#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:08:57 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232195 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/71/4347160.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_4347160
loop_
_publ_author_name
'Gómez, Manuel'
'Hernández-Prieto, Cristina'
'Martín, Avelino'
'Mena, Miguel'
'Santamaría, Cristina'
_publ_section_title
;
 Systematic Approach for the Construction of Niobium and Tantalum Sulfide
 Clusters.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3815
_journal_page_last               3821
_journal_paper_doi               10.1021/acs.inorgchem.5b02816
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H56 Cl4 N8 Nb4 S4, 2.5 (C6 H6)'
_chemical_formula_sum            'C51 H71 Cl4 N8 Nb4 S4'
_chemical_formula_weight         1437.83
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 133.014(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.196(2)
_cell_length_b                   12.090(4)
_cell_length_c                   32.329(8)
_cell_measurement_reflns_used    219
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     12631(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1359
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            85920
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.063
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  1.022
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5832
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     628
_refine_ls_number_reflns         14438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.15
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0294P)²+78.2033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0
_reflns_number_gt                8114
_reflns_number_total             14438
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02816_si_001.cif
_cod_data_source_block           5
_cod_original_cell_volume        12631(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347160
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C11 C 0.52677(18) 0.5259(5) 0.6174(2) 0.0341(14) Uani 1 1 d . .
C12 C 0.5364(2) 0.4415(6) 0.6607(3) 0.0512(19) Uani 1 1 d . .
H12A H 0.5316 0.4749 0.6828 0.077 Uiso 1 1 calc R U
H12B H 0.5648 0.4188 0.6851 0.077 Uiso 1 1 calc R U
H12C H 0.5187 0.3782 0.6411 0.077 Uiso 1 1 calc R U
C13 C 0.5342(2) 0.4748(6) 0.5814(3) 0.0516(18) Uani 1 1 d . .
H13A H 0.5166 0.4114 0.5616 0.077 Uiso 1 1 calc R U
H13B H 0.5626 0.4526 0.6056 0.077 Uiso 1 1 calc R U
H13C H 0.5279 0.5284 0.5546 0.077 Uiso 1 1 calc R U
C14 C 0.5530(2) 0.6298(6) 0.6480(3) 0.0517(19) Uani 1 1 d . .
H14A H 0.5472 0.6815 0.6208 0.078 Uiso 1 1 calc R U
H14B H 0.5818 0.6102 0.6741 0.078 Uiso 1 1 calc R U
H14C H 0.5466 0.6628 0.6682 0.078 Uiso 1 1 calc R U
C21 C 0.22814(19) 0.6670(5) 0.3759(3) 0.0363(15) Uani 1 1 d . .
C22 C 0.20747(19) 0.5666(6) 0.3757(3) 0.0471(17) Uani 1 1 d . .
H22A H 0.2021 0.5127 0.3495 0.071 Uiso 1 1 calc R U
H22B H 0.1819 0.5885 0.3645 0.071 Uiso 1 1 calc R U
H22C H 0.2254 0.5352 0.413 0.071 Uiso 1 1 calc R U
C23 C 0.2373(2) 0.7544(6) 0.4175(3) 0.0501(18) Uani 1 1 d . .
H23A H 0.2573 0.7259 0.4554 0.075 Uiso 1 1 calc R U
H23B H 0.2122 0.7722 0.4086 0.075 Uiso 1 1 calc R U
H23C H 0.248 0.8199 0.4146 0.075 Uiso 1 1 calc R U
C24 C 0.20106(19) 0.7162(6) 0.3164(3) 0.0481(18) Uani 1 1 d . .
H24A H 0.2135 0.7831 0.3179 0.072 Uiso 1 1 calc R U
H24B H 0.1741 0.7323 0.3022 0.072 Uiso 1 1 calc R U
H24C H 0.1986 0.664 0.2919 0.072 Uiso 1 1 calc R U
C31 C 0.34672(19) 0.2615(5) 0.3551(3) 0.0357(15) Uani 1 1 d . .
C32 C 0.30068(19) 0.2303(5) 0.3128(3) 0.0462(17) Uani 1 1 d . .
H32A H 0.296 0.1747 0.3292 0.069 Uiso 1 1 calc R U
H32B H 0.2927 0.2022 0.2788 0.069 Uiso 1 1 calc R U
H32C H 0.2845 0.2946 0.3041 0.069 Uiso 1 1 calc R U
C33 C 0.3546(2) 0.3568(5) 0.3324(3) 0.0431(16) Uani 1 1 d . .
H33A H 0.3384 0.4197 0.3254 0.065 Uiso 1 1 calc R U
H33B H 0.347 0.3346 0.2979 0.065 Uiso 1 1 calc R U
H33C H 0.3834 0.3761 0.3599 0.065 Uiso 1 1 calc R U
C34 C 0.3740(2) 0.1627(6) 0.3696(3) 0.0526(19) Uani 1 1 d . .
H34A H 0.4026 0.1846 0.397 0.079 Uiso 1 1 calc R U
H34B H 0.3673 0.1371 0.336 0.079 Uiso 1 1 calc R U
H34C H 0.3695 0.1043 0.3849 0.079 Uiso 1 1 calc R U
C41 C 0.40270(19) 0.6494(6) 0.6719(3) 0.0432(17) Uani 1 1 d . .
C42 C 0.3802(2) 0.6116(7) 0.6903(3) 0.055(2) Uani 1 1 d . .
H42A H 0.3509 0.621 0.6594 0.083 Uiso 1 1 calc R U
H42B H 0.3894 0.6551 0.7219 0.083 Uiso 1 1 calc R U
H42C H 0.3862 0.535 0.7009 0.083 Uiso 1 1 calc R U
C43 C 0.44893(19) 0.6228(7) 0.7177(3) 0.060(2) Uani 1 1 d . .
H43A H 0.4525 0.5456 0.727 0.09 Uiso 1 1 calc R U
H43B H 0.4613 0.6661 0.7508 0.09 Uiso 1 1 calc R U
H43C H 0.462 0.64 0.7039 0.09 Uiso 1 1 calc R U
C44 C 0.3955(2) 0.7737(6) 0.6578(3) 0.058(2) Uani 1 1 d . .
H44A H 0.407 0.7946 0.6423 0.087 Uiso 1 1 calc R U
H44B H 0.4086 0.8154 0.6917 0.087 Uiso 1 1 calc R U
H44C H 0.3663 0.7888 0.6308 0.087 Uiso 1 1 calc R U
C111 C 0.4576(2) 0.7499(5) 0.4943(3) 0.0403(16) Uani 1 1 d . .
H111 H 0.4692 0.6822 0.498 0.048 Uiso 1 1 calc R U
C112 C 0.4629(2) 0.8386(6) 0.4733(3) 0.0510(19) Uani 1 1 d . .
H112 H 0.4775 0.8305 0.4622 0.061 Uiso 1 1 calc R U
C113 C 0.4466(2) 0.9397(6) 0.4688(3) 0.0534(19) Uani 1 1 d . .
H113 H 0.4504 1.0009 0.4553 0.064 Uiso 1 1 calc R U
C114 C 0.4248(2) 0.9490(5) 0.4844(3) 0.0456(17) Uani 1 1 d . .
H114 H 0.4133 1.0163 0.4815 0.055 Uiso 1 1 calc R U
C115 C 0.42008(18) 0.8557(5) 0.5046(2) 0.0370(15) Uani 1 1 d . .
H115 H 0.4051 0.862 0.5152 0.044 Uiso 1 1 calc R U
C211 C 0.2996(2) 0.8362(5) 0.3719(3) 0.0473(17) Uani 1 1 d . .
H211 H 0.2869 0.8386 0.3858 0.057 Uiso 1 1 calc R U
C212 C 0.2938(2) 0.9225(6) 0.3398(3) 0.061(2) Uani 1 1 d . .
H212 H 0.2771 0.9815 0.3319 0.074 Uiso 1 1 calc R U
C213 C 0.3122(2) 0.9229(6) 0.3196(3) 0.0529(19) Uani 1 1 d . .
H213 H 0.3074 0.9801 0.2964 0.063 Uiso 1 1 calc R U
C214 C 0.3383(2) 0.8367(6) 0.3338(3) 0.0527(19) Uani 1 1 d . .
H214 H 0.3528 0.8362 0.3226 0.063 Uiso 1 1 calc R U
C215 C 0.3421(2) 0.7505(5) 0.3657(3) 0.0439(17) Uani 1 1 d . .
H215 H 0.3591 0.6912 0.3748 0.053 Uiso 1 1 calc R U
C311 C 0.3354(2) 0.1371(5) 0.4661(3) 0.0427(16) Uani 1 1 d . .
H311 H 0.3151 0.167 0.4301 0.051 Uiso 1 1 calc R U
C312 C 0.3280(2) 0.0364(6) 0.4789(3) 0.0525(19) Uani 1 1 d . .
H312 H 0.3028 0.0004 0.4516 0.063 Uiso 1 1 calc R U
C313 C 0.3575(3) -0.0096(6) 0.5311(4) 0.065(2) Uani 1 1 d . .
H313 H 0.3529 -0.0773 0.5398 0.077 Uiso 1 1 calc R U
C314 C 0.3939(3) 0.0463(6) 0.5705(3) 0.056(2) Uani 1 1 d . .
H314 H 0.4146 0.0173 0.6066 0.068 Uiso 1 1 calc R U
C315 C 0.3994(2) 0.1473(6) 0.5556(3) 0.0462(17) Uani 1 1 d . .
H315 H 0.424 0.1854 0.5828 0.055 Uiso 1 1 calc R U
C411 C 0.3248(2) 0.2778(6) 0.5536(3) 0.0452(17) Uani 1 1 d . .
H411 H 0.3029 0.2955 0.5157 0.054 Uiso 1 1 calc R U
C412 C 0.3233(2) 0.1800(5) 0.5745(3) 0.0518(19) Uani 1 1 d . .
H412 H 0.3006 0.1331 0.5509 0.062 Uiso 1 1 calc R U
C413 C 0.3551(3) 0.1530(6) 0.6296(4) 0.060(2) Uani 1 1 d . .
H413 H 0.3545 0.0878 0.6442 0.072 Uiso 1 1 calc R U
C414 C 0.3884(2) 0.2233(7) 0.6635(3) 0.062(2) Uani 1 1 d . .
H414 H 0.4106 0.2066 0.7014 0.075 Uiso 1 1 calc R U
C415 C 0.3884(2) 0.3194(6) 0.6403(3) 0.0472(17) Uani 1 1 d . .
H415 H 0.4112 0.366 0.6631 0.057 Uiso 1 1 calc R U
C501 C 0.5831(3) 0.9319(7) 0.7038(4) 0.148(6) Uani 1 1 d G .
H501 H 0.593 0.8627 0.7208 0.177 Uiso 1 1 calc R U
C502 C 0.60925(19) 1.0231(10) 0.7288(2) 0.138(6) Uani 1 1 d G .
H502 H 0.6367 1.015 0.7624 0.166 Uiso 1 1 calc R U
C503 C 0.5944(3) 1.1265(8) 0.7034(4) 0.111(4) Uani 1 1 d G .
H503 H 0.6119 1.1875 0.7201 0.133 Uiso 1 1 calc R U
C504 C 0.5534(3) 1.1387(4) 0.6531(4) 0.089(3) Uani 1 1 d G .
H504 H 0.5434 1.2079 0.6361 0.107 Uiso 1 1 calc R U
C505 C 0.52718(17) 1.0475(7) 0.6281(2) 0.084(3) Uani 1 1 d G .
H505 H 0.4997 1.0556 0.5945 0.101 Uiso 1 1 calc R U
C506 C 0.5420(3) 0.9441(5) 0.6535(4) 0.113(4) Uani 1 1 d G .
H506 H 0.5245 0.8831 0.6368 0.135 Uiso 1 1 calc R U
C601 C 0.3037(2) 0.5696(7) 0.2104(4) 0.154(7) Uani 1 1 d G .
H601 H 0.3129 0.5148 0.2369 0.185 Uiso 1 1 calc R U
C602 C 0.2906(2) 0.6710(8) 0.2138(3) 0.103(4) Uani 1 1 d G .
H602 H 0.2911 0.6839 0.2426 0.124 Uiso 1 1 calc R U
C603 C 0.2768(2) 0.7529(5) 0.1741(4) 0.084(3) Uani 1 1 d G .
H603 H 0.2681 0.8207 0.1764 0.101 Uiso 1 1 calc R U
C604 C 0.27612(19) 0.7336(7) 0.1311(3) 0.094(3) Uani 1 1 d G .
H604 H 0.2669 0.7885 0.1045 0.112 Uiso 1 1 calc R U
C605 C 0.2892(2) 0.6323(8) 0.1277(3) 0.118(5) Uani 1 1 d G .
H605 H 0.2887 0.6194 0.0989 0.142 Uiso 1 1 calc R U
C606 C 0.3030(2) 0.5503(5) 0.1674(5) 0.173(8) Uani 1 1 d G .
H606 H 0.3117 0.4825 0.1651 0.208 Uiso 1 1 calc R U
Nb1 Nb 0.43543(2) 0.60316(4) 0.55327(2) 0.02791(13) Uani 1 1 d . .
Nb2 Nb 0.31283(2) 0.58699(4) 0.41391(2) 0.02788(14) Uani 1 1 d . .
Nb3 Nb 0.38224(2) 0.35102(4) 0.47420(2) 0.02890(14) Uani 1 1 d . .
Nb4 Nb 0.35818(2) 0.52392(4) 0.55582(2) 0.02943(14) Uani 1 1 d . .
S1 S 0.35837(4) 0.68017(12) 0.50880(6) 0.0289(3) Uani 1 1 d . .
S2 S 0.39182(4) 0.53232(12) 0.45419(6) 0.0283(3) Uani 1 1 d . .
S3 S 0.31869(4) 0.41149(12) 0.45391(6) 0.0292(3) Uani 1 1 d . .
S4 S 0.42078(4) 0.44082(12) 0.58083(6) 0.0305(3) Uani 1 1 d . .
Cl1 Cl 0.46155(5) 0.74073(13) 0.62546(6) 0.0397(4) Uani 1 1 d . .
Cl2 Cl 0.28209(5) 0.52971(13) 0.32011(6) 0.0412(4) Uani 1 1 d . .
Cl3 Cl 0.44911(5) 0.26471(13) 0.52483(7) 0.0433(4) Uani 1 1 d . .
Cl4 Cl 0.29036(5) 0.52948(14) 0.52456(6) 0.0409(4) Uani 1 1 d . .
N11 N 0.48408(14) 0.5578(4) 0.58196(19) 0.0308(11) Uani 1 1 d . .
N12 N 0.43612(15) 0.7575(4) 0.5096(2) 0.0315(12) Uani 1 1 d . .
N21 N 0.26684(14) 0.6330(4) 0.39373(19) 0.0338(12) Uani 1 1 d . .
N22 N 0.32274(15) 0.7487(4) 0.3839(2) 0.0326(12) Uani 1 1 d . .
N31 N 0.35873(14) 0.2980(4) 0.4076(2) 0.0305(11) Uani 1 1 d . .
N32 N 0.37100(16) 0.1916(4) 0.5044(2) 0.0367(12) Uani 1 1 d . .
N41 N 0.38431(14) 0.5890(4) 0.6208(2) 0.0331(12) Uani 1 1 d . .
N42 N 0.35705(15) 0.3478(4) 0.5866(2) 0.0331(12) Uani 1 1 d . .
C702 C 0.4993(4) 0.1707(17) 0.7087(6) 0.134(7) Uani 1 1 d . .
H702 H 0.5003 0.1714 0.6808 0.16 Uiso 1 1 calc R U
C703 C 0.4988(3) 0.2677(13) 0.7280(5) 0.121(4) Uani 1 1 d . .
H703 H 0.4968 0.3338 0.7116 0.145 Uiso 1 1 calc R U
C701 C 0.4985(5) 0.0735(13) 0.7270(7) 0.176(12) Uani 1 1 d . .
H701 H 0.496 0.0078 0.7099 0.211 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
N11 C11 C14 107.5(5) . .
N11 C11 C12 107.5(5) . .
C14 C11 C12 109.9(5) . .
N11 C11 C13 110.2(5) . .
C14 C11 C13 111.0(5) . .
C12 C11 C13 110.7(5) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N21 C21 C22 108.7(5) . .
N21 C21 C24 108.2(5) . .
C22 C21 C24 110.7(5) . .
N21 C21 C23 108.4(5) . .
C22 C21 C23 110.5(5) . .
C24 C21 C23 110.3(5) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C21 C24 H24A 109.5 . .
C21 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C21 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
N31 C31 C34 107.1(5) . .
N31 C31 C33 107.9(5) . .
C34 C31 C33 110.3(5) . .
N31 C31 C32 108.6(5) . .
C34 C31 C32 111.8(5) . .
C33 C31 C32 110.9(5) . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C31 C33 H33A 109.5 . .
C31 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C31 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C31 C34 H34A 109.5 . .
C31 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C31 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
N41 C41 C43 109.7(5) . .
N41 C41 C42 106.5(5) . .
C43 C41 C42 110.7(5) . .
N41 C41 C44 108.3(5) . .
C43 C41 C44 111.2(6) . .
C42 C41 C44 110.2(6) . .
C41 C42 H42A 109.5 . .
C41 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C41 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C41 C43 H43A 109.5 . .
C41 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C41 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C41 C44 H44A 109.5 . .
C41 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C41 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
N12 C111 C112 122.2(6) . .
N12 C111 H111 118.9 . .
C112 C111 H111 118.9 . .
C113 C112 C111 119.4(6) . .
C113 C112 H112 120.3 . .
C111 C112 H112 120.3 . .
C114 C113 C112 119.1(6) . .
C114 C113 H113 120.4 . .
C112 C113 H113 120.4 . .
C113 C114 C115 118.6(6) . .
C113 C114 H114 120.7 . .
C115 C114 H114 120.7 . .
N12 C115 C114 122.8(6) . .
N12 C115 H115 118.6 . .
C114 C115 H115 118.6 . .
N22 C211 C212 122.3(7) . .
N22 C211 H211 118.9 . .
C212 C211 H211 118.9 . .
C213 C212 C211 120.7(7) . .
C213 C212 H212 119.6 . .
C211 C212 H212 119.6 . .
C212 C213 C214 118.6(7) . .
C212 C213 H213 120.7 . .
C214 C213 H213 120.7 . .
C213 C214 C215 117.5(7) . .
C213 C214 H214 121.2 . .
C215 C214 H214 121.2 . .
N22 C215 C214 123.5(6) . .
N22 C215 H215 118.3 . .
C214 C215 H215 118.3 . .
N32 C311 C312 121.5(6) . .
N32 C311 H311 119.3 . .
C312 C311 H311 119.3 . .
C313 C312 C311 120.2(7) . .
C313 C312 H312 119.9 . .
C311 C312 H312 119.9 . .
C312 C313 C314 118.4(7) . .
C312 C313 H313 120.8 . .
C314 C313 H313 120.8 . .
C313 C314 C315 118.9(7) . .
C313 C314 H314 120.5 . .
C315 C314 H314 120.5 . .
N32 C315 C314 123.0(7) . .
N32 C315 H315 118.5 . .
C314 C315 H315 118.5 . .
N42 C411 C412 121.8(7) . .
N42 C411 H411 119.1 . .
C412 C411 H411 119.1 . .
C413 C412 C411 119.5(7) . .
C413 C412 H412 120.2 . .
C411 C412 H412 120.2 . .
C412 C413 C414 119.2(7) . .
C412 C413 H413 120.4 . .
C414 C413 H413 120.4 . .
C413 C414 C415 118.8(7) . .
C413 C414 H414 120.6 . .
C415 C414 H414 120.6 . .
N42 C415 C414 122.8(7) . .
N42 C415 H415 118.6 . .
C414 C415 H415 118.6 . .
C502 C501 C506 120 . .
C502 C501 H501 120 . .
C506 C501 H501 120 . .
C503 C502 C501 120 . .
C503 C502 H502 120 . .
C501 C502 H502 120 . .
C502 C503 C504 120 . .
C502 C503 H503 120 . .
C504 C503 H503 120 . .
C503 C504 C505 120 . .
C503 C504 H504 120 . .
C505 C504 H504 120 . .
C506 C505 C504 120 . .
C506 C505 H505 120 . .
C504 C505 H505 120 . .
C505 C506 C501 120 . .
C505 C506 H506 120 . .
C501 C506 H506 120 . .
C602 C601 C606 120 . .
C602 C601 H601 120 . .
C606 C601 H601 120 . .
C601 C602 C603 120 . .
C601 C602 H602 120 . .
C603 C602 H602 120 . .
C604 C603 C602 120 . .
C604 C603 H603 120 . .
C602 C603 H603 120 . .
C603 C604 C605 120 . .
C603 C604 H604 120 . .
C605 C604 H604 120 . .
C606 C605 C604 120 . .
C606 C605 H605 120 . .
C604 C605 H605 120 . .
C605 C606 C601 120 . .
C605 C606 H606 120 . .
C601 C606 H606 120 . .
N11 Nb1 N12 93.03(19) . .
N11 Nb1 S4 95.21(16) . .
N12 Nb1 S4 168.77(12) . .
N11 Nb1 Cl1 95.68(15) . .
N12 Nb1 Cl1 80.81(12) . .
S4 Nb1 Cl1 105.88(6) . .
N11 Nb1 S2 99.53(15) . .
N12 Nb1 S2 79.53(12) . .
S4 Nb1 S2 91.59(5) . .
Cl1 Nb1 S2 155.66(6) . .
N11 Nb1 S1 178.72(17) . .
N12 Nb1 S1 86.39(12) . .
S4 Nb1 S1 85.51(5) . .
Cl1 Nb1 S1 83.10(5) . .
S2 Nb1 S1 81.49(5) . .
N21 Nb2 N22 94.5(2) . .
N21 Nb2 S3 98.78(16) . .
N22 Nb2 S3 166.60(13) . .
N21 Nb2 Cl2 96.15(16) . .
N22 Nb2 Cl2 79.92(12) . .
S3 Nb2 Cl2 100.55(6) . .
N21 Nb2 S1 94.12(16) . .
N22 Nb2 S1 84.92(12) . .
S3 Nb2 S1 92.08(5) . .
Cl2 Nb2 S1 162.29(6) . .
N21 Nb2 S2 173.92(16) . .
N22 Nb2 S2 82.33(12) . .
S3 Nb2 S2 84.29(5) . .
Cl2 Nb2 S2 88.40(5) . .
S1 Nb2 S2 80.49(5) . .
N31 Nb3 N32 95.40(19) . .
N31 Nb3 S2 93.94(15) . .
N32 Nb3 S2 168.80(12) . .
N31 Nb3 Cl3 95.72(16) . .
N32 Nb3 Cl3 82.72(13) . .
S2 Nb3 Cl3 102.50(6) . .
N31 Nb3 S3 99.49(15) . .
N32 Nb3 S3 80.37(13) . .
S2 Nb3 S3 92.01(5) . .
Cl3 Nb3 S3 158.18(6) . .
N31 Nb3 S4 178.57(16) . .
N32 Nb3 S4 86.01(13) . .
S2 Nb3 S4 84.69(5) . .
Cl3 Nb3 S4 84.21(5) . .
S3 Nb3 S4 80.97(5) . .
N41 Nb4 N42 94.9(2) . .
N41 Nb4 Cl4 95.96(15) . .
N42 Nb4 Cl4 79.93(12) . .
N41 Nb4 S1 96.92(16) . .
N42 Nb4 S1 166.88(12) . .
Cl4 Nb4 S1 104.40(5) . .
N41 Nb4 S4 96.55(15) . .
N42 Nb4 S4 80.74(12) . .
Cl4 Nb4 S4 157.76(6) . .
S1 Nb4 S4 92.25(5) . .
N41 Nb4 S3 177.46(17) . .
N42 Nb4 S3 83.33(12) . .
Cl4 Nb4 S3 85.55(5) . .
S1 Nb4 S3 84.66(5) . .
S4 Nb4 S3 81.38(5) . .
Nb4 S1 Nb2 94.22(6) . .
Nb4 S1 Nb1 86.70(5) . .
Nb2 S1 Nb1 99.11(5) . .
Nb3 S2 Nb1 95.21(5) . .
Nb3 S2 Nb2 87.06(5) . .
Nb1 S2 Nb2 97.99(5) . .
Nb2 S3 Nb3 95.06(5) . .
Nb2 S3 Nb4 87.51(5) . .
Nb3 S3 Nb4 98.32(5) . .
Nb1 S4 Nb4 94.00(5) . .
Nb1 S4 Nb3 87.28(5) . .
Nb4 S4 Nb3 98.44(5) . .
C11 N11 Nb1 167.2(4) . .
C115 N12 C111 117.9(5) . .
C115 N12 Nb1 123.7(4) . .
C111 N12 Nb1 118.0(4) . .
C21 N21 Nb2 177.7(4) . .
C215 N22 C211 117.2(5) . .
C215 N22 Nb2 123.6(4) . .
C211 N22 Nb2 117.2(4) . .
C31 N31 Nb3 168.5(4) . .
C315 N32 C311 118.0(5) . .
C315 N32 Nb3 123.9(4) . .
C311 N32 Nb3 117.8(4) . .
C41 N41 Nb4 174.8(4) . .
C415 N42 C411 118.0(6) . .
C415 N42 Nb4 118.7(4) . .
C411 N42 Nb4 123.2(4) . .
C701 C702 C703 123.5(16) . .
C701 C702 H702 118.2 . .
C703 C702 H702 118.2 . .
C702 C703 C703 118.6(10) . 2_656
C702 C703 H703 120.7 . .
C703 C703 H703 120.7 2_656 .
C702 C701 C701 117.6(10) . 2_656
C702 C701 H701 121.2 . .
C701 C701 H701 121.2 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C11 N11 1.439(7) .
C11 C14 1.529(9) .
C11 C12 1.538(9) .
C11 C13 1.536(8) .
C12 H12A 0.96 .
C12 H12B 0.96 .
C12 H12C 0.96 .
C13 H13A 0.96 .
C13 H13B 0.96 .
C13 H13C 0.96 .
C14 H14A 0.96 .
C14 H14B 0.96 .
C14 H14C 0.96 .
C21 N21 1.442(7) .
C21 C22 1.516(8) .
C21 C24 1.530(8) .
C21 C23 1.534(9) .
C22 H22A 0.96 .
C22 H22B 0.96 .
C22 H22C 0.96 .
C23 H23A 0.96 .
C23 H23B 0.96 .
C23 H23C 0.96 .
C24 H24A 0.96 .
C24 H24B 0.96 .
C24 H24C 0.96 .
C31 N31 1.460(7) .
C31 C34 1.526(8) .
C31 C33 1.527(8) .
C31 C32 1.535(8) .
C32 H32A 0.96 .
C32 H32B 0.96 .
C32 H32C 0.96 .
C33 H33A 0.96 .
C33 H33B 0.96 .
C33 H33C 0.96 .
C34 H34A 0.96 .
C34 H34B 0.96 .
C34 H34C 0.96 .
C41 N41 1.445(8) .
C41 C43 1.531(9) .
C41 C42 1.536(9) .
C41 C44 1.540(10) .
C42 H42A 0.96 .
C42 H42B 0.96 .
C42 H42C 0.96 .
C43 H43A 0.96 .
C43 H43B 0.96 .
C43 H43C 0.96 .
C44 H44A 0.96 .
C44 H44B 0.96 .
C44 H44C 0.96 .
C111 N12 1.339(7) .
C111 C112 1.374(9) .
C111 H111 0.93 .
C112 C113 1.376(9) .
C112 H112 0.93 .
C113 C114 1.363(9) .
C113 H113 0.93 .
C114 C115 1.389(8) .
C114 H114 0.93 .
C115 N12 1.335(7) .
C115 H115 0.93 .
C211 N22 1.333(8) .
C211 C212 1.368(9) .
C211 H211 0.93 .
C212 C213 1.344(10) .
C212 H212 0.93 .
C213 C214 1.379(10) .
C213 H213 0.93 .
C214 C215 1.394(9) .
C214 H214 0.93 .
C215 N22 1.326(7) .
C215 H215 0.93 .
C311 N32 1.336(8) .
C311 C312 1.395(9) .
C311 H311 0.93 .
C312 C313 1.363(10) .
C312 H312 0.93 .
C313 C314 1.368(11) .
C313 H313 0.93 .
C314 C315 1.394(9) .
C314 H314 0.93 .
C315 N32 1.330(8) .
C315 H315 0.93 .
C411 N42 1.347(8) .
C411 C412 1.385(9) .
C411 H411 0.93 .
C412 C413 1.356(10) .
C412 H412 0.93 .
C413 C414 1.375(10) .
C413 H413 0.93 .
C414 C415 1.382(9) .
C414 H414 0.93 .
C415 N42 1.329(8) .
C415 H415 0.93 .
C501 C502 1.39 .
C501 C506 1.39 .
C501 H501 0.93 .
C502 C503 1.39 .
C502 H502 0.93 .
C503 C504 1.39 .
C503 H503 0.93 .
C504 C505 1.39 .
C504 H504 0.93 .
C505 C506 1.39 .
C505 H505 0.93 .
C506 H506 0.93 .
C601 C602 1.39 .
C601 C606 1.39 .
C601 H601 0.93 .
C602 C603 1.39 .
C602 H602 0.93 .
C603 C604 1.39 .
C603 H603 0.93 .
C604 C605 1.39 .
C604 H604 0.93 .
C605 C606 1.39 .
C605 H605 0.93 .
C606 H606 0.93 .
Nb1 N11 1.751(5) .
Nb1 N12 2.352(5) .
Nb1 S4 2.4191(16) .
Nb1 Cl1 2.4227(16) .
Nb1 S2 2.5070(16) .
Nb1 S1 2.8022(16) .
Nb2 N21 1.749(5) .
Nb2 N22 2.353(5) .
Nb2 S3 2.4051(16) .
Nb2 Cl2 2.4288(17) .
Nb2 S1 2.5114(16) .
Nb2 S2 2.8490(15) .
Nb3 N31 1.753(5) .
Nb3 N32 2.362(5) .
Nb3 S2 2.4033(17) .
Nb3 Cl3 2.4295(16) .
Nb3 S3 2.5176(16) .
Nb3 S4 2.8198(17) .
Nb4 N41 1.749(5) .
Nb4 N42 2.366(5) .
Nb4 Cl4 2.4240(16) .
Nb4 S1 2.4283(16) .
Nb4 S4 2.5035(16) .
Nb4 S3 2.8114(17) .
C702 C701 1.33(2) .
C702 C703 1.337(17) .
C702 H702 0.93 .
C703 C703 1.35(2) 2_656
C703 H703 0.93 .
C701 C701 1.40(4) 2_656
C701 H701 0.93 .
