#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:46:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179262 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/82/4318261.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_4318261
loop_
_publ_author_name
'Zengquan Qin'
'Michael C. Jennings'
'Richard J. Puddephatt'
_publ_section_title
;
 Molecular Triangle of Palladium(II) and Its Anion Binding Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3967
_journal_page_last               3974
_journal_paper_doi               10.1021/ic020227q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C18 H24 Cl2 N2 Pd'
_chemical_formula_weight         445.69
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.632(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4164(7)
_cell_length_b                   19.215(2)
_cell_length_c                   13.0162(14)
_cell_measurement_temperature    200(2)
_cell_volume                     1842.5(3)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi/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  0.151
_diffrn_reflns_av_sigmaI/netI    0.2562
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12565
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.9427
_exptl_absorpt_correction_T_min  0.7915
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                1316
_reflns_number_total             3098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020227q_1.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318261
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Pd Pd 0.74161(8) 0.58060(3) 1.12720(5) 0.0311(2) Uani 1 1 d . . .
Cl1 Cl 0.7909(2) 0.69796(10) 1.14059(16) 0.0472(6) Uani 1 1 d . . .
Cl2 Cl 0.6946(2) 0.57687(11) 1.29715(14) 0.0454(6) Uani 1 1 d . . .
N1 N 0.7152(7) 0.4766(3) 1.1037(5) 0.0270(18) Uani 1 1 d . . .
C2 C 0.6913(8) 0.4288(5) 1.1755(5) 0.037(2) Uani 1 1 d . . .
H2A H 0.6747 0.4445 1.2430 0.045 Uiso 1 1 calc R . .
C3 C 0.6893(9) 0.3586(4) 1.1575(6) 0.039(2) Uani 1 1 d . . .
H3A H 0.6701 0.3272 1.2115 0.047 Uiso 1 1 calc R . .
C4 C 0.7153(9) 0.3331(4) 1.0607(6) 0.027(2) Uani 1 1 d . . .
C5 C 0.7375(8) 0.3834(4) 0.9845(6) 0.025(2) Uani 1 1 d . . .
H5A H 0.7510 0.3687 0.9162 0.030 Uiso 1 1 calc R . .
C6 C 0.7401(9) 0.4536(5) 1.0070(6) 0.023(2) Uani 1 1 d . . .
C7 C 0.7603(8) 0.5093(4) 0.9330(6) 0.021(2) Uani 1 1 d . . .
C8 C 0.7698(8) 0.5000(4) 0.8286(6) 0.028(2) Uani 1 1 d . . .
H8A H 0.7660 0.4541 0.8013 0.033 Uiso 1 1 calc R . .
C9 C 0.7847(9) 0.5557(4) 0.7623(6) 0.023(2) Uani 1 1 d . . .
C10 C 0.7937(8) 0.6212(4) 0.8083(6) 0.030(2) Uani 1 1 d . . .
H10A H 0.8060 0.6613 0.7668 0.036 Uiso 1 1 calc R . .
C11 C 0.7850(8) 0.6290(4) 0.9124(6) 0.027(2) Uani 1 1 d . . .
H11A H 0.7899 0.6745 0.9411 0.033 Uiso 1 1 calc R . .
N12 N 0.7699(6) 0.5750(4) 0.9742(4) 0.0247(16) Uani 1 1 d . . .
C13 C 0.7214(9) 0.2552(4) 1.0411(6) 0.033(2) Uani 1 1 d . . .
C14 C 0.5518(9) 0.2209(4) 1.0806(5) 0.047(2) Uani 1 1 d . . .
H14A H 0.5552 0.1705 1.0694 0.070 Uiso 1 1 calc R . .
H14B H 0.4413 0.2402 1.0426 0.070 Uiso 1 1 calc R . .
H14C H 0.5522 0.2304 1.1546 0.070 Uiso 1 1 calc R . .
C15 C 0.7206(8) 0.2379(4) 0.9271(5) 0.043(2) Uani 1 1 d . . .
H15A H 0.8288 0.2578 0.9017 0.065 Uiso 1 1 calc R . .
H15B H 0.6116 0.2576 0.8879 0.065 Uiso 1 1 calc R . .
H15C H 0.7209 0.1873 0.9181 0.065 Uiso 1 1 calc R . .
C16 C 0.8928(9) 0.2252(4) 1.1039(6) 0.057(3) Uani 1 1 d . . .
H16A H 1.0010 0.2455 1.0792 0.085 Uiso 1 1 calc R . .
H16B H 0.8949 0.1745 1.0951 0.085 Uiso 1 1 calc R . .
H16C H 0.8914 0.2363 1.1772 0.085 Uiso 1 1 calc R . .
C17 C 0.7825(9) 0.5483(4) 0.6450(6) 0.027(2) Uani 1 1 d . . .
C18 C 0.9402(9) 0.5893(4) 0.6062(5) 0.050(2) Uani 1 1 d . . .
H18A H 1.0560 0.5712 0.6396 0.075 Uiso 1 1 calc R . .
H18B H 0.9292 0.6386 0.6232 0.075 Uiso 1 1 calc R . .
H18C H 0.9356 0.5839 0.5311 0.075 Uiso 1 1 calc R . .
C19 C 0.5999(8) 0.5783(4) 0.5952(5) 0.046(2) Uani 1 1 d . . .
H19A H 0.4997 0.5526 0.6205 0.069 Uiso 1 1 calc R . .
H19B H 0.5923 0.5737 0.5198 0.069 Uiso 1 1 calc R . .
H19C H 0.5916 0.6275 0.6136 0.069 Uiso 1 1 calc R . .
C20 C 0.7958(9) 0.4718(4) 0.6134(5) 0.039(2) Uani 1 1 d . . .
H20A H 0.6949 0.4456 0.6370 0.058 Uiso 1 1 calc R . .
H20B H 0.9112 0.4524 0.6450 0.058 Uiso 1 1 calc R . .
H20C H 0.7897 0.4686 0.5379 0.058 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd N12 79.6(3) . . ?
N1 Pd Cl2 95.3(2) . . ?
N12 Pd Cl2 174.39(19) . . ?
N1 Pd Cl1 174.1(2) . . ?
N12 Pd Cl1 95.4(2) . . ?
Cl2 Pd Cl1 89.89(8) . . ?
C2 N1 C6 117.7(7) . . ?
C2 N1 Pd 126.2(6) . . ?
C6 N1 Pd 115.9(6) . . ?
N1 C2 C3 123.8(8) . . ?
C2 C3 C4 120.3(8) . . ?
C3 C4 C5 116.0(8) . . ?
C3 C4 C13 120.7(8) . . ?
C5 C4 C13 123.3(8) . . ?
C6 C5 C4 121.4(8) . . ?
N1 C6 C5 120.7(8) . . ?
N1 C6 C7 114.0(8) . . ?
C5 C6 C7 125.3(8) . . ?
N12 C7 C8 119.9(8) . . ?
N12 C7 C6 114.9(8) . . ?
C8 C7 C6 125.1(8) . . ?
C7 C8 C9 121.9(8) . . ?
C8 C9 C10 115.7(7) . . ?
C8 C9 C17 123.8(7) . . ?
C10 C9 C17 120.4(7) . . ?
C11 C10 C9 121.1(8) . . ?
N12 C11 C10 122.1(8) . . ?
C11 N12 C7 119.2(7) . . ?
C11 N12 Pd 125.4(6) . . ?
C7 N12 Pd 115.3(6) . . ?
C4 C13 C15 112.5(7) . . ?
C4 C13 C16 108.6(6) . . ?
C15 C13 C16 110.2(6) . . ?
C4 C13 C14 108.7(6) . . ?
C15 C13 C14 108.5(6) . . ?
C16 C13 C14 108.3(6) . . ?
C20 C17 C9 111.3(6) . . ?
C20 C17 C18 109.0(6) . . ?
C9 C17 C18 111.0(6) . . ?
C20 C17 C19 108.9(5) . . ?
C9 C17 C19 107.0(6) . . ?
C18 C17 C19 109.5(6) . . ?
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
Pd N1 2.028(6) . ?
Pd N12 2.029(6) . ?
Pd Cl2 2.280(2) . ?
Pd Cl1 2.288(2) . ?
N1 C2 1.336(8) . ?
N1 C6 1.367(8) . ?
C2 C3 1.370(9) . ?
C3 C4 1.385(9) . ?
C4 C5 1.408(9) . ?
C4 C13 1.520(9) . ?
C5 C6 1.380(9) . ?
C6 C7 1.460(9) . ?
C7 N12 1.370(8) . ?
C7 C8 1.380(8) . ?
C8 C9 1.387(9) . ?
C9 C10 1.392(9) . ?
C9 C17 1.531(9) . ?
C10 C11 1.373(8) . ?
C11 N12 1.325(8) . ?
C13 C15 1.520(9) . ?
C13 C16 1.542(8) . ?
C13 C14 1.559(9) . ?
C17 C20 1.533(8) . ?
C17 C18 1.542(9) . ?
C17 C19 1.544(8) . ?
