#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/66/2206600.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_2206600
loop_
_publ_author_name
'María Gabriela Ballinas-López'
'Itzia I. Padilla-Martínez'
'Francisco J. Martínez-Martínez'
'Herbert Höpfl'
'Efrén V. García-Báez'
_publ_section_title
;
 Di-μ-diphenylphosphido-bis[tricarbonyliron(II)] dichloromethane
 solvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1475
_journal_page_last               m1477
_journal_paper_doi               10.1107/S1600536805020982
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe2 (C12 H10 P)2 (C O)6], C H2 Cl2'
_chemical_formula_moiety         'C30 H20 Fe2 O6 P2, C H2 Cl2'
_chemical_formula_sum            'C31 H22 Cl2 Fe2 O6 P2'
_chemical_formula_weight         735.03
_chemical_name_systematic
;
Di-μ-diphenylphosphido-bis[tricarbonyliron(II)] dichloromethane solvate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 105.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3218(11)
_cell_length_b                   12.7214(13)
_cell_length_c                   11.8011(12)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1634.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXL97 and WinGX2003 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       'Bruker SMART area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8071
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0878P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.128
_refine_ls_wR_factor_ref         0.132
_reflns_number_gt                2896
_reflns_number_total             3826
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu6018.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2206600
_cod_database_fobs_code          2206600
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,-z
-x,-y,-z
x,1/2-y,z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_type_symbol
Fe 0.39139(3) 0.14753(3) 0.29892(3) 0.03350(10) Uani 1.000 Fe
P1 0.25204(8) 0.25000 0.34476(8) 0.0341(3) Uani 1.000 P
P2 0.34056(8) 0.25000 0.14062(8) 0.0323(3) Uani 1.000 P
O10 0.2581(2) -0.04789(18) 0.2297(2) 0.0665(8) Uani 1.000 O
O11 0.6258(2) 0.0945(2) 0.2550(3) 0.0899(11) Uani 1.000 O
O12 0.5111(3) 0.1175(2) 0.5507(2) 0.0752(9) Uani 1.000 O
C1 0.2380(4) 0.25000 0.4948(3) 0.0484(14) Uani 1.000 C
C2 0.2306(4) 0.1567(3) 0.5520(3) 0.0693(14) Uani 1.000 C
C3 0.2154(5) 0.1576(4) 0.6652(4) 0.099(2) Uani 1.000 C
C4 0.2076(6) 0.25000 0.7189(5) 0.102(3) Uani 1.000 C
C5 0.0890(3) 0.25000 0.2656(3) 0.0450(14) Uani 1.000 C
C6 0.0254(3) 0.1580(3) 0.2403(4) 0.0751(13) Uani 1.000 C
C7 -0.1013(3) 0.1586(4) 0.1867(4) 0.098(2) Uani 1.000 C
C8 -0.1627(5) 0.25000 0.1596(5) 0.090(3) Uani 1.000 C
C10 0.3093(2) 0.0285(2) 0.2564(2) 0.0427(9) Uani 1.000 C
C11 0.5349(3) 0.1158(3) 0.2707(3) 0.0518(10) Uani 1.000 C
C12 0.4628(3) 0.1281(2) 0.4536(3) 0.0489(10) Uani 1.000 C
C21 0.4315(3) 0.25000 0.0335(3) 0.0384(11) Uani 1.000 C
C22 0.4609(3) 0.1578(2) -0.0120(3) 0.0592(11) Uani 1.000 C
C23 0.5231(4) 0.1586(3) -0.0980(3) 0.0741(16) Uani 1.000 C
C24 0.5535(5) 0.25000 -0.1395(4) 0.0722(19) Uani 1.000 C
C25 0.1870(3) 0.25000 0.0380(3) 0.0379(11) Uani 1.000 C
C26 0.1306(3) 0.1576(3) -0.0043(3) 0.0626(12) Uani 1.000 C
C27 0.0153(4) 0.1579(3) -0.0865(3) 0.0823(16) Uani 1.000 C
C28 -0.0408(5) 0.25000 -0.1272(5) 0.080(2) Uani 1.000 C
Cl1 0.8433(4) 0.1424(3) 0.5360(3) 0.379(3) Uani 1.000 Cl
C30 0.8992(9) 0.25000 0.4969(9) 0.131(4) Uani 1.000 C
H2 0.23570 0.09307 0.51491 0.0831 Uiso 1.000 H
H3 0.21060 0.09458 0.70369 0.1184 Uiso 1.000 H
H4 0.19662 0.25000 0.79414 0.1233 Uiso 1.000 H
H6 0.06660 0.09433 0.25883 0.0899 Uiso 1.000 H
H7 -0.14349 0.09524 0.16963 0.1174 Uiso 1.000 H
H8 -0.24655 0.25000 0.12248 0.1081 Uiso 1.000 H
H22 0.43902 0.09403 0.01503 0.0708 Uiso 1.000 H
H23 0.54389 0.09538 -0.12716 0.0888 Uiso 1.000 H
H24 0.59558 0.25000 -0.19698 0.0865 Uiso 1.000 H
H26 0.16921 0.09410 0.02180 0.0757 Uiso 1.000 H
H27 -0.02326 0.09462 -0.11359 0.0989 Uiso 1.000 H
H28 -0.11719 0.25000 -0.18260 0.0962 Uiso 1.000 H
H30A 0.88361 0.25000 0.41182 0.1577 Uiso 1.000 H
H30B 0.98758 0.25000 0.53092 0.1577 Uiso 1.000 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'
O O 0.0106 0.0060 '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'
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'
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
P1 Fe P2 . . 79.84(3) yes
P1 Fe C10 . . 102.55(8) yes
P1 Fe C11 . . 156.48(12) yes
P1 Fe C12 . . 89.11(11) yes
Fe Fe P1 4_555 . 54.14(2) yes
P2 Fe C10 . . 105.59(8) yes
P2 Fe C11 . . 90.81(12) yes
P2 Fe C12 . . 151.02(9) yes
Fe Fe P2 4_555 . 54.04(2) yes
C10 Fe C11 . . 100.73(14) yes
C10 Fe C12 . . 102.93(12) yes
Fe Fe C10 4_555 . 148.53(8) yes
C11 Fe C12 . . 88.87(16) yes
Fe Fe C11 4_555 . 103.02(12) yes
Fe Fe C12 4_555 . 97.90(8) yes
Fe P1 C1 . . 119.60(11) y
Fe P1 C5 . . 124.09(8) y
Fe P1 Fe . 4_555 71.73(3) y
C1 P1 C5 . . 98.69(18) y
Fe P1 C1 4_555 . 119.60(11) y
Fe P1 C5 4_555 . 124.09(8) y
Fe P2 C21 . . 120.96(9) y
Fe P2 C25 . . 122.51(9) y
Fe P2 Fe . 4_555 71.91(3) y
C21 P2 C25 . . 98.94(16) y
Fe P2 C21 4_555 . 120.96(9) y
Fe P2 C25 4_555 . 122.51(9) y
P1 C1 C2 . . 120.6(2) no
P1 C1 C2 . 4_555 120.6(2) no
C2 C1 C2 . 4_555 118.7(3) no
C1 C2 C3 . . 120.2(4) no
C2 C3 C4 . . 119.9(5) no
C3 C4 C3 . 4_555 121.1(5) no
P1 C5 C6 . . 120.7(2) no
P1 C5 C6 . 4_555 120.7(2) no
C6 C5 C6 . 4_555 118.3(3) no
C5 C6 C7 . . 120.5(4) no
C6 C7 C8 . . 120.6(4) no
C7 C8 C7 . 4_555 119.3(5) no
Fe C10 O10 . . 179.3(2) no
Fe C11 O11 . . 178.5(3) no
Fe C12 O12 . . 177.8(3) no
P2 C21 C22 . . 120.86(19) no
P2 C21 C22 . 4_555 120.86(19) no
C22 C21 C22 . 4_555 118.0(3) no
C21 C22 C23 . . 120.6(3) no
C22 C23 C24 . . 120.4(4) no
C23 C24 C23 . 4_555 120.0(5) no
P2 C25 C26 . . 120.5(2) no
P2 C25 C26 . 4_555 120.5(2) no
C26 C25 C26 . 4_555 118.9(3) no
C25 C26 C27 . . 120.4(3) no
C26 C27 C28 . . 120.4(4) no
C27 C28 C27 . 4_555 119.5(5) no
C1 C2 H2 . . 119.93 no
C3 C2 H2 . . 119.92 no
C2 C3 H3 . . 120.02 no
C4 C3 H3 . . 120.07 no
C3 C4 H4 . . 119.44 no
C3 C4 H4 4_555 . 119.44 no
C5 C6 H6 . . 119.70 no
C7 C6 H6 . . 119.76 no
C6 C7 H7 . . 119.64 no
C8 C7 H7 . . 119.72 no
C7 C8 H8 . . 120.34 no
C7 C8 H8 4_555 . 120.34 no
C21 C22 H22 . . 119.77 no
C23 C22 H22 . . 119.66 no
C22 C23 H23 . . 119.74 no
C24 C23 H23 . . 119.83 no
C23 C24 H24 . . 120.01 no
C23 C24 H24 4_555 . 120.01 no
C25 C26 H26 . . 119.81 no
C27 C26 H26 . . 119.81 no
C26 C27 H27 . . 119.84 no
C28 C27 H27 . . 119.77 no
C27 C28 H28 . . 120.23 no
C27 C28 H28 4_555 . 120.23 no
Cl1 C30 Cl1 . 4_555 114.5(7) no
Cl1 C30 H30A . . 108.62 no
Cl1 C30 H30B . . 108.66 no
H30A C30 H30B . . 107.54 no
Cl1 C30 H30A 4_555 . 108.62 no
Cl1 C30 H30B 4_555 . 108.66 no
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
Fe P1 . 2.2250(9) yes
Fe P2 . 2.2200(8) yes
Fe C10 . 1.775(3) yes
Fe C11 . 1.792(4) yes
Fe C12 . 1.798(3) yes
Fe Fe 4_555 2.6071(6) yes
Cl1 C30 . 1.627(7) yes
P1 C1 . 1.821(4) yes
P1 C5 . 1.825(4) yes
P2 C21 . 1.837(4) yes
P2 C25 . 1.825(4) yes
O10 C10 . 1.131(3) yes
O11 C11 . 1.128(4) yes
O12 C12 . 1.134(4) yes
C1 C2 4_555 1.379(4) no
C1 C2 . 1.379(4) no
C2 C3 . 1.393(6) no
C3 C4 . 1.350(6) no
C5 C6 . 1.363(4) no
C5 C6 4_555 1.363(4) no
C6 C7 . 1.399(5) no
C7 C8 . 1.347(6) no
C21 C22 . 1.369(3) no
C21 C22 4_555 1.369(3) no
C22 C23 . 1.385(5) no
C23 C24 . 1.343(5) no
C25 C26 . 1.365(4) no
C25 C26 4_555 1.365(4) no
C26 C27 . 1.396(5) no
C27 C28 . 1.356(5) no
C2 H2 . 0.9295 no
C3 H3 . 0.9304 no
C4 H4 . 0.9298 no
C6 H6 . 0.9302 no
C7 H7 . 0.9303 no
C8 H8 . 0.9296 no
C22 H22 . 0.9299 no
C23 H23 . 0.9302 no
C24 H24 . 0.9301 no
C26 H26 . 0.9297 no
C27 H27 . 0.9295 no
C28 H28 . 0.9296 no
C30 H30A . 0.9704 no
C30 H30B . 0.9702 no
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
P1 Fe Fe P2 . . 4_555 . -104.81(4) no
P2 Fe Fe P1 . . 4_555 . 104.81(4) no
C10 Fe Fe P1 . . 4_555 . 48.13(15) no
C10 Fe Fe P2 . . 4_555 . -56.68(15) no
C10 Fe Fe C10 . . 4_555 4_555 0.0(2) no
C10 Fe Fe C11 . . 4_555 4_555 -138.07(18) no
C10 Fe Fe C12 . . 4_555 4_555 131.26(19) no
C11 Fe Fe P1 . . 4_555 . -173.80(12) no
C11 Fe Fe P2 . . 4_555 . 81.39(12) no
C11 Fe Fe C10 . . 4_555 4_555 138.07(18) no
C11 Fe Fe C11 . . 4_555 4_555 0.00(16) no
C11 Fe Fe C12 . . 4_555 4_555 -90.67(16) no
C12 Fe Fe P1 . . 4_555 . -83.13(12) no
C12 Fe Fe P2 . . 4_555 . 172.06(12) no
C12 Fe Fe C10 . . 4_555 4_555 -131.26(19) no
C12 Fe Fe C11 . . 4_555 4_555 90.67(16) no
C12 Fe Fe C12 . . 4_555 4_555 0.00(16) no
P2 Fe P1 C1 . . . . -166.91(12) no
C10 Fe P1 C1 . . . . 89.22(14) no
C11 Fe P1 C1 . . . . -99.0(3) no
C12 Fe P1 C1 . . . . -13.83(15) no
Fe Fe P1 C1 4_555 . . . -114.25(12) no
P2 Fe P1 C5 . . . . 66.63(10) no
C10 Fe P1 C5 . . . . -37.24(13) no
C11 Fe P1 C5 . . . . 134.6(3) no
C12 Fe P1 C5 . . . . -140.29(14) no
Fe Fe P1 C5 4_555 . . . 119.29(11) no
P2 Fe P1 Fe . . . 4_555 -52.66(3) no
C10 Fe P1 Fe . . . 4_555 -156.53(8) no
C11 Fe P1 Fe . . . 4_555 15.3(3) no
C12 Fe P1 Fe . . . 4_555 100.42(10) no
P2 Fe P1 Fe . 4_555 . . 52.66(3) no
Fe Fe P1 C1 . 4_555 . . 114.25(12) no
Fe Fe P1 C5 . 4_555 . . -119.29(11) no
P1 Fe P2 C21 . . . . 168.55(10) no
C10 Fe P2 C21 . . . . -91.13(12) no
C11 Fe P2 C21 . . . . 10.26(15) no
C12 Fe P2 C21 . . . . 99.4(3) no
Fe Fe P2 C21 4_555 . . . 115.80(10) no
P1 Fe P2 C25 . . . . -64.78(10) no
C10 Fe P2 C25 . . . . 35.54(13) no
C11 Fe P2 C25 . . . . 136.92(15) no
C12 Fe P2 C25 . . . . -133.9(2) no
Fe Fe P2 C25 4_555 . . . -117.53(10) no
P1 Fe P2 Fe . . . 4_555 52.75(3) no
C10 Fe P2 Fe . . . 4_555 153.07(8) no
C11 Fe P2 Fe . . . 4_555 -105.55(12) no
C12 Fe P2 Fe . . . 4_555 -16.4(2) no
P1 Fe P2 Fe . 4_555 . . -52.75(3) no
Fe Fe P2 C21 . 4_555 . . -115.80(10) no
Fe Fe P2 C25 . 4_555 . . 117.53(10) no
Fe P1 C1 C2 . . . . -48.7(4) no
C5 P1 C1 C2 . . . . 89.0(4) no
Fe P1 C1 C2 4_555 . . . -133.4(3) no
Fe P1 C1 C2 . . . 4_555 133.4(3) no
Fe P1 C5 C6 . . . 4_555 -138.2(3) no
Fe P1 C5 C6 . . . . 48.1(4) no
C1 P1 C5 C6 . . . . -86.9(3) no
Fe P1 C5 C6 4_555 . . . 138.2(3) no
Fe P2 C25 C26 . . . 4_555 136.6(3) no
Fe P2 C25 C26 4_555 . . . -136.6(3) no
Fe P2 C21 C22 . . . . 50.2(3) no
Fe P2 C21 C22 . . . 4_555 -136.6(3) no
Fe P2 C21 C22 4_555 . . . 136.6(3) no
C21 P2 C25 C26 . . . . 87.6(3) no
C25 P2 C21 C22 . . . . -86.6(3) no
Fe P2 C25 C26 . . . . -48.3(3) no
C2 C1 C2 C3 4_555 . . . 0.3(7) no
P1 C1 C2 C3 . . . . -177.7(4) no
C1 C2 C3 C4 . . . . 0.2(8) no
C2 C3 C4 C3 . . . 4_555 -0.6(9) no
P1 C5 C6 C7 . . . . 175.7(3) no
C6 C5 C6 C7 4_555 . . . 1.8(6) no
C5 C6 C7 C8 . . . . -0.3(7) no
C6 C7 C8 C7 . . . 4_555 -1.3(8) no
C22 C21 C22 C23 4_555 . . . 2.6(5) no
P2 C21 C22 C23 . . . . 176.1(3) no
C21 C22 C23 C24 . . . . -1.2(6) no
C22 C23 C24 C23 . . . 4_555 -0.3(7) no
P2 C25 C26 C27 . . . . -177.3(3) no
C26 C25 C26 C27 4_555 . . . -2.1(5) no
C25 C26 C27 C28 . . . . 1.4(6) no
C26 C27 C28 C27 . . . 4_555 -0.7(7) no
