Di-μ-chlorido-μ-(dimethyl sulfide)-bis{dichlorido[(dimethyl selenide-κ<i>Se</i>)(dimethyl sulfide-κ<i>S</i>)(0.65/0.35)]niobium(III)}(<i>Nb</i>—<i>Nb</i>)
Matsuura, Masatoshi; Fujihara, Takashi; Nagasawa, Akira; Ng, Seik Weng; Acta Crystallographica Section E 68 (2012) m1166–; doi:10.1107/S1600536812033673

data_2236093
_publ_section_title
;
 Di-\m-chlorido-\m-(dimethyl sulfide)-bis{dichlorido[(dimethyl
 selenide-\k<i>Se</i>)(dimethyl
 sulfide-\k<i>S</i>)(0.65/0.35)]niobium(III)}(<i>Nb</i>---<i>Nb</i>)
;
_journal_coeditor_code           BT5971
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1166
_journal_paper_doi               10.1107/S1600536812033673
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Nb2 Cl6 (C2 H6 S)1.7 (C2 H6 Se)1.3]'
_chemical_formula_moiety         'C6 H18 Cl6 Nb2 S1.70 Se1.30'
_chemical_formula_sum            'C6 H18 Cl6 Nb2 S1.7 Se1.3'
_chemical_formula_weight         645.87
_chemical_name_systematic
;
Di-\m-chlorido-\m-(dimethyl sulfide)-bis{dichlorido[(dimethyl
selenide-\k<i>Se</i>)(dimethyl
sulfide-\k<i>S</i>)(0.65/0.35)]niobium(III)}(<i>Nb</i>---<i>Nb</i>)
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3314(11)
_cell_length_b                   13.5952(12)
_cell_length_c                   10.6649(9)
_cell_measurement_reflns_used    3921
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.4863
_cell_measurement_theta_min      2.8683
_cell_volume                     1932.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10299
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.626
_exptl_absorpt_correction_T_max  0.7085
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1238
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.527
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2218
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+2.0744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                1975
_reflns_number_total             2218
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bt5971.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C6 H18 Cl6 Nb2 S1.70 Se1.30'
_cod_database_code               2236093
_cod_database_fobs_code          2236093