4) 0.0121(4) 0.0001(4)
N4B 0.0233(5) 0.0413(6) 0.0277(5) -0.0034(4) 0.0008(4) 0.0043(4)
C1B 0.0197(5) 0.0226(5) 0.0280(5) 0.0005(4) 0.0070(4) -0.0026(4)
C2B 0.0245(5) 0.0257(6) 0.0272(5) 0.0026(4) 0.0074(4) 0.0010(4)
C3B 0.0213(5) 0.0257(6) 0.0265(5) 0.0023(4) 0.0048(4) -0.0039(4)
C4B 0.0230(5) 0.0229(5) 0.0244(5) 0.0004(4) 0.0036(4) -0.0017(4)
C5B 0.0291(6) 0.0262(6) 0.0235(5) -0.0010(4) 0.0036(4) 0.0033(4)
C6B 0.0275(5) 0.0238(6) 0.0264(5) -0.0034(4) 0.0082(4) 0.0011(4)
C7B 0.0232(5) 0.0200(5) 0.0241(5) 0.0005(4) 0.0058(4) -0.0012(4)
C8B 0.0241(5) 0.0266(6) 0.0230(5) 0.0002(4) 0.0047(4) 0.0026(4)
C9B 0.0244(5) 0.0281(6) 0.0247(5) -0.0024(4) 0.0068(4) 0.0019(4)
C10B 0.0299(6) 0.0613(9) 0.0343(6) -0.0056(6) -0.0052(5) 0.0126(6)
C11B 0.0246(6) 0.0655(10) 0.0409(7) -0.0092(6) 0.0016(5) 0.0135(7)
C12B 0.0228(5) 0.0214(5) 0.0278(5) 0.0016(4) 0.0087(4) -0.0022(4)
C13B 0.0218(5) 0.0222(5) 0.0283(5) 0.0007(4) 0.0077(4) -0.0018(4)
C14B 0.0230(5) 0.0228(5) 0.0287(5) 0.0002(4) 0.0080(4) -0.0015(4)
C15B 0.0225(5) 0.0242(6) 0.0281(5) -0.0003(4) 0.0069(4) -0.0002(4)
C16B 0.0233(5) 0.0218(5) 0.0286(5) -0.0009(4) 0.0081(4) -0.0013(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
N N 0.0311 0.0180 '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
C4A N4A C10A 120.13(9)
C4A N4A C11A 120.78(9)
C10A N4A C11A 117.70(9)
C12A C1A C2A 121.72(10)
C12A C1A C3A 121.64(10)
C2A C1A C3A 116.64(10)
N2A C2A C1A 179.47(17)
N3A C3A C1A 178.40(12)
N4A C4A C5A 120.88(9)
N4A C4A C9A 121.80(9)
C5A C4A C9A 117.31(9)
C6A C5A C4A 120.66(9)
C6A C5A H5A 119.7
C4A C5A H5A 119.7
C5A C6A C7A 122.41(9)
C5A C6A H6A 118.8
C7A C6A H6A 118.8
C6A C7A C8A 116.79(9)
C6A C7A C16A 119.26(9)
C8A C7A C16A 123.94(9)
C9A C8A C7A 121.74(9)
C9A C8A H8A 119.1
C7A C8A H8A 119.1
C8A C9A C4A 121.05(9)
C8A C9A H9A 119.5
C4A C9A H9A 119.5
N4A C10A H10A 109.5
N4A C10A H10B 109.5
H10A C10A H10B 109.5
N4A C10A H10C 109.5
H10A C10A H10C 109.5
H10B C10A H10C 109.5
N4A C11A H11A 109.5
N4A C11A H11B 109.5
H11A C11A H11B 109.5
N4A C11A H11C 109.5
H11A C11A H11C 109.5
H11B C11A H11C 109.5
C1A C12A C13A 124.52(10)
C1A C12A H12A 117.7
C13A C12A H12A 117.7
C14A C13A C12A 122.42(10)
C14A C13A H13A 118.8
C12A C13A H13A 118.8
C13A C14A C15A 123.79(10)
C13A C14A H14A 118.1
C15A C14A H14A 118.1
C16A C15A C14A 122.79(10)
C16A C15A H15A 118.6
C14A C15A H15A 118.6
C15A C16A C7A 126.83(10)
C15A C16A H16A 116.6
C7A C16A H16A 116.6
C4B N4B C11B 121.91(10)
C4B N4B C10B 119.96(10)
C11B N4B C10B 118.06(10)
C12B C1B C2B 122.37(10)
C12B C1B C3B 121.41(10)
C2B C1B C3B 116.20(9)
N2B C2B C1B 179.34(12)
N3B C3B C1B 178.21(12)
N4B C4B C5B 121.20(10)
N4B C4B C9B 122.05(10)
C5B C4B C9B 116.75(10)
C6B C5B C4B 120.90(10)
C6B C5B H5B 119.6
C4B C5B H5B 119.6
C5B C6B C7B 122.77(10)
C5B C6B H6B 118.6
C7B C6B H6B 118.6
C6B C7B C8B 116.32(10)
C6B C7B C16B 119.26(9)
C8B C7B C16B 124.33(10)
C9B C8B C7B 121.89(10)
C9B C8B H8B 119.1
C7B C8B H8B 119.1
C8B C9B C4B 121.36(10)
C8B C9B H9B 119.3
C4B C9B H9B 119.3
N4B C10B H10D 109.5
N4B C10B H10E 109.5
H10D C10B H10E 109.5
N4B C10B H10F 109.5
H10D C10B H10F 109.5
H10E C10B H10F 109.5
N4B C11B H11D 109.5
N4B C11B H11E 109.5
H11D C11B H11E 109.5
N4B C11B H11F 109.5
H11D C11B H11F 109.5
H11E C11B H11F 109.5
C1B C12B C13B 124.82(10)
C1B C12B H12B 117.6
C13B C12B H12B 117.6
C14B C13B C12B 122.42(10)
C14B C13B H13B 118.8
C12B C13B H13B 118.8
C13B C14B C15B 123.98(10)
C13B C14B H14B 118.0
C15B C14B H14B 118.0
C16B C15B C14B 122.22(10)
C16B C15B H15B 118.9
C14B C15B H15B 118.9
C15B C16B C7B 127.95(10)
C15B C16B H16B 116.0
C7B C16B H16B 116.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N2A C2A 1.1429(16)
N3A C3A 1.1493(15)
N4A C4A 1.3673(13)
N4A C10A 1.4538(14)
N4A C11A 1.4560(13)
C1A C12A 1.3631(15)
C1A C2A 1.4304(15)
C1A C3A 1.4317(16)
C4A C5A 1.4140(14)
C4A C9A 1.4195(14)
C5A C6A 1.3785(14)
C5A H5A 0.9500
C6A C7A 1.4044(14)
C6A H6A 0.9500
C7A C8A 1.4099(15)
C7A C16A 1.4453(14)
C8A C9A 1.3786(14)
C8A H8A 0.9500
C9A H9A 0.9500
C10A H10A 0.9800
C10A H10B 0.9800
C10A H10C 0.9800
C11A H11A 0.9800
C11A H11B 0.9800
C11A H11C 0.9800
C12A C13A 1.4146(14)
C12A H12A 0.9500
C13A C14A 1.3603(15)
C13A H13A 0.9500
C14A C15A 1.4260(14)
C14A H14A 0.9500
C15A C16A 1.3543(15)
C15A H15A 0.9500
C16A H16A 0.9500
N2B C2B 1.1488(14)
N3B C3B 1.1499(15)
N4B C4B 1.3663(14)
N4B C11B 1.4321(16)
N4B C10B 1.4483(15)
C1B C12B 1.3637(15)
C1B C2B 1.4348(14)
C1B C3B 1.4354(15)
C4B C5B 1.4124(15)
C4B C9B 1.4189(15)
C5B C6B 1.3775(15)
C5B H5B 0.9500
C6B C7B 1.4014(15)
C6B H6B 0.9500
C7B C8B 1.4087(15)
C7B C16B 1.4487(14)
C8B C9B 1.3789(15)
C8B H8B 0.9500
C9B H9B 0.9500
C10B H10D 0.9800
C10B H10E 0.9800
C10B H10F 0.9800
C11B H11D 0.9800
C11B H11E 0.9800
C11B H11F 0.9800
C12B C13B 1.4213(14)
C12B H12B 0.9500
C13B C14B 1.3609(15)
C13B H13B 0.9500
C14B C15B 1.4287(14)
C14B H14B 0.9500
C15B C16B 1.3528(15)
C15B H15B 0.9500
C16B H16B 0.9500
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
C10A H10B N2A 4_676 0.98 2.50 3.4270(16) 157.8 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
C10A N4A C4A C5A -6.58(16)
C11A N4A C4A C5A -172.79(10)
C10A N4A C4A C9A 173.84(10)
C11A N4A C4A C9A 7.64(16)
N4A C4A C5A C6A -178.93(10)
C9A C4A C5A C6A 0.67(15)
C4A C5A C6A C7A 0.68(16)
C5A C6A C7A C8A -1.29(16)
C5A C6A C7A C16A 178.18(10)
C6A C7A C8A C9A 0.54(16)
C16A C7A C8A C9A -178.89(10)
C7A C8A C9A C4A 0.79(17)
N4A C4A C9A C8A 178.20(10)
C5A C4A C9A C8A -1.39(16)
C2A C1A C12A C13A -179.71(11)
C3A C1A C12A C13A 0.33(17)
C1A C12A C13A C14A -175.85(11)
C12A C13A C14A C15A 177.39(10)
C13A C14A C15A C16A -176.21(10)
C14A C15A C16A C7A 178.11(10)
C6A C7A C16A C15A -173.54(10)
C8A C7A C16A C15A 5.88(18)
C11B N4B C4B C5B -177.81(12)
C10B N4B C4B C5B -0.83(18)
C11B N4B C4B C9B 2.91(18)
C10B N4B C4B C9B 179.89(12)
N4B C4B C5B C6B -179.66(11)
C9B C4B C5B C6B -0.35(16)
C4B C5B C6B C7B -0.58(18)
C5B C6B C7B C8B 1.36(16)
C5B C6B C7B C16B -175.39(10)
C6B C7B C8B C9B -1.25(16)
C16B C7B C8B C9B 175.31(10)
C7B C8B C9B C4B 0.38(17)
N4B C4B C9B C8B 179.75(11)
C5B C4B C9B C8B 0.44(16)
C2B C1B C12B C13B -178.17(10)
C3B C1B C12B C13B 0.21(17)
C1B C12B C13B C14B -177.27(10)
C12B C13B C14B C15B -179.43(10)
C13B C14B C15B C16B 179.43(11)
C14B C15B C16B C7B -175.48(10)
C6B C7B C16B C15B 174.95(11)
C8B C7B C16B C15B -1.52(19)
_cod_database_fobs_code 2021735