# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a616_0m
_database_code_depnum_ccdc_archive 'CCDC 1987388'
loop_
_audit_author_name
_audit_author_address
'Ningxin Jiang'
;Georgia Institute of Technology
United States of America
;
_audit_update_record             
;
2020-05-20 deposited with the CCDC.	2020-09-30 downloaded from the CCDC.
;
_audit_creation_date             2020-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
njiang48@gatech.edu
''
_chemical_name_common            ?
_chemical_name_systematic        C2N2H12NaV3F12
_chemical_formula_moiety         
'0.67(F18 Na1.5 V4.5), 0.33(C3 N3), 2(C0.5 H6 N0.5)'
_chemical_formula_sum            'C2 H12 F12 N2 Na V3'
_chemical_formula_weight         467.96
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   7.5349(13)
_cell_length_b                   7.5349(13)
_cell_length_c                   19.100(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     939.1(4)
_cell_formula_units_Z            2.99988
_cell_measurement_reflns_used    4576
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      40.32
_cell_measurement_theta_min      3.30
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  0.8679
_exptl_absorpt_correction_T_min  0.6406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1450 before and 0.0664 after correction. The Ratio of minimum to maximum transmission is 0.7381. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             678
_exptl_crystal_preparation       'Hydrothermal methods,Magnetic properties'
_exptl_crystal_recrystallization_method 'Hydrothermal methods'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.124
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            3676
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.267
_diffrn_reflns_theta_min         3.782
_diffrn_ambient_temperature      299.2
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_special_details          N.A.
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                707
_reflns_number_total             761
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         761
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0281P)²+1.9108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0761
_refine_special_details          N.A.
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H) groups
2. Shared sites
{N1A, N1B}
3. Restrained distances
 N1A-C1
 1.45 with sigma of 0.005
 N1A-C1 \\sim N1B-C0
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C0) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1) = Uanis(C0)
Uanis(N1A) = Uanis(N1B)
5. Rigid body (RIGU) restrains
 N1A, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C0(0.08333) N1B(0.08333) N1A(0.08333) H1Aa(0.16667) H1Ab(0.16667)
 H1Ac(0.16667) C1(0.08333) H1a(0.16667) H1b(0.16667) H1c(0.16667)
7.a Idealised Me refined as rotating group:
 N1A(H1Aa,H1Ab,H1Ac), C1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.166667 0.333333 0.333333 0.01167(9) Uani 1 4 d S T P . .
Na1 Na 0.000000 0.000000 0.500000 0.0129(2) Uani 1 12 d S T P . .
F1 F 0.45670(9) 0.54330(9) 0.34598(6) 0.0231(2) Uani 1 2 d S T P . .
F2 F 0.14287(10) 0.2857(2) 0.43063(6) 0.0273(2) Uani 1 2 d S T P . .
C0 C 0.666667 0.333333 0.4356(6) 0.0496(17) Uani 0.5 6 d DS TU P A 2
N1B N 0.5774(5) 0.4226(5) 0.4795(3) 0.0382(11) Uani 0.1667 2 d DS T P A 2
N1A N 0.5774(5) 0.4226(5) 0.4795(3) 0.0382(11) Uani 0.0833 1 d DS TU P B -1
H1AA H 0.451913 0.316189 0.485571 0.057 Uiso 0.1667 1 calc GR . . B -1
H1AB H 0.571822 0.513096 0.451033 0.057 Uiso 0.1667 1 calc GR . . B -1
H1AC H 0.628335 0.481343 0.520724 0.057 Uiso 0.1667 1 calc GR . . B -1
C1 C 0.707(3) 0.353(4) 0.4493(8) 0.0496(17) Uani 0.0833 1 d DS TU P B -1
H1A H 0.638252 0.265389 0.410226 0.074 Uiso 0.1667 1 calc GR . . B -1
H1B H 0.736420 0.279002 0.483820 0.074 Uiso 0.1667 1 calc GR . . B -1
H1C H 0.832599 0.469352 0.433747 0.074 Uiso 0.1667 1 calc GR . . B -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.01039(11) 0.00819(12) 0.01571(14) 0.00081(8) 0.00040(4) 0.00409(6)
Na1 0.0137(4) 0.0137(4) 0.0112(5) 0.000 0.000 0.00686(18)
F1 0.0131(3) 0.0131(3) 0.0383(5) 0.0020(2) -0.0020(2) 0.0029(3)
F2 0.0334(5) 0.0259(5) 0.0201(4) 0.0008(4) 0.0004(2) 0.0129(3)
C0 0.0505(17) 0.0505(17) 0.048(2) 0.000 0.000 0.0253(8)
N1B 0.0371(19) 0.0371(19) 0.031(2) 0.0036(11) -0.0036(11) 0.012(2)
N1A 0.0371(19) 0.0371(19) 0.031(2) 0.0036(11) -0.0036(11) 0.012(2)
C1 0.0505(17) 0.0505(17) 0.048(2) 0.000 0.000 0.0253(8)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
V1 F1 1.9697(5) 33_545 ?
V1 F1 1.9697(5) . ?
V1 F1 1.9697(5) 3_565 ?
V1 F1 1.9697(5) 31 ?
V1 F2 1.8842(12) 31 ?
V1 F2 1.8841(12) . ?
Na1 F2 2.2874(13) 3 ?
Na1 F2 2.2874(13) 2 ?
Na1 F2 2.2874(13) 20_556 ?
Na1 F2 2.2874(13) 21_556 ?
Na1 F2 2.2874(13) 19_556 ?
Na1 F2 2.2874(13) . ?
C0 N1B 1.436(5) 3_665 ?
C0 N1B 1.436(5) 2_655 ?
C0 N1B 1.436(5) . ?
N1A C1 1.438(5) . ?

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
F1 V1 F1 89.87(7) 33_545 . ?
F1 V1 F1 180.0 . 31 ?
F1 V1 F1 90.13(7) 33_545 31 ?
F1 V1 F1 90.13(7) . 3_565 ?
F1 V1 F1 180.0 33_545 3_565 ?
F1 V1 F1 89.87(6) 31 3_565 ?
F2 V1 F1 89.64(5) . . ?
F2 V1 F1 90.36(5) 31 3_565 ?
F2 V1 F1 90.36(5) 31 . ?
F2 V1 F1 90.36(5) . 31 ?
F2 V1 F1 89.64(5) . 3_565 ?
F2 V1 F1 89.64(5) 31 33_545 ?
F2 V1 F1 89.64(5) 31 31 ?
F2 V1 F1 90.36(5) . 33_545 ?
F2 V1 F2 180.0 31 . ?
F2 Na1 F2 90.19(5) 20_556 . ?
F2 Na1 F2 89.81(4) 2 . ?
F2 Na1 F2 89.81(4) 2 3 ?
F2 Na1 F2 180.00(5) 21_556 3 ?
F2 Na1 F2 89.81(4) 20_556 21_556 ?
F2 Na1 F2 90.19(4) 21_556 . ?
F2 Na1 F2 89.81(4) 21_556 19_556 ?
F2 Na1 F2 180.0 20_556 2 ?
F2 Na1 F2 90.19(4) 20_556 3 ?
F2 Na1 F2 90.19(5) 2 19_556 ?
F2 Na1 F2 90.19(4) 3 19_556 ?
F2 Na1 F2 90.19(4) 2 21_556 ?
F2 Na1 F2 89.81(4) 20_556 19_556 ?
F2 Na1 F2 180.0 19_556 . ?
F2 Na1 F2 89.81(4) 3 . ?
V1 F1 V1 146.02(6) . 2_665 ?
V1 F2 Na1 134.89(7) . . ?
N1B C0 N1B 89.3(7) 3_665 2_655 ?
N1B C0 N1B 89.3(7) 3_665 . ?
N1B C0 N1B 89.3(7) 2_655 . ?

_iucr_refine_instructions_details 
;
TITL a616_0m_a.res in R-3m
    a616_0m.res
    created by SHELXL-2017/1 at 11:06:29 on 20-Nov-2019
REM Old TITL A616_0m in R-3m
REM SHELXT solution in R-3m: R1 0.090, Rweak 0.008, Alpha 0.018
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: N2 F12 Na V3
CELL 0.71073 7.5349 7.5349 19.0999 90 90 120
ZERR 2.99988 0.0013 0.0013 0.0032 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SFAC C H F N Na V
UNIT 6 36 36 6 3 9
DFIX 1.45 0.005 N1A C1
SADI 0.002 N1A C1 N1B C0
RIGU 0.002 0.002 N1A C1
ISOR 0.002 0.004 C1
ISOR 0.002 0.004 C0
EADP C1 C0
EADP N1A N1B
EXYZ N1A N1B

L.S. 20 0 0
PLAN  20
TEMP 26.05
list 4
fmap 2 53
acta
OMIT -2 2 5
OMIT -3 6 3
OMIT -1 1 1
OMIT 0 0 12
OMIT 0 2 4
REM <olex2.extras>
REM <HklSrc "%.\\A616_0m.hkl">
REM </olex2.extras>

WGHT    0.028100    1.910800
FVAR       0.39769
V1    6    0.166667    0.333333    0.333333    10.25000    0.01039    0.00819 =
         0.01571    0.00081    0.00040    0.00409
NA1   5    0.000000    0.000000    0.500000    10.08333    0.01371    0.01371 =
         0.01125    0.00000    0.00000    0.00686
F1    3    0.456703    0.543297    0.345978    10.50000    0.01307    0.01307 =
         0.03830    0.00197   -0.00197    0.00289
F2    3    0.142868    0.285736    0.430626    10.50000    0.03338    0.02586 =
         0.02013    0.00076    0.00038    0.01293
PART 2
C0    1    0.666667    0.333333    0.435589    10.08333    0.05053    0.05053 =
         0.04779    0.00000    0.00000    0.02527
N1B   4    0.577415    0.422585    0.479541    10.08333    0.03706    0.03706 =
         0.03110    0.00364   -0.00364    0.01159

PART 0
PART -1
N1A   4    0.577415    0.422585    0.479541    10.08333    0.03706    0.03706 =
         0.03110    0.00364   -0.00364    0.01159
AFIX 137
H1AA  2    0.451913    0.316189    0.485571    10.16667   -1.50000
H1AB  2    0.571822    0.513096    0.451033    10.16667   -1.50000
H1AC  2    0.628335    0.481343    0.520724    10.16667   -1.50000
AFIX   0
C1    1    0.706930    0.353329    0.449323    10.08333    0.05053    0.05053 =
         0.04779    0.00000    0.00000    0.02527
AFIX 137
H1A   2    0.638252    0.265389    0.410226    10.16667   -1.50000
H1B   2    0.736420    0.279002    0.483820    10.16667   -1.50000
H1C   2    0.832599    0.469352    0.433747    10.16667   -1.50000
AFIX   0
HKLF 4




REM  a616_0m_a.res in R-3m
REM R1 =  0.0300 for     707 Fo > 4sig(Fo)  and  0.0340 for all     761 data
REM     33 parameters refined using     17 restraints

END  
     
WGHT      0.0281      1.9097 

REM Highest difference peak  1.002,  deepest hole -1.119,  1-sigma level  0.110
Q1    1   0.6667  0.3333  0.3333  10.08333  0.05    1.00
Q2    1   0.1056  0.2111  0.4478  10.50000  0.05    0.78
Q3    1   0.6667  0.3333  0.5045  10.16667  0.05    0.58
Q4    1   0.5000  0.5000  0.5000  10.25000  0.05    0.53
Q5    1   0.1343  0.2686  0.4665  10.50000  0.05    0.43
Q6    1   0.0747  0.3333  0.3333  10.50000  0.05    0.42
Q7    1   0.5721  0.4279  0.3200  10.50000  0.05    0.36
Q8    1   0.3795  0.4398  0.3308  11.00000  0.05    0.36
Q9    1   0.3436  0.4451  0.3402  11.00000  0.05    0.34
Q10   1   0.7116  0.2884  0.3533  10.50000  0.05    0.34
Q11   1   0.5317  0.4683  0.4282  10.50000  0.05    0.34
Q12   1   0.2573  0.3759  0.3737  11.00000  0.05    0.32
Q13   1   0.6667  0.2383  0.3333  10.50000  0.05    0.30
Q14   1   0.7843  0.5685  0.3787  10.50000  0.05    0.28
Q15   1   0.1083  0.2166  0.3997  10.50000  0.05    0.28
Q16   1   0.6667  0.3333  0.3828  10.16667  0.05    0.27
Q17   1   0.2934  0.4900  0.3255  11.00000  0.05    0.27
Q18   1   0.5946  0.1893  0.3790  10.50000  0.05    0.26
Q19   1   0.4784  0.6343  0.3517  11.00000  0.05    0.26
Q20   1   0.3756  0.1878  0.4496  10.50000  0.05    0.25

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0300 for 707 Fo > 4sig(Fo) and 0.0340 for all 3703 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.00, deepest hole -1.12
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0340
  REM R1_gt = 0.0300
  REM wR_ref = 0.0761
  REM GOOF = 1.110
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3703
  REM Reflections_gt = 707
  REM Parameters = n/a
  REM Hole = -1.12
  REM Peak = 1.00
  REM Flack = n/a
;
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id C2N2H12NaV3F12
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_a617_0m
_database_code_depnum_ccdc_archive 'CCDC 1987389'
loop_
_audit_author_name
_audit_author_address
'Ningxin Jiang'
;Georgia Institute of Technology
United States of America
;
_audit_update_record             
;
2020-05-20 deposited with the CCDC.	2020-09-30 downloaded from the CCDC.
;
_audit_creation_date             2020-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
njiang48@gatech.edu
''
_chemical_name_common            ?
_chemical_name_systematic        C2N2H12NaV3F12
_chemical_formula_moiety         'F12 Na1 V3, 0.333(C3 N3), 2(C0.5 H6 N0.5)'
_chemical_formula_sum            'C2 H12 F12 N2 Na V3'
_chemical_formula_weight         467.96
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   7.5156(5)
_cell_length_b                   7.5156(5)
_cell_length_c                   19.0063(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     929.73(14)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.19
_cell_measurement_theta_min      3.22
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.389
_exptl_absorpt_correction_T_max  0.7875
_exptl_absorpt_correction_T_min  0.7290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1015 before and 0.0778 after correction. The Ratio of minimum to maximum transmission is 0.9257. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             678
_exptl_crystal_preparation       'Hydrothermal reaction,Magnetic properties'
_exptl_crystal_recrystallization_method 'Hydrothermal reaction'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.124
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3120
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.192
_diffrn_reflns_theta_min         3.216
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_special_details          N.A.
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                710
_reflns_number_total             761
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         761
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0321
_refine_ls_restrained_S_all      1.177
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0305P)²+2.7586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0802
_refine_special_details          N.A.
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N1A, N1B}
3. Restrained distances
 N1A-C1
 1.45 with sigma of 0.005
 N1A-C1 \\sim N1B-C0
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C0) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1) = Uanis(C0)
Uanis(N1A) = Uanis(N1B)
5. Rigid body (RIGU) restrains
 N1A, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C0(0.08333) N1B(0.08333) N1A(0.08333) H1AA(0.16667) H1AB(0.16667)
 H1AC(0.16667) C1(0.08333) H1A(0.16667) H1C(0.16667) H1D(0.16667)
7.a Idealised Me refined as rotating group:
 N1A(H1AA,H1AB,H1AC), C1(H1A,H1C,H1D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.833333 0.666667 0.666667 0.00587(9) Uani 1 4 d S T P . .
Na1 Na 1.000000 1.000000 0.500000 0.0042(2) Uani 1 12 d S T P . .
F2 F 0.54309(8) 0.45691(8) 0.65360(6) 0.01254(18) Uani 1 2 d S T P . .
F1 F 0.85785(9) 0.71570(19) 0.56903(5) 0.01439(19) Uani 1 2 d S T P . .
C0 C 0.666667 0.333333 0.4388(5) 0.0261(13) Uani 0.5 6 d DS TU P A 2
N1B N 0.5755(4) 0.4245(4) 0.4806(2) 0.0197(8) Uani 0.1667 2 d DS T P A 2
N1A N 0.5755(4) 0.4245(4) 0.4806(2) 0.0197(8) Uani 0.0833 1 d DS . P B -1
H1AA H 0.499217 0.438111 0.447554 0.024 Uiso 0.1667 1 calc R U P B -1
H1AB H 0.653702 0.545048 0.501504 0.024 Uiso 0.1667 1 calc R U P B -1
H1AC H 0.493978 0.332856 0.512337 0.024 Uiso 0.1667 1 calc R U P B -1
C1 C 0.7036(19) 0.356(3) 0.4490(7) 0.0261(13) Uani 0.0833 1 d D U P B -1
H1A H 0.821153 0.470849 0.428012 0.039 Uiso 0.1667 1 calc R U P B -1
H1C H 0.627356 0.255723 0.413409 0.039 Uiso 0.1667 1 calc R U P B -1
H1D H 0.748191 0.295598 0.484296 0.039 Uiso 0.1667 1 calc R U P B -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.00509(11) 0.00415(13) 0.00804(13) 0.00049(8) 0.00024(4) 0.00207(6)
Na1 0.0042(3) 0.0042(3) 0.0040(4) 0.000 0.000 0.00211(16)
F2 0.0072(3) 0.0072(3) 0.0208(4) 0.00082(16) -0.00082(16) 0.0018(3)
F1 0.0170(4) 0.0134(4) 0.0115(3) -0.0006(3) -0.00030(16) 0.0067(2)
C0 0.0278(13) 0.0278(13) 0.0227(19) 0.000 0.000 0.0139(7)
N1B 0.0208(15) 0.0208(15) 0.0142(14) 0.0023(7) -0.0023(7) 0.0079(17)
N1A 0.0208(15) 0.0208(15) 0.0142(14) 0.0023(7) -0.0023(7) 0.0079(17)
C1 0.0278(13) 0.0278(13) 0.0227(19) 0.000 0.000 0.0139(7)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
V1 F2 1.9663(3) 27_556 ?
V1 F2 1.9663(4) 25_666 ?
V1 F2 1.9663(3) 3_665 ?
V1 F2 1.9663(3) . ?
V1 F1 1.8830(10) 25_666 ?
V1 F1 1.8830(10) . ?
Na1 F1 2.2684(12) 2_765 ?
Na1 F1 2.2684(12) 20_566 ?
Na1 F1 2.2684(12) 19_776 ?
Na1 F1 2.2684(12) 3_675 ?
Na1 F1 2.2683(12) . ?
Na1 F1 2.2684(12) 21_656 ?
C0 N1B 1.428(5) 3_665 ?
C0 N1B 1.428(5) . ?
C0 N1B 1.428(5) 2_655 ?
N1A H1AA 0.8900 . ?
N1A H1AB 0.8900 . ?
N1A H1AC 0.8900 . ?
N1A C1 1.431(4) . ?
C1 H1A 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?

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
F2 V1 F2 90.22(6) 27_556 25_666 ?
F2 V1 F2 179.999(11) 27_556 3_665 ?
F2 V1 F2 89.78(6) 25_666 3_665 ?
F2 V1 F2 180.0 25_666 . ?
F2 V1 F2 89.78(6) 27_556 . ?
F2 V1 F2 90.22(6) . 3_665 ?
F1 V1 F2 90.39(4) . 25_666 ?
F1 V1 F2 89.61(4) 25_666 27_556 ?
F1 V1 F2 90.39(4) 25_666 3_665 ?
F1 V1 F2 89.61(4) . 3_665 ?
F1 V1 F2 89.61(4) 25_666 25_666 ?
F1 V1 F2 89.61(4) . . ?
F1 V1 F2 90.39(4) 25_666 . ?
F1 V1 F2 90.39(4) . 27_556 ?
F1 V1 F1 180.00(4) 25_666 . ?
F1 Na1 F1 180.00(4) . 19_776 ?
F1 Na1 F1 90.10(4) 2_765 21_656 ?
F1 Na1 F1 90.10(4) . 21_656 ?
F1 Na1 F1 89.90(4) 20_566 19_776 ?
F1 Na1 F1 89.90(4) . 3_675 ?
F1 Na1 F1 180.0 20_566 2_765 ?
F1 Na1 F1 90.10(4) 2_765 19_776 ?
F1 Na1 F1 89.90(4) 20_566 21_656 ?
F1 Na1 F1 89.90(4) . 2_765 ?
F1 Na1 F1 89.90(4) 21_656 19_776 ?
F1 Na1 F1 89.90(4) 2_765 3_675 ?
F1 Na1 F1 90.10(4) 20_566 3_675 ?
F1 Na1 F1 90.10(4) 3_675 19_776 ?
F1 Na1 F1 180.0 21_656 3_675 ?
F1 Na1 F1 90.10(4) . 20_566 ?
V1 F2 V1 145.70(6) . 2_655 ?
V1 F1 Na1 135.10(6) . . ?
N1B C0 N1B 92.1(5) 3_665 2_655 ?
N1B C0 N1B 92.1(5) 3_665 . ?
N1B C0 N1B 92.1(5) 2_655 . ?
H1AA N1A H1AB 109.5 . . ?
H1AA N1A H1AC 109.5 . . ?
H1AB N1A H1AC 109.5 . . ?
C1 N1A H1AA 109.5 . . ?
C1 N1A H1AB 109.5 . . ?
C1 N1A H1AC 109.5 . . ?
N1A C1 H1A 109.5 . . ?
N1A C1 H1C 109.5 . . ?
N1A C1 H1D 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1A C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F2 V1 F1 Na1 45.11(3) 27_556 . . . ?
F2 V1 F1 Na1 -45.11(3) 25_666 . . . ?
F2 V1 F1 Na1 134.89(3) . . . . ?
F2 V1 F1 Na1 -134.89(3) 3_665 . . . ?

_shelx_res_file                  
;
TITL C2N2H12NaV3F12-100K.res in R-3m
    a617_0m.res
    created by SHELXL-2017/1 at 22:27:54 on 19-May-2020
REM Old TITL A617_0m in R-3m
REM SHELXT solution in R-3m: R1 0.092, Rweak 0.006, Alpha 0.016
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: N2 F12 Na V3
CELL 0.71073 7.5156 7.5156 19.0063 90 90 120
ZERR 2.99988 0.0005 0.0005 0.0012 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SFAC C H F N Na V
UNIT 6 36 36 6 3 9
DFIX 1.45 0.005 N1A C1
SADI 0.002 N1A C1 N1B C0
RIGU 0.002 0.002 N1A C1
ISOR 0.002 0.004 C1
ISOR 0.002 0.004 C0
EADP C1 C0
EADP N1A N1B
EXYZ N1A N1B

L.S. 20 0 0
PLAN  3
list 4
fmap 2 53
acta
MORE -1
BOND $H
CONF
OMIT -2 2 5
REM <olex2.extras>
REM <HklSrc "%.\\A617_0m.hkl">
REM </olex2.extras>

WGHT    0.030500    2.758600
FVAR       0.37575
V1    6    0.833333    0.666667    0.666667    10.25000    0.00509    0.00415 =
         0.00804    0.00049    0.00024    0.00207
NA1   5    1.000000    1.000000    0.500000    10.08333    0.00422    0.00422 =
         0.00402    0.00000    0.00000    0.00211
F2    3    0.543094    0.456906    0.653597    10.50000    0.00722    0.00722 =
         0.02084    0.00082   -0.00082    0.00184
F1    3    0.857851    0.715702    0.569029    10.50000    0.01705    0.01339 =
         0.01151   -0.00061   -0.00030    0.00670
PART 2
C0    1    0.666667    0.333333    0.438793    10.08333    0.02785    0.02785 =
         0.02272    0.00000    0.00000    0.01392
N1B   4    0.575521    0.424479    0.480578    10.08333    0.02080    0.02080 =
         0.01417    0.00228   -0.00228    0.00793

PART -1
N1A   4    0.575521    0.424479    0.480578    10.08333    0.02080    0.02080 =
         0.01417    0.00228   -0.00228    0.00793
AFIX 137
H1AA  2    0.499217    0.438111    0.447554    10.16667   -1.20000
H1AB  2    0.653702    0.545048    0.501504    10.16667   -1.20000
H1AC  2    0.493978    0.332856    0.512337    10.16667   -1.20000
AFIX   0
C1    1    0.703590    0.356032    0.448974    10.08333    0.02785    0.02785 =
         0.02272    0.00000    0.00000    0.01392
AFIX 137
H1A   2    0.821153    0.470849    0.428012    10.16667   -1.50000
H1C   2    0.627356    0.255723    0.413409    10.16667   -1.50000
H1D   2    0.748191    0.295598    0.484296    10.16667   -1.50000
AFIX   0
HKLF 4




REM  C2N2H12NaV3F12-100K.res in R-3m
REM R1 =  0.0321 for     710 Fo > 4sig(Fo)  and  0.0351 for all     761 data
REM     33 parameters refined using     17 restraints

END

WGHT      0.0305      2.7590

REM Highest difference peak  1.334,  deepest hole -1.398,  1-sigma level  0.166
Q1    1   0.8934  0.7869  0.5534  10.50000  0.05    1.01
Q2    1   0.5000  0.5000  0.5000  10.25000  0.05    0.55
Q3    1   0.5462  0.4538  0.6201  10.50000  0.05    0.50
;
_shelx_res_checksum              58533
_olex2_exptl_crystal_mounting_method N.A.
_olex2_submission_original_sample_id C2N2H12NaV3F12
_olex2_submission_special_instructions 'No special instructions were received'
