#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:02:31 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/69/7716916.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_7716916
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         'C27 H39 N3 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C27 H39 Cl N3 Ni O6 P S2'
_chemical_formula_weight         690.86
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.736(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5858(5)
_cell_length_b                   19.6057(7)
_cell_length_c                   14.6622(5)
_cell_measurement_reflns_used    5066
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3050
_cell_measurement_theta_min      2.5660
_cell_volume                     3336.8(2)
_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 0.836
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  13.00   1.00   13.26    --  -10.64 -99.00  60.00   33
  2  ω     -6.00  67.00   1.00   13.26    --   12.51  37.00 -30.00   73
  3  ω    -41.00  45.00   1.00   13.26    --   12.51 -19.00 -30.00   86
;
_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      0.0166316000
_diffrn_orient_matrix_UB_12      -0.0341377000
_diffrn_orient_matrix_UB_13      -0.0036511000
_diffrn_orient_matrix_UB_21      -0.0559523000
_diffrn_orient_matrix_UB_22      -0.0069729000
_diffrn_orient_matrix_UB_23      -0.0356338000
_diffrn_orient_matrix_UB_31      0.0181017000
_diffrn_orient_matrix_UB_32      0.0097579000
_diffrn_orient_matrix_UB_33      -0.0383207000
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.677
_diffrn_reflns_theta_min         2.077
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.833
_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    1.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.149
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7911
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0793
_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)+(0.1104P)²+4.1394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4455
_reflns_number_total             7911
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01915f2.cif
_cod_data_source_block           m089pa
_cod_depositor_comments
'Adding full bibliography for 7716902--7716918.cif.'
_cod_database_code               7716916
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C108  H156  Cl4  N12  Ni4  O24  P4  S8  '
_chemical_oxdiff_usercomment     orange
_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 99.86
_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. Restrained distances
 C6-C7
 1.476 with sigma of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.795
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 0.33704(6) 0.53981(3) 0.21243(4) 0.0612(2) Uani 1 1 d . . . . .
S1 S 0.17509(15) 0.50315(10) 0.09604(12) 0.0898(5) Uani 1 1 d . . . . .
S2 S 0.43158(17) 0.45101(9) 0.17939(14) 0.0941(5) Uani 1 1 d . . . . .
P1 P 0.27853(18) 0.43060(9) 0.07846(12) 0.0885(5) Uani 1 1 d . . . . .
O1 O 0.2476(5) 0.3554(2) 0.0947(3) 0.1053(15) Uani 1 1 d . . . . .
O2 O 0.2714(5) 0.4277(2) -0.0313(3) 0.1183(19) Uani 1 1 d . . . . .
N1 N 0.5346(4) 0.5716(2) 0.3983(3) 0.0678(11) Uani 1 1 d . . . . .
N2 N 0.2772(5) 0.6772(2) 0.1825(4) 0.0696(12) Uani 1 1 d . . . . .
H2 H 0.245(6) 0.706(3) 0.177(5) 0.083 Uiso 1 1 d . U . . .
N3 N 0.2105(4) 0.6259(2) 0.2905(3) 0.0693(11) Uani 1 1 d . . . . .
C1 C 0.4610(5) 0.5603(3) 0.3242(4) 0.0649(13) Uani 1 1 d . . . . .
C2 C 0.2657(4) 0.6222(3) 0.2294(3) 0.0591(11) Uani 1 1 d . . . . .
C4 C 0.1533(8) 0.3228(6) 0.0337(6) 0.154(4) Uani 1 1 d . . . . .
H4A H 0.1554 0.3208 -0.0317 0.185 Uiso 1 1 calc R U . . .
H4B H 0.0858 0.3489 0.0288 0.185 Uiso 1 1 calc R U . . .
C5 C 0.1423(8) 0.2552(5) 0.0649(8) 0.150(4) Uani 1 1 d . . . . .
H5A H 0.0652 0.2391 0.0294 0.225 Uiso 1 1 calc R U . . .
H5B H 0.1586 0.2552 0.1345 0.225 Uiso 1 1 calc R U . . .
H5C H 0.1958 0.2257 0.0519 0.225 Uiso 1 1 calc R U . . .
C6 C 0.2946(14) 0.4897(5) -0.0725(7) 0.193(6) Uani 1 1 d D . . . .
H6A H 0.3633 0.5111 -0.0252 0.231 Uiso 1 1 calc R U . . .
H6B H 0.2308 0.5211 -0.0859 0.231 Uiso 1 1 calc R U . . .
C7 C 0.3111(12) 0.4759(6) -0.1638(8) 0.189(5) Uani 1 1 d D . . . .
H7A H 0.3683 0.4410 -0.1522 0.283 Uiso 1 1 calc R U . . .
H7B H 0.3363 0.5168 -0.1856 0.283 Uiso 1 1 calc R U . . .
H7C H 0.2397 0.4610 -0.2137 0.283 Uiso 1 1 calc R U . . .
C11 C 0.6206(4) 0.5913(3) 0.4877(3) 0.0633(12) Uani 1 1 d . . . . .
C12 C 0.7357(5) 0.5851(3) 0.4976(5) 0.0815(16) Uani 1 1 d . . . . .
C13 C 0.8184(6) 0.6068(4) 0.5871(5) 0.0915(19) Uani 1 1 d . . . . .
H13 H 0.8959 0.6045 0.5972 0.110 Uiso 1 1 calc R U . . .
C14 C 0.7876(7) 0.6313(4) 0.6598(5) 0.100(2) Uani 1 1 d . . . . .
H14 H 0.8448 0.6454 0.7190 0.121 Uiso 1 1 calc R U . . .
C15 C 0.6757(6) 0.6359(4) 0.6485(4) 0.0894(19) Uani 1 1 d . . . . .
H15 H 0.6575 0.6527 0.6999 0.107 Uiso 1 1 calc R U . . .
C16 C 0.5886(5) 0.6159(3) 0.5614(4) 0.0722(14) Uani 1 1 d . . . . .
C17 C 0.7651(7) 0.5579(4) 0.4141(6) 0.116(3) Uani 1 1 d . . . . .
H17A H 0.8465 0.5499 0.4373 0.174 Uiso 1 1 calc R U . . .
H17B H 0.7429 0.5906 0.3613 0.174 Uiso 1 1 calc R U . . .
H17C H 0.7245 0.5159 0.3904 0.174 Uiso 1 1 calc R U . . .
C18 C 0.4644(5) 0.6212(4) 0.5480(5) 0.0930(19) Uani 1 1 d . . . . .
H18A H 0.4264 0.6544 0.4979 0.139 Uiso 1 1 calc R U . . .
H18B H 0.4597 0.6348 0.6092 0.139 Uiso 1 1 calc R U . . .
H18C H 0.4277 0.5777 0.5282 0.139 Uiso 1 1 calc R U . . .
C21 C 0.3484(5) 0.6798(3) 0.1251(4) 0.0679(13) Uani 1 1 d . . . . .
C22 C 0.2949(6) 0.6698(3) 0.0228(4) 0.0810(16) Uani 1 1 d . . . . .
C23 C 0.3656(8) 0.6703(3) -0.0305(5) 0.100(2) Uani 1 1 d . . . . .
H23 H 0.3336 0.6632 -0.0985 0.119 Uiso 1 1 calc R U . . .
C24 C 0.4811(9) 0.6812(4) 0.0156(7) 0.112(3) Uani 1 1 d . . . . .
H24 H 0.5278 0.6789 -0.0204 0.135 Uiso 1 1 calc R U . . .
C25 C 0.5288(6) 0.6953(4) 0.1143(7) 0.107(2) Uani 1 1 d . . . . .
H25 H 0.6073 0.7043 0.1441 0.128 Uiso 1 1 calc R U . . .
C26 C 0.4628(5) 0.6968(3) 0.1713(5) 0.0832(17) Uani 1 1 d . . . . .
C27 C 0.1678(6) 0.6620(4) -0.0283(5) 0.106(2) Uani 1 1 d . . . . .
H27A H 0.1418 0.6262 0.0027 0.160 Uiso 1 1 calc R U . . .
H27B H 0.1488 0.6508 -0.0966 0.160 Uiso 1 1 calc R U . . .
H27C H 0.1307 0.7040 -0.0240 0.160 Uiso 1 1 calc R U . . .
C28 C 0.5135(7) 0.7207(4) 0.2778(5) 0.110(2) Uani 1 1 d . . . . .
H28A H 0.5305 0.7686 0.2797 0.165 Uiso 1 1 calc R U . . .
H28B H 0.5831 0.6960 0.3132 0.165 Uiso 1 1 calc R U . . .
H28C H 0.4591 0.7129 0.3080 0.165 Uiso 1 1 calc R U . . .
C31 C 0.1621(5) 0.6892(3) 0.3131(5) 0.0816(16) Uani 1 1 d . . . . .
H31A H 0.1899 0.7282 0.2880 0.098 Uiso 1 1 calc R U . . .
H31B H 0.1871 0.6943 0.3842 0.098 Uiso 1 1 calc R U . . .
C32 C 0.0321(6) 0.6870(4) 0.2663(5) 0.103(2) Uani 1 1 d . . . . .
H32A H 0.0068 0.6856 0.1949 0.124 Uiso 1 1 calc R U . . .
H32B H 0.0006 0.7277 0.2838 0.124 Uiso 1 1 calc R U . . .
C33 C -0.0112(6) 0.6240(4) 0.3021(6) 0.109(2) Uani 1 1 d . . . . .
H33A H -0.0940 0.6204 0.2670 0.131 Uiso 1 1 calc R U . . .
H33B H 0.0047 0.6288 0.3720 0.131 Uiso 1 1 calc R U . . .
C34 C 0.0465(6) 0.5582(4) 0.2855(6) 0.100(2) Uani 1 1 d . . . . .
H34A H 0.0241 0.5199 0.3159 0.120 Uiso 1 1 calc R U . . .
H34B H 0.0209 0.5492 0.2152 0.120 Uiso 1 1 calc R U . . .
C35 C 0.1762(5) 0.5657(3) 0.3299(4) 0.0774(15) Uani 1 1 d . . . . .
H35A H 0.2027 0.5695 0.4012 0.093 Uiso 1 1 calc R U . . .
H35B H 0.2114 0.5256 0.3148 0.093 Uiso 1 1 calc R U . . .
Cl1 Cl 0.16802(15) 0.85835(9) 0.13806(12) 0.0844(4) Uani 1 1 d . . . . .
O3 O 0.1191(8) 0.8991(7) 0.1787(11) 0.286(7) Uani 1 1 d . . . . .
O4 O 0.1567(19) 0.8870(8) 0.0613(7) 0.407(13) Uani 1 1 d . . . . .
O5 O 0.2782(6) 0.8467(6) 0.2027(7) 0.217(4) Uani 1 1 d . . . . .
O6 O 0.1109(7) 0.7981(4) 0.1150(8) 0.225(5) 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 0 0 0.0633
7 21 -12 0.0574
9 -17 -15 0.0953
2 -27 -5 0.0955
2 27 -1 0.1007
-11 0 20 0.1635
2 1 -2 0.0057
1 0 0 0.0856
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 S2 89.36(7) . . ?
S1 Ni1 P1 45.38(7) . . ?
S2 Ni1 P1 44.00(7) . . ?
C1 Ni1 S1 168.82(17) . . ?
C1 Ni1 S2 91.39(17) . . ?
C1 Ni1 P1 134.58(17) . . ?
C1 Ni1 C2 88.7(2) . . ?
C2 Ni1 S1 92.06(15) . . ?
C2 Ni1 S2 171.98(15) . . ?
C2 Ni1 P1 136.66(15) . . ?
P1 S1 Ni1 83.08(8) . . ?
P1 S2 Ni1 82.78(9) . . ?
S1 P1 Ni1 51.54(6) . . ?
S2 P1 Ni1 53.22(6) . . ?
S2 P1 S1 104.73(10) . . ?
O1 P1 Ni1 128.75(18) . . ?
O1 P1 S1 115.8(2) . . ?
O1 P1 S2 107.8(2) . . ?
O1 P1 O2 101.6(2) . . ?
O2 P1 Ni1 129.61(19) . . ?
O2 P1 S1 111.8(3) . . ?
O2 P1 S2 115.4(2) . . ?
C4 O1 P1 123.7(6) . . ?
C6 O2 P1 117.3(5) . . ?
C1 N1 C11 174.9(5) . . ?
C2 N2 H2 123(6) . . ?
C2 N2 C21 123.4(4) . . ?
C21 N2 H2 113(6) . . ?
C2 N3 C31 124.5(5) . . ?
C2 N3 C35 122.4(5) . . ?
C35 N3 C31 112.5(4) . . ?
N1 C1 Ni1 175.1(5) . . ?
N2 C2 Ni1 118.2(4) . . ?
N2 C2 N3 119.9(5) . . ?
N3 C2 Ni1 121.9(4) . . ?
O1 C4 H4A 108.9 . . ?
O1 C4 H4B 108.9 . . ?
O1 C4 C5 113.5(8) . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C6 H6A 109.5 . . ?
O2 C6 H6B 109.5 . . ?
O2 C6 C7 110.7(7) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C11 C12 117.9(5) . . ?
C16 C11 N1 118.6(5) . . ?
C16 C11 C12 123.5(5) . . ?
C11 C12 C17 120.9(6) . . ?
C13 C12 C11 115.9(6) . . ?
C13 C12 C17 123.1(6) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.9(6) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.8(6) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.7(6) . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C15 117.2(5) . . ?
C11 C16 C18 121.7(5) . . ?
C15 C16 C18 121.1(6) . . ?
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 117.9(5) . . ?
C26 C21 N2 119.2(5) . . ?
C26 C21 C22 122.7(5) . . ?
C21 C22 C27 122.1(6) . . ?
C23 C22 C21 116.9(7) . . ?
C23 C22 C27 120.9(6) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.8(7) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(7) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.2 . . ?
C24 C25 C26 121.5(7) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C25 117.1(7) . . ?
C21 C26 C28 121.8(6) . . ?
C25 C26 C28 121.0(7) . . ?
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 109.7 . . ?
N3 C31 H31B 109.7 . . ?
N3 C31 C32 110.0(5) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C31 C32 C33 109.7(6) . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
C32 C33 C34 111.6(6) . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C35 C34 C33 110.3(6) . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
N3 C35 C34 110.2(5) . . ?
N3 C35 H35A 109.6 . . ?
N3 C35 H35B 109.6 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
O3 Cl1 O5 108.8(6) . . ?
O3 Cl1 O6 110.7(7) . . ?
O4 Cl1 O3 103.7(12) . . ?
O4 Cl1 O5 116.4(12) . . ?
O4 Cl1 O6 108.1(8) . . ?
O6 Cl1 O5 109.1(6) . . ?
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 2.2124(17) . ?
Ni1 S2 2.2643(18) . ?
Ni1 P1 2.8048(17) . ?
Ni1 C1 1.818(6) . ?
Ni1 C2 1.910(5) . ?
S1 P1 2.011(3) . ?
S2 P1 1.964(3) . ?
P1 O1 1.567(5) . ?
P1 O2 1.577(4) . ?
O1 C4 1.340(9) . ?
O2 C6 1.438(10) . ?
N1 C1 1.145(7) . ?
N1 C11 1.393(7) . ?
N2 H2 0.68(6) . ?
N2 C2 1.317(6) . ?
N2 C21 1.446(7) . ?
N3 C2 1.331(6) . ?
N3 C31 1.475(7) . ?
N3 C35 1.451(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.427(12) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.457(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 C12 1.405(8) . ?
C11 C16 1.378(7) . ?
C12 C13 1.389(9) . ?
C12 C17 1.507(9) . ?
C13 H13 0.9300 . ?
C13 C14 1.355(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.356(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(8) . ?
C16 C18 1.501(8) . ?
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 1.401(8) . ?
C21 C26 1.375(8) . ?
C22 C23 1.394(9) . ?
C22 C27 1.489(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.362(11) . ?
C24 H24 0.9300 . ?
C24 C25 1.363(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(9) . ?
C26 C28 1.516(10) . ?
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 1.510(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.523(10) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.545(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.512(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
Cl1 O3 1.287(9) . ?
Cl1 O4 1.216(8) . ?
Cl1 O5 1.363(7) . ?
Cl1 O6 1.356(8) . ?
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 O1 C4 129.0(7) . . . . ?
Ni1 P1 O2 C6 -1.9(10) . . . . ?
S1 P1 O1 C4 68.9(8) . . . . ?
S1 P1 O2 C6 55.5(9) . . . . ?
S2 P1 O1 C4 -174.2(7) . . . . ?
S2 P1 O2 C6 -64.0(9) . . . . ?
P1 O1 C4 C5 -178.7(8) . . . . ?
P1 O2 C6 C7 166.8(9) . . . . ?
O1 P1 O2 C6 179.6(8) . . . . ?
O2 P1 O1 C4 -52.5(8) . . . . ?
N1 C11 C12 C13 178.5(5) . . . . ?
N1 C11 C12 C17 0.0(9) . . . . ?
N1 C11 C16 C15 -179.1(5) . . . . ?
N1 C11 C16 C18 0.6(8) . . . . ?
N2 C21 C22 C23 -178.0(5) . . . . ?
N2 C21 C22 C27 4.7(8) . . . . ?
N2 C21 C26 C25 177.0(5) . . . . ?
N2 C21 C26 C28 -7.2(8) . . . . ?
N3 C31 C32 C33 56.8(7) . . . . ?
C2 N2 C21 C22 96.5(7) . . . . ?
C2 N2 C21 C26 -88.3(7) . . . . ?
C2 N3 C31 C32 109.2(6) . . . . ?
C2 N3 C35 C34 -110.5(6) . . . . ?
C11 C12 C13 C14 1.1(10) . . . . ?
C12 C11 C16 C15 0.8(9) . . . . ?
C12 C11 C16 C18 -179.4(6) . . . . ?
C12 C13 C14 C15 -0.2(11) . . . . ?
C13 C14 C15 C16 -0.4(11) . . . . ?
C14 C15 C16 C11 0.1(10) . . . . ?
C14 C15 C16 C18 -179.7(7) . . . . ?
C16 C11 C12 C13 -1.4(9) . . . . ?
C16 C11 C12 C17 -179.9(6) . . . . ?
C17 C12 C13 C14 179.5(7) . . . . ?
C21 N2 C2 Ni1 -5.0(7) . . . . ?
C21 N2 C2 N3 171.7(5) . . . . ?
C21 C22 C23 C24 -1.0(10) . . . . ?
C22 C21 C26 C25 -8.1(9) . . . . ?
C22 C21 C26 C28 167.8(6) . . . . ?
C22 C23 C24 C25 -3.5(11) . . . . ?
C23 C24 C25 C26 2.4(12) . . . . ?
C24 C25 C26 C21 3.3(10) . . . . ?
C24 C25 C26 C28 -172.6(7) . . . . ?
C26 C21 C22 C23 6.9(9) . . . . ?
C26 C21 C22 C27 -170.4(6) . . . . ?
C27 C22 C23 C24 176.4(7) . . . . ?
C31 N3 C2 Ni1 174.7(4) . . . . ?
C31 N3 C2 N2 -1.9(8) . . . . ?
C31 N3 C35 C34 60.7(7) . . . . ?
C31 C32 C33 C34 -53.5(8) . . . . ?
C32 C33 C34 C35 52.6(8) . . . . ?
C33 C34 C35 N3 -55.0(7) . . . . ?
C35 N3 C2 Ni1 -15.2(7) . . . . ?
C35 N3 C2 N2 168.3(5) . . . . ?
C35 N3 C31 C32 -61.8(7) . . . . ?
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
-1.0005 0.0014 0.0008 -0.0167 0.0559 -0.0181
7.1652 21.4419 -12.4661 -0.5673 -0.1062 0.8166
9.2023 -17.3753 -15.1931 0.8017 0.1477 0.5792
1.5302 -26.7744 -5.1261 0.9582 0.2837 -0.0371
2.2191 27.4146 -1.4078 -0.8938 -0.2652 0.3616
-11.2722 -0.2269 19.7985 -0.2520 -0.0732 -0.9649
2.0001 0.9990 -2.0014 0.0065 -0.0476 0.1226
1.0005 -0.0014 -0.0008 0.0167 -0.0559 0.0181
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 0.005 0.073 0.676 9.9 0.0 ?
2 0.005 0.427 0.176 9.9 0.0 ?
3 -0.005 0.573 0.824 9.9 0.0 ?
4 -0.005 0.927 0.324 9.9 0.0 ?
