Phosphorus‒Carbon Bond Forming Reactions of Diphenylphosphenium and Diphenylphosphine Triflate Complexes of Tungsten
Jayaraman, Arumugam; Sterenberg, Brian T.; Organometallics 35 (2016) 2367–; doi:10.1021/acs.organomet.6b00348

data_4088720
_publ_section_title
;
 Phosphorus--Carbon Bond Forming Reactions of Diphenylphosphenium and
 Diphenylphosphine Triflate Complexes of Tungsten
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2367
_journal_paper_doi               10.1021/acs.organomet.6b00348
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C24 H19 O5 P W'
_chemical_formula_sum            'C24 H19 O5 P W'
_chemical_formula_weight         602.21
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.0200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8721(11)
_cell_length_b                   10.4975(7)
_cell_length_c                   13.7225(9)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.36
_cell_volume                     2186.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32181
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.619
_diffrn_reflns_theta_min         2.359
_exptl_absorpt_coefficient_mu    5.390
_exptl_absorpt_correction_T_max  0.5605
_exptl_absorpt_correction_T_min  0.2690
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0132
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+1.1995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4792
_reflns_number_total             5073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00348_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088720
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.283
_shelx_estimated_absorpt_t_max   0.499
_shelx_res_checksum              4533
_shelx_hkl_checksum              75852