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_4087150
_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            'C32.5 H46 P2 Pd'
_chemical_formula_weight         605.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5762(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.1059(11)
_cell_length_b                   10.3894(6)
_cell_length_c                   31.9405(19)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.26
_cell_volume                     5906.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            89377
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.437
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+4.8859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                7971
_reflns_number_total             10395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00924_si_002.cif
_cod_data_source_block           bb61b
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C65 H92 P4 Pd2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1210.07
_cod_database_code               4087150