#------------------------------------------------------------------------------
#$Date: 2024-07-05 18:29:21 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292965 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/87/7248794.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_7248794
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, 4[C3H7NO], 14[H2O]'
_chemical_formula_sum            'C128 H136 N24 Ni3 O34 S2'
_chemical_formula_weight         2794.85
_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                 104.0980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.61780(10)
_cell_length_b                   29.7718(2)
_cell_length_c                   17.1157(2)
_cell_measurement_reflns_used    31802
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      78.6090
_cell_measurement_theta_min      2.9890
_cell_volume                     6730.15(11)
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_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 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  -4.00   1.00    0.20    --   14.00 110.00-150.99   25
  2  ω    -44.00 -19.00   1.00    1.00    --  -87.58  57.00 -60.00   25
  3  ω    -37.00 -11.00   1.00    1.00    --  -87.58  46.00  92.00   26
  4  ω    -36.00  19.00   1.00    0.20    --  -51.89  46.00  92.00   55
  5  ω     -2.00  23.00   1.00    0.20    --   34.00  98.00 179.40   25
  6  ω     91.00 174.00   1.00    1.00    --  107.25  94.00  85.31   83
  7  ω     40.00 123.00   1.00    0.20    --   51.89  46.00  92.00   83
  8  ω    115.00 154.00   1.00    1.00    --  102.12  46.00  92.00   39
  9  ω    129.00 155.00   1.00    1.00    --  107.25  46.00  75.75   26
 10  ω     43.00 114.00   1.00    1.00    --  107.25   8.00-102.71   71
 11  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00-180.00   25
 12  ω     41.00  73.00   1.00    1.00    --  107.25 -76.00-146.10   32
 13  ω     47.00  73.00   1.00    1.00    --  107.25 -73.00-120.92   26
 14  ω     76.00 117.00   1.00    1.00    --  107.25 -73.00-120.92   41
 15  ω     42.00  71.00   1.00    1.00    --  102.12 -57.00 -90.00   29
 16  ω     51.00  86.00   1.00    1.00    --  107.25 -61.00  14.26   35
 17  ω     35.00  88.00   1.00    1.00    --  107.25 -62.00  57.53   53
 18  ω     28.00  64.00   1.00    1.00    --  102.12 -57.00  90.00   36
 19  ω     35.00  61.00   1.00    1.00    --  102.12 -57.00 150.00   26
 20  ω     34.00  84.00   1.00    1.00    --  107.25 -60.00 119.62   50
 21  ω     29.00  55.00   1.00    1.00    --  102.12 -46.00 -57.00   26
 22  ω     29.00  70.00   1.00    1.00    --  102.12 -57.00-120.00   41
 23  ω     33.00  63.00   1.00    1.00    --  107.25 -56.00-155.83   30
 24  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00   0.00   25
 25  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00 -30.00   25
 26  ω    -23.00  58.00   1.00    0.20    --   51.89 -46.00 -57.00   81
 27  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00  90.00   25
 28  ω    111.00 136.00   1.00    1.00    --  107.25 -84.00 -24.62   25
 29  ω     80.00 129.00   1.00    1.00    --  107.25 -88.00  11.98   49
 30  ω     41.00  76.00   1.00    1.00    --  107.25 -88.00  11.98   35
 31  ω     55.00  97.00   1.00    1.00    --  107.25 -84.00 -24.62   42
 32  ω     48.00 104.00   1.00    1.00    --  107.25-122.00-128.96   56
 33  ω   -112.00 -76.00   1.00    1.00    --  -87.58 -46.00 -57.00   36
 34  ω   -162.00-119.00   1.00    1.00    --  -87.58 -46.00 -57.00   43
 35  ω   -154.00 -87.00   1.00    1.00    --  -87.58 -99.00  60.00   67
 36  ω    -83.00 -37.00   1.00    0.20    --  -51.89 -46.00 -57.00   46
;
_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      -0.0771476000
_diffrn_orient_matrix_UB_12      0.0278587000
_diffrn_orient_matrix_UB_13      -0.0619654000
_diffrn_orient_matrix_UB_21      0.0808148000
_diffrn_orient_matrix_UB_22      0.0088437000
_diffrn_orient_matrix_UB_23      -0.0473955000
_diffrn_orient_matrix_UB_31      -0.0336525000
_diffrn_orient_matrix_UB_32      -0.0426801000
_diffrn_orient_matrix_UB_33      -0.0502710000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73390
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.073
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.737
_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    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         14350
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1010P)²+17.9068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2222
_refine_ls_wR_factor_ref         0.2267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12816
_reflns_number_total             14350
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-185n-dry_r_abs
_cod_depositor_comments
'Adding full bibliography for 7248786--7248794.cif.'
_cod_database_code               7248794
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H14 N4 O6 S1 Ni1'
_chemical_oxdiff_usercomment     'pale/light green cut 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   0.855
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N37-C38A \\sim N37-C38B
 with sigma of 0.02
 N37-C41A \\sim N37-C41B
 with sigma of 0.02
 N39-C38A \\sim N39-C38B
 with sigma of 0.02
 N39-C40A \\sim N39-C40B
 with sigma of 0.02
 C41A-C40A \\sim C41B-C40B
 with sigma of 0.02
 N37-C40A \\sim N37-C40B
 with sigma of 0.04
 N39-C41A \\sim N39-C41B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N39) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C41B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C40B) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.1
Uanis(C38A) \\sim Ueq, Uanis(C38B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C53) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) =
Uanis(C43) = Uanis(C55) = Uanis(C54) = Uanis(C52) = Uanis(C51) = Uanis(C50)
Uanis(N39) = Uanis(N37) = Uanis(N56) = Uanis(N58)
Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C7) = Uanis(C8) = Uanis(C9)
4. Others
 Fixed Sof: C38A(0.65) H38A(0.65) C41A(0.65) H41A(0.65) C40A(0.65) H40A(0.65)
 C41B(0.35) H41B(0.35) C40B(0.35) H40B(0.35) C38B(0.35) H38B(0.35)
5.a Rotating group:
 O77(H77A,H77B)
5.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C14(H14), C67(H67), C57(H57), C2(H2), C17(H17), C69(H69), C33(H33),
 C27(H27), C20(H20), C16(H16), C5(H5), C59(H59), C29(H29), C47(H47), C23(H23),
 C28(H28), C4(H4), C30(H30), C21(H21), C35(H35), C36(H36), C22(H22), C60(H60),
 C8(H8), C51(H51), C11(H11), C54(H54), C44(H44), C46(H46), C52(H52), C45(H45),
 C9(H9), C53(H53), C10(H10), C38A(H38A), C41A(H41A), C40A(H40A), C41B(H41B),
 C40B(H40B), C38B(H38B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.898
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 1.0000 0.5000 0.0000 0.02551(19) Uani 1 2 d S . P . .
Ni2 Ni 0.79204(4) 0.25859(2) 0.60675(3) 0.02440(15) Uani 1 1 d . . . . .
S70 S 0.52367(6) 0.04844(3) 0.32055(5) 0.0342(2) Uani 1 1 d . . . . .
O75 O 0.36859(18) 0.20377(9) 0.20039(13) 0.0329(5) Uani 1 1 d . . . . .
O72 O 0.48668(19) 0.02919(8) 0.38622(16) 0.0353(5) Uani 1 1 d . . . . .
O77 O 0.78042(19) 0.20738(10) 0.68855(15) 0.0384(6) Uani 1 1 d . . . . .
H77A H 0.7714 0.1816 0.6633 0.058 Uiso 1 1 d R U . . .
H77B H 0.8382 0.2044 0.7238 0.058 Uiso 1 1 d R U . . .
O61 O 0.7186(2) 0.21998(9) 0.51297(16) 0.0436(7) Uani 1 1 d . . . . .
O76 O 0.4553(2) 0.25895(9) 0.27742(15) 0.0423(6) Uani 1 1 d . . . . .
O62 O 0.7243(2) 0.15062(9) 0.56587(17) 0.0464(7) Uani 1 1 d . . . . .
N13 N 0.95692(19) 0.43969(9) 0.04447(17) 0.0284(6) Uani 1 1 d . . . . .
N58 N -0.0711(2) 0.23060(12) 0.5949(3) 0.0527(5) Uani 1 1 d . . . . .
O71 O 0.4478(2) 0.04581(11) 0.24447(17) 0.0490(7) Uani 1 1 d . . . . .
N15 N 0.9018(2) 0.39506(10) 0.12708(18) 0.0321(6) Uani 1 1 d . . . . .
N32 N 0.8273(2) 0.35142(10) 0.42829(17) 0.0322(6) Uani 1 1 d . . . . .
O73 O 0.6215(2) 0.03070(11) 0.3168(2) 0.0536(8) Uani 1 1 d . . . . .
N34 N 0.8077(2) 0.31331(10) 0.53344(16) 0.0299(6) Uani 1 1 d . . . . .
N1 N 0.84565(19) 0.51398(10) -0.04142(19) 0.0308(6) Uani 1 1 d . . . . .
N56 N 0.0921(2) 0.22384(12) 0.6056(3) 0.0527(5) Uani 1 1 d . . . . .
N3 N 0.6820(2) 0.51195(12) -0.0489(2) 0.0406(8) Uani 1 1 d . . . . .
C65 C 0.6072(2) 0.11858(12) 0.4162(2) 0.0310(7) Uani 1 1 d . . . . .
H65 H 0.6425 0.0964 0.4522 0.037 Uiso 1 1 calc R U . . .
C66 C 0.5408(2) 0.10607(12) 0.3446(2) 0.0298(7) Uani 1 1 d . . . . .
C68 C 0.4979(2) 0.18342(12) 0.31231(19) 0.0296(7) Uani 1 1 d . . . . .
C74 C 0.4365(3) 0.21879(13) 0.25935(19) 0.0335(7) Uani 1 1 d . . . . .
C18 C 0.8801(3) 0.38102(11) 0.2013(2) 0.0305(7) Uani 1 1 d . . . . .
C14 C 0.9567(2) 0.43200(12) 0.1200(2) 0.0298(7) Uani 1 1 d . . . . .
H14 H 0.9908 0.4501 0.1640 0.036 Uiso 1 1 calc R U . . .
C67 C 0.4846(2) 0.13793(12) 0.29278(19) 0.0287(7) Uani 1 1 d . . . . .
H67 H 0.4377 0.1288 0.2447 0.034 Uiso 1 1 calc R U . . .
C31 C 0.9549(3) 0.35841(12) 0.2576(2) 0.0327(7) Uani 1 1 d . . . . .
C57 C 0.0138(2) 0.25232(12) 0.5998(2) 0.0289(7) Uani 1 1 d . . . . .
H57 H 0.0194 0.2841 0.5993 0.035 Uiso 1 1 calc R U . . .
C25 C 0.8435(3) 0.36041(12) 0.3492(2) 0.0318(7) Uani 1 1 d . . . . .
C26 C 0.9368(3) 0.34886(12) 0.3352(2) 0.0323(7) Uani 1 1 d . . . . .
C2 C 0.7767(2) 0.50684(12) -0.0011(2) 0.0331(8) Uani 1 1 d . . . . .
H2 H 0.7911 0.4991 0.0543 0.040 Uiso 1 1 calc R U . . .
C17 C 0.8997(3) 0.40606(12) 0.0004(2) 0.0346(7) Uani 1 1 d . . . . .
H17 H 0.8867 0.4027 -0.0564 0.042 Uiso 1 1 calc R U . . .
C69 C 0.5677(3) 0.19589(12) 0.3825(2) 0.0312(7) Uani 1 1 d . . . . .
H69 H 0.5788 0.2268 0.3952 0.037 Uiso 1 1 calc R U . . .
C19 C 0.7873(2) 0.39372(12) 0.2161(2) 0.0308(7) Uani 1 1 d . . . . .
C24 C 0.7674(3) 0.38170(13) 0.2928(2) 0.0344(7) Uani 1 1 d . . . . .
C33 C 0.8119(3) 0.31086(13) 0.4584(2) 0.0346(7) Uani 1 1 d . . . . .
H33 H 0.8050 0.2837 0.4283 0.041 Uiso 1 1 calc R U . . .
C27 C 1.0175(3) 0.32923(14) 0.3959(2) 0.0388(8) Uani 1 1 d . . . . .
H27 H 1.0079 0.3232 0.4480 0.047 Uiso 1 1 calc R U . . .
C63 C 0.6942(3) 0.17853(14) 0.5118(2) 0.0389(8) Uani 1 1 d . . . . .
N37 N 0.6519(2) 0.28139(12) 0.6178(3) 0.0527(5) Uani 1 1 d D . . . .
C64 C 0.6216(2) 0.16356(12) 0.4347(2) 0.0318(7) Uani 1 1 d . . . . .
C6 C 0.5891(2) 0.50592(13) -0.0242(3) 0.0381(9) Uani 1 1 d . . . . .
C49 C 0.1941(2) 0.23570(13) 0.6074(3) 0.0420(10) Uani 1 1 d . . . . .
C20 C 0.7127(3) 0.41893(13) 0.1602(2) 0.0371(8) Uani 1 1 d . . . . .
H20 H 0.7254 0.4279 0.1103 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8648(3) 0.37841(13) 0.0510(2) 0.0412(9) Uani 1 1 d . . . . .
H16 H 0.8231 0.3527 0.0365 0.049 Uiso 1 1 calc R U . . .
C48 C 0.2274(4) 0.2309(2) 0.5367(4) 0.0670(5) Uani 1 1 d . . . . .
C12 C 0.5598(3) 0.53885(18) 0.0221(4) 0.0658(6) Uani 1 1 d . . . . .
C7 C 0.5329(3) 0.46684(18) -0.0483(4) 0.0658(6) Uani 1 1 d . . . . .
C5 C 0.7937(3) 0.52404(18) -0.1185(3) 0.0499(11) Uani 1 1 d . . . . .
H5 H 0.8239 0.5308 -0.1616 0.060 Uiso 1 1 calc R U . . .
C43 C 0.3277(4) 0.2467(2) 0.5362(4) 0.0670(5) Uani 1 1 d . . . . .
C59 C -0.0468(3) 0.18584(14) 0.5970(3) 0.0524(12) Uani 1 1 d . . . . .
H59 H -0.0934 0.1618 0.5947 0.063 Uiso 1 1 calc R U . . .
C50 C 0.2551(4) 0.2520(2) 0.6788(4) 0.0670(5) Uani 1 1 d . . . . .
C29 C 1.1236(3) 0.32676(17) 0.3021(3) 0.0545(12) Uani 1 1 d . . . . .
H29 H 1.1864 0.3185 0.2913 0.065 Uiso 1 1 calc R U . . .
C47 C 0.1668(4) 0.2122(2) 0.4655(4) 0.0670(5) Uani 1 1 d . . . . .
H47 H 0.1012 0.2012 0.4649 0.080 Uiso 1 1 calc R U . . .
C42 C 0.3877(3) 0.26221(15) 0.6073(4) 0.0628(16) Uani 1 1 d . . . . .
C23 C 0.6709(3) 0.39316(17) 0.3067(3) 0.0486(10) Uani 1 1 d . . . . .
H23 H 0.6551 0.3845 0.3557 0.058 Uiso 1 1 calc R U . . .
C28 C 1.1072(3) 0.31924(16) 0.3790(3) 0.0494(11) Uani 1 1 d . . . . .
H28 H 1.1601 0.3069 0.4201 0.059 Uiso 1 1 calc R U . . .
C4 C 0.6927(3) 0.5230(2) -0.1242(3) 0.0575(13) Uani 1 1 d . . . . .
H4 H 0.6400 0.5287 -0.1708 0.069 Uiso 1 1 calc R U . . .
C30 C 1.0503(3) 0.34577(14) 0.2430(3) 0.0417(9) Uani 1 1 d . . . . .
H30 H 1.0625 0.3507 0.1914 0.050 Uiso 1 1 calc R U . . .
C21 C 0.6238(3) 0.43022(17) 0.1776(3) 0.0491(10) Uani 1 1 d . . . . .
H21 H 0.5757 0.4477 0.1404 0.059 Uiso 1 1 calc R U . . .
C55 C 0.3575(4) 0.2644(2) 0.6805(4) 0.0670(5) Uani 1 1 d . . . . .
N39 N 0.4885(2) 0.27941(12) 0.6115(3) 0.0527(5) Uani 1 1 d D U . . .
C35 C 0.8177(4) 0.35729(15) 0.5530(3) 0.0569(13) Uani 1 1 d . . . . .
H35 H 0.8168 0.3695 0.6040 0.068 Uiso 1 1 calc R U . . .
C36 C 0.8293(4) 0.38129(15) 0.4887(3) 0.0551(12) Uani 1 1 d . . . . .
H36 H 0.8373 0.4129 0.4862 0.066 Uiso 1 1 calc R U . . .
C22 C 0.6019(3) 0.4162(2) 0.2505(3) 0.0609(14) Uani 1 1 d . . . . .
H22 H 0.5378 0.4230 0.2602 0.073 Uiso 1 1 calc R U . . .
C60 C 0.0536(3) 0.18098(15) 0.6030(4) 0.0614(15) Uani 1 1 d . . . . .
H60 H 0.0899 0.1536 0.6049 0.074 Uiso 1 1 calc R U . . .
C8 C 0.5616(4) 0.43312(17) -0.0961(4) 0.0658(6) Uani 1 1 d . . . . .
H8 H 0.6243 0.4357 -0.1108 0.079 Uiso 1 1 calc R U . . .
C51 C 0.2208(4) 0.2575(2) 0.7520(4) 0.0670(5) Uani 1 1 d . . . . .
H51 H 0.1526 0.2502 0.7510 0.080 Uiso 1 1 calc R U . . .
C11 C 0.6181(4) 0.57842(18) 0.0454(4) 0.0658(6) Uani 1 1 d . . . . .
H11 H 0.6767 0.5836 0.0258 0.079 Uiso 1 1 calc R U . . .
C54 C 0.4209(4) 0.2777(2) 0.7607(4) 0.0670(5) Uani 1 1 d . . . . .
H54 H 0.4902 0.2847 0.7655 0.080 Uiso 1 1 calc R U . . .
C44 C 0.3582(4) 0.2451(2) 0.4623(4) 0.0670(5) Uani 1 1 d . U . . .
H44 H 0.4228 0.2565 0.4603 0.080 Uiso 1 1 calc R U . . .
C46 C 0.2020(4) 0.2099(2) 0.3971(4) 0.0670(5) Uani 1 1 d . . . . .
H46 H 0.1624 0.1961 0.3498 0.080 Uiso 1 1 calc R U . . .
C52 C 0.2822(4) 0.2728(2) 0.8222(4) 0.0670(5) Uani 1 1 d . . . . .
H52 H 0.2556 0.2782 0.8677 0.080 Uiso 1 1 calc R U . . .
C45 C 0.2993(4) 0.2285(2) 0.3977(4) 0.0670(5) Uani 1 1 d . U . . .
H45 H 0.3213 0.2286 0.3492 0.080 Uiso 1 1 calc R U . . .
C9 C 0.5006(3) 0.39637(18) -0.1222(4) 0.0658(6) Uani 1 1 d . . . . .
H9 H 0.5189 0.3749 -0.1572 0.079 Uiso 1 1 calc R U . . .
C53 C 0.3842(4) 0.2802(2) 0.8265(4) 0.0670(5) Uani 1 1 d . U . . .
H53 H 0.4287 0.2872 0.8770 0.080 Uiso 1 1 calc R U . . .
C10 C 0.5909(3) 0.60888(18) 0.0954(4) 0.0658(6) Uani 1 1 d . . . . .
H10 H 0.6332 0.6341 0.1129 0.079 Uiso 1 1 calc R U . . .
C38A C 0.5744(6) 0.2564(4) 0.6165(10) 0.047(5) Uani 0.65 1 d D U P A 1
H38A H 0.5778 0.2246 0.6190 0.056 Uiso 0.65 1 calc R U P A 1
C41A C 0.6275(4) 0.3233(2) 0.6501(4) 0.0462(15) Uani 0.65 1 d D . P A 1
H41A H 0.6738 0.3469 0.6702 0.055 Uiso 0.65 1 calc R U P A 1
C40A C 0.5268(4) 0.3234(2) 0.6469(5) 0.0478(16) Uani 0.65 1 d D . P A 1
H40A H 0.4889 0.3467 0.6637 0.057 Uiso 0.65 1 calc R U P A 1
C41B C 0.5976(8) 0.3178(6) 0.5536(10) 0.075(6) Uani 0.35 1 d D U P A 2
H41B H 0.6302 0.3376 0.5243 0.089 Uiso 0.35 1 calc R U P A 2
C40B C 0.4966(8) 0.3157(5) 0.5479(10) 0.069(5) Uani 0.35 1 d D U P A 2
H40B H 0.4438 0.3323 0.5134 0.083 Uiso 0.35 1 calc R U P A 2
C38B C 0.5714(8) 0.2571(5) 0.6078(13) 0.023(6) Uani 0.35 1 d D U P A 2
H38B H 0.5715 0.2257 0.5986 0.028 Uiso 0.35 1 calc R U P A 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'
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
-1 0 1 0.0768
8 5 -6 0.0853
-1 19 -1 0.0616
4 -12 6 0.0613
0 15 7 0.0597
-1 10 -9 0.0509
-8 7 0 0.0568
-3 18 3 0.0488
-4 -9 -7 0.0439
2 -9 -10 0.0431
-1 -18 -4 0.0459
-6 13 4 0.0422
7 -7 3 0.0697
5 16 -1 0.0678
-4 -9 9 0.0772
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 180.00(14) 4_665 2_655 ?
N13 Ni1 O72 90.78(11) . 4_665 ?
N13 Ni1 O72 89.22(11) . 2_655 ?
N13 Ni1 O72 90.79(11) 3_765 2_655 ?
N13 Ni1 O72 89.21(11) 3_765 4_665 ?
N13 Ni1 N13 180.0 . 3_765 ?
N13 Ni1 N1 86.92(10) . . ?
N13 Ni1 N1 93.08(10) 3_765 . ?
N13 Ni1 N1 86.92(10) 3_765 3_765 ?
N13 Ni1 N1 93.08(10) . 3_765 ?
N1 Ni1 O72 94.86(11) . 2_655 ?
N1 Ni1 O72 94.86(11) 3_765 4_665 ?
N1 Ni1 O72 85.14(11) . 4_665 ?
N1 Ni1 O72 85.14(11) 3_765 2_655 ?
N1 Ni1 N1 180.0 . 3_765 ?
O75 Ni2 O77 88.96(10) 4_666 . ?
O75 Ni2 O61 178.54(12) 4_666 . ?
O75 Ni2 N58 89.91(14) 4_666 1_655 ?
O75 Ni2 N34 86.33(11) 4_666 . ?
O75 Ni2 N37 93.12(14) 4_666 . ?
O61 Ni2 O77 90.76(11) . . ?
O61 Ni2 N58 88.65(15) . 1_655 ?
O61 Ni2 N34 93.97(11) . . ?
O61 Ni2 N37 88.30(15) . . ?
N58 Ni2 O77 89.38(13) 1_655 . ?
N58 Ni2 N34 91.62(13) 1_655 . ?
N34 Ni2 O77 175.18(11) . . ?
N37 Ni2 O77 87.51(13) . . ?
N37 Ni2 N58 175.62(15) . 1_655 ?
N37 Ni2 N34 91.73(13) . . ?
O72 S70 C66 104.68(15) . . ?
O71 S70 O72 111.48(17) . . ?
O71 S70 C66 106.59(17) . . ?
O73 S70 O72 112.67(19) . . ?
O73 S70 O71 113.62(19) . . ?
O73 S70 C66 107.09(17) . . ?
C74 O75 Ni2 124.6(2) . 4_565 ?
S70 O72 Ni1 155.60(16) . 2_645 ?
Ni2 O77 H77A 109.4 . . ?
Ni2 O77 H77B 109.5 . . ?
H77A O77 H77B 104.2 . . ?
C63 O61 Ni2 129.5(2) . . ?
C14 N13 Ni1 125.2(2) . . ?
C14 N13 C17 106.1(3) . . ?
C17 N13 Ni1 126.7(2) . . ?
C57 N58 Ni2 126.1(3) . 1_455 ?
C57 N58 C59 105.9(3) . . ?
C59 N58 Ni2 126.8(3) . 1_455 ?
C14 N15 C18 123.7(3) . . ?
C14 N15 C16 107.0(3) . . ?
C16 N15 C18 129.0(3) . . ?
C33 N32 C25 126.5(3) . . ?
C33 N32 C36 105.8(3) . . ?
C36 N32 C25 127.6(3) . . ?
C33 N34 Ni2 125.6(3) . . ?
C33 N34 C35 105.8(3) . . ?
C35 N34 Ni2 128.6(3) . . ?
C2 N1 Ni1 125.4(2) . . ?
C2 N1 C5 105.9(3) . . ?
C5 N1 Ni1 127.7(2) . . ?
C57 N56 C49 126.5(3) . . ?
C57 N56 C60 107.0(3) . . ?
C60 N56 C49 126.3(3) . . ?
C2 N3 C6 125.6(3) . . ?
C2 N3 C4 106.9(3) . . ?
C4 N3 C6 127.5(3) . . ?
C66 C65 H65 120.3 . . ?
C64 C65 H65 120.3 . . ?
C64 C65 C66 119.4(3) . . ?
C65 C66 S70 119.2(3) . . ?
C65 C66 C67 121.3(3) . . ?
C67 C66 S70 119.5(2) . . ?
C67 C68 C74 120.9(3) . . ?
C69 C68 C74 119.8(3) . . ?
C69 C68 C67 119.2(3) . . ?
O75 C74 C68 115.0(3) . . ?
O76 C74 O75 126.9(3) . . ?
O76 C74 C68 118.2(3) . . ?
C31 C18 N15 118.7(3) . . ?
C31 C18 C19 123.0(3) . . ?
C19 C18 N15 118.1(3) . . ?
N13 C14 N15 111.3(3) . . ?
N13 C14 H14 124.3 . . ?
N15 C14 H14 124.3 . . ?
C66 C67 C68 119.3(3) . . ?
C66 C67 H67 120.4 . . ?
C68 C67 H67 120.4 . . ?
C18 C31 C26 118.3(3) . . ?
C18 C31 C30 123.2(3) . . ?
C30 C31 C26 118.4(3) . . ?
N58 C57 N56 111.4(3) . . ?
N58 C57 H57 124.3 . . ?
N56 C57 H57 124.3 . . ?
C26 C25 N32 117.9(3) . . ?
C24 C25 N32 118.5(3) . . ?
C24 C25 C26 123.6(3) . . ?
C31 C26 C27 118.3(3) . . ?
C25 C26 C31 118.6(3) . . ?
C25 C26 C27 123.0(3) . . ?
N1 C2 N3 111.3(3) . . ?
N1 C2 H2 124.4 . . ?
N3 C2 H2 124.4 . . ?
N13 C17 H17 125.4 . . ?
C16 C17 N13 109.2(3) . . ?
C16 C17 H17 125.4 . . ?
C68 C69 H69 119.6 . . ?
C68 C69 C64 120.8(3) . . ?
C64 C69 H69 119.6 . . ?
C18 C19 C24 118.3(3) . . ?
C18 C19 C20 123.2(3) . . ?
C20 C19 C24 118.5(3) . . ?
C25 C24 C19 118.0(3) . . ?
C25 C24 C23 123.7(3) . . ?
C23 C24 C19 118.2(3) . . ?
N32 C33 H33 124.0 . . ?
N34 C33 N32 112.0(3) . . ?
N34 C33 H33 124.0 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.4(4) . . ?
C28 C27 H27 119.8 . . ?
O61 C63 C64 114.3(3) . . ?
O62 C63 O61 126.9(3) . . ?
O62 C63 C64 118.8(3) . . ?
C38A N37 Ni2 125.3(5) . . ?
C38A N37 C41A 104.0(5) . . ?
C41A N37 Ni2 128.5(3) . . ?
C41B N37 Ni2 116.3(5) . . ?
C38B N37 Ni2 125.2(7) . . ?
C38B N37 C41B 93.0(10) . . ?
C65 C64 C69 120.0(3) . . ?
C65 C64 C63 120.9(3) . . ?
C69 C64 C63 119.1(3) . . ?
C12 C6 N3 118.6(4) . . ?
C12 C6 C7 123.1(4) . . ?
C7 C6 N3 118.3(4) . . ?
C48 C49 N56 118.4(4) . . ?
C50 C49 N56 118.4(4) . . ?
C50 C49 C48 123.2(4) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.7(4) . . ?
C21 C20 H20 119.7 . . ?
N15 C16 H16 126.8 . . ?
C17 C16 N15 106.4(3) . . ?
C17 C16 H16 126.8 . . ?
C49 C48 C43 118.5(6) . . ?
C49 C48 C47 122.9(5) . . ?
C47 C48 C43 118.6(5) . . ?
C6 C12 C7 119.4(4) . 3_665 ?
C6 C12 C11 122.0(4) . . ?
C11 C12 C7 118.6(5) . 3_665 ?
C6 C7 C12 117.5(5) . 3_665 ?
C6 C7 C8 123.7(4) . . ?
C8 C7 C12 118.8(5) . 3_665 ?
N1 C5 H5 125.1 . . ?
C4 C5 N1 109.9(4) . . ?
C4 C5 H5 125.1 . . ?
C42 C43 C48 117.7(5) . . ?
C42 C43 C44 124.0(5) . . ?
C44 C43 C48 118.3(6) . . ?
N58 C59 H59 125.1 . . ?
C60 C59 N58 109.8(4) . . ?
C60 C59 H59 125.1 . . ?
C49 C50 C55 118.5(5) . . ?
C49 C50 C51 123.5(5) . . ?
C55 C50 C51 118.0(6) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C30 C29 C28 120.4(4) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 C48 120.4(5) . . ?
C46 C47 H47 119.8 . . ?
C43 C42 C55 124.3(4) . . ?
C43 C42 N39 121.1(5) . . ?
C55 C42 N39 114.6(5) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 C24 120.6(4) . . ?
C22 C23 H23 119.7 . . ?
C27 C28 C29 121.4(4) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
N3 C4 H4 127.0 . . ?
C5 C4 N3 106.1(3) . . ?
C5 C4 H4 127.0 . . ?
C31 C30 H30 119.5 . . ?
C29 C30 C31 120.9(4) . . ?
C29 C30 H30 119.5 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.7(4) . . ?
C22 C21 H21 119.6 . . ?
C50 C55 C54 115.4(5) . . ?
C42 C55 C50 117.5(6) . . ?
C42 C55 C54 127.1(5) . . ?
C42 N39 C40A 124.5(4) . . ?
C42 N39 C40B 116.0(5) . . ?
C38A N39 C42 128.6(5) . . ?
C38A N39 C40A 102.2(6) . . ?
C38B N39 C42 128.9(7) . . ?
C38B N39 C40B 96.2(10) . . ?
N34 C35 H35 125.2 . . ?
N34 C35 C36 109.6(4) . . ?
C36 C35 H35 125.2 . . ?
N32 C36 H36 126.6 . . ?
C35 C36 N32 106.7(4) . . ?
C35 C36 H36 126.6 . . ?
C23 C22 C21 121.1(4) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N56 C60 H60 127.1 . . ?
C59 C60 N56 105.9(4) . . ?
C59 C60 H60 127.1 . . ?
C7 C8 H8 119.2 . . ?
C9 C8 C7 121.5(5) . . ?
C9 C8 H8 119.2 . . ?
C50 C51 H51 118.6 . . ?
C52 C51 C50 122.8(5) . . ?
C52 C51 H51 118.6 . . ?
C12 C11 H11 119.7 . . ?
C10 C11 C12 120.7(5) . . ?
C10 C11 H11 119.7 . . ?
C55 C54 H54 118.7 . . ?
C53 C54 C55 122.7(5) . . ?
C53 C54 H54 118.7 . . ?
C43 C44 H44 119.5 . . ?
C45 C44 C43 121.0(5) . . ?
C45 C44 H44 119.5 . . ?
C47 C46 H46 120.4 . . ?
C47 C46 C45 119.3(6) . . ?
C45 C46 H46 120.4 . . ?
C51 C52 H52 120.3 . . ?
C51 C52 C53 119.4(6) . . ?
C53 C52 H52 120.3 . . ?
C44 C45 C46 122.3(6) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C8 C9 H9 120.6 . . ?
C8 C9 C10 118.9(5) . 3_665 ?
C10 C9 H9 120.6 3_665 . ?
C54 C53 C52 121.2(6) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C11 C10 C9 121.3(5) . 3_665 ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 3_665 . ?
N37 C38A N39 114.0(8) . . ?
N37 C38A H38A 123.0 . . ?
N39 C38A H38A 123.0 . . ?
N37 C41A H41A 125.9 . . ?
C40A C41A N37 108.2(5) . . ?
C40A C41A H41A 125.9 . . ?
N39 C40A H40A 127.3 . . ?
C41A C40A N39 105.3(5) . . ?
C41A C40A H40A 127.3 . . ?
N37 C41B H41B 125.9 . . ?
C40B C41B N37 108.1(8) . . ?
C40B C41B H41B 125.9 . . ?
N39 C40B H40B 128.5 . . ?
C41B C40B N39 103.0(8) . . ?
C41B C40B H40B 128.5 . . ?
N37 C38B N39 114.9(11) . . ?
N37 C38B H38B 122.6 . . ?
N39 C38B H38B 122.6 . . ?
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 2.100(3) 4_665 ?
Ni1 O72 2.100(3) 2_655 ?
Ni1 N13 2.089(3) . ?
Ni1 N13 2.089(3) 3_765 ?
Ni1 N1 2.090(3) . ?
Ni1 N1 2.090(3) 3_765 ?
Ni2 O75 2.024(2) 4_666 ?
Ni2 O77 2.102(3) . ?
Ni2 O61 2.029(3) . ?
Ni2 N58 2.096(3) 1_655 ?
Ni2 N34 2.099(3) . ?
Ni2 N37 2.077(3) . ?
S70 O72 1.456(3) . ?
S70 O71 1.454(3) . ?
S70 O73 1.449(3) . ?
S70 C66 1.766(4) . ?
O75 Ni2 2.024(2) 4_565 ?
O75 C74 1.273(4) . ?
O72 Ni1 2.100(3) 2_645 ?
O77 H77A 0.8744 . ?
O77 H77B 0.8723 . ?
O61 C63 1.277(5) . ?
O76 C74 1.246(5) . ?
O62 C63 1.237(5) . ?
N13 C14 1.313(4) . ?
N13 C17 1.375(5) . ?
N58 Ni2 2.096(3) 1_455 ?
N58 C57 1.309(5) . ?
N58 C59 1.371(5) . ?
N15 C18 1.434(4) . ?
N15 C14 1.352(4) . ?
N15 C16 1.369(5) . ?
N32 C25 1.449(4) . ?
N32 C33 1.349(5) . ?
N32 C36 1.359(5) . ?
N34 C33 1.302(4) . ?
N34 C35 1.350(5) . ?
N1 C2 1.311(4) . ?
N1 C5 1.370(5) . ?
N56 C57 1.348(4) . ?
N56 C49 1.426(4) . ?
N56 C60 1.377(6) . ?
N3 C2 1.357(4) . ?
N3 C6 1.439(4) . ?
N3 C4 1.371(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.385(4) . ?
C65 C64 1.379(5) . ?
C66 C67 1.393(5) . ?
C68 C74 1.503(5) . ?
C68 C67 1.396(5) . ?
C68 C69 1.388(4) . ?
C18 C31 1.393(5) . ?
C18 C19 1.400(5) . ?
C14 H14 0.9500 . ?
C67 H67 0.9500 . ?
C31 C26 1.437(5) . ?
C31 C30 1.431(5) . ?
C57 H57 0.9500 . ?
C25 C26 1.393(5) . ?
C25 C24 1.385(5) . ?
C26 C27 1.439(5) . ?
C2 H2 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.362(5) . ?
C69 H69 0.9500 . ?
C69 C64 1.394(5) . ?
C19 C24 1.450(5) . ?
C19 C20 1.428(5) . ?
C24 C23 1.432(5) . ?
C33 H33 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.354(5) . ?
C63 C64 1.511(4) . ?
N37 C38A 1.287(9) . ?
N37 C41A 1.436(7) . ?
N37 C41B 1.592(10) . ?
N37 C38B 1.290(12) . ?
C6 C12 1.379(7) . ?
C6 C7 1.399(6) . ?
C49 C48 1.400(7) . ?
C49 C50 1.388(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.358(6) . ?
C16 H16 0.9500 . ?
C48 C43 1.446(7) . ?
C48 C47 1.408(9) . ?
C12 C7 1.449(6) 3_665 ?
C12 C11 1.423(7) . ?
C7 C12 1.449(6) 3_665 ?
C7 C8 1.410(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.355(5) . ?
C43 C42 1.370(9) . ?
C43 C44 1.426(8) . ?
C59 H59 0.9500 . ?
C59 C60 1.353(5) . ?
C50 C55 1.437(7) . ?
C50 C51 1.448(8) . ?
C29 H29 0.9500 . ?
C29 C28 1.407(6) . ?
C29 C30 1.359(6) . ?
C47 H47 0.9500 . ?
C47 C46 1.370(8) . ?
C42 C55 1.412(8) . ?
C42 N39 1.450(5) . ?
C23 H23 0.9500 . ?
C23 C22 1.356(6) . ?
C28 H28 0.9500 . ?
C4 H4 0.9500 . ?
C30 H30 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.415(7) . ?
C55 C54 1.486(9) . ?
N39 C38A 1.340(8) . ?
N39 C40A 1.484(8) . ?
N39 C40B 1.557(10) . ?
N39 C38B 1.324(13) . ?
C35 H35 0.9500 . ?
C35 C36 1.353(6) . ?
C36 H36 0.9500 . ?
C22 H22 0.9500 . ?
C60 H60 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.380(7) . ?
C51 H51 0.9500 . ?
C51 C52 1.364(9) . ?
C11 H11 0.9500 . ?
C11 C10 1.358(8) . ?
C54 H54 0.9500 . ?
C54 C53 1.341(8) . ?
C44 H44 0.9500 . ?
C44 C45 1.295(9) . ?
C46 H46 0.9500 . ?
C46 C45 1.434(7) . ?
C52 H52 0.9500 . ?
C52 C53 1.391(7) . ?
C45 H45 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.438(6) 3_665 ?
C53 H53 0.9500 . ?
C10 C9 1.438(7) 3_665 ?
C10 H10 0.9500 . ?
C38A H38A 0.9500 . ?
C41A H41A 0.9500 . ?
C41A C40A 1.360(7) . ?
C40A H40A 0.9500 . ?
C41B H41B 0.9500 . ?
C41B C40B 1.356(12) . ?
C40B H40B 0.9500 . ?
C38B H38B 0.9500 . ?
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 0.87 1.88 2.658(4) 147.8 .
O77 H77B O76 0.87 1.97 2.688(4) 139.3 4_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 N13 C14 N15 164.3(2) . . . . ?
Ni1 N13 C17 C16 -163.7(3) . . . . ?
Ni1 N1 C2 N3 -169.3(3) . . . . ?
Ni1 N1 C5 C4 169.0(4) . . . . ?
Ni2 O75 C74 O76 13.5(5) 4_565 . . . ?
Ni2 O75 C74 C68 -167.7(2) 4_565 . . . ?
Ni2 O61 C63 O62 -12.3(7) . . . . ?
Ni2 O61 C63 C64 168.1(3) . . . . ?
Ni2 N58 C57 N56 167.6(3) 1_455 . . . ?
Ni2 N58 C59 C60 -168.2(4) 1_455 . . . ?
Ni2 N34 C33 N32 -176.9(2) . . . . ?
Ni2 N34 C35 C36 177.9(3) . . . . ?
Ni2 N37 C38A N39 -169.6(7) . . . . ?
Ni2 N37 C41A C40A -178.7(5) . . . . ?
Ni2 N37 C41B C40B 156.0(13) . . . . ?
Ni2 N37 C38B N39 -174.8(9) . . . . ?
S70 C66 C67 C68 179.6(2) . . . . ?
O72 S70 C66 C65 59.7(3) . . . . ?
O72 S70 C66 C67 -118.0(3) . . . . ?
O61 C63 C64 C65 164.3(4) . . . . ?
O61 C63 C64 C69 -16.6(5) . . . . ?
O62 C63 C64 C65 -15.3(6) . . . . ?
O62 C63 C64 C69 163.8(4) . . . . ?
N13 C17 C16 N15 -0.5(5) . . . . ?
N58 C59 C60 N56 0.8(7) . . . . ?
O71 S70 O72 Ni1 158.2(4) . . . 2_645 ?
O71 S70 C66 C65 177.9(3) . . . . ?
O71 S70 C66 C67 0.3(3) . . . . ?
N15 C18 C31 C26 173.2(3) . . . . ?
N15 C18 C31 C30 -4.3(6) . . . . ?
N15 C18 C19 C24 -176.7(3) . . . . ?
N15 C18 C19 C20 1.5(5) . . . . ?
N32 C25 C26 C31 -178.7(3) . . . . ?
N32 C25 C26 C27 -1.0(6) . . . . ?
N32 C25 C24 C19 175.2(3) . . . . ?
N32 C25 C24 C23 -3.7(6) . . . . ?
O73 S70 O72 Ni1 29.1(4) . . . 2_645 ?
O73 S70 C66 C65 -60.2(3) . . . . ?
O73 S70 C66 C67 122.2(3) . . . . ?
N34 C35 C36 N32 -0.5(6) . . . . ?
N1 C5 C4 N3 0.0(6) . . . . ?
N56 C49 C48 C43 174.4(4) . . . . ?
N56 C49 C48 C47 -4.1(7) . . . . ?
N56 C49 C50 C55 -179.4(4) . . . . ?
N56 C49 C50 C51 0.2(7) . . . . ?
N3 C6 C12 C7 -179.4(5) . . . 3_665 ?
N3 C6 C12 C11 0.4(8) . . . . ?
N3 C6 C7 C12 179.4(4) . . . 3_665 ?
N3 C6 C7 C8 -0.6(8) . . . . ?
C65 C66 C67 C68 2.0(5) . . . . ?
C66 S70 O72 Ni1 -86.9(4) . . . 2_645 ?
C66 C65 C64 C69 1.6(5) . . . . ?
C66 C65 C64 C63 -179.3(3) . . . . ?
C68 C69 C64 C65 1.1(5) . . . . ?
C68 C69 C64 C63 -178.0(3) . . . . ?
C74 C68 C67 C66 -178.1(3) . . . . ?
C74 C68 C69 C64 176.6(3) . . . . ?
C18 N15 C14 N13 -173.8(3) . . . . ?
C18 N15 C16 C17 173.6(4) . . . . ?
C18 C31 C26 C25 3.4(5) . . . . ?
C18 C31 C26 C27 -174.4(3) . . . . ?
C18 C31 C30 C29 175.0(4) . . . . ?
C18 C19 C24 C25 3.4(5) . . . . ?
C18 C19 C24 C23 -177.6(4) . . . . ?
C18 C19 C20 C21 179.8(4) . . . . ?
C14 N13 C17 C16 0.5(4) . . . . ?
C14 N15 C18 C31 -79.1(5) . . . . ?
C14 N15 C18 C19 96.2(4) . . . . ?
C14 N15 C16 C17 0.4(4) . . . . ?
C67 C68 C74 O75 4.8(5) . . . . ?
C67 C68 C74 O76 -176.3(3) . . . . ?
C67 C68 C69 C64 -2.2(5) . . . . ?
C31 C18 C19 C24 -1.6(5) . . . . ?
C31 C18 C19 C20 176.6(3) . . . . ?
C31 C26 C27 C28 -1.4(6) . . . . ?
C57 N58 C59 C60 -0.2(6) . . . . ?
C57 N56 C49 C48 -101.1(6) . . . . ?
C57 N56 C49 C50 78.1(6) . . . . ?
C57 N56 C60 C59 -1.0(6) . . . . ?
C25 N32 C33 N34 175.0(3) . . . . ?
C25 N32 C36 C35 -175.5(4) . . . . ?
C25 C26 C27 C28 -179.1(4) . . . . ?
C25 C24 C23 C22 176.4(5) . . . . ?
C26 C31 C30 C29 -2.5(6) . . . . ?
C26 C25 C24 C19 -1.8(6) . . . . ?
C26 C25 C24 C23 179.2(4) . . . . ?
C26 C27 C28 C29 -1.3(7) . . . . ?
C2 N1 C5 C4 0.1(6) . . . . ?
C2 N3 C6 C12 75.4(6) . . . . ?
C2 N3 C6 C7 -104.6(5) . . . . ?
C2 N3 C4 C5 0.0(6) . . . . ?
C17 N13 C14 N15 -0.2(4) . . . . ?
C69 C68 C74 O75 -174.0(3) . . . . ?
C69 C68 C74 O76 4.9(5) . . . . ?
C69 C68 C67 C66 0.7(5) . . . . ?
C19 C18 C31 C26 -1.8(5) . . . . ?
C19 C18 C31 C30 -179.4(4) . . . . ?
C19 C24 C23 C22 -2.6(7) . . . . ?
C19 C20 C21 C22 -1.8(7) . . . . ?
C24 C25 C26 C31 -1.6(6) . . . . ?
C24 C25 C26 C27 176.1(4) . . . . ?
C24 C19 C20 C21 -2.0(6) . . . . ?
C24 C23 C22 C21 -1.2(9) . . . . ?
C33 N32 C25 C26 -73.6(5) . . . . ?
C33 N32 C25 C24 109.2(4) . . . . ?
C33 N32 C36 C35 1.6(5) . . . . ?
C33 N34 C35 C36 -0.7(6) . . . . ?
N37 C41A C40A N39 0.4(7) . . . . ?
N37 C41B C40B N39 2.5(18) . . . . ?
C64 C65 C66 S70 179.3(3) . . . . ?
C64 C65 C66 C67 -3.1(5) . . . . ?
C6 N3 C2 N1 179.0(4) . . . . ?
C6 N3 C4 C5 -178.9(4) . . . . ?
C6 C12 C11 C10 -175.6(5) . . . . ?
C6 C7 C8 C9 -176.3(6) . . . . ?
C49 N56 C57 N58 176.2(5) . . . . ?
C49 N56 C60 C59 -176.3(5) . . . . ?
C49 C48 C43 C42 5.4(7) . . . . ?
C49 C48 C43 C44 -174.9(5) . . . . ?
C49 C48 C47 C46 177.5(5) . . . . ?
C49 C50 C55 C42 4.4(7) . . . . ?
C49 C50 C55 C54 -174.8(5) . . . . ?
C49 C50 C51 C52 178.6(5) . . . . ?
C20 C19 C24 C25 -174.9(3) . . . . ?
C20 C19 C24 C23 4.1(5) . . . . ?
C20 C21 C22 C23 3.4(9) . . . . ?
C16 N15 C18 C31 108.7(5) . . . . ?
C16 N15 C18 C19 -76.0(5) . . . . ?
C16 N15 C14 N13 -0.1(4) . . . . ?
C48 C49 C50 C55 -0.2(7) . . . . ?
C48 C49 C50 C51 179.4(5) . . . . ?
C48 C43 C42 C55 -1.2(8) . . . . ?
C48 C43 C42 N39 -178.9(4) . . . . ?
C48 C43 C44 C45 -2.4(8) . . . . ?
C48 C47 C46 C45 -2.8(8) . . . . ?
C12 C6 C7 C12 -0.6(9) . . . 3_665 ?
C12 C6 C7 C8 179.4(6) . . . . ?
C12 C7 C8 C9 3.8(9) 3_665 . . . ?
C12 C11 C10 C9 -3.9(9) . . . 3_665 ?
C7 C6 C12 C7 0.7(9) . . . 3_665 ?
C7 C6 C12 C11 -179.6(5) . . . . ?
C7 C12 C11 C10 4.1(9) 3_665 . . . ?
C7 C8 C9 C10 -4.1(9) . . . 3_665 ?
C5 N1 C2 N3 -0.1(5) . . . . ?
C43 C48 C47 C46 -1.0(8) . . . . ?
C43 C42 C55 C50 -3.8(8) . . . . ?
C43 C42 C55 C54 175.3(5) . . . . ?
C43 C42 N39 C38A -80.2(11) . . . . ?
C43 C42 N39 C40A 128.7(6) . . . . ?
C43 C42 N39 C40B 51.0(10) . . . . ?
C43 C42 N39 C38B -72.3(14) . . . . ?
C43 C44 C45 C46 -1.5(8) . . . . ?
C59 N58 C57 N56 -0.5(5) . . . . ?
C50 C49 C48 C43 -4.8(7) . . . . ?
C50 C49 C48 C47 176.8(5) . . . . ?
C50 C55 C54 C53 -3.2(8) . . . . ?
C50 C51 C52 C53 -5.1(8) . . . . ?
C47 C48 C43 C42 -176.1(5) . . . . ?
C47 C48 C43 C44 3.6(8) . . . . ?
C47 C46 C45 C44 4.2(8) . . . . ?
C42 C43 C44 C45 177.3(5) . . . . ?
C42 C55 C54 C53 177.7(5) . . . . ?
C42 N39 C38A N37 178.7(8) . . . . ?
C42 N39 C40A C41A 170.8(5) . . . . ?
C42 N39 C40B C41B -166.6(12) . . . . ?
C42 N39 C38B N37 -176.3(9) . . . . ?
C28 C29 C30 C31 -0.2(8) . . . . ?
C4 N3 C2 N1 0.1(5) . . . . ?
C4 N3 C6 C12 -105.8(6) . . . . ?
C4 N3 C6 C7 74.1(6) . . . . ?
C30 C31 C26 C25 -178.9(4) . . . . ?
C30 C31 C26 C27 3.3(5) . . . . ?
C30 C29 C28 C27 2.2(8) . . . . ?
C55 C50 C51 C52 -1.7(8) . . . . ?
C55 C42 N39 C38A 101.8(11) . . . . ?
C55 C42 N39 C40A -49.2(7) . . . . ?
C55 C42 N39 C40B -127.0(9) . . . . ?
C55 C42 N39 C38B 109.8(13) . . . . ?
C55 C54 C53 C52 -3.5(9) . . . . ?
N39 C42 C55 C50 174.1(4) . . . . ?
N39 C42 C55 C54 -6.8(7) . . . . ?
C35 N34 C33 N32 1.8(4) . . . . ?
C36 N32 C25 C26 102.9(5) . . . . ?
C36 N32 C25 C24 -74.3(5) . . . . ?
C36 N32 C33 N34 -2.1(4) . . . . ?
C60 N56 C57 N58 0.9(6) . . . . ?
C60 N56 C49 C48 73.3(7) . . . . ?
C60 N56 C49 C50 -107.5(6) . . . . ?
C51 C50 C55 C42 -175.2(5) . . . . ?
C51 C50 C55 C54 5.6(7) . . . . ?
C51 C52 C53 C54 7.7(8) . . . . ?
C44 C43 C42 C55 179.2(5) . . . . ?
C44 C43 C42 N39 1.4(7) . . . . ?
C38A N37 C41A C40A -14.9(10) . . . . ?
C38A N37 C41B C40B 19.9(17) . . . . ?
C38A N37 C38B N39 92(8) . . . . ?
C38A N39 C40A C41A 13.6(10) . . . . ?
C38A N39 C40B C41B -23.4(17) . . . . ?
C38A N39 C38B N37 -87(8) . . . . ?
C41A N37 C38A N39 25.9(14) . . . . ?
C41A N37 C41B C40B -81.8(15) . . . . ?
C41A N37 C38B N39 14.5(19) . . . . ?
C40A N39 C38A N37 -25.4(14) . . . . ?
C40A N39 C40B C41B 75.2(14) . . . . ?
C40A N39 C38B N37 -14.1(18) . . . . ?
C41B N37 C38A N39 -39.2(15) . . . . ?
C41B N37 C41A C40A 77.3(7) . . . . ?
C41B N37 C38B N39 -49.4(17) . . . . ?
C40B N39 C38A N37 42.3(15) . . . . ?
C40B N39 C40A C41A -83.1(7) . . . . ?
C40B N39 C38B N37 52.8(18) . . . . ?
C38B N37 C38A N39 -79(8) . . . . ?
C38B N37 C41A C40A -8.4(12) . . . . ?
C38B N37 C41B C40B 24.0(17) . . . . ?
C38B N39 C38A N37 83(9) . . . . ?
C38B N39 C40A C41A 7.5(12) . . . . ?
C38B N39 C40B C41B -27.5(16) . . . . ?
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
-0.9978 -0.0011 0.9993 0.0150 -0.1280 -0.0166
7.9067 4.7938 -6.4262 -0.0782 0.9859 -0.1476
-1.0427 19.0742 -0.8892 0.6669 0.1266 -0.7343
3.7431 -12.4057 5.7424 -0.9902 -0.0794 0.1148
-0.1340 14.5617 7.1259 -0.0256 -0.2198 -0.9752
-0.5312 9.5113 -9.1955 0.8758 0.4770 0.0742
-8.0221 7.2915 0.4770 0.7925 -0.6064 -0.0652
-2.9198 17.9819 2.6247 0.5636 -0.2013 -0.8012
-4.3317 -8.9685 -6.6211 0.4946 -0.1156 0.8614
2.0265 -9.2787 -9.7459 0.1891 0.5436 0.8178
-0.7076 -17.8820 -3.7836 -0.2091 -0.0360 0.9772
-6.2640 13.1552 3.9299 0.6062 -0.5761 -0.5482
6.8835 -6.7723 3.4948 -0.9363 0.3308 -0.1183
4.9781 15.9680 -1.4136 0.1484 0.6105 -0.7780
-4.0853 -9.4716 9.2158 -0.5198 -0.8507 0.0784
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.787 0.000 0.000 1082.2 306.0 '4 DMF,14 H2O'
2 -0.423 0.500 0.500 1082.2 306.0 '4 DMF,14 H2O'
