#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/03/4120359.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_4120359
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 Mn Na O6'
_chemical_formula_sum            'C15 H3 F18 Mn Na O6'
_chemical_formula_weight         699.10
_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                   18.045(2)
_cell_length_b                   18.045(2)
_cell_length_c                   12.6335(14)
_cell_measurement_reflns_used    8094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8819
_cell_measurement_theta_min      2.2573
_cell_volume                     3562.6(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.970
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29558
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.9566
_exptl_absorpt_correction_T_min  0.7445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       needle
_exptl_crystal_F_000             2034
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0516
_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)+(0.0261P)²+12.5398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                2036
_reflns_number_total             2874
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja4069529_si_002_2.cif
_cod_data_source_block           NaMn(hfac)3
_cod_original_sg_symbol_Hall     '-P 3 2"c     '
_cod_original_sg_symbol_H-M      'P -3 c 1 '
_cod_database_code               4120359
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
Mn1 Mn 0.0000 0.0000 0.2500 0.0183(3) Uani 1 6 d S
Na1 Na 0.0000 0.0000 0.5000 0.0253(7) Uani 1 6 d S
O1 O -0.02170(15) 0.07865(14) 0.35918(16) 0.0235(5) Uani 1 1 d .
C1 C 0.0000 0.1950(3) 0.2500 0.0241(10) Uani 1 2 d S
H1 H 0.0000 0.2476 0.2500 0.029 Uiso 1 2 calc SR
C3 C -0.0423(2) 0.1858(2) 0.4398(3) 0.0306(8) Uani 1 1 d .
F1 F -0.04279(17) 0.14630(15) 0.52919(15) 0.0418(6) Uani 1 1 d .
F2 F 0.01293(16) 0.26886(14) 0.45246(16) 0.0405(6) Uani 1 1 d .
F3 F -0.11981(15) 0.17597(16) 0.42777(17) 0.0419(6) Uani 1 1 d .
C2 C -0.0190(2) 0.1487(2) 0.3438(2) 0.0233(7) Uani 1 1 d .
Mn2 Mn 0.6667 0.3333 0.03762(6) 0.0201(2) Uani 1 3 d S
Na2 Na 0.6667 0.3333 0.28790(16) 0.0278(5) Uani 1 3 d S
O2 O 0.69952(15) 0.26177(15) 0.14321(16) 0.0252(5) Uani 1 1 d .
O3 O 0.63230(15) 0.22871(14) -0.06867(16) 0.0251(5) Uani 1 1 d .
F4 F 0.72799(16) 0.19033(16) 0.30837(16) 0.0449(6) Uani 1 1 d .
F8 F 0.60381(16) 0.13023(15) -0.23405(16) 0.0454(6) Uani 1 1 d .
C6 C 0.6637(2) 0.1385(2) 0.0382(3) 0.0260(7) Uani 1 1 d .
H6 H 0.6624 0.0852 0.0386 0.031 Uiso 1 1 calc R
F9 F 0.6242(2) 0.04123(18) -0.1445(2) 0.0660(9) Uani 1 1 d .
F5 F 0.7091(2) 0.08286(18) 0.2172(2) 0.0796(11) Uani 1 1 d .
F7 F 0.50910(17) 0.04630(17) -0.1245(2) 0.0584(8) Uani 1 1 d .
C5 C 0.6964(2) 0.1916(2) 0.1267(2) 0.0243(7) Uani 1 1 d .
F6 F 0.82211(18) 0.2035(2) 0.1957(2) 0.0665(9) Uani 1 1 d .
C7 C 0.6330(2) 0.1604(2) -0.0507(2) 0.0244(7) Uani 1 1 d .
C4 C 0.7386(3) 0.1655(3) 0.2126(3) 0.0358(9) Uani 1 1 d .
C8 C 0.5931(3) 0.0935(2) -0.1397(3) 0.0336(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 0.0033 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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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 Mn1 O1 152.35(12) 5 3 yes
O1 Mn1 O1 82.66(11) 5 2 yes
O1 Mn1 O1 83.29(8) 3 2 yes
O1 Mn1 O1 83.29(8) 5 4 yes
O1 Mn1 O1 82.66(11) 3 4 yes
O1 Mn1 O1 118.41(12) 2 4 yes
O1 Mn1 O1 83.29(8) 5 6 yes
O1 Mn1 O1 118.41(12) 3 6 yes
O1 Mn1 O1 152.35(12) 2 6 yes
O1 Mn1 O1 83.29(8) 4 6 yes
O1 Mn1 O1 118.41(12) 5 . yes
O1 Mn1 O1 83.29(8) 3 . yes
O1 Mn1 O1 83.29(8) 2 . yes
O1 Mn1 O1 152.36(12) 4 . yes
O1 Mn1 O1 82.66(11) 6 . yes
O1 Mn1 Na1 50.11(6) 5 4 yes
O1 Mn1 Na1 129.89(6) 3 4 yes
O1 Mn1 Na1 129.89(6) 2 4 yes
O1 Mn1 Na1 50.11(6) 4 4 yes
O1 Mn1 Na1 50.11(6) 6 4 yes
O1 Mn1 Na1 129.89(6) . 4 yes
O1 Mn1 Na1 129.89(6) 5 . yes
O1 Mn1 Na1 50.11(6) 3 . yes
O1 Mn1 Na1 50.11(6) 2 . yes
O1 Mn1 Na1 129.89(6) 4 . yes
O1 Mn1 Na1 129.89(6) 6 . yes
O1 Mn1 Na1 50.11(6) . . yes
Na1 Mn1 Na1 180.0 4 . yes
O1 Na1 O1 107.84(8) . 8_556 ?
O1 Na1 O1 72.16(8) . 2 ?
O1 Na1 O1 180.00(11) 8_556 2 ?
O1 Na1 O1 180.0 . 7_556 ?
O1 Na1 O1 72.16(8) 8_556 7_556 ?
O1 Na1 O1 107.84(8) 2 7_556 ?
O1 Na1 O1 107.83(8) . 9_556 ?
O1 Na1 O1 72.16(8) 8_556 9_556 ?
O1 Na1 O1 107.84(8) 2 9_556 ?
O1 Na1 O1 72.16(8) 7_556 9_556 ?
O1 Na1 O1 72.17(8) . 3 ?
O1 Na1 O1 107.84(8) 8_556 3 ?
O1 Na1 O1 72.16(8) 2 3 ?
O1 Na1 O1 107.84(8) 7_556 3 ?
O1 Na1 O1 180.0 9_556 3 ?
O1 Na1 Mn1 137.15(5) . 7_556 ?
O1 Na1 Mn1 42.85(5) 8_556 7_556 ?
O1 Na1 Mn1 137.15(5) 2 7_556 ?
O1 Na1 Mn1 42.85(5) 7_556 7_556 ?
O1 Na1 Mn1 42.85(5) 9_556 7_556 ?
O1 Na1 Mn1 137.15(5) 3 7_556 ?
O1 Na1 Mn1 42.85(5) . . ?
O1 Na1 Mn1 137.15(5) 8_556 . ?
O1 Na1 Mn1 42.85(5) 2 . ?
O1 Na1 Mn1 137.15(5) 7_556 . ?
O1 Na1 Mn1 137.15(5) 9_556 . ?
O1 Na1 Mn1 42.85(5) 3 . ?
Mn1 Na1 Mn1 180.0 7_556 . ?
C2 O1 Mn1 129.5(2) . . ?
C2 O1 Na1 140.0(2) . . ?
Mn1 O1 Na1 87.04(8) . . ?
C2 C1 C2 123.0(4) 6 . ?
C2 C1 H1 118.5 6 . ?
C2 C1 H1 118.5 . . ?
F3 C3 F2 108.0(3) . . ?
F3 C3 F1 107.5(3) . . ?
F2 C3 F1 107.6(3) . . ?
F3 C3 C2 110.5(3) . . ?
F2 C3 C2 111.7(3) . . ?
F1 C3 C2 111.4(3) . . ?
O1 C2 C1 127.6(3) . . ?
O1 C2 C3 115.6(3) . . ?
C1 C2 C3 116.7(3) . . ?
O2 Mn2 O2 85.14(9) . 2_655 yes
O2 Mn2 O2 85.13(9) . 3_665 yes
O2 Mn2 O2 85.13(9) 2_655 3_665 yes
O2 Mn2 O3 108.70(9) . 2_655 yes
O2 Mn2 O3 84.50(8) 2_655 2_655 yes
O2 Mn2 O3 161.89(9) 3_665 2_655 yes
O2 Mn2 O3 161.89(9) . 3_665 yes
O2 Mn2 O3 108.70(9) 2_655 3_665 yes
O2 Mn2 O3 84.50(8) 3_665 3_665 yes
O3 Mn2 O3 84.81(9) 2_655 3_665 yes
O2 Mn2 O3 84.50(8) . . yes
O2 Mn2 O3 161.89(9) 2_655 . yes
O2 Mn2 O3 108.70(9) 3_665 . yes
O3 Mn2 O3 84.81(9) 2_655 . yes
O3 Mn2 O3 84.81(9) 3_665 . yes
O2 Mn2 Na2 128.64(6) . 10_665 yes
O2 Mn2 Na2 128.64(6) 2_655 10_665 yes
O2 Mn2 Na2 128.64(6) 3_665 10_665 yes
O3 Mn2 Na2 51.14(6) 2_655 10_665 yes
O3 Mn2 Na2 51.14(6) 3_665 10_665 yes
O3 Mn2 Na2 51.14(6) . 10_665 yes
O2 Mn2 Na2 51.36(6) . . yes
O2 Mn2 Na2 51.36(6) 2_655 . yes
O2 Mn2 Na2 51.36(6) 3_665 . yes
O3 Mn2 Na2 128.86(6) 2_655 . yes
O3 Mn2 Na2 128.86(6) 3_665 . yes
O3 Mn2 Na2 128.86(6) . . yes
Na2 Mn2 Na2 180.0 10_665 . yes
O3 Na2 O3 71.79(9) 10_666 11_656 ?
O3 Na2 O3 71.79(9) 10_666 12_556 ?
O3 Na2 O3 71.79(9) 11_656 12_556 ?
O3 Na2 O2 108.75(7) 10_666 . ?
O3 Na2 O2 108.02(7) 11_656 . ?
O3 Na2 O2 179.37(8) 12_556 . ?
O3 Na2 O2 108.02(7) 10_666 2_655 ?
O3 Na2 O2 179.37(8) 11_656 2_655 ?
O3 Na2 O2 108.75(7) 12_556 2_655 ?
O2 Na2 O2 71.45(9) . 2_655 ?
O3 Na2 O2 179.37(8) 10_666 3_665 ?
O3 Na2 O2 108.75(7) 11_656 3_665 ?
O3 Na2 O2 108.02(7) 12_556 3_665 ?
O2 Na2 O2 71.45(9) . 3_665 ?
O2 Na2 O2 71.45(9) 2_655 3_665 ?
O3 Na2 Mn2 42.61(6) 10_666 10_666 ?
O3 Na2 Mn2 42.61(6) 11_656 10_666 ?
O3 Na2 Mn2 42.61(6) 12_556 10_666 ?
O2 Na2 Mn2 137.61(6) . 10_666 ?
O2 Na2 Mn2 137.61(6) 2_655 10_666 ?
O2 Na2 Mn2 137.61(6) 3_665 10_666 ?
O3 Na2 Mn2 137.39(6) 10_666 . ?
O3 Na2 Mn2 137.39(6) 11_656 . ?
O3 Na2 Mn2 137.39(6) 12_556 . ?
O2 Na2 Mn2 42.39(6) . . ?
O2 Na2 Mn2 42.39(6) 2_655 . ?
O2 Na2 Mn2 42.39(6) 3_665 . ?
Mn2 Na2 Mn2 180.0 10_666 . ?
C5 O2 Mn2 128.2(2) . . ?
C5 O2 Na2 138.3(2) . . ?
Mn2 O2 Na2 86.25(9) . . ?
C7 O3 Mn2 127.6(2) . . ?
C7 O3 Na2 139.6(2) . 10_665 ?
Mn2 O3 Na2 86.25(9) . 10_665 ?
C7 C6 C5 122.7(3) . . ?
C7 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
O2 C5 C6 128.0(3) . . ?
O2 C5 C4 114.5(3) . . ?
C6 C5 C4 117.4(3) . . ?
O3 C7 C6 128.6(3) . . ?
O3 C7 C8 114.0(3) . . ?
C6 C7 C8 117.5(3) . . ?
F5 C4 F6 107.9(4) . . ?
F5 C4 F4 107.3(3) . . ?
F6 C4 F4 106.8(3) . . ?
F5 C4 C5 113.6(3) . . ?
F6 C4 C5 109.7(3) . . ?
F4 C4 C5 111.2(3) . . ?
F9 C8 F8 107.9(3) . . ?
F9 C8 F7 107.7(3) . . ?
F8 C8 F7 106.5(3) . . ?
F9 C8 C7 113.3(3) . . ?
F8 C8 C7 111.7(3) . . ?
F7 C8 C7 109.4(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
Mn1 O1 2.151(2) 5 yes
Mn1 O1 2.151(2) 3 yes
Mn1 O1 2.151(2) 2 yes
Mn1 O1 2.151(2) 4 yes
Mn1 O1 2.151(2) 6 yes
Mn1 O1 2.151(2) . yes
Mn1 Na1 3.1584(4) 4 yes
Mn1 Na1 3.1584(4) . yes
Na1 O1 2.427(2) . ?
Na1 O1 2.427(2) 8_556 ?
Na1 O1 2.427(2) 2 ?
Na1 O1 2.427(2) 7_556 ?
Na1 O1 2.427(2) 9_556 ?
Na1 O1 2.427(2) 3 ?
Na1 Mn1 3.1584(4) 7_556 yes
O1 C2 1.256(4) . ?
C1 C2 1.390(4) 6 ?
C1 C2 1.390(4) . ?
C1 H1 0.9500 . ?
C3 F3 1.328(4) . ?
C3 F2 1.331(4) . ?
C3 F1 1.332(4) . ?
C3 C2 1.542(4) . ?
Mn2 O2 2.136(2) . yes
Mn2 O2 2.136(2) 2_655 yes
Mn2 O2 2.136(2) 3_665 yes
Mn2 O3 2.140(2) 2_655 yes
Mn2 O3 2.140(2) 3_665 yes
Mn2 O3 2.140(2) . yes
Mn2 Na2 3.155(2) 10_665 yes
Mn2 Na2 3.162(2) . yes
Na2 O3 2.462(3) 10_666 ?
Na2 O3 2.462(3) 11_656 ?
Na2 O3 2.462(3) 12_556 ?
Na2 O2 2.475(3) . ?
Na2 O2 2.475(3) 2_655 ?
Na2 O2 2.475(3) 3_665 ?
Na2 Mn2 3.155(2) 10_666 yes
O2 C5 1.256(4) . ?
O3 C7 1.259(4) . ?
O3 Na2 2.462(3) 10_665 ?
F4 C4 1.337(4) . ?
F8 C8 1.330(4) . ?
C6 C7 1.395(5) . ?
C6 C5 1.397(5) . ?
C6 H6 0.9500 . ?
F9 C8 1.318(4) . ?
F5 C4 1.310(5) . ?
F7 C8 1.331(5) . ?
C5 C4 1.531(5) . ?
F6 C4 1.324(5) . ?
C7 C8 1.540(5) . ?
