A Transient Vinylphosphinidene via a Phosphirene-Phosphinidene Rearrangement.
Liu, Liu Leo; Zhou, Jiliang; Cao, Levy L.; Andrews, Ryan; Falconer, Rosalyn L.; Russell, Christopher A.; Stephan, Douglas W.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b11791

data_4126943
_publ_section_title
;
 A Transient Vinylphosphinidene via a Phosphirene-Phosphinidene
 Rearrangement.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11791
_journal_year                    2017
_chemical_formula_sum            'C42 H45 Cl4 N2 O4 P'
_chemical_formula_weight         814.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.489(11)
_cell_angle_beta                 75.254(9)
_cell_angle_gamma                85.778(10)
_cell_formula_units_Z            2
_cell_length_a                   9.814(3)
_cell_length_b                   12.140(5)
_cell_length_c                   17.306(6)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.72
_cell_volume                     1946.2(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep 3'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.1404
_diffrn_reflns_av_unetI/netI     0.1678
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30878
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.201
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       blcok
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1909
_refine_ls_R_factor_gt           0.0928
_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^)+(0.1379P)^2^+3.6421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3617
_reflns_number_total             7093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11791_si_002.cif
_cod_data_source_block           3
_cod_database_code               4126943
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              14202
_shelx_hkl_checksum              39813