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#$Date: 2019-11-23 19:16:20 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234607 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/52/7125219.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_7125219
loop_
_publ_author_name
'Duda, Katharina'
'Himmelspach, Alexander'
'Landmann, Johannes'
'Kraus, Florian'
'Finze, Maik'
_publ_section_title
;
 Synthesis of the fluorohydridoborate anions [BHF₃]⁻
 and
 [1-HF₂B-9,12-X₂-closo-1,2-C₂B₁₀H₉]⁻
 (X = H, I): deboronation of 1,2- and 1,7-dicarba-closo-dodecaboranes with
 anhydrous [Me₄N]F.
;
_journal_issue                   90
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13241
_journal_page_last               13244
_journal_paper_doi               10.1039/c6cc07711k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C4 H12 N, B F3 H'
_chemical_formula_sum            'C4 H13 B F3 N'
_chemical_formula_weight         142.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5770(13)
_cell_length_b                   11.436(3)
_cell_length_c                   11.447(3)
_cell_measurement_reflns_used    2438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.0545
_cell_measurement_theta_min      3.5595
_cell_volume                     730.1(3)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1394
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5381
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.837
_diffrn_reflns_theta_min         1.779
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0365
_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)+(0.0385P)²+0.1017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                792
_reflns_number_total             883
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc07711k2.cif
_cod_data_source_block           Me4NBHF3
_cod_database_code               7125219
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
N1 N -1.4864(3) 0.2500 0.5000 0.0152(4) Uani 1 2 d S T P
C1 C -1.6412(2) 0.18259(14) 0.41681(14) 0.0202(4) Uani 1 1 d . . .
H1A H -1.7418 0.1278 0.4607 0.030 Uiso 1 1 calc R U .
H1B H -1.5395 0.1391 0.3622 0.030 Uiso 1 1 calc R U .
H1C H -1.7435 0.2369 0.3732 0.030 Uiso 1 1 calc R U .
C2 C -1.3316(2) 0.33444(14) 0.43364(15) 0.0219(4) Uani 1 1 d . . .
H2A H -1.2250 0.2911 0.3812 0.033 Uiso 1 1 calc R U .
H2B H -1.2354 0.3803 0.4887 0.033 Uiso 1 1 calc R U .
H2C H -1.4334 0.3871 0.3877 0.033 Uiso 1 1 calc R U .
F1 F -0.16042(19) -0.03680(11) 0.15104(12) 0.0473(4) Uani 1 1 d . . .
F2 F -0.1190(3) 0.13373(12) 0.2500 0.0303(4) Uani 1 2 d S T P
B1 B -0.0596(4) 0.0136(2) 0.2500 0.0165(5) Uani 1 2 d S T P
H1 H 0.142(4) 0.000(2) 0.2500 0.025 Uiso 1 2 d S U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C1 N1 C1 109.66(14) . 3_556
C1 N1 C2 108.77(9) . 3_556
C1 N1 C2 109.91(9) 3_556 3_556
C1 N1 C2 109.91(9) . .
C1 N1 C2 108.77(9) 3_556 .
C2 N1 C2 109.81(14) 3_556 .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
F1 B1 F1 109.2(2) 6_556 .
F1 B1 F2 107.96(13) 6_556 .
F1 B1 F2 107.96(13) . .
F1 B1 H1 110.2(6) 6_556 .
F1 B1 H1 110.2(6) . .
F2 B1 H1 111.3(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.4988(16) .
N1 C1 1.4988(16) 3_556
N1 C2 1.5016(16) 3_556
N1 C2 1.5016(16) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
F1 B1 1.3899(18) .
F2 B1 1.413(3) .
B1 F1 1.3899(18) 6_556
B1 H1 1.13(2) .
