#------------------------------------------------------------------------------
#$Date: 2020-12-09 05:10:04 +0200 (Wed, 09 Dec 2020) $
#$Revision: 259689 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/58/7705861.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_7705861
loop_
_publ_author_name
'Li, Simin'
'Takahashi, Kiyonori'
'Hisaki, Ichiro'
'Kokado, Kenta'
'Nakamura, Takayoshi'
_publ_section_title
;
 One-dimensional DABCO hydrogen-bonding chain in a hexagonal channel of
 magnetic [Ni(dmit)₂].
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16772
_journal_page_last               16777
_journal_paper_doi               10.1039/d0dt03386c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'9(C6 Ni S10), 9(C6 H13 N2),(C6 H12 N2), 6(C2 H3 N)'
_chemical_formula_sum            'C126 H147 N26 Ni9 S90'
_chemical_formula_weight         5440.49
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-08-24 deposited with the CCDC.	2020-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.28410(10)
_cell_length_b                   15.28410(10)
_cell_length_c                   155.7874(9)
_cell_measurement_reflns_used    34615
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.4440
_cell_measurement_theta_min      2.5810
_cell_volume                     31516.8(3)
_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      223
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00 -41.90   0.15    0.37    --    0.00  55.00   0.00  294
  2  ω    -44.00  75.10   0.15    0.37    --    0.00  46.00 150.00  794
  3  ω    -81.00 -54.00   0.15    0.37    --    0.00  46.00 150.00  180
  4  ω   -115.00 -82.00   0.15    1.47    --  -94.70  46.00-180.00  220
  5  ω    -91.00 -64.00   0.15    1.47    --  -94.70   0.00-150.00  180
  6  ω   -184.00-154.00   0.15    1.47    --  -94.70  37.00   0.00  200
  7  ω   -113.00  -5.00   0.15    1.47    --  -94.70  18.00-180.00  720
  8  ω   -182.00-128.00   0.15    1.47    --  -94.70  18.00-180.00  360
  9  ω   -149.00  -9.95   0.15    1.47    --  -94.70  37.00   0.00  927
 10  ω   -184.00-124.90   0.15    1.47    --  -94.70   0.00-150.00  394
 11  ω    -47.00  -5.90   0.15    1.47    --  -94.70  46.00-180.00  274
 12  ω    -65.00 -40.85   0.15    1.47    --  -94.70  28.00 150.00  161
 13  ω    -36.00  -9.90   0.15    1.47    --  -94.70  28.00 150.00  174
 14  ω   -173.00-148.85   0.15    1.47    --  -94.70  46.00-180.00  161
 15  ω    -71.00 -33.05   0.15    1.47    --  -94.70   0.00-120.00  253
 16  ω   -181.00  -5.95   0.15    1.47    --  -94.70  37.00  30.00 1167
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0025562000
_diffrn_orient_matrix_UB_12      -0.1020407000
_diffrn_orient_matrix_UB_13      -0.0001209000
_diffrn_orient_matrix_UB_21      -0.0301031000
_diffrn_orient_matrix_UB_22      -0.0156589000
_diffrn_orient_matrix_UB_23      0.0095524000
_diffrn_orient_matrix_UB_31      -0.1123990000
_diffrn_orient_matrix_UB_32      -0.0537390000
_diffrn_orient_matrix_UB_33      -0.0025564000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       188
_diffrn_reflns_limit_l_min       -190
_diffrn_reflns_number            74900
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.848
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    9.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44869
_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            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       plate
_exptl_crystal_F_000             16668
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         13824
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0754P)²+47.9327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12117
_reflns_number_total             13824
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03386c2.cif
_cod_data_source_block           1_223K
_cod_original_cell_volume        31516.8(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7705861
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N OSNi'
_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   0.573
_shelx_estimated_absorpt_t_min   0.254
_diffrn_oxdiff_digest_frames
;
01e646be389c07ffc9572f06043232c87d064598ea3
;
_diffrn_oxdiff_digest_hkl
;
018edb8cc00981a54a7c6bace09cef8b5e0f32
;
_reflns_odcompleteness_completeness 99.98
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-N15
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: H18(0.16667) H17(0.16667) H19(0.16667) H42A(0.33333) H42B(0.33333)
 H42C(0.33333) H20(0.16667) H44A(0.33333) H44B(0.33333) H44C(0.33333)
 H40A(0.33333) H40B(0.33333) H40C(0.33333) H16(0.16667) H15(0.16667)
5.a Ternary CH refined with riding coordinates:
 N18(H18), N12(H12), N17(H17), N14(H14), N4(H4), N6(H6), N19(H19), N8(H8),
 N20(H20), N9(H9), N1(H1), N16(H16), N15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C36(H36A,H36B), C29(H29A,H29B), C23(H23A,H23B), C35(H35A,
 H35B), C22(H22A,H22B), C24(H24A,H24B), C31(H31A,H31B), C21(H21A,H21B),
 C37(H37A,H37B), C32(H32A,H32B), C38(H38A,H38B), C25(H25A,H25B), C26(H26A,H26B),
  C19(H19A,H19B), C20(H20A,H20B), C34(H34A,H34B), C27(H27A,H27B), C28(H28A,
 H28B), C33(H33A,H33B)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C46(H46A,H46B,
 H46C)
;
_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 1.975
_oxdiff_exptl_absorpt_empirical_full_min 0.759
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.36807(3) -0.00275(3) 0.67292(2) 0.03450(10) Uani 1 1 d . . . . .
Ni3 Ni 0.39508(3) -0.00772(3) 0.56093(2) 0.03667(11) Uani 1 1 d . . . . .
Ni2 Ni 0.32465(3) 0.26493(3) 0.54939(2) 0.03826(11) Uani 1 1 d . . . . .
S6 S 0.30708(5) 0.04788(5) 0.66274(2) 0.03971(13) Uani 1 1 d . . . . .
S7 S 0.43855(5) -0.05697(5) 0.66399(2) 0.04207(14) Uani 1 1 d . . . . .
S4 S 0.30323(5) 0.05639(5) 0.68203(2) 0.04154(14) Uani 1 1 d . . . . .
S27 S 0.27990(4) -0.07227(5) 0.55108(2) 0.04195(14) Uani 1 1 d . . . . .
S26 S 0.51653(4) 0.05654(5) 0.55164(2) 0.04474(15) Uani 1 1 d . . . . .
S14 S 0.26303(5) 0.31696(5) 0.55942(2) 0.04215(14) Uani 1 1 d . . . . .
S5 S 0.43270(5) -0.05154(5) 0.68292(2) 0.04321(14) Uani 1 1 d . . . . .
S25 S 0.27497(4) -0.07469(5) 0.57050(2) 0.04319(14) Uani 1 1 d . . . . .
S15 S 0.38667(5) 0.20333(5) 0.55848(2) 0.04486(15) Uani 1 1 d . . . . .
S24 S 0.51395(5) 0.05583(5) 0.57048(2) 0.04700(15) Uani 1 1 d . . . . .
S16 S 0.25893(5) 0.32184(5) 0.54015(2) 0.04688(15) Uani 1 1 d . . . . .
S8 S 0.31751(5) 0.03425(5) 0.64335(2) 0.04697(15) Uani 1 1 d . . . . .
S17 S 0.38587(6) 0.21124(5) 0.53948(2) 0.05021(16) Uani 1 1 d . . . . .
S12 S 0.27341(5) 0.30665(5) 0.57885(2) 0.04867(15) Uani 1 1 d . . . . .
S9 S 0.44025(5) -0.06053(6) 0.64458(2) 0.04970(16) Uani 1 1 d . . . . .
S13 S 0.38514(6) 0.20035(5) 0.57795(2) 0.05199(17) Uani 1 1 d . . . . .
S29 S 0.29633(5) -0.05982(6) 0.53161(2) 0.05140(16) Uani 1 1 d . . . . .
S28 S 0.51442(5) 0.05728(6) 0.53224(2) 0.05310(17) Uani 1 1 d . . . . .
S2 S 0.30306(7) 0.05612(6) 0.70153(2) 0.05887(19) Uani 1 1 d . . . . .
S23 S 0.28760(6) -0.07260(6) 0.59002(2) 0.05580(18) Uani 1 1 d . . . . .
S22 S 0.50529(6) 0.04578(7) 0.58984(2) 0.0615(2) Uani 1 1 d . . . . .
S3 S 0.42452(7) -0.03972(7) 0.70230(2) 0.0616(2) Uani 1 1 d . . . . .
S18 S 0.27149(8) 0.33284(8) 0.52072(2) 0.0709(2) Uani 1 1 d . . . . .
S11 S 0.32658(7) 0.24154(7) 0.59506(2) 0.0718(2) Uani 1 1 d . . . . .
S19 S 0.38624(8) 0.22959(8) 0.52012(2) 0.0752(3) Uani 1 1 d . . . . .
S10 S 0.39166(8) -0.01475(9) 0.62735(2) 0.0776(3) Uani 1 1 d . . . . .
S30 S 0.41324(9) -0.00188(9) 0.51528(2) 0.0843(3) Uani 1 1 d . . . . .
S21 S 0.40010(10) -0.01592(10) 0.60661(2) 0.0909(3) Uani 1 1 d . . . . .
S1 S 0.35659(13) 0.00866(11) 0.71860(2) 0.1063(4) Uani 1 1 d . . . . .
S20 S 0.33864(15) 0.29815(15) 0.50384(2) 0.1351(6) Uani 1 1 d . . . . .
N18 N 0.000000 0.000000 0.55873(3) 0.0557(10) Uani 1 3 d S T P . .
H18 H 0.000006 0.000001 0.565082 0.067 Uiso 0.5 3 calc RS T P A 2
N12 N 0.666667 0.333333 0.65662(3) 0.0559(11) Uani 1 3 d S T P . .
H12 H 0.666671 0.333337 0.662971 0.067 Uiso 1 3 calc RS T P . .
N17 N 0.000000 0.000000 0.54252(3) 0.0610(11) Uani 1 3 d S T P . .
H17 H 0.000012 0.000000 0.536161 0.073 Uiso 0.5 3 calc RS T P B 1
N14 N 0.666667 0.333333 0.69049(4) 0.0628(12) Uani 1 3 d S T P . .
H14 H 0.666665 0.333346 0.696849 0.075 Uiso 1 3 calc RS T P . .
N4 N 0.333333 0.666667 0.54863(4) 0.0613(12) Uani 1 3 d S T P . .
H4 H 0.333332 0.666674 0.554989 0.074 Uiso 1 3 calc RS T P . .
N5 N 0.333333 0.666667 0.56688(3) 0.0616(12) Uani 1 3 d S T P . .
N6 N 0.333333 0.666667 0.58318(4) 0.0649(12) Uani 1 3 d S T P . .
H6 H 0.333333 0.666681 0.589539 0.078 Uiso 1 3 calc RS T P . .
N11 N 0.666667 0.333333 0.64032(4) 0.0692(13) Uani 1 3 d S T P . .
N13 N 0.666667 0.333333 0.67426(4) 0.0595(12) Uani 1 3 d S T P . .
C4 C 0.40374(17) -0.03216(18) 0.65428(2) 0.0390(5) Uani 1 1 d . . . . .
C5 C 0.34583(17) 0.01286(17) 0.65369(2) 0.0369(5) Uani 1 1 d . . . . .
N19 N 0.000000 0.000000 0.57609(4) 0.0632(12) Uani 1 3 d S T P . .
H19 H 0.000012 0.000000 0.569731 0.076 Uiso 0.5 3 calc RS T P C 1
C15 C 0.3442(2) -0.04000(19) 0.57991(2) 0.0425(5) Uani 1 1 d . . . . .
C3 C 0.33787(19) 0.02868(19) 0.69172(2) 0.0408(5) Uani 1 1 d . . . . .
C8 C 0.35250(19) 0.23101(18) 0.56813(2) 0.0414(5) Uani 1 1 d . . . . .
C16 C 0.45265(19) 0.02326(18) 0.54212(2) 0.0410(5) Uani 1 1 d . . . . .
C9 C 0.29900(18) 0.28066(18) 0.56855(2) 0.0401(5) Uani 1 1 d . . . . .
C14 C 0.4462(2) 0.0160(2) 0.57986(2) 0.0440(5) Uani 1 1 d . . . . .
C2 C 0.39433(19) -0.01676(19) 0.69207(2) 0.0418(5) Uani 1 1 d . . . . .
C17 C 0.35016(19) -0.03240(18) 0.54183(2) 0.0402(5) Uani 1 1 d . . . . .
N3 N 0.333333 0.666667 0.53238(4) 0.0716(14) Uani 1 3 d S T P . .
N7 N 0.333333 0.666667 0.60166(3) 0.0707(13) Uani 1 3 d S T P . .
C42 C 0.333333 0.666667 0.65277(3) 0.0578(12) Uani 1 3 d S T P . .
H42A H 0.270007 0.658932 0.654842 0.087 Uiso 0.3333 1 calc GR . . D -1
H42B H 0.388925 0.729993 0.654842 0.087 Uiso 0.3333 1 calc GR . . D -1
H42C H 0.341068 0.611075 0.654842 0.087 Uiso 0.3333 1 calc GR . . D -1
C10 C 0.3509(2) 0.2475(2) 0.53031(2) 0.0502(6) Uani 1 1 d . . . . .
C11 C 0.2962(2) 0.2954(2) 0.53057(2) 0.0497(6) Uani 1 1 d . . . . .
N8 N 0.333333 0.666667 0.61786(3) 0.0720(13) Uani 1 3 d S T P . .
H8 H 0.333335 0.666666 0.624215 0.086 Uiso 1 3 calc RS T P . .
C41 C 0.333333 0.666667 0.64349(4) 0.0594(13) Uani 1 3 d S T P . .
C7 C 0.3286(2) 0.2490(2) 0.58454(2) 0.0498(6) Uani 1 1 d . . . . .
N20 N 0.000000 0.000000 0.59246(4) 0.0761(14) Uani 1 3 d S T P . .
H20 H 0.000010 -0.000001 0.598810 0.091 Uiso 0.5 3 calc RS T P E 2
N22 N 0.333333 0.666667 0.63618(3) 0.0846(16) Uani 1 3 d S T P . .
C30 C 0.5848(2) 0.2330(2) 0.65339(2) 0.0630(8) Uani 1 1 d . . . . .
H30A H 0.518820 0.220174 0.655444 0.076 Uiso 1 1 calc R . . . .
H30B H 0.595800 0.178820 0.655500 0.076 Uiso 1 1 calc R . . . .
N23 N 0.666667 0.333333 0.58493(4) 0.104(2) Uani 1 3 d S T P . .
C6 C 0.3825(2) -0.0144(2) 0.63785(2) 0.0508(6) Uani 1 1 d . . . . .
C36 C 0.0944(2) 0.0070(2) 0.55551(2) 0.0657(9) Uani 1 1 d . . . . .
H36A H 0.100714 -0.049339 0.557789 0.079 Uiso 1 1 calc R . . . .
H36B H 0.152533 0.070147 0.557521 0.079 Uiso 1 1 calc R . . . .
N21 N 0.333333 0.666667 0.47576(5) 0.112(2) Uani 1 3 d S T P . .
C29 C 0.5874(3) 0.2355(2) 0.64362(3) 0.0729(10) Uani 1 1 d . . . . .
H29A H 0.599374 0.181973 0.641497 0.087 Uiso 1 1 calc R . . . .
H29B H 0.521703 0.222045 0.641439 0.087 Uiso 1 1 calc R . . . .
C18 C 0.4085(2) -0.0011(2) 0.52583(2) 0.0548(7) Uani 1 1 d . . . . .
C23 C 0.3444(2) 0.5818(2) 0.57025(2) 0.0675(9) Uani 1 1 d . . . . .
H23A H 0.409708 0.590516 0.568445 0.081 Uiso 1 1 calc R . . . .
H23B H 0.291053 0.517998 0.567851 0.081 Uiso 1 1 calc R . . . .
C13 C 0.3982(3) -0.0133(3) 0.59602(2) 0.0620(8) Uani 1 1 d . . . . .
C39 C 0.333333 0.666667 0.46851(6) 0.0828(19) Uani 1 3 d S T P . .
C35 C 0.0943(2) 0.0041(3) 0.54568(3) 0.0691(9) Uani 1 1 d . . . . .
H35A H 0.153728 0.064500 0.543443 0.083 Uiso 1 1 calc R . . . .
H35B H 0.096806 -0.055476 0.543705 0.083 Uiso 1 1 calc R . . . .
C22 C 0.3440(3) 0.5801(2) 0.54545(3) 0.0704(9) Uani 1 1 d . . . . .
H22A H 0.288611 0.516189 0.547645 0.085 Uiso 1 1 calc R . . . .
H22B H 0.408011 0.587010 0.547453 0.085 Uiso 1 1 calc R . . . .
C24 C 0.3378(3) 0.5775(2) 0.57999(2) 0.0689(9) Uani 1 1 d . . . . .
H24A H 0.277248 0.515244 0.581806 0.083 Uiso 1 1 calc R . . . .
H24B H 0.397036 0.577394 0.582394 0.083 Uiso 1 1 calc R . . . .
C31 C 0.6516(2) 0.4159(2) 0.67751(2) 0.0645(8) Uani 1 1 d . . . . .
H31A H 0.586441 0.405717 0.675502 0.077 Uiso 1 1 calc R . . . .
H31B H 0.704871 0.480674 0.675255 0.077 Uiso 1 1 calc R . . . .
C21 C 0.3416(3) 0.5808(2) 0.53560(3) 0.0761(10) Uani 1 1 d . . . . .
H21A H 0.403412 0.584826 0.533349 0.091 Uiso 1 1 calc R . . . .
H21B H 0.283941 0.517591 0.533548 0.091 Uiso 1 1 calc R . . . .
C1 C 0.3607(3) 0.0080(3) 0.70801(2) 0.0669(8) Uani 1 1 d . . . . .
C37 C 0.0925(2) 0.0004(3) 0.57945(3) 0.0723(10) Uani 1 1 d . . . . .
H37A H 0.153133 0.064331 0.577981 0.087 Uiso 1 1 calc R . . . .
H37B H 0.098268 -0.054833 0.576836 0.087 Uiso 1 1 calc R . . . .
C44 C 0.666667 0.333333 0.56840(4) 0.0717(16) Uani 1 3 d S T P . .
H44A H 0.598359 0.290191 0.566322 0.107 Uiso 0.3333 1 calc GR . . F -1
H44B H 0.709809 0.308168 0.566322 0.107 Uiso 0.3333 1 calc GR . . F -1
H44C H 0.691832 0.401641 0.566322 0.107 Uiso 0.3333 1 calc GR . . F -1
C32 C 0.6542(3) 0.4187(2) 0.68726(3) 0.0701(9) Uani 1 1 d . . . . .
H32A H 0.710519 0.483250 0.689241 0.084 Uiso 1 1 calc R . . . .
H32B H 0.591236 0.412294 0.689482 0.084 Uiso 1 1 calc R . . . .
C38 C 0.0834(3) -0.0127(3) 0.58917(3) 0.0790(10) Uani 1 1 d . . . . .
H38A H 0.071265 -0.080101 0.590683 0.095 Uiso 1 1 calc R . . . .
H38B H 0.146911 0.037308 0.591866 0.095 Uiso 1 1 calc R . . . .
C43 C 0.666667 0.333333 0.57763(5) 0.0783(18) Uani 1 3 d S T P . .
C40 C 0.333333 0.666667 0.45916(5) 0.0756(17) Uani 1 3 d S T P . .
H40A H 0.269225 0.612301 0.457083 0.113 Uiso 0.3333 1 calc GR . . G -1
H40B H 0.387699 0.656924 0.457083 0.113 Uiso 0.3333 1 calc GR . . G -1
H40C H 0.343076 0.730775 0.457083 0.113 Uiso 0.3333 1 calc GR . . G -1
N9 N 0.666667 0.333333 0.60397(4) 0.103(2) Uani 1 3 d S T P . .
H9 H 0.666676 0.333336 0.597617 0.124 Uiso 1 3 calc RS T P . .
N1 N 0.333333 0.666667 0.49487(5) 0.124(3) Uani 1 3 d S T P . .
H1 H 0.333333 0.666675 0.488513 0.149 Uiso 1 3 calc RS T P . .
C25 C 0.2536(3) 0.6851(3) 0.60492(2) 0.0784(10) Uani 1 1 d . . . . .
H25A H 0.187660 0.631761 0.602866 0.094 Uiso 1 1 calc R . . . .
H25B H 0.264422 0.749818 0.602700 0.094 Uiso 1 1 calc R . . . .
C26 C 0.2537(3) 0.6872(4) 0.61480(2) 0.0810(11) Uani 1 1 d . . . . .
H26A H 0.267239 0.753542 0.616836 0.097 Uiso 1 1 calc R . . . .
H26B H 0.187631 0.635859 0.616999 0.097 Uiso 1 1 calc R . . . .
C12 C 0.3327(4) 0.2868(3) 0.51437(2) 0.0833(11) Uani 1 1 d . . . . .
C45 C 0.5138(4) 0.3183(4) 0.71212(4) 0.1004(14) Uani 1 1 d . . . . .
N24 N 0.5334(4) 0.3156(5) 0.70531(4) 0.142(2) Uani 1 1 d . . . . .
N2 N 0.333333 0.666667 0.51055(7) 0.164(4) Uani 1 3 d S T P . .
C19 C 0.3378(6) 0.5778(5) 0.49819(5) 0.169(3) Uani 1 1 d . . . . .
H19A H 0.284929 0.515671 0.495526 0.203 Uiso 1 1 calc R . . . .
H19B H 0.403552 0.584439 0.496861 0.203 Uiso 1 1 calc R . . . .
C20 C 0.3227(7) 0.5740(6) 0.50763(5) 0.176(4) Uani 1 1 d . . . . .
H20A H 0.255184 0.518460 0.509067 0.211 Uiso 1 1 calc R . . . .
H20B H 0.372569 0.561533 0.510485 0.211 Uiso 1 1 calc R . . . .
C46 C 0.4941(7) 0.3239(7) 0.72084(4) 0.186(4) Uani 1 1 d . . . . .
H46A H 0.423015 0.278360 0.721990 0.279 Uiso 1 1 calc GR . . . .
H46B H 0.511153 0.392488 0.722236 0.279 Uiso 1 1 calc GR . . . .
H46C H 0.534478 0.304729 0.724313 0.279 Uiso 1 1 calc GR . . . .
N10 N 0.666667 0.333333 0.61961(10) 0.293(14) Uani 1 3 d S T P . .
C34 C -0.0979(6) -0.1093(6) 0.52251(6) 0.188(4) Uani 1 1 d . U . . .
H34A H -0.157402 -0.118535 0.525664 0.225 Uiso 1 1 calc R . . . .
H34B H -0.085098 -0.163596 0.524237 0.225 Uiso 1 1 calc R . . . .
C27 C 0.5665(5) 0.3020(8) 0.60728(6) 0.195(4) Uani 1 1 d . . . . .
H27A H 0.517727 0.234357 0.605193 0.234 Uiso 1 1 calc R . . . .
H27B H 0.544318 0.349220 0.605451 0.234 Uiso 1 1 calc R . . . .
C28 C 0.5744(8) 0.3020(12) 0.61670(6) 0.269(7) Uani 1 1 d . . . . .
H28A H 0.550189 0.345291 0.619091 0.323 Uiso 1 1 calc R . . . .
H28B H 0.529765 0.233179 0.618793 0.323 Uiso 1 1 calc R . . . .
N16 N 0.000000 0.000000 0.52524(10) 0.199(5) Uani 1 3 d S T P . .
H16 H -0.000003 -0.000004 0.531592 0.239 Uiso 0.5 3 calc RS T P H 2
N15 N 0.000000 0.000000 0.50893(12) 0.267(9) Uani 1 3 d DS T P . .
H15 H 0.000001 0.000001 0.502571 0.321 Uiso 0.1667 1 calc RS T P I -1
C33 C -0.1231(9) -0.1194(8) 0.51187(6) 0.249(6) Uani 1 1 d D U . . .
H33A H -0.183160 -0.114608 0.510487 0.299 Uiso 1 1 calc R . . . .
H33B H -0.128581 -0.180597 0.509336 0.299 Uiso 1 1 calc R . . . .
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'
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'
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
S6 Ni1 S4 87.85(3) . . ?
S7 Ni1 S6 92.95(3) . . ?
S7 Ni1 S4 177.74(4) . . ?
S7 Ni1 S5 86.04(3) . . ?
S5 Ni1 S6 178.54(3) . . ?
S5 Ni1 S4 93.12(3) . . ?
S27 Ni3 S25 88.23(3) . . ?
S27 Ni3 S24 177.87(3) . . ?
S26 Ni3 S27 92.86(3) . . ?
S26 Ni3 S25 178.22(3) . . ?
S26 Ni3 S24 85.37(3) . . ?
S24 Ni3 S25 93.51(3) . . ?
S14 Ni2 S16 87.60(3) . . ?
S15 Ni2 S14 93.04(3) . . ?
S15 Ni2 S16 178.17(4) . . ?
S15 Ni2 S17 86.31(3) . . ?
S17 Ni2 S14 179.23(3) . . ?
S17 Ni2 S16 93.04(3) . . ?
C5 S6 Ni1 102.27(8) . . ?
C4 S7 Ni1 102.38(9) . . ?
C3 S4 Ni1 102.14(9) . . ?
C17 S27 Ni3 102.21(9) . . ?
C16 S26 Ni3 102.30(9) . . ?
C9 S14 Ni2 102.15(9) . . ?
C2 S5 Ni1 101.82(9) . . ?
C15 S25 Ni3 101.11(9) . . ?
C8 S15 Ni2 102.28(9) . . ?
C14 S24 Ni3 101.75(10) . . ?
C11 S16 Ni2 102.02(10) . . ?
C6 S8 C5 97.31(13) . . ?
C10 S17 Ni2 102.01(10) . . ?
C7 S12 C9 97.63(13) . . ?
C6 S9 C4 97.60(13) . . ?
C7 S13 C8 97.69(13) . . ?
C18 S29 C17 97.11(14) . . ?
C18 S28 C16 97.38(14) . . ?
C1 S2 C3 97.35(14) . . ?
C13 S23 C15 97.05(15) . . ?
C13 S22 C14 97.49(15) . . ?
C1 S3 C2 97.10(14) . . ?
C12 S18 C11 96.88(17) . . ?
C12 S19 C10 97.52(16) . . ?
C36 N18 C36 109.2(2) 3 2 ?
C36 N18 C36 109.2(2) 2 . ?
C36 N18 C36 109.2(2) 3 . ?
C30 N12 C30 109.4(2) 2_655 . ?
C30 N12 C30 109.4(2) 2_655 3_665 ?
C30 N12 C30 109.4(2) . 3_665 ?
C35 N17 C35 109.7(3) 3 2 ?
C35 N17 C35 109.7(3) 3 . ?
C35 N17 C35 109.7(3) 2 . ?
C32 N14 C32 109.3(3) 3_665 2_655 ?
C32 N14 C32 109.3(3) 3_665 . ?
C32 N14 C32 109.3(3) 2_655 . ?
C22 N4 C22 109.6(3) 3_565 2_665 ?
C22 N4 C22 109.6(3) . 2_665 ?
C22 N4 C22 109.6(3) 3_565 . ?
C23 N5 C23 108.2(3) 3_565 2_665 ?
C23 N5 C23 108.2(3) 3_565 . ?
C23 N5 C23 108.2(3) 2_665 . ?
C24 N6 C24 109.4(3) . 2_665 ?
C24 N6 C24 109.4(3) 3_565 2_665 ?
C24 N6 C24 109.4(3) . 3_565 ?
C29 N11 C29 108.4(3) 2_655 . ?
C29 N11 C29 108.4(3) 2_655 3_665 ?
C29 N11 C29 108.4(3) . 3_665 ?
C31 N13 C31 108.9(3) 2_655 . ?
C31 N13 C31 108.9(3) 3_665 . ?
C31 N13 C31 108.9(3) 3_665 2_655 ?
S7 C4 S9 122.67(15) . . ?
C5 C4 S7 121.54(18) . . ?
C5 C4 S9 115.79(18) . . ?
S6 C5 S8 123.02(14) . . ?
C4 C5 S6 120.82(18) . . ?
C4 C5 S8 116.14(18) . . ?
C37 N19 C37 108.6(3) 3 . ?
C37 N19 C37 108.6(3) 2 . ?
C37 N19 C37 108.6(3) 2 3 ?
S25 C15 S23 122.49(16) . . ?
C14 C15 S25 121.7(2) . . ?
C14 C15 S23 115.8(2) . . ?
S4 C3 S2 122.89(15) . . ?
C2 C3 S4 121.07(19) . . ?
C2 C3 S2 116.04(19) . . ?
S15 C8 S13 122.68(15) . . ?
C9 C8 S15 121.34(19) . . ?
C9 C8 S13 115.97(19) . . ?
S26 C16 S28 122.29(15) . . ?
C17 C16 S26 121.55(19) . . ?
C17 C16 S28 116.16(19) . . ?
S14 C9 S12 123.02(15) . . ?
C8 C9 S14 121.19(19) . . ?
C8 C9 S12 115.78(19) . . ?
S24 C14 S22 121.72(16) . . ?
C15 C14 S24 121.9(2) . . ?
C15 C14 S22 116.3(2) . . ?
S5 C2 S3 121.93(15) . . ?
C3 C2 S5 121.8(2) . . ?
C3 C2 S3 116.2(2) . . ?
S27 C17 S29 123.00(15) . . ?
C16 C17 S27 121.04(19) . . ?
C16 C17 S29 115.96(19) . . ?
C21 N3 C21 109.0(3) 2_665 . ?
C21 N3 C21 109.0(3) 3_565 . ?
C21 N3 C21 109.0(3) 3_565 2_665 ?
C25 N7 C25 108.8(2) . 3_565 ?
C25 N7 C25 108.8(2) 3_565 2_665 ?
C25 N7 C25 108.8(2) . 2_665 ?
S17 C10 S19 122.53(17) . . ?
C11 C10 S17 121.7(2) . . ?
C11 C10 S19 115.8(2) . . ?
S16 C11 S18 122.47(17) . . ?
C10 C11 S16 121.2(2) . . ?
C10 C11 S18 116.3(2) . . ?
C26 N8 C26 110.1(2) . 2_665 ?
C26 N8 C26 110.1(2) . 3_565 ?
C26 N8 C26 110.1(2) 3_565 2_665 ?
N22 C41 C42 180.0 . . ?
S13 C7 S12 112.87(16) . . ?
S11 C7 S12 123.17(19) . . ?
S11 C7 S13 123.96(18) . . ?
C38 N20 C38 108.6(3) 2 . ?
C38 N20 C38 108.6(3) 3 . ?
C38 N20 C38 108.6(3) 2 3 ?
N12 C30 C29 108.1(3) . . ?
S9 C6 S8 113.15(15) . . ?
S10 C6 S8 124.14(18) . . ?
S10 C6 S9 122.69(18) . . ?
N18 C36 C35 110.5(3) . . ?
N11 C29 C30 111.9(3) . . ?
S28 C18 S29 113.34(16) . . ?
S30 C18 S29 123.33(19) . . ?
S30 C18 S28 123.32(19) . . ?
N5 C23 C24 110.9(3) . . ?
S22 C13 S23 113.30(17) . . ?
S21 C13 S23 123.3(2) . . ?
S21 C13 S22 123.3(2) . . ?
N21 C39 C40 180.0 . . ?
N17 C35 C36 108.5(3) . . ?
N4 C22 C21 108.1(3) . . ?
N6 C24 C23 109.1(3) . . ?
N13 C31 C32 110.7(3) . . ?
N3 C21 C22 111.2(4) . . ?
S3 C1 S2 113.26(17) . . ?
S1 C1 S2 123.5(2) . . ?
S1 C1 S3 123.3(2) . . ?
N19 C37 C38 108.7(3) . . ?
N14 C32 C31 108.9(3) . . ?
N20 C38 C37 110.8(4) . . ?
N23 C43 C44 180.0 . . ?
C27 N9 C27 108.1(5) 2_655 . ?
C27 N9 C27 108.1(4) . 3_665 ?
C27 N9 C27 108.1(4) 2_655 3_665 ?
C19 N1 C19 108.5(4) 3_565 2_665 ?
C19 N1 C19 108.5(4) 3_565 . ?
C19 N1 C19 108.5(4) 2_665 . ?
N7 C25 C26 110.9(3) . . ?
N8 C26 C25 108.1(3) . . ?
S19 C12 S18 113.6(2) . . ?
S20 C12 S18 122.5(3) . . ?
S20 C12 S19 123.9(2) . . ?
N24 C45 C46 177.2(7) . . ?
C20 N2 C20 110.2(5) 3_565 2_665 ?
C20 N2 C20 110.2(5) 3_565 . ?
C20 N2 C20 110.2(5) 2_665 . ?
C20 C19 N1 107.7(6) . . ?
N2 C20 C19 109.9(7) . . ?
C28 N10 C28 108.9(9) 2_655 3_665 ?
C28 N10 C28 108.9(9) 2_655 . ?
C28 N10 C28 108.9(9) 3_665 . ?
N16 C34 C33 113.3(8) . . ?
N9 C27 C28 106.3(7) . . ?
N10 C28 C27 114.6(11) . . ?
C34 N16 C34 113.6(5) 2 3 ?
C34 N16 C34 113.6(5) 2 . ?
C34 N16 C34 113.6(5) 3 . ?
C33 N15 C33 114.4(6) . 3 ?
C33 N15 C33 114.4(5) . 2 ?
C33 N15 C33 114.4(6) 3 2 ?
C34 C33 N15 94.4(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 S6 2.1691(7) . ?
Ni1 S7 2.1625(7) . ?
Ni1 S4 2.1705(7) . ?
Ni1 S5 2.1673(7) . ?
Ni3 S27 2.1659(7) . ?
Ni3 S26 2.1644(7) . ?
Ni3 S25 2.1823(7) . ?
Ni3 S24 2.1665(7) . ?
Ni2 S14 2.1703(7) . ?
Ni2 S15 2.1638(7) . ?
Ni2 S16 2.1704(8) . ?
Ni2 S17 2.1687(8) . ?
S6 C5 1.715(2) . ?
S7 C4 1.707(2) . ?
S4 C3 1.721(3) . ?
S27 C17 1.717(3) . ?
S26 C16 1.708(3) . ?
S14 C9 1.713(3) . ?
S5 C2 1.723(3) . ?
S25 C15 1.728(3) . ?
S15 C8 1.712(3) . ?
S24 C14 1.716(3) . ?
S16 C11 1.717(3) . ?
S8 C5 1.742(2) . ?
S8 C6 1.735(3) . ?
S17 C10 1.712(3) . ?
S12 C9 1.745(2) . ?
S12 C7 1.737(3) . ?
S9 C4 1.740(2) . ?
S9 C6 1.732(3) . ?
S13 C8 1.744(2) . ?
S13 C7 1.731(3) . ?
S29 C17 1.744(2) . ?
S29 C18 1.737(3) . ?
S28 C16 1.743(3) . ?
S28 C18 1.723(3) . ?
S2 C3 1.737(2) . ?
S2 C1 1.728(4) . ?
S23 C15 1.746(3) . ?
S23 C13 1.738(4) . ?
S22 C14 1.740(3) . ?
S22 C13 1.716(4) . ?
S3 C2 1.742(3) . ?
S3 C1 1.727(4) . ?
S18 C11 1.743(3) . ?
S18 C12 1.734(4) . ?
S11 C7 1.642(3) . ?
S19 C10 1.742(3) . ?
S19 C12 1.718(4) . ?
S10 C6 1.642(3) . ?
S30 C18 1.645(3) . ?
S21 C13 1.650(3) . ?
S1 C1 1.652(3) . ?
S20 C12 1.647(4) . ?
N18 C36 1.480(3) . ?
N18 C36 1.479(4) 3 ?
N18 C36 1.479(3) 2 ?
N12 C30 1.501(3) 2_655 ?
N12 C30 1.501(3) . ?
N12 C30 1.501(3) 3_665 ?
N17 C35 1.495(4) 3 ?
N17 C35 1.495(4) 2 ?
N17 C35 1.495(4) . ?
N14 C32 1.497(4) . ?
N14 C32 1.497(4) 3_665 ?
N14 C32 1.497(4) 2_655 ?
N4 C22 1.497(4) 3_565 ?
N4 C22 1.497(4) . ?
N4 C22 1.497(4) 2_665 ?
N5 C23 1.485(4) 3_565 ?
N5 C23 1.485(4) 2_665 ?
N5 C23 1.485(4) . ?
N6 C24 1.485(4) 2_665 ?
N6 C24 1.485(4) . ?
N6 C24 1.485(4) 3_565 ?
N11 C29 1.468(4) 2_655 ?
N11 C29 1.468(4) . ?
N11 C29 1.468(4) 3_665 ?
N13 C31 1.481(3) 3_665 ?
N13 C31 1.481(4) 2_655 ?
N13 C31 1.481(3) . ?
C4 C5 1.369(3) . ?
N19 C37 1.505(4) 2 ?
N19 C37 1.505(4) 3 ?
N19 C37 1.505(4) . ?
C15 C14 1.352(4) . ?
C3 C2 1.353(4) . ?
C8 C9 1.367(4) . ?
C16 C17 1.359(4) . ?
N3 C21 1.469(4) . ?
N3 C21 1.469(4) 3_565 ?
N3 C21 1.469(4) 2_665 ?
N7 C25 1.472(4) . ?
N7 C25 1.472(5) 3_565 ?
N7 C25 1.472(4) 2_665 ?
C42 C41 1.445(8) . ?
C10 C11 1.360(4) . ?
N8 C26 1.481(4) . ?
N8 C26 1.481(5) 3_565 ?
N8 C26 1.481(4) 2_665 ?
C41 N22 1.139(7) . ?
N20 C38 1.474(4) 3 ?
N20 C38 1.474(4) . ?
N20 C38 1.473(4) 2 ?
C30 C29 1.523(5) . ?
N23 C43 1.137(9) . ?
C36 C35 1.532(5) . ?
N21 C39 1.130(10) . ?
C23 C24 1.520(5) . ?
C39 C40 1.456(11) . ?
C22 C21 1.536(6) . ?
C31 C32 1.519(5) . ?
C37 C38 1.525(5) . ?
C44 C43 1.438(10) . ?
N9 C27 1.452(8) 2_655 ?
N9 C27 1.452(8) . ?
N9 C27 1.452(8) 3_665 ?
N1 C19 1.487(8) 3_565 ?
N1 C19 1.487(8) 2_665 ?
N1 C19 1.487(8) . ?
C25 C26 1.539(5) . ?
C45 N24 1.109(6) . ?
C45 C46 1.403(7) . ?
N2 C20 1.418(8) 3_565 ?
N2 C20 1.418(9) 2_665 ?
N2 C20 1.418(8) . ?
C19 C20 1.484(10) . ?
N10 C28 1.322(12) 2_655 ?
N10 C28 1.322(12) 3_665 ?
N10 C28 1.322(12) . ?
C34 N16 1.646(9) . ?
C34 C33 1.692(12) . ?
C27 C28 1.472(11) . ?
N15 C33 1.910(11) . ?
N15 C33 1.910(11) 3 ?
N15 C33 1.910(11) 2 ?
