data_s93
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. Dervisi
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C58 H48 P2 Pd S2'
_chemical_formula_sum
 'C58 H48 P2 Pd S2'
_chemical_formula_weight          977.42
 
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'
 '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'
 'Pd'  'Pd'  -0.9988   1.0072
 '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)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    14.174(2)
_cell_length_b                    14.715(2)
_cell_length_c                    11.8000(13)
_cell_angle_alpha                 90.00
_cell_angle_beta                  102.312(4)
_cell_angle_gamma                 90.00
_cell_volume                      2404.5(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4454
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.350
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1008
_exptl_absorpt_coefficient_mu     0.577
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9445
_exptl_absorpt_correction_T_max   0.9943
_exptl_absorpt_process_details    'SORTAV Blessing (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             21577
_diffrn_reflns_av_R_equivalents   0.1775
_diffrn_reflns_av_sigmaI/netI     0.1495
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4705
_reflns_number_gt                 3015
_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)+(0.0247P)²+11.5357P] 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        0.0014(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4705
_refine_ls_number_parameters      287
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1683
_refine_ls_R_factor_gt            0.1011
_refine_ls_wR_factor_ref          0.1844
_refine_ls_wR_factor_gt           0.1598
_refine_ls_goodness_of_fit_ref    1.107
_refine_ls_restrained_S_all       1.107
_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
C1 C 0.6831(5) 0.1203(5) 0.6542(6) 0.0317(18) Uani 1 1 d . . .
H1A H 0.7486 0.1413 0.6497 0.038 Uiso 1 1 calc R . .
H1B H 0.6559 0.1646 0.7017 0.038 Uiso 1 1 calc R . .
C2 C 0.6909(5) 0.0259(5) 0.7145(6) 0.0348(19) Uani 1 1 d . . .
C3 C 0.7323(5) 0.0368(5) 0.8469(6) 0.0371(19) Uani 1 1 d . . .
H3A H 0.6858 0.0126 0.8911 0.045 Uiso 1 1 calc R . .
H3B H 0.7433 0.1019 0.8665 0.045 Uiso 1 1 calc R . .
C4 C 0.8294(5) -0.0165(5) 0.8792(7) 0.041(2) Uani 1 1 d . . .
H4 H 0.8603 -0.0086 0.9630 0.049 Uiso 1 1 calc R . .
C5 C 0.7578(5) -0.0408(5) 0.6634(7) 0.0348(18) Uani 1 1 d . . .
H5 H 0.7322 -0.0521 0.5788 0.042 Uiso 1 1 calc R . .
C6 C 0.8057(5) -0.1156(5) 0.8508(7) 0.0350(19) Uani 1 1 d . . .
C7 C 0.8162(6) -0.1884(5) 0.9263(7) 0.044(2) Uani 1 1 d . . .
H7 H 0.8434 -0.1799 1.0064 0.053 Uiso 1 1 calc R . .
C8 C 0.7863(6) -0.2745(6) 0.8837(8) 0.046(2) Uani 1 1 d . . .
H8 H 0.7964 -0.3252 0.9348 0.056 Uiso 1 1 calc R . .
C9 C 0.7423(6) -0.2876(6) 0.7685(8) 0.045(2) Uani 1 1 d . . .
H9 H 0.7197 -0.3461 0.7417 0.054 Uiso 1 1 calc R . .
C10 C 0.7314(6) -0.2141(5) 0.6916(7) 0.044(2) Uani 1 1 d . . .
H10 H 0.7021 -0.2226 0.6120 0.052 Uiso 1 1 calc R . .
C11 C 0.7641(5) -0.1277(5) 0.7327(7) 0.0361(19) Uani 1 1 d . . .
C12 C 0.8934(5) 0.0189(5) 0.8027(7) 0.040(2) Uani 1 1 d . . .
C13 C 0.9795(6) 0.0670(6) 0.8370(8) 0.050(2) Uani 1 1 d . . .
H13 H 1.0052 0.0781 0.9169 0.060 Uiso 1 1 calc R . .
C14 C 1.0268(6) 0.0980(6) 0.7552(9) 0.055(3) Uani 1 1 d . . .
H14 H 1.0849 0.1316 0.7788 0.066 Uiso 1 1 calc R . .
C15 C 0.9914(6) 0.0812(6) 0.6389(9) 0.055(2) Uani 1 1 d . . .
H15 H 1.0255 0.1017 0.5827 0.066 Uiso 1 1 calc R . .
C16 C 0.9047(6) 0.0337(6) 0.6050(8) 0.046(2) Uani 1 1 d . . .
H16 H 0.8793 0.0228 0.5249 0.055 Uiso 1 1 calc R . .
C17 C 0.8559(5) 0.0028(6) 0.6850(6) 0.0380(18) Uani 1 1 d . . .
C18 C 0.5427(5) 0.2253(5) 0.4978(7) 0.037(2) Uani 1 1 d . . .
C19 C 0.4880(5) 0.2428(5) 0.5788(7) 0.039(2) Uani 1 1 d . . .
H19 H 0.4851 0.1990 0.6370 0.047 Uiso 1 1 calc R . .
C20 C 0.4372(6) 0.3234(6) 0.5766(8) 0.045(2) Uani 1 1 d . . .
H20 H 0.4002 0.3350 0.6334 0.054 Uiso 1 1 calc R . .
C21 C 0.4407(6) 0.3867(6) 0.4913(8) 0.046(2) Uani 1 1 d . . .
H21 H 0.4065 0.4423 0.4902 0.055 Uiso 1 1 calc R . .
C22 C 0.4921(6) 0.3707(6) 0.4093(8) 0.047(2) Uani 1 1 d . . .
H22 H 0.4929 0.4142 0.3501 0.057 Uiso 1 1 calc R . .
C23 C 0.5445(6) 0.2893(5) 0.4120(7) 0.042(2) Uani 1 1 d . . .
H23 H 0.5812 0.2782 0.3548 0.050 Uiso 1 1 calc R . .
C24 C 0.6882(5) 0.1238(5) 0.4068(7) 0.0377(19) Uani 1 1 d . . .
C25 C 0.7605(6) 0.1905(5) 0.4212(7) 0.040(2) Uani 1 1 d . . .
H25 H 0.7651 0.2341 0.4815 0.048 Uiso 1 1 calc R . .
C26 C 0.8249(6) 0.1932(6) 0.3486(8) 0.050(2) Uani 1 1 d . . .
H26 H 0.8735 0.2387 0.3581 0.060 Uiso 1 1 calc R . .
C27 C 0.8178(7) 0.1290(7) 0.2619(9) 0.063(3) Uani 1 1 d . . .
H27 H 0.8629 0.1301 0.2128 0.075 Uiso 1 1 calc R . .
C28 C 0.7473(7) 0.0636(7) 0.2449(9) 0.068(3) Uani 1 1 d . . .
H28 H 0.7429 0.0205 0.1841 0.081 Uiso 1 1 calc R . .
C29 C 0.6825(6) 0.0612(6) 0.3179(7) 0.049(2) Uani 1 1 d . . .
H29 H 0.6334 0.0161 0.3067 0.058 Uiso 1 1 calc R . .
P1 P 0.60677(14) 0.11729(13) 0.50737(17) 0.0332(5) Uani 1 1 d . . .
S1 S 0.56720(13) -0.02157(12) 0.69318(17) 0.0341(5) Uani 1 1 d . . .
Pd1 Pd 0.5000 0.0000 0.5000 0.0309(3) Uani 1 2 d S . .
 
 
_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
C1 C2 1.554(10) . ?
C1 P1 1.837(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.556(10) . ?
C2 C5 1.571(10) . ?
C2 S1 1.854(7) . ?
C3 C4 1.559(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C12 1.503(11) . ?
C4 C6 1.518(11) . ?
C4 H4 1.0000 . ?
C5 C17 1.503(10) . ?
C5 C11 1.512(10) . ?
C5 H5 1.0000 . ?
C6 C7 1.380(10) . ?
C6 C11 1.403(10) . ?
C7 C8 1.396(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.403(11) . ?
C10 H10 0.9500 . ?
C12 C13 1.394(11) . ?
C12 C17 1.397(10) . ?
C13 C14 1.366(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.362(11) . ?
C16 H16 0.9500 . ?
C18 C19 1.378(12) . ?
C18 C23 1.387(11) . ?
C18 P1 1.822(8) . ?
C19 C20 1.385(11) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(12) . ?
C20 H20 0.9500 . ?
C21 C22 1.350(12) . ?
C21 H21 0.9500 . ?
C22 C23 1.405(11) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.385(11) . ?
C24 C25 1.402(10) . ?
C24 P1 1.827(9) . ?
C25 C26 1.379(12) . ?
C25 H25 0.9500 . ?
C26 C27 1.381(13) . ?
C26 H26 0.9500 . ?
C27 C28 1.371(13) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(12) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
P1 Pd1 2.2848(19) . ?
S1 Pd1 2.2975(18) . ?
Pd1 P1 2.285(2) 3_656 ?
Pd1 S1 2.2975(18) 3_656 ?
 
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
C2 C1 P1 112.3(5) . . ?
C2 C1 H1A 109.1 . . ?
P1 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
P1 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C1 110.0(6) . . ?
C3 C2 C5 108.7(6) . . ?
C1 C2 C5 111.9(6) . . ?
C3 C2 S1 108.5(5) . . ?
C1 C2 S1 107.6(5) . . ?
C5 C2 S1 110.1(5) . . ?
C2 C3 C4 108.5(6) . . ?
C2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
C12 C4 C6 109.5(7) . . ?
C12 C4 C3 107.0(6) . . ?
C6 C4 C3 106.7(6) . . ?
C12 C4 H4 111.1 . . ?
C6 C4 H4 111.1 . . ?
C3 C4 H4 111.1 . . ?
C17 C5 C11 108.9(6) . . ?
C17 C5 C2 106.3(6) . . ?
C11 C5 C2 107.0(6) . . ?
C17 C5 H5 111.5 . . ?
C11 C5 H5 111.5 . . ?
C2 C5 H5 111.5 . . ?
C7 C6 C11 120.4(7) . . ?
C7 C6 C4 127.9(7) . . ?
C11 C6 C4 111.6(6) . . ?
C6 C7 C8 119.3(8) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C9 C8 C7 121.2(7) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 119.7(8) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C11 119.5(8) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C6 C11 C10 119.8(7) . . ?
C6 C11 C5 113.2(6) . . ?
C10 C11 C5 127.0(7) . . ?
C13 C12 C17 119.9(8) . . ?
C13 C12 C4 127.2(7) . . ?
C17 C12 C4 112.8(6) . . ?
C14 C13 C12 119.7(8) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 120.9(8) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C16 119.1(9) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 120.9(8) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C12 119.4(7) . . ?
C16 C17 C5 127.8(7) . . ?
C12 C17 C5 112.5(7) . . ?
C19 C18 C23 118.6(8) . . ?
C19 C18 P1 117.8(6) . . ?
C23 C18 P1 123.5(7) . . ?
C18 C19 C20 121.0(8) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C19 C20 C21 119.4(9) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 120.9(8) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 119.7(8) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C18 C23 C22 120.2(9) . . ?
C18 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C29 C24 C25 118.7(8) . . ?
C29 C24 P1 120.9(6) . . ?
C25 C24 P1 120.3(6) . . ?
C26 C25 C24 120.5(8) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 119.1(8) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C28 C27 C26 121.6(9) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 119.0(9) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C24 C29 C28 120.9(8) . . ?
C24 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C18 P1 C24 106.8(4) . . ?
C18 P1 C1 102.9(3) . . ?
C24 P1 C1 106.5(3) . . ?
C18 P1 Pd1 109.8(3) . . ?
C24 P1 Pd1 121.4(3) . . ?
C1 P1 Pd1 107.8(2) . . ?
C2 S1 Pd1 105.2(2) . . ?
P1 Pd1 P1 180.00(10) 3_656 . ?
P1 Pd1 S1 93.70(7) 3_656 . ?
P1 Pd1 S1 86.30(7) . . ?
P1 Pd1 S1 86.30(7) 3_656 3_656 ?
P1 Pd1 S1 93.70(7) . 3_656 ?
S1 Pd1 S1 180.0 . 3_656 ?
 
_diffrn_measured_fraction_theta_max    0.851
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.851
_refine_diff_density_max    1.079
_refine_diff_density_min   -1.102
_refine_diff_density_rms    0.117
