#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:37:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179069 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/31/4303128.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_4303128
loop_
_publ_author_name
'Alexander G. Tskhovrebov'
'Nadezhda A. Bokach'
'Matti Haukka'
'Vadim Yu. Kukushkin'
_publ_section_title
;
Different Routes for Amination of Platinum(II)-Bound Cyanoguanidine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8678
_journal_page_last               8688
_journal_paper_doi               10.1021/ic900263e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C8 H20 I N6 Pt, C2 H4 Cl2, C F3 O3 S'
_chemical_formula_sum            'C11 H24 Cl2 F3 I N6 O3 Pt S'
_chemical_formula_weight         770.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.957(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5269(2)
_cell_length_b                   21.033(2)
_cell_length_c                   12.9561(10)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2288.6(3)
_computing_cell_refinement       'EvalCCD (Duisenberg, 1998-2003)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998-2003)'
_computing_molecular_graphics    'Diamond v.3.1e (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42686
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    7.853
_exptl_absorpt_correction_T_max  0.5331
_exptl_absorpt_correction_T_min  0.2158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.141
_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     257
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0203P)²+3.6415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0492
_reflns_number_gt                4402
_reflns_number_total             5178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900263e_si_001_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303128
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.409917(15) 0.100171(6) 0.392681(10) 0.01255(5) Uani 1 1 d . . .
I1 I 0.18413(3) 0.085274(13) 0.502087(19) 0.02218(7) Uani 1 1 d . . .
Cl2 Cl 0.89975(14) 0.27914(6) 0.29838(9) 0.0412(3) Uani 1 1 d . . .
Cl3 Cl 1.03124(17) 0.20184(8) 0.10419(13) 0.0660(4) Uani 1 1 d . . .
S1 S -0.45003(10) -0.14891(4) 0.12900(7) 0.01661(19) Uani 1 1 d . . .
F1 F -0.5888(3) -0.04629(12) 0.0437(2) 0.0382(6) Uani 1 1 d . . .
F2 F -0.7220(3) -0.13200(13) 0.00466(17) 0.0337(6) Uani 1 1 d . . .
F3 F -0.7079(3) -0.09088(12) 0.15776(19) 0.0344(6) Uani 1 1 d . . .
O1 O -0.3718(3) -0.15380(13) 0.0388(2) 0.0252(6) Uani 1 1 d . . .
O2 O -0.3647(3) -0.11024(13) 0.2129(2) 0.0232(6) Uani 1 1 d . . .
O3 O -0.5122(3) -0.20748(13) 0.1621(2) 0.0256(6) Uani 1 1 d . . .
N1 N 0.5738(3) 0.13923(14) 0.5110(2) 0.0156(6) Uani 1 1 d . . .
N2 N 0.5885(4) 0.10555(14) 0.3023(2) 0.0163(6) Uani 1 1 d . . .
N3 N 0.2608(4) 0.06300(16) 0.2749(2) 0.0216(7) Uani 1 1 d . . .
N4 N 0.0631(3) 0.01732(16) 0.1354(2) 0.0191(7) Uani 1 1 d . . .
N5 N -0.0542(3) -0.04694(16) 0.2506(2) 0.0198(7) Uani 1 1 d . . .
H5N H -0.1403 -0.0707 0.2537 0.030 Uiso 1 1 d R . .
H5M H -0.0118 -0.0247 0.3007 0.030 Uiso 1 1 d R . .
N6 N -0.1215(4) -0.05654(16) 0.0719(2) 0.0225(7) Uani 1 1 d . . .
H6N H -0.1924 -0.0831 0.0774 0.034 Uiso 1 1 d R . .
H6M H -0.1028 -0.0416 0.0162 0.034 Uiso 1 1 d R . .
C1 C 0.6348(5) 0.09054(19) 0.5908(3) 0.0240(9) Uani 1 1 d . . .
H1A H 0.7225 0.1085 0.6412 0.036 Uiso 1 1 calc R . .
H1B H 0.6732 0.0536 0.5563 0.036 Uiso 1 1 calc R . .
H1C H 0.5490 0.0773 0.6276 0.036 Uiso 1 1 calc R . .
C2 C 0.5133(5) 0.19359(19) 0.5666(3) 0.0228(9) Uani 1 1 d . . .
H2A H 0.4333 0.1782 0.6066 0.034 Uiso 1 1 calc R . .
H2B H 0.4648 0.2252 0.5153 0.034 Uiso 1 1 calc R . .
H2C H 0.6018 0.2131 0.6144 0.034 Uiso 1 1 calc R . .
C3 C 0.7047(4) 0.16421(19) 0.4585(3) 0.0195(8) Uani 1 1 d . . .
H3A H 0.6727 0.2056 0.4251 0.023 Uiso 1 1 calc R . .
H3B H 0.8019 0.1709 0.5114 0.023 Uiso 1 1 calc R . .
C4 C 0.7389(4) 0.1182(2) 0.3777(3) 0.0217(8) Uani 1 1 d . . .
H4A H 0.7805 0.0780 0.4118 0.026 Uiso 1 1 calc R . .
H4B H 0.8205 0.1359 0.3400 0.026 Uiso 1 1 calc R . .
C5 C 0.6079(5) 0.04523(19) 0.2461(3) 0.0255(9) Uani 1 1 d . . .
H5A H 0.5121 0.0372 0.1940 0.038 Uiso 1 1 calc R . .
H5B H 0.6241 0.0101 0.2964 0.038 Uiso 1 1 calc R . .
H5C H 0.7004 0.0486 0.2108 0.038 Uiso 1 1 calc R . .
C6 C 0.5569(4) 0.15744(18) 0.2229(3) 0.0181(8) Uani 1 1 d . . .
H6A H 0.6440 0.1593 0.1826 0.027 Uiso 1 1 calc R . .
H6B H 0.5493 0.1981 0.2585 0.027 Uiso 1 1 calc R . .
H6C H 0.4565 0.1489 0.1754 0.027 Uiso 1 1 calc R . .
C7 C 0.1637(4) 0.04061(18) 0.2131(3) 0.0178(8) Uani 1 1 d . . .
C8 C -0.0372(4) -0.02889(18) 0.1546(3) 0.0162(8) Uani 1 1 d . . .
C9 C -0.6264(5) -0.10218(19) 0.0806(3) 0.0226(8) Uani 1 1 d . . .
C10 C 1.0891(5) 0.2426(2) 0.3066(4) 0.0384(11) Uani 1 1 d . . .
H10A H 1.1659 0.2637 0.3621 0.046 Uiso 1 1 calc R . .
H10B H 1.0813 0.1974 0.3263 0.046 Uiso 1 1 calc R . .
C11 C 1.1486(5) 0.2466(2) 0.2054(4) 0.0393(12) Uani 1 1 d . . .
H11A H 1.2597 0.2310 0.2156 0.047 Uiso 1 1 calc R . .
H11B H 1.1491 0.2917 0.1835 0.047 Uiso 1 1 calc R . .
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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N3 Pt1 N1 177.20(12) . . ?
N3 Pt1 N2 91.29(12) . . ?
N1 Pt1 N2 85.92(11) . . yes
N3 Pt1 I1 86.28(9) . . yes
N1 Pt1 I1 96.52(8) . . ?
N2 Pt1 I1 176.06(8) . . ?
O3 S1 O1 115.22(17) . . ?
O3 S1 O2 114.92(16) . . ?
O1 S1 O2 113.82(16) . . ?
O3 S1 C9 103.95(17) . . ?
O1 S1 C9 103.28(17) . . ?
O2 S1 C9 103.53(17) . . ?
C1 N1 C2 107.6(3) . . ?
C1 N1 C3 111.0(3) . . ?
C2 N1 C3 107.3(3) . . ?
C1 N1 Pt1 110.8(2) . . ?
C2 N1 Pt1 114.8(2) . . ?
C3 N1 Pt1 105.4(2) . . ?
C5 N2 C6 108.0(3) . . ?
C5 N2 C4 108.4(3) . . ?
C6 N2 C4 110.7(3) . . ?
C5 N2 Pt1 112.6(2) . . ?
C6 N2 Pt1 111.4(2) . . ?
C4 N2 Pt1 105.7(2) . . ?
C7 N3 Pt1 173.2(3) . . yes
C7 N4 C8 119.0(3) . . yes
C8 N5 H5N 115.1 . . ?
C8 N5 H5M 117.8 . . ?
H5N N5 H5M 121.9 . . ?
C8 N6 H6N 121.8 . . ?
C8 N6 H6M 112.4 . . ?
H6N N6 H6M 125.4 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 110.0(3) . . ?
C4 C3 H3A 109.7 . . ?
N1 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
N1 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 N2 108.9(3) . . ?
C3 C4 H4A 109.9 . . ?
N2 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
N2 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 N4 173.7(4) . . ?
N6 C8 N5 120.1(3) . . yes
N6 C8 N4 116.3(3) . . ?
N5 C8 N4 123.6(3) . . ?
F2 C9 F1 107.9(3) . . ?
F2 C9 F3 107.9(3) . . ?
F1 C9 F3 107.6(3) . . ?
F2 C9 S1 111.6(3) . . ?
F1 C9 S1 111.5(3) . . ?
F3 C9 S1 110.2(3) . . ?
C11 C10 Cl2 111.6(3) . . ?
C11 C10 H10A 109.3 . . ?
Cl2 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
Cl2 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 Cl3 112.7(3) . . ?
C10 C11 H11A 109.1 . . ?
Cl3 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
Cl3 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
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 N3 1.971(3) . yes
Pt1 N1 2.058(3) . yes
Pt1 N2 2.079(3) . yes
Pt1 I1 2.5996(3) . yes
Cl2 C10 1.774(5) . ?
Cl3 C11 1.776(5) . ?
S1 O3 1.436(3) . ?
S1 O1 1.446(3) . ?
S1 O2 1.449(3) . ?
S1 C9 1.815(4) . ?
F1 C9 1.329(5) . ?
F2 C9 1.322(4) . ?
F3 C9 1.334(4) . ?
N1 C1 1.484(5) . ?
N1 C2 1.490(5) . ?
N1 C3 1.499(5) . ?
N2 C5 1.486(5) . ?
N2 C6 1.492(5) . ?
N2 C4 1.496(5) . ?
N3 C7 1.149(5) . yes
N4 C7 1.300(5) . yes
N4 C8 1.346(5) . yes
N5 C8 1.332(5) . yes
N5 H5N 0.8952 . ?
N5 H5M 0.8309 . ?
N6 C8 1.317(5) . yes
N6 H6N 0.8345 . ?
N6 H6M 0.8274 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.492(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C10 C11 1.488(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
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
_geom_hbond_publ_flag
N5 H5N O2 0.90 2.07 2.928(4) 160.4 . yes
N6 H6N O1 0.83 2.13 2.934(4) 161.5 . yes
N6 H6N O2 0.83 2.54 3.197(4) 136.3 . yes
N6 H6M N4 0.83 2.11 2.934(4) 171.3 3 yes
