Synthesis and characterisation of cyclometallated palladium(II) complexes with phosphine‒carboxylate and phosphine‒amide ligands
Gregorio Sánchez; Joaquín García; David Meseguer; José L. Serrano; Luis García; José Pérez; Gregorio López; Dalton Trans.  (2003) 4709–4717; doi:10.1039/b310843k

data_7013635
_publ_section_title
;
 Synthesis and characterisation of cyclometallated palladium(II)
 complexes with phosphine--carboxylate and phosphine--amide ligands
;
_journal_issue                   24
_journal_name_full               'Dalton Trans.'
_journal_page_first              4709
_journal_page_last               4717
_journal_paper_doi               10.1039/b310843k
_journal_year                    2003
_chemical_formula_moiety         'C33 H33 N2 O4 P Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C33.5 H34 Cl N2 O4 P Pd'
_chemical_formula_weight         701.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.315(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.380(2)
_cell_length_b                   9.5746(7)
_cell_length_c                   16.9787(11)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.986
_cell_measurement_theta_min      10.038
_cell_volume                     6501.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8124
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                4440
_reflns_number_total             5715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310843k.txt
_cod_data_source_block           compound_16a
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C33.50 H34 Cl N2 O4 P Pd'
_cod_database_code               7013635