#------------------------------------------------------------------------------
#$Date: 2019-01-19 01:01:12 +0200 (Sat, 19 Jan 2019) $
#$Revision: 213212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/28/7122876.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_7122876
loop_
_publ_author_name
'Kempe, David Kenneth'
'Dolinar, Brian'
'Vignesh, Kuduva R.'
'Woods, Toby'
'Saber, Mohamed R.'
'Dunbar, Kim R.'
_publ_section_title
;
 A cyanide-bridged wheel featuring a seven-coordinate Mo(III) center
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09373C
_journal_year                    2019
_chemical_formula_moiety         'C38 H46 Mo N16 Ni2 O'
_chemical_formula_sum            'C38 H46 Mo N16 Ni2 O'
_chemical_formula_weight         956.27
_chemical_name_systematic        '[MoIV(CN)8]6[Ni(L)]12(H2O)6'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-21 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   33.6548(8)
_cell_length_b                   33.6548(8)
_cell_length_c                   24.8190(6)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      70.174
_cell_measurement_theta_min      2.338
_cell_volume                     24345.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.203
_diffrn_reflns_theta_min         3.517
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  0.8399
_exptl_absorpt_correction_T_min  0.6380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0976 before and 0.0661 after correction. The Ratio of minimum to maximum transmission is 0.7596. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8856
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10294
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0430P)²+59.9499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8878
_reflns_number_total             10294
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc09373c2.cif
_cod_data_source_block           dkk2_098_octawheel
_cod_original_cell_volume        24344.9(13)
_cod_database_code               7122876
_shelx_shelxl_version_number     2018/3
_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   0.585
_shelx_estimated_absorpt_t_min   0.197
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C27(H27), C28(H28), C29(H29)
2.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Mo01 Mo 0.75756(2) 0.80031(2) 0.63676(2) 0.02460(6) Uani 1 1 d .
Ni02 Ni 0.65930(2) 0.71666(2) 0.81057(2) 0.02617(10) Uani 1 1 d .
Ni03 Ni 0.75380(2) 0.88438(2) 0.46403(2) 0.03260(11) Uani 1 1 d .
O1 O 0.61687(7) 0.66658(7) 0.87198(7) 0.0319(4) Uani 1 1 d .
N1 N 0.67673(7) 0.76440(7) 0.86509(8) 0.0284(4) Uani 1 1 d .
N2 N 0.71664(7) 0.71896(7) 0.84275(8) 0.0260(4) Uani 1 1 d .
N3 N 0.63605(8) 0.66082(8) 0.76276(9) 0.0358(5) Uani 1 1 d .
N4 N 0.60874(8) 0.73333(8) 0.80021(9) 0.0359(5) Uani 1 1 d .
N5 N 0.69733(8) 0.75855(8) 0.74829(8) 0.0313(5) Uani 1 1 d .
N6 N 0.76819(9) 0.89636(8) 0.68776(10) 0.0412(6) Uani 1 1 d .
N7 N 0.82325(11) 0.79483(11) 0.73221(11) 0.0585(8) Uani 1 1 d .
N8 N 0.68952(9) 0.69056(8) 0.60747(9) 0.0386(5) Uani 1 1 d .
N9 N 0.65547(8) 0.79068(8) 0.61506(8) 0.0317(5) Uani 1 1 d .
N10 N 0.85945(10) 0.89257(10) 0.61357(12) 0.0561(7) Uani 1 1 d .
N11 N 0.81874(8) 0.76056(9) 0.57756(9) 0.0402(6) Uani 1 1 d .
N12 N 0.75266(7) 0.83074(7) 0.51158(8) 0.0286(4) Uani 1 1 d .
N13 N 0.72208(9) 0.84040(7) 0.40568(8) 0.0366(5) Uani 1 1 d .
N14 N 0.80904(9) 0.89149(8) 0.42105(10) 0.0430(6) Uani 1 1 d .
N15 N 0.78679(9) 0.92618(8) 0.52894(10) 0.0429(6) Uani 1 1 d .
N16 N 0.68652(8) 0.86214(8) 0.48264(9) 0.0353(5) Uani 1 1 d .
C1 C 0.57739(11) 0.78145(12) 0.83578(14) 0.0503(8) Uani 1 1 d .
H1C H 0.556441 0.767051 0.866203 0.075 Uiso 1 1 calc GR
H1D H 0.559710 0.774111 0.802258 0.075 Uiso 1 1 calc GR
H1E H 0.594533 0.814793 0.840854 0.075 Uiso 1 1 calc GR
C2 C 0.61029(10) 0.76370(10) 0.83276(11) 0.0375(6) Uani 1 1 d .
C3 C 0.64916(10) 0.78191(9) 0.87233(10) 0.0341(6) Uani 1 1 d .
C4 C 0.65884(11) 0.81343(10) 0.91363(11) 0.0423(7) Uani 1 1 d .
H4 H 0.640228 0.826936 0.919177 0.051 Uiso 1 1 calc R
C5 C 0.69601(13) 0.82454(10) 0.94621(12) 0.0488(8) Uani 1 1 d .
H5 H 0.702879 0.845819 0.974750 0.059 Uiso 1 1 calc R
C6 C 0.72356(12) 0.80549(10) 0.93839(11) 0.0420(7) Uani 1 1 d .
H6 H 0.749031 0.813119 0.961237 0.050 Uiso 1 1 calc R
C7 C 0.71281(10) 0.77460(9) 0.89578(9) 0.0318(6) Uani 1 1 d .
C8 C 0.73689(9) 0.74910(8) 0.87942(9) 0.0280(5) Uani 1 1 d .
C9 C 0.78118(11) 0.76017(11) 0.90535(13) 0.0469(7) Uani 1 1 d .
H9A H 0.803738 0.764827 0.877490 0.070 Uiso 1 1 calc GR
H9B H 0.776464 0.734761 0.928827 0.070 Uiso 1 1 calc GR
H9C H 0.792465 0.788225 0.926808 0.070 Uiso 1 1 calc GR
C10 C 0.73542(9) 0.69145(9) 0.82086(10) 0.0302(5) Uani 1 1 d .
H10A H 0.749959 0.683377 0.850303 0.036 Uiso 1 1 calc R
H10B H 0.759446 0.709892 0.794045 0.036 Uiso 1 1 calc R
C11 C 0.69834(10) 0.64732(9) 0.79403(10) 0.0352(6) Uani 1 1 d .
H11A H 0.712884 0.629467 0.782244 0.042 Uiso 1 1 calc R
H11B H 0.675344 0.628907 0.821844 0.042 Uiso 1 1 calc R
C12 C 0.67296(10) 0.65198(10) 0.74618(11) 0.0369(6) Uani 1 1 d .
H12A H 0.694974 0.677471 0.723009 0.044 Uiso 1 1 calc R
H12B H 0.659628 0.623417 0.724620 0.044 Uiso 1 1 calc R
C13 C 0.60619(11) 0.66080(11) 0.71938(12) 0.0449(7) Uani 1 1 d .
H13A H 0.594201 0.632006 0.698468 0.054 Uiso 1 1 calc R
H13B H 0.624539 0.686715 0.694659 0.054 Uiso 1 1 calc R
C14 C 0.56603(12) 0.66496(12) 0.74097(14) 0.0536(8) Uani 1 1 d .
H14A H 0.553713 0.644886 0.772999 0.064 Uiso 1 1 calc R
H14B H 0.541582 0.652668 0.713271 0.064 Uiso 1 1 calc R
C15 C 0.57529(11) 0.71278(12) 0.75679(13) 0.0479(7) Uani 1 1 d .
H15A H 0.586618 0.733058 0.724826 0.057 Uiso 1 1 calc R
H15B H 0.546108 0.710677 0.768209 0.057 Uiso 1 1 calc R
C16 C 0.71824(9) 0.77351(9) 0.70988(9) 0.0263(5) Uani 1 1 d .
C17 C 0.76378(9) 0.86251(9) 0.67072(10) 0.0312(6) Uani 1 1 d .
C18 C 0.80026(10) 0.79696(11) 0.69938(11) 0.0405(7) Uani 1 1 d .
C19 C 0.69082(9) 0.79401(8) 0.62268(9) 0.0261(5) Uani 1 1 d .
C20 C 0.82474(10) 0.85965(11) 0.62125(12) 0.0412(7) Uani 1 1 d .
C21 C 0.79702(10) 0.77360(10) 0.59799(10) 0.0334(6) Uani 1 1 d .
C22 C 0.71302(9) 0.72864(9) 0.61831(9) 0.0300(5) Uani 1 1 d .
C23 C 0.75404(8) 0.81781(8) 0.55417(9) 0.0244(5) Uani 1 1 d .
C24 C 0.60590(11) 0.80945(12) 0.45778(13) 0.0522(8) Uani 1 1 d .
H24A H 0.596758 0.832142 0.449002 0.078 Uiso 1 1 calc GR
H24B H 0.596952 0.798861 0.494927 0.078 Uiso 1 1 calc GR
H24C H 0.590665 0.783312 0.433120 0.078 Uiso 1 1 calc GR
C25 C 0.65683(11) 0.83090(10) 0.45212(11) 0.0396(7) Uani 1 1 d .
C26 C 0.67663(11) 0.81613(9) 0.40698(11) 0.0386(7) Uani 1 1 d .
C27 C 0.65341(12) 0.78166(10) 0.36919(11) 0.0468(8) Uani 1 1 d .
H27 H 0.620845 0.764293 0.368634 0.056 Uiso 1 1 calc R
C28 C 0.67936(13) 0.77353(10) 0.33245(11) 0.0513(9) Uani 1 1 d .
H28 H 0.664277 0.750174 0.306161 0.062 Uiso 1 1 calc R
C29 C 0.72745(14) 0.79894(11) 0.33304(12) 0.0524(9) Uani 1 1 d .
H29 H 0.745126 0.792795 0.308112 0.063 Uiso 1 1 calc R
C30 C 0.74805(12) 0.83299(9) 0.37088(11) 0.0424(7) Uani 1 1 d .
C31 C 0.79862(13) 0.86553(10) 0.37904(13) 0.0511(8) Uani 1 1 d .
C32 C 0.83157(15) 0.86648(14) 0.33833(16) 0.0793(13) Uani 1 1 d .
H32A H 0.861658 0.893859 0.343877 0.119 Uiso 1 1 calc GR
H32B H 0.820432 0.867249 0.302071 0.119 Uiso 1 1 calc GR
H32C H 0.834296 0.838969 0.342231 0.119 Uiso 1 1 calc GR
C33 C 0.85543(12) 0.92790(11) 0.43270(14) 0.0513(8) Uani 1 1 d .
H33A H 0.862412 0.955165 0.410691 0.062 Uiso 1 1 calc R
H33B H 0.877339 0.917682 0.422457 0.062 Uiso 1 1 calc R
C34 C 0.86184(13) 0.94113(11) 0.49191(14) 0.0540(8) Uani 1 1 d .
H34A H 0.894756 0.963440 0.497770 0.065 Uiso 1 1 calc R
H34B H 0.854491 0.913364 0.513109 0.065 Uiso 1 1 calc R
C35 C 0.83414(11) 0.96173(10) 0.51528(13) 0.0456(7) Uani 1 1 d .
H35A H 0.849627 0.979431 0.548116 0.055 Uiso 1 1 calc R
H35B H 0.833200 0.983212 0.488758 0.055 Uiso 1 1 calc R
C36 C 0.75934(12) 0.94441(10) 0.55263(12) 0.0461(7) Uani 1 1 d .
H36A H 0.756218 0.964740 0.526240 0.055 Uiso 1 1 calc R
H36B H 0.775314 0.962986 0.584779 0.055 Uiso 1 1 calc R
C37 C 0.71163(11) 0.90587(10) 0.56888(12) 0.0440(7) Uani 1 1 d .
H37A H 0.715360 0.881248 0.585681 0.053 Uiso 1 1 calc R
H37B H 0.699896 0.918089 0.597158 0.053 Uiso 1 1 calc R
C38 C 0.67467(12) 0.88381(11) 0.52576(12) 0.0455(7) Uani 1 1 d .
H38A H 0.645783 0.860432 0.542905 0.055 Uiso 1 1 calc R
H38B H 0.669065 0.907575 0.509959 0.055 Uiso 1 1 calc R
H15 H 0.7890(12) 0.9082(12) 0.5564(15) 0.058(10) Uiso 1 1 d .
H3 H 0.6173(14) 0.6368(14) 0.7866(16) 0.079(13) Uiso 1 1 d .
H1A H 0.6022(12) 0.6740(12) 0.8909(14) 0.047(10) Uiso 1 1 d .
H1B H 0.6319(14) 0.6598(14) 0.8983(17) 0.073(12) Uiso 1 1 d .
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'
Mo Mo -0.0483 2.7339 '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'
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
C16 Mo01 C17 79.61(9) . .
C16 Mo01 C19 72.97(9) . .
C16 Mo01 C20 132.11(10) . .
C16 Mo01 C21 125.09(9) . .
C17 Mo01 C19 75.69(9) . .
C17 Mo01 C20 68.17(10) . .
C18 Mo01 C16 70.00(10) . .
C18 Mo01 C17 91.44(11) . .
C18 Mo01 C19 142.42(10) . .
C18 Mo01 C20 76.22(12) . .
C18 Mo01 C21 74.68(10) . .
C18 Mo01 C22 101.71(11) . .
C20 Mo01 C19 127.53(10) . .
C21 Mo01 C17 142.23(11) . .
C21 Mo01 C19 134.86(9) . .
C21 Mo01 C20 74.39(11) . .
C22 Mo01 C16 76.90(9) . .
C22 Mo01 C17 147.08(10) . .
C22 Mo01 C19 75.57(9) . .
C22 Mo01 C20 144.16(10) . .
C22 Mo01 C21 70.69(10) . .
C23 Mo01 C16 143.93(9) . .
C23 Mo01 C17 95.61(9) . .
C23 Mo01 C18 146.06(10) . .
C23 Mo01 C19 71.23(9) . .
C23 Mo01 C20 75.79(10) . .
C23 Mo01 C21 79.61(9) . .
C23 Mo01 C22 90.07(9) . .
N1 Ni02 O1 87.89(8) . .
N1 Ni02 N2 79.02(9) . .
N1 Ni02 N3 171.72(9) . .
N1 Ni02 N4 79.12(9) . .
N1 Ni02 N5 97.41(9) . .
N2 Ni02 O1 89.84(8) . .
N2 Ni02 N4 158.14(9) . .
N3 Ni02 O1 83.84(9) . .
N3 Ni02 N2 100.56(9) . .
N3 Ni02 N4 101.05(10) . .
N3 Ni02 N5 90.87(10) . .
N4 Ni02 O1 89.25(8) . .
N5 Ni02 O1 174.70(8) . .
N5 Ni02 N2 90.90(8) . .
N5 Ni02 N4 92.01(9) . .
N11 Ni03 N12 174.07(9) 11_566 .
N13 Ni03 N11 95.69(9) . 11_566
N13 Ni03 N12 89.83(8) . .
N13 Ni03 N14 79.84(10) . .
N13 Ni03 N15 175.31(9) . .
N13 Ni03 N16 78.80(10) . .
N14 Ni03 N11 87.84(10) . 11_566
N14 Ni03 N12 91.04(9) . .
N14 Ni03 N15 100.34(11) . .
N15 Ni03 N11 89.00(10) . 11_566
N15 Ni03 N12 85.48(9) . .
N16 Ni03 N11 92.19(9) . 11_566
N16 Ni03 N12 90.98(8) . .
N16 Ni03 N14 158.54(10) . .
N16 Ni03 N15 101.12(10) . .
Ni02 O1 H1A 116(2) . .
Ni02 O1 H1B 117(3) . .
H1A O1 H1B 99(3) . .
C3 N1 Ni02 117.82(19) . .
C7 N1 Ni02 118.09(17) . .
C7 N1 C3 123.8(2) . .
C8 N2 Ni02 115.19(17) . .
C8 N2 C10 122.7(2) . .
C10 N2 Ni02 121.81(16) . .
Ni02 N3 H3 102(2) . .
C12 N3 Ni02 112.22(17) . .
C12 N3 H3 106(3) . .
C13 N3 Ni02 112.14(18) . .
C13 N3 C12 116.1(2) . .
C13 N3 H3 107(3) . .
C2 N4 Ni02 115.4(2) . .
C2 N4 C15 123.8(2) . .
C15 N4 Ni02 120.71(19) . .
C16 N5 Ni02 165.3(2) . .
C21 N11 Ni03 165.9(3) . 12_656
C23 N12 Ni03 146.77(19) . .
C26 N13 Ni03 118.14(19) . .
C26 N13 C30 124.1(3) . .
C30 N13 Ni03 117.2(2) . .
C31 N14 Ni03 114.7(2) . .
C31 N14 C33 123.1(3) . .
C33 N14 Ni03 121.6(2) . .
Ni03 N15 H15 108(2) . .
C35 N15 Ni03 111.63(19) . .
C35 N15 H15 107(2) . .
C36 N15 Ni03 111.27(19) . .
C36 N15 C35 113.9(2) . .
C36 N15 H15 104(2) . .
C25 N16 Ni03 115.7(2) . .
C25 N16 C38 123.4(3) . .
C38 N16 Ni03 120.7(2) . .
H1C C1 H1D 109.5 . .
H1C C1 H1E 109.5 . .
H1D C1 H1E 109.5 . .
C2 C1 H1C 109.5 . .
C2 C1 H1D 109.5 . .
C2 C1 H1E 109.5 . .
N4 C2 C1 127.2(3) . .
N4 C2 C3 114.7(2) . .
C3 C2 C1 118.1(3) . .
N1 C3 C2 112.8(2) . .
N1 C3 C4 119.0(3) . .
C4 C3 C2 128.2(3) . .
C3 C4 H4 120.8 . .
C5 C4 C3 118.3(3) . .
C5 C4 H4 120.8 . .
C4 C5 H5 119.3 . .
C4 C5 C6 121.5(3) . .
C6 C5 H5 119.3 . .
C5 C6 H6 121.0 . .
C5 C6 C7 117.9(3) . .
C7 C6 H6 121.0 . .
N1 C7 C6 119.4(3) . .
N1 C7 C8 112.5(2) . .
C6 C7 C8 128.1(3) . .
N2 C8 C7 114.9(2) . .
N2 C8 C9 125.2(2) . .
C9 C8 C7 119.9(2) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N2 C10 H10A 109.2 . .
N2 C10 H10B 109.2 . .
N2 C10 C11 112.0(2) . .
H10A C10 H10B 107.9 . .
C11 C10 H10A 109.2 . .
C11 C10 H10B 109.2 . .
C10 C11 H11A 107.8 . .
C10 C11 H11B 107.8 . .
H11A C11 H11B 107.2 . .
C12 C11 C10 117.9(2) . .
C12 C11 H11A 107.8 . .
C12 C11 H11B 107.8 . .
N3 C12 C11 112.2(2) . .
N3 C12 H12A 109.2 . .
N3 C12 H12B 109.2 . .
C11 C12 H12A 109.2 . .
C11 C12 H12B 109.2 . .
H12A C12 H12B 107.9 . .
N3 C13 H13A 109.1 . .
N3 C13 H13B 109.1 . .
N3 C13 C14 112.3(3) . .
H13A C13 H13B 107.9 . .
C14 C13 H13A 109.1 . .
C14 C13 H13B 109.1 . .
C13 C14 H14A 107.9 . .
C13 C14 H14B 107.9 . .
C13 C14 C15 117.6(3) . .
H14A C14 H14B 107.2 . .
C15 C14 H14A 107.9 . .
C15 C14 H14B 107.9 . .
N4 C15 C14 113.0(2) . .
N4 C15 H15A 109.0 . .
N4 C15 H15B 109.0 . .
C14 C15 H15A 109.0 . .
C14 C15 H15B 109.0 . .
H15A C15 H15B 107.8 . .
N5 C16 Mo01 178.7(2) . .
N6 C17 Mo01 177.9(3) . .
N7 C18 Mo01 178.9(3) . .
N9 C19 Mo01 179.8(2) . .
N10 C20 Mo01 176.5(3) . .
N11 C21 Mo01 178.3(3) . .
N8 C22 Mo01 178.7(3) . .
N12 C23 Mo01 174.1(2) . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C25 C24 H24A 109.5 . .
C25 C24 H24B 109.5 . .
C25 C24 H24C 109.5 . .
N16 C25 C24 125.3(3) . .
N16 C25 C26 114.8(3) . .
C24 C25 C26 119.9(3) . .
N13 C26 C25 112.2(2) . .
N13 C26 C27 119.5(3) . .
C27 C26 C25 128.3(3) . .
C26 C27 H27 121.2 . .
C28 C27 C26 117.6(3) . .
C28 C27 H27 121.2 . .
C27 C28 H28 119.2 . .
C27 C28 C29 121.6(3) . .
C29 C28 H28 119.2 . .
C28 C29 H29 121.2 . .
C30 C29 C28 117.6(3) . .
C30 C29 H29 121.2 . .
N13 C30 C29 119.6(3) . .
N13 C30 C31 112.5(3) . .
C29 C30 C31 127.9(3) . .
N14 C31 C30 115.2(3) . .
N14 C31 C32 125.9(3) . .
C32 C31 C30 118.9(3) . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
N14 C33 H33A 109.2 . .
N14 C33 H33B 109.2 . .
N14 C33 C34 112.0(3) . .
H33A C33 H33B 107.9 . .
C34 C33 H33A 109.2 . .
C34 C33 H33B 109.2 . .
C33 C34 H34A 107.8 . .
C33 C34 H34B 107.8 . .
C33 C34 C35 118.1(3) . .
H34A C34 H34B 107.1 . .
C35 C34 H34A 107.8 . .
C35 C34 H34B 107.8 . .
N15 C35 C34 112.1(2) . .
N15 C35 H35A 109.2 . .
N15 C35 H35B 109.2 . .
C34 C35 H35A 109.2 . .
C34 C35 H35B 109.2 . .
H35A C35 H35B 107.9 . .
N15 C36 H36A 109.3 . .
N15 C36 H36B 109.3 . .
N15 C36 C37 111.4(2) . .
H36A C36 H36B 108.0 . .
C37 C36 H36A 109.3 . .
C37 C36 H36B 109.3 . .
C36 C37 H37A 107.6 . .
C36 C37 H37B 107.6 . .
H37A C37 H37B 107.0 . .
C38 C37 C36 118.9(3) . .
C38 C37 H37A 107.6 . .
C38 C37 H37B 107.6 . .
N16 C38 C37 113.5(3) . .
N16 C38 H38A 108.9 . .
N16 C38 H38B 108.9 . .
C37 C38 H38A 108.9 . .
C37 C38 H38B 108.9 . .
H38A C38 H38B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo01 C16 2.160(2) .
Mo01 C17 2.168(3) .
Mo01 C18 2.157(3) .
Mo01 C19 2.176(3) .
Mo01 C20 2.176(3) .
Mo01 C21 2.166(3) .
Mo01 C22 2.158(3) .
Mo01 C23 2.152(2) .
Ni02 O1 2.1899(19) .
Ni02 N1 1.953(2) .
Ni02 N2 2.054(2) .
Ni02 N3 2.020(2) .
Ni02 N4 2.057(2) .
Ni02 N5 2.052(2) .
Ni03 N11 2.101(2) 11_566
Ni03 N12 2.141(2) .
Ni03 N13 1.962(2) .
Ni03 N14 2.051(3) .
Ni03 N15 2.060(3) .
Ni03 N16 2.051(2) .
O1 H1A 0.81(4) .
O1 H1B 0.92(4) .
N1 C3 1.337(3) .
N1 C7 1.325(3) .
N2 C8 1.277(3) .
N2 C10 1.462(3) .
N3 C12 1.473(4) .
N3 C13 1.472(3) .
N3 H3 0.95(4) .
N4 C2 1.283(4) .
N4 C15 1.459(4) .
N5 C16 1.141(3) .
N6 C17 1.153(3) .
N7 C18 1.150(4) .
N8 C22 1.152(4) .
N9 C19 1.153(3) .
N10 C20 1.155(4) .
N11 C21 1.142(3) .
N12 C23 1.153(3) .
N13 C26 1.326(4) .
N13 C30 1.338(4) .
N14 C31 1.291(4) .
N14 C33 1.452(4) .
N15 C35 1.476(4) .
N15 C36 1.464(4) .
N15 H15 0.94(4) .
N16 C25 1.276(4) .
N16 C38 1.458(4) .
C1 H1C 0.9800 .
C1 H1D 0.9800 .
C1 H1E 0.9800 .
C1 C2 1.500(4) .
C2 C3 1.500(4) .
C3 C4 1.392(4) .
C4 H4 0.9500 .
C4 C5 1.375(5) .
C5 H5 0.9500 .
C5 C6 1.379(4) .
C6 H6 0.9500 .
C6 C7 1.398(4) .
C7 C8 1.502(4) .
C8 C9 1.490(4) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C10 C11 1.534(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C11 C12 1.516(4) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C13 C14 1.524(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C14 C15 1.530(5) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C24 C25 1.497(4) .
C25 C26 1.509(4) .
C26 C27 1.389(4) .
C27 H27 0.9500 .
C27 C28 1.381(5) .
C28 H28 0.9500 .
C28 C29 1.402(5) .
C29 H29 0.9500 .
C29 C30 1.372(4) .
C30 C31 1.508(5) .
C31 C32 1.489(5) .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C33 C34 1.519(5) .
C34 H34A 0.9900 .
C34 H34B 0.9900 .
C34 C35 1.527(5) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C36 H36A 0.9900 .
C36 H36B 0.9900 .
C36 C37 1.530(4) .
C37 H37A 0.9900 .
C37 H37B 0.9900 .
C37 C38 1.523(4) .
C38 H38A 0.9900 .
C38 H38B 0.9900 .
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
Ni02 N1 C3 C2 -4.7(3)
Ni02 N1 C3 C4 175.16(19)
Ni02 N1 C7 C6 -174.06(19)
Ni02 N1 C7 C8 4.7(3)
Ni02 N2 C8 C7 5.1(3)
Ni02 N2 C8 C9 -174.4(2)
Ni02 N2 C10 C11 -27.8(3)
Ni02 N3 C12 C11 55.7(3)
Ni02 N3 C13 C14 -55.5(3)
Ni02 N4 C2 C1 -178.1(2)
Ni02 N4 C2 C3 0.5(3)
Ni02 N4 C15 C14 28.8(3)
Ni03 N13 C26 C25 5.9(3)
Ni03 N13 C26 C27 -173.86(19)
Ni03 N13 C30 C29 172.7(2)
Ni03 N13 C30 C31 -8.0(3)
Ni03 N14 C31 C30 -3.2(3)
Ni03 N14 C31 C32 174.5(3)
Ni03 N14 C33 C34 30.8(3)
Ni03 N15 C35 C34 -54.3(3)
Ni03 N15 C36 C37 56.1(3)
Ni03 N16 C25 C24 -179.9(2)
Ni03 N16 C25 C26 -0.7(3)
Ni03 N16 C38 C37 -26.3(3)
N1 C3 C4 C5 -1.4(4)
N1 C7 C8 N2 -6.4(3)
N1 C7 C8 C9 173.1(2)
N2 C10 C11 C12 61.3(3)
N3 C13 C14 C15 79.9(4)
N4 C2 C3 N1 2.6(3)
N4 C2 C3 C4 -177.3(3)
N13 C26 C27 C28 1.7(4)
N13 C30 C31 N14 7.2(4)
N13 C30 C31 C32 -170.6(3)
N14 C33 C34 C35 -63.8(4)
N15 C36 C37 C38 -80.8(3)
N16 C25 C26 N13 -3.2(3)
N16 C25 C26 C27 176.5(3)
C1 C2 C3 N1 -178.7(2)
C1 C2 C3 C4 1.5(4)
C2 N4 C15 C14 -154.1(3)
C2 C3 C4 C5 178.5(3)
C3 N1 C7 C6 -0.2(4)
C3 N1 C7 C8 178.5(2)
C3 C4 C5 C6 0.5(4)
C4 C5 C6 C7 0.5(4)
C5 C6 C7 N1 -0.7(4)
C5 C6 C7 C8 -179.3(3)
C6 C7 C8 N2 172.2(3)
C6 C7 C8 C9 -8.3(4)
C7 N1 C3 C2 -178.6(2)
C7 N1 C3 C4 1.3(4)
C8 N2 C10 C11 159.1(2)
C10 N2 C8 C7 178.6(2)
C10 N2 C8 C9 -0.8(4)
C10 C11 C12 N3 -80.6(3)
C12 N3 C13 C14 173.7(3)
C13 N3 C12 C11 -173.5(2)
C13 C14 C15 N4 -61.6(4)
C15 N4 C2 C1 4.7(4)
C15 N4 C2 C3 -176.7(2)
C24 C25 C26 N13 176.0(2)
C24 C25 C26 C27 -4.2(4)
C25 N16 C38 C37 158.4(3)
C25 C26 C27 C28 -178.1(3)
C26 N13 C30 C29 1.2(4)
C26 N13 C30 C31 -179.5(2)
C26 C27 C28 C29 0.1(4)
C27 C28 C29 C30 -1.2(5)
C28 C29 C30 N13 0.6(4)
C28 C29 C30 C31 -178.5(3)
C29 C30 C31 N14 -173.6(3)
C29 C30 C31 C32 8.6(5)
C30 N13 C26 C25 177.4(2)
C30 N13 C26 C27 -2.4(4)
C31 N14 C33 C34 -159.0(3)
C33 N14 C31 C30 -173.9(3)
C33 N14 C31 C32 3.8(5)
C33 C34 C35 N15 80.8(4)
C35 N15 C36 C37 -176.7(2)
C36 N15 C35 C34 178.7(3)
C36 C37 C38 N16 60.5(3)
C38 N16 C25 C24 -4.4(4)
C38 N16 C25 C26 174.8(2)
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
1 0.000 0.000 -0.656 2537.8 796.4
2 -0.333 0.333 -0.541 2537.8 796.4
3 0.333 0.667 -0.395 2537.8 796.4
