#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001474.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_7001474
loop_
_publ_author_name
'Sarkar, Biprajit'
'Hübner, Ralph'
'Pattacini, Roberto'
'Hartenbach, Ingo'
_publ_section_title
;
 Combining two non-innocent ligands in isomeric complexes [Pt(pap)mQn]0
 (pap = phenylazopyridine, Q = 3,5-di-tert-butyl-benzoquinone
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4653
_journal_page_last               4655
_journal_paper_doi               10.1039/b902645b
_journal_year                    2009
_chemical_formula_moiety         'C25 H29 N3 O2 Pt'
_chemical_formula_sum            'C25 H29 N3 O2 Pt'
_chemical_formula_weight         598.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                101.695(2)
_cell_angle_beta                 95.843(3)
_cell_angle_gamma                91.407(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9677(3)
_cell_length_b                   10.7867(6)
_cell_length_c                   15.6342(7)
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      0.998
_cell_volume                     1143.44(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9059
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.162
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.627
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0620P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                5701
_reflns_number_total             6626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902645b.txt
_cod_data_source_block           Bipro2
_cod_database_code               7001474
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 0.25582(3) 0.11812(2) 0.463629(13) 0.01971(8) Uani 1 1 d . . .
O1 O 0.2755(7) 0.1539(4) 0.3445(3) 0.0247(9) Uani 1 1 d . . .
O2 O 0.2758(6) -0.0581(4) 0.4017(3) 0.0249(9) Uani 1 1 d . . .
N1 N 0.2345(7) 0.2885(5) 0.5379(3) 0.0208(10) Uani 1 1 d . . .
N2 N 0.2359(7) 0.0778(5) 0.5796(3) 0.0200(10) Uani 1 1 d . . .
N3 N 0.2201(8) 0.2979(5) 0.6216(3) 0.0249(11) Uani 1 1 d . . .
C1 C 0.2797(9) 0.0456(6) 0.2828(4) 0.0221(12) Uani 1 1 d . . .
C2 C 0.2833(8) -0.0685(6) 0.3145(4) 0.0213(11) Uani 1 1 d . . .
C3 C 0.2870(9) -0.1845(6) 0.2581(4) 0.0244(12) Uani 1 1 d . . .
H3 H 0.2940 -0.2581 0.2804 0.029 Uiso 1 1 calc R . .
C4 C 0.2802(9) -0.1917(6) 0.1677(4) 0.0243(12) Uani 1 1 d . . .
C5 C 0.2759(9) -0.0782(6) 0.1378(4) 0.0264(13) Uani 1 1 d . . .
H5 H 0.2724 -0.0825 0.0777 0.032 Uiso 1 1 calc R . .
C6 C 0.2765(9) 0.0404(6) 0.1922(4) 0.0235(12) Uani 1 1 d . . .
C7 C 0.2766(9) -0.3219(6) 0.1060(4) 0.0263(13) Uani 1 1 d . . .
C8 C 0.1018(13) -0.4031(8) 0.1201(5) 0.047(2) Uani 1 1 d . . .
H8A H 0.1082 -0.4083 0.1809 0.070 Uiso 1 1 calc R . .
H8B H 0.1040 -0.4866 0.0846 0.070 Uiso 1 1 calc R . .
H8C H -0.0155 -0.3647 0.1038 0.070 Uiso 1 1 calc R . .
C9 C 0.4618(14) -0.3919(8) 0.1261(5) 0.055(2) Uani 1 1 d . . .
H9A H 0.5721 -0.3456 0.1143 0.083 Uiso 1 1 calc R . .
H9B H 0.4529 -0.4754 0.0897 0.083 Uiso 1 1 calc R . .
H9C H 0.4752 -0.3981 0.1868 0.083 Uiso 1 1 calc R . .
C10 C 0.2540(11) -0.3136(7) 0.0088(4) 0.0361(16) Uani 1 1 d . . .
H10A H 0.1334 -0.2770 -0.0050 0.054 Uiso 1 1 calc R . .
H10B H 0.2559 -0.3971 -0.0270 0.054 Uiso 1 1 calc R . .
H10C H 0.3584 -0.2616 -0.0025 0.054 Uiso 1 1 calc R . .
C11 C 0.2661(10) 0.1633(7) 0.1558(4) 0.0292(14) Uani 1 1 d . . .
C12 C 0.0763(11) 0.2280(7) 0.1775(5) 0.0354(15) Uani 1 1 d . . .
H12A H 0.0724 0.2465 0.2400 0.053 Uiso 1 1 calc R . .
H12B H -0.0319 0.1724 0.1499 0.053 Uiso 1 1 calc R . .
H12C H 0.0706 0.3054 0.1561 0.053 Uiso 1 1 calc R . .
C13 C 0.4407(11) 0.2542(7) 0.1972(5) 0.0397(18) Uani 1 1 d . . .
H13A H 0.4407 0.2741 0.2599 0.060 Uiso 1 1 calc R . .
H13B H 0.4320 0.3307 0.1749 0.060 Uiso 1 1 calc R . .
H13C H 0.5581 0.2142 0.1826 0.060 Uiso 1 1 calc R . .
C14 C 0.2640(11) 0.1364(7) 0.0548(5) 0.0364(16) Uani 1 1 d . . .
H14A H 0.2784 0.2150 0.0357 0.055 Uiso 1 1 calc R . .
H14B H 0.1436 0.0938 0.0280 0.055 Uiso 1 1 calc R . .
H14C H 0.3686 0.0838 0.0379 0.055 Uiso 1 1 calc R . .
C15 C 0.2179(9) 0.1802(6) 0.6449(4) 0.0237(12) Uani 1 1 d . . .
C16 C 0.1948(10) 0.1689(7) 0.7285(4) 0.0303(14) Uani 1 1 d . . .
H16 H 0.1786 0.2402 0.7714 0.036 Uiso 1 1 calc R . .
C17 C 0.1959(10) 0.0495(7) 0.7486(5) 0.0329(15) Uani 1 1 d . . .
H17 H 0.1823 0.0396 0.8055 0.039 Uiso 1 1 calc R . .
C18 C 0.2177(10) -0.0545(7) 0.6830(4) 0.0307(14) Uani 1 1 d . . .
H18 H 0.2199 -0.1354 0.6953 0.037 Uiso 1 1 calc R . .
C19 C 0.2361(9) -0.0372(6) 0.5989(4) 0.0272(13) Uani 1 1 d . . .
H19 H 0.2489 -0.1075 0.5546 0.033 Uiso 1 1 calc R . .
C20 C 0.2399(9) 0.4088(6) 0.5122(4) 0.0244(12) Uani 1 1 d . . .
C21 C 0.3189(9) 0.5154(6) 0.5707(4) 0.0249(12) Uani 1 1 d . . .
H21 H 0.3653 0.5115 0.6280 0.030 Uiso 1 1 calc R . .
C22 C 0.3269(9) 0.6272(6) 0.5419(4) 0.0272(13) Uani 1 1 d . . .
H22 H 0.3818 0.6998 0.5801 0.033 Uiso 1 1 calc R . .
C23 C 0.2553(9) 0.6344(6) 0.4577(4) 0.0301(15) Uani 1 1 d . . .
H23 H 0.2621 0.7112 0.4396 0.036 Uiso 1 1 calc R . .
C24 C 0.1736(10) 0.5275(6) 0.4002(4) 0.0284(13) Uani 1 1 d . . .
H24 H 0.1241 0.5325 0.3435 0.034 Uiso 1 1 calc R . .
C25 C 0.1652(9) 0.4136(6) 0.4266(4) 0.0249(12) Uani 1 1 d . . .
H25 H 0.1108 0.3411 0.3882 0.030 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
Pt Pt -1.7033 8.3905 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N2 Pt1 O2 95.60(19) . . ?
N2 Pt1 N1 78.1(2) . . ?
O2 Pt1 N1 173.74(17) . . ?
N2 Pt1 O1 178.42(18) . . ?
O2 Pt1 O1 82.84(17) . . ?
N1 Pt1 O1 103.4(2) . . ?
C1 O1 Pt1 111.8(4) . . ?
C2 O2 Pt1 112.5(4) . . ?
N3 N1 C20 113.3(5) . . ?
N3 N1 Pt1 118.7(4) . . ?
C20 N1 Pt1 128.0(4) . . ?
C19 N2 C15 118.7(5) . . ?
C19 N2 Pt1 126.7(5) . . ?
C15 N2 Pt1 114.5(4) . . ?
N1 N3 C15 112.1(5) . . ?
O1 C1 C6 124.7(5) . . ?
O1 C1 C2 115.9(5) . . ?
C6 C1 C2 119.4(6) . . ?
O2 C2 C3 121.9(5) . . ?
O2 C2 C1 116.8(5) . . ?
C3 C2 C1 121.2(5) . . ?
C2 C3 C4 120.2(6) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 117.6(6) . . ?
C3 C4 C7 119.4(5) . . ?
C5 C4 C7 123.0(5) . . ?
C6 C5 C4 124.1(6) . . ?
C6 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
C5 C6 C1 117.4(5) . . ?
C5 C6 C11 122.2(6) . . ?
C1 C6 C11 120.4(6) . . ?
C4 C7 C10 112.7(5) . . ?
C4 C7 C8 109.2(5) . . ?
C10 C7 C8 106.8(6) . . ?
C4 C7 C9 110.7(5) . . ?
C10 C7 C9 109.4(6) . . ?
C8 C7 C9 107.9(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C6 110.1(5) . . ?
C13 C11 C14 108.8(6) . . ?
C6 C11 C14 112.0(6) . . ?
C13 C11 C12 109.8(6) . . ?
C6 C11 C12 109.2(5) . . ?
C14 C11 C12 107.0(5) . . ?
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 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 122.2(6) . . ?
N2 C15 N3 116.5(5) . . ?
C16 C15 N3 121.2(6) . . ?
C15 C16 C17 119.0(7) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C18 C17 C16 119.0(6) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 119.3(6) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
N2 C19 C18 121.7(6) . . ?
N2 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C21 C20 C25 121.7(6) . . ?
C21 C20 N1 120.2(6) . . ?
C25 C20 N1 118.0(5) . . ?
C22 C21 C20 118.0(6) . . ?
C22 C21 H21 121.0 . . ?
C20 C21 H21 121.0 . . ?
C21 C22 C23 121.5(6) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C24 120.0(6) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.1(6) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C20 118.8(6) . . ?
C24 C25 H25 120.6 . . ?
C20 C25 H25 120.6 . . ?
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 N2 1.966(5) . ?
Pt1 O2 1.966(5) . ?
Pt1 N1 1.983(5) . ?
Pt1 O1 1.994(4) . ?
O1 C1 1.360(7) . ?
O2 C2 1.353(7) . ?
N1 N3 1.307(7) . ?
N1 C20 1.435(8) . ?
N2 C19 1.334(8) . ?
N2 C15 1.362(8) . ?
N3 C15 1.390(8) . ?
C1 C6 1.405(9) . ?
C1 C2 1.416(8) . ?
C2 C3 1.379(9) . ?
C3 C4 1.395(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(9) . ?
C4 C7 1.532(9) . ?
C5 C6 1.385(9) . ?
C5 H5 0.9300 . ?
C6 C11 1.545(8) . ?
C7 C10 1.533(8) . ?
C7 C8 1.542(9) . ?
C7 C9 1.548(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.544(10) . ?
C11 C14 1.545(9) . ?
C11 C12 1.546(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.362(9) . ?
C16 C17 1.386(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(9) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.379(9) . ?
C20 C25 1.397(9) . ?
C21 C22 1.373(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.378(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.380(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(8) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
