C‒H Activation Reactions of a Nucleophilic Palladium Carbene
Comanescu, Cezar C.; Iluc, Vlad M.; Organometallics 34 (2015) 4684–; doi:10.1021/acs.organomet.5b00414

data_4087617
_publ_section_title
;
 C--H Activation Reactions of a Nucleophilic Palladium Carbene
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4684
_journal_paper_doi               10.1021/acs.organomet.5b00414
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C28 H42 O P2 Pd'
_chemical_formula_weight         562.45
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.4973(17)
_cell_angle_beta                 91.1235(19)
_cell_angle_gamma                92.877(2)
_cell_formula_units_Z            4
_cell_length_a                   9.6415(3)
_cell_length_b                   15.7069(5)
_cell_length_c                   18.6884(6)
_cell_measurement_temperature    120(2)
_cell_volume                     2786.71(15)
_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  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85027
_diffrn_reflns_theta_full        72.05
_diffrn_reflns_theta_max         72.05
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    6.575
_exptl_absorpt_correction_T_max  0.8529
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.484
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00149(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         10468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1351P)^2^+4.4163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                8194
_reflns_number_total             10468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00414_si_002.cif
_cod_data_source_block           cc196
_cod_depositor_comments
;

2020-06-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H83 O2 P4 Pd2'
_cod_original_formula_weight         1124.90
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4087617