Mechanism and Scope of Phosphinidene Transfer from Dibenzo-7-phosphanorbornadiene Compounds.
Transue, Wesley J.; Velian, Alexandra; Nava, Matthew; García-Iriepa, Cristina; Temprado, Manuel; Cummins, Christopher C.; Journal of the American Chemical Society 139 (2017) 10822–10831; doi:10.1021/jacs.7b05464

data_4131451
_publ_section_title
;
 Mechanism and Scope of Phosphinidene Transfer from
 Dibenzo-7-phosphanorbornadiene Compounds.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10822
_journal_page_last               10831
_journal_paper_doi               10.1021/jacs.7b05464
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C14 H12 N P'
_chemical_formula_weight         225.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           42
_space_group_name_Hall           'F 2 -2'
_space_group_name_H-M_alt        'F m m 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.779(3)
_cell_length_b                   16.542(6)
_cell_length_c                   6.543(3)
_cell_measurement_reflns_used    1890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.46
_cell_volume                     1058.4(7)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7834
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.517
_diffrn_reflns_theta_min         2.462
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.7463
_exptl_transmission_factor_min   0.6748
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
; 
 Flack x determined using 288 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         834
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.8809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.875
_reflns_number_gt                755
_reflns_number_total             834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05464_si_002.cif
_cod_data_source_block           X8_15165
_cod_original_cell_volume        1058.5(6)
_cod_database_code               4131451
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              24139
_shelx_hkl_checksum              13239