Structure, formation and catalytic studies of a meso-palladioporphyrin intermediate in a Heck reaction
Jiang, Michael Y.; Shin, Ji-Young; Patrick, Brian O.; Dolphin, David; Dalton Transactions  (2008) 2598–2602; doi:10.1039/b801163j

data_7003904
_publ_section_title
;
 Structure, formation and catalytic studies of a meso-palladioporphyrin
 intermediate in a Heck reaction
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              2598
_journal_page_last               2602
_journal_paper_doi               10.1039/b801163j
_journal_year                    2008
_chemical_formula_sum            'C136.84 H99.68 Cl3.68 N8 P4 Pd2 Zn2'
_chemical_formula_weight         2453.88
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.820(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3040(10)
_cell_length_b                   29.414(3)
_cell_length_c                   14.4270(10)
_cell_measurement_reflns_used    26806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.06
_cell_volume                     5645.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_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  0.087
_diffrn_reflns_av_sigmaI/netI    0.1571
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22575
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7531
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.4444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2503
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.841
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(2)
_refine_ls_extinction_coef       0.0038(3)
_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   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1417
_refine_ls_number_reflns         22575
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2204
_reflns_number_gt                15404
_reflns_number_total             22575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801163j.txt
_cod_data_source_block           dd179
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7003904