 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C30 H24 N4 P2 Pt S2'
_chemical_formula_weight          761.68
 
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'
 'P'  'P'   0.1023   0.0942
 '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'
 'Pt'  'Pt'  -1.7033   8.3905
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/n
_symmetry_space_group_name_hall   '-P 2yn'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    14.9089(3)
_cell_length_b                    11.4831(2)
_cell_length_c                    16.9207(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.3450(10)
_cell_angle_gamma                 90.00
_cell_volume                      2849.74(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     9170
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.775
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1488
_exptl_absorpt_coefficient_mu     5.211
_exptl_absorpt_correction_type    Empirical
_exptl_absorpt_correction_T_min   0.6238
_exptl_absorpt_correction_T_max   0.6238
_exptl_absorpt_process_details    'SORTAV (R.H. Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             18559
_diffrn_reflns_av_R_equivalents   0.0533
_diffrn_reflns_av_sigmaI/netI     0.0517
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          3.02
_diffrn_reflns_theta_max          25.03
_reflns_number_total              5022
_reflns_number_gt                 4354
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ?
_computing_publication_material   SHELXL-97
 
_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 > 2σ(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)+(0.0323P)²+4.6860P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00102(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          5022
_refine_ls_number_parameters      353
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0387
_refine_ls_R_factor_gt            0.0311
_refine_ls_wR_factor_ref          0.0791
_refine_ls_wR_factor_gt           0.0753
_refine_ls_goodness_of_fit_ref    1.037
_refine_ls_restrained_S_all       1.037
_refine_ls_shift/su_max           0.006
_refine_ls_shift/su_mean          0.000
 
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
C1 C 0.2289(3) -0.0603(4) 0.3299(3) 0.0211(11) Uani 1 1 d . . .
C2 C 0.2376(4) 0.0925(5) 0.2279(3) 0.0310(13) Uani 1 1 d . . .
H2 H 0.2398 0.1400 0.1824 0.037 Uiso 1 1 calc R . .
C3 C 0.2485(3) 0.1307(4) 0.3038(3) 0.0247(12) Uani 1 1 d . . .
H3 H 0.2610 0.2101 0.3173 0.030 Uiso 1 1 calc R . .
C4 C 0.1974(3) 0.3221(4) 0.4408(3) 0.0232(11) Uani 1 1 d . . .
H4 H 0.1791 0.3064 0.3852 0.028 Uiso 1 1 calc R . .
C5 C 0.1965(4) 0.4306(4) 0.4705(3) 0.0279(12) Uani 1 1 d . . .
H5 H 0.1804 0.4987 0.4393 0.033 Uiso 1 1 calc R . .
C6 C 0.2417(3) 0.2769(4) 0.5723(3) 0.0204(11) Uani 1 1 d . . .
C7 C 0.1748(3) -0.2276(4) 0.5101(3) 0.0218(11) Uani 1 1 d . . .
C8 C 0.0890(4) -0.2535(5) 0.4646(3) 0.0322(13) Uani 1 1 d . . .
H8 H 0.0744 -0.2290 0.4102 0.039 Uiso 1 1 calc R . .
C9 C 0.0258(4) -0.3144(5) 0.4984(3) 0.0377(14) Uani 1 1 d . . .
H9 H -0.0318 -0.3327 0.4668 0.045 Uiso 1 1 calc R . .
C10 C 0.0451(4) -0.3490(5) 0.5775(4) 0.0395(15) Uani 1 1 d . . .
H10 H 0.0010 -0.3908 0.6002 0.047 Uiso 1 1 calc R . .
C11 C 0.1288(4) -0.3226(5) 0.6238(3) 0.0330(13) Uani 1 1 d . . .
H11 H 0.1418 -0.3454 0.6786 0.040 Uiso 1 1 calc R . .
C12 C 0.1937(3) -0.2631(4) 0.5904(3) 0.0235(11) Uani 1 1 d . . .
H12 H 0.2515 -0.2463 0.6222 0.028 Uiso 1 1 calc R . .
C13 C 0.3640(4) -0.2020(4) 0.5006(3) 0.0287(12) Uani 1 1 d . . .
C14 C 0.3738(5) -0.3194(7) 0.5086(5) 0.074(2) Uani 1 1 d . . .
H14 H 0.3215 -0.3682 0.5003 0.089 Uiso 1 1 calc R . .
C15 C 0.4610(7) -0.3685(9) 0.5291(7) 0.109(4) Uani 1 1 d . . .
H15 H 0.4675 -0.4502 0.5370 0.130 Uiso 1 1 calc R . .
C16 C 0.5377(5) -0.2983(7) 0.5381(5) 0.071(3) Uani 1 1 d . . .
H16 H 0.5970 -0.3311 0.5437 0.086 Uiso 1 1 calc R . .
C17 C 0.5262(5) -0.1883(10) 0.5385(6) 0.096(3) Uani 1 1 d . . .
H17 H 0.5784 -0.1400 0.5523 0.115 Uiso 1 1 calc R . .
C18 C 0.4383(5) -0.1337(7) 0.5191(5) 0.071(2) Uani 1 1 d . . .
H18 H 0.4328 -0.0513 0.5194 0.086 Uiso 1 1 calc R . .
C19 C 0.1534(3) 0.0236(4) 0.6569(3) 0.0220(11) Uani 1 1 d . . .
C20 C 0.0764(4) -0.0154(5) 0.6047(3) 0.0268(12) Uani 1 1 d . . .
H20 H 0.0768 -0.0181 0.5486 0.032 Uiso 1 1 calc R . .
C21 C -0.0009(4) -0.0504(5) 0.6333(3) 0.0333(14) Uani 1 1 d . . .
H21 H -0.0529 -0.0775 0.5971 0.040 Uiso 1 1 calc R . .
C22 C -0.0014(4) -0.0454(5) 0.7147(4) 0.0402(16) Uani 1 1 d . . .
H22 H -0.0535 -0.0716 0.7348 0.048 Uiso 1 1 calc R . .
C23 C 0.0727(4) -0.0030(7) 0.7669(3) 0.0498(17) Uani 1 1 d . . .
H23 H 0.0707 0.0026 0.8226 0.060 Uiso 1 1 calc R . .
C24 C 0.1507(4) 0.0317(5) 0.7388(3) 0.0367(14) Uani 1 1 d . . .
H24 H 0.2018 0.0607 0.7752 0.044 Uiso 1 1 calc R . .
C25 C 0.3509(3) 0.0078(5) 0.6810(3) 0.0253(11) Uani 1 1 d . . .
C26 C 0.3471(4) -0.0918(5) 0.7277(3) 0.0304(12) Uani 1 1 d . . .
H26 H 0.2899 -0.1260 0.7310 0.036 Uiso 1 1 calc R . .
C27 C 0.4272(4) -0.1411(6) 0.7692(3) 0.0427(15) Uani 1 1 d . . .
H27 H 0.4246 -0.2086 0.8012 0.051 Uiso 1 1 calc R . .
C28 C 0.5100(5) -0.0922(7) 0.7640(4) 0.0529(18) Uani 1 1 d . . .
H28 H 0.5645 -0.1269 0.7917 0.063 Uiso 1 1 calc R . .
C29 C 0.5145(4) 0.0070(8) 0.7188(4) 0.058(2) Uani 1 1 d . . .
H29 H 0.5719 0.0408 0.7158 0.070 Uiso 1 1 calc R . .
C30 C 0.4357(4) 0.0568(5) 0.6779(4) 0.0400(16) Uani 1 1 d . . .
H30 H 0.4392 0.1255 0.6473 0.048 Uiso 1 1 calc R . .
N1 N 0.2405(3) 0.0480(3) 0.3609(2) 0.0186(9) Uani 1 1 d . . .
N2 N 0.2262(3) 0.2350(4) 0.4954(2) 0.0217(9) Uani 1 1 d . . .
N3 N 0.2261(3) -0.1592(4) 0.3694(2) 0.0236(9) Uani 1 1 d . . .
N4 N 0.2624(3) 0.2145(4) 0.6383(2) 0.0268(10) Uani 1 1 d . . .
P1 P 0.25265(9) -0.13768(11) 0.46848(8) 0.0199(3) Uani 1 1 d . . .
P2 P 0.25258(9) 0.07254(11) 0.61857(7) 0.0203(3) Uani 1 1 d . . .
S1 S 0.21876(10) -0.05647(11) 0.22509(8) 0.0287(3) Uani 1 1 d . . .
S2 S 0.22895(10) 0.42760(11) 0.57406(8) 0.0314(3) Uani 1 1 d . . .
Pt1 Pt 0.243703(12) 0.055932(15) 0.485312(10) 0.01725(10) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 N3 1.322(6) . ?
C1 N1 1.348(6) . ?
C1 S1 1.754(5) . ?
C2 C3 1.338(7) . ?
C2 S1 1.733(6) . ?
C2 H2 0.9500 . ?
C3 N1 1.376(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.343(7) . ?
C4 N2 1.377(6) . ?
C4 H4 0.9500 . ?
C5 S2 1.733(5) . ?
C5 H5 0.9500 . ?
C6 N4 1.316(6) . ?
C6 N2 1.367(6) . ?
C6 S2 1.742(5) . ?
C7 C12 1.397(7) . ?
C7 C8 1.402(7) . ?
C7 P1 1.790(5) . ?
C8 C9 1.378(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(7) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.349(9) . ?
C13 C14 1.360(9) . ?
C13 P1 1.808(5) . ?
C14 C15 1.403(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.275(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.436(11) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.391(7) . ?
C19 C24 1.397(7) . ?
C19 P2 1.808(5) . ?
C20 C21 1.387(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.374(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.394(8) . ?
C25 C26 1.397(7) . ?
C25 P2 1.806(5) . ?
C26 C27 1.392(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.373(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(9) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
N1 Pt1 2.099(4) . ?
N2 Pt1 2.084(4) . ?
N3 P1 1.670(4) . ?
N4 P2 1.665(4) . ?
P1 Pt1 2.2484(13) . ?
P2 Pt1 2.2430(13) . ?
 
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 C1 N1 127.5(4) . . ?
N3 C1 S1 121.9(4) . . ?
N1 C1 S1 110.6(3) . . ?
C3 C2 S1 110.0(4) . . ?
C3 C2 H2 125.0 . . ?
S1 C2 H2 125.0 . . ?
C2 C3 N1 115.9(5) . . ?
C2 C3 H3 122.0 . . ?
N1 C3 H3 122.0 . . ?
C5 C4 N2 116.5(4) . . ?
C5 C4 H4 121.8 . . ?
N2 C4 H4 121.8 . . ?
C4 C5 S2 109.9(4) . . ?
C4 C5 H5 125.1 . . ?
S2 C5 H5 125.1 . . ?
N4 C6 N2 126.1(5) . . ?
N4 C6 S2 122.4(4) . . ?
N2 C6 S2 111.4(4) . . ?
C12 C7 C8 118.5(5) . . ?
C12 C7 P1 121.2(4) . . ?
C8 C7 P1 119.9(4) . . ?
C9 C8 C7 120.3(5) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 120.8(5) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 119.9(5) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 120.2(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.4(5) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
C18 C13 C14 118.9(6) . . ?
C18 C13 P1 120.3(5) . . ?
C14 C13 P1 120.8(5) . . ?
C13 C14 C15 120.1(8) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 120.2(8) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 117.9(8) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
C16 C17 C18 123.3(8) . . ?
C16 C17 H17 118.3 . . ?
C18 C17 H17 118.3 . . ?
C13 C18 C17 118.5(8) . . ?
C13 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C20 C19 C24 118.9(5) . . ?
C20 C19 P2 120.4(4) . . ?
C24 C19 P2 120.5(4) . . ?
C21 C20 C19 120.9(5) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 119.4(5) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C23 C22 C21 120.5(5) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 120.4(5) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C19 119.7(5) . . ?
C23 C24 H24 120.2 . . ?
C19 C24 H24 120.2 . . ?
C30 C25 C26 118.7(5) . . ?
C30 C25 P2 117.3(4) . . ?
C26 C25 P2 123.8(4) . . ?
C27 C26 C25 120.0(5) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 120.0(6) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.4(6) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C30 C29 C28 120.0(6) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 120.8(6) . . ?
C29 C30 H30 119.6 . . ?
C25 C30 H30 119.6 . . ?
C1 N1 C3 112.6(4) . . ?
C1 N1 Pt1 114.1(3) . . ?
C3 N1 Pt1 133.3(3) . . ?
C6 N2 C4 111.2(4) . . ?
C6 N2 Pt1 115.0(3) . . ?
C4 N2 Pt1 133.7(3) . . ?
C1 N3 P1 110.9(3) . . ?
C6 N4 P2 111.4(3) . . ?
N3 P1 C7 104.8(2) . . ?
N3 P1 C13 106.3(2) . . ?
C7 P1 C13 105.8(2) . . ?
N3 P1 Pt1 105.35(15) . . ?
C7 P1 Pt1 117.58(16) . . ?
C13 P1 Pt1 115.97(17) . . ?
N4 P2 C25 104.6(2) . . ?
N4 P2 C19 106.3(2) . . ?
C25 P2 C19 107.0(2) . . ?
N4 P2 Pt1 105.80(14) . . ?
C25 P2 Pt1 116.63(16) . . ?
C19 P2 Pt1 115.47(16) . . ?
C2 S1 C1 90.7(2) . . ?
C5 S2 C6 90.8(2) . . ?
N2 Pt1 N1 98.32(14) . . ?
N2 Pt1 P2 79.57(11) . . ?
N1 Pt1 P2 176.85(11) . . ?
N2 Pt1 P1 175.84(11) . . ?
N1 Pt1 P1 79.70(11) . . ?
P2 Pt1 P1 102.55(5) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.03
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.462
_refine_diff_density_min   -1.601
_refine_diff_density_rms    0.146
