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_7129860
_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         'C53 H42 B Cl3.75 N0.74 P'
_chemical_formula_sum            'C53 H42 B Cl3.75 N0.74 P'
_chemical_formula_weight         864.07
_chemical_name_common
'tetraphenylphosphonium salts of mixed chloro/azido-2,3,4,5-tetraphenylborolates'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-01-20 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.531(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.758(2)
_cell_length_b                   12.3357(14)
_cell_length_c                   18.957(2)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.26
_cell_volume                     4385.0(8)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_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  0.0494
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79940
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.548
_diffrn_source                   'rotating-anode (Nonius FR-591)'
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_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       prism
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8972
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0136P)^2^+5.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8245
_reflns_number_total             8972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00543c2.cif
_cod_data_source_block           PPh4[4-mix]
_cod_original_cell_volume        4385.1(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7129860
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              56205