#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:14:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178641 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/52/4075238.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4075238
loop_
_publ_author_name
'Huynh, Han Vinh'
'Han, Yuan'
'Ho, Joanne Hui Hui'
'Tan, Geok Kheng'
_publ_section_title
;
 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
;
_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            'C33 H44 Br4 N4 Pd2'
_chemical_formula_weight         1029.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.5090(10)
_cell_angle_beta                 96.3810(10)
_cell_angle_gamma                110.5480(10)
_cell_formula_units_Z            1
_cell_length_a                   8.6931(6)
_cell_length_b                   9.2111(6)
_cell_length_c                   12.6637(8)
_cell_measurement_reflns_used    3020
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.46
_cell_volume                     907.33(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      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11885
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    5.423
_exptl_absorpt_correction_T_max  0.6131
_exptl_absorpt_correction_T_min  0.3120
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin Plate'
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4150
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0312
_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/[σ²(Fo²)+(0.0366P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                3283
_reflns_number_total             4150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060151wsi20060217_020100.cif
_cod_data_source_block           Complex_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               4075238
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.03764(3) 0.08331(3) 0.646734(19) 0.02254(8) Uani 1 1 d . . .
Br1 Br 1.11975(4) -0.11223(4) 0.51533(3) 0.03268(10) Uani 1 1 d . . .
Br2 Br 1.18368(5) 0.06206(4) 0.81311(3) 0.03799(11) Uani 1 1 d . . .
N1 N 0.8411(3) 0.2077(3) 0.7900(2) 0.0245(6) Uani 1 1 d . . .
N2 N 1.0510(3) 0.4003(3) 0.7621(2) 0.0227(5) Uani 1 1 d . . .
C1 C 0.9739(4) 0.2403(3) 0.7413(2) 0.0221(6) Uani 1 1 d . . .
C2 C 0.8305(4) 0.3520(4) 0.8444(3) 0.0244(7) Uani 1 1 d . . .
C3 C 0.7149(4) 0.3867(4) 0.9024(3) 0.0310(7) Uani 1 1 d . . .
H3 H 0.6217 0.3044 0.9128 0.037 Uiso 1 1 calc R . .
C4 C 0.7434(4) 0.5461(4) 0.9437(3) 0.0354(8) Uani 1 1 d . . .
H4 H 0.6683 0.5732 0.9840 0.042 Uiso 1 1 calc R . .
C5 C 0.8794(4) 0.6693(4) 0.9281(3) 0.0345(8) Uani 1 1 d . . .
H5 H 0.8940 0.7770 0.9583 0.041 Uiso 1 1 calc R . .
C6 C 0.9934(4) 0.6371(4) 0.8693(3) 0.0306(7) Uani 1 1 d . . .
H6 H 1.0851 0.7201 0.8582 0.037 Uiso 1 1 calc R . .
C7 C 0.9661(4) 0.4757(4) 0.8273(2) 0.0232(6) Uani 1 1 d . . .
C8 C 0.7225(4) 0.0415(4) 0.7790(3) 0.0309(7) Uani 1 1 d . . .
H8 H 0.7732 -0.0323 0.7434 0.037 Uiso 1 1 calc R . .
C9 C 0.7021(5) 0.0131(4) 0.8911(3) 0.0473(10) Uani 1 1 d . . .
H9A H 0.8118 0.0510 0.9386 0.071 Uiso 1 1 calc R . .
H9B H 0.6436 -0.1012 0.8823 0.071 Uiso 1 1 calc R . .
H9C H 0.6379 0.0714 0.9242 0.071 Uiso 1 1 calc R . .
C10 C 0.5592(4) 0.0037(5) 0.7018(3) 0.0486(10) Uani 1 1 d . . .
H10A H 0.5068 0.0757 0.7329 0.073 Uiso 1 1 calc R . .
H10B H 0.4847 -0.1070 0.6925 0.073 Uiso 1 1 calc R . .
H10C H 0.5815 0.0183 0.6307 0.073 Uiso 1 1 calc R . .
C11 C 1.1969(4) 0.4793(4) 0.7151(3) 0.0281(7) Uani 1 1 d . . .
H11 H 1.2174 0.3921 0.6653 0.034 Uiso 1 1 calc R . .
C12 C 1.3540(4) 0.5717(5) 0.8038(3) 0.0452(10) Uani 1 1 d . . .
H12A H 1.3375 0.6560 0.8563 0.068 Uiso 1 1 calc R . .
H12B H 1.4474 0.6196 0.7703 0.068 Uiso 1 1 calc R . .
H12C H 1.3779 0.4988 0.8418 0.068 Uiso 1 1 calc R . .
C13 C 1.1569(5) 0.5792(4) 0.6449(3) 0.0411(9) Uani 1 1 d . . .
H13A H 1.0482 0.5173 0.5960 0.062 Uiso 1 1 calc R . .
H13B H 1.2422 0.6084 0.6014 0.062 Uiso 1 1 calc R . .
H13C H 1.1547 0.6763 0.6922 0.062 Uiso 1 1 calc R . .
C1S C 0.409(2) 0.625(3) 0.3853(14) 0.126(8) Uani 0.50 1 d PD A -1
H1SA H 0.4846 0.7353 0.3956 0.189 Uiso 0.50 1 calc PR A -1
H1SB H 0.3005 0.6225 0.3989 0.189 Uiso 0.50 1 calc PR A -1
H1SC H 0.3953 0.5624 0.3101 0.189 Uiso 0.50 1 calc PR A -1
C2S C 0.4768(10) 0.5564(8) 0.4612(6) 0.049(2) Uani 0.50 1 d PGD A -1
C3S C 0.6301(10) 0.6527(6) 0.5325(7) 0.050(3) Uani 0.50 1 d PG A -1
H3SA H 0.6862 0.7594 0.5302 0.061 Uiso 0.50 1 calc PR A -1
C4S C 0.7003(9) 0.5912(10) 0.6070(6) 0.060(2) Uani 0.50 1 d PG A -1
H4SA H 0.8039 0.6563 0.6552 0.072 Uiso 0.50 1 calc PR A -1
C5S C 0.6174(12) 0.4334(11) 0.6103(7) 0.088(6) Uani 0.50 1 d PG A -1
H5SA H 0.6649 0.3918 0.6607 0.105 Uiso 0.50 1 calc PR A -1
C6S C 0.4641(12) 0.3371(7) 0.5391(8) 0.071(3) Uani 0.50 1 d PG A -1
H6SA H 0.4080 0.2303 0.5413 0.085 Uiso 0.50 1 calc PR A -1
C7S C 0.3939(9) 0.3986(8) 0.4645(7) 0.050(3) Uani 0.50 1 d PG A -1
H7SA H 0.2903 0.3335 0.4163 0.060 Uiso 0.50 1 calc PR A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Pd1 Br2 87.50(9) . .
C1 Pd1 Br1 89.26(9) . 2_756
Br2 Pd1 Br1 176.603(15) . 2_756
C1 Pd1 Br1 176.67(9) . .
Br2 Pd1 Br1 95.413(14) . .
Br1 Pd1 Br1 87.857(13) 2_756 .
Pd1 Br1 Pd1 92.143(13) 2_756 .
C1 N1 C2 109.4(2) . .
C1 N1 C8 123.0(2) . .
C2 N1 C8 127.5(2) . .
C1 N2 C7 109.4(2) . .
C1 N2 C11 123.5(2) . .
C7 N2 C11 127.0(2) . .
N2 C1 N1 108.8(2) . .
N2 C1 Pd1 124.7(2) . .
N1 C1 Pd1 126.4(2) . .
C3 C2 N1 133.0(3) . .
C3 C2 C7 120.8(3) . .
N1 C2 C7 106.1(3) . .
C4 C3 C2 116.9(3) . .
C3 C4 C5 122.4(3) . .
C6 C5 C4 121.5(3) . .
C5 C6 C7 116.7(3) . .
C6 C7 C2 121.8(3) . .
C6 C7 N2 132.0(3) . .
C2 C7 N2 106.3(3) . .
N1 C8 C10 110.2(3) . .
N1 C8 C9 111.4(3) . .
C10 C8 C9 114.2(3) . .
N2 C11 C13 110.9(3) . .
N2 C11 C12 111.5(3) . .
C13 C11 C12 113.5(3) . .
C3S C2S C7S 120.0 . .
C3S C2S C1S 118.2(10) . .
C7S C2S C1S 121.8(10) . .
C4S C3S C2S 120.0 . .
C3S C4S C5S 120.0 . .
C6S C5S C4S 120.0 . .
C5S C6S C7S 120.0 . .
C6S C7S C2S 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 1.947(3) .
Pd1 Br2 2.4182(4) .
Pd1 Br1 2.4543(4) 2_756
Pd1 Br1 2.5281(4) .
Br1 Pd1 2.4543(4) 2_756
N1 C1 1.341(4) .
N1 C2 1.398(4) .
N1 C8 1.482(4) .
N2 C1 1.338(4) .
N2 C7 1.399(4) .
N2 C11 1.483(4) .
C2 C3 1.392(4) .
C2 C7 1.398(4) .
C3 C4 1.369(4) .
C4 C5 1.390(5) .
C5 C6 1.378(5) .
C6 C7 1.389(4) .
C8 C10 1.513(5) .
C8 C9 1.517(5) .
C11 C13 1.506(4) .
C11 C12 1.510(5) .
C1S C2S 1.438(13) .
C2S C3S 1.3900 .
C2S C7S 1.3900 .
C3S C4S 1.3900 .
C4S C5S 1.3900 .
C5S C6S 1.3900 .
C6S C7S 1.3900 .
