#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:09:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180005 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/99/7029940.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_7029940
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_absolute_configuration unk
_chemical_formula_moiety         'C12 H16 Cl4 N4 O2 Pt'
_chemical_formula_sum            'C12 H16 Cl4 N4 O2 Pt'
_chemical_formula_weight         585.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   7.8439(3)
_cell_length_b                   7.8439(3)
_cell_length_c                   25.4480(7)
_cell_measurement_temperature    120(2)
_cell_volume                     1355.96(8)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'CrystaMaker (CrystalMaker Software ltd., 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8574
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    8.364
_exptl_absorpt_correction_T_max  0.5198
_exptl_absorpt_correction_T_min  0.4335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2958
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0230
_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)+(0.0263P)²+0.3938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                2884
_reflns_number_total             2958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30986f.txt
_cod_data_source_block           6
_cod_database_code               7029940
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
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 0.55541(3) 0.86764(3) 0.500000(6) 0.01508(7) Uani 1 1 d .
Cl1 Cl 0.6219(2) 0.9651(2) 0.58721(6) 0.0224(3) Uani 1 1 d .
Cl2 Cl 0.4843(2) 0.7644(2) 0.41329(6) 0.0238(3) Uani 1 1 d .
Cl3 Cl 0.8117(2) 0.7984(2) 0.50102(6) 0.0197(3) Uani 1 1 d .
Cl4 Cl 0.2970(2) 0.9292(3) 0.50095(5) 0.0231(4) Uani 1 1 d .
O1 O 1.5859(7) 1.1875(7) 0.26353(19) 0.0316(11) Uani 1 1 d .
O2 O 1.5309(7) 1.4069(7) 0.22739(18) 0.0263(10) Uani 1 1 d .
N1 N 0.7255(7) 1.1493(7) 0.47763(19) 0.0159(11) Uani 1 1 d .
H1 H 0.7029 1.2326 0.4952 0.019 Uiso 1 1 calc R
N2 N 0.3739(7) 0.5919(8) 0.5247(2) 0.0219(11) Uani 1 1 d .
N3 N 0.9302(7) 1.1278(7) 0.4171(2) 0.0203(11) Uani 1 1 d .
H3 H 0.8740 1.0036 0.4267 0.024 Uiso 1 1 calc R
N4 N 1.4993(7) 1.2827(8) 0.2613(2) 0.0220(12) Uani 1 1 d .
C1 C 0.8629(8) 1.2326(8) 0.4422(2) 0.0169(12) Uani 1 1 d .
C2 C 0.9414(9) 1.4478(9) 0.4308(2) 0.0194(13) Uani 1 1 d .
H2A H 1.0726 1.5038 0.4141 0.023 Uiso 1 1 calc R
H2B H 0.9572 1.5187 0.4643 0.023 Uiso 1 1 calc R
C3 C 0.8025(10) 1.4784(10) 0.3942(3) 0.0269(15) Uani 1 1 d .
H3A H 0.7813 1.4029 0.3618 0.040 Uiso 1 1 calc R
H3B H 0.8617 1.6185 0.3857 0.040 Uiso 1 1 calc R
H3C H 0.6761 1.4333 0.4119 0.040 Uiso 1 1 calc R
C4 C 1.0760(9) 1.1822(9) 0.3776(2) 0.0184(13) Uani 1 1 d .
C5 C 1.1064(9) 1.3096(9) 0.3364(2) 0.0211(13) Uani 1 1 d .
H5 H 1.0306 1.3732 0.3341 0.025 Uiso 1 1 calc R
C6 C 1.2474(9) 1.3444(9) 0.2986(2) 0.0197(13) Uani 1 1 d .
H6 H 1.2718 1.4341 0.2707 0.024 Uiso 1 1 calc R
C7 C 1.3518(8) 1.2455(8) 0.3024(2) 0.0150(12) Uani 1 1 d .
C8 C 1.3216(8) 1.1143(9) 0.3417(3) 0.0206(13) Uani 1 1 d .
H8 H 1.3933 1.0462 0.3428 0.025 Uiso 1 1 calc R
C9 C 1.1830(10) 1.0837(9) 0.3800(3) 0.0226(14) Uani 1 1 d .
H9 H 1.1608 0.9951 0.4081 0.027 Uiso 1 1 calc R
C10 C 0.2771(9) 0.4413(9) 0.5421(3) 0.0219(14) Uani 1 1 d .
C11 C 0.1518(10) 0.2534(9) 0.5676(3) 0.0247(14) Uani 1 1 d .
H11A H 0.2095 0.1673 0.5630 0.030 Uiso 1 1 calc R
H11B H 0.0206 0.1883 0.5507 0.030 Uiso 1 1 calc R
C12 C 0.1293(10) 0.2790(10) 0.6252(3) 0.0276(15) Uani 1 1 d .
H12A H 0.2577 0.3338 0.6425 0.041 Uiso 1 1 calc R
H12B H 0.0377 0.1510 0.6408 0.041 Uiso 1 1 calc R
H12C H 0.0778 0.3690 0.6298 0.041 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'
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 N1 176.2(2) yes
N2 Pt1 Cl4 89.89(15) ?
N1 Pt1 Cl4 86.72(15) ?
N2 Pt1 Cl1 88.66(16) ?
N1 Pt1 Cl1 89.56(14) ?
Cl4 Pt1 Cl1 89.85(5) ?
N2 Pt1 Cl2 90.28(16) ?
N1 Pt1 Cl2 91.49(14) ?
Cl4 Pt1 Cl2 89.99(5) ?
Cl1 Pt1 Cl2 178.93(6) yes
N2 Pt1 Cl3 88.59(15) ?
N1 Pt1 Cl3 94.78(15) ?
Cl4 Pt1 Cl3 178.28(6) yes
Cl1 Pt1 Cl3 89.32(5) ?
Cl2 Pt1 Cl3 90.82(5) ?
C1 N1 Pt1 132.5(4) ?
C1 N1 H1 113.8 ?
Pt1 N1 H1 113.8 ?
C10 N2 Pt1 175.1(6) ?
C1 N3 C4 131.2(5) ?
C1 N3 H3 114.4 ?
C4 N3 H3 114.4 ?
O2 N4 O1 123.8(5) ?
O2 N4 C7 118.8(5) ?
O1 N4 C7 117.4(5) ?
N1 C1 N3 120.2(5) ?
N1 C1 C2 117.8(5) ?
N3 C1 C2 122.0(5) ?
C1 C2 C3 111.4(5) ?
C1 C2 H2A 109.3 ?
C3 C2 H2A 109.3 ?
C1 C2 H2B 109.3 ?
C3 C2 H2B 109.3 ?
H2A C2 H2B 108.0 ?
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 ?
C5 C4 C9 119.9(5) ?
C5 C4 N3 125.1(6) ?
C9 C4 N3 114.8(5) ?
C4 C5 C6 120.0(6) ?
C4 C5 H5 120.0 ?
C6 C5 H5 120.0 ?
C7 C6 C5 118.6(5) ?
C7 C6 H6 120.7 ?
C5 C6 H6 120.7 ?
C8 C7 C6 122.9(6) ?
C8 C7 N4 119.4(5) ?
C6 C7 N4 117.7(5) ?
C7 C8 C9 118.0(5) ?
C7 C8 H8 121.0 ?
C9 C8 H8 121.0 ?
C8 C9 C4 120.5(6) ?
C8 C9 H9 119.7 ?
C4 C9 H9 119.7 ?
N2 C10 C11 176.3(7) ?
C10 C11 C12 111.4(6) ?
C10 C11 H11A 109.3 ?
C12 C11 H11A 109.3 ?
C10 C11 H11B 109.3 ?
C12 C11 H11B 109.3 ?
H11A C11 H11B 108.0 ?
C11 C12 H12A 109.5 ?
C11 C12 H12B 109.5 ?
H12A C12 H12B 109.5 ?
C11 C12 H12C 109.5 ?
H12A C12 H12C 109.5 ?
H12B C12 H12C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 N2 2.005(5) yes
Pt1 N1 2.009(5) yes
Pt1 Cl4 2.3064(15) yes
Pt1 Cl1 2.3202(15) yes
Pt1 Cl2 2.3205(15) yes
Pt1 Cl3 2.3297(14) yes
O1 N4 1.236(7) ?
O2 N4 1.230(7) ?
N1 C1 1.303(7) yes
N1 H1 0.8800 ?
N2 C10 1.128(8) yes
N3 C1 1.340(8) yes
N3 C4 1.418(8) ?
N3 H3 0.8800 ?
N4 C7 1.476(8) ?
C1 C2 1.507(8) ?
C2 C3 1.541(9) ?
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 H3A 0.9800 ?
C3 H3B 0.9800 ?
C3 H3C 0.9800 ?
C4 C5 1.384(9) ?
C4 C9 1.398(9) ?
C5 C6 1.387(9) ?
C5 H5 0.9500 ?
C6 C7 1.385(9) ?
C6 H6 0.9500 ?
C7 C8 1.368(9) ?
C8 C9 1.389(9) ?
C8 H8 0.9500 ?
C9 H9 0.9500 ?
C10 C11 1.452(9) ?
C11 C12 1.501(9) ?
C11 H11A 0.9900 ?
C11 H11B 0.9900 ?
C12 H12A 0.9800 ?
C12 H12B 0.9800 ?
C12 H12C 0.9800 ?
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 O2 0.88 2.36 3.032(7) 133.9 3_685
N1 H1 N4 0.88 3.15 3.926(7) 149.0 3_685
N3 H3 Cl3 0.88 2.37 3.115(5) 142.5 .
N3 H3 Cl2 0.88 2.69 3.225(5) 120.1 .
