Interception of intermediates in phosphine oxidation by mesityl nitrile-N-oxide using frustrated Lewis pairs.
Szkop, Kevin M.; Zhu, Diya; Longobardi, Lauren E.; Heck, Julian; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8933–8939; doi:10.1039/c8dt01717d

data_7046557
_publ_section_title
;
 Interception of intermediates in phosphine oxidation by mesityl
 nitrile-N-oxide using frustrated Lewis pairs.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8933
_journal_page_last               8939
_journal_paper_doi               10.1039/c8dt01717d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C46 H29 B F12 N O P'
_chemical_formula_weight         881.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   10.496(2)
_cell_length_c                   15.154(3)
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_cell_measurement_temperature    123(2)
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_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_number            61540
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.811
_diffrn_reflns_theta_min         2.875
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
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_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2454 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8956
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0400P)^2^+0.2117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                6686
_reflns_number_total             8956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01717d2.cif
_cod_data_source_block           ortho_a
_cod_depositor_comments
'Adding full bibliography for 7046555--7046558.cif.'
_cod_database_code               7046557
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              23659