#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009378.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_7009378
loop_
_publ_author_name
'Schneider, Alexandra'
'Freisinger, Eva'
'Beck, Bettina'
'Lippert, Bernhard'
_publ_section_title
;
 Ready formation of water-stable PtII-(μ-NH2)-PdII species through
 combination of trans-[(NH3)2PtIIL2] (L = N,N'-heterocycle) and [enPd(H2O)2]2+
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              837
_journal_paper_doi               10.1039/b000456l
_journal_year                    2000
_chemical_formula_sum            'C5 H15 Br N5 O Pd Pt0.5'
_chemical_formula_weight         445.07
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                105.65(3)
_cell_angle_beta                 98.84(3)
_cell_angle_gamma                98.60(3)
_cell_formula_units_Z            2
_cell_length_a                   5.0470(10)
_cell_length_b                   9.580(2)
_cell_length_c                   13.568(3)
_cell_measurement_reflns_used    2464
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      3.13
_cell_volume                     611.5(3)
_computing_cell_refinement       'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius BV, Netherlands)'
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       Enraf-Nonius-KappaCCD
_diffrn_measurement_method
;
360 frames via ω-rotation (Δω\=1°) and two times 60s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2464
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    10.452
_exptl_absorpt_correction_T_max  0.6799
_exptl_absorpt_correction_T_min  0.0674
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.417
_exptl_crystal_description       stick
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0069(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.069
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.069
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_obs          0.0325
_refine_ls_shift/esd_max         -0.029
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0587P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_obs         0.0827
_reflns_number_observed          2070
_reflns_number_total             2464
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000456l.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] 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^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        611.5(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C5 H15 Br N5 O Pd Pt0.50'
_cod_database_code               7009378
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0.5000 0.0000 0.0000 0.03600(14) Uani 1 d S .
N11 N 0.2518(11) 0.1513(6) 0.0209(4) 0.0406(11) Uani 1 d . .
H11A H 0.3398(11) 0.2343(6) 0.0117(4) 0.045(13) Uiso 1 calc R .
H11B H 0.1012(11) 0.1157(6) -0.0303(4) 0.045(13) Uiso 1 calc R .
Pd1 Pd 0.12825(9) 0.20894(5) 0.15775(3) 0.0404(2) Uani 1 d . .
N21 N -0.0053(14) 0.2819(8) 0.2968(5) 0.061(2) Uani 1 d . .
H21A H -0.1208(14) 0.2072(8) 0.3058(5) 0.090(11) Uiso 1 calc R .
H21B H 0.1386(14) 0.3121(8) 0.3510(5) 0.090(11) Uiso 1 calc R .
N22 N 0.0130(11) 0.3924(6) 0.1325(5) 0.0508(13) Uani 1 d . .
H22A H 0.1363(11) 0.4367(6) 0.1034(5) 0.090(11) Uiso 1 calc R .
H22B H -0.1503(11) 0.3668(6) 0.0881(5) 0.090(11) Uiso 1 calc R .
C21 C -0.1468(17) 0.4063(9) 0.2934(6) 0.059(2) Uani 1 d . .
H21C H -0.1376(17) 0.4685(9) 0.3638(6) 0.090(11) Uiso 1 calc R .
H21D H -0.3378(17) 0.3683(9) 0.2598(6) 0.090(11) Uiso 1 calc R .
C22 C -0.0061(18) 0.4952(9) 0.2324(6) 0.063(2) Uani 1 d . .
H22C H -0.1104(18) 0.5681(9) 0.2197(6) 0.090(11) Uiso 1 calc R .
H22D H 0.1754(18) 0.5468(9) 0.2718(6) 0.090(11) Uiso 1 calc R .
N1 N 0.4329(10) -0.0352(6) 0.1344(4) 0.0412(11) Uani 1 d . .
N2 N 0.2697(12) 0.0395(6) 0.1916(4) 0.0465(13) Uani 1 d . .
C3 C 0.2684(17) -0.0089(9) 0.2763(6) 0.060(2) Uani 1 d . .
H3 H 0.1735(17) 0.0242(9) 0.3288(6) 0.058(12) Uiso 1 calc R .
C4 C 0.4230(17) -0.1109(9) 0.2741(6) 0.059(2) Uani 1 d . .
H4 H 0.4545(17) -0.1613(9) 0.3232(6) 0.058(12) Uiso 1 calc R .
C5 C 0.5248(16) -0.1262(8) 0.1856(5) 0.054(2) Uani 1 d . .
H5 H 0.6407(16) -0.1899(8) 0.1638(5) 0.058(12) Uiso 1 calc R .
O1W O 0.0135(18) 0.8529(10) 0.4953(7) 0.120(3) Uani 1 d . .
Br1 Br 0.5000 -0.5000 0.0000 0.0544(3) Uani 1 d S .
Br2 Br 0.4745(3) 0.6350(2) 0.48973(13) 0.0667(4) Uani 0.50 d P .
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'
O O 0.0106 0.0060 '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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 Pt1 N1 180.0 2_655 . ?
N1 Pt1 N11 92.0(2) 2_655 . ?
N1 Pt1 N11 88.0(2) . . ?
N1 Pt1 N11 88.0(2) 2_655 2_655 ?
N1 Pt1 N11 92.0(2) . 2_655 ?
N11 Pt1 N11 180.0 . 2_655 ?
Pd1 N11 Pt1 118.5(2) . . ?
Pd1 N11 H11A 107.7(2) . . ?
Pt1 N11 H11A 107.68(15) . . ?
Pd1 N11 H11B 107.68(15) . . ?
Pt1 N11 H11B 107.68(15) . . ?
H11A N11 H11B 107.1 . . ?
N2 Pd1 N11 88.4(2) . . ?
N2 Pd1 N22 175.1(2) . . ?
N11 Pd1 N22 93.0(2) . . ?
N2 Pd1 N21 95.6(2) . . ?
N11 Pd1 N21 176.0(2) . . ?
N22 Pd1 N21 83.0(2) . . ?
C21 N21 Pd1 109.4(5) . . ?
C21 N21 H21A 109.8(4) . . ?
Pd1 N21 H21A 109.8(2) . . ?
C21 N21 H21B 109.8(4) . . ?
Pd1 N21 H21B 109.8(2) . . ?
H21A N21 H21B 108.2 . . ?
C22 N22 Pd1 109.5(5) . . ?
C22 N22 H22A 109.8(4) . . ?
Pd1 N22 H22A 109.8(2) . . ?
C22 N22 H22B 109.8(4) . . ?
Pd1 N22 H22B 109.8(2) . . ?
H22A N22 H22B 108.2 . . ?
N21 C21 C22 108.2(6) . . ?
N21 C21 H21C 110.1(4) . . ?
C22 C21 H21C 110.1(4) . . ?
N21 C21 H21D 110.1(4) . . ?
C22 C21 H21D 110.1(5) . . ?
H21C C21 H21D 108.4 . . ?
N22 C22 C21 108.2(6) . . ?
N22 C22 H22C 110.1(4) . . ?
C21 C22 H22C 110.1(4) . . ?
N22 C22 H22D 110.1(4) . . ?
C21 C22 H22D 110.1(5) . . ?
H22C C22 H22D 108.4 . . ?
C5 N1 N2 107.2(5) . . ?
C5 N1 Pt1 131.2(5) . . ?
N2 N1 Pt1 121.6(4) . . ?
C3 N2 N1 106.7(5) . . ?
C3 N2 Pd1 130.6(5) . . ?
N1 N2 Pd1 121.9(4) . . ?
C4 C3 N2 110.4(6) . . ?
C4 C3 H3 124.8(4) . . ?
N2 C3 H3 124.8(4) . . ?
C3 C4 C5 106.0(6) . . ?
C3 C4 H4 127.0(4) . . ?
C5 C4 H4 127.0(4) . . ?
N1 C5 C4 109.7(6) . . ?
N1 C5 H5 125.2(4) . . ?
C4 C5 H5 125.2(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
Pt1 N1 2.010(5) 2_655 ?
Pt1 N1 2.010(5) . ?
Pt1 N11 2.044(5) . ?
Pt1 N11 2.044(5) 2_655 ?
N11 Pd1 2.011(5) . ?
N11 H11A 0.90 . ?
N11 H11B 0.90 . ?
Pd1 N2 2.001(5) . ?
Pd1 N22 2.028(5) . ?
Pd1 N21 2.079(6) . ?
N21 C21 1.486(9) . ?
N21 H21A 0.90 . ?
N21 H21B 0.90 . ?
N22 C22 1.472(9) . ?
N22 H22A 0.90 . ?
N22 H22B 0.90 . ?
C21 C22 1.515(12) . ?
C21 H21C 0.97 . ?
C21 H21D 0.97 . ?
C22 H22C 0.97 . ?
C22 H22D 0.97 . ?
N1 C5 1.344(8) . ?
N1 N2 1.366(7) . ?
N2 C3 1.351(8) . ?
C3 C4 1.336(10) . ?
C3 H3 0.93 . ?
C4 C5 1.358(10) . ?
C4 H4 0.93 . ?
C5 H5 0.93 . ?
Br2 Br2 2.721(4) 2_666 ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Pt1 N11 Pd1 -171.2(3) 2_655 . . . ?
N1 Pt1 N11 Pd1 8.8(3) . . . . ?
N11 Pt1 N11 Pd1 -103.7(1000) 2_655 . . . ?
Pt1 N11 Pd1 N2 -11.8(3) . . . . ?
Pt1 N11 Pd1 N22 163.5(3) . . . . ?
Pt1 N11 Pd1 N21 159.9(32) . . . . ?
N2 Pd1 N21 C21 -175.7(5) . . . . ?
N11 Pd1 N21 C21 12.7(36) . . . . ?
N22 Pd1 N21 C21 9.1(5) . . . . ?
N2 Pd1 N22 C22 -54.9(26) . . . . ?
N11 Pd1 N22 C22 -160.8(5) . . . . ?
N21 Pd1 N22 C22 18.9(5) . . . . ?
Pd1 N21 C21 C22 -34.4(7) . . . . ?
Pd1 N22 C22 C21 -43.0(7) . . . . ?
N21 C21 C22 N22 51.1(8) . . . . ?
N1 Pt1 N1 C5 -40.4(10) 2_655 . . . ?
N11 Pt1 N1 C5 180.0(6) . . . . ?
N11 Pt1 N1 C5 0.0(6) 2_655 . . . ?
N1 Pt1 N1 N2 139.4(5) 2_655 . . . ?
N11 Pt1 N1 N2 -0.2(5) . . . . ?
N11 Pt1 N1 N2 179.8(5) 2_655 . . . ?
C5 N1 N2 C3 0.1(7) . . . . ?
Pt1 N1 N2 C3 -179.7(5) . . . . ?
C5 N1 N2 Pd1 171.0(5) . . . . ?
Pt1 N1 N2 Pd1 -8.9(7) . . . . ?
N11 Pd1 N2 C3 -179.3(7) . . . . ?
N22 Pd1 N2 C3 74.6(26) . . . . ?
N21 Pd1 N2 C3 1.3(7) . . . . ?
N11 Pd1 N2 N1 12.2(5) . . . . ?
N22 Pd1 N2 N1 -93.9(24) . . . . ?
N21 Pd1 N2 N1 -167.2(5) . . . . ?
N1 N2 C3 C4 -0.3(9) . . . . ?
Pd1 N2 C3 C4 -170.1(6) . . . . ?
N2 C3 C4 C5 0.3(10) . . . . ?
N2 N1 C5 C4 0.1(8) . . . . ?
Pt1 N1 C5 C4 179.9(5) . . . . ?
C3 C4 C5 N1 -0.2(10) . . . . ?
