#------------------------------------------------------------------------------
#$Date: 2024-08-24 05:18:55 +0300 (Sat, 24 Aug 2024) $
#$Revision: 294212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312587.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_2312587
loop_
_publ_author_name
'Dival, Bruno'
'Pitinato, Leonardo'
'Develly, Letícia'
'Oliveira, Willian X. C.'
_publ_section_title
;
Crystal structures of two unexpected products of vicinal diamines left to
crystallize in acetone.
;
_journal_coeditor_code EF3057
_journal_issue 9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624007320
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C26 H30 N4 O4 S2'
_chemical_formula_moiety 'C26 H30 N4 O4 S2'
_chemical_formula_sum 'C26 H30 N4 O4 S2'
_chemical_formula_weight 526.66
_chemical_name_systematic
2,2,4-Trimethyl-8,9-bis(4-methylbenzenesulfonamido)-2,3-dihydro-5H-1,5-benzodiazepine
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 129.744(5)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 30.0416(9)
_cell_length_b 9.70180(10)
_cell_length_c 24.0984(7)
_cell_measurement_reflns_used 17655
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 73.4160
_cell_measurement_theta_min 3.7370
_cell_volume 5400.6(5)
_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)
;
_computing_publication_material
;
SHELXL2019 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus et al., 2007)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0690
_diffrn_reflns_av_unetI/netI 0.0255
_diffrn_reflns_limit_h_max 36
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 76569
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.244
_diffrn_reflns_theta_min 3.750
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 2.104
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.603
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour Yellow
_exptl_crystal_density_diffrn 1.295
_exptl_crystal_description Needle
_exptl_crystal_F_000 2224
_exptl_crystal_size_max 0.190
_exptl_crystal_size_mid 0.067
_exptl_crystal_size_min 0.058
_refine_diff_density_max 0.414
_refine_diff_density_min -0.340
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.067
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 334
_refine_ls_number_reflns 4942
_refine_ls_number_restraints 9
_refine_ls_restrained_S_all 5.229
_refine_ls_R_factor_all 0.0533
_refine_ls_R_factor_gt 0.0425
_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^)+(0.0632P)^2^+2.9523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1176
_refine_ls_wR_factor_ref 0.1262
_reflns_number_gt 3970
_reflns_number_total 4942
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ef3057sup1.cif
_cod_data_source_block 2
_cod_original_cell_volume 5400.6(4)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 2312587
_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_hkl_file
;
0 0 -1 11.1543 18.4757 7
0 0 1 11.8230 15.0347 8
0 0 -1-3.73267 17.6431 4
0 0 2 153005. 7868.22 8
0 0 -2 156000. 7878.62 7
0 0 -3-12.9760 46.6586 88
0 0 3-17.3242 44.0484 8
0 0 -3 101.204 61.5621 7
0 0 3-42.1839 57.7360 6
0 0 -4 128324. 7880.30 88
0 0 -4 151432. 7884.91 7
0 0 4 149987. 7876.64 6
0 0 4 152534. 7862.72 8
0 0 -5-20.1966 78.9464 88
0 0 -5-38.5395 87.3933 7
0 0 5 52.5026 78.2289 6
0 0 -6 38.1275 54.4238 69
0 0 -6 23.3127 71.6209 88
0 0 -6 212.516 104.079 7
0 0 6 211.348 88.8503 6
0 0 -7-22.5312 66.8985 79
0 0 -7-20.5587 63.0441 70
0 0 7-17.5557 60.1900 73
0 0 -7 14.7508 55.4010 69
0 0 7 24.9798 85.6414 6
0 0 -7-28.1903 99.0344 7
0 0 -7-27.3496 69.5398 88
0 0 -7-14.8803 51.0184 10
0 0 -8 12437.2 828.785 79
0 0 8 12651.6 801.343 73
0 0 -8 13330.5 826.698 70
0 0 -8 13405.3 789.156 69
0 0 -8 13164.9 789.200 10
0 0 -8 13012.7 817.489 12
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0 0 -8 12412.5 866.915 7
0 0 -8 13417.0 859.837 88
0 0 -9-33.3381 88.5344 88
0 0 -9-30.3375 77.1366 79
0 0 9-22.4368 68.8033 73
0 0 -9-53.7806 87.4607 70
0 0 -9 18.8118 64.4967 69
0 0 -9-18.6430 60.6383 10
0 0 9 76.5774 99.7802 17
0 0 -9-26.0871 74.8302 12
0 0 9 59.5552 82.3085 47
0 0 -9-29.4700 90.3692 51
0 0 9-66.3075 91.6398 6
0 0 -9 76.8646 114.108 7
0 0 -9-28.3104 97.0598 22
0 0 9 29.1273 74.0599 21
0 0 9-27.9097 67.6622 41
0 0 -9 29.8634 97.1301 37
0 0 -10 12225.8 809.636 88
0 0 -10 10655.0 784.465 79
0 0 -10 11323.3 805.127 78
0 0 -10 11677.2 776.149 70
0 0 10 10507.0 737.975 73
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0 0 10 12751.8 779.999 17
0 0 -10 11369.7 771.362 12
0 0 -10 11805.4 727.943 10
0 0 -10 11096.5 783.275 51
0 0 10 13089.4 813.230 47
0 0 -10 12846.8 782.608 52
0 0 10 10544.2 796.954 6
0 0 -10 11386.5 835.834 7
0 0 10 12334.8 797.191 21
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0 0 10 11588.2 784.355 41
0 0 10 10719.6 755.577 42
0 0 -10 10952.9 786.966 37
0 0 11-32.1583 77.9643 42
0 0 11-71.9540 110.324 41
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0 0 11-37.6325 95.6865 21
0 0 11 42.0065 106.807 6
0 0 -11-39.4430 74.0717 88
0 0 -11 42.8014 86.8166 78
0 0 -11-39.2080 90.1757 79
0 0 -11-67.9214 82.3333 70
0 0 11 51.2883 65.2082 73
0 0 11-30.9717 75.0881 63
0 0 -11-114.040 142.765 51
0 0 11 76.2771 101.285 47
0 0 -11 97.4587 86.2753 52
0 0 -11 29.9703 82.8441 26
0 0 11 45.4031 62.7551 29
0 0 -11 62.0376 57.1659 10
0 0 11 32.5255 93.2998 17
0 0 -11-53.6847 68.2543 19
0 0 -11-33.3297 88.5150 12
0 0 -12 1685.40 208.180 19
0 0 12 2032.61 247.080 17
0 0 -12 1767.80 240.461 12
0 0 12 1579.09 231.982 42
0 0 12 1611.18 238.803 41
0 0 12 1732.57 253.022 21
0 0 -12 1777.68 256.225 22
0 0 12 1808.36 272.219 6
0 0 -12 1823.62 255.886 88
0 0 -12 2370.25 306.033 78
0 0 -12 1364.34 239.473 79
0 0 -12 2071.13 251.797 70
0 0 12 1754.64 228.527 63
0 0 12 1963.79 267.568 47
0 0 -12 1106.35 211.138 51
0 0 -12 1776.54 233.987 52
0 0 -12 1373.74 202.715 26
0 0 12 1867.90 200.284 29
0 0 -12 1986.31 270.278 36
0 0 -13 32.0503 85.1139 19
0 0 -13 39.9108 74.9455 12
0 0 13 40.0835 81.3004 17
0 0 13 44.5836 96.6708 41
0 0 13 39.5072 85.6639 42
0 0 -13-91.9217 111.420 22
0 0 13-46.9581 124.702 21
0 0 13 50.2629 108.985 6
0 0 -13 45.1612 77.4158 88
0 0 -13-54.1365 124.504 78
0 0 -13-48.9400 99.2631 79
0 0 13-68.6067 166.317 75
0 0 -13 41.1276 99.7030 70
0 0 13 189.327 108.613 63
0 0 -13-47.0002 108.092 51
0 0 -13 39.9296 96.7989 52
0 0 13-47.3321 114.744 47
0 0 -13-30.1710 73.1426 49
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0 0 -13 35.0707 71.1334 26
0 0 13-80.9037 62.0231 29
0 0 -14 535.794 172.953 79
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0 0 14 1054.04 266.809 75
0 0 -14 674.798 162.234 12
0 0 -14 680.121 204.959 11
0 0 -14 510.033 127.201 19
0 0 14 781.705 164.609 63
0 0 -14 818.101 191.233 51
0 0 -14 519.091 145.005 52
0 0 -14 679.392 191.164 36
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0 0 14 598.276 160.985 42
0 0 14 438.420 166.520 41
0 0 -15-73.3174 186.419 11
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0 0 -15-167.769 186.877 36
0 0 15 45.1464 103.843 42
0 0 15 52.0352 119.684 41
0 0 15-162.071 240.603 75
0 0 -15 64.8704 121.825 78
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0 0 -16 962.611 253.624 78
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0 0 -16 1366.05 221.003 52
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0 0 -16 1280.05 250.773 36
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0 0 21 61.2868 74.3027 15
0 0 -22 1624.94 202.608 35
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0 0 -22 1600.54 192.788 22
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0 -2 -1 330729. 18671.2 2
0 -2 -1 349970. 18644.3 7
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0 2 -9 4110.11 385.551 10
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0 2 -9 5311.82 426.582 12
0 -2 9 3750.31 355.480 15
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0 -2 9 4449.63 385.202 42
0 -2 9 4566.47 381.469 44
0 -2 -9 4690.71 377.231 22
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0 -2 -9 4649.44 401.649 37
0 -2 10 34794.7 1945.90 15
0 2 -10 33691.3 1990.96 12
0 -2 -10 32637.8 1875.21 12
0 2 10 33348.6 1950.96 17
0 2 -10 34183.7 1966.33 10
0 -2 10 32561.7 1945.34 44
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0 2 10 33146.2 1951.71 39
0 -2 10 35965.6 1993.41 41
0 -2 -10 32565.2 1936.07 22
0 2 -10 36636.2 1982.20 22
0 2 10 33020.8 1955.37 8
0 -2 -10 34570.9 1988.11 88
0 2 -10 29322.5 2016.66 88
0 -2 -10 32824.0 2004.63 78
0 -2 10 36943.8 2033.78 75
0 2 -10 32756.0 1998.69 78
0 2 10 32178.4 1994.45 73
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0 -2 10 31603.4 1938.18 58
0 -2 10 32797.5 1941.75 63
0 2 10 33267.8 1952.05 62
0 -2 -10 31933.7 1979.09 51
0 -2 -10 33145.8 1953.82 53
0 2 10 33700.9 1976.18 47
0 2 -10 34638.0 1969.75 53
0 2 -10 33717.0 1927.24 51
0 2 10 35264.5 1916.47 30
0 -2 10 33378.7 1909.81 29
0 -2 -10 32328.7 1972.17 37
0 -2 -10 31815.6 1958.28 38
0 -2 -10 29629.0 1891.49 34
0 2 -10 31439.2 1926.80 36
0 2 -11-37.3050 99.0704 10
0 -2 11-69.6735 92.5160 15
0 2 -11-45.2356 98.0871 12
0 2 11-36.6391 93.1601 17
0 2 -11 34.8187 96.2434 19
0 -2 -11 21.5791 52.3197 12
0 -2 11-42.5422 112.978 41
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0 -2 -11 34.8107 92.4467 22
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0 -2 -11 43.1662 87.5556 88
0 2 -11-54.3819 102.121 88
0 -2 11-101.589 150.812 75
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0 2 11 185.276 106.528 73
0 2 11-36.8439 101.841 62
0 -2 11 34.5396 87.8222 58
0 -2 11 106.919 77.2814 63
0 -2 -11-37.1762 90.1270 61
0 2 -11-78.8767 141.810 53
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0 -2 -11-38.0625 139.939 53
0 2 11-36.8390 89.3094 39
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0 -2 -11-41.8250 101.396 26
0 -2 11 54.0177 58.5693 29
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0 -2 12 211.967 117.481 42
0 2 -12 175.528 111.891 22
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0 2 12-43.0282 93.6799 21
0 2 12 146.833 106.461 6
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0 2 -12 272.569 138.861 88
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14 -8 -6 3715.06 451.156 24
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14 -8 -4 5079.95 550.905 24
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22 -4 -17 14321.2 1265.14 80
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22 -4 -17 14512.8 1043.52 33
22 -4 -17 15009.6 1084.13 34
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22 -4 -16 1085.10 280.879 4
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22 -4 -16 1909.36 368.015 67
22 -4 -16 1494.12 331.762 55
22 -4 -16 1623.34 329.631 56
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22 -4 -16 2053.87 325.133 34
22 -4 -16 1727.03 295.831 33
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22 -4 -15 7566.45 695.711 33
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22 -4 -14 978.357 270.696 56
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22 -4 -14 237.542 184.215 33
22 -4 -14 960.933 270.423 34
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22 4 -13 792.416 253.897 5
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22 -4 -13 451.924 144.232 24
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22 -4 -13 387.379 223.617 80
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22 -4 -13 894.372 249.847 68
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22 -4 -13 130.430 235.339 56
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22 -4 -13 261.994 219.775 34
22 -4 -13 369.407 177.724 33
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22 -4 -12 2588.90 440.635 80
22 -4 -12 2388.66 367.291 66
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22 -4 -12 2722.14 404.603 68
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22 -4 -12 2540.96 330.485 24
22 -4 -12 1782.38 359.586 5
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22 -4 -12 2480.07 376.579 33
22 -4 -12 3006.99 409.944 34
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22 -4 -11 1905.05 384.516 80
22 -4 -11 1718.27 330.430 66
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22 -4 -11 1464.28 304.944 68
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22 -4 -11 1944.32 299.649 24
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22 -4 -11 2326.82 382.015 5
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22 -4 -10 1745.53 351.157 33
22 -4 -10 2005.45 357.000 34
22 -4 -10 1844.51 352.385 66
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22 -4 -10 1419.53 323.175 68
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22 -4 -10 1500.87 289.533 24
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22 -4 -10 2213.33 375.802 5
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22 -4 -9 1991.43 388.332 33
22 -4 -9 2313.64 376.981 34
22 -4 -9 2309.98 388.131 66
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22 -4 -9 2633.35 366.100 24
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22 -4 -8 139.529 200.176 66
-22 4 8 72.3558 78.6134 65
22 4 -8 169.245 183.557 74
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0 0 0 0.00 0.00 0
TITL Dival_bequer_auto in C2/c
REM C2/c (#15 in standard setting)
CELL 1.54184 30.041627 9.701783 24.098451 90.0000 129.7444 90.0000
ZERR 1.00 0.000911 0.000149 0.000663 0.0000 0.0046 0.0000
LATT 7
SYMM -x, y,-z+1/2
SFAC C H N O S
UNIT 208.00 240.00 32.00 32.00 16.00
REM CrysAlisPro recorded range (K): Min=299.1; max=299.3; aver:299.2
TEMP 26
SIZE 0.06 0.07 0.19
TREF
HKLF 4
END
;
_shelx_hkl_checksum 27453
_shelx_res_file
;
TITL 2 in space group C 1 2/c 1
shelx.res
created by SHELXL-2019/3 at 11:54:06 on 01-Aug-2024
CELL 1.54184 30.0416 9.7018 24.0984 90.000 129.744 90.000
ZERR 8.00 0.0009 0.0001 0.0007 0.000 0.005 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H N O S
UNIT 208 240 32 32 16
MERG 2
SHEL 50 0.83
HTAB N3 O3
EQIV $11 1-x, 1-y, -z
HTAB N4 N1_$11
HTAB C1 C16_$11
HTAB C1 C17_$11
HTAB C1 O4_$11
HTAB C26 C16_$11
EQIV $12 1-x, y, 1/2-z
HTAB N2 O2_$12
EQIV $13 1/2-x, 1/2-y, -z
HTAB C14 O1_$13
EQIV $14 1/2+x, 1/2-y, 1/2+z
HTAB C1 O4_$14
MPLA 3 C9 N3 S1
MPLA 6 C7 C8 C9 C10 C11 C12 N3 N4 N1 N2
MPLA 3 C10 N4 S2
CONF C10 C9 N3 S1
CONF C9 C10 N4 S2
DFIX 0.90 0.002 N2 h2 N3 H3 N4 H4
DANG 2.07 0.01 C10 H4 C9 H2
DANG 2.25 0.01 S2 H4 S1 H2
DANG 1.98 0.002 H2 C4
DANG 1.93 0.002 C7 H2
BOND $H
CONF
FMAP 2
PLAN 20
ACTA
LIST 4
L.S. 10
WGHT 0.063200 2.952300
FVAR 1.70099
C1 1 0.714229 0.432916 0.194018 11.00000 0.03743 0.09432 =
0.06128 0.01156 0.02646 -0.00133
AFIX 123
H1A 2 0.748099 0.382180 0.231771 10.50000 -1.50000
H1B 2 0.712625 0.439205 0.153013 10.50000 -1.50000
H1C 2 0.715882 0.523891 0.210925 10.50000 -1.50000
H1D 2 0.702971 0.514671 0.165368 10.50000 -1.50000
H1E 2 0.738446 0.457646 0.244126 10.50000 -1.50000
H1F 2 0.735188 0.372960 0.186215 10.50000 -1.50000
AFIX 0
C2 1 0.661583 0.360699 0.172826 11.00000 0.03714 0.06442 =
0.04162 0.00257 0.02375 0.00264
C3 1 0.667998 0.226663 0.208546 11.00000 0.04337 0.05884 =
0.04634 0.00397 0.02616 0.00995
AFIX 23
H3A 2 0.706441 0.190225 0.232322 11.00000 -1.20000
H3B 2 0.640257 0.161156 0.171684 11.00000 -1.20000
AFIX 0
C4 1 0.658874 0.238917 0.264304 11.00000 0.04125 0.05798 =
0.03846 0.00499 0.02200 0.00442
C5 1 0.711140 0.307008 0.332938 11.00000 0.04710 0.09606 =
0.04392 -0.00537 0.02148 -0.00318
AFIX 33
H5A 2 0.744875 0.251282 0.353661 11.00000 -1.50000
H5B 2 0.716995 0.396575 0.321630 11.00000 -1.50000
H5C 2 0.704515 0.316115 0.366814 11.00000 -1.50000
AFIX 0
C6 1 0.648973 0.096258 0.280544 11.00000 0.06981 0.06696 =
0.06623 0.01374 0.04278 0.00729
AFIX 33
H6A 2 0.682163 0.039472 0.299776 11.00000 -1.50000
H6B 2 0.643105 0.103426 0.315199 11.00000 -1.50000
H6C 2 0.615391 0.055690 0.236924 11.00000 -1.50000
AFIX 0
C7 1 0.558545 0.316899 0.159605 11.00000 0.03810 0.04814 =
0.04164 0.00080 0.02418 0.00370
C8 1 0.505672 0.278596 0.140680 11.00000 0.04449 0.05988 =
0.04632 0.00753 0.03132 0.00467
AFIX 43
H8 2 0.503867 0.252706 0.176358 11.00000 -1.20000
AFIX 0
C9 1 0.456396 0.278885 0.069864 11.00000 0.03818 0.04949 =
0.05249 0.00339 0.02933 -0.00047
C10 1 0.458685 0.313729 0.015275 11.00000 0.03564 0.04758 =
0.04011 0.00130 0.02054 0.00052
C11 1 0.511670 0.349378 0.035039 11.00000 0.03909 0.05213 =
0.03990 0.00371 0.02434 -0.00019
AFIX 43
H11 2 0.513870 0.371146 -0.000732 11.00000 -1.20000
AFIX 0
C12 1 0.561605 0.353584 0.106669 11.00000 0.03602 0.04749 =
0.04130 0.00179 0.02313 0.00036
C13 1 0.339105 0.465422 0.024076 11.00000 0.05082 0.07237 =
0.05835 -0.00619 0.03680 -0.00187
C14 1 0.281000 0.491681 -0.014456 11.00000 0.05331 0.08412 =
0.07326 -0.00697 0.03576 0.00122
AFIX 43
H14 2 0.257394 0.427948 -0.015412 11.00000 -1.20000
AFIX 0
C15 1 0.258429 0.615697 -0.051910 11.00000 0.07045 0.09825 =
0.08248 -0.00029 0.03760 0.02487
AFIX 43
H15 2 0.219378 0.634561 -0.077511 11.00000 -1.20000
AFIX 0
C16 1 0.292000 0.710693 -0.052177 11.00000 0.11901 0.07166 =
0.09032 0.00343 0.06984 0.01681
C17 1 0.349215 0.680764 -0.014893 11.00000 0.11386 0.06900 =
0.11498 0.00133 0.08479 0.00070
AFIX 43
H17 2 0.372295 0.742935 -0.015821 11.00000 -1.20000
AFIX 0
C18 1 0.373284 0.560818 0.023881 11.00000 0.07423 0.07468 =
0.09826 -0.00243 0.06122 -0.00394
AFIX 43
H18 2 0.412529 0.543677 0.049999 11.00000 -1.20000
AFIX 0
C19 1 0.265875 0.845549 -0.093989 11.00000 0.19583 0.09841 =
0.14745 0.03945 0.11207 0.06169
AFIX 33
H19A 2 0.225538 0.848871 -0.116638 11.00000 -1.50000
H19B 2 0.285586 0.921905 -0.061396 11.00000 -1.50000
H19C 2 0.270076 0.850652 -0.130220 11.00000 -1.50000
AFIX 0
C20 1 0.438944 0.185986 -0.124968 11.00000 0.06415 0.06051 =
0.04677 -0.01058 0.02703 -0.00134
C21 1 0.480013 0.082133 -0.092368 11.00000 0.08095 0.05911 =
0.07164 -0.00163 0.03704 0.00389
AFIX 43
H21 2 0.480013 0.015334 -0.064689 11.00000 -1.20000
AFIX 0
C22 1 0.520973 0.078820 -0.101398 11.00000 0.08115 0.08092 =
0.09104 -0.00800 0.04394 0.02004
AFIX 43
H22 2 0.548284 0.008389 -0.079624 11.00000 -1.20000
AFIX 0
C23 1 0.522862 0.176398 -0.141633 11.00000 0.08818 0.10882 =
0.07409 -0.00779 0.05173 0.01661
C24 1 0.482143 0.281641 -0.172118 11.00000 0.10351 0.10617 =
0.07699 0.01189 0.06423 0.01946
AFIX 43
H24 2 0.483135 0.350438 -0.198185 11.00000 -1.20000
AFIX 0
C25 1 0.440440 0.286727 -0.164756 11.00000 0.08140 0.07939 =
0.06065 0.00722 0.04368 0.01762
AFIX 43
H25 2 0.413262 0.357449 -0.186358 11.00000 -1.20000
AFIX 0
C26 1 0.567668 0.167454 -0.151094 11.00000 0.11561 0.20094 =
0.11061 -0.00823 0.08227 0.03432
AFIX 33
H26A 2 0.562704 0.242966 -0.180352 11.00000 -1.50000
H26B 2 0.605636 0.171689 -0.104721 11.00000 -1.50000
H26C 2 0.563253 0.082000 -0.174247 11.00000 -1.50000
AFIX 0
N1 3 0.611758 0.413135 0.122798 11.00000 0.03521 0.05965 =
0.04270 0.00400 0.02266 -0.00145
N2 3 0.607995 0.328807 0.234431 11.00000 0.04135 0.06656 =
0.03762 0.00056 0.02338 0.00532
H2 2 0.593832 0.309970 0.258258 11.00000 -1.20000
N3 3 0.401861 0.234563 0.048870 11.00000 0.04102 0.06736 =
0.05824 0.00075 0.03141 -0.00585
H3 2 0.377007 0.206325 0.002678 11.00000 -1.20000
N4 3 0.405908 0.323072 -0.058406 11.00000 0.03692 0.05645 =
0.04311 0.00076 0.01893 -0.00314
H4 2 0.396448 0.408319 -0.078083 11.00000 -1.20000
O1 4 0.322797 0.222840 0.052073 11.00000 0.06016 0.10478 =
0.10984 0.02225 0.06193 -0.00494
O2 4 0.412655 0.346255 0.148655 11.00000 0.05973 0.14250 =
0.05540 0.00649 0.03956 0.01006
O3 4 0.390192 0.072393 -0.078750 11.00000 0.10364 0.06799 =
0.09851 -0.01448 0.06047 -0.03598
O4 4 0.333426 0.237548 -0.180789 11.00000 0.04851 0.12455 =
0.05508 -0.02047 0.01250 -0.01822
S1 5 0.369286 0.311893 0.074226 11.00000 0.04510 0.08720 =
0.06183 0.01067 0.03803 0.00080
S2 5 0.386989 0.196032 -0.113736 11.00000 0.05384 0.06925 =
0.05347 -0.01260 0.02376 -0.01888
HKLF 4
REM 2 in space group C 1 2/c 1
REM wR2 = 0.1262, GooF = S = 1.067, Restrained GooF = 5.229 for all data
REM R1 = 0.0425 for 3970 Fo > 4sig(Fo) and 0.0533 for all 4942 data
REM 334 parameters refined using 9 restraints
END
WGHT 0.0632 2.9484
REM Highest difference peak 0.414, deepest hole -0.340, 1-sigma level 0.038
Q1 1 0.5000 0.4872 -0.2500 10.50000 0.05 0.19
Q2 1 0.3692 0.1433 -0.0795 11.00000 0.05 0.15
Q3 1 0.4344 0.4179 0.1576 11.00000 0.05 0.14
Q4 1 0.6003 0.0694 -0.0992 11.00000 0.05 0.14
Q5 1 0.2535 0.9071 -0.0710 11.00000 0.05 0.14
Q6 1 0.4858 0.2994 0.0216 11.00000 0.05 0.14
Q7 1 0.3462 0.2761 0.0989 11.00000 0.05 0.14
Q8 1 0.6051 0.3717 0.2709 11.00000 0.05 0.12
Q9 1 0.4366 0.3049 -0.0173 11.00000 0.05 0.12
Q10 1 0.5881 0.3882 0.1181 11.00000 0.05 0.12
Q11 1 0.6621 0.2899 0.1901 11.00000 0.05 0.12
Q12 1 0.5318 0.3826 0.0696 11.00000 0.05 0.12
Q13 1 0.4215 0.1998 -0.1081 11.00000 0.05 0.12
Q14 1 0.4349 0.1956 -0.1516 11.00000 0.05 0.12
Q15 1 0.7471 0.3264 0.3392 11.00000 0.05 0.12
Q16 1 0.3923 0.3678 0.1136 11.00000 0.05 0.11
Q17 1 0.5871 0.2986 -0.1506 11.00000 0.05 0.11
Q18 1 0.3869 0.2781 -0.0793 11.00000 0.05 0.11
Q19 1 0.4407 0.5048 0.0876 11.00000 0.05 0.11
Q20 1 0.5558 0.1572 -0.2080 11.00000 0.05 0.10
;
_shelx_res_checksum 66814
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C C1 0.71423(9) 0.4329(3) 0.19402(12) 0.0680(6) Uani d 1 . .
H H1A 0.748099 0.382180 0.231771 0.102 Uiso calc 0.5 . .
H H1B 0.712625 0.439205 0.153013 0.102 Uiso calc 0.5 . .
H H1C 0.715882 0.523891 0.210925 0.102 Uiso calc 0.5 . .
H H1D 0.702971 0.514671 0.165368 0.102 Uiso calc 0.5 . .
H H1E 0.738446 0.457646 0.244126 0.102 Uiso calc 0.5 . .
H H1F 0.735188 0.372960 0.186215 0.102 Uiso calc 0.5 . .
C C2 0.66158(8) 0.3607(2) 0.17283(10) 0.0488(4) Uani d 1 . .
C C3 0.66800(8) 0.2267(2) 0.20855(10) 0.0513(5) Uani d 1 . .
H H3A 0.706441 0.190225 0.232322 0.062 Uiso calc 1 . .
H H3B 0.640257 0.161156 0.171684 0.062 Uiso calc 1 . .
C C4 0.65887(8) 0.2389(2) 0.26430(9) 0.0484(4) Uani d 1 . .
C C5 0.71114(9) 0.3070(3) 0.33294(11) 0.0679(6) Uani d 1 . .
H H5A 0.744875 0.251282 0.353661 0.102 Uiso calc 1 . .
H H5B 0.716995 0.396575 0.321630 0.102 Uiso calc 1 . .
H H5C 0.704515 0.316115 0.366814 0.102 Uiso calc 1 . .
C C6 0.64897(11) 0.0963(2) 0.28054(13) 0.0682(6) Uani d 1 . .
H H6A 0.682163 0.039472 0.299776 0.102 Uiso calc 1 . .
H H6B 0.643105 0.103426 0.315199 0.102 Uiso calc 1 . .
H H6C 0.615391 0.055690 0.236924 0.102 Uiso calc 1 . .
C C7 0.55854(8) 0.31690(18) 0.15961(9) 0.0436(4) Uani d 1 . .
C C8 0.50567(8) 0.2786(2) 0.14068(10) 0.0486(4) Uani d 1 . .
H H8 0.503867 0.252706 0.176358 0.058 Uiso calc 1 . .
C C9 0.45640(8) 0.27889(19) 0.06986(10) 0.0465(4) Uani d 1 . .
C C10 0.45868(8) 0.31373(18) 0.01528(9) 0.0438(4) Uani d 1 . .
C C11 0.51167(8) 0.34938(19) 0.03504(9) 0.0444(4) Uani d 1 . .
H H11 0.513870 0.371146 -0.000732 0.053 Uiso calc 1 . .
C C12 0.56160(7) 0.35358(19) 0.10667(9) 0.0427(4) Uani d 1 . .
C C13 0.33911(9) 0.4654(2) 0.02408(11) 0.0591(5) Uani d 1 . .
C C14 0.28100(10) 0.4917(3) -0.01446(13) 0.0736(7) Uani d 1 . .
H H14 0.257394 0.427948 -0.015412 0.088 Uiso calc 1 . .
C C15 0.25843(13) 0.6157(3) -0.05191(16) 0.0919(9) Uani d 1 . .
H H15 0.219378 0.634561 -0.077511 0.110 Uiso calc 1 . .
C C16 0.29200(17) 0.7107(3) -0.05218(17) 0.0916(9) Uani d 1 . .
C C17 0.34921(16) 0.6808(3) -0.01489(19) 0.0909(9) Uani d 1 . .
H H17 0.372295 0.742935 -0.015821 0.109 Uiso calc 1 . .
C C18 0.37328(12) 0.5608(3) 0.02388(16) 0.0780(7) Uani d 1 . .
H H18 0.412529 0.543677 0.049999 0.094 Uiso calc 1 . .
C C19 0.2659(2) 0.8455(4) -0.0940(2) 0.1455(17) Uani d 1 . .
H H19A 0.225538 0.848871 -0.116638 0.218 Uiso calc 1 . .
H H19B 0.285586 0.921905 -0.061396 0.218 Uiso calc 1 . .
H H19C 0.270076 0.850652 -0.130220 0.218 Uiso calc 1 . .
C C20 0.43894(10) 0.1860(2) -0.12497(11) 0.0632(6) Uani d 1 . .
C C21 0.48001(12) 0.0821(3) -0.09237(14) 0.0790(7) Uani d 1 . .
H H21 0.480013 0.015334 -0.064689 0.095 Uiso calc 1 . .
C C22 0.52097(13) 0.0788(3) -0.10140(17) 0.0924(9) Uani d 1 . .
H H22 0.548284 0.008389 -0.079624 0.111 Uiso calc 1 . .
C C23 0.52286(14) 0.1764(4) -0.14163(16) 0.0905(9) Uani d 1 . .
C C24 0.48214(14) 0.2816(3) -0.17212(16) 0.0909(9) Uani d 1 . .
H H24 0.483135 0.350438 -0.198185 0.109 Uiso calc 1 . .
C C25 0.44044(12) 0.2867(3) -0.16476(13) 0.0751(7) Uani d 1 . .
H H25 0.413262 0.357449 -0.186358 0.090 Uiso calc 1 . .
C C26 0.56767(18) 0.1675(5) -0.1511(2) 0.1352(16) Uani d 1 . .
H H26A 0.562704 0.242966 -0.180352 0.203 Uiso calc 1 . .
H H26B 0.605636 0.171689 -0.104721 0.203 Uiso calc 1 . .
H H26C 0.563253 0.082000 -0.174247 0.203 Uiso calc 1 . .
N N1 0.61176(6) 0.41314(17) 0.12280(8) 0.0475(4) Uani d 1 . .
N N2 0.60800(7) 0.32881(17) 0.23443(8) 0.0499(4) Uani d 1 . .
H H2 0.59383(15) 0.3100(8) 0.25826(17) 0.060 Uiso d 1 . .
N N3 0.40186(7) 0.23456(19) 0.04887(9) 0.0558(4) Uani d 1 . .
H H3 0.3770(8) 0.206(2) 0.0027(4) 0.067 Uiso d 1 . .
N N4 0.40591(7) 0.32307(17) -0.05841(8) 0.0503(4) Uani d 1 . .
H H4 0.3964(7) 0.4083(5) -0.0781(5) 0.060 Uiso d 1 . .
O O1 0.32280(7) 0.2228(2) 0.05207(11) 0.0861(6) Uani d 1 . .
O O2 0.41265(7) 0.3463(2) 0.14866(8) 0.0839(5) Uani d 1 . .
O O3 0.39019(9) 0.07239(18) -0.07875(11) 0.0930(6) Uani d 1 . .
O O4 0.33343(7) 0.2375(2) -0.18079(9) 0.0909(6) Uani d 1 . .
S S1 0.36929(2) 0.31189(6) 0.07423(3) 0.06194(18) Uani d 1 . .
S S2 0.38699(2) 0.19603(6) -0.11374(3) 0.06646(19) 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 0.0374(10) 0.0943(17) 0.0613(12) -0.0013(10) 0.0265(10) 0.0116(12)
C2 0.0371(9) 0.0644(12) 0.0416(9) 0.0026(8) 0.0237(8) 0.0026(8)
C3 0.0434(10) 0.0588(12) 0.0463(10) 0.0100(9) 0.0262(9) 0.0040(8)
C4 0.0413(10) 0.0580(11) 0.0385(9) 0.0044(8) 0.0220(8) 0.0050(8)
C5 0.0471(12) 0.0961(18) 0.0439(11) -0.0032(11) 0.0215(10) -0.0054(11)
C6 0.0698(14) 0.0670(14) 0.0662(13) 0.0073(11) 0.0428(12) 0.0137(11)
C7 0.0381(9) 0.0481(10) 0.0416(9) 0.0037(7) 0.0242(8) 0.0008(7)
C8 0.0445(10) 0.0599(11) 0.0463(10) 0.0047(8) 0.0313(9) 0.0075(8)
C9 0.0382(9) 0.0495(10) 0.0525(10) -0.0005(8) 0.0293(9) 0.0034(8)
C10 0.0356(9) 0.0476(10) 0.0401(9) 0.0005(7) 0.0205(8) 0.0013(7)
C11 0.0391(9) 0.0521(10) 0.0399(9) -0.0002(8) 0.0243(8) 0.0037(8)
C12 0.0360(9) 0.0475(10) 0.0413(9) 0.0004(7) 0.0231(8) 0.0018(7)
C13 0.0508(11) 0.0724(14) 0.0584(12) -0.0019(10) 0.0368(10) -0.0062(10)
C14 0.0533(13) 0.0841(17) 0.0733(15) 0.0012(12) 0.0358(12) -0.0070(13)
C15 0.0704(17) 0.098(2) 0.0825(18) 0.0249(16) 0.0376(15) -0.0003(16)
C16 0.119(3) 0.0717(17) 0.090(2) 0.0168(18) 0.070(2) 0.0034(14)
C17 0.114(3) 0.0690(17) 0.115(2) 0.0007(16) 0.085(2) 0.0013(15)
C18 0.0742(16) 0.0747(16) 0.0983(19) -0.0039(13) 0.0612(16) -0.0024(14)
C19 0.196(5) 0.098(3) 0.147(4) 0.062(3) 0.112(4) 0.039(2)
C20 0.0641(14) 0.0605(13) 0.0468(11) -0.0013(10) 0.0270(10) -0.0106(9)
C21 0.0810(17) 0.0591(14) 0.0716(15) 0.0039(12) 0.0370(14) -0.0016(11)
C22 0.0811(19) 0.0809(19) 0.091(2) 0.0200(15) 0.0439(17) -0.0080(16)
C23 0.088(2) 0.109(2) 0.0741(17) 0.0166(17) 0.0517(16) -0.0078(16)
C24 0.104(2) 0.106(2) 0.0770(17) 0.0195(18) 0.0642(17) 0.0119(16)
C25 0.0814(17) 0.0794(16) 0.0606(14) 0.0176(13) 0.0437(13) 0.0072(12)
C26 0.116(3) 0.201(5) 0.111(3) 0.034(3) 0.082(3) -0.008(3)
N1 0.0352(8) 0.0597(9) 0.0427(8) -0.0015(7) 0.0227(7) 0.0040(7)
N2 0.0413(8) 0.0666(10) 0.0376(8) 0.0053(7) 0.0234(7) 0.0006(7)
N3 0.0410(9) 0.0674(11) 0.0582(10) -0.0059(8) 0.0314(8) 0.0007(8)
N4 0.0369(8) 0.0565(10) 0.0431(8) -0.0031(7) 0.0189(7) 0.0008(7)
O1 0.0602(10) 0.1048(14) 0.1098(14) -0.0049(9) 0.0619(11) 0.0222(11)
O2 0.0597(10) 0.1425(17) 0.0554(9) 0.0101(10) 0.0396(8) 0.0065(10)
O3 0.1036(14) 0.0680(11) 0.0985(13) -0.0360(10) 0.0605(12) -0.0145(10)
O4 0.0485(9) 0.1245(15) 0.0551(9) -0.0182(10) 0.0125(8) -0.0205(10)
S1 0.0451(3) 0.0872(4) 0.0618(3) 0.0008(2) 0.0380(3) 0.0107(3)
S2 0.0538(3) 0.0693(4) 0.0535(3) -0.0189(2) 0.0238(3) -0.0126(2)
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C2 C1 H1D . . 109.5 ?
C2 C1 H1E . . 109.5 ?
H1D C1 H1E . . 109.5 ?
C2 C1 H1F . . 109.5 ?
H1D C1 H1F . . 109.5 ?
H1E C1 H1F . . 109.5 ?
N1 C2 C1 . . 118.73(19) ?
N1 C2 C3 . . 121.80(17) ?
C1 C2 C3 . . 119.43(17) ?
C2 C3 C4 . . 113.85(16) ?
C2 C3 H3A . . 108.8 ?
C4 C3 H3A . . 108.8 ?
C2 C3 H3B . . 108.8 ?
C4 C3 H3B . . 108.8 ?
H3A C3 H3B . . 107.7 ?
N2 C4 C6 . . 110.45(17) ?
N2 C4 C5 . . 107.38(17) ?
C6 C4 C5 . . 110.58(17) ?
N2 C4 C3 . . 108.95(14) ?
C6 C4 C3 . . 109.17(18) ?
C5 C4 C3 . . 110.28(17) ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
C4 C6 H6A . . 109.5 ?
C4 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C4 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C12 C7 C8 . . 120.05(16) ?
C12 C7 N2 . . 120.93(16) ?
C8 C7 N2 . . 118.80(16) ?
C9 C8 C7 . . 120.35(17) ?
C9 C8 H8 . . 119.8 ?
C7 C8 H8 . . 119.8 ?
C8 C9 C10 . . 120.51(17) ?
C8 C9 N3 . . 121.27(17) ?
C10 C9 N3 . . 118.08(16) ?
C11 C10 C9 . . 118.27(16) ?
C11 C10 N4 . . 121.76(16) ?
C9 C10 N4 . . 119.75(16) ?
C10 C11 C12 . . 121.84(17) ?
C10 C11 H11 . . 119.1 ?
C12 C11 H11 . . 119.1 ?
C7 C12 C11 . . 118.95(17) ?
C7 C12 N1 . . 122.57(16) ?
C11 C12 N1 . . 117.92(16) ?
C14 C13 C18 . . 119.8(2) ?
C14 C13 S1 . . 119.55(19) ?
C18 C13 S1 . . 120.68(18) ?
C13 C14 C15 . . 118.6(3) ?
C13 C14 H14 . . 120.7 ?
C15 C14 H14 . . 120.7 ?
C16 C15 C14 . . 122.0(3) ?
C16 C15 H15 . . 119.0 ?
C14 C15 H15 . . 119.0 ?
C17 C16 C15 . . 118.3(3) ?
C17 C16 C19 . . 121.0(4) ?
C15 C16 C19 . . 120.7(4) ?
C16 C17 C18 . . 121.4(3) ?
C16 C17 H17 . . 119.3 ?
C18 C17 H17 . . 119.3 ?
C17 C18 C13 . . 120.0(3) ?
C17 C18 H18 . . 120.0 ?
C13 C18 H18 . . 120.0 ?
C16 C19 H19A . . 109.5 ?
C16 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C16 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C21 C20 C25 . . 119.6(3) ?
C21 C20 S2 . . 120.8(2) ?
C25 C20 S2 . . 119.55(19) ?
C22 C21 C20 . . 119.2(3) ?
C22 C21 H21 . . 120.4 ?
C20 C21 H21 . . 120.4 ?
C21 C22 C23 . . 122.4(3) ?
C21 C22 H22 . . 118.8 ?
C23 C22 H22 . . 118.8 ?
C22 C23 C24 . . 117.2(3) ?
C22 C23 C26 . . 120.6(3) ?
C24 C23 C26 . . 122.2(3) ?
C25 C24 C23 . . 121.7(3) ?
C25 C24 H24 . . 119.1 ?
C23 C24 H24 . . 119.1 ?
C24 C25 C20 . . 119.9(3) ?
C24 C25 H25 . . 120.1 ?
C20 C25 H25 . . 120.1 ?
C23 C26 H26A . . 109.5 ?
C23 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C23 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C2 N1 C12 . . 119.57(16) ?
C7 N2 C4 . . 118.74(15) ?
C7 N2 H2 . . 104.3(3) ?
C4 N2 H2 . . 108.8(3) ?
C9 N3 S1 . . 123.55(15) ?
C9 N3 H3 . . 112.6(16) ?
S1 N3 H3 . . 112.4(16) ?
C10 N4 S2 . . 119.65(13) ?
C10 N4 H4 . . 115.7(7) ?
S2 N4 H4 . . 115.8(7) ?
O1 S1 O2 . . 120.08(12) ?
O1 S1 N3 . . 105.07(11) ?
O2 S1 N3 . . 107.10(10) ?
O1 S1 C13 . . 107.74(11) ?
O2 S1 C13 . . 108.70(12) ?
N3 S1 C13 . . 107.52(10) ?
O4 S2 O3 . . 120.33(12) ?
O4 S2 N4 . . 105.31(11) ?
O3 S2 N4 . . 107.14(10) ?
O4 S2 C20 . . 108.19(12) ?
O3 S2 C20 . . 108.26(13) ?
N4 S2 C20 . . 106.86(9) ?
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 C2 . 1.490(3) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C1 H1D . 0.9600 ?
C1 H1E . 0.9600 ?
C1 H1F . 0.9600 ?
C2 N1 . 1.283(2) ?
C2 C3 . 1.502(3) ?
C3 C4 . 1.538(3) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 N2 . 1.486(2) ?
C4 C6 . 1.519(3) ?
C4 C5 . 1.522(3) ?
C5 H5A . 0.9600 ?
C5 H5B . 0.9600 ?
C5 H5C . 0.9600 ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C7 C12 . 1.383(3) ?
C7 C8 . 1.394(3) ?
C7 N2 . 1.431(2) ?
C8 C9 . 1.369(3) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.402(3) ?
C9 N3 . 1.437(2) ?
C10 C11 . 1.382(3) ?
C10 N4 . 1.440(2) ?
C11 C12 . 1.386(2) ?
C11 H11 . 0.9300 ?
C12 N1 . 1.416(2) ?
C13 C14 . 1.379(3) ?
C13 C18 . 1.385(3) ?
C13 S1 . 1.761(2) ?
C14 C15 . 1.393(4) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.369(5) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.368(5) ?
C16 C19 . 1.527(5) ?
C17 C18 . 1.373(4) ?
C17 H17 . 0.9300 ?
C18 H18 . 0.9300 ?
C19 H19A . 0.9600 ?
C19 H19B . 0.9600 ?
C19 H19C . 0.9600 ?
C20 C21 . 1.384(3) ?
C20 C25 . 1.390(4) ?
C20 S2 . 1.749(3) ?
C21 C22 . 1.380(4) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.382(5) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.389(4) ?
C23 C26 . 1.505(5) ?
C24 C25 . 1.374(4) ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
C26 H26A . 0.9600 ?
C26 H26B . 0.9600 ?
C26 H26C . 0.9600 ?
N2 H2 . 0.926(2) ?
N3 S1 . 1.6305(19) ?
N3 H3 . 0.899(2) ?
N4 S2 . 1.6282(17) ?
N4 H4 . 0.904(2) ?
O1 S1 . 1.4243(17) ?
O2 S1 . 1.4274(17) ?
O3 S2 . 1.4336(19) ?
O4 S2 . 1.4275(18) ?
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
N3 H3 O3 . 0.899(2) 2.586(18) 3.268(3) 133.1(19) yes
N4 H4 N1 5_665 0.904(2) 1.970(5) 2.861(2) 168.1(18) yes
C1 H1B C16 5_665 0.96 2.76 3.584(4) 144.5 yes
C1 H1B C17 5_665 0.96 2.82 3.600(4) 138.5 yes
C1 H1C O4 5_665 0.96 2.59 3.434(4) 146.9 yes
C26 H26B C16 5_665 0.96 3.19 4.094(5) 157.2 yes
N2 H2 O2 2_655 0.926(2) 2.399(3) 3.254(2) 153.6(6) yes
C14 H14 O1 7 0.93 2.45 3.356(3) 164.7 yes
C1 H1A O4 8_556 0.96 2.34 3.293(3) 175.6 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C2 C3 C4 . . . . -77.0(2) ?
C1 C2 C3 C4 . . . . 105.2(2) ?
C2 C3 C4 N2 . . . . 43.0(2) ?
C2 C3 C4 C6 . . . . 163.73(17) ?
C2 C3 C4 C5 . . . . -74.6(2) ?
C12 C7 C8 C9 . . . . -0.9(3) ?
N2 C7 C8 C9 . . . . 173.77(17) ?
C7 C8 C9 C10 . . . . 1.9(3) ?
C7 C8 C9 N3 . . . . 177.50(18) ?
C8 C9 C10 C11 . . . . -0.9(3) ?
N3 C9 C10 C11 . . . . -176.63(17) ?
C8 C9 C10 N4 . . . . -175.58(17) ?
N3 C9 C10 N4 . . . . 8.7(3) ?
C9 C10 C11 C12 . . . . -1.1(3) ?
N4 C10 C11 C12 . . . . 173.48(17) ?
C8 C7 C12 C11 . . . . -1.0(3) ?
N2 C7 C12 C11 . . . . -175.60(17) ?
C8 C7 C12 N1 . . . . 170.16(17) ?
N2 C7 C12 N1 . . . . -4.4(3) ?
C10 C11 C12 C7 . . . . 2.0(3) ?
C10 C11 C12 N1 . . . . -169.54(17) ?
C18 C13 C14 C15 . . . . -1.0(4) ?
S1 C13 C14 C15 . . . . 178.0(2) ?
C13 C14 C15 C16 . . . . 0.8(4) ?
C14 C15 C16 C17 . . . . 0.7(5) ?
C14 C15 C16 C19 . . . . 179.8(3) ?
C15 C16 C17 C18 . . . . -2.0(5) ?
C19 C16 C17 C18 . . . . 178.8(3) ?
C16 C17 C18 C13 . . . . 1.9(4) ?
C14 C13 C18 C17 . . . . -0.3(4) ?
S1 C13 C18 C17 . . . . -179.3(2) ?
C25 C20 C21 C22 . . . . -1.5(4) ?
S2 C20 C21 C22 . . . . -178.9(2) ?
C20 C21 C22 C23 . . . . 0.4(4) ?
C21 C22 C23 C24 . . . . 1.3(5) ?
C21 C22 C23 C26 . . . . -179.0(3) ?
C22 C23 C24 C25 . . . . -2.0(5) ?
C26 C23 C24 C25 . . . . 178.2(3) ?
C23 C24 C25 C20 . . . . 1.1(4) ?
C21 C20 C25 C24 . . . . 0.7(4) ?
S2 C20 C25 C24 . . . . 178.2(2) ?
C1 C2 N1 C12 . . . . -173.93(18) ?
C3 C2 N1 C12 . . . . 8.2(3) ?
C7 C12 N1 C2 . . . . 46.0(3) ?
C11 C12 N1 C2 . . . . -142.70(19) ?
C12 C7 N2 C4 . . . . -66.2(2) ?
C8 C7 N2 C4 . . . . 119.17(19) ?
C6 C4 N2 C7 . . . . -80.7(2) ?
C5 C4 N2 C7 . . . . 158.70(17) ?
C3 C4 N2 C7 . . . . 39.3(2) ?
C8 C9 N3 S1 . . . . 63.0(2) ?
C10 C9 N3 S1 . . . . -121.29(18) ?
C11 C10 N4 S2 . . . . 84.8(2) ?
C9 C10 N4 S2 . . . . -100.66(19) ?
C9 N3 S1 O1 . . . . -170.52(16) ?
C9 N3 S1 O2 . . . . -41.78(19) ?
C9 N3 S1 C13 . . . . 74.90(18) ?
C14 C13 S1 O1 . . . . 13.3(2) ?
C18 C13 S1 O1 . . . . -167.7(2) ?
C14 C13 S1 O2 . . . . -118.3(2) ?
C18 C13 S1 O2 . . . . 60.7(2) ?
C14 C13 S1 N3 . . . . 126.10(19) ?
C18 C13 S1 N3 . . . . -54.9(2) ?
C10 N4 S2 O4 . . . . 179.53(15) ?
C10 N4 S2 O3 . . . . 50.30(18) ?
C10 N4 S2 C20 . . . . -65.56(17) ?
C21 C20 S2 O4 . . . . -141.53(19) ?
C25 C20 S2 O4 . . . . 41.1(2) ?
C21 C20 S2 O3 . . . . -9.6(2) ?
C25 C20 S2 O3 . . . . 173.00(18) ?
C21 C20 S2 N4 . . . . 105.52(19) ?
C25 C20 S2 N4 . . . . -71.9(2) ?
C10 C9 N3 S1 . . . . -121.29(18) ?
C9 C10 N4 S2 . . . . -100.66(19) ?
_cod_database_fobs_code 2312587