An Adaptable Chelating Diphosphine Ligand for the Stabilization of Palladium and Platinum Carbenes
Barrett, Brittany J.; Iluc, Vlad M.; Organometallics 36 (2017) 730–; doi:10.1021/acs.organomet.6b00924

data_4087153
_publ_section_title
;
 An Adaptable Chelating Diphosphine Ligand for the Stabilization of
 Palladium and Platinum Carbenes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              730
_journal_paper_doi               10.1021/acs.organomet.6b00924
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C47 H62.15 P2 Pd Si'
_chemical_formula_weight         823.54
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                72.9060(10)
_cell_angle_beta                 83.9190(10)
_cell_angle_gamma                81.8410(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7476(3)
_cell_length_b                   13.3740(5)
_cell_length_c                   17.3877(6)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.37
_cell_volume                     2139.73(13)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57530
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.228
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+1.6239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6926
_reflns_number_total             7535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00924_si_002.cif
_cod_data_source_block           bb86b
_cod_database_code               4087153
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2013-4
_shelx_res_checksum              57416
_shelx_hkl_checksum              76697