Carboboration of isocyanates with tris(pentafluorophenyl)borane and evidence for dissociative FLP chemistry of an acid‒base pair
Mehta, Meera; Goicoechea, Jose M.; Chemical Communications  (2019) –; doi:10.1039/C9CC02707F

data_7123524
_publ_section_title
;
 Carboboration of isocyanates with tris(pentafluorophenyl)borane and
 evidence for dissociative FLP chemistry of an acid--base pair
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02707F
_journal_year                    2019
_chemical_formula_moiety         'C50 H10 F30 Ga2 N2 O2, C6 H14'
_chemical_formula_sum            'C56 H24 F30 Ga2 N2 O2'
_chemical_formula_weight         1466.21
_chemical_name_systematic
;
 cyclo-[Ga(C6F5)2N(C6H5)C(C6H11)OGa(C6F5)2N(C6H5)C(C6H11)O]*hex
;
_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   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-04-04 deposited with the CCDC.    2019-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                67.685(4)
_cell_angle_beta                 79.756(4)
_cell_angle_gamma                71.222(4)
_cell_formula_units_Z            1
_cell_length_a                   9.8455(5)
_cell_length_b                   11.6923(5)
_cell_length_c                   13.4043(7)
_cell_measurement_reflns_used    6743
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0810
_cell_measurement_theta_min      4.2430
_cell_volume                     1348.79(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.171
_diffrn_reflns_theta_min         4.257
_exptl_absorpt_coefficient_mu    2.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       needle
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0438P)^2^+0.2864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4948
_reflns_number_total             5570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02707f2.cif
_cod_data_source_block           MM339
_cod_database_code               7123524
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.597
_shelx_estimated_absorpt_t_max   0.818
_shelx_res_checksum              4539