#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:27:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179845 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/41/7014154.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_7014154
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            'C38 H38 Cl2 N10 O8 Pt'
_chemical_formula_weight         1028.77
_chemical_name_common
trans-[PtCl2{NHC(Et)ONC(Me)C(Ph)NNCH(C6H3-2-OH-5-NO2}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                109.4880(10)
_cell_angle_beta                 101.5020(10)
_cell_angle_gamma                100.2610(10)
_cell_formula_units_Z            1
_cell_length_a                   8.7209(2)
_cell_length_b                   10.9317(2)
_cell_length_c                   11.9651(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1016.11(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.6.12 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16718
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    3.648
_exptl_absorpt_correction_T_max  0.37318
_exptl_absorpt_correction_T_min  0.31969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v. 6.12 (Bruker AXS, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0300
_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)+(0.0181P)²+0.9555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                3878
_reflns_number_total             3974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402105c.txt
_cod_data_source_block           structure_5
_cod_original_cell_volume        1016.11(3)
_cod_database_code               7014154
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 1.0000 1.0000 1.0000 0.02264(8) Uani 1 2 d S . .
Cl1 Cl 0.91517(12) 1.12819(10) 1.16033(8) 0.0331(2) Uani 1 1 d . . .
O1 O 0.5128(3) 0.7522(3) 0.8262(2) 0.0271(6) Uani 1 1 d . . .
O2 O 0.4023(3) 0.6095(3) 0.1284(2) 0.0372(7) Uani 1 1 d . . .
O3 O -0.2030(4) 0.1288(3) -0.2053(3) 0.0420(7) Uani 1 1 d . . .
O4 O -0.1162(4) 0.1871(3) -0.3419(2) 0.0443(8) Uani 1 1 d . . .
N1 N 0.7738(4) 0.8931(3) 0.8956(3) 0.0257(7) Uani 1 1 d . . .
H1 H 0.7540 0.8892 0.8193 0.031 Uiso 1 1 calc R . .
N2 N 0.5237(4) 0.7486(3) 0.7081(3) 0.0282(7) Uani 1 1 d . . .
N3 N 0.2744(4) 0.5702(3) 0.4114(3) 0.0309(7) Uani 1 1 d . . .
N4 N 0.2848(4) 0.5531(3) 0.2919(3) 0.0301(7) Uani 1 1 d . . .
N5 N -0.1075(4) 0.2005(3) -0.2347(3) 0.0310(7) Uani 1 1 d . . .
C1 C 0.6543(4) 0.8304(4) 0.9174(3) 0.0231(8) Uani 1 1 d . . .
C2 C 0.6391(5) 0.8251(4) 1.0382(3) 0.0258(8) Uani 1 1 d . . .
H2A H 0.7453 0.8708 1.1011 0.031 Uiso 1 1 calc R . .
H2B H 0.6105 0.7299 1.0295 0.031 Uiso 1 1 calc R . .
C3 C 0.5108(5) 0.8917(4) 1.0828(3) 0.0324(9) Uani 1 1 d . . .
H3A H 0.5514 0.9897 1.1116 0.049 Uiso 1 1 calc R . .
H3B H 0.4873 0.8678 1.1508 0.049 Uiso 1 1 calc R . .
H3C H 0.4113 0.8604 1.0147 0.049 Uiso 1 1 calc R . .
C4 C 0.3922(5) 0.6734(4) 0.6251(3) 0.0262(8) Uani 1 1 d . . .
C5 C 0.2448(5) 0.6037(4) 0.6479(4) 0.0391(10) Uani 1 1 d . . .
H5A H 0.2635 0.5242 0.6630 0.059 Uiso 1 1 calc R . .
H5B H 0.1516 0.5761 0.5754 0.059 Uiso 1 1 calc R . .
H5C H 0.2227 0.6653 0.7200 0.059 Uiso 1 1 calc R . .
C6 C 0.3982(5) 0.6586(4) 0.4980(3) 0.0264(8) Uani 1 1 d . . .
C7 C 0.5389(5) 0.7394(4) 0.4782(3) 0.0278(8) Uani 1 1 d . . .
C8 C 0.5161(5) 0.8340(4) 0.4256(3) 0.0319(9) Uani 1 1 d . . .
H8 H 0.4116 0.8483 0.4051 0.038 Uiso 1 1 calc R . .
C9 C 0.6450(5) 0.9064(4) 0.4035(3) 0.0363(10) Uani 1 1 d . . .
H9 H 0.6288 0.9707 0.3682 0.044 Uiso 1 1 calc R . .
C10 C 0.7960(6) 0.8864(5) 0.4319(4) 0.0428(11) Uani 1 1 d . . .
H10 H 0.8834 0.9347 0.4139 0.051 Uiso 1 1 calc R . .
C11 C 0.8217(5) 0.7953(4) 0.4872(4) 0.0391(10) Uani 1 1 d . . .
H11 H 0.9270 0.7827 0.5083 0.047 Uiso 1 1 calc R . .
C12 C 0.6946(5) 0.7234(4) 0.5113(4) 0.0328(9) Uani 1 1 d . . .
H12 H 0.7130 0.6627 0.5506 0.039 Uiso 1 1 calc R . .
C13 C 0.1679(5) 0.4600(4) 0.2067(3) 0.0270(8) Uani 1 1 d . . .
H13 H 0.0866 0.4085 0.2274 0.032 Uiso 1 1 calc R . .
C14 C 0.1604(4) 0.4337(3) 0.0781(3) 0.0228(7) Uani 1 1 d . . .
C15 C 0.0335(4) 0.3312(4) -0.0152(3) 0.0255(8) Uani 1 1 d . . .
H15 H -0.0466 0.2778 0.0050 0.031 Uiso 1 1 calc R . .
C16 C 0.0260(4) 0.3086(4) -0.1373(3) 0.0265(8) Uani 1 1 d . . .
C17 C 0.1381(5) 0.3839(4) -0.1703(3) 0.0287(8) Uani 1 1 d . . .
H17 H 0.1296 0.3657 -0.2550 0.034 Uiso 1 1 calc R . .
C18 C 0.2634(5) 0.4866(4) -0.0798(3) 0.0307(9) Uani 1 1 d . . .
H18 H 0.3401 0.5405 -0.1022 0.037 Uiso 1 1 calc R . .
C19 C 0.2773(5) 0.5113(4) 0.0447(3) 0.0283(8) Uani 1 1 d . . .
H02 H 0.4029 0.6194 0.2132 0.050 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_777 . ?
N1 Pt1 Cl1 85.88(9) 2_777 . ?
N1 Pt1 Cl1 94.12(9) . . ?
N1 Pt1 Cl1 94.12(9) 2_777 2_777 ?
N1 Pt1 Cl1 85.88(9) . 2_777 ?
Cl1 Pt1 Cl1 180.0 . 2_777 ?
C1 O1 N2 111.5(3) . . ?
C19 O2 H02 112.2 . . ?
C1 N1 Pt1 133.0(2) . . ?
C1 N1 H1 113.5 . . ?
Pt1 N1 H1 113.5 . . ?
C4 N2 O1 110.1(3) . . ?
C6 N3 N4 113.6(3) . . ?
C13 N4 N3 113.5(3) . . ?
O3 N5 O4 123.6(3) . . ?
O3 N5 C16 118.8(3) . . ?
O4 N5 C16 117.5(3) . . ?
N1 C1 O1 122.6(3) . . ?
N1 C1 C2 128.2(3) . . ?
O1 C1 C2 109.2(3) . . ?
C1 C2 C3 112.6(3) . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
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 113.2(3) . . ?
N2 C4 C5 125.6(3) . . ?
C6 C4 C5 121.2(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 C7 125.5(3) . . ?
N3 C6 C4 114.1(3) . . ?
C7 C6 C4 120.4(3) . . ?
C12 C7 C8 118.9(4) . . ?
C12 C7 C6 121.3(3) . . ?
C8 C7 C6 119.8(3) . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 120.6(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.0(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.1(4) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 120.2(4) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N4 C13 C14 119.6(3) . . ?
N4 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C19 118.9(3) . . ?
C15 C14 C13 119.7(3) . . ?
C19 C14 C13 121.4(3) . . ?
C16 C15 C14 119.2(3) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C17 C16 C15 122.2(3) . . ?
C17 C16 N5 118.9(3) . . ?
C15 C16 N5 118.8(3) . . ?
C16 C17 C18 119.6(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
O2 C19 C18 117.7(3) . . ?
O2 C19 C14 122.3(3) . . ?
C18 C19 C14 120.0(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 2.009(3) 2_777 ?
Pt1 N1 2.009(3) . ?
Pt1 Cl1 2.3092(9) . ?
Pt1 Cl1 2.3092(9) 2_777 ?
O1 C1 1.381(4) . ?
O1 N2 1.423(4) . ?
O2 C19 1.332(4) . ?
O2 H02 0.9827 . ?
O3 N5 1.225(4) . ?
O4 N5 1.225(4) . ?
N1 C1 1.264(5) . ?
N1 H1 0.8800 . ?
N2 C4 1.282(5) . ?
N3 C6 1.299(5) . ?
N3 N4 1.402(4) . ?
N4 C13 1.280(5) . ?
N5 C16 1.470(5) . ?
C1 C2 1.497(5) . ?
C2 C3 1.529(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C6 1.488(5) . ?
C4 C5 1.495(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.487(5) . ?
C7 C12 1.396(6) . ?
C7 C8 1.401(5) . ?
C8 C9 1.379(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.368(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.393(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.453(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(5) . ?
C14 C19 1.414(5) . ?
C15 C16 1.383(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.369(5) . ?
C17 C18 1.381(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.399(5) . ?
C18 H18 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
O2 H02 N4 0.98 1.75 2.576(4) 139.8 .
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 -161(100) 2_777 . . . ?
Cl1 Pt1 N1 C1 -49.7(4) . . . . ?
Cl1 Pt1 N1 C1 130.3(4) 2_777 . . . ?
C1 O1 N2 C4 178.8(3) . . . . ?
C6 N3 N4 C13 175.8(3) . . . . ?
Pt1 N1 C1 O1 -173.7(2) . . . . ?
Pt1 N1 C1 C2 5.7(6) . . . . ?
N2 O1 C1 N1 2.2(5) . . . . ?
N2 O1 C1 C2 -177.2(3) . . . . ?
N1 C1 C2 C3 114.2(4) . . . . ?
O1 C1 C2 C3 -66.4(4) . . . . ?
O1 N2 C4 C6 -176.8(3) . . . . ?
O1 N2 C4 C5 2.5(5) . . . . ?
N4 N3 C6 C7 1.5(6) . . . . ?
N4 N3 C6 C4 -177.4(3) . . . . ?
N2 C4 C6 N3 172.0(3) . . . . ?
C5 C4 C6 N3 -7.3(5) . . . . ?
N2 C4 C6 C7 -6.9(5) . . . . ?
C5 C4 C6 C7 173.8(4) . . . . ?
N3 C6 C7 C12 -114.7(4) . . . . ?
C4 C6 C7 C12 64.1(5) . . . . ?
N3 C6 C7 C8 65.5(5) . . . . ?
C4 C6 C7 C8 -115.7(4) . . . . ?
C12 C7 C8 C9 2.1(5) . . . . ?
C6 C7 C8 C9 -178.0(3) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C8 C9 C10 C11 -2.0(6) . . . . ?
C9 C10 C11 C12 1.2(6) . . . . ?
C10 C11 C12 C7 1.3(6) . . . . ?
C8 C7 C12 C11 -2.9(6) . . . . ?
C6 C7 C12 C11 177.2(3) . . . . ?
N3 N4 C13 C14 178.2(3) . . . . ?
N4 C13 C14 C15 179.4(4) . . . . ?
N4 C13 C14 C19 -1.8(6) . . . . ?
C19 C14 C15 C16 0.1(5) . . . . ?
C13 C14 C15 C16 178.9(3) . . . . ?
C14 C15 C16 C17 -0.6(6) . . . . ?
C14 C15 C16 N5 179.8(3) . . . . ?
O3 N5 C16 C17 176.4(3) . . . . ?
O4 N5 C16 C17 -3.3(5) . . . . ?
O3 N5 C16 C15 -4.0(5) . . . . ?
O4 N5 C16 C15 176.2(3) . . . . ?
C15 C16 C17 C18 -0.1(6) . . . . ?
N5 C16 C17 C18 179.4(3) . . . . ?
C16 C17 C18 C19 1.4(6) . . . . ?
C17 C18 C19 O2 178.6(4) . . . . ?
C17 C18 C19 C14 -1.9(6) . . . . ?
C15 C14 C19 O2 -179.3(4) . . . . ?
C13 C14 C19 O2 1.9(6) . . . . ?
C15 C14 C19 C18 1.1(6) . . . . ?
C13 C14 C19 C18 -177.7(4) . . . . ?
