#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:02:31 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/69/7716915.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_7716915
loop_
_publ_author_name
'Álvarez-Miguel, Lucía'
'Del Carmen-Rodríguez, Clara'
'Valle, María'
'Álvarez, Celedonio M'
'Martín-Álvarez, José M'
'García-Rodríguez, Raúl'
'Miguel, Daniel'
_publ_section_title
;
 Synthesis and reactivity of air stable Ni(II) complexes with isocyanides
 and dialkyldithiophosphate ligands: acyclic diaminocarbene formation.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15101
_journal_page_last               15112
_journal_paper_doi               10.1039/d4dt01915f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H43 N3 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C28 H43 Cl N3 Ni O6 P S2'
_chemical_formula_weight         706.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.038(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2715(2)
_cell_length_b                   21.9434(4)
_cell_length_c                   18.2332(4)
_cell_measurement_reflns_used    12980
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5840
_cell_measurement_theta_min      2.4530
_cell_volume                     3598.73(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00  14.00   1.00   10.71    --  -10.48 -37.00 150.00   99
  2  ω    -20.00  30.00   1.00   10.71    --  -10.48 -99.00  30.00   50
  3  ω    -84.00  18.00   1.00   10.71    --  -10.48 -57.00  60.00  102
  4  ω    -20.00  53.00   1.00   10.71    --   12.36 -99.00  90.00   73
  5  ω    -20.00  11.00   1.00   10.71    --   12.36 -99.00 -30.00   31
  6  ω     35.00 101.00   1.00   10.71    --   12.36 178.00 -60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081270000
_diffrn_orient_matrix_UB_12      0.0011644000
_diffrn_orient_matrix_UB_13      0.0396718000
_diffrn_orient_matrix_UB_21      0.0738213000
_diffrn_orient_matrix_UB_22      -0.0110384000
_diffrn_orient_matrix_UB_23      0.0058090000
_diffrn_orient_matrix_UB_31      0.0265174000
_diffrn_orient_matrix_UB_32      0.0303571000
_diffrn_orient_matrix_UB_33      0.0005910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.732
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         9086
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0495
_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/[σ²(Fo²)+(0.0570P)²+2.0926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6194
_reflns_number_total             9086
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01915f2.cif
_cod_data_source_block           m086b
_cod_depositor_comments
'Adding full bibliography for 7716902--7716918.cif.'
_cod_original_cell_volume        3598.71(15)
_cod_database_code               7716915
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C112  H172  Cl4  N12  Ni4  O24  P4  S8  '
_chemical_oxdiff_usercomment     'yellow block'
_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.
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Rigid bond restraints
 O51, C51, C53, C52
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C52 \\sim C51 \\sim C53: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02 within 2A
C51 \\sim C53 \\sim C52: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C51, C52, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C41(H41), C51(H51)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.291
_oxdiff_exptl_absorpt_empirical_full_min 0.734
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_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 -0.39103(4) -0.50711(2) -0.25330(2) 0.04409(11) Uani 1 1 d . . . . .
S1 S -0.44336(11) -0.44122(4) -0.16919(5) 0.0695(2) Uani 1 1 d . . . . .
S2 S -0.31416(9) -0.42894(3) -0.31076(5) 0.0609(2) Uani 1 1 d . . . . .
P1 P -0.35774(9) -0.37935(3) -0.22676(5) 0.05514(19) Uani 1 1 d . . . . .
O41 O -0.2215(2) -0.34468(9) -0.17775(13) 0.0681(6) Uani 1 1 d . . . . .
O51 O -0.4587(2) -0.32282(9) -0.25310(12) 0.0661(5) Uani 1 1 d . U . . .
N1 N -0.5274(2) -0.60287(10) -0.17677(13) 0.0520(5) Uani 1 1 d . . . . .
N2 N -0.2106(3) -0.58044(11) -0.32242(14) 0.0531(6) Uani 1 1 d . . . . .
H2 H -0.195(4) -0.6012(15) -0.3490(18) 0.064 Uiso 1 1 d . U . . .
N3 N -0.4584(2) -0.58158(11) -0.38249(12) 0.0538(5) Uani 1 1 d . . . . .
C1 C -0.4696(3) -0.56780(12) -0.20666(15) 0.0467(6) Uani 1 1 d . . . . .
C2 C -0.3493(3) -0.56150(11) -0.32712(14) 0.0434(5) Uani 1 1 d . . . . .
C11 C -0.5961(3) -0.64229(12) -0.13540(18) 0.0564(7) Uani 1 1 d . . . . .
C12 C -0.5489(4) -0.63913(16) -0.0565(2) 0.0722(9) Uani 1 1 d . . . . .
C13 C -0.6203(5) -0.6777(2) -0.0168(3) 0.0981(14) Uani 1 1 d . . . . .
H13 H -0.5940 -0.6771 0.0358 0.118 Uiso 1 1 calc R U . . .
C14 C -0.7279(6) -0.7164(2) -0.0533(4) 0.1118(18) Uani 1 1 d . . . . .
H14 H -0.7733 -0.7422 -0.0251 0.134 Uiso 1 1 calc R U . . .
C15 C -0.7714(4) -0.71851(18) -0.1306(4) 0.1050(16) Uani 1 1 d . . . . .
H15 H -0.8458 -0.7455 -0.1540 0.126 Uiso 1 1 calc R U . . .
C16 C -0.7054(3) -0.68065(14) -0.1749(2) 0.0726(9) Uani 1 1 d . . . . .
C17 C -0.4284(5) -0.5963(2) -0.0175(2) 0.1028(14) Uani 1 1 d . . . . .
H17A H -0.4532 -0.5555 -0.0354 0.154 Uiso 1 1 calc R U . . .
H17B H -0.3360 -0.6080 -0.0284 0.154 Uiso 1 1 calc R U . . .
H17C H -0.4189 -0.5979 0.0360 0.154 Uiso 1 1 calc R U . . .
C18 C -0.7503(5) -0.68114(18) -0.2598(3) 0.1024(14) Uani 1 1 d . . . . .
H18A H -0.6636 -0.6861 -0.2792 0.154 Uiso 1 1 calc R U . . .
H18B H -0.7983 -0.6434 -0.2776 0.154 Uiso 1 1 calc R U . . .
H18C H -0.8177 -0.7143 -0.2767 0.154 Uiso 1 1 calc R U . . .
C21 C -0.0828(3) -0.55884(12) -0.26758(16) 0.0502(6) Uani 1 1 d . . . . .
C22 C -0.0508(3) -0.58278(14) -0.19438(17) 0.0608(7) Uani 1 1 d . . . . .
C23 C 0.0746(4) -0.55903(19) -0.1432(2) 0.0816(11) Uani 1 1 d . . . . .
H23 H 0.0980 -0.5726 -0.0934 0.098 Uiso 1 1 calc R U . . .
C24 C 0.1636(4) -0.51611(19) -0.1652(3) 0.0877(12) Uani 1 1 d . . . . .
H24 H 0.2448 -0.5004 -0.1299 0.105 Uiso 1 1 calc R U . . .
C25 C 0.1337(4) -0.49656(16) -0.2378(3) 0.0797(11) Uani 1 1 d . . . . .
H25 H 0.1973 -0.4687 -0.2523 0.096 Uiso 1 1 calc R U . . .
C26 C 0.0099(3) -0.51733(14) -0.29097(19) 0.0617(7) Uani 1 1 d . . . . .
C27 C -0.1365(4) -0.63395(19) -0.1722(2) 0.0925(12) Uani 1 1 d . . . . .
H27A H -0.0719 -0.6683 -0.1572 0.139 Uiso 1 1 calc R U . . .
H27B H -0.2161 -0.6451 -0.2144 0.139 Uiso 1 1 calc R U . . .
H27C H -0.1766 -0.6215 -0.1308 0.139 Uiso 1 1 calc R U . . .
C28 C -0.0194(4) -0.49589(19) -0.3716(2) 0.0871(11) Uani 1 1 d . . . . .
H28A H -0.1221 -0.4847 -0.3891 0.131 Uiso 1 1 calc R U . . .
H28B H 0.0031 -0.5281 -0.4027 0.131 Uiso 1 1 calc R U . . .
H28C H 0.0421 -0.4612 -0.3746 0.131 Uiso 1 1 calc R U . . .
C31 C -0.4361(4) -0.62730(16) -0.43800(18) 0.0731(9) Uani 1 1 d . . . . .
H31A H -0.3444 -0.6185 -0.4526 0.088 Uiso 1 1 calc R U . . .
H31B H -0.5172 -0.6247 -0.4829 0.088 Uiso 1 1 calc R U . . .
C32 C -0.4290(6) -0.69077(18) -0.4064(3) 0.1096(15) Uani 1 1 d . . . . .
H32A H -0.5218 -0.7004 -0.3945 0.164 Uiso 1 1 calc R U . . .
H32B H -0.3501 -0.6932 -0.3613 0.164 Uiso 1 1 calc R U . . .
H32C H -0.4107 -0.7192 -0.4431 0.164 Uiso 1 1 calc R U . . .
C33 C -0.6117(3) -0.55987(16) -0.39153(17) 0.0664(8) Uani 1 1 d . . . . .
H33A H -0.6215 -0.5421 -0.3442 0.080 Uiso 1 1 calc R U . . .
H33B H -0.6791 -0.5943 -0.4028 0.080 Uiso 1 1 calc R U . . .
C34 C -0.6556(4) -0.5132(2) -0.4534(2) 0.1029(15) Uani 1 1 d . . . . .
H34A H -0.5888 -0.4791 -0.4427 0.154 Uiso 1 1 calc R U . . .
H34B H -0.7552 -0.4996 -0.4563 0.154 Uiso 1 1 calc R U . . .
H34C H -0.6507 -0.5311 -0.5008 0.154 Uiso 1 1 calc R U . . .
C41 C -0.0791(4) -0.37593(17) -0.1446(2) 0.0795(10) Uani 1 1 d . . . . .
H41 H -0.0796 -0.4163 -0.1676 0.095 Uiso 1 1 calc R U . . .
C42 C -0.0635(6) -0.3826(3) -0.0624(3) 0.1322(19) Uani 1 1 d . . . . .
H42A H -0.1485 -0.4038 -0.0537 0.198 Uiso 1 1 calc R U . . .
H42B H -0.0568 -0.3430 -0.0394 0.198 Uiso 1 1 calc R U . . .
H42C H 0.0249 -0.4054 -0.0407 0.198 Uiso 1 1 calc R U . . .
C43 C 0.0378(5) -0.3385(3) -0.1637(4) 0.144(2) Uani 1 1 d . . . . .
H43A H 0.0360 -0.2984 -0.1427 0.216 Uiso 1 1 calc R U . . .
H43B H 0.0210 -0.3356 -0.2176 0.216 Uiso 1 1 calc R U . . .
H43C H 0.1330 -0.3569 -0.1431 0.216 Uiso 1 1 calc R U . . .
C51 C -0.6007(3) -0.32718(15) -0.3115(2) 0.0722(9) Uani 1 1 d . U . . .
H51 H -0.6185 -0.3698 -0.3273 0.087 Uiso 1 1 calc R U . . .
C52 C -0.5872(6) -0.2902(3) -0.3764(3) 0.162(3) Uani 1 1 d . U . . .
H52A H -0.4968 -0.3005 -0.3903 0.243 Uiso 1 1 calc R U . . .
H52B H -0.5855 -0.2478 -0.3632 0.243 Uiso 1 1 calc R U . . .
H52C H -0.6705 -0.2980 -0.4183 0.243 Uiso 1 1 calc R U . . .
C53 C -0.7189(6) -0.3066(4) -0.2774(4) 0.177(3) Uani 1 1 d . U . . .
H53A H -0.7105 -0.2635 -0.2690 0.265 Uiso 1 1 calc R U . . .
H53B H -0.7105 -0.3272 -0.2300 0.265 Uiso 1 1 calc R U . . .
H53C H -0.8136 -0.3158 -0.3107 0.265 Uiso 1 1 calc R U . . .
Cl1 Cl -0.02124(11) -0.66742(5) -0.47684(7) 0.0928(3) Uani 1 1 d . . . . .
O1 O -0.0653(5) -0.6652(2) -0.4080(2) 0.1749(19) Uani 1 1 d . . . . .
O2 O 0.1268(4) -0.6625(3) -0.4625(4) 0.252(3) Uani 1 1 d . . . . .
O3 O -0.0602(5) -0.72347(18) -0.5102(3) 0.1618(17) Uani 1 1 d . . . . .
O4 O -0.1144(6) -0.6235(2) -0.5232(3) 0.1835(19) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
1 -15 -22 0.1371
0 -31 -2 0.1096
-6 25 -6 0.1613
5 21 -18 0.1929
-13 -2 7 0.0560
13 8 -4 0.1377
-2 -8 25 0.0866
1 -28 -10 0.1213
-1 29 10 0.0941
0 3 -25 0.1257
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 44.16(3) . . ?
S2 Ni1 S1 88.40(3) . . ?
S2 Ni1 P1 44.32(2) . . ?
C1 Ni1 S1 88.55(8) . . ?
C1 Ni1 S2 174.95(8) . . ?
C1 Ni1 P1 132.70(8) . . ?
C1 Ni1 C2 92.55(11) . . ?
C2 Ni1 S1 178.30(8) . . ?
C2 Ni1 S2 90.42(8) . . ?
C2 Ni1 P1 134.71(8) . . ?
P1 S1 Ni1 84.22(3) . . ?
P1 S2 Ni1 84.90(3) . . ?
S1 P1 Ni1 51.62(3) . . ?
S1 P1 S2 102.29(4) . . ?
S2 P1 Ni1 50.78(3) . . ?
O41 P1 Ni1 128.14(9) . . ?
O41 P1 S1 113.66(10) . . ?
O41 P1 S2 114.78(9) . . ?
O41 P1 O51 97.53(11) . . ?
O51 P1 Ni1 134.34(9) . . ?
O51 P1 S1 114.72(10) . . ?
O51 P1 S2 114.54(10) . . ?
C41 O41 P1 121.8(2) . . ?
C51 O51 P1 122.19(18) . . ?
C1 N1 C11 175.3(3) . . ?
C2 N2 H2 121(3) . . ?
C2 N2 C21 124.2(2) . . ?
C21 N2 H2 115(3) . . ?
C2 N3 C31 122.9(2) . . ?
C2 N3 C33 121.2(2) . . ?
C33 N3 C31 115.9(2) . . ?
N1 C1 Ni1 174.7(2) . . ?
N2 C2 Ni1 120.44(19) . . ?
N3 C2 Ni1 120.02(19) . . ?
N3 C2 N2 119.5(2) . . ?
N1 C11 C12 117.0(3) . . ?
C16 C11 N1 118.0(3) . . ?
C16 C11 C12 125.0(3) . . ?
C11 C12 C17 121.9(3) . . ?
C13 C12 C11 116.0(4) . . ?
C13 C12 C17 122.1(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.6(4) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 120.9(4) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 115.5(4) . . ?
C11 C16 C18 121.8(3) . . ?
C15 C16 C18 122.7(4) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 119.4(3) . . ?
C26 C21 N2 118.1(3) . . ?
C26 C21 C22 122.4(3) . . ?
C21 C22 C23 116.4(3) . . ?
C21 C22 C27 122.7(3) . . ?
C23 C22 C27 120.7(3) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.4(3) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.1(3) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 C28 121.8(3) . . ?
C25 C26 C21 118.0(3) . . ?
C25 C26 C28 120.2(3) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C31 H31A 109.3 . . ?
N3 C31 H31B 109.3 . . ?
N3 C31 C32 111.5(3) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.1 . . ?
N3 C33 H33B 109.1 . . ?
N3 C33 C34 112.5(3) . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O41 C41 H41 109.4 . . ?
C42 C41 O41 108.6(3) . . ?
C42 C41 H41 109.4 . . ?
C43 C41 O41 106.3(3) . . ?
C43 C41 H41 109.4 . . ?
C43 C41 C42 113.6(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O51 C51 H51 109.3 . . ?
C52 C51 O51 108.0(3) . . ?
C52 C51 H51 109.3 . . ?
C53 C51 O51 107.7(4) . . ?
C53 C51 H51 109.3 . . ?
C53 C51 C52 113.2(5) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O1 Cl1 O4 103.8(3) . . ?
O2 Cl1 O1 109.1(3) . . ?
O2 Cl1 O3 107.7(3) . . ?
O2 Cl1 O4 120.4(4) . . ?
O3 Cl1 O1 108.7(3) . . ?
O3 Cl1 O4 106.6(3) . . ?
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 2.2447(8) . ?
Ni1 S2 2.2159(8) . ?
Ni1 P1 2.8490(8) . ?
Ni1 C1 1.824(3) . ?
Ni1 C2 1.907(2) . ?
S1 P1 1.9949(11) . ?
S2 P1 1.9984(10) . ?
P1 O41 1.557(2) . ?
P1 O51 1.558(2) . ?
O41 C41 1.481(4) . ?
O51 C51 1.482(4) . ?
N1 C1 1.148(3) . ?
N1 C11 1.398(4) . ?
N2 H2 0.71(3) . ?
N2 C2 1.335(3) . ?
N2 C21 1.433(3) . ?
N3 C2 1.319(3) . ?
N3 C31 1.475(4) . ?
N3 C33 1.470(4) . ?
C11 C12 1.400(5) . ?
C11 C16 1.379(4) . ?
C12 C13 1.383(5) . ?
C12 C17 1.501(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.355(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.370(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(5) . ?
C16 C18 1.502(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.398(4) . ?
C21 C26 1.389(4) . ?
C22 C23 1.402(5) . ?
C22 C27 1.487(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.374(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.356(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(5) . ?
C26 C28 1.505(5) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.503(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.505(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C41 H41 0.9800 . ?
C41 C42 1.478(6) . ?
C41 C43 1.467(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C51 H51 0.9800 . ?
C51 C52 1.466(6) . ?
C51 C53 1.456(6) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
Cl1 O1 1.412(4) . ?
Cl1 O2 1.337(4) . ?
Cl1 O3 1.381(4) . ?
Cl1 O4 1.427(4) . ?
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 P1 O41 C41 7.5(3) . . . . ?
Ni1 P1 O51 C51 -8.5(3) . . . . ?
S1 P1 O41 C41 66.4(3) . . . . ?
S1 P1 O51 C51 -68.1(2) . . . . ?
S2 P1 O41 C41 -50.9(3) . . . . ?
S2 P1 O51 C51 49.8(3) . . . . ?
P1 O41 C41 C42 -106.7(4) . . . . ?
P1 O41 C41 C43 130.8(4) . . . . ?
P1 O51 C51 C52 -116.8(4) . . . . ?
P1 O51 C51 C53 120.7(4) . . . . ?
O41 P1 O51 C51 171.5(2) . . . . ?
O51 P1 O41 C41 -172.4(2) . . . . ?
N1 C11 C12 C13 178.9(3) . . . . ?
N1 C11 C12 C17 -1.0(5) . . . . ?
N1 C11 C16 C15 -179.3(3) . . . . ?
N1 C11 C16 C18 0.4(4) . . . . ?
N2 C21 C22 C23 -179.1(3) . . . . ?
N2 C21 C22 C27 5.5(4) . . . . ?
N2 C21 C26 C25 -179.9(3) . . . . ?
N2 C21 C26 C28 -1.1(4) . . . . ?
C2 N2 C21 C22 80.5(4) . . . . ?
C2 N2 C21 C26 -103.5(3) . . . . ?
C2 N3 C31 C32 79.9(4) . . . . ?
C2 N3 C33 C34 102.1(3) . . . . ?
C11 C12 C13 C14 0.7(5) . . . . ?
C12 C11 C16 C15 0.0(5) . . . . ?
C12 C11 C16 C18 179.7(3) . . . . ?
C12 C13 C14 C15 -0.6(7) . . . . ?
C13 C14 C15 C16 0.2(7) . . . . ?
C14 C15 C16 C11 0.1(5) . . . . ?
C14 C15 C16 C18 -179.6(4) . . . . ?
C16 C11 C12 C13 -0.4(5) . . . . ?
C16 C11 C12 C17 179.7(3) . . . . ?
C17 C12 C13 C14 -179.4(4) . . . . ?
C21 N2 C2 Ni1 -5.3(4) . . . . ?
C21 N2 C2 N3 176.0(3) . . . . ?
C21 C22 C23 C24 -2.3(5) . . . . ?
C22 C21 C26 C25 -3.9(4) . . . . ?
C22 C21 C26 C28 174.9(3) . . . . ?
C22 C23 C24 C25 -1.5(6) . . . . ?
C23 C24 C25 C26 2.6(6) . . . . ?
C24 C25 C26 C21 0.0(5) . . . . ?
C24 C25 C26 C28 -178.9(3) . . . . ?
C26 C21 C22 C23 5.0(4) . . . . ?
C26 C21 C22 C27 -170.5(3) . . . . ?
C27 C22 C23 C24 173.3(3) . . . . ?
C31 N3 C2 Ni1 -175.1(2) . . . . ?
C31 N3 C2 N2 3.6(4) . . . . ?
C31 N3 C33 C34 -78.8(4) . . . . ?
C33 N3 C2 Ni1 3.9(4) . . . . ?
C33 N3 C2 N2 -177.4(3) . . . . ?
C33 N3 C31 C32 -99.2(4) . . . . ?
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
1.0217 -15.2979 -22.0753 -0.8853 0.1160 -0.4504
0.0547 -30.9996 -2.0700 -0.1178 0.3342 -0.9408
-6.1267 24.8379 -6.2625 -0.2693 -0.7628 0.5878
4.7799 20.8560 -18.2854 -0.6623 0.0164 0.7491
-13.0461 -1.6837 6.9545 0.1679 -0.9041 -0.3930
12.6053 7.9579 -4.4507 -0.0649 0.8168 0.5732
-2.1325 -7.9979 24.7618 0.9557 0.0747 -0.2847
1.1157 -28.2798 -10.4178 -0.4372 0.3340 -0.8351
-0.8809 28.5065 9.9633 0.4213 -0.3218 0.8479
-0.1226 2.6079 -24.7898 -0.9814 -0.1818 0.0613
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 49.7 0.2 ?
2 0.086 0.147 0.873 14.4 0.1 ?
3 0.086 0.353 0.373 14.4 0.1 ?
4 0.000 0.500 1.000 49.7 0.2 ?
5 -0.086 0.647 0.627 14.4 0.1 ?
6 -0.086 0.853 0.127 14.4 0.1 ?
