# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_LT
_database_code_depnum_ccdc_archive 'CCDC 1835794'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H16 N3 O12 Re3'
_chemical_formula_weight         892.86

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'
N N 0.0061 0.0033 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3825(8)
_cell_length_b                   11.2230(5)
_cell_length_c                   15.1415(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.205(6)
_cell_angle_gamma                90
_cell_volume                     1764.32(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12840
_cell_measurement_theta_min      2.989
_cell_measurement_theta_max      27.474

_exptl_crystal_description       block
_exptl_crystal_colour            coroless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.361
_exptl_crystal_F_000             1600.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    20.595
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12840
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.989
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4043
_reflns_number_gt                3576
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²+1.5465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00239(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3997
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1212
_refine_ls_wR_factor_gt          0.1161
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Re1 Re 0.75845(4) 0.26285(4) 0.48275(3) 0.02804(16) Uani 1 1 d . . . . .
Re2 Re 0.99856(4) 0.52635(4) 0.25267(3) 0.02635(16) Uani 1 1 d . . . . .
Re3 Re 0.48859(4) 0.03291(4) 0.24323(3) 0.03179(17) Uani 1 1 d . . . . .
O2 O 0.6719(8) 0.3549(8) 0.5509(5) 0.038(2) Uani 1 1 d . . . . .
O3 O 1.0699(8) 0.5625(8) 0.3509(6) 0.042(2) Uani 1 1 d . . . . .
O4 O 0.8646(8) 0.3446(7) 0.4216(6) 0.043(2) Uani 1 1 d . . . . .
O5 O 1.0685(8) 0.6109(7) 0.1712(6) 0.043(2) Uani 1 1 d . . . . .
O6 O 0.8372(8) 0.5583(8) 0.2562(6) 0.045(2) Uani 1 1 d . . . . .
O7 O 0.6535(8) 0.1907(8) 0.4128(6) 0.045(2) Uani 1 1 d . . . . .
O9 O 0.4048(8) -0.0333(8) 0.1591(6) 0.046(2) Uani 1 1 d . . . . .
O10 O 0.4370(9) -0.0266(9) 0.3398(6) 0.055(3) Uani 1 1 d . . . . .
O11 O 0.8397(9) 0.1620(8) 0.5472(6) 0.050(2) Uani 1 1 d . . . . .
O12 O 0.4623(9) 0.1840(8) 0.2407(6) 0.053(3) Uani 1 1 d . . . . .
O13 O 0.6499(8) 0.0044(9) 0.2289(6) 0.045(2) Uani 1 1 d . . . . .
O14 O 1.0202(8) 0.3767(8) 0.2318(6) 0.044(2) Uani 1 1 d . . . . .
N1 N 0.7498(8) 0.2747(9) 0.2313(6) 0.035(2) Uani 1 1 d . . . . .
N2 N 0.2528(9) 0.1233(9) 0.9366(6) 0.035(2) Uani 1 1 d . . . . .
H2C H 0.2519 0.0491 0.9023 0.042 Uiso 1 1 calc R U . . .
N3 N 0.2536(8) 0.3115(8) 1.0222(5) 0.0226(18) Uani 1 1 d . . . . .
C7 C 0.2571(14) 0.4238(10) 1.0741(9) 0.048(3) Uani 1 1 d . . . . .
H7A H 0.3132 0.4799 1.0458 0.072 Uiso 1 1 calc R U . . .
H7B H 0.2884 0.4074 1.1326 0.072 Uiso 1 1 calc R U . . .
H7C H 0.1719 0.4566 1.0775 0.072 Uiso 1 1 calc R U . . .
C4 C 0.2139(17) 0.2235(13) 0.8773(10) 0.063(5) Uani 1 1 d . . . . .
H4A H 0.1299 0.2082 0.8515 0.076 Uiso 1 1 calc R U . . .
H4B H 0.2759 0.2334 0.8301 0.076 Uiso 1 1 calc R U . . .
C3 C 0.1699(17) 0.2234(13) 1.0627(12) 0.071(5) Uani 1 1 d . . . . .
H3A H 0.0845 0.2571 1.0697 0.085 Uiso 1 1 calc R U . . .
H3B H 0.2027 0.2041 1.1211 0.085 Uiso 1 1 calc R U . . .
C6 C 0.1604(14) 0.1121(12) 1.0095(10) 0.055(4) Uani 1 1 d . . . . .
H6A H 0.1812 0.0434 1.0457 0.065 Uiso 1 1 calc R U . . .
H6B H 0.0737 0.1025 0.9866 0.065 Uiso 1 1 calc R U . . .
C5 C 0.3835(12) 0.1425(14) 0.9712(11) 0.065(5) Uani 1 1 d . . . . .
H5A H 0.4454 0.1442 0.9234 0.078 Uiso 1 1 calc R U . . .
H5B H 0.4072 0.0793 1.0118 0.078 Uiso 1 1 calc R U . . .
C2 C 0.3806(16) 0.2617(14) 1.0186(12) 0.070(5) Uani 1 1 d . . . . .
H2A H 0.4130 0.2513 1.0783 0.084 Uiso 1 1 calc R U . . .
H2B H 0.4373 0.3169 0.9885 0.084 Uiso 1 1 calc R U . . .
C1 C 0.2099(17) 0.3347(12) 0.9354(9) 0.061(4) Uani 1 1 d . . . . .
H1A H 0.2632 0.3962 0.9093 0.073 Uiso 1 1 calc R U . . .
H1B H 0.1222 0.3644 0.9377 0.073 Uiso 1 1 calc R U . . .


_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
Re1 O4 1.709(8) . ?
Re1 O11 1.715(8) . ?
Re1 O2 1.717(8) . ?
Re1 O7 1.719(8) . ?
Re2 O3 1.708(8) . ?
Re2 O6 1.715(8) . ?
Re2 O5 1.720(8) . ?
Re2 O14 1.724(9) . ?
Re3 O10 1.696(9) . ?
Re3 O9 1.710(8) . ?
Re3 O12 1.718(9) . ?
Re3 O13 1.719(8) . ?
N2 C6 1.471(15) . ?
N2 C5 1.469(14) . ?
N2 C4 1.493(16) . ?
N3 C1 1.413(15) . ?
N3 C2 1.434(17) . ?
N3 C3 1.454(17) . ?
N3 C7 1.485(13) . ?
C4 C1 1.528(19) . ?
C3 C6 1.489(18) . ?
C5 C2 1.518(18) . ?

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
O4 Re1 O11 110.2(4) . . ?
O4 Re1 O2 110.0(4) . . ?
O11 Re1 O2 108.2(4) . . ?
O4 Re1 O7 109.1(4) . . ?
O11 Re1 O7 110.5(4) . . ?
O2 Re1 O7 108.7(4) . . ?
O3 Re2 O6 110.1(4) . . ?
O3 Re2 O5 108.1(4) . . ?
O6 Re2 O5 108.8(4) . . ?
O3 Re2 O14 109.6(4) . . ?
O6 Re2 O14 109.7(4) . . ?
O5 Re2 O14 110.5(4) . . ?
O10 Re3 O9 108.0(5) . . ?
O10 Re3 O12 110.9(5) . . ?
O9 Re3 O12 109.4(4) . . ?
O10 Re3 O13 110.3(4) . . ?
O9 Re3 O13 108.6(4) . . ?
O12 Re3 O13 109.6(5) . . ?
C6 N2 C5 110.4(11) . . ?
C6 N2 C4 109.8(11) . . ?
C5 N2 C4 110.5(12) . . ?
C1 N3 C2 109.2(12) . . ?
C1 N3 C3 109.1(12) . . ?
C2 N3 C3 107.6(12) . . ?
C1 N3 C7 110.1(10) . . ?
C2 N3 C7 109.3(9) . . ?
C3 N3 C7 111.5(10) . . ?
N2 C4 C1 106.1(12) . . ?
N3 C3 C6 112.4(12) . . ?
N2 C6 C3 107.0(11) . . ?
N2 C5 C2 106.2(11) . . ?
N3 C2 C5 112.4(12) . . ?
N3 C1 C4 112.1(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1B O5 0.97 2.59 3.361(17) 136.9 3_666
C1 H1A O10 0.97 2.55 3.51(2) 168.9 4_566
C2 H2B O7 0.97 2.53 3.30(2) 137.2 4_566
C2 H2A O12 0.97 2.62 3.57(2) 167.0 1_556
C5 H5B O9 0.97 2.56 3.47(2) 155.3 1_556
C5 H5A O9 0.97 2.35 3.203(17) 145.7 3_656
C6 H6B O4 0.97 2.45 3.378(17) 159.3 4_466
C6 H6A O4 0.97 2.33 3.189(15) 146.5 2_646
C3 H3B O6 0.97 2.51 3.31(2) 139.6 2_646
C4 H4B O12 0.97 2.54 3.47(2) 160.6 4_566
C4 H4A O14 0.97 2.34 3.184(17) 145.0 4_466
C7 H7C O5 0.96 2.48 3.229(15) 134.3 1_456
C7 H7B O13 0.96 2.45 3.260(15) 142.4 2_656
C7 H7A O7 0.96 2.47 3.143(14) 126.8 2_656

_refine_diff_density_max         2.003
_refine_diff_density_min         -2.617
_refine_diff_density_rms         0.334

####################################################################### 
# 
# 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_HT
_database_code_depnum_ccdc_archive 'CCDC 1835795'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 N O12 Re3'
_chemical_formula_weight         848.71
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'
N N 0.0061 0.0033 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   7.699(4)
_cell_length_b                   7.699(4)
_cell_length_c                   7.699(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     456.4(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    403(2)
_cell_measurement_reflns_used    1677
_cell_measurement_theta_min      3.743
_cell_measurement_theta_max      27.341

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.088
_exptl_crystal_F_000             370.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    19.893
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      403(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1677
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.743
_diffrn_reflns_theta_max         27.341
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             139
_reflns_number_gt                137
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0645P)²+1.0323P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.041(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         139
_refine_ls_number_parameters     16
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.352
_refine_ls_restrained_S_all      1.342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Re1 Re 0.5000 0.5000 0.0000 0.0898(15) Uani 1 16 d S T P . .
N1 N 0.5000 0.5000 0.5000 0.088(15) Uani 1 48 d S T P . .
O1 O 0.322(4) 0.5000 0.132(4) 0.122(8) Uani 0.5 2 d S T P . .
C1 C 0.0000 0.11789(6) 0.0000 0.68(18) Uani 1 8 d DS T P . .
C2 C 0.0000 0.0000 0.0000 0.20(11) Uani 1 48 d DS T P . .


_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
Re1 O1 1.70(3) 37_665 ?
Re1 O1 1.70(3) 13 ?
Re1 O1 1.70(3) 26 ?
Re1 O1 1.70(3) 2_665 ?
Re1 O1 1.70(3) 38 ?
Re1 O1 1.70(3) 25_665 ?
Re1 O1 1.70(3) 14_665 ?
Re1 O1 1.70(3) . ?
C1 C2 0.9076(6) . ?
C1 C1 1.2835(9) 33 ?
C1 C1 1.2835(9) 29 ?
C1 C1 1.2835(9) 9 ?
C1 C1 1.2835(9) 5 ?
C1 C1 1.8152(13) 25 ?
C2 C1 0.9076(6) 33 ?
C2 C1 0.9076(6) 9 ?
C2 C1 0.9076(6) 29 ?
C2 C1 0.9076(6) 5 ?
C2 C1 0.9076(6) 25 ?

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 Re1 O1 180(2) 37_665 13 ?
O1 Re1 O1 110.8(10) 37_665 26 ?
O1 Re1 O1 69.2(10) 13 26 ?
O1 Re1 O1 69.2(10) 37_665 2_665 ?
O1 Re1 O1 110.8(10) 13 2_665 ?
O1 Re1 O1 180.0 26 2_665 ?
O1 Re1 O1 106.8(19) 37_665 38 ?
O1 Re1 O1 73.2(19) 13 38 ?
O1 Re1 O1 110.8(10) 26 38 ?
O1 Re1 O1 69.2(10) 2_665 38 ?
O1 Re1 O1 110.8(10) 37_665 25_665 ?
O1 Re1 O1 69.2(10) 13 25_665 ?
O1 Re1 O1 106.8(19) 26 25_665 ?
O1 Re1 O1 73.2(19) 2_665 25_665 ?
O1 Re1 O1 110.8(10) 38 25_665 ?
O1 Re1 O1 73.2(19) 37_665 14_665 ?
O1 Re1 O1 106.8(19) 13 14_665 ?
O1 Re1 O1 69.2(10) 26 14_665 ?
O1 Re1 O1 110.8(10) 2_665 14_665 ?
O1 Re1 O1 180(2) 38 14_665 ?
O1 Re1 O1 69.2(10) 25_665 14_665 ?
O1 Re1 O1 69.2(10) 37_665 . ?
O1 Re1 O1 110.8(10) 13 . ?
O1 Re1 O1 73.2(19) 26 . ?
O1 Re1 O1 106.8(19) 2_665 . ?
O1 Re1 O1 69.2(10) 38 . ?
O1 Re1 O1 180.0 25_665 . ?
O1 Re1 O1 110.8(10) 14_665 . ?
C2 C1 C1 45.0 . 33 ?
C2 C1 C1 45.0 . 29 ?
C1 C1 C1 60.0 33 29 ?
C2 C1 C1 45.0 . 9 ?
C1 C1 C1 90.0 33 9 ?
C1 C1 C1 60.0 29 9 ?
C2 C1 C1 45.0 . 5 ?
C1 C1 C1 60.0 33 5 ?
C1 C1 C1 90.0 29 5 ?
C1 C1 C1 60.0 9 5 ?
C2 C1 C1 0.0 . 25 ?
C1 C1 C1 45.0 33 25 ?
C1 C1 C1 45.0 29 25 ?
C1 C1 C1 45.0 9 25 ?
C1 C1 C1 45.0 5 25 ?
C1 C2 C1 180.0 33 9 ?
C1 C2 C1 90.0 33 29 ?
C1 C2 C1 90.0 9 29 ?
C1 C2 C1 90.0 33 5 ?
C1 C2 C1 90.0 9 5 ?
C1 C2 C1 180.0 29 5 ?
C1 C2 C1 90.0 33 . ?
C1 C2 C1 90.0 9 . ?
C1 C2 C1 90.0 29 . ?
C1 C2 C1 90.0 5 . ?
C1 C2 C1 90.0 33 25 ?
C1 C2 C1 90.0 9 25 ?
C1 C2 C1 90.0 29 25 ?
C1 C2 C1 90.0 5 25 ?
C1 C2 C1 180.0 . 25 ?

_refine_diff_density_max         0.987
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.166

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1843340'
_audit_update_record             
;
2018-05-17 deposited with the CCDC.
2018-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H20 B3 F12 N3'
_chemical_formula_weight         406.69

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'
N N 0.0061 0.0033 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   7.4699(6)
_cell_length_b                   7.4699(6)
_cell_length_c                   7.4699(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     416.82(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    408(2)
_cell_measurement_reflns_used    123
_cell_measurement_theta_min      3.8340
_cell_measurement_theta_max      19.2050

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_F_000             184.6
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.189
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.51539
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      408(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku-oxford Xtlab synerngy'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            666
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.727
_diffrn_reflns_theta_max         29.930
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             144
_reflns_number_gt                68
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         144
_refine_ls_number_parameters     17
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.2701
_refine_ls_R_factor_gt           0.2214
_refine_ls_wR_factor_ref         0.6333
_refine_ls_wR_factor_gt          0.6111
_refine_ls_goodness_of_fit_ref   2.454
_refine_ls_restrained_S_all      2.439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
N1 N 0.0000 0.0000 -1.0000 0.136(10) Uani 1 48 d S T P . .
F1 F 0.145(2) -0.602(2) 1.0000 0.325(12) Uani 0.5 2 d S T P . .
B1 B 0.0000 -0.5000 1.0000 0.121(8) Uani 1 16 d S T P . .
C2 C 0.374(3) -0.626(3) 1.374(3) 0.271(16) Uani 0.6500(1) 6 d DS T P . .
C1 C 0.5000 -0.5000 1.259(5) 0.32(3) Uani 0.6500(1) 8 d DS T P . .


_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
F1 B1 1.33(2) . ?
F1 F1 1.53(3) 27_545 ?
F1 F1 1.53(3) 21_456 ?
F1 F1 1.53(3) 23_656 ?
B1 F1 1.33(2) 45_646 ?
B1 F1 1.33(2) 21_456 ?
B1 F1 1.33(2) 27_545 ?
B1 F1 1.33(2) 3_557 ?
B1 F1 1.33(2) 47_446 ?
B1 F1 1.33(2) 25_547 ?
B1 F1 1.33(2) 23_656 ?
C2 C1 1.587(17) 9_636 ?
C2 C1 1.587(17) 5_447 ?
C2 C1 1.587(17) . ?
C2 C2 1.89(5) 27_545 ?
C2 C2 1.89(5) 28_655 ?
C2 C2 1.89(5) 26_558 ?
C1 C2 1.587(17) 2_645 ?
C1 C2 1.587(17) 28_655 ?
C1 C2 1.587(17) 27_545 ?

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
B1 F1 F1 54.8(5) . 27_545 ?
B1 F1 F1 54.7(2) . 21_456 ?
F1 F1 F1 89.999(3) 27_545 21_456 ?
B1 F1 F1 54.7(2) . 23_656 ?
F1 F1 F1 89.999(2) 27_545 23_656 ?
F1 F1 F1 90.000(1) 21_456 23_656 ?
F1 B1 F1 180.0 45_646 21_456 ?
F1 B1 F1 70.6(5) 45_646 27_545 ?
F1 B1 F1 109.4(5) 21_456 27_545 ?
F1 B1 F1 109.4(5) 45_646 3_557 ?
F1 B1 F1 70.6(5) 21_456 3_557 ?
F1 B1 F1 180.0 27_545 3_557 ?
F1 B1 F1 109.6(10) 45_646 47_446 ?
F1 B1 F1 70.4(10) 21_456 47_446 ?
F1 B1 F1 70.6(5) 27_545 47_446 ?
F1 B1 F1 109.4(5) 3_557 47_446 ?
F1 B1 F1 70.6(5) 45_646 25_547 ?
F1 B1 F1 109.4(5) 21_456 25_547 ?
F1 B1 F1 109.6(10) 27_545 25_547 ?
F1 B1 F1 70.4(10) 3_557 25_547 ?
F1 B1 F1 70.6(5) 47_446 25_547 ?
F1 B1 F1 70.4(10) 45_646 23_656 ?
F1 B1 F1 109.6(10) 21_456 23_656 ?
F1 B1 F1 109.4(5) 27_545 23_656 ?
F1 B1 F1 70.6(5) 3_557 23_656 ?
F1 B1 F1 180.0 47_446 23_656 ?
F1 B1 F1 109.4(5) 25_547 23_656 ?
F1 B1 F1 109.4(5) 45_646 . ?
F1 B1 F1 70.6(5) 21_456 . ?
F1 B1 F1 70.4(10) 27_545 . ?
F1 B1 F1 109.6(10) 3_557 . ?
F1 B1 F1 109.4(5) 47_446 . ?
F1 B1 F1 180.0(11) 25_547 . ?
F1 B1 F1 70.6(5) 23_656 . ?
C1 C2 C1 107(2) 9_636 5_447 ?
C1 C2 C1 107(2) 9_636 . ?
C1 C2 C1 107(2) 5_447 . ?
C1 C2 C2 123(2) 9_636 27_545 ?
C1 C2 C2 53.5(11) 5_447 27_545 ?
C1 C2 C2 53.5(11) . 27_545 ?
C1 C2 C2 53.5(11) 9_636 28_655 ?
C1 C2 C2 123(2) 5_447 28_655 ?
C1 C2 C2 53.5(11) . 28_655 ?
C2 C2 C2 90.000(9) 27_545 28_655 ?
C1 C2 C2 53.5(11) 9_636 26_558 ?
C1 C2 C2 53.5(11) 5_447 26_558 ?
C1 C2 C2 123(2) . 26_558 ?
C2 C2 C2 90.000(4) 27_545 26_558 ?
C2 C2 C2 90.000(3) 28_655 26_558 ?
C2 C1 C2 73(2) 2_645 28_655 ?
C2 C1 C2 73(2) 2_645 27_545 ?
C2 C1 C2 114(4) 28_655 27_545 ?
C2 C1 C2 114(4) 2_645 . ?
C2 C1 C2 73(2) 28_655 . ?
C2 C1 C2 73(2) 27_545 . ?

_refine_diff_density_max         0.107
_refine_diff_density_min         -0.097
_refine_diff_density_rms         0.032

# start Validation Reply Form

_vrf_PLAT082_1                   
;
PROBLEM: High R1 Value ..................................       0.22 Report.  
RESPONSE: High temperature resulted in poor quality of the crystal.
;
_vrf_PLAT084_1                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.63 Report.  
RESPONSE: High temperature resulted in poor quality of the crystal.
;
_vrf_PLAT043_1                   
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      22.96 Check.  
RESPONSE: The mistake was caused by the disorder behaviour.
;
_vrf_CHEMW03_1                   
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      22.96 Check.  
RESPONSE: The mistake was caused by the disorder behaviour in high temperature.
;
# end Validation Reply Form



####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1843338'
_audit_update_record             
;
2018-05-17 deposited with the CCDC.
2018-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H20 B3 F12 N3'
_chemical_formula_weight         406.69

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'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+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'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+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-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-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-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+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'

_cell_length_a                   10.213(2)
_cell_length_b                   10.213(2)
_cell_length_c                   53.387(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4823(2)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3115
_cell_measurement_theta_min      2.7621
_cell_measurement_theta_max      27.4546

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_F_000             2472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.196
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8777
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku saturn 724'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6151
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_theta_min         3.825
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             1216
_reflns_number_gt                948
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1554P)²+30.7018P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1216
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.1254
_refine_ls_wR_factor_ref         0.3425
_refine_ls_wR_factor_gt          0.3255
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
F1 F 0.4262(5) 0.0823(5) 0.04575(13) 0.128(2) Uani 1 1 d . . . . .
F2 F 0.3718(6) 0.2539(5) 0.05601(13) 0.126(2) Uani 1 1 d . . . . .
F3 F 0.1815(4) 0.0133(4) 0.05216(8) 0.0745(13) Uani 1 1 d . . . . .
F4 F 0.3055(13) 0.1882(16) 0.0215(3) 0.083(5) Uani 0.46(4) 1 d . . P . .
F5 F 0.3074(15) 0.095(5) 0.01935(19) 0.195(15) Uani 0.54(4) 1 d . . P . .
B1 B 0.3188(5) 0.1208(5) 0.04340(9) 0.0337(11) Uani 1 1 d . . . . .
N2 N 0.3333 0.6667 0.02381(11) 0.0303(13) Uani 1 3 d S T P . .
N1 N 0.3333 0.6667 0.07102(11) 0.0346(13) Uani 1 3 d S T P . .
H21A H 0.3333 0.6667 0.0894 0.042 Uiso 1 3 calc R U P . .
C1 C 0.3333 0.6667 -0.00421(14) 0.053(2) Uani 1 3 d S T P . .
H1A H 0.2404 0.5831 -0.0102 0.079 Uiso 1 1 d R U . . .
C2 C 0.3193(5) 0.5222(4) 0.03362(9) 0.0414(11) Uani 1 1 d . . . . .
H2A H 0.2330 0.4363 0.0259 0.050 Uiso 1 1 calc R U . . .
H2B H 0.4093 0.5177 0.0294 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2994(6) 0.5151(5) 0.06155(8) 0.0430(11) Uani 1 1 d . . . . .
H3A H 0.1965 0.4398 0.0658 0.052 Uiso 1 1 calc R U . . .
H3B H 0.3671 0.4862 0.0693 0.052 Uiso 1 1 calc R U . . .
N3 N 0.0000 0.0000 0.0000 0.048(2) Uani 1 6 d S T P . .
N4 N 0.6667 0.3333 0.0833 0.046(2) Uani 1 6 d S T P . .


_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
F1 B1 1.344(6) . ?
F2 B1 1.363(6) . ?
F3 B1 1.361(5) . ?
F4 F5 0.96(4) . ?
F4 B1 1.396(11) . ?
F5 B1 1.304(11) . ?
N2 C1 1.496(9) . ?
N2 C2 1.504(4) . ?
N2 C2 1.504(4) 3_565 ?
N2 C2 1.504(4) 2_665 ?
N1 C3 1.495(5) 2_665 ?
N1 C3 1.496(5) 3_565 ?
N1 C3 1.496(5) . ?
N1 H21A 0.9800 . ?
C1 H1A 0.9599 . ?
C2 C3 1.502(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

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
F5 F4 B1 64.0(11) . . ?
F4 F5 B1 74.3(15) . . ?
F5 B1 F1 92(2) . . ?
F5 B1 F3 102.9(8) . . ?
F1 B1 F3 113.2(4) . . ?
F5 B1 F2 130(2) . . ?
F1 B1 F2 105.7(5) . . ?
F3 B1 F2 111.7(4) . . ?
F5 B1 F4 41.7(18) . . ?
F1 B1 F4 121.1(7) . . ?
F3 B1 F4 111.7(6) . . ?
F2 B1 F4 90.6(9) . . ?
C1 N2 C2 110.4(3) . . ?
C1 N2 C2 110.4(3) . 3_565 ?
C2 N2 C2 108.5(3) . 3_565 ?
C1 N2 C2 110.4(3) . 2_665 ?
C2 N2 C2 108.5(3) . 2_665 ?
C2 N2 C2 108.5(3) 3_565 2_665 ?
C3 N1 C3 109.2(3) 2_665 3_565 ?
C3 N1 C3 109.2(3) 2_665 . ?
C3 N1 C3 109.2(3) 3_565 . ?
C3 N1 H21A 109.7 2_665 . ?
C3 N1 H21A 109.7 3_565 . ?
C3 N1 H21A 109.7 . . ?
N2 C1 H1A 109.5 . . ?
C3 C2 N2 109.7(4) . . ?
C3 C2 H2A 109.7 . . ?
N2 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
N2 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C2 109.3(4) . . ?
N1 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?

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
F4 F5 B1 F1 -137.3(13) . . . . ?
F4 F5 B1 F3 108.2(11) . . . . ?
F4 F5 B1 F2 -25(2) . . . . ?
F5 F4 B1 F1 52.3(16) . . . . ?
F5 F4 B1 F3 -85.1(13) . . . . ?
F5 F4 B1 F2 161.1(13) . . . . ?
C1 N2 C2 C3 -172.8(3) . . . . ?
C2 N2 C2 C3 -51.7(4) 3_565 . . . ?
C2 N2 C2 C3 66.1(4) 2_665 . . . ?
C3 N1 C3 C2 -52.5(5) 2_665 . . . ?
C3 N1 C3 C2 66.9(4) 3_565 . . . ?
N2 C2 C3 N1 -12.1(5) . . . . ?

_refine_diff_density_max         0.514
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.085

# start Validation Reply Form


_vrf_PLAT242_3                   
;
PROBLEM:  Low    'MainMol' Ueq as Compared to Neighbors of         B1 Check.  
RESPONSE: The movement of the tetrafluoroboric acid was occurred like the t-butyl moiety.
;
# end Validation Reply Form


