#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:31:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179451 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/48/4334857.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_4334857
loop_
_publ_author_name
'Luca Rigamonti'
'Marco Piccioli'
'Luigi Malavolti'
'Lorenzo Poggini'
'Matteo Mannini'
'Federico Totti'
'Brunetto Cortigiani'
'Agnese Magnani'
'Roberta Sessoli'
'Andrea Cornia'
_publ_contact_author             'Cornia, Andrea'
_publ_contact_author_email       acornia@unimore.it
_publ_section_title
;
 Enhanced Vapor-Phase Processing in Fluorinated Fe4 Single-Molecule
 Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5897
_journal_page_last               5905
_journal_paper_doi               10.1021/ic400037c
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        synthesis
_chemical_formula_iupac          '[Fe2(C2H5O)2(C8H10F3O2)4]'
_chemical_formula_moiety         'C36 H50 F12 Fe2 O10'
_chemical_formula_sum            'C36 H50 F12 Fe2 O10'
_chemical_formula_weight         982.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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-97
_cell_angle_alpha                67.7850(14)
_cell_angle_beta                 89.1974(15)
_cell_angle_gamma                80.9034(15)
_cell_formula_units_Z            1
_cell_length_a                   8.7808(4)
_cell_length_b                   10.5584(4)
_cell_length_c                   13.6098(6)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.11
_cell_volume                     1151.98(9)
_computing_cell_refinement       'Bruker-Nonius X8APEX package'
_computing_data_collection       'Bruker-Nonius X8APEX package'
_computing_data_reduction        'Bruker-Nonius X8APEX package'
_computing_molecular_graphics    'MERCURY (Macrae, 2008)'
_computing_publication_material
'WINGX publication routines v1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8APEX four-circle diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23381
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.8450
_exptl_absorpt_correction_T_min  0.7501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS - Bruker Nonius area detector scaling 
and absorption correction - V2.10
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       blocks
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0368
_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)+(0.0567P)²+0.5799P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                4424
_reflns_number_total             5257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400037c_si_002.cif
_cod_data_source_block           120112mpa_2_work4
_cod_database_code               4334857
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
Fe1 Fe 0.49245(3) 0.06209(3) 0.37831(2) 0.02625(9) Uani 1 1 d .
O1 O 0.62516(14) 0.03699(13) 0.50013(10) 0.0267(3) Uani 1 1 d .
O2 O 0.61272(16) -0.10466(14) 0.35839(11) 0.0341(3) Uani 1 1 d .
O3 O 0.34039(16) 0.06438(15) 0.26837(11) 0.0346(3) Uani 1 1 d .
O4 O 0.61966(16) 0.17938(15) 0.26954(11) 0.0350(3) Uani 1 1 d .
O5 O 0.35719(15) 0.24236(13) 0.36466(10) 0.0296(3) Uani 1 1 d .
F1 F 0.85248(19) -0.2460(2) 0.2982(2) 0.1004(8) Uani 1 1 d .
F2 F 0.7021(3) -0.3079(2) 0.20880(15) 0.0936(7) Uani 1 1 d .
F3 F 0.6992(2) -0.38100(16) 0.37434(15) 0.0768(5) Uani 1 1 d .
F4 F 0.6614(2) 0.48987(17) 0.06229(15) 0.0798(6) Uani 1 1 d .
F5 F 0.83782(19) 0.3354(2) 0.16736(17) 0.0837(6) Uani 1 1 d .
F6 F 0.7040(2) 0.28578(19) 0.06216(14) 0.0768(5) Uani 1 1 d .
C1 C 0.7831(2) 0.0535(3) 0.50162(19) 0.0410(5) Uani 1 1 d .
C2 C 0.7955(4) 0.1882(4) 0.5115(3) 0.0717(9) Uani 1 1 d .
H2A H 0.7411 0.2652 0.4503 0.108 Uiso 1 1 calc R
H2B H 0.9045 0.1976 0.5138 0.108 Uiso 1 1 calc R
H2C H 0.7489 0.1899 0.5770 0.108 Uiso 1 1 calc R
C3 C 0.7131(3) -0.2696(2) 0.28953(19) 0.0448(5) Uani 1 1 d .
C4 C 0.5907(2) -0.1463(2) 0.28498(16) 0.0327(4) Uani 1 1 d .
C5 C 0.4735(3) -0.0991(2) 0.20703(17) 0.0364(4) Uani 1 1 d .
C6 C 0.3504(2) 0.0058(2) 0.20272(15) 0.0314(4) Uani 1 1 d .
C7 C 0.2167(3) 0.0554(2) 0.11943(18) 0.0417(5) Uani 1 1 d .
C8 C 0.2354(3) -0.0162(3) 0.0401(2) 0.0596(7) Uani 1 1 d .
H8A H 0.3339 -0.0031 0.0060 0.089 Uiso 1 1 calc R
H8B H 0.1504 0.0241 -0.0142 0.089 Uiso 1 1 calc R
H8C H 0.2339 -0.1156 0.0775 0.089 Uiso 1 1 calc R
C9 C 0.0685(3) 0.0262(4) 0.1787(2) 0.0639(8) Uani 1 1 d .
H9A H 0.0746 -0.0740 0.2170 0.096 Uiso 1 1 calc R
H9B H -0.0205 0.0616 0.1275 0.096 Uiso 1 1 calc R
H9C H 0.0566 0.0724 0.2293 0.096 Uiso 1 1 calc R
C10 C 0.2093(4) 0.2119(3) 0.0601(2) 0.0725(10) Uani 1 1 d .
H10A H 0.1907 0.2584 0.1104 0.109 Uiso 1 1 calc R
H10B H 0.1251 0.2474 0.0053 0.109 Uiso 1 1 calc R
H10C H 0.3074 0.2302 0.0267 0.109 Uiso 1 1 calc R
C11 C 0.6962(3) 0.3557(3) 0.1248(2) 0.0513(6) Uani 1 1 d .
C12 C 0.5819(2) 0.3069(2) 0.21124(16) 0.0332(4) Uani 1 1 d .
C13 C 0.4569(3) 0.3990(2) 0.21608(18) 0.0386(5) Uani 1 1 d .
C14 C 0.3468(2) 0.36229(19) 0.29491(15) 0.0291(4) Uani 1 1 d .
C15 C 0.2106(2) 0.4699(2) 0.29845(17) 0.0354(4) Uani 1 1 d .
C16 C 0.0939(3) 0.3991(3) 0.3747(2) 0.0558(7) Uani 1 1 d .
H16A H 0.0535 0.3348 0.3494 0.084 Uiso 1 1 calc R
H16B H 0.0088 0.4692 0.3783 0.084 Uiso 1 1 calc R
H16C H 0.1443 0.3476 0.4456 0.084 Uiso 1 1 calc R
C17 C 0.1319(3) 0.5483(3) 0.1876(2) 0.0596(7) Uani 1 1 d .
H17A H 0.1000 0.4821 0.1608 0.089 Uiso 1 1 calc R
H17B H 0.2043 0.6003 0.1396 0.089 Uiso 1 1 calc R
H17C H 0.0409 0.6129 0.1917 0.089 Uiso 1 1 calc R
C18 C 0.2727(4) 0.5704(3) 0.3371(3) 0.0650(8) Uani 1 1 d .
H18A H 0.1869 0.6386 0.3427 0.098 Uiso 1 1 calc R
H18B H 0.3452 0.6183 0.2866 0.098 Uiso 1 1 calc R
H18C H 0.3261 0.5190 0.4070 0.098 Uiso 1 1 calc R
H1 H 0.480(3) -0.138(3) 0.162(2) 0.043(7) Uiso 1 1 d .
H2 H 0.443(3) 0.486(3) 0.165(2) 0.057(8) Uiso 1 1 d .
H4 H 0.836(3) -0.029(3) 0.560(2) 0.043(7) Uiso 1 1 d .
H5 H 0.828(3) 0.046(3) 0.439(2) 0.043(7) 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'
F F 0.0171 0.0103 '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
O1 Fe1 O1 77.24(6) . 2_656
O1 Fe1 O4 95.51(6) . .
O1 Fe1 O4 170.64(6) 2_656 .
O1 Fe1 O3 171.21(6) . .
O1 Fe1 O3 94.45(6) 2_656 .
O4 Fe1 O3 93.05(6) . .
O1 Fe1 O2 92.59(5) . .
O1 Fe1 O2 97.97(6) 2_656 .
O4 Fe1 O2 88.16(6) . .
O3 Fe1 O2 85.67(6) . .
O1 Fe1 O5 98.97(5) . .
O1 Fe1 O5 89.24(5) 2_656 .
O4 Fe1 O5 86.04(6) . .
O3 Fe1 O5 83.60(6) . .
O2 Fe1 O5 167.51(6) . .
C1 O1 Fe1 128.14(12) . .
C1 O1 Fe1 127.38(12) . 2_656
Fe1 O1 Fe1 102.76(6) . 2_656
C4 O2 Fe1 126.67(13) . .
C6 O3 Fe1 131.92(13) . .
C12 O4 Fe1 126.72(13) . .
C14 O5 Fe1 131.33(12) . .
O1 C1 C2 110.2(2) . .
O1 C1 H4 106.0(15) . .
C2 C1 H4 114.8(15) . .
O1 C1 H5 108.7(15) . .
C2 C1 H5 112.9(15) . .
H4 C1 H5 104(2) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
F1 C3 F2 109.4(2) . .
F1 C3 F3 105.6(2) . .
F2 C3 F3 104.7(2) . .
F1 C3 C4 111.7(2) . .
F2 C3 C4 114.0(2) . .
F3 C3 C4 110.77(19) . .
O2 C4 C5 129.23(19) . .
O2 C4 C3 112.29(18) . .
C5 C4 C3 118.46(19) . .
C4 C5 C6 121.89(19) . .
C4 C5 H1 115.5(17) . .
C6 C5 H1 122.6(17) . .
O3 C6 C5 122.62(18) . .
O3 C6 C7 114.87(18) . .
C5 C6 C7 122.50(18) . .
C6 C7 C8 113.1(2) . .
C6 C7 C10 107.19(19) . .
C8 C7 C10 109.5(2) . .
C6 C7 C9 107.44(19) . .
C8 C7 C9 109.6(2) . .
C10 C7 C9 109.9(3) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
F6 C11 F5 106.7(2) . .
F6 C11 F4 106.7(2) . .
F5 C11 F4 107.2(2) . .
F6 C11 C12 111.3(2) . .
F5 C11 C12 110.8(2) . .
F4 C11 C12 113.80(19) . .
O4 C12 C13 128.99(19) . .
O4 C12 C11 111.87(18) . .
C13 C12 C11 119.14(19) . .
C12 C13 C14 122.54(19) . .
C12 C13 H2 118.0(18) . .
C14 C13 H2 119.4(18) . .
O5 C14 C13 122.11(18) . .
O5 C14 C15 117.30(17) . .
C13 C14 C15 120.58(17) . .
C16 C15 C18 109.6(2) . .
C16 C15 C14 110.05(17) . .
C18 C15 C14 107.88(19) . .
C16 C15 C17 109.2(2) . .
C18 C15 C17 110.0(2) . .
C14 C15 C17 110.16(17) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Fe1 3.0630(5) 2_656
Fe1 O1 1.9497(13) .
Fe1 O1 1.9706(13) 2_656
Fe1 O4 1.9943(14) .
Fe1 O3 2.0102(14) .
Fe1 O2 2.0133(13) .
Fe1 O5 2.0229(13) .
O1 C1 1.426(2) .
O1 Fe1 1.9706(13) 2_656
O2 C4 1.263(2) .
O3 C6 1.260(2) .
O4 C12 1.269(2) .
O5 C14 1.253(2) .
F1 C3 1.303(3) .
F2 C3 1.316(3) .
F3 C3 1.321(3) .
F4 C11 1.335(3) .
F5 C11 1.330(3) .
F6 C11 1.318(3) .
C1 C2 1.499(4) .
C1 H4 0.98(3) .
C1 H5 0.96(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.533(3) .
C4 C5 1.379(3) .
C5 C6 1.404(3) .
C5 H1 0.85(3) .
C6 C7 1.527(3) .
C7 C8 1.529(3) .
C7 C10 1.532(3) .
C7 C9 1.532(4) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.526(3) .
C12 C13 1.365(3) .
C13 C14 1.418(3) .
C13 H2 0.91(3) .
C14 C15 1.528(3) .
C15 C16 1.521(3) .
C15 C18 1.521(4) .
C15 C17 1.530(3) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
