Tungsten carbonyl σ-complexes with C-thioethers based on 9-Me3N-7,8-C2B9H11
Timofeev, Sergey V.; Prikaznova, Elena A.; Zhidkova, Olga B.; Druzina, Anna A.; Starikova, Zoya A.; Suponitsky, Kyrill Y.; Godovikov, Ivan A.; Sivaev, Igor B.; Bregadze, Vladimir I.; New Journal of Chemistry 44 (2020) 13934–13938; doi:10.1039/D0NJ03212C

data_7059855
_publ_section_title
;
 Tungsten carbonyl \s-complexes with C-thioethers based on
 9-Me3N-7,8-C2B9H11
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13934
_journal_page_last               13938
_journal_paper_doi               10.1039/D0NJ03212C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C6 H22 B9 N S'
_chemical_formula_sum            'C6 H22 B9 N S'
_chemical_formula_weight         237.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9801(11)
_cell_length_b                   10.0922(12)
_cell_length_c                   14.8274(19)
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.51
_cell_measurement_theta_min      2.65
_cell_volume                     1343.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material
'SHELXL-2014/6 (Sheldrick, 2014) and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.0888
_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       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17444
_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         29.991
_diffrn_reflns_theta_min         2.441
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prizm
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 995 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.56(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0673P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2829
_reflns_number_total             3918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03212c2.cif
_cod_data_source_block           l23
_cod_depositor_comments
;Adding full bibliography for 7059855--7059857.cif.

 Adding full bibliography for 7059855--7059857.cif.
;
_cod_database_code               7059855
_shelxl_version_number           2014/6
_shelx_res_checksum              69255