data_s93
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. I. Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety           'C22 H36 Cl2 Fe P2 Pd'
_chemical_formula_sum
 'C22 H36 Cl2 Fe P2 Pd'
_chemical_formula_weight          595.60
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 '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            orthorhombic
_symmetry_space_group_name_H-M    Pnma
_symmetry_space_group_name_hall   '-P 2ac 2n'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 '-x-1/2, y-1/2, z-1/2'
 'x, -y-1/2, z'
 
_cell_length_a                    10.0317(5)
_cell_length_b                    16.1909(10)
_cell_length_c                    15.0201(9)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2439.6(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5391
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             'Dark Orange'
_exptl_crystal_size_max           0.28
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.622
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1216
_exptl_absorpt_coefficient_mu     1.689
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6492
_exptl_absorpt_correction_T_max   0.9203
_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             31579
_diffrn_reflns_av_R_equivalents   0.1830
_diffrn_reflns_av_sigmaI/netI     0.0721
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.39
_diffrn_reflns_theta_max          27.48
_reflns_number_total              2871
_reflns_number_gt                 2284
_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)'
 
_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)+(0.0546P)²+2.3740P] 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        0.0022(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2871
_refine_ls_number_parameters      138
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0607
_refine_ls_R_factor_gt            0.0449
_refine_ls_wR_factor_ref          0.1198
_refine_ls_wR_factor_gt           0.1095
_refine_ls_goodness_of_fit_ref    1.045
_refine_ls_restrained_S_all       1.045
_refine_ls_shift/su_max           0.001
_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 0.1263(3) 0.20517(19) 0.54251(19) 0.0184(7) Uani 1 1 d . . .
C2 C -0.0062(3) 0.1790(2) 0.5623(2) 0.0208(7) Uani 1 1 d . . .
H2 H -0.0357 0.1234 0.5658 0.025 Uiso 1 1 calc R . .
C3 C -0.0868(5) 0.2500 0.5759(3) 0.0214(10) Uani 1 2 d S . .
H3 H -0.1786 0.2500 0.5914 0.026 Uiso 1 2 calc SR . .
C4 C 0.0089(4) 0.2067(3) 0.3205(3) 0.0447(11) Uani 1 1 d . . .
H4 H 0.0782 0.1721 0.2988 0.054 Uiso 1 1 calc R . .
C5 C -0.1119(4) 0.1801(2) 0.3583(3) 0.0392(9) Uani 1 1 d . . .
H5 H -0.1387 0.1243 0.3665 0.047 Uiso 1 1 calc R . .
C6 C -0.1855(5) 0.2500 0.3817(3) 0.0365(13) Uani 1 2 d S . .
H6 H -0.2710 0.2500 0.4089 0.044 Uiso 1 2 calc SR . .
C7 C 0.3719(4) 0.0201(2) 0.6572(2) 0.0309(8) Uani 1 1 d . . .
H7A H 0.4587 0.0471 0.6647 0.046 Uiso 1 1 calc R . .
H7B H 0.3740 -0.0151 0.6042 0.046 Uiso 1 1 calc R . .
H7C H 0.3525 -0.0137 0.7097 0.046 Uiso 1 1 calc R . .
C8 C 0.2634(3) 0.08599(18) 0.6463(2) 0.0232(7) Uani 1 1 d . . .
H8 H 0.1772 0.0558 0.6384 0.028 Uiso 1 1 calc R . .
C9 C 0.2485(4) 0.1387(2) 0.7297(2) 0.0364(9) Uani 1 1 d . . .
H9A H 0.2222 0.1036 0.7799 0.055 Uiso 1 1 calc R . .
H9B H 0.1802 0.1809 0.7197 0.055 Uiso 1 1 calc R . .
H9C H 0.3338 0.1656 0.7432 0.055 Uiso 1 1 calc R . .
C10 C 0.3025(3) 0.0801(2) 0.4526(2) 0.0218(7) Uani 1 1 d . . .
H10 H 0.3755 0.0407 0.4684 0.026 Uiso 1 1 calc R . .
C11 C 0.1759(4) 0.0289(2) 0.4394(2) 0.0261(8) Uani 1 1 d . . .
H11A H 0.1013 0.0657 0.4251 0.039 Uiso 1 1 calc R . .
H11B H 0.1560 -0.0016 0.4941 0.039 Uiso 1 1 calc R . .
H11C H 0.1894 -0.0102 0.3904 0.039 Uiso 1 1 calc R . .
C12 C 0.3462(4) 0.1252(2) 0.3680(2) 0.0273(7) Uani 1 1 d . . .
H12A H 0.3513 0.0858 0.3186 0.041 Uiso 1 1 calc R . .
H12B H 0.4339 0.1503 0.3776 0.041 Uiso 1 1 calc R . .
H12C H 0.2812 0.1685 0.3537 0.041 Uiso 1 1 calc R . .
P1 P 0.28488(8) 0.15249(5) 0.54658(5) 0.0172(2) Uani 1 1 d . . .
Cl1 Cl 0.60401(9) 0.35706(5) 0.54292(5) 0.0253(2) Uani 1 1 d . . .
Fe1 Fe -0.00949(7) 0.2500 0.44923(4) 0.0200(2) Uani 1 2 d S . .
Pd1 Pd 0.44376(3) 0.2500 0.54914(2) 0.01749(16) 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 1.426(5) . ?
C1 C1 1.452(6) 8_565 ?
C1 P1 1.807(3) . ?
C1 Fe1 2.084(3) . ?
C2 C3 1.420(4) . ?
C2 Fe1 2.050(3) . ?
C2 H2 0.9500 . ?
C3 C2 1.420(4) 8_565 ?
C3 Fe1 2.054(5) . ?
C3 H3 0.9500 . ?
C4 C4 1.403(9) 8_565 ?
C4 C5 1.405(6) . ?
C4 Fe1 2.065(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(5) . ?
C5 Fe1 2.050(4) . ?
C5 H5 0.9500 . ?
C6 C5 1.397(5) 8_565 ?
C6 Fe1 2.036(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.533(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.523(5) . ?
C8 P1 1.858(3) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.529(5) . ?
C10 C11 1.529(5) . ?
C10 P1 1.843(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
P1 Pd1 2.2438(8) . ?
Cl1 Pd1 2.3659(8) . ?
Fe1 C5 2.050(4) 8_565 ?
Fe1 C2 2.050(3) 8_565 ?
Fe1 C4 2.065(4) 8_565 ?
Fe1 C1 2.084(3) 8_565 ?
Pd1 P1 2.2438(8) 8_565 ?
Pd1 Cl1 2.3659(8) 8_565 ?
 
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 C1 107.25(19) . 8_565 ?
C2 C1 P1 132.4(2) . . ?
C1 C1 P1 118.18(10) 8_565 . ?
C2 C1 Fe1 68.56(18) . . ?
C1 C1 Fe1 69.62(8) 8_565 . ?
P1 C1 Fe1 139.70(16) . . ?
C3 C2 C1 108.7(3) . . ?
C3 C2 Fe1 69.9(2) . . ?
C1 C2 Fe1 71.11(18) . . ?
C3 C2 H2 125.6 . . ?
C1 C2 H2 125.6 . . ?
Fe1 C2 H2 124.9 . . ?
C2 C3 C2 108.0(4) 8_565 . ?
C2 C3 Fe1 69.6(2) 8_565 . ?
C2 C3 Fe1 69.6(2) . . ?
C2 C3 H3 126.0 8_565 . ?
C2 C3 H3 126.0 . . ?
Fe1 C3 H3 126.4 . . ?
C4 C4 C5 107.9(2) 8_565 . ?
C4 C4 Fe1 70.14(13) 8_565 . ?
C5 C4 Fe1 69.5(2) . . ?
C4 C4 H4 126.1 8_565 . ?
C5 C4 H4 126.1 . . ?
Fe1 C4 H4 125.9 . . ?
C6 C5 C4 108.0(4) . . ?
C6 C5 Fe1 69.5(2) . . ?
C4 C5 Fe1 70.6(2) . . ?
C6 C5 H5 126.0 . . ?
C4 C5 H5 126.0 . . ?
Fe1 C5 H5 125.5 . . ?
C5 C6 C5 108.3(5) 8_565 . ?
C5 C6 Fe1 70.5(3) 8_565 . ?
C5 C6 Fe1 70.5(3) . . ?
C5 C6 H6 125.8 8_565 . ?
C5 C6 H6 125.8 . . ?
Fe1 C6 H6 124.7 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C7 111.8(3) . . ?
C9 C8 P1 110.5(2) . . ?
C7 C8 P1 114.0(2) . . ?
C9 C8 H8 106.7 . . ?
C7 C8 H8 106.7 . . ?
P1 C8 H8 106.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C11 112.9(3) . . ?
C12 C10 P1 111.1(2) . . ?
C11 C10 P1 111.4(2) . . ?
C12 C10 H10 107.0 . . ?
C11 C10 H10 107.0 . . ?
P1 C10 H10 107.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 P1 C10 111.02(15) . . ?
C1 P1 C8 101.47(14) . . ?
C10 P1 C8 105.11(15) . . ?
C1 P1 Pd1 107.10(10) . . ?
C10 P1 Pd1 113.09(11) . . ?
C8 P1 Pd1 118.45(11) . . ?
C6 Fe1 C5 39.98(14) . . ?
C6 Fe1 C5 39.98(14) . 8_565 ?
C5 Fe1 C5 67.1(2) . 8_565 ?
C6 Fe1 C2 115.23(15) . 8_565 ?
C5 Fe1 C2 150.37(16) . 8_565 ?
C5 Fe1 C2 104.49(15) 8_565 8_565 ?
C6 Fe1 C2 115.23(15) . . ?
C5 Fe1 C2 104.49(15) . . ?
C5 Fe1 C2 150.37(16) 8_565 . ?
C2 Fe1 C2 68.15(18) 8_565 . ?
C6 Fe1 C3 97.7(2) . . ?
C5 Fe1 C3 115.32(16) . . ?
C5 Fe1 C3 115.32(16) 8_565 . ?
C2 Fe1 C3 40.46(12) 8_565 . ?
C2 Fe1 C3 40.46(12) . . ?
C6 Fe1 C4 67.11(18) . . ?
C5 Fe1 C4 39.94(17) . . ?
C5 Fe1 C4 66.96(16) 8_565 . ?
C2 Fe1 C4 164.64(17) 8_565 . ?
C2 Fe1 C4 125.71(16) . . ?
C3 Fe1 C4 154.25(16) . . ?
C6 Fe1 C4 67.11(18) . 8_565 ?
C5 Fe1 C4 66.96(16) . 8_565 ?
C5 Fe1 C4 39.94(17) 8_565 8_565 ?
C2 Fe1 C4 125.71(16) 8_565 8_565 ?
C2 Fe1 C4 164.64(16) . 8_565 ?
C3 Fe1 C4 154.25(16) . 8_565 ?
C4 Fe1 C4 39.7(3) . 8_565 ?
C6 Fe1 C1 154.33(13) . 8_565 ?
C5 Fe1 C1 165.36(14) . 8_565 ?
C5 Fe1 C1 125.65(14) 8_565 8_565 ?
C2 Fe1 C1 40.34(13) 8_565 8_565 ?
C2 Fe1 C1 68.16(12) . 8_565 ?
C3 Fe1 C1 67.93(15) . 8_565 ?
C4 Fe1 C1 133.58(15) . 8_565 ?
C4 Fe1 C1 116.92(14) 8_565 8_565 ?
C6 Fe1 C1 154.33(13) . . ?
C5 Fe1 C1 125.65(14) . . ?
C5 Fe1 C1 165.36(14) 8_565 . ?
C2 Fe1 C1 68.16(12) 8_565 . ?
C2 Fe1 C1 40.34(13) . . ?
C3 Fe1 C1 67.93(15) . . ?
C4 Fe1 C1 116.92(14) . . ?
C4 Fe1 C1 133.58(15) 8_565 . ?
C1 Fe1 C1 40.76(17) 8_565 . ?
P1 Pd1 P1 89.44(4) . 8_565 ?
P1 Pd1 Cl1 175.95(3) . . ?
P1 Pd1 Cl1 88.08(3) 8_565 . ?
P1 Pd1 Cl1 88.08(3) . 8_565 ?
P1 Pd1 Cl1 175.95(3) 8_565 8_565 ?
Cl1 Pd1 Cl1 94.22(4) . 8_565 ?
 
_diffrn_measured_fraction_theta_max    0.990
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.990
_refine_diff_density_max    1.328
_refine_diff_density_min   -1.403
_refine_diff_density_rms    0.150
