#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/78/2227821.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_2227821
loop_
_publ_author_name
'Reiss, Guido J.'
_publ_section_title
;
 Redetermination of
 (η⁴-s-cis-1,3-butadiene)tricarbonyliron(0)
;
_journal_coeditor_code           NC2198
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1369
_journal_paper_doi               10.1107/S1600536810039218
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Fe (C4 H6) (C O)3]'
_chemical_formula_moiety         'C7 H6 Fe O3'
_chemical_formula_sum            'C7 H6 Fe O3'
_chemical_formula_weight         193.97
_chemical_name_systematic
;
(η⁴-s-cis-1,3-butadiene)tricarbonyliron(0)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4323(6)
_cell_length_b                   10.9146(6)
_cell_length_c                   6.1664(4)
_cell_measurement_reflns_used    10152
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      31.0976
_cell_measurement_theta_min      3.2957
_cell_volume                     769.44(8)
_computing_cell_refinement
;
CrysAlisPro (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlisPro (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis ro (Oxford Diffraction, 2009)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       ω
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0070
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13021
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         3.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis Pro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.02P)²+0.3P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0395
_refine_ls_wR_factor_ref         0.0399
_reflns_number_gt                1131
_reflns_number_total             1177
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            nc2198.cif
_cod_data_source_block           I
_cod_database_code               2227821
_cod_database_fobs_code          2227821
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_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
Fe Fe 0.422257(14) 0.2500 0.10001(3) 0.01195(6) Uani d S 1 . .
C C1 0.40416(9) 0.31478(9) 0.41329(14) 0.02025(18) Uani d . 1 . .
H H1 0.3372(11) 0.3551(12) 0.451(2) 0.025(3) Uiso d . 1 . .
C C2 0.50116(10) 0.37495(11) 0.31685(16) 0.0293(2) Uani d . 1 . .
H H2A 0.4931(13) 0.4628(14) 0.294(2) 0.039(4) Uiso d . 1 . .
H H2B 0.5783(12) 0.3456(14) 0.346(2) 0.033(4) Uiso d . 1 . .
C C3 0.54866(12) 0.2500 -0.0711(2) 0.0220(2) Uani d S 1 . .
O O3 0.63206(10) 0.2500 -0.1730(2) 0.0381(3) Uani d S 1 . .
C C4 0.33599(8) 0.36948(8) -0.02057(14) 0.01764(16) Uani d . 1 . .
O O4 0.28356(7) 0.44729(7) -0.09743(12) 0.02909(17) Uani d . 1 . .
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 0.01180(8) 0.01336(9) 0.01068(9) 0.000 0.00004(5) 0.000
C1 0.0273(4) 0.0212(4) 0.0123(4) -0.0003(3) -0.0005(3) -0.0032(3)
C2 0.0371(5) 0.0323(5) 0.0185(4) -0.0166(4) -0.0030(4) -0.0046(4)
C3 0.0174(5) 0.0313(7) 0.0174(5) 0.000 -0.0004(4) 0.000
O3 0.0198(5) 0.0651(8) 0.0294(6) 0.000 0.0089(4) 0.000
C4 0.0198(4) 0.0180(4) 0.0151(4) 0.0000(3) 0.0025(3) 0.0001(3)
O4 0.0338(4) 0.0254(4) 0.0280(4) 0.0108(3) 0.0010(3) 0.0072(3)
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_
_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
C4 Fe C4 8_565 . 93.11(6) ?
C4 Fe C3 8_565 . 101.50(4) ?
C4 Fe C3 . . 101.50(4) ?
C4 Fe C1 8_565 . 125.46(4) ?
C4 Fe C1 . . 94.79(4) ?
C3 Fe C1 . . 129.18(5) ?
C4 Fe C1 8_565 8_565 94.79(4) ?
C4 Fe C1 . 8_565 125.46(4) ?
C3 Fe C1 . 8_565 129.18(5) ?
C1 Fe C1 . 8_565 40.00(5) ?
C4 Fe C2 8_565 . 164.87(4) ?
C4 Fe C2 . . 91.59(4) ?
C3 Fe C2 . . 91.63(4) ?
C1 Fe C2 . . 39.69(4) ?
C1 Fe C2 8_565 . 70.86(4) ?
C4 Fe C2 8_565 8_565 91.59(4) ?
C4 Fe C2 . 8_565 164.87(4) ?
C3 Fe C2 . 8_565 91.63(4) ?
C1 Fe C2 . 8_565 70.86(4) ?
C1 Fe C2 8_565 8_565 39.69(4) ?
C2 Fe C2 . 8_565 80.43(7) ?
C2 C1 C1 . 8_565 117.56(6) ?
C2 C1 Fe . . 71.86(5) ?
C1 C1 Fe 8_565 . 70.00(3) ?
C2 C1 H1 . . 122.6(8) ?
C1 C1 H1 8_565 . 118.8(8) ?
Fe C1 H1 . . 119.0(8) ?
C1 C2 Fe . . 68.46(5) ?
C1 C2 H2A . . 116.3(9) ?
Fe C2 H2A . . 120.3(9) ?
C1 C2 H2B . . 119.2(9) ?
Fe C2 H2B . . 107.2(9) ?
H2A C2 H2B . . 116.4(13) ?
O3 C3 Fe . . 177.25(13) ?
O4 C4 Fe . . 178.28(8) ?
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 C4 8_565 1.7961(9) ?
Fe C4 . 1.7961(9) ?
Fe C3 . 1.7893(14) ?
Fe C1 . 2.0675(9) ?
Fe C1 8_565 2.0675(9) ?
Fe C2 . 2.1123(10) ?
Fe C2 8_565 2.1123(10) ?
C1 C2 . 1.4194(14) ?
C1 C1 8_565 1.4142(19) ?
C1 H1 . 0.912(13) ?
C2 H2A . 0.974(15) ?
C2 H2B . 0.955(14) ?
C3 O3 . 1.1418(18) ?
C4 O4 . 1.1425(11) ?
