#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:27:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179845 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/41/7014153.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_7014153
loop_
_publ_author_name
'Garnovskii, Dmitrii A.'
'Pombeiro, Armando J. L.'
'Haukka, Matti'
'Sobota, Piotr'
'Kukushkin, Vadim Yu'
_publ_section_title
;
 Regioselective HON-addition of bifunctional hydrazone oximes to
 Pt(IV)-bound nitriles.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1097
_journal_page_last               1103
_journal_paper_doi               10.1039/b402105c
_journal_year                    2004
_chemical_formula_sum            'C24 H32 Cl2 N8 O2 Pt'
_chemical_formula_weight         730.57
_chemical_name_common            trans-[PtCl2{NHC(Et)ONC(Me)C(ph)CCH2}2]
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.9160(10)
_cell_angle_beta                 104.1450(10)
_cell_angle_gamma                98.463(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0753(2)
_cell_length_b                   8.6907(3)
_cell_length_c                   10.6485(4)
_cell_measurement_reflns_used    13568
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     704.91(4)
_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    'XP in SHELXTL v.5.1 (Bruker Axs, 1998)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally 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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10837
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    5.203
_exptl_absorpt_correction_T_max  0.26538
_exptl_absorpt_correction_T_min  0.19314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.469
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0260
_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)+(0.0180P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                2697
_reflns_number_total             2761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402105c.txt
_cod_data_source_block           structure_4
_cod_original_cell_volume        704.913(40)
_cod_database_code               7014153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.5000 0.0000 0.02948(8) Uani 1 2 d S . .
Cl1 Cl 0.25928(11) 0.31998(11) 0.00027(9) 0.0397(2) Uani 1 1 d . . .
N1 N 0.3444(4) 0.6299(3) -0.0995(3) 0.0309(7) Uani 1 1 d . . .
N2 N 0.1568(3) 0.7750(3) -0.2648(3) 0.0269(6) Uani 1 1 d . . .
N3 N -0.1429(4) 0.8084(4) -0.5460(3) 0.0375(7) Uani 1 1 d . . .
N4 N -0.1877(5) 0.7619(6) -0.6786(3) 0.0582(11) Uani 1 1 d . . .
O1 O 0.1651(3) 0.8142(3) -0.1271(2) 0.0290(5) Uani 1 1 d . . .
C1 C 0.2673(4) 0.7323(4) -0.0531(3) 0.0261(7) Uani 1 1 d . . .
C2 C 0.2808(5) 0.7802(4) 0.0890(3) 0.0335(8) Uani 1 1 d . . .
H2A H 0.3174 0.6956 0.1368 0.040 Uiso 1 1 calc R . .
H2B H 0.1655 0.7946 0.1000 0.040 Uiso 1 1 calc R . .
C3 C 0.4121(5) 0.9341(5) 0.1475(4) 0.0419(9) Uani 1 1 d . . .
H3A H 0.5261 0.9200 0.1362 0.063 Uiso 1 1 calc R . .
H3B H 0.4209 0.9623 0.2416 0.063 Uiso 1 1 calc R . .
H3C H 0.3736 1.0188 0.1024 0.063 Uiso 1 1 calc R . .
C4 C 0.0332(4) 0.8304(4) -0.3324(3) 0.0276(7) Uani 1 1 d . . .
C5 C -0.0842(5) 0.9213(5) -0.2757(4) 0.0389(9) Uani 1 1 d . . .
H5A H -0.1639 0.8491 -0.2446 0.058 Uiso 1 1 calc R . .
H5B H -0.1512 0.9703 -0.3437 0.058 Uiso 1 1 calc R . .
H5C H -0.0140 1.0037 -0.2019 0.058 Uiso 1 1 calc R . .
C6 C 0.0057(4) 0.7898(4) -0.4762(3) 0.0278(7) Uani 1 1 d . . .
C7 C 0.1423(4) 0.7267(4) -0.5283(3) 0.0278(7) Uani 1 1 d . . .
C8 C 0.1039(5) 0.5832(4) -0.6152(4) 0.0389(9) Uani 1 1 d . . .
H8 H -0.0117 0.5245 -0.6430 0.047 Uiso 1 1 calc R . .
C9 C 0.2328(6) 0.5250(5) -0.6615(4) 0.0495(11) Uani 1 1 d . . .
H9 H 0.2048 0.4275 -0.7216 0.059 Uiso 1 1 calc R . .
C10 C 0.4009(6) 0.6078(5) -0.6207(4) 0.0466(10) Uani 1 1 d . . .
H10 H 0.4894 0.5666 -0.6513 0.056 Uiso 1 1 calc R . .
C11 C 0.4413(5) 0.7517(5) -0.5349(4) 0.0414(9) Uani 1 1 d . . .
H11 H 0.5571 0.8099 -0.5072 0.050 Uiso 1 1 calc R . .
C12 C 0.3122(4) 0.8096(4) -0.4901(3) 0.0351(8) Uani 1 1 d . . .
H12 H 0.3402 0.9084 -0.4318 0.042 Uiso 1 1 calc R . .
H1 H 0.320(5) 0.617(4) -0.188(4) 0.038(10) Uiso 1 1 d . . .
H4A H -0.097(6) 0.746(6) -0.718(5) 0.069(15) Uiso 1 1 d . . .
H4B H -0.286(6) 0.797(6) -0.725(5) 0.067(14) Uiso 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pt1 N1 180.0 2_665 . ?
N1 Pt1 Cl1 90.30(9) 2_665 2_665 ?
N1 Pt1 Cl1 89.70(9) . 2_665 ?
N1 Pt1 Cl1 89.70(9) 2_665 . ?
N1 Pt1 Cl1 90.30(9) . . ?
Cl1 Pt1 Cl1 180.00(4) 2_665 . ?
C1 N1 Pt1 127.9(2) . . ?
C1 N1 H1 112(2) . . ?
Pt1 N1 H1 121(2) . . ?
C4 N2 O1 109.2(2) . . ?
C6 N3 N4 119.6(3) . . ?
N3 N4 H4A 117(3) . . ?
N3 N4 H4B 115(3) . . ?
H4A N4 H4B 120(4) . . ?
C1 O1 N2 112.1(2) . . ?
N1 C1 O1 124.1(3) . . ?
N1 C1 C2 124.8(3) . . ?
O1 C1 C2 111.2(3) . . ?
C1 C2 C3 110.8(3) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
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 . . ?
N2 C4 C6 114.1(3) . . ?
N2 C4 C5 124.8(3) . . ?
C6 C4 C5 121.0(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C4 114.8(3) . . ?
N3 C6 C7 125.9(3) . . ?
C4 C6 C7 119.3(3) . . ?
C12 C7 C8 118.2(3) . . ?
C12 C7 C6 120.6(3) . . ?
C8 C7 C6 121.2(3) . . ?
C9 C8 C7 120.6(4) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.0(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 119.5(4) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C7 121.5(3) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
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 N1 2.018(3) 2_665 ?
Pt1 N1 2.018(3) . ?
Pt1 Cl1 2.3098(9) 2_665 ?
Pt1 Cl1 2.3098(9) . ?
N1 C1 1.271(4) . ?
N1 H1 0.90(4) . ?
N2 C4 1.278(4) . ?
N2 O1 1.442(3) . ?
N3 C6 1.293(4) . ?
N3 N4 1.355(4) . ?
N4 H4A 0.94(5) . ?
N4 H4B 0.94(5) . ?
O1 C1 1.348(4) . ?
C1 C2 1.486(5) . ?
C2 C3 1.527(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C6 1.476(5) . ?
C4 C5 1.502(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.489(5) . ?
C7 C12 1.386(5) . ?
C7 C8 1.392(5) . ?
C8 C9 1.385(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
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 N2 0.90(4) 2.14(4) 2.618(4) 112(3) .
C5 H5B N3 0.98 2.43 2.809(5) 102.6 .
C11 H11 N3 0.95 2.56 3.355(5) 141.8 1_655
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Pt1 N1 C1 79(80) 2_665 . . . ?
Cl1 Pt1 N1 C1 -97.0(3) 2_665 . . . ?
Cl1 Pt1 N1 C1 83.0(3) . . . . ?
C4 N2 O1 C1 167.1(3) . . . . ?
Pt1 N1 C1 O1 180.0(2) . . . . ?
Pt1 N1 C1 C2 1.5(5) . . . . ?
N2 O1 C1 N1 -1.4(4) . . . . ?
N2 O1 C1 C2 177.3(2) . . . . ?
N1 C1 C2 C3 98.8(4) . . . . ?
O1 C1 C2 C3 -79.9(4) . . . . ?
O1 N2 C4 C6 -176.7(2) . . . . ?
O1 N2 C4 C5 -0.3(4) . . . . ?
N4 N3 C6 C4 -174.4(3) . . . . ?
N4 N3 C6 C7 3.1(6) . . . . ?
N2 C4 C6 N3 163.0(3) . . . . ?
C5 C4 C6 N3 -13.6(5) . . . . ?
N2 C4 C6 C7 -14.7(5) . . . . ?
C5 C4 C6 C7 168.7(3) . . . . ?
N3 C6 C7 C12 128.0(4) . . . . ?
C4 C6 C7 C12 -54.6(5) . . . . ?
N3 C6 C7 C8 -52.6(5) . . . . ?
C4 C6 C7 C8 124.8(4) . . . . ?
C12 C7 C8 C9 0.2(6) . . . . ?
C6 C7 C8 C9 -179.2(4) . . . . ?
C7 C8 C9 C10 0.8(6) . . . . ?
C8 C9 C10 C11 -1.2(6) . . . . ?
C9 C10 C11 C12 0.6(6) . . . . ?
C10 C11 C12 C7 0.4(6) . . . . ?
C8 C7 C12 C11 -0.8(5) . . . . ?
C6 C7 C12 C11 178.6(3) . . . . ?
