Palladium(II) Complexes of a Sterically Bulky, Benzannulated N-Heterocyclic Carbene with Unusual Intramolecular C−H···Pd and Ccarbene···Br Interactions and Their Catalytic Activities
Huynh, Han Vinh; Han, Yuan; Ho, Joanne Hui Hui; Tan, Geok Kheng; Organometallics 25 (2006) 3267–; doi:10.1021/om060151w

data_4075240
_publ_section_title
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 Palladium(II) Complexes of a Sterically Bulky, Benzannulated
 N-Heterocyclic Carbene with Unusual Intramolecular
 C&#x2212;H&#x00B7;&#x00B7;&#x00B7;Pd and
 Ccarbene&#x00B7;&#x00B7;&#x00B7;Br Interactions and Their Catalytic
 Activities
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3267
_journal_paper_doi               10.1021/om060151w
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C30 H41 Br3 Cl12 N4 Pd'
_chemical_formula_weight         1229.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.0060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7290(7)
_cell_length_b                   8.9604(4)
_cell_length_c                   33.5536(16)
_cell_measurement_reflns_used    3709
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.58
_cell_volume                     4722.5(4)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            32676
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    3.637
_exptl_absorpt_correction_T_max  0.5605
_exptl_absorpt_correction_T_min  0.3543
_exptl_absorpt_correction_type   'Sadabds, (Sheldrick 2001)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         10858
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                6502
_reflns_number_total             10858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060151wsi20060217_020148.cif
_cod_data_source_block           Complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4075240