#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:03:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179090 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/52/4305206.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_4305206
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         'C27 H22 Cl N5 Pt'
_chemical_formula_sum            'C27 H22 Cl N5 Pt'
_chemical_formula_weight         647.04
_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                99.329(3)
_cell_angle_beta                 105.703(2)
_cell_angle_gamma                93.557(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1616(5)
_cell_length_b                   10.1225(4)
_cell_length_c                   13.6355(8)
_cell_measurement_reflns_used    5210
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.81
_cell_volume                     1193.75(11)
_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    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18018
_diffrn_reflns_theta_full        27.07
_diffrn_reflns_theta_max         27.07
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    6.015
_exptl_absorpt_correction_T_max  0.7949
_exptl_absorpt_correction_T_min  0.4500
_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    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.953
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0419
_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)+(0.0530P)²+2.5934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                4510
_reflns_number_total             5210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702483w-gushchin_7.cif
_cod_data_source_block           13
_cod_database_code               4305206
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 0.91397(2) 0.23265(2) 0.362876(18) 0.02041(9) Uani 1 1 d . . .
Cl1 Cl 0.70130(16) 0.26694(15) 0.23587(12) 0.0266(3) Uani 1 1 d . . .
N1 N 1.0976(5) 0.2083(5) 0.4747(4) 0.0214(10) Uani 1 1 d . . .
N2 N 1.0266(5) 0.3234(5) 0.6233(4) 0.0229(11) Uani 1 1 d . . .
N3 N 0.8427(6) 0.3459(5) 0.4655(4) 0.0217(10) Uani 1 1 d . . .
H3N H 0.7634 0.3880 0.4412 0.026 Uiso 1 1 calc R . ..
N4 N 0.9796(6) 0.1109(5) 0.2579(4) 0.0248(11) Uani 1 1 d . . .
N5 N 1.2454(6) 0.2206(6) 0.6438(4) 0.0310(13) Uani 1 1 d . . .
H5N H 1.3095 0.1795 0.6150 0.037 Uiso 1 1 calc R . ..
C1 C 1.1176(7) 0.2534(6) 0.5770(5) 0.0244(13) Uani 1 1 d . . .
C2 C 0.8992(6) 0.3676(6) 0.5681(5) 0.0202(12) Uani 1 1 d . . .
C3 C 1.0222(6) 0.0317(6) 0.2043(5) 0.0244(13) Uani 1 1 d . . .
C4 C 1.0766(7) -0.0677(6) 0.1394(5) 0.0244(13) Uani 1 1 d . . .
C5 C 1.0434(8) -0.2039(7) 0.1412(6) 0.0331(15) Uani 1 1 d . . .
H5 H 0.9868 -0.2301 0.1851 0.040 Uiso 1 1 calc R . ..
C6 C 1.0946(9) -0.2993(7) 0.0779(6) 0.0407(18) Uani 1 1 d . . .
H6 H 1.0763 -0.3921 0.0797 0.049 Uiso 1 1 calc R . ..
C7 C 1.1733(8) -0.2595(7) 0.0111(6) 0.0375(17) Uani 1 1 d . . .
H7 H 1.2038 -0.3258 -0.0349 0.045 Uiso 1 1 calc R .. .
C8 C 1.2068(7) -0.1260(7) 0.0113(5) 0.0324(15) Uani 1 1 d . . .
H8 H 1.2635 -0.1002 -0.0328 0.039 Uiso 1 1 calc R .. .
C9 C 1.1591(7) -0.0281(7) 0.0750(5) 0.0296(14) Uani 1 1 d . . .
H9 H 1.1822 0.0646 0.0750 0.035 Uiso 1 1 calc R . ..
C10 C 1.2106(6) 0.1355(6) 0.4453(5) 0.0219(12) Uani 1 1 d . . .
C11 C 1.2062(7) -0.0024(6) 0.4408(5) 0.0257(13) Uani 1 1 d . . .
H11 H 1.1358 -0.0481 0.4672 0.031 Uiso 1 1 calc R .. .
C12 C 1.3056(7) -0.0735(7) 0.3973(6) 0.0304(14) Uani 1 1 d . . .
H12 H 1.3027 -0.1680 0.3943 0.037 Uiso 1 1 calc R .. .
C13 C 1.4087(7) -0.0084(7) 0.3581(5) 0.0294(14) Uani 1 1 d . . .
H13 H 1.4743 -0.0583 0.3269 0.035 Uiso 1 1 calc R .. .
C14 C 1.4153(7) 0.1305(7) 0.3651(5) 0.0292(14) Uani 1 1 d . . .
H14 H 1.4875 0.1765 0.3403 0.035 Uiso 1 1 calc R . ..
C15 C 1.3161(7) 0.2019(6) 0.4084(5) 0.0245(13) Uani 1 1 d . . .
H15 H 1.3203 0.2968 0.4127 0.029 Uiso 1 1 calc R . ..
C16 C 1.2871(6) 0.2449(6) 0.7541(5) 0.0232(13) Uani 1 1 d . . .
C17 C 1.3319(7) 0.1371(6) 0.8027(5) 0.0285(14) Uani 1 1 d . . .
H17 H 1.3258 0.0499 0.7626 0.034 Uiso 1 1 calc R . ..
C18 C 1.3848(8) 0.1574(8) 0.9091(6) 0.0400(17) Uani 1 1 d . . .
H18 H 1.4176 0.0844 0.9421 0.048 Uiso 1 1 calc R . ..
C19 C 1.3907(9) 0.2814(10) 0.9674(6) 0.050(2) Uani 1 1 d . . .
H19 H 1.4274 0.2945 1.0409 0.060 Uiso 1 1 calc R . ..
C20 C 1.3423(8) 0.3906(8) 0.9188(6) 0.045(2) Uani 1 1 d . . .
H20 H 1.3440 0.4767 0.9592 0.054 Uiso 1 1 calc R . ..
C21 C 1.2929(7) 0.3710(6) 0.8130(6) 0.0305(15) Uani 1 1 d . . .
H21 H 1.2624 0.4444 0.7798 0.037 Uiso 1 1 calc R . ..
C22 C 0.8115(6) 0.4406(6) 0.6329(5) 0.0204(12) Uani 1 1 d . . .
C23 C 0.6507(7) 0.4224(6) 0.5992(5) 0.0227(12) Uani 1 1 d . . .
H23 H 0.5988 0.3683 0.5337 0.027 Uiso 1 1 calc R . ..
C24 C 0.5684(7) 0.4837(6) 0.6621(5) 0.0283(14) Uani 1 1 d . . .
H24 H 0.4601 0.4692 0.6404 0.034 Uiso 1 1 calc R . ..
C25 C 0.6433(8) 0.5662(7) 0.7566(5) 0.0308(15) Uani 1 1 d . . .
H25 H 0.5863 0.6092 0.7988 0.037 Uiso 1 1 calc R . ..
C26 C 0.8018(8) 0.5857(7) 0.7890(5) 0.0308(15) Uani 1 1 d . . .
H26 H 0.8532 0.6417 0.8538 0.037 Uiso 1 1 calc R . ..
C27 C 0.8861(7) 0.5231(6) 0.7269(5) 0.0261(13) Uani 1 1 d . . .
H27 H 0.9944 0.5373 0.7492 0.031 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'
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
N3 Pt1 N4 177.5(2) . . ?
N3 Pt1 N1 89.6(2) . . yes
N4 Pt1 N1 91.1(2) . . ?
N3 Pt1 Cl1 89.06(15) . . ?
N4 Pt1 Cl1 90.26(15) . . yes
N1 Pt1 Cl1 178.40(14) . . ?
C1 N1 C10 118.1(5) . . ?
C1 N1 Pt1 123.9(4) . . ?
C10 N1 Pt1 118.0(4) . . ?
C1 N2 C2 121.9(5) . . yes
C2 N3 Pt1 127.9(4) . . ?
C2 N3 H3N 116.0 . . ?
Pt1 N3 H3N 116.0 . . ?
C3 N4 Pt1 172.9(5) . . yes
C1 N5 C16 127.9(5) . . yes
C1 N5 H5N 116.0 . . ?
C16 N5 H5N 116.0 . . ?
N2 C1 N1 128.9(6) . . ?
N2 C1 N5 114.7(6) . . ?
N1 C1 N5 116.4(5) . . ?
N3 C2 N2 127.0(5) . . ?
N3 C2 C22 118.7(5) . . ?
N2 C2 C22 114.1(5) . . ?
N4 C3 C4 179.0(7) . . ?
C9 C4 C5 121.1(6) . . ?
C9 C4 C3 120.1(6) . . ?
C5 C4 C3 118.9(6) . . ?
C6 C5 C4 118.7(7) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C7 120.1(7) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.5(6) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 120.6(7) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C4 118.9(6) . . ?
C8 C9 H9 120.5 . . ?
C4 C9 H9 120.5 . . ?
C11 C10 C15 119.8(5) . . ?
C11 C10 N1 121.2(5) . . ?
C15 C10 N1 118.5(5) . . ?
C10 C11 C12 119.5(6) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C13 C12 C11 121.0(6) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 119.3(6) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C15 C14 C13 119.8(6) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C10 120.5(6) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C21 C16 C17 119.9(6) . . ?
C21 C16 N5 122.7(6) . . ?
C17 C16 N5 117.3(6) . . ?
C18 C17 C16 119.7(6) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 120.6(7) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 120.0(7) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 119.4(7) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C16 120.4(7) . . ?
C20 C21 H21 119.8 . . ?
C16 C21 H21 119.8 . . ?
C27 C22 C23 119.7(5) . . ?
C27 C22 C2 120.8(5) . . ?
C23 C22 C2 119.5(5) . . ?
C24 C23 C22 119.8(6) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.5(6) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C26 119.7(6) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C25 C26 C27 120.4(6) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C22 C27 C26 120.0(6) . . ?
C22 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
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 1.941(5) . yes
Pt1 N4 1.979(5) . yes
Pt1 N1 2.001(5) . yes
Pt1 Cl1 2.3169(15) . yes
N1 C1 1.354(8) . yes
N1 C10 1.413(7) . ?
N2 C1 1.345(8) . yes
N2 C2 1.352(8) . yes
N3 C2 1.330(8) . ?
N3 H3N 0.8800 . ?
N4 C3 1.154(8) . yes
N5 C1 1.372(8) . yes
N5 C16 1.422(8) . ?
N5 H5N 0.8800 . ?
C2 C22 1.488(8) . ?
C3 C4 1.434(8) . yes
C4 C9 1.392(9) . ?
C4 C5 1.399(9) . ?
C5 C6 1.379(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.367(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(9) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.385(8) . ?
C10 C15 1.390(9) . ?
C11 C12 1.391(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.384(9) . ?
C16 C17 1.394(9) . ?
C17 C18 1.375(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.363(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.413(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.366(11) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C27 1.384(9) . ?
C22 C23 1.411(8) . ?
C23 C24 1.387(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(10) . ?
C25 H25 0.9500 . ?
C26 C27 1.398(9) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
