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_7123029
_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         'C14 H31 B11 N4 S, C4 H8 O'
_chemical_formula_sum            'C18 H39 B11 N4 O S'
_chemical_formula_weight         478.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                71.461(5)
_cell_angle_beta                 76.041(12)
_cell_angle_gamma                71.517(12)
_cell_formula_units_Z            2
_cell_length_a                   8.831(3)
_cell_length_b                   10.884(2)
_cell_length_c                   15.634(3)
_cell_measurement_reflns_used    849
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.63
_cell_volume                     1334.6(6)
_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    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.421
_diffrn_measured_fraction_theta_max 0.411
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1347
_diffrn_reflns_av_unetI/netI     0.1449
_diffrn_reflns_Laue_measured_fraction_full 0.421
_diffrn_reflns_Laue_measured_fraction_max 0.411
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2691
_diffrn_reflns_point_group_measured_fraction_full 0.421
_diffrn_reflns_point_group_measured_fraction_max 0.411
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7246
_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    1.191
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         2161
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.0813
_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^)+(0.1222P)^2^+0.6611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1505
_reflns_number_total             2161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00952c2.cif
_cod_data_source_block           4a_prime
_cod_original_cell_volume        1334.7(6)
_cod_database_code               7123029
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.991
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.972
;
_shelx_res_checksum              33817
_shelx_hkl_checksum              80014