Azidoborolate anions and azidoborole adducts: isolable forms of an unstable borole azide
Lindl, Felix Dr.; Fantuzzi, Felipe; Mailänder, Lisa; Hörl, Christian; Bélanger-Chabot, Guillaume; Braunschweig, Holger; Chemical Communications  (2022) –; doi:10.1039/D2CC00543C

data_7129861
_publ_section_title
;
 Azidoborolate anions and azidoborole adducts: isolable forms of an
 unstable borole azide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00543C
_journal_year                    2022
_chemical_formula_moiety         'C65 H52 B Cl4 N P2'
_chemical_formula_sum            'C65 H52 B Cl4 N P2'
_chemical_formula_weight         1061.48
_chemical_name_common
'bis(triphenylphosphine)iminium dichloro-2,3,4,5-tetraphenylborolate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-20 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                81.894(2)
_cell_angle_beta                 75.6420(10)
_cell_angle_gamma                85.430(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4915(6)
_cell_length_b                   13.6720(7)
_cell_length_c                   17.9784(8)
_cell_measurement_reflns_used    9522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.30
_cell_volume                     2706.1(2)
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            67016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11075
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+2.8235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9575
_reflns_number_total             11075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00543c2.cif
_cod_data_source_block           PPN[6]
_cod_database_code               7129861
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              5048