#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:14:42 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 265974 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/24/7242434.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_7242434
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                115.833(4)
_cell_angle_beta                 91.587(3)
_cell_angle_gamma                100.906(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9869(3)
_cell_length_b                   12.0485(4)
_cell_length_c                   13.7559(5)
_cell_measurement_reflns_used    10627
_cell_measurement_temperature    106
_cell_measurement_theta_max      30.5700
_cell_measurement_theta_min      1.9220
_cell_volume                     1596.83(11)
_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      106
_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 0.779
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  39.00   0.50    0.67    --    5.18 -99.00   0.00  100
  2  ω    -17.00  26.00   0.50    0.67    --   -4.95 -99.00 150.00   86
  3  ω    -76.00   1.00   0.50    0.67    --   -4.95 -37.00  60.00  154
  4  ω    -10.00  68.00   0.50    0.67    --   -4.95  37.00   0.00  156
  5  ω     25.00  74.00   0.50    0.67    --    5.18  37.00 -90.00   98
  6  ω    -43.00  10.00   0.50    0.67    --   -4.95 -57.00-180.00  106
;
_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      0.0310318000
_diffrn_orient_matrix_UB_12      -0.0436389000
_diffrn_orient_matrix_UB_13      -0.0378793000
_diffrn_orient_matrix_UB_21      -0.0300486000
_diffrn_orient_matrix_UB_22      0.0064051000
_diffrn_orient_matrix_UB_23      -0.0429805000
_diffrn_orient_matrix_UB_31      0.0502480000
_diffrn_orient_matrix_UB_32      0.0505765000
_diffrn_orient_matrix_UB_33      0.0071785000
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.957
_diffrn_reflns_theta_min         1.895
_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    2.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85539
_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    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0356
_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)+(0.0155P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5867
_reflns_number_total             7891
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           106k
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_original_cell_volume        1596.83(10)
_cod_database_code               7242434
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         BrCHNONiS
_chemical_oxdiff_usercomment     223K
_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   0.842
_shelx_estimated_absorpt_t_min   0.429
_reflns_odcompleteness_completeness 99.95
_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 2.239
_oxdiff_exptl_absorpt_empirical_full_min 0.447
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 0.13912(3) 0.14919(3) 0.11364(3) 0.01407(8) Uani 1 1 d . . . . .
Br1B Br 0.10533(3) 0.80471(3) 0.52744(3) 0.02529(13) Uani 0.9342(17) 1 d . . P
A 1
S1 S 0.10558(5) 0.33876(6) 0.17838(5) 0.01549(13) Uani 1 1 d . . . . .
S2 S 0.26828(5) 0.18041(6) 0.00725(5) 0.01748(14) Uani 1 1 d . . . . .
S3 S 0.21065(5) 0.55675(6) 0.12782(5) 0.01556(13) Uani 1 1 d . . . . .
S4 S 0.35799(5) 0.41139(6) -0.02987(5) 0.01561(13) Uani 1 1 d . . . . .
S7 S 0.16695(5) -0.04112(6) 0.04134(5) 0.01761(14) Uani 1 1 d . . . . .
S5 S 0.36464(6) 0.67560(6) 0.00815(5) 0.02007(14) Uani 1 1 d . . . . .
S9 S 0.05954(5) -0.26736(6) 0.07860(5) 0.01671(14) Uani 1 1 d . . . . .
S8 S -0.07420(6) -0.12304(6) 0.25119(6) 0.02051(15) Uani 1 1 d . . . . .
S6 S 0.01396(6) 0.11463(6) 0.22152(5) 0.01914(14) Uani 1 1 d . . . . .
S10 S -0.08302(6) -0.39320(6) 0.19788(6) 0.02263(15) Uani 1 1 d . . . . .
O6 O 0.57826(15) 0.65134(17) 0.37307(14) 0.0192(4) Uani 1 1 d . . . . .
O5 O 0.36637(15) 0.48494(16) 0.37809(14) 0.0191(4) Uani 1 1 d . . . . .
O1 O 0.64542(14) 0.89979(17) 0.53634(15) 0.0201(4) Uani 1 1 d . . . . .
O4 O 0.25652(15) 0.54176(17) 0.57149(15) 0.0217(4) Uani 1 1 d . . . . .
O2 O 0.54360(16) 0.93365(17) 0.72982(15) 0.0254(4) Uani 1 1 d . . . . .
O3 O 0.31399(15) 0.78431(18) 0.73465(15) 0.0245(4) Uani 1 1 d . . . . .
N1 N 0.39491(18) 0.7446(2) 0.52465(18) 0.0198(5) Uani 1 1 d . U . . .
H1AA H 0.391579 0.661949 0.490085 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1AB H 0.350518 0.760804 0.580493 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1AC H 0.473979 0.786425 0.549079 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1BD H 0.344020 0.674272 0.475050 0.024 Uiso 0.051(5) 1 calc R U P B 2
H1BE H 0.387988 0.749013 0.590479 0.024 Uiso 0.051(5) 1 calc R U P B 2
H1BF H 0.473352 0.743616 0.510496 0.024 Uiso 0.051(5) 1 calc R U P B 2
C13 C 0.2013(2) 0.4031(2) 0.1104(2) 0.0136(5) Uani 1 1 d . . . . .
C15 C 0.3132(2) 0.5537(2) 0.0333(2) 0.0147(5) Uani 1 1 d . . . . .
C14 C 0.2699(2) 0.3347(2) 0.0358(2) 0.0142(5) Uani 1 1 d . . . . .
C17 C 0.0737(2) -0.1098(2) 0.1072(2) 0.0158(5) Uani 1 1 d . . . . .
C18 C -0.0355(2) -0.2678(2) 0.1771(2) 0.0170(5) Uani 1 1 d . . . . .
C11 C 0.4564(2) 0.4417(2) 0.3055(2) 0.0214(6) Uani 1 1 d . . . . .
H11A H 0.416025 0.366372 0.240338 0.026 Uiso 1 1 calc R U . . .
H11B H 0.520056 0.420273 0.340248 0.026 Uiso 1 1 calc R U . . .
C16 C 0.0092(2) -0.0411(2) 0.1868(2) 0.0166(5) Uani 1 1 d . . . . .
C3 C 0.7142(2) 0.9767(3) 0.6421(2) 0.0225(6) Uani 1 1 d . . . . .
H3A H 0.777978 1.043209 0.640171 0.027 Uiso 1 1 calc R U . . .
H3B H 0.755010 0.925619 0.664762 0.027 Uiso 1 1 calc R U . . .
C12 C 0.5153(2) 0.5439(2) 0.2760(2) 0.0208(6) Uani 1 1 d . . . . .
H12A H 0.574194 0.514322 0.224466 0.025 Uiso 1 1 calc R U . . .
H12B H 0.451623 0.566606 0.242444 0.025 Uiso 1 1 calc R U . . .
C8 C 0.1681(2) 0.5861(3) 0.6442(2) 0.0236(6) Uani 1 1 d . . . . .
H8A H 0.117557 0.516763 0.653238 0.028 Uiso 1 1 calc R U . . .
H8B H 0.113326 0.622272 0.615726 0.028 Uiso 1 1 calc R U . . .
C9 C 0.2048(2) 0.4327(3) 0.4736(2) 0.0232(6) Uani 1 1 d . . . . .
H9A H 0.146491 0.452086 0.432218 0.028 Uiso 1 1 calc R U . . .
H9B H 0.159901 0.366340 0.489617 0.028 Uiso 1 1 calc R U . . .
C33 C 0.7255(2) 0.8460(3) 0.4569(2) 0.0247(6) Uani 1 1 d . . . . .
H33A H 0.779117 0.806757 0.482962 0.030 Uiso 1 1 calc R U . . .
H33B H 0.778041 0.911869 0.444595 0.030 Uiso 1 1 calc R U . . .
C32 C 0.6483(2) 0.7494(3) 0.3529(2) 0.0225(6) Uani 1 1 d . . . . .
H32A H 0.592552 0.787482 0.327633 0.027 Uiso 1 1 calc R U . . .
H32B H 0.701832 0.715369 0.297308 0.027 Uiso 1 1 calc R U . . .
C10 C 0.3090(2) 0.3894(3) 0.4088(2) 0.0228(6) Uani 1 1 d . . . . .
H10A H 0.370319 0.375755 0.452189 0.027 Uiso 1 1 calc R U . . .
H10B H 0.276469 0.310210 0.344334 0.027 Uiso 1 1 calc R U . . .
C7 C 0.2385(2) 0.6844(3) 0.7511(2) 0.0235(6) Uani 1 1 d . . . . .
H7A H 0.180497 0.717705 0.802473 0.028 Uiso 1 1 calc R U . . .
H7B H 0.291074 0.647306 0.780597 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6266(2) 1.0332(3) 0.7206(2) 0.0250(6) Uani 1 1 d . . . . .
H4A H 0.672895 1.092816 0.791005 0.030 Uiso 1 1 calc R U . . .
H4B H 0.580131 1.078046 0.694697 0.030 Uiso 1 1 calc R U . . .
C2 C 0.2057(3) 0.7291(3) 0.4114(2) 0.0217(7) Uani 0.949(5) 1 d . . P A 1
H2A H 0.190325 0.638799 0.388522 0.026 Uiso 0.949(5) 1 calc R U P B 1
H2B H 0.180838 0.741582 0.349345 0.026 Uiso 0.949(5) 1 calc R U P B 1
C6 C 0.3970(3) 0.8715(3) 0.8306(2) 0.0310(7) Uani 1 1 d . . . . .
H6A H 0.455819 0.829300 0.846718 0.037 Uiso 1 1 calc R U . . .
H6B H 0.349909 0.902617 0.891858 0.037 Uiso 1 1 calc R U . . .
C5 C 0.4661(3) 0.9799(3) 0.8133(3) 0.0350(7) Uani 1 1 d . . . . .
H5A H 0.407305 1.018628 0.792287 0.042 Uiso 1 1 calc R U . . .
H5B H 0.516882 1.043324 0.880297 0.042 Uiso 1 1 calc R U . . .
C1 C 0.3422(2) 0.7861(3) 0.4479(2) 0.0203(7) Uani 0.949(5) 1 d . . P A 1
H1A H 0.386962 0.762450 0.384604 0.024 Uiso 0.949(5) 1 calc R U P B 1
H1B H 0.355173 0.877556 0.483322 0.024 Uiso 0.949(5) 1 calc R U P B 1
Br1A Br 0.0702(14) 0.8288(19) 0.4736(19) 0.072(8) Uani 0.0294(18) 1 d . . P C 3
C2A C 0.214(5) 0.846(6) 0.553(5) 0.030(8) Uani 0.051(5) 1 d . U P B 2
H2AA H 0.187749 0.925648 0.574936 0.036 Uiso 0.051(5) 1 calc R U P B 2
H2AB H 0.207297 0.822829 0.612066 0.036 Uiso 0.051(5) 1 calc R U P B 2
Br1 Br 0.1198(13) 0.7259(15) 0.4326(13) 0.078(6) Uani 0.0364(15) 1 d . . P B 2
C1A C 0.359(5) 0.860(6) 0.521(5) 0.029(6) Uani 0.051(5) 1 d . U P B 2
H1AD H 0.362161 0.855315 0.449173 0.034 Uiso 0.051(5) 1 calc R U P B 2
H1AE H 0.413957 0.937811 0.573935 0.034 Uiso 0.051(5) 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 93.58(2) . . ?
S2 Ni1 S6 178.07(3) . . ?
S7 Ni1 S1 176.96(3) . . ?
S7 Ni1 S2 85.41(2) . . ?
S7 Ni1 S6 93.22(2) . . ?
S6 Ni1 S1 87.85(2) . . ?
C13 S1 Ni1 101.51(9) . . ?
C14 S2 Ni1 101.72(8) . . ?
C15 S3 C13 97.43(11) . . ?
C15 S4 C14 97.35(11) . . ?
C17 S7 Ni1 102.50(9) . . ?
C18 S9 C17 97.25(12) . . ?
C18 S8 C16 97.65(12) . . ?
C16 S6 Ni1 101.87(8) . . ?
C32 O6 C12 113.02(18) . . ?
C11 O5 C10 110.68(19) . . ?
C33 O1 C3 111.47(18) . . ?
C9 O4 C8 113.98(18) . . ?
C4 O2 C5 112.1(2) . . ?
C6 O3 C7 111.1(2) . . ?
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 122.39(14) . . ?
C14 C13 S1 121.70(18) . . ?
C14 C13 S3 115.83(16) . . ?
S4 C15 S3 113.08(12) . . ?
S5 C15 S3 123.37(15) . . ?
S5 C15 S4 123.54(14) . . ?
S2 C14 S4 122.23(14) . . ?
C13 C14 S2 121.47(16) . . ?
C13 C14 S4 116.29(18) . . ?
S7 C17 S9 122.13(15) . . ?
C16 C17 S7 120.85(19) . . ?
C16 C17 S9 117.01(16) . . ?
S9 C18 S8 113.00(13) . . ?
S10 C18 S9 123.10(16) . . ?
S10 C18 S8 123.90(14) . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.3(2) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
S6 C16 S8 123.41(15) . . ?
C17 C16 S8 115.04(18) . . ?
C17 C16 S6 121.53(17) . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 109.0(2) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O6 C12 C11 108.4(2) . . ?
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 107.90(19) . . ?
H8A C8 H8B 108.4 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
O4 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
O4 C9 C10 108.54(19) . . ?
H9A C9 H9B 108.4 . . ?
C10 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
O1 C33 H33A 109.8 . . ?
O1 C33 H33B 109.8 . . ?
O1 C33 C32 109.54(19) . . ?
H33A C33 H33B 108.2 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
O6 C32 C33 107.9(2) . . ?
O6 C32 H32A 110.1 . . ?
O6 C32 H32B 110.1 . . ?
C33 C32 H32A 110.1 . . ?
C33 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
O5 C10 C9 108.6(2) . . ?
O5 C10 H10A 110.0 . . ?
O5 C10 H10B 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
O3 C7 C8 108.7(2) . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
O2 C4 C3 108.0(2) . . ?
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 108.0 . . ?
C1 C2 Br1B 111.5(2) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.4(2) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.8(2) . . ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N1 C1 C2 112.7(2) . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
H2AA C2A H2AB 108.8 . . ?
Br1 C2A H2AA 110.7 . . ?
Br1 C2A H2AB 110.7 . . ?
C1A C2A H2AA 110.7 . . ?
C1A C2A H2AB 110.7 . . ?
C1A C2A Br1 105(4) . . ?
N1 C1A C2A 102(4) . . ?
N1 C1A H1AD 111.4 . . ?
N1 C1A H1AE 111.4 . . ?
C2A C1A H1AD 111.4 . . ?
C2A C1A H1AE 111.4 . . ?
H1AD C1A H1AE 109.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1702(7) . ?
Ni1 S2 2.1656(6) . ?
Ni1 S7 2.1528(7) . ?
Ni1 S6 2.1684(6) . ?
Br1B C2 1.950(3) . ?
S1 C13 1.720(2) . ?
S2 C14 1.721(2) . ?
S3 C13 1.742(2) . ?
S3 C15 1.737(2) . ?
S4 C15 1.726(3) . ?
S4 C14 1.744(2) . ?
S7 C17 1.714(2) . ?
S5 C15 1.654(2) . ?
S9 C17 1.737(2) . ?
S9 C18 1.734(2) . ?
S8 C18 1.737(3) . ?
S8 C16 1.750(2) . ?
S6 C16 1.713(3) . ?
S10 C18 1.650(2) . ?
O6 C12 1.429(3) . ?
O6 C32 1.421(3) . ?
O5 C11 1.429(3) . ?
O5 C10 1.437(3) . ?
O1 C3 1.430(3) . ?
O1 C33 1.428(3) . ?
O4 C8 1.419(3) . ?
O4 C9 1.413(3) . ?
O2 C4 1.419(3) . ?
O2 C5 1.425(3) . ?
O3 C7 1.435(3) . ?
O3 C6 1.428(3) . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 C1 1.495(3) . ?
N1 C1A 1.53(6) . ?
C13 C14 1.358(3) . ?
C17 C16 1.365(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.500(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.490(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.495(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.502(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C32 1.493(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.497(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.497(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A Br1 1.78(6) . ?
C2A C1A 1.67(7) . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?
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 178.48(13) . . . . ?
Ni1 S1 C13 C14 1.7(2) . . . . ?
Ni1 S2 C14 S4 -178.68(13) . . . . ?
Ni1 S2 C14 C13 0.7(2) . . . . ?
Ni1 S7 C17 S9 179.37(13) . . . . ?
Ni1 S7 C17 C16 -2.1(2) . . . . ?
Ni1 S6 C16 S8 177.55(13) . . . . ?
Ni1 S6 C16 C17 -0.9(2) . . . . ?
Br1B C2 C1 N1 72.9(3) . . . . ?
S1 C13 C14 S2 -1.7(3) . . . . ?
S1 C13 C14 S4 177.71(12) . . . . ?
S3 C13 C14 S2 -178.70(13) . . . . ?
S3 C13 C14 S4 0.7(3) . . . . ?
S7 C17 C16 S8 -176.41(13) . . . . ?
S7 C17 C16 S6 2.2(3) . . . . ?
S9 C17 C16 S8 2.2(3) . . . . ?
S9 C17 C16 S6 -179.24(13) . . . . ?
O5 C11 C12 O6 61.9(3) . . . . ?
O1 C3 C4 O2 65.9(3) . . . . ?
O1 C33 C32 O6 -62.7(3) . . . . ?
O4 C8 C7 O3 58.7(3) . . . . ?
O4 C9 C10 O5 -64.8(3) . . . . ?
O3 C6 C5 O2 -64.9(3) . . . . ?
C13 S3 C15 S4 -0.61(15) . . . . ?
C13 S3 C15 S5 -179.50(16) . . . . ?
C15 S3 C13 S1 -177.04(16) . . . . ?
C15 S3 C13 C14 0.0(2) . . . . ?
C15 S4 C14 S2 178.41(16) . . . . ?
C15 S4 C14 C13 -1.0(2) . . . . ?
C14 S4 C15 S3 0.90(16) . . . . ?
C14 S4 C15 S5 179.79(16) . . . . ?
C17 S9 C18 S8 1.70(15) . . . . ?
C17 S9 C18 S10 -178.06(16) . . . . ?
C18 S9 C17 S7 176.19(16) . . . . ?
C18 S9 C17 C16 -2.4(2) . . . . ?
C18 S8 C16 S6 -179.37(16) . . . . ?
C18 S8 C16 C17 -0.8(2) . . . . ?
C11 O5 C10 C9 -173.2(2) . . . . ?
C16 S8 C18 S9 -0.78(15) . . . . ?
C16 S8 C18 S10 178.98(16) . . . . ?
C3 O1 C33 C32 170.1(2) . . . . ?
C12 O6 C32 C33 -170.9(2) . . . . ?
C8 O4 C9 C10 -175.1(2) . . . . ?
C9 O4 C8 C7 169.1(2) . . . . ?
C33 O1 C3 C4 178.3(2) . . . . ?
C32 O6 C12 C11 173.9(2) . . . . ?
C10 O5 C11 C12 -179.5(2) . . . . ?
C7 O3 C6 C5 -175.2(2) . . . . ?
C4 O2 C5 C6 -170.7(2) . . . . ?
C6 O3 C7 C8 -171.4(2) . . . . ?
C5 O2 C4 C3 172.7(2) . . . . ?
Br1 C2A C1A N1 -77(4) . . . . ?
