#------------------------------------------------------------------------------
#$Date: 2024-07-05 18:29:21 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292965 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/87/7248793.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_7248793
loop_
_publ_author_name
'Marttinen, Antti'
'Lahtinen, Manu'
_publ_section_title
;
 Aqueous syntheses of anthracene-based mixed-ligand coordination polymers
 and their structural and optical properties
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              3388
_journal_page_last               3400
_journal_paper_doi               10.1039/D4CE00399C
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C116 H80 N20 Ni3 O16 S2, 12(H2 O), 6(C3 H7 N O)'
_chemical_formula_sum            'C134 H146 N26 Ni3 O34 S2'
_chemical_formula_weight         2905.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.63110(10)
_cell_length_b                   30.64140(10)
_cell_length_c                   16.96660(10)
_cell_measurement_reflns_used    40685
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      78.6090
_cell_measurement_theta_min      3.0300
_cell_volume                     6875.65(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00 -13.00   1.00    2.00    --  -87.71  57.00  30.00   41
  2  ω     -3.00  23.00   1.00    1.00    --  -54.15  19.00 -30.00   26
  3  ω    -51.00 -13.00   1.00    2.00    --  -87.71  57.00 -60.00   38
  4  ω    -24.00  20.00   1.00    1.00    --  -54.15  35.00-116.00   44
  5  ω    -30.00  -5.00   1.00    1.00    --   14.00 112.00  -4.51   25
  6  ω    -54.00 -29.00   1.00    1.00    --   18.00 154.00-149.09   25
  7  ω     95.00 127.00   1.00    2.00    --  107.25 139.00  48.60   32
  8  ω    145.00 173.00   1.00    2.00    --  107.25 139.00  48.60   28
  9  ω     37.00 101.00   1.00    1.00    --   52.65  35.00-116.00   64
 10  ω     77.00 104.00   1.00    2.00    --  106.00  20.00-135.90   27
 11  ω     86.00 122.00   1.00    2.00    --  101.96  35.00-116.00   36
 12  ω    134.00 176.00   1.00    2.00    --  101.96  35.00-116.00   42
 13  ω    150.00 175.00   1.00    2.00    --  106.00  20.00-135.90   25
 14  ω    123.00 172.00   1.00    2.00    --  107.25  32.00 -22.88   49
 15  ω     48.00  76.00   1.00    2.00    --  107.25 -78.00-111.66   28
 16  ω     36.00  70.00   1.00    2.00    --  107.25 -66.00-142.47   34
 17  ω     34.00  79.00   1.00    2.00    --  101.96 -57.00 -90.00   45
 18  ω    101.00 132.00   1.00    2.00    --  107.25 -78.00-111.66   31
 19  ω     39.00  72.00   1.00    2.00    --  107.25 -57.00-122.12   33
 20  ω     33.00  61.00   1.00    2.00    --  107.25 -52.00 -71.91   28
 21  ω     37.00  71.00   1.00    2.00    --  107.25 -55.00 -49.88   34
 22  ω     59.00  85.00   1.00    2.00    --  107.25 -67.00 -19.91   26
 23  ω     30.00  55.00   1.00    2.00    --  107.25 -43.00  63.79   25
 24  ω     38.00  68.00   1.00    2.00    --  107.25 -51.00  99.72   30
 25  ω     31.00  56.00   1.00    2.00    --  107.25 -42.00 138.20   25
 26  ω     25.00  50.00   1.00    2.00    --  101.96 -38.00 120.00   25
 27  ω     25.00  50.00   1.00    2.00    --  101.96 -38.00  90.00   25
 28  ω     27.00  52.00   1.00    2.00    --  101.96 -38.00-150.00   25
 29  ω     30.00  55.00   1.00    2.00    --  107.25 -41.00 -31.72   25
 30  ω    -20.00  45.00   1.00    1.00    --   52.65 -35.00  86.00   65
 31  ω     27.00  52.00   1.00    2.00    --  101.96 -38.00 150.00   25
 32  ω     54.00 110.00   1.00    2.00    --  107.25 -73.00 108.74   56
 33  ω     38.00 104.00   1.00    2.00    --  101.96 -99.00 120.00   66
 34  ω     48.00  92.00   1.00    2.00    --  107.25-165.00 151.04   44
 35  ω     96.00 131.00   1.00    2.00    --  107.25-165.00 151.04   35
 36  ω     45.00 119.00   1.00    2.00    --  107.25-158.00  91.56   74
 37  ω     38.00  65.00   1.00    2.00    --  107.25-103.00-138.89   27
 38  ω     69.00  95.00   1.00    2.00    --  107.25-103.00-138.89   26
 39  ω    -63.00 -38.00   1.00    1.00    --  -54.15 -35.00  86.00   25
 40  ω   -131.00 -84.00   1.00    1.00    --  -54.15 -35.00  86.00   47
 41  ω   -143.00-118.00   1.00    2.00    --  -87.71 -35.00  86.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0265367000
_diffrn_orient_matrix_UB_12      0.0221656000
_diffrn_orient_matrix_UB_13      0.0736343000
_diffrn_orient_matrix_UB_21      0.1100802000
_diffrn_orient_matrix_UB_22      -0.0057725000
_diffrn_orient_matrix_UB_23      0.0492374000
_diffrn_orient_matrix_UB_31      0.0273719000
_diffrn_orient_matrix_UB_32      0.0447637000
_diffrn_orient_matrix_UB_33      -0.0301428000
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.076
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0506
_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)+(0.0694P)²+8.9673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13557
_reflns_number_total             14648
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-185h_r_abs_2
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248793
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H20 N6 O4 S1 Ni1'
_chemical_oxdiff_usercomment     'light green block'
_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   0.889
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O98A(0.8) H98A(0.8) H98B(0.8) O98B(0.2) H98C(0.2) H98D(0.2)
3.a Free rotating group:
 O94(H94A,H94B), O95(H95A,H95B), O96(H96A,H96B), O97(H97A,H97B), O83(H83A,
 H83B), O98A(H98A,H98B), O98B(H98C,H98D)
3.b Rotating group:
 O77(H77A,H77B)
3.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C2(H2), C65(H65), C69(H69), C67(H67), C14(H14), C36(H36), C57(H57),
 C35(H35), C17(H17), C41(H41), C5(H5), C54(H54), C33(H33), C4(H4), C27(H27),
 C30(H30), C16(H16), C53(H53), C23(H23), C8(H8), C28(H28), C11(H11), C40(H40),
 C29(H29), C20(H20), C51(H51), C52(H52), C44(H44), C21(H21), C22(H22), C47(H47),
  C9(H9), C10(H10), C87(H87), C59(H59), C45(H45), C60(H60), C46(H46), C81(H81),
 C92(H92)
3.d Idealised Me refined as rotating group:
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C78(H78A,H78B,H78C), C89(H89A,H89B,
 H89C), C79(H79A,H79B,H79C), C90(H90A,H90B,H90C)
;
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.899
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.5000 0.5000 1.0000 0.01169(11) Uani 1 2 d S . P . .
Ni2 Ni 0.70331(2) 0.73945(2) 0.38767(2) 0.01122(9) Uani 1 1 d . . . . .
S70 S 0.45585(4) 0.55132(2) 0.17465(3) 0.01411(10) Uani 1 1 d . . . . .
O61 O 0.62415(10) 0.70121(5) 0.29395(8) 0.0153(3) Uani 1 1 d . . . . .
O72 O 0.49734(11) 0.53120(5) 0.11154(9) 0.0187(3) Uani 1 1 d . . . . .
O76 O 0.27194(11) 0.71934(5) -0.01922(9) 0.0194(3) Uani 1 1 d . . . . .
O77 O 0.72127(11) 0.78534(5) 0.30188(8) 0.0168(3) Uani 1 1 d . . . . .
H77A H 0.6669 0.7871 0.2645 0.025 Uiso 1 1 d R U . . .
H77B H 0.7283 0.8106 0.3234 0.025 Uiso 1 1 d R U . . .
O71 O 0.52617(13) 0.54881(5) 0.25389(9) 0.0235(3) Uani 1 1 d . . . . .
O75 O 0.27713(12) 0.65433(5) -0.07993(9) 0.0242(3) Uani 1 1 d . . . . .
O62 O 0.54416(12) 0.75523(5) 0.21418(9) 0.0225(3) Uani 1 1 d . . . . .
O73 O 0.35521(12) 0.53573(5) 0.17396(10) 0.0227(3) Uani 1 1 d . . . . .
N1 N 0.34406(12) 0.50682(6) 0.95354(10) 0.0155(3) Uani 1 1 d . . . . .
N13 N 0.53167(13) 0.55911(5) 0.95139(10) 0.0152(3) Uani 1 1 d . . . . .
N34 N 0.68354(12) 0.68833(5) 0.46290(10) 0.0145(3) Uani 1 1 d . . . . .
N37 N 0.56661(12) 0.76823(6) 0.39564(10) 0.0160(3) Uani 1 1 d . . . . .
N32 N 0.66306(14) 0.65051(6) 0.56816(11) 0.0196(4) Uani 1 1 d . . . . .
N3 N 0.18051(13) 0.50472(6) 0.94618(11) 0.0171(3) Uani 1 1 d . . . . .
N39 N 0.40385(13) 0.77650(6) 0.38553(12) 0.0205(4) Uani 1 1 d . . . . .
N58 N -0.14994(14) 0.71732(6) 0.39185(13) 0.0251(4) Uani 1 1 d . . . . .
N15 N 0.57706(15) 0.60440(6) 0.86605(11) 0.0217(4) Uani 1 1 d . . . . .
O94 O 0.14759(17) 0.61045(7) -0.21470(13) 0.0436(5) Uani 1 1 d G . . . .
H94A H 0.1780 0.5937 -0.2410 0.065 Uiso 1 1 d G U . . .
H94B H 0.1910 0.6155 -0.1705 0.065 Uiso 1 1 d G U . . .
O95 O 0.03591(18) 0.65656(7) -0.34979(12) 0.0429(5) Uani 1 1 d G . . . .
H95A H 0.0691 0.6458 -0.3050 0.064 Uiso 1 1 d G U . . .
H95B H 0.0329 0.6837 -0.3405 0.064 Uiso 1 1 d G U . . .
N56 N 0.01331(14) 0.72451(7) 0.39980(14) 0.0295(5) Uani 1 1 d . . . . .
C63 C 0.55794(15) 0.71600(7) 0.23414(12) 0.0153(4) Uani 1 1 d . . . . .
C38 C 0.48092(15) 0.74783(7) 0.39153(13) 0.0169(4) Uani 1 1 d . . . . .
H38 H 0.4739 0.7170 0.3926 0.020 Uiso 1 1 calc R U . . .
C2 C 0.27506(14) 0.50252(7) 0.99529(12) 0.0157(4) Uani 1 1 d . . . . .
H2 H 0.2895 0.4984 1.0524 0.019 Uiso 1 1 calc R U . . .
C65 C 0.50067(15) 0.63822(6) 0.20216(12) 0.0147(4) Uani 1 1 d . . . . .
H65 H 0.5441 0.6292 0.2521 0.018 Uiso 1 1 calc R U . . .
C69 C 0.42560(15) 0.69527(6) 0.10986(12) 0.0147(4) Uani 1 1 d . . . . .
H69 H 0.4171 0.7254 0.0971 0.018 Uiso 1 1 calc R U . . .
C67 C 0.38205(14) 0.62039(7) 0.07531(12) 0.0149(4) Uani 1 1 d . . . . .
H67 H 0.3473 0.5991 0.0381 0.018 Uiso 1 1 calc R U . . .
C14 C 0.52998(15) 0.56647(7) 0.87451(13) 0.0171(4) Uani 1 1 d . . . . .
H14 H 0.4997 0.5476 0.8309 0.021 Uiso 1 1 calc R U . . .
C66 C 0.44505(15) 0.60759(6) 0.14951(12) 0.0143(4) Uani 1 1 d . . . . .
O88 O 0.16784(18) 0.61149(9) 0.42873(16) 0.0589(6) Uani 1 1 d . . . . .
C74 C 0.30065(15) 0.68021(7) -0.02137(12) 0.0169(4) Uani 1 1 d . . . . .
C68 C 0.37070(14) 0.66442(7) 0.05652(12) 0.0150(4) Uani 1 1 d . . . . .
C64 C 0.49254(15) 0.68229(7) 0.18137(12) 0.0150(4) Uani 1 1 d . . . . .
O96 O 0.0668(2) 0.58818(8) -0.45066(15) 0.0592(7) Uani 1 1 d G . . . .
H96A H 0.0468 0.6090 -0.4254 0.089 Uiso 1 1 d G U . . .
H96B H 0.1035 0.6004 -0.4782 0.089 Uiso 1 1 d G U . . .
C6 C 0.08812(15) 0.50239(7) 0.97260(13) 0.0170(4) Uani 1 1 d . . . . .
N86 N 0.30603(19) 0.61150(8) 0.37605(16) 0.0407(5) Uani 1 1 d . . . . .
C31 C 0.69572(18) 0.60842(7) 0.78033(13) 0.0212(4) Uani 1 1 d . . . . .
C12 C 0.06197(15) 0.53777(7) 1.01523(13) 0.0191(4) Uani 1 1 d . . . . .
C36 C 0.66304(17) 0.62079(7) 0.50745(13) 0.0212(4) Uani 1 1 d . . . . .
H36 H 0.6560 0.5900 0.5100 0.025 Uiso 1 1 calc R U . . .
C57 C -0.08082(15) 0.74011(7) 0.36882(13) 0.0183(4) Uani 1 1 d . . . . .
H57 H -0.0951 0.7649 0.3342 0.022 Uiso 1 1 calc R U . . .
C7 C 0.02883(15) 0.46467(7) 0.95581(13) 0.0194(4) Uani 1 1 d . . . . .
C26 C 0.71921(17) 0.62127(7) 0.70538(13) 0.0211(4) Uani 1 1 d . . . . .
C42 C 0.30199(15) 0.76589(7) 0.38595(14) 0.0218(4) Uani 1 1 d . . . . .
C55 C 0.23836(16) 0.74929(7) 0.31520(14) 0.0222(4) Uani 1 1 d . . . . .
C35 C 0.67527(17) 0.64468(7) 0.44286(13) 0.0200(4) Uani 1 1 d . . . . .
H35 H 0.6777 0.6330 0.3915 0.024 Uiso 1 1 calc R U . . .
C17 C 0.58213(17) 0.59389(7) 0.99439(13) 0.0215(4) Uani 1 1 d . . . . .
H17 H 0.5946 0.5976 1.0515 0.026 Uiso 1 1 calc R U . . .
C18 C 0.60004(18) 0.61855(7) 0.79186(13) 0.0220(4) Uani 1 1 d . . . . .
C24 C 0.54694(18) 0.65052(7) 0.65686(13) 0.0228(4) Uani 1 1 d . . . . .
C41 C 0.54435(17) 0.81195(7) 0.39267(16) 0.0253(5) Uani 1 1 d . . . . .
H41 H 0.5920 0.8348 0.3947 0.030 Uiso 1 1 calc R U . . .
C5 C 0.29197(16) 0.51189(8) 0.87371(13) 0.0247(5) Uani 1 1 d . . . . .
H5 H 0.3223 0.5156 0.8293 0.030 Uiso 1 1 calc R U . . .
O82 O 0.6499(2) 0.51958(9) 0.58466(17) 0.0673(7) Uani 1 1 d . . . . .
C54 C 0.27044(17) 0.74336(8) 0.24153(15) 0.0247(5) Uani 1 1 d . . . . .
H54 H 0.3368 0.7516 0.2392 0.030 Uiso 1 1 calc R U . . .
C43 C 0.27179(17) 0.77240(8) 0.45844(15) 0.0257(5) Uani 1 1 d . . . . .
C19 C 0.52509(19) 0.63960(7) 0.73325(14) 0.0234(5) Uani 1 1 d . . . . .
C25 C 0.64306(18) 0.64114(7) 0.64567(13) 0.0213(4) Uani 1 1 d . . . . .
C33 C 0.67565(18) 0.69047(7) 0.53829(13) 0.0217(4) Uani 1 1 d . . . . .
H33 H 0.6784 0.7168 0.5682 0.026 Uiso 1 1 calc R U . . .
C4 C 0.19087(16) 0.51074(9) 0.86794(14) 0.0262(5) Uani 1 1 d . . . . .
H4 H 0.1382 0.5135 0.8200 0.031 Uiso 1 1 calc R U . . .
C27 C 0.81808(18) 0.61269(8) 0.69473(14) 0.0255(5) Uani 1 1 d . . . . .
H27 H 0.8354 0.6219 0.6463 0.031 Uiso 1 1 calc R U . . .
C30 C 0.77056(19) 0.58508(8) 0.83880(14) 0.0256(5) Uani 1 1 d . . . . .
H30 H 0.7555 0.5754 0.8877 0.031 Uiso 1 1 calc R U . . .
C16 C 0.6113(2) 0.62212(8) 0.94262(14) 0.0276(5) Uani 1 1 d . . . . .
H16 H 0.6478 0.6486 0.9563 0.033 Uiso 1 1 calc R U . . .
C50 C 0.13738(16) 0.73666(7) 0.31785(16) 0.0254(5) Uani 1 1 d . . . . .
C53 C 0.20609(19) 0.72595(8) 0.17495(16) 0.0292(5) Uani 1 1 d . . . . .
H53 H 0.2283 0.7212 0.1267 0.035 Uiso 1 1 calc R U . . .
C49 C 0.10891(17) 0.74120(8) 0.39217(17) 0.0273(5) Uani 1 1 d . . . . .
C23 C 0.4685(2) 0.66978(8) 0.59514(15) 0.0297(5) Uani 1 1 d . . . . .
H23 H 0.4814 0.6770 0.5441 0.036 Uiso 1 1 calc R U . . .
C8 C 0.05399(18) 0.42844(8) 0.91159(16) 0.0274(5) Uani 1 1 d . . . . .
H8 H 0.1138 0.4294 0.8922 0.033 Uiso 1 1 calc R U . . .
C28 C 0.88803(19) 0.59144(8) 0.75325(15) 0.0286(5) Uani 1 1 d . . . . .
H28 H 0.9540 0.5865 0.7459 0.034 Uiso 1 1 calc R U . . .
C48 C 0.17202(17) 0.75920(8) 0.46200(16) 0.0280(5) Uani 1 1 d . . . . .
C11 C -0.12065(17) 0.42317(8) 0.97077(17) 0.0288(5) Uani 1 1 d . . . . .
H11 H -0.1789 0.4206 0.9918 0.035 Uiso 1 1 calc R U . . .
C40 C 0.44406(18) 0.81767(8) 0.38640(17) 0.0296(5) Uani 1 1 d . . . . .
H40 H 0.4089 0.8446 0.3833 0.036 Uiso 1 1 calc R U . . .
C29 C 0.86264(19) 0.57664(8) 0.82527(15) 0.0290(5) Uani 1 1 d . . . . .
H29 H 0.9109 0.5606 0.8644 0.035 Uiso 1 1 calc R U . . .
C20 C 0.4270(2) 0.64937(8) 0.74495(15) 0.0305(5) Uani 1 1 d . . . . .
H20 H 0.4120 0.6429 0.7955 0.037 Uiso 1 1 calc R U . . .
C51 C 0.07214(18) 0.71965(8) 0.24632(18) 0.0321(5) Uani 1 1 d . . . . .
H51 H 0.0049 0.7116 0.2466 0.039 Uiso 1 1 calc R U . . .
O97 O 0.1766(3) 0.54519(10) -0.31437(16) 0.0731(9) Uani 1 1 d G . . . .
H97A H 0.1411 0.5565 -0.3577 0.110 Uiso 1 1 d G U . . .
H97B H 0.2373 0.5502 -0.3163 0.110 Uiso 1 1 d G U . . .
C52 C 0.1051(2) 0.71481(9) 0.17748(18) 0.0349(6) Uani 1 1 d . . . . .
H52 H 0.0600 0.7038 0.1299 0.042 Uiso 1 1 calc R U . . .
C44 C 0.33664(19) 0.79147(10) 0.52845(16) 0.0340(6) Uani 1 1 d . . . . .
H44 H 0.4029 0.8001 0.5264 0.041 Uiso 1 1 calc R U . . .
C21 C 0.3554(2) 0.66777(10) 0.68488(17) 0.0374(6) Uani 1 1 d . . . . .
H21 H 0.2906 0.6740 0.6937 0.045 Uiso 1 1 calc R U . . .
C22 C 0.3759(2) 0.67788(9) 0.60856(17) 0.0359(6) Uani 1 1 d . . . . .
H22 H 0.3245 0.6904 0.5667 0.043 Uiso 1 1 calc R U . . .
C47 C 0.1444(2) 0.76600(10) 0.53802(18) 0.0386(6) Uani 1 1 d . . . . .
H47 H 0.0791 0.7573 0.5427 0.046 Uiso 1 1 calc R U . . .
N91 N -0.1516(2) 0.59060(10) 0.3102(2) 0.0519(7) Uani 1 1 d . . . . .
C9 C -0.0061(2) 0.39263(9) 0.89680(19) 0.0372(6) Uani 1 1 d . . . . .
H9 H 0.0107 0.3693 0.8656 0.045 Uiso 1 1 calc R U . . .
N80 N 0.8053(3) 0.49554(9) 0.6496(2) 0.0603(8) Uani 1 1 d . . . . .
C10 C -0.0942(2) 0.38969(9) 0.9277(2) 0.0390(7) Uani 1 1 d . . . . .
H10 H -0.1348 0.3641 0.9181 0.047 Uiso 1 1 calc R U . . .
C87 C 0.2587(2) 0.60594(11) 0.43491(19) 0.0436(7) Uani 1 1 d . . . . .
H87 H 0.2984 0.5969 0.4863 0.052 Uiso 1 1 calc R U . . .
O83 O 0.4482(3) 0.53849(11) 0.55437(19) 0.0775(8) Uani 1 1 d G . . . .
H83A H 0.5085 0.5289 0.5648 0.116 Uiso 1 1 d G U . . .
H83B H 0.4137 0.5191 0.5239 0.116 Uiso 1 1 d G U . . .
O93 O -0.0746(3) 0.64107(11) 0.2511(2) 0.0829(10) Uani 1 1 d . . . . .
C59 C -0.0961(2) 0.68656(9) 0.44639(18) 0.0351(6) Uani 1 1 d . . . . .
H59 H -0.1255 0.6659 0.4755 0.042 Uiso 1 1 calc R U . . .
C45 C 0.3061(2) 0.79767(12) 0.59827(18) 0.0431(7) Uani 1 1 d . . . . .
H45 H 0.3503 0.8109 0.6440 0.052 Uiso 1 1 calc R U . . .
C60 C 0.0045(2) 0.69061(9) 0.45171(19) 0.0383(6) Uani 1 1 d . . . . .
H60 H 0.0576 0.6738 0.4842 0.046 Uiso 1 1 calc R U . . .
C46 C 0.2085(2) 0.78434(12) 0.60235(18) 0.0464(7) Uani 1 1 d . . . . .
H46 H 0.1877 0.7884 0.6514 0.056 Uiso 1 1 calc R U . . .
C81 C 0.7102(3) 0.50435(10) 0.6450(2) 0.0522(8) Uani 1 1 d . . . . .
H81 H 0.6854 0.4986 0.6917 0.063 Uiso 1 1 calc R U . . .
C84 C 0.4138(3) 0.60503(13) 0.3890(2) 0.0533(8) Uani 1 1 d . . . . .
H84A H 0.4415 0.5943 0.4443 0.080 Uiso 1 1 calc R U . . .
H84B H 0.4461 0.6328 0.3815 0.080 Uiso 1 1 calc R U . . .
H84C H 0.4268 0.5836 0.3498 0.080 Uiso 1 1 calc R U . . .
C85 C 0.2539(3) 0.62533(13) 0.2953(2) 0.0606(9) Uani 1 1 d . . . . .
H85A H 0.1826 0.6308 0.2937 0.091 Uiso 1 1 calc R U . . .
H85B H 0.2589 0.6024 0.2562 0.091 Uiso 1 1 calc R U . . .
H85C H 0.2849 0.6522 0.2814 0.091 Uiso 1 1 calc R U . . .
C92 C -0.0730(3) 0.61475(13) 0.3059(2) 0.0560(9) Uani 1 1 d . . . . .
H92 H -0.0124 0.6116 0.3471 0.067 Uiso 1 1 calc R U . . .
C78 C 0.8693(4) 0.47704(14) 0.7229(3) 0.0820(14) Uani 1 1 d . . . . .
H78A H 0.8293 0.4723 0.7630 0.123 Uiso 1 1 calc R U . . .
H78B H 0.9249 0.4972 0.7452 0.123 Uiso 1 1 calc R U . . .
H78C H 0.8968 0.4491 0.7100 0.123 Uiso 1 1 calc R U . . .
C89 C -0.2464(3) 0.59470(18) 0.2505(3) 0.0809(14) Uani 1 1 d . . . . .
H89A H -0.2405 0.5812 0.1995 0.121 Uiso 1 1 calc R U . . .
H89B H -0.2633 0.6257 0.2412 0.121 Uiso 1 1 calc R U . . .
H89C H -0.2998 0.5801 0.2702 0.121 Uiso 1 1 calc R U . . .
C79 C 0.8497(5) 0.50496(16) 0.5812(4) 0.0934(17) Uani 1 1 d . . . . .
H79A H 0.8979 0.5291 0.5955 0.140 Uiso 1 1 calc R U . . .
H79B H 0.7961 0.5131 0.5337 0.140 Uiso 1 1 calc R U . . .
H79C H 0.8850 0.4790 0.5685 0.140 Uiso 1 1 calc R U . . .
C90 C -0.1444(5) 0.56125(15) 0.3797(4) 0.0939(18) Uani 1 1 d . . . . .
H90A H -0.1933 0.5702 0.4104 0.141 Uiso 1 1 calc R U . . .
H90B H -0.0759 0.5626 0.4149 0.141 Uiso 1 1 calc R U . . .
H90C H -0.1591 0.5313 0.3601 0.141 Uiso 1 1 calc R U . . .
O98A O 0.3773(3) 0.52889(9) -0.30631(17) 0.0482(7) Uani 0.8 1 d G . P A 2
H98A H 0.4068 0.5051 -0.2884 0.072 Uiso 0.8 1 d G U P A 2
H98B H 0.4023 0.5358 -0.3458 0.072 Uiso 0.8 1 d G U P A 2
O98B O 0.4503(13) 0.5342(4) -0.3316(9) 0.067(4) Uani 0.2 1 d G . P B 1
H98C H 0.5075 0.5453 -0.3096 0.100 Uiso 0.2 1 d G U P B 1
H98D H 0.4643 0.5097 -0.3495 0.100 Uiso 0.2 1 d G U P B 1
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 0 -10 0.0533
3 18 -4 0.0668
0 -19 3 0.0417
-8 -8 -1 0.0588
-5 -7 9 0.0466
0 20 0 0.0461
4 -14 -7 0.0500
6 0 -10 0.0578
-5 17 0 0.0600
8 0 1 0.0810
0 5 10 0.0237
-2 -3 -10 0.0654
-9 1 1 0.0605
3 -7 -10 0.0415
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
O72 Ni1 O72 180.0 3_666 1_556 ?
N1 Ni1 O72 93.19(6) 3_667 3_666 ?
N1 Ni1 O72 86.81(6) 3_667 1_556 ?
N1 Ni1 O72 93.19(6) . 1_556 ?
N1 Ni1 O72 86.81(6) . 3_666 ?
N1 Ni1 N1 180.0 3_667 . ?
N13 Ni1 O72 89.35(6) . 3_666 ?
N13 Ni1 O72 90.65(6) . 1_556 ?
N13 Ni1 O72 89.35(6) 3_667 1_556 ?
N13 Ni1 O72 90.65(6) 3_667 3_666 ?
N13 Ni1 N1 86.96(7) . 3_667 ?
N13 Ni1 N1 86.95(7) 3_667 . ?
N13 Ni1 N1 93.05(7) . . ?
N13 Ni1 N1 93.04(7) 3_667 3_667 ?
N13 Ni1 N13 180.0 . 3_667 ?
O61 Ni2 O76 175.31(6) . 4_676 ?
O61 Ni2 O77 88.44(6) . . ?
O61 Ni2 N34 85.63(6) . . ?
O61 Ni2 N37 88.93(6) . . ?
O61 Ni2 N58 99.18(7) . 1_655 ?
O76 Ni2 O77 90.78(6) 4_676 . ?
O76 Ni2 N34 95.36(6) 4_676 . ?
O76 Ni2 N37 86.46(7) 4_676 . ?
O76 Ni2 N58 85.41(7) 4_676 1_655 ?
O77 Ni2 N37 91.02(6) . . ?
O77 Ni2 N58 88.24(7) . 1_655 ?
N34 Ni2 O77 173.47(6) . . ?
N34 Ni2 N37 91.60(7) . . ?
N34 Ni2 N58 90.01(7) . 1_655 ?
N37 Ni2 N58 171.82(8) . 1_655 ?
O72 S70 C66 104.94(9) . . ?
O71 S70 O72 111.71(9) . . ?
O71 S70 C66 105.78(9) . . ?
O73 S70 O72 112.83(9) . . ?
O73 S70 O71 113.65(10) . . ?
O73 S70 C66 107.17(9) . . ?
C63 O61 Ni2 123.63(13) . . ?
S70 O72 Ni1 158.91(10) . 1_554 ?
C74 O76 Ni2 130.16(13) . 4_575 ?
Ni2 O77 H77A 109.5 . . ?
Ni2 O77 H77B 109.5 . . ?
H77A O77 H77B 104.4 . . ?
C2 N1 Ni1 125.58(14) . . ?
C2 N1 C5 105.99(17) . . ?
C5 N1 Ni1 128.10(14) . . ?
C14 N13 Ni1 125.88(14) . . ?
C14 N13 C17 106.17(17) . . ?
C17 N13 Ni1 126.09(14) . . ?
C35 N34 Ni2 126.51(13) . . ?
C33 N34 Ni2 127.94(14) . . ?
C33 N34 C35 105.56(17) . . ?
C38 N37 Ni2 126.18(14) . . ?
C38 N37 C41 106.10(17) . . ?
C41 N37 Ni2 126.93(14) . . ?
C36 N32 C25 126.04(18) . . ?
C33 N32 C36 107.22(17) . . ?
C33 N32 C25 126.46(18) . . ?
C2 N3 C6 125.45(18) . . ?
C2 N3 C4 107.10(17) . . ?
C4 N3 C6 127.43(18) . . ?
C38 N39 C42 126.14(19) . . ?
C38 N39 C40 107.13(18) . . ?
C40 N39 C42 126.49(19) . . ?
C57 N58 Ni2 124.64(15) . 1_455 ?
C57 N58 C59 104.89(19) . . ?
C59 N58 Ni2 125.74(16) . 1_455 ?
C14 N15 C18 124.24(18) . . ?
C14 N15 C16 107.42(17) . . ?
C16 N15 C18 127.58(19) . . ?
H94A O94 H94B 104.4 . . ?
H95A O95 H95B 104.6 . . ?
C57 N56 C49 129.6(2) . . ?
C57 N56 C60 106.99(19) . . ?
C60 N56 C49 123.0(2) . . ?
O61 C63 C64 115.75(17) . . ?
O62 C63 O61 126.27(18) . . ?
O62 C63 C64 117.95(17) . . ?
N37 C38 N39 111.07(19) . . ?
N37 C38 H38 124.5 . . ?
N39 C38 H38 124.5 . . ?
N1 C2 N3 111.20(18) . . ?
N1 C2 H2 124.4 . . ?
N3 C2 H2 124.4 . . ?
C66 C65 H65 120.2 . . ?
C66 C65 C64 119.67(18) . . ?
C64 C65 H65 120.2 . . ?
C68 C69 H69 119.7 . . ?
C64 C69 H69 119.7 . . ?
C64 C69 C68 120.60(18) . . ?
C66 C67 H67 120.3 . . ?
C68 C67 H67 120.3 . . ?
C68 C67 C66 119.36(18) . . ?
N13 C14 N15 110.92(18) . . ?
N13 C14 H14 124.5 . . ?
N15 C14 H14 124.5 . . ?
C65 C66 S70 120.14(15) . . ?
C65 C66 C67 120.73(18) . . ?
C67 C66 S70 119.11(15) . . ?
O76 C74 C68 114.40(17) . . ?
O75 C74 O76 127.04(19) . . ?
O75 C74 C68 118.56(18) . . ?
C69 C68 C74 118.48(18) . . ?
C67 C68 C69 119.86(18) . . ?
C67 C68 C74 121.66(18) . . ?
C65 C64 C63 120.92(17) . . ?
C69 C64 C63 119.44(18) . . ?
C69 C64 C65 119.61(18) . . ?
H96A O96 H96B 104.5 . . ?
C12 C6 N3 118.41(18) . . ?
C12 C6 C7 122.63(19) . . ?
C7 C6 N3 118.96(19) . . ?
C87 N86 C84 122.0(3) . . ?
C87 N86 C85 122.3(3) . . ?
C84 N86 C85 115.6(3) . . ?
C18 C31 C26 118.5(2) . . ?
C18 C31 C30 123.1(2) . . ?
C30 C31 C26 118.4(2) . . ?
C6 C12 C7 119.00(19) . 3_567 ?
C6 C12 C11 122.28(19) . 3_567 ?
C11 C12 C7 118.7(2) 3_567 3_567 ?
N32 C36 H36 127.2 . . ?
C35 C36 N32 105.61(18) . . ?
C35 C36 H36 127.2 . . ?
N58 C57 N56 112.36(19) . . ?
N58 C57 H57 123.8 . . ?
N56 C57 H57 123.8 . . ?
C6 C7 C12 118.4(2) . 3_567 ?
C6 C7 C8 123.3(2) . . ?
C8 C7 C12 118.3(2) . 3_567 ?
C25 C26 C31 118.2(2) . . ?
C25 C26 C27 123.0(2) . . ?
C27 C26 C31 118.7(2) . . ?
C55 C42 N39 118.8(2) . . ?
C55 C42 C43 123.6(2) . . ?
C43 C42 N39 117.7(2) . . ?
C42 C55 C54 122.6(2) . . ?
C42 C55 C50 118.1(2) . . ?
C54 C55 C50 119.3(2) . . ?
N34 C35 H35 125.0 . . ?
C36 C35 N34 110.00(18) . . ?
C36 C35 H35 125.0 . . ?
N13 C17 H17 125.2 . . ?
C16 C17 N13 109.69(19) . . ?
C16 C17 H17 125.2 . . ?
C31 C18 N15 117.6(2) . . ?
C19 C18 N15 119.1(2) . . ?
C19 C18 C31 123.21(19) . . ?
C25 C24 C19 118.7(2) . . ?
C25 C24 C23 123.0(2) . . ?
C23 C24 C19 118.3(2) . . ?
N37 C41 H41 125.1 . . ?
C40 C41 N37 109.8(2) . . ?
C40 C41 H41 125.1 . . ?
N1 C5 H5 125.0 . . ?
C4 C5 N1 109.90(19) . . ?
C4 C5 H5 125.0 . . ?
C55 C54 H54 119.9 . . ?
C53 C54 C55 120.2(2) . . ?
C53 C54 H54 119.9 . . ?
C42 C43 C48 118.7(2) . . ?
C42 C43 C44 122.4(2) . . ?
C44 C43 C48 119.0(2) . . ?
C18 C19 C24 118.2(2) . . ?
C18 C19 C20 123.0(2) . . ?
C20 C19 C24 118.8(2) . . ?
C26 C25 N32 118.5(2) . . ?
C24 C25 N32 118.4(2) . . ?
C24 C25 C26 123.05(19) . . ?
N34 C33 N32 111.61(19) . . ?
N34 C33 H33 124.2 . . ?
N32 C33 H33 124.2 . . ?
N3 C4 H4 127.1 . . ?
C5 C4 N3 105.81(19) . . ?
C5 C4 H4 127.1 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.7(2) . . ?
C28 C27 H27 119.6 . . ?
C31 C30 H30 119.6 . . ?
C29 C30 C31 120.8(2) . . ?
C29 C30 H30 119.6 . . ?
N15 C16 H16 127.1 . . ?
C17 C16 N15 105.79(19) . . ?
C17 C16 H16 127.1 . . ?
C49 C50 C55 118.2(2) . . ?
C49 C50 C51 123.3(2) . . ?
C51 C50 C55 118.5(2) . . ?
C54 C53 H53 120.0 . . ?
C54 C53 C52 120.1(2) . . ?
C52 C53 H53 120.0 . . ?
C50 C49 N56 119.8(2) . . ?
C48 C49 N56 116.7(2) . . ?
C48 C49 C50 123.3(2) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(2) . . ?
C22 C23 H23 119.6 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.3(2) . . ?
C29 C28 H28 119.8 . . ?
C43 C48 C47 116.9(2) . . ?
C49 C48 C43 118.1(2) . . ?
C49 C48 C47 125.0(2) . . ?
C12 C11 H11 119.6 3_567 . ?
C10 C11 C12 120.8(2) . 3_567 ?
C10 C11 H11 119.6 . . ?
N39 C40 H40 127.1 . . ?
C41 C40 N39 105.9(2) . . ?
C41 C40 H40 127.1 . . ?
C30 C29 C28 120.9(2) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.6 . . ?
C50 C51 H51 119.8 . . ?
C52 C51 C50 120.5(2) . . ?
C52 C51 H51 119.8 . . ?
H97A O97 H97B 104.5 . . ?
C53 C52 H52 119.3 . . ?
C51 C52 C53 121.4(2) . . ?
C51 C52 H52 119.3 . . ?
C43 C44 H44 119.2 . . ?
C45 C44 C43 121.6(3) . . ?
C45 C44 H44 119.2 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.8(2) . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 120.5(2) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C48 C47 H47 119.1 . . ?
C46 C47 C48 121.7(3) . . ?
C46 C47 H47 119.1 . . ?
C92 N91 C89 120.9(4) . . ?
C92 N91 C90 119.5(4) . . ?
C89 N91 C90 119.5(4) . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.5(2) . . ?
C10 C9 H9 119.7 . . ?
C81 N80 C78 120.9(4) . . ?
C81 N80 C79 120.4(4) . . ?
C78 N80 C79 118.7(4) . . ?
C11 C10 C9 120.5(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O88 C87 N86 125.6(3) . . ?
O88 C87 H87 117.2 . . ?
N86 C87 H87 117.2 . . ?
H83A O83 H83B 104.5 . . ?
N58 C59 H59 125.0 . . ?
C60 C59 N58 110.0(2) . . ?
C60 C59 H59 125.0 . . ?
C44 C45 H45 120.2 . . ?
C44 C45 C46 119.6(3) . . ?
C46 C45 H45 120.2 . . ?
N56 C60 H60 127.2 . . ?
C59 C60 N56 105.6(2) . . ?
C59 C60 H60 127.2 . . ?
C47 C46 C45 121.1(3) . . ?
C47 C46 H46 119.4 . . ?
C45 C46 H46 119.4 . . ?
O82 C81 N80 125.3(4) . . ?
O82 C81 H81 117.4 . . ?
N80 C81 H81 117.4 . . ?
N86 C84 H84A 109.5 . . ?
N86 C84 H84B 109.5 . . ?
N86 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
N86 C85 H85A 109.5 . . ?
N86 C85 H85B 109.5 . . ?
N86 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
N91 C92 H92 118.4 . . ?
O93 C92 N91 123.1(4) . . ?
O93 C92 H92 118.4 . . ?
N80 C78 H78A 109.5 . . ?
N80 C78 H78B 109.5 . . ?
N80 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N91 C89 H89A 109.5 . . ?
N91 C89 H89B 109.5 . . ?
N91 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
N80 C79 H79A 109.5 . . ?
N80 C79 H79B 109.5 . . ?
N80 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
N91 C90 H90A 109.5 . . ?
N91 C90 H90B 109.5 . . ?
N91 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
H98A O98A H98B 104.4 . . ?
H98C O98B H98D 104.5 . . ?
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 O72 2.1284(14) 1_556 ?
Ni1 O72 2.1284(14) 3_666 ?
Ni1 N1 2.0909(17) . ?
Ni1 N1 2.0909(17) 3_667 ?
Ni1 N13 2.0784(17) . ?
Ni1 N13 2.0784(17) 3_667 ?
Ni2 O61 2.0578(14) . ?
Ni2 O76 2.0616(15) 4_676 ?
Ni2 O77 2.0806(14) . ?
Ni2 N34 2.0789(17) . ?
Ni2 N37 2.0955(17) . ?
Ni2 N58 2.0968(18) 1_655 ?
S70 O72 1.4627(15) . ?
S70 O71 1.4520(15) . ?
S70 O73 1.4500(15) . ?
S70 C66 1.774(2) . ?
O61 C63 1.267(2) . ?
O72 Ni1 2.1284(14) 1_554 ?
O76 Ni2 2.0616(14) 4_575 ?
O76 C74 1.264(3) . ?
O77 H77A 0.8522 . ?
O77 H77B 0.8522 . ?
O75 C74 1.251(3) . ?
O62 C63 1.251(3) . ?
N1 C2 1.314(3) . ?
N1 C5 1.377(3) . ?
N13 C14 1.318(3) . ?
N13 C17 1.378(3) . ?
N34 C35 1.378(3) . ?
N34 C33 1.311(3) . ?
N37 C38 1.312(3) . ?
N37 C41 1.372(3) . ?
N32 C36 1.375(3) . ?
N32 C25 1.435(3) . ?
N32 C33 1.352(3) . ?
N3 C2 1.356(3) . ?
N3 C6 1.437(2) . ?
N3 C4 1.381(3) . ?
N39 C38 1.354(3) . ?
N39 C42 1.428(3) . ?
N39 C40 1.374(3) . ?
N58 Ni2 2.0969(18) 1_455 ?
N58 C57 1.306(3) . ?
N58 C59 1.398(3) . ?
N15 C14 1.352(3) . ?
N15 C18 1.436(3) . ?
N15 C16 1.381(3) . ?
O94 H94A 0.8510 . ?
O94 H94B 0.8490 . ?
O95 H95A 0.8512 . ?
O95 H95B 0.8495 . ?
N56 C57 1.351(3) . ?
N56 C49 1.435(3) . ?
N56 C60 1.386(3) . ?
C63 C64 1.509(3) . ?
C38 H38 0.9500 . ?
C2 H2 0.9500 . ?
C65 H65 0.9500 . ?
C65 C66 1.388(3) . ?
C65 C64 1.393(3) . ?
C69 H69 0.9500 . ?
C69 C68 1.395(3) . ?
C69 C64 1.388(3) . ?
C67 H67 0.9500 . ?
C67 C66 1.397(3) . ?
C67 C68 1.386(3) . ?
C14 H14 0.9500 . ?
O88 C87 1.230(4) . ?
C74 C68 1.510(3) . ?
O96 H96A 0.8491 . ?
O96 H96B 0.8500 . ?
C6 C12 1.397(3) . ?
C6 C7 1.399(3) . ?
N86 C87 1.324(4) . ?
N86 C84 1.445(4) . ?
N86 C85 1.446(4) . ?
C31 C26 1.439(3) . ?
C31 C18 1.400(3) . ?
C31 C30 1.431(3) . ?
C12 C7 1.440(3) 3_567 ?
C12 C11 1.427(3) 3_567 ?
C36 H36 0.9500 . ?
C36 C35 1.361(3) . ?
C57 H57 0.9500 . ?
C7 C12 1.440(3) 3_567 ?
C7 C8 1.427(3) . ?
C26 C25 1.402(3) . ?
C26 C27 1.427(3) . ?
C42 C55 1.396(3) . ?
C42 C43 1.402(3) . ?
C55 C54 1.432(3) . ?
C55 C50 1.441(3) . ?
C35 H35 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.359(3) . ?
C18 C19 1.399(3) . ?
C24 C19 1.438(3) . ?
C24 C25 1.398(3) . ?
C24 C23 1.430(3) . ?
C41 H41 0.9500 . ?
C41 C40 1.357(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.358(3) . ?
O82 C81 1.238(4) . ?
C54 H54 0.9500 . ?
C54 C53 1.360(4) . ?
C43 C48 1.434(3) . ?
C43 C44 1.423(4) . ?
C19 C20 1.430(3) . ?
C33 H33 0.9500 . ?
C4 H4 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.364(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.354(4) . ?
C16 H16 0.9500 . ?
C50 C49 1.413(4) . ?
C50 C51 1.419(4) . ?
C53 H53 0.9500 . ?
C53 C52 1.430(4) . ?
C49 C48 1.398(4) . ?
C23 H23 0.9500 . ?
C23 C22 1.359(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.356(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.423(3) . ?
C48 C47 1.444(4) . ?
C11 C12 1.427(3) 3_567 ?
C11 H11 0.9500 . ?
C11 C10 1.358(4) . ?
C40 H40 0.9500 . ?
C29 H29 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.352(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.357(4) . ?
O97 H97A 0.8505 . ?
O97 H97B 0.8497 . ?
C52 H52 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.361(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.424(4) . ?
C22 H22 0.9500 . ?
C47 H47 0.9500 . ?
C47 C46 1.345(5) . ?
N91 C92 1.318(4) . ?
N91 C89 1.442(5) . ?
N91 C90 1.466(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.425(4) . ?
N80 C81 1.308(5) . ?
N80 C78 1.449(6) . ?
N80 C79 1.463(6) . ?
C10 H10 0.9500 . ?
C87 H87 0.9500 . ?
O83 H83A 0.8501 . ?
O83 H83B 0.8497 . ?
O93 C92 1.227(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.357(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.409(4) . ?
C60 H60 0.9500 . ?
C46 H46 0.9500 . ?
C81 H81 0.9500 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C92 H92 0.9500 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
O98A H98A 0.8511 . ?
O98A H98B 0.8496 . ?
O98B H98C 0.8502 . ?
O98B H98D 0.8502 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O77 H77A O62 0.85 1.95 2.675(2) 142.7 .
O77 H77B O75 0.85 1.94 2.698(2) 147.8 4_676
O94 H94A O97 0.85 1.94 2.709(3) 150.5 .
O94 H94B O75 0.85 2.07 2.863(2) 155.5 .
O95 H95A O94 0.85 1.97 2.807(3) 168.3 .
O95 H95B O62 0.85 2.08 2.905(2) 164.3 4_575
O96 H96A O95 0.85 1.97 2.801(3) 165.4 .
O97 H97A O96 0.85 1.92 2.765(4) 173.6 .
O97 H97B O98A 0.85 1.98 2.751(5) 149.6 .
O83 H83A O82 0.85 1.90 2.735(5) 168.4 .
O83 H83B O82 0.85 2.19 2.998(5) 160.0 3_666
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 N1 C2 N3 -174.03(13) . . . . ?
Ni1 N1 C5 C4 173.82(17) . . . . ?
Ni1 N13 C14 N15 -165.16(14) . . . . ?
Ni1 N13 C17 C16 164.74(17) . . . . ?
Ni2 O61 C63 O62 14.7(3) . . . . ?
Ni2 O61 C63 C64 -167.30(12) . . . . ?
Ni2 O76 C74 O75 -14.6(3) 4_575 . . . ?
Ni2 O76 C74 C68 165.49(13) 4_575 . . . ?
Ni2 N34 C35 C36 179.99(15) . . . . ?
Ni2 N34 C33 N32 179.80(14) . . . . ?
Ni2 N37 C38 N39 -170.02(14) . . . . ?
Ni2 N37 C41 C40 170.05(17) . . . . ?
Ni2 N58 C57 N56 161.09(17) 1_455 . . . ?
Ni2 N58 C59 C60 -159.1(2) 1_455 . . . ?
O61 C63 C64 C65 4.9(3) . . . . ?
O61 C63 C64 C69 -173.14(18) . . . . ?
O72 S70 C66 C65 -116.96(17) . . . . ?
O72 S70 C66 C67 61.37(17) . . . . ?
O76 C74 C68 C69 -22.9(3) . . . . ?
O76 C74 C68 C67 157.74(19) . . . . ?
O71 S70 O72 Ni1 155.8(2) . . . 1_554 ?
O71 S70 C66 C65 1.28(19) . . . . ?
O71 S70 C66 C67 179.61(16) . . . . ?
O75 C74 C68 C69 157.1(2) . . . . ?
O75 C74 C68 C67 -22.2(3) . . . . ?
O62 C63 C64 C65 -177.00(19) . . . . ?
O62 C63 C64 C69 5.0(3) . . . . ?
O73 S70 O72 Ni1 26.3(3) . . . 1_554 ?
O73 S70 C66 C65 122.85(17) . . . . ?
O73 S70 C66 C67 -58.81(18) . . . . ?
N1 C5 C4 N3 -0.1(3) . . . . ?
N13 C17 C16 N15 0.6(3) . . . . ?
N37 C41 C40 N39 0.0(3) . . . . ?
N32 C36 C35 N34 0.5(3) . . . . ?
N3 C6 C12 C7 -178.15(18) . . . 3_567 ?
N3 C6 C12 C11 3.6(3) . . . 3_567 ?
N3 C6 C7 C12 178.14(18) . . . 3_567 ?
N3 C6 C7 C8 -1.7(3) . . . . ?
N39 C42 C55 C54 -1.4(3) . . . . ?
N39 C42 C55 C50 176.88(19) . . . . ?
N39 C42 C43 C48 -175.8(2) . . . . ?
N39 C42 C43 C44 4.0(3) . . . . ?
N58 C59 C60 N56 0.1(4) . . . . ?
N15 C18 C19 C24 -175.29(19) . . . . ?
N15 C18 C19 C20 2.6(3) . . . . ?
N56 C49 C48 C43 174.2(2) . . . . ?
N56 C49 C48 C47 -6.3(4) . . . . ?
C38 N37 C41 C40 -0.2(3) . . . . ?
C38 N39 C42 C55 -78.1(3) . . . . ?
C38 N39 C42 C43 101.2(3) . . . . ?
C38 N39 C40 C41 0.2(3) . . . . ?
C2 N1 C5 C4 0.2(3) . . . . ?
C2 N3 C6 C12 71.1(3) . . . . ?
C2 N3 C6 C7 -107.9(2) . . . . ?
C2 N3 C4 C5 0.0(3) . . . . ?
C14 N13 C17 C16 -0.4(3) . . . . ?
C14 N15 C18 C31 -93.6(3) . . . . ?
C14 N15 C18 C19 83.2(3) . . . . ?
C14 N15 C16 C17 -0.6(3) . . . . ?
C66 S70 O72 Ni1 -90.1(3) . . . 1_554 ?
C66 C65 C64 C63 -175.23(18) . . . . ?
C66 C65 C64 C69 2.8(3) . . . . ?
C66 C67 C68 C69 3.0(3) . . . . ?
C66 C67 C68 C74 -177.70(18) . . . . ?
C68 C69 C64 C63 174.42(18) . . . . ?
C68 C69 C64 C65 -3.6(3) . . . . ?
C68 C67 C66 S70 177.86(15) . . . . ?
C68 C67 C66 C65 -3.8(3) . . . . ?
C64 C65 C66 S70 179.23(15) . . . . ?
C64 C65 C66 C67 0.9(3) . . . . ?
C64 C69 C68 C67 0.7(3) . . . . ?
C64 C69 C68 C74 -178.62(18) . . . . ?
C6 N3 C2 N1 -178.25(19) . . . . ?
C6 N3 C4 C5 178.3(2) . . . . ?
C6 C7 C8 C9 -179.9(3) . . . . ?
C31 C26 C25 N32 -174.56(19) . . . . ?
C31 C26 C25 C24 2.5(3) . . . . ?
C31 C26 C27 C28 2.1(3) . . . . ?
C31 C18 C19 C24 1.3(3) . . . . ?
C31 C18 C19 C20 179.2(2) . . . . ?
C31 C30 C29 C28 1.2(4) . . . . ?
C12 C6 C7 C12 -0.8(3) . . . 3_567 ?
C12 C6 C7 C8 179.3(2) . . . . ?
C12 C7 C8 C9 0.2(4) 3_567 . . . ?
C12 C11 C10 C9 1.1(5) 3_567 . . . ?
C36 N32 C25 C26 76.9(3) . . . . ?
C36 N32 C25 C24 -100.4(3) . . . . ?
C36 N32 C33 N34 0.1(3) . . . . ?
C57 N58 C59 C60 -2.7(3) . . . . ?
C57 N56 C49 C50 -73.6(3) . . . . ?
C57 N56 C49 C48 110.0(3) . . . . ?
C57 N56 C60 C59 2.4(3) . . . . ?
C7 C6 C12 C7 0.8(4) . . . 3_567 ?
C7 C6 C12 C11 -177.4(2) . . . 3_567 ?
C7 C8 C9 C10 -2.2(5) . . . . ?
C26 C31 C18 N15 178.31(19) . . . . ?
C26 C31 C18 C19 1.7(3) . . . . ?
C26 C31 C30 C29 2.3(3) . . . . ?
C26 C27 C28 C29 1.4(4) . . . . ?
C42 N39 C38 N37 -175.0(2) . . . . ?
C42 N39 C40 C41 174.8(2) . . . . ?
C42 C55 C54 C53 178.2(2) . . . . ?
C42 C55 C50 C49 -0.9(3) . . . . ?
C42 C55 C50 C51 -179.9(2) . . . . ?
C42 C43 C48 C49 -1.2(3) . . . . ?
C42 C43 C48 C47 179.3(2) . . . . ?
C42 C43 C44 C45 179.8(3) . . . . ?
C55 C42 C43 C48 3.5(4) . . . . ?
C55 C42 C43 C44 -176.7(2) . . . . ?
C55 C54 C53 C52 2.0(4) . . . . ?
C55 C50 C49 N56 -173.1(2) . . . . ?
C55 C50 C49 C48 3.1(3) . . . . ?
C55 C50 C51 C52 1.0(4) . . . . ?
C35 N34 C33 N32 0.2(3) . . . . ?
C17 N13 C14 N15 0.0(2) . . . . ?
C18 N15 C14 N13 171.1(2) . . . . ?
C18 N15 C16 C17 -170.9(2) . . . . ?
C18 C31 C26 C25 -3.5(3) . . . . ?
C18 C31 C26 C27 177.3(2) . . . . ?
C18 C31 C30 C29 -179.0(2) . . . . ?
C18 C19 C20 C21 -176.6(3) . . . . ?
C24 C19 C20 C21 1.3(4) . . . . ?
C24 C23 C22 C21 0.7(4) . . . . ?
C41 N37 C38 N39 0.4(2) . . . . ?
C5 N1 C2 N3 -0.2(2) . . . . ?
C54 C55 C50 C49 177.5(2) . . . . ?
C54 C55 C50 C51 -1.5(3) . . . . ?
C54 C53 C52 C51 -2.5(4) . . . . ?
C43 C42 C55 C54 179.3(2) . . . . ?
C43 C42 C55 C50 -2.4(3) . . . . ?
C43 C48 C47 C46 0.8(4) . . . . ?
C43 C44 C45 C46 1.0(5) . . . . ?
C19 C24 C25 N32 177.53(19) . . . . ?
C19 C24 C25 C26 0.4(3) . . . . ?
C19 C24 C23 C22 0.5(4) . . . . ?
C19 C20 C21 C22 -0.1(4) . . . . ?
C25 N32 C36 C35 173.9(2) . . . . ?
C25 N32 C33 N34 -174.1(2) . . . . ?
C25 C26 C27 C28 -176.9(2) . . . . ?
C25 C24 C19 C18 -2.4(3) . . . . ?
C25 C24 C19 C20 179.7(2) . . . . ?
C25 C24 C23 C22 179.3(3) . . . . ?
C33 N34 C35 C36 -0.4(3) . . . . ?
C33 N32 C36 C35 -0.3(2) . . . . ?
C33 N32 C25 C26 -110.0(3) . . . . ?
C33 N32 C25 C24 72.8(3) . . . . ?
C4 N3 C2 N1 0.1(2) . . . . ?
C4 N3 C6 C12 -106.9(3) . . . . ?
C4 N3 C6 C7 74.0(3) . . . . ?
C27 C26 C25 N32 4.5(3) . . . . ?
C27 C26 C25 C24 -178.4(2) . . . . ?
C27 C28 C29 C30 -3.1(4) . . . . ?
C30 C31 C26 C25 175.2(2) . . . . ?
C30 C31 C26 C27 -3.9(3) . . . . ?
C30 C31 C18 N15 -0.3(3) . . . . ?
C30 C31 C18 C19 -177.0(2) . . . . ?
C16 N15 C14 N13 0.4(3) . . . . ?
C16 N15 C18 C31 75.2(3) . . . . ?
C16 N15 C18 C19 -108.0(3) . . . . ?
C50 C55 C54 C53 0.0(3) . . . . ?
C50 C49 C48 C43 -2.1(4) . . . . ?
C50 C49 C48 C47 177.4(2) . . . . ?
C50 C51 C52 C53 0.9(4) . . . . ?
C49 N56 C57 N58 -176.9(3) . . . . ?
C49 N56 C60 C59 175.5(3) . . . . ?
C49 C50 C51 C52 -177.9(2) . . . . ?
C49 C48 C47 C46 -178.6(3) . . . . ?
C23 C24 C19 C18 176.5(2) . . . . ?
C23 C24 C19 C20 -1.5(3) . . . . ?
C23 C24 C25 N32 -1.3(3) . . . . ?
C23 C24 C25 C26 -178.4(2) . . . . ?
C8 C9 C10 C11 1.6(5) . . . . ?
C48 C43 C44 C45 -0.4(4) . . . . ?
C48 C47 C46 C45 -0.2(5) . . . . ?
C40 N39 C38 N37 -0.4(3) . . . . ?
C40 N39 C42 C55 108.3(3) . . . . ?
C40 N39 C42 C43 -72.4(3) . . . . ?
C20 C21 C22 C23 -1.0(5) . . . . ?
C51 C50 C49 N56 5.9(3) . . . . ?
C51 C50 C49 C48 -177.9(2) . . . . ?
C44 C43 C48 C49 179.0(2) . . . . ?
C44 C43 C48 C47 -0.5(4) . . . . ?
C44 C45 C46 C47 -0.8(5) . . . . ?
C59 N58 C57 N56 4.4(3) . . . . ?
C60 N56 C57 N58 -4.4(3) . . . . ?
C60 N56 C49 C50 115.0(3) . . . . ?
C60 N56 C49 C48 -61.4(3) . . . . ?
C84 N86 C87 O88 178.8(3) . . . . ?
C85 N86 C87 O88 0.2(5) . . . . ?
C78 N80 C81 O82 -179.0(3) . . . . ?
C89 N91 C92 O93 -1.5(6) . . . . ?
C79 N80 C81 O82 2.1(6) . . . . ?
C90 N91 C92 O93 -177.5(4) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.8494 0.1251 -10.4017 -0.8918 0.0209 0.4519
2.9474 17.5508 -4.4306 -0.0154 0.0050 0.9999
0.2940 -18.9676 3.1015 -0.1999 0.2946 -0.9345
-7.6837 -8.3182 -0.5234 -0.0190 -0.8236 -0.5669
-5.3395 -6.8087 9.3048 0.6759 -0.0903 -0.7314
0.4383 19.8517 0.2232 0.4448 -0.0554 0.8939
3.7714 -13.5763 -7.4850 -0.9522 0.1250 -0.2789
5.5135 -0.1775 -10.0213 -0.8882 0.1145 0.4450
-4.5631 16.8946 0.1774 0.5086 -0.5911 0.6260
8.4720 0.3350 0.5203 -0.1791 0.9563 0.2312
-0.0199 5.1667 10.3273 0.8755 0.4765 -0.0806
-1.6731 -3.4826 -9.8221 -0.7560 -0.6477 0.0944
-8.7701 1.4728 1.4739 0.3739 -0.9013 -0.2186
2.5296 -7.2711 -10.2313 -0.9817 -0.1833 0.0522
