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_1550576
_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            'C21 H28 Cl3 O P Ru'
_chemical_formula_weight         534.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.282(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7335(9)
_cell_length_b                   7.0904(4)
_cell_length_c                   20.8392(11)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.68
_cell_volume                     2242.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0543
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            173034
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.580
_diffrn_reflns_theta_min         2.026
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.7462
_exptl_transmission_factor_min   0.6790
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+8.8459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6855
_reflns_number_total             7510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05657a2.cif
_cod_data_source_block           P8_18132
_cod_database_code               1550576
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              10748