#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:14:42 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 265974 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/24/7242451.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_7242451
loop_
_publ_author_name
'Hasuo, Naohiro'
'Takahashi, Kiyonori'
'Hisaki, Ichiro'
'Kokado, Kenta'
'Nakamura, Takayoshi'
_publ_section_title
;
 Molecular motion of halogenated ethylammonium/[18]crown-6 supramolecular
 ions in nickel dithiolate magnetic crystals
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2756
_journal_page_last               2763
_journal_paper_doi               10.1039/D1CE00253H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C6 Ni S10, C2 H7 Cl N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Cl N Ni O6 S10'
_chemical_formula_weight         796.22
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-10
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                92.2792(18)
_cell_angle_beta                 112.126(2)
_cell_angle_gamma                96.0601(18)
_cell_formula_units_Z            2
_cell_length_a                   11.2107(3)
_cell_length_b                   12.3150(2)
_cell_length_c                   12.7451(3)
_cell_measurement_reflns_used    29610
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.9190
_cell_measurement_theta_min      2.1280
_cell_volume                     1614.84(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  18.00   0.50    0.24    --    5.18 -30.00 -11.44  120
  2  ω    -67.00  18.00   0.50    0.24    --    5.18 -32.00 -57.00  170
  3  ω    -63.00  18.00   0.50    0.24    --    5.18 -29.00  28.00  162
  4  ω    -64.00  19.00   0.50    0.24    --    5.18 -33.00 132.51  166
  5  ω    -40.00  18.00   0.50    0.24    --    5.18 -31.00 173.49  116
  6  ω    -69.00  18.00   0.50    0.24    --    5.18 -19.00  60.00  174
  7  ω    -10.00  78.00   0.50    0.24    --    5.18  57.00 -30.00  176
  8  ω     43.00  80.00   0.50    0.24    --    5.18  29.00-170.00   74
  9  ω    -63.00  19.00   0.50    0.24    --    5.18 -28.00-113.26  164
 10  ω    -17.00  28.00   0.50    0.24    --   -4.95 -99.00 150.00   90
 11  ω    -80.00 -25.00   0.50    0.24    --   -4.95 -29.00  28.00  110
 12  ω     37.00  66.00   0.50    0.24    --   -4.95  29.00-170.00   58
 13  ω    -17.00  12.00   0.50    0.24    --   -4.95  29.00-170.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0061888000
_diffrn_orient_matrix_UB_12      -0.0073309000
_diffrn_orient_matrix_UB_13      -0.0531169000
_diffrn_orient_matrix_UB_21      0.0668493000
_diffrn_orient_matrix_UB_22      0.0208920000
_diffrn_orient_matrix_UB_23      0.0260276000
_diffrn_orient_matrix_UB_31      0.0154338000
_diffrn_orient_matrix_UB_32      -0.0537563000
_diffrn_orient_matrix_UB_33      0.0117284000
_diffrn_radiation_collimation    0.3
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45358
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.014
_diffrn_reflns_theta_min         1.978
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0608
_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)+(0.0915P)²+0.2292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6983
_reflns_number_total             8651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           93k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_original_cell_volume        1614.83(7)
_cod_database_code               7242451
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         ClCNNiSHO
_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   0.791
_shelx_estimated_absorpt_t_min   0.452
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Others
 Sof(H7BC)=Sof(H7BD)=Sof(O4A)=Sof(O1A)=Sof(O6A)=Sof(H9BC)=Sof(H9BD)=Sof(O2A)=
 Sof(H3BC)=Sof(H3BD)=Sof(O3A)=Sof(O5A)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C7A)=
 Sof(H7AC)=Sof(H7AD)=Sof(C9A)=Sof(H9AC)=Sof(H9AD)=Sof(C12A)=Sof(H12C)=Sof(H12D)=
 Sof(C3A)=Sof(H3AC)=Sof(H3AD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(O3)=Sof(O6)=Sof(O1)=Sof(H9AA)=Sof(H9AB)=Sof(O2)=
 Sof(H3AA)=Sof(H3AB)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(O5)=
 Sof(O4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C11)=Sof(H11C)=Sof(H11D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C7(H7BC,H7BD), C7(H7AA,H7AB), C9(H9BC,H9BD), C9(H9AA,H9AB),
 C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C13(H13A,H13B), C11A(H11A,H11B),
 C5(H5A,H5B), C7A(H7AC,H7AD), C12(H12A,H12B), C10(H10A,H10B), C9A(H9AC,H9AD),
 C12A(H12C,H12D), C4(H4A,H4B), C14(H14A,H14B), C8(H8A,H8B), C6(H6A,H6B),
 C3A(H3AC,H3AD), C5A(H5AA,H5AB), C13A(H13C,H13D), C11(H11C,H11D), C6A(H6AA,
 H6AB), C14A(H14C,H14D)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_olex2_exptl_crystal_mounting_method loop
_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 4.420
_oxdiff_exptl_absorpt_empirical_full_min 0.405
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 0.34548(3) 0.89101(2) 1.01186(2) 0.02019(10) Uani 1 1 d . . . . .
S1 S 0.50591(5) 0.81058(5) 1.00747(5) 0.02375(14) Uani 1 1 d . . . . .
S4 S 0.41293(6) 0.89460(5) 0.66564(5) 0.02523(14) Uani 1 1 d . . . . .
S9 S 0.11356(6) 1.02893(5) 1.22145(6) 0.02665(14) Uani 1 1 d . . . . .
S8 S 0.30080(6) 0.90040(5) 1.36740(5) 0.02393(14) Uani 1 1 d . . . . .
S6 S 0.39674(6) 0.84120(4) 1.18222(5) 0.02295(14) Uani 1 1 d . . . . .
S2 S 0.29582(6) 0.93836(5) 0.84065(5) 0.02454(14) Uani 1 1 d . . . . .
S3 S 0.60051(6) 0.76998(5) 0.81704(6) 0.02876(15) Uani 1 1 d . . . . .
S7 S 0.19190(6) 0.97894(5) 1.02199(5) 0.02682(14) Uani 1 1 d . . . . .
S5 S 0.59276(7) 0.78908(6) 0.58295(6) 0.03366(16) Uani 1 1 d . . . . .
S10 S 0.12498(7) 1.00324(5) 1.45656(6) 0.03159(16) Uani 1 1 d . . . . .
Cl1 Cl 0.34018(8) 0.45202(6) 1.01407(7) 0.0553(2) Uani 1 1 d . . . . .
N1 N 0.16862(18) 0.50265(14) 0.75522(17) 0.0210(4) Uani 1 1 d . . . . .
H1A H 0.162935 0.519449 0.684740 0.025 Uiso 1 1 calc R U . . .
H1B H 0.089500 0.502365 0.759750 0.025 Uiso 1 1 calc R U . . .
H1C H 0.194810 0.435232 0.767949 0.025 Uiso 1 1 calc R U . . .
C19 C 0.2087(2) 0.96714(17) 1.1612(2) 0.0227(5) Uani 1 1 d . . . . .
C16 C 0.4075(2) 0.88311(17) 0.8002(2) 0.0220(4) Uani 1 1 d . . . . .
C18 C 0.2963(2) 0.90710(17) 1.2297(2) 0.0207(4) Uani 1 1 d . . . . .
C17 C 0.5386(2) 0.8167(2) 0.6835(2) 0.0260(5) Uani 1 1 d . . . . .
C1 C 0.2643(2) 0.58569(19) 0.8420(2) 0.0280(5) Uani 1 1 d . . . . .
H1D H 0.241208 0.659744 0.822430 0.034 Uiso 1 1 calc R U . . .
H1E H 0.351517 0.581548 0.840969 0.034 Uiso 1 1 calc R U . . .
C15 C 0.4978(2) 0.82606(18) 0.8723(2) 0.0233(5) Uani 1 1 d . . . . .
C20 C 0.1773(2) 0.97922(18) 1.3539(2) 0.0247(5) Uani 1 1 d . . . . .
C7 C 0.1454(3) 0.2024(2) 0.7981(3) 0.0416(7) Uani 1 1 d . . . . .
H7BC H 0.215043 0.213068 0.875026 0.050 Uiso 0.495(2) 1 calc R U P A 2
H7BD H 0.095679 0.129100 0.790248 0.050 Uiso 0.495(2) 1 calc R U P A 2
H7AA H 0.203156 0.151312 0.843255 0.050 Uiso 0.505(2) 1 calc R U P A 1
H7AB H 0.082078 0.159566 0.728342 0.050 Uiso 0.505(2) 1 calc R U P A 1
O4A O 0.0599(3) 0.2846(3) 0.7874(3) 0.0263(8) Uani 0.495(2) 1 d . . P A 2
O1A O 0.1420(3) 0.6620(3) 0.5905(3) 0.0246(7) Uani 0.495(2) 1 d . . P A 2
O3 O 0.2204(3) 0.2807(2) 0.7658(3) 0.0250(7) Uani 0.505(2) 1 d . . P A 1
O6 O -0.0008(3) 0.6542(3) 0.6359(3) 0.0275(8) Uani 0.505(2) 1 d . . P A 1
O6A O -0.0452(3) 0.6350(3) 0.6898(3) 0.0240(7) Uani 0.495(2) 1 d . . P A 2
O1 O 0.2165(3) 0.6170(3) 0.5831(3) 0.0250(7) Uani 0.505(2) 1 d . . P A 1
C9 C -0.0833(3) 0.3624(2) 0.8544(3) 0.0457(8) Uani 1 1 d . . . . .
H9BC H -0.109290 0.364910 0.920505 0.055 Uiso 0.495(2) 1 calc R U P A 2
H9BD H -0.160923 0.331701 0.787041 0.055 Uiso 0.495(2) 1 calc R U P A 2
H9AA H -0.144494 0.300284 0.858692 0.055 Uiso 0.505(2) 1 calc R U P A 1
H9AB H -0.029611 0.392701 0.933377 0.055 Uiso 0.505(2) 1 calc R U P A 1
C2 C 0.2688(3) 0.5692(2) 0.9598(3) 0.0396(6) Uani 1 1 d . . . . .
H2A H 0.179273 0.562210 0.958120 0.048 Uiso 1 1 calc R U . . .
H2B H 0.318802 0.634612 1.011346 0.048 Uiso 1 1 calc R U . . .
O2A O 0.2742(3) 0.4830(3) 0.5774(3) 0.0240(8) Uani 0.495(2) 1 d . . P A 2
O2 O 0.2974(4) 0.4101(3) 0.6181(3) 0.0260(8) Uani 0.505(2) 1 d . . P A 1
C3 C 0.2945(4) 0.5792(3) 0.5348(4) 0.0578(10) Uani 1 1 d . . . . .
H3AA H 0.354320 0.642436 0.530351 0.069 Uiso 0.505(2) 1 calc R U P A 1
H3AB H 0.239505 0.549933 0.455801 0.069 Uiso 0.505(2) 1 calc R U P A 1
H3BC H 0.313713 0.562872 0.466504 0.069 Uiso 0.495(2) 1 calc R U P A 2
H3BD H 0.373011 0.623025 0.591789 0.069 Uiso 0.495(2) 1 calc R U P A 2
O3A O 0.2694(3) 0.3102(3) 0.7133(3) 0.0238(7) Uani 0.495(2) 1 d . . P A 2
O5A O -0.0438(3) 0.4726(3) 0.8366(3) 0.0258(8) Uani 0.495(2) 1 d . . P A 2
C13 C 0.0245(8) 0.7083(6) 0.5489(7) 0.0321(15) Uani 0.505(2) 1 d . . P A 1
H13A H -0.057320 0.698981 0.480670 0.038 Uiso 0.505(2) 1 calc R U P A 1
H13B H 0.046067 0.787561 0.573682 0.038 Uiso 0.505(2) 1 calc R U P A 1
C11A C -0.1409(5) 0.5454(4) 0.8049(5) 0.0281(11) Uani 0.495(2) 1 d . . P A 2
H11A H -0.172080 0.556688 0.867124 0.034 Uiso 0.495(2) 1 calc R U P A 2
H11B H -0.215832 0.512860 0.736165 0.034 Uiso 0.495(2) 1 calc R U P A 2
C5 C 0.3219(6) 0.3065(4) 0.6284(6) 0.0285(11) Uani 0.505(2) 1 d . . P A 1
H5A H 0.417140 0.308264 0.653515 0.034 Uiso 0.505(2) 1 calc R U P A 1
H5B H 0.283134 0.268423 0.550914 0.034 Uiso 0.505(2) 1 calc R U P A 1
C7A C 0.2022(5) 0.2050(4) 0.7173(4) 0.0249(10) Uani 0.495(2) 1 d . . P A 2
H7AC H 0.133467 0.182445 0.641316 0.030 Uiso 0.495(2) 1 calc R U P A 2
H7AD H 0.264384 0.150533 0.733696 0.030 Uiso 0.495(2) 1 calc R U P A 2
C12 C -0.0568(5) 0.7015(4) 0.7067(5) 0.0300(11) Uani 0.505(2) 1 d . . P A 1
H12A H -0.105825 0.760871 0.669292 0.036 Uiso 0.505(2) 1 calc R U P A 1
H12B H 0.012124 0.733073 0.779713 0.036 Uiso 0.505(2) 1 calc R U P A 1
C10 C -0.1533(5) 0.4404(4) 0.8004(5) 0.0304(11) Uani 0.505(2) 1 d . . P A 1
H10A H -0.203749 0.465114 0.843952 0.036 Uiso 0.505(2) 1 calc R U P A 1
H10B H -0.215527 0.408974 0.724325 0.036 Uiso 0.505(2) 1 calc R U P A 1
C9A C 0.0096(5) 0.2919(4) 0.8733(5) 0.0281(11) Uani 0.495(2) 1 d . . P A 2
H9AC H -0.029122 0.217862 0.880302 0.034 Uiso 0.495(2) 1 calc R U P A 2
H9AD H 0.082169 0.316604 0.946599 0.034 Uiso 0.495(2) 1 calc R U P A 2
C12A C -0.0839(6) 0.6540(4) 0.7814(5) 0.0296(11) Uani 0.495(2) 1 d . . P A 2
H12C H -0.149514 0.705621 0.761798 0.035 Uiso 0.495(2) 1 calc R U P A 2
H12D H -0.008274 0.686444 0.849557 0.035 Uiso 0.495(2) 1 calc R U P A 2
C4 C 0.3703(5) 0.4972(4) 0.5886(5) 0.0299(11) Uani 0.505(2) 1 d . . P A 1
H4A H 0.442787 0.531160 0.658343 0.036 Uiso 0.505(2) 1 calc R U P A 1
H4B H 0.408340 0.466547 0.537079 0.036 Uiso 0.505(2) 1 calc R U P A 1
C14 C 0.1170(5) 0.6789(4) 0.5171(5) 0.0301(11) Uani 0.505(2) 1 d . . P A 1
H14A H 0.162208 0.747294 0.503979 0.036 Uiso 0.505(2) 1 calc R U P A 1
H14B H 0.072348 0.636834 0.441992 0.036 Uiso 0.505(2) 1 calc R U P A 1
C8 C 0.0771(5) 0.2398(4) 0.8608(5) 0.0332(12) Uani 0.505(2) 1 d . . P A 1
H8A H 0.139276 0.270891 0.936958 0.040 Uiso 0.505(2) 1 calc R U P A 1
H8B H 0.020524 0.177233 0.871085 0.040 Uiso 0.505(2) 1 calc R U P A 1
O5 O -0.0723(3) 0.5316(3) 0.7882(3) 0.0273(8) Uani 0.505(2) 1 d . . P A 1
O4 O 0.0004(4) 0.3202(3) 0.8065(3) 0.0282(8) Uani 0.505(2) 1 d . . P A 1
C6 C 0.2844(5) 0.2416(4) 0.6964(4) 0.0260(10) Uani 0.505(2) 1 d . . P A 1
H6A H 0.363185 0.213244 0.747931 0.031 Uiso 0.505(2) 1 calc R U P A 1
H6B H 0.226518 0.177810 0.647043 0.031 Uiso 0.505(2) 1 calc R U P A 1
C3A C 0.1932(5) 0.6445(4) 0.5047(5) 0.0280(11) Uani 0.495(2) 1 d . . P A 2
H3AC H 0.121875 0.609463 0.434756 0.034 Uiso 0.495(2) 1 calc R U P A 2
H3AD H 0.225270 0.716605 0.486747 0.034 Uiso 0.495(2) 1 calc R U P A 2
C5A C 0.3783(5) 0.4205(4) 0.6200(5) 0.0278(11) Uani 0.495(2) 1 d . . P A 2
H5AA H 0.394128 0.391132 0.553603 0.033 Uiso 0.495(2) 1 calc R U P A 2
H5AB H 0.456117 0.472453 0.665778 0.033 Uiso 0.495(2) 1 calc R U P A 2
C13A C -0.0163(5) 0.7350(4) 0.6455(5) 0.0272(10) Uani 0.495(2) 1 d . . P A 2
H13C H -0.099156 0.755808 0.591912 0.033 Uiso 0.495(2) 1 calc R U P A 2
H13D H 0.019785 0.793011 0.709332 0.033 Uiso 0.495(2) 1 calc R U P A 2
C11 C -0.1464(6) 0.6134(5) 0.7279(6) 0.0341(12) Uani 0.505(2) 1 d . . P A 1
H11C H -0.191071 0.645424 0.773170 0.041 Uiso 0.505(2) 1 calc R U P A 1
H11D H -0.213137 0.579844 0.654630 0.041 Uiso 0.505(2) 1 calc R U P A 1
C6A C 0.3749(5) 0.3350(4) 0.6839(6) 0.0263(11) Uani 0.495(2) 1 d . . P A 2
H6AA H 0.453033 0.348901 0.755319 0.032 Uiso 0.495(2) 1 calc R U P A 2
H6AB H 0.383844 0.268532 0.642585 0.032 Uiso 0.495(2) 1 calc R U P A 2
C14A C 0.0652(8) 0.7353(5) 0.5924(7) 0.0310(16) Uani 0.495(2) 1 d . . P A 2
H14C H 0.011526 0.741898 0.511582 0.037 Uiso 0.495(2) 1 calc R U P A 2
H14D H 0.123275 0.805522 0.620092 0.037 Uiso 0.495(2) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
S S 0.1246 0.1234 '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 S2 93.00(2) . . ?
S1 Ni1 S7 176.93(3) . . ?
S6 Ni1 S1 86.05(2) . . ?
S6 Ni1 S2 178.95(2) . . ?
S6 Ni1 S7 93.19(2) . . ?
S2 Ni1 S7 87.78(2) . . ?
C15 S1 Ni1 102.43(8) . . ?
C17 S4 C16 97.23(11) . . ?
C20 S9 C19 97.23(11) . . ?
C20 S8 C18 97.26(11) . . ?
C18 S6 Ni1 102.15(8) . . ?
C16 S2 Ni1 102.28(8) . . ?
C17 S3 C15 97.75(12) . . ?
C19 S7 Ni1 101.80(8) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
S7 C19 S9 122.71(14) . . ?
C18 C19 S9 116.10(18) . . ?
C18 C19 S7 121.19(17) . . ?
S2 C16 S4 122.85(14) . . ?
C15 C16 S4 115.99(17) . . ?
C15 C16 S2 121.15(18) . . ?
S6 C18 S8 122.32(14) . . ?
C19 C18 S8 116.27(17) . . ?
C19 C18 S6 121.41(18) . . ?
S3 C17 S4 113.16(13) . . ?
S5 C17 S4 123.57(16) . . ?
S5 C17 S3 123.28(15) . . ?
N1 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
N1 C1 C2 112.23(19) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.2 . . ?
C2 C1 H1E 109.2 . . ?
S1 C15 S3 123.10(14) . . ?
C16 C15 S1 121.07(17) . . ?
C16 C15 S3 115.82(18) . . ?
S9 C20 S8 113.10(13) . . ?
S10 C20 S9 123.55(13) . . ?
S10 C20 S8 123.34(15) . . ?
H7BC C7 H7BD 107.7 . . ?
H7AA C7 H7AB 107.2 . . ?
O4A C7 H7BC 108.9 . . ?
O4A C7 H7BD 108.9 . . ?
O3 C7 H7AA 108.0 . . ?
O3 C7 H7AB 108.0 . . ?
O3 C7 C8 117.2(3) . . ?
C7A C7 H7BC 108.9 . . ?
C7A C7 H7BD 108.9 . . ?
C7A C7 O4A 113.3(3) . . ?
C8 C7 H7AA 108.0 . . ?
C8 C7 H7AB 108.0 . . ?
C9A O4A C7 115.5(4) . . ?
C14A O1A C3A 126.0(5) . . ?
C7 O3 C6 116.6(3) . . ?
C12 O6 C13 124.0(4) . . ?
C12A O6A C13A 111.8(4) . . ?
C3 O1 C14 118.1(4) . . ?
H9BC C9 H9BD 107.5 . . ?
H9AA C9 H9AB 107.2 . . ?
O5A C9 H9BC 108.4 . . ?
O5A C9 H9BD 108.4 . . ?
C10 C9 H9AA 108.0 . . ?
C10 C9 H9AB 108.0 . . ?
C10 C9 O4 117.3(3) . . ?
C9A C9 H9BC 108.4 . . ?
C9A C9 H9BD 108.4 . . ?
C9A C9 O5A 115.4(3) . . ?
O4 C9 H9AA 108.0 . . ?
O4 C9 H9AB 108.0 . . ?
Cl1 C2 H2A 109.1 . . ?
Cl1 C2 H2B 109.1 . . ?
C1 C2 Cl1 112.7(2) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 O2A C5A 118.7(4) . . ?
C5 O2 C4 126.8(4) . . ?
O1 C3 H3AA 107.9 . . ?
O1 C3 H3AB 107.9 . . ?
O1 C3 C4 117.5(3) . . ?
O2A C3 H3BC 108.1 . . ?
O2A C3 H3BD 108.1 . . ?
O2A C3 C3A 116.9(3) . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.3 . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C3A C3 H3BC 108.1 . . ?
C3A C3 H3BD 108.1 . . ?
C6A O3A C7A 129.7(4) . . ?
C11A O5A C9 117.3(3) . . ?
O6 C13 H13A 107.5 . . ?
O6 C13 H13B 107.5 . . ?
H13A C13 H13B 107.0 . . ?
C14 C13 O6 119.1(6) . . ?
C14 C13 H13A 107.5 . . ?
C14 C13 H13B 107.5 . . ?
O5A C11A H11A 109.8 . . ?
O5A C11A H11B 109.8 . . ?
O5A C11A C12A 109.5(4) . . ?
H11A C11A H11B 108.2 . . ?
C12A C11A H11A 109.8 . . ?
C12A C11A H11B 109.8 . . ?
O2 C5 H5A 106.8 . . ?
O2 C5 H5B 106.8 . . ?
O2 C5 C6 122.3(4) . . ?
H5A C5 H5B 106.6 . . ?
C6 C5 H5A 106.8 . . ?
C6 C5 H5B 106.8 . . ?
C7 C7A O3A 114.7(4) . . ?
C7 C7A H7AC 108.6 . . ?
C7 C7A H7AD 108.6 . . ?
O3A C7A H7AC 108.6 . . ?
O3A C7A H7AD 108.6 . . ?
H7AC C7A H7AD 107.6 . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
O6 C12 C11 108.4(4) . . ?
H12A C12 H12B 108.4 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C9 C10 O5 111.4(4) . . ?
H10A C10 H10B 108.0 . . ?
O5 C10 H10A 109.3 . . ?
O5 C10 H10B 109.3 . . ?
O4A C9A H9AC 108.7 . . ?
O4A C9A H9AD 108.7 . . ?
C9 C9A O4A 114.3(5) . . ?
C9 C9A H9AC 108.7 . . ?
C9 C9A H9AD 108.7 . . ?
H9AC C9A H9AD 107.6 . . ?
O6A C12A C11A 108.0(4) . . ?
O6A C12A H12C 110.1 . . ?
O6A C12A H12D 110.1 . . ?
C11A C12A H12C 110.1 . . ?
C11A C12A H12D 110.1 . . ?
H12C C12A H12D 108.4 . . ?
O2 C4 H4A 109.0 . . ?
O2 C4 H4B 109.0 . . ?
C3 C4 O2 113.0(4) . . ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O1 C14 H14A 106.4 . . ?
O1 C14 H14B 106.4 . . ?
C13 C14 O1 123.9(6) . . ?
C13 C14 H14A 106.4 . . ?
C13 C14 H14B 106.4 . . ?
H14A C14 H14B 106.4 . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C7 C8 O4 111.7(4) . . ?
H8A C8 H8B 108.0 . . ?
O4 C8 H8A 109.3 . . ?
O4 C8 H8B 109.3 . . ?
C10 O5 C11 111.7(4) . . ?
C8 O4 C9 119.5(4) . . ?
O3 C6 H6A 106.8 . . ?
O3 C6 H6B 106.8 . . ?
C5 C6 O3 122.2(4) . . ?
C5 C6 H6A 106.8 . . ?
C5 C6 H6B 106.8 . . ?
H6A C6 H6B 106.6 . . ?
O1A C3A H3AC 108.6 . . ?
O1A C3A H3AD 108.6 . . ?
C3 C3A O1A 114.5(4) . . ?
C3 C3A H3AC 108.6 . . ?
C3 C3A H3AD 108.6 . . ?
H3AC C3A H3AD 107.6 . . ?
O2A C5A H5AA 106.7 . . ?
O2A C5A H5AB 106.7 . . ?
H5AA C5A H5AB 106.6 . . ?
C6A C5A O2A 122.4(5) . . ?
C6A C5A H5AA 106.7 . . ?
C6A C5A H5AB 106.7 . . ?
O6A C13A H13C 108.0 . . ?
O6A C13A H13D 108.0 . . ?
H13C C13A H13D 107.2 . . ?
C14A C13A O6A 117.3(5) . . ?
C14A C13A H13C 108.0 . . ?
C14A C13A H13D 108.0 . . ?
C12 C11 H11C 109.9 . . ?
C12 C11 H11D 109.9 . . ?
O5 C11 C12 109.1(4) . . ?
O5 C11 H11C 109.9 . . ?
O5 C11 H11D 109.9 . . ?
H11C C11 H11D 108.3 . . ?
O3A C6A H6AA 107.4 . . ?
O3A C6A H6AB 107.4 . . ?
C5A C6A O3A 119.8(4) . . ?
C5A C6A H6AA 107.4 . . ?
C5A C6A H6AB 107.4 . . ?
H6AA C6A H6AB 106.9 . . ?
O1A C14A C13A 128.7(6) . . ?
O1A C14A H14C 105.1 . . ?
O1A C14A H14D 105.1 . . ?
C13A C14A H14C 105.1 . . ?
C13A C14A H14D 105.1 . . ?
H14C C14A H14D 105.9 . . ?
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 2.1601(6) . ?
Ni1 S6 2.1590(6) . ?
Ni1 S2 2.1602(6) . ?
Ni1 S7 2.1688(6) . ?
S1 C15 1.709(2) . ?
S4 C16 1.749(2) . ?
S4 C17 1.738(2) . ?
S9 C19 1.746(2) . ?
S9 C20 1.733(3) . ?
S8 C18 1.742(2) . ?
S8 C20 1.734(2) . ?
S6 C18 1.720(2) . ?
S2 C16 1.713(2) . ?
S3 C17 1.727(3) . ?
S3 C15 1.744(2) . ?
S7 C19 1.726(2) . ?
S5 C17 1.650(2) . ?
S10 C20 1.651(2) . ?
Cl1 C2 1.763(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.485(3) . ?
C19 C18 1.354(3) . ?
C16 C15 1.365(3) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.505(4) . ?
C7 H7BC 0.9900 . ?
C7 H7BD 0.9900 . ?
C7 H7AA 0.9900 . ?
C7 H7AB 0.9900 . ?
C7 O4A 1.443(4) . ?
C7 O3 1.388(4) . ?
C7 C7A 1.399(6) . ?
C7 C8 1.394(6) . ?
O4A C9A 1.412(6) . ?
O1A C3A 1.433(6) . ?
O1A C14A 1.317(8) . ?
O3 C6 1.431(5) . ?
O6 C13 1.418(9) . ?
O6 C12 1.417(6) . ?
O6A C12A 1.410(6) . ?
O6A C13A 1.432(5) . ?
O1 C3 1.354(4) . ?
O1 C14 1.434(6) . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 O5A 1.436(4) . ?
C9 C10 1.348(6) . ?
C9 C9A 1.383(6) . ?
C9 O4 1.425(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O2A C3 1.356(4) . ?
O2A C5A 1.413(6) . ?
O2 C5 1.335(6) . ?
O2 C4 1.428(6) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.418(6) . ?
C3 C3A 1.404(6) . ?
O3A C7A 1.440(5) . ?
O3A C6A 1.378(6) . ?
O5A C11A 1.434(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.324(10) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A C12A 1.511(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.351(7) . ?
C7A H7AC 0.9900 . ?
C7A H7AD 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.502(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 O5 1.420(6) . ?
C9A H9AC 0.9900 . ?
C9A H9AD 0.9900 . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 O4 1.409(6) . ?
O5 C11 1.433(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C3A H3AC 0.9900 . ?
C3A H3AD 0.9900 . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C5A C6A 1.362(7) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A C14A 1.326(9) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
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 C15 S3 -176.58(12) . . . . ?
Ni1 S1 C15 C16 2.6(2) . . . . ?
Ni1 S6 C18 S8 -177.34(12) . . . . ?
Ni1 S6 C18 C19 2.8(2) . . . . ?
Ni1 S2 C16 S4 179.33(12) . . . . ?
Ni1 S2 C16 C15 -0.1(2) . . . . ?
Ni1 S7 C19 S9 176.97(12) . . . . ?
Ni1 S7 C19 C18 -4.1(2) . . . . ?
S4 C16 C15 S1 178.72(12) . . . . ?
S4 C16 C15 S3 -2.0(2) . . . . ?
S9 C19 C18 S8 0.1(3) . . . . ?
S9 C19 C18 S6 179.91(12) . . . . ?
S2 C16 C15 S1 -1.8(3) . . . . ?
S2 C16 C15 S3 177.45(12) . . . . ?
S7 C19 C18 S8 -178.91(12) . . . . ?
S7 C19 C18 S6 0.9(3) . . . . ?
N1 C1 C2 Cl1 70.8(3) . . . . ?
C19 S9 C20 S8 1.85(15) . . . . ?
C19 S9 C20 S10 -177.56(16) . . . . ?
C16 S4 C17 S3 -1.75(15) . . . . ?
C16 S4 C17 S5 177.75(16) . . . . ?
C18 S8 C20 S9 -1.82(15) . . . . ?
C18 S8 C20 S10 177.60(16) . . . . ?
C17 S4 C16 S2 -177.17(15) . . . . ?
C17 S4 C16 C15 2.3(2) . . . . ?
C17 S3 C15 S1 179.92(15) . . . . ?
C17 S3 C15 C16 0.7(2) . . . . ?
C15 S3 C17 S4 0.89(15) . . . . ?
C15 S3 C17 S5 -178.61(16) . . . . ?
C20 S9 C19 S7 177.79(15) . . . . ?
C20 S9 C19 C18 -1.2(2) . . . . ?
C20 S8 C18 S6 -178.76(15) . . . . ?
C20 S8 C18 C19 1.1(2) . . . . ?
C7 O4A C9A C9 -173.0(3) . . . . ?
C7 O3 C6 C5 156.9(5) . . . . ?
C7 C8 O4 C9 175.7(3) . . . . ?
O4A C7 C7A O3A 54.0(5) . . . . ?
O3 C7 C8 O4 52.9(5) . . . . ?
O6 C13 C14 O1 -17.1(10) . . . . ?
O6 C12 C11 O5 63.1(6) . . . . ?
O6A C13A C14A O1A -12.9(11) . . . . ?
O1 C3 C4 O2 47.3(6) . . . . ?
C9 O5A C11A C12A -175.7(4) . . . . ?
C9 C10 O5 C11 178.3(4) . . . . ?
O2A C3 C3A O1A 49.4(6) . . . . ?
O2A C5A C6A O3A -2.9(9) . . . . ?
O2 C5 C6 O3 -2.6(9) . . . . ?
C3 O1 C14 C13 171.1(5) . . . . ?
C3 O2A C5A C6A 166.8(5) . . . . ?
O5A C9 C9A O4A -55.4(5) . . . . ?
O5A C11A C12A O6A 61.5(6) . . . . ?
C13 O6 C12 C11 142.6(6) . . . . ?
C5 O2 C4 C3 152.8(5) . . . . ?
C7A C7 O4A C9A -174.4(4) . . . . ?
C7A O3A C6A C5A 139.6(5) . . . . ?
C12 O6 C13 C14 154.8(6) . . . . ?
C10 C9 O4 C8 179.1(4) . . . . ?
C10 O5 C11 C12 -173.9(4) . . . . ?
C9A C9 O5A C11A 173.6(4) . . . . ?
C12A O6A C13A C14A 154.9(6) . . . . ?
C4 O2 C5 C6 153.5(6) . . . . ?
C14 O1 C3 C4 -165.0(4) . . . . ?
C8 C7 O3 C6 -176.8(4) . . . . ?
O4 C9 C10 O5 -56.3(5) . . . . ?
C3A O1A C14A C13A 156.9(7) . . . . ?
C5A O2A C3 C3A -173.3(4) . . . . ?
C13A O6A C12A C11A 167.3(4) . . . . ?
C6A O3A C7A C7 150.3(5) . . . . ?
C14A O1A C3A C3 166.5(5) . . . . ?
