#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:33:48 +0100 (jue 07 de nov de 2019) $
#$Revision: 224284 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/91/7049163.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_7049163
loop_
_publ_author_name
'Kar, Sourav'
'Bairagi, Subhash'
'Saha, Koushik'
'Raghavendra, Beesam'
'Ghosh, Sundargopal'
_publ_section_title
;
 Chalcogen stabilized trimetallic clusters: synthesis, structures, and
 bonding of [(Cp*M)₃(E)₆₊ₘ(BH)ₙ] (M = Nb
 or Ta; E = S or Se; m = 0 or 1 or 2; n = 0 or 1).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4203
_journal_page_last               4210
_journal_paper_doi               10.1039/c8dt05061a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '(C30 H45 B Nb3 S7) + 0.5(CH2Cl2)'
_chemical_formula_sum            'C30.5 H46 B Cl Nb3 S7'
_chemical_formula_weight         962.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-02-05 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7274(5)
_cell_length_b                   16.7472(5)
_cell_length_c                   15.8653(4)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.8
_cell_volume                     4178.8(2)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17535
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.771
_diffrn_reflns_theta_min         1.776
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 1772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0516P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                4151
_reflns_number_total             4459
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt05061a2.cif
_cod_data_source_block           NBSH
_cod_depositor_comments
'Adding full bibliography for 7049161--7049163.cif.'
_cod_original_formula_sum        'C30.50 H46 B Cl Nb3 S7'
_cod_database_code               7049163
_shelx_shelxl_version_number     2017/1
_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_min   0.746
_shelx_estimated_absorpt_t_max   0.826
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
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
S5 S 0.0697(2) 0.4844(2) 0.3092(2) 0.0374(7) Uani 0.5 1 d . . P . .
B1 B -0.0295(8) 0.4261(9) 0.3335(8) 0.029(3) Uani 0.5 1 d . . P . .
C1 C 0.2159(4) 0.2782(5) 0.3653(5) 0.0423(17) Uani 1 1 d . . . . .
C2 C 0.1771(4) 0.2054(5) 0.3870(4) 0.0420(17) Uani 1 1 d . . . . .
C3 C 0.1931(5) 0.1505(5) 0.3199(6) 0.051(2) Uani 1 1 d . . . . .
C4 C 0.2393(4) 0.1909(5) 0.2579(5) 0.0479(19) Uani 1 1 d . . . . .
C5 C 0.2538(4) 0.2687(5) 0.2850(4) 0.0453(19) Uani 1 1 d . . . . .
C6 C 0.3090(5) 0.3296(7) 0.2428(7) 0.086(3) Uani 1 1 d . . . . .
H6A H 0.303322 0.379940 0.271296 0.130 Uiso 1 1 calc R U . . .
H6B H 0.291909 0.335491 0.185074 0.130 Uiso 1 1 calc R U . . .
H6C H 0.367253 0.312557 0.245066 0.130 Uiso 1 1 calc R U . . .
C7 C 0.2232(6) 0.3508(6) 0.4215(7) 0.076(3) Uani 1 1 d . . . . .
H7A H 0.174756 0.353359 0.458231 0.114 Uiso 1 1 calc R U . . .
H7B H 0.225196 0.398109 0.387293 0.114 Uiso 1 1 calc R U . . .
H7C H 0.274148 0.347193 0.454525 0.114 Uiso 1 1 calc R U . . .
C8 C 0.1365(6) 0.1895(8) 0.4704(6) 0.081(3) Uani 1 1 d . . . . .
H8A H 0.179282 0.173593 0.510173 0.121 Uiso 1 1 calc R U . . .
H8B H 0.095337 0.147528 0.464545 0.121 Uiso 1 1 calc R U . . .
H8C H 0.108892 0.237067 0.490038 0.121 Uiso 1 1 calc R U . . .
C9 C 0.1746(7) 0.0625(5) 0.3230(8) 0.093(4) Uani 1 1 d . . . . .
H9A H 0.181853 0.039926 0.267820 0.139 Uiso 1 1 calc R U . . .
H9B H 0.117198 0.054159 0.341508 0.139 Uiso 1 1 calc R U . . .
H9C H 0.213083 0.037085 0.361609 0.139 Uiso 1 1 calc R U . . .
C10 C 0.2778(7) 0.1494(8) 0.1834(6) 0.094(4) Uani 1 1 d . . . . .
H10A H 0.287607 0.187411 0.139144 0.141 Uiso 1 1 calc R U . . .
H10B H 0.239560 0.108751 0.163653 0.141 Uiso 1 1 calc R U . . .
H10C H 0.330720 0.125382 0.199559 0.141 Uiso 1 1 calc R U . . .
C11 C 0.0455(4) 0.3700(4) -0.0257(4) 0.0314(14) Uani 1 1 d . . . . .
C12 C 0.0725(4) 0.4367(4) 0.0215(4) 0.0300(14) Uani 1 1 d . . . . .
C13 C 0.000000 0.4798(5) 0.0493(5) 0.0296(19) Uani 1 2 d S T P . .
C14 C 0.000000 0.5574(6) 0.0954(7) 0.051(3) Uani 1 2 d S T P . .
H14A H -0.037181 0.594306 0.067354 0.076 Uiso 0.5 1 calc R U P . .
H14B H 0.056631 0.578794 0.096461 0.076 Uiso 0.5 1 calc R U P . .
H14C H -0.019450 0.549143 0.152101 0.076 Uiso 0.5 1 calc R U P . .
C15 C 0.1639(4) 0.4630(5) 0.0315(5) 0.050(2) Uani 1 1 d . . . . .
H15A H 0.200175 0.416951 0.033001 0.075 Uiso 1 1 calc R U . . .
H15B H 0.169939 0.492496 0.083062 0.075 Uiso 1 1 calc R U . . .
H15C H 0.179652 0.496365 -0.015194 0.075 Uiso 1 1 calc R U . . .
C16 C 0.0992(5) 0.3174(5) -0.0779(5) 0.052(2) Uani 1 1 d . . . . .
H16A H 0.114422 0.344568 -0.128988 0.079 Uiso 1 1 calc R U . . .
H16B H 0.068381 0.269593 -0.091344 0.079 Uiso 1 1 calc R U . . .
H16C H 0.149844 0.303764 -0.047284 0.079 Uiso 1 1 calc R U . . .
Nb1 Nb 0.09979(3) 0.25663(3) 0.26498(4) 0.02474(14) Uani 1 1 d . . . . .
Nb2 Nb 0.000000 0.34860(4) 0.12063(4) 0.02067(17) Uani 1 2 d S T P . .
S1 S 0.11492(10) 0.25594(9) 0.11547(11) 0.0333(4) Uani 1 1 d . . . . .
S2 S 0.10408(11) 0.40466(11) 0.22720(11) 0.0396(4) Uani 1 1 d . . . . .
S3 S 0.000000 0.31967(15) 0.37122(13) 0.0294(5) Uani 1 2 d S T P . .
S4 S 0.000000 0.15060(13) 0.27279(17) 0.0347(5) Uani 1 2 d S T P . .
Cl1 Cl 0.000000 -0.0799(11) 0.4504(10) 0.120(6) Uani 0.364(6) 2 d DS TU P A 1
Cl2 Cl -0.0821(12) -0.0058(10) 0.5855(10) 0.110(6) Uani 0.182(3) 1 d D U P A 1
C17 C 0.000000 -0.0711(19) 0.5609(17) 0.078(8) Uani 0.364(6) 2 d DS TU P A 1
Cl1' Cl 0.000000 0.0281(16) 0.609(2) 0.103(9) Uani 0.136(6) 2 d DS TU P B 2
Cl2' Cl -0.043(3) -0.063(2) 0.468(2) 0.077(8) Uani 0.068(3) 1 d D U P B 2
C17' C 0.000000 -0.068(3) 0.569(3) 0.083(10) Uani 0.136(6) 2 d DS TU P B 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
Nb Nb -2.0727 0.6215 '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_
_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
B1 S5 S2 90.7(4) . .
S5 B1 S3 110.0(7) . .
S5 B1 S2 113.0(6) . 4
S3 B1 S2 103.0(6) . 4
C2 C1 C5 107.8(7) . .
C2 C1 C7 125.9(8) . .
C5 C1 C7 126.0(8) . .
C2 C1 Nb1 73.0(4) . .
C5 C1 Nb1 73.3(4) . .
C7 C1 Nb1 123.9(5) . .
C1 C2 C3 107.4(7) . .
C1 C2 C8 123.8(8) . .
C3 C2 C8 128.4(8) . .
C1 C2 Nb1 73.6(4) . .
C3 C2 Nb1 73.9(4) . .
C8 C2 Nb1 123.6(5) . .
C4 C3 C2 107.8(7) . .
C4 C3 C9 126.7(9) . .
C2 C3 C9 124.9(9) . .
C4 C3 Nb1 73.2(4) . .
C2 C3 Nb1 72.2(4) . .
C9 C3 Nb1 127.2(5) . .
C5 C4 C3 108.7(6) . .
C5 C4 C10 127.8(9) . .
C3 C4 C10 122.7(9) . .
C5 C4 Nb1 73.3(4) . .
C3 C4 Nb1 73.7(4) . .
C10 C4 Nb1 127.2(5) . .
C4 C5 C1 108.3(7) . .
C4 C5 C6 126.5(8) . .
C1 C5 C6 124.8(8) . .
C4 C5 Nb1 73.8(4) . .
C1 C5 Nb1 73.1(4) . .
C6 C5 Nb1 124.8(5) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C1 C7 H7A 109.5 . .
C1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C2 C8 H8A 109.5 . .
C2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C3 C9 H9A 109.5 . .
C3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C4 C10 H10A 109.5 . .
C4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 C11 107.5(4) . 4
C12 C11 C16 126.8(6) . .
C11 C11 C16 125.0(4) 4 .
C12 C11 Nb2 72.6(3) . .
C11 C11 Nb2 73.07(14) 4 .
C16 C11 Nb2 127.6(5) . .
C11 C12 C13 109.0(5) . .
C11 C12 C15 125.0(6) . .
C13 C12 C15 125.7(7) . .
C11 C12 Nb2 73.9(3) . .
C13 C12 Nb2 74.4(4) . .
C15 C12 Nb2 123.5(4) . .
C12 C13 C12 106.9(8) 4 .
C12 C13 C14 126.5(4) 4 .
C12 C13 C14 126.5(4) . .
C12 C13 Nb2 72.0(4) 4 .
C12 C13 Nb2 72.0(4) . .
C14 C13 Nb2 123.4(6) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C14 H14A 109.5(19) . 4
H14A C14 H14A 75.1 . 4
H14B C14 H14A 37.2 . 4
H14C C14 H14A 136.2 . 4
C13 C14 H14B 109.5(7) . 4
H14A C14 H14B 37.2 . 4
H14B C14 H14B 136.2 . 4
H14C C14 H14B 75.1 . 4
H14A C14 H14B 109.5 4 4
C13 C14 H14C 109.5(13) . 4
H14A C14 H14C 136.2 . 4
H14B C14 H14C 75.1 . 4
H14C C14 H14C 37.2 . 4
H14A C14 H14C 109.5 4 4
H14B C14 H14C 109.5 4 4
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C11 C16 H16A 109.5 . .
C11 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C11 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
S4 Nb1 S1 96.56(8) . .
S4 Nb1 C2 91.41(19) . .
S1 Nb1 C2 137.52(17) . .
S4 Nb1 C1 124.7(2) . .
S1 Nb1 C1 124.96(19) . .
C2 Nb1 C1 33.4(3) . .
S4 Nb1 C5 135.1(2) . .
S1 Nb1 C5 91.76(17) . .
C2 Nb1 C5 55.6(2) . .
C1 Nb1 C5 33.6(2) . .
S4 Nb1 C4 104.9(2) . .
S1 Nb1 C4 82.12(17) . .
C2 Nb1 C4 55.6(2) . .
C1 Nb1 C4 55.2(2) . .
C5 Nb1 C4 32.9(3) . .
S4 Nb1 C3 80.54(19) . .
S1 Nb1 C3 106.8(2) . .
C2 Nb1 C3 33.8(3) . .
C1 Nb1 C3 55.4(3) . .
C5 Nb1 C3 54.9(3) . .
C4 Nb1 C3 33.0(3) . .
S4 Nb1 S3 82.38(7) . .
S1 Nb1 S3 136.54(6) . .
C2 Nb1 S3 85.83(17) . .
C1 Nb1 S3 88.18(19) . .
C5 Nb1 S3 119.44(19) . .
C4 Nb1 S3 140.39(17) . .
C3 Nb1 S3 115.7(2) . .
S4 Nb1 S2 139.18(6) . .
S1 Nb1 S2 76.61(6) . .
C2 Nb1 S2 121.0(2) . .
C1 Nb1 S2 89.43(19) . .
C5 Nb1 S2 85.6(2) . .
C4 Nb1 S2 113.6(2) . .
C3 Nb1 S2 140.20(19) . .
S3 Nb1 S2 76.57(7) . .
S4 Nb1 Nb1 48.60(4) . 4
S1 Nb1 Nb1 95.73(4) . 4
C2 Nb1 Nb1 119.85(17) . 4
C1 Nb1 Nb1 138.22(18) . 4
C5 Nb1 Nb1 171.16(19) . 4
C4 Nb1 Nb1 153.2(2) . 4
C3 Nb1 Nb1 126.5(2) . 4
S3 Nb1 Nb1 51.72(3) . 4
S2 Nb1 Nb1 91.52(4) . 4
S4 Nb1 Nb2 94.23(5) . .
S1 Nb1 Nb2 48.24(4) . .
C2 Nb1 Nb2 171.31(19) . .
C1 Nb1 Nb2 140.00(19) . .
C5 Nb1 Nb2 122.81(17) . .
C4 Nb1 Nb2 128.72(18) . .
C3 Nb1 Nb2 154.1(2) . .
S3 Nb1 Nb2 88.37(4) . .
S2 Nb1 Nb2 51.12(4) . .
Nb1 Nb1 Nb2 60.373(11) 4 .
S1 Nb2 S1 98.62(9) . 4
S1 Nb2 C12 91.00(16) . .
S1 Nb2 C12 136.54(15) 4 .
S1 Nb2 C12 136.54(15) . 4
S1 Nb2 C12 91.00(16) 4 4
C12 Nb2 C12 55.7(3) . 4
S1 Nb2 C11 80.89(15) . .
S1 Nb2 C11 106.46(16) 4 .
C12 Nb2 C11 33.5(2) . .
C12 Nb2 C11 55.81(19) 4 .
S1 Nb2 C11 106.46(16) . 4
S1 Nb2 C11 80.89(15) 4 4
C12 Nb2 C11 55.81(19) . 4
C12 Nb2 C11 33.5(2) 4 4
C11 Nb2 C11 33.9(3) . 4
S1 Nb2 C13 124.27(9) . .
S1 Nb2 C13 124.26(9) 4 .
C12 Nb2 C13 33.59(19) . .
C12 Nb2 C13 33.58(19) 4 .
C11 Nb2 C13 55.8(2) . .
C11 Nb2 C13 55.8(2) 4 .
S1 Nb2 S2 138.94(6) . 4
S1 Nb2 S2 76.96(6) 4 4
C12 Nb2 S2 120.53(17) . 4
C12 Nb2 S2 84.51(14) 4 4
C11 Nb2 S2 139.90(15) . 4
C11 Nb2 S2 112.87(15) 4 4
C13 Nb2 S2 88.64(16) . 4
S1 Nb2 S2 76.96(6) . .
S1 Nb2 S2 138.95(6) 4 .
C12 Nb2 S2 84.51(14) . .
C12 Nb2 S2 120.53(17) 4 .
C11 Nb2 S2 112.87(15) . .
C11 Nb2 S2 139.90(15) 4 .
C13 Nb2 S2 88.64(16) . .
S2 Nb2 S2 80.49(9) 4 .
S1 Nb2 Nb1 94.81(5) . 4
S1 Nb2 Nb1 48.25(4) 4 4
C12 Nb2 Nb1 171.71(16) . 4
C12 Nb2 Nb1 121.85(14) 4 4
C11 Nb2 Nb1 153.73(16) . 4
C11 Nb2 Nb1 127.50(14) 4 4
C13 Nb2 Nb1 139.61(13) . 4
S2 Nb2 Nb1 51.62(4) 4 4
S2 Nb2 Nb1 91.02(5) . 4
S1 Nb2 Nb1 48.25(4) . .
S1 Nb2 Nb1 94.81(5) 4 .
C12 Nb2 Nb1 121.85(14) . .
C12 Nb2 Nb1 171.70(16) 4 .
C11 Nb2 Nb1 127.50(14) . .
C11 Nb2 Nb1 153.73(16) 4 .
C13 Nb2 Nb1 139.61(13) . .
S2 Nb2 Nb1 91.02(5) 4 .
S2 Nb2 Nb1 51.61(4) . .
Nb1 Nb2 Nb1 59.25(2) 4 .
Nb2 S1 Nb1 83.51(5) . .
S5 S2 B1 35.2(4) . 4
S5 S2 Nb2 121.48(13) . .
B1 S2 Nb2 103.9(4) 4 .
S5 S2 Nb1 120.24(14) . .
B1 S2 Nb1 87.9(4) 4 .
Nb2 S2 Nb1 77.27(5) . .
B1 S3 B1 27.7(8) 4 .
B1 S3 Nb1 91.7(4) 4 .
B1 S3 Nb1 109.1(4) . .
B1 S3 Nb1 109.1(4) 4 4
B1 S3 Nb1 91.7(4) . 4
Nb1 S3 Nb1 76.56(6) . 4
Nb1 S4 Nb1 82.80(7) 4 .
Cl2 C17 Cl2 96(2) 4 .
Cl2 C17 Cl1 106.1(13) 4 .
Cl2 C17 Cl1 106.1(13) . .
Cl2' Cl2' C17' 67.1(17) 4 .
Cl1' C17' Cl2' 107(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S5 B1 1.880(14) .
S5 S2 1.941(4) .
B1 S3 1.937(15) .
B1 S2 2.086(13) 4
C1 C2 1.406(11) .
C1 C5 1.416(10) .
C1 C7 1.513(11) .
C1 Nb1 2.449(6) .
C2 C3 1.428(11) .
C2 C8 1.492(11) .
C2 Nb1 2.441(6) .
C3 C4 1.399(12) .
C3 C9 1.504(11) .
C3 Nb1 2.464(7) .
C4 C5 1.391(11) .
C4 C10 1.499(11) .
C4 Nb1 2.457(6) .
C5 C6 1.498(12) .
C5 Nb1 2.452(7) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.410(9) .
C11 C11 1.430(12) 4
C11 C16 1.475(9) .
C11 Nb2 2.456(6) .
C12 C13 1.419(9) .
C12 C15 1.512(8) .
C12 Nb2 2.440(6) .
C13 C14 1.492(14) .
C13 Nb2 2.471(9) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C14 H14A 0.96(9) 4
C14 H14B 0.96(3) 4
C14 H14C 0.96(6) 4
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
Nb1 S4 2.3732(16) .
Nb1 S1 2.3840(18) .
Nb1 S3 2.5336(18) .
Nb1 S2 2.5514(18) .
Nb1 Nb1 3.1390(9) 4
Nb1 Nb2 3.1750(9) .
Nb2 S1 2.3837(15) .
Nb2 S1 2.3837(15) 4
Nb2 S2 2.5337(17) 4
Nb2 S2 2.5337(17) .
Cl1 C17 1.76(2) .
Cl2 C17 1.74(2) .
Cl1' C17' 1.73(3) .
Cl2' Cl2' 1.35(9) 4
Cl2' C17' 1.74(3) .
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_4
S2 S5 B1 S3 58.1(5) . .
S2 S5 B1 S2 -56.5(6) . 4
C5 C1 C2 C3 1.3(8) . .
C7 C1 C2 C3 -173.4(7) . .
Nb1 C1 C2 C3 66.8(5) . .
C5 C1 C2 C8 174.7(6) . .
C7 C1 C2 C8 0.1(11) . .
Nb1 C1 C2 C8 -119.8(7) . .
C5 C1 C2 Nb1 -65.5(5) . .
C7 C1 C2 Nb1 119.9(7) . .
C1 C2 C3 C4 -1.4(8) . .
C8 C2 C3 C4 -174.5(7) . .
Nb1 C2 C3 C4 65.1(5) . .
C1 C2 C3 C9 170.1(7) . .
C8 C2 C3 C9 -2.9(12) . .
Nb1 C2 C3 C9 -123.3(7) . .
C1 C2 C3 Nb1 -66.6(5) . .
C8 C2 C3 Nb1 120.4(7) . .
C2 C3 C4 C5 1.1(8) . .
C9 C3 C4 C5 -170.3(7) . .
Nb1 C3 C4 C5 65.5(5) . .
C2 C3 C4 C10 171.4(7) . .
C9 C3 C4 C10 0.1(11) . .
Nb1 C3 C4 C10 -124.1(7) . .
C2 C3 C4 Nb1 -64.4(5) . .
C9 C3 C4 Nb1 124.2(8) . .
C3 C4 C5 C1 -0.3(7) . .
C10 C4 C5 C1 -170.0(7) . .
Nb1 C4 C5 C1 65.5(5) . .
C3 C4 C5 C6 172.6(7) . .
C10 C4 C5 C6 2.8(12) . .
Nb1 C4 C5 C6 -121.6(7) . .
C3 C4 C5 Nb1 -65.8(5) . .
C10 C4 C5 Nb1 124.5(8) . .
C2 C1 C5 C4 -0.6(7) . .
C7 C1 C5 C4 174.0(7) . .
Nb1 C1 C5 C4 -65.9(5) . .
C2 C1 C5 C6 -173.6(7) . .
C7 C1 C5 C6 1.0(11) . .
Nb1 C1 C5 C6 121.1(7) . .
C2 C1 C5 Nb1 65.3(5) . .
C7 C1 C5 Nb1 -120.1(7) . .
C11 C11 C12 C13 -1.5(6) 4 .
C16 C11 C12 C13 168.9(7) . .
Nb2 C11 C12 C13 -66.7(5) . .
C11 C11 C12 C15 -174.8(5) 4 .
C16 C11 C12 C15 -4.4(10) . .
Nb2 C11 C12 C15 120.0(6) . .
C11 C11 C12 Nb2 65.25(15) 4 .
C16 C11 C12 Nb2 -124.4(7) . .
C11 C12 C13 C12 2.3(9) . 4
C15 C12 C13 C12 175.6(4) . 4
Nb2 C12 C13 C12 -64.0(5) . 4
C11 C12 C13 C14 -175.0(8) . .
C15 C12 C13 C14 -1.7(12) . .
Nb2 C12 C13 C14 118.6(9) . .
C11 C12 C13 Nb2 66.3(4) . .
C15 C12 C13 Nb2 -120.4(6) . .
Cl2' Cl2' C17' Cl1' 97.4(12) 4 .
