#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:14:42 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 265974 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/24/7242447.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_7242447
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             2020-11-24
_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                92.239(2)
_cell_angle_beta                 111.956(2)
_cell_angle_gamma                96.066(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2193(3)
_cell_length_b                   12.3191(2)
_cell_length_c                   12.7473(3)
_cell_measurement_reflns_used    28482
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.9490
_cell_measurement_theta_min      2.2900
_cell_volume                     1618.98(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 n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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      9.00  77.00   0.50    0.26    --    5.18  51.00 -78.00  136
  2  ω    -21.00  19.00   0.50    0.26    --    5.18 -28.00-171.52   80
  3  ω    -51.00 -25.00   0.50    0.26    --    5.18 -28.00-171.52   52
  4  ω    -64.00  18.00   0.50    0.26    --    5.18 -23.00 -77.67  164
  5  ω    -68.00  19.00   0.50    0.26    --    5.18 -28.00  13.21  174
  6  ω    -69.00  18.00   0.50    0.26    --    5.18 -19.00  60.00  174
  7  ω    -67.00  19.00   0.50    0.26    --    5.18 -51.00 135.00  172
  8  ω    -66.00  18.00   0.50    0.26    --    5.18 -19.00 150.00  168
  9  ω    -79.00   8.00   0.50    0.26    --   -5.03 -19.00 -30.00  174
 10  ω    -18.00  55.00   0.50    0.26    --   -5.03  51.00 -78.00  146
 11  ω      5.00  39.00   0.50    0.26    --    5.18 -99.00 -90.00   68
 12  ω    -18.00  28.00   0.50    0.26    --   -5.03 -99.00 120.00   92
 13  ω    -72.00 -35.00   0.50    0.26    --   -5.03 -51.00 135.00   74
;
_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      -0.0542762000
_diffrn_orient_matrix_UB_12      -0.0318274000
_diffrn_orient_matrix_UB_13      0.0042190000
_diffrn_orient_matrix_UB_21      -0.0230247000
_diffrn_orient_matrix_UB_22      -0.0172823000
_diffrn_orient_matrix_UB_23      -0.0586853000
_diffrn_orient_matrix_UB_31      0.0353571000
_diffrn_orient_matrix_UB_32      -0.0454469000
_diffrn_orient_matrix_UB_33      0.0128022000
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            37298
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.974
_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    1.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42668
_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    1.633
_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         0.839
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0848P)²+0.5937P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5734
_reflns_number_total             6613
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           113k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242447
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H30NO6NiS10Cl
_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   0.453
_reflns_odcompleteness_completeness 99.88
_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 0.414
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 0.34546(3) 0.89088(2) 1.01193(3) 0.02122(12) Uani 1 1 d . . . . .
S1 S 0.50583(6) 0.81062(5) 1.00748(6) 0.02575(16) Uani 1 1 d . . . . .
S4 S 0.41266(7) 0.89401(5) 0.66579(6) 0.02726(16) Uani 1 1 d . . . . .
S9 S 0.11354(6) 1.02865(5) 1.22144(6) 0.02823(17) Uani 1 1 d . . . . .
S8 S 0.30080(6) 0.90052(5) 1.36729(6) 0.02597(16) Uani 1 1 d . . . . .
S6 S 0.39688(6) 0.84143(5) 1.18225(6) 0.02478(16) Uani 1 1 d . . . . .
S2 S 0.29539(6) 0.93766(5) 0.84066(6) 0.02630(16) Uani 1 1 d . . . . .
S3 S 0.60048(7) 0.77015(6) 0.81729(6) 0.03081(17) Uani 1 1 d . . . . .
S7 S 0.19192(7) 0.97869(5) 1.02215(6) 0.02862(17) Uani 1 1 d . . . . .
S5 S 0.59259(7) 0.78886(6) 0.58339(7) 0.03641(19) Uani 1 1 d . . . . .
S10 S 0.12509(7) 1.00323(6) 1.45628(6) 0.03392(18) Uani 1 1 d . . . . .
Cl1 Cl 0.33929(10) 0.45257(7) 1.01425(8) 0.0595(3) Uani 1 1 d . . . . .
N1 N 0.1686(2) 0.50270(16) 0.75536(19) 0.0229(4) Uani 1 1 d . . . . .
H1A H 0.164307 0.518221 0.684933 0.027 Uiso 1 1 calc R U . . .
H1B H 0.089308 0.504083 0.759079 0.027 Uiso 1 1 calc R U . . .
H1C H 0.193305 0.434977 0.769266 0.027 Uiso 1 1 calc R U . . .
C19 C 0.2087(2) 0.96693(19) 1.1608(2) 0.0239(5) Uani 1 1 d . . . . .
C16 C 0.4071(2) 0.88283(19) 0.7999(2) 0.0235(5) Uani 1 1 d . . . . .
C18 C 0.2964(2) 0.90711(19) 1.2299(2) 0.0220(5) Uani 1 1 d . . . . .
C17 C 0.5386(3) 0.8166(2) 0.6840(2) 0.0279(5) Uani 1 1 d . . . . .
C1 C 0.2643(3) 0.5854(2) 0.8413(2) 0.0304(6) Uani 1 1 d . . . . .
H1D H 0.241699 0.659492 0.821496 0.036 Uiso 1 1 calc R U . . .
H1E H 0.351225 0.580705 0.839877 0.036 Uiso 1 1 calc R U . . .
C15 C 0.4973(2) 0.8255(2) 0.8723(2) 0.0240(5) Uani 1 1 d . . . . .
C20 C 0.1771(3) 0.9792(2) 1.3535(2) 0.0269(5) Uani 1 1 d . . . . .
C7 C 0.1461(3) 0.2027(2) 0.7988(3) 0.0457(8) Uani 1 1 d . . . . .
H7BC H 0.215789 0.214038 0.875466 0.055 Uiso 0.498(3) 1 calc R U P A 2
H7BD H 0.097017 0.129328 0.791991 0.055 Uiso 0.498(3) 1 calc R U P A 2
H7AA H 0.204246 0.151927 0.843903 0.055 Uiso 0.502(3) 1 calc R U P A 1
H7AB H 0.082879 0.159502 0.729614 0.055 Uiso 0.502(3) 1 calc R U P A 1
O4A O 0.0599(4) 0.2847(3) 0.7880(3) 0.0278(9) Uani 0.498(3) 1 d . . P A 2
O1A O 0.1428(4) 0.6613(3) 0.5906(4) 0.0278(9) Uani 0.498(3) 1 d . . P A 2
O3 O 0.2202(3) 0.2807(3) 0.7655(3) 0.0267(9) Uani 0.502(3) 1 d . . P A 1
O6 O -0.0010(4) 0.6541(3) 0.6359(4) 0.0292(9) Uani 0.502(3) 1 d . . P A 1
O6A O -0.0447(4) 0.6348(3) 0.6895(4) 0.0283(9) Uani 0.498(3) 1 d . . P A 2
O1 O 0.2160(4) 0.6168(3) 0.5827(3) 0.0268(9) Uani 0.502(3) 1 d . . P A 1
C9 C -0.0826(4) 0.3620(2) 0.8552(4) 0.0491(9) Uani 1 1 d . . . . .
H9BC H -0.108406 0.364497 0.921400 0.059 Uiso 0.498(3) 1 calc R U P A 2
H9BD H -0.160158 0.330970 0.788202 0.059 Uiso 0.498(3) 1 calc R U P A 2
H9AA H -0.143336 0.299686 0.859872 0.059 Uiso 0.502(3) 1 calc R U P A 1
H9AB H -0.028985 0.392484 0.933803 0.059 Uiso 0.502(3) 1 calc R U P A 1
C2 C 0.2691(4) 0.5697(2) 0.9594(3) 0.0442(8) Uani 1 1 d . . . . .
H2A H 0.179897 0.563489 0.958247 0.053 Uiso 1 1 calc R U . . .
H2B H 0.319585 0.635097 1.010449 0.053 Uiso 1 1 calc R U . . .
O2A O 0.2744(4) 0.4828(3) 0.5778(3) 0.0259(9) Uani 0.498(3) 1 d . . P A 2
O2 O 0.2965(4) 0.4107(3) 0.6177(3) 0.0289(9) Uani 0.502(3) 1 d . . P A 1
C3 C 0.2942(4) 0.5790(3) 0.5348(4) 0.0616(12) Uani 1 1 d . . . . .
H3AA H 0.353930 0.642178 0.530225 0.074 Uiso 0.502(3) 1 calc R U P A 1
H3AB H 0.239603 0.549670 0.455945 0.074 Uiso 0.502(3) 1 calc R U P A 1
H3BC H 0.313301 0.562530 0.466440 0.074 Uiso 0.498(3) 1 calc R U P A 2
H3BD H 0.372659 0.622744 0.591398 0.074 Uiso 0.498(3) 1 calc R U P A 2
O3A O 0.2690(4) 0.3097(3) 0.7134(3) 0.0271(9) Uani 0.498(3) 1 d . . P A 2
O5A O -0.0438(4) 0.4730(3) 0.8365(4) 0.0292(9) Uani 0.498(3) 1 d . . P A 2
C13 C 0.0252(10) 0.7083(8) 0.5488(8) 0.036(2) Uani 0.502(3) 1 d . . P A 1
H13A H -0.056589 0.700044 0.480940 0.043 Uiso 0.502(3) 1 calc R U P A 1
H13B H 0.047806 0.787392 0.574037 0.043 Uiso 0.502(3) 1 calc R U P A 1
C11A C -0.1408(6) 0.5452(5) 0.8043(5) 0.0325(13) Uani 0.498(3) 1 d . . P A 2
H11A H -0.172992 0.556178 0.865956 0.039 Uiso 0.498(3) 1 calc R U P A 2
H11B H -0.214757 0.512786 0.735278 0.039 Uiso 0.498(3) 1 calc R U P A 2
C5 C 0.3219(7) 0.3052(5) 0.6287(7) 0.0319(14) Uani 0.502(3) 1 d . . P A 1
H5A H 0.283954 0.266881 0.551491 0.038 Uiso 0.502(3) 1 calc R U P A 1
H5B H 0.417056 0.307167 0.654316 0.038 Uiso 0.502(3) 1 calc R U P A 1
C7A C 0.2025(6) 0.2046(4) 0.7179(5) 0.0290(12) Uani 0.498(3) 1 d . . P A 2
H7AC H 0.133865 0.181694 0.642215 0.035 Uiso 0.498(3) 1 calc R U P A 2
H7AD H 0.264760 0.150289 0.734457 0.035 Uiso 0.498(3) 1 calc R U P A 2
C12 C -0.0577(6) 0.7011(6) 0.7069(6) 0.0337(14) Uani 0.502(3) 1 d . . P A 1
H12A H -0.107129 0.760089 0.669222 0.040 Uiso 0.502(3) 1 calc R U P A 1
H12B H 0.010878 0.733111 0.779522 0.040 Uiso 0.502(3) 1 calc R U P A 1
C10 C -0.1533(5) 0.4399(5) 0.8007(5) 0.0333(13) Uani 0.502(3) 1 d . . P A 1
H10A H -0.204153 0.464503 0.843924 0.040 Uiso 0.502(3) 1 calc R U P A 1
H10B H -0.214883 0.408500 0.724626 0.040 Uiso 0.502(3) 1 calc R U P A 1
C9A C 0.0093(6) 0.2924(5) 0.8737(6) 0.0315(13) Uani 0.498(3) 1 d . . P A 2
H9AC H -0.029145 0.218421 0.881074 0.038 Uiso 0.498(3) 1 calc R U P A 2
H9AD H 0.081653 0.317294 0.946723 0.038 Uiso 0.498(3) 1 calc R U P A 2
C12A C -0.0835(7) 0.6536(5) 0.7816(6) 0.0332(14) Uani 0.498(3) 1 d . . P A 2
H12C H -0.148720 0.705482 0.762569 0.040 Uiso 0.498(3) 1 calc R U P A 2
H12D H -0.007997 0.685500 0.849816 0.040 Uiso 0.498(3) 1 calc R U P A 2
C4 C 0.3696(6) 0.4975(5) 0.5882(5) 0.0323(13) Uani 0.502(3) 1 d . . P A 1
H4A H 0.441945 0.531336 0.657713 0.039 Uiso 0.502(3) 1 calc R U P A 1
H4B H 0.407562 0.466706 0.536599 0.039 Uiso 0.502(3) 1 calc R U P A 1
C14 C 0.1155(6) 0.6787(5) 0.5164(6) 0.0335(13) Uani 0.502(3) 1 d . . P A 1
H14A H 0.160129 0.746762 0.501971 0.040 Uiso 0.502(3) 1 calc R U P A 1
H14B H 0.070214 0.636007 0.441908 0.040 Uiso 0.502(3) 1 calc R U P A 1
C8 C 0.0782(6) 0.2393(5) 0.8617(6) 0.0376(14) Uani 0.502(3) 1 d . . P A 1
H8A H 0.140185 0.270522 0.937673 0.045 Uiso 0.502(3) 1 calc R U P A 1
H8B H 0.021972 0.176626 0.872175 0.045 Uiso 0.502(3) 1 calc R U P A 1
O5 O -0.0718(4) 0.5315(4) 0.7887(4) 0.0311(9) Uani 0.502(3) 1 d . . P A 1
O4 O 0.0006(4) 0.3204(3) 0.8066(4) 0.0315(9) Uani 0.502(3) 1 d . . P A 1
C6 C 0.2839(5) 0.2417(5) 0.6961(5) 0.0289(12) Uani 0.502(3) 1 d . . P A 1
H6A H 0.362092 0.212786 0.747566 0.035 Uiso 0.502(3) 1 calc R U P A 1
H6B H 0.225790 0.178066 0.646911 0.035 Uiso 0.502(3) 1 calc R U P A 1
C3A C 0.1934(6) 0.6446(5) 0.5048(6) 0.0331(13) Uani 0.498(3) 1 d . . P A 2
H3AC H 0.122206 0.610033 0.434929 0.040 Uiso 0.498(3) 1 calc R U P A 2
H3AD H 0.225740 0.716832 0.487322 0.040 Uiso 0.498(3) 1 calc R U P A 2
C5A C 0.3774(6) 0.4197(5) 0.6202(5) 0.0314(13) Uani 0.498(3) 1 d . . P A 2
H5AA H 0.393467 0.390375 0.553982 0.038 Uiso 0.498(3) 1 calc R U P A 2
H5AB H 0.455221 0.471317 0.666131 0.038 Uiso 0.498(3) 1 calc R U P A 2
C13A C -0.0154(6) 0.7343(5) 0.6453(5) 0.0316(13) Uani 0.498(3) 1 d . . P A 2
H13C H -0.097899 0.755512 0.592210 0.038 Uiso 0.498(3) 1 calc R U P A 2
H13D H 0.021211 0.792095 0.709094 0.038 Uiso 0.498(3) 1 calc R U P A 2
C11 C -0.1456(7) 0.6136(6) 0.7285(7) 0.0373(15) Uani 0.502(3) 1 d . . P A 1
H11C H -0.190208 0.645611 0.773834 0.045 Uiso 0.502(3) 1 calc R U P A 1
H11D H -0.212265 0.580068 0.655466 0.045 Uiso 0.502(3) 1 calc R U P A 1
C6A C 0.3733(6) 0.3354(5) 0.6830(7) 0.0304(14) Uani 0.498(3) 1 d . . P A 2
H6AA H 0.451489 0.348871 0.753944 0.036 Uiso 0.498(3) 1 calc R U P A 2
H6AB H 0.381982 0.269068 0.641287 0.036 Uiso 0.498(3) 1 calc R U P A 2
C14A C 0.0646(10) 0.7342(7) 0.5924(9) 0.034(2) Uani 0.498(3) 1 d . . P A 2
H14C H 0.121744 0.804844 0.618815 0.040 Uiso 0.498(3) 1 calc R U P A 2
H14D H 0.010428 0.739769 0.511649 0.040 Uiso 0.498(3) 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 S7 176.92(3) . . ?
S6 Ni1 S1 85.97(2) . . ?
S6 Ni1 S2 178.91(3) . . ?
S6 Ni1 S7 93.25(3) . . ?
S2 Ni1 S1 93.09(3) . . ?
S2 Ni1 S7 87.72(3) . . ?
C15 S1 Ni1 102.37(9) . . ?
C17 S4 C16 97.19(13) . . ?
C20 S9 C19 97.32(12) . . ?
C20 S8 C18 97.10(12) . . ?
C18 S6 Ni1 102.16(9) . . ?
C16 S2 Ni1 102.38(9) . . ?
C17 S3 C15 97.68(13) . . ?
C19 S7 Ni1 101.71(9) . . ?
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 122.75(15) . . ?
C18 C19 S9 115.7(2) . . ?
C18 C19 S7 121.54(19) . . ?
S2 C16 S4 123.08(16) . . ?
C15 C16 S4 116.02(19) . . ?
C15 C16 S2 120.9(2) . . ?
S6 C18 S8 122.35(15) . . ?
C19 C18 S8 116.57(19) . . ?
C19 C18 S6 121.1(2) . . ?
S3 C17 S4 113.33(15) . . ?
S5 C17 S4 123.41(17) . . ?
S5 C17 S3 123.25(16) . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 H1E 109.1 . . ?
N1 C1 C2 112.3(2) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.1 . . ?
C2 C1 H1E 109.1 . . ?
S1 C15 S3 123.06(16) . . ?
C16 C15 S1 121.19(19) . . ?
C16 C15 S3 115.7(2) . . ?
S9 C20 S8 113.28(15) . . ?
S10 C20 S9 123.61(15) . . ?
S10 C20 S8 123.11(17) . . ?
H7BC C7 H7BD 107.7 . . ?
H7AA C7 H7AB 107.2 . . ?
O4A C7 H7BC 108.8 . . ?
O4A C7 H7BD 108.8 . . ?
O3 C7 H7AA 107.9 . . ?
O3 C7 H7AB 107.9 . . ?
O3 C7 C8 117.7(4) . . ?
C7A C7 H7BC 108.8 . . ?
C7A C7 H7BD 108.8 . . ?
C7A C7 O4A 113.6(3) . . ?
C8 C7 H7AA 107.9 . . ?
C8 C7 H7AB 107.9 . . ?
C9A O4A C7 115.8(4) . . ?
C14A O1A C3A 125.8(6) . . ?
C7 O3 C6 116.8(4) . . ?
C12 O6 C13 124.2(6) . . ?
C12A O6A C13A 112.1(5) . . ?
C3 O1 C14 118.5(5) . . ?
H9BC C9 H9BD 107.4 . . ?
H9AA C9 H9AB 107.3 . . ?
O5A C9 H9BC 108.4 . . ?
O5A C9 H9BD 108.4 . . ?
C10 C9 H9AA 108.1 . . ?
C10 C9 H9AB 108.1 . . ?
C10 C9 O4 116.9(4) . . ?
C9A C9 H9BC 108.4 . . ?
C9A C9 H9BD 108.4 . . ?
C9A C9 O5A 115.6(3) . . ?
O4 C9 H9AA 108.1 . . ?
O4 C9 H9AB 108.1 . . ?
Cl1 C2 H2A 109.0 . . ?
Cl1 C2 H2B 109.0 . . ?
C1 C2 Cl1 112.9(2) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C3 O2A C5A 119.3(4) . . ?
C5 O2 C4 126.4(5) . . ?
O1 C3 H3AA 107.9 . . ?
O1 C3 H3AB 107.9 . . ?
O1 C3 C4 117.8(4) . . ?
O2A C3 H3BC 108.0 . . ?
O2A C3 H3BD 108.0 . . ?
O2A C3 C3A 117.3(4) . . ?
H3AA C3 H3AB 107.2 . . ?
H3BC C3 H3BD 107.2 . . ?
C4 C3 H3AA 107.9 . . ?
C4 C3 H3AB 107.9 . . ?
C3A C3 H3BC 108.0 . . ?
C3A C3 H3BD 108.0 . . ?
C6A O3A C7A 130.0(5) . . ?
C11A O5A C9 117.6(4) . . ?
O6 C13 H13A 107.5 . . ?
O6 C13 H13B 107.5 . . ?
H13A C13 H13B 107.0 . . ?
C14 C13 O6 119.4(8) . . ?
C14 C13 H13A 107.5 . . ?
C14 C13 H13B 107.5 . . ?
O5A C11A H11A 109.8 . . ?
O5A C11A H11B 109.8 . . ?
O5A C11A C12A 109.4(5) . . ?
H11A C11A H11B 108.2 . . ?
C12A C11A H11A 109.8 . . ?
C12A C11A H11B 109.8 . . ?
O2 C5 H5A 106.9 . . ?
O2 C5 H5B 106.9 . . ?
H5A C5 H5B 106.7 . . ?
C6 C5 O2 121.8(5) . . ?
C6 C5 H5A 106.9 . . ?
C6 C5 H5B 106.9 . . ?
C7 C7A O3A 114.3(4) . . ?
C7 C7A H7AC 108.7 . . ?
C7 C7A H7AD 108.7 . . ?
O3A C7A H7AC 108.7 . . ?
O3A C7A H7AD 108.7 . . ?
H7AC C7A H7AD 107.6 . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
O6 C12 C11 108.5(6) . . ?
H12A C12 H12B 108.4 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C9 C10 O5 111.1(5) . . ?
H10A C10 H10B 108.0 . . ?
O5 C10 H10A 109.4 . . ?
O5 C10 H10B 109.4 . . ?
O4A C9A H9AC 108.6 . . ?
O4A C9A H9AD 108.6 . . ?
C9 C9A O4A 114.7(6) . . ?
C9 C9A H9AC 108.6 . . ?
C9 C9A H9AD 108.6 . . ?
H9AC C9A H9AD 107.6 . . ?
O6A C12A C11A 107.8(5) . . ?
O6A C12A H12C 110.1 . . ?
O6A C12A H12D 110.1 . . ?
C11A C12A H12C 110.1 . . ?
C11A C12A H12D 110.1 . . ?
H12C C12A H12D 108.5 . . ?
O2 C4 H4A 109.1 . . ?
O2 C4 H4B 109.1 . . ?
C3 C4 O2 112.7(5) . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
O1 C14 H14A 106.4 . . ?
O1 C14 H14B 106.4 . . ?
C13 C14 O1 123.8(7) . . ?
C13 C14 H14A 106.4 . . ?
C13 C14 H14B 106.4 . . ?
H14A C14 H14B 106.5 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C7 C8 O4 111.2(5) . . ?
H8A C8 H8B 108.0 . . ?
O4 C8 H8A 109.4 . . ?
O4 C8 H8B 109.4 . . ?
C10 O5 C11 111.7(5) . . ?
C9 O4 C8 118.9(5) . . ?
O3 C6 H6A 106.6 . . ?
O3 C6 H6B 106.6 . . ?
C5 C6 O3 122.7(6) . . ?
C5 C6 H6A 106.6 . . ?
C5 C6 H6B 106.6 . . ?
H6A C6 H6B 106.6 . . ?
O1A C3A H3AC 108.8 . . ?
O1A C3A H3AD 108.8 . . ?
C3 C3A O1A 114.0(5) . . ?
C3 C3A H3AC 108.8 . . ?
C3 C3A H3AD 108.8 . . ?
H3AC C3A H3AD 107.6 . . ?
O2A C5A H5AA 106.7 . . ?
O2A C5A H5AB 106.7 . . ?
H5AA C5A H5AB 106.6 . . ?
C6A C5A O2A 122.6(6) . . ?
C6A C5A H5AA 106.7 . . ?
C6A C5A H5AB 106.7 . . ?
O6A C13A H13C 107.9 . . ?
O6A C13A H13D 107.9 . . ?
H13C C13A H13D 107.2 . . ?
C14A C13A O6A 117.5(6) . . ?
C14A C13A H13C 107.9 . . ?
C14A C13A H13D 107.9 . . ?
C12 C11 H11C 109.8 . . ?
C12 C11 H11D 109.8 . . ?
O5 C11 C12 109.6(5) . . ?
O5 C11 H11C 109.8 . . ?
O5 C11 H11D 109.8 . . ?
H11C C11 H11D 108.2 . . ?
O3A C6A H6AA 107.1 . . ?
O3A C6A H6AB 107.1 . . ?
C5A C6A O3A 120.8(5) . . ?
C5A C6A H6AA 107.1 . . ?
C5A C6A H6AB 107.1 . . ?
H6AA C6A H6AB 106.8 . . ?
O1A C14A H14C 105.0 . . ?
O1A C14A H14D 105.0 . . ?
C13A C14A O1A 129.2(8) . . ?
C13A C14A H14C 105.0 . . ?
C13A C14A H14D 105.0 . . ?
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(7) . ?
Ni1 S6 2.1584(7) . ?
Ni1 S2 2.1596(7) . ?
Ni1 S7 2.1691(7) . ?
S1 C15 1.708(3) . ?
S4 C16 1.744(3) . ?
S4 C17 1.737(3) . ?
S9 C19 1.748(2) . ?
S9 C20 1.729(3) . ?
S8 C18 1.739(3) . ?
S8 C20 1.735(2) . ?
S6 C18 1.721(2) . ?
S2 C16 1.713(3) . ?
S3 C17 1.725(3) . ?
S3 C15 1.741(2) . ?
S7 C19 1.720(3) . ?
S5 C17 1.649(3) . ?
S10 C20 1.650(3) . ?
Cl1 C2 1.760(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.481(3) . ?
C19 C18 1.357(4) . ?
C16 C15 1.371(4) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.507(4) . ?
C7 H7BC 0.9900 . ?
C7 H7BD 0.9900 . ?
C7 H7AA 0.9900 . ?
C7 H7AB 0.9900 . ?
C7 O4A 1.447(5) . ?
C7 O3 1.386(4) . ?
C7 C7A 1.397(6) . ?
C7 C8 1.388(7) . ?
O4A C9A 1.410(7) . ?
O1A C3A 1.424(7) . ?
O1A C14A 1.325(10) . ?
O3 C6 1.427(6) . ?
O6 C13 1.424(10) . ?
O6 C12 1.423(7) . ?
O6A C12A 1.416(7) . ?
O6A C13A 1.426(7) . ?
O1 C3 1.351(5) . ?
O1 C14 1.444(7) . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 O5A 1.447(5) . ?
C9 C10 1.355(7) . ?
C9 C9A 1.369(7) . ?
C9 O4 1.424(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O2A C3 1.357(5) . ?
O2A C5A 1.410(7) . ?
O2 C5 1.361(7) . ?
O2 C4 1.427(7) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.411(7) . ?
C3 C3A 1.405(7) . ?
O3A C7A 1.439(6) . ?
O3A C6A 1.375(7) . ?
O5A C11A 1.430(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.307(13) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A C12A 1.505(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.338(8) . ?
C7A H7AC 0.9900 . ?
C7A H7AD 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.487(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 O5 1.425(7) . ?
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 1.425(7) . ?
O5 C11 1.436(7) . ?
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 1.343(9) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A C14A 1.309(12) . ?
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 -177.02(13) . . . . ?
Ni1 S1 C15 C16 3.0(2) . . . . ?
Ni1 S6 C18 S8 -177.39(13) . . . . ?
Ni1 S6 C18 C19 2.8(2) . . . . ?
Ni1 S2 C16 S4 179.42(13) . . . . ?
Ni1 S2 C16 C15 0.3(2) . . . . ?
Ni1 S7 C19 S9 176.97(13) . . . . ?
Ni1 S7 C19 C18 -4.0(2) . . . . ?
S4 C16 C15 S1 178.46(13) . . . . ?
S4 C16 C15 S3 -1.5(3) . . . . ?
S9 C19 C18 S8 0.1(3) . . . . ?
S9 C19 C18 S6 179.97(13) . . . . ?
S2 C16 C15 S1 -2.4(3) . . . . ?
S2 C16 C15 S3 177.64(13) . . . . ?
S7 C19 C18 S8 -178.94(13) . . . . ?
S7 C19 C18 S6 0.9(3) . . . . ?
N1 C1 C2 Cl1 70.7(3) . . . . ?
C19 S9 C20 S8 1.89(17) . . . . ?
C19 S9 C20 S10 -177.61(18) . . . . ?
C16 S4 C17 S3 -1.70(17) . . . . ?
C16 S4 C17 S5 177.63(18) . . . . ?
C18 S8 C20 S9 -1.83(17) . . . . ?
C18 S8 C20 S10 177.67(18) . . . . ?
C17 S4 C16 S2 -177.18(16) . . . . ?
C17 S4 C16 C15 1.9(2) . . . . ?
C17 S3 C15 S1 -179.70(17) . . . . ?
C17 S3 C15 C16 0.3(2) . . . . ?
C15 S3 C17 S4 1.05(17) . . . . ?
C15 S3 C17 S5 -178.28(18) . . . . ?
C20 S9 C19 S7 177.83(17) . . . . ?
C20 S9 C19 C18 -1.2(2) . . . . ?
C20 S8 C18 S6 -178.80(16) . . . . ?
C20 S8 C18 C19 1.0(2) . . . . ?
C7 O4A C9A C9 -173.2(4) . . . . ?
C7 O3 C6 C5 157.7(6) . . . . ?
C7 C8 O4 C9 175.8(4) . . . . ?
O4A C7 C7A O3A 54.2(6) . . . . ?
O3 C7 C8 O4 52.6(6) . . . . ?
O6 C13 C14 O1 -18.3(12) . . . . ?
O6 C12 C11 O5 62.9(7) . . . . ?
O6A C13A C14A O1A -13.9(13) . . . . ?
O1 C3 C4 O2 47.1(7) . . . . ?
C9 O5A C11A C12A -176.3(4) . . . . ?
C9 C10 O5 C11 178.5(5) . . . . ?
O2A C3 C3A O1A 49.0(7) . . . . ?
O2A C5A C6A O3A -3.2(11) . . . . ?
O2 C5 C6 O3 -3.2(11) . . . . ?
C3 O1 C14 C13 171.8(7) . . . . ?
C3 O2A C5A C6A 167.0(6) . . . . ?
O5A C9 C9A O4A -55.3(6) . . . . ?
O5A C11A C12A O6A 62.3(7) . . . . ?
C13 O6 C12 C11 143.1(7) . . . . ?
C5 O2 C4 C3 153.1(6) . . . . ?
C7A C7 O4A C9A -174.7(4) . . . . ?
C7A O3A C6A C5A 139.6(7) . . . . ?
C12 O6 C13 C14 155.6(7) . . . . ?
C10 C9 O4 C8 179.2(5) . . . . ?
C10 O5 C11 C12 -173.6(5) . . . . ?
C9A C9 O5A C11A 173.2(5) . . . . ?
C12A O6A C13A C14A 155.1(7) . . . . ?
C4 O2 C5 C6 153.6(7) . . . . ?
C14 O1 C3 C4 -164.7(5) . . . . ?
C8 C7 O3 C6 -176.9(5) . . . . ?
O4 C9 C10 O5 -56.7(6) . . . . ?
C3A O1A C14A C13A 157.3(8) . . . . ?
C5A O2A C3 C3A -173.3(5) . . . . ?
C13A O6A C12A C11A 167.3(5) . . . . ?
C6A O3A C7A C7 150.9(6) . . . . ?
C14A O1A C3A C3 167.4(6) . . . . ?
