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_7133796
_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
'C50 H30 Al F10 N4 P2, Al C24 F20, C7 H8, 0.5[], 1[]'
_chemical_formula_sum            'C81 H38 Al2 F30 N4 P2'
_chemical_formula_weight         1753.05
_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
_audit_creation_date             2024-08-26
_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                94.3340(10)
_cell_angle_beta                 99.0020(10)
_cell_angle_gamma                100.3890(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2784(2)
_cell_length_b                   17.5791(4)
_cell_length_c                   20.1614(5)
_cell_measurement_reflns_used    8454
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      67.874
_cell_measurement_theta_min      2.232
_cell_volume                     3861.10(15)
_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 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0751
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50107
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.346
_diffrn_reflns_theta_min         2.231
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0981 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.8622.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         14089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0707P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9263
_reflns_number_total             14089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04490h2.cif
_cod_data_source_block           m1
_cod_depositor_comments
'Adding full bibliography for 7133795--7133800.cif.'
_cod_database_code               7133796
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C01C(H01C), C01F(H01F), C01I(H01I), C01J(H01J), C01L(H01L), C01N(H01N),
 C01O(H01O), C01P(H01P), C01R(H01R), C01S(H01S), C01T(H01T), C01Y(H01Y),
 C01Z(H01Z), C023(H023), C026(H026), C027(H027), C029(H029), C02B(H02B),
 C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02H(H02H), C02K(H02K),
 C02O(H02O), C02P(H02P), C02R(H02R), C02U(H02U), C02Z(H02Z), C033(H033),
 C035(H035), C037(H037), C038(H038), C039(H039), C03A(H03A)
2.b Idealised Me refined as rotating group:
 C03C(H03B,H03C,H03D)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 54 electrons were 
found in a volume of 270\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.5[None] per formula unit 
which account for 0 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83074
_shelx_hkl_checksum              58068
_shelx_fab_checksum              49280
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'