#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:14:42 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 265974 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/24/7242449.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_7242449
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, 1(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 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.3720(10)
_cell_angle_beta                 110.9960(10)
_cell_angle_gamma                96.4500(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2637(2)
_cell_length_b                   12.34200(10)
_cell_length_c                   12.8337(2)
_cell_measurement_reflns_used    28392
_cell_measurement_temperature    213
_cell_measurement_theta_max      72.4910
_cell_measurement_theta_min      3.6050
_cell_volume                     1651.13(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      213
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  71.00   0.50    0.50    --  -18.00  53.00  60.93  144
  2  ω   -104.00 -17.00   0.50    0.50    --  -18.00  53.00  60.93  174
  3  ω    -82.00 -56.00   0.50    0.50    --  -30.00  53.00 174.93   52
  4  ω     25.00  58.00   0.50    0.50    --  -30.00  53.00 174.93   66
  5  ω    -88.00 -63.00   0.50    0.50    --  -38.00  55.00 -52.83   50
  6  ω     22.00  50.00   0.50    0.50    --  -38.00  55.00 -52.83   56
  7  ω   -134.00 -88.00   0.50    0.50    --  -46.00  55.00 -90.71   92
  8  ω    -84.00   4.00   0.50    0.50    --  -46.00  55.00 -90.71  176
  9  ω     12.00  43.00   0.50    0.50    --  -46.00  55.00 -90.71   62
 10  ω     13.00  43.00   0.50    0.50    --  -46.00  55.00  38.00   60
 11  ω      9.00  39.00   0.50    0.50    --  -50.00  54.00  77.48   60
 12  ω      7.00  35.00   0.50    0.50    --  -54.00  55.00 146.66   56
 13  ω     -3.00  35.00   0.50    0.50    --  -54.00  55.00-174.84   76
 14  ω      2.00  31.00   0.50    0.50    --  -58.00  55.00  22.77   58
 15  ω     -6.00  26.00   0.50    0.50    --  -62.00  55.00-110.54   64
 16  ω    -11.00  27.00   0.50    0.50    --  -62.00  55.00   0.36   76
 17  ω      2.00  27.00   0.50    0.50    --  -62.00  55.00 -58.51   50
 18  ω     -2.00  27.00   0.50    0.50    --  -62.00  55.00 137.86   58
 19  ω   -138.00-112.00   0.50    0.50    --  -62.00  55.00   0.36   52
 20  ω      0.00  26.00   0.50    0.50    --  -62.00  55.00 -27.78   52
 21  ω    -64.00 -23.00   0.50    0.50    --  -62.00  55.00   0.36   82
 22  ω     -7.00  19.00   0.50    0.50    --  -70.00  54.00  91.98   52
 23  ω    -22.00  19.00   0.50    0.50    --  -70.00  55.00-153.98   82
 24  ω    -32.00  19.00   0.50    0.50    --  -70.00  55.00 116.69  102
 25  ω    -14.00  18.00   0.50    0.50    --  -70.00  55.00  75.10   64
 26  ω    -13.00  15.00   0.50    0.50    --  -74.00  52.00  38.56   56
 27  ω   -160.00-135.00   0.50    0.50    --  -74.00  52.00  38.56   50
 28  ω    -20.00  14.00   0.50    0.50    --  -74.00  55.00 -29.52   68
 29  ω    -17.00  10.00   0.50    0.50    --  -78.00  55.00 140.76   54
 30  ω    -76.00 -50.00   0.50    0.50    --  -78.00  55.00 140.76   52
 31  ω    -27.00  11.00   0.50    0.50    --  -78.00  54.00 -70.29   76
 32  ω    -32.00   6.00   0.50    0.50    --  -82.00  55.00  96.85   76
 33  ω    -23.00   5.00   0.50    0.50    --  -82.00  55.00-125.27   56
 34  ω    -24.00   7.00   0.50    0.50    --  -82.00  55.00-173.94   62
 35  ω    -20.00   7.00   0.50    0.50    --  -82.00  51.00-159.78   54
 36  ω   -129.00-103.00   0.50    0.50    --  -82.00  51.00-159.78   52
 37  ω    -24.00   7.00   0.50    0.50    --  -82.00  55.00-112.98   62
 38  ω    -43.00   3.00   0.50    0.50    --  -86.00  55.00 -36.76   92
 39  ω   -154.00-128.00   0.50    0.50    --  -86.00  55.00 -36.76   52
 40  ω   -178.00  -2.00   0.50    0.50    --  -90.00  54.00 134.64  352
 41  ω    -29.00  -1.00   0.50    0.50    --  -90.00  55.00  43.18   56
 42  ω    -29.00  -4.00   0.50    0.50    --  -90.00  52.00-158.22   50
 43  ω    -76.00 -50.00   0.50    0.50    --  -90.00  52.00-158.22   52
 44  ω    -99.00  -3.00   0.50    0.50    --  -90.00  50.00 163.25  192
 45  ω   -135.00-109.00   0.50    0.50    --  -90.00  50.00 163.25   52
 46  ω    -33.00  -1.00   0.50    0.50    --  -90.00  54.00  23.56   64
 47  ω    -92.00 -66.00   0.50    0.50    --  -90.00  54.00  23.56   52
 48  ω   -156.00-131.00   0.50    0.50    --  -90.00  54.00  23.56   50
 49  ω   -180.00-139.00   0.50    0.50    --  -94.70  55.00 -78.67   82
 50  ω   -166.00  -6.00   0.50    0.50    --  -94.70  55.00-176.23  320
 51  ω    -70.00 -32.00   0.50    0.50    --  -94.70   0.00 -60.00   76
 52  ω   -126.00-100.00   0.50    0.50    --  -94.70   0.00 -60.00   52
 53  ω   -123.00  -6.00   0.50    0.50    --  -94.70  55.00  62.17  234
 54  ω   -183.00-141.00   0.50    0.50    --  -94.70  55.00  62.17   84
 55  ω   -153.00  -5.00   0.50    0.50    --  -94.70  52.00 -98.91  296
 56  ω    -61.00  -5.00   0.50    0.50    --  -94.70  55.00 -62.11  112
 57  ω   -177.00  -5.00   0.50    0.50    --  -94.70  53.00  82.44  344
 58  ω   -132.00 -78.00   0.50    0.50    --  -94.70  55.00 -62.11  108
 59  ω   -183.00  -7.00   0.50    0.50    --  -94.70  55.00  -8.81  352
 60  ω   -113.00  -8.00   0.50    0.50    --  -94.70  55.00-123.56  210
 61  ω   -169.00-143.00   0.50    0.50    --  -94.70  55.00-123.56   52
 62  ω   -112.00  -5.00   0.50    0.50    --  -94.70  55.00 125.23  214
 63  ω   -175.00-149.00   0.50    0.50    --  -94.70  55.00 125.23   52
 64  ω   -123.00  -7.00   0.50    0.50    --  -94.70  54.00  11.95  232
 65  ω    -98.00  -5.00   0.50    0.50    --  -94.70  55.00 -78.67  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0737264000
_diffrn_orient_matrix_UB_12      -0.0641685000
_diffrn_orient_matrix_UB_13      -0.0556791000
_diffrn_orient_matrix_UB_21      0.1118378000
_diffrn_orient_matrix_UB_22      0.0035014000
_diffrn_orient_matrix_UB_23      0.1132271000
_diffrn_orient_matrix_UB_31      -0.0623292000
_diffrn_orient_matrix_UB_32      -0.1082864000
_diffrn_orient_matrix_UB_33      0.0262855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            42270
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.738
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0310
_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)+(0.0505P)²+0.3777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5870
_reflns_number_total             6349
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00253h3.cif
_cod_data_source_block           213k-f
_cod_depositor_comments
'Adding full bibliography for 7242434--7242480.cif.'
_cod_database_code               7242449
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H31NO6NiS10Cl
_chemical_oxdiff_usercomment     '213K friedel mates as non-equivalent'
_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.
;
_diffrn_oxdiff_digest_frames
;
013a4eda4640e4bdb21471fcaf4e14a3520670477a2
;
_diffrn_oxdiff_digest_hkl
;
0148df7b613291ed60056540b4060fcc91d988
;
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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(H20C)=Sof(H20D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(Cl)=1-FVAR(1)
 Sof(Cl18)=Sof(H20A)=Sof(H20B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O1A)=Sof(O23A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C27A)=Sof(H27C)=
 Sof(H27D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(O6A)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C40A)=Sof(H40C)=
 Sof(H40D)=Sof(O28A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C31A)=Sof(H31C)=Sof(H31D)=
 Sof(O2A)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(O3A)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(2)
 Sof(O23)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(O28)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(O6)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20(H20C,H20D), C30(H30A,H30B), C32(H32A,H32B), C22(H22A,
 H22B), C37(H37A,H37B), C19(H19A,H19B), C27(H27A,H27B), C40(H40A,H40B),
 C24(H24A,H24B), C31(H31A,H31B), C26(H26A,H26B), C19A(H19C,H19D), C8(H8A,H8B),
 C4(H4A,H4B), C1(H1A,H1B), C22A(H22C,H22D), C27A(H27C,H27D), C24A(H24C,H24D),
 C26A(H26C,H26D), C8A(H8AA,H8AB), C32A(H32C,H32D), C40A(H40C,H40D), C4A(H4AA,
 H4AB), C31A(H31C,H31D), C30A(H30C,H30D), C37A(H37C,H37D), C1A(H1AA,H1AB)
3.b Idealised Me refined as rotating group:
 N21(H21A,H21B,H21C)
;
_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 1.788
_oxdiff_exptl_absorpt_empirical_full_min 0.798
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 0.34530(2) 0.88988(2) 0.51227(2) 0.03758(9) Uani 1 1 d . . . . .
S6 S 0.11408(4) 1.02636(4) 0.72102(3) 0.04582(11) Uani 1 1 d . . . . .
S9 S 0.39844(4) 0.84359(4) 0.68262(3) 0.04695(11) Uani 1 1 d . . . . .
S7 S 0.19206(4) 0.97605(4) 0.52299(3) 0.04662(11) Uani 1 1 d . . . . .
S16 S 0.50579(4) 0.81186(4) 0.50739(3) 0.04632(11) Uani 1 1 d . . . . .
S15 S 0.29161(4) 0.93103(4) 0.34016(3) 0.04697(11) Uani 1 1 d . . . . .
S4 S 0.30176(4) 0.90197(4) 0.86615(3) 0.04904(12) Uani 1 1 d . . . . .
S13 S 0.59956(4) 0.77107(4) 0.31781(4) 0.05129(12) Uani 1 1 d . . . . .
S11 S 0.40899(5) 0.88813(4) 0.16617(3) 0.05067(12) Uani 1 1 d . . . . .
S8 S 0.12630(5) 1.00315(4) 0.95482(4) 0.05719(13) Uani 1 1 d . . . . .
S17 S 0.59019(5) 0.78658(5) 0.08458(4) 0.06295(14) Uani 1 1 d . . . . .
Cl18 Cl 0.6600(3) 0.54690(19) 0.4855(2) 0.0808(6) Uani 0.709(5) 1 d . . P A 1
N21 N 0.83440(14) 0.49778(11) 0.74474(11) 0.0443(3) Uani 1 1 d . . . . .
H21A H 0.811616 0.564282 0.731144 0.053 Uiso 1 1 calc GR . . . .
H21B H 0.910297 0.495188 0.738627 0.053 Uiso 1 1 calc GR . . . .
H21C H 0.839657 0.482912 0.813660 0.053 Uiso 1 1 calc GR . . . .
C3 C 0.29727(15) 0.90746(13) 0.72960(13) 0.0395(3) Uani 1 1 d . . . . .
C2 C 0.20869(15) 0.96556(13) 0.66072(13) 0.0387(3) Uani 1 1 d . . . . .
C12 C 0.53582(17) 0.81396(15) 0.18428(14) 0.0478(4) Uani 1 1 d . . . . .
C10 C 0.40407(16) 0.87836(13) 0.29987(13) 0.0413(3) Uani 1 1 d . . . . .
C5 C 0.17824(16) 0.97878(14) 0.85276(14) 0.0441(4) Uani 1 1 d . . . . .
C14 C 0.49551(15) 0.82496(13) 0.37201(13) 0.0410(3) Uani 1 1 d . . . . .
O23 O 0.8531(4) 0.3434(3) 0.9108(3) 0.0572(9) Uani 0.462(3) 1 d . . P B 1
C20 C 0.7369(2) 0.41589(16) 0.66259(16) 0.0605(5) Uani 1 1 d . . . . .
H20A H 0.653200 0.423496 0.665080 0.073 Uiso 0.709(5) 1 calc R . P A 1
H20B H 0.756144 0.343088 0.683734 0.073 Uiso 0.709(5) 1 calc R . P A 1
H20C H 0.776542 0.377997 0.619159 0.073 Uiso 0.291(5) 1 calc R . P A 2
H20D H 0.702195 0.362320 0.701716 0.073 Uiso 0.291(5) 1 calc R . P A 2
C30 C 0.8508(16) 0.7862(10) 0.6811(11) 0.059(3) Uani 0.462(3) 1 d . . P B 1
H30A H 0.780584 0.760259 0.612052 0.070 Uiso 0.462(3) 1 calc R . P B 1
H30B H 0.889616 0.857200 0.670182 0.070 Uiso 0.462(3) 1 calc R . P B 1
C32 C 0.6790(6) 0.7003(5) 0.8647(5) 0.0616(14) Uani 0.462(3) 1 d . . P B 1
H32A H 0.612456 0.747797 0.842682 0.074 Uiso 0.462(3) 1 calc R . P B 1
H32B H 0.743762 0.730356 0.935352 0.074 Uiso 0.462(3) 1 calc R . P B 1
C22 C 0.6853(9) 0.4209(9) 0.9471(7) 0.068(2) Uani 0.462(3) 1 d . . P B 1
H22A H 0.623535 0.379292 0.881130 0.082 Uiso 0.462(3) 1 calc R . P B 1
H22B H 0.645006 0.428438 1.001760 0.082 Uiso 0.462(3) 1 calc R . P B 1
C37 C 1.0992(15) 0.6310(13) 0.6574(12) 0.075(4) Uani 0.462(3) 1 d . . P B 1
H37A H 1.139988 0.630756 0.602470 0.090 Uiso 0.462(3) 1 calc R . P B 1
H37B H 1.163842 0.658462 0.729094 0.090 Uiso 0.462(3) 1 calc R . P B 1
C19 C 0.7325(4) 0.4281(2) 0.5454(2) 0.0671(10) Uani 0.709(5) 1 d . . P A 1
H19A H 0.684059 0.363119 0.499038 0.080 Uiso 0.709(5) 1 calc R . P A 1
H19B H 0.819080 0.433886 0.545361 0.080 Uiso 0.709(5) 1 calc R . P A 1
O28 O 0.7349(4) 0.6947(3) 0.7820(3) 0.0554(9) Uani 0.462(3) 1 d . . P B 1
C27 C 0.9675(10) 0.2943(7) 0.9532(7) 0.070(2) Uani 0.462(3) 1 d . . P B 1
H27A H 0.952074 0.228084 0.988132 0.084 Uiso 0.462(3) 1 calc R . P B 1
H27B H 1.033570 0.344000 1.009277 0.084 Uiso 0.462(3) 1 calc R . P B 1
C40 C 1.1490(6) 0.3927(6) 0.7665(7) 0.0723(18) Uani 0.462(3) 1 d . . P B 1
H40A H 1.227536 0.416137 0.829744 0.087 Uiso 0.462(3) 1 calc R . P B 1
H40B H 1.160489 0.324178 0.735084 0.087 Uiso 0.462(3) 1 calc R . P B 1
C24 C 0.8036(7) 0.3623(5) 0.9956(5) 0.0714(16) Uani 0.462(3) 1 d . . P B 1
H24A H 0.868007 0.406870 1.057843 0.086 Uiso 0.462(3) 1 calc R . P B 1
H24B H 0.780789 0.293381 1.022722 0.086 Uiso 0.462(3) 1 calc R . P B 1
C31 C 0.7999(5) 0.7972(4) 0.7749(4) 0.0646(14) Uani 0.462(3) 1 d . . P B 1
H31A H 0.870128 0.819281 0.845086 0.078 Uiso 0.462(3) 1 calc R . P B 1
H31B H 0.741722 0.852085 0.759485 0.078 Uiso 0.462(3) 1 calc R . P B 1
C26 C 1.0110(6) 0.2677(5) 0.8597(5) 0.0684(14) Uani 0.462(3) 1 d . . P B 1
H26A H 1.085626 0.229293 0.887064 0.082 Uiso 0.462(3) 1 calc R . P B 1
H26B H 0.943455 0.220724 0.801901 0.082 Uiso 0.462(3) 1 calc R . P B 1
C19A C 0.6373(6) 0.4692(6) 0.5907(6) 0.061(2) Uani 0.291(5) 1 d . . P A 2
H19C H 0.617657 0.526285 0.632814 0.074 Uiso 0.291(5) 1 calc R . P A 2
H19D H 0.560522 0.417340 0.556329 0.074 Uiso 0.291(5) 1 calc R . P A 2
Cl Cl 0.6888(7) 0.5266(6) 0.4860(4) 0.0854(17) Uani 0.291(5) 1 d . . P A 2
O1 O 0.7246(4) 0.5239(4) 0.9191(3) 0.0574(9) Uani 0.462(3) 1 d . . P B 1
O2 O 1.0471(4) 0.5257(4) 0.6650(3) 0.0616(9) Uani 0.462(3) 1 d . . P B 1
O3 O 0.9404(4) 0.7143(3) 0.7062(3) 0.0564(9) Uani 0.462(3) 1 d . . P B 1
O6 O 1.0420(4) 0.3660(3) 0.8149(3) 0.0554(9) Uani 0.462(3) 1 d . . P B 1
C8 C 0.6232(6) 0.5884(5) 0.8778(5) 0.0711(16) Uani 0.462(3) 1 d . . P B 1
H8A H 0.578535 0.591883 0.929618 0.085 Uiso 0.462(3) 1 calc R . P B 1
H8B H 0.562295 0.556283 0.806215 0.085 Uiso 0.462(3) 1 calc R . P B 1
C4 C 1.1432(7) 0.4543(6) 0.7017(5) 0.0744(17) Uani 0.462(3) 1 d . . P B 1
H4A H 1.139663 0.413282 0.635009 0.089 Uiso 0.462(3) 1 calc R . P B 1
H4B H 1.224848 0.500917 0.728536 0.089 Uiso 0.462(3) 1 calc R . P B 1
C1 C 0.9938(6) 0.7049(5) 0.6233(6) 0.0694(16) Uani 0.462(3) 1 d . . P B 1
H1A H 1.029013 0.776735 0.611064 0.083 Uiso 0.462(3) 1 calc R . P B 1
H1B H 0.927112 0.674963 0.553545 0.083 Uiso 0.462(3) 1 calc R . P B 1
O1A O 0.7089(3) 0.5847(3) 0.8832(3) 0.0567(7) Uani 0.538(3) 1 d . . P B 2
O23A O 0.7936(3) 0.3804(2) 0.9203(3) 0.0558(7) Uani 0.538(3) 1 d . . P B 2
C22A C 0.6387(6) 0.4973(5) 0.9152(4) 0.0695(12) Uani 0.538(3) 1 d . . P B 2
H22C H 0.577641 0.454965 0.849382 0.083 Uiso 0.538(3) 1 calc R . P B 2
H22D H 0.591906 0.525613 0.957973 0.083 Uiso 0.538(3) 1 calc R . P B 2
C27A C 0.8933(6) 0.3207(4) 0.9833(5) 0.0688(12) Uani 0.538(3) 1 d . . P B 2
H27C H 0.860029 0.266337 1.022632 0.083 Uiso 0.538(3) 1 calc R . P B 2
H27D H 0.961069 0.369957 1.038393 0.083 Uiso 0.538(3) 1 calc R . P B 2
C24A C 0.7346(8) 0.4256(7) 0.9862(6) 0.0649(18) Uani 0.538(3) 1 d . . P B 2
H24C H 0.798436 0.469076 1.049620 0.078 Uiso 0.538(3) 1 calc R . P B 2
H24D H 0.690716 0.367954 1.014250 0.078 Uiso 0.538(3) 1 calc R . P B 2
C26A C 0.9457(8) 0.2663(5) 0.9087(6) 0.0664(18) Uani 0.538(3) 1 d . . P B 2
H26C H 1.006999 0.219365 0.950796 0.080 Uiso 0.538(3) 1 calc R . P B 2
H26D H 0.877060 0.221378 0.849791 0.080 Uiso 0.538(3) 1 calc R . P B 2
C8A C 0.6323(5) 0.6623(5) 0.8237(5) 0.0579(12) Uani 0.538(3) 1 d . . P B 2
H8AA H 0.583764 0.688487 0.865944 0.069 Uiso 0.538(3) 1 calc R . P B 2
H8AB H 0.572244 0.629032 0.752264 0.069 Uiso 0.538(3) 1 calc R . P B 2
O6A O 1.0072(3) 0.3479(3) 0.8611(3) 0.0594(8) Uani 0.538(3) 1 d . . P B 2
C32A C 0.7180(4) 0.7546(4) 0.8058(4) 0.0565(11) Uani 0.538(3) 1 d . . P B 2
H32C H 0.668397 0.812555 0.772196 0.068 Uiso 0.538(3) 1 calc R . P B 2
H32D H 0.782299 0.783735 0.876993 0.068 Uiso 0.538(3) 1 calc R . P B 2
C40A C 1.0610(5) 0.3022(4) 0.7893(5) 0.0737(14) Uani 0.538(3) 1 d . . P B 2
H40C H 1.137592 0.273777 0.836839 0.088 Uiso 0.538(3) 1 calc R . P B 2
H40D H 1.000988 0.239574 0.748158 0.088 Uiso 0.538(3) 1 calc R . P B 2
O28A O 0.7787(2) 0.7175(2) 0.7344(2) 0.0492(7) Uani 0.538(3) 1 d . . P B 2
C4A C 1.0881(9) 0.3488(7) 0.7274(6) 0.0847(18) Uani 0.538(3) 1 d . . P B 2
H4AA H 1.042792 0.307952 0.655908 0.102 Uiso 0.538(3) 1 calc R . P B 2
H4AB H 1.178412 0.343651 0.744973 0.102 Uiso 0.538(3) 1 calc R . P B 2
C31A C 0.8578(14) 0.8049(10) 0.7121(10) 0.064(3) Uani 0.538(3) 1 d . . P B 2
H31C H 0.925559 0.835061 0.781001 0.077 Uiso 0.538(3) 1 calc R . P B 2
H31D H 0.807373 0.862471 0.678843 0.077 Uiso 0.538(3) 1 calc R . P B 2
O2A O 1.0715(4) 0.4706(3) 0.7056(3) 0.0650(8) Uani 0.538(3) 1 d . . P B 2
C30A C 0.9144(5) 0.7602(3) 0.6325(4) 0.0641(11) Uani 0.538(3) 1 d . . P B 2
H30C H 0.846381 0.727326 0.564865 0.077 Uiso 0.538(3) 1 calc R . P B 2
H30D H 0.964970 0.818787 0.611972 0.077 Uiso 0.538(3) 1 calc R . P B 2
C37A C 1.1493(5) 0.5646(5) 0.6913(4) 0.0737(13) Uani 0.538(3) 1 d . . P B 2
H37C H 1.202891 0.542773 0.651949 0.088 Uiso 0.538(3) 1 calc R . P B 2
H37D H 1.204800 0.598742 0.763925 0.088 Uiso 0.538(3) 1 calc R . P B 2
O3A O 0.9939(3) 0.6797(3) 0.6864(3) 0.0571(7) Uani 0.538(3) 1 d . . P B 2
C1A C 1.0640(12) 0.6456(11) 0.6250(9) 0.064(2) Uani 0.538(3) 1 d . . P B 2
H1AA H 1.116228 0.707891 0.611769 0.077 Uiso 0.538(3) 1 calc R . P B 2
H1AB H 1.006578 0.611179 0.553217 0.077 Uiso 0.538(3) 1 calc R . 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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
S9 Ni1 S7 93.102(17) . . ?
S9 Ni1 S16 86.034(17) . . ?
S9 Ni1 S15 178.26(2) . . ?
S16 Ni1 S7 176.68(2) . . ?
S15 Ni1 S7 87.930(17) . . ?
S15 Ni1 S16 93.014(17) . . ?
C5 S6 C2 97.47(8) . . ?
C3 S9 Ni1 102.29(5) . . ?
C2 S7 Ni1 101.98(6) . . ?
C14 S16 Ni1 102.19(6) . . ?
C10 S15 Ni1 102.36(6) . . ?
C5 S4 C3 97.35(8) . . ?
C12 S13 C14 97.59(8) . . ?
C12 S11 C10 97.46(8) . . ?
S9 C3 S4 122.49(9) . . ?
C2 C3 S9 121.17(12) . . ?
C2 C3 S4 116.33(12) . . ?
S7 C2 S6 123.02(9) . . ?
C3 C2 S6 115.71(12) . . ?
C3 C2 S7 121.27(12) . . ?
S13 C12 S11 113.06(9) . . ?
S17 C12 S13 123.26(11) . . ?
S17 C12 S11 123.68(11) . . ?
S15 C10 S11 123.09(10) . . ?
C14 C10 S15 121.01(13) . . ?
C14 C10 S11 115.90(12) . . ?
S6 C5 S4 113.10(9) . . ?
S8 C5 S6 123.49(10) . . ?
S8 C5 S4 123.42(10) . . ?
S16 C14 S13 122.68(10) . . ?
C10 C14 S16 121.39(13) . . ?
C10 C14 S13 115.93(12) . . ?
C24 O23 C27 111.1(6) . . ?
N21 C20 C19 112.67(18) . . ?
C19A C20 N21 109.5(3) . . ?
O3 C30 C31 110.4(9) . . ?
O28 C32 C8 109.3(5) . . ?
O1 C22 C24 108.0(6) . . ?
O2 C37 C1 109.7(11) . . ?
C20 C19 Cl18 112.6(2) . . ?
C31 O28 C32 111.0(5) . . ?
O23 C27 C26 109.4(6) . . ?
C4 C40 O6 122.9(6) . . ?
O23 C24 C22 108.8(6) . . ?
O28 C31 C30 108.0(6) . . ?
O6 C26 C27 109.1(5) . . ?
C20 C19A Cl 108.3(5) . . ?
C22 O1 C8 113.2(6) . . ?
C37 O2 C4 111.8(7) . . ?
C30 O3 C1 112.3(7) . . ?
C26 O6 C40 127.9(5) . . ?
O1 C8 C32 108.2(6) . . ?
C40 C4 O2 125.0(6) . . ?
O3 C1 C37 111.0(8) . . ?
C8A O1A C22A 113.5(5) . . ?
C24A O23A C27A 112.1(5) . . ?
O1A C22A C24A 107.7(5) . . ?
O23A C27A C26A 110.3(5) . . ?
O23A C24A C22A 108.7(5) . . ?
O6A C26A C27A 108.9(5) . . ?
O1A C8A C32A 108.3(4) . . ?
C40A O6A C26A 112.3(5) . . ?
O28A C32A C8A 109.6(4) . . ?
C4A C40A O6A 123.1(6) . . ?
C32A O28A C31A 111.0(6) . . ?
C40A C4A O2A 125.8(5) . . ?
O28A C31A C30A 107.9(8) . . ?
C37A O2A C4A 135.9(5) . . ?
O3A C30A C31A 108.7(7) . . ?
O2A C37A C1A 109.7(7) . . ?
C1A O3A C30A 112.3(6) . . ?
O3A C1A C37A 108.3(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 S9 2.1594(5) . ?
Ni1 S7 2.1691(5) . ?
Ni1 S16 2.1606(5) . ?
Ni1 S15 2.1606(5) . ?
S6 C2 1.7438(16) . ?
S6 C5 1.7300(17) . ?
S9 C3 1.7189(16) . ?
S7 C2 1.7191(16) . ?
S16 C14 1.7122(16) . ?
S15 C10 1.7126(17) . ?
S4 C3 1.7382(16) . ?
S4 C5 1.7311(17) . ?
S13 C12 1.7262(19) . ?
S13 C14 1.7426(16) . ?
S11 C12 1.7317(19) . ?
S11 C10 1.7431(16) . ?
S8 C5 1.6486(16) . ?
S17 C12 1.6473(17) . ?
Cl18 C19 1.812(4) . ?
N21 C20 1.486(2) . ?
C3 C2 1.360(2) . ?
C10 C14 1.360(2) . ?
O23 C27 1.418(11) . ?
O23 C24 1.414(7) . ?
C20 C19 1.498(3) . ?
C20 C19A 1.413(7) . ?
C30 C31 1.517(15) . ?
C30 O3 1.376(16) . ?
C32 O28 1.418(7) . ?
C32 C8 1.491(9) . ?
C22 C24 1.527(12) . ?
C22 O1 1.397(12) . ?
C37 O2 1.386(16) . ?
C37 C1 1.524(15) . ?
O28 C31 1.410(7) . ?
C27 C26 1.492(11) . ?
C40 O6 1.551(8) . ?
C40 C4 1.129(9) . ?
C26 O6 1.416(7) . ?
C19A Cl 1.776(9) . ?
O1 C8 1.418(8) . ?
O2 C4 1.427(9) . ?
O3 C1 1.406(7) . ?
O1A C22A 1.422(7) . ?
O1A C8A 1.412(6) . ?
O23A C27A 1.421(6) . ?
O23A C24A 1.390(10) . ?
C22A C24A 1.526(10) . ?
C27A C26A 1.476(10) . ?
C26A O6A 1.430(9) . ?
C8A C32A 1.486(7) . ?
O6A C40A 1.409(7) . ?
C32A O28A 1.419(5) . ?
C40A C4A 1.100(8) . ?
O28A C31A 1.422(14) . ?
C4A O2A 1.556(8) . ?
C31A C30A 1.508(13) . ?
O2A C37A 1.429(7) . ?
C30A O3A 1.433(6) . ?
C37A C1A 1.523(11) . ?
O3A C1A 1.388(14) . ?
