Synthesis of acyl(chloro)phosphines enabled by phosphinidene transfer
Szkop, Kevin M.; Geeson, Michael Baily; Stephan, Douglas W.; Cummins, Christopher; Chemical Science  (2019) –; doi:10.1039/C8SC05657A

data_1550575
_publ_section_title
;
 Synthesis of acyl(chloro)phosphines enabled by phosphinidene transfer
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05657A
_journal_year                    2019
_chemical_formula_sum            'C22 H29 O2 P'
_chemical_formula_weight         356.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-03 deposited with the CCDC.
2019-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.615(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4762(6)
_cell_length_b                   7.8291(7)
_cell_length_c                   18.9197(17)
_cell_measurement_reflns_used    6009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.08
_cell_measurement_theta_min      2.82
_cell_volume                     958.28(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.790
_diffrn_reflns_theta_min         1.077
_exptl_absorpt_coefficient_mu    0.156
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.059
_exptl_transmission_factor_max   0.746070
_exptl_transmission_factor_min   0.687769
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2153 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.14(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5983
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0368P)^2^+0.1564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                5347
_reflns_number_total             5983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05657a2.cif
_cod_data_source_block           X8_18108_t5
_cod_database_code               1550575
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              53915