#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322119.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_4322119
loop_
_publ_author_name
'Jens Müller'
'Frank Glahé,'
'Eva Freisinger'
'Bernhard Lippert'
_publ_contact_author_address
; Fachbereich Chemie
  Universität Dortmund
  Otto-Hahn-Str. 6
  D-44221 Dortmund
  Germany
;
_publ_contact_author_email       lippert@pop.uni-dortmund.de
_publ_contact_author_fax         'Int. code + (231) 755-3797'
_publ_contact_author_name        'Prof. Bernhard Lippert'
_publ_contact_author_phone       'Int. code + (231) 755-3840'
_publ_section_title
;
 A Major, pH-Induced Stereochemical Switch of Pairs of trans-Oriented
 Ligands in Complexes of trans-a2PtII (a = NH3, CH3NH2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3160
_journal_page_last               3166
_journal_paper_doi               10.1021/ic990044c
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C6 H12 Cl N4 O5 Pt0.5'
_chemical_formula_weight         353.19
_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                112.40(3)
_cell_angle_beta                 106.07(3)
_cell_angle_gamma                94.66(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3920(10)
_cell_length_b                   9.072(2)
_cell_length_c                   10.047(2)
_cell_measurement_reflns_used    22225
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.59
_cell_volume                     585.2(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
;
475 frames via ω-rotation (Δω\=1°) and two times 45s 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  0.038
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22225
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    6.287
_exptl_absorpt_correction_T_max  0.4954
_exptl_absorpt_correction_T_min  0.3025
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0170(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.459
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_obs          0.0297
_refine_ls_shift/esd_max         -0.374
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0333P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0871
_refine_ls_wR_factor_obs         0.0600
_reflns_number_observed          2979
_reflns_number_total             3329
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990044c_2.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0333P)^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^)+(0.0333P)^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        585.2(2)
_cod_original_formula_sum        'C6 H12 Cl N4 O5 Pt0.50'
_cod_database_code               4322119
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 0.0000 0.0000 0.0000 0.04353(9) Uani 1 d S .
N8 N 0.2177(4) -0.0719(4) 0.1184(4) 0.0537(7) Uani 1 d . .
H8A H 0.2605(4) -0.1455(4) 0.0511(4) 0.075(10) Uiso 1 calc R .
H8B H 0.3155(4) 0.0151(4) 0.1773(4) 0.075(10) Uiso 1 calc R .
C8 C 0.1694(9) -0.1434(10) 0.2157(8) 0.107(2) Uani 1 d . .
H8C H 0.2821(20) -0.1697(61) 0.2692(47) 0.144(17) Uiso 1 calc R .
H8D H 0.0712(55) -0.2408(34) 0.1537(10) 0.144(17) Uiso 1 calc R .
H8E H 0.1232(71) -0.0666(24) 0.2882(39) 0.144(17) Uiso 1 calc R .
N1 N 0.5910(4) 0.5372(3) 0.2429(3) 0.0493(6) Uani 1 d . .
C1 C 0.7747(7) 0.6421(6) 0.2763(6) 0.0736(12) Uani 1 d . .
H1A H 0.8792(7) 0.5950(34) 0.3114(59) 0.153(17) Uiso 1 calc R .
H1B H 0.7858(35) 0.7482(20) 0.3541(44) 0.153(17) Uiso 1 calc R .
H1C H 0.7792(33) 0.6519(54) 0.1854(16) 0.153(17) Uiso 1 calc R .
C2 C 0.5321(5) 0.3922(4) 0.1162(4) 0.0456(7) Uani 1 d . .
O2 O 0.6193(4) 0.3496(3) 0.0267(3) 0.0601(6) Uani 1 d . .
N3 N 0.3614(4) 0.2965(3) 0.0945(3) 0.0442(6) Uani 1 d . .
H3 H 0.3201(4) 0.2050(3) 0.0148(3) 0.053(5) Uiso 1 calc R .
C4 C 0.2528(5) 0.3342(4) 0.1882(4) 0.0438(7) Uani 1 d . .
N4 N 0.1000(4) 0.2287(3) 0.1588(3) 0.0502(6) Uani 1 d . .
H4 H 0.0320(4) 0.2632(3) 0.2169(3) 0.053(5) Uiso 1 calc R .
C5 C 0.3187(6) 0.4910(4) 0.3145(4) 0.0529(8) Uani 1 d . .
H5 H 0.2470(6) 0.5282(4) 0.3788(4) 0.053(5) Uiso 1 calc R .
C6 C 0.4853(6) 0.5834(4) 0.3385(4) 0.0539(8) Uani 1 d . .
H6 H 0.5311(6) 0.6831(4) 0.4237(4) 0.053(5) Uiso 1 calc R .
Cl1 Cl 0.26818(12) -0.13889(10) -0.32602(9) 0.0508(2) Uani 1 d . .
O11 O 0.3418(37) -0.0444(34) -0.1544(24) 0.064(3) Uani 0.50 d P .
O12 O 0.1685(29) -0.2951(18) -0.3532(21) 0.084(5) Uani 0.50 d P .
O13 O 0.4194(24) -0.1617(25) -0.3847(24) 0.114(7) Uani 0.50 d P .
O14 O 0.1931(42) -0.0720(32) -0.4144(34) 0.179(14) Uani 0.50 d P .
O11A O 0.3238(44) -0.0252(35) -0.1832(26) 0.099(8) Uani 0.50 d P .
O12A O 0.1382(27) -0.2814(17) -0.3644(18) 0.106(6) Uani 0.50 d P .
O13A O 0.4379(22) -0.1817(22) -0.3563(21) 0.092(6) Uani 0.50 d P .
O14A O 0.1351(32) -0.0637(20) -0.4013(29) 0.119(6) 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'
Cl Cl 0.1484 0.1585 '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'
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
N4 Pt1 N4 180.0 2 . ?
N4 Pt1 N8 89.96(13) 2 2 ?
N4 Pt1 N8 90.04(13) . 2 ?
N4 Pt1 N8 90.04(13) 2 . ?
N4 Pt1 N8 89.96(13) . . ?
N8 Pt1 N8 180.0 2 . ?
C8 N8 Pt1 115.8(3) . . ?
C8 N8 H8A 108.3(3) . . ?
Pt1 N8 H8A 108.33(9) . . ?
C8 N8 H8B 108.3(3) . . ?
Pt1 N8 H8B 108.33(9) . . ?
H8A N8 H8B 107.4 . . ?
N8 C8 H8C 109.5(3) . . ?
N8 C8 H8D 109.5(3) . . ?
H8C C8 H8D 109.5 . . ?
N8 C8 H8E 109.5(3) . . ?
H8C C8 H8E 109.5 . . ?
H8D C8 H8E 109.5 . . ?
C2 N1 C6 121.5(3) . . ?
C2 N1 C1 118.1(3) . . ?
C6 N1 C1 120.4(3) . . ?
N1 C1 H1A 109.5(2) . . ?
N1 C1 H1B 109.5(2) . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5(2) . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 N1 123.2(3) . . ?
O2 C2 N3 121.6(3) . . ?
N1 C2 N3 115.2(3) . . ?
C4 N3 C2 125.9(3) . . ?
C4 N3 H3 117.1(2) . . ?
C2 N3 H3 117.1(2) . . ?
N4 C4 N3 119.6(3) . . ?
N4 C4 C5 124.6(3) . . ?
N3 C4 C5 115.8(3) . . ?
C4 N4 Pt1 129.9(2) . . ?
C4 N4 H4 115.0(2) . . ?
Pt1 N4 H4 115.04(8) . . ?
C6 C5 C4 118.8(3) . . ?
C6 C5 H5 120.6(2) . . ?
C4 C5 H5 120.6(2) . . ?
C5 C6 N1 122.7(3) . . ?
C5 C6 H6 118.7(2) . . ?
N1 C6 H6 118.7(2) . . ?
O14 Cl1 O11A 107.4(17) . . ?
O14 Cl1 O13 91.2(18) . . ?
O11A Cl1 O13 112.8(15) . . ?
O14 Cl1 O12A 108.2(15) . . ?
O11A Cl1 O12A 118.0(13) . . ?
O13 Cl1 O12A 115.4(11) . . ?
O14 Cl1 O13A 107.2(18) . . ?
O11A Cl1 O13A 106.8(15) . . ?
O13 Cl1 O13A 16.0(17) . . ?
O12A Cl1 O13A 108.8(11) . . ?
O14 Cl1 O12 118.3(14) . . ?
O11A Cl1 O12 116.2(14) . . ?
O13 Cl1 O12 108.3(11) . . ?
O12A Cl1 O12 11.4(14) . . ?
O13A Cl1 O12 99.7(11) . . ?
O14 Cl1 O14A 19.3(26) . . ?
O11A Cl1 O14A 99.7(14) . . ?
O13 Cl1 O14A 110.4(16) . . ?
O12A Cl1 O14A 97.7(12) . . ?
O13A Cl1 O14A 126.5(15) . . ?
O12 Cl1 O14A 109.0(11) . . ?
O14 Cl1 O11 121.3(16) . . ?
O11A Cl1 O11 14.0(20) . . ?
O13 Cl1 O11 111.4(12) . . ?
O12A Cl1 O11 108.8(12) . . ?
O13A Cl1 O11 101.9(12) . . ?
O12 Cl1 O11 105.0(12) . . ?
O14A Cl1 O11 112.4(13) . . ?
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 N4 1.993(3) 2 ?
Pt1 N4 1.993(3) . ?
Pt1 N8 2.033(3) 2 ?
Pt1 N8 2.033(3) . ?
N8 C8 1.464(6) . ?
N8 H8A 0.90 . ?
N8 H8B 0.90 . ?
C8 H8C 0.96 . ?
C8 H8D 0.96 . ?
C8 H8E 0.96 . ?
N1 C2 1.365(4) . ?
N1 C6 1.368(5) . ?
N1 C1 1.468(5) . ?
C1 H1A 0.96 . ?
C1 H1B 0.96 . ?
C1 H1C 0.96 . ?
C2 O2 1.213(4) . ?
C2 N3 1.385(4) . ?
N3 C4 1.366(4) . ?
N3 H3 0.86 . ?
C4 N4 1.305(4) . ?
C4 C5 1.428(5) . ?
N4 H4 0.86 . ?
C5 C6 1.338(6) . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
Cl1 O14 1.29(2) . ?
Cl1 O11A 1.33(3) . ?
Cl1 O13 1.40(2) . ?
Cl1 O12A 1.399(15) . ?
Cl1 O13A 1.420(11) . ?
Cl1 O12 1.431(14) . ?
Cl1 O14A 1.45(2) . ?
Cl1 O11 1.51(2) . ?
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
N4 Pt1 N8 C8 -81.9(4) 2 . . . ?
N4 Pt1 N8 C8 98.1(4) . . . . ?
N8 Pt1 N8 C8 0.0(2) 2 . . . ?
C6 N1 C2 O2 177.8(4) . . . . ?
C1 N1 C2 O2 -3.5(5) . . . . ?
C6 N1 C2 N3 -1.0(5) . . . . ?
C1 N1 C2 N3 177.7(3) . . . . ?
O2 C2 N3 C4 -179.7(3) . . . . ?
N1 C2 N3 C4 -0.9(5) . . . . ?
C2 N3 C4 N4 -176.2(3) . . . . ?
C2 N3 C4 C5 3.7(5) . . . . ?
N3 C4 N4 Pt1 5.6(5) . . . . ?
C5 C4 N4 Pt1 -174.3(3) . . . . ?
N4 Pt1 N4 C4 0.00(15) 2 . . . ?
N8 Pt1 N4 C4 -107.6(3) 2 . . . ?
N8 Pt1 N4 C4 72.4(3) . . . . ?
N4 C4 C5 C6 175.2(4) . . . . ?
N3 C4 C5 C6 -4.7(5) . . . . ?
C4 C5 C6 N1 3.2(6) . . . . ?
C2 N1 C6 C5 -0.2(6) . . . . ?
C1 N1 C6 C5 -178.9(4) . . . . ?
