#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:08:57 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232195 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/71/4347166.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_4347166
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 Cl1 N6 Nb4 S4, C5 H5'
_chemical_formula_sum            'C41 H61 Cl N6 Nb4 S4'
_chemical_formula_weight         1173.28
_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                 102.631(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.814(3)
_cell_length_b                   17.643(3)
_cell_length_c                   23.430(2)
_cell_measurement_reflns_used    97
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     6378.9(17)
_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    'SHELXS-2013/1 (Sheldrick, 2008)'
_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 0.998
_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  0.0781
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53181
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.041
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     290
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0658
_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)+(0.1066P)²+33.8496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.205
_reflns_Friedel_coverage         0
_reflns_number_gt                5061
_reflns_number_total             7328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02816_si_001.cif
_cod_data_source_block           11
_cod_original_cell_volume        6379.2(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C41 H61 Cl1 N6 Nb4 S4'
_cod_database_code               4347166
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C21 C 0.6255(5) 0.5282(4) 0.4353(3) 0.0565(18) Uani 1 1 d . . . . .
C22 C 0.5817(8) 0.4521(5) 0.4285(4) 0.093(3) Uani 1 1 d . . . . .
H22A H 0.6055 0.4206 0.4627 0.139 Uiso 1 1 calc R U . . .
H22B H 0.5919 0.4272 0.3932 0.139 Uiso 1 1 calc R U . . .
H22C H 0.5193 0.4588 0.4251 0.139 Uiso 1 1 calc R U . . .
C23 C 0.7223(6) 0.5170(7) 0.4458(4) 0.100(4) Uani 1 1 d . . . . .
H23A H 0.751 0.5666 0.4488 0.15 Uiso 1 1 calc R U . . .
H23B H 0.7363 0.4884 0.4132 0.15 Uiso 1 1 calc R U . . .
H23C H 0.7424 0.4889 0.4823 0.15 Uiso 1 1 calc R U . . .
C24 C 0.6032(6) 0.5726(5) 0.4850(3) 0.076(3) Uani 1 1 d . . . . .
H24A H 0.6213 0.5439 0.5215 0.113 Uiso 1 1 calc R U . . .
H24B H 0.5405 0.5812 0.4771 0.113 Uiso 1 1 calc R U . . .
H24C H 0.6334 0.6214 0.4887 0.113 Uiso 1 1 calc R U . . .
C41 C 0.8203(5) 0.7879(5) 0.2144(3) 0.0597(19) Uani 1 1 d . . . . .
C42 C 0.8803(7) 0.7933(7) 0.2754(5) 0.098(3) Uani 1 1 d . . . . .
H42A H 0.9323 0.8222 0.273 0.148 Uiso 1 1 calc R U . . .
H42B H 0.897 0.7421 0.29 0.148 Uiso 1 1 calc R U . . .
H42C H 0.8498 0.8188 0.3021 0.148 Uiso 1 1 calc R U . . .
C43 C 0.7671(7) 0.8582(5) 0.2014(5) 0.088(3) Uani 1 1 d . . . . .
H43A H 0.7338 0.8657 0.2316 0.132 Uiso 1 1 calc R U . . .
H43B H 0.7273 0.8532 0.1632 0.132 Uiso 1 1 calc R U . . .
H43C H 0.8053 0.9018 0.2009 0.132 Uiso 1 1 calc R U . . .
C44 C 0.8733(7) 0.7737(6) 0.1697(5) 0.091(3) Uani 1 1 d . . . . .
H44A H 0.9132 0.8161 0.1695 0.137 Uiso 1 1 calc R U . . .
H44B H 0.8348 0.7688 0.131 0.137 Uiso 1 1 calc R U . . .
H44C H 0.9066 0.7268 0.1794 0.137 Uiso 1 1 calc R U . . .
C51 C 0.6617(8) 0.5153(5) 0.1573(4) 0.089(3) Uani 1 1 d . . . . .
H51 H 0.6247 0.4809 0.1713 0.106 Uiso 1 1 calc R U . . .
C52 C 0.7518(8) 0.5191(6) 0.1748(4) 0.084(3) Uani 1 1 d . . . . .
H52 H 0.7867 0.4868 0.2028 0.101 Uiso 1 1 calc R U . . .
C53 C 0.7809(6) 0.5745(6) 0.1467(5) 0.080(3) Uani 1 1 d . . . . .
H53 H 0.8398 0.5893 0.1512 0.097 Uiso 1 1 calc R U . . .
C54 C 0.7103(8) 0.6076(5) 0.1091(4) 0.076(3) Uani 1 1 d . . . . .
H54 H 0.7135 0.6486 0.0834 0.091 Uiso 1 1 calc R U . . .
C55 C 0.6362(6) 0.5725(6) 0.1147(4) 0.074(3) Uani 1 1 d . . . . .
H55 H 0.5789 0.5841 0.0942 0.088 Uiso 1 1 calc R U . . .
N2 N 0.5963(3) 0.5695(3) 0.3806(2) 0.0447(12) Uani 1 1 d . . . . .
N4 N 0.7624(3) 0.7242(3) 0.2147(2) 0.0471(13) Uani 1 1 d . . . . .
Nb1 Nb 0.58109(3) 0.61395(3) 0.31186(2) 0.03743(18) Uani 1 1 d . . . . .
Nb2 Nb 0.69869(4) 0.64066(3) 0.20605(2) 0.04038(19) Uani 1 1 d . . . . .
S1 S 0.56076(9) 0.69333(9) 0.20480(6) 0.0385(3) Uani 1 1 d . . . . .
Cl1 Cl 0.5 0.51731(12) 0.25 0.0457(5) Uani 1 2 d S T P A .
S4 S 0.72673(10) 0.58713(10) 0.30223(7) 0.0474(4) Uani 1 1 d . . . . .
N1 N 0.6221(5) 0.7311(4) 0.3590(3) 0.035(3) Uani 0.619(9) 1 d G . P A 1
C11 C 0.5851(4) 0.7543(4) 0.4047(3) 0.055(3) Uani 0.619(9) 1 d G . P A 1
H11 H 0.5418 0.724 0.416 0.066 Uiso 0.619(9) 1 calc R U P A 1
C12 C 0.6113(5) 0.8217(4) 0.4339(3) 0.061(3) Uani 0.619(9) 1 d G . P A 1
H12 H 0.5859 0.8376 0.4651 0.074 Uiso 0.619(9) 1 calc R U P A 1
C13 C 0.6745(6) 0.8660(4) 0.4174(4) 0.061(4) Uani 0.619(9) 1 d G . P A 1
H13 H 0.6925 0.9121 0.4373 0.073 Uiso 0.619(9) 1 calc R U P A 1
C14 C 0.7116(6) 0.8429(5) 0.3717(4) 0.068(4) Uani 0.619(9) 1 d G . P A 1
H14 H 0.7549 0.8731 0.3604 0.081 Uiso 0.619(9) 1 calc R U P A 1
C15 C 0.6854(5) 0.7754(5) 0.3425(3) 0.055(3) Uani 0.619(9) 1 d G . P A 1
H15 H 0.7108 0.7595 0.3113 0.066 Uiso 0.619(9) 1 calc R U P A 1
N1A N 0.6437(9) 0.7300(6) 0.3457(6) 0.047(5) Uani 0.381(9) 1 d G . P A 2
C11A C 0.6125(8) 0.8001(8) 0.3234(5) 0.065(6) Uani 0.381(9) 1 d G . P A 2
H11A H 0.5672 0.8028 0.2893 0.078 Uiso 0.381(9) 1 calc R U P A 2
C12A C 0.6475(10) 0.8663(6) 0.3510(7) 0.068(6) Uani 0.381(9) 1 d G . P A 2
H12A H 0.6262 0.9142 0.3358 0.081 Uiso 0.381(9) 1 calc R U P A 2
C13A C 0.7138(11) 0.8623(8) 0.4009(7) 0.077(9) Uani 0.381(9) 1 d G . P A 2
H13A H 0.7377 0.9076 0.4198 0.092 Uiso 0.381(9) 1 calc R U P A 2
C14A C 0.7450(10) 0.7922(11) 0.4231(6) 0.113(12) Uani 0.381(9) 1 d G . P A 2
H14A H 0.7902 0.7896 0.4572 0.135 Uiso 0.381(9) 1 calc R U P A 2
C15A C 0.7099(10) 0.7261(8) 0.3955(7) 0.077(7) Uani 0.381(9) 1 d G . P A 2
H15A H 0.7312 0.6782 0.4107 0.092 Uiso 0.381(9) 1 calc R U P A 2
C1 C 0.4588(14) 0.7590(10) 0.5316(10) 0.049(6) Uiso 0.25 1 d G . P B 1
H1 H 0.4419 0.7081 0.5219 0.058 Uiso 0.25 1 calc R U P B 1
C2 C 0.4121(13) 0.8250(13) 0.5087(11) 0.081(13) Uiso 0.25 1 d G . P B 1
H2 H 0.3584 0.826 0.481 0.097 Uiso 0.25 1 calc R U P B 1
C3 C 0.4597(16) 0.8892(10) 0.5345(11) 0.068(8) Uiso 0.25 1 d G . P B 1
H3 H 0.4435 0.9407 0.5271 0.082 Uiso 0.25 1 calc R U P B 1
C4 C 0.5359(14) 0.8629(13) 0.5734(10) 0.075(9) Uiso 0.25 1 d G . P B 1
H4 H 0.5796 0.8937 0.5965 0.09 Uiso 0.25 1 calc R U P B 1
C5 C 0.5354(13) 0.7824(13) 0.5716(10) 0.084(11) Uiso 0.25 1 d G . P B 1
H5 H 0.5786 0.75 0.5933 0.101 Uiso 0.25 1 calc R U P B 1
C1A C 0.498(2) 0.798(3) 0.5222(12) 0.44(10) Uiso 0.25 1 d G . P C 2
H1A H 0.5443 0.7956 0.5554 0.524 Uiso 0.25 1 calc R U P C 2
C2A C 0.411(3) 0.818(3) 0.5225(12) 0.14(3) Uiso 0.25 1 d G . P C 2
H2A H 0.3889 0.8308 0.5559 0.166 Uiso 0.25 1 calc R U P C 2
C3A C 0.3617(16) 0.8146(18) 0.4640(14) 0.081(10) Uiso 0.25 1 d G . P C 2
H3A H 0.3016 0.8251 0.4514 0.097 Uiso 0.25 1 calc R U P C 2
C4A C 0.4184(17) 0.7929(18) 0.4275(10) 0.082(10) Uiso 0.25 1 d G . P C 2
H4A H 0.4029 0.7864 0.3863 0.099 Uiso 0.25 1 calc R U P C 2
C5A C 0.5024(15) 0.7827(19) 0.4635(14) 0.076(9) Uiso 0.25 1 d G . P C 2
H5A H 0.5529 0.7682 0.4506 0.091 Uiso 0.25 1 calc R U P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 -1 0.057
3 0 1 0.086
1 0 -3 0.074
-1 0 2 0.038
0 -9 1 0.077
0 1 0 0.062
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
N2 C21 C22 107.6(6) . .
N2 C21 C24 109.6(6) . .
C22 C21 C24 111.5(8) . .
N2 C21 C23 108.9(6) . .
C22 C21 C23 109.2(8) . .
C24 C21 C23 109.9(7) . .
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 . .
N4 C41 C43 108.5(6) . .
N4 C41 C44 108.8(7) . .
C43 C41 C44 111.9(8) . .
N4 C41 C42 107.8(7) . .
C43 C41 C42 110.2(8) . .
C44 C41 C42 109.6(8) . .
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 . .
C52 C51 C55 106.7(9) . .
C52 C51 Nb2 72.6(5) . .
C55 C51 Nb2 72.1(5) . .
C52 C51 H51 126.6 . .
C55 C51 H51 126.6 . .
Nb2 C51 H51 120.5 . .
C53 C52 C51 109.6(9) . .
C53 C52 Nb2 71.5(5) . .
C51 C52 Nb2 74.8(5) . .
C53 C52 H52 125.2 . .
C51 C52 H52 125.2 . .
Nb2 C52 H52 120.1 . .
C52 C53 C54 107.9(9) . .
C52 C53 Nb2 77.1(5) . .
C54 C53 Nb2 72.6(5) . .
C52 C53 H53 126 . .
C54 C53 H53 126 . .
Nb2 C53 H53 116.3 . .
C55 C54 C53 109.8(9) . .
C55 C54 Nb2 76.8(5) . .
C53 C54 Nb2 73.7(5) . .
C55 C54 H54 125.1 . .
C53 C54 H54 125.1 . .
Nb2 C54 H54 116.3 . .
C54 C55 C51 105.9(8) . .
C54 C55 Nb2 70.8(5) . .
C51 C55 Nb2 74.8(5) . .
C54 C55 H55 127 . .
C51 C55 H55 127 . .
Nb2 C55 H55 119.4 . .
C21 N2 Nb1 168.6(5) . .
C41 N4 Nb2 171.1(5) . .
N2 Nb1 N1A 96.7(4) . .
N2 Nb1 N1 89.6(3) . .
N2 Nb1 S4 93.20(18) . .
N1A Nb1 S4 82.0(3) . .
N1 Nb1 S4 92.58(19) . .
N2 Nb1 Cl1 100.55(18) . .
N1A Nb1 Cl1 162.1(4) . .
N1 Nb1 Cl1 162.12(19) . .
S4 Nb1 Cl1 101.42(5) . .
N2 Nb1 S1 108.55(18) . 2_655
N1A Nb1 S1 82.3(3) . 2_655
N1 Nb1 S1 74.89(18) . 2_655
S4 Nb1 S1 154.49(6) . 2_655
Cl1 Nb1 S1 87.86(5) . 2_655
N2 Nb1 S1 176.60(19) . .
N1A Nb1 S1 79.9(4) . .
N1 Nb1 S1 87.04(19) . .
S4 Nb1 S1 86.55(5) . .
Cl1 Nb1 S1 82.82(5) . .
S1 Nb1 S1 70.93(6) 2_655 .
N4 Nb2 S1 100.07(18) . .
N4 Nb2 C54 98.7(3) . .
S1 Nb2 C54 110.3(3) . .
N4 Nb2 S4 103.69(19) . .
S1 Nb2 S4 98.47(6) . .
C54 Nb2 S4 139.6(2) . .
N4 Nb2 C53 95.9(3) . .
S1 Nb2 C53 142.9(3) . .
C54 Nb2 C53 33.7(3) . .
S4 Nb2 C53 109.9(3) . .
N4 Nb2 C55 127.9(3) . .
S1 Nb2 C55 89.3(2) . .
C54 Nb2 C55 32.4(3) . .
S4 Nb2 C55 125.6(3) . .
C53 Nb2 C55 54.9(3) . .
N4 Nb2 C52 122.3(4) . .
S1 Nb2 C52 135.2(3) . .
C54 Nb2 C52 53.5(3) . .
S4 Nb2 C52 86.1(2) . .
C53 Nb2 C52 31.3(3) . .
C55 Nb2 C52 54.4(3) . .
N4 Nb2 C51 149.2(3) . .
S1 Nb2 C51 102.7(3) . .
C54 Nb2 C51 53.8(3) . .
S4 Nb2 C51 93.3(3) . .
C53 Nb2 C51 53.7(3) . .
C55 Nb2 C51 33.1(3) . .
C52 Nb2 C51 32.6(3) . .
Nb2 S1 Nb1 123.59(7) . 2_655
Nb2 S1 Nb1 82.46(5) . .
Nb1 S1 Nb1 78.09(5) 2_655 .
Nb1 Cl1 Nb1 90.24(8) 2_655 .
Nb2 S4 Nb1 91.52(6) . .
C11 N1 C15 120 . .
C11 N1 Nb1 119.9(4) . .
C15 N1 Nb1 120.1(4) . .
C12 C11 N1 120 . .
C12 C11 H11 120 . .
N1 C11 H11 120 . .
C13 C12 C11 120 . .
C13 C12 H12 120 . .
C11 C12 H12 120 . .
C14 C13 C12 120 . .
C14 C13 H13 120 . .
C12 C13 H13 120 . .
C15 C14 C13 120 . .
C15 C14 H14 120 . .
C13 C14 H14 120 . .
C14 C15 N1 120 . .
C14 C15 H15 120 . .
N1 C15 H15 120 . .
C11A N1A C15A 120 . .
C11A N1A Nb1 124.3(8) . .
C15A N1A Nb1 115.3(8) . .
C12A C11A N1A 120 . .
C12A C11A H11A 120 . .
N1A C11A H11A 120 . .
C13A C12A C11A 120 . .
C13A C12A H12A 120 . .
C11A C12A H12A 120 . .
C12A C13A C14A 120 . .
C12A C13A H13A 120 . .
C14A C13A H13A 120 . .
C13A C14A C15A 120 . .
C13A C14A H14A 120 . .
C15A C14A H14A 120 . .
C14A C15A N1A 120 . .
C14A C15A H15A 120 . .
N1A C15A H15A 120 . .
C2 C1 C5 108 . .
C2 C1 H1 126 . .
C5 C1 H1 126 . .
C3 C2 C1 108 . .
C3 C2 H2 126 . .
C1 C2 H2 126 . .
C2 C3 C4 108 . .
C2 C3 H3 126 . .
C4 C3 H3 126 . .
C5 C4 C3 108 . .
C5 C4 H4 126 . .
C3 C4 H4 126 . .
C4 C5 C1 108 . .
C4 C5 H5 126 . .
C1 C5 H5 126 . .
C2A C1A C5A 108 . .
C2A C1A H1A 126 . .
C5A C1A H1A 126 . .
C3A C2A C1A 108 . .
C3A C2A H2A 126 . .
C1A C2A H2A 126 . .
C4A C3A C2A 108 . .
C4A C3A H3A 126 . .
C2A C3A H3A 126 . .
C3A C4A C5A 108 . .
C3A C4A H4A 126 . .
C5A C4A H4A 126 . .
C4A C5A C1A 108 . .
C4A C5A H5A 126 . .
C1A C5A H5A 126 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C21 N2 1.459(8) .
C21 C22 1.502(13) .
C21 C24 1.507(10) .
C21 C23 1.509(12) .
C22 H22A 0.98 .
C22 H22B 0.98 .
C22 H22C 0.98 .
C23 H23A 0.98 .
C23 H23B 0.98 .
C23 H23C 0.98 .
C24 H24A 0.98 .
C24 H24B 0.98 .
C24 H24C 0.98 .
C41 N4 1.452(9) .
C41 C43 1.492(12) .
C41 C44 1.499(12) .
C41 C42 1.534(12) .
C42 H42A 0.98 .
C42 H42B 0.98 .
C42 H42C 0.98 .
C43 H43A 0.98 .
C43 H43B 0.98 .
C43 H43C 0.98 .
C44 H44A 0.98 .
C44 H44B 0.98 .
C44 H44C 0.98 .
C51 C52 1.395(14) .
C51 C55 1.416(14) .
C51 Nb2 2.500(8) .
C51 H51 0.95 .
C52 C53 1.318(14) .
C52 Nb2 2.471(9) .
C52 H52 0.95 .
C53 C54 1.390(13) .
C53 Nb2 2.404(8) .
C53 H53 0.95 .
C54 C55 1.356(13) .
C54 Nb2 2.391(8) .
C54 H54 0.95 .
C55 Nb2 2.466(7) .
C55 H55 0.95 .
N2 Nb1 1.760(5) .
N4 Nb2 1.772(6) .
Nb1 N1A 2.336(10) .
Nb1 N1 2.367(6) .
Nb1 S4 2.4098(18) .
Nb1 Cl1 2.4166(17) .
Nb1 S1 2.6006(16) 2_655
Nb1 S1 2.8291(16) .
Nb2 S1 2.3652(16) .
Nb2 S4 2.3937(17) .
S1 Nb1 2.6005(16) 2_655
Cl1 Nb1 2.4165(17) 2_655
N1 C11 1.39 .
N1 C15 1.39 .
C11 C12 1.39 .
C11 H11 0.95 .
C12 C13 1.39 .
C12 H12 0.95 .
C13 C14 1.39 .
C13 H13 0.95 .
C14 C15 1.39 .
C14 H14 0.95 .
C15 H15 0.95 .
N1A C11A 1.39 .
N1A C15A 1.39 .
C11A C12A 1.39 .
C11A H11A 0.95 .
C12A C13A 1.39 .
C12A H12A 0.95 .
C13A C14A 1.39 .
C13A H13A 0.95 .
C14A C15A 1.39 .
C14A H14A 0.95 .
C15A H15A 0.95 .
C1 C2 1.42 .
C1 C5 1.42 .
C1 H1 0.95 .
C2 C3 1.42 .
C2 H2 0.95 .
C3 C4 1.42 .
C3 H3 0.95 .
C4 C5 1.42 .
C4 H4 0.95 .
C5 H5 0.95 .
C1A C2A 1.42 .
C1A C5A 1.42 .
C1A H1A 0.95 .
C2A C3A 1.42 .
C2A H2A 0.95 .
C3A C4A 1.42 .
C3A H3A 0.95 .
C4A C5A 1.42 .
C4A H4A 0.95 .
C5A H5A 0.95 .
