Benzenedicarbonyl and benzenetricarbonyl linker pyrazolyl complexes of palladium(II): synthesis, X-ray structures and evaluation as ethylene polymerisation catalysts
Guzei, Ilia A.; Li, Kelin; Bikzhanova, Galina A.; Darkwa, James; Mapolie, Selwyn F.; Dalton Transactions  (2003) 715–722; doi:10.1039/b208376k

data_7012188
_publ_section_title
;
 Benzenedicarbonyl and benzenetricarbonyl linker pyrazolyl complexes of
 palladium(II): synthesis, X-ray structures and evaluation as ethylene
 polymerisation catalysts
;
_journal_coden_ASTM              DTARAF
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              715
_journal_page_last               722
_journal_paper_doi               10.1039/b208376k
_journal_year                    2003
_chemical_formula_sum            'C30 H42 N4 O2'
_chemical_formula_weight         490.68
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.554(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2718(11)
_cell_length_b                   18.6937(18)
_cell_length_c                   13.9240(15)
_cell_measurement_temperature    173(2)
_cell_volume                     2920.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11835
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9696
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0424P)^2^+0.5568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                3903
_reflns_number_total             5094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208376k.txt
_cod_data_source_block           darr
_cod_database_code               7012188