#------------------------------------------------------------------------------
#$Date: 2024-06-07 00:45:43 +0200 (Fri 07 de Jun de 2024) $
#$Revision: 292242 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/87/7248792.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_7248792
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_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00399C
_journal_year                    2024
_chemical_formula_moiety         'C116 H80 N20 Ni3 O16 S2, 12[H2O], 4[C3H7NO]'
_chemical_formula_sum            'C128 H132 N24 Ni3 O32 S2'
_chemical_formula_weight         2758.82
_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                 104.823(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5935(3)
_cell_length_b                   29.6842(9)
_cell_length_c                   17.6639(5)
_cell_measurement_reflns_used    21924
_cell_measurement_temperature    273.00(10)
_cell_measurement_theta_max      77.4390
_cell_measurement_theta_min      2.9540
_cell_volume                     6890.4(3)
_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      air
_diffrn_ambient_temperature      273.00(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 0.996
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -46.00   1.00    1.50    --  -51.89 -43.00 -99.00   37
  2  ω    -30.00  24.00   1.00    1.50    --  -51.89  43.00  51.00   54
  3  ω    -19.00   7.00   1.00    1.50    --   51.89 -43.00 -99.00   26
  4  ω     44.00 112.00   1.00    1.50    --   51.89  43.00  51.00   68
  5  ω   -143.00 -78.00   1.00    5.50    --  -87.58 -43.00 -99.00   65
  6  ω     28.00  54.00   1.00    5.50    --  102.12 -43.00 -99.00   26
  7  ω     92.00 154.00   1.00    5.50    --  102.12  43.00  51.00   62
  8  ω    -44.00 -11.00   1.00    1.50    --    6.00 122.00 178.16   33
  9  ω     -3.00  24.00   1.00    1.50    --  -51.89  19.00 -30.00   27
 10  ω     -4.00  21.00   1.00    1.50    --  -51.89  19.00-180.00   25
 11  ω   -154.00 -87.00   1.00    5.50    --  -87.58 -99.00  60.00   67
 12  ω     25.00  51.00   1.00    5.50    --  102.12 -38.00 -60.00   26
 13  ω    143.00 172.00   1.00    5.50    --  102.12 125.00 -60.00   29
 14  ω     44.00  77.00   1.00    5.50    --  102.12 -57.00-180.00   33
 15  ω     25.00  51.00   1.00    5.50    --  102.12 -38.00 120.00   26
 16  ω     37.00  66.00   1.00    5.50    --  102.12 -57.00 -60.00   29
 17  ω    104.00 175.00   1.00    5.50    --  102.12  38.00  90.00   71
 18  ω     25.00  51.00   1.00    5.50    --  102.12 -38.00 -30.00   26
 19  ω     87.00 134.00   1.00    5.50    --  102.12 125.00 -60.00   47
 20  ω     26.00  52.00   1.00    5.50    --  102.12 -38.00  90.00   26
 21  ω     42.00  93.00   1.00    5.50    --  107.25 -86.00-109.69   51
 22  ω     51.00  76.00   1.00    5.50    --  107.25 -65.00 -49.27   25
 23  ω     97.00 127.00   1.00    5.50    --  107.25-147.00 146.59   30
 24  ω     38.00  94.00   1.00    5.50    --  107.25-147.00 146.59   56
 25  ω    106.00 163.00   1.00    5.50    --  107.25   3.00 -23.04   57
 26  ω     45.00  86.00   1.00    5.50    --  107.25 -66.00  21.08   41
 27  ω     39.00  86.00   1.00    5.50    --  107.25   3.00 -23.04   47
 28  ω     44.00 130.00   1.00    5.50    --  107.25 -79.00 -66.96   86
 29  ω     68.00 141.00   1.00    5.50    --  107.25  19.00-135.88   73
 30  ω     59.00  90.00   1.00    5.50    --  107.25 -63.00 163.26   31
 31  ω    142.00 175.00   1.00    5.50    --  107.25 112.00 -93.21   33
 32  ω     99.00 126.00   1.00    5.50    --  107.25 -81.00 167.35   27
 33  ω     62.00  88.00   1.00    5.50    --  107.25-116.00-101.18   26
 34  ω     43.00  89.00   1.00    5.50    --  107.25 -81.00 167.35   46
 35  ω     40.00  76.00   1.00    5.50    --  107.25 -73.00  -8.76   36
;
_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      -0.0341867000
_diffrn_orient_matrix_UB_12      -0.0263049000
_diffrn_orient_matrix_UB_13      -0.0774694000
_diffrn_orient_matrix_UB_21      -0.1118348000
_diffrn_orient_matrix_UB_22      0.0112049000
_diffrn_orient_matrix_UB_23      -0.0038977000
_diffrn_orient_matrix_UB_31      0.0082779000
_diffrn_orient_matrix_UB_32      0.0432744000
_diffrn_orient_matrix_UB_33      -0.0461043000
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74695
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.445
_diffrn_reflns_theta_min         2.977
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.849
_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    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14655
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0809
_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)+(0.1234P)²+8.7724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11541
_reflns_number_total             14655
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00399c2.cif
_cod_data_source_block           ebj-185n-dry-273k_r_abs
_cod_database_code               7248792
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H14 N4 O6 S1 Ni1'
_chemical_oxdiff_usercomment     'light blue/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   0.925
_shelx_estimated_absorpt_t_min   0.837
_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(C2) = Uanis(C5) = Uanis(C4)
Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C6) = Uanis(C12) = Uanis(C11) =
Uanis(C10)
4. Others
 Fixed Sof: C38A(0.55) H38A(0.55) C41A(0.55) H41A(0.55) C40A(0.55) H40A(0.55)
 C40B(0.45) H40B(0.45) C41B(0.45) H41B(0.45) C38B(0.45) H38B(0.45)
5.a Rotating group:
 O77(H77A,H77B)
5.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C67(H67), C69(H69), C2(H2), C14(H14), C57(H57), C33(H33),
 C38A(H38A), C17(H17), C16(H16), C35(H35), C59(H59), C23(H23), C5(H5), C20(H20),
  C36(H36), C51(H51), C54(H54), C47(H47), C30(H30), C60(H60), C52(H52), C4(H4),
 C27(H27), C44(H44), C21(H21), C22(H22), C53(H53), C29(H29), C28(H28), C45(H45),
  C46(H46), C41A(H41A), C40A(H40A), C40B(H40B), C41B(H41B), C38B(H38B),
 C11(H11), C8(H8), C10(H10), C9(H9)
;
_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.751
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 0.0000 0.02768(18) Uani 1 2 d S . P . .
Ni2 Ni 0.30631(3) 0.25917(2) 0.59448(3) 0.02791(15) Uani 1 1 d . . . . .
S70 S 0.51906(8) 0.45154(3) 0.82474(5) 0.0461(2) Uani 1 1 d . . . . .
O61 O 0.38285(18) 0.29661(9) 0.68759(13) 0.0402(5) Uani 1 1 d . . . . .
O77 O 0.2893(2) 0.20779(9) 0.67253(15) 0.0454(6) Uani 1 1 d . . . . .
H77A H 0.2746 0.1830 0.6475 0.068 Uiso 1 1 d R U . . .
H77B H 0.3467 0.2026 0.7051 0.068 Uiso 1 1 d R U . . .
O76 O 0.73029(19) 0.27792(9) 0.99928(14) 0.0434(6) Uani 1 1 d . . . . .
O71 O 0.4868(2) 0.46755(9) 0.89145(15) 0.0460(6) Uani 1 1 d . . . . .
O75 O 0.7349(2) 0.34734(9) 1.05047(16) 0.0552(7) Uani 1 1 d . . . . .
N13 N 0.4587(2) 0.44014(9) 0.04566(16) 0.0330(6) Uani 1 1 d . . . . .
N1 N 0.65572(19) 0.48586(10) 0.04124(16) 0.0356(6) Uani 1 1 d . . . . .
N34 N 0.3259(2) 0.31345(10) 0.52343(16) 0.0353(6) Uani 1 1 d . . . . .
O62 O 0.4632(3) 0.24101(10) 0.76399(18) 0.0665(10) Uani 1 1 d . . . . .
N58 N -0.5555(2) 0.23044(11) 0.58611(19) 0.0409(7) Uani 1 1 d . . . . .
N15 N 0.4071(3) 0.39544(11) 0.12693(18) 0.0454(7) Uani 1 1 d . . . . .
N32 N 0.3459(3) 0.35097(11) 0.42133(19) 0.0465(7) Uani 1 1 d . . . . .
N3 N 0.8194(2) 0.48654(12) 0.04790(19) 0.0459(8) Uani 1 1 d . . . . .
N37 N 0.1657(2) 0.28348(12) 0.6016(3) 0.0565(9) Uani 1 1 d D . . . .
N56 N -0.3914(2) 0.22417(13) 0.5980(2) 0.0560(9) Uani 1 1 d . . . . .
O73 O 0.4446(3) 0.45629(12) 0.75342(19) 0.0821(12) Uani 1 1 d . . . . .
O72 O 0.6162(3) 0.47132(11) 0.8225(2) 0.0744(10) Uani 1 1 d . . . . .
C68 C 0.6293(2) 0.33416(11) 0.92363(18) 0.0332(7) Uani 1 1 d . . . . .
C65 C 0.4874(3) 0.36153(12) 0.78915(18) 0.0368(7) Uani 1 1 d . . . . .
H65 H 0.4393 0.3710 0.7444 0.044 Uiso 1 1 calc R U . . .
C64 C 0.5060(2) 0.31588(12) 0.80295(18) 0.0350(7) Uani 1 1 d . . . . .
C67 C 0.6092(2) 0.37936(12) 0.91031(19) 0.0364(7) Uani 1 1 d . . . . .
H67 H 0.6417 0.4006 0.9470 0.044 Uiso 1 1 calc R U . . .
C66 C 0.5405(3) 0.39306(12) 0.84204(19) 0.0368(7) Uani 1 1 d . . . . .
C69 C 0.5778(3) 0.30273(12) 0.87023(19) 0.0363(7) Uani 1 1 d . . . . .
H69 H 0.5915 0.2723 0.8796 0.044 Uiso 1 1 calc R U . . .
C2 C 0.7241(3) 0.49255(19) 0.0022(3) 0.0624(8) Uani 1 1 d . . . . .
H2 H 0.7090 0.5005 -0.0505 0.075 Uiso 1 1 calc R U . . .
C74 C 0.7048(2) 0.31886(12) 0.99771(19) 0.0375(7) Uani 1 1 d . . . . .
C14 C 0.4579(3) 0.43367(12) 0.1192(2) 0.0367(7) Uani 1 1 d . . . . .
H14 H 0.4881 0.4528 0.1603 0.044 Uiso 1 1 calc R U . . .
C57 C -0.4713(2) 0.25245(13) 0.5902(2) 0.0419(8) Uani 1 1 d . . . . .
H57 H -0.4668 0.2837 0.5880 0.050 Uiso 1 1 calc R U . . .
C25 C 0.3581(3) 0.35992(14) 0.3439(2) 0.0474(9) Uani 1 1 d . . . . .
C18 C 0.3882(3) 0.38106(13) 0.1993(2) 0.0439(8) Uani 1 1 d . . . . .
C63 C 0.4476(3) 0.28106(13) 0.74767(19) 0.0402(8) Uani 1 1 d . . . . .
C33 C 0.3186(3) 0.31176(13) 0.4484(2) 0.0413(8) Uani 1 1 d . . . . .
H33 H 0.2971 0.2865 0.4173 0.050 Uiso 1 1 calc R U . . .
C19 C 0.4645(3) 0.35750(14) 0.2522(2) 0.0490(9) Uani 1 1 d . . . . .
C31 C 0.2978(3) 0.39440(14) 0.2154(2) 0.0477(9) Uani 1 1 d . . . . .
N39 N 0.0044(3) 0.28139(14) 0.6011(4) 0.0852(17) Uani 1 1 d D . . . .
C38A C 0.0858(7) 0.2573(5) 0.5953(12) 0.041(5) Uani 0.55 1 d D . P A 1
H38A H 0.0858 0.2262 0.5878 0.049 Uiso 0.55 1 calc R U P A 1
C48 C -0.2559(3) 0.23152(17) 0.5327(3) 0.0623(12) Uani 1 1 d . . . . .
C49 C -0.2886(3) 0.23686(15) 0.6005(3) 0.0588(12) Uani 1 1 d . . . . .
C24 C 0.4491(3) 0.34704(15) 0.3277(2) 0.0504(9) Uani 1 1 d . . . . .
C26 C 0.2809(3) 0.38285(15) 0.2904(2) 0.0517(10) Uani 1 1 d . . . . .
C17 C 0.4084(4) 0.40411(15) 0.0052(2) 0.0547(10) Uani 1 1 d . . . . .
H17 H 0.3985 0.3992 -0.0482 0.066 Uiso 1 1 calc R U . . .
C55 C -0.1249(3) 0.26697(16) 0.6714(4) 0.0701(15) Uani 1 1 d . . . . .
C16 C 0.3755(4) 0.37684(16) 0.0545(3) 0.0674(14) Uani 1 1 d . . . . .
H16 H 0.3384 0.3504 0.0415 0.081 Uiso 1 1 calc R U . . .
C35 C 0.3594(4) 0.35587(15) 0.5462(2) 0.0600(12) Uani 1 1 d . . . . .
H35 H 0.3714 0.3669 0.5970 0.072 Uiso 1 1 calc R U . . .
C43 C -0.1553(3) 0.24704(18) 0.5329(4) 0.0698(15) Uani 1 1 d . . . . .
C50 C -0.2275(3) 0.25368(16) 0.6702(3) 0.0581(12) Uani 1 1 d . . . . .
C59 C -0.5289(3) 0.18613(16) 0.5920(4) 0.0686(14) Uani 1 1 d . . . . .
H59 H -0.5738 0.1623 0.5907 0.082 Uiso 1 1 calc R U . . .
C23 C 0.5295(4) 0.32661(18) 0.3837(3) 0.0661(13) Uani 1 1 d . . . . .
H23 H 0.5220 0.3206 0.4336 0.079 Uiso 1 1 calc R U . . .
C42 C -0.0941(3) 0.26434(16) 0.6017(4) 0.0691(15) Uani 1 1 d . . . . .
C5 C 0.7092(3) 0.47526(19) 0.1162(3) 0.0624(8) Uani 1 1 d . . . . .
H5 H 0.6805 0.4691 0.1575 0.075 Uiso 1 1 calc R U . . .
C20 C 0.5570(4) 0.34384(17) 0.2352(3) 0.0651(12) Uani 1 1 d . . . . .
H20 H 0.5668 0.3492 0.1858 0.078 Uiso 1 1 calc R U . . .
C36 C 0.3726(5) 0.37936(17) 0.4843(3) 0.0721(15) Uani 1 1 d . . . . .
H36 H 0.3953 0.4089 0.4844 0.087 Uiso 1 1 calc R U . . .
C51 C -0.2596(4) 0.25909(18) 0.7407(4) 0.0720(15) Uani 1 1 d . . . . .
H51 H -0.3261 0.2514 0.7403 0.086 Uiso 1 1 calc R U . . .
C54 C -0.0604(3) 0.2819(2) 0.7441(5) 0.0864(19) Uani 1 1 d . . . . .
H54 H 0.0066 0.2898 0.7467 0.104 Uiso 1 1 calc R U . . .
C47 C -0.3173(4) 0.2117(2) 0.4633(4) 0.0786(16) Uani 1 1 d . . . . .
H47 H -0.3827 0.2021 0.4625 0.094 Uiso 1 1 calc R U . . .
C30 C 0.2216(4) 0.42013(19) 0.1625(3) 0.0655(13) Uani 1 1 d . . . . .
H30 H 0.2308 0.4279 0.1138 0.079 Uiso 1 1 calc R U . . .
C60 C -0.4278(4) 0.18172(17) 0.6001(5) 0.087(2) Uani 1 1 d . . . . .
H60 H -0.3907 0.1550 0.6059 0.105 Uiso 1 1 calc R U . . .
C52 C -0.1974(4) 0.2749(2) 0.8078(4) 0.0785(15) Uani 1 1 d . . . . .
H52 H -0.2210 0.2791 0.8522 0.094 Uiso 1 1 calc R U . . .
C4 C 0.8099(3) 0.47519(19) 0.1206(3) 0.0624(8) Uani 1 1 d . . . . .
H4 H 0.8624 0.4687 0.1644 0.075 Uiso 1 1 calc R U . . .
C27 C 0.1884(4) 0.3964(2) 0.3058(3) 0.0795(17) Uani 1 1 d . . . . .
H27 H 0.1754 0.3883 0.3531 0.095 Uiso 1 1 calc R U . . .
C44 C -0.1247(5) 0.2426(3) 0.4622(5) 0.094(2) Uani 1 1 d . . . . .
H44 H -0.0609 0.2532 0.4605 0.113 Uiso 1 1 calc R U . . .
C21 C 0.6292(4) 0.3236(2) 0.2893(4) 0.0834(18) Uani 1 1 d . . . . .
H21 H 0.6887 0.3145 0.2769 0.100 Uiso 1 1 calc R U . . .
C22 C 0.6175(4) 0.3156(2) 0.3657(4) 0.0869(19) Uani 1 1 d . . . . .
H22 H 0.6704 0.3028 0.4036 0.104 Uiso 1 1 calc R U . . .
C53 C -0.0948(4) 0.2848(2) 0.8086(5) 0.096(2) Uani 1 1 d . . . . .
H53 H -0.0501 0.2936 0.8555 0.115 Uiso 1 1 calc R U . . .
C29 C 0.1370(4) 0.4333(2) 0.1819(4) 0.0882(19) Uani 1 1 d . . . . .
H29 H 0.0896 0.4511 0.1475 0.106 Uiso 1 1 calc R U . . .
C28 C 0.1191(5) 0.4204(3) 0.2548(4) 0.102(2) Uani 1 1 d . . . . .
H28 H 0.0589 0.4287 0.2668 0.122 Uiso 1 1 calc R U . . .
C45 C -0.1848(6) 0.2235(3) 0.3977(5) 0.109(3) Uani 1 1 d . . . . .
H45 H -0.1623 0.2214 0.3523 0.131 Uiso 1 1 calc R U . . .
C46 C -0.2830(5) 0.2065(3) 0.3985(4) 0.099(2) Uani 1 1 d . . . . .
H46 H -0.3230 0.1920 0.3547 0.119 Uiso 1 1 calc R U . . .
C41A C 0.1415(7) 0.3256(3) 0.6251(9) 0.076(4) Uani 0.55 1 d D . P A 1
H41A H 0.1862 0.3498 0.6386 0.092 Uiso 0.55 1 calc R U P A 1
C40A C 0.0409(7) 0.3258(3) 0.6253(10) 0.087(4) Uani 0.55 1 d D . P A 1
H40A H 0.0040 0.3496 0.6383 0.105 Uiso 0.55 1 calc R U P A 1
C40B C 0.0131(8) 0.3212(5) 0.5570(12) 0.091(5) Uani 0.45 1 d D . P A 2
H40B H -0.0374 0.3411 0.5315 0.109 Uiso 0.45 1 calc R U P A 2
C41B C 0.1156(8) 0.3223(4) 0.5623(11) 0.081(4) Uani 0.45 1 d D . P A 2
H41B H 0.1482 0.3454 0.5427 0.097 Uiso 0.45 1 calc R U P A 2
C38B C 0.0923(9) 0.2587(5) 0.6155(14) 0.032(4) Uani 0.45 1 d D . P A 2
H38B H 0.1004 0.2291 0.6331 0.038 Uiso 0.45 1 calc R U P A 2
C6 C 0.9120(4) 0.49316(19) 0.0240(4) 0.0713(6) Uani 1 1 d . . . . .
C7 C 0.9427(3) 0.46021(19) -0.0200(4) 0.0713(6) Uani 1 1 d . . . . .
C12 C 0.9655(3) 0.53294(19) 0.0453(4) 0.0713(6) Uani 1 1 d . . . . .
C11 C 0.9345(3) 0.56776(19) 0.0896(4) 0.0713(6) Uani 1 1 d . . . . .
H11 H 0.8748 0.5644 0.1057 0.086 Uiso 1 1 calc R U . . .
C8 C 0.8889(3) 0.41931(19) -0.0382(4) 0.0713(6) Uani 1 1 d . . . . .
H8 H 0.8321 0.4140 -0.0193 0.086 Uiso 1 1 calc R U . . .
C10 C 0.9898(3) 0.60521(19) 0.1085(4) 0.0713(6) Uani 1 1 d . . . . .
H10 H 0.9690 0.6271 0.1388 0.086 Uiso 1 1 calc R U . . .
C9 C 0.9195(3) 0.38754(19) -0.0830(4) 0.0713(6) Uani 1 1 d . . . . .
H9 H 0.8817 0.3613 -0.0969 0.086 Uiso 1 1 calc R U . . .
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
0 17 -5 0.0236
0 -17 6 0.0285
9 0 -5 0.0560
-9 1 3 0.0688
0 -10 -9 0.0220
1 10 9 0.0474
0 0 -11 0.0223
-2 -19 1 0.0326
1 -18 -5 0.0251
-2 8 10 0.0520
8 4 0 0.0568
-6 -12 -2 0.0470
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
O71 Ni1 O71 180.00(13) 3_666 1_554 ?
N13 Ni1 O71 90.36(11) . 3_666 ?
N13 Ni1 O71 89.64(11) . 1_554 ?
N13 Ni1 O71 90.36(11) 3_665 1_554 ?
N13 Ni1 O71 89.64(11) 3_665 3_666 ?
N13 Ni1 N13 180.00(14) . 3_665 ?
N13 Ni1 N1 92.45(11) . . ?
N13 Ni1 N1 87.55(11) 3_665 . ?
N13 Ni1 N1 92.46(11) 3_665 3_665 ?
N13 Ni1 N1 87.54(11) . 3_665 ?
N1 Ni1 O71 93.89(11) . 1_554 ?
N1 Ni1 O71 93.89(11) 3_665 3_666 ?
N1 Ni1 O71 86.11(11) . 3_666 ?
N1 Ni1 O71 86.11(11) 3_665 1_554 ?
N1 Ni1 N1 180.0 . 3_665 ?
O61 Ni2 O77 89.17(10) . . ?
O61 Ni2 O76 178.96(11) . 4_565 ?
O61 Ni2 N34 86.97(11) . . ?
O61 Ni2 N58 89.83(12) . 1_655 ?
O61 Ni2 N37 92.84(14) . . ?
O76 Ni2 O77 91.79(10) 4_565 . ?
O76 Ni2 N34 92.07(11) 4_565 . ?
O76 Ni2 N58 89.79(12) 4_565 1_655 ?
O76 Ni2 N37 87.58(14) 4_565 . ?
N34 Ni2 O77 175.99(11) . . ?
N34 Ni2 N58 90.97(11) . 1_655 ?
N58 Ni2 O77 90.12(11) 1_655 . ?
N37 Ni2 O77 87.43(13) . . ?
N37 Ni2 N34 91.66(13) . . ?
N37 Ni2 N58 176.35(13) . 1_655 ?
O71 S70 O72 110.9(2) . . ?
O71 S70 C66 104.66(16) . . ?
O73 S70 O71 113.6(2) . . ?
O73 S70 O72 112.7(3) . . ?
O73 S70 C66 107.53(19) . . ?
O72 S70 C66 106.83(19) . . ?
C63 O61 Ni2 125.0(2) . . ?
Ni2 O77 H77A 109.6 . . ?
Ni2 O77 H77B 109.6 . . ?
H77A O77 H77B 104.1 . . ?
C74 O76 Ni2 127.7(2) . 4_666 ?
S70 O71 Ni1 157.08(19) . 1_556 ?
C14 N13 Ni1 125.2(2) . . ?
C14 N13 C17 105.8(3) . . ?
C17 N13 Ni1 127.7(2) . . ?
C2 N1 Ni1 125.2(2) . . ?
C2 N1 C5 105.8(3) . . ?
C5 N1 Ni1 128.2(2) . . ?
C33 N34 Ni2 126.1(3) . . ?
C33 N34 C35 105.5(3) . . ?
C35 N34 Ni2 128.0(2) . . ?
C57 N58 Ni2 125.5(3) . 1_455 ?
C57 N58 C59 105.6(3) . . ?
C59 N58 Ni2 127.7(2) . 1_455 ?
C14 N15 C18 123.5(3) . . ?
C14 N15 C16 107.0(3) . . ?
C16 N15 C18 129.4(3) . . ?
C33 N32 C25 127.2(3) . . ?
C33 N32 C36 106.5(3) . . ?
C36 N32 C25 125.9(4) . . ?
C2 N3 C4 106.7(3) . . ?
C2 N3 C6 125.6(4) . . ?
C4 N3 C6 127.6(4) . . ?
C38A N37 Ni2 122.8(6) . . ?
C38A N37 C41A 107.8(7) . . ?
C41A N37 Ni2 128.7(4) . . ?
C41B N37 Ni2 125.8(5) . . ?
C38B N37 Ni2 124.9(6) . . ?
C38B N37 C41B 104.6(8) . . ?
C57 N56 C49 126.2(4) . . ?
C57 N56 C60 106.8(3) . . ?
C60 N56 C49 127.0(3) . . ?
C67 C68 C69 119.8(3) . . ?
C67 C68 C74 120.1(3) . . ?
C69 C68 C74 120.1(3) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C66 C65 C64 120.0(3) . . ?
C65 C64 C63 121.0(3) . . ?
C69 C64 C65 118.8(3) . . ?
C69 C64 C63 120.2(3) . . ?
C68 C67 H67 120.2 . . ?
C68 C67 C66 119.7(3) . . ?
C66 C67 H67 120.2 . . ?
C65 C66 S70 120.7(3) . . ?
C67 C66 S70 118.8(3) . . ?
C67 C66 C65 120.5(3) . . ?
C68 C69 C64 121.1(3) . . ?
C68 C69 H69 119.4 . . ?
C64 C69 H69 119.4 . . ?
N1 C2 N3 111.5(3) . . ?
N1 C2 H2 124.2 . . ?
N3 C2 H2 124.2 . . ?
O76 C74 C68 115.5(3) . . ?
O75 C74 O76 126.9(3) . . ?
O75 C74 C68 117.6(3) . . ?
N13 C14 N15 110.8(3) . . ?
N13 C14 H14 124.6 . . ?
N15 C14 H14 124.6 . . ?
N58 C57 N56 111.5(3) . . ?
N58 C57 H57 124.3 . . ?
N56 C57 H57 124.3 . . ?
C24 C25 N32 117.9(4) . . ?
C24 C25 C26 123.2(3) . . ?
C26 C25 N32 118.8(3) . . ?
C19 C18 N15 118.4(3) . . ?
C31 C18 N15 117.9(3) . . ?
C31 C18 C19 123.5(3) . . ?
O61 C63 C64 115.3(3) . . ?
O62 C63 O61 125.8(3) . . ?
O62 C63 C64 118.8(3) . . ?
N34 C33 N32 111.8(3) . . ?
N34 C33 H33 124.1 . . ?
N32 C33 H33 124.1 . . ?
C18 C19 C24 118.1(4) . . ?
C18 C19 C20 123.2(4) . . ?
C20 C19 C24 118.7(4) . . ?
C18 C31 C26 118.5(4) . . ?
C18 C31 C30 123.5(4) . . ?
C30 C31 C26 118.0(4) . . ?
C38A N39 C42 126.9(6) . . ?
C38A N39 C40A 106.4(7) . . ?
C42 N39 C40A 125.1(5) . . ?
C42 N39 C40B 120.1(6) . . ?
C38B N39 C42 127.7(6) . . ?
C38B N39 C40B 108.8(8) . . ?
N37 C38A N39 110.8(10) . . ?
N37 C38A H38A 124.6 . . ?
N39 C38A H38A 124.6 . . ?
C49 C48 C43 118.3(5) . . ?
C49 C48 C47 122.9(4) . . ?
C47 C48 C43 118.8(5) . . ?
C48 C49 N56 117.8(5) . . ?
C50 C49 N56 118.6(4) . . ?
C50 C49 C48 123.6(4) . . ?
C25 C24 C19 118.7(4) . . ?
C25 C24 C23 123.0(4) . . ?
C23 C24 C19 118.2(4) . . ?
C25 C26 C31 117.9(4) . . ?
C25 C26 C27 124.2(4) . . ?
C27 C26 C31 117.9(4) . . ?
N13 C17 H17 125.2 . . ?
C16 C17 N13 109.7(4) . . ?
C16 C17 H17 125.2 . . ?
C42 C55 C50 118.5(5) . . ?
C42 C55 C54 123.7(4) . . ?
C54 C55 C50 117.8(5) . . ?
N15 C16 H16 126.6 . . ?
C17 C16 N15 106.7(4) . . ?
C17 C16 H16 126.6 . . ?
N34 C35 H35 125.0 . . ?
C36 C35 N34 110.0(4) . . ?
C36 C35 H35 125.0 . . ?
C42 C43 C48 118.5(5) . . ?
C42 C43 C44 124.2(5) . . ?
C44 C43 C48 117.3(6) . . ?
C49 C50 C55 117.9(5) . . ?
C49 C50 C51 124.4(4) . . ?
C51 C50 C55 117.7(5) . . ?
N58 C59 H59 124.9 . . ?
C60 C59 N58 110.1(4) . . ?
C60 C59 H59 124.9 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(4) . . ?
C22 C23 H23 119.6 . . ?
C55 C42 N39 118.4(5) . . ?
C43 C42 N39 118.5(5) . . ?
C43 C42 C55 123.0(4) . . ?
N1 C5 H5 125.2 . . ?
C4 C5 N1 109.5(3) . . ?
C4 C5 H5 125.2 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
N32 C36 H36 126.9 . . ?
C35 C36 N32 106.2(4) . . ?
C35 C36 H36 126.9 . . ?
C50 C51 H51 118.6 . . ?
C52 C51 C50 122.7(5) . . ?
C52 C51 H51 118.6 . . ?
C55 C54 H54 119.4 . . ?
C53 C54 C55 121.1(5) . . ?
C53 C54 H54 119.4 . . ?
C48 C47 H47 119.2 . . ?
C46 C47 C48 121.6(5) . . ?
C46 C47 H47 119.2 . . ?
C31 C30 H30 119.4 . . ?
C29 C30 C31 121.1(5) . . ?
C29 C30 H30 119.4 . . ?
N56 C60 H60 127.0 . . ?
C59 C60 N56 106.0(4) . . ?
C59 C60 H60 127.0 . . ?
C51 C52 H52 120.9 . . ?
C51 C52 C53 118.3(6) . . ?
C53 C52 H52 120.9 . . ?
N3 C4 H4 126.7 . . ?
C5 C4 N3 106.5(3) . . ?
C5 C4 H4 126.7 . . ?
C26 C27 H27 118.9 . . ?
C28 C27 C26 122.3(5) . . ?
C28 C27 H27 118.9 . . ?
C43 C44 H44 118.9 . . ?
C45 C44 C43 122.3(6) . . ?
C45 C44 H44 118.9 . . ?
C20 C21 H21 119.4 . . ?
C20 C21 C22 121.2(5) . . ?
C22 C21 H21 119.4 . . ?
C23 C22 C21 120.3(5) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C54 C53 C52 122.2(6) . . ?
C54 C53 H53 118.9 . . ?
C52 C53 H53 118.9 . . ?
C30 C29 H29 119.7 . . ?
C30 C29 C28 120.6(5) . . ?
C28 C29 H29 119.7 . . ?
C27 C28 C29 120.1(5) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.4(7) . . ?
C46 C45 H45 119.8 . . ?
C47 C46 C45 119.5(7) . . ?
C47 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
N37 C41A H41A 125.7 . . ?
C40A C41A N37 108.5(7) . . ?
C40A C41A H41A 125.7 . . ?
N39 C40A H40A 127.3 . . ?
C41A C40A N39 105.5(7) . . ?
C41A C40A H40A 127.3 . . ?
N39 C40B H40B 129.1 . . ?
C41B C40B N39 101.8(9) . . ?
C41B C40B H40B 129.1 . . ?
N37 C41B H41B 124.3 . . ?
C40B C41B N37 111.5(9) . . ?
C40B C41B H41B 124.3 . . ?
N37 C38B N39 111.6(10) . . ?
N37 C38B H38B 124.2 . . ?
N39 C38B H38B 124.2 . . ?
C7 C6 N3 118.8(4) . . ?
C7 C6 C12 123.0(4) . . ?
C12 C6 N3 118.2(4) . . ?
C6 C7 C12 119.0(5) . 3_765 ?
C6 C7 C8 121.6(4) . . ?
C8 C7 C12 119.3(5) . 3_765 ?
C6 C12 C7 118.0(5) . 3_765 ?
C6 C12 C11 124.0(4) . . ?
C11 C12 C7 118.0(5) . 3_765 ?
C12 C11 H11 119.5 . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 H11 119.5 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.7(4) . . ?
C9 C8 H8 119.7 . . ?
C11 C10 H10 119.3 . . ?
C11 C10 C9 121.4(5) . 3_765 ?
C9 C10 H10 119.3 3_765 . ?
C8 C9 C10 119.5(5) . 3_765 ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 3_765 . ?
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 O71 2.112(3) 3_666 ?
Ni1 O71 2.112(3) 1_554 ?
Ni1 N13 2.087(3) . ?
Ni1 N13 2.087(3) 3_665 ?
Ni1 N1 2.097(3) . ?
Ni1 N1 2.097(3) 3_665 ?
Ni2 O61 2.037(2) . ?
Ni2 O77 2.108(3) . ?
Ni2 O76 2.054(2) 4_565 ?
Ni2 N34 2.101(3) . ?
Ni2 N58 2.103(3) 1_655 ?
Ni2 N37 2.077(3) . ?
S70 O71 1.439(3) . ?
S70 O73 1.407(3) . ?
S70 O72 1.454(3) . ?
S70 C66 1.774(4) . ?
O61 C63 1.279(4) . ?
O77 H77A 0.8561 . ?
O77 H77B 0.8561 . ?
O76 Ni2 2.054(2) 4_666 ?
O76 C74 1.262(4) . ?
O71 Ni1 2.112(3) 1_556 ?
O75 C74 1.247(4) . ?
N13 C14 1.317(4) . ?
N13 C17 1.368(5) . ?
N1 C2 1.307(5) . ?
N1 C5 1.374(5) . ?
N34 C33 1.305(4) . ?
N34 C35 1.364(5) . ?
O62 C63 1.229(5) . ?
N58 Ni2 2.103(3) 1_455 ?
N58 C57 1.303(4) . ?
N58 C59 1.361(6) . ?
N15 C14 1.353(4) . ?
N15 C18 1.432(4) . ?
N15 C16 1.358(5) . ?
N32 C25 1.444(5) . ?
N32 C33 1.346(5) . ?
N32 C36 1.369(6) . ?
N3 C2 1.352(5) . ?
N3 C4 1.365(5) . ?
N3 C6 1.441(5) . ?
N37 C38A 1.318(11) . ?
N37 C41A 1.384(8) . ?
N37 C41B 1.425(11) . ?
N37 C38B 1.312(12) . ?
N56 C57 1.352(5) . ?
N56 C49 1.436(4) . ?
N56 C60 1.358(6) . ?
C68 C67 1.377(5) . ?
C68 C69 1.383(5) . ?
C68 C74 1.511(4) . ?
C65 H65 0.9300 . ?
C65 C64 1.389(5) . ?
C65 C66 1.387(5) . ?
C64 C69 1.387(4) . ?
C64 C63 1.502(5) . ?
C67 H67 0.9300 . ?
C67 C66 1.384(4) . ?
C69 H69 0.9300 . ?
C2 H2 0.9300 . ?
C14 H14 0.9300 . ?
C57 H57 0.9300 . ?
C25 C24 1.392(6) . ?
C25 C26 1.396(6) . ?
C18 C19 1.393(6) . ?
C18 C31 1.387(6) . ?
C33 H33 0.9300 . ?
C19 C24 1.436(5) . ?
C19 C20 1.424(6) . ?
C31 C26 1.444(5) . ?
C31 C30 1.426(6) . ?
N39 C38A 1.345(11) . ?
N39 C42 1.433(5) . ?
N39 C40A 1.434(10) . ?
N39 C40B 1.438(12) . ?
N39 C38B 1.339(12) . ?
C38A H38A 0.9300 . ?
C48 C49 1.391(7) . ?
C48 C43 1.442(6) . ?
C48 C47 1.422(8) . ?
C49 C50 1.389(7) . ?
C24 C23 1.411(6) . ?
C26 C27 1.412(6) . ?
C17 H17 0.9300 . ?
C17 C16 1.346(6) . ?
C55 C50 1.445(5) . ?
C55 C42 1.401(8) . ?
C55 C54 1.427(9) . ?
C16 H16 0.9300 . ?
C35 H35 0.9300 . ?
C35 C36 1.346(6) . ?
C43 C42 1.384(9) . ?
C43 C44 1.419(9) . ?
C50 C51 1.429(8) . ?
C59 H59 0.9300 . ?
C59 C60 1.352(6) . ?
C23 H23 0.9300 . ?
C23 C22 1.352(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.351(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.326(8) . ?
C36 H36 0.9300 . ?
C51 H51 0.9300 . ?
C51 C52 1.352(9) . ?
C54 H54 0.9300 . ?
C54 C53 1.341(10) . ?
C47 H47 0.9300 . ?
C47 C46 1.349(9) . ?
C30 H30 0.9300 . ?
C30 C29 1.340(8) . ?
C60 H60 0.9300 . ?
C52 H52 0.9300 . ?
C52 C53 1.421(8) . ?
C4 H4 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.330(8) . ?
C44 H44 0.9300 . ?
C44 C45 1.345(11) . ?
C21 H21 0.9300 . ?
C21 C22 1.420(8) . ?
C22 H22 0.9300 . ?
C53 H53 0.9300 . ?
C29 H29 0.9300 . ?
C29 C28 1.423(8) . ?
C28 H28 0.9300 . ?
C45 H45 0.9300 . ?
C45 C46 1.432(10) . ?
C46 H46 0.9300 . ?
C41A H41A 0.9300 . ?
C41A C40A 1.368(10) . ?
C40A H40A 0.9300 . ?
C40B H40B 0.9300 . ?
C40B C41B 1.372(12) . ?
C41B H41B 0.9300 . ?
C38B H38B 0.9300 . ?
C6 C7 1.378(7) . ?
C6 C12 1.387(7) . ?
C7 C12 1.443(6) 3_765 ?
C7 C8 1.411(7) . ?
C12 C7 1.443(6) 3_765 ?
C12 C11 1.424(7) . ?
C11 H11 0.9300 . ?
C11 C10 1.336(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.362(7) . ?
C10 H10 0.9300 . ?
C10 C9 1.433(6) 3_765 ?
C9 C10 1.433(6) 3_765 ?
C9 H9 0.9300 . ?
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 O75 0.86 1.89 2.657(4) 148.5 4_565
O77 H77B O62 0.86 2.01 2.687(4) 135.0 .
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 166.6(2) . . . . ?
Ni1 N13 C17 C16 -166.0(4) . . . . ?
Ni1 N1 C2 N3 170.9(3) . . . . ?
Ni1 N1 C5 C4 -170.9(4) . . . . ?
Ni2 O61 C63 O62 -10.9(6) . . . . ?
Ni2 O61 C63 C64 171.0(2) . . . . ?
Ni2 O76 C74 O75 13.1(6) 4_666 . . . ?
Ni2 O76 C74 C68 -166.6(2) 4_666 . . . ?
Ni2 N34 C33 N32 -173.4(2) . . . . ?
Ni2 N34 C35 C36 173.0(4) . . . . ?
Ni2 N58 C57 N56 168.1(3) 1_455 . . . ?
Ni2 N58 C59 C60 -167.1(4) 1_455 . . . ?
Ni2 N37 C38A N39 -179.3(8) . . . . ?
Ni2 N37 C41A C40A -176.2(9) . . . . ?
Ni2 N37 C41B C40B 159.6(12) . . . . ?
Ni2 N37 C38B N39 -167.3(9) . . . . ?
O71 S70 C66 C65 121.1(3) . . . . ?
O71 S70 C66 C67 -57.2(3) . . . . ?
N13 C17 C16 N15 -1.2(6) . . . . ?
N1 C5 C4 N3 0.9(6) . . . . ?
N34 C35 C36 N32 0.5(6) . . . . ?
N58 C59 C60 N56 -0.9(8) . . . . ?
N15 C18 C19 C24 174.0(4) . . . . ?
N15 C18 C19 C20 -5.3(6) . . . . ?
N15 C18 C31 C26 -175.7(4) . . . . ?
N15 C18 C31 C30 2.4(6) . . . . ?
N32 C25 C24 C19 -177.2(4) . . . . ?
N32 C25 C24 C23 -1.2(7) . . . . ?
N32 C25 C26 C31 175.5(4) . . . . ?
N32 C25 C26 C27 -2.9(7) . . . . ?
N3 C6 C7 C12 178.9(5) . . . 3_765 ?
N3 C6 C7 C8 -3.7(9) . . . . ?
N3 C6 C12 C7 -178.9(5) . . . 3_765 ?
N3 C6 C12 C11 0.1(9) . . . . ?
N37 C41A C40A N39 0.4(16) . . . . ?
N56 C49 C50 C55 -179.0(4) . . . . ?
N56 C49 C50 C51 0.4(7) . . . . ?
O73 S70 O71 Ni1 -140.0(4) . . . 1_556 ?
O73 S70 C66 C65 0.0(4) . . . . ?
O73 S70 C66 C67 -178.3(3) . . . . ?
O72 S70 O71 Ni1 -11.9(5) . . . 1_556 ?
O72 S70 C66 C65 -121.2(3) . . . . ?
O72 S70 C66 C67 60.5(3) . . . . ?
C68 C67 C66 S70 -177.9(3) . . . . ?
C68 C67 C66 C65 3.7(5) . . . . ?
C65 C64 C69 C68 0.9(5) . . . . ?
C65 C64 C63 O61 1.6(5) . . . . ?
C65 C64 C63 O62 -176.7(4) . . . . ?
C64 C65 C66 S70 179.1(3) . . . . ?
C64 C65 C66 C67 -2.6(5) . . . . ?
C67 C68 C69 C64 0.2(5) . . . . ?
C67 C68 C74 O76 -169.3(3) . . . . ?
C67 C68 C74 O75 11.0(5) . . . . ?
C66 S70 O71 Ni1 103.0(5) . . . 1_556 ?
C66 C65 C64 C69 0.3(5) . . . . ?
C66 C65 C64 C63 178.4(3) . . . . ?
C69 C68 C67 C66 -2.5(5) . . . . ?
C69 C68 C74 O76 12.9(5) . . . . ?
C69 C68 C74 O75 -166.9(3) . . . . ?
C69 C64 C63 O61 179.7(3) . . . . ?
C69 C64 C63 O62 1.4(6) . . . . ?
C2 N1 C5 C4 -0.8(6) . . . . ?
C2 N3 C4 C5 -0.7(6) . . . . ?
C2 N3 C6 C7 -78.5(7) . . . . ?
C2 N3 C6 C12 100.4(7) . . . . ?
C74 C68 C67 C66 179.6(3) . . . . ?
C74 C68 C69 C64 178.1(3) . . . . ?
C14 N13 C17 C16 1.6(5) . . . . ?
C14 N15 C18 C19 -83.3(5) . . . . ?
C14 N15 C18 C31 91.9(5) . . . . ?
C14 N15 C16 C17 0.3(6) . . . . ?
C57 N58 C59 C60 0.3(6) . . . . ?
C57 N56 C49 C48 -100.8(6) . . . . ?
C57 N56 C49 C50 79.2(6) . . . . ?
C57 N56 C60 C59 1.1(7) . . . . ?
C25 N32 C33 N34 172.6(3) . . . . ?
C25 N32 C36 C35 -172.9(4) . . . . ?
C25 C24 C23 C22 -178.4(6) . . . . ?
C25 C26 C27 C28 176.2(7) . . . . ?
C18 N15 C14 N13 -176.0(3) . . . . ?
C18 N15 C16 C17 176.7(4) . . . . ?
C18 C19 C24 C25 1.5(6) . . . . ?
C18 C19 C24 C23 -174.7(4) . . . . ?
C18 C19 C20 C21 176.4(5) . . . . ?
C18 C31 C26 C25 1.9(6) . . . . ?
C18 C31 C26 C27 -179.7(5) . . . . ?
C18 C31 C30 C29 -177.9(6) . . . . ?
C63 C64 C69 C68 -177.2(3) . . . . ?
C33 N34 C35 C36 -0.3(6) . . . . ?
C33 N32 C25 C24 -81.3(5) . . . . ?
C33 N32 C25 C26 101.8(5) . . . . ?
C33 N32 C36 C35 -0.4(6) . . . . ?
C19 C18 C31 C26 -0.8(6) . . . . ?
C19 C18 C31 C30 177.3(4) . . . . ?
C19 C24 C23 C22 -2.4(8) . . . . ?
C19 C20 C21 C22 -1.1(10) . . . . ?
C31 C18 C19 C24 -0.9(6) . . . . ?
C31 C18 C19 C20 179.9(4) . . . . ?
C31 C26 C27 C28 -2.2(10) . . . . ?
C31 C30 C29 C28 -2.6(11) . . . . ?
N39 C40B C41B N37 5(2) . . . . ?
C38A N37 C41A C40A -6.2(17) . . . . ?
C38A N37 C41B C40B 17.7(19) . . . . ?
C38A N37 C38B N39 -80(4) . . . . ?
C38A N39 C42 C55 110.6(12) . . . . ?
C38A N39 C42 C43 -70.9(13) . . . . ?
C38A N39 C40A C41A 5.4(16) . . . . ?
C38A N39 C40B C41B -24.9(18) . . . . ?
C38A N39 C38B N37 80(4) . . . . ?
C48 C49 C50 C55 1.0(7) . . . . ?
C48 C49 C50 C51 -179.5(4) . . . . ?
C48 C43 C42 N39 -177.6(4) . . . . ?
C48 C43 C42 C55 0.8(7) . . . . ?
C48 C43 C44 C45 -1.9(9) . . . . ?
C48 C47 C46 C45 -3.6(10) . . . . ?
C49 N56 C57 N58 177.0(4) . . . . ?
C49 N56 C60 C59 -176.8(5) . . . . ?
C49 C48 C43 C42 3.3(7) . . . . ?
C49 C48 C43 C44 -178.0(5) . . . . ?
C49 C48 C47 C46 -179.2(6) . . . . ?
C49 C50 C51 C52 178.8(5) . . . . ?
C24 C25 C26 C31 -1.2(7) . . . . ?
C24 C25 C26 C27 -179.6(5) . . . . ?
C24 C19 C20 C21 -2.9(8) . . . . ?
C24 C23 C22 C21 -1.5(10) . . . . ?
C26 C25 C24 C19 -0.4(7) . . . . ?
C26 C25 C24 C23 175.6(5) . . . . ?
C26 C31 C30 C29 0.2(8) . . . . ?
C26 C27 C28 C29 -0.1(12) . . . . ?
C17 N13 C14 N15 -1.4(4) . . . . ?
C55 C50 C51 C52 -1.7(7) . . . . ?
C55 C54 C53 C52 -2.4(10) . . . . ?
C16 N15 C14 N13 0.7(5) . . . . ?
C16 N15 C18 C19 100.8(6) . . . . ?
C16 N15 C18 C31 -84.0(6) . . . . ?
C35 N34 C33 N32 0.1(4) . . . . ?
C43 C48 C49 N56 175.8(4) . . . . ?
C43 C48 C49 C50 -4.3(7) . . . . ?
C43 C48 C47 C46 1.1(8) . . . . ?
C43 C44 C45 C46 -0.5(11) . . . . ?
C50 C55 C42 N39 174.3(4) . . . . ?
C50 C55 C42 C43 -4.1(7) . . . . ?
C50 C55 C54 C53 -1.9(8) . . . . ?
C50 C51 C52 C53 -2.4(9) . . . . ?
C59 N58 C57 N56 0.4(5) . . . . ?
C42 N39 C38A N37 -176.1(8) . . . . ?
C42 N39 C40A C41A 172.2(9) . . . . ?
C42 N39 C40B C41B -171.7(11) . . . . ?
C42 N39 C38B N37 173.1(9) . . . . ?
C42 C55 C50 C49 3.1(6) . . . . ?
C42 C55 C50 C51 -176.4(4) . . . . ?
C42 C55 C54 C53 178.3(6) . . . . ?
C42 C43 C44 C45 176.7(6) . . . . ?
C5 N1 C2 N3 0.4(6) . . . . ?
C20 C19 C24 C25 -179.2(4) . . . . ?
C20 C19 C24 C23 4.6(7) . . . . ?
C20 C21 C22 C23 3.4(11) . . . . ?
C36 N32 C25 C24 89.8(6) . . . . ?
C36 N32 C25 C26 -87.1(6) . . . . ?
C36 N32 C33 N34 0.2(5) . . . . ?
C51 C52 C53 C54 4.6(10) . . . . ?
C54 C55 C50 C49 -176.6(4) . . . . ?
C54 C55 C50 C51 3.9(7) . . . . ?
C54 C55 C42 N39 -5.9(7) . . . . ?
C54 C55 C42 C43 175.7(5) . . . . ?
C47 C48 C49 N56 -3.9(7) . . . . ?
C47 C48 C49 C50 176.1(5) . . . . ?
C47 C48 C43 C42 -177.0(5) . . . . ?
C47 C48 C43 C44 1.6(7) . . . . ?
C30 C31 C26 C25 -176.4(4) . . . . ?
C30 C31 C26 C27 2.1(7) . . . . ?
C30 C29 C28 C27 2.6(13) . . . . ?
C60 N56 C57 N58 -0.9(6) . . . . ?
C60 N56 C49 C48 76.7(7) . . . . ?
C60 N56 C49 C50 -103.3(7) . . . . ?
C4 N3 C2 N1 0.2(6) . . . . ?
C4 N3 C6 C7 104.7(7) . . . . ?
C4 N3 C6 C12 -76.4(7) . . . . ?
C44 C43 C42 N39 3.9(7) . . . . ?
C44 C43 C42 C55 -177.7(5) . . . . ?
C44 C45 C46 C47 3.3(11) . . . . ?
C41A N37 C38A N39 9.9(17) . . . . ?
C41A N37 C41B C40B -88.6(17) . . . . ?
C41A N37 C38B N39 35.6(19) . . . . ?
C40A N39 C38A N37 -9.6(17) . . . . ?
C40A N39 C42 C55 -53.5(11) . . . . ?
C40A N39 C42 C43 125.0(10) . . . . ?
C40A N39 C40B C41B 76.3(14) . . . . ?
C40A N39 C38B N37 -35.1(19) . . . . ?
C40B N39 C38A N37 40.3(17) . . . . ?
C40B N39 C42 C55 -111.3(11) . . . . ?
C40B N39 C42 C43 67.1(12) . . . . ?
C40B N39 C40A C41A -86.6(13) . . . . ?
C40B N39 C38B N37 14(2) . . . . ?
C41B N37 C38A N39 -35.8(16) . . . . ?
C41B N37 C41A C40A 78.7(13) . . . . ?
C41B N37 C38B N39 -11(2) . . . . ?
C38B N37 C38A N39 78(4) . . . . ?
C38B N37 C41A C40A -20.5(17) . . . . ?
C38B N37 C41B C40B 3(2) . . . . ?
C38B N39 C38A N37 -77(4) . . . . ?
C38B N39 C42 C55 91.9(15) . . . . ?
C38B N39 C42 C43 -89.6(15) . . . . ?
C38B N39 C40A C41A 19.4(17) . . . . ?
C38B N39 C40B C41B -11(2) . . . . ?
C6 N3 C2 N1 -177.2(4) . . . . ?
C6 N3 C4 C5 176.6(5) . . . . ?
C6 C7 C8 C9 178.8(6) . . . . ?
C6 C12 C11 C10 179.7(6) . . . . ?
C7 C6 C12 C7 0.0(11) . . . 3_765 ?
C7 C6 C12 C11 178.9(6) . . . . ?
C7 C12 C11 C10 -1.3(9) 3_765 . . . ?
C7 C8 C9 C10 3.3(9) . . . 3_765 ?
C12 C6 C7 C12 0.0(11) . . . 3_765 ?
C12 C6 C7 C8 177.4(6) . . . . ?
C12 C7 C8 C9 -3.8(9) 3_765 . . . ?
C12 C11 C10 C9 2.0(10) . . . 3_765 ?
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
-0.4705 16.5810 -5.4668 0.0034 0.2597 0.9657
0.0772 -16.5817 5.6261 -0.0023 -0.2164 -0.9763
8.7073 -0.4905 -4.6552 0.0759 -0.9611 0.2655
-8.8109 0.7470 3.3091 0.0252 0.9808 -0.1932
-0.4227 -9.7329 -9.4123 0.9996 -0.0251 0.0093
1.4193 10.1184 8.7926 -0.9958 -0.0796 0.0442
-0.2315 -0.1200 -11.0013 0.8633 0.0674 0.5001
-2.2816 -18.6172 0.5601 0.5243 0.0444 -0.8504
0.8936 -17.6780 -4.5791 0.7892 -0.2802 -0.5465
-2.4816 8.2725 10.3385 -0.9337 0.3299 -0.1392
8.2584 4.3322 0.2531 -0.4159 -0.8760 0.2442
-6.2083 -12.0525 -1.6716 0.6588 0.5658 -0.4959
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 -0.306 0.000 0.000 1167.7 279.6 '12 H2O,4 DMF'
2 -0.476 0.500 0.500 1167.7 279.6 '12 H2O,4 DMF'
