data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. R. Bedford
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C30 H26 Cl2 N2 Pd S4, 2(C2 H3 N)'
_chemical_formula_sum
 'C34 H32 Cl2 N4 Pd S4'
_chemical_formula_weight          802.18
 
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'
 'S'  'S'   0.1246   0.1234
 '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'
 'Pd'  'Pd'  -0.9988   1.0072
 '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
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    6.2568(3)
_cell_length_b                    11.4708(5)
_cell_length_c                    12.9370(9)
_cell_angle_alpha                 100.823(2)
_cell_angle_beta                  94.201(2)
_cell_angle_gamma                 105.230(2)
_cell_volume                      872.56(8)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3527
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Needle
_exptl_crystal_colour             'Pale yellow'
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.527
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              408
_exptl_absorpt_coefficient_mu     0.955
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8320
_exptl_absorpt_correction_T_max   0.9812
_exptl_absorpt_process_details    'SORTAV (R.H.Blessing, 1995, 1997)'
_exptl_special_details    
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             11258
_diffrn_reflns_av_R_equivalents   0.0734
_diffrn_reflns_av_sigmaI/netI     0.0767
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.37
_diffrn_reflns_theta_max          25.03
_reflns_number_total              3047
_reflns_number_gt                 2491
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_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)+(0.0438P)²+1.2655P] 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        0.0061(18)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3047
_refine_ls_number_parameters      226
_refine_ls_number_restraints      20
_refine_ls_R_factor_all           0.0648
_refine_ls_R_factor_gt            0.0463
_refine_ls_wR_factor_ref          0.1083
_refine_ls_wR_factor_gt           0.1021
_refine_ls_goodness_of_fit_ref    1.025
_refine_ls_restrained_S_all       1.029
_refine_ls_shift/su_max           0.000
_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
Pd1 Pd -0.5000 0.0000 0.5000 0.0155(2) Uani 1 2 d S . .
Cl1 Cl -0.24492(18) -0.02750(10) 0.38681(9) 0.0237(3) Uani 1 1 d . . .
N1 N -0.4058(5) 0.1859(3) 0.5044(3) 0.0147(8) Uani 1 1 d . . .
C2 C -0.5010(7) 0.2292(4) 0.4279(3) 0.0162(9) Uani 1 1 d . C .
C3 C -0.4350(7) 0.3546(4) 0.4265(3) 0.0187(10) Uani 1 1 d . . .
H3 H -0.4985 0.3838 0.3711 0.022 Uiso 1 1 calc R . .
C5 C -0.1849(7) 0.3911(4) 0.5841(4) 0.0184(9) Uani 1 1 d . . .
H5 H -0.0775 0.4463 0.6396 0.022 Uiso 1 1 calc R . .
C7 C -0.6796(7) 0.1370(4) 0.3461(4) 0.0203(10) Uani 1 1 d . . .
H7A H -0.6130 0.0763 0.3055 0.024 Uiso 1 1 calc R A 1
H7B H -0.7967 0.0913 0.3828 0.024 Uiso 1 1 calc R A 1
C4 C -0.2777(7) 0.4362(4) 0.5054(4) 0.0204(10) Uani 1 1 d . . .
H4 H -0.2338 0.5222 0.5058 0.025 Uiso 1 1 calc R . .
C6 C -0.2480(7) 0.2653(4) 0.5824(3) 0.0177(9) Uani 1 1 d . D .
C12 C -0.1476(7) 0.2104(4) 0.6642(4) 0.0203(10) Uani 1 1 d . . .
H12A H -0.2657 0.1725 0.7046 0.024 Uiso 1 1 calc R B 3
H12B H -0.0873 0.1443 0.6279 0.024 Uiso 1 1 calc R B 3
C8 C -0.785(4) 0.196(3) 0.2704(19) 0.017(2) Uani 0.681(4) 1 d PD C 1
C9 C -0.7623(19) 0.2158(11) 0.1640(13) 0.0276(5) Uani 0.681(4) 1 d PD C 1
H9 H -0.6596 0.1901 0.1207 0.033 Uiso 0.681(4) 1 calc PR C 1
C10 C -0.918(2) 0.2809(13) 0.1325(13) 0.034(2) Uani 0.681(4) 1 d PD C 1
H10 H -0.9274 0.3072 0.0673 0.041 Uiso 0.681(4) 1 calc PR C 1
C11 C -1.049(2) 0.2985(12) 0.2093(7) 0.034(2) Uani 0.681(4) 1 d PD C 1
H11 H -1.1622 0.3382 0.2009 0.041 Uiso 0.681(4) 1 calc PR C 1
S1 S -1.0067(6) 0.2524(3) 0.31009(16) 0.0276(5) Uani 0.681(4) 1 d PD C 1
C28 C -0.826(9) 0.192(8) 0.280(4) 0.017(2) Uani 0.319(4) 1 d PD C 2
C29 C -1.005(5) 0.250(3) 0.2812(17) 0.0276(5) Uani 0.319(4) 1 d PD C 2
H29 H -1.0951 0.2556 0.3370 0.033 Uiso 0.319(4) 1 calc PR C 2
C30 C -1.032(5) 0.299(3) 0.1818(18) 0.034(2) Uani 0.319(4) 1 d PD C 2
H30 H -1.1355 0.3423 0.1649 0.041 Uiso 0.319(4) 1 calc PR C 2
C31 C -0.878(5) 0.269(3) 0.122(3) 0.034(2) Uani 0.319(4) 1 d PD C 2
H31 H -0.8729 0.2862 0.0534 0.041 Uiso 0.319(4) 1 calc PR C 2
S6 S -0.7215(9) 0.2102(6) 0.1618(7) 0.0276(5) Uani 0.319(4) 1 d PD C 2
C13 C 0.036(3) 0.306(4) 0.740(3) 0.020(5) Uani 0.680(4) 1 d PD D 3
C14 C 0.0455(17) 0.3717(10) 0.8432(9) 0.0309(6) Uani 0.680(4) 1 d PD D 3
H14 H -0.0819 0.3585 0.8798 0.037 Uiso 0.680(4) 1 calc PR D 3
C15 C 0.2363(15) 0.4526(13) 0.8887(14) 0.0344(14) Uani 0.680(4) 1 d PD D 3
H15 H 0.2564 0.5049 0.9570 0.041 Uiso 0.680(4) 1 calc PR D 3
C16 C 0.400(3) 0.4516(12) 0.8258(7) 0.0344(14) Uani 0.680(4) 1 d PD D 3
H16 H 0.5498 0.5021 0.8454 0.041 Uiso 0.680(4) 1 calc PR D 3
S2 S 0.3039(5) 0.3471(3) 0.7049(2) 0.0309(6) Uani 0.680(4) 1 d PD D 3
C33 C 0.053(7) 0.295(9) 0.742(7) 0.020(5) Uani 0.320(4) 1 d PD D 4
C34 C 0.276(4) 0.344(3) 0.7286(19) 0.0309(6) Uani 0.320(4) 1 d PD D 4
H34 H 0.3352 0.3110 0.6682 0.037 Uiso 0.320(4) 1 calc PR D 4
C35 C 0.399(6) 0.437(3) 0.8006(17) 0.0344(14) Uani 0.320(4) 1 d PD D 4
H35 H 0.5489 0.4801 0.7956 0.041 Uiso 0.320(4) 1 calc PR D 4
C36 C 0.288(3) 0.466(3) 0.884(3) 0.0344(14) Uani 0.320(4) 1 d PD D 4
H36 H 0.3559 0.5240 0.9480 0.041 Uiso 0.320(4) 1 calc PR D 4
S7 S -0.0034(8) 0.3813(5) 0.8568(5) 0.0309(6) Uani 0.320(4) 1 d PD D 4
C1A C -0.2228(14) -0.0605(9) 0.1135(6) 0.036(2) Uani 0.686(7) 1 d P E 5
H1A1 H -0.1798 -0.1374 0.1090 0.053 Uiso 0.686(7) 1 calc PR E 5
H1A2 H -0.1598 -0.0052 0.1825 0.053 Uiso 0.686(7) 1 calc PR E 5
H1A3 H -0.1656 -0.0201 0.0568 0.053 Uiso 0.686(7) 1 calc PR E 5
C2A C -0.483(3) -0.0907(11) 0.1010(8) 0.067(3) Uani 0.686(7) 1 d P E 5
N1A N -0.6395(15) -0.1073(9) 0.0891(7) 0.061(3) Uani 0.686(7) 1 d P E 5
C1B C -0.138(3) -0.1075(19) 0.1131(16) 0.036(2) Uani 0.314(7) 1 d P E 6
H1B1 H -0.0991 -0.1109 0.1870 0.053 Uiso 0.314(7) 1 calc PR E 6
H1B2 H -0.0765 -0.0229 0.1036 0.053 Uiso 0.314(7) 1 calc PR E 6
H1B3 H -0.0751 -0.1638 0.0662 0.053 Uiso 0.314(7) 1 calc PR E 6
C2B C -0.418(6) -0.150(2) 0.0829(19) 0.067(3) Uani 0.314(7) 1 d P E 6
N1B N -0.584(3) -0.2203(18) 0.0592(15) 0.061(3) Uani 0.314(7) 1 d P E 6
 
 
_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
Pd1 N1 2.046(3) 2_456 ?
Pd1 N1 2.046(3) . ?
Pd1 Cl1 2.2857(10) 2_456 ?
Pd1 Cl1 2.2857(10) . ?
N1 C2 1.354(5) . ?
N1 C6 1.364(5) . ?
C2 C3 1.392(6) . ?
C2 C7 1.508(6) . ?
C3 C4 1.377(6) . ?
C3 H3 0.9500 . ?
C5 C4 1.383(6) . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C7 C8 1.496(10) . ?
C7 C28 1.54(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C4 H4 0.9500 . ?
C6 C12 1.508(6) . ?
C12 C13 1.500(11) . ?
C12 C33 1.53(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 C9 1.45(2) . ?
C8 S1 1.749(15) . ?
C9 C10 1.454(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.349(11) . ?
C10 H10 0.9500 . ?
C11 S1 1.527(9) . ?
C11 H11 0.9500 . ?
C28 C29 1.44(3) . ?
C28 S6 1.74(3) . ?
C29 C30 1.52(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.353(16) . ?
C30 H30 0.9500 . ?
C31 S6 1.439(17) . ?
C31 H31 0.9500 . ?
C13 C14 1.39(3) . ?
C13 S2 1.74(2) . ?
C14 C15 1.321(15) . ?
C14 H14 0.9500 . ?
C15 C16 1.355(11) . ?
C15 H15 0.9500 . ?
C16 S2 1.739(8) . ?
C16 H16 0.9500 . ?
C33 C34 1.40(3) . ?
C33 S7 1.74(3) . ?
C34 C35 1.30(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.358(17) . ?
C35 H35 0.9500 . ?
C36 S7 1.802(16) . ?
C36 H36 0.9500 . ?
C1A C2A 1.560(18) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C1A H1A3 0.9800 . ?
C2A N1A 0.945(15) . ?
C1B C2B 1.68(4) . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C1B H1B3 0.9800 . ?
C2B N1B 1.12(3) . ?
 
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 Pd1 N1 180.0 2_456 . ?
N1 Pd1 Cl1 90.17(10) 2_456 2_456 ?
N1 Pd1 Cl1 89.83(10) . 2_456 ?
N1 Pd1 Cl1 89.83(10) 2_456 . ?
N1 Pd1 Cl1 90.17(10) . . ?
Cl1 Pd1 Cl1 180.00(4) 2_456 . ?
C2 N1 C6 120.2(3) . . ?
C2 N1 Pd1 119.0(3) . . ?
C6 N1 Pd1 120.7(3) . . ?
N1 C2 C3 120.5(4) . . ?
N1 C2 C7 117.5(4) . . ?
C3 C2 C7 122.1(4) . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C8 C7 C2 113.1(15) . . ?
C2 C7 C28 116(3) . . ?
C8 C7 H7A 109.0 . . ?
C2 C7 H7A 109.0 . . ?
C28 C7 H7A 116.2 . . ?
C8 C7 H7B 109.0 . . ?
C2 C7 H7B 109.0 . . ?
C28 C7 H7B 98.4 . . ?
H7A C7 H7B 107.8 . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C6 C5 120.1(4) . . ?
N1 C6 C12 117.3(4) . . ?
C5 C6 C12 122.6(4) . . ?
C13 C12 C6 112(2) . . ?
C6 C12 C33 118(6) . . ?
C13 C12 H12A 109.3 . . ?
C6 C12 H12A 109.3 . . ?
C33 C12 H12A 109.1 . . ?
C13 C12 H12B 109.3 . . ?
C6 C12 H12B 109.3 . . ?
C33 C12 H12B 102.9 . . ?
H12A C12 H12B 107.9 . . ?
C9 C8 C7 136.9(13) . . ?
C9 C8 S1 105.9(6) . . ?
C7 C8 S1 117.0(10) . . ?
C8 C9 C10 110.5(12) . . ?
C8 C9 H9 124.7 . . ?
C10 C9 H9 124.7 . . ?
C11 C10 C9 110.2(15) . . ?
C11 C10 H10 124.9 . . ?
C9 C10 H10 124.9 . . ?
C10 C11 S1 117.7(14) . . ?
C10 C11 H11 121.2 . . ?
S1 C11 H11 121.2 . . ?
C11 S1 C8 95.6(7) . . ?
C29 C28 C7 145(3) . . ?
C29 C28 S6 104.0(12) . . ?
C7 C28 S6 110.4(19) . . ?
C28 C29 C30 111(2) . . ?
C28 C29 H29 124.3 . . ?
C30 C29 H29 124.3 . . ?
C31 C30 C29 106(3) . . ?
C31 C30 H30 127.2 . . ?
C29 C30 H30 127.2 . . ?
C30 C31 S6 121(3) . . ?
C30 C31 H31 119.6 . . ?
S6 C31 H31 119.6 . . ?
C31 S6 C28 98.0(17) . . ?
C14 C13 C12 133.1(19) . . ?
C14 C13 S2 106.9(8) . . ?
C12 C13 S2 119.9(15) . . ?
C15 C14 C13 118.2(14) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 111.5(16) . . ?
C14 C15 H15 124.2 . . ?
C16 C15 H15 124.2 . . ?
C15 C16 S2 112.1(14) . . ?
C15 C16 H16 124.0 . . ?
S2 C16 H16 124.0 . . ?
C13 S2 C16 91.1(8) . . ?
C34 C33 C12 131(5) . . ?
C34 C33 S7 108.7(14) . . ?
C12 C33 S7 117(2) . . ?
C35 C34 C33 118(2) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C34 C35 C36 112(3) . . ?
C34 C35 H35 124.0 . . ?
C36 C35 H35 124.0 . . ?
C35 C36 S7 111(3) . . ?
C35 C36 H36 124.3 . . ?
S7 C36 H36 124.3 . . ?
C33 S7 C36 88.8(15) . . ?
N1A C2A C1A 176.3(13) . . ?
N1B C2B C1B 153(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.983
_diffrn_reflns_theta_full              25.03
_diffrn_measured_fraction_theta_full   0.983
_refine_diff_density_max    0.774
_refine_diff_density_min   -0.510
_refine_diff_density_rms    0.108
