#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:32:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178874 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/03/4110353.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_4110353
loop_
_publ_author_name
'Andrei N. Vedernikov'
'Seth A. Binfield'
'Peter Y. Zavalij'
'Julia R. Khusnutdinova'
_publ_section_title
;
 Stoichiometric Aerobic PtII-Me Bond Cleavage in Aqueous Solutions to
 Produce Methanol and a PtII(OH) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              82
_journal_page_last               83
_journal_paper_doi               10.1021/ja0575171
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C22 H20 N4 O8 Pt2 S2'
_chemical_formula_sum            'C22 H20 N4 O8 Pt2 S2'
_chemical_formula_weight         922.72
_chemical_name_common            trans-Pt2-complex
_chemical_name_systematic
;
trans-Pt2-complex
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.767(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.169(3)
_cell_length_b                   13.873(5)
_cell_length_c                   10.637(4)
_cell_measurement_reflns_used    6599
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.4
_cell_volume                     1201.3(8)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Platon (Spek, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      NFRAMES=606,606,50,1206,50
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0669815
_diffrn_orient_matrix_UB_12      0.0182255
_diffrn_orient_matrix_UB_13      0.0708921
_diffrn_orient_matrix_UB_21      -0.0534653
_diffrn_orient_matrix_UB_22      -0.0648227
_diffrn_orient_matrix_UB_23      -0.0046527
_diffrn_orient_matrix_UB_31      0.0880105
_diffrn_orient_matrix_UB_32      -0.0257285
_diffrn_orient_matrix_UB_33      0.0620692
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11780
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.42
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.17
_exptl_absorpt_coefficient_mu    11.866
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.551
_exptl_crystal_density_method    not_measure
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_id                'Vedern AV050924 Pt2-complex new crystals'
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.006
_refine_diff_density_max         2.952
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.02P)²+7.73P], P=(max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                2399
_reflns_number_total             2752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0575171si20051103_033709.cif
_cod_data_source_block           1274
_cod_original_cell_volume        1201.2(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4110353
#BEGIN Tags that were not found in dictionaries:
_diffrn_measurement_total_frames-ccd 2518
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.958
_diffrn_measurement_frame_time-ccd 8
_diffrn_measurement_total_time-ccd 10.6
_diffrn_measurement_frame_size-ccd 512
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Pt1 Pt 0.04001(2) 0.037259(13) 0.366250(18) 0.02611(8) Uani 1 1 d .
O1 O 0.1467(5) 0.0228(3) 0.5443(4) 0.0309(9) Uani 1 1 d D
H1 H 0.190(9) 0.070(4) 0.577(7) 0.06(2) Uiso 1 1 d D
S1 S -0.0398(2) 0.29416(10) 0.21072(15) 0.0359(3) Uani 1 1 d .
O2 O -0.0812(7) 0.2632(4) 0.3332(5) 0.0576(14) Uani 1 1 d .
O3 O 0.0809(7) 0.3694(3) 0.2105(6) 0.0591(14) Uani 1 1 d .
O4 O -0.1829(6) 0.3127(3) 0.1237(5) 0.0457(11) Uani 1 1 d .
N1 N 0.2333(6) 0.1026(3) 0.3004(4) 0.0294(9) Uani 1 1 d .
C2 C 0.3830(8) 0.0814(4) 0.3582(6) 0.0375(13) Uani 1 1 d .
H2 H 0.3913 0.0357 0.4223 0.045 Uiso 1 1 calc R
C3 C 0.5231(8) 0.1261(5) 0.3242(7) 0.0439(15) Uani 1 1 d .
H3 H 0.6248 0.1103 0.3648 0.053 Uiso 1 1 calc R
C4 C 0.5123(8) 0.1938(5) 0.2304(8) 0.0504(17) Uani 1 1 d .
H4 H 0.6059 0.2253 0.2076 0.060 Uiso 1 1 calc R
C5 C 0.3601(8) 0.2146(5) 0.1701(7) 0.0435(15) Uani 1 1 d .
H5 H 0.3505 0.2595 0.1050 0.052 Uiso 1 1 calc R
C6 C 0.2222(7) 0.1684(4) 0.2070(5) 0.0313(12) Uani 1 1 d .
C7 C 0.0579(7) 0.1918(4) 0.1375(5) 0.0304(12) Uani 1 1 d .
H7 H 0.078(7) 0.217(4) 0.063(6) 0.028(15) Uiso 1 1 d .
C8 C -0.0624(7) 0.1113(4) 0.1088(5) 0.0291(11) Uani 1 1 d .
C9 C -0.1582(7) 0.1122(4) -0.0055(5) 0.0343(12) Uani 1 1 d .
H9 H -0.1460 0.1616 -0.0632 0.041 Uiso 1 1 calc R
C10 C -0.2720(8) 0.0397(4) -0.0335(6) 0.0378(14) Uani 1 1 d .
H10 H -0.3378 0.0401 -0.1091 0.045 Uiso 1 1 calc R
C11 C -0.2858(8) -0.0332(4) 0.0532(6) 0.0372(13) Uani 1 1 d .
H11 H -0.3602 -0.0833 0.0371 0.045 Uiso 1 1 calc R
C12 C -0.1871(9) -0.0299(5) 0.1632(7) 0.0456(16) Uani 1 1 d .
H12 H -0.1956 -0.0801 0.2204 0.055 Uiso 1 1 calc R
N2 N -0.0787(6) 0.0406(3) 0.1947(4) 0.0259(9) Uani 1 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'
S S 0.1246 0.1234 '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
N2 Pt1 N1 90.42(19) . .
N2 Pt1 O1 174.41(16) . .
N1 Pt1 O1 94.68(18) . .
N2 Pt1 O1 96.33(17) . 3_556
N1 Pt1 O1 172.66(17) . 3_556
O1 Pt1 O1 78.71(17) . 3_556
N2 Pt1 O2 76.22(15) . .
N1 Pt1 O2 76.74(16) . .
O1 Pt1 O2 107.18(15) . .
O1 Pt1 O2 102.02(16) 3_556 .
Pt1 O1 Pt1 101.29(17) . 3_556
Pt1 O1 H1 117(6) . .
Pt1 O1 H1 117(6) 3_556 .
O3 S1 O2 115.6(4) . .
O3 S1 O4 112.7(3) . .
O2 S1 O4 113.1(3) . .
O3 S1 C7 103.8(3) . .
O2 S1 C7 107.3(3) . .
O4 S1 C7 102.8(3) . .
S1 O2 Pt1 106.8(2) . .
C6 N1 C2 119.0(5) . .
C6 N1 Pt1 124.0(4) . .
C2 N1 Pt1 116.9(4) . .
N1 C2 C3 121.5(6) . .
N1 C2 H2 119.3 . .
C3 C2 H2 119.3 . .
C4 C3 C2 119.8(6) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C5 118.9(6) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
C4 C5 C6 119.6(6) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
N1 C6 C5 121.2(5) . .
N1 C6 C7 120.6(5) . .
C5 C6 C7 118.2(5) . .
C8 C7 C6 118.6(5) . .
C8 C7 S1 111.2(4) . .
C6 C7 S1 111.0(4) . .
C8 C7 H7 106(4) . .
C6 C7 H7 107(4) . .
S1 C7 H7 101(4) . .
N2 C8 C9 121.1(5) . .
N2 C8 C7 120.0(5) . .
C9 C8 C7 118.8(5) . .
C10 C9 C8 120.0(5) . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
C11 C10 C9 118.7(6) . .
C11 C10 H10 120.7 . .
C9 C10 H10 120.7 . .
C12 C11 C10 118.2(6) . .
C12 C11 H11 120.9 . .
C10 C11 H11 120.9 . .
N2 C12 C11 124.6(6) . .
N2 C12 H12 117.7 . .
C11 C12 H12 117.7 . .
C12 N2 C8 117.3(5) . .
C12 N2 Pt1 118.2(4) . .
C8 N2 Pt1 124.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N2 1.994(5) .
Pt1 N1 1.997(5) .
Pt1 O1 2.028(4) .
Pt1 O1 2.041(4) 3_556
Pt1 Pt1 3.1466(11) 3_556
Pt1 O2 3.297(5) .
O1 H1 0.81(4) .
S1 O3 1.436(5) .
S1 O2 1.439(5) .
S1 O4 1.452(5) .
S1 C7 1.834(6) .
N1 C6 1.346(7) .
N1 C2 1.354(7) .
C2 C3 1.376(9) .
C2 H2 0.9300 .
C3 C4 1.369(10) .
C3 H3 0.9300 .
C4 C5 1.381(10) .
C4 H4 0.9300 .
C5 C6 1.382(8) .
C5 H5 0.9300 .
C6 C7 1.512(8) .
C7 C8 1.502(8) .
C7 H7 0.90(6) .
C8 N2 1.355(7) .
C8 C9 1.391(8) .
C9 C10 1.385(8) .
C9 H9 0.9300 .
C10 C11 1.379(9) .
C10 H10 0.9300 .
C11 C12 1.366(9) .
C11 H11 0.9300 .
C12 N2 1.343(8) .
C12 H12 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O4 0.81(4) 1.97(5) 2.768(6) 168(8) 4_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_4
N1 Pt1 O1 Pt1 176.79(18) . 3_556
O1 Pt1 O1 Pt1 0.0 3_556 3_556
O2 Pt1 O1 Pt1 99.24(18) . 3_556
O3 S1 O2 Pt1 -115.1(3) . .
O4 S1 O2 Pt1 112.8(3) . .
C7 S1 O2 Pt1 0.1(3) . .
N2 Pt1 O2 S1 -47.1(3) . .
N1 Pt1 O2 S1 46.7(3) . .
O1 Pt1 O2 S1 137.6(3) . .
O1 Pt1 O2 S1 -140.7(3) 3_556 .
N2 Pt1 N1 C6 33.4(4) . .
O1 Pt1 N1 C6 -149.0(4) . .
O2 Pt1 N1 C6 -42.4(4) . .
N2 Pt1 N1 C2 -149.6(4) . .
O1 Pt1 N1 C2 28.1(4) . .
O2 Pt1 N1 C2 134.7(4) . .
C6 N1 C2 C3 0.5(9) . .
Pt1 N1 C2 C3 -176.7(5) . .
N1 C2 C3 C4 0.3(10) . .
C2 C3 C4 C5 -1.1(10) . .
C3 C4 C5 C6 1.2(10) . .
C2 N1 C6 C5 -0.3(8) . .
Pt1 N1 C6 C5 176.6(4) . .
C2 N1 C6 C7 178.2(5) . .
Pt1 N1 C6 C7 -4.8(7) . .
C4 C5 C6 N1 -0.5(9) . .
C4 C5 C6 C7 -179.1(6) . .
N1 C6 C7 C8 -38.1(8) . .
C5 C6 C7 C8 140.4(6) . .
N1 C6 C7 S1 92.4(5) . .
C5 C6 C7 S1 -89.0(6) . .
O3 S1 C7 C8 -169.9(4) . .
O2 S1 C7 C8 67.3(5) . .
O4 S1 C7 C8 -52.3(5) . .
O3 S1 C7 C6 55.8(5) . .
O2 S1 C7 C6 -67.1(5) . .
O4 S1 C7 C6 173.4(4) . .
C6 C7 C8 N2 38.9(8) . .
S1 C7 C8 N2 -91.6(5) . .
C6 C7 C8 C9 -142.6(6) . .
S1 C7 C8 C9 86.9(6) . .
N2 C8 C9 C10 -0.5(9) . .
C7 C8 C9 C10 -178.9(5) . .
C8 C9 C10 C11 -0.9(9) . .
C9 C10 C11 C12 0.5(10) . .
C10 C11 C12 N2 1.3(11) . .
C11 C12 N2 C8 -2.6(10) . .
C11 C12 N2 Pt1 175.0(6) . .
C9 C8 N2 C12 2.1(8) . .
C7 C8 N2 C12 -179.4(5) . .
C9 C8 N2 Pt1 -175.3(4) . .
C7 C8 N2 Pt1 3.2(7) . .
N1 Pt1 N2 C12 150.0(5) . .
O1 Pt1 N2 C12 -32.9(5) 3_556 .
O2 Pt1 N2 C12 -133.8(5) . .
N1 Pt1 N2 C8 -32.6(5) . .
O1 Pt1 N2 C8 144.5(4) 3_556 .
O2 Pt1 N2 C8 43.6(4) . .
