#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:05:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179276 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/96/4319647.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_4319647
loop_
_publ_author_name
'Vladimir Arion'
'Jean-Jacques Brunet'
'Denis Neibecker'
_publ_section_title
;
 Crystal Structure, Mössbauer Spectra, and Thermal Behavior of
 H2Fe(CO)2[P(OPh)3]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2628
_journal_page_last               2630
_journal_paper_doi               10.1021/ic0006899
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C38 H32 Fe O8 P2'
_chemical_formula_sum            'C38 H32 Fe O8 P2'
_chemical_formula_weight         734.43
_chemical_melting_point          365.6(5)
_chemical_name_systematic
; 
Dicarbonyl-cis-dihydrido-trans-bis(triphenylphosphite)iron(II)
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                102.148(15)
_cell_angle_beta                 94.667(15)
_cell_angle_gamma                107.402(14)
_cell_formula_units_Z            2
_cell_length_a                   9.6397(12)
_cell_length_b                   10.4410(13)
_cell_length_c                   18.381(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_volume                     1705.0(4)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '(1.60 - 26.1)'
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'rotation en phi'
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16806
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         6202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0452P)²+0.0246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                5084
_reflns_number_total             6202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006899.cif
_cod_data_source_block           FeH2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '92-93 C' was changed to '365.6(5)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4319647
#BEGIN Tags that were not found in dictionaries:
_cell_measurement_2heta_min      3.3
_cell_measurement_2heta_max      52.1
#END Tags that were not found in dictionaries
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
Fe1 Fe 0.53170(2) 0.83647(3) 0.270681(12) 0.01966(8) Uani 1 1 d . . .
P1 P 0.35103(4) 0.72598(5) 0.18545(2) 0.01938(10) Uani 1 1 d . . .
P2 P 0.72487(4) 1.00380(5) 0.32211(2) 0.01925(10) Uani 1 1 d . . .
O1 O 0.30703(13) 0.79718(12) 0.12199(6) 0.0249(3) Uani 1 1 d . . .
O2 O 0.37127(12) 0.59233(13) 0.13060(6) 0.0229(3) Uani 1 1 d . . .
O3 O 0.18560(12) 0.66736(13) 0.20458(7) 0.0241(3) Uani 1 1 d . . .
O4 O 0.71946(13) 1.12306(13) 0.39192(6) 0.0249(3) Uani 1 1 d . . .
O5 O 0.84476(12) 0.95196(13) 0.36170(7) 0.0238(3) Uani 1 1 d . . .
O6 O 0.82077(13) 1.10514(13) 0.27692(6) 0.0250(3) Uani 1 1 d . . .
O7 O 0.40857(18) 0.8193(2) 0.41021(8) 0.0550(5) Uani 1 1 d . . .
O8 O 0.67909(16) 0.62692(16) 0.25559(9) 0.0415(4) Uani 1 1 d . . .
C1 C 0.32788(18) 0.93779(18) 0.13019(9) 0.0207(3) Uani 1 1 d . . .
C2 C 0.2251(2) 0.9927(2) 0.15922(10) 0.0276(4) Uani 1 1 d . . .
C3 C 0.2388(2) 1.1292(2) 0.15974(11) 0.0359(5) Uani 1 1 d . . .
C4 C 0.3546(2) 1.2083(2) 0.13214(12) 0.0366(5) Uani 1 1 d . . .
C5 C 0.4575(2) 1.1512(2) 0.10381(12) 0.0331(5) Uani 1 1 d . . .
C6 C 0.44538(19) 1.0153(2) 0.10291(10) 0.0266(4) Uani 1 1 d . . .
C7 C 0.29317(18) 0.53137(18) 0.05712(9) 0.0220(4) Uani 1 1 d . . .
C8 C 0.3625(2) 0.5674(2) -0.00199(11) 0.0314(4) Uani 1 1 d . . .
C9 C 0.2890(3) 0.5051(2) -0.07499(11) 0.0380(5) Uani 1 1 d . . .
C10 C 0.1485(2) 0.4101(2) -0.08762(11) 0.0359(5) Uani 1 1 d . . .
C11 C 0.0824(2) 0.3760(2) -0.02780(12) 0.0357(5) Uani 1 1 d . . .
C12 C 0.1546(2) 0.4356(2) 0.04578(11) 0.0292(4) Uani 1 1 d . . .
C13 C 0.14859(17) 0.58849(18) 0.25723(9) 0.0220(4) Uani 1 1 d . . .
C14 C 0.0356(2) 0.6067(2) 0.29560(11) 0.0305(4) Uani 1 1 d . . .
C15 C -0.0105(2) 0.5279(2) 0.34650(12) 0.0377(5) Uani 1 1 d . . .
C16 C 0.0558(2) 0.4328(2) 0.35942(11) 0.0352(5) Uani 1 1 d . . .
C17 C 0.1680(2) 0.4155(2) 0.32060(11) 0.0326(4) Uani 1 1 d . . .
C18 C 0.21533(19) 0.4929(2) 0.26890(11) 0.0274(4) Uani 1 1 d . . .
C19 C 0.67114(17) 1.23528(18) 0.38984(9) 0.0221(4) Uani 1 1 d . . .
C20 C 0.69973(19) 1.3331(2) 0.45773(10) 0.0263(4) Uani 1 1 d . . .
C21 C 0.6532(2) 1.4470(2) 0.46161(11) 0.0329(4) Uani 1 1 d . . .
C22 C 0.5795(2) 1.4639(2) 0.39844(12) 0.0340(4) Uani 1 1 d . . .
C23 C 0.5529(2) 1.3657(2) 0.33077(11) 0.0306(4) Uani 1 1 d . . .
C24 C 0.59877(19) 1.2511(2) 0.32574(10) 0.0261(4) Uani 1 1 d . . .
C25 C 0.99054(18) 1.03592(19) 0.39249(10) 0.0239(4) Uani 1 1 d . . .
C26 C 1.0999(2) 1.0150(2) 0.35263(12) 0.0343(4) Uani 1 1 d . . .
C27 C 1.2456(2) 1.0867(3) 0.38462(15) 0.0463(6) Uani 1 1 d . . .
C28 C 1.2785(2) 1.1760(2) 0.45505(14) 0.0442(6) Uani 1 1 d . . .
C29 C 1.1675(2) 1.1958(2) 0.49388(12) 0.0382(5) Uani 1 1 d . . .
C30 C 1.0207(2) 1.1253(2) 0.46260(11) 0.0291(4) Uani 1 1 d . . .
C31 C 0.82818(17) 1.08482(19) 0.20015(9) 0.0208(4) Uani 1 1 d . . .
C32 C 0.83567(18) 0.9632(2) 0.15684(10) 0.0253(4) Uani 1 1 d . . .
C33 C 0.8457(2) 0.9531(2) 0.08085(10) 0.0305(4) Uani 1 1 d . . .
C34 C 0.8499(2) 1.0638(2) 0.05012(10) 0.0324(5) Uani 1 1 d . . .
C35 C 0.84411(19) 1.1853(2) 0.09465(11) 0.0301(4) Uani 1 1 d . . .
C36 C 0.83321(18) 1.1976(2) 0.17073(10) 0.0254(4) Uani 1 1 d . . .
C37 C 0.4560(2) 0.8231(2) 0.35551(10) 0.0318(4) Uani 1 1 d . . .
C38 C 0.61916(19) 0.7077(2) 0.26269(10) 0.0267(4) Uani 1 1 d . . .
H100 H 0.470(2) 0.945(2) 0.2676(12) 0.041(6) Uiso 1 1 d . . .
H200 H 0.577(2) 0.872(2) 0.2039(12) 0.036(6) Uiso 1 1 d . . .
H2 H 0.145(2) 0.934(2) 0.1776(12) 0.036(6) Uiso 1 1 d . . .
H3 H 0.164(3) 1.164(3) 0.1779(14) 0.048(7) Uiso 1 1 d . . .
H4 H 0.364(2) 1.302(3) 0.1320(12) 0.035(6) Uiso 1 1 d . . .
H5 H 0.535(3) 1.203(3) 0.0871(13) 0.045(6) Uiso 1 1 d . . .
H6 H 0.511(2) 0.974(2) 0.0804(12) 0.035(6) Uiso 1 1 d . . .
H8 H 0.459(3) 0.633(3) 0.0081(12) 0.039(6) Uiso 1 1 d . . .
H9 H 0.337(3) 0.527(3) -0.1176(14) 0.048(7) Uiso 1 1 d . . .
H10 H 0.103(2) 0.375(2) -0.1367(13) 0.038(6) Uiso 1 1 d . . .
H11 H -0.017(3) 0.310(3) -0.0354(14) 0.059(8) Uiso 1 1 d . . .
H12 H 0.110(2) 0.410(2) 0.0870(12) 0.029(5) Uiso 1 1 d . . .
H14 H -0.005(3) 0.675(3) 0.2864(13) 0.043(6) Uiso 1 1 d . . .
H15 H -0.091(3) 0.541(3) 0.3733(13) 0.044(6) Uiso 1 1 d . . .
H16 H 0.025(3) 0.379(3) 0.3942(14) 0.050(7) Uiso 1 1 d . . .
H17 H 0.213(3) 0.349(3) 0.3288(13) 0.044(6) Uiso 1 1 d . . .
H18 H 0.287(2) 0.477(2) 0.2401(12) 0.034(6) Uiso 1 1 d . . .
H20 H 0.753(2) 1.319(2) 0.5006(12) 0.033(5) Uiso 1 1 d . . .
H21 H 0.672(2) 1.509(3) 0.5069(14) 0.041(6) Uiso 1 1 d . . .
H22 H 0.548(2) 1.537(3) 0.4021(13) 0.040(6) Uiso 1 1 d . . .
H23 H 0.499(2) 1.376(2) 0.2851(13) 0.037(6) Uiso 1 1 d . . .
H24 H 0.583(2) 1.188(2) 0.2778(13) 0.034(6) Uiso 1 1 d . . .
H26 H 1.074(2) 0.950(3) 0.3052(13) 0.038(6) Uiso 1 1 d . . .
H27 H 1.321(3) 1.072(3) 0.3586(14) 0.054(7) Uiso 1 1 d . . .
H28 H 1.383(3) 1.225(3) 0.4776(15) 0.061(8) Uiso 1 1 d . . .
H29 H 1.187(2) 1.257(3) 0.5421(13) 0.039(6) Uiso 1 1 d . . .
H30 H 0.944(2) 1.136(2) 0.4887(12) 0.030(5) Uiso 1 1 d . . .
H32 H 0.834(2) 0.883(3) 0.1776(12) 0.038(6) Uiso 1 1 d . . .
H33 H 0.852(2) 0.872(3) 0.0533(13) 0.041(6) Uiso 1 1 d . . .
H34 H 0.855(3) 1.053(3) -0.0018(14) 0.047(7) Uiso 1 1 d . . .
H35 H 0.849(2) 1.265(3) 0.0758(13) 0.037(6) Uiso 1 1 d . . .
H36 H 0.829(2) 1.282(2) 0.2005(11) 0.027(5) 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'
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
H200 Fe1 H100 79.1(13) . . ?
H200 Fe1 C38 92.6(9) . . ?
H100 Fe1 C38 171.7(9) . . ?
H200 Fe1 C37 166.6(9) . . ?
H100 Fe1 C37 87.5(9) . . ?
C38 Fe1 C37 100.77(9) . . ?
H200 Fe1 P1 74.7(8) . . ?
H100 Fe1 P1 80.9(9) . . ?
C38 Fe1 P1 97.53(6) . . ?
C37 Fe1 P1 103.46(6) . . ?
H200 Fe1 P2 82.5(8) . . ?
H100 Fe1 P2 83.5(9) . . ?
C38 Fe1 P2 95.04(6) . . ?
C37 Fe1 P2 95.99(6) . . ?
P1 Fe1 P2 154.35(2) . . ?
O1 P1 O2 98.13(7) . . ?
O1 P1 O3 95.65(6) . . ?
O2 P1 O3 103.33(7) . . ?
O1 P1 Fe1 120.19(5) . . ?
O2 P1 Fe1 113.79(5) . . ?
O3 P1 Fe1 121.71(5) . . ?
O5 P2 O6 102.56(7) . . ?
O5 P2 O4 98.99(7) . . ?
O6 P2 O4 96.52(7) . . ?
O5 P2 Fe1 111.33(5) . . ?
O6 P2 Fe1 123.23(5) . . ?
O4 P2 Fe1 120.30(5) . . ?
C1 O1 P1 126.65(10) . . ?
C7 O2 P1 123.50(11) . . ?
C13 O3 P1 124.16(10) . . ?
C19 O4 P2 127.79(10) . . ?
C25 O5 P2 124.54(11) . . ?
C31 O6 P2 130.04(11) . . ?
C2 C1 C6 121.79(17) . . ?
C2 C1 O1 119.49(16) . . ?
C6 C1 O1 118.49(16) . . ?
C1 C2 C3 118.95(18) . . ?
C4 C3 C2 120.2(2) . . ?
C3 C4 C5 119.82(19) . . ?
C4 C5 C6 120.61(19) . . ?
C1 C6 C5 118.57(18) . . ?
C12 C7 C8 122.11(16) . . ?
C12 C7 O2 120.12(16) . . ?
C8 C7 O2 117.73(15) . . ?
C7 C8 C9 118.55(18) . . ?
C10 C9 C8 120.3(2) . . ?
C11 C10 C9 119.93(17) . . ?
C10 C11 C12 120.84(18) . . ?
C7 C12 C11 118.28(19) . . ?
C18 C13 C14 120.84(17) . . ?
C18 C13 O3 122.84(16) . . ?
C14 C13 O3 116.27(16) . . ?
C13 C14 C15 119.25(19) . . ?
C16 C15 C14 120.73(19) . . ?
C15 C16 C17 119.37(19) . . ?
C16 C17 C18 120.8(2) . . ?
C13 C18 C17 118.95(18) . . ?
C20 C19 C24 120.98(17) . . ?
C20 C19 O4 115.05(15) . . ?
C24 C19 O4 123.97(16) . . ?
C21 C20 C19 119.29(17) . . ?
C20 C21 C22 120.59(18) . . ?
C21 C22 C23 119.4(2) . . ?
C24 C23 C22 120.86(18) . . ?
C23 C24 C19 118.88(17) . . ?
C30 C25 C26 122.20(17) . . ?
C30 C25 O5 120.33(16) . . ?
C26 C25 O5 117.21(17) . . ?
C25 C26 C27 118.7(2) . . ?
C28 C27 C26 120.2(2) . . ?
C29 C28 C27 120.24(19) . . ?
C28 C29 C30 120.5(2) . . ?
C25 C30 C29 118.3(2) . . ?
C32 C31 C36 121.99(16) . . ?
C32 C31 O6 122.53(16) . . ?
C36 C31 O6 115.44(16) . . ?
C31 C32 C33 118.58(18) . . ?
C34 C33 C32 120.5(2) . . ?
C35 C34 C33 120.06(18) . . ?
C34 C35 C36 120.47(18) . . ?
C31 C36 C35 118.41(19) . . ?
O7 C37 Fe1 177.7(2) . . ?
O8 C38 Fe1 177.25(17) . . ?
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 H200 1.42(2) . ?
Fe1 H100 1.44(2) . ?
Fe1 C38 1.776(2) . ?
Fe1 C37 1.789(2) . ?
Fe1 P1 2.1004(7) . ?
Fe1 P2 2.1180(7) . ?
P1 O1 1.6020(12) . ?
P1 O2 1.6139(14) . ?
P1 O3 1.6246(12) . ?
P2 O5 1.6004(12) . ?
P2 O6 1.6044(12) . ?
P2 O4 1.6053(13) . ?
O1 C1 1.394(2) . ?
O2 C7 1.4079(19) . ?
O3 C13 1.399(2) . ?
O4 C19 1.391(2) . ?
O5 C25 1.410(2) . ?
O6 C31 1.393(2) . ?
O7 C37 1.141(2) . ?
O8 C38 1.149(2) . ?
C1 C2 1.376(3) . ?
C1 C6 1.380(2) . ?
C2 C3 1.389(3) . ?
C3 C4 1.379(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.385(3) . ?
C7 C12 1.376(3) . ?
C7 C8 1.382(3) . ?
C8 C9 1.389(3) . ?
C9 C10 1.386(3) . ?
C10 C11 1.373(3) . ?
C11 C12 1.391(3) . ?
C13 C18 1.381(3) . ?
C13 C14 1.383(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.379(3) . ?
C16 C17 1.379(3) . ?
C17 C18 1.392(3) . ?
C19 C20 1.384(3) . ?
C19 C24 1.385(2) . ?
C20 C21 1.381(3) . ?
C21 C22 1.383(3) . ?
C22 C23 1.385(3) . ?
C23 C24 1.382(3) . ?
C25 C30 1.374(3) . ?
C25 C26 1.376(3) . ?
C26 C27 1.389(3) . ?
C27 C28 1.376(4) . ?
C28 C29 1.376(4) . ?
C29 C30 1.393(3) . ?
C31 C32 1.375(3) . ?
C31 C36 1.385(3) . ?
C32 C33 1.392(3) . ?
C33 C34 1.381(3) . ?
C34 C35 1.377(3) . ?
C35 C36 1.393(3) . ?
