#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322118.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_4322118
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 H15 N5 O6 Pt0.5'
_chemical_formula_weight         350.77
_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
_cell_angle_alpha                80.36(3)
_cell_angle_beta                 80.80(3)
_cell_angle_gamma                80.54(3)
_cell_formula_units_Z            2
_cell_length_a                   5.9370(10)
_cell_length_b                   8.228(2)
_cell_length_c                   12.470(2)
_cell_measurement_reflns_used    2797
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      1.67
_cell_volume                     586.9(2)
_computing_cell_refinement       'DENZO, SCALEPACK (Otwinowski, Minor, 1997)'
_computing_data_collection
'Collect, datacollection software, Nonius, 1998'
_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
;
1205 frames via ω-rotation (Δω\=1°) and two times 237s 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2797
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    6.056
_exptl_absorpt_correction_T_max  0.5065
_exptl_absorpt_correction_T_min  0.1149
_exptl_absorpt_correction_type   SCALEPACK
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.300
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0112(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   1.055
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_hydrogen_treatment    'refU, except H1 and H4C refall'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_obs          0.0232
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0274P)²+0.8410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0565
_refine_ls_wR_factor_obs         0.0546
_reflns_number_observed          2793
_reflns_number_total             2797
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990044c_1.cif
_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^)+(0.0274P)^2^+0.8410P] 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^)+(0.0274P)^2^+0.8410P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C6 H15 N5 O6 Pt0.50'
_cod_database_code               4322118
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 0.5000 0.5000 0.02280(8) Uani 1 d S .
O1 O -0.2718(4) 0.6108(3) 0.4233(2) 0.0282(5) Uani 1 d . .
H1 H -0.2563(78) 0.6974(61) 0.4106(37) 0.031(12) Uiso 1 d . .
N7 N 0.1997(5) 0.6857(4) 0.4378(3) 0.0315(6) Uani 1 d . .
H7A H 0.1421(5) 0.7739(4) 0.4729(3) 0.075(13) Uiso 1 calc R .
H7B H 0.3422(5) 0.6495(4) 0.4557(3) 0.075(13) Uiso 1 calc R .
C7 C 0.2229(7) 0.7456(5) 0.3188(3) 0.0415(9) Uani 1 d . .
H7C H 0.3085(59) 0.8381(32) 0.3026(5) 0.076(8) Uiso 1 calc R .
H7D H 0.0726(7) 0.7802(46) 0.2967(7) 0.076(8) Uiso 1 calc R .
H7E H 0.3026(60) 0.6574(16) 0.2796(4) 0.076(8) Uiso 1 calc R .
N1C N -0.1002(6) 0.3235(4) 0.0999(3) 0.0384(7) Uani 1 d . .
C1C C -0.2061(9) 0.3011(7) 0.0054(4) 0.0561(12) Uani 1 d . .
H1C1 H -0.2565(60) 0.4080(7) -0.0340(18) 0.076(8) Uiso 1 calc R .
H1C2 H -0.3360(41) 0.2423(42) 0.0310(4) 0.076(8) Uiso 1 calc R .
H1C3 H -0.0950(22) 0.2382(41) -0.0423(16) 0.076(8) Uiso 1 calc R .
C2C C -0.2088(7) 0.4433(5) 0.1617(3) 0.0357(8) Uani 1 d . .
O2C O -0.3806(6) 0.5379(5) 0.1387(3) 0.0555(8) Uani 1 d . .
N3C N -0.1080(5) 0.4552(4) 0.2519(2) 0.0299(6) Uani 1 d . .
H3C H -0.1682(5) 0.5337(4) 0.2896(2) 0.049(8) Uiso 1 calc R .
C4C C 0.0791(6) 0.3526(4) 0.2857(3) 0.0267(6) Uani 1 d . .
N4C N 0.1459(5) 0.3677(4) 0.3779(2) 0.0284(6) Uani 1 d . .
H4C H 0.2432(83) 0.3159(59) 0.3883(37) 0.031(12) Uiso 1 d . .
C5C C 0.1917(7) 0.2339(5) 0.2161(3) 0.0350(8) Uani 1 d . .
H5C H 0.3278(7) 0.1664(5) 0.2314(3) 0.049(8) Uiso 1 calc R .
C6C C 0.0948(7) 0.2226(5) 0.1276(3) 0.0399(9) Uani 1 d . .
H6C H 0.1637(7) 0.1425(5) 0.0835(3) 0.049(8) Uiso 1 calc R .
N10 N 0.3090(5) 0.9549(4) 0.6136(3) 0.0386(7) Uani 1 d . .
O11 O 0.3707(5) 0.8038(4) 0.6304(3) 0.0512(8) Uani 1 d . .
O12 O 0.2172(7) 1.0187(5) 0.5310(3) 0.0672(10) Uani 1 d . .
O13 O 0.3396(8) 1.0474(5) 0.6771(4) 0.0749(12) Uani 1 d . .
O1W O 0.3467(15) 0.1018(8) 0.8936(5) 0.134(3) Uani 1 d . .
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'
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
O1 Pt1 O1 180.0 . 2_566 ?
O1 Pt1 N4C 94.40(12) . . ?
O1 Pt1 N4C 85.60(12) 2_566 . ?
O1 Pt1 N4C 85.60(12) . 2_566 ?
O1 Pt1 N4C 94.40(12) 2_566 2_566 ?
N4C Pt1 N4C 180.0 . 2_566 ?
O1 Pt1 N7 85.16(12) . 2_566 ?
O1 Pt1 N7 94.84(12) 2_566 2_566 ?
N4C Pt1 N7 88.69(13) . 2_566 ?
N4C Pt1 N7 91.31(13) 2_566 2_566 ?
O1 Pt1 N7 94.84(12) . . ?
O1 Pt1 N7 85.16(12) 2_566 . ?
N4C Pt1 N7 91.31(13) . . ?
N4C Pt1 N7 88.69(13) 2_566 . ?
N7 Pt1 N7 180.0 2_566 . ?
C7 N7 Pt1 118.6(2) . . ?
C6C N1C C2C 121.2(3) . . ?
C6C N1C C1C 120.9(4) . . ?
C2C N1C C1C 117.9(4) . . ?
O2C C2C N1C 123.2(4) . . ?
O2C C2C N3C 121.0(4) . . ?
N1C C2C N3C 115.8(3) . . ?
C4C N3C C2C 125.1(3) . . ?
N4C C4C N3C 119.2(3) . . ?
N4C C4C C5C 124.0(3) . . ?
N3C C4C C5C 116.8(3) . . ?
C4C N4C Pt1 132.3(3) . . ?
C6C C5C C4C 118.0(3) . . ?
C5C C6C N1C 122.8(4) . . ?
O11 N10 O13 121.4(4) . . ?
O11 N10 O12 120.3(4) . . ?
O13 N10 O12 118.3(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 O1 2.017(2) . ?
Pt1 O1 2.017(2) 2_566 ?
Pt1 N4C 2.019(3) . ?
Pt1 N4C 2.019(3) 2_566 ?
Pt1 N7 2.061(3) 2_566 ?
Pt1 N7 2.061(3) . ?
N7 C7 1.476(5) . ?
N1C C6C 1.366(5) . ?
N1C C2C 1.366(5) . ?
N1C C1C 1.472(5) . ?
C2C O2C 1.219(5) . ?
C2C N3C 1.380(5) . ?
N3C C4C 1.359(4) . ?
C4C N4C 1.306(5) . ?
C4C C5C 1.427(5) . ?
C5C C6C 1.346(5) . ?
N10 O11 1.229(4) . ?
N10 O13 1.238(5) . ?
N10 O12 1.241(5) . ?
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
O1 Pt1 N7 C7 -48.9(3) . . . . ?
O1 Pt1 N7 C7 131.1(3) 2_566 . . . ?
N4C Pt1 N7 C7 45.7(3) . . . . ?
N4C Pt1 N7 C7 -134.3(3) 2_566 . . . ?
N7 Pt1 N7 C7 110.5(1000) 2_566 . . . ?
C6C N1C C2C O2C 178.6(4) . . . . ?
C1C N1C C2C O2C -4.3(6) . . . . ?
C6C N1C C2C N3C 0.4(6) . . . . ?
C1C N1C C2C N3C 177.5(4) . . . . ?
O2C C2C N3C C4C 178.0(4) . . . . ?
N1C C2C N3C C4C -3.8(6) . . . . ?
C2C N3C C4C N4C -174.0(3) . . . . ?
C2C N3C C4C C5C 6.3(5) . . . . ?
N3C C4C N4C Pt1 9.5(5) . . . . ?
C5C C4C N4C Pt1 -170.8(3) . . . . ?
O1 Pt1 N4C C4C -3.6(4) . . . . ?
O1 Pt1 N4C C4C 176.4(4) 2_566 . . . ?
N4C Pt1 N4C C4C 172.9(1000) 2_566 . . . ?
N7 Pt1 N4C C4C 81.4(4) 2_566 . . . ?
N7 Pt1 N4C C4C -98.6(4) . . . . ?
N4C C4C C5C C6C 174.9(4) . . . . ?
N3C C4C C5C C6C -5.4(5) . . . . ?
C4C C5C C6C N1C 2.5(6) . . . . ?
C2C N1C C6C C5C 0.0(7) . . . . ?
C1C N1C C6C C5C -177.0(4) . . . . ?
