#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:20:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179686 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/08/7000803.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_7000803
loop_
_publ_author_name
'Han, Yuan'
'Huynh, Han Vinh'
_publ_section_title
;
 Mixed carbene--isocyanide Pd(ii) complexes: synthesis, structures and
 reactivity towards nucleophiles
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2201
_journal_page_last               2209
_journal_paper_doi               10.1039/b816471a
_journal_year                    2009
_chemical_formula_sum            'C28 H42 Br4 Cl6 N6 Pd2'
_chemical_formula_weight         1207.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            4
_cell_length_a                   18.1241(9)
_cell_length_b                   26.0307(12)
_cell_length_c                   9.1762(4)
_cell_measurement_reflns_used    4196
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.60
_cell_volume                     4329.2(3)
_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 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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23435
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    4.920
_exptl_absorpt_correction_T_max  0.7567
_exptl_absorpt_correction_T_min  0.2105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.755
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0679
_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)+(0.0619P)²+71.7484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                3201
_reflns_number_total             3814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816471a.txt
_cod_data_source_block           7531a
_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_sg_symbol_H-M      Pccn
_cod_database_code               7000803
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
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 0.65688(4) 0.32350(2) 0.38702(7) 0.0282(2) Uani 1 1 d . . .
Br1 Br 0.61091(6) 0.27961(4) 0.17317(11) 0.0432(3) Uani 1 1 d . . .
Br2 Br 0.69683(6) 0.36873(4) 0.60515(12) 0.0467(3) Uani 1 1 d . . .
N1 N 0.5732(4) 0.4143(3) 0.2962(8) 0.0296(16) Uani 1 1 d . . .
N2 N 0.5117(4) 0.3705(3) 0.4572(8) 0.0292(16) Uani 1 1 d . . .
N3 N 0.7542(5) 0.2774(3) 0.3931(9) 0.0372(17) Uani 1 1 d . . .
H3A H 0.7824 0.2861 0.3148 0.045 Uiso 1 1 calc R . .
H3B H 0.7800 0.2863 0.4743 0.045 Uiso 1 1 calc R . .
C1 C 0.5743(4) 0.3719(3) 0.3787(9) 0.0239(17) Uani 1 1 d . . .
C2 C 0.5089(5) 0.4417(3) 0.3230(10) 0.034(2) Uani 1 1 d . . .
C3 C 0.4820(6) 0.4885(4) 0.2704(12) 0.051(3) Uani 1 1 d . . .
H3 H 0.5090 0.5082 0.2029 0.061 Uiso 1 1 calc R . .
C4 C 0.4148(7) 0.5046(5) 0.3211(13) 0.064(4) Uani 1 1 d . . .
H4 H 0.3956 0.5360 0.2870 0.076 Uiso 1 1 calc R . .
C5 C 0.3740(7) 0.4765(5) 0.4205(13) 0.061(3) Uani 1 1 d . . .
H5 H 0.3280 0.4889 0.4520 0.073 Uiso 1 1 calc R . .
C6 C 0.4002(5) 0.4303(5) 0.4742(12) 0.050(3) Uani 1 1 d . . .
H6 H 0.3727 0.4108 0.5412 0.060 Uiso 1 1 calc R . .
C7 C 0.4696(5) 0.4137(3) 0.4246(10) 0.033(2) Uani 1 1 d . . .
C8 C 0.6312(6) 0.4266(4) 0.1867(12) 0.044(2) Uani 1 1 d . . .
H8 H 0.6660 0.3973 0.1872 0.053 Uiso 1 1 calc R . .
C9 C 0.6748(8) 0.4728(5) 0.2352(18) 0.079(5) Uani 1 1 d . . .
H9A H 0.7119 0.4809 0.1625 0.119 Uiso 1 1 calc R . .
H9B H 0.6987 0.4654 0.3274 0.119 Uiso 1 1 calc R . .
H9C H 0.6419 0.5019 0.2470 0.119 Uiso 1 1 calc R . .
C10 C 0.6016(8) 0.4301(6) 0.0364(12) 0.070(4) Uani 1 1 d . . .
H10A H 0.5682 0.4016 0.0190 0.105 Uiso 1 1 calc R . .
H10B H 0.6421 0.4285 -0.0327 0.105 Uiso 1 1 calc R . .
H10C H 0.5754 0.4623 0.0245 0.105 Uiso 1 1 calc R . .
C11 C 0.4941(5) 0.3289(4) 0.5590(12) 0.043(2) Uani 1 1 d . . .
H11 H 0.5364 0.3049 0.5588 0.052 Uiso 1 1 calc R . .
C12 C 0.4854(8) 0.3486(6) 0.7134(14) 0.073(4) Uani 1 1 d . . .
H12A H 0.5295 0.3671 0.7417 0.109 Uiso 1 1 calc R . .
H12B H 0.4778 0.3199 0.7789 0.109 Uiso 1 1 calc R . .
H12C H 0.4431 0.3715 0.7183 0.109 Uiso 1 1 calc R . .
C13 C 0.4269(7) 0.2992(5) 0.5039(18) 0.076(4) Uani 1 1 d . . .
H13A H 0.3832 0.3205 0.5123 0.113 Uiso 1 1 calc R . .
H13B H 0.4206 0.2683 0.5617 0.113 Uiso 1 1 calc R . .
H13C H 0.4344 0.2898 0.4026 0.113 Uiso 1 1 calc R . .
C1S C 0.3383(11) 0.3738(8) 0.135(2) 0.120(8) Uani 1 1 d . . .
H1S H 0.3408 0.3939 0.2261 0.144 Uiso 1 1 calc R . .
Cl1 Cl 0.4243(3) 0.34495(19) 0.1050(5) 0.0998(14) Uani 1 1 d . . .
Cl2 Cl 0.2740(4) 0.3281(5) 0.1539(13) 0.247(6) Uani 1 1 d . . .
Cl3 Cl 0.3187(5) 0.4147(3) -0.0048(13) 0.233(5) Uani 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C1 Pd1 N3 174.1(3) . . ?
C1 Pd1 Br1 90.5(2) . . ?
N3 Pd1 Br1 92.3(2) . . ?
C1 Pd1 Br2 87.0(2) . . ?
N3 Pd1 Br2 90.3(2) . . ?
Br1 Pd1 Br2 177.16(4) . . ?
C1 N1 C2 109.5(7) . . ?
C1 N1 C8 123.3(7) . . ?
C2 N1 C8 127.0(7) . . ?
C1 N2 C7 109.0(7) . . ?
C1 N2 C11 123.1(7) . . ?
C7 N2 C11 128.0(7) . . ?
N3 N3 Pd1 118.2(8) 2_655 . ?
N1 C1 N2 108.2(7) . . ?
N1 C1 Pd1 124.3(6) . . ?
N2 C1 Pd1 127.4(6) . . ?
C7 C2 N1 106.4(7) . . ?
C7 C2 C3 121.0(9) . . ?
N1 C2 C3 132.7(9) . . ?
C4 C3 C2 117.3(11) . . ?
C3 C4 C5 122.5(10) . . ?
C4 C5 C6 120.8(10) . . ?
C5 C6 C7 117.3(11) . . ?
C2 C7 N2 106.9(7) . . ?
C2 C7 C6 121.2(9) . . ?
N2 C7 C6 132.0(9) . . ?
C10 C8 N1 112.7(9) . . ?
C10 C8 C9 114.6(11) . . ?
N1 C8 C9 110.1(9) . . ?
N2 C11 C12 111.7(9) . . ?
N2 C11 C13 109.7(9) . . ?
C12 C11 C13 113.5(10) . . ?
Cl2 C1S Cl3 112.3(11) . . ?
Cl2 C1S Cl1 109.3(11) . . ?
Cl3 C1S Cl1 109.7(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.958(8) . ?
Pd1 N3 2.133(8) . ?
Pd1 Br1 2.4187(12) . ?
Pd1 Br2 2.4324(12) . ?
N1 C1 1.340(10) . ?
N1 C2 1.389(11) . ?
N1 C8 1.488(12) . ?
N2 C1 1.344(11) . ?
N2 C7 1.391(11) . ?
N2 C11 1.465(12) . ?
N3 N3 1.437(14) 2_655 ?
C2 C7 1.381(14) . ?
C2 C3 1.398(13) . ?
C3 C4 1.371(16) . ?
C4 C5 1.384(18) . ?
C5 C6 1.384(16) . ?
C6 C7 1.406(13) . ?
C8 C10 1.483(16) . ?
C8 C9 1.505(16) . ?
C11 C12 1.514(17) . ?
C11 C13 1.529(16) . ?
C1S Cl2 1.67(2) . ?
C1S Cl3 1.70(2) . ?
C1S Cl1 1.75(2) . ?
