Direct synthesis of dicarbollides
Tok, Oleg L.; Holub, Josef; Růžička, Aleš; Růžičková, Zdeńka; Štíbr, Bohumil; New Journal of Chemistry 42 (2018) 8524–; doi:10.1039/C8NJ00819A

data_7057301
_publ_section_title
;
 Direct synthesis of dicarbollides
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8524
_journal_paper_doi               10.1039/C8NJ00819A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C5 H20 B9 Si, C6 H16 N'
_chemical_formula_sum            'C11 H36 B9 N Si'
_chemical_formula_weight         307.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'APEX3 v2016.5-0'
_audit_update_record
;
2018-02-07 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.748(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1704(8)
_cell_length_b                   9.1463(6)
_cell_length_c                   14.3457(9)
_cell_measurement_reflns_used    27319
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.539
_cell_measurement_theta_min      2.572
_cell_volume                     2077.3(2)
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Platon (Spek, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.963
_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  0.1127
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26531
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.572
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.075(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0352P)^2^+2.4161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2908
_reflns_number_total             4611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00819a2.cif
_cod_data_source_block           mo_jhl171121Si1_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7057300--7057301.cif.'
_cod_database_code               7057301
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.784
;
_shelx_res_checksum              40052