ortho-Phenylene bridged palladium bis-N-heterocyclic carbene complexes: synthesis, structure and catalysis.
Munz, Dominik; Poethig, Alexander; Tronnier, Alexander; Strassner, Thomas; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7297–7304; doi:10.1039/c3dt33006k

data_7021227
_publ_section_title
;
 ortho-Phenylene bridged palladium bis-N-heterocyclic carbene complexes:
 synthesis, structure and catalysis.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7297
_journal_page_last               7304
_journal_paper_doi               10.1039/c3dt33006k
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'see text'
_chemical_formula_moiety         '(C26 H21 Br4 N4 Pd), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C27.5 H24 Br4 Cl3 N4 Pd'
_chemical_formula_weight         942.906
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.297(2)
_cell_length_b                   18.653(5)
_cell_length_c                   15.986(4)
_cell_measurement_reflns_used    791
_cell_measurement_temperature    198
_cell_measurement_theta_max      24.234
_cell_measurement_theta_min      4.081
_cell_volume                     6350(2)
_computing_cell_refinement       'Dirax/lsq (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius BV, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92(Altomare et al., 1994)'
_diffrn_ambient_temperature      198
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  x-ray
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            148489
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         4.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.896
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2002'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0056P)^2^+16.6044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                4896
_reflns_number_total             6472
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt33006k.txt
_cod_data_source_block           Compound_11a
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6351(2)
_cod_original_formula_sum        'C27.50 H24 Br4 Cl3 N4 Pd'
_cod_database_code               7021227