#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/03/4330371.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_4330371
loop_
_publ_author_name
'Justin J. Wilson'
'Stephen J. Lippard'
_publ_contact_author_address
;77 Massachusetts Ave, 18-498
Cambridge, MA 02139
;
_publ_contact_author_email       lippard@mit.edu
_publ_contact_author_fax         (617)258-8150
_publ_contact_author_name        'Stephen J. Lippard'
_publ_contact_author_phone       (617)253-1892
_publ_section_title
;
 Acetate-Bridged Platinum(III) Complexes Derived from Cisplatin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9852
_journal_page_last               9864
_journal_paper_doi               10.1021/ic301289j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C4 H18 N6 O10.5 Pt2'
_chemical_formula_weight         708.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.4520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.1794(9)
_cell_length_b                   15.7804(7)
_cell_length_c                   10.8811(5)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.58
_cell_volume                     3238.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35449
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    17.320
_exptl_absorpt_correction_T_max  0.7233
_exptl_absorpt_correction_T_min  0.0782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.906
_exptl_crystal_description       shard
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4748
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0161P)²+9.1384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0383
_reflns_number_gt                4318
_reflns_number_total             4748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301289j_si_002_2.cif
_cod_data_source_block           '[1](NO3)2*0.5H2O'
_cod_original_formula_sum        'C4 H18 N6 O10.50 Pt2'
_cod_database_code               4330371
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.444007(6) 0.205133(8) 0.839622(10) 0.01462(3) Uani 1 1 d . . .
Pt2 Pt 0.324086(6) 0.226451(7) 0.968375(10) 0.01287(3) Uani 1 1 d . . .
O1 O 0.41643(12) 0.32506(15) 0.7799(2) 0.0196(5) Uani 1 1 d . . .
O3 O 0.33351(11) 0.34639(14) 0.89979(19) 0.0177(4) Uani 1 1 d . . .
N3 N 0.36823(14) 0.27068(17) 1.1389(2) 0.0171(5) Uani 1 1 d . . .
H3A H 0.3336 0.2809 1.1842 0.026 Uiso 1 1 calc R . .
H3B H 0.3920 0.3196 1.1303 0.026 Uiso 1 1 calc R . .
H3C H 0.3990 0.2315 1.1790 0.026 Uiso 1 1 calc R . .
N2 N 0.46721(16) 0.08462(19) 0.8942(3) 0.0251(6) Uani 1 1 d . . .
H2A H 0.5083 0.0686 0.8701 0.038 Uiso 1 1 calc R . .
H2B H 0.4314 0.0498 0.8583 0.038 Uiso 1 1 calc R . .
H2C H 0.4724 0.0811 0.9789 0.038 Uiso 1 1 calc R . .
N1 N 0.52910(15) 0.2520(2) 0.9588(3) 0.0253(6) Uani 1 1 d . . .
H1A H 0.5547 0.2860 0.9159 0.038 Uiso 1 1 calc R . .
H1B H 0.5568 0.2084 0.9940 0.038 Uiso 1 1 calc R . .
H1C H 0.5140 0.2826 1.0197 0.038 Uiso 1 1 calc R . .
O2 O 0.36450(12) 0.16070(15) 0.7038(2) 0.0205(5) Uani 1 1 d . . .
N4 N 0.30936(14) 0.11010(16) 1.0385(2) 0.0167(5) Uani 1 1 d . . .
H4A H 0.3478 0.0960 1.0969 0.025 Uiso 1 1 calc R . .
H4B H 0.3036 0.0713 0.9757 0.025 Uiso 1 1 calc R . .
H4C H 0.2700 0.1108 1.0744 0.025 Uiso 1 1 calc R . .
C3 C 0.29944(17) 0.1608(2) 0.7078(3) 0.0165(6) Uani 1 1 d . . .
C4 C 0.24989(18) 0.1320(2) 0.5925(3) 0.0246(7) Uani 1 1 d . . .
H4D H 0.2647 0.1564 0.5185 0.037 Uiso 1 1 calc R . .
H4E H 0.2016 0.1508 0.5963 0.037 Uiso 1 1 calc R . .
H4F H 0.2509 0.0701 0.5874 0.037 Uiso 1 1 calc R . .
O9 O 0.45175(12) 0.06219(15) 0.1801(2) 0.0201(5) Uani 1 1 d . . .
N6 N 0.5000 0.1025(3) 0.2500 0.0184(8) Uani 1 2 d S . .
O8 O 0.5000 0.1815(2) 0.2500 0.0321(9) Uani 1 2 d S . .
O7 O 0.40112(15) 0.0894(2) 0.4401(3) 0.0475(9) Uani 1 1 d D . .
O5 O 0.31537(17) 0.15015(17) 0.3155(2) 0.0389(7) Uani 1 1 d D . .
O6 O 0.31987(14) 0.01394(16) 0.3290(2) 0.0287(6) Uani 1 1 d D . .
N5 N 0.34555(15) 0.08511(19) 0.3615(2) 0.0211(6) Uani 1 1 d D . .
O4 O 0.27153(11) 0.18377(14) 0.79921(19) 0.0164(4) Uani 1 1 d . . .
C1 C 0.37078(17) 0.3696(2) 0.8205(3) 0.0176(6) Uani 1 1 d . . .
C2 C 0.36020(19) 0.4581(2) 0.7723(3) 0.0255(7) Uani 1 1 d . . .
H2D H 0.3106 0.4660 0.7324 0.038 Uiso 1 1 calc R . .
H2E H 0.3910 0.4684 0.7111 0.038 Uiso 1 1 calc R . .
H2F H 0.3721 0.4981 0.8419 0.038 Uiso 1 1 calc R . .
O10W O 0.4836(14) 0.3851(12) 1.127(2) 0.034(4) Uani 0.50 1 d P A -2
O10 O 0.4888(13) 0.3811(11) 1.1183(16) 0.027(4) Uani 0.50 1 d PD B -1
N7 N 0.4969(4) 0.4463(4) 1.0562(6) 0.0307(14) Uani 0.50 1 d PD B -1
O11 O 0.5351(4) 0.4428(5) 0.9747(7) 0.056(2) Uani 0.50 1 d PD B -1
O12 O 0.4696(5) 0.5139(5) 1.0738(8) 0.063(2) Uani 0.50 1 d PD B -1
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_3
N2 Pt1 N1 92.67(13) .
N2 Pt1 O1 177.47(11) .
N1 Pt1 O1 89.84(11) .
N2 Pt1 O2 89.16(11) .
N1 Pt1 O2 173.54(10) .
O1 Pt1 O2 88.38(9) .
N2 Pt1 Pt2 96.78(8) .
N1 Pt1 Pt2 105.27(8) .
O1 Pt1 Pt2 82.21(6) .
O2 Pt1 Pt2 80.63(6) .
N2 Pt1 Pt1 92.50(8) 2_656
N1 Pt1 Pt1 80.56(8) 2_656
O1 Pt1 Pt1 88.25(6) 2_656
O2 Pt1 Pt1 93.17(6) 2_656
Pt2 Pt1 Pt1 168.740(6) 2_656
N3 Pt2 N4 91.78(10) .
N3 Pt2 O4 175.36(10) .
N4 Pt2 O4 87.76(10) .
N3 Pt2 O3 88.02(10) .
N4 Pt2 O3 176.71(9) .
O4 Pt2 O3 92.17(9) .
N3 Pt2 Pt1 104.19(8) .
N4 Pt2 Pt1 104.58(7) .
O4 Pt2 Pt1 80.38(6) .
O3 Pt2 Pt1 78.64(6) .
N3 Pt2 Pt2 87.82(8) 7_557
N4 Pt2 Pt2 86.46(7) 7_557
O4 Pt2 Pt2 87.55(6) 7_557
O3 Pt2 Pt2 90.25(6) 7_557
Pt1 Pt2 Pt2 163.185(6) 7_557
C1 O1 Pt1 124.1(2) .
C1 O3 Pt2 127.6(2) .
Pt2 N3 H3A 109.5 .
Pt2 N3 H3B 109.5 .
H3A N3 H3B 109.5 .
Pt2 N3 H3C 109.5 .
H3A N3 H3C 109.5 .
H3B N3 H3C 109.5 .
Pt1 N2 H2A 109.5 .
Pt1 N2 H2B 109.5 .
H2A N2 H2B 109.5 .
Pt1 N2 H2C 109.5 .
H2A N2 H2C 109.5 .
H2B N2 H2C 109.5 .
Pt1 N1 H1A 109.5 .
Pt1 N1 H1B 109.5 .
H1A N1 H1B 109.5 .
Pt1 N1 H1C 109.5 .
H1A N1 H1C 109.5 .
H1B N1 H1C 109.5 .
C3 O2 Pt1 126.1(2) .
Pt2 N4 H4A 109.5 .
Pt2 N4 H4B 109.5 .
H4A N4 H4B 109.5 .
Pt2 N4 H4C 109.5 .
H4A N4 H4C 109.5 .
H4B N4 H4C 109.5 .
O2 C3 O4 126.3(3) .
O2 C3 C4 117.0(3) .
O4 C3 C4 116.7(3) .
C3 C4 H4D 109.5 .
C3 C4 H4E 109.5 .
H4D C4 H4E 109.5 .
C3 C4 H4F 109.5 .
H4D C4 H4F 109.5 .
H4E C4 H4F 109.5 .
O8 N6 O9 120.33(19) .
O8 N6 O9 120.33(19) 2_655
O9 N6 O9 119.3(4) 2_655
O5 N5 O7 120.9(3) .
O5 N5 O6 119.9(3) .
O7 N5 O6 119.2(3) .
C3 O4 Pt2 126.3(2) .
O1 C1 O3 126.1(3) .
O1 C1 C2 117.1(3) .
O3 C1 C2 116.8(3) .
C1 C2 H2D 109.5 .
C1 C2 H2E 109.5 .
H2D C2 H2E 109.5 .
C1 C2 H2F 109.5 .
H2D C2 H2F 109.5 .
H2E C2 H2F 109.5 .
O12 N7 O11 118.3(7) .
O12 N7 O10 122.2(12) .
O11 N7 O10 119.5(12) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N2 2.018(3) .
Pt1 N1 2.031(3) .
Pt1 O1 2.039(2) .
Pt1 O2 2.045(2) .
Pt1 Pt2 2.92149(18) .
Pt1 Pt1 3.1523(2) 2_656
Pt2 N3 2.019(3) .
Pt2 N4 2.028(3) .
Pt2 O4 2.046(2) .
Pt2 O3 2.054(2) .
Pt2 Pt2 3.1324(3) 7_557
O1 C1 1.263(4) .
O3 C1 1.270(4) .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
N3 H3C 0.9100 .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N2 H2C 0.9100 .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
O2 C3 1.256(4) .
N4 H4A 0.9100 .
N4 H4B 0.9100 .
N4 H4C 0.9100 .
C3 O4 1.265(3) .
C3 C4 1.500(4) .
C4 H4D 0.9800 .
C4 H4E 0.9800 .
C4 H4F 0.9800 .
O9 N6 1.258(3) .
N6 O8 1.248(5) .
N6 O9 1.258(3) 2_655
O7 N5 1.242(4) .
O5 N5 1.239(4) .
O6 N5 1.251(4) .
C1 C2 1.494(4) .
C2 H2D 0.9800 .
C2 H2E 0.9800 .
C2 H2F 0.9800 .
O10 N7 1.258(13) .
N7 O12 1.219(10) .
N7 O11 1.248(8) .
