#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:26:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179631 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/95/4509507.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509507
loop_
_publ_author_name
'Boldog, Ishtvan'
'Daran, Jean-Claude'
'Chernega, Alexander N.'
'Rusanov, Eduard B.'
'Krautscheid, Harald'
'Domasevitch, Konstantin V.'
_publ_section_title
;
 Hydrogen Bonding Patterns and Supramolecular Structure of
 4,4′-Bipyrazolium Salts
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2895
_journal_paper_doi               10.1021/cg9002109
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C6 H8 N4, 2(F6 Ta)'
_chemical_formula_sum            'C6 H8 F12 N4 Ta2'
_chemical_formula_weight         726.06
_chemical_name_systematic
; 
4,4'-bipyrazolium hexafluorotantalate(V)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.984(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.2630(5)
_cell_length_b                   13.6973(14)
_cell_length_c                   10.6349(11)
_cell_measurement_reflns_used    4927
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.46
_cell_volume                     747.06(13)
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.700.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'Siemens SMART CCD area-detector diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4927
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    14.770
_exptl_absorpt_correction_T_max  0.10987
_exptl_absorpt_correction_T_min  0.05933
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.0120(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0437P)²+3.1292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                1697
_reflns_number_total             2003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9002109sup1.cif
_cod_data_source_block           (8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4509507
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
N1 N 0.2156(10) 0.4439(4) 0.2442(5) 0.0286(11) Uani 1 d .
H1A H 0.1796 0.4106 0.1694 0.080 Uiso 1 d R
N2 N 0.0719(11) 0.5157(4) 0.2749(5) 0.0300(11) Uani 1 d .
H2A H -0.0781 0.5384 0.2254 0.080 Uiso 1 d R
C1 C 0.4213(12) 0.4287(5) 0.3406(6) 0.0262(11) Uani 1 d .
H1B H 0.5549 0.3805 0.3433 0.080 Uiso 1 d R
C2 C 0.4085(11) 0.4949(4) 0.4374(5) 0.0213(11) Uani 1 d .
C3 C 0.1830(13) 0.5481(5) 0.3909(6) 0.0330(14) Uani 1 d .
H3A H 0.1203 0.6006 0.4355 0.080 Uiso 1 d R
Ta1 Ta -0.60843(4) 0.687928(17) 0.04632(2) 0.02210(13) Uani 1 d .
F1 F -0.4135(9) 0.7980(3) 0.1182(5) 0.0426(11) Uani 1 d .
F2 F -0.8297(9) 0.7032(3) 0.1614(5) 0.0415(10) Uani 1 d .
F3 F -0.8090(10) 0.5791(3) -0.0301(5) 0.0497(11) Uani 1 d .
F4 F -0.3785(11) 0.6696(4) -0.0651(5) 0.0552(14) Uani 1 d .
F5 F -0.3950(8) 0.6014(3) 0.1656(4) 0.0378(9) Uani 1 d .
F6 F -0.8145(11) 0.7715(4) -0.0750(5) 0.0578(13) Uani 1 d .
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
N1 0.027(3) 0.032(3) 0.026(3) -0.003(2) 0.006(2) -0.001(2)
N2 0.028(3) 0.029(3) 0.028(2) 0.003(2) -0.005(2) 0.004(2)
C1 0.026(3) 0.027(3) 0.025(3) -0.001(2) 0.003(2) -0.001(2)
C2 0.023(3) 0.021(3) 0.017(3) 0.0016(19) -0.002(2) 0.002(2)
C3 0.037(3) 0.031(3) 0.026(3) 0.000(2) -0.002(3) 0.012(3)
Ta1 0.02158(17) 0.02109(17) 0.02269(17) -0.00030(8) 0.00302(10) -0.00017(8)
F1 0.039(2) 0.029(2) 0.062(3) -0.0122(19) 0.016(2) -0.0115(16)
F2 0.041(2) 0.044(2) 0.048(3) 0.0047(19) 0.028(2) 0.0009(18)
F3 0.043(2) 0.038(2) 0.058(3) -0.012(2) -0.010(2) -0.006(2)
F4 0.064(4) 0.065(3) 0.047(3) -0.010(2) 0.035(3) 0.004(2)
F5 0.032(2) 0.036(2) 0.039(2) 0.0047(17) -0.0058(17) 0.0071(16)
F6 0.070(3) 0.059(3) 0.041(2) 0.020(2) 0.004(2) 0.020(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
N2 N1 C1 109.7(5) .
C3 N2 N1 108.8(5) .
N1 C1 C2 107.7(5) .
C3 C2 C1 105.1(5) .
C3 C2 C2 127.6(7) 3_666
C1 C2 C2 127.3(7) 3_666
N2 C3 C2 108.7(5) .
F6 Ta1 F2 91.9(2) .
F6 Ta1 F1 88.2(2) .
F2 Ta1 F1 90.4(2) .
F6 Ta1 F4 90.1(3) .
F2 Ta1 F4 178.0(2) .
F1 Ta1 F4 89.6(2) .
F6 Ta1 F3 90.3(2) .
F2 Ta1 F3 90.0(2) .
F1 Ta1 F3 178.5(2) .
F4 Ta1 F3 90.0(2) .
F6 Ta1 F5 178.3(2) .
F2 Ta1 F5 89.7(2) .
F1 Ta1 F5 92.4(2) .
F4 Ta1 F5 88.3(2) .
F3 Ta1 F5 89.1(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 N2 1.326(7) .
N1 C1 1.329(8) .
N2 C3 1.317(8) .
C1 C2 1.385(8) .
C2 C3 1.386(8) .
C2 C2 1.464(10) 3_666
Ta1 F6 1.877(5) .
Ta1 F2 1.881(4) .
Ta1 F1 1.886(4) .
Ta1 F4 1.891(5) .
Ta1 F3 1.901(4) .
Ta1 F5 1.906(4) .
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
N1 H1A F4 0.90 2.01 2.742(7) 137.0 3_565
N1 H1A F3 0.90 2.17 2.770(7) 123.3 3_465
N2 H2A F5 0.90 1.86 2.736(7) 164.2 .
