data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_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'
 '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'
 'P'  'P'   0.1023   0.0942
 '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'
 'H'  'H'   0.0000   0.0000
 '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                    10.0076(4)
_cell_length_b                    16.1532(4)
_cell_length_c                    14.9664(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2419.39(16)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     14697 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        Shard
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.635
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1216
_exptl_absorpt_coefficient_mu     1.703
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.6290
_exptl_absorpt_correction_T_max   0.8481
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker Nonius Kappa CCD Area detector'
_diffrn_measurement_method        'φ and ω scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             19305
_diffrn_reflns_av_R_equivalents   0.0556
_diffrn_reflns_av_sigmaI/netI     0.0373
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.40
_diffrn_reflns_theta_max          27.55
_reflns_number_total              2869
_reflns_number_gt                 2186
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO (Otwinowski and MInor, 1997)'
_computing_data_reduction         'DENZO, COLLECT, MAXUS (Mackay et al., 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'CAMERON (Watkin, et al., 1993)'
_computing_publication_material   'WINGX (Farrugia, 1998)'
 
_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)+(0.0443P)²+0.4368P] 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      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2869
_refine_ls_number_parameters      137
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0515
_refine_ls_R_factor_gt            0.0319
_refine_ls_wR_factor_ref          0.0781
_refine_ls_wR_factor_gt           0.0709
_refine_ls_goodness_of_fit_ref    0.995
_refine_ls_restrained_S_all       0.995
_refine_ls_shift/su_max           0.002
_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 0.4914(3) 0.2936(2) 0.3203(2) 0.0438(9) Uani 1 1 d . . .
H1 H 0.4221 0.3283 0.2986 0.053 Uiso 1 1 calc R . .
C2 C 0.6125(3) 0.31983(19) 0.3584(2) 0.0385(8) Uani 1 1 d . . .
H2 H 0.6394 0.3757 0.3669 0.046 Uiso 1 1 calc R . .
C3 C 0.6861(4) 0.2500 0.3815(3) 0.0345(10) Uani 1 2 d S . .
H3 H 0.7721 0.2500 0.4084 0.041 Uiso 1 2 calc SR . .
C4 C 0.5869(4) 0.2500 0.5756(2) 0.0183(8) Uani 1 2 d S . .
H4 H 0.6792 0.2500 0.5905 0.022 Uiso 1 2 calc SR . .
C5 C 0.5063(3) 0.17883(15) 0.56269(16) 0.0186(5) Uani 1 1 d . . .
H5 H 0.5355 0.1230 0.5668 0.022 Uiso 1 1 calc R . .
C6 C 0.3742(2) 0.20535(15) 0.54247(15) 0.0155(5) Uani 1 1 d . . .
C7 C 0.2509(3) 0.13853(18) 0.72995(18) 0.0355(7) Uani 1 1 d . . .
H7A H 0.1680 0.1694 0.7403 0.053 Uiso 1 1 calc R . .
H7B H 0.3251 0.1775 0.7220 0.053 Uiso 1 1 calc R . .
H7C H 0.2690 0.1027 0.7814 0.053 Uiso 1 1 calc R . .
C8 C 0.2362(3) 0.08583(14) 0.64639(16) 0.0198(5) Uani 1 1 d . . .
H8 H 0.3226 0.0557 0.6385 0.024 Uiso 1 1 calc R . .
C9 C 0.1284(3) 0.02016(16) 0.65795(19) 0.0284(6) Uani 1 1 d . . .
H9A H 0.1510 -0.0154 0.7088 0.043 Uiso 1 1 calc R . .
H9B H 0.1227 -0.0135 0.6036 0.043 Uiso 1 1 calc R . .
H9C H 0.0422 0.0471 0.6689 0.043 Uiso 1 1 calc R . .
C10 C 0.1545(3) 0.12519(16) 0.36782(17) 0.0238(6) Uani 1 1 d . . .
H10A H 0.2187 0.1692 0.3541 0.036 Uiso 1 1 calc R . .
H10B H 0.0658 0.1495 0.3769 0.036 Uiso 1 1 calc R . .
H10C H 0.1511 0.0859 0.3180 0.036 Uiso 1 1 calc R . .
C11 C 0.1980(3) 0.08001(15) 0.45291(16) 0.0174(5) Uani 1 1 d . . .
H11 H 0.1246 0.0407 0.4688 0.021 Uiso 1 1 calc R . .
C12 C 0.3241(3) 0.02838(16) 0.43971(18) 0.0233(6) Uani 1 1 d . . .
H12A H 0.3098 -0.0113 0.3911 0.035 Uiso 1 1 calc R . .
H12B H 0.3444 -0.0017 0.4949 0.035 Uiso 1 1 calc R . .
H12C H 0.3990 0.0649 0.4247 0.035 Uiso 1 1 calc R . .
Cl1 Cl -0.10395(6) 0.14290(4) 0.54305(4) 0.02313(16) Uani 1 1 d . . .
Fe1 Fe 0.50979(5) 0.2500 0.44928(3) 0.01755(13) Uani 1 2 d S . .
P1 P 0.21525(6) 0.15238(4) 0.54689(4) 0.01332(15) Uani 1 1 d . . .
Pd1 Pd 0.05650(3) 0.2500 0.549348(18) 0.01414(10) 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 1.404(5) . ?
C1 C1 1.407(7) 8_565 ?
C1 Fe1 2.062(3) . ?
C2 C3 1.391(4) . ?
C2 Fe1 2.044(3) . ?
C3 C2 1.391(4) 8_565 ?
C3 Fe1 2.036(4) . ?
C4 C5 1.418(3) 8_565 ?
C4 C5 1.418(3) . ?
C4 Fe1 2.043(4) . ?
C5 C6 1.422(4) . ?
C5 Fe1 2.050(2) . ?
C6 C6 1.443(5) 8_565 ?
C6 P1 1.807(2) . ?
C6 Fe1 2.075(2) . ?
C7 C8 1.520(4) . ?
C8 C9 1.523(4) . ?
C8 P1 1.849(2) . ?
C10 C11 1.531(3) . ?
C11 C12 1.525(3) . ?
C11 P1 1.837(2) . ?
Cl1 Pd1 2.3622(6) . ?
Fe1 C2 2.044(3) 8_565 ?
Fe1 C5 2.050(2) 8_565 ?
Fe1 C1 2.062(3) 8_565 ?
Fe1 C6 2.075(2) 8_565 ?
P1 Pd1 2.2388(6) . ?
Pd1 P1 2.2388(6) 8_565 ?
Pd1 Cl1 2.3622(6) 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 107.60(19) . 8_565 ?
C2 C1 Fe1 69.33(17) . . ?
C1 C1 Fe1 70.05(10) 8_565 . ?
C3 C2 C1 108.2(3) . . ?
C3 C2 Fe1 69.7(2) . . ?
C1 C2 Fe1 70.69(17) . . ?
C2 C3 C2 108.3(4) . 8_565 ?
C2 C3 Fe1 70.4(2) . . ?
C2 C3 Fe1 70.4(2) 8_565 . ?
C5 C4 C5 108.3(3) 8_565 . ?
C5 C4 Fe1 70.02(17) 8_565 . ?
C5 C4 Fe1 70.02(17) . . ?
C4 C5 C6 108.3(2) . . ?
C4 C5 Fe1 69.45(17) . . ?
C6 C5 Fe1 70.78(14) . . ?
C5 C6 C6 107.53(14) . 8_565 ?
C5 C6 P1 131.89(19) . . ?
C6 C6 P1 118.25(8) 8_565 . ?
C5 C6 Fe1 68.90(14) . . ?
C6 C6 Fe1 69.66(7) 8_565 . ?
P1 C6 Fe1 139.87(13) . . ?
C7 C8 C9 111.4(2) . . ?
C7 C8 P1 110.37(17) . . ?
C9 C8 P1 114.61(18) . . ?
C12 C11 C10 112.8(2) . . ?
C12 C11 P1 111.68(17) . . ?
C10 C11 P1 111.11(17) . . ?
C3 Fe1 C4 97.70(16) . . ?
C3 Fe1 C2 39.87(11) . 8_565 ?
C4 Fe1 C2 115.23(13) . 8_565 ?
C3 Fe1 C2 39.87(11) . . ?
C4 Fe1 C2 115.23(13) . . ?
C2 Fe1 C2 66.97(18) 8_565 . ?
C3 Fe1 C5 115.31(12) . 8_565 ?
C4 Fe1 C5 40.54(9) . 8_565 ?
C2 Fe1 C5 150.34(12) 8_565 8_565 ?
C2 Fe1 C5 104.49(11) . 8_565 ?
C3 Fe1 C5 115.31(12) . . ?
C4 Fe1 C5 40.54(9) . . ?
C2 Fe1 C5 104.49(11) 8_565 . ?
C2 Fe1 C5 150.34(12) . . ?
C5 Fe1 C5 68.21(14) 8_565 . ?
C3 Fe1 C1 67.09(14) . 8_565 ?
C4 Fe1 C1 154.16(12) . 8_565 ?
C2 Fe1 C1 39.98(13) 8_565 8_565 ?
C2 Fe1 C1 67.06(12) . 8_565 ?
C5 Fe1 C1 164.68(13) 8_565 8_565 ?
C5 Fe1 C1 125.58(12) . 8_565 ?
C3 Fe1 C1 67.09(14) . . ?
C4 Fe1 C1 154.16(13) . . ?
C2 Fe1 C1 67.06(12) 8_565 . ?
C2 Fe1 C1 39.98(13) . . ?
C5 Fe1 C1 125.58(12) 8_565 . ?
C5 Fe1 C1 164.68(13) . . ?
C1 Fe1 C1 39.9(2) 8_565 . ?
C3 Fe1 C6 154.40(10) . . ?
C4 Fe1 C6 67.97(12) . . ?
C2 Fe1 C6 125.74(11) 8_565 . ?
C2 Fe1 C6 165.40(12) . . ?
C5 Fe1 C6 68.12(10) 8_565 . ?
C5 Fe1 C6 40.32(10) . . ?
C1 Fe1 C6 116.88(11) 8_565 . ?
C1 Fe1 C6 133.57(12) . . ?
C3 Fe1 C6 154.40(10) . 8_565 ?
C4 Fe1 C6 67.97(12) . 8_565 ?
C2 Fe1 C6 165.40(12) 8_565 8_565 ?
C2 Fe1 C6 125.74(11) . 8_565 ?
C5 Fe1 C6 40.32(10) 8_565 8_565 ?
C5 Fe1 C6 68.12(10) . 8_565 ?
C1 Fe1 C6 133.57(12) 8_565 8_565 ?
C1 Fe1 C6 116.88(11) . 8_565 ?
C6 Fe1 C6 40.68(13) . 8_565 ?
C6 P1 C11 110.85(11) . . ?
C6 P1 C8 101.83(11) . . ?
C11 P1 C8 104.92(11) . . ?
C6 P1 Pd1 106.96(8) . . ?
C11 P1 Pd1 113.21(8) . . ?
C8 P1 Pd1 118.48(9) . . ?
P1 Pd1 P1 89.56(3) 8_565 . ?
P1 Pd1 Cl1 176.01(2) 8_565 . ?
P1 Pd1 Cl1 88.04(2) . . ?
P1 Pd1 Cl1 88.05(2) 8_565 8_565 ?
P1 Pd1 Cl1 176.01(2) . 8_565 ?
Cl1 Pd1 Cl1 94.17(3) . 8_565 ?
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              27.55
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    0.817
_refine_diff_density_min   -0.705
_refine_diff_density_rms    0.103
