#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:27:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179111 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/73/4307385.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_4307385
loop_
_publ_author_name
'Pavel V. Gushchin'
'Nadezhda A. Bokach'
'Konstantin V. Luzyanin'
'Alexey A. Nazarov'
'Matti Haukka'
'Vadim Yu. Kukushkin'
_publ_section_title
;
PtII-Mediated Nitrile-Tetramethylguanidine Coupling as a Key Step for a
Novel Synthesis of 1,6-Dihydro-1,3,5-triazines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1684
_journal_page_last               1693
_journal_paper_doi               10.1021/ic061884b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C16 H36 Cl2 N8 Pt, C H Cl3'
_chemical_formula_sum            'C17 H37 Cl5 N8 Pt'
_chemical_formula_weight         725.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.268(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0947(11)
_cell_length_b                   12.4624(8)
_cell_length_c                   12.5981(6)
_cell_measurement_reflns_used    11726
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2862.8(3)
_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    'Diamond v.3.1d (Crystal Impact GbR, 2006)'
_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 0.997
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21418
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    5.389
_exptl_absorpt_correction_T_max  0.7273
_exptl_absorpt_correction_T_min  0.4672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.710
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0303
_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)+(0.0210P)²+12.6099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                2900
_reflns_number_total             3299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061884bsi20060930_061616_5.cif
_cod_data_source_block           structure_4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4307385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 -0.013683(16) 0.2500 0.01468(7) Uani 1 2 d S . .
Cl1 Cl 0.53388(5) 0.11704(8) 0.14381(8) 0.0225(2) Uani 1 1 d . . .
Cl98 Cl 0.48921(10) -0.55859(13) 0.13240(12) 0.0618(4) Uani 1 1 d . . .
Cl99 Cl 0.37273(17) -0.6155(3) 0.2110(3) 0.0731(10) Uani 0.50 1 d P . .
N1 N 0.46661(17) -0.1222(2) 0.3416(3) 0.0172(7) Uani 1 1 d . . .
H1 H 0.4919 -0.1198 0.4221 0.026 Uiso 1 1 d R . ..
N2 N 0.38053(18) -0.2300(3) 0.2122(3) 0.0191(7) Uani 1 1 d . . .
N3 N 0.32609(18) -0.0727(3) 0.1201(3) 0.0215(7) Uani 1 1 d . . .
N4 N 0.35858(18) -0.2130(3) 0.0248(3) 0.0210(7) Uani 1 1 d . . .
C1 C 0.4177(2) -0.1978(3) 0.3144(3) 0.0196(8) Uani 1 1 d . . .
C2 C 0.4049(2) -0.2670(3) 0.4060(3) 0.0260(9) Uani 1 1 d . . .
H2A H 0.4264 -0.3388 0.4028 0.031 Uiso 1 1 calc R .. .
H2B H 0.4312 -0.2347 0.4787 0.031 Uiso 1 1 calc R .. .
C3 C 0.3256(3) -0.2807(4) 0.3999(4) 0.0393(12) Uani 1 1 d . . .
H3A H 0.3049 -0.2109 0.4104 0.059 Uiso 1 1 calc R .. .
H3B H 0.3217 -0.3302 0.4583 0.059 Uiso 1 1 calc R .. .
H3C H 0.2985 -0.3098 0.3271 0.059 Uiso 1 1 calc R .. .
C4 C 0.3582(2) -0.1697(3) 0.1226(3) 0.0167(8) Uani 1 1 d . . .
C5 C 0.3007(2) -0.0377(3) 0.2116(4) 0.0279(10) Uani 1 1 d . . .
H5A H 0.2864 -0.1003 0.2474 0.042 Uiso 1 1 calc R .. .
H5B H 0.2585 0.0100 0.1838 0.042 Uiso 1 1 calc R . ..
H5C H 0.3402 0.0009 0.2658 0.042 Uiso 1 1 calc R . ..
C6 C 0.3336(2) 0.0120(3) 0.0446(4) 0.0315(10) Uani 1 1 d . . .
H6A H 0.3563 0.0750 0.0876 0.047 Uiso 1 1 calc R . ..
H6B H 0.2850 0.0313 -0.0046 0.047 Uiso 1 1 calc R .. .
H6C H 0.3644 -0.0135 -0.0001 0.047 Uiso 1 1 calc R .. .
C7 C 0.4000(2) -0.3107(3) 0.0247(4) 0.0299(10) Uani 1 1 d . . .
H7A H 0.4403 -0.3155 0.0941 0.045 Uiso 1 1 calc R .. .
H7B H 0.4200 -0.3097 -0.0385 0.045 Uiso 1 1 calc R .. .
H7C H 0.3676 -0.3729 0.0185 0.045 Uiso 1 1 calc R .. .
C8 C 0.3019(2) -0.1925(4) -0.0797(3) 0.0275(10) Uani 1 1 d . . .
H8A H 0.2650 -0.1439 -0.0665 0.041 Uiso 1 1 calc R .. .
H8B H 0.2785 -0.2604 -0.1102 0.041 Uiso 1 1 calc R .. .
H8C H 0.3240 -0.1596 -0.1327 0.041 Uiso 1 1 calc R .. .
C99 C 0.4658(6) -0.6218(8) 0.2338(9) 0.043(2) Uani 0.50 1 d P . .
H99 H 0.4813 -0.6986 0.2362 0.051 Uiso 0.50 1 calc PR . .
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
N1 Pt1 N1 94.94(18) . 2_655 ?
N1 Pt1 Cl1 177.27(10) . . ?
N1 Pt1 Cl1 87.19(9) 2_655 . ?
N1 Pt1 Cl1 87.19(9) . 2_655 ?
N1 Pt1 Cl1 177.27(10) 2_655 2_655 ?
Cl1 Pt1 Cl1 90.73(5) . 2_655 ?
C1 N1 Pt1 131.7(3) . . ?
C1 N1 H1 112.8 . . ?
Pt1 N1 H1 115.5 . . ?
C4 N2 C1 126.8(3) . . ?
C4 N3 C5 120.6(3) . . ?
C4 N3 C6 122.1(4) . . ?
C5 N3 C6 115.1(3) . . ?
C4 N4 C7 119.2(3) . . ?
C4 N4 C8 123.5(4) . . ?
C7 N4 C8 113.9(3) . . ?
N1 C1 N2 127.4(4) . . ?
N1 C1 C2 118.5(3) . . ?
N2 C1 C2 113.8(3) . . ?
C3 C2 C1 114.4(4) . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
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 N4 117.8(4) . . ?
N2 C4 N3 124.0(4) . . ?
N4 C4 N3 117.6(3) . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Cl98 C99 Cl99 110.5(6) . . ?
Cl98 C99 Cl98 110.1(5) . 2_655 ?
Cl99 C99 Cl98 108.3(6) . 2_655 ?
Cl98 C99 H99 109.3 . . ?
Cl99 C99 H99 109.3 . . ?
Cl98 C99 H99 109.3 2_655 . ?
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 2.001(3) . ?
Pt1 N1 2.001(3) 2_655 ?
Pt1 Cl1 2.3187(9) . ?
Pt1 Cl1 2.3187(9) 2_655 ?
Cl98 C99 1.670(10) . ?
Cl98 C99 1.828(11) 2_655 ?
Cl99 C99 1.716(11) . ?
N1 C1 1.300(5) . ?
N1 H1 0.9867 . ?
N2 C4 1.317(5) . ?
N2 C1 1.334(5) . ?
N3 C4 1.352(5) . ?
N3 C5 1.443(5) . ?
N3 C6 1.456(5) . ?
N4 C4 1.347(5) . ?
N4 C7 1.452(5) . ?
N4 C8 1.458(5) . ?
C1 C2 1.518(5) . ?
C2 C3 1.503(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C99 Cl98 1.828(11) 2_655 ?
C99 H99 1.0000 . ?
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 Cl1 0.99 2.67 3.640(3) 168.7 6_556
