#------------------------------------------------------------------------------
#$Date: 2019-11-23 15:47:25 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233890 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/93/4349352.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_4349352
loop_
_publ_author_name
'LeBlanc, Francis A.'
'Decken, Andreas'
'Cameron, T. Stanley'
'Passmore, Jack'
'Rautiainen, J. Mikko'
'Whidden, Thomas K.'
_publ_section_title
;
 Synthesis, Characterization, and Properties of Weakly Coordinating Anions
 Based on tris-Perfluoro-tert-Butoxyborane.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              974
_journal_page_last               983
_journal_paper_doi               10.1021/acs.inorgchem.6b02670
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C12 B F27 O3'
_chemical_formula_sum            'C12 B F27 O3'
_chemical_formula_weight         715.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.00
_cell_angle_beta                 91.358(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.712(2)
_cell_length_b                   6.8568(9)
_cell_length_c                   18.657(2)
_cell_measurement_reflns_used    5804
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.44
_cell_volume                     2137.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14057
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.9006
_exptl_absorpt_correction_T_min  0.8499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1017P)²+3.3439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3489
_reflns_number_total             4766
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02670_si_002.cif
_cod_data_source_block           jp070753
_cod_original_cell_volume        2137.3(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349352
_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.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
B1 B 0.24624(19) 0.4705(5) 0.30649(17) 0.0326(7) Uani 1 1 d
O1 O 0.16675(12) 0.4956(3) 0.31657(10) 0.0322(4) Uani 1 1 d
O2 O 0.29526(12) 0.4163(4) 0.36242(11) 0.0423(5) Uani 1 1 d
O3 O 0.27706(12) 0.4998(3) 0.24036(11) 0.0377(5) Uani 1 1 d
C1 C 0.11880(16) 0.4851(4) 0.37701(15) 0.0308(6) Uani 1 1 d
C2 C 0.03830(18) 0.5822(5) 0.35158(17) 0.0393(7) Uani 1 1 d
C3 C 0.1038(2) 0.2696(5) 0.3968(2) 0.0467(8) Uani 1 1 d
C4 C 0.1553(2) 0.6011(5) 0.44186(17) 0.0445(8) Uani 1 1 d
C5 C 0.37658(18) 0.3677(5) 0.36809(18) 0.0431(7) Uani 1 1 d
C6 C 0.4289(3) 0.5563(8) 0.3654(3) 0.0769(14) Uani 1 1 d
C7 C 0.4025(3) 0.2266(7) 0.3079(3) 0.0659(12) Uani 1 1 d
C8 C 0.3858(3) 0.2728(12) 0.4427(3) 0.093(2) Uani 1 1 d
C9 C 0.24306(17) 0.5677(5) 0.17560(15) 0.0350(6) Uani 1 1 d
C10 C 0.3161(2) 0.6289(7) 0.13031(19) 0.0549(9) Uani 1 1 d
C11 C 0.1963(3) 0.4008(6) 0.13762(19) 0.0560(9) Uani 1 1 d
C12 C 0.1887(2) 0.7497(5) 0.18616(19) 0.0482(8) Uani 1 1 d
F1 F 0.01408(11) 0.5145(3) 0.28874(11) 0.0484(5) Uani 1 1 d
F2 F 0.04848(13) 0.7733(3) 0.34523(13) 0.0552(5) Uani 1 1 d
F3 F -0.01933(11) 0.5498(4) 0.39810(12) 0.0562(6) Uani 1 1 d
F4 F 0.06763(15) 0.2560(4) 0.45928(14) 0.0721(8) Uani 1 1 d
F5 F 0.17164(13) 0.1714(3) 0.40168(14) 0.0594(6) Uani 1 1 d
F6 F 0.05737(16) 0.1841(3) 0.34738(16) 0.0707(7) Uani 1 1 d
F7 F 0.09800(15) 0.6735(4) 0.48211(12) 0.0691(7) Uani 1 1 d
F8 F 0.20163(13) 0.4900(4) 0.48314(10) 0.0573(6) Uani 1 1 d
F9 F 0.19938(14) 0.7466(3) 0.41853(13) 0.0594(6) Uani 1 1 d
F10 F 0.4180(3) 0.6550(7) 0.4291(3) 0.1407(19) Uani 1 1 d
F11 F 0.50454(15) 0.5134(5) 0.3656(2) 0.0927(10) Uani 1 1 d
F12 F 0.40658(17) 0.6719(4) 0.3160(2) 0.0914(10) Uani 1 1 d
F13 F 0.46218(16) 0.1119(4) 0.33004(17) 0.0786(8) Uani 1 1 d
F14 F 0.42884(17) 0.3299(5) 0.25095(15) 0.0915(10) Uani 1 1 d
F15 F 0.34391(18) 0.1232(4) 0.28355(19) 0.0875(10) Uani 1 1 d
F16 F 0.3516(2) 0.0885(8) 0.4345(3) 0.149(2) Uani 1 1 d
F17 F 0.3500(2) 0.3565(10) 0.49114(15) 0.170(3) Uani 1 1 d
F18 F 0.46131(16) 0.2421(6) 0.46243(16) 0.0948(11) Uani 1 1 d
F19 F 0.34767(17) 0.7906(5) 0.15691(15) 0.0836(9) Uani 1 1 d
F20 F 0.37210(15) 0.4936(5) 0.13241(14) 0.0785(9) Uani 1 1 d
F21 F 0.29510(16) 0.6574(4) 0.06213(11) 0.0697(7) Uani 1 1 d
F22 F 0.2468(2) 0.2664(4) 0.11405(15) 0.0863(9) Uani 1 1 d
F23 F 0.15346(19) 0.4672(5) 0.08249(13) 0.0838(9) Uani 1 1 d
F24 F 0.14818(15) 0.3130(4) 0.18287(12) 0.0630(6) Uani 1 1 d
F25 F 0.11332(12) 0.6989(4) 0.19690(12) 0.0610(6) Uani 1 1 d
F26 F 0.21372(17) 0.8513(3) 0.24200(12) 0.0628(6) Uani 1 1 d
F27 F 0.18820(16) 0.8631(4) 0.12819(13) 0.0672(7) 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'
B B 0.0013 0.0007 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 B1 O2 120.1(3)
O1 B1 O3 119.9(3)
O2 B1 O3 120.0(3)
B1 O1 C1 133.3(2)
B1 O2 C5 133.4(2)
B1 O3 C9 132.4(2)
O1 C1 C3 110.0(2)
O1 C1 C4 112.2(2)
C3 C1 C4 111.4(3)
O1 C1 C2 103.8(2)
C3 C1 C2 109.7(2)
C4 C1 C2 109.6(2)
F1 C2 F2 107.8(3)
F1 C2 F3 108.1(3)
F2 C2 F3 108.6(3)
F1 C2 C1 111.3(3)
F2 C2 C1 109.7(3)
F3 C2 C1 111.2(3)
F5 C3 F6 108.0(3)
F5 C3 F4 108.2(3)
F6 C3 F4 107.9(3)
F5 C3 C1 111.1(3)
F6 C3 C1 110.6(3)
F4 C3 C1 110.9(3)
F9 C4 F8 107.7(3)
F9 C4 F7 108.6(3)
F8 C4 F7 107.9(3)
F9 C4 C1 109.9(3)
F8 C4 C1 111.8(3)
F7 C4 C1 110.8(3)
O2 C5 C8 104.2(3)
O2 C5 C7 112.4(3)
C8 C5 C7 111.5(4)
O2 C5 C6 110.1(3)
C8 C5 C6 109.5(4)
C7 C5 C6 109.1(4)
F12 C6 F11 114.4(5)
F12 C6 F10 106.1(5)
F11 C6 F10 104.8(4)
F12 C6 C5 112.8(4)
F11 C6 C5 111.0(4)
F10 C6 C5 107.0(5)
F15 C7 F13 110.1(4)
F15 C7 F14 105.6(4)
F13 C7 F14 107.3(4)
F15 C7 C5 112.1(4)
F13 C7 C5 111.4(4)
F14 C7 C5 110.0(4)
F17 C8 F18 110.2(5)
F17 C8 F16 107.2(6)
F18 C8 F16 105.8(5)
F17 C8 C5 115.1(5)
F18 C8 C5 113.2(4)
F16 C8 C5 104.6(5)
O3 C9 C11 109.8(3)
O3 C9 C10 104.5(2)
C11 C9 C10 110.1(3)
O3 C9 C12 112.5(2)
C11 C9 C12 111.1(3)
C10 C9 C12 108.6(3)
F20 C10 F19 107.6(3)
F20 C10 F21 107.7(3)
F19 C10 F21 109.3(3)
F20 C10 C9 111.1(3)
F19 C10 C9 109.5(3)
F21 C10 C9 111.5(3)
F23 C11 F24 109.1(4)
F23 C11 F22 108.5(3)
F24 C11 F22 107.2(3)
F23 C11 C9 111.1(3)
F24 C11 C9 110.6(3)
F22 C11 C9 110.2(3)
F26 C12 F25 107.8(3)
F26 C12 F27 109.3(3)
F25 C12 F27 106.8(3)
F26 C12 C9 110.4(3)
F25 C12 C9 111.5(3)
F27 C12 C9 110.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
B1 O1 1.357(4)
B1 O2 1.363(4)
B1 O3 1.363(4)
O1 C1 1.401(3)
O2 C5 1.401(4)
O3 C9 1.403(3)
C1 C3 1.545(4)
C1 C4 1.560(4)
C1 C2 1.565(4)
C2 F1 1.316(4)
C2 F2 1.327(4)
C2 F3 1.330(4)
C3 F5 1.320(4)
C3 F6 1.328(4)
C3 F4 1.328(4)
C4 F9 1.320(4)
C4 F8 1.321(4)
C4 F7 1.327(4)
C5 C8 1.540(6)
C5 C7 1.552(6)
C5 C6 1.562(6)
C6 F12 1.266(6)
C6 F11 1.298(5)
C6 F10 1.384(7)
C7 F15 1.284(5)
C7 F13 1.328(5)
C7 F14 1.359(6)
C8 F17 1.237(7)
C8 F18 1.323(5)
C8 F16 1.394(9)
C9 C11 1.548(5)
C9 C10 1.558(4)
C9 C12 1.559(5)
C10 F20 1.318(5)
C10 F19 1.320(5)
C10 F21 1.326(4)
C11 F23 1.320(5)
C11 F24 1.324(5)
C11 F22 1.332(5)
C12 F26 1.313(4)
C12 F25 1.326(4)
C12 F27 1.332(4)
