#------------------------------------------------------------------------------
#$Date: 2019-11-08 03:07:40 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224977 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058187.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_7058187
loop_
_publ_author_name
'Vosáhlo, Petr'
'Schulz, Jiří'
'Škoch, Karel'
'Císařová, Ivana'
'Štěpnička, Petr'
_publ_section_title
;
 Synthesis and characterisation of palladium(ii) complexes with hybrid
 phosphinoferrocene ligands bearing additional O-donor substituents
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4463
_journal_paper_doi               10.1039/C9NJ00298G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C46 H38 Cl2 Fe2 O2 P2 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H42 Cl6 Fe2 O2 P2 Pd'
_chemical_formula_weight         1143.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-29 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                105.0080(10)
_cell_angle_beta                 101.0690(10)
_cell_angle_gamma                108.0470(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1991(3)
_cell_length_b                   11.0936(3)
_cell_length_c                   12.7081(4)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.54
_cell_volume                     1137.49(6)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v2016.1.0.1'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD - Bruker Apex2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20022
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.563
_diffrn_reflns_theta_min         1.737
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS-2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0198P)²+0.8747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4874
_reflns_number_total             5253
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj00298g3.cif
_cod_data_source_block           pv119
_cod_depositor_comments
'Adding full bibliography for 7058185--7058194.cif.'
_cod_database_code               7058187
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.708
_shelx_estimated_absorpt_t_max   0.819
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd Pd 0.5000 0.0000 0.5000 0.01015(4) Uani 1 2 d S . P
Fe Fe 0.25498(2) 0.22431(2) 0.68344(2) 0.01215(5) Uani 1 1 d . . .
Cl Cl 0.27312(4) -0.08723(4) 0.34801(3) 0.01728(8) Uani 1 1 d . . .
P P 0.49942(4) 0.21248(4) 0.50623(3) 0.01109(8) Uani 1 1 d . . .
O O 0.2655(2) 0.47033(17) 0.96528(13) 0.0473(4) Uani 1 1 d . . .
C1 C 0.2323(2) 0.25581(17) 0.84308(13) 0.0188(3) Uani 1 1 d . . .
C2 C 0.12612(19) 0.12297(17) 0.76797(13) 0.0181(3) Uani 1 1 d . . .
H2 H 0.0127 0.0877 0.7495 0.022 Uiso 1 1 calc R U .
C3 C 0.22076(19) 0.05363(17) 0.72625(14) 0.0186(3) Uani 1 1 d . . .
H3 H 0.1816 -0.0364 0.6749 0.022 Uiso 1 1 calc R U .
C4 C 0.38470(19) 0.14234(17) 0.77471(13) 0.0179(3) Uani 1 1 d . . .
H4 H 0.4734 0.1213 0.7611 0.021 Uiso 1 1 calc R U .
C5 C 0.39328(19) 0.26742(17) 0.84667(13) 0.0187(3) Uani 1 1 d . . .
H5 H 0.4880 0.3446 0.8893 0.022 Uiso 1 1 calc R U .
C6 C 0.33879(18) 0.25025(15) 0.54956(12) 0.0135(3) Uani 1 1 d . . .
C7 C 0.3514(2) 0.37737(16) 0.62444(13) 0.0173(3) Uani 1 1 d . . .
H7 H 0.4471 0.4549 0.6633 0.021 Uiso 1 1 calc R U .
C8 C 0.1952(2) 0.36649(17) 0.62995(14) 0.0202(3) Uani 1 1 d . . .
H8 H 0.1687 0.4357 0.6735 0.024 Uiso 1 1 calc R U .
C9 C 0.0852(2) 0.23461(18) 0.55930(14) 0.0197(3) Uani 1 1 d . . .
H9 H -0.0272 0.2009 0.5471 0.024 Uiso 1 1 calc R U .
C10 C 0.17276(18) 0.16178(17) 0.51007(13) 0.0161(3) Uani 1 1 d . . .
H10 H 0.1292 0.0708 0.4600 0.019 Uiso 1 1 calc R U .
C11 C 0.1794(2) 0.3622(2) 0.89458(16) 0.0291(4) Uani 1 1 d . . .
H11 H 0.0683 0.3448 0.8704 0.035 Uiso 1 1 calc R U .
C12 C 0.47770(18) 0.22646(15) 0.36521(12) 0.0135(3) Uani 1 1 d . . .
C13 C 0.5819(2) 0.19360(18) 0.30669(14) 0.0227(3) Uani 1 1 d . . .
H13 H 0.6579 0.1622 0.3400 0.027 Uiso 1 1 calc R U .
C14 C 0.5751(2) 0.2065(2) 0.20057(16) 0.0305(4) Uani 1 1 d . . .
H14 H 0.6477 0.1856 0.1621 0.037 Uiso 1 1 calc R U .
C15 C 0.4630(2) 0.24968(19) 0.15042(15) 0.0294(4) Uani 1 1 d . . .
H15 H 0.4591 0.2592 0.0779 0.035 Uiso 1 1 calc R U .
C16 C 0.3566(2) 0.27906(18) 0.20631(15) 0.0266(4) Uani 1 1 d . . .
H16 H 0.2780 0.3068 0.1711 0.032 Uiso 1 1 calc R U .
C17 C 0.3640(2) 0.26826(16) 0.31375(13) 0.0188(3) Uani 1 1 d . . .
H17 H 0.2912 0.2895 0.3519 0.023 Uiso 1 1 calc R U .
C18 C 0.67900(18) 0.35830(15) 0.59755(13) 0.0134(3) Uani 1 1 d . . .
C19 C 0.77521(19) 0.44317(16) 0.55301(14) 0.0169(3) Uani 1 1 d . . .
H19 H 0.7456 0.4275 0.4734 0.020 Uiso 1 1 calc R U .
C20 C 0.9143(2) 0.55065(17) 0.62454(15) 0.0214(3) Uani 1 1 d . . .
H20 H 0.9795 0.6078 0.5934 0.026 Uiso 1 1 calc R U .
C21 C 0.9584(2) 0.57492(17) 0.74059(15) 0.0215(3) Uani 1 1 d . . .
H21 H 1.0538 0.6483 0.7891 0.026 Uiso 1 1 calc R U .
C22 C 0.8626(2) 0.49159(17) 0.78628(14) 0.0200(3) Uani 1 1 d . . .
H22 H 0.8920 0.5086 0.8661 0.024 Uiso 1 1 calc R U .
C23 C 0.72434(19) 0.38376(16) 0.71527(13) 0.0168(3) Uani 1 1 d . . .
H23 H 0.6598 0.3267 0.7467 0.020 Uiso 1 1 calc R U .
C1S C 0.1786(3) 0.9025(2) 1.06276(18) 0.0421(5) Uani 1 1 d . . .
H1S1 H 0.0799 0.8896 1.0863 0.051 Uiso 1 1 calc R U .
H1S2 H 0.2689 0.9742 1.1268 0.051 Uiso 1 1 calc R U .
Cl1S Cl 0.21302(6) 0.75039(5) 1.03437(4) 0.02915(10) Uani 1 1 d . . .
Cl2S Cl 0.15852(7) 0.95419(5) 0.94312(4) 0.03868(12) Uani 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
Cl Pd Cl 180.0 . 2_656
Cl Pd P 93.509(13) . 2_656
Cl Pd P 86.491(13) 2_656 2_656
Cl Pd P 86.491(13) . .
Cl Pd P 93.509(13) 2_656 .
P Pd P 180.0 2_656 .
C2 Fe C1 41.41(7) . .
C2 Fe C10 118.99(7) . .
C1 Fe C10 154.94(6) . .
C2 Fe C6 156.68(7) . .
C1 Fe C6 161.53(7) . .
C10 Fe C6 41.24(6) . .
C2 Fe C9 103.95(7) . .
C1 Fe C9 119.21(7) . .
C10 Fe C9 40.79(6) . .
C6 Fe C9 68.82(6) . .
C2 Fe C8 121.02(7) . .
C1 Fe C8 105.78(7) . .
C10 Fe C8 68.69(7) . .
C6 Fe C8 68.69(6) . .
C9 Fe C8 40.62(7) . .
C2 Fe C3 40.68(6) . .
C1 Fe C3 68.76(7) . .
C10 Fe C3 106.61(7) . .
C6 Fe C3 123.05(6) . .
C9 Fe C3 121.70(7) . .
C8 Fe C3 157.69(7) . .
C2 Fe C7 158.68(7) . .
C1 Fe C7 123.48(7) . .
C10 Fe C7 69.10(6) . .
C6 Fe C7 41.08(6) . .
C9 Fe C7 68.50(7) . .
C8 Fe C7 40.53(6) . .
C3 Fe C7 160.13(6) . .
C2 Fe C5 69.23(6) . .
C1 Fe C5 41.11(6) . .
C10 Fe C5 162.05(6) . .
C6 Fe C5 125.90(6) . .
C9 Fe C5 156.67(7) . .
C8 Fe C5 122.57(7) . .
C3 Fe C5 68.39(7) . .
C7 Fe C5 109.40(7) . .
C2 Fe C4 68.42(6) . .
C1 Fe C4 68.31(6) . .
C10 Fe C4 125.04(7) . .
C6 Fe C4 110.34(6) . .
C9 Fe C4 159.65(7) . .
C8 Fe C4 159.46(7) . .
C3 Fe C4 40.47(6) . .
C7 Fe C4 125.15(7) . .
C5 Fe C4 40.21(7) . .
C6 P C12 104.97(7) . .
C6 P C18 104.10(7) . .
C12 P C18 104.34(7) . .
C6 P Pd 115.27(5) . .
C12 P Pd 110.13(5) . .
C18 P Pd 116.84(5) . .
C2 C1 C5 107.96(14) . .
C2 C1 C11 124.21(16) . .
C5 C1 C11 127.48(16) . .
C2 C1 Fe 69.20(9) . .
C5 C1 Fe 70.58(9) . .
C11 C1 Fe 120.52(12) . .
C3 C2 C1 107.79(14) . .
C3 C2 Fe 70.57(9) . .
C1 C2 Fe 69.38(9) . .
C3 C2 H2 126.1 . .
C1 C2 H2 126.1 . .
Fe C2 H2 125.5 . .
C2 C3 C4 108.21(15) . .
C2 C3 Fe 68.74(9) . .
C4 C3 Fe 70.43(9) . .
C2 C3 H3 125.9 . .
C4 C3 H3 125.9 . .
Fe C3 H3 126.5 . .
C5 C4 C3 108.65(14) . .
C5 C4 Fe 69.55(9) . .
C3 C4 Fe 69.10(9) . .
C5 C4 H4 125.7 . .
C3 C4 H4 125.7 . .
Fe C4 H4 127.3 . .
C4 C5 C1 107.40(14) . .
C4 C5 Fe 70.24(9) . .
C1 C5 Fe 68.31(9) . .
C4 C5 H5 126.3 . .
C1 C5 H5 126.3 . .
Fe C5 H5 126.7 . .
C7 C6 C10 107.45(13) . .
C7 C6 P 126.17(12) . .
C10 C6 P 126.27(12) . .
C7 C6 Fe 69.66(9) . .
C10 C6 Fe 69.01(8) . .
P C6 Fe 129.51(8) . .
C8 C7 C6 107.87(14) . .
C8 C7 Fe 69.62(9) . .
C6 C7 Fe 69.26(8) . .
C8 C7 H7 126.1 . .
C6 C7 H7 126.1 . .
Fe C7 H7 126.6 . .
C7 C8 C9 108.54(14) . .
C7 C8 Fe 69.84(9) . .
C9 C8 Fe 69.67(9) . .
C7 C8 H8 125.7 . .
C9 C8 H8 125.7 . .
Fe C8 H8 126.3 . .
C8 C9 C10 108.21(14) . .
C8 C9 Fe 69.72(9) . .
C10 C9 Fe 69.16(9) . .
C8 C9 H9 125.9 . .
C10 C9 H9 125.9 . .
Fe C9 H9 126.8 . .
C9 C10 C6 107.93(14) . .
C9 C10 Fe 70.05(9) . .
C6 C10 Fe 69.75(8) . .
C9 C10 H10 126.0 . .
C6 C10 H10 126.0 . .
Fe C10 H10 125.7 . .
O C11 C1 125.26(19) . .
O C11 H11 117.4 . .
C1 C11 H11 117.4 . .
C17 C12 C13 119.03(14) . .
C17 C12 P 123.35(12) . .
C13 C12 P 117.62(12) . .
C14 C13 C12 120.44(16) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C15 C14 C13 120.26(17) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C14 C15 C16 119.74(16) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C15 C16 C17 120.44(17) . .
C15 C16 H16 119.8 . .
C17 C16 H16 119.8 . .
C12 C17 C16 120.07(16) . .
C12 C17 H17 120.0 . .
C16 C17 H17 120.0 . .
C19 C18 C23 118.90(14) . .
C19 C18 P 121.79(12) . .
C23 C18 P 119.29(11) . .
C20 C19 C18 120.33(15) . .
C20 C19 H19 119.8 . .
C18 C19 H19 119.8 . .
C21 C20 C19 120.42(15) . .
C21 C20 H20 119.8 . .
C19 C20 H20 119.8 . .
C20 C21 C22 119.82(15) . .
C20 C21 H21 120.1 . .
C22 C21 H21 120.1 . .
C23 C22 C21 120.01(15) . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C22 C23 C18 120.52(15) . .
C22 C23 H23 119.7 . .
C18 C23 H23 119.7 . .
Cl2S C1S Cl1S 111.92(11) . .
Cl2S C1S H1S1 109.2 . .
Cl1S C1S H1S1 109.2 . .
Cl2S C1S H1S2 109.2 . .
Cl1S C1S H1S2 109.2 . .
H1S1 C1S H1S2 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd Cl 2.2925(4) .
Pd Cl 2.2925(4) 2_656
Pd P 2.3396(4) 2_656
Pd P 2.3396(4) .
Fe C2 2.0278(16) .
Fe C1 2.0302(15) .
Fe C10 2.0374(15) .
Fe C6 2.0474(15) .
Fe C9 2.0492(15) .
Fe C8 2.0498(16) .
Fe C3 2.0519(16) .
Fe C7 2.0527(16) .
Fe C5 2.0605(15) .
Fe C4 2.0696(15) .
P C6 1.7997(15) .
P C12 1.8170(15) .
P C18 1.8244(15) .
O C11 1.205(2) .
C1 C2 1.435(2) .
C1 C5 1.437(2) .
C1 C11 1.462(2) .
C2 C3 1.418(2) .
C2 H2 0.9500 .
C3 C4 1.426(2) .
C3 H3 0.9500 .
C4 C5 1.420(2) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.438(2) .
C6 C10 1.439(2) .
C7 C8 1.421(2) .
C7 H7 0.9500 .
C8 C9 1.423(3) .
C8 H8 0.9500 .
C9 C10 1.424(2) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 H11 0.9500 .
C12 C17 1.390(2) .
C12 C13 1.398(2) .
C13 C14 1.384(2) .
C13 H13 0.9500 .
C14 C15 1.382(3) .
C14 H14 0.9500 .
C15 C16 1.383(3) .
C15 H15 0.9500 .
C16 C17 1.392(2) .
C16 H16 0.9500 .
C17 H17 0.9500 .
C18 C19 1.394(2) .
C18 C23 1.400(2) .
C19 C20 1.390(2) .
C19 H19 0.9500 .
C20 C21 1.382(2) .
C20 H20 0.9500 .
C21 C22 1.392(2) .
C21 H21 0.9500 .
C22 C23 1.386(2) .
C22 H22 0.9500 .
C23 H23 0.9500 .
C1S Cl2S 1.756(2) .
C1S Cl1S 1.771(2) .
C1S H1S1 0.9900 .
C1S H1S2 0.9900 .
