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_7012184
_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            'C42 H60 N6 O3'
_chemical_formula_weight         696.96
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3167(13)
_cell_length_b                   14.3940(11)
_cell_length_c                   29.844(2)
_cell_measurement_temperature    173(2)
_cell_volume                     8298.0(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7311
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9654
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7311
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1243P)^2^+6.1531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                5507
_reflns_number_total             7311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208376k.txt
_cod_data_source_block           darj
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8297.8(11)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7012184