#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075473.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_4075473
loop_
_publ_author_name
'Wang, Xin'
'Liu, Shuang'
'Weng, Lin-Hong'
'Jin, Guo-Xin'
_publ_section_title
;
 A Trinuclear Silver(I) Functionalized N-Heterocyclic Carbene Complex and
 Its Use in Transmetalation:  Structure and Catalytic Activity for
 Olefin Polymerization†
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3565
_journal_paper_doi               10.1021/om060309c
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C10 H11 Cl2 N3 Pd'
_chemical_formula_weight         350.52
_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                104.258(4)
_cell_angle_beta                 98.156(5)
_cell_angle_gamma                98.661(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4682(18)
_cell_length_b                   8.5914(18)
_cell_length_c                   9.122(2)
_cell_measurement_temperature    293(2)
_cell_volume                     624.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.626
_diffrn_measured_fraction_theta_max 0.626
_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  0.0064
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            1409
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.888
_exptl_absorpt_correction_T_max  0.9115
_exptl_absorpt_correction_T_min  0.6497
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0464P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                1146
_reflns_number_total             1376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060309csi20060406_041759.cif
_cod_data_source_block           f50826a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075473
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 0.77089(6) 0.99909(8) 0.07883(7) 0.0347(2) Uani 1 1 d .
Cl1 Cl 0.9023(2) 1.2640(3) 0.2102(2) 0.0504(7) Uani 1 1 d .
Cl2 Cl 0.7092(2) 1.0712(3) -0.1536(2) 0.0508(6) Uani 1 1 d .
N1 N 0.7772(7) 0.9754(9) 0.4066(8) 0.039(2) Uani 1 1 d .
N2 N 0.8641(7) 0.7836(9) 0.2575(8) 0.039(2) Uani 1 1 d .
N3 N 0.6755(6) 0.7587(8) -0.0361(7) 0.0350(18) Uani 1 1 d .
C1 C 0.8071(8) 0.9261(12) 0.2670(10) 0.047(3) Uani 1 1 d .
C2 C 0.8183(10) 0.8681(13) 0.4917(10) 0.054(3) Uani 1 1 d .
H2 H 0.8107 0.8780 0.5942 0.064 Uiso 1 1 calc R
C3 C 0.8697(9) 0.7506(12) 0.4002(10) 0.047(3) Uani 1 1 d .
H3 H 0.9038 0.6612 0.4260 0.056 Uiso 1 1 calc R
C4 C 0.8975(8) 0.6859(12) 0.1196(10) 0.041(2) Uani 1 1 d .
H4A H 0.9296 0.5876 0.1380 0.049 Uiso 1 1 calc R
H4B H 0.9872 0.7462 0.0885 0.049 Uiso 1 1 calc R
C5 C 0.7490(9) 0.6388(11) -0.0086(9) 0.038(2) Uani 1 1 d .
C6 C 0.6951(9) 0.4794(11) -0.0945(10) 0.048(3) Uani 1 1 d .
H6 H 0.7503 0.3977 -0.0779 0.057 Uiso 1 1 calc R
C7 C 0.5579(10) 0.4438(12) -0.2053(12) 0.053(3) Uani 1 1 d .
H7 H 0.5172 0.3358 -0.2622 0.063 Uiso 1 1 calc R
C8 C 0.4808(10) 0.5625(12) -0.2334(11) 0.053(3) Uani 1 1 d .
H8 H 0.3897 0.5382 -0.3112 0.064 Uiso 1 1 calc R
C9 C 0.5403(9) 0.7208(12) -0.1440(9) 0.048(3) Uani 1 1 d .
H9 H 0.4854 0.8032 -0.1589 0.058 Uiso 1 1 calc R
C10 C 0.7046(10) 1.1161(12) 0.4615(10) 0.058(3) Uani 1 1 d .
H10A H 0.7648 1.2107 0.4423 0.087 Uiso 1 1 calc R
H10B H 0.7069 1.1352 0.5701 0.087 Uiso 1 1 calc R
H10C H 0.5940 1.0956 0.4085 0.087 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'
Cl Cl 0.1484 0.1585 '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 86.9(3)
C1 Pd1 Cl1 91.6(3)
N3 Pd1 Cl1 174.68(17)
C1 Pd1 Cl2 175.6(2)
N3 Pd1 Cl2 89.53(16)
Cl1 Pd1 Cl2 92.18(7)
C1 N1 C2 110.0(9)
C1 N1 C10 124.9(6)
C2 N1 C10 125.0(8)
C1 N2 C3 107.8(8)
C1 N2 C4 123.7(6)
C3 N2 C4 128.4(7)
C5 N3 C9 119.2(8)
C5 N3 Pd1 121.0(5)
C9 N3 Pd1 119.8(6)
N1 C1 N2 107.0(6)
N1 C1 Pd1 134.9(7)
N2 C1 Pd1 117.8(7)
C3 C2 N1 107.2(7)
C2 C3 N2 107.9(7)
N2 C4 C5 110.8(7)
N3 C5 C6 121.5(7)
N3 C5 C4 117.6(8)
C6 C5 C4 120.8(8)
C7 C6 C5 118.2(8)
C8 C7 C6 121.1(10)
C7 C8 C9 118.3(8)
N3 C9 C8 121.5(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C1 1.968(7)
Pd1 N3 2.051(7)
Pd1 Cl1 2.317(2)
Pd1 Cl2 2.3626(17)
N1 C1 1.312(11)
N1 C2 1.395(9)
N1 C10 1.451(12)
N2 C1 1.370(11)
N2 C3 1.394(9)
N2 C4 1.421(12)
N3 C5 1.337(9)
N3 C9 1.339(9)
C2 C3 1.314(13)
C4 C5 1.519(10)
C5 C6 1.371(12)
C6 C7 1.369(11)
C7 C8 1.346(11)
C8 C9 1.379(13)
