#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/87/1518764.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_1518764
loop_
_publ_author_name
'Lieberman, Craig M.'
'Filatov, Alexander S.'
'Wei, Zheng'
'Rogachev, Andrey Yu.'
'Abakumov, Artem M.'
'Dikarev, Evgeny V.'
_publ_section_title
;
 Mixed-valent, heteroleptic homometallic diketonates as templates for the
 design of volatile heterometallic precursors
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              2835
_journal_paper_doi               10.1039/C4SC04002C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety
;
C35 H19 F30 Fe3 O14
;
_chemical_formula_sum            'C35 H19 F30 Fe3 O14'
_chemical_formula_weight         1401.05
_chemical_melting_point          ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_audit_update_record
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.848(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.934(3)
_cell_length_b                   13.481(2)
_cell_length_c                   17.739(3)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.16
_cell_volume                     5000.0(13)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21346
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.8524
_exptl_absorpt_correction_T_min  0.7473
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5851
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0422
_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)+(0.0563P)²+11.5693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                5035
_reflns_number_total             5851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc04002c2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 1518761--1518766.cif.
;
_cod_original_cell_volume        4999.8(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1518764
#BEGIN Tags that were not found in dictionaries:
_publcif_datablock.id            {3aa1466c-c655-48d4-8c5f-edb9801ab9c4}
#END Tags that were not found in dictionaries
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 0.17770(3) 0.2500 0.02158(12) Uani 1 2 d S . .
Fe2 Fe 0.123880(16) 0.31698(2) 0.30584(2) 0.02489(11) Uani 1 1 d . . .
O1 O -0.01675(9) 0.06750(12) 0.17542(9) 0.0276(4) Uani 1 1 d . . .
O2 O -0.02876(8) 0.26591(12) 0.16333(9) 0.0228(3) Uani 1 1 d . . .
O3 O 0.08856(8) 0.20326(12) 0.21962(9) 0.0251(3) Uani 1 1 d . . .
O4 O 0.15847(8) 0.20728(13) 0.37373(10) 0.0297(4) Uani 1 1 d . . .
O5 O 0.21716(9) 0.34114(14) 0.27849(11) 0.0338(4) Uani 1 1 d . A .
O6 O 0.13121(8) 0.44038(12) 0.37351(9) 0.0277(4) Uani 1 1 d . B .
O7 O 0.08541(8) 0.40919(12) 0.22488(9) 0.0276(4) Uani 1 1 d . . .
C2 C 0.06472(13) 0.5485(2) 0.14851(15) 0.0332(6) Uani 1 1 d . . .
C3 C -0.01401(11) -0.02516(18) 0.18352(13) 0.0254(5) Uani 1 1 d . . .
C4 C -0.00276(12) 0.26299(17) 0.09863(13) 0.0256(5) Uani 1 1 d . . .
C5 C 0.10544(13) 0.56617(19) 0.28327(15) 0.0311(5) Uani 1 1 d . B .
H5 H 0.1043 0.6358 0.2752 0.037 Uiso 1 1 calc R . .
C6 C 0.08626(11) 0.50240(18) 0.22487(14) 0.0269(5) Uani 1 1 d . . .
C7 C 0.12640(12) 0.52883(19) 0.35404(14) 0.0280(5) Uani 1 1 d . . .
C8 C 0.06045(12) 0.23176(19) 0.09057(14) 0.0289(5) Uani 1 1 d . . .
H8 H 0.0744 0.2253 0.0407 0.035 Uiso 1 1 calc R . .
C9 C 0.10417(12) 0.20962(18) 0.14925(14) 0.0281(5) Uani 1 1 d . . .
C10 C 0.22516(14) 0.1037(2) 0.44957(17) 0.0404(6) Uani 1 1 d . . .
C11 C -0.02730(14) -0.08274(19) 0.10996(15) 0.0335(6) Uani 1 1 d . . .
C12 C 0.27060(13) 0.2337(2) 0.36669(17) 0.0373(6) Uani 1 1 d . A .
H12 H 0.3115 0.2135 0.3867 0.045 Uiso 1 1 calc R . .
C13 C 0.21614(13) 0.18854(19) 0.39243(15) 0.0315(5) Uani 1 1 d . . .
C14 C 0.26627(12) 0.3078(2) 0.31227(16) 0.0333(6) Uani 1 1 d . . .
C15 C -0.04284(13) 0.2951(2) 0.03082(14) 0.0323(5) Uani 1 1 d . . .
H15A H -0.0780 0.2478 0.0215 0.048 Uiso 1 1 calc R . .
H15B H -0.0164 0.2972 -0.0132 0.048 Uiso 1 1 calc R . .
H15C H -0.0604 0.3612 0.0397 0.048 Uiso 1 1 calc R . .
C17 C 0.0000 -0.0766(2) 0.2500 0.0263(7) Uani 1 2 d S . .
H17 H 0.0000 -0.1470 0.2500 0.032 Uiso 1 2 calc SR . .
C18 C 0.17310(13) 0.1949(2) 0.13515(17) 0.0396(6) Uani 1 1 d . . .
H18A H 0.1966 0.2563 0.1468 0.059 Uiso 1 1 calc R . .
H18B H 0.1776 0.1775 0.0820 0.059 Uiso 1 1 calc R . .
H18C H 0.1904 0.1413 0.1674 0.059 Uiso 1 1 calc R . .
F1 F -0.08053(11) -0.05337(16) 0.07450(12) 0.0627(6) Uani 1 1 d . . .
F2 F -0.03024(11) -0.18000(12) 0.12111(11) 0.0528(5) Uani 1 1 d . . .
F3 F 0.02039(11) -0.06683(15) 0.06384(10) 0.0567(5) Uani 1 1 d . . .
F4 F 0.17761(9) 0.10050(15) 0.49688(11) 0.0528(5) Uani 1 1 d . . .
F5 F 0.22666(12) 0.01696(14) 0.41492(12) 0.0633(6) Uani 1 1 d . . .
F6 F 0.27969(9) 0.11335(15) 0.49180(10) 0.0529(5) Uani 1 1 d . . .
F10 F 0.01862(8) 0.49610(12) 0.11314(9) 0.0384(4) Uani 1 1 d . . .
F11 F 0.11363(9) 0.55272(16) 0.10354(9) 0.0509(5) Uani 1 1 d . . .
F12 F 0.04214(11) 0.64078(13) 0.15546(10) 0.0549(5) Uani 1 1 d . . .
C1 C 0.32885(14) 0.3573(2) 0.28896(19) 0.0425(7) Uani 1 1 d D A 1
F7 F 0.3343(4) 0.3430(7) 0.2130(4) 0.0410(16) Uiso 0.34 1 d PD A 1
F8 F 0.3285(3) 0.4523(4) 0.3051(5) 0.0272(13) Uiso 0.34 1 d PD A 1
F9 F 0.3812(3) 0.3145(5) 0.3278(4) 0.0321(12) Uiso 0.34 1 d PD A 1
F7X F 0.3284(4) 0.3750(6) 0.2125(4) 0.054(2) Uiso 0.33 1 d PD A 2
F8X F 0.3368(4) 0.4437(5) 0.3240(4) 0.049(2) Uiso 0.33 1 d PD A 2
F9X F 0.3806(3) 0.3039(4) 0.2991(4) 0.0381(14) Uiso 0.33 1 d PD A 2
F7Y F 0.3482(4) 0.3227(5) 0.2298(4) 0.052(2) Uiso 0.33 1 d PD A 3
F8Y F 0.3227(3) 0.4555(5) 0.2794(4) 0.051(2) Uiso 0.33 1 d PD A 3
F9Y F 0.3779(3) 0.3456(6) 0.3438(4) 0.062(2) Uiso 0.33 1 d PD A 3
C16 C 0.14567(14) 0.6024(2) 0.41693(16) 0.0375(6) Uani 1 1 d D B 1
F13 F 0.1424(4) 0.6977(3) 0.3981(3) 0.0217(11) Uiso 0.34 1 d PD B 1
F14 F 0.1076(4) 0.5847(6) 0.4771(4) 0.0312(17) Uiso 0.34 1 d PD B 1
F15 F 0.2112(3) 0.5780(5) 0.4377(4) 0.0230(12) Uiso 0.34 1 d PD B 1
F13X F 0.1601(3) 0.6956(4) 0.3841(3) 0.0369(17) Uiso 0.33 1 d PD B 2
F14X F 0.1016(3) 0.6134(5) 0.4635(4) 0.0478(19) Uiso 0.33 1 d PD B 2
F15X F 0.1977(3) 0.5849(5) 0.4550(3) 0.0305(14) Uiso 0.33 1 d PD B 2
F13Y F 0.1209(3) 0.6937(4) 0.4056(3) 0.0420(18) Uiso 0.33 1 d PD B 3
F14Y F 0.1214(4) 0.5763(6) 0.4834(4) 0.048(3) Uiso 0.33 1 d PD B 3
F15Y F 0.2058(3) 0.6048(6) 0.4336(4) 0.0423(19) Uiso 0.33 1 d PD B 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'
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
O3 Fe1 O3 160.02(10) 2 .
O3 Fe1 O1 99.92(7) 2 .
O3 Fe1 O1 94.84(7) . .
O3 Fe1 O1 94.84(7) 2 2
O3 Fe1 O1 99.92(7) . 2
O1 Fe1 O1 84.59(10) . 2
O3 Fe1 O2 86.45(7) 2 2
O3 Fe1 O2 81.77(7) . 2
O1 Fe1 O2 167.50(7) . 2
O1 Fe1 O2 84.15(7) 2 2
O3 Fe1 O2 81.77(7) 2 .
O3 Fe1 O2 86.45(7) . .
O1 Fe1 O2 84.15(7) . .
O1 Fe1 O2 167.50(7) 2 .
O2 Fe1 O2 107.54(9) 2 .
O4 Fe2 O7 170.45(7) . .
O4 Fe2 O6 103.34(7) . .
O7 Fe2 O6 86.16(7) . .
O4 Fe2 O5 86.58(7) . .
O7 Fe2 O5 94.80(7) . .
O6 Fe2 O5 88.02(7) . .
O4 Fe2 O2 85.69(7) . 2
O7 Fe2 O2 92.02(6) . 2
O6 Fe2 O2 98.65(6) . 2
O5 Fe2 O2 170.77(7) . 2
O4 Fe2 O3 90.14(7) . .
O7 Fe2 O3 80.35(7) . .
O6 Fe2 O3 163.02(6) . .
O5 Fe2 O3 103.26(7) . .
O2 Fe2 O3 71.75(6) 2 .
C3 O1 Fe1 130.81(16) . .
C4 O2 Fe1 122.43(15) . .
C4 O2 Fe2 130.91(15) . 2
Fe1 O2 Fe2 103.59(7) . 2
C9 O3 Fe1 123.42(16) . .
C9 O3 Fe2 120.76(15) . .
Fe1 O3 Fe2 102.25(7) . .
C13 O4 Fe2 127.86(17) . .
C14 O5 Fe2 126.70(18) . .
C7 O6 Fe2 127.71(16) . .
C6 O7 Fe2 127.29(16) . .
F10 C2 F11 107.6(2) . .
F10 C2 F12 106.6(2) . .
F11 C2 F12 107.5(2) . .
F10 C2 C6 112.1(2) . .
F11 C2 C6 110.2(2) . .
F12 C2 C6 112.6(2) . .
O1 C3 C17 126.9(2) . .
O1 C3 C11 113.6(2) . .
C17 C3 C11 119.5(2) . .
O2 C4 C8 122.7(2) . .
O2 C4 C15 117.4(2) . .
C8 C4 C15 119.9(2) . .
C6 C5 C7 120.7(2) . .
C6 C5 H5 119.6 . .
C7 C5 H5 119.6 . .
O7 C6 C5 128.5(2) . .
O7 C6 C2 113.6(2) . .
C5 C6 C2 117.9(2) . .
O6 C7 C5 127.6(2) . .
O6 C7 C16 113.8(2) . .
C5 C7 C16 118.6(2) . .
C9 C8 C4 125.5(2) . .
C9 C8 H8 117.3 . .
C4 C8 H8 117.3 . .
O3 C9 C8 123.0(2) . .
O3 C9 C18 116.2(2) . .
C8 C9 C18 120.8(2) . .
F5 C10 F4 107.4(3) . .
F5 C10 F6 107.8(2) . .
F4 C10 F6 107.0(2) . .
F5 C10 C13 110.9(2) . .
F4 C10 C13 111.7(2) . .
F6 C10 C13 111.8(2) . .
F1 C11 F2 108.9(2) . .
F1 C11 F3 107.4(2) . .
F2 C11 F3 106.9(2) . .
F1 C11 C3 111.7(2) . .
F2 C11 C3 112.4(2) . .
F3 C11 C3 109.3(2) . .
C13 C12 C14 121.1(2) . .
C13 C12 H12 119.4 . .
C14 C12 H12 119.4 . .
O4 C13 C12 128.0(2) . .
O4 C13 C10 114.1(2) . .
C12 C13 C10 117.9(2) . .
O5 C14 C12 128.1(3) . .
O5 C14 C1 113.9(3) . .
C12 C14 C1 118.0(2) . .
C4 C15 H15A 109.5 . .
C4 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C4 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C3 C17 C3 120.0(3) 2 .
C3 C17 H17 120.0 2 .
C3 C17 H17 120.0 . .
C9 C18 H18A 109.5 . .
C9 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C9 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
F8 C1 F7 110.6(6) . .
F8 C1 F9 108.0(5) . .
F7 C1 F9 109.1(5) . .
F8 C1 C14 110.5(4) . .
F7 C1 C14 108.4(4) . .
F9 C1 C14 110.3(3) . .
F13 C16 F14 109.6(5) . .
F13 C16 F15 108.8(4) . .
F14 C16 F15 109.9(5) . .
F13 C16 C7 115.7(3) . .
F14 C16 C7 108.0(4) . .
F15 C16 C7 104.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O3 1.9862(17) 2
Fe1 O3 1.9862(17) .
Fe1 O1 2.0084(17) .
Fe1 O1 2.0084(17) 2
Fe1 O2 2.0120(16) 2
Fe1 O2 2.0120(16) .
Fe2 O4 2.0186(17) .
Fe2 O7 2.0350(17) .
Fe2 O6 2.0527(18) .
Fe2 O5 2.0613(19) .
Fe2 O2 2.2013(17) 2
Fe2 O3 2.2636(17) .
O1 C3 1.258(3) .
O2 C4 1.295(3) .
O2 Fe2 2.2013(17) 2
O3 C9 1.309(3) .
O4 C13 1.262(3) .
O5 C14 1.248(3) .
O6 C7 1.244(3) .
O7 C6 1.257(3) .
C2 F10 1.328(3) .
C2 F11 1.330(3) .
C2 F12 1.339(3) .
C2 C6 1.537(3) .
C3 C17 1.387(3) .
C3 C11 1.532(3) .
C4 C8 1.403(3) .
C4 C15 1.496(3) .
C5 C6 1.390(4) .
C5 C7 1.403(3) .
C5 H5 0.9500 .
C7 C16 1.532(4) .
C8 C9 1.384(4) .
C8 H8 0.9500 .
C9 C18 1.490(4) .
C10 F5 1.322(4) .
C10 F4 1.334(4) .
C10 F6 1.340(3) .
C10 C13 1.533(4) .
C11 F1 1.313(3) .
C11 F2 1.328(3) .
C11 F3 1.339(3) .
C12 C13 1.389(4) .
C12 C14 1.389(4) .
C12 H12 0.9500 .
C14 C1 1.544(4) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C17 C3 1.387(3) 2
C17 H17 0.9500 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C1 F8 1.313(6) .
C1 F7 1.371(7) .
C1 F9 1.391(6) .
C16 F13 1.329(5) .
C16 F14 1.385(7) .
C16 F15 1.441(6) .
