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_7702107
_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         'C4 H10 Cl3 Nb O S2'
_chemical_formula_sum            'C4 H10 Cl3 Nb O S2'
_chemical_formula_weight         337.50
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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                108.917(4)
_cell_angle_beta                 99.404(4)
_cell_angle_gamma                113.677(4)
_cell_formula_units_Z            1
_cell_length_a                   6.7898(3)
_cell_length_b                   6.9745(3)
_cell_length_c                   7.2523(4)
_cell_measurement_reflns_used    6549
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1680
_cell_measurement_theta_min      3.1020
_cell_volume                     279.93(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6650
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       Chip
_exptl_crystal_F_000             166
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
; 
 Flack x determined using 1030 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2205
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2156
_reflns_number_total             2205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02979e2.cif
_cod_data_source_block           2016_1405r3
_cod_database_code               7702107
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              1063