#------------------------------------------------------------------------------
#$Date: 2024-08-05 22:05:10 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293858 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/65/7716562.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_7716562
loop_
_publ_author_name
'Bag, Jayanta'
'Das, Surajit'
'Pal, Kuntal'
_publ_section_title
;
 Terminal {Ni(II)-SH} complex promoted anaerobic catalytic sulfur atom
 transfer reaction: implication to the sulfide oxidase function of
 Cu/Zn-superoxide dismutase.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12773
_journal_page_last               12782
_journal_paper_doi               10.1039/d4dt01364f
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H40 N Ni O P S'
_chemical_formula_sum            'C39 H40 N Ni O P S'
_chemical_formula_weight         660.46
_chemical_name_systematic        'ND-249_auto__ final clear data'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2j6h6g
_audit_creation_date             2024-01-31
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.25730(10)
_cell_length_b                   13.21440(10)
_cell_length_c                   13.09390(10)
_cell_measurement_reflns_used    39802
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      68.0200
_cell_measurement_theta_min      3.3160
_cell_volume                     3332.05(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00  26.00   0.50    0.25    --  -40.58  38.00-150.00  138
  2  ω    -57.00  26.00   0.50    0.25    --  -40.58  50.00  60.00  166
  3  ω    -31.00  30.00   0.50    0.25    --  -40.58  25.00-150.00  122
  4  ω    -24.00  35.00   0.50    0.25    --  -40.58  12.00 150.00  118
  5  ω    -31.00  30.00   0.50    0.25    --  -40.58  25.00  90.00  122
  6  ω   -113.00 -17.00   0.50    0.25    --  -40.58 -18.00-160.34  192
  7  ω    -24.00  35.00   0.50    0.25    --  -40.58  12.00   0.00  118
  8  ω    -78.00   4.00   0.50    0.25    --  -40.58 104.00-120.00  164
  9  ω   -107.00 -25.00   0.50    0.25    --  -40.58 -38.00  60.00  164
 10  ω     41.00 100.00   0.50    0.25    --   40.58-138.00-180.00  118
 11  ω      4.00 116.00   0.50    0.25    --   40.58  12.00-150.00  224
 12  ω      8.00  42.00   0.50    0.25    --   40.58  92.00 109.42   68
 13  ω     18.00  78.00   0.50    0.25    --   40.58-104.00   0.00  120
 14  ω     41.00 100.00   0.50    0.25    --   40.58-138.00  30.00  118
 15  ω    -29.00  31.00   0.50    0.25    --   40.58 -25.00-120.00  120
 16  ω     12.00  43.00   0.50    0.25    --   40.58  83.00 -20.37   62
 17  ω     13.00  43.00   0.50    0.25    --   40.58  81.00-170.89   60
 18  ω      8.00  42.00   0.50    0.25    --   40.58  92.00  -2.84   68
 19  ω    -47.00 -15.00   0.50    1.45    --  -82.50  42.00  90.00   64
 20  ω    -47.00 -15.00   0.50    1.45    --  -82.50  42.00 -60.00   64
 21  ω    -47.00 -15.00   0.50    1.45    --  -82.50  42.00   0.00   64
 22  ω    -47.00 -15.00   0.50    1.45    --  -82.50  42.00  60.00   64
 23  ω    -47.00 -15.00   0.50    1.45    --  -82.50  42.00 -90.00   64
 24  ω   -101.00 -23.00   0.50    1.45    --  -82.50 145.00  30.00  156
 25  ω    -47.00 -15.00   0.50    1.45    --  -82.50  42.00  30.00   64
 26  ω    -57.00 -16.00   0.50    1.45    --  -82.50  50.00 -30.00   82
 27  ω   -146.00 -78.00   0.50    1.45    --  -82.50-117.00 -60.00  136
 28  ω     44.00 127.00   0.50    1.45    --   96.35-145.00  60.00  166
 29  ω     33.00 110.00   0.50    1.45    --   96.35-117.00 -60.00  154
 30  ω     99.00 160.00   0.50    1.45    --   96.35 117.00 -90.00  122
 31  ω    105.00 170.00   0.50    1.45    --   96.35  96.00 -60.00  130
 32  ω     29.00  83.00   0.50    1.45    --   96.35 -68.00 -90.00  108
 33  ω     44.00 127.00   0.50    1.45    --   96.35-145.00 -90.00  166
 34  ω     30.00  57.00   0.50    1.45    --   96.35 -50.00 150.00   54
 35  ω     71.00 170.00   0.50    1.45    --   96.35  17.00 120.00  198
 36  ω     80.00 164.00   0.50    1.45    --   96.35  42.00  60.00  168
 37  ω     70.00 165.00   0.50    1.45    --   96.35  77.00-150.00  190
 38  ω     28.00  68.00   0.50    1.45    --   96.35 -59.00   0.00   80
 39  ω     26.00 127.00   0.50    1.45    --   96.35 -87.00-120.00  202
 40  ω     28.00  68.00   0.50    1.45    --   96.35 -59.00 -60.00   80
 41  ω     44.00 127.00   0.50    1.45    --   96.35-145.00-120.00  166
 42  ω     80.00 164.00   0.50    1.45    --   96.35  42.00 -30.00  168
 43  ω     29.00  83.00   0.50    1.45    --   96.35 -68.00-120.00  108
 44  ω     26.00 127.00   0.50    1.45    --   96.35 -87.00  60.00  202
 45  ω     33.00 110.00   0.50    1.45    --   96.35-117.00  60.00  154
 46  ω     29.00  83.00   0.50    1.45    --   96.35 -68.00  90.00  108
 47  ω     33.00 110.00   0.50    1.45    --   96.35-117.00 -90.00  154
 48  ω     70.00 165.00   0.50    1.45    --   96.35  77.00 -30.00  190
 49  ω     29.00  83.00   0.50    1.45    --   96.35 -68.00  60.00  108
 50  ω     30.00  57.00   0.50    1.45    --   96.35 -50.00  90.00   54
 51  ω     28.00 105.00   0.50    1.45    --   96.35 -77.00 150.00  154
 52  ω     33.00 110.00   0.50    1.45    --   96.35-117.00  90.00  154
 53  ω     72.00 164.00   0.50    1.45    --   96.35  68.00 -90.00  184
 54  ω     72.00 164.00   0.50    1.45    --   96.35  68.00-120.00  184
 55  ω     99.00 160.00   0.50    1.45    --   96.35 117.00 -30.00  122
 56  ω     83.00 164.00   0.50    1.45    --   96.35  33.00  30.00  162
 57  ω   -108.00 -17.00   0.50    0.25    --  -40.58 -64.00 -60.00  182
 58  ω   -107.00 -21.00   0.50    0.25    --  -40.58 -50.00  30.00  172
 59  ω   -108.00 -17.00   0.50    0.25    --  -40.58 -64.00  90.00  182
 60  ω   -109.00 -14.00   0.50    0.25    --  -40.58 -77.00-150.00  190
 61  ω   -107.00 -21.00   0.50    0.25    --  -40.58 -50.00 150.00  172
 62  ω   -108.00 -17.00   0.50    0.25    --  -40.58 -64.00   0.00  182
 63  ω     18.00 108.00   0.50    0.25    --   40.58  64.00 -60.00  180
 64  ω      8.00  42.00   0.50    0.25    --   40.58  92.00  94.05   68
 65  ω     12.00  43.00   0.50    0.25    --   40.58  83.00 -44.34   62
 66  ω     18.00 108.00   0.50    0.25    --   40.58  64.00  30.00  180
 67  ω     13.00  43.00   0.50    0.25    --   40.58  81.00 176.93   60
 68  ω      8.00  42.00   0.50    0.25    --   40.58  92.00-103.87   68
 69  ω     13.00  43.00   0.50    0.25    --   40.58  81.00 142.71   60
 70  ω      8.00  35.00   0.50    0.25    --   40.58  93.00 -61.98   54
 71  ω     10.00  43.00   0.50    0.25    --   40.58  87.00-151.16   66
 72  ω     13.00  43.00   0.50    0.25    --   40.58  80.00 -96.61   60
 73  ω     72.00 148.00   0.50    1.45    --   96.35  68.00 120.00  152
 74  ω     83.00 164.00   0.50    1.45    --   96.35  33.00-180.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0725593000
_diffrn_orient_matrix_UB_12      0.0479118000
_diffrn_orient_matrix_UB_13      -0.0109731000
_diffrn_orient_matrix_UB_21      -0.0247726000
_diffrn_orient_matrix_UB_22      -0.0932500000
_diffrn_orient_matrix_UB_23      -0.0605269000
_diffrn_orient_matrix_UB_31      -0.0228368000
_diffrn_orient_matrix_UB_32      -0.0510074000
_diffrn_orient_matrix_UB_33      0.1002830000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            54454
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.136
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_preparation       'slow diffusion CH2Cl2 with Et2O'
_exptl_crystal_recrystallization_method '100 k'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 2595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0338
_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)+(0.0646P)²+0.6936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                5803
_reflns_number_total             5907
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01364f2.cif
_cod_data_source_block           2tBu
_cod_depositor_comments
'Adding full bibliography for 7716561--7716564.cif.'
_cod_database_code               7716562
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O Ni P S'
_chemical_oxdiff_usercomment     100K
_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   0.785
_shelx_estimated_absorpt_t_min   0.665
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32),
  C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
1.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id 'ND-249_auto__ final clear data'
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.685
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
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 0.40369(2) 0.66725(4) 0.45464(4) 0.01953(15) Uani 1 1 d . . . . .
S1 S 0.39191(4) 0.81210(6) 0.38374(7) 0.02670(19) Uani 1 1 d . . . . .
P1 P 0.47672(4) 0.73633(6) 0.56574(7) 0.02062(18) Uani 1 1 d . . . . .
O1 O 0.40760(11) 0.54771(16) 0.53269(18) 0.0206(5) Uani 1 1 d . . . . .
N1 N 0.35269(13) 0.60842(19) 0.3446(2) 0.0192(5) Uani 1 1 d . . . . .
C1 C 0.34405(16) 0.5109(2) 0.3364(3) 0.0210(6) Uani 1 1 d . . . . .
H1 H 0.325960 0.487825 0.273053 0.025 Uiso 1 1 calc R U . . .
C2 C 0.35821(15) 0.4349(2) 0.4101(2) 0.0197(6) Uani 1 1 d . . . . .
C3 C 0.38632(15) 0.4569(2) 0.5080(3) 0.0196(6) Uani 1 1 d . . . . .
C4 C 0.39039(15) 0.3751(2) 0.5805(3) 0.0207(6) Uani 1 1 d . . . . .
C5 C 0.37098(15) 0.2790(2) 0.5481(3) 0.0210(6) Uani 1 1 d . . . . .
H5 H 0.375269 0.225137 0.595682 0.025 Uiso 1 1 calc R U . . .
C6 C 0.34533(15) 0.2551(2) 0.4498(3) 0.0220(6) Uani 1 1 d . . . . .
C7 C 0.33869(16) 0.3345(2) 0.3834(3) 0.0220(6) Uani 1 1 d . . . . .
H7 H 0.320406 0.322175 0.317140 0.026 Uiso 1 1 calc R U . . .
C8 C 0.32914(16) 0.6727(2) 0.2638(3) 0.0205(6) Uani 1 1 d . . . . .
C9 C 0.29133(16) 0.6412(3) 0.1784(2) 0.0231(7) Uani 1 1 d . . . . .
H9 H 0.278887 0.571992 0.171255 0.028 Uiso 1 1 calc R U . . .
C10 C 0.27201(17) 0.7099(3) 0.1046(3) 0.0255(7) Uani 1 1 d . . . . .
H10 H 0.247229 0.687458 0.046085 0.031 Uiso 1 1 calc R U . . .
C11 C 0.28850(17) 0.8119(3) 0.1150(3) 0.0255(7) Uani 1 1 d . . . . .
H11 H 0.275041 0.858927 0.063872 0.031 Uiso 1 1 calc R U . . .
C12 C 0.32453(18) 0.8445(2) 0.2001(3) 0.0276(7) Uani 1 1 d . . . . .
H12 H 0.335130 0.914246 0.207887 0.033 Uiso 1 1 calc R U . . .
C13 C 0.34561(16) 0.7751(2) 0.2753(3) 0.0233(7) Uani 1 1 d . . . . .
C14 C 0.32799(18) 0.1458(2) 0.4186(3) 0.0260(7) Uani 1 1 d . . . . .
C15 C 0.3186(2) 0.0757(3) 0.5108(3) 0.0334(8) Uani 1 1 d . . . . .
H15A H 0.361731 0.073744 0.550496 0.050 Uiso 1 1 calc R U . . .
H15B H 0.307281 0.007301 0.487025 0.050 Uiso 1 1 calc R U . . .
H15C H 0.280804 0.101068 0.553857 0.050 Uiso 1 1 calc R U . . .
C16 C 0.3883(2) 0.1060(3) 0.3540(3) 0.0343(8) Uani 1 1 d . . . . .
H16A H 0.391882 0.145810 0.291063 0.052 Uiso 1 1 calc R U . . .
H16B H 0.380051 0.034836 0.336801 0.052 Uiso 1 1 calc R U . . .
H16C H 0.431676 0.111866 0.392744 0.052 Uiso 1 1 calc R U . . .
C17 C 0.2607(2) 0.1425(3) 0.3555(3) 0.0376(9) Uani 1 1 d . . . . .
H17A H 0.222359 0.170100 0.396057 0.056 Uiso 1 1 calc R U . . .
H17B H 0.250287 0.072238 0.336926 0.056 Uiso 1 1 calc R U . . .
H17C H 0.266567 0.182877 0.293372 0.056 Uiso 1 1 calc R U . . .
C18 C 0.41262(17) 0.3930(2) 0.6909(3) 0.0221(6) Uani 1 1 d . . . . .
C19 C 0.40877(19) 0.2964(3) 0.7560(3) 0.0302(8) Uani 1 1 d . . . . .
H19A H 0.361046 0.270667 0.755895 0.045 Uiso 1 1 calc R U . . .
H19B H 0.422897 0.311845 0.826151 0.045 Uiso 1 1 calc R U . . .
H19C H 0.439912 0.245097 0.727289 0.045 Uiso 1 1 calc R U . . .
C20 C 0.48848(17) 0.4298(3) 0.6957(3) 0.0279(7) Uani 1 1 d . . . . .
H20A H 0.518742 0.379614 0.663157 0.042 Uiso 1 1 calc R U . . .
H20B H 0.502304 0.438582 0.767137 0.042 Uiso 1 1 calc R U . . .
H20C H 0.492633 0.494536 0.659681 0.042 Uiso 1 1 calc R U . . .
C21 C 0.36347(18) 0.4710(3) 0.7399(3) 0.0269(7) Uani 1 1 d . . . . .
H21A H 0.362518 0.532464 0.697975 0.040 Uiso 1 1 calc R U . . .
H21B H 0.380009 0.487732 0.808600 0.040 Uiso 1 1 calc R U . . .
H21C H 0.316579 0.442515 0.744156 0.040 Uiso 1 1 calc R U . . .
C22 C 0.56352(17) 0.6810(2) 0.5586(3) 0.0221(6) Uani 1 1 d . . . . .
C23 C 0.57341(17) 0.5845(2) 0.5185(3) 0.0239(7) Uani 1 1 d . . . . .
H23 H 0.534725 0.547043 0.494020 0.029 Uiso 1 1 calc R U . . .
C24 C 0.63983(18) 0.5423(3) 0.5142(3) 0.0272(7) Uani 1 1 d . . . . .
H24 H 0.646107 0.476129 0.487421 0.033 Uiso 1 1 calc R U . . .
C25 C 0.69660(17) 0.5969(3) 0.5487(3) 0.0280(7) Uani 1 1 d . . . . .
H25 H 0.741809 0.568304 0.545319 0.034 Uiso 1 1 calc R U . . .
C26 C 0.68735(17) 0.6931(3) 0.5883(3) 0.0292(8) Uani 1 1 d . . . . .
H26 H 0.726286 0.730294 0.612301 0.035 Uiso 1 1 calc R U . . .
C27 C 0.62146(18) 0.7356(3) 0.5931(3) 0.0264(7) Uani 1 1 d . . . . .
H27 H 0.615590 0.801828 0.619809 0.032 Uiso 1 1 calc R U . . .
C28 C 0.49734(16) 0.8718(2) 0.5601(3) 0.0262(7) Uani 1 1 d . . . . .
C29 C 0.53144(19) 0.9089(3) 0.4739(3) 0.0345(8) Uani 1 1 d . . . . .
H29 H 0.540357 0.865489 0.417539 0.041 Uiso 1 1 calc R U . . .
C30 C 0.5524(2) 1.0100(3) 0.4705(4) 0.0445(11) Uani 1 1 d . . . . .
H30 H 0.575276 1.035567 0.411649 0.053 Uiso 1 1 calc R U . . .
C31 C 0.5400(2) 1.0730(3) 0.5530(4) 0.0467(11) Uani 1 1 d . . . . .
H31 H 0.554101 1.141870 0.550327 0.056 Uiso 1 1 calc R U . . .
C32 C 0.5072(2) 1.0366(3) 0.6387(4) 0.0403(10) Uani 1 1 d . . . . .
H32 H 0.499444 1.079990 0.695446 0.048 Uiso 1 1 calc R U . . .
C33 C 0.48542(19) 0.9358(3) 0.6426(3) 0.0316(8) Uani 1 1 d . . . . .
H33 H 0.462400 0.910989 0.701674 0.038 Uiso 1 1 calc R U . . .
C34 C 0.44906(16) 0.7198(2) 0.6977(3) 0.0224(6) Uani 1 1 d . . . . .
C35 C 0.49242(17) 0.6848(2) 0.7740(3) 0.0241(7) Uani 1 1 d . . . . .
H35 H 0.538239 0.663508 0.757799 0.029 Uiso 1 1 calc R U . . .
C36 C 0.46907(18) 0.6805(3) 0.8749(3) 0.0269(7) Uani 1 1 d . . . . .
H36 H 0.498925 0.656433 0.927300 0.032 Uiso 1 1 calc R U . . .
C37 C 0.40204(17) 0.7117(3) 0.8985(3) 0.0286(7) Uani 1 1 d . . . . .
H37 H 0.386194 0.708963 0.967109 0.034 Uiso 1 1 calc R U . . .
C38 C 0.35825(18) 0.7467(3) 0.8226(3) 0.0307(8) Uani 1 1 d . . . . .
H38 H 0.312475 0.767885 0.839080 0.037 Uiso 1 1 calc R U . . .
C39 C 0.38128(18) 0.7508(3) 0.7222(3) 0.0282(7) Uani 1 1 d . . . . .
H39 H 0.351150 0.774513 0.669999 0.034 Uiso 1 1 calc R U . . .
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'
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'
P P 0.2955 0.4335 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 P1 89.06(4) . . ?
O1 Ni1 S1 172.03(8) . . ?
O1 Ni1 P1 87.93(7) . . ?
O1 Ni1 N1 95.08(10) . . ?
N1 Ni1 S1 88.98(8) . . ?
N1 Ni1 P1 171.09(8) . . ?
C13 S1 Ni1 99.01(12) . . ?
C22 P1 Ni1 112.43(11) . . ?
C22 P1 C28 100.96(14) . . ?
C28 P1 Ni1 120.79(11) . . ?
C34 P1 Ni1 112.77(10) . . ?
C34 P1 C22 105.58(15) . . ?
C34 P1 C28 102.61(16) . . ?
C3 O1 Ni1 128.5(2) . . ?
C1 N1 Ni1 122.0(2) . . ?
C1 N1 C8 119.1(3) . . ?
C8 N1 Ni1 118.6(2) . . ?
N1 C1 H1 115.9 . . ?
N1 C1 C2 128.3(3) . . ?
C2 C1 H1 115.9 . . ?
C1 C2 C3 122.8(3) . . ?
C1 C2 C7 116.2(3) . . ?
C3 C2 C7 120.8(3) . . ?
O1 C3 C2 121.9(3) . . ?
O1 C3 C4 120.6(3) . . ?
C2 C3 C4 117.5(3) . . ?
C3 C4 C18 121.5(3) . . ?
C5 C4 C3 118.0(3) . . ?
C5 C4 C18 120.5(3) . . ?
C4 C5 H5 117.4 . . ?
C4 C5 C6 125.2(3) . . ?
C6 C5 H5 117.4 . . ?
C5 C6 C14 121.8(3) . . ?
C7 C6 C5 116.1(3) . . ?
C7 C6 C14 122.1(3) . . ?
C2 C7 H7 118.9 . . ?
C6 C7 C2 122.3(3) . . ?
C6 C7 H7 118.9 . . ?
C9 C8 N1 125.4(3) . . ?
C13 C8 N1 115.1(3) . . ?
C13 C8 C9 119.5(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.5(3) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.7(3) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(3) . . ?
C13 C12 H12 119.8 . . ?
C8 C13 S1 118.3(3) . . ?
C8 C13 C12 119.4(3) . . ?
C12 C13 S1 122.3(3) . . ?
C15 C14 C6 112.6(3) . . ?
C15 C14 C17 107.8(3) . . ?
C16 C14 C6 107.7(3) . . ?
C16 C14 C15 108.5(3) . . ?
C16 C14 C17 109.4(3) . . ?
C17 C14 C6 110.7(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 C18 C19 112.4(3) . . ?
C4 C18 C20 110.7(3) . . ?
C4 C18 C21 109.0(3) . . ?
C19 C18 C20 106.6(3) . . ?
C19 C18 C21 107.2(3) . . ?
C21 C18 C20 110.8(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 P1 120.7(2) . . ?
C23 C22 C27 118.9(3) . . ?
C27 C22 P1 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.4(3) . . ?
C27 C26 H26 119.8 . . ?
C22 C27 H27 119.8 . . ?
C26 C27 C22 120.3(3) . . ?
C26 C27 H27 119.8 . . ?
C29 C28 P1 118.5(3) . . ?
C33 C28 P1 121.8(3) . . ?
C33 C28 C29 119.5(3) . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.9(4) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 C29 120.1(4) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.4(3) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.1(4) . . ?
C33 C32 H32 120.0 . . ?
C28 C33 C32 120.2(4) . . ?
C28 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 P1 123.3(2) . . ?
C35 C34 C39 119.6(3) . . ?
C39 C34 P1 117.0(3) . . ?
C34 C35 H35 119.9 . . ?
C34 C35 C36 120.2(3) . . ?
C36 C35 H35 119.9 . . ?
C35 C36 H36 120.1 . . ?
C37 C36 C35 119.8(3) . . ?
C37 C36 H36 120.1 . . ?
C36 C37 H37 119.8 . . ?
C38 C37 C36 120.4(3) . . ?
C38 C37 H37 119.8 . . ?
C37 C38 H38 120.0 . . ?
C37 C38 C39 119.9(3) . . ?
C39 C38 H38 120.0 . . ?
C34 C39 H39 119.9 . . ?
C38 C39 C34 120.1(3) . . ?
C38 C39 H39 119.9 . . ?
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 2.1394(10) . ?
Ni1 P1 2.2198(9) . ?
Ni1 O1 1.883(2) . ?
Ni1 N1 1.909(3) . ?
S1 C13 1.746(3) . ?
P1 C22 1.827(3) . ?
P1 C28 1.835(3) . ?
P1 C34 1.821(3) . ?
O1 C3 1.309(4) . ?
N1 C1 1.303(4) . ?
N1 C8 1.430(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.419(5) . ?
C2 C3 1.422(4) . ?
C2 C7 1.422(4) . ?
C3 C4 1.441(4) . ?
C4 C5 1.389(5) . ?
C4 C18 1.527(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.414(5) . ?
C6 C7 1.369(5) . ?
C6 C14 1.538(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(5) . ?
C8 C13 1.398(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.377(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.392(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.405(5) . ?
C14 C15 1.533(5) . ?
C14 C16 1.531(5) . ?
C14 C17 1.537(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.537(5) . ?
C18 C20 1.541(4) . ?
C18 C21 1.539(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.393(5) . ?
C22 C27 1.403(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.396(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.389(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.396(5) . ?
C28 C33 1.391(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.397(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.385(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.374(7) . ?
C32 H32 0.9500 . ?
C32 C33 1.398(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(5) . ?
C34 C39 1.405(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.397(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.389(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.383(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.388(6) . ?
C39 H39 0.9500 . ?
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 C13 C8 0.6(3) . . . . ?
Ni1 S1 C13 C12 -179.5(3) . . . . ?
Ni1 P1 C22 C23 -22.9(3) . . . . ?
Ni1 P1 C22 C27 156.8(2) . . . . ?
Ni1 P1 C28 C29 -63.9(3) . . . . ?
Ni1 P1 C28 C33 121.8(3) . . . . ?
Ni1 P1 C34 C35 131.1(2) . . . . ?
Ni1 P1 C34 C39 -53.0(3) . . . . ?
Ni1 O1 C3 C2 2.9(4) . . . . ?
Ni1 O1 C3 C4 -176.7(2) . . . . ?
Ni1 N1 C1 C2 11.7(5) . . . . ?
Ni1 N1 C8 C9 -179.9(2) . . . . ?
Ni1 N1 C8 C13 -0.9(4) . . . . ?
P1 Ni1 O1 C3 -166.3(2) . . . . ?
P1 C22 C23 C24 -179.4(3) . . . . ?
P1 C22 C27 C26 179.5(3) . . . . ?
P1 C28 C29 C30 -175.3(3) . . . . ?
P1 C28 C33 C32 174.5(3) . . . . ?
P1 C34 C35 C36 175.6(2) . . . . ?
P1 C34 C39 C38 -175.7(3) . . . . ?
O1 C3 C4 C5 -176.2(3) . . . . ?
O1 C3 C4 C18 6.1(4) . . . . ?
N1 Ni1 O1 C3 5.3(3) . . . . ?
N1 C1 C2 C3 -0.9(5) . . . . ?
N1 C1 C2 C7 175.3(3) . . . . ?
N1 C8 C9 C10 -179.3(3) . . . . ?
N1 C8 C13 S1 0.1(4) . . . . ?
N1 C8 C13 C12 -179.8(3) . . . . ?
C1 N1 C8 C9 6.0(5) . . . . ?
C1 N1 C8 C13 -175.0(3) . . . . ?
C1 C2 C3 O1 -7.1(4) . . . . ?
C1 C2 C3 C4 172.5(3) . . . . ?
C1 C2 C7 C6 -175.8(3) . . . . ?
C2 C3 C4 C5 4.1(4) . . . . ?
C2 C3 C4 C18 -173.5(3) . . . . ?
C3 C2 C7 C6 0.5(5) . . . . ?
C3 C4 C5 C6 -2.0(5) . . . . ?
C3 C4 C18 C19 176.4(3) . . . . ?
C3 C4 C18 C20 -64.6(4) . . . . ?
C3 C4 C18 C21 57.6(4) . . . . ?
C4 C5 C6 C7 -1.0(5) . . . . ?
C4 C5 C6 C14 177.3(3) . . . . ?
C5 C4 C18 C19 -1.3(4) . . . . ?
C5 C4 C18 C20 117.8(3) . . . . ?
C5 C4 C18 C21 -120.0(3) . . . . ?
C5 C6 C7 C2 1.8(4) . . . . ?
C5 C6 C14 C15 18.6(4) . . . . ?
C5 C6 C14 C16 -101.0(4) . . . . ?
C5 C6 C14 C17 139.4(3) . . . . ?
C7 C2 C3 O1 176.8(3) . . . . ?
C7 C2 C3 C4 -3.5(4) . . . . ?
C7 C6 C14 C15 -163.2(3) . . . . ?
C7 C6 C14 C16 77.2(4) . . . . ?
C7 C6 C14 C17 -42.4(4) . . . . ?
C8 N1 C1 C2 -174.4(3) . . . . ?
C8 C9 C10 C11 -1.4(5) . . . . ?
C9 C8 C13 S1 179.2(2) . . . . ?
C9 C8 C13 C12 -0.7(5) . . . . ?
C9 C10 C11 C12 0.0(5) . . . . ?
C10 C11 C12 C13 1.1(5) . . . . ?
C11 C12 C13 S1 179.4(3) . . . . ?
C11 C12 C13 C8 -0.7(5) . . . . ?
C13 C8 C9 C10 1.8(5) . . . . ?
C14 C6 C7 C2 -176.5(3) . . . . ?
C18 C4 C5 C6 175.7(3) . . . . ?
C22 P1 C28 C29 60.7(3) . . . . ?
C22 P1 C28 C33 -113.6(3) . . . . ?
C22 P1 C34 C35 7.9(3) . . . . ?
C22 P1 C34 C39 -176.1(2) . . . . ?
C22 C23 C24 C25 -0.7(5) . . . . ?
C23 C22 C27 C26 -0.8(5) . . . . ?
C23 C24 C25 C26 0.4(5) . . . . ?
C24 C25 C26 C27 -0.3(5) . . . . ?
C25 C26 C27 C22 0.5(5) . . . . ?
C27 C22 C23 C24 0.8(5) . . . . ?
C28 P1 C22 C23 -153.0(3) . . . . ?
C28 P1 C22 C27 26.7(3) . . . . ?
C28 P1 C34 C35 -97.4(3) . . . . ?
C28 P1 C34 C39 78.5(3) . . . . ?
C28 C29 C30 C31 0.6(6) . . . . ?
C29 C28 C33 C32 0.2(5) . . . . ?
C29 C30 C31 C32 0.3(6) . . . . ?
C30 C31 C32 C33 -0.9(6) . . . . ?
C31 C32 C33 C28 0.6(6) . . . . ?
C33 C28 C29 C30 -0.8(5) . . . . ?
C34 P1 C22 C23 100.4(3) . . . . ?
C34 P1 C22 C27 -79.8(3) . . . . ?
C34 P1 C28 C29 169.6(3) . . . . ?
C34 P1 C28 C33 -4.7(3) . . . . ?
C34 C35 C36 C37 0.0(5) . . . . ?
C35 C34 C39 C38 0.4(5) . . . . ?
C35 C36 C37 C38 0.1(5) . . . . ?
C36 C37 C38 C39 0.0(5) . . . . ?
C37 C38 C39 C34 -0.3(5) . . . . ?
C39 C34 C35 C36 -0.2(5) . . . . ?
