Reactivity of <i>N</i>-(isocyanoimino)triphenylphosphorane toward group 13 Lewis acids.
Tang, Beili; Ju, Shaoying; Yan, Weili; Chen, Ting; Stephan, Douglas W.; Wu, Yile; Chemical communications (Cambridge, England) 60 (2024) 12932–12935; doi:10.1039/d4cc04490h

data_7133795
_publ_section_title
;
 Reactivity of <i>N</i>-(isocyanoimino)triphenylphosphorane toward group
 13 Lewis acids.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12932
_journal_page_last               12935
_journal_paper_doi               10.1039/d4cc04490h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C37 H15 B F15 N2 P'
_chemical_formula_sum            'C37 H15 B F15 N2 P'
_chemical_formula_weight         814.29
_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
_audit_creation_date             2024-05-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-26 deposited with the CCDC.	2024-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6295(3)
_cell_length_b                   11.5884(3)
_cell_length_c                   24.2727(6)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      68.585
_cell_measurement_theta_min      4.014
_cell_volume                     3237.52(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37185
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.745
_diffrn_reflns_theta_min         4.014
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.862
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0882 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.9148.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0411P)^2^+1.1822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5323
_reflns_number_total             5926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04490h2.cif
_cod_data_source_block           222
_cod_depositor_comments
'Adding full bibliography for 7133795--7133800.cif.'
_cod_database_code               7133795
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00V(H00V), C00W(H00W), C013(H013), C015(H015), C016(H016),
 C017(H017), C019(H019), C01B(H01B), C01C(H01C), C01E(H01E), C01F(H01F),
 C01H(H01H), C01I(H01I), C01J(H01J)
;
_shelx_res_checksum              65118
_shelx_hkl_checksum              27904
_olex2_submission_special_instructions 'No special instructions were received'