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_7123526
_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         'C33 H15 B F18 N2 O2'
_chemical_formula_sum            'C33 H15 B F18 N2 O2'
_chemical_formula_weight         824.28
_chemical_name_systematic
;
 cyclo-[B(C6F5)2N(C3H5CF3)C(O)N(C6H11)C(C6F5)O]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.5724(2)
_cell_length_b                   15.9011(3)
_cell_length_c                   41.7343(6)
_cell_measurement_reflns_used    12920
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.6230
_cell_measurement_theta_min      2.1130
_cell_volume                     6352.4(2)
_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 0.991
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            44949
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.964
_diffrn_reflns_theta_min         2.117
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85439
_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    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 3976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         12989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0533P)^2^+1.2272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                10820
_reflns_number_total             12989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02707f2.cif
_cod_data_source_block           MM463
_cod_database_code               7123526
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.758
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              47720