#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/91/1519149.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1519149
loop_
_publ_author_name
'Butler, Ian R.'
'Coles, Simon J.'
'Hursthouse, Michael B.'
_publ_section_title
;
 C45.5H46Cl2Fe2O3P2Pd
;
_journal_name_full               'Crystal Structure Report Archive'
_journal_page_first              1194
_journal_year                    1994
_chemical_formula_moiety         'C45.5 H46 Cl2 Fe2 O3 P2 Pd'
_chemical_formula_sum            'C45.5 H46 Cl2 Fe2 O3 P2 Pd'
_chemical_formula_weight         991.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.157(14)
_cell_angle_beta                 97.17(2)
_cell_angle_gamma                112.543(9)
_cell_formula_units_Z            1
_cell_length_a                   9.697(3)
_cell_length_b                   10.0628(13)
_cell_length_c                   13.213(2)
_cell_measurement_temperature    120(2)
_cell_volume                     1112.1(4)
_computing_cell_refinement       REFINE
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'ABSURD (Karaulov, 1992)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
'SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.671
_diffrn_measured_fraction_theta_max 0.671
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2617
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_correction_T_min  0.7412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (R.H.Blessing, 1995, 1997)'
_exptl_crystal_colour            unk
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unk
_exptl_crystal_F_000             505
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.582
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2617
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1255P)²+0.7242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                2462
_reflns_number_total             2617
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            eCrystal-1194.cif
_cod_data_source_block           94src094
_cod_depositor_comments
;
Citation :
Butler, Ian R. and Coles, Simon J. and Hursthouse, Michael B. (1994)
 University of Southampton, Crystal Structure Report Archive. 
(doi:10.5258/ecrystals/1194)

http://ecrystals.chem.soton.ac.uk/1194/
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1519149
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.0000 0.0000 0.0000 0.0200(3) Uani 1 2 d S . .
Fe1 Fe 0.17045(8) -0.15249(8) 0.25840(5) 0.0229(3) Uani 1 1 d . . .
Cl1 Cl -0.12503(15) -0.24751(14) -0.12067(10) 0.0273(4) Uani 1 1 d . . .
P1 P -0.11689(14) -0.09033(13) 0.12742(9) 0.0213(4) Uani 1 1 d . . .
O1 O 0.2310(5) 0.0988(5) 0.5510(3) 0.0538(12) Uani 1 1 d . . .
C1 C 0.2324(7) 0.1162(7) 0.4643(4) 0.0408(15) Uani 1 1 d . . .
C2 C 0.2988(6) 0.0503(6) 0.3841(4) 0.0311(14) Uani 1 1 d . . .
C3 C 0.3534(6) -0.0633(6) 0.3893(4) 0.0335(13) Uani 1 1 d . . .
H3 H 0.3568 -0.1033 0.4468 0.040 Uiso 1 1 calc R . .
C4 C 0.4012(6) -0.1048(7) 0.2929(4) 0.0374(14) Uani 1 1 d . . .
H4 H 0.4443 -0.1757 0.2755 0.045 Uiso 1 1 calc R . .
C5 C 0.3738(6) -0.0226(7) 0.2280(4) 0.0337(14) Uani 1 1 d . . .
H5 H 0.3953 -0.0291 0.1592 0.040 Uiso 1 1 calc R . .
C6 C 0.3084(6) 0.0721(6) 0.2817(4) 0.0313(13) Uani 1 1 d . . .
H6 H 0.2771 0.1374 0.2546 0.038 Uiso 1 1 calc R . .
C7 C 0.0228(6) -0.2997(6) 0.1112(4) 0.0267(12) Uani 1 1 d . . .
H7 H 0.0418 -0.2994 0.0424 0.032 Uiso 1 1 calc R . .
C8 C 0.0597(6) -0.3848(6) 0.1714(5) 0.0310(13) Uani 1 1 d . . .
H8 H 0.1060 -0.4521 0.1503 0.037 Uiso 1 1 calc R . .
C9 C 0.0128(6) -0.3490(6) 0.2716(4) 0.0335(13) Uani 1 1 d . . .
H9 H 0.0246 -0.3885 0.3283 0.040 Uiso 1 1 calc R . .
C10 C -0.0525(6) -0.2470(6) 0.2710(4) 0.0303(13) Uani 1 1 d . . .
H10 H -0.0930 -0.2064 0.3268 0.036 Uiso 1 1 calc R . .
C11 C -0.0479(5) -0.2137(5) 0.1711(4) 0.0222(11) Uani 1 1 d . . .
C12 C -0.3258(5) -0.2005(6) 0.0743(4) 0.0270(12) Uani 1 1 d . . .
C13 C -0.4133(6) -0.3095(6) 0.1153(5) 0.0328(13) Uani 1 1 d . . .
H13 H -0.3645 -0.3308 0.1719 0.039 Uiso 1 1 calc R . .
C14 C -0.5723(7) -0.3873(6) 0.0735(6) 0.0454(17) Uani 1 1 d . . .
H14 H -0.6317 -0.4638 0.1003 0.054 Uiso 1 1 calc R . .
C15 C -0.6436(7) -0.3540(8) -0.0061(6) 0.0493(19) Uani 1 1 d . . .
H15 H -0.7525 -0.4069 -0.0337 0.059 Uiso 1 1 calc R . .
C16 C -0.5599(7) -0.2462(9) -0.0459(5) 0.0538(18) Uani 1 1 d . . .
H16 H -0.6106 -0.2232 -0.1005 0.065 Uiso 1 1 calc R . .
C17 C -0.3998(7) -0.1690(7) -0.0067(5) 0.0418(15) Uani 1 1 d . . .
H17 H -0.3414 -0.0948 -0.0355 0.050 Uiso 1 1 calc R . .
C18 C -0.0968(6) 0.0534(6) 0.2530(4) 0.0288(13) Uani 1 1 d . B .
H18A H -0.1325 0.0016 0.3054 0.035 Uiso 1 1 calc R . .
H18B H 0.0140 0.1242 0.2842 0.035 Uiso 1 1 calc R . .
C19 C -0.1861(7) 0.1465(7) 0.2398(6) 0.0442(17) Uani 1 1 d . . .
H19A H -0.1839 0.1604 0.1684 0.053 Uiso 1 1 calc R A 1
H19B H -0.2951 0.0835 0.2363 0.053 Uiso 1 1 calc R A 1
C20 C -0.1384(19) 0.298(2) 0.3206(14) 0.027(4) Uani 0.44(3) 1 d P B 1
H20A H -0.1974 0.3497 0.2962 0.033 Uiso 0.44(3) 1 calc PR B 1
H20B H -0.0271 0.3618 0.3317 0.033 Uiso 0.44(3) 1 calc PR B 1
C21 C -0.171(3) 0.271(2) 0.4272(13) 0.055(6) Uani 0.44(3) 1 d P B 1
H21A H -0.1502 0.3682 0.4817 0.083 Uiso 0.44(3) 1 calc PR B 1
H21B H -0.1051 0.2279 0.4540 0.083 Uiso 0.44(3) 1 calc PR B 1
H21C H -0.2799 0.1992 0.4134 0.083 Uiso 0.44(3) 1 calc PR B 1
C20' C -0.145(2) 0.267(2) 0.368(2) 0.070(7) Uani 0.56(3) 1 d P B 2
H20C H -0.1642 0.2071 0.4182 0.084 Uiso 0.56(3) 1 calc PR B 2
H20D H -0.0347 0.3403 0.3914 0.084 Uiso 0.56(3) 1 calc PR B 2
C21' C -0.244(2) 0.354(2) 0.375(2) 0.129(13) Uani 0.56(3) 1 d P B 2
H21D H -0.2364 0.3888 0.4585 0.193 Uiso 0.56 1 d P B 2
H21E H -0.3451 0.2832 0.3431 0.193 Uiso 0.56 1 d P B 2
H21F H -0.2028 0.4354 0.3567 0.193 Uiso 0.56 1 d P B 2
O30 O -0.6252 0.4876 0.6699 0.167 Uani 0.50 1 d PDU . .
C33 C -0.5000 0.5000 0.5000 0.012 Uani 0.50 2 d SPDU . .
C31 C -0.4781 0.4923 0.6636 0.088 Uani 0.50 1 d PDU . .
C30 C -0.5898 0.5334 0.5811 0.122 Uani 0.50 1 d PDU . .
C32 C -0.3705 0.4354 0.6128 0.061 Uani 0.50 1 d PDU . .
H1 H 0.1782 0.1662 0.4502 0.045 Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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'
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
Cl1 Pd1 Cl1 180.00(6) 2 .
Cl1 Pd1 P1 87.92(4) 2 2
Cl1 Pd1 P1 92.08(4) . 2
Cl1 Pd1 P1 92.08(4) 2 .
Cl1 Pd1 P1 87.92(4) . .
P1 Pd1 P1 180.00(10) 2 .
C3 Fe1 C7 157.9(2) . .
C3 Fe1 C10 121.6(2) . .
C7 Fe1 C10 68.9(2) . .
C3 Fe1 C6 69.2(2) . .
C7 Fe1 C6 121.8(2) . .
C10 Fe1 C6 128.1(2) . .
C3 Fe1 C11 158.8(2) . .
C7 Fe1 C11 41.1(2) . .
C10 Fe1 C11 41.3(2) . .
C6 Fe1 C11 109.8(2) . .
C3 Fe1 C9 106.3(2) . .
C7 Fe1 C9 68.4(2) . .
C10 Fe1 C9 39.9(2) . .
C6 Fe1 C9 163.6(2) . .
C11 Fe1 C9 68.5(2) . .
C3 Fe1 C2 41.3(2) . .
C7 Fe1 C2 158.7(3) . .
C10 Fe1 C2 110.3(2) . .
C6 Fe1 C2 40.9(2) . .
C11 Fe1 C2 123.9(2) . .
C9 Fe1 C2 125.5(2) . .
C3 Fe1 C4 40.7(2) . .
C7 Fe1 C4 121.7(2) . .
C10 Fe1 C4 155.1(2) . .
C6 Fe1 C4 68.3(2) . .
C11 Fe1 C4 160.1(2) . .
C9 Fe1 C4 119.2(2) . .
C2 Fe1 C4 68.5(2) . .
C3 Fe1 C5 68.0(2) . .
C7 Fe1 C5 106.9(2) . .
C10 Fe1 C5 164.6(2) . .
C6 Fe1 C5 40.6(2) . .
C11 Fe1 C5 125.9(2) . .
C9 Fe1 C5 153.8(2) . .
C2 Fe1 C5 68.0(2) . .
C4 Fe1 C5 39.8(2) . .
C3 Fe1 C8 121.7(2) . .
C7 Fe1 C8 40.3(2) . .
C10 Fe1 C8 68.6(2) . .
C6 Fe1 C8 154.6(2) . .
C11 Fe1 C8 68.8(2) . .
C9 Fe1 C8 41.3(2) . .
C2 Fe1 C8 160.8(2) . .
C4 Fe1 C8 104.1(2) . .
C5 Fe1 C8 118.3(2) . .
C11 P1 C18 104.4(2) . .
C11 P1 C12 106.2(2) . .
C18 P1 C12 103.4(2) . .
C11 P1 Pd1 113.30(16) . .
C18 P1 Pd1 116.63(17) . .
C12 P1 Pd1 111.78(17) . .
O1 C1 C2 125.3(7) . .
O1 C1 H1 112.6 . .
C2 C1 H1 121.8 . .
C6 C2 C3 107.3(5) . .
C6 C2 C1 127.4(7) . .
C3 C2 C1 125.0(6) . .
C6 C2 Fe1 69.3(3) . .
C3 C2 Fe1 68.5(3) . .
C1 C2 Fe1 122.7(4) . .
C4 C3 C2 107.8(5) . .
C4 C3 Fe1 70.6(3) . .
C2 C3 Fe1 70.1(3) . .
C4 C3 H3 126.1 . .
C2 C3 H3 126.1 . .
Fe1 C3 H3 124.7 . .
C5 C4 C3 108.2(5) . .
C5 C4 Fe1 70.1(3) . .
C3 C4 Fe1 68.7(3) . .
C5 C4 H4 125.9 . .
C3 C4 H4 125.9 . .
Fe1 C4 H4 126.9 . .
C4 C5 C6 109.3(5) . .
C4 C5 Fe1 70.1(3) . .
C6 C5 Fe1 69.3(3) . .
C4 C5 H5 125.3 . .
C6 C5 H5 125.3 . .
Fe1 C5 H5 126.9 . .
C5 C6 C2 107.3(6) . .
C5 C6 Fe1 70.1(3) . .
C2 C6 Fe1 69.8(3) . .
C5 C6 H6 126.3 . .
C2 C6 H6 126.3 . .
Fe1 C6 H6 125.3 . .
C8 C7 C11 109.2(5) . .
C8 C7 Fe1 70.8(3) . .
C11 C7 Fe1 69.6(3) . .
C8 C7 H7 125.4 . .
C11 C7 H7 125.4 . .
Fe1 C7 H7 125.8 . .
C7 C8 C9 106.6(5) . .
C7 C8 Fe1 68.9(3) . .
C9 C8 Fe1 68.5(3) . .
C7 C8 H8 126.7 . .
C9 C8 H8 126.7 . .
Fe1 C8 H8 127.4 . .
C10 C9 C8 109.1(5) . .
C10 C9 Fe1 70.0(3) . .
C8 C9 Fe1 70.2(3) . .
C10 C9 H9 125.5 . .
C8 C9 H9 125.5 . .
Fe1 C9 H9 125.9 . .
C9 C10 C11 108.4(5) . .
C9 C10 Fe1 70.1(3) . .
C11 C10 Fe1 69.4(3) . .
C9 C10 H10 125.8 . .
C11 C10 H10 125.8 . .
Fe1 C10 H10 126.3 . .
C7 C11 C10 106.8(5) . .
C7 C11 P1 125.8(4) . .
C10 C11 P1 127.5(4) . .
C7 C11 Fe1 69.3(3) . .
C10 C11 Fe1 69.3(3) . .
P1 C11 Fe1 126.6(2) . .
C13 C12 C17 119.0(5) . .
C13 C12 P1 122.4(4) . .
C17 C12 P1 118.5(4) . .
C12 C13 C14 119.9(6) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C15 C14 C13 120.2(6) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C16 C15 C14 120.5(6) . .
C16 C15 H15 119.7 . .
C14 C15 H15 119.7 . .
C15 C16 C17 120.2(7) . .
C15 C16 H16 119.9 . .
C17 C16 H16 119.9 . .
C12 C17 C16 120.1(6) . .
C12 C17 H17 120.0 . .
C16 C17 H17 120.0 . .
C19 C18 P1 114.4(4) . .
C19 C18 H18A 108.7 . .
P1 C18 H18A 108.7 . .
C19 C18 H18B 108.7 . .
P1 C18 H18B 108.7 . .
H18A C18 H18B 107.6 . .
C20 C19 C18 119.6(9) . .
C18 C19 C20' 103.0(9) . .
C20 C19 H19A 107.4 . .
C18 C19 H19A 107.4 . .
C20' C19 H19A 134.3 . .
C20 C19 H19B 107.4 . .
C18 C19 H19B 107.4 . .
C20' C19 H19B 95.3 . .
H19A C19 H19B 106.9 . .
C19 C20 C21 106.8(14) . .
C19 C20 H20A 110.4 . .
C21 C20 H20A 110.4 . .
C19 C20 H20B 110.4 . .
C21 C20 H20B 110.4 . .
H20A C20 H20B 108.6 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C20 C21 H21D 96.3 . .
H21B C21 H21D 145.2 . .
H21C C21 H21D 81.9 . .
C21' C20' C19 111.0(18) . .
C21' C20' H20C 109.4 . .
C19 C20' H20C 109.4 . .
C21' C20' H20D 109.4 . .
C19 C20' H20D 109.4 . .
H20C C20' H20D 108.0 . .
C20' C21' H21D 101.5 . .
C20' C21' H21E 107.5 . .
H21D C21' H21E 105.4 . .
C20' C21' H21F 111.2 . .
H21D C21' H21F 108.7 . .
H21E C21' H21F 120.7 . .
C30 O30 C31 72.9 . .
C30 C33 C30 180.0 2_466 .
O30 C31 C32 153.9 . .
O30 C30 C33 134.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl1 2.3109(13) 2
Pd1 Cl1 2.3109(13) .
Pd1 P1 2.3308(13) 2
Pd1 P1 2.3308(13) .
Fe1 C3 2.036(5) .
Fe1 C7 2.049(5) .
Fe1 C10 2.050(5) .
Fe1 C6 2.051(5) .
Fe1 C11 2.052(5) .
Fe1 C9 2.051(5) .
Fe1 C2 2.058(5) .
Fe1 C4 2.062(6) .
Fe1 C5 2.062(5) .
Fe1 C8 2.074(5) .
P1 C11 1.799(6) .
P1 C18 1.825(5) .
P1 C12 1.828(5) .
O1 C1 1.205(7) .
C1 C2 1.452(8) .
C1 H1 0.8898 .
C2 C6 1.435(8) .
C2 C3 1.445(9) .
C3 C4 1.425(8) .
C3 H3 0.9500 .
C4 C5 1.404(9) .
C4 H4 0.9500 .
C5 C6 1.426(8) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.419(8) .
C7 C11 1.441(7) .
C7 H7 0.9500 .
C8 C9 1.455(8) .
C8 H8 0.9500 .
C9 C10 1.398(8) .
C9 H9 0.9500 .
C10 C11 1.447(7) .
C10 H10 0.9500 .
C12 C13 1.389(8) .
C12 C17 1.385(8) .
C13 C14 1.390(8) .
C13 H13 0.9500 .
C14 C15 1.370(10) .
C14 H14 0.9500 .
C15 C16 1.357(11) .
C15 H15 0.9500 .
C16 C17 1.396(9) .
C16 H16 0.9500 .
C17 H17 0.9500 .
C18 C19 1.527(8) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.467(19) .
C19 C20' 1.70(2) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.55(2) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C20' C21' 1.52(3) .
C20' H20C 0.9900 .
C20' H20D 0.9900 .
C21' H21D 1.0453 .
C21' H21E 0.9233 .
C21' H21F 0.8802 .
O30 C30 1.4030 .
O30 C31 1.4231 .
C33 C30 1.5124 2_466
C33 C30 1.5124 .
C31 C32 1.5159 .
