Synthesis of 9-Borafluorene Analogues Featuring a Three-Dimensional 1,1’-Bis(o-carborane) Backbone
Yruegas, Sam; Axtell, Jonathan; Kirlikovali, Kent; Spokoyny, Alex; Martin, Caleb Daniel; Chemical Communications  (2019) –; doi:10.1039/C8CC10087J

data_7122899
_publ_section_title
;
 Synthesis of 9-Borafluorene Analogues Featuring a Three-Dimensional
 1,1&#x2019;-Bis(o-carborane) Backbone
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10087J
_journal_year                    2019
_chemical_formula_moiety         'C14 H36 B21 N, 4(C)'
_chemical_formula_sum            'C18 H36 B21 N'
_chemical_formula_weight         493.49
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-12-12 deposited with the CCDC.
2019-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.680(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7390(7)
_cell_length_b                   16.5577(11)
_cell_length_c                   19.2181(13)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.30
_cell_volume                     3710.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63721
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.460
_exptl_absorpt_coefficient_mu    0.042
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.883
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6544
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0988
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1617P)^2^+3.3718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2753
_refine_ls_wR_factor_ref         0.2898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             6544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc10087j2.cif
_cod_data_source_block           1BMe8
_cod_database_code               7122899
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.989
_shelx_res_checksum              52412
_shelx_fab_checksum              51586