#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:14:42 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 265974 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/24/7242438.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_7242438
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 H29 Br N Ni O6 S10'
_chemical_formula_weight         838.66
_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                115.825(3)
_cell_angle_beta                 91.535(2)
_cell_angle_gamma                100.927(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9810(3)
_cell_length_b                   12.0448(3)
_cell_length_c                   13.7409(4)
_cell_measurement_reflns_used    20361
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.9380
_cell_measurement_theta_min      1.9240
_cell_volume                     1593.91(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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  17.00   0.50    0.68    --    5.18 -22.00  55.21  122
  2  ω    -63.00  19.00   0.50    0.68    --    5.18 -28.00 121.78  164
  3  ω    -64.00  19.00   0.50    0.68    --    5.18 -20.00  -2.46  166
  4  ω    -70.00  18.00   0.50    0.68    --    5.18 -30.00 -65.58  176
  5  ω    -26.00  18.00   0.50    0.68    --    5.18 -19.00-150.00   88
  6  ω    -58.00  19.00   0.50    0.68    --    5.18 -28.00-175.10  154
  7  ω    -62.00 -34.00   0.50    0.68    --    5.18 -19.00-150.00   56
  8  ω    -15.00  27.00   0.50    0.68    --   -4.95 -99.00 120.00   84
  9  ω    -18.00  28.00   0.50    0.68    --   -4.95 -99.00  30.00   92
 10  ω    -13.00  24.00   0.50    0.68    --   -4.95 -99.00 -60.00   74
 11  ω    -18.00  26.00   0.50    0.68    --   -4.95 -99.00-120.00   88
 12  ω    -14.00  29.00   0.50    0.68    --   -4.95 -99.00-180.00   86
;
_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      0.0310094000
_diffrn_orient_matrix_UB_12      -0.0436313000
_diffrn_orient_matrix_UB_13      -0.0380035000
_diffrn_orient_matrix_UB_21      -0.0300922000
_diffrn_orient_matrix_UB_22      0.0064974000
_diffrn_orient_matrix_UB_23      -0.0429436000
_diffrn_orient_matrix_UB_31      0.0502791000
_diffrn_orient_matrix_UB_32      0.0505919000
_diffrn_orient_matrix_UB_33      0.0071668000
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.823
_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       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.043
_diffrn_reflns_theta_min         1.896
_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    2.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58143
_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    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8378
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0315
_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)+(0.0321P)²+0.0488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6461
_reflns_number_total             8378
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           113k
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_original_cell_volume        1593.91(8)
_cod_database_code               7242438
_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   0.784
_shelx_estimated_absorpt_t_min   0.629
_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(H2A1)=Sof(H2A2)=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(H2A1,H2A2), 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 1.997
_oxdiff_exptl_absorpt_empirical_full_min 0.588
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 0.86093(2) 0.85079(2) 0.88634(2) 0.01526(7) Uani 1 1 d . . . . .
Br1B Br 0.10538(2) 0.80453(2) 0.52733(3) 0.02716(11) Uani 0.9269(14) 1 d . . P
A 1
S1 S 0.89458(5) 0.66151(5) 0.82181(4) 0.01683(11) Uani 1 1 d . . . . .
S2 S 0.73170(5) 0.81942(5) 0.99250(4) 0.01913(11) Uani 1 1 d . . . . .
S3 S 0.78939(5) 0.44329(4) 0.87218(4) 0.01687(11) Uani 1 1 d . . . . .
S4 S 0.64198(5) 0.58851(4) 1.02980(4) 0.01688(11) Uani 1 1 d . . . . .
S7 S 0.83315(5) 1.04105(5) 0.95847(4) 0.01888(11) Uani 1 1 d . . . . .
S5 S 0.63550(5) 0.32460(5) 0.99190(5) 0.02171(12) Uani 1 1 d . . . . .
S9 S 0.94047(5) 1.26717(5) 0.92117(4) 0.01777(11) Uani 1 1 d . . . . .
S8 S 1.07415(5) 1.12281(5) 0.74857(5) 0.02215(12) Uani 1 1 d . . . . .
S6 S 0.98598(5) 0.88524(5) 0.77826(4) 0.02035(12) Uani 1 1 d . . . . .
S10 S 1.08308(5) 1.39300(5) 0.80198(5) 0.02402(13) Uani 1 1 d . . . . .
O6 O 0.57794(13) 0.65139(13) 0.37300(12) 0.0207(3) Uani 1 1 d . . . . .
O5 O 0.36598(13) 0.48505(13) 0.37810(12) 0.0211(3) Uani 1 1 d . . . . .
O1 O 0.64547(13) 0.89991(13) 0.53632(12) 0.0214(3) Uani 1 1 d . . . . .
O4 O 0.25677(13) 0.54192(14) 0.57159(12) 0.0237(3) Uani 1 1 d . . . . .
O2 O 0.54356(14) 0.93376(14) 0.73017(12) 0.0262(3) Uani 1 1 d . . . . .
O3 O 0.31348(13) 0.78444(14) 0.73434(13) 0.0255(3) Uani 1 1 d . . . . .
N1 N 0.39537(15) 0.74463(16) 0.52498(15) 0.0198(4) Uani 1 1 d . U . . .
H1AA H 0.391196 0.659943 0.489468 0.024 Uiso 0.946(4) 1 calc R U P B 1
H1AB H 0.350429 0.761596 0.582490 0.024 Uiso 0.946(4) 1 calc R U P B 1
H1AC H 0.476504 0.786711 0.549482 0.024 Uiso 0.946(4) 1 calc R U P B 1
H1BD H 0.330697 0.677747 0.485757 0.024 Uiso 0.054(4) 1 calc R U P B 2
H1BE H 0.411811 0.748901 0.591942 0.024 Uiso 0.054(4) 1 calc R U P B 2
H1BF H 0.464370 0.734484 0.489635 0.024 Uiso 0.054(4) 1 calc R U P B 2
C13 C 0.79912(18) 0.59703(17) 0.88978(16) 0.0151(4) Uani 1 1 d . . . . .
C15 C 0.68680(17) 0.44602(18) 0.96641(16) 0.0157(4) Uani 1 1 d . . . . .
C14 C 0.72955(17) 0.66506(18) 0.96392(16) 0.0159(4) Uani 1 1 d . . . . .
C17 C 0.92599(18) 1.10921(18) 0.89206(17) 0.0165(4) Uani 1 1 d . . . . .
C18 C 1.03491(18) 1.26714(19) 0.82272(18) 0.0190(4) Uani 1 1 d . . . . .
C11 C 0.4567(2) 0.4418(2) 0.30602(18) 0.0228(5) Uani 1 1 d . . . . .
H11A H 0.416049 0.364685 0.239443 0.027 Uiso 1 1 calc R U . . .
H11B H 0.521673 0.420550 0.342012 0.027 Uiso 1 1 calc R U . . .
C16 C 0.99143(18) 1.04131(19) 0.81351(17) 0.0185(4) Uani 1 1 d . . . . .
C3 C 0.7142(2) 0.9772(2) 0.64213(18) 0.0244(5) Uani 1 1 d . . . . .
H3A H 0.779018 1.045262 0.640065 0.029 Uiso 1 1 calc R U . . .
H3B H 0.756319 0.925300 0.665313 0.029 Uiso 1 1 calc R U . . .
C12 C 0.5157(2) 0.5443(2) 0.27613(17) 0.0220(5) Uani 1 1 d . . . . .
H12A H 0.576180 0.514275 0.223726 0.026 Uiso 1 1 calc R U . . .
H12B H 0.450755 0.567239 0.241658 0.026 Uiso 1 1 calc R U . . .
C8 C 0.16776(19) 0.5867(2) 0.64490(19) 0.0259(5) Uani 1 1 d . . . . .
H8A H 0.116233 0.516050 0.654459 0.031 Uiso 1 1 calc R U . . .
H8B H 0.111710 0.623480 0.615773 0.031 Uiso 1 1 calc R U . . .
C9 C 0.2045(2) 0.4323(2) 0.47332(19) 0.0261(5) Uani 1 1 d . . . . .
H9A H 0.144883 0.451915 0.430999 0.031 Uiso 1 1 calc R U . . .
H9B H 0.158949 0.364412 0.489670 0.031 Uiso 1 1 calc R U . . .
C33 C 0.7258(2) 0.8458(2) 0.45710(19) 0.0255(5) Uani 1 1 d . . . . .
H33A H 0.779825 0.805222 0.483748 0.031 Uiso 1 1 calc R U . . .
H33B H 0.780081 0.912915 0.444741 0.031 Uiso 1 1 calc R U . . .
C32 C 0.6482(2) 0.7496(2) 0.35283(19) 0.0249(5) Uani 1 1 d . . . . .
H32A H 0.591328 0.788951 0.327457 0.030 Uiso 1 1 calc R U . . .
H32B H 0.702650 0.714983 0.295824 0.030 Uiso 1 1 calc R U . . .
C10 C 0.3087(2) 0.3902(2) 0.40942(19) 0.0244(5) Uani 1 1 d . . . . .
H10A H 0.371284 0.376960 0.454111 0.029 Uiso 1 1 calc R U . . .
H10B H 0.275986 0.309099 0.343709 0.029 Uiso 1 1 calc R U . . .
C7 C 0.2387(2) 0.6850(2) 0.75133(19) 0.0273(5) Uani 1 1 d . . . . .
H7A H 0.179814 0.719178 0.804192 0.033 Uiso 1 1 calc R U . . .
H7B H 0.292719 0.647276 0.781228 0.033 Uiso 1 1 calc R U . . .
C4 C 0.6267(2) 1.0333(2) 0.72079(19) 0.0263(5) Uani 1 1 d . . . . .
H4A H 0.674012 1.094044 0.792712 0.032 Uiso 1 1 calc R U . . .
H4B H 0.579187 1.079189 0.694566 0.032 Uiso 1 1 calc R U . . .
C2 C 0.2061(2) 0.7292(2) 0.41166(19) 0.0228(5) Uani 0.946(4) 1 d . . P A 1
H2A H 0.190526 0.636978 0.388321 0.027 Uiso 0.946(4) 1 calc R U P B 1
H2B H 0.180956 0.741832 0.348148 0.027 Uiso 0.946(4) 1 calc R U P B 1
C6 C 0.3967(2) 0.8718(2) 0.83012(19) 0.0333(6) Uani 1 1 d . . . . .
H6A H 0.456914 0.828744 0.846495 0.040 Uiso 1 1 calc R U . . .
H6B H 0.348794 0.903545 0.892884 0.040 Uiso 1 1 calc R U . . .
C5 C 0.4656(2) 0.9800(2) 0.8128(2) 0.0374(6) Uani 1 1 d . . . . .
H5A H 0.405525 1.018975 0.790510 0.045 Uiso 1 1 calc R U . . .
H5B H 0.516846 1.045295 0.881286 0.045 Uiso 1 1 calc R U . . .
C1 C 0.3428(2) 0.7867(2) 0.44873(19) 0.0214(5) Uani 0.946(4) 1 d . . P A 1
H1A H 0.388862 0.763320 0.384264 0.026 Uiso 0.946(4) 1 calc R U P B 1
H1B H 0.355683 0.880011 0.485445 0.026 Uiso 0.946(4) 1 calc R U P B 1
Br1A Br 0.0726(10) 0.8249(12) 0.4704(13) 0.067(5) Uani 0.0346(15) 1 d . . P C 3
C2A C 0.218(3) 0.848(4) 0.555(3) 0.023(7) Uani 0.054(4) 1 d . U P B 2
H2A1 H 0.190154 0.928558 0.577746 0.028 Uiso 0.054(4) 1 calc R U P B 2
H2A2 H 0.207449 0.822074 0.613570 0.028 Uiso 0.054(4) 1 calc R U P B 2
Br1 Br 0.1172(9) 0.7252(10) 0.4290(10) 0.069(4) Uani 0.0384(12) 1 d . . P B 2
C1A C 0.359(4) 0.871(4) 0.538(4) 0.028(6) Uani 0.054(4) 1 d . U P B 2
H1AD H 0.371395 0.883245 0.472225 0.034 Uiso 0.054(4) 1 calc R U P B 2
H1AE H 0.409594 0.945030 0.602176 0.034 Uiso 0.054(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 93.53(2) . . ?
S2 Ni1 S6 178.02(2) . . ?
S7 Ni1 S1 176.94(2) . . ?
S7 Ni1 S2 85.51(2) . . ?
S7 Ni1 S6 93.17(2) . . ?
S6 Ni1 S1 87.86(2) . . ?
C13 S1 Ni1 101.63(7) . . ?
C14 S2 Ni1 101.86(7) . . ?
C15 S3 C13 97.54(10) . . ?
C15 S4 C14 97.38(10) . . ?
C17 S7 Ni1 102.42(7) . . ?
C18 S9 C17 96.98(10) . . ?
C18 S8 C16 97.42(10) . . ?
C16 S6 Ni1 101.85(7) . . ?
C32 O6 C12 112.97(16) . . ?
C11 O5 C10 110.82(16) . . ?
C33 O1 C3 111.37(16) . . ?
C9 O4 C8 113.86(16) . . ?
C5 O2 C4 111.98(17) . . ?
C6 O3 C7 110.93(17) . . ?
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 122.52(12) . . ?
C14 C13 S1 121.69(15) . . ?
C14 C13 S3 115.75(14) . . ?
S4 C15 S3 113.02(10) . . ?
S5 C15 S3 123.57(12) . . ?
S5 C15 S4 123.40(12) . . ?
S2 C14 S4 122.39(12) . . ?
C13 C14 S2 121.29(14) . . ?
C13 C14 S4 116.31(15) . . ?
S7 C17 S9 121.89(13) . . ?
C16 C17 S7 121.07(15) . . ?
C16 C17 S9 117.04(15) . . ?
S9 C18 S8 113.35(11) . . ?
S10 C18 S9 122.99(13) . . ?
S10 C18 S8 123.66(13) . . ?
O5 C11 H11A 109.8 . . ?
O5 C11 H11B 109.8 . . ?
O5 C11 C12 109.22(17) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
S6 C16 S8 123.35(13) . . ?
C17 C16 S8 115.11(15) . . ?
C17 C16 S6 121.48(15) . . ?
O1 C3 H3A 109.9 . . ?
O1 C3 H3B 109.9 . . ?
O1 C3 C4 109.12(17) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
O6 C12 C11 108.22(17) . . ?
O6 C12 H12A 110.1 . . ?
O6 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O4 C8 H8A 110.2 . . ?
O4 C8 H8B 110.2 . . ?
O4 C8 C7 107.60(17) . . ?
H8A C8 H8B 108.5 . . ?
C7 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
O4 C9 C10 107.99(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 109.29(17) . . ?
H33A C33 H33B 108.3 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
O6 C32 C33 107.75(17) . . ?
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 109.17(18) . . ?
O5 C10 H10A 109.8 . . ?
O5 C10 H10B 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O3 C7 C8 108.75(18) . . ?
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 108.23(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 109.4 . . ?
Br1B C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 Br1B 111.39(16) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
O3 C6 H6A 109.8 . . ?
O3 C6 H6B 109.8 . . ?
O3 C6 C5 109.5(2) . . ?
H6A C6 H6B 108.2 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
O2 C5 C6 108.6(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 112.69(17) . . ?
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 . . ?
H2A1 C2A H2A2 107.8 . . ?
Br1 C2A H2A1 109.1 . . ?
Br1 C2A H2A2 109.1 . . ?
C1A C2A H2A1 109.1 . . ?
C1A C2A H2A2 109.1 . . ?
C1A C2A Br1 112(3) . . ?
N1 C1A C2A 103(3) . . ?
N1 C1A H1AD 111.2 . . ?
N1 C1A H1AE 111.2 . . ?
C2A C1A H1AD 111.2 . . ?
C2A C1A H1AE 111.2 . . ?
H1AD C1A H1AE 109.1 . . ?
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 2.1671(6) . ?
Ni1 S2 2.1616(5) . ?
Ni1 S7 2.1516(6) . ?
Ni1 S6 2.1664(6) . ?
Br1B C2 1.947(3) . ?
S1 C13 1.7175(19) . ?
S2 C14 1.720(2) . ?
S3 C13 1.7415(19) . ?
S3 C15 1.733(2) . ?
S4 C15 1.728(2) . ?
S4 C14 1.7412(19) . ?
S7 C17 1.712(2) . ?
S5 C15 1.6502(19) . ?
S9 C17 1.739(2) . ?
S9 C18 1.726(2) . ?
S8 C18 1.735(2) . ?
S8 C16 1.747(2) . ?
S6 C16 1.713(2) . ?
S10 C18 1.655(2) . ?
O6 C12 1.423(2) . ?
O6 C32 1.423(2) . ?
O5 C11 1.430(3) . ?
O5 C10 1.434(2) . ?
O1 C3 1.430(3) . ?
O1 C33 1.428(3) . ?
O4 C8 1.428(3) . ?
O4 C9 1.419(3) . ?
O2 C4 1.419(2) . ?
O2 C5 1.419(3) . ?
O3 C7 1.430(2) . ?
O3 C6 1.428(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 1.493(3) . ?
N1 C1A 1.58(4) . ?
C13 C14 1.358(3) . ?
C17 C16 1.358(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.505(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.488(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.493(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.491(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.495(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 1.500(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.495(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C2A Br1 1.86(4) . ?
C2A C1A 1.57(5) . ?
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 -178.75(10) . . . . ?
Ni1 S1 C13 C14 -1.14(18) . . . . ?
Ni1 S2 C14 S4 178.35(10) . . . . ?
Ni1 S2 C14 C13 -0.10(18) . . . . ?
Ni1 S7 C17 S9 -179.02(10) . . . . ?
Ni1 S7 C17 C16 1.27(18) . . . . ?
Ni1 S6 C16 S8 -177.13(11) . . . . ?
Ni1 S6 C16 C17 -0.09(19) . . . . ?
Br1B C2 C1 N1 73.4(2) . . . . ?
S1 C13 C14 S2 0.9(2) . . . . ?
S1 C13 C14 S4 -177.65(10) . . . . ?
S3 C13 C14 S2 178.65(10) . . . . ?
S3 C13 C14 S4 0.1(2) . . . . ?
S7 C17 C16 S8 176.42(11) . . . . ?
S7 C17 C16 S6 -0.8(3) . . . . ?
S9 C17 C16 S8 -3.3(2) . . . . ?
S9 C17 C16 S6 179.44(11) . . . . ?
O5 C11 C12 O6 62.1(2) . . . . ?
O1 C3 C4 O2 65.6(2) . . . . ?
O1 C33 C32 O6 -63.2(2) . . . . ?
O4 C8 C7 O3 58.9(2) . . . . ?
O4 C9 C10 O5 -65.0(2) . . . . ?
O3 C6 C5 O2 -65.5(3) . . . . ?
C13 S3 C15 S4 0.64(12) . . . . ?
C13 S3 C15 S5 179.83(13) . . . . ?
C15 S3 C13 S1 177.28(13) . . . . ?
C15 S3 C13 C14 -0.46(17) . . . . ?
C15 S4 C14 S2 -178.22(12) . . . . ?
C15 S4 C14 C13 0.30(17) . . . . ?
C14 S4 C15 S3 -0.59(12) . . . . ?
C14 S4 C15 S5 -179.78(13) . . . . ?
C17 S9 C18 S8 -2.05(13) . . . . ?
C17 S9 C18 S10 178.10(13) . . . . ?
C18 S9 C17 S7 -176.45(13) . . . . ?
C18 S9 C17 C16 3.27(18) . . . . ?
C18 S8 C16 S6 178.77(13) . . . . ?
C18 S8 C16 C17 1.56(18) . . . . ?
C11 O5 C10 C9 -173.24(17) . . . . ?
C16 S8 C18 S9 0.65(13) . . . . ?
C16 S8 C18 S10 -179.50(14) . . . . ?
C3 O1 C33 C32 170.57(17) . . . . ?
C12 O6 C32 C33 -170.41(17) . . . . ?
C8 O4 C9 C10 -175.30(17) . . . . ?
C9 O4 C8 C7 169.27(17) . . . . ?
C33 O1 C3 C4 178.73(17) . . . . ?
C32 O6 C12 C11 173.84(17) . . . . ?
C10 O5 C11 C12 -179.33(16) . . . . ?
C7 O3 C6 C5 -175.2(2) . . . . ?
C4 O2 C5 C6 -170.7(2) . . . . ?
C6 O3 C7 C8 -171.55(19) . . . . ?
C5 O2 C4 C3 173.44(19) . . . . ?
Br1 C2A C1A N1 -70(3) . . . . ?
