#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:03:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179090 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/52/4305207.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_4305207
loop_
_publ_author_name
'Pavel V. Gushchin'
'Marina R. Tyan'
'Nadezhda A. Bokach'
'Mikhail D. Revenco'
'Matti Haukka'
'Meng-Jiy Wang'
'Cheng-Hsuan Lai'
'Pi-Tai Chou'
'Vadim Yu. Kukushkin'
_publ_section_title
;
Novel Tailoring Reaction for Two Adjacent Coordinated Nitriles Giving
Platinum 1,3,5-Triazapentadiene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11487
_journal_page_last               11500
_journal_paper_doi               10.1021/ic702483w
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C32 H34 N8 Pt'
_chemical_formula_sum            'C32 H34 N8 Pt'
_chemical_formula_weight         725.76
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.3050(10)
_cell_angle_beta                 101.928(2)
_cell_angle_gamma                103.712(2)
_cell_formula_units_Z            1
_cell_length_a                   5.9465(2)
_cell_length_b                   11.2920(3)
_cell_length_c                   12.0993(4)
_cell_measurement_reflns_used    3225
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.27
_cell_volume                     707.99(4)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1e (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      120(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  '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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9087
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    4.992
_exptl_absorpt_correction_T_max  0.4502
_exptl_absorpt_correction_T_min  0.2832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.883
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0212P)²+0.1050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                3225
_reflns_number_total             3225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702483w-gushchin_8.cif
_cod_data_source_block           14
_cod_database_code               4305207
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 0.0000 0.0000 0.01338(5) Uani 1 2 d S .. .
N1 N -0.2139(4) 0.12267(19) -0.02038(18) 0.0155(4) Uani 1 1 d . . .
N2 N -0.0220(4) 0.27086(19) 0.19242(19) 0.0178(4) Uani 1 1 d . . .
N3 N -0.4148(4) 0.13676(19) 0.16967(19) 0.0166(4) Uani 1 1 d . . .
H3 H -0.5331 0.1257 0.2074 0.025 Uiso 1 1 d . . ..
N5 N 0.1618(4) 0.2872(2) 0.0470(2) 0.0222(4) Uani 1 1 d . . .
H5N H 0.1690 0.2514 -0.0233 0.033 Uiso 1 1 d . . ..
C1 C -0.0349(4) 0.2233(2) 0.0740(2) 0.0173(5) Uani 1 1 d . . .
C2 C -0.2129(4) 0.2368(2) 0.2320(2) 0.0178(5) Uani 1 1 d . . .
C10 C -0.2016(4) 0.0958(2) -0.1427(2) 0.0154(4) Uani 1 1 d . . .
C11 C -0.3449(4) 0.1356(2) -0.2204(2) 0.0188(5) Uani 1 1 d . . .
H11 H -0.4489 0.1822 -0.1918 0.023 Uiso 1 1 calc R .. .
C12 C -0.3350(5) 0.1069(3) -0.3395(2) 0.0228(5) Uani 1 1 d . . .
H12 H -0.4334 0.1338 -0.3923 0.027 Uiso 1 1 calc R .. .
C13 C -0.1828(5) 0.0391(3) -0.3826(2) 0.0243(5) Uani 1 1 d . . .
H13 H -0.1759 0.0207 -0.4641 0.029 Uiso 1 1 calc R .. .
C14 C -0.0424(5) -0.0011(3) -0.3063(2) 0.0237(5) Uani 1 1 d . . .
H14 H 0.0619 -0.0474 -0.3353 0.028 Uiso 1 1 calc R .. .
C15 C -0.0524(4) 0.0257(2) -0.1868(2) 0.0197(5) Uani 1 1 d . . .
H15 H 0.0425 -0.0039 -0.1351 0.024 Uiso 1 1 calc R .. .
C16 C 0.3722(4) 0.3976(2) 0.1241(2) 0.0191(5) Uani 1 1 d . . .
C17 C 0.5707(5) 0.4103(2) 0.0792(3) 0.0223(5) Uani 1 1 d . . .
H17 H 0.5604 0.3440 0.0037 0.027 Uiso 1 1 calc R . ..
C18 C 0.7823(5) 0.5181(3) 0.1431(3) 0.0269(6) Uani 1 1 d . . .
H18 H 0.9153 0.5258 0.1109 0.032 Uiso 1 1 calc R . ..
C19 C 0.8007(5) 0.6144(3) 0.2536(3) 0.0313(6) Uani 1 1 d . . .
H19 H 0.9465 0.6880 0.2982 0.038 Uiso 1 1 calc R . ..
C20 C 0.6044(5) 0.6028(3) 0.2988(3) 0.0310(6) Uani 1 1 d . . .
H20 H 0.6169 0.6692 0.3748 0.037 Uiso 1 1 calc R . ..
C21 C 0.3889(5) 0.4955(2) 0.2351(3) 0.0258(6) Uani 1 1 d . . .
H21 H 0.2551 0.4891 0.2668 0.031 Uiso 1 1 calc R . ..
C22 C -0.1717(5) 0.3290(3) 0.3635(2) 0.0252(5) Uani 1 1 d . . .
H22A H -0.1450 0.4203 0.3669 0.030 Uiso 1 1 calc R .. .
H22B H -0.0200 0.3295 0.4163 0.030 Uiso 1 1 calc R .. .
C23 C -0.3743(6) 0.2965(3) 0.4189(3) 0.0373(7) Uani 1 1 d . . .
H23A H -0.5255 0.2977 0.3691 0.056 Uiso 1 1 calc R .. .
H23B H -0.3291 0.3627 0.5033 0.056 Uiso 1 1 calc R .. .
H23C H -0.3984 0.2080 0.4200 0.056 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'
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
N3 Pt1 N3 180.0 2_455 . ?
N3 Pt1 N1 87.23(8) 2_455 2_455 ?
N3 Pt1 N1 92.77(8) . 2_455 ?
N3 Pt1 N1 92.77(8) 2_455 . ?
N3 Pt1 N1 87.23(8) . . ?
N1 Pt1 N1 180.0 2_455 . ?
C1 N1 C10 118.72(19) . . ?
C1 N1 Pt1 123.78(16) . . ?
C10 N1 Pt1 117.46(14) . . ?
C1 N2 C2 122.8(2) . . ?
C2 N3 Pt1 127.65(16) . . ?
C2 N3 H3 117.7 . . ?
Pt1 N3 H3 114.6 . . ?
C1 N5 C16 130.5(2) . . ?
C1 N5 H5N 116.4 . . ?
C16 N5 H5N 112.6 . . ?
N2 C1 N1 128.0(2) . . ?
N2 C1 N5 115.0(2) . . ?
N1 C1 N5 117.0(2) . . ?
N3 C2 N2 126.6(2) . . ?
N3 C2 C22 121.1(2) . . ?
N2 C2 C22 112.3(2) . . ?
C11 C10 C15 119.4(2) . . ?
C11 C10 N1 120.2(2) . . ?
C15 C10 N1 120.4(2) . . ?
C12 C11 C10 119.7(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.9(2) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 119.5(2) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.3(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C10 120.2(2) . . ?
C14 C15 H15 119.9 . . ?
C10 C15 H15 119.9 . . ?
C21 C16 C17 119.1(2) . . ?
C21 C16 N5 125.2(2) . . ?
C17 C16 N5 115.5(2) . . ?
C18 C17 C16 120.9(2) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C19 C18 C17 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 119.3(2) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 121.3(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C20 C21 C16 119.1(2) . . ?
C20 C21 H21 120.4 . . ?
C16 C21 H21 120.4 . . ?
C2 C22 C23 116.5(2) . . ?
C2 C22 H22A 108.2 . . ?
C23 C22 H22A 108.2 . . ?
C2 C22 H22B 108.2 . . ?
C23 C22 H22B 108.2 . . ?
H22A C22 H22B 107.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
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 N3 1.990(2) 2_455 ?
Pt1 N3 1.990(2) . ?
Pt1 N1 2.0385(19) 2_455 ?
Pt1 N1 2.0385(19) . ?
N1 C1 1.339(3) . ?
N1 C10 1.431(3) . ?
N2 C1 1.332(3) . ?
N2 C2 1.344(3) . ?
N3 C2 1.306(3) . ?
N3 H3 0.9209 . ?
N5 C1 1.381(3) . ?
N5 C16 1.414(3) . ?
N5 H5N 0.8272 . ?
C2 C22 1.516(3) . ?
C10 C11 1.393(3) . ?
C10 C15 1.395(3) . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.377(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.395(4) . ?
C16 C17 1.395(3) . ?
C17 C18 1.382(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.380(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.394(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.524(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
