#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:50:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178980 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/03/4120360.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_4120360
loop_
_publ_author_name
'Zheng Wei'
'Alexander S. Filatov'
'Evgeny V. Dikarev'
_publ_contact_author_address
;
Department of Chemistry
University at Albany
1400 Washington Avenue
Albany NY 12222
USA
;
_publ_contact_author_email       dikarev@albany.edu
_publ_contact_author_fax         518-442-3462
_publ_contact_author_name
;
Dikarev, Evgeny V. 
;
_publ_contact_author_phone       518-442-4401
_publ_section_title
;
 Volatile Heterometallic Precursors for the Low-Temperature Synthesis of
 Prospective Sodium Ion Battery Cathode Materials
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12216
_journal_page_last               12219
_journal_paper_doi               10.1021/ja4069529
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C15 H3 F18 Fe Na O6'
_chemical_formula_sum            'C15 H3 F18 Fe Na O6'
_chemical_formula_weight         700.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.0016(4)
_cell_length_b                   18.0016(4)
_cell_length_c                   12.3451(3)
_cell_measurement_reflns_used    1813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      3.85
_cell_volume                     3464.55(14)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_source         'INCOATEC ImuS micro-focus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34616
_diffrn_reflns_theta_full        66.77
_diffrn_reflns_theta_max         66.77
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    7.149
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_correction_T_min  0.1226
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       needle
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0501
_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)+(0.0205P)²+6.0020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                1664
_reflns_number_total             2054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4069529_si_002_3.cif
_cod_data_source_block           NaFe(hfac)3
_cod_database_code               4120360
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
Fe1 Fe 0.0000 0.0000 0.7500 0.0168(3) Uani 1 6 d S
Fe2 Fe 0.6667 0.3333 0.03809(6) 0.0171(2) Uani 1 3 d S
Na1 Na 0.0000 0.0000 1.0000 0.0244(7) Uani 1 6 d S
Na2 Na 0.6667 0.3333 -0.21184(16) 0.0274(5) Uani 1 3 d S
O1 O 0.10334(14) 0.06686(15) 0.85445(16) 0.0219(5) Uani 1 1 d .
O2 O 0.60512(15) 0.37714(14) -0.06291(16) 0.0211(5) Uani 1 1 d .
O3 O 0.56160(14) 0.29088(15) 0.13926(15) 0.0217(5) Uani 1 1 d .
C1 C 0.1919(3) 0.1919(3) 0.7500 0.0257(12) Uani 1 2 d S
H1 H 0.2447 0.2447 0.7500 0.031 Uiso 1 2 calc SR
C2 C 0.1694(2) 0.1388(2) 0.8402(3) 0.0214(8) Uani 1 1 d .
C3 C 0.2336(2) 0.1698(3) 0.9340(3) 0.0319(9) Uani 1 1 d .
C4 C 0.5111(3) 0.4190(3) -0.1340(3) 0.0313(9) Uani 1 1 d .
C5 C 0.5343(2) 0.3740(2) -0.0470(3) 0.0211(8) Uani 1 1 d .
C6 C 0.4782(2) 0.3362(2) 0.0391(3) 0.0236(8) Uani 1 1 d .
H6 H 0.4259 0.3372 0.0396 0.028 Uiso 1 1 calc R
C7 C 0.4953(2) 0.2974(2) 0.1241(2) 0.0219(8) Uani 1 1 d .
C8 C 0.4265(2) 0.2522(3) 0.2116(3) 0.0299(9) Uani 1 1 d .
F1 F 0.19569(13) 0.13374(14) 1.02769(15) 0.0363(6) Uani 1 1 d .
F2 F 0.29398(15) 0.1499(2) 0.91769(17) 0.0573(8) Uani 1 1 d .
F3 F 0.27207(17) 0.25469(15) 0.94861(19) 0.0591(8) Uani 1 1 d .
F4 F 0.42842(16) 0.3934(2) -0.1372(2) 0.0637(9) Uani 1 1 d .
F5 F 0.53427(14) 0.40706(15) -0.23214(15) 0.0418(6) Uani 1 1 d .
F6 F 0.55314(18) 0.50315(16) -0.11685(19) 0.0557(7) Uani 1 1 d .
F7 F 0.46060(13) 0.25977(15) 0.30857(15) 0.0389(6) Uani 1 1 d .
F8 F 0.38135(16) 0.16837(16) 0.18950(18) 0.0559(8) Uani 1 1 d .
F9 F 0.37166(16) 0.28043(19) 0.21735(18) 0.0576(8) Uani 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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 164.90(13) . 6_556
O1 Fe1 O1 105.61(12) . 5_556
O1 Fe1 O1 85.66(9) 6_556 5_556
O1 Fe1 O1 85.22(12) . 4_556
O1 Fe1 O1 85.66(9) 6_556 4_556
O1 Fe1 O1 85.66(9) 5_556 4_556
O1 Fe1 O1 85.66(8) . 2
O1 Fe1 O1 85.22(12) 6_556 2
O1 Fe1 O1 164.90(13) 5_556 2
O1 Fe1 O1 105.61(12) 4_556 2
O1 Fe1 O1 85.66(8) . 3
O1 Fe1 O1 105.61(12) 6_556 3
O1 Fe1 O1 85.22(12) 5_556 3
O1 Fe1 O1 164.90(13) 4_556 3
O1 Fe1 O1 85.66(9) 2 3
O1 Fe1 Na1 51.72(6) . .
O1 Fe1 Na1 128.28(6) 6_556 .
O1 Fe1 Na1 128.28(6) 5_556 .
O1 Fe1 Na1 128.28(6) 4_556 .
O1 Fe1 Na1 51.72(6) 2 .
O1 Fe1 Na1 51.72(6) 3 .
O1 Fe1 Na1 128.28(6) . 4_556
O1 Fe1 Na1 51.72(6) 6_556 4_556
O1 Fe1 Na1 51.72(6) 5_556 4_556
O1 Fe1 Na1 51.72(6) 4_556 4_556
O1 Fe1 Na1 128.28(6) 2 4_556
O1 Fe1 Na1 128.28(6) 3 4_556
Na1 Fe1 Na1 180.0 . 4_556
O3 Fe2 O3 87.29(8) . 2_655
O3 Fe2 O3 87.29(8) . 3_665
O3 Fe2 O3 87.29(8) 2_655 3_665
O3 Fe2 O2 86.54(8) . .
O3 Fe2 O2 170.54(9) 2_655 .
O3 Fe2 O2 99.57(8) 3_665 .
O3 Fe2 O2 99.57(8) . 2_655
O3 Fe2 O2 86.54(8) 2_655 2_655
O3 Fe2 O2 170.54(9) 3_665 2_655
O2 Fe2 O2 87.41(9) . 2_655
O3 Fe2 O2 170.54(9) . 3_665
O3 Fe2 O2 99.57(8) 2_655 3_665
O3 Fe2 O2 86.54(8) 3_665 3_665
O2 Fe2 O2 87.41(9) . 3_665
O2 Fe2 O2 87.41(9) 2_655 3_665
O3 Fe2 Na2 127.16(6) . .
O3 Fe2 Na2 127.16(6) 2_655 .
O3 Fe2 Na2 127.16(6) 3_665 .
O2 Fe2 Na2 52.93(6) . .
O2 Fe2 Na2 52.93(6) 2_655 .
O2 Fe2 Na2 52.93(6) 3_665 .
O3 Fe2 Na2 52.84(6) . 10_666
O3 Fe2 Na2 52.84(6) 2_655 10_666
O3 Fe2 Na2 52.84(6) 3_665 10_666
O2 Fe2 Na2 127.07(6) . 10_666
O2 Fe2 Na2 127.08(6) 2_655 10_666
O2 Fe2 Na2 127.07(6) 3_665 10_666
Na2 Fe2 Na2 180.0 . 10_666
O1 Na1 O1 180.0 9_557 3
O1 Na1 O1 71.28(8) 9_557 8_557
O1 Na1 O1 108.72(8) 3 8_557
O1 Na1 O1 108.72(8) 9_557 2
O1 Na1 O1 71.28(8) 3 2
O1 Na1 O1 180.0 8_557 2
O1 Na1 O1 71.28(8) 9_557 7_557
O1 Na1 O1 108.72(8) 3 7_557
O1 Na1 O1 71.28(8) 8_557 7_557
O1 Na1 O1 108.72(8) 2 7_557
O1 Na1 O1 108.72(8) 9_557 .
O1 Na1 O1 71.28(8) 3 .
O1 Na1 O1 108.72(8) 8_557 .
O1 Na1 O1 71.28(8) 2 .
O1 Na1 O1 180.0 7_557 .
O1 Na1 Fe1 137.71(5) 9_557 .
O1 Na1 Fe1 42.29(5) 3 .
O1 Na1 Fe1 137.71(5) 8_557 .
O1 Na1 Fe1 42.29(5) 2 .
O1 Na1 Fe1 137.71(5) 7_557 .
O1 Na1 Fe1 42.28(5) . .
O1 Na1 Fe1 42.29(5) 9_557 7_557
O1 Na1 Fe1 137.71(5) 3 7_557
O1 Na1 Fe1 42.29(5) 8_557 7_557
O1 Na1 Fe1 137.71(5) 2 7_557
O1 Na1 Fe1 42.29(5) 7_557 7_557
O1 Na1 Fe1 137.72(5) . 7_557
Fe1 Na1 Fe1 180.0 . 7_557
O3 Na2 O3 70.64(9) 11_655 12
O3 Na2 O3 70.64(9) 11_655 10_665
O3 Na2 O3 70.64(9) 12 10_665
O3 Na2 O2 109.02(7) 11_655 3_665
O3 Na2 O2 179.49(8) 12 3_665
O3 Na2 O2 109.65(7) 10_665 3_665
O3 Na2 O2 109.65(7) 11_655 2_655
O3 Na2 O2 109.02(7) 12 2_655
O3 Na2 O2 179.49(8) 10_665 2_655
O2 Na2 O2 70.69(9) 3_665 2_655
O3 Na2 O2 179.49(8) 11_655 .
O3 Na2 O2 109.65(7) 12 .
O3 Na2 O2 109.03(7) 10_665 .
O2 Na2 O2 70.69(9) 3_665 .
O2 Na2 O2 70.69(9) 2_655 .
O3 Na2 Fe2 138.12(6) 11_655 .
O3 Na2 Fe2 138.12(6) 12 .
O3 Na2 Fe2 138.12(6) 10_665 .
O2 Na2 Fe2 41.91(6) 3_665 .
O2 Na2 Fe2 41.91(6) 2_655 .
O2 Na2 Fe2 41.91(6) . .
O3 Na2 Fe2 41.88(6) 11_655 10_665
O3 Na2 Fe2 41.88(6) 12 10_665
O3 Na2 Fe2 41.88(6) 10_665 10_665
O2 Na2 Fe2 138.09(6) 3_665 10_665
O2 Na2 Fe2 138.09(6) 2_655 10_665
O2 Na2 Fe2 138.09(6) . 10_665
Fe2 Na2 Fe2 180.0 . 10_665
C2 O1 Fe1 128.3(2) . .
C2 O1 Na1 135.2(2) . .
Fe1 O1 Na1 85.99(8) . .
C5 O2 Fe2 127.6(2) . .
C5 O2 Na2 134.8(2) . .
Fe2 O2 Na2 85.16(8) . .
C7 O3 Fe2 127.2(2) . .
C7 O3 Na2 133.7(2) . 10_666
Fe2 O3 Na2 85.28(9) . 10_666
C2 C1 C2 121.3(5) . 4_556
C2 C1 H1 119.3 . .
C2 C1 H1 119.3 4_556 .
O1 C2 C1 128.4(3) . .
O1 C2 C3 115.0(3) . .
C1 C2 C3 116.6(3) . .
F2 C3 F1 106.9(3) . .
F2 C3 F3 107.7(3) . .
F1 C3 F3 106.6(3) . .
F2 C3 C2 111.1(3) . .
F1 C3 C2 111.7(3) . .
F3 C3 C2 112.6(3) . .
F4 C4 F6 107.6(3) . .
F4 C4 F5 107.8(3) . .
F6 C4 F5 106.5(3) . .
F4 C4 C5 113.3(3) . .
F6 C4 C5 110.0(3) . .
F5 C4 C5 111.3(3) . .
O2 C5 C6 127.8(3) . .
O2 C5 C4 113.9(3) . .
C6 C5 C4 118.3(3) . .
C7 C6 C5 122.6(3) . .
C7 C6 H6 118.7 . .
C5 C6 H6 118.7 . .
O3 C7 C6 128.2(3) . .
O3 C7 C8 113.2(3) . .
C6 C7 C8 118.6(3) . .
F9 C8 F7 108.0(3) . .
F9 C8 F8 107.2(3) . .
F7 C8 F8 106.9(3) . .
F9 C8 C7 113.2(3) . .
F7 C8 C7 111.9(3) . .
F8 C8 C7 109.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.082(2) .
Fe1 O1 2.082(2) 6_556
Fe1 O1 2.082(2) 5_556
Fe1 O1 2.082(2) 4_556
Fe1 O1 2.082(2) 2
Fe1 O1 2.082(2) 3
Fe1 Na1 3.0863 .
Fe1 Na1 3.0863 4_556
Fe2 O3 2.068(2) .
Fe2 O3 2.068(2) 2_655
Fe2 O3 2.068(2) 3_665
Fe2 O2 2.068(2) .
Fe2 O2 2.068(2) 2_655
Fe2 O2 2.068(2) 3_665
Fe2 Na2 3.085(2) .
Fe2 Na2 3.087(2) 10_666
Na1 O1 2.429(2) 9_557
Na1 O1 2.429(2) 3
Na1 O1 2.429(2) 8_557
Na1 O1 2.429(2) 2
Na1 O1 2.429(2) 7_557
Na1 O1 2.429(2) .
Na1 Fe1 3.0863 7_557
Na2 O3 2.469(2) 11_655
Na2 O3 2.469(2) 12
Na2 O3 2.469(2) 10_665
Na2 O2 2.471(2) 3_665
Na2 O2 2.471(2) 2_655
Na2 O2 2.471(2) .
Na2 Fe2 3.087(2) 10_665
O1 C2 1.257(4) .
O2 C5 1.263(4) .
O3 C7 1.270(4) .
O3 Na2 2.469(2) 10_666
C1 C2 1.390(4) .
C1 C2 1.390(4) 4_556
C1 H1 0.9500 .
C2 C3 1.530(5) .
C3 F2 1.319(5) .
C3 F1 1.335(4) .
C3 F3 1.338(5) .
C4 F4 1.321(4) .
C4 F6 1.329(5) .
C4 F5 1.333(4) .
C4 C5 1.525(5) .
C5 C6 1.388(5) .
C6 C7 1.378(5) .
C6 H6 0.9500 .
C7 C8 1.535(5) .
C8 F9 1.320(4) .
C8 F7 1.321(4) .
C8 F8 1.336(4) .
