#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:09:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180005 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/99/7029941.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_7029941
loop_
_publ_author_name
'Chernyshev, Alexander N.'
'Bokach, Nadezhda A.'
'Gushchin, Pavel V.'
'Haukka, Matti'
'Kukushkin, Vadim Yu'
_publ_section_title
;
 Reactions of platinum(IV)-bound nitriles with isomeric nitroanilines:
 addition vs. substitution.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12857
_journal_page_last               12864
_journal_paper_doi               10.1039/c2dt30986f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C18 H20 Cl3 N6 O4 Pt, H2 O'
_chemical_formula_sum            'C18 H22 Cl3 N6 O5 Pt'
_chemical_formula_weight         703.86
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9646(7)
_cell_length_b                   11.9025(5)
_cell_length_c                   13.2546(6)
_cell_measurement_reflns_used    6746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.30
_cell_volume                     2513.93(19)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics
'CrystaMaker (CrystalMaker Software ltd., 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19613
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    5.940
_exptl_absorpt_correction_T_max  0.5908
_exptl_absorpt_correction_T_min  0.4229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.148
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5771
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0319
_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)+(0.0295P)²+9.5552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                4885
_reflns_number_total             5771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30986f.txt
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7029941
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 0.201317(11) 0.033010(15) 0.073475(14) 0.01856(6) Uani 1 1 d . . .
Cl1 Cl 0.21128(8) 0.15944(10) -0.05663(9) 0.0270(3) Uani 1 1 d . . .
Cl2 Cl 0.10345(8) -0.08127(11) -0.03330(10) 0.0274(3) Uani 1 1 d . . .
Cl3 Cl 0.18863(10) -0.08905(11) 0.20730(10) 0.0371(3) Uani 1 1 d . . .
O1 O 0.4854(3) -0.5442(4) 0.1161(4) 0.0430(11) Uani 1 1 d . . .
O2 O 0.4379(3) -0.6821(3) 0.0224(3) 0.0422(11) Uani 1 1 d . . .
O3 O 0.5263(2) 0.3006(3) 0.3473(3) 0.0287(8) Uani 1 1 d . . .
O4 O 0.4298(2) 0.4255(3) 0.3569(3) 0.0388(10) Uani 1 1 d . . .
N1 N 0.3005(3) -0.0463(3) 0.0140(3) 0.0231(9) Uani 1 1 d D . .
H1 H 0.3310 0.0010 -0.0197 0.035 Uiso 1 1 d RD . .
N3 N 0.2768(3) -0.2320(4) 0.0416(3) 0.0291(10) Uani 1 1 d D . .
H3 H 0.2325 -0.2261 0.0771 0.044 Uiso 1 1 d RD . .
N5 N 0.4319(3) -0.5869(4) 0.0570(4) 0.0323(10) Uani 1 1 d . . .
N2 N 0.1037(3) 0.1213(4) 0.1190(3) 0.0244(9) Uani 1 1 d D . .
H2 H 0.0529 0.0945 0.1094 0.037 Uiso 1 1 d RD . .
N4 N 0.1773(2) 0.2812(4) 0.1756(3) 0.0230(9) Uani 1 1 d . . .
N6 N 0.4545(3) 0.3341(4) 0.3288(3) 0.0250(9) Uani 1 1 d . . .
C1 C 0.3184(3) -0.1511(4) -0.0019(4) 0.0218(10) Uani 1 1 d . . .
C2 C 0.3841(3) -0.1793(4) -0.0753(4) 0.0253(11) Uani 1 1 d . . .
H2A H 0.4129 -0.2501 -0.0547 0.030 Uiso 1 1 calc R . .
H2B H 0.4265 -0.1187 -0.0754 0.030 Uiso 1 1 calc R . .
C3 C 0.3415(4) -0.1924(6) -0.1809(4) 0.0389(14) Uani 1 1 d . . .
H3A H 0.2998 -0.2527 -0.1804 0.058 Uiso 1 1 calc R . .
H3B H 0.3837 -0.2109 -0.2289 0.058 Uiso 1 1 calc R . .
H3C H 0.3137 -0.1218 -0.2012 0.058 Uiso 1 1 calc R . .
C4 C 0.2832(3) -0.3498(4) 0.0202(4) 0.0275(11) Uani 1 1 d . . .
C5 C 0.3543(3) -0.4100(4) 0.0517(4) 0.0269(11) Uani 1 1 d . . .
H5 H 0.3998 -0.3752 0.0894 0.032 Uiso 1 1 calc R . .
C6 C 0.3566(3) -0.5226(4) 0.0261(4) 0.0265(11) Uani 1 1 d . . .
C7 C 0.2927(4) -0.5765(5) -0.0259(4) 0.0324(12) Uani 1 1 d . . .
H7 H 0.2972 -0.6539 -0.0426 0.039 Uiso 1 1 calc R . .
C8 C 0.2211(4) -0.5166(5) -0.0540(5) 0.0370(14) Uani 1 1 d . . .
H8 H 0.1748 -0.5533 -0.0883 0.044 Uiso 1 1 calc R . .
C9 C 0.2166(4) -0.4019(5) -0.0322(5) 0.0352(13) Uani 1 1 d . . .
H9 H 0.1680 -0.3601 -0.0532 0.042 Uiso 1 1 calc R . .
C10 C 0.1058(3) 0.2251(4) 0.1495(4) 0.0251(11) Uani 1 1 d . A .
C11 C 0.0265(4) 0.2922(5) 0.1590(6) 0.0485(19) Uani 1 1 d D . .
C12 C 0.0145(7) 0.3675(11) 0.0569(9) 0.057(4) Uani 0.580(14) 1 d PDU A 1
H12A H 0.0648 0.4131 0.0494 0.086 Uiso 0.580(14) 1 calc PR A 1
H12B H -0.0343 0.4169 0.0614 0.086 Uiso 0.580(14) 1 calc PR A 1
H12C H 0.0055 0.3179 -0.0018 0.086 Uiso 0.580(14) 1 calc PR A 1
H11A H 0.0319 0.3428 0.2165 0.068 Uiso 0.58 1 d P A 1
H11B H -0.0219 0.2431 0.1627 0.068 Uiso 0.58 1 d P A 1
C12B C 0.0160(18) 0.287(3) 0.2823(9) 0.119(11) Uani 0.420(14) 1 d PDU A 2
H12D H -0.0027 0.2119 0.3009 0.179 Uiso 0.420(14) 1 calc PR A 2
H12E H -0.0255 0.3428 0.3008 0.179 Uiso 0.420(14) 1 calc PR A 2
H12F H 0.0701 0.3035 0.3182 0.179 Uiso 0.420(14) 1 calc PR A 2
H11C H -0.0221 0.2617 0.1167 0.143 Uiso 0.42 1 d P A 2
H11D H 0.0344 0.3736 0.1370 0.143 Uiso 0.42 1 d P A 2
C13 C 0.2579(3) 0.2349(4) 0.1910(4) 0.0198(10) Uani 1 1 d . . .
C14 C 0.3166(3) 0.3031(4) 0.2442(4) 0.0223(10) Uani 1 1 d . . .
H14 H 0.3022 0.3776 0.2621 0.027 Uiso 1 1 calc R . .
C15 C 0.3947(3) 0.2617(4) 0.2703(4) 0.0212(10) Uani 1 1 d . . .
C16 C 0.4186(3) 0.1533(4) 0.2462(4) 0.0244(11) Uani 1 1 d . . .
H16 H 0.4726 0.1253 0.2669 0.029 Uiso 1 1 calc R . .
C17 C 0.3610(3) 0.0876(4) 0.1910(4) 0.0245(11) Uani 1 1 d . . .
H17 H 0.3762 0.0135 0.1729 0.029 Uiso 1 1 calc R . .
C18 C 0.2811(3) 0.1274(4) 0.1612(4) 0.0198(10) Uani 1 1 d . . .
O5 O -0.1614(3) 0.0048(4) 0.2570(3) 0.0259(10) Uani 0.795(6) 1 d P B 3
H5A H -0.1442 0.0009 0.1988 0.039 Uiso 0.795(6) 1 d PR B 3
H5B H -0.1652 -0.0652 0.2807 0.039 Uiso 0.795(6) 1 d PR B 3
O5B O -0.1205(11) 0.0890(13) 0.2949(12) 0.0259(10) Uani 0.205(6) 1 d P B 4
H5BA H -0.1487 0.0306 0.2904 0.039 Uiso 0.205(6) 1 d PR B 4
H5BB H -0.0796 0.0831 0.2560 0.039 Uiso 0.205(6) 1 d PR B 4
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_publ_flag
N2 Pt1 C18 90.57(18) yes
N2 Pt1 N1 173.98(18) yes
C18 Pt1 N1 90.14(18) ?
N2 Pt1 Cl1 88.47(13) ?
C18 Pt1 Cl1 89.85(14) ?
N1 Pt1 Cl1 85.56(13) ?
N2 Pt1 Cl3 89.56(13) ?
C18 Pt1 Cl3 89.42(14) ?
N1 Pt1 Cl3 96.42(13) ?
Cl1 Pt1 Cl3 177.89(5) yes
N2 Pt1 Cl2 89.13(12) ?
C18 Pt1 Cl2 179.69(15) ?
N1 Pt1 Cl2 90.14(12) ?
Cl1 Pt1 Cl2 90.06(4) yes
Cl3 Pt1 Cl2 90.67(5) ?
C1 N1 Pt1 133.6(4) ?
C1 N1 H1 113.3 ?
Pt1 N1 H1 111.4 ?
C1 N3 C4 125.5(5) ?
C1 N3 H3 128.2 ?
C4 N3 H3 104.8 ?
O2 N5 O1 123.4(5) ?
O2 N5 C6 117.3(5) ?
O1 N5 C6 119.2(5) ?
C10 N2 Pt1 125.9(4) ?
C10 N2 H2 113.5 ?
Pt1 N2 H2 119.8 ?
C10 N4 C13 126.7(4) ?
O3 N6 O4 123.0(4) ?
O3 N6 C15 119.0(4) ?
O4 N6 C15 118.0(4) ?
N1 C1 N3 120.5(5) ?
N1 C1 C2 119.1(5) ?
N3 C1 C2 120.4(4) ?
C1 C2 C3 109.0(4) ?
C1 C2 H2A 109.9 ?
C3 C2 H2A 109.9 ?
C1 C2 H2B 109.9 ?
C3 C2 H2B 109.9 ?
H2A C2 H2B 108.3 ?
C2 C3 H3A 109.5 ?
C2 C3 H3B 109.5 ?
H3A C3 H3B 109.5 ?
C2 C3 H3C 109.5 ?
H3A C3 H3C 109.5 ?
H3B C3 H3C 109.5 ?
C9 C4 C5 120.7(5) ?
C9 C4 N3 118.4(5) ?
C5 C4 N3 120.9(5) ?
C6 C5 C4 117.4(5) ?
C6 C5 H5 121.3 ?
C4 C5 H5 121.3 ?
C7 C6 C5 123.5(5) ?
C7 C6 N5 118.4(5) ?
C5 C6 N5 118.1(5) ?
C6 C7 C8 118.5(5) ?
C6 C7 H7 120.7 ?
C8 C7 H7 120.7 ?
C7 C8 C9 120.0(5) ?
C7 C8 H8 120.0 ?
C9 C8 H8 120.0 ?
C4 C9 C8 119.7(5) ?
C4 C9 H9 120.1 ?
C8 C9 H9 120.1 ?
N2 C10 N4 123.8(5) ?
N2 C10 C11 121.5(5) ?
N4 C10 C11 114.7(5) ?
C10 C11 C12 106.2(6) ?
C10 C11 C12B 101.5(11) ?
C12 C11 C12B 146.1(13) ?
C10 C11 H11A 111.1 ?
C12 C11 H11A 108.2 ?
C12B C11 H11A 42.0 ?
C10 C11 H11B 111.1 ?
C12 C11 H11B 108.6 ?
C12B C11 H11B 78.4 ?
H11A C11 H11B 111.5 ?
C10 C11 H11C 112.8 ?
C12 C11 H11C 71.6 ?
C12B C11 H11C 114.9 ?
H11A C11 H11C 134.1 ?
H11B C11 H11C 38.5 ?
C10 C11 H11D 111.0 ?
C12 C11 H11D 41.3 ?
C12B C11 H11D 109.9 ?
H11A C11 H11D 68.3 ?
H11B C11 H11D 134.2 ?
H11C C11 H11D 106.8 ?
C11 C12 H12A 109.5 ?
C11 C12 H12B 109.5 ?
C11 C12 H12C 109.5 ?
C11 C12 H11D 38.2 ?
H12A C12 H11D 82.5 ?
H12B C12 H11D 94.9 ?
H12C C12 H11D 146.2 ?
C11 C12B H11A 34.9 ?
C11 C12B H12D 109.5 ?
C11 C12B H12E 109.5 ?
H12D C12B H12E 109.5 ?
C11 C12B H12F 109.5 ?
H12D C12B H12F 109.5 ?
H12E C12B H12F 109.5 ?
C18 C13 C14 119.5(4) ?
C18 C13 N4 125.2(4) ?
C14 C13 N4 115.2(4) ?
C15 C14 C13 119.5(4) ?
C15 C14 H14 120.3 ?
C13 C14 H14 120.3 ?
C14 C15 C16 122.4(5) ?
C14 C15 N6 118.4(4) ?
C16 C15 N6 119.1(4) ?
C17 C16 C15 117.7(5) ?
C17 C16 H16 121.2 ?
C15 C16 H16 121.2 ?
C16 C17 C18 121.7(5) ?
C16 C17 H17 119.1 ?
C18 C17 H17 119.1 ?
C17 C18 C13 119.0(4) ?
C17 C18 Pt1 120.6(3) ?
C13 C18 Pt1 120.3(4) ?
H5A O5 H5B 107.8 ?
H5A O5 H5BA 129.0 ?
H5B O5 H5BA 105.0 ?
H5BA O5B H5BB 108.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 N2 2.003(4) yes
Pt1 C18 2.014(5) yes
Pt1 N1 2.043(4) yes
Pt1 Cl1 2.3015(12) yes
Pt1 Cl3 2.3113(13) yes
Pt1 Cl2 2.4545(12) yes
O1 N5 1.232(6) ?
O2 N5 1.228(6) ?
O3 N6 1.223(5) ?
O4 N6 1.224(6) ?
N1 C1 1.299(6) yes
N1 H1 0.8831 ?
N3 C1 1.323(7) yes
N3 C4 1.435(6) ?
N3 H3 0.8752 ?
N5 C6 1.462(7) ?
N2 C10 1.299(6) yes
N2 H2 0.8739 ?
N4 C10 1.349(6) yes
N4 C13 1.402(6) ?
N6 C15 1.472(6) ?
C1 C2 1.512(7) ?
C2 C3 1.526(7) ?
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 H3A 0.9800 ?
C3 H3B 0.9800 ?
C3 H3C 0.9800 ?
C4 C9 1.381(8) ?
C4 C5 1.385(7) ?
C5 C6 1.385(7) ?
C5 H5 0.9500 ?
C6 C7 1.358(8) ?
C7 C8 1.379(8) ?
C7 H7 0.9500 ?
C8 C9 1.398(8) ?
C8 H8 0.9500 ?
C9 H9 0.9500 ?
C10 C11 1.510(7) ?
C11 C12 1.626(8) ?
C11 C12B 1.653(9) ?
C11 H11A 0.9703 ?
C11 H11B 0.9730 ?
C11 H11C 0.9971 ?
C11 H11D 1.0217 ?
C12 H12A 0.9800 ?
C12 H12B 0.9800 ?
C12 H12C 0.9800 ?
C12 H11D 1.0921 ?
C12B H11A 1.1360 ?
C12B H12D 0.9800 ?
C12B H12E 0.9800 ?
C12B H12F 0.9800 ?
C13 C18 1.396(6) ?
C13 C14 1.397(7) ?
C14 C15 1.367(7) ?
C14 H14 0.9500 ?
C15 C16 1.388(7) ?
C16 C17 1.382(7) ?
C16 H16 0.9500 ?
C17 C18 1.394(7) ?
C17 H17 0.9500 ?
O5 H5A 0.8352 ?
O5 H5B 0.8944 ?
O5 H5BA 0.5672 ?
O5B H5BA 0.8288 ?
O5B H5BB 0.8594 ?
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
N1 H1 O4 0.88 2.50 3.345(6) 160.7 4_565
N3 H3 Cl3 0.88 2.51 3.174(5) 133.7 .
N2 H2 Cl2 0.87 2.64 3.463(4) 157.8 3
O5 H5A Cl2 0.84 2.52 3.288(5) 154.3 3
O5 H5A Cl1 0.84 2.85 3.354(5) 121.1 3
O5 H5B N4 0.89 1.93 2.824(6) 176.4 2_545
O5B H5BB Cl2 0.86 2.95 3.496(17) 123.0 3
