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_4087151
_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            'C45 H54 P2 Pd'
_chemical_formula_weight         763.22
_chemical_name_systematic
; 
 ? 
;
_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                 91.1130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1666(3)
_cell_length_b                   12.6383(3)
_cell_length_c                   25.2046(6)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.58
_cell_measurement_theta_min      3.50
_cell_volume                     3874.86(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            74785
_diffrn_reflns_theta_full        72.10
_diffrn_reflns_theta_max         72.10
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    4.856
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+2.6277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                7051
_reflns_number_total             7560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00924_si_002.cif
_cod_data_source_block           bb72
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4087151