#------------------------------------------------------------------------------
#$Date: 2023-07-29 05:03:55 +0300 (Sat, 29 Jul 2023) $
#$Revision: 285386 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022831.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_2022831
loop_
_publ_author_name
'Nasr, Tamer'
'Kariuki, Benson M.'
'Elansary, Mai M.'
'Elhaggar, Radwan'
'Zaghary, Wafaa'
_publ_section_title
;
Synthesis and crystal structures of
(E)-N′-(4-chloro-3-nitrobenzylidene)acetohydrazide and
(E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine
;
_journal_coeditor_code JQ2029
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 762
_journal_page_last 766
_journal_paper_doi 10.1107/S2056989023006412
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C16 H12 Cl N3'
_chemical_formula_moiety 'C16 H12 Cl N3'
_chemical_formula_sum 'C16 H12 Cl N3'
_chemical_formula_weight 281.74
_chemical_name_common
;
8-{(E)-2-[(4-Chlorophenyl)methylidene]hydrazin-1-yl}quinoline
;
_chemical_name_systematic
;
(E)-2-(4-Chlorobenzylidene)-1-(quinolin-8-yl)hydrazine
;
_space_group_crystal_system monoclinic
_space_group_IT_number 7
_space_group_name_Hall 'P -2yac'
_space_group_name_H-M_alt 'P 1 n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 90
_cell_angle_beta 100.601(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.7968(3)
_cell_length_b 12.0926(4)
_cell_length_c 14.8738(5)
_cell_measurement_reflns_used 6539
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 72.6860
_cell_measurement_theta_min 3.6340
_cell_volume 1378.42(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Rigaku OD 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 0.0240
_diffrn_reflns_av_unetI/netI 0.0216
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 11753
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 72.752
_diffrn_reflns_theta_min 3.655
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 2.381
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.713
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.358
_exptl_crystal_description plate
_exptl_crystal_F_000 584
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.140
_exptl_crystal_size_min 0.070
_refine_diff_density_max 0.117
_refine_diff_density_min -0.138
_refine_ls_abs_structure_details
;
Flack x determined using 995 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.016(12)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 3869
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.038
_refine_ls_R_factor_all 0.0344
_refine_ls_R_factor_gt 0.0314
_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^)+(0.0484P)^2^+0.0525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0809
_refine_ls_wR_factor_ref 0.0847
_reflns_number_gt 3609
_reflns_number_total 3869
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jq2029sup1.cif
_cod_data_source_block VII
_cod_original_sg_symbol_H-M 'P n'
_cod_database_code 2022831
_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 0.576
_shelx_estimated_absorpt_t_max 0.851
_shelx_hkl_file
;
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0 0 -6 22625.0 493.827 4
0 0 -6 23510.0 622.184 2
0 0 -7-54.1198 52.6497 2
0 0 -7 183.032 50.2511 4
0 0 -8 10770.1 507.641 2
0 0 -9-38.0889 58.9033 2
0 0 10 5241.29 225.594 8
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0 0 11 4.68493 25.6803 10
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0 0 11 2.84428 28.0719 8
0 0 -11 5.70409 35.9439 2
0 0 12 1492.43 127.031 10
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0 0 12 1569.89 139.381 8
0 0 -12 1912.76 275.644 2
0 0 13 11.7352 35.2505 10
0 0 13-31.3269 39.3720 25
0 0 -13-15.8554 21.0368 29
0 0 13-46.4746 42.8275 8
0 0 14 195.540 55.5737 10
0 0 15 30.3158 42.9348 10
0 0 17 21.0239 23.1929 28
0 1 0 222.487 26.4243 4
0 1 0 242.140 28.9952 3
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0 1 -1 15274.6 184.884 2
0 -1 -2 19319.8 346.720 1
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0 1 -2 19290.4 268.598 3
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0 1 -9 219.641 78.2427 2
0 -1 -9 267.674 95.7589 2
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0 -1 -12 49.6681 57.4690 2
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0 -1 13 129.368 51.7892 8
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0 -1 14 190.745 58.0368 10
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0 2 -2 208071. 1075.33 3
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0 -2 -3 999999. 3238.24 1
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0 2 -4 607183. 2342.46 2
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-8 -3 -3 53.0907 31.3930 18
-8 3 -3 59.3171 33.1033 23
-8 3 -4 122.496 38.9719 16
-8 -3 -4 130.109 40.3700 16
-8 -3 -4 86.9980 28.8889 18
-8 3 -4 102.100 35.2463 23
-8 -3 -5 368.435 54.7629 16
-8 3 -5 308.848 41.6648 23
-8 -3 -6 7.73557 23.8716 16
-8 -4 11 79.3509 28.9628 13
-8 4 11 182.422 33.1520 23
-8 -4 10 15.1865 26.1732 13
-8 -4 10-32.9714 24.7969 18
-8 4 10 18.4977 20.6632 23
-8 -4 9 285.605 49.5689 13
-8 -4 9 278.198 48.9338 18
-8 4 9 304.798 46.3167 23
-8 -4 8 150.067 44.4180 18
-8 4 8 164.603 46.3307 23
-8 -4 7 878.597 90.1410 18
-8 4 7 898.362 85.1278 23
-8 -4 6 60.3432 45.2090 18
-8 4 6 50.1713 34.6688 23
-8 -4 5 841.537 94.7038 18
-8 4 5 529.861 71.3582 18
-8 4 5 733.639 83.9712 23
-8 4 4 614.075 91.6554 16
-8 4 4 463.837 66.7222 18
-8 4 4 582.789 76.3989 23
-8 -4 4 596.511 83.0622 18
-8 4 3 443.528 80.3469 16
-8 -4 3 488.520 63.5175 16
-8 4 3 575.196 75.8319 23
-8 -4 3 512.289 77.5293 18
-8 4 2 88.4139 51.0557 16
-8 -4 2 66.5694 32.9142 16
-8 -4 2 87.8438 50.0761 18
-8 4 2 103.275 43.1380 23
-8 -4 1 3297.15 164.132 16
-8 -4 1 3800.24 193.093 18
-8 4 1 3169.19 185.608 16
-8 4 1 3448.71 177.916 23
-8 4 0 35.4483 44.6554 16
-8 -4 0-7.57733 31.9637 16
-8 -4 0 44.4104 41.7778 18
-8 4 0 17.5850 34.0327 23
-8 4 -1 279.647 59.2796 16
-8 -4 -1 306.202 56.6959 16
-8 -4 -1 466.448 71.7011 18
-8 4 -1 337.590 58.2288 23
-8 4 -2 57.5525 33.9761 16
-8 -4 -2 77.8045 36.7674 16
-8 -4 -2 113.202 40.9288 18
-8 4 -2 67.8512 36.4849 23
-8 4 -3 273.516 48.5785 16
-8 -4 -3 283.662 54.0009 16
-8 -4 -3 292.802 52.8214 18
-8 4 -3 303.410 53.4028 23
-8 -4 -4 125.343 39.0334 16
-8 -4 -4 89.3005 28.8854 18
-8 4 -4 93.3181 33.3564 23
-8 -4 -5-33.8312 24.4233 16
-8 -4 -5-75.4680 23.5682 18
-8 4 -5 0.68769 19.9335 23
-8 -4 -6 12.0823 19.6139 16
-8 -5 10 300.651 43.0024 13
-8 5 10 483.068 51.1258 23
-8 -5 9 55.4120 27.4388 13
-8 -5 9 48.2700 24.2341 18
-8 5 9 51.0208 24.7309 23
-8 -5 8 251.459 44.4982 18
-8 5 8 325.406 52.1661 23
-8 -5 7 135.168 39.7530 18
-8 5 7 117.344 35.5218 23
-8 -5 6 614.920 72.7904 18
-8 5 6 677.620 77.0870 23
-8 -5 5 588.714 73.3501 18
-8 5 5 615.386 74.2206 23
-8 5 4 6.27616 35.7713 23
-8 -5 4 63.3538 36.2669 18
-8 5 3 424.111 64.4308 23
-8 -5 3 339.286 60.7232 18
-8 5 2 63.6806 47.5540 16
-8 -5 2 127.690 46.5071 18
-8 5 2 85.1903 42.2540 23
-8 5 1-13.5865 41.9237 16
-8 -5 1-21.6225 31.3802 16
-8 -5 1 74.1257 39.3058 18
-8 5 1 23.0361 35.5069 23
-8 5 0 321.792 59.4522 16
-8 -5 0 340.572 53.1609 16
-8 -5 0 377.594 64.1207 18
-8 5 0 347.988 62.0293 23
-8 5 -1-6.84415 30.1050 16
-8 -5 -1-4.07359 27.9433 16
-8 -5 -1 31.1171 31.9414 18
-8 5 -1-0.48624 31.9352 23
-8 5 -2 175.771 39.0805 16
-8 -5 -2 198.052 43.8236 16
-8 -5 -2 341.864 57.0266 18
-8 5 -2 281.184 50.9289 23
-8 -5 -3 43.7346 29.0340 16
-8 -5 -3 82.8792 34.3297 18
-8 5 -3 44.4175 32.1262 23
-8 -5 -4 208.862 39.8855 16
-8 -5 -4 262.911 43.9027 18
-8 5 -4 223.606 39.9056 23
-8 -5 -5 231.456 37.7950 16
-8 5 -5 235.291 35.7687 23
-8 -6 9 115.472 30.0603 13
-8 6 9 112.526 29.1088 23
-8 6 8 296.605 46.7700 23
-8 6 7 502.758 59.2582 23
-8 -6 7 421.143 51.3124 18
-8 -6 6 244.842 43.8293 18
-8 6 6 202.467 44.4402 23
-8 -6 5 453.053 60.0397 18
-8 6 5 521.039 67.9786 23
-8 -6 4 536.327 64.7575 18
-8 6 4 666.373 76.8411 23
-8 6 3 69.7071 33.4845 23
-8 -6 3 28.3202 30.0232 18
-8 -6 2 171.870 44.3272 18
-8 6 2 112.988 39.2724 23
-8 -6 1 251.398 51.3369 18
-8 6 1 207.914 48.2231 23
-8 -6 0 502.062 67.2886 18
-8 6 0 469.842 66.1536 23
-8 -6 -1 112.874 30.8776 16
-8 -6 -1 69.4061 32.9750 18
-8 6 -1 114.174 39.2048 23
-8 -6 -2 321.880 43.8312 16
-8 -6 -2 409.202 58.1391 18
-8 6 -2 416.386 57.9410 23
-8 -6 -3 118.617 27.9801 16
-8 -6 -3 44.0166 29.0573 18
-8 6 -3 61.2455 29.8044 23
-8 -6 -4 110.542 28.5841 18
-8 6 -4 146.329 30.6620 23
-8 -7 8 203.113 34.7763 13
-8 7 8 267.147 38.2188 23
-8 7 7 291.524 43.5229 23
-8 7 6 362.239 51.3087 23
-8 -7 5 22.2736 21.3664 18
-8 7 5-56.6683 33.6789 23
-8 7 4-18.5104 25.7789 23
-8 -7 4-24.0518 24.7995 18
-8 7 3 36.0271 31.6401 23
-8 -7 3 91.0504 29.0779 18
-8 -7 2 614.737 61.8560 18
-8 7 2 622.971 68.7193 23
-8 -7 1 272.803 45.0461 18
-8 7 1 387.545 55.3618 23
-8 -7 0 163.556 38.8155 18
-8 7 0 104.450 33.9799 23
-8 -7 -1 125.329 33.1435 18
-8 7 -1 129.348 35.0991 23
-8 -7 -2 170.040 33.9565 18
-8 7 -2 145.414 33.1654 23
-8 8 5 96.5917 26.8321 23
-8 8 4 84.0119 26.4500 23
-8 8 3 166.894 33.8903 23
-8 8 2 790.034 63.7562 23
-8 8 1 224.160 36.1914 23
-8 -8 1 176.015 30.4756 18
-8 8 0 99.4233 27.1479 23
-9 0 9 1364.04 86.3271 13
-9 0 8 2.26409 21.8065 13
-9 0 8 38.4862 27.2483 18
-9 0 7 524.819 59.2430 13
-9 0 7 567.084 69.3866 18
-9 0 6-51.0175 28.4570 13
-9 0 6-25.3107 36.2967 18
-9 0 5 172.360 44.4863 16
-9 0 5 201.986 50.0022 18
-9 0 4 68.3965 40.8689 16
-9 0 4 46.9738 34.7561 18
-9 0 3 94.7202 40.2634 16
-9 0 3 66.0602 36.1678 18
-9 0 2-45.7870 38.4169 16
-9 0 2 40.2292 31.2477 18
-9 0 1 346.180 61.1028 16
-9 0 1 311.486 48.5123 18
-9 0 0-13.7638 31.0637 16
-9 0 -1 504.883 66.2724 16
-9 0 -2-76.4022 33.3094 16
-9 0 -3 1022.50 74.4037 16
-9 -1 9 72.3996 28.7255 13
-9 1 8 637.819 59.6669 13
-9 -1 8 717.257 69.5796 13
-9 -1 8 797.217 74.2121 18
-9 1 7 58.7747 26.7399 13
-9 -1 7 76.2615 34.4521 13
-9 1 7 63.1562 33.6837 18
-9 -1 7 16.7364 31.4821 18
-9 -1 6 26.8656 24.5870 13
-9 1 6 61.9523 36.8041 18
-9 -1 6 56.1255 39.1295 18
-9 1 5 27.9401 31.6793 16
-9 -1 5 37.3405 26.5650 16
-9 -1 5 94.3417 32.6391 13
-9 1 5-40.9971 33.8841 18
-9 -1 5 22.3696 36.0305 18
-9 1 4 224.188 52.6184 16
-9 -1 4 205.173 48.7517 16
-9 1 4 203.665 47.3452 18
-9 -1 4 347.569 61.7099 18
-9 1 3-23.7580 36.9828 16
-9 -1 3-56.4810 31.0377 16
-9 1 3-18.1882 27.5096 18
-9 -1 3-41.4714 36.3071 18
-9 1 2 29.8114 32.3744 16
-9 -1 2 2.44566 32.5410 16
-9 1 2-26.3656 25.8643 18
-9 -1 2 29.8745 31.6638 18
-9 1 1 195.928 51.5548 16
-9 -1 1 185.342 49.5022 16
-9 -1 1 216.918 42.8211 18
-9 1 0 142.273 45.6967 16
-9 -1 0 163.692 45.0607 16
-9 -1 0 265.229 43.6738 18
-9 1 -1 168.481 44.6986 16
-9 -1 -1 162.150 42.1132 16
-9 1 -2 70.1713 32.7628 16
-9 -1 -2 12.2899 24.3558 16
-9 -1 -3 93.9416 29.9710 16
-9 -2 9 40.7956 25.4951 13
-9 -2 9 40.3283 21.8359 18
-9 -2 8 99.8051 30.6978 13
-9 -2 8 81.6428 29.9138 18
-9 -2 7 157.852 38.8424 13
-9 -2 7 186.163 42.6556 18
-9 -2 6 552.876 65.8551 13
-9 2 6 480.336 61.0933 18
-9 -2 6 483.971 64.5276 18
-9 -2 5 236.388 45.7162 13
-9 2 5 248.950 47.3749 18
-9 -2 5 270.275 54.9053 18
-9 2 4 114.475 42.0096 16
-9 -2 4 134.998 35.1815 16
-9 -2 4 151.951 38.7219 13
-9 2 4 109.830 34.9713 18
-9 2 3 273.944 57.0337 16
-9 -2 3 280.102 50.7155 16
-9 2 2 117.032 45.9292 16
-9 -2 2 70.7156 33.7512 16
-9 -2 2 75.2961 33.9066 18
-9 2 1 310.682 55.4049 16
-9 -2 1 328.415 55.7201 16
-9 -2 1 277.190 48.4810 18
-9 2 0 157.303 43.8020 16
-9 -2 0 37.4980 29.9354 16
-9 -2 0 113.609 34.0958 18
-9 2 -1 237.376 45.4893 16
-9 -2 -1 186.202 43.9671 16
-9 -2 -1 163.412 32.8763 18
-9 2 -2 15.8578 25.2833 16
-9 -2 -2-27.0016 25.1676 16
-9 -3 8 55.5160 25.7735 13
-9 -3 8 40.0675 22.0437 18
-9 -3 7 390.073 54.0815 13
-9 -3 7 395.424 52.1796 18
-9 -3 6 460.933 59.8089 13
-9 -3 6 392.232 55.8003 18
-9 -3 5 226.504 46.5316 13
-9 -3 5 238.063 49.1148 18
-9 -3 4 169.196 41.7224 18
-9 3 4 26.9018 21.9474 23
-9 3 3 221.839 49.5219 16
-9 -3 3 222.820 37.9844 16
-9 -3 3 311.858 54.4027 18
-9 3 3 191.209 33.5759 23
-9 3 2 189.140 47.9686 16
-9 -3 2 174.278 37.4521 16
-9 -3 2 166.156 41.8396 18
-9 3 1-8.36356 28.3023 16
-9 -3 1-67.2680 34.1148 18
-9 3 0 115.367 34.0901 16
-9 -3 0 70.5611 28.5037 16
-9 -3 0 91.8064 29.7733 18
-9 3 -1 274.376 42.8155 16
-9 -3 -1 195.740 36.7805 16
-9 -3 -1 300.137 42.1621 18
-9 -4 7 58.2581 26.8401 13
-9 -4 7 31.9143 19.9559 18
-9 -4 6 235.007 42.1577 13
-9 -4 6 179.717 35.5235 18
-9 -4 5 109.700 33.7866 18
-9 4 5 140.836 30.3259 23
-9 -4 4 277.192 48.3409 18
-9 4 4 141.645 27.7984 23
-9 -4 3 28.8467 25.8920 18
-9 4 3 5.37940 24.3866 23
-9 -4 2 691.479 69.5800 18
-9 4 2 703.542 61.0744 23
-9 -4 1 50.5992 27.0445 18
-9 -4 0 120.976 30.9707 18
-9 -5 5 546.582 53.5242 18
-9 -5 4 46.0097 22.8977 18
-9 -5 3 331.608 44.8561 18
-9 -5 2 72.4573 26.5818 18
-9 -5 1-2.38357 20.1195 18
0 0 0 0.00 0.00 0
TITL bmk2261c_auto in P2/n
REM P2/n (#13 in standard setting)
CELL 1.54184 7.796841 12.092623 14.873827 90.0000 100.6010 90.0000
ZERR 4.00 0.000270 0.000352 0.000493 0.0000 0.0031 0.0000
LATT 1
SYMM -x+1/2, y,-z+1/2
SFAC C H N Cl
UNIT 64.00 48.00 12.00 4.00
SIZE 0.07 0.14 0.26
TREF
HKLF 4
END
;
_shelx_hkl_checksum 9884
_shelx_res_file
;
TITL bmk2261c in Pn
shelx.res
created by SHELXL-2018/1 at 15:56:14 on 09-Jan-2023
CELL 1.54184 7.7968 12.0926 14.8738 90.000 100.601 90.000
ZERR 4.00 0.0003 0.0004 0.0005 0.000 0.003 0.000
LATT -1
SYMM 1/2 + X, - Y, 1/2 + Z
SFAC C H N CL
UNIT 64 48 12 4
MERG 2
MPLA C17 C18 C19 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32
MPLA N4 N5 N6 CL2
MPLA C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 N1 N2 N3
MPLA CL1
FMAP 2
PLAN 10
SIZE 0.070 0.140 0.260
ACTA
BOND $H
LIST 4
L.S. 4
TEMP 23.00
WGHT 0.048400 0.052500
FVAR 6.03699
C1 1 0.674958 0.457179 0.587923 11.00000 0.05600 0.04883 =
0.05297 0.00454 0.00936 -0.00264
C2 1 0.517809 0.515126 0.581219 11.00000 0.06856 0.04531 =
0.06000 0.00924 0.01431 0.00008
AFIX 43
H2 2 0.507242 0.585152 0.554930 11.00000 -1.20000
AFIX 0
C3 1 0.378460 0.469523 0.613170 11.00000 0.06103 0.05672 =
0.06077 0.00658 0.01430 0.00262
AFIX 43
H3 2 0.274364 0.508481 0.608568 11.00000 -1.20000
AFIX 0
C4 1 0.394856 0.365260 0.652152 11.00000 0.06387 0.05475 =
0.05013 0.00294 0.01362 -0.01172
C5 1 0.547037 0.306723 0.660037 11.00000 0.07755 0.04915 =
0.05807 0.01358 0.01048 -0.00729
AFIX 43
H5 2 0.556356 0.236933 0.686762 11.00000 -1.20000
AFIX 0
C6 1 0.687616 0.352503 0.627741 11.00000 0.06246 0.05236 =
0.06483 0.01292 0.00897 0.00046
AFIX 43
H6 2 0.791158 0.312863 0.632762 11.00000 -1.20000
AFIX 0
C7 1 0.825313 0.503053 0.554133 11.00000 0.05963 0.05241 =
0.06316 0.00820 0.01347 -0.00188
AFIX 43
H7 2 0.925239 0.460403 0.556268 11.00000 -1.20000
AFIX 0
C8 1 0.965677 0.737124 0.447867 11.00000 0.05552 0.04620 =
0.05032 -0.00061 0.01012 -0.00532
C9 1 0.835418 0.814204 0.443851 11.00000 0.06045 0.05152 =
0.06099 -0.00297 0.02025 -0.00187
AFIX 43
H9 2 0.740133 0.800018 0.471623 11.00000 -1.20000
AFIX 0
C10 1 0.846213 0.914768 0.397642 11.00000 0.07061 0.04871 =
0.06760 -0.00051 0.01551 0.00843
AFIX 43
H10 2 0.755828 0.965694 0.394070 11.00000 -1.20000
AFIX 0
C11 1 0.986245 0.939507 0.357856 11.00000 0.07265 0.04298 =
0.06206 0.00285 0.01265 -0.00484
AFIX 43
H11 2 0.990642 1.006567 0.327755 11.00000 -1.20000
AFIX 0
C12 1 1.123716 0.863025 0.362661 11.00000 0.06099 0.04744 =
0.04562 -0.00112 0.00779 -0.00825
C13 1 1.113174 0.759637 0.406684 11.00000 0.05465 0.04688 =
0.04841 -0.00067 0.00774 -0.00506
C14 1 1.276608 0.882749 0.327369 11.00000 0.06840 0.06048 =
0.05274 0.00197 0.01235 -0.01594
AFIX 43
H14 2 1.292238 0.950267 0.300041 11.00000 -1.20000
AFIX 0
C15 1 1.400929 0.803461 0.333191 11.00000 0.05470 0.08205 =
0.06375 0.00688 0.01582 -0.00666
AFIX 43
H15 2 1.500980 0.815666 0.308877 11.00000 -1.20000
AFIX 0
C16 1 1.377515 0.703095 0.376083 11.00000 0.05674 0.07081 =
0.07578 0.00486 0.01785 0.00454
AFIX 43
H16 2 1.463862 0.649448 0.379133 11.00000 -1.20000
AFIX 0
C17 1 0.129444 0.280314 0.419108 11.00000 0.07490 0.04544 =
0.04812 -0.00061 0.00668 0.00356
C18 1 -0.023006 0.222824 0.424315 11.00000 0.08286 0.04267 =
0.06621 0.00567 0.01019 0.00047
AFIX 43
H18 2 -0.015814 0.154010 0.452680 11.00000 -1.20000
AFIX 0
C19 1 -0.184845 0.266218 0.388073 11.00000 0.07478 0.05430 =
0.07395 0.00268 0.01056 -0.00407
AFIX 43
H19 2 -0.285878 0.226660 0.391183 11.00000 -1.20000
AFIX 0
C20 1 -0.194694 0.369362 0.347058 11.00000 0.07878 0.05439 =
0.06200 0.00031 0.00305 0.00711
C21 1 -0.045433 0.429450 0.342657 11.00000 0.08677 0.04639 =
0.06120 0.00818 0.00359 0.00361
AFIX 43
H21 2 -0.053490 0.499214 0.315895 11.00000 -1.20000
AFIX 0
C22 1 0.115720 0.384672 0.378457 11.00000 0.07917 0.04822 =
0.05915 0.00462 0.00934 -0.00134
AFIX 43
H22 2 0.216388 0.424649 0.375408 11.00000 -1.20000
AFIX 0
C23 1 0.301684 0.233669 0.452878 11.00000 0.07359 0.05207 =
0.05510 0.00297 0.00798 0.00558
AFIX 43
H23 2 0.400830 0.275359 0.450152 11.00000 -1.20000
AFIX 0
C24 1 0.509192 0.000052 0.565490 11.00000 0.07405 0.04277 =
0.05167 -0.00256 0.01002 0.00558
C25 1 0.378621 -0.073031 0.572779 11.00000 0.07214 0.05520 =
0.06167 -0.00599 0.00677 0.00070
AFIX 43
H25 2 0.264350 -0.057283 0.545057 11.00000 -1.20000
AFIX 0
C26 1 0.416776 -0.171937 0.622100 11.00000 0.08858 0.05326 =
0.07209 -0.00065 0.01584 -0.00818
AFIX 43
H26 2 0.327195 -0.221627 0.625588 11.00000 -1.20000
AFIX 0
C27 1 0.582398 -0.196496 0.664917 11.00000 0.10111 0.04934 =
0.06347 0.00655 0.01332 0.00684
AFIX 43
H27 2 0.604432 -0.261624 0.698298 11.00000 -1.20000
AFIX 0
C28 1 0.720213 -0.123208 0.658603 11.00000 0.07872 0.05166 =
0.05120 -0.00065 0.01228 0.01179
C29 1 0.684873 -0.023367 0.608444 11.00000 0.06885 0.04654 =
0.05103 -0.00539 0.01353 0.00710
C30 1 0.896118 -0.142651 0.699712 11.00000 0.08937 0.06806 =
0.06498 0.00239 0.00977 0.02390
AFIX 43
H30 2 0.926770 -0.207020 0.733023 11.00000 -1.20000
AFIX 0
C31 1 1.019992 -0.066723 0.690233 11.00000 0.06832 0.08867 =
0.07769 -0.00591 0.00967 0.02049
AFIX 43
H31 2 1.135851 -0.078429 0.717383 11.00000 -1.20000
AFIX 0
C32 1 0.971659 0.029401 0.639184 11.00000 0.06822 0.07883 =
0.07697 -0.01026 0.01642 0.00221
AFIX 43
H32 2 1.058474 0.080213 0.633341 11.00000 -1.20000
AFIX 0
N1 3 0.820115 0.601350 0.521719 11.00000 0.06349 0.04983 =
0.06107 0.00472 0.01850 -0.00676
N2 3 0.965843 0.636520 0.492158 11.00000 0.05946 0.05214 =
0.07992 0.01267 0.02411 0.00007
AFIX 43
H2A 2 1.058243 0.596165 0.501010 11.00000 -1.20000
AFIX 0
N3 3 1.238871 0.680400 0.412590 11.00000 0.05634 0.05654 =
0.06996 0.00639 0.01525 0.00157
N4 3 0.317678 0.135646 0.486314 11.00000 0.07246 0.04892 =
0.06195 0.00053 0.00313 0.00831
N5 3 0.483238 0.098281 0.516230 11.00000 0.07096 0.05308 =
0.07618 0.01176 0.00751 0.00584
AFIX 43
H5A 2 0.571013 0.135167 0.504734 11.00000 -1.20000
AFIX 0
N6 3 0.810369 0.051988 0.598978 11.00000 0.06926 0.05725 =
0.06665 -0.00455 0.01542 0.00399
CL1 4 0.219417 0.307456 0.692196 11.00000 0.08375 0.07921 =
0.09401 0.01094 0.03583 -0.01968
CL2 4 -0.398627 0.424163 0.301363 11.00000 0.08343 0.07684 =
0.12364 0.01363 -0.00634 0.01327
HKLF 4
REM bmk2261c in Pn
REM R1 = 0.0314 for 3609 Fo > 4sig(Fo) and 0.0344 for all 3869 data
REM 361 parameters refined using 2 restraints
END
WGHT 0.0483 0.0528
REM Highest difference peak 0.117, deepest hole -0.138, 1-sigma level 0.029
Q1 1 1.1169 0.8080 0.3984 11.00000 0.05 0.12
Q2 1 0.3785 0.4302 0.6251 11.00000 0.05 0.12
Q3 1 0.2118 -0.1784 0.6795 11.00000 0.05 0.10
Q4 1 0.6924 -0.0689 0.6236 11.00000 0.05 0.10
Q5 1 0.5904 0.1675 0.5535 11.00000 0.05 0.10
Q6 1 0.4933 0.2647 0.3539 11.00000 0.05 0.10
Q7 1 0.6759 0.4282 0.6037 11.00000 0.05 0.10
Q8 1 0.1798 -0.2182 0.6650 11.00000 0.05 0.09
Q9 1 1.5823 0.9249 0.3251 11.00000 0.05 0.09
Q10 1 0.2962 0.4012 0.3389 11.00000 0.05 0.09
;
_shelx_res_checksum 36128
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.6750(3) 0.4572(2) 0.58792(17) 0.0527(5) Uani d 1 . .
C C2 0.5178(4) 0.5151(2) 0.58122(18) 0.0576(6) Uani d 1 . .
H H2 0.507242 0.585152 0.554930 0.069 Uiso calc 1 . .
C C3 0.3785(4) 0.4695(2) 0.61317(19) 0.0591(6) Uani d 1 . .
H H3 0.274364 0.508481 0.608568 0.071 Uiso calc 1 . .
C C4 0.3949(4) 0.3653(2) 0.65215(17) 0.0559(6) Uani d 1 . .
C C5 0.5470(4) 0.3067(2) 0.66004(18) 0.0618(6) Uani d 1 . .
H H5 0.556356 0.236933 0.686762 0.074 Uiso calc 1 . .
C C6 0.6876(4) 0.3525(2) 0.62774(19) 0.0602(6) Uani d 1 . .
H H6 0.791158 0.312863 0.632762 0.072 Uiso calc 1 . .
C C7 0.8253(4) 0.5031(2) 0.55413(19) 0.0581(6) Uani d 1 . .
H H7 0.925239 0.460403 0.556268 0.070 Uiso calc 1 . .
C C8 0.9657(3) 0.73712(19) 0.44787(16) 0.0506(5) Uani d 1 . .
C C9 0.8354(4) 0.8142(2) 0.44385(18) 0.0565(6) Uani d 1 . .
H H9 0.740133 0.800018 0.471623 0.068 Uiso calc 1 . .
C C10 0.8462(4) 0.9148(2) 0.39764(19) 0.0620(6) Uani d 1 . .
H H10 0.755828 0.965694 0.394070 0.074 Uiso calc 1 . .
C C11 0.9862(4) 0.9395(2) 0.35786(19) 0.0592(6) Uani d 1 . .
H H11 0.990642 1.006567 0.327755 0.071 Uiso calc 1 . .
C C12 1.1237(3) 0.8630(2) 0.36266(16) 0.0516(5) Uani d 1 . .
C C13 1.1132(3) 0.75964(19) 0.40668(16) 0.0502(5) Uani d 1 . .
C C14 1.2766(4) 0.8827(2) 0.32737(18) 0.0604(6) Uani d 1 . .
H H14 1.292238 0.950267 0.300041 0.072 Uiso calc 1 . .
C C15 1.4009(4) 0.8035(3) 0.3332(2) 0.0662(7) Uani d 1 . .
H H15 1.500980 0.815666 0.308877 0.079 Uiso calc 1 . .
C C16 1.3775(4) 0.7031(3) 0.3761(2) 0.0671(7) Uani d 1 . .
H H16 1.463862 0.649448 0.379133 0.080 Uiso calc 1 . .
C C17 0.1294(4) 0.2803(2) 0.41911(17) 0.0567(6) Uani d 1 . .
C C18 -0.0230(4) 0.2228(2) 0.4243(2) 0.0644(7) Uani d 1 . .
H H18 -0.015814 0.154010 0.452680 0.077 Uiso calc 1 . .
C C19 -0.1848(4) 0.2662(2) 0.3881(2) 0.0681(7) Uani d 1 . .
H H19 -0.285878 0.226660 0.391183 0.082 Uiso calc 1 . .
C C20 -0.1947(4) 0.3694(2) 0.34706(19) 0.0663(7) Uani d 1 . .
C C21 -0.0454(4) 0.4295(2) 0.34266(19) 0.0661(7) Uani d 1 . .
H H21 -0.053490 0.499214 0.315895 0.079 Uiso calc 1 . .
C C22 0.1157(4) 0.3847(2) 0.37846(19) 0.0626(6) Uani d 1 . .
H H22 0.216388 0.424649 0.375408 0.075 Uiso calc 1 . .
C C23 0.3017(4) 0.2337(2) 0.45288(18) 0.0607(6) Uani d 1 . .
H H23 0.400830 0.275359 0.450152 0.073 Uiso calc 1 . .
C C24 0.5092(4) 0.0001(2) 0.56549(17) 0.0564(6) Uani d 1 . .
C C25 0.3786(4) -0.0730(2) 0.57278(19) 0.0637(7) Uani d 1 . .
H H25 0.264350 -0.057283 0.545057 0.076 Uiso calc 1 . .
C C26 0.4168(5) -0.1719(2) 0.6221(2) 0.0712(8) Uani d 1 . .
H H26 0.327195 -0.221627 0.625588 0.085 Uiso calc 1 . .
C C27 0.5824(5) -0.1965(2) 0.6649(2) 0.0715(8) Uani d 1 . .
H H27 0.604432 -0.261624 0.698298 0.086 Uiso calc 1 . .
C C28 0.7202(4) -0.1232(2) 0.65860(17) 0.0605(6) Uani d 1 . .
C C29 0.6849(4) -0.0234(2) 0.60844(17) 0.0552(5) Uani d 1 . .
C C30 0.8961(5) -0.1427(3) 0.6997(2) 0.0747(8) Uani d 1 . .
H H30 0.926770 -0.207020 0.733023 0.090 Uiso calc 1 . .
C C31 1.0200(5) -0.0667(3) 0.6902(2) 0.0787(9) Uani d 1 . .
H H31 1.135851 -0.078429 0.717383 0.094 Uiso calc 1 . .
C C32 0.9717(4) 0.0294(3) 0.6392(2) 0.0743(8) Uani d 1 . .
H H32 1.058474 0.080213 0.633341 0.089 Uiso calc 1 . .
N N1 0.8201(3) 0.60135(18) 0.52172(15) 0.0572(5) Uani d 1 . .
N N2 0.9658(3) 0.63652(19) 0.49216(18) 0.0624(5) Uani d 1 . .
H H2A 1.058243 0.596165 0.501010 0.075 Uiso calc 1 . .
N N3 1.2389(3) 0.68040(19) 0.41259(17) 0.0605(5) Uani d 1 . .
N N4 0.3177(3) 0.13565(18) 0.48631(16) 0.0623(6) Uani d 1 . .
N N5 0.4832(3) 0.0983(2) 0.51623(18) 0.0675(6) Uani d 1 . .
H H5A 0.571013 0.135167 0.504734 0.081 Uiso calc 1 . .
N N6 0.8104(3) 0.05199(19) 0.59898(17) 0.0640(5) Uani d 1 . .
Cl Cl1 0.21942(11) 0.30746(7) 0.69220(7) 0.0832(2) Uani d 1 . .
Cl Cl2 -0.39863(14) 0.42416(8) 0.30136(9) 0.0979(3) 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
C1 0.0560(13) 0.0488(12) 0.0530(12) -0.0026(10) 0.0094(10) 0.0045(9)
C2 0.0686(15) 0.0453(12) 0.0600(14) 0.0001(11) 0.0143(11) 0.0092(9)
C3 0.0610(15) 0.0567(14) 0.0608(14) 0.0026(11) 0.0143(11) 0.0066(11)
C4 0.0639(15) 0.0548(13) 0.0501(12) -0.0117(11) 0.0136(11) 0.0029(9)
C5 0.0776(18) 0.0491(13) 0.0581(14) -0.0073(12) 0.0105(12) 0.0136(10)
C6 0.0625(15) 0.0524(13) 0.0648(15) 0.0005(11) 0.0090(12) 0.0129(11)
C7 0.0596(15) 0.0524(13) 0.0632(14) -0.0019(11) 0.0135(11) 0.0082(10)
C8 0.0555(14) 0.0462(12) 0.0503(12) -0.0053(10) 0.0101(10) -0.0006(9)
C9 0.0605(14) 0.0515(13) 0.0610(14) -0.0019(11) 0.0202(11) -0.0030(10)
C10 0.0706(17) 0.0487(13) 0.0676(15) 0.0084(11) 0.0155(13) -0.0005(10)
C11 0.0727(16) 0.0430(12) 0.0621(14) -0.0048(11) 0.0127(12) 0.0028(10)
C12 0.0610(14) 0.0474(12) 0.0456(11) -0.0083(10) 0.0078(9) -0.0011(9)
C13 0.0546(13) 0.0469(12) 0.0484(12) -0.0051(9) 0.0077(10) -0.0007(9)
C14 0.0684(15) 0.0605(14) 0.0527(13) -0.0159(13) 0.0124(11) 0.0020(10)
C15 0.0547(15) 0.0821(19) 0.0638(15) -0.0067(13) 0.0158(12) 0.0069(13)
C16 0.0567(15) 0.0708(17) 0.0758(17) 0.0045(13) 0.0179(13) 0.0049(13)
C17 0.0749(17) 0.0454(12) 0.0481(12) 0.0036(11) 0.0067(11) -0.0006(9)
C18 0.0829(19) 0.0427(13) 0.0662(15) 0.0005(12) 0.0102(13) 0.0057(10)
C19 0.0748(18) 0.0543(15) 0.0740(17) -0.0041(13) 0.0106(13) 0.0027(12)
C20 0.079(2) 0.0544(15) 0.0620(15) 0.0071(13) 0.0031(13) 0.0003(10)
C21 0.087(2) 0.0464(13) 0.0612(15) 0.0036(12) 0.0036(14) 0.0082(10)
C22 0.0792(18) 0.0482(13) 0.0591(15) -0.0013(12) 0.0093(13) 0.0046(10)
C23 0.0736(18) 0.0521(14) 0.0551(14) 0.0056(12) 0.0080(12) 0.0030(10)
C24 0.0741(16) 0.0428(11) 0.0517(13) 0.0056(11) 0.0100(11) -0.0026(9)
C25 0.0721(18) 0.0552(14) 0.0617(16) 0.0007(12) 0.0068(12) -0.0060(11)
C26 0.089(2) 0.0533(15) 0.0721(17) -0.0082(14) 0.0158(15) -0.0006(12)
C27 0.101(2) 0.0493(14) 0.0635(16) 0.0068(14) 0.0133(15) 0.0066(11)
C28 0.0787(18) 0.0517(14) 0.0512(13) 0.0118(12) 0.0123(12) -0.0007(9)
C29 0.0689(15) 0.0465(12) 0.0510(12) 0.0071(11) 0.0135(11) -0.0054(9)
C30 0.089(2) 0.0681(18) 0.0650(17) 0.0239(17) 0.0098(15) 0.0024(13)
C31 0.0683(19) 0.089(2) 0.0777(19) 0.0205(16) 0.0097(14) -0.0059(15)
C32 0.0682(18) 0.0788(19) 0.0770(18) 0.0022(15) 0.0164(15) -0.0103(14)
N1 0.0635(13) 0.0498(11) 0.0611(12) -0.0068(9) 0.0185(10) 0.0047(9)
N2 0.0595(13) 0.0521(11) 0.0799(14) 0.0001(10) 0.0241(11) 0.0127(10)
N3 0.0563(12) 0.0565(12) 0.0700(13) 0.0016(9) 0.0152(10) 0.0064(9)
N4 0.0725(15) 0.0489(11) 0.0620(12) 0.0083(10) 0.0031(10) 0.0005(9)
N5 0.0710(15) 0.0531(12) 0.0762(15) 0.0058(11) 0.0075(12) 0.0118(10)
N6 0.0693(14) 0.0572(12) 0.0667(13) 0.0040(10) 0.0154(11) -0.0046(10)
Cl1 0.0837(5) 0.0792(5) 0.0940(5) -0.0197(4) 0.0358(4) 0.0109(4)
Cl2 0.0834(6) 0.0768(5) 0.1236(7) 0.0133(4) -0.0063(5) 0.0136(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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
C6 C1 C2 . . 118.6(2) ?
C6 C1 C7 . . 119.4(2) ?
C2 C1 C7 . . 122.1(2) ?
C3 C2 C1 . . 120.7(2) ?
C3 C2 H2 . . 119.7 ?
C1 C2 H2 . . 119.7 ?
C2 C3 C4 . . 119.4(3) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C5 C4 C3 . . 121.3(2) ?
C5 C4 Cl1 . . 119.20(19) ?
C3 C4 Cl1 . . 119.5(2) ?
C4 C5 C6 . . 119.4(2) ?
C4 C5 H5 . . 120.3 ?
C6 C5 H5 . . 120.3 ?
C5 C6 C1 . . 120.7(3) ?
C5 C6 H6 . . 119.7 ?
C1 C6 H6 . . 119.7 ?
N1 C7 C1 . . 120.5(3) ?
N1 C7 H7 . . 119.7 ?
C1 C7 H7 . . 119.7 ?
C9 C8 N2 . . 123.7(2) ?
C9 C8 C13 . . 120.1(2) ?
N2 C8 C13 . . 116.3(2) ?
C8 C9 C10 . . 119.9(2) ?
C8 C9 H9 . . 120.1 ?
C10 C9 H9 . . 120.1 ?
C11 C10 C9 . . 121.7(3) ?
C11 C10 H10 . . 119.2 ?
C9 C10 H10 . . 119.2 ?
C10 C11 C12 . . 119.7(2) ?
C10 C11 H11 . . 120.1 ?
C12 C11 H11 . . 120.1 ?
C11 C12 C14 . . 124.0(2) ?
C11 C12 C13 . . 119.6(2) ?
C14 C12 C13 . . 116.5(2) ?
N3 C13 C12 . . 123.2(2) ?
N3 C13 C8 . . 117.8(2) ?
C12 C13 C8 . . 119.1(2) ?
C15 C14 C12 . . 120.1(2) ?
C15 C14 H14 . . 120.0 ?
C12 C14 H14 . . 120.0 ?
C14 C15 C16 . . 119.4(3) ?
C14 C15 H15 . . 120.3 ?
C16 C15 H15 . . 120.3 ?
N3 C16 C15 . . 123.5(3) ?
N3 C16 H16 . . 118.3 ?
C15 C16 H16 . . 118.3 ?
C18 C17 C22 . . 118.6(3) ?
C18 C17 C23 . . 122.0(2) ?
C22 C17 C23 . . 119.5(3) ?
C19 C18 C17 . . 121.1(2) ?
C19 C18 H18 . . 119.4 ?
C17 C18 H18 . . 119.4 ?
C18 C19 C20 . . 119.1(3) ?
C18 C19 H19 . . 120.4 ?
C20 C19 H19 . . 120.4 ?
C21 C20 C19 . . 121.0(3) ?
C21 C20 Cl2 . . 119.8(2) ?
C19 C20 Cl2 . . 119.2(3) ?
C22 C21 C20 . . 119.3(2) ?
C22 C21 H21 . . 120.4 ?
C20 C21 H21 . . 120.4 ?
C21 C22 C17 . . 120.9(3) ?
C21 C22 H22 . . 119.6 ?
C17 C22 H22 . . 119.6 ?
N4 C23 C17 . . 120.6(3) ?
N4 C23 H23 . . 119.7 ?
C17 C23 H23 . . 119.7 ?
C25 C24 N5 . . 123.7(3) ?
C25 C24 C29 . . 120.2(2) ?
N5 C24 C29 . . 116.1(2) ?
C24 C25 C26 . . 120.1(3) ?
C24 C25 H25 . . 119.9 ?
C26 C25 H25 . . 119.9 ?
C27 C26 C25 . . 121.4(3) ?
C27 C26 H26 . . 119.3 ?
C25 C26 H26 . . 119.3 ?
C26 C27 C28 . . 120.0(3) ?
C26 C27 H27 . . 120.0 ?
C28 C27 H27 . . 120.0 ?
C27 C28 C30 . . 123.9(3) ?
C27 C28 C29 . . 119.6(3) ?
C30 C28 C29 . . 116.6(3) ?
N6 C29 C28 . . 123.3(3) ?
N6 C29 C24 . . 117.9(2) ?
C28 C29 C24 . . 118.7(3) ?
C31 C30 C28 . . 119.6(3) ?
C31 C30 H30 . . 120.2 ?
C28 C30 H30 . . 120.2 ?
C30 C31 C32 . . 119.4(3) ?
C30 C31 H31 . . 120.3 ?
C32 C31 H31 . . 120.3 ?
N6 C32 C31 . . 123.8(3) ?
N6 C32 H32 . . 118.1 ?
C31 C32 H32 . . 118.1 ?
C7 N1 N2 . . 116.2(2) ?
N1 N2 C8 . . 120.1(2) ?
N1 N2 H2A . . 120.0 ?
C8 N2 H2A . . 120.0 ?
C16 N3 C13 . . 117.4(2) ?
C23 N4 N5 . . 116.9(3) ?
N4 N5 C24 . . 119.5(2) ?
N4 N5 H5A . . 120.2 ?
C24 N5 H5A . . 120.2 ?
C32 N6 C29 . . 117.2(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
C1 C6 . 1.393(4) ?
C1 C2 . 1.399(4) ?
C1 C7 . 1.467(4) ?
C2 C3 . 1.379(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.384(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.368(4) ?
C4 Cl1 . 1.736(3) ?
C5 C6 . 1.390(4) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 N1 . 1.281(3) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.372(4) ?
C8 N2 . 1.383(3) ?
C8 C13 . 1.425(3) ?
C9 C10 . 1.407(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.367(4) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.408(4) ?
C11 H11 . 0.9300 ?
C12 C14 . 1.408(4) ?
C12 C13 . 1.421(3) ?
C13 N3 . 1.362(3) ?
C14 C15 . 1.355(4) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.399(4) ?
C15 H15 . 0.9300 ?
C16 N3 . 1.325(4) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.391(4) ?
C17 C22 . 1.395(4) ?
C17 C23 . 1.458(4) ?
C18 C19 . 1.381(5) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.384(4) ?
C19 H19 . 0.9300 ?
C20 C21 . 1.384(5) ?
C20 Cl2 . 1.741(3) ?
C21 C22 . 1.382(4) ?
C21 H21 . 0.9300 ?
C22 H22 . 0.9300 ?
C23 N4 . 1.283(4) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.367(4) ?
C24 N5 . 1.391(3) ?
C24 C29 . 1.429(4) ?
C25 C26 . 1.406(4) ?
C25 H25 . 0.9300 ?
C26 C27 . 1.363(5) ?
C26 H26 . 0.9300 ?
C27 C28 . 1.409(5) ?
C27 H27 . 0.9300 ?
C28 C30 . 1.415(5) ?
C28 C29 . 1.419(4) ?
C29 N6 . 1.363(4) ?
C30 C31 . 1.359(5) ?
C30 H30 . 0.9300 ?
C31 C32 . 1.402(5) ?
C31 H31 . 0.9300 ?
C32 N6 . 1.318(4) ?
C32 H32 . 0.9300 ?
N1 N2 . 1.360(3) ?
N2 H2A . 0.8600 ?
N4 N5 . 1.363(3) ?
N5 H5A . 0.8600 ?
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
C15 H15 Cl1 2_664 0.93 3.04 3.779(3) 138.0 yes
C30 H30 Cl2 2_655 0.93 3.05 3.943(3) 162.7 yes
_cod_database_fobs_code 2022831