#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:48:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178535 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/41/4064181.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_4064181
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            'C38 H62 I4 N10 Pd2'
_chemical_formula_weight         1379.38
_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                81.020(3)
_cell_angle_beta                 85.403(3)
_cell_angle_gamma                66.200(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7000(11)
_cell_length_b                   10.0247(13)
_cell_length_c                   15.825(2)
_cell_measurement_reflns_used    879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.65
_cell_volume                     1247.1(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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15513
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    3.232
_exptl_absorpt_correction_T_max  0.7820
_exptl_absorpt_correction_T_min  0.2742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.704
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0477P)²+0.6900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                5112
_reflns_number_total             5698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101169x_si_001.cif
_cod_data_source_block           a374
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064181
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 0.10505(3) 0.49470(3) 0.105198(16) 0.01356(8) Uani 1 1 d .
I1 I 0.17020(3) 0.67940(3) 0.182307(17) 0.02217(8) Uani 1 1 d .
I2 I 0.01097(3) 0.31119(2) 0.043509(14) 0.01681(7) Uani 1 1 d .
N1 N 0.5436(4) -0.0083(3) 0.16436(19) 0.0178(6) Uani 1 1 d .
N2 N 0.6054(4) 0.0886(3) 0.1214(2) 0.0187(6) Uani 1 1 d .
N3 N 0.1298(4) 0.3204(3) 0.2740(2) 0.0207(7) Uani 1 1 d .
C1 C 0.1989(4) 0.3374(4) 0.2023(2) 0.0176(7) Uani 1 1 d .
C2 C 0.4968(4) 0.2266(4) 0.1303(2) 0.0179(7) Uani 1 1 d .
C3 C 0.3595(4) 0.2174(4) 0.1805(2) 0.0166(7) Uani 1 1 d .
C4 C 0.3942(4) 0.0671(4) 0.2011(2) 0.0169(7) Uani 1 1 d .
C5 C 0.5331(5) 0.3546(4) 0.0909(3) 0.0253(8) Uani 1 1 d .
H5A H 0.6333 0.3517 0.1168 0.038 Uiso 1 1 calc R
H5B H 0.4372 0.4455 0.1005 0.038 Uiso 1 1 calc R
H5C H 0.5531 0.3514 0.0293 0.038 Uiso 1 1 calc R
C6 C 0.7710(5) 0.0393(4) 0.0811(3) 0.0271(9) Uani 1 1 d .
H6A H 0.7910 0.1247 0.0518 0.041 Uiso 1 1 calc R
H6B H 0.7778 -0.0257 0.0394 0.041 Uiso 1 1 calc R
H6C H 0.8562 -0.0144 0.1247 0.041 Uiso 1 1 calc R
C7 C 0.6326(5) -0.1685(4) 0.1665(3) 0.0249(8) Uani 1 1 d .
H7A H 0.6072 -0.2183 0.2216 0.030 Uiso 1 1 calc R
H7B H 0.7552 -0.1944 0.1630 0.030 Uiso 1 1 calc R
C8 C 0.5823(5) -0.2232(5) 0.0935(3) 0.0301(9) Uani 1 1 d .
H8A H 0.4619 -0.2020 0.0983 0.045 Uiso 1 1 calc R
H8B H 0.6463 -0.3296 0.0960 0.045 Uiso 1 1 calc R
H8C H 0.6062 -0.1734 0.0389 0.045 Uiso 1 1 calc R
C9 C 0.2922(5) -0.0075(4) 0.2506(3) 0.0258(8) Uani 1 1 d .
H9A H 0.2943 -0.0870 0.2209 0.039 Uiso 1 1 calc R
H9B H 0.1761 0.0637 0.2558 0.039 Uiso 1 1 calc R
H9C H 0.3390 -0.0485 0.3077 0.039 Uiso 1 1 calc R
C10 C -0.0394(5) 0.4245(4) 0.2944(2) 0.0224(8) Uani 1 1 d .
H10 H -0.0738 0.5117 0.2488 0.027 Uiso 1 1 calc R
C11 C -0.0393(6) 0.4755(5) 0.3800(3) 0.0319(10) Uani 1 1 d .
H11A H 0.0374 0.5271 0.3766 0.038 Uiso 1 1 calc R
H11B H 0.0016 0.3892 0.4250 0.038 Uiso 1 1 calc R
C12 C -0.2185(6) 0.5801(6) 0.4037(3) 0.0457(13) Uani 1 1 d .
H12A H -0.2181 0.6082 0.4609 0.055 Uiso 1 1 calc R
H12B H -0.2543 0.6709 0.3618 0.055 Uiso 1 1 calc R
C13 C -0.3417(6) 0.5094(6) 0.4045(3) 0.0498(14) Uani 1 1 d .
H13A H -0.4562 0.5818 0.4159 0.060 Uiso 1 1 calc R
H13B H -0.3141 0.4258 0.4513 0.060 Uiso 1 1 calc R
C14 C -0.3389(6) 0.4542(5) 0.3197(3) 0.0404(12) Uani 1 1 d .
H14A H -0.3799 0.5390 0.2739 0.048 Uiso 1 1 calc R
H14B H -0.4152 0.4020 0.3239 0.048 Uiso 1 1 calc R
C15 C -0.1613(5) 0.3501(5) 0.2968(3) 0.0315(10) Uani 1 1 d .
H15A H -0.1245 0.2607 0.3397 0.038 Uiso 1 1 calc R
H15B H -0.1612 0.3197 0.2402 0.038 Uiso 1 1 calc R
N2S N 0.6568(6) 0.1051(5) 0.5208(3) 0.0465(11) Uani 1 1 d .
C3S C 0.5559(6) 0.1508(5) 0.4711(3) 0.0338(10) Uani 1 1 d .
C4S C 0.4251(6) 0.2101(5) 0.4053(3) 0.0351(10) Uani 1 1 d .
H4S1 H 0.3763 0.3178 0.3995 0.053 Uiso 1 1 calc R
H4S2 H 0.3369 0.1734 0.4223 0.053 Uiso 1 1 calc R
H4S3 H 0.4754 0.1784 0.3504 0.053 Uiso 1 1 calc R
C2S C 1.0041(6) -0.1388(6) 0.4042(3) 0.0439(12) Uani 1 1 d .
H1SA H 1.0685 -0.0800 0.4098 0.066 Uiso 1 1 calc R
H1SB H 1.0787 -0.2317 0.3841 0.066 Uiso 1 1 calc R
H1SC H 0.9546 -0.1596 0.4599 0.066 Uiso 1 1 calc R
N1S N 0.7676(6) 0.0057(5) 0.2962(3) 0.0529(12) Uani 1 1 d .
C1S C 0.8723(6) -0.0584(5) 0.3436(3) 0.0356(10) 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'
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'
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 I1 90.42(10) .
C1 Pd1 I2 86.91(10) .
I1 Pd1 I2 172.711(13) .
C1 Pd1 I2 173.12(10) 2_565
I1 Pd1 I2 95.230(14) 2_565
I2 Pd1 I2 87.937(13) 2_565
Pd1 I2 Pd1 92.063(13) 2_565
C4 N1 N2 109.1(3) .
C4 N1 C7 128.3(3) .
N2 N1 C7 122.6(3) .
C2 N2 N1 109.2(3) .
C2 N2 C6 128.9(3) .
N1 N2 C6 121.7(3) .
C1 N3 C10 120.9(3) .
N3 C1 C3 118.3(3) .
N3 C1 Pd1 127.7(3) .
C3 C1 Pd1 113.3(2) .
N2 C2 C3 107.7(3) .
N2 C2 C5 120.9(3) .
C3 C2 C5 131.4(3) .
C4 C3 C2 106.2(3) .
C4 C3 C1 124.2(3) .
C2 C3 C1 129.3(3) .
N1 C4 C3 107.8(3) .
N1 C4 C9 122.2(3) .
C3 C4 C9 130.0(3) .
N1 C7 C8 111.8(3) .
N3 C10 C15 109.1(3) .
N3 C10 C11 109.7(3) .
C15 C10 C11 110.8(3) .
C10 C11 C12 110.0(4) .
C13 C12 C11 111.6(4) .
C12 C13 C14 111.6(4) .
C13 C14 C15 110.8(4) .
C10 C15 C14 110.7(4) .
N2S C3S C4S 179.4(5) .
N1S C1S C2S 179.5(6) .
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(4) .
Pd1 I1 2.6271(4) .
Pd1 I2 2.6290(4) .
Pd1 I2 2.7765(4) 2_565
I2 Pd1 2.7765(4) 2_565
N1 C4 1.350(4) .
N1 N2 1.361(4) .
N1 C7 1.471(5) .
N2 C2 1.346(4) .
N2 C6 1.451(5) .
N3 C1 1.261(5) .
N3 C10 1.466(5) .
C1 C3 1.489(5) .
C2 C3 1.407(5) .
C2 C5 1.476(5) .
C3 C4 1.401(5) .
C4 C9 1.484(5) .
C7 C8 1.517(6) .
C10 C15 1.518(6) .
C10 C11 1.522(5) .
C11 C12 1.542(6) .
C12 C13 1.503(8) .
C13 C14 1.525(8) .
C14 C15 1.528(6) .
N2S C3S 1.129(6) .
C3S C4S 1.478(6) .
C2S C1S 1.439(7) .
N1S C1S 1.137(6) .
