data_2008sjc0017
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C26 H20 Cl2 N6 O Pt S'
_chemical_formula_weight          730.53
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 'Pt'  'Pt'  -1.7033   8.3905
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.9136(3)
_cell_length_b                    12.5634(3)
_cell_length_c                    12.8377(3)
_cell_angle_alpha                 109.7700(10)
_cell_angle_beta                  111.1540(10)
_cell_angle_gamma                 101.6710(10)
_cell_volume                      1303.93(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     55159
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.861
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              708
_exptl_absorpt_coefficient_mu     5.698
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5026
_exptl_absorpt_correction_T_max   0.7637
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             27964
_diffrn_reflns_av_R_equivalents   0.0321
_diffrn_reflns_av_sigmaI/netI     0.0309
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.24
_diffrn_reflns_theta_max          27.50
_reflns_number_total              5957
_reflns_number_gt                 5718
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 2003)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0320P)²+2.8376P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5957
_refine_ls_number_parameters      344
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0272
_refine_ls_R_factor_gt            0.0255
_refine_ls_wR_factor_ref          0.0653
_refine_ls_wR_factor_gt           0.0641
_refine_ls_goodness_of_fit_ref    1.068
_refine_ls_restrained_S_all       1.068
_refine_ls_shift/su_max           0.052
_refine_ls_shift/su_mean          0.002
 
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 0.581824(13) 0.361322(10) 0.581731(10) 0.01445(5) Uani 1 1 d . . .
Cl1 Cl 0.46886(10) 0.32296(7) 0.37493(7) 0.01981(16) Uani 1 1 d . . .
Cl2 Cl 0.82750(9) 0.42304(8) 0.59978(8) 0.02069(17) Uani 1 1 d . . .
N1 N 0.6743(3) 0.3963(2) 0.7632(3) 0.0157(5) Uani 1 1 d . . .
N2 N 0.7326(4) 0.3595(3) 0.9280(3) 0.0204(6) Uani 1 1 d . . .
N3 N 0.3165(4) 0.0265(3) 0.5515(3) 0.0212(6) Uani 1 1 d . . .
N4 N 0.3691(3) 0.3121(2) 0.5728(2) 0.0152(5) Uani 1 1 d . . .
N5 N 0.2510(4) 0.1350(3) 0.7780(3) 0.0243(6) Uani 1 1 d . . .
N6 N -0.0016(4) 0.0629(3) 0.6401(3) 0.0216(6) Uani 1 1 d . . .
C1 C 0.6534(4) 0.3128(3) 0.8030(3) 0.0162(6) Uani 1 1 d . . .
C2 C 0.7715(4) 0.5063(3) 0.8693(3) 0.0181(7) Uani 1 1 d . . .
C3 C 0.8093(4) 0.4828(3) 0.9737(3) 0.0204(7) Uani 1 1 d . . .
C4 C 0.9055(4) 0.5742(3) 1.0950(3) 0.0245(7) Uani 1 1 d . . .
H4 H 0.9307 0.5576 1.1652 0.029 Uiso 1 1 calc R . .
C5 C 0.9624(5) 0.6901(3) 1.1083(4) 0.0277(8) Uani 1 1 d . . .
H5 H 1.0291 0.7551 1.1898 0.033 Uiso 1 1 calc R . .
C6 C 0.9244(4) 0.7151(3) 1.0041(4) 0.0250(8) Uani 1 1 d . . .
H6 H 0.9644 0.7965 1.0174 0.030 Uiso 1 1 calc R . .
C7 C 0.8302(4) 0.6234(3) 0.8829(3) 0.0221(7) Uani 1 1 d . . .
H7 H 0.8067 0.6397 0.8126 0.027 Uiso 1 1 calc R . .
C8 C 0.5571(4) 0.1827(3) 0.7215(3) 0.0184(7) Uani 1 1 d . . .
C9 C 0.6142(4) 0.0951(3) 0.7428(4) 0.0230(7) Uani 1 1 d . . .
H9 H 0.7152 0.1184 0.8084 0.028 Uiso 1 1 calc R . .
C10 C 0.5200(5) -0.0268(3) 0.6658(4) 0.0279(8) Uani 1 1 d . . .
H10 H 0.5545 -0.0887 0.6790 0.034 Uiso 1 1 calc R . .
C11 C 0.3766(5) -0.0566(3) 0.5706(4) 0.0253(8) Uani 1 1 d . . .
H11 H 0.3162 -0.1403 0.5149 0.030 Uiso 1 1 calc R . .
C12 C 0.4063(4) 0.1448(3) 0.6273(3) 0.0173(6) Uani 1 1 d . . .
C13 C 0.3209(4) 0.2286(3) 0.6092(3) 0.0172(6) Uani 1 1 d . . .
C14 C 0.1839(4) 0.2125(3) 0.6212(3) 0.0197(7) Uani 1 1 d . . .
C15 C 0.0916(4) 0.2758(3) 0.5851(3) 0.0227(7) Uani 1 1 d . . .
H15 H -0.0030 0.2645 0.5904 0.027 Uiso 1 1 calc R . .
C16 C 0.1385(4) 0.3558(3) 0.5410(3) 0.0236(7) Uani 1 1 d . . .
H16 H 0.0744 0.3972 0.5127 0.028 Uiso 1 1 calc R . .
C17 C 0.2792(4) 0.3742(3) 0.5390(3) 0.0202(7) Uani 1 1 d . . .
H17 H 0.3138 0.4321 0.5131 0.024 Uiso 1 1 calc R . .
C18 C 0.1468(4) 0.1358(3) 0.6802(3) 0.0201(7) Uani 1 1 d . . .
C19 C 0.1655(5) 0.0562(3) 0.8053(4) 0.0252(8) Uani 1 1 d . . .
C20 C 0.2152(5) 0.0215(4) 0.9014(4) 0.0363(9) Uani 1 1 d . . .
H20 H 0.3221 0.0516 0.9602 0.044 Uiso 1 1 calc R . .
C21 C 0.1027(6) -0.0582(4) 0.9075(5) 0.0393(10) Uani 1 1 d . . .
H21 H 0.1333 -0.0838 0.9712 0.047 Uiso 1 1 calc R . .
C22 C -0.0543(5) -0.1019(4) 0.8221(4) 0.0339(9) Uani 1 1 d . . .
H22 H -0.1283 -0.1555 0.8301 0.041 Uiso 1 1 calc R . .
C23 C -0.1055(5) -0.0697(3) 0.7266(4) 0.0272(8) Uani 1 1 d . . .
H23 H -0.2124 -0.1008 0.6676 0.033 Uiso 1 1 calc R . .
C24 C 0.0078(4) 0.0110(3) 0.7206(3) 0.0233(7) Uani 1 1 d . . .
S1 S 0.62595(14) 0.23169(12) 0.12452(11) 0.0432(3) Uani 1 1 d . . .
O1 O 0.6913(5) 0.2174(3) 0.0348(3) 0.0482(9) Uani 1 1 d . . .
C25 C 0.5500(7) 0.3506(6) 0.1257(5) 0.0561(14) Uani 1 1 d . . .
H25A H 0.4680 0.3258 0.0416 0.084 Uiso 1 1 calc R . .
H25B H 0.6340 0.4254 0.1514 0.084 Uiso 1 1 calc R . .
H25C H 0.5069 0.3652 0.1846 0.084 Uiso 1 1 calc R . .
C26 C 0.7887(6) 0.3070(6) 0.2755(5) 0.0569(15) Uani 1 1 d . . .
H26A H 0.8439 0.2522 0.2874 0.085 Uiso 1 1 calc R . .
H26B H 0.7532 0.3304 0.3390 0.085 Uiso 1 1 calc R . .
H26C H 0.8589 0.3800 0.2837 0.085 Uiso 1 1 calc R . .
H6N H -0.083(6) 0.044(5) 0.574(5) 0.038(14) Uiso 1 1 d . . .
H2N H 0.728(6) 0.316(5) 0.972(5) 0.050(16) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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 2.016(3) . ?
Pt1 N4 2.023(3) . ?
Pt1 Cl2 2.3009(8) . ?
Pt1 Cl1 2.3032(8) . ?
N1 C1 1.325(4) . ?
N1 C2 1.391(4) . ?
N2 C1 1.343(4) . ?
N2 C3 1.382(5) . ?
N2 H2N 0.91(6) . ?
N3 C12 1.345(4) . ?
N3 C11 1.351(5) . ?
N4 C17 1.350(4) . ?
N4 C13 1.355(4) . ?
N5 C18 1.311(5) . ?
N5 C19 1.390(5) . ?
N6 C18 1.363(5) . ?
N6 C24 1.383(5) . ?
N6 H6N 0.85(5) . ?
C1 C8 1.472(5) . ?
C2 C7 1.393(5) . ?
C2 C3 1.404(5) . ?
C3 C4 1.389(5) . ?
C4 C5 1.378(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.414(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C12 1.393(5) . ?
C8 C9 1.397(5) . ?
C9 C10 1.388(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.370(6) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.504(5) . ?
C13 C14 1.404(5) . ?
C14 C15 1.387(5) . ?
C14 C18 1.479(5) . ?
C15 C16 1.390(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C19 C24 1.394(5) . ?
C19 C20 1.402(6) . ?
C20 C21 1.384(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(5) . ?
C23 H23 0.9500 . ?
S1 O1 1.491(4) . ?
S1 C26 1.772(5) . ?
S1 C25 1.802(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
 
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 N4 87.96(11) . . ?
N1 Pt1 Cl2 90.21(8) . . ?
N4 Pt1 Cl2 177.76(8) . . ?
N1 Pt1 Cl1 177.99(8) . . ?
N4 Pt1 Cl1 90.28(8) . . ?
Cl2 Pt1 Cl1 91.53(3) . . ?
C1 N1 C2 106.4(3) . . ?
C1 N1 Pt1 124.4(2) . . ?
C2 N1 Pt1 129.2(2) . . ?
C1 N2 C3 107.2(3) . . ?
C1 N2 H2N 124(4) . . ?
C3 N2 H2N 128(4) . . ?
C12 N3 C11 117.6(3) . . ?
C17 N4 C13 119.9(3) . . ?
C17 N4 Pt1 117.0(2) . . ?
C13 N4 Pt1 122.9(2) . . ?
C18 N5 C19 104.5(3) . . ?
C18 N6 C24 106.1(3) . . ?
C18 N6 H6N 128(4) . . ?
C24 N6 H6N 125(4) . . ?
N1 C1 N2 112.3(3) . . ?
N1 C1 C8 124.9(3) . . ?
N2 C1 C8 122.8(3) . . ?
N1 C2 C7 131.2(3) . . ?
N1 C2 C3 107.6(3) . . ?
C7 C2 C3 121.2(3) . . ?
N2 C3 C4 131.4(3) . . ?
N2 C3 C2 106.4(3) . . ?
C4 C3 C2 122.2(3) . . ?
C5 C4 C3 116.5(3) . . ?
C5 C4 H4 121.7 . . ?
C3 C4 H4 121.7 . . ?
C4 C5 C6 121.8(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 121.5(3) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C6 C7 C2 116.7(3) . . ?
C6 C7 H7 121.6 . . ?
C2 C7 H7 121.6 . . ?
C12 C8 C9 119.0(3) . . ?
C12 C8 C1 121.3(3) . . ?
C9 C8 C1 119.6(3) . . ?
C10 C9 C8 118.4(3) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C11 C10 C9 118.9(3) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
N3 C11 C10 123.6(3) . . ?
N3 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
N3 C12 C8 122.3(3) . . ?
N3 C12 C13 113.1(3) . . ?
C8 C12 C13 124.3(3) . . ?
N4 C13 C14 120.6(3) . . ?
N4 C13 C12 120.4(3) . . ?
C14 C13 C12 118.8(3) . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 C18 121.3(3) . . ?
C13 C14 C18 119.6(3) . . ?
C14 C15 C16 119.5(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 119.1(3) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
N4 C17 C16 121.7(3) . . ?
N4 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
N5 C18 N6 113.9(3) . . ?
N5 C18 C14 123.8(3) . . ?
N6 C18 C14 122.3(3) . . ?
N5 C19 C24 110.0(3) . . ?
N5 C19 C20 129.9(4) . . ?
C24 C19 C20 120.1(4) . . ?
C21 C20 C19 117.5(4) . . ?
C21 C20 H20 121.3 . . ?
C19 C20 H20 121.3 . . ?
C22 C21 C20 121.5(4) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C23 C22 C21 121.9(4) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C22 C23 C24 116.6(4) . . ?
C22 C23 H23 121.7 . . ?
C24 C23 H23 121.7 . . ?
N6 C24 C19 105.6(3) . . ?
N6 C24 C23 132.1(4) . . ?
C19 C24 C23 122.4(4) . . ?
O1 S1 C26 105.8(3) . . ?
O1 S1 C25 105.8(2) . . ?
C26 S1 C25 100.5(3) . . ?
S1 C25 H25A 109.5 . . ?
S1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
S1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
S1 C26 H26A 109.5 . . ?
S1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
S1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    1.340
_refine_diff_density_min   -1.753
_refine_diff_density_rms    0.137
 
