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_4088721
_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         'C31 H19 O5 P W'
_chemical_formula_sum            'C31 H19 O5 P W'
_chemical_formula_weight         686.28
_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                 98.8060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8459(6)
_cell_length_b                   11.9834(6)
_cell_length_c                   20.5150(11)
_cell_measurement_reflns_used    9256
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.55
_cell_volume                     2634.9(2)
_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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23333
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.353
_diffrn_reflns_theta_min         1.900
_exptl_absorpt_coefficient_mu    4.485
_exptl_absorpt_correction_T_max  0.7773
_exptl_absorpt_correction_T_min  0.3724
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       rod
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.729
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0274P)^2^+0.7446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5515
_reflns_number_total             6539
_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               4088721
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.288
_shelx_estimated_absorpt_t_max   0.716
_shelx_res_checksum              12158
_shelx_hkl_checksum              63214