#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/67/2206779.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2206779
loop_
_publ_author_name
'Seewald, Oliver'
'Flörke, Ulrich'
'Henkel, Gerald'
_publ_section_title
;
 Dichlorobis(triphenylphosphine)iron(II)
;
_journal_coeditor_code           OM6256
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1829
_journal_page_last               m1830
_journal_paper_doi               10.1107/S1600536805026206
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe Cl2 (C18 H15 P)2]'
_chemical_formula_moiety         'C36 H30 Cl2 Fe P2'
_chemical_formula_sum            'C36 H30 Cl2 Fe P2'
_chemical_formula_weight         651.29
_chemical_name_systematic
;
Dichlorobis(triphenylphosphine)iron(II)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.202(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7937(13)
_cell_length_b                   8.1652(9)
_cell_length_c                   17.0760(19)
_cell_measurement_reflns_used    4456
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.48
_cell_volume                     1579.1(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2002)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9234
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  420
_diffrn_standards_number         4461
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.8423
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0551P)²+0.7177P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                2956
_reflns_number_total             3455
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om6256.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2206779
_cod_database_fobs_code          2206779
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Fe1 0.0000 0.27766(5) 0.2500 0.02809(14) Uani d S 1 Fe
Cl1 -0.00591(5) 0.15095(8) 0.36377(4) 0.04365(17) Uani d . 1 Cl
P1 0.18020(5) 0.44889(7) 0.29099(3) 0.02799(15) Uani d . 1 P
C11 0.30637(18) 0.3151(3) 0.33139(13) 0.0306(5) Uani d . 1 C
C12 0.3948(2) 0.3503(3) 0.40173(16) 0.0446(6) Uani d . 1 C
H12A 0.3907 0.4473 0.4316 0.053 Uiso calc R 1 H
C13 0.4892(3) 0.2440(4) 0.4287(2) 0.0621(8) Uani d . 1 C
H13A 0.5499 0.2682 0.4770 0.075 Uiso calc R 1 H
C14 0.4952(3) 0.1040(4) 0.3858(2) 0.0603(8) Uani d . 1 C
H14A 0.5603 0.0317 0.4044 0.072 Uiso calc R 1 H
C15 0.4079(2) 0.0676(3) 0.31629(19) 0.0501(7) Uani d . 1 C
H15A 0.4127 -0.0297 0.2869 0.060 Uiso calc R 1 H
C16 0.3130(2) 0.1716(3) 0.28878(16) 0.0411(6) Uani d . 1 C
H16A 0.2522 0.1455 0.2408 0.049 Uiso calc R 1 H
C21 0.22042(18) 0.5669(3) 0.21243(13) 0.0288(4) Uani d . 1 C
C22 0.13676(19) 0.6730(3) 0.16466(14) 0.0338(5) Uani d . 1 C
H22A 0.0614 0.6825 0.1741 0.041 Uiso calc R 1 H
C23 0.1623(2) 0.7648(3) 0.10363(15) 0.0385(5) Uani d . 1 C
H23A 0.1049 0.8375 0.0717 0.046 Uiso calc R 1 H
C24 0.2711(2) 0.7505(3) 0.08924(15) 0.0401(5) Uani d . 1 C
H24A 0.2884 0.8121 0.0468 0.048 Uiso calc R 1 H
C25 0.3550(2) 0.6466(3) 0.13662(16) 0.0443(6) Uani d . 1 C
H25A 0.4305 0.6384 0.1272 0.053 Uiso calc R 1 H
C26 0.3301(2) 0.5544(3) 0.19761(15) 0.0376(5) Uani d . 1 C
H26A 0.3880 0.4824 0.2295 0.045 Uiso calc R 1 H
C31 0.18683(17) 0.5950(3) 0.37216(12) 0.0284(4) Uani d . 1 C
C32 0.2217(2) 0.7562(3) 0.36954(14) 0.0349(5) Uani d . 1 C
H32A 0.2464 0.7941 0.3243 0.042 Uiso calc R 1 H
C33 0.2209(2) 0.8627(3) 0.43250(15) 0.0404(5) Uani d . 1 C
H33A 0.2450 0.9732 0.4302 0.048 Uiso calc R 1 H
C34 0.1854(2) 0.8092(3) 0.49816(15) 0.0382(5) Uani d . 1 C
H34A 0.1843 0.8828 0.5410 0.046 Uiso calc R 1 H
C35 0.1513(2) 0.6485(3) 0.50169(14) 0.0387(5) Uani d . 1 C
H35A 0.1282 0.6110 0.5476 0.046 Uiso calc R 1 H
C36 0.1507(2) 0.5419(3) 0.43889(13) 0.0338(5) Uani d . 1 C
H36A 0.1256 0.4319 0.4412 0.041 Uiso calc R 1 H
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'
Fe Fe 0.3463 0.8444 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Fe1 Cl1 . 2 124.42(4) y
Cl1 Fe1 P1 . 2 106.06(2) y
Cl1 Fe1 P1 2 2 104.47(2) ?
Cl1 Fe1 P1 . . 104.47(2) y
Cl1 Fe1 P1 2 . 106.06(2) ?
P1 Fe1 P1 2 . 111.25(3) y
C31 P1 C21 . . 104.51(10) ?
C31 P1 C11 . . 104.41(10) ?
C21 P1 C11 . . 104.11(10) ?
C31 P1 Fe1 . . 115.97(7) ?
C21 P1 Fe1 . . 118.07(7) ?
C11 P1 Fe1 . . 108.35(7) ?
C12 C11 C16 . . 119.3(2) ?
C12 C11 P1 . . 122.89(18) ?
C16 C11 P1 . . 117.77(18) ?
C11 C12 C13 . . 120.0(3) ?
C11 C12 H12A . . 120.0 ?
C13 C12 H12A . . 120.0 ?
C14 C13 C12 . . 120.1(3) ?
C14 C13 H13A . . 119.9 ?
C12 C13 H13A . . 119.9 ?
C15 C14 C13 . . 120.4(3) ?
C15 C14 H14A . . 119.8 ?
C13 C14 H14A . . 119.8 ?
C14 C15 C16 . . 120.3(3) ?
C14 C15 H15A . . 119.9 ?
C16 C15 H15A . . 119.9 ?
C15 C16 C11 . . 119.9(2) ?
C15 C16 H16A . . 120.0 ?
C11 C16 H16A . . 120.0 ?
C26 C21 C22 . . 118.8(2) ?
C26 C21 P1 . . 122.90(17) ?
C22 C21 P1 . . 118.26(16) ?
C23 C22 C21 . . 120.7(2) ?
C23 C22 H22A . . 119.7 ?
C21 C22 H22A . . 119.7 ?
C24 C23 C22 . . 119.9(2) ?
C24 C23 H23A . . 120.1 ?
C22 C23 H23A . . 120.1 ?
C23 C24 C25 . . 119.9(2) ?
C23 C24 H24A . . 120.0 ?
C25 C24 H24A . . 120.0 ?
C26 C25 C24 . . 120.5(2) ?
C26 C25 H25A . . 119.7 ?
C24 C25 H25A . . 119.7 ?
C25 C26 C21 . . 120.2(2) ?
C25 C26 H26A . . 119.9 ?
C21 C26 H26A . . 119.9 ?
C32 C31 C36 . . 119.0(2) ?
C32 C31 P1 . . 123.43(17) ?
C36 C31 P1 . . 117.57(17) ?
C31 C32 C33 . . 120.4(2) ?
C31 C32 H32A . . 119.8 ?
C33 C32 H32A . . 119.8 ?
C34 C33 C32 . . 120.3(2) ?
C34 C33 H33A . . 119.8 ?
C32 C33 H33A . . 119.8 ?
C33 C34 C35 . . 119.8(2) ?
C33 C34 H34A . . 120.1 ?
C35 C34 H34A . . 120.1 ?
C34 C35 C36 . . 120.3(2) ?
C34 C35 H35A . . 119.8 ?
C36 C35 H35A . . 119.8 ?
C35 C36 C31 . . 120.2(2) ?
C35 C36 H36A . . 119.9 ?
C31 C36 H36A . . 119.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl1 . 2.2192(6) y
Fe1 Cl1 2 2.2192(6) ?
Fe1 P1 2 2.4761(6) ?
Fe1 P1 . 2.4761(6) y
P1 C31 . 1.814(2) ?
P1 C21 . 1.819(2) ?
P1 C11 . 1.819(2) ?
C11 C12 . 1.383(3) ?
C11 C16 . 1.393(3) ?
C12 C13 . 1.386(4) ?
C12 H12A . 0.9500 ?
C13 C14 . 1.370(4) ?
C13 H13A . 0.9500 ?
C14 C15 . 1.369(4) ?
C14 H14A . 0.9500 ?
C15 C16 . 1.379(4) ?
C15 H15A . 0.9500 ?
C16 H16A . 0.9500 ?
C21 C26 . 1.389(3) ?
C21 C22 . 1.393(3) ?
C22 C23 . 1.383(3) ?
C22 H22A . 0.9500 ?
C23 C24 . 1.377(4) ?
C23 H23A . 0.9500 ?
C24 C25 . 1.381(3) ?
C24 H24A . 0.9500 ?
C25 C26 . 1.381(3) ?
C25 H25A . 0.9500 ?
C26 H26A . 0.9500 ?
C31 C32 . 1.384(3) ?
C31 C36 . 1.392(3) ?
C32 C33 . 1.385(3) ?
C32 H32A . 0.9500 ?
C33 C34 . 1.373(4) ?
C33 H33A . 0.9500 ?
C34 C35 . 1.379(4) ?
C34 H34A . 0.9500 ?
C35 C36 . 1.380(3) ?
C35 H35A . 0.9500 ?
C36 H36A . 0.9500 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
Cl1 Fe1 P1 C31 . -57.59(8)
Cl1 Fe1 P1 C31 2 169.43(8)
P1 Fe1 P1 C31 2 56.42(7)
Cl1 Fe1 P1 C21 . 177.26(8)
Cl1 Fe1 P1 C21 2 44.28(8)
P1 Fe1 P1 C21 2 -68.73(8)
Cl1 Fe1 P1 C11 . 59.36(8)
Cl1 Fe1 P1 C11 2 -73.62(8)
P1 Fe1 P1 C11 2 173.37(8)
C31 P1 C11 C12 . -11.6(2)
C21 P1 C11 C12 . 97.7(2)
Fe1 P1 C11 C12 . -135.78(19)
C31 P1 C11 C16 . 168.50(18)
C21 P1 C11 C16 . -82.15(19)
Fe1 P1 C11 C16 . 44.33(19)
C16 C11 C12 C13 . 0.6(4)
P1 C11 C12 C13 . -179.3(2)
C11 C12 C13 C14 . 0.0(5)
C12 C13 C14 C15 . -0.3(5)
C13 C14 C15 C16 . 0.0(5)
C14 C15 C16 C11 . 0.6(4)
C12 C11 C16 C15 . -0.9(4)
P1 C11 C16 C15 . 178.98(19)
C31 P1 C21 C26 . 104.8(2)
C11 P1 C21 C26 . -4.5(2)
Fe1 P1 C21 C26 . -124.61(18)
C31 P1 C21 C22 . -75.90(18)
C11 P1 C21 C22 . 174.83(17)
Fe1 P1 C21 C22 . 54.70(19)
C26 C21 C22 C23 . -0.1(3)
P1 C21 C22 C23 . -179.49(18)
C21 C22 C23 C24 . 0.5(4)
C22 C23 C24 C25 . -1.0(4)
C23 C24 C25 C26 . 1.1(4)
C24 C25 C26 C21 . -0.7(4)
C22 C21 C26 C25 . 0.2(3)
P1 C21 C26 C25 . 179.53(19)
C21 P1 C31 C32 . -2.7(2)
C11 P1 C31 C32 . 106.33(19)
Fe1 P1 C31 C32 . -134.54(16)
C21 P1 C31 C36 . 174.96(16)
C11 P1 C31 C36 . -75.98(18)
Fe1 P1 C31 C36 . 43.14(18)
C36 C31 C32 C33 . 0.1(3)
P1 C31 C32 C33 . 177.80(17)
C31 C32 C33 C34 . 0.0(4)
C32 C33 C34 C35 . 0.5(4)
C33 C34 C35 C36 . -1.2(4)
C34 C35 C36 C31 . 1.3(3)
C32 C31 C36 C35 . -0.8(3)
P1 C31 C36 C35 . -178.57(17)
