#------------------------------------------------------------------------------
#$Date: 2019-11-24 05:12:48 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236805 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/70/7237071.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7237071
loop_
_publ_author_name
'Rok, M.'
'Szklarz, P.'
'Bator, G.'
_publ_section_title
;
 Structures and phase transitions in molecular complexes containing
 tetrafluoroboric acid and tetramethylpyrazine
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5772
_journal_paper_doi               10.1039/C8CE01231H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C8 H14 B2 F8 N2'
_chemical_formula_weight         311.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-07-17 deposited with the CCDC.
2018-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.870(4)
_cell_length_b                   9.528(3)
_cell_length_c                   12.575(5)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.7766
_cell_measurement_theta_min      3.2336
_cell_volume                     1302.4(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20344
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.863
_diffrn_reflns_theta_min         3.240
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         3199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0884P)²+0.3099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2487
_reflns_number_total             3199
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01231h1.cif
_cod_data_source_block           bf4_150
_cod_database_code               7237071
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.968
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
N N 0.05601(7) 0.50509(8) 0.40785(6) 0.02231(16) Uani 1 1 d . .
H1 H 0.093080 0.508460 0.345694 0.041(5) Uiso 1 1 calc R .
C1 C 0.02662(8) 0.62816(9) 0.45328(6) 0.02242(17) Uani 1 1 d . .
C2 C 0.03396(8) 0.37750(9) 0.44867(7) 0.02250(17) Uani 1 1 d . .
C11 C 0.05973(11) 0.76190(11) 0.39982(8) 0.0318(2) Uani 1 1 d . .
H111 H 0.103722 0.741550 0.333571 0.048 Uiso 1 1 calc R U
H112 H 0.112606 0.817523 0.446811 0.048 Uiso 1 1 calc R U
H113 H -0.015296 0.814878 0.383816 0.048 Uiso 1 1 calc R U
C21 C 0.07470(11) 0.25019(11) 0.39037(9) 0.0326(2) Uani 1 1 d . .
H211 H 0.121021 0.278109 0.326948 0.049 Uiso 1 1 calc R U
H212 H 0.002609 0.195204 0.369055 0.049 Uiso 1 1 calc R U
H213 H 0.127347 0.193249 0.436637 0.049 Uiso 1 1 calc R U
B B 0.24842(10) 0.53447(13) 0.15899(9) 0.0271(2) Uani 1 1 d . .
F1 F 0.24743(9) 0.47500(10) 0.05935(6) 0.0456(2) Uani 1 1 d . .
F2 F 0.13181(7) 0.51001(9) 0.20633(6) 0.0390(2) Uani 1 1 d . .
F3 F 0.33782(9) 0.47632(12) 0.22220(8) 0.0568(3) Uani 1 1 d . .
F4 F 0.26684(11) 0.67574(10) 0.15001(9) 0.0663(3) Uani 1 1 d . .
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'
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
C2 N C1 125.89(9) . .
N C1 C2 116.95(8) . 5_566
N C1 C11 119.94(8) . .
C2 C1 C11 123.10(8) 5_566 .
N C2 C1 117.15(8) . 5_566
N C2 C21 119.88(9) . .
C1 C2 C21 122.96(8) 5_566 .
F4 B F3 110.01(11) . .
F4 B F1 109.39(10) . .
F3 B F1 111.53(11) . .
F4 B F2 109.11(10) . .
F3 B F2 108.85(9) . .
F1 B F2 107.90(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N C2 1.3412(12) .
N C1 1.3429(12) .
C1 C2 1.3988(14) 5_566
C1 C11 1.4850(13) .
C2 C21 1.4848(14) .
B F4 1.3655(15) .
B F3 1.3723(15) .
B F1 1.3752(15) .
B F2 1.4198(13) .
