#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:38:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179254 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317471.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_4317471
loop_
_publ_author_name
'Jianfeng Jiang'
'Stephen A. Koch'
_publ_section_title
;
 fac-[FeII(CN)3(CO)3]- and cis-[FeII(CN)4(CO)2]2-: New Members of the
 Class of [FeII(CN)x(CO)y] Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              158
_journal_page_last               160
_journal_paper_doi               10.1021/ic015604y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C38 H40 Fe N5 O2 P'
_chemical_formula_weight         685.57
_chemical_name_systematic
'tetraphenylphosphoniumtetraethylammonium cis-Irontetracyanidedicarbonyl'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.476(2)
_cell_length_b                   29.561(6)
_cell_length_c                   11.246(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3602.2(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8231
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0589
_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)+(0.1166P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                1528
_reflns_number_total             2609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015604y_s1_3.cif
_cod_data_source_block           cisPh4PEt4NFe(CN)4(CO)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3602.2(12)
_cod_database_code               4317471
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Fe1 Fe 0.0000 0.18521(3) 0.2500 0.0522(4) Uani 1 2 d S . .
P1 P 1.0000 0.45641(5) 0.2500 0.0444(5) Uani 1 2 d S . .
N1 N 1.0000 0.17780(19) 0.7500 0.0666(17) Uani 1 2 d S . .
O1 O -0.1124(5) 0.25367(15) 0.0622(5) 0.1089(15) Uani 1 1 d . . .
C9 C 0.9258(5) 0.38772(16) 0.0764(5) 0.0585(13) Uani 1 1 d . . .
H9 H 0.8609 0.3841 0.1079 0.070 Uiso 1 1 calc R . .
N3 N -0.1140(4) 0.11257(16) 0.0518(4) 0.0700(13) Uani 1 1 d . . .
C3 C -0.0721(4) 0.13894(16) 0.1258(5) 0.0503(12) Uani 1 1 d . . .
C1 C -0.0687(5) 0.22634(18) 0.1354(6) 0.0662(15) Uani 1 1 d . . .
C2 C 0.1473(5) 0.18356(17) 0.1997(5) 0.0611(14) Uani 1 1 d . . .
C10 C 0.8664(4) 0.49145(14) 0.1964(4) 0.0452(11) Uani 1 1 d . . .
N2 N 0.2319(5) 0.18262(17) 0.1714(5) 0.0905(16) Uani 1 1 d . . .
C4 C 1.0139(4) 0.42093(14) 0.1266(4) 0.0468(12) Uani 1 1 d . . .
C8 C 0.9334(6) 0.36029(18) -0.0188(5) 0.0724(16) Uani 1 1 d . . .
H8 H 0.8731 0.3386 -0.0532 0.087 Uiso 1 1 calc R . .
C7 C 1.0294(7) 0.3650(2) -0.0624(5) 0.0795(18) Uani 1 1 d . . .
H7 H 1.0350 0.3462 -0.1264 0.095 Uiso 1 1 calc R . .
C11 C 0.7715(5) 0.48224(16) 0.0866(5) 0.0609(14) Uani 1 1 d . . .
H11 H 0.7780 0.4584 0.0353 0.073 Uiso 1 1 calc R . .
C5 C 1.1110(5) 0.42515(17) 0.0805(5) 0.0600(14) Uani 1 1 d . . .
H5 H 1.1716 0.4469 0.1133 0.072 Uiso 1 1 calc R . .
C12 C 0.6660(5) 0.50895(19) 0.0532(6) 0.0744(16) Uani 1 1 d . . .
H12 H 0.6027 0.5032 -0.0218 0.089 Uiso 1 1 calc R . .
C14 C 0.7491(5) 0.55368(17) 0.2394(6) 0.0687(15) Uani 1 1 d . . .
H14 H 0.7413 0.5773 0.2908 0.082 Uiso 1 1 calc R . .
C15 C 0.8556(5) 0.52801(15) 0.2716(5) 0.0578(13) Uani 1 1 d . . .
H15 H 0.9208 0.5351 0.3440 0.069 Uiso 1 1 calc R . .
C22 C 0.7792(7) 0.1820(2) 0.7570(7) 0.107(2) Uani 1 1 d . . .
C13 C 0.6539(5) 0.54366(19) 0.1293(6) 0.0744(17) Uani 1 1 d . . .
H13 H 0.5815 0.5606 0.1069 0.089 Uiso 1 1 calc R . .
C6 C 1.1175(6) 0.3968(2) -0.0146(5) 0.0758(17) Uani 1 1 d . . .
H6 H 1.1827 0.3996 -0.0460 0.091 Uiso 1 1 calc R . .
C17 C 1.0455(13) 0.2034(4) 0.8838(10) 0.078(3) Uani 0.50 1 d P . .
C18 C 0.9262(16) 0.1898(4) 0.8281(14) 0.094(4) Uani 0.50 1 d P . .
C16 C 1.1350(12) 0.1894(4) 0.8218(12) 0.087(4) Uani 0.50 1 d P . .
C20 C 1.0381(14) 0.2548(4) 0.8699(15) 0.103(5) Uani 0.50 1 d P . .
C19 C 1.0187(15) 0.1269(4) 0.8029(11) 0.086(5) Uani 0.50 1 d P . .
C21 C 1.0000 0.0937(5) 0.7500 0.308(17) Uani 1 2 d S . .
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'
N N 0.0061 0.0033 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C1 92.5(4) . 2 ?
C1 Fe1 C3 178.5(2) . 2 ?
C1 Fe1 C3 88.7(2) 2 2 ?
C1 Fe1 C3 88.7(2) . . ?
C1 Fe1 C3 178.5(2) 2 . ?
C3 Fe1 C3 90.0(3) 2 . ?
C1 Fe1 C2 90.5(2) . 2 ?
C1 Fe1 C2 91.5(2) 2 2 ?
C3 Fe1 C2 88.7(2) 2 2 ?
C3 Fe1 C2 89.2(2) . 2 ?
C1 Fe1 C2 91.5(2) . . ?
C1 Fe1 C2 90.5(2) 2 . ?
C3 Fe1 C2 89.2(2) 2 . ?
C3 Fe1 C2 88.7(2) . . ?
C2 Fe1 C2 177.1(3) 2 . ?
C10 P1 C10 108.9(3) 2_755 . ?
C10 P1 C4 108.5(2) 2_755 . ?
C10 P1 C4 111.4(2) . . ?
C10 P1 C4 111.4(2) 2_755 2_755 ?
C10 P1 C4 108.5(2) . 2_755 ?
C4 P1 C4 108.2(3) . 2_755 ?
C18 N1 C18 151.8(11) . 2_756 ?
C18 N1 C16 108.5(8) . . ?
C18 N1 C16 64.7(8) 2_756 . ?
C18 N1 C16 64.7(8) . 2_756 ?
C18 N1 C16 108.5(8) 2_756 2_756 ?
C16 N1 C16 154.2(10) . 2_756 ?
C18 N1 C19 114.8(7) . 2_756 ?
C18 N1 C19 92.1(7) 2_756 2_756 ?
C16 N1 C19 113.1(8) . 2_756 ?
C16 N1 C19 91.4(8) 2_756 2_756 ?
C18 N1 C19 92.1(7) . . ?
C18 N1 C19 114.8(7) 2_756 . ?
C16 N1 C19 91.4(8) . . ?
C16 N1 C19 113.1(8) 2_756 . ?
C19 N1 C19 41.0(8) 2_756 . ?
C18 N1 C17 52.7(7) . . ?
C18 N1 C17 112.2(7) 2_756 . ?
C16 N1 C17 56.1(7) . . ?
C16 N1 C17 110.4(7) 2_756 . ?
C19 N1 C17 138.5(7) 2_756 . ?
C19 N1 C17 97.6(6) . . ?
C18 N1 C17 112.2(7) . 2_756 ?
C18 N1 C17 52.7(7) 2_756 2_756 ?
C16 N1 C17 110.4(7) . 2_756 ?
C16 N1 C17 56.1(7) 2_756 2_756 ?
C19 N1 C17 97.5(6) 2_756 2_756 ?
C19 N1 C17 138.5(7) . 2_756 ?
C17 N1 C17 123.9(10) . 2_756 ?
C8 C9 C4 120.7(5) . . ?
N3 C3 Fe1 178.7(5) . . ?
O1 C1 Fe1 178.8(6) . . ?
N2 C2 Fe1 179.7(6) . . ?
C11 C10 C15 119.4(4) . . ?
C11 C10 P1 121.7(3) . . ?
C15 C10 P1 118.8(4) . . ?
C5 C4 C9 118.8(4) . . ?
C5 C4 P1 121.8(4) . . ?
C9 C4 P1 119.4(3) . . ?
C7 C8 C9 119.5(5) . . ?
C8 C7 C6 121.2(5) . . ?
C10 C11 C12 119.4(5) . . ?
C6 C5 C4 119.5(5) . . ?
C13 C12 C11 121.0(5) . . ?
C15 C14 C13 119.0(5) . . ?
C14 C15 C10 120.8(5) . . ?
C16 C22 C18 60.5(7) 2_756 . ?
C12 C13 C14 120.3(5) . . ?
C7 C6 C5 120.3(5) . . ?
C18 C17 C16 116.6(10) . . ?
C18 C17 C20 103.5(13) . . ?
C16 C17 C20 104.8(10) . . ?
C18 C17 N1 57.6(6) . . ?
C16 C17 N1 59.2(6) . . ?
C20 C17 N1 112.5(10) . . ?
C17 C18 N1 69.7(8) . . ?
C17 C18 C16 120.8(10) . 2_756 ?
N1 C18 C16 60.1(7) . 2_756 ?
C17 C18 C22 170.9(12) . . ?
N1 C18 C22 112.7(10) . . ?
C16 C18 C22 57.1(8) 2_756 . ?
C17 C16 N1 64.7(7) . . ?
C17 C16 C22 170.2(11) . 2_756 ?
N1 C16 C22 113.1(9) . 2_756 ?
C17 C16 C18 111.3(10) . 2_756 ?
N1 C16 C18 55.2(7) . 2_756 ?
C22 C16 C18 62.4(8) 2_756 2_756 ?
C19 C19 C21 60.2(7) 2_756 . ?
C19 C19 N1 69.5(4) 2_756 . ?
C21 C19 N1 129.7(10) . . ?
C19 C21 C19 59.6(13) . 2_756 ?
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
Fe1 C1 1.758(6) . ?
Fe1 C1 1.758(6) 2 ?
Fe1 C3 1.935(5) 2 ?
Fe1 C3 1.935(5) . ?
Fe1 C2 1.952(6) 2 ?
Fe1 C2 1.952(6) . ?
P1 C10 1.782(4) 2_755 ?
P1 C10 1.782(4) . ?
P1 C4 1.788(4) . ?
P1 C4 1.788(4) 2_755 ?
N1 C18 1.450(12) . ?
N1 C18 1.450(12) 2_756 ?
N1 C16 1.531(13) . ?
N1 C16 1.531(13) 2_756 ?
N1 C19 1.607(12) 2_756 ?
N1 C19 1.607(12) . ?
N1 C17 1.610(11) . ?
N1 C17 1.610(11) 2_756 ?
O1 C1 1.145(6) . ?
C9 C8 1.369(7) . ?
C9 C4 1.389(6) . ?
N3 C3 1.126(6) . ?
C2 N2 1.117(7) . ?
C10 C11 1.378(6) . ?
C10 C15 1.403(6) . ?
C4 C5 1.381(6) . ?
C8 C7 1.353(8) . ?
C7 C6 1.355(8) . ?
C11 C12 1.390(7) . ?
C5 C6 1.379(7) . ?
C12 C13 1.372(7) . ?
C14 C15 1.382(7) . ?
C14 C13 1.386(7) . ?
C22 C16 1.542(14) 2_756 ?
C22 C18 1.628(19) . ?
C17 C18 1.365(18) . ?
C17 C16 1.479(17) . ?
C17 C20 1.526(16) . ?
C18 C16 1.598(19) 2_756 ?
C16 C22 1.542(14) 2_756 ?
C16 C18 1.598(19) 2_756 ?
C19 C19 1.12(2) 2_756 ?
C19 C21 1.132(12) . ?
C21 C19 1.132(12) 2_756 ?
