Niobium tetrachloride complexes with thio-, seleno- and telluro-ether coordination - synthesis and structures.
Chang, Yao-Pang; Levason, William; Light, Mark E.; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16262–16274; doi:10.1039/c6dt02979e

data_7702102
_publ_section_title
;
 Niobium tetrachloride complexes with thio-, seleno- and telluro-ether
 coordination - synthesis and structures.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16262
_journal_page_last               16274
_journal_paper_doi               10.1039/c6dt02979e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C5 H12 Cl4 Nb S2'
_chemical_formula_sum            'C5 H12 Cl4 Nb S2'
_chemical_formula_weight         370.98
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-18 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.964(3)
_cell_length_b                   9.964(3)
_cell_length_c                   25.113(12)
_cell_measurement_reflns_used    2212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.9
_cell_volume                     2493.3(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            3934
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         2.199
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.108
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0521
_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/[\s^2^(Fo^2^)+(0.0618P)^2^+1.5104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                841
_reflns_number_total             1225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2493(2)
_cod_database_code               7702102
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              55139