Thiaborane clusters with the exoskeletal B-H group
Vrana, Jan; Holub, Josef; Samsonov, Maksim Andreevich; Ruzickova, Zdenka; Fanfrlik, Jindrich; Hnyk, Drahomír; Růžička, Aleš; Chemical Communications  (2019) –; doi:10.1039/C9CC00952C

data_7123035
_publ_section_title
;
 Thiaborane clusters with the exoskeletal B-H group
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00952C
_journal_year                    2019
_chemical_formula_moiety         'H11 B10 S, 3(H12 N2 C6), H'
_chemical_formula_sum            'C18 H48 B10 N6 S'
_chemical_formula_weight         488.78
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-02-01 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   22.2424(5)
_cell_length_b                   22.2424(5)
_cell_length_c                   14.5434(3)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.38
_cell_measurement_theta_min      3.81
_cell_volume                     6231.0(2)
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            73941
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.362
_diffrn_reflns_theta_min         2.294
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.2518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       needle
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         16651
_refine_ls_number_restraints     1097
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.1139
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2926
_refine_ls_wR_factor_ref         0.3213
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                13230
_reflns_number_total             16651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00952c2.cif
_cod_data_source_block           7a
_cod_original_cell_volume        6231.0(3)
_cod_database_code               7123035
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.581
_shelx_estimated_absorpt_t_max   0.930
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.334
;
_shelx_res_checksum              23188
_shelx_hkl_checksum              95535