#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:14:42 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 265974 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/24/7242442.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_7242442
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 Br1 N, C12 H24 O6'
_chemical_formula_sum            'C20 H31 Br N Ni O6 S10'
_chemical_formula_weight         840.68
_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                115.895(3)
_cell_angle_beta                 91.351(2)
_cell_angle_gamma                101.004(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0117(3)
_cell_length_b                   12.0652(3)
_cell_length_c                   13.7791(4)
_cell_measurement_reflns_used    19815
_cell_measurement_temperature    133
_cell_measurement_theta_max      31.2050
_cell_measurement_theta_min      1.9130
_cell_volume                     1604.69(9)
_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      133
_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 0.830
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  19.00   0.50    0.77    --    5.18 -28.00  51.29  176
  2  ω    -63.00  19.00   0.50    0.77    --    5.18 -28.00 120.90  164
  3  ω    -56.00  18.00   0.50    0.77    --    5.18 -19.00 -30.00  148
  4  ω    -22.00  19.00   0.50    0.77    --    5.18 -20.00 -76.51   82
  5  ω    -62.00  19.00   0.50    0.77    --    5.18 -33.00-104.04  162
  6  ω    -70.00 -44.00   0.50    0.77    --    5.18 -20.00 -76.51   52
  7  ω    -66.00  18.00   0.50    0.77    --    5.18 -34.00-163.07  168
  8  ω    -18.00  29.00   0.50    0.77    --   -4.95 -99.00 150.00   94
  9  ω    -18.00  23.00   0.50    0.77    --   -4.95 -99.00  90.00   82
 10  ω     -8.00  23.00   0.50    0.77    --   -4.95 -99.00   0.00   62
 11  ω    -12.00  24.00   0.50    0.77    --   -4.95 -99.00 -60.00   72
 12  ω    -18.00  26.00   0.50    0.77    --   -4.95 -99.00-120.00   88
;
_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      0.0307990000
_diffrn_orient_matrix_UB_12      -0.0434757000
_diffrn_orient_matrix_UB_13      -0.0382843000
_diffrn_orient_matrix_UB_21      -0.0299683000
_diffrn_orient_matrix_UB_22      0.0069898000
_diffrn_orient_matrix_UB_23      -0.0424709000
_diffrn_orient_matrix_UB_31      0.0502334000
_diffrn_orient_matrix_UB_32      0.0505636000
_diffrn_orient_matrix_UB_33      0.0073224000
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38326
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.917
_diffrn_reflns_theta_min         1.892
_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    2.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54335
_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    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0325
_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)+(0.0305P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6316
_reflns_number_total             8423
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           133k
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_original_cell_volume        1604.68(8)
_cod_database_code               7242442
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         BrC20H31NO6NiS10
_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   0.786
_shelx_estimated_absorpt_t_min   0.631
_reflns_odcompleteness_completeness 99.98
_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 N(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C1A \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
3. Others
 1*[Sof(Br1B)]+1*[Sof(Br1A)]+1*[Sof(Br1)]=1 with esd of 0.0001
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=Sof(H1AD)=
 Sof(H1AE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C3(H3A,H3B), C12(H12A,H12B), C8(H8A,H8B), C9(H9A,H9B),
 C33(H33A,H33B), C32(H32A,H32B), C10(H10A,H10B), C7(H7A,H7B), C4(H4A,H4B),
 C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B), C2A(H2AA,H2AB), C1A(H1AD,
 H1AE)
4.b Idealised Me refined as rotating group:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_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 2.568
_oxdiff_exptl_absorpt_empirical_full_min 0.571
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 0.13868(2) 0.14926(2) 0.11385(2) 0.01765(7) Uani 1 1 d . . . . .
Br1B Br 0.10558(3) 0.80400(3) 0.52710(3) 0.03151(12) Uani 0.8800(14) 1 d . . P
A 1
S1 S 0.10508(4) 0.33857(4) 0.17832(4) 0.01928(11) Uani 1 1 d . . . . .
S2 S 0.26800(5) 0.18064(4) 0.00779(4) 0.02184(12) Uani 1 1 d . . . . .
S3 S 0.21040(4) 0.55669(4) 0.12797(4) 0.01965(11) Uani 1 1 d . . . . .
S4 S 0.35780(5) 0.41132(4) -0.02956(4) 0.01974(11) Uani 1 1 d . . . . .
S7 S 0.16642(5) -0.04101(4) 0.04162(4) 0.02184(12) Uani 1 1 d . . . . .
S5 S 0.36436(5) 0.67494(5) 0.00804(5) 0.02532(13) Uani 1 1 d . . . . .
S9 S 0.05929(5) -0.26696(4) 0.07906(4) 0.02058(11) Uani 1 1 d . . . . .
S8 S -0.07434(5) -0.12249(5) 0.25160(5) 0.02582(13) Uani 1 1 d . . . . .
S6 S 0.01404(5) 0.11500(5) 0.22226(5) 0.02361(12) Uani 1 1 d . . . . .
S10 S -0.08346(5) -0.39279(5) 0.19792(5) 0.02853(13) Uani 1 1 d . . . . .
O6 O 0.57741(13) 0.65159(13) 0.37348(12) 0.0239(3) Uani 1 1 d . . . . .
O5 O 0.36564(12) 0.48520(13) 0.37803(12) 0.0241(3) Uani 1 1 d . . . . .
O1 O 0.64552(13) 0.90014(13) 0.53693(12) 0.0249(3) Uani 1 1 d . . . . .
O4 O 0.25669(12) 0.54223(14) 0.57225(13) 0.0275(3) Uani 1 1 d . . . . .
O2 O 0.54344(14) 0.93381(14) 0.73024(13) 0.0322(4) Uani 1 1 d . . . . .
O3 O 0.31397(13) 0.78455(14) 0.73497(13) 0.0296(4) Uani 1 1 d . . . . .
N1 N 0.39563(15) 0.74521(16) 0.52590(15) 0.0241(4) Uani 1 1 d . U . . .
H1AA H 0.391844 0.660662 0.490882 0.029 Uiso 0.911(4) 1 calc R U P B 1
H1AB H 0.350751 0.762410 0.583350 0.029 Uiso 0.911(4) 1 calc R U P B 1
H1AC H 0.476429 0.787648 0.550131 0.029 Uiso 0.911(4) 1 calc R U P B 1
H1BD H 0.348485 0.673953 0.470590 0.029 Uiso 0.089(4) 1 calc R U P B 2
H1BE H 0.384320 0.742616 0.590142 0.029 Uiso 0.089(4) 1 calc R U P B 2
H1BF H 0.477445 0.750093 0.515657 0.029 Uiso 0.089(4) 1 calc R U P B 2
C13 C 0.20076(17) 0.40291(17) 0.11069(17) 0.0174(4) Uani 1 1 d . . . . .
C15 C 0.31290(17) 0.55358(17) 0.03372(16) 0.0180(4) Uani 1 1 d . . . . .
C14 C 0.26983(17) 0.33498(17) 0.03605(17) 0.0188(4) Uani 1 1 d . . . . .
C17 C 0.07380(17) -0.10885(17) 0.10812(17) 0.0182(4) Uani 1 1 d . . . . .
C18 C -0.03511(18) -0.26701(18) 0.17744(18) 0.0214(4) Uani 1 1 d . . . . .
C11 C 0.4564(2) 0.44256(19) 0.30615(19) 0.0262(5) Uani 1 1 d . . . . .
H11A H 0.416162 0.365566 0.239604 0.031 Uiso 1 1 calc R U . . .
H11B H 0.521122 0.421271 0.341925 0.031 Uiso 1 1 calc R U . . .
C16 C 0.00918(18) -0.04090(18) 0.18742(18) 0.0206(4) Uani 1 1 d . . . . .
C3 C 0.7135(2) 0.9764(2) 0.6420(2) 0.0293(5) Uani 1 1 d . . . . .
H3A H 0.778735 1.044026 0.639949 0.035 Uiso 1 1 calc R U . . .
H3B H 0.754738 0.924048 0.664803 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5150(2) 0.5445(2) 0.27687(18) 0.0272(5) Uani 1 1 d . . . . .
H12A H 0.575233 0.514555 0.224306 0.033 Uiso 1 1 calc R U . . .
H12B H 0.450293 0.567623 0.242828 0.033 Uiso 1 1 calc R U . . .
C8 C 0.16856(19) 0.5870(2) 0.6459(2) 0.0293(5) Uani 1 1 d . . . . .
H8A H 0.117199 0.516474 0.655478 0.035 Uiso 1 1 calc R U . . .
H8B H 0.112591 0.623918 0.617250 0.035 Uiso 1 1 calc R U . . .
C9 C 0.2044(2) 0.4334(2) 0.4741(2) 0.0297(5) Uani 1 1 d . . . . .
H9A H 0.145518 0.453603 0.432221 0.036 Uiso 1 1 calc R U . . .
H9B H 0.158441 0.365502 0.490117 0.036 Uiso 1 1 calc R U . . .
C33 C 0.72536(19) 0.8451(2) 0.4575(2) 0.0297(5) Uani 1 1 d . . . . .
H33A H 0.778375 0.803843 0.483894 0.036 Uiso 1 1 calc R U . . .
H33B H 0.780475 0.911890 0.445440 0.036 Uiso 1 1 calc R U . . .
C32 C 0.6483(2) 0.7498(2) 0.35327(19) 0.0292(5) Uani 1 1 d . . . . .
H32A H 0.592062 0.789483 0.328176 0.035 Uiso 1 1 calc R U . . .
H32B H 0.702674 0.714991 0.296370 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3085(2) 0.39071(19) 0.40988(19) 0.0283(5) Uani 1 1 d . . . . .
H10A H 0.370959 0.377696 0.454404 0.034 Uiso 1 1 calc R U . . .
H10B H 0.275737 0.309462 0.344563 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2395(2) 0.6853(2) 0.7521(2) 0.0307(5) Uani 1 1 d . . . . .
H7A H 0.180881 0.719390 0.805104 0.037 Uiso 1 1 calc R U . . .
H7B H 0.293434 0.647508 0.781614 0.037 Uiso 1 1 calc R U . . .
C4 C 0.6269(2) 1.0333(2) 0.7209(2) 0.0319(5) Uani 1 1 d . . . . .
H4A H 0.674340 1.093729 0.792534 0.038 Uiso 1 1 calc R U . . .
H4B H 0.579858 1.079534 0.695079 0.038 Uiso 1 1 calc R U . . .
C2 C 0.2066(2) 0.7302(2) 0.4121(2) 0.0268(6) Uani 0.911(4) 1 d . . P A 1
H2A H 0.190465 0.637898 0.387728 0.032 Uiso 0.911(4) 1 calc R U P B 1
H2B H 0.182258 0.744136 0.349389 0.032 Uiso 0.911(4) 1 calc R U P B 1
C6 C 0.3970(2) 0.8717(2) 0.8309(2) 0.0395(6) Uani 1 1 d . . . . .
H6A H 0.457288 0.828674 0.846738 0.047 Uiso 1 1 calc R U . . .
H6B H 0.349231 0.902962 0.893697 0.047 Uiso 1 1 calc R U . . .
C5 C 0.4654(2) 0.9804(2) 0.8137(2) 0.0450(7) Uani 1 1 d . . . . .
H5A H 0.405257 1.019202 0.791792 0.054 Uiso 1 1 calc R U . . .
H5B H 0.516599 1.045641 0.881868 0.054 Uiso 1 1 calc R U . . .
C1 C 0.3426(2) 0.7863(2) 0.4490(2) 0.0256(6) Uani 0.911(4) 1 d . . P A 1
H1A H 0.388485 0.762103 0.384495 0.031 Uiso 0.911(4) 1 calc R U P B 1
H1B H 0.356090 0.879572 0.485031 0.031 Uiso 0.911(4) 1 calc R U P B 1
Br1A Br 0.0732(5) 0.8234(5) 0.4706(6) 0.058(2) Uani 0.0615(14) 1 d . . P C 3
C2A C 0.220(2) 0.847(3) 0.553(2) 0.034(6) Uani 0.089(4) 1 d . U P B 2
H2AA H 0.201406 0.931022 0.573460 0.041 Uiso 0.089(4) 1 calc R U P B 2
H2AB H 0.207098 0.826283 0.614713 0.041 Uiso 0.089(4) 1 calc R U P B 2
Br1 Br 0.1164(5) 0.7245(5) 0.4284(5) 0.056(2) Uani 0.0584(11) 1 d . . P B 2
C1A C 0.360(3) 0.850(3) 0.528(3) 0.044(5) Uani 0.089(4) 1 d . U P B 2
H1AD H 0.367938 0.850867 0.456684 0.053 Uiso 0.089(4) 1 calc R U P B 2
H1AE H 0.415412 0.928157 0.584258 0.053 Uiso 0.089(4) 1 calc R U P B 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'
Br Br -0.2901 2.4595 '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
S2 Ni1 S1 93.49(2) . . ?
S2 Ni1 S6 177.87(2) . . ?
S7 Ni1 S1 176.89(3) . . ?
S7 Ni1 S2 85.50(2) . . ?
S7 Ni1 S6 93.18(2) . . ?
S6 Ni1 S1 87.91(2) . . ?
C13 S1 Ni1 101.60(7) . . ?
C14 S2 Ni1 101.89(7) . . ?
C15 S3 C13 97.51(9) . . ?
C15 S4 C14 97.25(9) . . ?
C17 S7 Ni1 102.35(7) . . ?
C18 S9 C17 97.06(10) . . ?
C18 S8 C16 97.44(10) . . ?
C16 S6 Ni1 101.84(7) . . ?
C32 O6 C12 113.07(16) . . ?
C11 O5 C10 111.16(16) . . ?
C33 O1 C3 111.55(16) . . ?
C9 O4 C8 114.07(16) . . ?
C4 O2 C5 112.03(17) . . ?
C6 O3 C7 110.58(18) . . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
S1 C13 S3 122.54(12) . . ?
C14 C13 S1 121.91(14) . . ?
C14 C13 S3 115.48(14) . . ?
S4 C15 S3 113.16(10) . . ?
S5 C15 S3 123.55(12) . . ?
S5 C15 S4 123.29(12) . . ?
S2 C14 S4 122.32(12) . . ?
C13 C14 S2 121.08(15) . . ?
C13 C14 S4 116.60(14) . . ?
S7 C17 S9 121.86(12) . . ?
C16 C17 S7 121.28(14) . . ?
C16 C17 S9 116.85(14) . . ?
S9 C18 S8 113.26(11) . . ?
S10 C18 S9 123.02(13) . . ?
S10 C18 S8 123.72(13) . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.30(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
S6 C16 S8 123.34(13) . . ?
C17 C16 S8 115.32(15) . . ?
C17 C16 S6 121.32(15) . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.44(18) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
O6 C12 C11 108.43(18) . . ?
O6 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
O4 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
O4 C8 C7 107.79(17) . . ?
H8A C8 H8B 108.5 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
O4 C9 C10 108.08(17) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
O1 C33 H33A 109.8 . . ?
O1 C33 H33B 109.8 . . ?
O1 C33 C32 109.59(17) . . ?
H33A C33 H33B 108.2 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
O6 C32 C33 107.40(18) . . ?
O6 C32 H32A 110.2 . . ?
O6 C32 H32B 110.2 . . ?
C33 C32 H32A 110.2 . . ?
C33 C32 H32B 110.2 . . ?
H32A C32 H32B 108.5 . . ?
O5 C10 C9 109.09(17) . . ?
O5 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O3 C7 C8 108.65(19) . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 107.92(18) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
Br1B C2 H2A 109.3 . . ?
Br1B C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 Br1B 111.82(18) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.2(2) . . ?
H6A C6 H6B 108.3 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.3(2) . . ?
O2 C5 H5A 110.0 . . ?
O2 C5 H5B 110.0 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N1 C1 C2 113.54(18) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
H2AA C2A H2AB 108.4 . . ?
Br1 C2A H2AA 110.1 . . ?
Br1 C2A H2AB 110.1 . . ?
C1A C2A H2AA 110.1 . . ?
C1A C2A H2AB 110.1 . . ?
C1A C2A Br1 108(2) . . ?
N1 C1A C2A 110(2) . . ?
N1 C1A H1AD 109.7 . . ?
N1 C1A H1AE 109.7 . . ?
C2A C1A H1AD 109.7 . . ?
C2A C1A H1AE 109.7 . . ?
H1AD C1A H1AE 108.2 . . ?
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 2.1700(5) . ?
Ni1 S2 2.1640(5) . ?
Ni1 S7 2.1541(5) . ?
Ni1 S6 2.1692(6) . ?
Br1B C2 1.941(3) . ?
S1 C13 1.7166(19) . ?
S2 C14 1.7238(19) . ?
S3 C13 1.7459(18) . ?
S3 C15 1.733(2) . ?
S4 C15 1.729(2) . ?
S4 C14 1.7414(19) . ?
S7 C17 1.7118(19) . ?
S5 C15 1.6539(19) . ?
S9 C17 1.7431(18) . ?
S9 C18 1.728(2) . ?
S8 C18 1.739(2) . ?
S8 C16 1.7464(19) . ?
S6 C16 1.716(2) . ?
S10 C18 1.6551(19) . ?
O6 C12 1.424(3) . ?
O6 C32 1.427(2) . ?
O5 C11 1.430(3) . ?
O5 C10 1.437(2) . ?
O1 C3 1.423(3) . ?
O1 C33 1.430(3) . ?
O4 C8 1.425(3) . ?
O4 C9 1.417(3) . ?
O2 C4 1.422(2) . ?
O2 C5 1.429(3) . ?
O3 C7 1.430(2) . ?
O3 C6 1.432(3) . ?
N1 H1AA 0.9100 . ?
N1 H1AB 0.9100 . ?
N1 H1AC 0.9100 . ?
N1 H1BD 0.9100 . ?
N1 H1BE 0.9100 . ?
N1 H1BF 0.9100 . ?
N1 C1 1.500(3) . ?
N1 C1A 1.39(3) . ?
C13 C14 1.359(3) . ?
C17 C16 1.360(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.495(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.487(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.495(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.495(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.494(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.496(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.500(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A Br1 1.87(3) . ?
C2A C1A 1.58(4) . ?
C1A H1AD 0.9900 . ?
C1A H1AE 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 C13 S3 178.54(10) . . . . ?
Ni1 S1 C13 C14 1.71(18) . . . . ?
Ni1 S2 C14 S4 -178.60(11) . . . . ?
Ni1 S2 C14 C13 0.69(18) . . . . ?
Ni1 S7 C17 S9 179.05(11) . . . . ?
Ni1 S7 C17 C16 -1.83(19) . . . . ?
Ni1 S6 C16 S8 177.88(11) . . . . ?
Ni1 S6 C16 C17 -0.60(19) . . . . ?
Br1B C2 C1 N1 72.3(2) . . . . ?
S1 C13 C14 S2 -1.7(3) . . . . ?
S1 C13 C14 S4 177.61(11) . . . . ?
S3 C13 C14 S2 -178.77(11) . . . . ?
S3 C13 C14 S4 0.6(2) . . . . ?
S7 C17 C16 S8 -176.86(11) . . . . ?
S7 C17 C16 S6 1.7(3) . . . . ?
S9 C17 C16 S8 2.3(2) . . . . ?
S9 C17 C16 S6 -179.09(11) . . . . ?
O5 C11 C12 O6 62.4(2) . . . . ?
O1 C3 C4 O2 65.8(2) . . . . ?
O1 C33 C32 O6 -63.4(2) . . . . ?
O4 C8 C7 O3 58.9(2) . . . . ?
O4 C9 C10 O5 -65.6(2) . . . . ?
O3 C6 C5 O2 -65.5(3) . . . . ?
C13 S3 C15 S4 -0.59(13) . . . . ?
C13 S3 C15 S5 -179.72(13) . . . . ?
C15 S3 C13 S1 -177.00(13) . . . . ?
C15 S3 C13 C14 0.02(17) . . . . ?
C15 S4 C14 S2 178.47(13) . . . . ?
C15 S4 C14 C13 -0.85(18) . . . . ?
C14 S4 C15 S3 0.82(13) . . . . ?
C14 S4 C15 S5 179.97(13) . . . . ?
C17 S9 C18 S8 2.04(13) . . . . ?
C17 S9 C18 S10 -178.26(14) . . . . ?
C18 S9 C17 S7 176.50(13) . . . . ?
C18 S9 C17 C16 -2.66(18) . . . . ?
C18 S8 C16 S6 -179.29(14) . . . . ?
C18 S8 C16 C17 -0.72(18) . . . . ?
C11 O5 C10 C9 -173.47(17) . . . . ?
C16 S8 C18 S9 -1.07(13) . . . . ?
C16 S8 C18 S10 179.24(14) . . . . ?
C3 O1 C33 C32 170.69(17) . . . . ?
C12 O6 C32 C33 -170.39(17) . . . . ?
C8 O4 C9 C10 -174.99(17) . . . . ?
C9 O4 C8 C7 169.54(18) . . . . ?
C33 O1 C3 C4 178.84(18) . . . . ?
C32 O6 C12 C11 173.50(17) . . . . ?
C10 O5 C11 C12 -178.95(17) . . . . ?
C7 O3 C6 C5 -174.95(19) . . . . ?
C4 O2 C5 C6 -170.3(2) . . . . ?
C6 O3 C7 C8 -171.60(19) . . . . ?
C5 O2 C4 C3 173.4(2) . . . . ?
Br1 C2A C1A N1 -74(3) . . . . ?
