#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:50:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178980 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/03/4120361.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_4120361
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 Co F18 Na O6'
_chemical_formula_sum            'C15 H3 Co F18 Na O6'
_chemical_formula_weight         703.09
_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                   17.958(5)
_cell_length_b                   17.958(5)
_cell_length_c                   12.531(3)
_cell_measurement_reflns_used    6094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.84
_cell_measurement_theta_min      2.27
_cell_volume                     3499.7(16)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17769
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_correction_T_min  0.7679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       needle
_exptl_crystal_F_000             2046
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0565
_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)+(0.0779P)²+1.7280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1537
_reflns_number_gt                1718
_reflns_number_total             2713
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja4069529_si_002_4.cif
_cod_data_source_block           NaCo(hfac)3
_cod_original_cell_volume        3499.9(16)
_cod_database_code               4120361
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
Co1 Co 1.0000 0.0000 0.2500 0.0204(3) Uani 1 6 d S
Na1 Na 1.0000 0.0000 0.0000 0.0261(8) Uani 1 6 d S
F1 F 0.93556(16) 0.13170(16) -0.02510(18) 0.0360(6) Uani 1 1 d .
O1 O 0.96241(16) 0.06442(16) 0.14564(19) 0.0250(6) Uani 1 1 d .
C2 C 0.9691(2) 0.1376(2) 0.1606(3) 0.0242(8) Uani 1 1 d .
F3 F 0.9825(2) 0.25385(17) 0.0525(2) 0.0564(8) Uani 1 1 d .
C1 C 1.0000 0.1902(3) 0.2500 0.0271(12) Uani 1 2 d S
H1 H 1.0000 0.2431 0.2500 0.032 Uiso 1 2 calc SR
F2 F 0.85446(18) 0.1494(2) 0.0855(2) 0.0553(8) Uani 1 1 d .
C3 C 0.9352(3) 0.1683(3) 0.0675(3) 0.0321(9) Uani 1 1 d .
Co2 Co 0.6667 0.3333 0.46446(6) 0.0200(2) Uani 1 3 d S
Na2 Na 0.6667 0.3333 0.21421(18) 0.0274(6) Uani 1 3 d S
O2 O 0.77068(15) 0.39329(15) 0.56632(19) 0.0236(5) Uani 1 1 d .
F9 F 0.79793(17) 0.53856(16) 0.19565(18) 0.0407(6) Uani 1 1 d .
O3 O 0.72721(16) 0.43676(16) 0.36235(19) 0.0239(6) Uani 1 1 d .
F5 F 0.87283(16) 0.46478(17) 0.73265(19) 0.0425(6) Uani 1 1 d .
F7 F 0.90910(17) 0.62735(18) 0.2860(2) 0.0586(9) Uani 1 1 d .
F4 F 0.95067(18) 0.4467(2) 0.6174(2) 0.0569(8) Uani 1 1 d .
F8 F 0.7866(2) 0.61881(17) 0.3137(2) 0.0561(8) Uani 1 1 d .
C6 C 0.8569(2) 0.5204(2) 0.4631(3) 0.0256(8) Uani 1 1 d .
H6 H 0.9106 0.5724 0.4623 0.031 Uiso 1 1 calc R
F6 F 0.96461(18) 0.57181(17) 0.6382(2) 0.0622(9) Uani 1 1 d .
C7 C 0.8002(2) 0.5033(2) 0.3782(3) 0.0240(8) Uani 1 1 d .
C8 C 0.8250(3) 0.5733(3) 0.2919(3) 0.0320(9) Uani 1 1 d .
C5 C 0.8378(2) 0.4642(2) 0.5495(3) 0.0249(8) Uani 1 1 d .
C4 C 0.9078(3) 0.4885(3) 0.6355(3) 0.0340(10) 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 0.0033 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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
O1 Co1 O1 166.63(14) 2_645 6_765 yes
O1 Co1 O1 105.47(14) 2_645 4_645 yes
O1 Co1 O1 84.34(10) 6_765 4_645 yes
O1 Co1 O1 87.58(13) 2_645 5 yes
O1 Co1 O1 84.34(10) 6_765 5 yes
O1 Co1 O1 84.34(10) 4_645 5 yes
O1 Co1 O1 84.34(10) 2_645 3_765 yes
O1 Co1 O1 105.47(14) 6_765 3_765 yes
O1 Co1 O1 87.58(13) 4_645 3_765 yes
O1 Co1 O1 166.63(14) 5 3_765 yes
O1 Co1 O1 84.34(10) 2_645 . yes
O1 Co1 O1 87.58(13) 6_765 . yes
O1 Co1 O1 166.63(14) 4_645 . yes
O1 Co1 O1 105.47(14) 5 . yes
O1 Co1 O1 84.34(10) 3_765 . yes
O1 Co1 Na1 129.18(7) 2_645 4_645 yes
O1 Co1 Na1 50.82(7) 6_765 4_645 yes
O1 Co1 Na1 50.82(7) 4_645 4_645 yes
O1 Co1 Na1 50.82(7) 5 4_645 yes
O1 Co1 Na1 129.18(7) 3_765 4_645 yes
O1 Co1 Na1 129.18(7) . 4_645 yes
O1 Co1 Na1 50.82(7) 2_645 . yes
O1 Co1 Na1 129.18(7) 6_765 . yes
O1 Co1 Na1 129.18(7) 4_645 . yes
O1 Co1 Na1 129.18(7) 5 . yes
O1 Co1 Na1 50.82(7) 3_765 . yes
O1 Co1 Na1 50.82(7) . . yes
Na1 Co1 Na1 180.0 4_645 . yes
O1 Na1 O1 180.00(14) 9_545 3_765 ?
O1 Na1 O1 69.76(9) 9_545 7_755 ?
O1 Na1 O1 110.24(9) 3_765 7_755 ?
O1 Na1 O1 69.76(9) 9_545 8_665 ?
O1 Na1 O1 110.24(9) 3_765 8_665 ?
O1 Na1 O1 69.76(9) 7_755 8_665 ?
O1 Na1 O1 110.24(9) 9_545 2_645 ?
O1 Na1 O1 69.76(9) 3_765 2_645 ?
O1 Na1 O1 110.24(9) 7_755 2_645 ?
O1 Na1 O1 180.00(14) 8_665 2_645 ?
O1 Na1 O1 110.24(9) 9_545 . ?
O1 Na1 O1 69.76(9) 3_765 . ?
O1 Na1 O1 180.00(11) 7_755 . ?
O1 Na1 O1 110.24(9) 8_665 . ?
O1 Na1 O1 69.76(9) 2_645 . ?
O1 Na1 Co1 138.68(6) 9_545 . ?
O1 Na1 Co1 41.32(6) 3_765 . ?
O1 Na1 Co1 138.68(6) 7_755 . ?
O1 Na1 Co1 138.68(6) 8_665 . ?
O1 Na1 Co1 41.32(6) 2_645 . ?
O1 Na1 Co1 41.32(6) . . ?
O1 Na1 Co1 41.32(6) 9_545 7_755 ?
O1 Na1 Co1 138.68(6) 3_765 7_755 ?
O1 Na1 Co1 41.32(6) 7_755 7_755 ?
O1 Na1 Co1 41.32(6) 8_665 7_755 ?
O1 Na1 Co1 138.68(6) 2_645 7_755 ?
O1 Na1 Co1 138.68(6) . 7_755 ?
Co1 Na1 Co1 180.0 . 7_755 ?
C2 O1 Co1 126.6(2) . . ?
C2 O1 Na1 134.2(2) . . ?
Co1 O1 Na1 87.86(9) . . ?
O1 C2 C1 128.3(4) . . ?
O1 C2 C3 114.1(3) . . ?
C1 C2 C3 117.6(3) . . ?
C2 C1 C2 122.7(5) . 6_765 ?
C2 C1 H1 118.6 . . ?
C2 C1 H1 118.6 6_765 . ?
F2 C3 F1 107.2(3) . . ?
F2 C3 F3 107.5(3) . . ?
F1 C3 F3 106.6(3) . . ?
F2 C3 C2 110.8(3) . . ?
F1 C3 C2 112.4(3) . . ?
F3 C3 C2 112.1(3) . . ?
O3 Co2 O3 85.53(10) 3_665 2_655 yes
O3 Co2 O3 85.53(10) 3_665 . yes
O3 Co2 O3 85.53(10) 2_655 . yes
O3 Co2 O2 100.34(10) 3_665 . yes
O3 Co2 O2 171.63(10) 2_655 . yes
O3 Co2 O2 88.96(10) . . yes
O3 Co2 O2 88.96(10) 3_665 3_665 yes
O3 Co2 O2 100.34(10) 2_655 3_665 yes
O3 Co2 O2 171.63(10) . 3_665 yes
O2 Co2 O2 85.82(10) . 3_665 yes
O3 Co2 O2 171.63(10) 3_665 2_655 yes
O3 Co2 O2 88.96(10) 2_655 2_655 yes
O3 Co2 O2 100.34(10) . 2_655 yes
O2 Co2 O2 85.82(10) . 2_655 yes
O2 Co2 O2 85.82(10) 3_665 2_655 yes
O3 Co2 Na2 128.37(7) 3_665 10_666 yes
O3 Co2 Na2 128.37(7) 2_655 10_666 yes
O3 Co2 Na2 128.37(7) . 10_666 yes
O2 Co2 Na2 51.83(7) . 10_666 yes
O2 Co2 Na2 51.83(7) 3_665 10_666 yes
O2 Co2 Na2 51.83(7) 2_655 10_666 yes
O3 Co2 Na2 51.63(7) 3_665 . yes
O3 Co2 Na2 51.63(7) 2_655 . yes
O3 Co2 Na2 51.63(7) . . yes
O2 Co2 Na2 128.17(7) . . yes
O2 Co2 Na2 128.17(7) 3_665 . yes
O2 Co2 Na2 128.17(7) 2_655 . yes
Na2 Co2 Na2 180.0 10_666 . yes
O3 Na2 O3 69.32(10) 3_665 2_655 ?
O3 Na2 O3 69.32(10) 3_665 . ?
O3 Na2 O3 69.32(10) 2_655 . ?
O3 Na2 O2 110.30(8) 3_665 10_665 ?
O3 Na2 O2 110.77(8) 2_655 10_665 ?
O3 Na2 O2 179.57(9) . 10_665 ?
O3 Na2 O2 110.77(8) 3_665 12 ?
O3 Na2 O2 179.57(9) 2_655 12 ?
O3 Na2 O2 110.30(8) . 12 ?
O2 Na2 O2 69.61(10) 10_665 12 ?
O3 Na2 O2 179.57(9) 3_665 11_655 ?
O3 Na2 O2 110.30(8) 2_655 11_655 ?
O3 Na2 O2 110.77(8) . 11_655 ?
O2 Na2 O2 69.61(10) 10_665 11_655 ?
O2 Na2 O2 69.61(10) 12 11_655 ?
O3 Na2 Co2 138.96(7) 3_665 10_665 ?
O3 Na2 Co2 138.95(7) 2_655 10_665 ?
O3 Na2 Co2 138.95(7) . 10_665 ?
O2 Na2 Co2 41.23(7) 10_665 10_665 ?
O2 Na2 Co2 41.23(7) 12 10_665 ?
O2 Na2 Co2 41.23(7) 11_655 10_665 ?
O3 Na2 Co2 41.05(7) 3_665 . ?
O3 Na2 Co2 41.05(7) 2_655 . ?
O3 Na2 Co2 41.05(7) . . ?
O2 Na2 Co2 138.77(7) 10_665 . ?
O2 Na2 Co2 138.77(7) 12 . ?
O2 Na2 Co2 138.77(7) 11_655 . ?
Co2 Na2 Co2 180.0 10_665 . ?
C5 O2 Co2 125.6(2) . . ?
C5 O2 Na2 134.6(2) . 10_666 ?
Co2 O2 Na2 86.94(9) . 10_666 ?
C7 O3 Co2 125.5(2) . . ?
C7 O3 Na2 133.3(2) . . ?
Co2 O3 Na2 87.32(10) . . ?
C7 C6 C5 122.8(3) . . ?
C7 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
O3 C7 C6 128.3(3) . . ?
O3 C7 C8 113.5(3) . . ?
C6 C7 C8 118.2(3) . . ?
F7 C8 F9 107.9(3) . . ?
F7 C8 F8 108.1(4) . . ?
F9 C8 F8 106.9(3) . . ?
F7 C8 C7 113.3(3) . . ?
F9 C8 C7 111.3(3) . . ?
F8 C8 C7 109.1(3) . . ?
O2 C5 C6 128.6(3) . . ?
O2 C5 C4 113.6(3) . . ?
C6 C5 C4 117.7(3) . . ?
F6 C4 F4 107.7(4) . . ?
F6 C4 F5 108.0(3) . . ?
F4 C4 F5 106.6(3) . . ?
F6 C4 C5 113.3(3) . . ?
F4 C4 C5 109.8(3) . . ?
F5 C4 C5 111.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.070(2) 2_645 yes
Co1 O1 2.070(2) 6_765 yes
Co1 O1 2.070(2) 4_645 yes
Co1 O1 2.070(2) 5 yes
Co1 O1 2.070(2) 3_765 yes
Co1 O1 2.070(2) . yes
Co1 Na1 3.1328(8) 4_645 yes
Co1 Na1 3.1328(8) . yes
Na1 O1 2.430(2) 9_545 ?
Na1 O1 2.430(2) 3_765 ?
Na1 O1 2.430(2) 7_755 ?
Na1 O1 2.430(2) 8_665 ?
Na1 O1 2.430(2) 2_645 ?
Na1 O1 2.430(2) . ?
Na1 Co1 3.1328(8) 7_755 yes
F1 C3 1.335(4) . ?
O1 C2 1.273(4) . ?
C2 C1 1.390(4) . ?
C2 C3 1.540(5) . ?
F3 C3 1.346(5) . ?
C1 C2 1.390(4) 6_765 ?
C1 H1 0.9500 . ?
F2 C3 1.332(5) . ?
Co2 O3 2.062(2) 3_665 yes
Co2 O3 2.062(2) 2_655 yes
Co2 O3 2.062(3) . yes
Co2 O2 2.066(2) . yes
Co2 O2 2.066(2) 3_665 yes
Co2 O2 2.066(2) 2_655 yes
Co2 Na2 3.130(3) 10_666 yes
Co2 Na2 3.136(3) . yes
Na2 O3 2.461(3) 3_665 ?
Na2 O3 2.461(3) 2_655 ?
Na2 O3 2.461(3) . ?
Na2 O2 2.464(3) 10_665 ?
Na2 O2 2.464(3) 12 ?
Na2 O2 2.464(3) 11_655 ?
Na2 Co2 3.130(3) 10_665 yes
O2 C5 1.259(4) . ?
O2 Na2 2.464(3) 10_666 ?
F9 C8 1.333(5) . ?
O3 C7 1.272(4) . ?
F5 C4 1.338(5) . ?
F7 C8 1.327(5) . ?
F4 C4 1.336(5) . ?
F8 C8 1.336(5) . ?
C6 C7 1.397(5) . ?
C6 C5 1.401(5) . ?
C6 H6 0.9500 . ?
F6 C4 1.325(5) . ?
C7 C8 1.544(5) . ?
C5 C4 1.544(5) . ?
