# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_0_29

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate'
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.4241(6)
_cell_length_b                   7.4241(6)
_cell_length_c                   8.7784(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     419.03(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    475
_cell_measurement_theta_min      7.852
_cell_measurement_theta_max      27.58

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Data were collected at room temperature and pressure of 0.29(5)GPa
(290000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         290000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            537
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         7.88
_diffrn_reflns_theta_max         27.64
_reflns_number_total             134
_reflns_number_gt                129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0538P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.8(19)
_refine_ls_number_reflns         134
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.165
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.3123(6) 0.0377(10) Uani 1 6 d S . .
N N 0.43551(18) 0.56449(18) 0.3109(3) 0.0506(8) Uani 1 2 d S . .
H0A H 0.3686 0.4308 0.3090 0.061 Uiso 0.50 1 calc PR . .
H0B H 0.5693 0.6314 0.3118 0.061 Uiso 0.50 1 calc PR . .
F1 F 0.89899(13) 0.10101(13) 0.28449(16) 0.0582(8) Uani 1 2 d S . .
F2 F 1.0000 0.0000 0.0728(4) 0.0576(9) Uani 1 6 d S . .
B B 1.0000 0.0000 0.2304(7) 0.0403(12) Uani 1 6 d S . .

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
C 0.0387(16) 0.0387(16) 0.036(2) 0.000 0.000 0.0193(8)
N 0.0417(11) 0.0417(11) 0.070(2) 0.0022(6) -0.0022(6) 0.0221(11)
F1 0.0556(10) 0.0556(10) 0.0771(19) -0.0038(5) 0.0038(5) 0.0382(9)
F2 0.0601(13) 0.0601(13) 0.053(2) 0.000 0.000 0.0301(6)
B 0.0326(18) 0.0326(18) 0.056(4) 0.000 0.000 0.0163(9)

_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
C N 1.314(2) 3_565 ?
C N 1.314(2) 2_665 ?
C N 1.314(2) . ?
F1 B 1.383(3) . ?
F2 B 1.384(7) . ?
B F1 1.383(3) 3_765 ?
B F1 1.383(3) 2_645 ?

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
N C N 119.991(9) 3_565 2_665 ?
N C N 119.991(9) 3_565 . ?
N C N 119.991(10) 2_665 . ?
F1 B F1 108.9(3) 3_765 2_645 ?
F1 B F1 108.9(3) 3_765 . ?
F1 B F1 108.9(3) 2_645 . ?
F1 B F2 110.1(3) 3_765 . ?
F1 B F2 110.1(3) 2_645 . ?
F1 B F2 110.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.500
_diffrn_reflns_theta_full        27.64
_diffrn_measured_fraction_theta_full 0.500
_refine_diff_density_max         0.112
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.039
_database_code_depnum_ccdc_archive 'CCDC 993802'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_0_49

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate'
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.4121(4)
_cell_length_b                   7.4121(4)
_cell_length_c                   8.650(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     411.6(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    503
_cell_measurement_theta_min      6.77
_cell_measurement_theta_max      27.07

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 0.49(5)GPa
(490000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell.  
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         490000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            543
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_theta_min         6.78
_diffrn_reflns_theta_max         27.15
_reflns_number_total             84
_reflns_number_gt                76
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0448P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_number_reflns         84
_refine_ls_number_parameters     20
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_restrained_S_all      1.242
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.302(2) 0.0369(14) Uiso 1 6 d S . .
N N 0.4359(2) 0.5641(2) 0.2970(13) 0.049(4) Uani 1 2 d S . .
H0A H 0.3689 0.4305 0.2904 0.059 Uiso 0.50 1 calc PR . .
H0B H 0.5698 0.6309 0.3003 0.059 Uiso 0.50 1 calc PR . .
F1 F 0.8985(2) 0.1015(2) 0.2708(9) 0.060(4) Uani 1 2 d S . .
F2 F 1.0000 0.0000 0.0612(18) 0.071(9) Uani 1 6 d S . .
B B 1.0000 0.0000 0.220(3) 0.040(3) Uiso 1 6 d S . .

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
N 0.0464(12) 0.0464(12) 0.059(14) 0.0029(16) -0.0029(16) 0.0272(11)
F1 0.0523(10) 0.0523(10) 0.087(12) -0.0034(7) 0.0034(7) 0.0344(9)
F2 0.059(2) 0.059(2) 0.09(3) 0.000 0.000 0.0294(12)

_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
C N 1.317(3) 3_565 ?
C N 1.317(3) 2_665 ?
C N 1.317(3) . ?
F1 B 1.375(10) . ?
F2 B 1.37(2) . ?
B F1 1.375(10) 3_765 ?
B F1 1.375(10) 2_645 ?

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
N C N 119.89(11) 3_565 2_665 ?
N C N 119.89(11) 3_565 . ?
N C N 119.89(11) 2_665 . ?
F2 B F1 108.6(13) . 3_765 ?
F2 B F1 108.6(13) . 2_645 ?
F1 B F1 110.3(13) 3_765 2_645 ?
F2 B F1 108.6(13) . . ?
F1 B F1 110.3(13) 3_765 . ?
F1 B F1 110.3(13) 2_645 . ?

_diffrn_measured_fraction_theta_max 0.336
_diffrn_reflns_theta_full        27.15
_diffrn_measured_fraction_theta_full 0.336
_refine_diff_density_max         0.071
_refine_diff_density_min         -0.048
_refine_diff_density_rms         0.015
_database_code_depnum_ccdc_archive 'CCDC 993803'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_0_67

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate' 
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.4031(4)
_cell_length_b                   7.4031(4)
_cell_length_c                   8.5486(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     405.74(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    466
_cell_measurement_theta_min      9.02
_cell_measurement_theta_max      27.43

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 0.67(5)GPa
(670000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         670000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            485
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         9.06
_diffrn_reflns_theta_max         27.47
_reflns_number_total             130
_reflns_number_gt                126
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0527P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.03(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(16)
_refine_ls_number_reflns         130
_refine_ls_number_parameters     23
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_restrained_S_all      1.200
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.2986(6) 0.0337(10) Uani 1 6 d S . .
N N 0.4366(2) 0.5634(2) 0.2977(3) 0.0488(9) Uani 1 2 d S . .
H0A H 0.3695 0.4293 0.2966 0.059 Uiso 0.50 1 calc PR . .
H0B H 0.5707 0.6305 0.2983 0.059 Uiso 0.50 1 calc PR . .
F1 F 0.89878(14) 0.10122(14) 0.27163(9) 0.0534(9) Uani 1 2 d S . .
F2 F 1.0000 0.0000 0.0544(4) 0.0550(10) Uani 1 6 d S . .
B B 1.0000 0.0000 0.2155(6) 0.0368(13) Uani 1 6 d S . .

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
C 0.0352(16) 0.0352(16) 0.0308(18) 0.000 0.000 0.0176(8)
N 0.0466(11) 0.0466(11) 0.0579(19) 0.0026(6) -0.0026(6) 0.0269(12)
F1 0.0504(11) 0.0504(11) 0.0719(16) -0.0045(4) 0.0045(4) 0.0346(9)
F2 0.0601(13) 0.0601(13) 0.0447(17) 0.000 0.000 0.0300(6)
B 0.033(2) 0.033(2) 0.045(3) 0.000 0.000 0.0163(10)

_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
C N 1.324(3) 3_565 ?
C N 1.324(3) 2_665 ?
C N 1.324(3) . ?
F1 B 1.384(2) . ?
F2 B 1.377(5) . ?
B F1 1.384(2) 3_765 ?
B F1 1.384(2) 2_645 ?

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
N C N 119.997(5) 3_565 2_665 ?
N C N 119.997(5) 3_565 . ?
N C N 119.997(5) 2_665 . ?
F2 B F1 110.29(19) . 3_765 ?
F2 B F1 110.29(19) . 2_645 ?
F1 B F1 108.6(2) 3_765 2_645 ?
F2 B F1 110.29(19) . . ?
F1 B F1 108.6(2) 3_765 . ?
F1 B F1 108.6(2) 2_645 . ?

_diffrn_measured_fraction_theta_max 0.492
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.492
_refine_diff_density_max         0.076
_refine_diff_density_min         -0.097
_refine_diff_density_rms         0.024
_database_code_depnum_ccdc_archive 'CCDC 993804'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_0_78

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate' 
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'

_cell_length_a                   7.4011(5)
_cell_length_b                   7.4011(5)
_cell_length_c                   8.3856(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     397.79(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    458
_cell_measurement_theta_min      3.99
_cell_measurement_theta_max      26.20

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 0.78(5)GPa
(780000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         780000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            511
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         4.00
_diffrn_reflns_theta_max         26.24
_reflns_number_total             138
_reflns_number_gt                134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0242P)²+0.1833P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2.2(17)
_refine_ls_number_reflns         138
_refine_ls_number_parameters     28
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0522
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.170
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.2707(8) 0.0302(19) Uani 1 3 d S . .
N N 0.4572(4) 0.5868(3) 0.2718(6) 0.0456(13) Uani 1 1 d . . .
H0A H 0.5904 0.6677 0.2732 0.055 Uiso 1 1 calc R . .
H0B H 0.4051 0.4536 0.2711 0.055 Uiso 1 1 calc R . .
F1 F 0.8714(2) 0.0715(3) 0.2405(3) 0.0500(12) Uani 1 1 d . . .
F2 F 1.0000 0.0000 0.0186(6) 0.0506(18) Uani 1 3 d S . .
B B 1.0000 0.0000 0.1824(12) 0.0274(12) Uiso 1 3 d S . .

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
C 0.037(2) 0.037(2) 0.016(7) 0.000 0.000 0.0187(11)
N 0.0377(14) 0.0393(13) 0.064(4) 0.0037(15) -0.0022(14) 0.0226(12)
F1 0.0464(12) 0.0549(12) 0.060(3) 0.0020(8) 0.0077(11) 0.0338(9)
F2 0.0528(16) 0.0528(16) 0.046(7) 0.000 0.000 0.0264(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
C N 1.316(2) 2_665 ?
C N 1.316(2) 3_565 ?
C N 1.316(2) . ?
F1 B 1.388(5) . ?
F2 B 1.374(11) . ?
B F1 1.388(5) 3_765 ?
B F1 1.388(5) 2_645 ?

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
N C N 119.995(12) 2_665 3_565 ?
N C N 119.995(13) 2_665 . ?
N C N 119.995(12) 3_565 . ?
F2 B F1 110.6(4) . 3_765 ?
F2 B F1 110.6(4) . . ?
F1 B F1 108.4(5) 3_765 . ?
F2 B F1 110.6(4) . 2_645 ?
F1 B F1 108.4(5) 3_765 2_645 ?
F1 B F1 108.4(5) . 2_645 ?

_diffrn_measured_fraction_theta_max 0.378
_diffrn_reflns_theta_full        26.24
_diffrn_measured_fraction_theta_full 0.378
_refine_diff_density_max         0.049
_refine_diff_density_min         -0.077
_refine_diff_density_rms         0.015
_database_code_depnum_ccdc_archive 'CCDC 993805'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_0_81

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate' 
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'

_cell_length_a                   7.3983(10)
_cell_length_b                   7.3983(10)
_cell_length_c                   8.346(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     395.61(13)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    310
_cell_measurement_theta_min      3.97
_cell_measurement_theta_max      26.68

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 0.81(5)GPa
(810000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         780000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            342
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.01
_diffrn_reflns_theta_max         27.48
_reflns_number_total             145
_reflns_number_gt                141
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0655P)²+0.1003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   5(3)
_refine_ls_number_reflns         145
_refine_ls_number_parameters     28
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0923
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.083
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.2732(10) 0.040(2) Uani 1 3 d S . .
N N 0.4124(5) 0.5415(6) 0.2714(8) 0.0491(16) Uani 1 1 d . . .
H0A H 0.3308 0.4085 0.2691 0.059 Uiso 1 1 calc R . .
H0B H 0.5455 0.5931 0.2726 0.059 Uiso 1 1 calc R . .
F1 F 0.9295(4) 0.1293(4) 0.2390(5) 0.0542(12) Uani 1 1 d . . .
F2 F 1.0000 0.0000 0.0172(7) 0.0551(16) Uani 1 3 d S . .
B B 1.0000 0.0000 0.1833(17) 0.039(2) Uani 1 3 d S . .

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
C 0.042(2) 0.042(2) 0.036(8) 0.000 0.000 0.0211(12)
N 0.047(2) 0.045(2) 0.062(5) 0.002(2) -0.007(2) 0.028(2)
F1 0.0614(17) 0.0542(18) 0.058(3) -0.0096(19) -0.0020(14) 0.0369(15)
F2 0.0572(19) 0.0572(19) 0.051(6) 0.000 0.000 0.0286(10)
B 0.038(3) 0.038(3) 0.041(9) 0.000 0.000 0.0188(15)

_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
C N 1.319(4) 3_565 ?
C N 1.319(4) 2_665 ?
C N 1.319(4) . ?
F1 B 1.379(6) . ?
F2 B 1.386(16) . ?
B F1 1.379(6) 3_765 ?
B F1 1.379(6) 2_645 ?

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
N C N 119.99(2) 3_565 2_665 ?
N C N 119.99(2) 3_565 . ?
N C N 119.99(2) 2_665 . ?
F1 B F1 109.2(6) 3_765 2_645 ?
F1 B F1 109.2(6) 3_765 . ?
F1 B F1 109.2(6) 2_645 . ?
F1 B F2 109.7(6) 3_765 . ?
F1 B F2 109.7(6) 2_645 . ?
F1 B F2 109.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.368
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.368
_refine_diff_density_max         0.102
_refine_diff_density_min         -0.121
_refine_diff_density_rms         0.031
_database_code_depnum_ccdc_archive 'CCDC 993806'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_1_03

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate' 
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'

_cell_length_a                   7.3952(10)
_cell_length_b                   7.3952(10)
_cell_length_c                   8.2763(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     391.98(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    332
_cell_measurement_theta_min      3.99
_cell_measurement_theta_max      25.75

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 1.03(5)GPa
(1030000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell.  
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1030000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            344
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.02
_diffrn_reflns_theta_max         27.31
_reflns_number_total             127
_reflns_number_gt                114
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+1.0455P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.03(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(4)
_refine_ls_number_reflns         127
_refine_ls_number_parameters     29
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0842
_refine_ls_wR_factor_gt          0.0815
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_restrained_S_all      1.191
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.2742(11) 0.033(3) Uani 1 3 d S . .
N N 0.4099(9) 0.5388(10) 0.2719(10) 0.044(2) Uani 1 1 d . . .
H0A H 0.3267 0.4060 0.2689 0.053 Uiso 1 1 calc R . .
H0B H 0.5427 0.5885 0.2734 0.053 Uiso 1 1 calc R . .
F1 F 0.9354(6) 0.1335(7) 0.2395(4) 0.053(2) Uani 1 1 d . . .
F2 F 1.0000 0.0000 0.0160(9) 0.056(3) Uani 1 3 d S . .
B B 1.0000 0.0000 0.180(2) 0.038(4) Uani 1 3 d S . .

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
C 0.035(5) 0.035(5) 0.029(7) 0.000 0.000 0.017(3)
N 0.039(4) 0.034(4) 0.061(5) 0.006(3) -0.001(2) 0.020(3)
F1 0.057(3) 0.048(3) 0.064(4) -0.009(2) -0.0018(18) 0.035(3)
F2 0.063(4) 0.063(4) 0.041(6) 0.000 0.000 0.032(2)
B 0.033(7) 0.033(7) 0.046(10) 0.000 0.000 0.017(4)

_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
C N 1.323(7) 3_565 ?
C N 1.323(7) 2_665 ?
C N 1.323(7) . ?
F1 B 1.385(9) . ?
F2 B 1.358(19) . ?
B F1 1.385(9) 3_765 ?
B F1 1.385(9) 2_645 ?

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
N C N 119.98(3) 3_565 2_665 ?
N C N 119.98(3) 3_565 . ?
N C N 119.98(3) 2_665 . ?
F2 B F1 110.8(7) . 3_765 ?
F2 B F1 110.8(7) . 2_645 ?
F1 B F1 108.1(7) 3_765 2_645 ?
F2 B F1 110.8(7) . . ?
F1 B F1 108.1(7) 3_765 . ?
F1 B F1 108.1(7) 2_645 . ?

_diffrn_measured_fraction_theta_max 0.338
_diffrn_reflns_theta_full        27.31
_diffrn_measured_fraction_theta_full 0.338
_refine_diff_density_max         0.100
_refine_diff_density_min         -0.110
_refine_diff_density_rms         0.030
_database_code_depnum_ccdc_archive 'CCDC 993807'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_1_38

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate'  
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'

_cell_length_a                   7.3751(6)
_cell_length_b                   7.3751(6)
_cell_length_c                   8.1270(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     382.83(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    465
_cell_measurement_theta_min      4.06
_cell_measurement_theta_max      28.45

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 1.38(5)GPa
(1380000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell.  
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1380000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            470
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.06
_diffrn_reflns_theta_max         28.51
_reflns_number_total             149
_reflns_number_gt                147
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0368P)²+1.8136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.19(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(5)
_refine_ls_number_reflns         149
_refine_ls_number_parameters     29
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.312
_refine_ls_restrained_S_all      1.306
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.2784(15) 0.035(3) Uani 1 3 d S . .
N N 0.4636(10) 0.5909(11) 0.2733(8) 0.042(2) Uani 1 1 d . . .
H0A H 0.5964 0.6749 0.2667 0.050 Uiso 1 1 calc R . .
H0B H 0.4148 0.4579 0.2766 0.050 Uiso 1 1 calc R . .
F1 F 0.8656(8) 0.0641(7) 0.2410(5) 0.049(2) Uani 1 1 d . . .
F2 F 1.0000 0.0000 0.0112(9) 0.040(3) Uani 1 3 d S . .
B B 1.0000 0.0000 0.1847(19) 0.030(3) Uani 1 3 d S . .

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
C 0.037(5) 0.037(5) 0.031(6) 0.000 0.000 0.019(2)
N 0.033(5) 0.061(5) 0.040(4) -0.006(3) -0.010(3) 0.029(4)
F1 0.059(5) 0.048(3) 0.063(3) 0.012(2) 0.013(3) 0.043(3)
F2 0.042(3) 0.042(3) 0.037(4) 0.000 0.000 0.0209(16)
B 0.023(5) 0.023(5) 0.044(9) 0.000 0.000 0.012(2)

_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
C N 1.332(7) 2_665 ?
C N 1.332(7) 3_565 ?
C N 1.332(7) . ?
F1 B 1.373(7) . ?
F2 B 1.409(17) . ?
B F1 1.373(7) 3_765 ?
B F1 1.373(7) 2_645 ?

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
N C N 119.90(6) 2_665 3_565 ?
N C N 119.90(6) 2_665 . ?
N C N 119.90(6) 3_565 . ?
F1 B F1 109.5(6) 3_765 2_645 ?
F1 B F1 109.5(6) 3_765 . ?
F1 B F1 109.5(6) 2_645 . ?
F1 B F2 109.5(6) 3_765 . ?
F1 B F2 109.5(6) 2_645 . ?
F1 B F2 109.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.355
_diffrn_reflns_theta_full        28.51
_diffrn_measured_fraction_theta_full 0.355
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.048
_database_code_depnum_ccdc_archive 'CCDC 993808'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gbf4_1_87

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium tetrafluoroborate'  
;
_chemical_name_common            'guanidinium tetrafluoroborate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C H6 N3, B F4'
_chemical_formula_sum            'C H6 B F4 N3'
_chemical_formula_weight         146.90

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'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'

_cell_length_a                   7.3558(4)
_cell_length_b                   7.3558(4)
_cell_length_c                   7.989(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     374.34(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    424
_cell_measurement_theta_min      4.07
_cell_measurement_theta_max      26.66

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             222
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 1.87(5)GPa
(1870000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell.  
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1870000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            456
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         4.09
_diffrn_reflns_theta_max         26.70
_reflns_number_total             121
_reflns_number_gt                120
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0586P)²+0.1194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_number_reflns         121
_refine_ls_number_parameters     27
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0837
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_restrained_S_all      1.208
_refine_ls_shift/su_max          0.181
_refine_ls_shift/su_mean         0.088

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C C 0.3333 0.6667 0.2761(14) 0.0281(17) Uiso 1 3 d S . .
N N 0.4664(5) 0.5955(6) 0.2767(9) 0.0340(15) Uani 1 1 d . . .
H0A H 0.5994 0.6822 0.2775 0.041 Uiso 1 1 calc R . .
H0B H 0.4201 0.4626 0.2763 0.041 Uiso 1 1 calc R . .
F1 F 0.8588(3) 0.0577(3) 0.2426(5) 0.0383(14) Uani 1 1 d . . .
F2 F 1.0000 0.0000 0.0116(11) 0.041(3) Uani 1 3 d S . .
B B 1.0000 0.0000 0.1809(17) 0.023(4) Uani 1 3 d S . .

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
N 0.029(2) 0.0350(17) 0.041(5) 0.0023(19) -0.007(2) 0.0182(13)
F1 0.0357(14) 0.0399(14) 0.047(4) 0.0017(11) 0.0062(19) 0.0244(12)
F2 0.043(2) 0.043(2) 0.037(11) 0.000 0.000 0.0217(11)
B 0.026(4) 0.026(4) 0.017(18) 0.000 0.000 0.0128(18)

_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
C N 1.321(3) 2_665 ?
C N 1.321(3) 3_565 ?
C N 1.321(3) . ?
F1 B 1.394(6) . ?
F2 B 1.352(14) . ?
B F1 1.394(6) 3_765 ?
B F1 1.394(6) 2_645 ?

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
N C N 119.999(11) 2_665 3_565 ?
N C N 119.999(11) 2_665 . ?
N C N 119.999(11) 3_565 . ?
F2 B F1 110.7(6) . 3_765 ?
F2 B F1 110.7(6) . . ?
F1 B F1 108.2(6) 3_765 . ?
F2 B F1 110.7(6) . 2_645 ?
F1 B F1 108.2(6) 3_765 2_645 ?
F1 B F1 108.2(6) . 2_645 ?

_diffrn_measured_fraction_theta_max 0.332
_diffrn_reflns_theta_full        26.70
_diffrn_measured_fraction_theta_full 0.332
_refine_diff_density_max         0.063
_refine_diff_density_min         -0.085
_refine_diff_density_rms         0.021
_database_code_depnum_ccdc_archive 'CCDC 993809'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gclo4_0_38

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium perchlorate'
;
_chemical_name_common            'guanidinium perchlorate'
_chemical_melting_point          526(2)
_chemical_formula_moiety         'C H6 N3, Cl O4'
_chemical_formula_sum            'C H6 Cl N3 O4'
_chemical_formula_weight         159.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.5595(6)
_cell_length_b                   7.5595(6)
_cell_length_c                   8.7694(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     434.00(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    575
_cell_measurement_theta_min      3.853
_cell_measurement_theta_max      26.803

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             246
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Data were collected at room temperature and pressure of 0.38(5)GPa
(380000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         380000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            553
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         6.65
_diffrn_reflns_theta_max         26.85
_reflns_number_total             141
_reflns_number_gt                134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+3.8724P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.12(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(4)
_refine_ls_number_reflns         141
_refine_ls_number_parameters     23
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1295
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_restrained_S_all      1.285
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl 0.3333 0.6667 0.8970(6) 0.0367(16) Uani 1 6 d S . .
O1 O 0.2297(6) 0.4594(13) 0.9543(8) 0.049(3) Uani 1 2 d S . .
O2 O 0.3333 0.6667 0.7342(15) 0.053(4) Uani 1 6 d S . .
C C 0.6667 0.3333 0.980(2) 0.037(4) Uani 1 6 d S . .
N N 0.4676(15) 0.2338(7) 0.9799(9) 0.042(3) Uani 1 2 d S . .
H0A H 0.4019 0.1024 0.9802 0.051 Uiso 0.50 1 calc PR . .
H0B H 0.4019 0.2995 0.9797 0.051 Uiso 0.50 1 calc PR . .

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
Cl 0.0303(18) 0.0303(18) 0.049(3) 0.000 0.000 0.0152(9)
O1 0.048(4) 0.034(5) 0.060(7) 0.014(3) 0.0072(16) 0.017(2)
O2 0.062(6) 0.062(6) 0.034(10) 0.000 0.000 0.031(3)
C 0.042(6) 0.042(6) 0.025(10) 0.000 0.000 0.021(3)
N 0.038(6) 0.039(4) 0.050(8) 0.004(2) 0.007(4) 0.019(3)

_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
Cl O2 1.428(15) . ?
Cl O1 1.447(8) 3_565 ?
Cl O1 1.447(8) 2_665 ?
Cl O1 1.447(8) . ?
C N 1.303(10) 2_655 ?
C N 1.303(10) . ?
C N 1.303(10) 3_665 ?

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
O2 Cl O1 110.3(4) . 3_565 ?
O2 Cl O1 110.3(4) . 2_665 ?
O1 Cl O1 108.6(4) 3_565 2_665 ?
O2 Cl O1 110.3(4) . . ?
O1 Cl O1 108.6(4) 3_565 . ?
O1 Cl O1 108.6(4) 2_665 . ?
N C N 120.000(11) 2_655 . ?
N C N 120.000(12) 2_655 3_665 ?
N C N 120.000(8) . 3_665 ?

_diffrn_measured_fraction_theta_max 0.534
_diffrn_reflns_theta_full        26.85
_diffrn_measured_fraction_theta_full 0.534
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 993810'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gclo4_0_57

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 'guanidinium perchlorate' 
;
_chemical_name_common            'guanidinium perchlorate'
_chemical_melting_point          526(2)
_chemical_formula_moiety         'C H6 N3, Cl O4'
_chemical_formula_sum            'C H6 Cl N3 O4'
_chemical_formula_weight         159.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.5534(4)
_cell_length_b                   7.5534(4)
_cell_length_c                   8.6935(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     429.55(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    569
_cell_measurement_theta_min      7.825
_cell_measurement_theta_max      26.962

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             246
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Data were collected at room temperature and pressure of 0.57(5)GPa
(570000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond- anvil cell.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         570000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            569
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         7.81
_diffrn_reflns_theta_max         27.05
_reflns_number_total             115
_reflns_number_gt                113
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0505P)²+0.2627P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.14(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_number_reflns         115
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_restrained_S_all      1.301
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl 0.3333 0.6667 0.8971(3) 0.0325(15) Uani 1 6 d S . .
O1 O 0.2299(3) 0.4599(6) 0.9547(5) 0.042(2) Uani 1 2 d S . .
O2 O 0.3333 0.6667 0.7321(19) 0.049(3) Uiso 1 6 d S . .
C C 0.6667 0.3333 0.979(2) 0.045(5) Uani 1 6 d S . .
N N 0.4653(7) 0.2327(4) 0.9805(11) 0.047(2) Uani 1 2 d S . .
H0A H 0.3996 0.1012 0.9829 0.056 Uiso 0.50 1 calc PR . .
H0B H 0.3996 0.2984 0.9794 0.056 Uiso 0.50 1 calc PR . .

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
Cl 0.0256(11) 0.0256(11) 0.046(4) 0.000 0.000 0.0128(6)
O1 0.039(2) 0.027(3) 0.057(8) 0.006(2) 0.0030(10) 0.0134(13)
C 0.030(4) 0.030(4) 0.08(2) 0.000 0.000 0.0152(18)
N 0.027(3) 0.035(2) 0.076(8) 0.0037(11) 0.007(2) 0.0134(14)

_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
Cl O2 1.434(17) . ?
Cl O1 1.443(4) 3_565 ?
Cl O1 1.443(4) 2_665 ?
Cl O1 1.443(4) . ?
C N 1.317(5) 2_655 ?
C N 1.317(5) . ?
C N 1.317(5) 3_665 ?

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
O2 Cl O1 110.3(2) . 3_565 ?
O2 Cl O1 110.3(2) . 2_665 ?
O1 Cl O1 108.6(2) 3_565 2_665 ?
O2 Cl O1 110.3(2) . . ?
O1 Cl O1 108.6(2) 3_565 . ?
O1 Cl O1 108.6(2) 2_665 . ?
N C N 119.99(4) 2_655 . ?
N C N 119.99(4) 2_655 3_665 ?
N C N 119.99(3) . 3_665 ?

_diffrn_measured_fraction_theta_max 0.440
_diffrn_reflns_theta_full        27.05
_diffrn_measured_fraction_theta_full 0.440
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.048
_database_code_depnum_ccdc_archive 'CCDC 993811'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gclo4_1_03

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium perchlorate' 
;
_chemical_name_common            'guanidinium perchlorate'
_chemical_melting_point          526(2)
_chemical_formula_moiety         'C H6 N3, Cl O4'
_chemical_formula_sum            'C H6 Cl N3 O4'
_chemical_formula_weight         159.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.5310(4)
_cell_length_b                   7.5310(4)
_cell_length_c                   8.4767(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     416.36(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    557
_cell_measurement_theta_min      9.386
_cell_measurement_theta_max      26.573

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             246
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 Data were collected at room temperature and pressure of 1.03(5)GPa
(1030000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell.
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1030000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            552
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         9.41
_diffrn_reflns_theta_max         26.61
_reflns_number_total             111
_reflns_number_gt                110
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0609P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.14(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_number_reflns         111
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_restrained_S_all      1.313
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl 0.6667 0.3333 0.1035(2) 0.0296(14) Uani 1 6 d S . .
O1 O 0.7699(3) 0.5398(5) 0.0446(6) 0.040(2) Uani 1 2 d S . .
O2 O 0.6667 0.3333 0.274(2) 0.044(2) Uiso 1 6 d S . .
C C 0.3333 0.6667 0.0172(19) 0.036(5) Uani 1 6 d S . .
N N 0.5360(7) 0.7680(3) 0.0163(10) 0.040(2) Uani 1 2 d S . .
H0A H 0.6019 0.8998 0.0152 0.048 Uiso 0.50 1 calc PR . .
H0B H 0.6019 0.7021 0.0169 0.048 Uiso 0.50 1 calc PR . .

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
Cl 0.0248(12) 0.0248(12) 0.039(4) 0.000 0.000 0.0124(6)
O1 0.0371(19) 0.027(2) 0.052(7) 0.005(2) 0.0023(11) 0.0133(12)
C 0.031(4) 0.031(4) 0.05(2) 0.000 0.000 0.0154(18)
N 0.030(3) 0.034(2) 0.054(7) 0.0024(11) 0.005(2) 0.0150(13)

_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
Cl O1 1.436(3) 3_665 ?
Cl O1 1.436(3) 2_655 ?
Cl O1 1.436(3) . ?
Cl O2 1.448(18) . ?
C N 1.322(4) 2_665 ?
C N 1.322(4) 3_565 ?
C N 1.322(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 Cl O1 108.6(3) 3_665 2_655 ?
O1 Cl O1 108.6(3) 3_665 . ?
O1 Cl O1 108.6(3) 2_655 . ?
O1 Cl O2 110.3(3) 3_665 . ?
O1 Cl O2 110.3(3) 2_655 . ?
O1 Cl O2 110.3(3) . . ?
N C N 119.997(17) 2_665 3_565 ?
N C N 119.997(17) 2_665 . ?
N C N 119.997(16) 3_565 . ?

_diffrn_measured_fraction_theta_max 0.452
_diffrn_reflns_theta_full        26.61
_diffrn_measured_fraction_theta_full 0.452
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.038
_database_code_depnum_ccdc_archive 'CCDC 993812'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gclo4_1_35

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'guanidinium perchlorate' 
;
_chemical_name_common            'guanidinium perchlorate'
_chemical_melting_point          526(2)
_chemical_formula_moiety         'C H6 N3, Cl O4'
_chemical_formula_sum            'C H6 Cl N3 O4'
_chemical_formula_weight         159.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.5123(4)
_cell_length_b                   7.5123(4)
_cell_length_c                   8.3522(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     408.21(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    550
_cell_measurement_theta_min      6.708
_cell_measurement_theta_max      27.281

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             246
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Data were collected at room temperature and pressure of 1.35(5)GPa
(1350000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1350000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            485
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         6.73
_diffrn_reflns_theta_max         28.47
_reflns_number_total             131
_reflns_number_gt                130
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0900P)²+2.1664P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.43(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.3(5)
_refine_ls_number_reflns         131
_refine_ls_number_parameters     23
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1526
_refine_ls_wR_factor_gt          0.1513
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.225
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl 0.6667 0.3333 0.1035(4) 0.0310(19) Uani 1 6 d S . .
O1 O 0.7713(8) 0.5427(16) 0.0461(10) 0.044(3) Uani 1 2 d S . .
O2 O 0.6667 0.3333 0.274(2) 0.043(4) Uani 1 6 d S . .
C C 0.3333 0.6667 0.015(2) 0.030(3) Uani 1 6 d S . .
N N 0.5370(17) 0.7685(8) 0.0152(14) 0.043(3) Uani 1 2 d S . .
H0A H 0.6031 0.9007 0.0155 0.051 Uiso 0.50 1 calc PR . .
H0B H 0.6031 0.7024 0.0150 0.051 Uiso 0.50 1 calc PR . .

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
Cl 0.029(2) 0.029(2) 0.035(3) 0.000 0.000 0.0146(10)
O1 0.044(4) 0.040(6) 0.045(9) 0.011(3) 0.0056(16) 0.020(3)
O2 0.047(6) 0.047(6) 0.036(10) 0.000 0.000 0.024(3)
C 0.031(6) 0.031(6) 0.029(9) 0.000 0.000 0.015(3)
N 0.026(6) 0.035(5) 0.064(9) 0.004(2) 0.008(4) 0.013(3)

_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
Cl O2 1.424(19) . ?
Cl O1 1.444(10) 3_665 ?
Cl O1 1.444(10) 2_655 ?
Cl O1 1.444(10) . ?
C N 1.325(11) 2_665 ?
C N 1.325(11) 3_565 ?
C N 1.325(11) . ?

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
O2 Cl O1 109.4(4) . 3_665 ?
O2 Cl O1 109.4(4) . 2_655 ?
O1 Cl O1 109.6(4) 3_665 2_655 ?
O2 Cl O1 109.4(4) . . ?
O1 Cl O1 109.6(4) 3_665 . ?
O1 Cl O1 109.6(4) 2_655 . ?
N C N 120.000(9) 2_665 3_565 ?
N C N 120.000(9) 2_665 . ?
N C N 120.000(9) 3_565 . ?

_diffrn_measured_fraction_theta_max 0.468
_diffrn_reflns_theta_full        28.47
_diffrn_measured_fraction_theta_full 0.468
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.078
_database_code_depnum_ccdc_archive 'CCDC 993813'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gclo4_1_73

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
'guanidinium perchlorate'
;
_chemical_name_common            'guanidinium perchlorate'
_chemical_melting_point          526(2)
_chemical_formula_moiety         'C H6 N3, Cl O4'
_chemical_formula_sum            'C H6 Cl N3 O4'
_chemical_formula_weight         159.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 m'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   7.4965(3)
_cell_length_b                   7.4965(3)
_cell_length_c                   8.2508(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     401.55(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    542
_cell_measurement_theta_min      6.741
_cell_measurement_theta_max      27.905

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.979
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             246
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
Data were collected at room temperature and pressure of 1.73(5)GPa
(1730000 kPa). The crystal was obtained by the in-situ crystallization 
under high pressure.The completness of data is limited due to the diamond-anvil cell. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1730000
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Gemini A Ultra'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            542
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         6.76
_diffrn_reflns_theta_max         28.63
_reflns_number_total             123
_reflns_number_gt                122
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrysAlisCCD
_computing_cell_refinement       CrysAlisRED
_computing_data_reduction        CrysAlisRED
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0588P)²+1.8261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.09(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(4)
_refine_ls_number_reflns         123
_refine_ls_number_parameters     23
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1161
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_restrained_S_all      1.250
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl 0.3333 0.6667 0.8965(4) 0.0299(14) Uani 1 6 d S . .
O1 O 0.2288(5) 0.4576(11) 0.9565(9) 0.042(3) Uani 1 2 d S . .
O2 O 0.3333 0.6667 0.7229(16) 0.038(3) Uani 1 6 d S . .
C C 0.6667 0.3333 0.981(2) 0.032(3) Uani 1 6 d S . .
N N 0.4629(14) 0.2314(7) 0.9840(13) 0.044(3) Uani 1 2 d S . .
H0A H 0.3967 0.0991 0.9883 0.053 Uiso 0.50 1 calc PR . .
H0B H 0.3966 0.2976 0.9819 0.053 Uiso 0.50 1 calc PR . .

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
Cl 0.0261(16) 0.0261(16) 0.037(3) 0.000 0.000 0.0131(8)
O1 0.033(3) 0.025(4) 0.064(7) 0.002(3) 0.0012(16) 0.013(2)
O2 0.046(5) 0.046(5) 0.023(10) 0.000 0.000 0.023(3)
C 0.029(5) 0.029(5) 0.039(11) 0.000 0.000 0.014(3)
N 0.028(4) 0.032(3) 0.071(8) 0.003(2) 0.007(4) 0.014(2)

_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
Cl O2 1.433(14) . ?
Cl O1 1.445(7) 3_565 ?
Cl O1 1.445(8) 2_665 ?
Cl O1 1.445(8) . ?
C N 1.323(9) 2_655 ?
C N 1.323(9) . ?
C N 1.323(9) 3_665 ?

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
O2 Cl O1 110.0(3) . 3_565 ?
O2 Cl O1 110.0(3) . 2_665 ?
O1 Cl O1 108.9(3) 3_565 2_665 ?
O2 Cl O1 110.0(3) . . ?
O1 Cl O1 108.9(3) 3_565 . ?
O1 Cl O1 108.9(3) 2_665 . ?
N C N 119.96(7) 2_655 . ?
N C N 119.96(7) 2_655 3_665 ?
N C N 119.96(7) . 3_665 ?

_diffrn_measured_fraction_theta_max 0.451
_diffrn_reflns_theta_full        28.63
_diffrn_measured_fraction_theta_full 0.451
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.040
_database_code_depnum_ccdc_archive 'CCDC 993814'
