 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety           'C21 H20 Cl N2 P Pd S'
_chemical_formula_sum
 'C21 H20 Cl N2 P Pd S'
_chemical_formula_weight          505.27
 
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'
 '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                    7.7501(16)
_cell_length_b                    9.3637(19)
_cell_length_c                    14.660(3)
_cell_angle_alpha                 83.37(3)
_cell_angle_beta                  79.63(3)
_cell_angle_gamma                 88.23(3)
_cell_volume                      1039.5(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     18684
_cell_measurement_theta_min       1.00
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             'pale yellow'
_exptl_crystal_size_max           0.28
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.614
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              508
_exptl_absorpt_coefficient_mu     1.207
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7286
_exptl_absorpt_correction_T_max   0.8120
_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             15539
_diffrn_reflns_av_R_equivalents   0.0496
_diffrn_reflns_av_sigmaI/netI     0.0384
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.79
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4662
_reflns_number_gt                 4246
_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)+(0.0442P)²+0.8299P] 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        0.0083(14)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4662
_refine_ls_number_parameters      247
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0369
_refine_ls_R_factor_gt            0.0321
_refine_ls_wR_factor_ref          0.0837
_refine_ls_wR_factor_gt           0.0806
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.040
_refine_ls_shift/su_max           0.007
_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
C21 C 0.2740(4) 0.8896(3) 0.0346(2) 0.0350(6) Uani 1 1 d . . .
H21A H 0.2223 0.9377 -0.0172 0.052 Uiso 1 1 calc R . .
H21B H 0.3302 0.9610 0.0632 0.052 Uiso 1 1 calc R . .
H21C H 0.1818 0.8408 0.0813 0.052 Uiso 1 1 calc R . .
C3 C 0.4088(3) 0.7809(3) -0.00140(18) 0.0288(5) Uani 1 1 d . . .
C2 C 0.4037(4) 0.7239(3) -0.08460(19) 0.0357(6) Uani 1 1 d . . .
H3 H 0.3081 0.7491 -0.1159 0.043 Uiso 1 1 calc R . .
C1 C 0.5334(4) 0.6313(3) -0.12360(19) 0.0392(7) Uani 1 1 d . . .
H1 H 0.5210 0.5911 -0.1787 0.047 Uiso 1 1 calc R . .
C6 C 0.6796(4) 0.5969(3) -0.08355(18) 0.0329(6) Uani 1 1 d . . .
H6 H 0.7705 0.5364 -0.1108 0.039 Uiso 1 1 calc R . .
C5 C 0.6871(3) 0.6550(3) -0.00146(17) 0.0284(5) Uani 1 1 d . . .
C4 C 0.5506(3) 0.7376(3) 0.04270(17) 0.0256(5) Uani 1 1 d . . .
C7 C 0.7368(3) 0.7411(3) 0.14249(18) 0.0281(5) Uani 1 1 d . . .
C8 C 0.7204(3) 0.7773(3) 0.40636(19) 0.0297(5) Uani 1 1 d . . .
C9 C 0.6843(7) 0.6328(4) 0.4300(3) 0.0710(14) Uani 1 1 d . . .
H9 H 0.6259 0.5832 0.3916 0.085 Uiso 1 1 calc R . .
C10 C 0.7323(8) 0.5604(4) 0.5088(4) 0.0858(17) Uani 1 1 d . . .
H10 H 0.7101 0.4604 0.5233 0.103 Uiso 1 1 calc R . .
C11 C 0.8117(5) 0.6310(4) 0.5666(3) 0.0519(9) Uani 1 1 d . . .
H11 H 0.8434 0.5806 0.6212 0.062 Uiso 1 1 calc R . .
C12 C 0.8450(4) 0.7750(4) 0.5449(2) 0.0411(7) Uani 1 1 d . . .
H12 H 0.8995 0.8247 0.5849 0.049 Uiso 1 1 calc R . .
C13 C 0.7992(4) 0.8486(3) 0.46441(19) 0.0335(6) Uani 1 1 d . . .
H13 H 0.8226 0.9484 0.4496 0.040 Uiso 1 1 calc R . .
C14 C 0.7421(3) 1.0428(3) 0.28775(17) 0.0281(5) Uani 1 1 d . . .
C15 C 0.6294(4) 1.1467(3) 0.3257(2) 0.0369(6) Uani 1 1 d . . .
H15 H 0.5122 1.1227 0.3538 0.044 Uiso 1 1 calc R . .
C16 C 0.6881(5) 1.2866(4) 0.3225(2) 0.0510(9) Uani 1 1 d . . .
H16 H 0.6119 1.3579 0.3494 0.061 Uiso 1 1 calc R . .
C17 C 0.8576(6) 1.3210(4) 0.2801(3) 0.0598(11) Uani 1 1 d . . .
H17 H 0.8973 1.4166 0.2772 0.072 Uiso 1 1 calc R . .
C18 C 0.9690(5) 1.2192(5) 0.2421(3) 0.0568(10) Uani 1 1 d . . .
H18 H 1.0854 1.2444 0.2129 0.068 Uiso 1 1 calc R . .
C19 C 0.9127(4) 1.0787(4) 0.2459(2) 0.0412(7) Uani 1 1 d . . .
H19 H 0.9907 1.0077 0.2201 0.049 Uiso 1 1 calc R . .
C20 C 0.2805(4) 0.8456(3) 0.3918(2) 0.0367(6) Uani 1 1 d . . .
H20A H 0.3648 0.8566 0.4328 0.055 Uiso 1 1 calc R . .
H20B H 0.2036 0.7644 0.4182 0.055 Uiso 1 1 calc R . .
H20C H 0.2097 0.9337 0.3863 0.055 Uiso 1 1 calc R . .
N1 N 0.5787(3) 0.7781(2) 0.12834(14) 0.0251(4) Uani 1 1 d . . .
N2 N 0.7997(3) 0.7745(3) 0.21780(16) 0.0359(6) Uani 1 1 d . . .
H2 H 0.9079 0.7519 0.2249 0.043 Uiso 1 1 calc R . .
P1 P 0.66270(8) 0.86137(7) 0.29815(4) 0.02500(15) Uani 1 1 d . . .
S1 S 0.86115(8) 0.64113(8) 0.06045(5) 0.03141(16) Uani 1 1 d . . .
Cl1 Cl 0.17111(8) 0.66940(7) 0.24250(5) 0.03125(15) Uani 1 1 d . . .
Pd1 Pd 0.41175(2) 0.808548(19) 0.263337(12) 0.02400(9) 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
C21 C3 1.505(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C3 C2 1.394(4) . ?
C3 C4 1.400(4) . ?
C2 C1 1.394(5) . ?
C2 H3 0.9500 . ?
C1 C6 1.380(4) . ?
C1 H1 0.9500 . ?
C6 C5 1.388(4) . ?
C6 H6 0.9500 . ?
C5 C4 1.398(4) . ?
C5 S1 1.750(3) . ?
C4 N1 1.407(3) . ?
C7 N1 1.309(3) . ?
C7 N2 1.355(3) . ?
C7 S1 1.743(3) . ?
C8 C13 1.373(4) . ?
C8 C9 1.382(4) . ?
C8 P1 1.811(3) . ?
C9 C10 1.375(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.370(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.384(4) . ?
C14 C19 1.388(4) . ?
C14 P1 1.805(3) . ?
C15 C16 1.393(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.364(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 Pd1 2.035(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N1 Pd1 2.204(2) . ?
N2 P1 1.701(2) . ?
N2 H2 0.8800 . ?
P1 Pd1 2.1824(8) . ?
Cl1 Pd1 2.3909(9) . ?
 
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
C3 C21 H21A 109.5 . . ?
C3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C3 C4 116.2(3) . . ?
C2 C3 C21 121.0(2) . . ?
C4 C3 C21 122.7(2) . . ?
C3 C2 C1 122.6(3) . . ?
C3 C2 H3 118.7 . . ?
C1 C2 H3 118.7 . . ?
C6 C1 C2 121.1(3) . . ?
C6 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C1 C6 C5 116.7(3) . . ?
C1 C6 H6 121.7 . . ?
C5 C6 H6 121.7 . . ?
C6 C5 C4 122.7(2) . . ?
C6 C5 S1 127.0(2) . . ?
C4 C5 S1 110.28(18) . . ?
C5 C4 C3 120.3(2) . . ?
C5 C4 N1 113.8(2) . . ?
C3 C4 N1 125.7(2) . . ?
N1 C7 N2 122.4(2) . . ?
N1 C7 S1 116.16(19) . . ?
N2 C7 S1 121.44(19) . . ?
C13 C8 C9 119.0(3) . . ?
C13 C8 P1 123.7(2) . . ?
C9 C8 P1 117.3(2) . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.5(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 120.1(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C8 C13 C12 120.2(3) . . ?
C8 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C19 119.9(3) . . ?
C15 C14 P1 118.2(2) . . ?
C19 C14 P1 121.9(2) . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 119.6(4) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 120.8(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 120.2(3) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 119.7(3) . . ?
C14 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
Pd1 C20 H20A 109.5 . . ?
Pd1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Pd1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 N1 C4 110.7(2) . . ?
C7 N1 Pd1 108.87(16) . . ?
C4 N1 Pd1 135.47(16) . . ?
C7 N2 P1 117.87(17) . . ?
C7 N2 H2 121.1 . . ?
P1 N2 H2 121.1 . . ?
N2 P1 C14 106.76(13) . . ?
N2 P1 C8 101.69(12) . . ?
C14 P1 C8 104.29(12) . . ?
N2 P1 Pd1 99.27(8) . . ?
C14 P1 Pd1 123.34(9) . . ?
C8 P1 Pd1 118.56(9) . . ?
C7 S1 C5 88.64(12) . . ?
C20 Pd1 P1 91.90(9) . . ?
C20 Pd1 N1 173.89(10) . . ?
P1 Pd1 N1 82.07(6) . . ?
C20 Pd1 Cl1 89.77(9) . . ?
P1 Pd1 Cl1 160.12(3) . . ?
N1 Pd1 Cl1 96.22(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.981
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.981
_refine_diff_density_max    0.650
_refine_diff_density_min   -1.092
_refine_diff_density_rms    0.092
