#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:12:02 +0100 (Tue 22 de Mar de 2016) $
#$Revision: 178940 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/69/4116919.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_4116919
loop_
_publ_author_name
'F. Albert Cotton'
'Jiande Gu'
'Carlos A. Murillo'
'Daren J. Timmons'
_publ_section_title
;
 The First Dinuclear Complex of Palladium(III)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13280
_journal_page_last               13281
_journal_paper_doi               10.1021/ja9832313
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C28 H48 Cl2 N12 Pd2'
_chemical_formula_weight         836.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.502(3)
_cell_length_b                   10.502(3)
_cell_length_c                   14.500(8)
_cell_measurement_reflns_used    190
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      6.75
_cell_volume                     1599.2(11)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5 (SIEMENS)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5310
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.392
_refine_ls_goodness_of_fit_obs   1.428
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.399
_refine_ls_restrained_S_obs      1.428
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_obs          0.0469
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+14.0706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0955
_refine_ls_wR_factor_obs         0.0917
_reflns_number_observed          479
_reflns_number_total             534
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9832313.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'NOREF' changed to 'noref'
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 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+14.0706P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+14.0706P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               4116919
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0194(4) 0.0194(4) 0.0118(5) 0.000 0.000 0.000
Cl1 0.0333(13) 0.0333(13) 0.012(2) 0.000 0.000 0.000
N11 0.025(3) 0.025(3) 0.015(3) 0.000(3) 0.006(3) 0.006(3)
N13 0.038(3) 0.038(3) 0.027(4) 0.005(4) 0.005(4) 0.026(5)
C11 0.038(5) 0.038(5) 0.029(4) 0.013(4) 0.011(4) 0.015(4)
C12 0.046(6) 0.065(7) 0.049(6) 0.023(5) 0.026(5) 0.016(5)
C13 0.049(6) 0.060(6) 0.036(5) 0.006(5) 0.015(5) 0.029(5)
C17 0.025(3) 0.025(3) 0.021(5) 0.007(4) 0.007(4) -0.001(5)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.2500 0.2500 0.66755(7) 0.0168(4) Uani 1 d S
Cl1 Cl 0.2500 0.2500 0.4969(2) 0.0261(8) Uani 1 d S
N11 N 0.4122(6) 0.1447(6) 0.6755(4) 0.0220(15) Uani 1 d .
N13 N 0.5200(5) -0.0200(5) 0.7500 0.034(2) Uani 1 d S
C11 C 0.5098(8) 0.1600(8) 0.6074(6) 0.035(2) Uani 1 d .
H11A H 0.5320(8) 0.2495(8) 0.6033(6) 0.042 Uiso 1 calc R
H11B H 0.4765(8) 0.1339(8) 0.5480(6) 0.042 Uiso 1 calc R
C12 C 0.6274(9) 0.0854(9) 0.6274(7) 0.053(3) Uani 1 d .
H12A H 0.6743(9) 0.0719(9) 0.5706(7) 0.064 Uiso 1 calc R
H12B H 0.6813(9) 0.1332(9) 0.6692(7) 0.064 Uiso 1 calc R
C13 C 0.5956(9) -0.0391(9) 0.6692(6) 0.048(3) Uani 1 d .
H13A H 0.5489(9) -0.0907(9) 0.6251(6) 0.058 Uiso 1 calc R
H13B H 0.6732(9) -0.0840(9) 0.6853(6) 0.058 Uiso 1 calc R
C17 C 0.4284(7) 0.0716(7) 0.7500 0.023(2) Uani 1 d S
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
N11 Pd1 N11 89.81(2) . 3 y
N11 Pd1 N11 173.5(3) . 2 y
N11 Pd1 N11 89.82(2) 3 2 ?
N11 Pd1 N11 89.81(2) . 4 ?
N11 Pd1 N11 173.5(3) 3 4 ?
N11 Pd1 N11 89.81(2) 2 4 ?
N11 Pd1 Pd1 86.7(2) . 5_556 y
N11 Pd1 Pd1 86.7(2) 3 5_556 ?
N11 Pd1 Pd1 86.7(2) 2 5_556 ?
N11 Pd1 Pd1 86.7(2) 4 5_556 ?
N11 Pd1 Cl1 93.3(2) . . ?
N11 Pd1 Cl1 93.3(2) 3 . ?
N11 Pd1 Cl1 93.3(2) 2 . ?
N11 Pd1 Cl1 93.3(2) 4 . ?
Pd1 Pd1 Cl1 180.0 5_556 . ?
C17 N11 C11 122.0(6) . . ?
C17 N11 Pd1 117.7(5) . . ?
C11 N11 Pd1 120.0(5) . . ?
C17 N13 C13 119.5(4) . . ?
C17 N13 C13 119.5(4) . 8_556 ?
C13 N13 C13 121.0(9) . 8_556 ?
N11 C11 C12 113.6(6) . . ?
C13 C12 C11 110.9(8) . . ?
N13 C13 C12 109.7(7) . . ?
N11 C17 N11 120.4(9) 8_556 . y
N11 C17 N13 119.8(4) 8_556 . ?
N11 C17 N13 119.8(4) . . ?
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 Pd1 2.391(2) 5_556 y
Pd1 Cl1 2.474(4) . y
Pd1 N11 2.034(6) . y
Pd1 N11 2.034(6) 3 ?
Pd1 N11 2.034(6) 2 ?
Pd1 N11 2.034(6) 4 ?
N11 C17 1.336(7) . ?
N11 C11 1.433(9) . ?
N13 C17 1.359(12) . ?
N13 C13 1.430(9) . ?
N13 C13 1.430(9) 8_556 ?
C11 C12 1.490(12) . ?
C12 C13 1.479(12) . ?
C17 N11 1.336(7) 8_556 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 Pd1 Pd1 N11 -24.0(3) 5_556 8_556 y
