#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:14:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178641 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/52/4075239.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_4075239
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            'C15 H21 Br2 N3 Pd'
_chemical_formula_weight         509.57
_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                103.1770(10)
_cell_angle_beta                 99.5350(10)
_cell_angle_gamma                109.9120(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6495(4)
_cell_length_b                   9.7830(4)
_cell_length_c                   12.3440(5)
_cell_measurement_reflns_used    7373
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      2.45
_cell_volume                     921.84(7)
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12169
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    5.338
_exptl_absorpt_correction_T_max  0.2362
_exptl_absorpt_correction_T_min  0.2240
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0215
_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)+(0.0282P)²+0.3236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                3856
_reflns_number_total             4220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060151wsi20060217_020125.cif
_cod_data_source_block           Complex2
_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               4075239
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
Pd1 Pd 0.801687(17) 0.496394(16) 0.228018(12) 0.02272(5) Uani 1 1 d .
Br1 Br 0.84216(3) 0.26618(3) 0.14644(3) 0.04681(8) Uani 1 1 d .
Br2 Br 0.72643(3) 0.70894(2) 0.30651(2) 0.03838(7) Uani 1 1 d .
N1 N 0.44334(19) 0.29463(18) 0.18769(13) 0.0223(3) Uani 1 1 d .
N2 N 0.5979(2) 0.32302(18) 0.35668(13) 0.0241(3) Uani 1 1 d .
N3 N 1.0239(2) 0.6351(2) 0.19916(15) 0.0319(4) Uani 1 1 d .
C1 C 0.6018(2) 0.3642(2) 0.25972(16) 0.0224(4) Uani 1 1 d .
C2 C 0.3336(2) 0.2063(2) 0.23966(16) 0.0236(4) Uani 1 1 d .
C3 C 0.1599(2) 0.1165(2) 0.20325(18) 0.0297(4) Uani 1 1 d .
H3 H 0.0930 0.1054 0.1310 0.036 Uiso 1 1 calc R
C4 C 0.0897(3) 0.0441(3) 0.2781(2) 0.0352(5) Uani 1 1 d .
H4 H -0.0275 -0.0179 0.2560 0.042 Uiso 1 1 calc R
C5 C 0.1883(3) 0.0609(3) 0.3852(2) 0.0355(5) Uani 1 1 d .
H5 H 0.1362 0.0098 0.4336 0.043 Uiso 1 1 calc R
C6 C 0.3609(3) 0.1508(2) 0.42205(18) 0.0307(4) Uani 1 1 d .
H6 H 0.4270 0.1622 0.4946 0.037 Uiso 1 1 calc R
C7 C 0.4331(2) 0.2239(2) 0.34725(17) 0.0242(4) Uani 1 1 d .
C8 C 0.4007(2) 0.3096(2) 0.07143(17) 0.0285(4) Uani 1 1 d .
H8 H 0.5081 0.3749 0.0592 0.034 Uiso 1 1 calc R
C9 C 0.2809(3) 0.3919(3) 0.0650(2) 0.0482(6) Uani 1 1 d .
H9A H 0.1704 0.3272 0.0697 0.072 Uiso 1 1 calc R
H9B H 0.2683 0.4150 -0.0076 0.072 Uiso 1 1 calc R
H9C H 0.3275 0.4861 0.1286 0.072 Uiso 1 1 calc R
C10 C 0.3365(3) 0.1547(3) -0.0200(2) 0.0465(6) Uani 1 1 d .
H10A H 0.4181 0.1082 -0.0085 0.070 Uiso 1 1 calc R
H10B H 0.3231 0.1680 -0.0960 0.070 Uiso 1 1 calc R
H10C H 0.2274 0.0892 -0.0138 0.070 Uiso 1 1 calc R
C11 C 0.7504(3) 0.3764(2) 0.45478(17) 0.0302(4) Uani 1 1 d .
H11 H 0.8475 0.4429 0.4332 0.036 Uiso 1 1 calc R
C12 C 0.7923(3) 0.2427(3) 0.4723(2) 0.0455(6) Uani 1 1 d .
H12A H 0.7032 0.1777 0.4982 0.068 Uiso 1 1 calc R
H12B H 0.9004 0.2809 0.5299 0.068 Uiso 1 1 calc R
H12C H 0.7999 0.1842 0.4000 0.068 Uiso 1 1 calc R
C13 C 0.7307(3) 0.4744(3) 0.5616(2) 0.0444(6) Uani 1 1 d .
H13A H 0.7097 0.5595 0.5445 0.067 Uiso 1 1 calc R
H13B H 0.8343 0.5129 0.6235 0.067 Uiso 1 1 calc R
H13C H 0.6354 0.4135 0.5850 0.067 Uiso 1 1 calc R
C14 C 1.1505(3) 0.7085(2) 0.18942(19) 0.0308(4) Uani 1 1 d .
C15 C 1.3146(3) 0.8039(3) 0.1785(2) 0.0446(6) Uani 1 1 d .
H15A H 1.3440 0.9095 0.2217 0.067 Uiso 1 1 calc R
H15B H 1.3075 0.7952 0.0978 0.067 Uiso 1 1 calc R
H15C H 1.4016 0.7705 0.2086 0.067 Uiso 1 1 calc R
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
C1 Pd1 N3 177.20(7)
C1 Pd1 Br1 85.90(6)
N3 Pd1 Br1 92.76(5)
C1 Pd1 Br2 87.89(6)
N3 Pd1 Br2 93.55(5)
Br1 Pd1 Br2 173.329(10)
C1 N1 C2 109.38(15)
C1 N1 C8 123.32(15)
C2 N1 C8 127.28(15)
C1 N2 C7 109.55(15)
C1 N2 C11 123.27(16)
C7 N2 C11 127.17(16)
C14 N3 Pd1 175.35(18)
N1 C1 N2 108.25(16)
N1 C1 Pd1 125.90(14)
N2 C1 Pd1 125.83(13)
C3 C2 C7 121.64(18)
C3 C2 N1 132.03(18)
C7 C2 N1 106.33(16)
C4 C3 C2 117.01(19)
C3 C4 C5 121.57(19)
C6 C5 C4 121.65(19)
C5 C6 C7 117.27(19)
N2 C7 C6 132.63(18)
N2 C7 C2 106.49(16)
C6 C7 C2 120.86(18)
N1 C8 C9 110.49(18)
N1 C8 C10 110.36(18)
C9 C8 C10 114.5(2)
N2 C11 C13 110.76(18)
N2 C11 C12 110.67(18)
C13 C11 C12 114.4(2)
N3 C14 C15 179.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C1 1.9359(19)
Pd1 N3 2.0814(17)
Pd1 Br1 2.4143(3)
Pd1 Br2 2.4287(3)
N1 C1 1.348(2)
N1 C2 1.398(2)
N1 C8 1.475(2)
N2 C1 1.349(2)
N2 C7 1.392(2)
N2 C11 1.481(2)
N3 C14 1.130(3)
C2 C3 1.388(3)
C2 C7 1.397(3)
C3 C4 1.384(3)
C4 C5 1.391(3)
C5 C6 1.381(3)
C6 C7 1.393(3)
C8 C9 1.515(3)
C8 C10 1.523(3)
C11 C13 1.515(3)
C11 C12 1.521(3)
C14 C15 1.457(3)
