#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:48:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178535 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/41/4064177.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_4064177
loop_
_publ_author_name
'Han, Yuan'
'Yuan, Dan'
'Teng, Qiaoqiao'
'Huynh, Han Vinh'
_publ_section_title
;
 Reactivity Differences of Palladium(II) Dimers Bearing Heterocyclic
 Carbenes with Two, One, or No α-Nitrogen Atoms toward Isocyanides
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1224
_journal_paper_doi               10.1021/om101169x
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C20 H36 Cl8 I4 N4 Pd2'
_chemical_formula_weight         1336.53
_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                66.564(17)
_cell_angle_beta                 75.026(16)
_cell_angle_gamma                80.789(16)
_cell_formula_units_Z            1
_cell_length_a                   9.306(8)
_cell_length_b                   10.916(8)
_cell_length_c                   10.961(9)
_cell_measurement_reflns_used    2456
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.27
_cell_volume                     984.9(14)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6632
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    4.609
_exptl_absorpt_correction_T_max  0.6557
_exptl_absorpt_correction_T_min  0.1407
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0467
_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)+(0.0690P)²+2.3384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                3411
_reflns_number_total             4446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101169x_si_001.cif
_cod_data_source_block           7555
_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_cell_volume        984.9(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064177
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 0.10908(5) 0.34972(4) -0.03168(5) 0.03229(14) Uani 1 1 d . . .
I1 I 0.12226(5) 0.48365(5) 0.11185(5) 0.04422(16) Uani 1 1 d . . .
I2 I 0.09862(5) 0.20888(5) -0.16765(5) 0.04749(16) Uani 1 1 d . . .
N1 N 0.4194(6) 0.0653(5) 0.1437(6) 0.0419(13) Uani 1 1 d . . .
N2 N 0.5130(6) 0.1607(6) 0.0529(6) 0.0430(13) Uani 1 1 d . . .
C1 C 0.2812(7) 0.2321(6) 0.0330(7) 0.0359(13) Uani 1 1 d . . .
C2 C 0.2809(7) 0.1078(6) 0.1310(7) 0.0375(14) Uani 1 1 d . . .
C3 C 0.4277(7) 0.2638(6) -0.0129(7) 0.0407(15) Uani 1 1 d . . .
C4 C 0.1522(8) 0.0261(7) 0.2153(8) 0.0527(18) Uani 1 1 d . . .
H4A H 0.1353 -0.0294 0.1704 0.079 Uiso 1 1 calc R . .
H4B H 0.0640 0.0846 0.2269 0.079 Uiso 1 1 calc R . .
H4C H 0.1731 -0.0304 0.3037 0.079 Uiso 1 1 calc R . .
C5 C 0.4948(8) 0.3873(8) -0.1231(9) 0.056(2) Uani 1 1 d . . .
H5A H 0.4176 0.4590 -0.1423 0.084 Uiso 1 1 calc R . .
H5B H 0.5400 0.3690 -0.2048 0.084 Uiso 1 1 calc R . .
H5C H 0.5703 0.4139 -0.0934 0.084 Uiso 1 1 calc R . .
C6 C 0.4760(9) -0.0611(8) 0.2388(9) 0.065(2) Uani 1 1 d . . .
H6A H 0.4868 -0.0477 0.3182 0.097 Uiso 1 1 calc R . .
H6B H 0.5720 -0.0893 0.1939 0.097 Uiso 1 1 calc R . .
H6C H 0.4063 -0.1294 0.2666 0.097 Uiso 1 1 calc R . .
C7 C 0.6700(8) 0.1499(8) 0.0476(9) 0.058(2) Uani 1 1 d . . .
H7A H 0.7201 0.2078 -0.0431 0.069 Uiso 1 1 calc R . .
H7B H 0.7082 0.0576 0.0605 0.069 Uiso 1 1 calc R . .
C8 C 0.7086(12) 0.1865(12) 0.1500(11) 0.093(4) Uani 1 1 d . . .
H8A H 0.6626 0.2743 0.1443 0.140 Uiso 1 1 calc R . .
H8B H 0.8160 0.1881 0.1332 0.140 Uiso 1 1 calc R . .
H8C H 0.6726 0.1212 0.2401 0.140 Uiso 1 1 calc R . .
C1S C 0.2179(13) 0.2279(11) 0.4539(12) 0.121(5) Uani 1 1 d D . .
H1S1 H 0.1594 0.2689 0.3832 0.146 Uiso 1 1 calc R . .
H1S2 H 0.1789 0.2667 0.5236 0.146 Uiso 1 1 calc R . .
Cl1A Cl 0.3965(5) 0.2621(6) 0.3852(7) 0.201(3) Uani 1 1 d D . .
Cl1B Cl 0.1984(6) 0.0602(5) 0.5253(5) 0.1492(16) Uani 1 1 d D . .
C2S C 0.7921(14) 0.4324(12) 0.4285(13) 0.125(5) Uani 1 1 d D . .
H2S1 H 0.6948 0.4825 0.4330 0.150 Uiso 1 1 calc R A .
H2S2 H 0.8652 0.4894 0.3541 0.150 Uiso 1 1 calc R . .
Cl2A Cl 0.8481(4) 0.3777(4) 0.5842(4) 0.1224(12) Uani 1 1 d DU A .
Cl2B Cl 0.7819(10) 0.2844(8) 0.4058(8) 0.151(3) Uani 0.60 1 d PDU A -1
Cl2C Cl 0.633(2) 0.370(2) 0.4533(16) 0.158(8) Uani 0.25 1 d PDU A -2
Cl2D Cl 0.626(2) 0.492(2) 0.494(2) 0.121(8) Uani 0.15 1 d PDU A -3
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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_3
C1 Pd1 I2 89.10(19) .
C1 Pd1 I1 89.25(19) .
I2 Pd1 I1 177.94(2) .
C1 Pd1 I1 177.00(19) 2_565
I2 Pd1 I1 93.90(5) 2_565
I1 Pd1 I1 87.76(5) 2_565
Pd1 I1 Pd1 92.24(5) 2_565
C2 N1 N2 109.2(5) .
C2 N1 C6 129.4(6) .
N2 N1 C6 121.3(6) .
C3 N2 N1 106.6(5) .
C3 N2 C7 129.8(6) .
N1 N2 C7 123.2(6) .
C2 C1 C3 106.0(6) .
C2 C1 Pd1 128.3(5) .
C3 C1 Pd1 125.7(5) .
N1 C2 C1 108.9(6) .
N1 C2 C4 122.5(6) .
C1 C2 C4 128.7(6) .
N2 C3 C1 109.2(6) .
N2 C3 C5 121.2(6) .
C1 C3 C5 129.5(6) .
N2 C7 C8 114.0(8) .
Cl1A C1S Cl1B 111.4(7) .
Cl2C C2S Cl2D 55.7(11) .
Cl2C C2S Cl2B 57.3(10) .
Cl2D C2S Cl2B 112.7(10) .
Cl2C C2S Cl2A 109.4(8) .
Cl2D C2S Cl2A 91.7(12) .
Cl2B C2S Cl2A 104.1(7) .
C2S Cl2A Cl2D 42.7(6) .
C2S Cl2D Cl2A 45.6(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 1.980(6) .
Pd1 I2 2.5572(15) .
Pd1 I1 2.5719(15) .
Pd1 I1 2.6774(17) 2_565
I1 Pd1 2.6774(17) 2_565
N1 C2 1.321(8) .
N1 N2 1.361(8) .
N1 C6 1.475(9) .
N2 C3 1.334(8) .
N2 C7 1.435(9) .
C1 C2 1.354(9) .
C1 C3 1.374(9) .
C2 C4 1.483(9) .
C3 C5 1.501(9) .
C7 C8 1.469(14) .
C1S Cl1A 1.673(12) .
C1S Cl1B 1.699(12) .
C2S Cl2C 1.647(14) .
C2S Cl2D 1.670(16) .
C2S Cl2B 1.750(12) .
C2S Cl2A 1.758(12) .
Cl2A Cl2D 2.46(3) .
