#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:33:30 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289425 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/05/1570562.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570562
loop_
_publ_author_name
'Dharmasivam, Mahendiran'
'Kaya, Busra'
'Wijesinghe, Tharushi P.'
'Richardson, Vera'
'Harmer, Jeffrey R.'
'Gonzalvez, Miguel A.'
'Lewis, William'
'Azad, Mahan Gholam'
'Bernhardt, Paul V.'
'Richardson, Des R.'
_publ_section_title
;
 Differential transmetallation of complexes of the anti-cancer
 thiosemicarbazone, Dp4e4mT: effects on anti-proliferative efficacy, redox
 activity, oxy-myoglobin and oxy-hemoglobin oxidation.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              974
_journal_page_last               990
_journal_paper_doi               10.1039/d3sc05723b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C30 H34 N10 Ni S2, 2(Cl), H2 O'
_chemical_formula_sum            'C30 H36 Cl2 N10 Ni O S2'
_chemical_formula_weight         746.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-17 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                94.82(2)
_cell_angle_beta                 92.36(2)
_cell_angle_gamma                107.67(3)
_cell_formula_units_Z            2
_cell_length_a                   9.141(3)
_cell_length_b                   14.090(4)
_cell_length_c                   14.188(3)
_cell_measurement_reflns_used    738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.7590
_cell_measurement_theta_min      5.1360
_cell_volume                     1730.7(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  34.00   1.00   30.00    --  -39.89  38.00 120.00   79
  2  ω    -79.00 -51.00   1.00   30.00    --  -39.89 178.00-150.00   28
  3  ω    -57.00  26.00   1.00   30.00    --  -39.89  57.00 -60.00   83
  4  ω    -84.00  36.00   1.00   30.00    --  -39.89  19.00-120.00  120
  5  ω     57.00 130.00   1.00   30.00    --   39.89 178.00 120.00   73
  6  ω     80.00 130.00   1.00   30.00    --   39.89 178.00 -90.00   50
  7  ω     57.00  86.00   1.00  120.00    --  108.56 -30.00 -60.00   29
  8  ω     37.00  94.00   1.00  120.00    --  108.56 -45.00  60.00   57
  9  ω     36.00  97.00   1.00  120.00    --  108.56 -45.00 120.00   61
 10  ω     43.00 118.00   1.00  120.00    --  108.56-125.00 150.00   75
 11  ω     31.00  87.00   1.00  120.00    --  108.56 -30.00-180.00   56
 12  ω     27.00 110.00   1.00  120.00    --  108.56 -95.00 -60.00   83
 13  ω     98.00 125.00   1.00  120.00    --  108.56 125.00 -90.00   27
 14  ω     85.00 178.00   1.00  120.00    --  108.56  30.00   0.00   93
 15  ω     34.00  98.00   1.00  120.00    --  108.56 -45.00 -90.00   64
 16  ω     59.00 117.00   1.00  120.00    --  108.56-125.00 -90.00   58
 17  ω     35.00  93.00   1.00  120.00    --  108.56 -45.00   0.00   58
 18  ω     69.00  97.00   1.00  120.00    --  108.56-125.00-150.00   28
 19  ω     57.00  82.00   1.00  120.00    --  108.56 -61.00-150.00   25
 20  ω    102.00 129.00   1.00  120.00    --  108.56 125.00-180.00   27
 21  ω     50.00 101.00   1.00  120.00    --  108.56 -95.00  30.00   51
 22  ω     85.00 177.00   1.00  120.00    --  108.56  30.00  90.00   92
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0345128000
_diffrn_orient_matrix_UB_12      0.0176234000
_diffrn_orient_matrix_UB_13      -0.1031422000
_diffrn_orient_matrix_UB_21      -0.1729235000
_diffrn_orient_matrix_UB_22      -0.0280451000
_diffrn_orient_matrix_UB_23      0.0161855000
_diffrn_orient_matrix_UB_31      0.0186916000
_diffrn_orient_matrix_UB_32      0.1104828000
_diffrn_orient_matrix_UB_33      0.0321221000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.1703
_diffrn_reflns_av_unetI/netI     0.2578
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11803
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.368
_diffrn_reflns_theta_min         4.322
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_recrystallization_method 'crystallised from methanol'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.2326
_refine_ls_R_factor_gt           0.1045
_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/[σ²(Fo²)+(0.0781P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2267
_refine_ls_wR_factor_ref         0.2878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2584
_reflns_number_total             6761
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc05723b2.cif
_cod_data_source_block           drr18_s1677
_cod_depositor_comments
'Adding full bibliography for 1570562--1570567.cif.'
_cod_original_cell_volume        1730.8(9)
_cod_database_code               1570562
_sydney_internal_submission_code drr18_s1677
_sydney_internal_submission_date 2018-09-21
_sydney_internal_submission_number s1677
_sydney_internal_client_code     dm1
_sydney_internal_client_email    mahendiran.dharmasivam@sydney.edu.au
_sydney_internal_client_name     'Mahendiran Dharmasivam'
_sydney_internal_supervisor_code drr
_sydney_internal_supervisor_name 'Des Richardson'
_sydney_internal_collection_date 2018-09-24
_sydney_internal_collection_user wlew0588
_sydney_internal_process_date    2018-09-27
_sydney_internal_process_user    wlew0588
_sydney_internal_solution_date   2018-09-27
_sydney_internal_solution_user   wlew0588
_sydney_internal_refine_date     2018-10-04
_sydney_internal_refine_user     wlew0588
_sydney_internal_check_and_archive_date 2018-10-05
_sydney_internal_check_user      wlew0588
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30H34N10S2Ni H2Cl2 H2O'
_chemical_oxdiff_usercomment     ' '
_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_max   0.943
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N22(H22), C1(H1), C2(H2A), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10),
 C11(H11), C21(H21), C22(H22A), C23(H23), C24(H24), C28(H28), C29(H29),
 C30(H30), C31(H31)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C)
;
_olex2_date_sample_data_collection 2018-10-24
_olex2_date_sample_submission    2018-09-19
_olex2_exptl_crystal_mounting_method 'in paratone on a loop'
_olex2_submission_original_sample_id Ni(Dp4e4mT)2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.396
_oxdiff_exptl_absorpt_empirical_full_min 0.328
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2782(2) 0.50700(16) 0.24779(12) 0.0439(5) Uani 1 1 d . . . . .
S1 S 0.5375(3) 0.6150(2) 0.28546(17) 0.0450(7) Uani 1 1 d . . . . .
S21 S 0.3240(3) 0.4479(2) 0.09327(17) 0.0455(7) Uani 1 1 d . . . . .
N1 N 0.0391(9) 0.4612(7) 0.2123(5) 0.040(2) Uani 1 1 d . . . . .
N2 N 0.1120(10) 0.8018(7) 0.1737(6) 0.046(2) Uani 1 1 d . . . . .
H2 H 0.134212 0.807125 0.235272 0.056 Uiso 1 1 calc R . . . .
N3 N 0.2539(10) 0.6364(8) 0.2125(5) 0.046(2) Uani 1 1 d . . . . .
N4 N 0.3648(10) 0.7247(8) 0.2137(6) 0.050(2) Uani 1 1 d . . . . .
N5 N 0.6150(10) 0.8086(8) 0.2560(6) 0.048(2) Uani 1 1 d . . . . .
N21 N 0.2357(9) 0.5109(7) 0.3911(5) 0.042(2) Uani 1 1 d . . . . .
N22 N 0.2397(10) 0.1738(7) 0.3618(6) 0.045(2) Uani 1 1 d . . . . .
H22 H 0.168262 0.166796 0.315910 0.054 Uiso 1 1 calc R . . . .
N23 N 0.2906(9) 0.3711(7) 0.2765(6) 0.042(2) Uani 1 1 d . . . . .
N24 N 0.3160(9) 0.3024(8) 0.2117(5) 0.046(2) Uani 1 1 d . . . . .
N25 N 0.3449(10) 0.2638(8) 0.0564(6) 0.048(2) Uani 1 1 d . . . . .
C1 C -0.0627(13) 0.3758(9) 0.2221(6) 0.042(3) Uani 1 1 d . . . . .
H1 H -0.029029 0.325641 0.248586 0.051 Uiso 1 1 calc R . . . .
C2 C -0.2168(13) 0.3546(10) 0.1959(8) 0.053(3) Uani 1 1 d . . . . .
H2A H -0.288723 0.292236 0.205935 0.063 Uiso 1 1 calc R . . . .
C3 C -0.2633(12) 0.4263(10) 0.1547(7) 0.053(3) Uani 1 1 d . . . . .
H3 H -0.367932 0.413046 0.133012 0.063 Uiso 1 1 calc R . . . .
C4 C -0.1579(12) 0.5173(9) 0.1451(7) 0.044(3) Uani 1 1 d . . . . .
H4 H -0.189282 0.568217 0.118491 0.053 Uiso 1 1 calc R . . . .
C5 C -0.0064(12) 0.5338(9) 0.1745(6) 0.046(3) Uani 1 1 d . . . . .
C6 C 0.1185(11) 0.6302(9) 0.1721(7) 0.041(3) Uani 1 1 d . . . . .
C7 C 0.0914(11) 0.7141(9) 0.1241(8) 0.044(3) Uani 1 1 d . . . . .
C8 C 0.0504(12) 0.7036(9) 0.0269(7) 0.046(3) Uani 1 1 d . . . . .
H8 H 0.030167 0.640630 -0.009481 0.055 Uiso 1 1 calc R . . . .
C9 C 0.0397(11) 0.7856(10) -0.0151(7) 0.051(3) Uani 1 1 d . . . . .
H9 H 0.014429 0.780187 -0.081403 0.061 Uiso 1 1 calc R . . . .
C10 C 0.0662(13) 0.8775(10) 0.0399(9) 0.053(3) Uani 1 1 d . . . . .
H10 H 0.060424 0.935136 0.011584 0.064 Uiso 1 1 calc R . . . .
C11 C 0.1004(13) 0.8822(10) 0.1346(9) 0.055(3) Uani 1 1 d . . . . .
H11 H 0.116151 0.943342 0.173226 0.066 Uiso 1 1 calc R . . . .
C12 C 0.5025(11) 0.7205(9) 0.2508(6) 0.042(3) Uani 1 1 d . . . . .
C14 C 0.7685(12) 0.8180(9) 0.2959(8) 0.051(3) Uani 1 1 d . . . . .
H14A H 0.764668 0.808493 0.363439 0.076 Uiso 1 1 calc GR . . . .
H14B H 0.837971 0.884781 0.288125 0.076 Uiso 1 1 calc GR . . . .
H14C H 0.806355 0.767127 0.262868 0.076 Uiso 1 1 calc GR . . . .
C15 C 0.5936(13) 0.8991(9) 0.2219(8) 0.048(3) Uani 1 1 d . . . . .
H15A H 0.504473 0.879742 0.174461 0.057 Uiso 1 1 calc R . . . .
H15B H 0.685981 0.934560 0.190025 0.057 Uiso 1 1 calc R . . . .
C16 C 0.5672(16) 0.9684(11) 0.3001(9) 0.066(4) Uani 1 1 d . . . . .
H16A H 0.540265 1.023267 0.273229 0.099 Uiso 1 1 calc GR . . . .
H16B H 0.661160 0.995821 0.342159 0.099 Uiso 1 1 calc GR . . . .
H16C H 0.482878 0.931715 0.336269 0.099 Uiso 1 1 calc GR . . . .
C21 C 0.2005(10) 0.5827(9) 0.4428(7) 0.042(3) Uani 1 1 d . . . . .
H21 H 0.189508 0.638530 0.413361 0.050 Uiso 1 1 calc R . . . .
C22 C 0.1790(12) 0.5782(9) 0.5410(8) 0.049(3) Uani 1 1 d . . . . .
H22A H 0.155235 0.629951 0.578426 0.059 Uiso 1 1 calc R . . . .
C23 C 0.1943(12) 0.4960(10) 0.5786(7) 0.052(3) Uani 1 1 d . . . . .
H23 H 0.181739 0.490942 0.644325 0.063 Uiso 1 1 calc R . . . .
C24 C 0.2275(11) 0.4189(9) 0.5247(6) 0.045(3) Uani 1 1 d . . . . .
H24 H 0.236496 0.361671 0.552491 0.054 Uiso 1 1 calc R . . . .
C25 C 0.2471(11) 0.4283(9) 0.4289(8) 0.046(3) Uani 1 1 d . . . . .
C26 C 0.2832(11) 0.3536(9) 0.3649(7) 0.040(3) Uani 1 1 d . . . . .
C27 C 0.3180(11) 0.2679(9) 0.3992(7) 0.044(3) Uani 1 1 d . . . . .
C28 C 0.4338(12) 0.2758(10) 0.4693(7) 0.047(3) Uani 1 1 d . . . . .
H28 H 0.492278 0.340308 0.498033 0.057 Uiso 1 1 calc R . . . .
C29 C 0.4655(13) 0.1935(10) 0.4981(7) 0.055(3) Uani 1 1 d . . . . .
H29 H 0.546314 0.201099 0.545147 0.066 Uiso 1 1 calc R . . . .
C30 C 0.3796(15) 0.0994(11) 0.4583(7) 0.060(4) Uani 1 1 d . . . . .
H30 H 0.400431 0.041694 0.477949 0.072 Uiso 1 1 calc R . . . .
C31 C 0.2627(13) 0.0897(10) 0.3894(7) 0.051(3) Uani 1 1 d . . . . .
H31 H 0.200200 0.025500 0.362288 0.061 Uiso 1 1 calc R . . . .
C32 C 0.3279(11) 0.3327(8) 0.1230(6) 0.038(2) Uani 1 1 d . . . . .
C34 C 0.3790(14) 0.2864(11) -0.0385(7) 0.062(4) Uani 1 1 d . . . . .
H34A H 0.449526 0.250993 -0.062038 0.092 Uiso 1 1 calc GR . . . .
H34B H 0.427287 0.358683 -0.038840 0.092 Uiso 1 1 calc GR . . . .
H34C H 0.283520 0.264937 -0.079567 0.092 Uiso 1 1 calc GR . . . .
C35 C 0.3132(13) 0.1578(10) 0.0701(7) 0.053(3) Uani 1 1 d . . . . .
H35A H 0.265761 0.117045 0.010058 0.064 Uiso 1 1 calc R . . . .
H35B H 0.237343 0.140603 0.118711 0.064 Uiso 1 1 calc R . . . .
C36 C 0.4553(15) 0.1293(11) 0.1008(11) 0.075(4) Uani 1 1 d . . . . .
H36A H 0.535617 0.152432 0.056869 0.112 Uiso 1 1 calc GR . . . .
H36B H 0.427870 0.056391 0.100255 0.112 Uiso 1 1 calc GR . . . .
H36C H 0.493581 0.160831 0.164998 0.112 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.1604(4) 0.8320(3) 0.38687(19) 0.0595(8) Uani 1 1 d . . . . .
Cl2 Cl -0.0310(3) 0.0843(2) 0.21613(18) 0.0543(8) Uani 1 1 d . . . . .
O1 O -0.0797(16) 0.2201(8) 0.3987(7) 0.090(3) Uani 1 1 d . . . . .
H1A H -0.098829 0.174422 0.352666 0.134 Uiso 1 1 d G . . . .
H1B H -0.104094 0.188722 0.447176 0.134 Uiso 1 1 d G . . . .
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'
Cl Cl 0.3639 0.7018 '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'
Ni Ni -3.0029 0.5091 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0060
0 -1 0 0.0100
1 -2 5 0.0024
5 -3 -3 0.0478
-5 3 3 0.0288
-1 2 -5 0.0295
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S21 Ni1 S1 95.20(11) . . ?
N1 Ni1 S1 160.0(3) . . ?
N1 Ni1 S21 91.0(2) . . ?
N3 Ni1 S1 80.4(3) . . ?
N3 Ni1 S21 96.2(2) . . ?
N3 Ni1 N1 80.1(4) . . ?
N3 Ni1 N21 102.6(3) . . ?
N3 Ni1 N23 176.0(4) . . ?
N21 Ni1 S1 90.7(2) . . ?
N21 Ni1 S21 161.0(3) . . ?
N21 Ni1 N1 89.5(3) . . ?
N23 Ni1 S1 103.1(2) . . ?
N23 Ni1 S21 81.6(3) . . ?
N23 Ni1 N1 96.5(4) . . ?
N23 Ni1 N21 79.5(4) . . ?
C12 S1 Ni1 95.1(4) . . ?
C32 S21 Ni1 95.4(3) . . ?
C1 N1 Ni1 128.6(7) . . ?
C1 N1 C5 119.4(9) . . ?
C5 N1 Ni1 112.0(7) . . ?
C7 N2 H2 118.5 . . ?
C7 N2 C11 122.9(10) . . ?
C11 N2 H2 118.5 . . ?
N4 N3 Ni1 127.2(7) . . ?
C6 N3 Ni1 115.5(9) . . ?
C6 N3 N4 116.6(10) . . ?
N3 N4 C12 111.7(10) . . ?
C12 N5 C14 120.4(10) . . ?
C12 N5 C15 123.5(9) . . ?
C14 N5 C15 116.1(10) . . ?
C21 N21 Ni1 126.8(7) . . ?
C21 N21 C25 121.4(9) . . ?
C25 N21 Ni1 111.8(7) . . ?
C27 N22 H22 117.5 . . ?
C31 N22 H22 117.5 . . ?
C31 N22 C27 125.0(10) . . ?
N24 N23 Ni1 124.6(7) . . ?
C26 N23 Ni1 115.9(8) . . ?
C26 N23 N24 119.4(9) . . ?
N23 N24 C32 112.9(9) . . ?
C32 N25 C34 122.1(10) . . ?
C32 N25 C35 123.6(9) . . ?
C34 N25 C35 113.9(10) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(11) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 C1 117.9(12) . . ?
C3 C2 H2A 121.1 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.7(10) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(10) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 120.7(11) . . ?
N1 C5 C6 114.6(9) . . ?
C4 C5 C6 124.7(10) . . ?
N3 C6 C5 116.6(10) . . ?
N3 C6 C7 122.1(10) . . ?
C5 C6 C7 121.3(9) . . ?
N2 C7 C6 119.4(9) . . ?
N2 C7 C8 119.1(11) . . ?
C8 C7 C6 121.4(11) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 118.9(11) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 119.9(10) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 120.8 . . ?
C11 C10 C9 118.5(12) . . ?
C11 C10 H10 120.8 . . ?
N2 C11 C10 120.6(12) . . ?
N2 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
N4 C12 S1 125.4(9) . . ?
N5 C12 S1 121.3(7) . . ?
N5 C12 N4 113.2(10) . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 H15A 109.1 . . ?
N5 C15 H15B 109.1 . . ?
N5 C15 C16 112.4(10) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N21 C21 H21 119.2 . . ?
N21 C21 C22 121.5(10) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22A 121.7 . . ?
C23 C22 C21 116.5(11) . . ?
C23 C22 H22A 121.7 . . ?
C22 C23 H23 118.7 . . ?
C22 C23 C24 122.6(9) . . ?
C24 C23 H23 118.7 . . ?
C23 C24 H24 121.1 . . ?
C25 C24 C23 117.8(11) . . ?
C25 C24 H24 121.1 . . ?
N21 C25 C24 120.1(11) . . ?
N21 C25 C26 116.5(9) . . ?
C24 C25 C26 123.4(11) . . ?
N23 C26 C25 115.9(10) . . ?
N23 C26 C27 122.2(10) . . ?
C27 C26 C25 121.7(9) . . ?
N22 C27 C26 120.7(9) . . ?
N22 C27 C28 115.6(11) . . ?
C28 C27 C26 123.7(11) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 C27 122.0(12) . . ?
C29 C28 H28 119.0 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.6(11) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 120.3 . . ?
C29 C30 C31 119.4(12) . . ?
C31 C30 H30 120.3 . . ?
N22 C31 C30 118.4(12) . . ?
N22 C31 H31 120.8 . . ?
C30 C31 H31 120.8 . . ?
N24 C32 S21 125.4(8) . . ?
N25 C32 S21 120.5(8) . . ?
N25 C32 N24 114.1(10) . . ?
N25 C34 H34A 109.5 . . ?
N25 C34 H34B 109.5 . . ?
N25 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N25 C35 H35A 108.7 . . ?
N25 C35 H35B 108.7 . . ?
N25 C35 C36 114.2(10) . . ?
H35A C35 H35B 107.6 . . ?
C36 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H1A O1 H1B 104.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.406(3) . ?
Ni1 S21 2.378(3) . ?
Ni1 N1 2.108(8) . ?
Ni1 N3 2.003(10) . ?
Ni1 N21 2.085(7) . ?
Ni1 N23 2.026(9) . ?
S1 C12 1.719(12) . ?
S21 C32 1.720(12) . ?
N1 C1 1.300(13) . ?
N1 C5 1.356(13) . ?
N2 H2 0.8800 . ?
N2 C7 1.327(14) . ?
N2 C11 1.333(14) . ?
N3 N4 1.343(13) . ?
N3 C6 1.317(12) . ?
N4 C12 1.364(13) . ?
N5 C12 1.345(14) . ?
N5 C14 1.455(13) . ?
N5 C15 1.465(14) . ?
N21 C21 1.326(14) . ?
N21 C25 1.352(14) . ?
N22 H22 0.8800 . ?
N22 C27 1.352(14) . ?
N22 C31 1.351(14) . ?
N23 N24 1.356(13) . ?
N23 C26 1.300(13) . ?
N24 C32 1.361(13) . ?
N25 C32 1.346(14) . ?
N25 C34 1.435(13) . ?
N25 C35 1.464(15) . ?
C1 H1 0.9500 . ?
C1 C2 1.377(15) . ?
C2 H2A 0.9500 . ?
C2 C3 1.372(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(14) . ?
C5 C6 1.491(16) . ?
C6 C7 1.490(15) . ?
C7 C8 1.398(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.404(17) . ?
C10 H10 0.9500 . ?
C10 C11 1.358(17) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.492(16) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.420(15) . ?
C22 H22A 0.9500 . ?
C22 C23 1.356(15) . ?
C23 H23 0.9500 . ?
C23 C24 1.393(16) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(14) . ?
C25 C26 1.455(15) . ?
C26 C27 1.453(15) . ?
C27 C28 1.395(14) . ?
C28 H28 0.9500 . ?
C28 C29 1.368(16) . ?
C29 H29 0.9500 . ?
C29 C30 1.377(17) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(16) . ?
C31 H31 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.529(16) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 Cl1 0.88 2.14 3.013(9) 170.7 . yes
N22 H22 Cl2 0.88 2.21 3.038(9) 155.9 . yes
O1 H1A Cl2 0.85 2.43 3.217(11) 153.8 . yes
O1 H1B Cl1 0.85 2.45 3.252(10) 156.7 2_566 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C12 N4 -1.3(8) . . . . ?
Ni1 S1 C12 N5 -179.4(7) . . . . ?
Ni1 S21 C32 N24 -3.4(9) . . . . ?
Ni1 S21 C32 N25 177.1(8) . . . . ?
Ni1 N1 C1 C2 -179.9(8) . . . . ?
Ni1 N1 C5 C4 178.7(7) . . . . ?
Ni1 N1 C5 C6 -3.6(10) . . . . ?
Ni1 N3 N4 C12 -5.4(11) . . . . ?
Ni1 N3 C6 C5 11.3(11) . . . . ?
Ni1 N3 C6 C7 -167.3(7) . . . . ?
Ni1 N21 C21 C22 -177.9(7) . . . . ?
Ni1 N21 C25 C24 177.9(8) . . . . ?
Ni1 N21 C25 C26 -0.9(11) . . . . ?
Ni1 N23 N24 C32 -1.9(11) . . . . ?
Ni1 N23 C26 C25 7.7(12) . . . . ?
Ni1 N23 C26 C27 -168.7(8) . . . . ?
N1 C1 C2 C3 2.1(16) . . . . ?
N1 C5 C6 N3 -4.8(12) . . . . ?
N1 C5 C6 C7 173.7(8) . . . . ?
N2 C7 C8 C9 3.1(16) . . . . ?
N3 N4 C12 S1 3.9(12) . . . . ?
N3 N4 C12 N5 -177.9(8) . . . . ?
N3 C6 C7 N2 -60.9(13) . . . . ?
N3 C6 C7 C8 116.6(12) . . . . ?
N4 N3 C6 C5 -177.4(8) . . . . ?
N4 N3 C6 C7 4.0(13) . . . . ?
N21 C21 C22 C23 -0.9(15) . . . . ?
N21 C25 C26 N23 -4.4(14) . . . . ?
N21 C25 C26 C27 172.0(9) . . . . ?
N22 C27 C28 C29 0.1(14) . . . . ?
N23 N24 C32 S21 3.8(12) . . . . ?
N23 N24 C32 N25 -176.6(8) . . . . ?
N23 C26 C27 N22 -57.6(14) . . . . ?
N23 C26 C27 C28 120.8(12) . . . . ?
N24 N23 C26 C25 -176.7(9) . . . . ?
N24 N23 C26 C27 6.9(15) . . . . ?
C1 N1 C5 C4 -1.2(14) . . . . ?
C1 N1 C5 C6 176.6(8) . . . . ?
C1 C2 C3 C4 -3.0(16) . . . . ?
C2 C3 C4 C5 1.9(15) . . . . ?
C3 C4 C5 N1 0.3(15) . . . . ?
C3 C4 C5 C6 -177.3(9) . . . . ?
C4 C5 C6 N3 172.8(9) . . . . ?
C4 C5 C6 C7 -8.6(15) . . . . ?
C5 N1 C1 C2 0.0(14) . . . . ?
C5 C6 C7 N2 120.6(10) . . . . ?
C5 C6 C7 C8 -61.8(14) . . . . ?
C6 N3 N4 C12 -175.5(8) . . . . ?
C6 C7 C8 C9 -174.5(9) . . . . ?
C7 N2 C11 C10 0.0(17) . . . . ?
C7 C8 C9 C10 -1.6(16) . . . . ?
C8 C9 C10 C11 -0.7(16) . . . . ?
C9 C10 C11 N2 1.6(17) . . . . ?
C11 N2 C7 C6 175.2(9) . . . . ?
C11 N2 C7 C8 -2.4(15) . . . . ?
C12 N5 C15 C16 99.0(12) . . . . ?
C14 N5 C12 S1 -3.1(12) . . . . ?
C14 N5 C12 N4 178.6(9) . . . . ?
C14 N5 C15 C16 -81.7(12) . . . . ?
C15 N5 C12 S1 176.1(8) . . . . ?
C15 N5 C12 N4 -2.2(13) . . . . ?
C21 N21 C25 C24 -2.4(15) . . . . ?
C21 N21 C25 C26 178.8(9) . . . . ?
C21 C22 C23 C24 -0.7(17) . . . . ?
C22 C23 C24 C25 0.7(17) . . . . ?
C23 C24 C25 N21 0.8(15) . . . . ?
C23 C24 C25 C26 179.6(10) . . . . ?
C24 C25 C26 N23 176.8(10) . . . . ?
C24 C25 C26 C27 -6.8(16) . . . . ?
C25 N21 C21 C22 2.4(15) . . . . ?
C25 C26 C27 N22 126.2(11) . . . . ?
C25 C26 C27 C28 -55.4(15) . . . . ?
C26 N23 N24 C32 -177.2(9) . . . . ?
C26 C27 C28 C29 -178.4(9) . . . . ?
C27 N22 C31 C30 -3.1(15) . . . . ?
C27 C28 C29 C30 -1.2(16) . . . . ?
C28 C29 C30 C31 0.3(16) . . . . ?
C29 C30 C31 N22 1.7(16) . . . . ?
C31 N22 C27 C26 -179.4(9) . . . . ?
C31 N22 C27 C28 2.2(14) . . . . ?
C32 N25 C35 C36 -96.1(12) . . . . ?
C34 N25 C32 S21 7.8(14) . . . . ?
C34 N25 C32 N24 -171.8(10) . . . . ?
C34 N25 C35 C36 90.7(12) . . . . ?
C35 N25 C32 S21 -164.9(8) . . . . ?
C35 N25 C32 N24 15.5(14) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0028 1.0027 -0.0030 0.0181 -0.0277 0.1106
0.0028 -1.0027 0.0030 -0.0181 0.0277 -0.1106
1.0366 -2.0054 4.9845 -0.5852 -0.0423 -0.0421
4.9895 -2.9761 -3.0832 0.0934 -0.8292 -0.3346
-4.9895 2.9761 3.0832 -0.0934 0.8292 0.3346
-1.0366 2.0054 -4.9845 0.5852 0.0423 0.0421
