#------------------------------------------------------------------------------
#$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $
#$Revision: 32112 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/81/2008111.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_2008111
loop_
_publ_author_name
'Boese, Roland'
'Roth, Wolfgang R.'
'Bl\"aser, Dieter'
'Latz, R\"udiger'
'B\"aumen, Anja'
_publ_section_title
;
 Tricarbonyl[(2,3,6,7-\h)-2,3-dimethylene-2,3-dihydrofuran]iron(0) at
 120K
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800082
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Fe (C6 H6 O1) (CO)3]'
_chemical_formula_moiety         'C9 H6 Fe O4'
_chemical_formula_sum            'C9 H6 Fe O4'
_chemical_formula_weight         233.99
_chemical_name_systematic
;
 Tricarbonyl(2,3,6,7-\h)-(2,3-diylidenfurane)-iron(0)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 108.866(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2502(16)
_cell_length_b                   6.5155(11)
_cell_length_c                   12.415(2)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     937.7(3)
_computing_cell_refinement       P3-VMS
_computing_data_collection       'P3-VMS (Siemens 1987)'
_computing_data_reduction        'XPLAT in P3-VMS'
_computing_molecular_graphics    SHELXL97
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1984)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device_type  'Nicolet R3m/V four-circle'
_diffrn_measurement_method       'Wyckoff scan mode'
_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  0.012
_diffrn_reflns_av_sigmaI/netI    0.014
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1777
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ' ?'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylindrical
_exptl_crystal_F_000             472
_exptl_crystal_size_max          3.0
_exptl_crystal_size_rad          0.15
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.030
_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/[\s^2^(Fo^2^)+(0.0363P)^2^+1.0554P] where P = (Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.081
_reflns_number_gt                1590
_reflns_number_total             1658
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    qa0078.cif
_[local]_cod_data_source_block   qa0078
_[local]_cod_cif_authors_sg_H-M  'P 2/n'
_cod_database_code               2008111
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, 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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe 0.20218(3) 0.28114(5) -0.00747(3) 0.02488(15) Uani d . 1 . . Fe
O1 0.32671(17) -0.0996(3) -0.06149(19) 0.0455(5) Uani d . 1 . . O
O2 0.00790(16) 0.0182(3) -0.13197(18) 0.0472(5) Uani d . 1 . . O
O3 0.11419(19) 0.4934(4) 0.15598(18) 0.0534(6) Uani d . 1 . . O
O4 0.13983(17) 0.5821(3) -0.19320(16) 0.0397(5) Uani d . 1 . . O
C2 0.3258(2) 0.0487(4) 0.0162(2) 0.0296(6) Uani d . 1 . . C
C3 0.37206(19) 0.2340(4) -0.0086(2) 0.0250(5) Uani d . 1 . . C
C4 0.4022(2) 0.1904(5) -0.1101(2) 0.0352(6) Uani d . 1 . . C
H4 0.4352 0.2837 -0.1509 0.042 Uiso d R 1 . . H
C5 0.3744(2) -0.0074(5) -0.1354(2) 0.0418(7) Uani d . 1 . . C
H5 0.3867 -0.0766 -0.1988 0.050 Uiso d R 1 . . H
C6 0.2742(2) 0.0336(5) 0.1024(2) 0.0384(7) Uani d . 1 . . C
H6A 0.2250 -0.0827 0.0989 0.046 Uiso d R 1 . . H
H6B 0.3217 0.0680 0.1783 0.046 Uiso d R 1 . . H
C7 0.3675(2) 0.4102(4) 0.0578(2) 0.0318(6) Uani d . 1 . . C
H7A 0.4050 0.3993 0.1385 0.038 Uiso d R 1 . . H
H7B 0.3789 0.5405 0.0270 0.038 Uiso d R 1 . . H
C8 0.0829(2) 0.1199(4) -0.0830(2) 0.0323(6) Uani d . 1 . . C
C9 0.1470(2) 0.4099(5) 0.0918(2) 0.0364(6) Uani d . 1 . . C
C10 0.1652(2) 0.4659(4) -0.1207(2) 0.0289(5) Uani d . 1 . . C
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Fe 0.0158(2) 0.0267(2) 0.0278(2) 0.00123(13) 0.00102(15) 0.00393(14)
O1 0.0313(10) 0.0312(10) 0.0620(13) 0.0038(8) -0.0017(9) -0.0055(10)
O2 0.0274(10) 0.0512(13) 0.0556(13) -0.0144(10) 0.0034(9) -0.0016(11)
O3 0.0425(12) 0.0760(17) 0.0410(11) 0.0225(12) 0.0126(10) -0.0014(11)
O4 0.0431(11) 0.0314(10) 0.0346(10) 0.0012(9) -0.0012(8) 0.0080(9)
C2 0.0173(11) 0.0261(13) 0.0370(13) 0.0024(10) -0.0027(10) 0.0038(11)
C3 0.0116(10) 0.0284(13) 0.0284(12) -0.0007(9) -0.0029(9) 0.0024(10)
C4 0.0153(12) 0.0580(18) 0.0291(13) 0.0063(11) 0.0025(10) 0.0129(13)
C5 0.0286(14) 0.0489(18) 0.0378(15) 0.0117(13) -0.0032(12) -0.0126(13)
C6 0.0251(13) 0.0414(16) 0.0447(15) 0.0041(11) 0.0060(11) 0.0209(13)
C7 0.0198(12) 0.0331(14) 0.0337(13) -0.0028(10) -0.0034(10) -0.0012(11)
C8 0.0211(12) 0.0361(14) 0.0370(14) 0.0025(11) 0.0056(11) 0.0054(12)
C9 0.0252(12) 0.0449(16) 0.0340(14) 0.0092(12) 0.0027(11) 0.0066(13)
C10 0.0213(12) 0.0257(13) 0.0341(13) 0.0011(10) 0.0012(10) -0.0030(11)
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 C9 . 1.794(3) ?
Fe C10 . 1.794(3) ?
Fe C8 . 1.798(3) ?
Fe C2 . 2.095(3) ?
Fe C7 . 2.099(2) ?
Fe C3 . 2.108(2) ?
Fe C6 . 2.112(3) ?
O1 C2 . 1.368(3) ?
O1 C5 . 1.376(4) ?
O2 C8 . 1.136(3) ?
O3 C9 . 1.140(3) ?
O4 C10 . 1.140(3) ?
C2 C3 . 1.410(3) ?
C2 C6 . 1.411(4) ?
C3 C7 . 1.425(4) ?
C3 C4 . 1.452(4) ?
C4 C5 . 1.344(4) ?
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 -1 6
6 -1 1
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C9 Fe C10 99.72(12)
C9 Fe C8 102.05(12)
C10 Fe C8 91.52(11)
C9 Fe C2 131.11(11)
C10 Fe C2 125.68(11)
C8 Fe C2 94.56(11)
C9 Fe C7 94.47(12)
C10 Fe C7 90.09(11)
C8 Fe C7 162.87(11)
C2 Fe C7 70.83(10)
C9 Fe C3 131.63(11)
C10 Fe C3 95.30(10)
C8 Fe C3 123.30(11)
C2 Fe C3 39.19(9)
C7 Fe C3 39.59(10)
C9 Fe C6 94.86(12)
C10 Fe C6 164.85(11)
C8 Fe C6 89.43(12)
C2 Fe C6 39.20(11)
C7 Fe C6 84.66(11)
C3 Fe C6 71.70(10)
C2 O1 C5 105.3(2)
O1 C2 C3 110.8(2)
O1 C2 C6 126.4(2)
C3 C2 C6 122.4(2)
O1 C2 Fe 125.58(16)
C3 C2 Fe 70.91(14)
C6 C2 Fe 71.07(15)
C2 C3 C7 118.1(2)
C2 C3 C4 104.7(2)
C7 C3 C4 136.8(2)
C2 C3 Fe 69.89(14)
C7 C3 Fe 69.87(14)
C4 C3 Fe 124.25(16)
C5 C4 C3 105.9(3)
C4 C5 O1 113.1(3)
C2 C6 Fe 69.73(14)
C3 C7 Fe 70.55(14)
O2 C8 Fe 179.2(2)
O3 C9 Fe 178.6(3)
O4 C10 Fe 178.8(2)