# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_rs1n300a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Tris[pyrazol-3-ylpyrazine]iron(II) ditetrafluoroborate trihydrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Fe N12, 2[B F4], 3[H2 O]'
_chemical_formula_sum            'C21 H24 B2 F8 Fe N12 O3'
_chemical_formula_weight         721.99

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P 31c'

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

_cell_length_a                   12.6729(5)
_cell_length_b                   12.6729(5)
_cell_length_c                   10.9338(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1520.74(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    11971
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      30.51

_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11971
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         30.51
_reflns_number_total             2366
_reflns_number_gt                2218
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_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. 

 The asymmetric unit contains one-third of a complex cation and one-third 
 of a BF₄⁻ anion, all lying on a crystallographic three-fold axis; and, a 
 very badly disordered region, which lies within a channel running parallel to 
 the c-vector of the unit cell. These channels contain another one-third 
 equivalent BF₄⁻ ion (which is required for electroneutrality), and 
 approximately one mole equivalent of water per asymmetric unit. A SQUEEZE 
 analysis showed that the channels contain 71 electrons per formula unit, 
 which agrees well with one BF₄⁻ and 3 water molecules (71 electrons in 
 total) as predicted by elemental microanalysis.

 The strongest Fourier peaks in the disordered region were refined as a 
 partial BF₄⁻ site, whose occupancy refined to 0.10 and 0.09 against the 
 average isotropic Ueq value of the ordered BF₄⁻ ion B13-F15 
 (0.08 Å²). That corresponds to 58 % in total, of the BF₄⁻ content of 
 the disordered channels. The refined restraints B---F = 1.40(2) and F...F = 
 2.29(2) Å were applied to this residue. The remaining contents of the 
 asymmetric unit were not included in the final model, but are accounted for 
 in the density and F000 calculations.

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and all H atoms were placed in calculated positions and refined using 
 a riding model. 
;

_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)+(0.0769P)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   0.010(18)
_refine_ls_number_reflns         2366
_refine_ls_number_parameters     161
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_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
Fe1 Fe 0.6667 0.3333 0.32787(4) 0.02863(14) Uani 1 3 d S . .
N2 N 0.55412(18) 0.3678(2) 0.42350(16) 0.0345(4) Uani 1 1 d . . .
C3 C 0.4834(3) 0.3053(3) 0.5190(2) 0.0466(6) Uani 1 1 d . . .
H3 H 0.4856 0.2376 0.5486 0.056 Uiso 1 1 calc R . .
C4 C 0.4073(3) 0.3406(3) 0.5737(3) 0.0575(8) Uani 1 1 d . . .
H4 H 0.3601 0.2959 0.6399 0.069 Uiso 1 1 calc R . .
N5 N 0.3990(2) 0.4355(3) 0.5355(2) 0.0549(6) Uani 1 1 d . . .
C6 C 0.4676(3) 0.4970(3) 0.4417(3) 0.0484(6) Uani 1 1 d . . .
H6 H 0.4636 0.5639 0.4127 0.058 Uiso 1 1 calc R . .
C7 C 0.5458(2) 0.4652(2) 0.3846(2) 0.0371(5) Uani 1 1 d . . .
C8 C 0.6233(2) 0.5282(2) 0.2815(2) 0.0379(5) Uani 1 1 d . . .
N9 N 0.68321(18) 0.4744(2) 0.23615(18) 0.0333(4) Uani 1 1 d . . .
N10 N 0.75454(19) 0.54807(19) 0.14688(19) 0.0418(4) Uani 1 1 d . . .
H10 H 0.8027 0.5344 0.1030 0.050 Uiso 1 1 calc R . .
C11 C 0.7410(3) 0.6454(3) 0.1350(3) 0.0590(8) Uani 1 1 d . . .
H11 H 0.7813 0.7083 0.0790 0.071 Uiso 1 1 calc R . .
C12 C 0.6575(3) 0.6367(3) 0.2198(3) 0.0557(8) Uani 1 1 d . . .
H12 H 0.6297 0.6912 0.2332 0.067 Uiso 1 1 calc R . .
B13 B 0.6667 0.3333 0.8196(9) 0.0549(13) Uani 1 3 d S . .
F14 F 0.6667 0.3333 0.9453(4) 0.0770(11) Uani 1 3 d S . .
F15 F 0.7172(3) 0.4516(2) 0.7829(3) 0.1045(9) Uani 1 1 d . . .
B16A B 0.149(2) 0.159(2) 0.858(2) 0.053(8) Uiso 0.10 1 d PD A 1
F17A F 0.2255(16) 0.2763(17) 0.8216(17) 0.061(4) Uiso 0.10 1 d PD A 1
F18A F 0.118(4) 0.090(3) 0.758(3) 0.158(16) Uiso 0.10 1 d PD A 1
F19A F 0.205(4) 0.121(3) 0.933(3) 0.161(17) Uiso 0.10 1 d PD A 1
F20A F 0.053(3) 0.154(3) 0.913(3) 0.154(16) Uiso 0.10 1 d PD A 1
B16B B 0.124(2) 0.157(2) 0.882(2) 0.049(8) Uiso 0.09 1 d PD B 2
F17B F 0.217(3) 0.223(3) 0.807(3) 0.119(12) Uiso 0.09 1 d PD B 2
F18B F 0.029(3) 0.075(2) 0.816(2) 0.090(7) Uiso 0.09 1 d PD . 2
F19B F 0.151(3) 0.095(3) 0.961(3) 0.111(11) Uiso 0.09 1 d PD B 2
F20B F 0.089(2) 0.227(2) 0.938(2) 0.082(7) Uiso 0.09 1 d PD B 2

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
Fe1 0.02616(17) 0.02616(17) 0.0336(2) 0.000 0.000 0.01308(9)
N2 0.0310(10) 0.0366(10) 0.0353(9) 0.0033(8) 0.0056(7) 0.0165(9)
C3 0.0485(15) 0.0502(14) 0.0454(12) 0.0145(11) 0.0179(10) 0.0279(13)
C4 0.0581(18) 0.0641(19) 0.0559(16) 0.0170(13) 0.0284(14) 0.0348(16)
N5 0.0535(14) 0.0690(17) 0.0542(12) 0.0081(11) 0.0233(10) 0.0397(14)
C6 0.0515(15) 0.0567(16) 0.0521(13) 0.0105(11) 0.0170(11) 0.0383(14)
C7 0.0356(11) 0.0389(12) 0.0403(10) 0.0040(8) 0.0083(8) 0.0214(10)
C8 0.0381(12) 0.0371(12) 0.0443(11) 0.0059(9) 0.0113(9) 0.0230(11)
N9 0.0319(10) 0.0303(10) 0.0394(9) 0.0038(7) 0.0081(7) 0.0167(8)
N10 0.0420(11) 0.0416(11) 0.0449(10) 0.0107(8) 0.0182(9) 0.0232(9)
C11 0.068(2) 0.0467(15) 0.0677(18) 0.0253(13) 0.0338(16) 0.0328(14)
C12 0.067(2) 0.0448(14) 0.0686(19) 0.0191(13) 0.0284(15) 0.0376(15)
B13 0.0519(17) 0.0519(17) 0.061(3) 0.000 0.000 0.0260(8)
F14 0.0853(17) 0.0853(17) 0.060(2) 0.000 0.000 0.0427(9)
F15 0.112(2) 0.0773(16) 0.122(2) 0.0459(14) 0.0381(19) 0.0459(16)

_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
Fe1 N9 1.967(2) . ?
Fe1 N2 1.985(2) . ?
N2 C3 1.346(3) . ?
N2 C7 1.359(3) . ?
C3 C4 1.385(4) . ?
C4 N5 1.326(4) . ?
N5 C6 1.319(3) . ?
C6 C7 1.390(3) . ?
C7 C8 1.445(3) . ?
C8 N9 1.344(3) . ?
C8 C12 1.392(4) . ?
N9 N10 1.341(3) . ?
N10 C11 1.334(4) . ?
C11 C12 1.370(4) . ?
B13 F15 1.363(4) . ?
B13 F14 1.374(10) . ?
B16A F18A 1.33(2) . ?
B16A F20A 1.33(2) . ?
B16A F19A 1.33(2) . ?
B16A F17A 1.36(2) . ?
B16B F20B 1.32(2) . ?
B16B F19B 1.33(2) . ?
B16B F17B 1.34(2) . ?
B16B F18B 1.34(2) . ?
F18B F18B 1.45(4) 2 ?
F18B F18B 1.45(4) 3 ?

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
N9 Fe1 N9 96.33(8) 2_655 . ?
N9 Fe1 N2 174.09(10) . 2_655 ?
N9 Fe1 N2 88.87(9) 2_655 . ?
N9 Fe1 N2 80.25(8) . . ?
N2 Fe1 N2 94.80(7) 2_655 . ?
C3 N2 C7 116.5(2) . . ?
C3 N2 Fe1 128.31(19) . . ?
C7 N2 Fe1 115.19(15) . . ?
N2 C3 C4 120.7(3) . . ?
N5 C4 C3 122.7(2) . . ?
C6 N5 C4 116.9(2) . . ?
N5 C6 C7 122.2(3) . . ?
N2 C7 C6 120.9(2) . . ?
N2 C7 C8 114.00(19) . . ?
C6 C7 C8 125.1(2) . . ?
N9 C8 C12 110.3(2) . . ?
N9 C8 C7 114.0(2) . . ?
C12 C8 C7 135.6(2) . . ?
N10 N9 C8 105.7(2) . . ?
N10 N9 Fe1 137.08(16) . . ?
C8 N9 Fe1 116.27(15) . . ?
C11 N10 N9 111.2(2) . . ?
N10 C11 C12 108.2(2) . . ?
C11 C12 C8 104.7(2) . . ?
F15 B13 F15 111.7(4) 2_655 . ?
F15 B13 F14 107.1(4) . . ?
F18A B16A F20A 111.9(18) . . ?
F18A B16A F19A 107.7(17) . . ?
F20A B16A F19A 110.3(17) . . ?
F18A B16A F17A 107.0(17) . . ?
F20A B16A F17A 108.7(16) . . ?
F19A B16A F17A 111.1(17) . . ?
F20B B16B F19B 111.3(17) . . ?
F20B B16B F17B 111.2(17) . . ?
F19B B16B F17B 111.1(17) . . ?
F20B B16B F18B 107.0(16) . . ?
F19B B16B F18B 107.3(17) . . ?
F17B B16B F18B 108.9(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 N5 0.86 2.02 2.826(3) 156.7 5_664
C4 H4 F17A 0.93 2.55 3.383(19) 149.5 .
C4 H4 F17B 0.93 2.40 3.30(3) 163.1 .

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 992761'
#######################################################################
#
#                 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_rs1n110b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Tris[pyrazol-3-ylpyrazine]iron(II) ditetrafluoroborate trihydrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Fe N12, 2[B F4], 3[H2 O]'
_chemical_formula_sum            'C21 H24 B2 F8 Fe N12 O3'
_chemical_formula_weight         721.99

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P 31c'

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

_cell_length_a                   12.6653(9)
_cell_length_b                   12.6653(9)
_cell_length_c                   11.0258(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1531.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    13308
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      30.38

_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 This structure was obtained by rapidly quenching the crystal to 110 K.
 This procedure was only sometimes successful, as the crystal undergoes a
 reversible twinning transition undergone below ca. 240 K if cooled more 
 slowly. 

 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13308
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         30.38
_reflns_number_total             1850
_reflns_number_gt                1819
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_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. 

 The asymmetric unit contains one-third of a complex cation and one-third 
 of a BF₄⁻ anion, all lying on a crystallographic three-fold axis; and, a 
 very badly disordered region, which lies within a channel running parallel to 
 the c-vector of the unit cell. These channels contain another one-third 
 equivalent BF₄⁻ ion (which is required for electroneutrality), and 
 approximately one mole equivalent of water per asymmetric unit. A SQUEEZE 
 analysis showed that the channels contain 79 electrons per formula unit, 
 which is roughly consistent with one BF₄⁻ and 3 water molecules (71 
 electrons in total) as predicted by elemental microanalysis.

 The strongest Fourier peaks in the disordered region were refined as a 
 partial BF₄⁻ site, whose occupancy refined to 0.14 and 0.12 against the 
 average isotropic Ueq value of the ordered BF₄⁻ ion B13-B15 
 (0.04 Å²). That corresponds to 78 % in total, of the BF₄⁻ content of 
 the disordered channels. The refined restraints B---F = 1.40(2) and F...F = 
 2.29(2) Å were applied to this residue. One other Fourier peak above 
 1.0 e.Å⁻³ was also present in the same region of the model, but attempts 
 to include this in a third partial BF₄⁻ site were not successful. Hence, 
 the remaining contents of the asymmetric unit were not included in the final 
 model, but are accounted for in the density and F000 calculations.

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and all H atoms were placed in calculated positions and refined using 
 a riding model. 
;

_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)+(0.1148P)²+0.3905P] 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   0.01(2)
_refine_ls_number_reflns         1850
_refine_ls_number_parameters     161
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1444
_refine_ls_wR_factor_gt          0.1431
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.117
_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
Fe1 Fe 0.6667 0.3333 0.32839(5) 0.0137(2) Uani 1 3 d S . .
N2 N 0.5571(2) 0.3712(3) 0.4241(2) 0.0173(5) Uani 1 1 d . . .
C3 C 0.4885(3) 0.3118(3) 0.5215(3) 0.0241(7) Uani 1 1 d . . .
H3 H 0.4920 0.2438 0.5530 0.029 Uiso 1 1 calc R . .
C4 C 0.4131(4) 0.3478(4) 0.5765(3) 0.0281(8) Uani 1 1 d . . .
H4 H 0.3675 0.3047 0.6459 0.034 Uiso 1 1 calc R . .
N5 N 0.4026(3) 0.4417(3) 0.5348(3) 0.0269(6) Uani 1 1 d . . .
C6 C 0.4700(3) 0.5011(3) 0.4383(3) 0.0243(7) Uani 1 1 d . . .
H6 H 0.4654 0.5686 0.4071 0.029 Uiso 1 1 calc R . .
C7 C 0.5471(3) 0.4668(3) 0.3821(3) 0.0179(6) Uani 1 1 d . . .
C8 C 0.6241(3) 0.5287(3) 0.2782(3) 0.0201(6) Uani 1 1 d . . .
N9 N 0.6843(2) 0.4736(3) 0.2358(2) 0.0156(5) Uani 1 1 d . . .
N10 N 0.7535(3) 0.5439(3) 0.1440(2) 0.0213(5) Uani 1 1 d . . .
H10 H 0.8026 0.5287 0.1004 0.026 Uiso 1 1 calc R . .
C11 C 0.7381(4) 0.6406(4) 0.1272(4) 0.0291(8) Uani 1 1 d . . .
H11 H 0.7774 0.7022 0.0674 0.035 Uiso 1 1 calc R . .
C12 C 0.6548(4) 0.6342(4) 0.2126(4) 0.0287(8) Uani 1 1 d . . .
H12 H 0.6254 0.6894 0.2238 0.034 Uiso 1 1 calc R . .
B13 B 0.6667 0.3333 0.8195(8) 0.0240(13) Uani 1 3 d S . .
F14 F 0.6667 0.3333 0.9466(4) 0.0315(9) Uani 1 3 d S . .
F15 F 0.7163(3) 0.4524(2) 0.7782(3) 0.0411(6) Uani 1 1 d . . .
B16A B 0.1428(19) 0.1732(19) 0.8648(19) 0.040(7) Uiso 0.14 1 d PD A 1
F17A F 0.2411(13) 0.2872(17) 0.8263(14) 0.022(4) Uiso 0.14 1 d PD A 1
F18A F 0.112(2) 0.095(2) 0.765(2) 0.091(10) Uiso 0.14 1 d PD A 1
F19A F 0.1780(19) 0.1250(19) 0.9604(18) 0.054(5) Uiso 0.14 1 d PD A 1
F20A F 0.0474(14) 0.1912(15) 0.9056(15) 0.037(4) Uiso 0.14 1 d PD A 1
B16B B 0.124(2) 0.191(2) 0.893(2) 0.037(8) Uiso 0.12 1 d PD B 2
F17B F 0.228(2) 0.255(2) 0.819(2) 0.049(9) Uiso 0.12 1 d PD B 2
F18B F 0.032(2) 0.099(2) 0.822(2) 0.062(7) Uiso 0.12 1 d PD B 2
F19B F 0.148(3) 0.142(3) 0.997(2) 0.071(8) Uiso 0.12 1 d PD B 2
F20B F 0.086(2) 0.270(2) 0.939(3) 0.064(7) Uiso 0.12 1 d PD B 2

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
Fe1 0.0132(3) 0.0132(3) 0.0148(3) 0.000 0.000 0.00661(13)
N2 0.0161(13) 0.0177(13) 0.0176(10) 0.0011(9) 0.0006(9) 0.0080(11)
C3 0.0283(18) 0.0281(17) 0.0207(13) 0.0068(12) 0.0074(12) 0.0177(15)
C4 0.0273(18) 0.0327(19) 0.0259(16) 0.0091(13) 0.0135(13) 0.0162(16)
N5 0.0261(15) 0.0333(17) 0.0260(13) 0.0050(11) 0.0119(11) 0.0184(14)
C6 0.0255(17) 0.0284(18) 0.0250(14) 0.0062(12) 0.0089(11) 0.0180(15)
C7 0.0179(15) 0.0189(15) 0.0189(12) 0.0020(10) 0.0039(10) 0.0107(12)
C8 0.0215(16) 0.0209(15) 0.0211(13) 0.0038(11) 0.0065(11) 0.0130(13)
N9 0.0152(12) 0.0151(13) 0.0164(10) 0.0009(8) 0.0041(9) 0.0075(11)
N10 0.0231(14) 0.0211(14) 0.0227(12) 0.0053(9) 0.0087(10) 0.0134(12)
C11 0.032(2) 0.0238(16) 0.0345(17) 0.0127(14) 0.0166(15) 0.0164(15)
C12 0.037(2) 0.0262(18) 0.0331(18) 0.0135(15) 0.0181(14) 0.0234(17)
B13 0.023(2) 0.023(2) 0.025(3) 0.000 0.000 0.0117(10)
F14 0.0348(15) 0.0348(15) 0.025(2) 0.000 0.000 0.0174(7)
F15 0.0432(16) 0.0331(13) 0.0446(14) 0.0150(10) 0.0132(11) 0.0173(11)

_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
Fe1 N9 1.963(3) . ?
Fe1 N2 1.984(3) . ?
N2 C3 1.349(4) . ?
N2 C7 1.361(4) . ?
C3 C4 1.388(5) . ?
C4 N5 1.343(5) . ?
N5 C6 1.336(4) . ?
C6 C7 1.397(4) . ?
C7 C8 1.453(4) . ?
C8 N9 1.349(4) . ?
C8 C12 1.393(5) . ?
N9 N10 1.344(4) . ?
N10 C11 1.346(5) . ?
C11 C12 1.386(5) . ?
B13 F15 1.389(4) . ?
B13 F14 1.402(10) . ?
B16A F18A 1.39(2) . ?
B16A F19A 1.398(19) . ?
B16A F20A 1.411(19) . ?
B16A F17A 1.420(19) . ?
B16B F20B 1.40(2) . ?
B16B F18B 1.40(2) . ?
B16B F19B 1.41(2) . ?
B16B F17B 1.418(19) . ?

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
N9 Fe1 N9 95.42(10) 2_655 . ?
N9 Fe1 N2 173.42(13) . 2_655 ?
N9 Fe1 N2 90.11(12) 2_655 . ?
N9 Fe1 N2 80.47(11) . . ?
N2 Fe1 N2 94.33(10) 2_655 . ?
C3 N2 C7 116.6(3) . . ?
C3 N2 Fe1 128.4(2) . . ?
C7 N2 Fe1 114.9(2) . . ?
N2 C3 C4 121.4(3) . . ?
N5 C4 C3 122.1(3) . . ?
C6 N5 C4 116.9(3) . . ?
N5 C6 C7 121.9(3) . . ?
N2 C7 C6 121.1(3) . . ?
N2 C7 C8 114.4(3) . . ?
C6 C7 C8 124.5(3) . . ?
N9 C8 C12 110.9(3) . . ?
N9 C8 C7 113.2(3) . . ?
C12 C8 C7 135.8(3) . . ?
N10 N9 C8 105.6(3) . . ?
N10 N9 Fe1 137.1(2) . . ?
C8 N9 Fe1 116.8(2) . . ?
N9 N10 C11 111.3(3) . . ?
N10 C11 C12 107.8(3) . . ?
C11 C12 C8 104.4(3) . . ?
F15 B13 F14 109.1(4) 2_655 . ?
F15 B13 F14 109.1(4) . . ?
F18A B16A F19A 108.7(16) . . ?
F18A B16A F20A 114.0(16) . . ?
F19A B16A F20A 108.5(15) . . ?
F18A B16A F17A 106.0(15) . . ?
F19A B16A F17A 111.1(15) . . ?
F20A B16A F17A 108.5(15) . . ?
F20B B16B F18B 110.9(16) . . ?
F20B B16B F19B 104.3(15) . . ?
F18B B16B F19B 111.2(17) . . ?
F20B B16B F17B 110.8(16) . . ?
F18B B16B F17B 107.6(15) . . ?
F19B B16B F17B 112.0(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4 F17A 0.95 2.49 3.354(14) 150.8 .
C4 H4 F17B 0.95 2.45 3.35(2) 157.7 .
N10 H10 N5 0.88 1.98 2.810(4) 156.4 5_664

_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full        30.38
_diffrn_measured_fraction_theta_full 0.883
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.188
_database_code_depnum_ccdc_archive 'CCDC 992762'
#######################################################################
#
#                 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_rs1300ka

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Tris[pyrazol-3-ylpyrazine]iron(II) ditetrafluoroborate trihydrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Fe N12, 2[B F4], 3[H2 O]'
_chemical_formula_sum            'C21 H24 B2 F8 Fe N12 O3'
_chemical_formula_weight         721.99

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P 31c'

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

_cell_length_a                   12.6778(7)
_cell_length_b                   12.6778(7)
_cell_length_c                   10.9308(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1521.49(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    21264
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      28.87

_exptl_crystal_description       fragment
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 This measurement was taken before the crystal was cooled slowly to 150 K, 
 then rewarmed to 300 K. This was done to examine the effects of a 
 reversible twinning transition undergone by the crystal below ca. 240 K. 

 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21264
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         28.87
_reflns_number_total             2090
_reflns_number_gt                2022
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_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. 

 The asymmetric unit contains one-third of a complex cation and one-third 
 of a BF₄⁻ anion, all lying on a crystallographic three-fold axis; and, a 
 very badly disordered region, which lies within a channel running parallel to 
 the c-vector of the unit cell. These channels contain another one-third 
 equivalent BF₄⁻ ion (which is required for electroneutrality), and 
 approximately one mole equivalent of water per asymmetric unit. A SQUEEZE 
 analysis showed that the channels contain 61 electrons per formula unit, 
 which is roughly consistent with one BF₄⁻ and 2 water molecules (71 
 electrons in total) as predicted by elemental microanalysis.

 The strongest Fourier peaks in the disordered region were refined as a 
 partial BF₄⁻ site, whose occupancy refined to 10.10 (corresponding to 
 30% of the BF₄⁻ content of the disordered channels). The refined restraints 
 B---F = 1.35(2) and F...F = 2.20(2) Å were applied to this residue. There 
 were no other residual Fourier pewaks in the final model, indicating that 
 the remaining electron density in the channels is very diffuse.

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and all H atoms were placed in calculated positions and refined using 
 a riding model. 
;

_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)+(0.0876P)²+0.1630P] 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   0.04(2)
_refine_ls_number_reflns         2090
_refine_ls_number_parameters     139
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.162
_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
Fe1 Fe 0.3333 0.6667 0.44181(5) 0.02993(18) Uani 1 3 d S . .
N2 N 0.4460(2) 0.6323(2) 0.5379(2) 0.0357(5) Uani 1 1 d . . .
C3 C 0.5163(3) 0.6947(3) 0.6335(3) 0.0482(7) Uani 1 1 d . . .
H3 H 0.5132 0.7617 0.6636 0.058 Uiso 1 1 calc R . .
C4 C 0.5934(4) 0.6604(3) 0.6877(4) 0.0597(10) Uani 1 1 d . . .
H4 H 0.6416 0.7060 0.7531 0.072 Uiso 1 1 calc R . .
N5 N 0.6012(3) 0.5647(3) 0.6499(3) 0.0565(7) Uani 1 1 d . . .
C6 C 0.5325(3) 0.5032(3) 0.5558(3) 0.0509(7) Uani 1 1 d . . .
H6 H 0.5365 0.4363 0.5269 0.061 Uiso 1 1 calc R . .
C7 C 0.4540(3) 0.5350(3) 0.4983(3) 0.0382(6) Uani 1 1 d . . .
C8 C 0.3765(3) 0.4715(3) 0.3957(3) 0.0398(6) Uani 1 1 d . . .
N9 N 0.3167(2) 0.5256(2) 0.3503(2) 0.0348(5) Uani 1 1 d . . .
N10 N 0.2455(2) 0.4520(2) 0.2609(2) 0.0436(5) Uani 1 1 d . . .
H10 H 0.1979 0.4661 0.2164 0.052 Uiso 1 1 calc R . .
C11 C 0.2581(4) 0.3541(3) 0.2501(4) 0.0620(10) Uani 1 1 d . . .
H11 H 0.2172 0.2909 0.1944 0.074 Uiso 1 1 calc R . .
C12 C 0.3414(4) 0.3622(3) 0.3345(4) 0.0578(10) Uani 1 1 d . . .
H12 H 0.3686 0.3074 0.3481 0.069 Uiso 1 1 calc R . .
B13 B 0.6667 0.3333 0.4347(12) 0.0577(15) Uani 1 3 d S . .
F14 F 0.6667 0.3333 0.5589(5) 0.0774(13) Uani 1 3 d S . .
F15 F 0.5481(3) 0.2828(4) 0.3972(4) 0.1082(12) Uani 1 1 d . . .
B16 B 0.8619(18) 0.8356(17) 0.9874(18) 0.035(5) Uiso 0.10 1 d PD A 1
F17 F 0.7752(18) 0.7371(17) 0.9269(18) 0.061(5) Uiso 0.10 1 d PD A 1
F18 F 0.913(2) 0.793(3) 1.069(3) 0.096(8) Uiso 0.10 1 d PD A 1
F19 F 0.819(2) 0.900(2) 1.046(3) 0.096(9) Uiso 0.10 1 d PD A 1
F20 F 0.954(3) 0.912(2) 0.915(2) 0.107(10) Uiso 0.10 1 d PD . 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0284(2) 0.0284(2) 0.0330(3) 0.000 0.000 0.01419(10)
N2 0.0339(11) 0.0404(12) 0.0332(12) -0.0040(10) -0.0055(9) 0.0190(10)
C3 0.0491(16) 0.0546(16) 0.0455(17) -0.0142(14) -0.0174(13) 0.0293(14)
C4 0.061(2) 0.066(2) 0.058(2) -0.0180(16) -0.0287(18) 0.0359(18)
N5 0.0569(16) 0.0703(19) 0.0538(16) -0.0079(14) -0.0232(13) 0.0403(15)
C6 0.0551(17) 0.0588(18) 0.0534(19) -0.0097(14) -0.0179(14) 0.0395(16)
C7 0.0382(12) 0.0425(13) 0.0391(14) -0.0029(11) -0.0079(10) 0.0241(11)
C8 0.0398(14) 0.0407(13) 0.0459(15) -0.0060(12) -0.0100(11) 0.0253(12)
N9 0.0343(10) 0.0333(11) 0.0383(12) -0.0034(9) -0.0080(9) 0.0181(9)
N10 0.0443(12) 0.0444(12) 0.0440(13) -0.0108(10) -0.0171(11) 0.0237(11)
C11 0.074(2) 0.0481(16) 0.070(3) -0.0265(16) -0.036(2) 0.0348(16)
C12 0.070(2) 0.0466(16) 0.071(3) -0.0200(17) -0.0292(18) 0.0394(16)
B13 0.0544(19) 0.0544(19) 0.064(4) 0.000 0.000 0.0272(9)
F14 0.085(2) 0.085(2) 0.061(3) 0.000 0.000 0.0427(10)
F15 0.0814(19) 0.119(3) 0.125(3) -0.044(2) -0.0473(18) 0.0506(19)

_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
Fe1 N9 1.967(3) . ?
Fe1 N2 1.988(2) . ?
N2 C3 1.344(4) . ?
N2 C7 1.359(4) . ?
C3 C4 1.386(5) . ?
C4 N5 1.331(5) . ?
N5 C6 1.321(4) . ?
C6 C7 1.395(4) . ?
C7 C8 1.442(4) . ?
C8 N9 1.346(4) . ?
C8 C12 1.396(4) . ?
N9 N10 1.341(3) . ?
N10 C11 1.334(4) . ?
C11 C12 1.367(5) . ?
B13 F14 1.357(14) . ?
B13 F15 1.369(5) . ?
B16 F19 1.34(2) . ?
B16 F20 1.34(2) . ?
B16 F17 1.35(2) . ?
B16 F18 1.37(2) . ?

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
N9 Fe1 N9 96.43(10) 2_665 . ?
N9 Fe1 N2 174.12(12) . 2_665 ?
N9 Fe1 N2 88.83(11) 2_665 . ?
N9 Fe1 N2 80.31(10) . . ?
N2 Fe1 N2 94.67(9) 2_665 . ?
C3 N2 C7 116.9(2) . . ?
C3 N2 Fe1 128.3(2) . . ?
C7 N2 Fe1 114.76(18) . . ?
N2 C3 C4 120.8(3) . . ?
N5 C4 C3 122.6(3) . . ?
C6 N5 C4 116.9(3) . . ?
N5 C6 C7 122.4(3) . . ?
N2 C7 C6 120.4(3) . . ?
N2 C7 C8 114.5(2) . . ?
C6 C7 C8 125.1(3) . . ?
N9 C8 C12 110.3(3) . . ?
N9 C8 C7 113.8(2) . . ?
C12 C8 C7 135.8(3) . . ?
N10 N9 C8 105.6(2) . . ?
N10 N9 Fe1 137.06(19) . . ?
C8 N9 Fe1 116.36(19) . . ?
C11 N10 N9 111.1(3) . . ?
N10 C11 C12 108.5(3) . . ?
C11 C12 C8 104.5(3) . . ?
F14 B13 F15 107.4(6) . . ?
F15 B13 F15 111.4(5) 2_655 . ?
F19 B16 F20 108.2(16) . . ?
F19 B16 F17 113.7(16) . . ?
F20 B16 F17 113.0(16) . . ?
F19 B16 F18 110.2(16) . . ?
F20 B16 F18 104.9(15) . . ?
F17 B16 F18 106.4(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 N5 0.86 2.02 2.824(4) 155.8 5_564
C4 H4 F17 0.93 2.44 3.29(2) 152.3 .

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        28.87
_diffrn_measured_fraction_theta_full 0.919
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.169
_database_code_depnum_ccdc_archive 'CCDC 992763'
#######################################################################
#
#                 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_rs1300kc

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Tris[pyrazol-3-ylpyrazine]iron(II) ditetrafluoroborate trihydrate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Fe N12, 2[B F4], 3[H2 O]'
_chemical_formula_sum            'C21 H24 B2 F8 Fe N12 O3'
_chemical_formula_weight         721.99

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P 31c'

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

_cell_length_a                   12.660(2)
_cell_length_b                   12.660(2)
_cell_length_c                   10.9359(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1517.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    12294
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      28.95

_exptl_crystal_description       fragment
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 The crystal was cooled slowly to 150 K, then rewarmed to 300 K and re-measured.
 This was to examine the effects of a reversible twinning transition undergone 
 by the crystal below ca. 240 K. 

 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12294
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         28.95
_reflns_number_total             1709
_reflns_number_gt                1672
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_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. 

 The asymmetric unit contains one-third of a complex cation and one-third 
 of a BF₄⁻ anion, all lying on a crystallographic three-fold axis; and, a 
 very badly disordered region, which lies within a channel running parallel to 
 the c-vector of the unit cell. These channels contain another one-third 
 equivalent BF₄⁻ ion (which is required for electroneutrality), and 
 approximately one mole equivalent of water per asymmetric unit. A SQUEEZE 
 analysis showed that the channels contain 65 electrons per formula unit, 
 which is roughly consistent with one BF₄⁻ and 2 water molecules (71 
 electrons in total) as predicted by elemental microanalysis.

 The strongest Fourier peaks in the disordered region were refined as a 
 partial BF₄⁻ site, whose occupancy refined to 10.10 (corresponding to 
 30% of the BF₄⁻ content of the disordered channels). The refined restraints 
 B---F = 1.34(2) and F...F = 2.19(2) Å were applied to this residue. There 
 were no other residual Fourier peaks in the final model, indicating that 
 the remaining electron density in the channels is very diffuse.

 All crystallographically ordered non-H atoms were refined anisotropically, 
 and all H atoms were placed in calculated positions and refined using 
 a riding model. 
;

_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)+(0.0954P)²+0.3844P] 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   0.03(3)
_refine_ls_number_reflns         1709
_refine_ls_number_parameters     139
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1280
_refine_ls_wR_factor_gt          0.1247
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.112
_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
Fe1 Fe 0.6667 0.3333 0.79893(7) 0.0299(2) Uani 1 3 d S . .
N2 N 0.6320(3) 0.4454(3) 0.7029(3) 0.0356(6) Uani 1 1 d . . .
C3 C 0.6947(4) 0.5167(4) 0.6072(4) 0.0488(9) Uani 1 1 d . . .
H3 H 0.7623 0.5143 0.5775 0.059 Uiso 1 1 calc R . .
C4 C 0.6600(4) 0.5931(5) 0.5526(5) 0.0592(12) Uani 1 1 d . . .
H4 H 0.7050 0.6405 0.4866 0.071 Uiso 1 1 calc R . .
N5 N 0.5645(4) 0.6015(3) 0.5910(4) 0.0575(10) Uani 1 1 d . . .
C6 C 0.5034(4) 0.5325(4) 0.6851(4) 0.0511(10) Uani 1 1 d . . .
H6 H 0.4365 0.5366 0.7142 0.061 Uiso 1 1 calc R . .
C7 C 0.5346(3) 0.4540(3) 0.7422(4) 0.0388(7) Uani 1 1 d . . .
C8 C 0.4715(3) 0.3765(3) 0.8439(4) 0.0394(8) Uani 1 1 d . . .
N9 N 0.5256(3) 0.3172(2) 0.8909(3) 0.0333(6) Uani 1 1 d . . .
N10 N 0.4518(3) 0.2457(3) 0.9797(3) 0.0431(7) Uani 1 1 d . . .
H10 H 0.4656 0.1980 1.0244 0.052 Uiso 1 1 calc R . .
C11 C 0.3540(4) 0.2585(5) 0.9895(5) 0.0619(13) Uani 1 1 d . . .
H11 H 0.2904 0.2171 1.0446 0.074 Uiso 1 1 calc R . .
C12 C 0.3620(4) 0.3418(4) 0.9061(5) 0.0571(13) Uani 1 1 d . . .
H12 H 0.3073 0.3695 0.8933 0.069 Uiso 1 1 calc R . .
B13 B 0.3333 0.6667 0.8047(16) 0.0585(19) Uani 1 3 d S . .
F14 F 0.2824(4) 0.5480(3) 0.8435(5) 0.1097(14) Uani 1 1 d . . .
F15 F 0.3333 0.6667 0.6815(6) 0.0789(16) Uani 1 3 d S . .
B16 B 0.834(2) 0.866(2) 0.252(2) 0.041(8) Uiso 0.10 1 d PD . .
F17 F 0.740(2) 0.779(2) 0.315(2) 0.062(6) Uiso 0.10 1 d PD . .
F18 F 0.914(3) 0.957(3) 0.322(3) 0.097(10) Uiso 0.10 1 d PD . .
F19 F 0.895(3) 0.822(3) 0.190(3) 0.097(10) Uiso 0.10 1 d PD . .
F20 F 0.790(3) 0.915(3) 0.173(3) 0.089(9) Uiso 0.10 1 d PD . .

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
Fe1 0.0283(2) 0.0283(2) 0.0331(4) 0.000 0.000 0.01415(12)
N2 0.0382(14) 0.0330(14) 0.0355(17) 0.0059(12) 0.0051(12) 0.0177(12)
C3 0.054(2) 0.049(2) 0.047(2) 0.0195(17) 0.0142(19) 0.0282(17)
C4 0.067(3) 0.060(2) 0.056(3) 0.029(2) 0.018(2) 0.036(2)
N5 0.072(2) 0.0560(19) 0.054(2) 0.0225(16) 0.0095(18) 0.0390(18)
C6 0.058(2) 0.055(2) 0.054(3) 0.0190(18) 0.0113(18) 0.0388(19)
C7 0.0425(16) 0.0405(16) 0.0387(19) 0.0072(14) 0.0043(14) 0.0246(14)
C8 0.0403(16) 0.0411(17) 0.044(2) 0.0107(14) 0.0060(15) 0.0258(15)
N9 0.0317(13) 0.0330(12) 0.0349(16) 0.0084(12) 0.0032(12) 0.0160(10)
N10 0.0437(15) 0.0454(15) 0.0417(18) 0.0169(14) 0.0099(13) 0.0234(13)
C11 0.0482(19) 0.073(3) 0.071(3) 0.035(3) 0.026(2) 0.036(2)
C12 0.0461(19) 0.069(3) 0.069(3) 0.029(2) 0.022(2) 0.0386(19)
B13 0.057(2) 0.057(2) 0.062(6) 0.000 0.000 0.0283(12)
F14 0.121(3) 0.082(2) 0.126(4) 0.047(2) 0.041(3) 0.050(2)
F15 0.088(2) 0.088(2) 0.060(4) 0.000 0.000 0.0442(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
Fe1 N9 1.969(3) . ?
Fe1 N2 1.982(3) . ?
N2 C3 1.351(5) . ?
N2 C7 1.361(5) . ?
C3 C4 1.382(6) . ?
C4 N5 1.333(6) . ?
N5 C6 1.321(5) . ?
C6 C7 1.388(5) . ?
C7 C8 1.433(5) . ?
C8 N9 1.345(4) . ?
C8 C12 1.403(5) . ?
N9 N10 1.338(4) . ?
N10 C11 1.330(5) . ?
C11 C12 1.358(6) . ?
B13 F15 1.348(19) . ?
B13 F14 1.373(7) . ?
B16 F18 1.32(2) . ?
B16 F19 1.34(2) . ?
B16 F17 1.34(2) . ?
B16 F20 1.34(2) . ?

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
N9 Fe1 N9 96.25(12) 2_655 . ?
N9 Fe1 N2 89.22(14) . 2_655 ?
N9 Fe1 N2 173.82(14) 2_655 . ?
N9 Fe1 N2 80.26(13) . . ?
N2 Fe1 N2 94.54(12) 2_655 . ?
C3 N2 C7 116.4(3) . . ?
C3 N2 Fe1 128.5(3) . . ?
C7 N2 Fe1 115.1(2) . . ?
N2 C3 C4 121.1(4) . . ?
N5 C4 C3 122.6(4) . . ?
C6 N5 C4 116.6(4) . . ?
N5 C6 C7 122.8(4) . . ?
N2 C7 C6 120.6(4) . . ?
N2 C7 C8 114.0(3) . . ?
C6 C7 C8 125.4(3) . . ?
N9 C8 C12 109.8(3) . . ?
N9 C8 C7 114.4(3) . . ?
C12 C8 C7 135.7(3) . . ?
N10 N9 C8 106.0(3) . . ?
N10 N9 Fe1 137.0(2) . . ?
C8 N9 Fe1 115.8(3) . . ?
C11 N10 N9 110.7(3) . . ?
N10 C11 C12 109.1(4) . . ?
C11 C12 C8 104.3(3) . . ?
F15 B13 F14 108.0(7) . . ?
F14 B13 F14 110.9(7) 2_665 . ?
F18 B16 F19 107.7(17) . . ?
F18 B16 F17 113.3(17) . . ?
F19 B16 F17 112.1(17) . . ?
F18 B16 F20 106.7(17) . . ?
F19 B16 F20 109.1(17) . . ?
F17 B16 F20 107.7(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 N5 0.86 2.01 2.822(5) 156.1 6_655
C4 H4 F17 0.93 2.45 3.31(2) 152.8 .

_diffrn_measured_fraction_theta_max 0.810
_diffrn_reflns_theta_full        28.95
_diffrn_measured_fraction_theta_full 0.810
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 992764'
