#------------------------------------------------------------------------------
#$Date: 2020-01-11 08:37:02 +0200 (Sat, 11 Jan 2020) $
#$Revision: 246738 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/32/2243243.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2243243
loop_
_publ_author_name
'Tanaka, Ryo'
'Shiono, Takeshi'
_publ_section_title
;
 Crystal structure of
 di-μ-trihydro(pentafluorophenyl)borato-tetrakis(tetrahydrofuran)disodium
;
_journal_coeditor_code           IS5529
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              145
_journal_page_last               147
_journal_paper_doi               10.1107/S2056989019017201
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Na2 (C6 F5 B H3)2 (C4 H8 O)4]'
_chemical_formula_sum            'C28 H38 B2 F10 Na2 O4'
_chemical_formula_weight         696.18
_chemical_name_systematic
;
Di-μ-trihydro(pentafluoropheny)borato-tetrakis(tetrahydrofuran)disodium
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_cell_angle_alpha                113.461(2)
_cell_angle_beta                 105.685(3)
_cell_angle_gamma                91.805(2)
_cell_formula_units_Z            1
_cell_length_a                   7.9698(5)
_cell_length_b                   10.1104(6)
_cell_length_c                   11.5208(7)
_cell_measurement_reflns_used    4126
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.69
_cell_volume                     809.63(9)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2006)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare et al.,  1999)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4506
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.399
_diffrn_reflns_theta_min         2.026
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.450
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0469
_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)+(0.0819P)²+0.2169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                3068
_reflns_number_total             3471
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            is5529sup1.cif
_cod_data_source_block           I
_cod_database_code               2243243
_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   0.914
_shelx_estimated_absorpt_t_max   0.970
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Na NA1 0.55346(7) -0.03356(7) -0.15797(5) 0.02597(18) Uani d 1
B B1 0.5516(2) -0.20185(19) -0.02053(16) 0.0272(3) Uani d 1
H H1 0.412(3) -0.193(2) -0.022(2) 0.043(6) Uiso d 1
H H2 0.560(3) -0.244(3) -0.120(2) 0.053(6) Uiso d 1
H H3 0.638(3) -0.092(2) 0.037(2) 0.037(5) Uiso d 1
C C1 0.63209(18) -0.30571(15) 0.04965(13) 0.0217(3) Uani d 1
C C2 0.71559(19) -0.42272(17) -0.00498(14) 0.0256(3) Uani d 1
C C3 0.78844(19) -0.50723(17) 0.05860(16) 0.0296(3) Uani d 1
C C4 0.7778(2) -0.47796(18) 0.18383(16) 0.0310(3) Uani d 1
C C5 0.6944(2) -0.36360(18) 0.24263(14) 0.0296(3) Uani d 1
C C6 0.62500(19) -0.28259(16) 0.17530(13) 0.0238(3) Uani d 1
F F1 0.72989(14) -0.45982(12) -0.12796(10) 0.0395(3) Uani d 1
F F2 0.86728(14) -0.61935(12) -0.00036(13) 0.0453(3) Uani d 1
F F3 0.84800(15) -0.55697(12) 0.24888(12) 0.0469(3) Uani d 1
F F4 0.68262(17) -0.33360(13) 0.36492(10) 0.0475(3) Uani d 1
F F5 0.54502(14) -0.17008(11) 0.23880(9) 0.0343(2) Uani d 1
O O1 0.83333(15) -0.03501(13) -0.16984(12) 0.0327(3) Uani d 1
C C7 0.9190(3) 0.0619(2) -0.2058(2) 0.0436(4) Uani d 1
H H4 1.016334 0.130984 -0.128474 0.052 Uiso calc 1
H H5 0.834348 0.118300 -0.238397 0.052 Uiso calc 1
C C8 0.9905(3) -0.0347(2) -0.31551(19) 0.0430(4) Uani d 1
H H6 0.911623 -0.050243 -0.404062 0.052 Uiso calc 1
H H7 1.109827 0.009804 -0.303714 0.052 Uiso calc 1
C C9 0.9967(3) -0.1771(2) -0.30160(18) 0.0391(4) Uani d 1
H H8 1.118106 -0.200710 -0.286654 0.047 Uiso calc 1
H H9 0.917077 -0.258235 -0.382236 0.047 Uiso calc 1
C C10 0.9356(2) -0.1511(2) -0.18186(17) 0.0348(4) Uani d 1
H H10 0.862781 -0.240318 -0.195466 0.042 Uiso calc 1
H H11 1.037924 -0.122799 -0.100803 0.042 Uiso calc 1
O O2 0.40793(15) -0.18090(12) -0.37962(10) 0.0319(3) Uani d 1
C C11 0.3406(2) -0.15236(19) -0.49440(15) 0.0328(4) Uani d 1
H H12 0.434473 -0.146717 -0.534402 0.039 Uiso calc 1
H H13 0.292566 -0.059350 -0.470737 0.039 Uiso calc 1
C C12 0.1955(3) -0.2805(2) -0.59003(16) 0.0392(4) Uani d 1
H H14 0.192110 -0.307211 -0.683241 0.047 Uiso calc 1
H H15 0.078771 -0.257016 -0.580757 0.047 Uiso calc 1
C C13 0.2449(3) -0.4036(2) -0.54953(17) 0.0411(4) Uani d 1
H H16 0.149650 -0.439183 -0.524004 0.049 Uiso calc 1
H H17 0.267784 -0.486333 -0.623172 0.049 Uiso calc 1
C C14 0.4109(2) -0.33571(19) -0.43176(16) 0.0362(4) Uani d 1
H H18 0.410810 -0.372273 -0.363810 0.043 Uiso calc 1
H H19 0.517132 -0.358754 -0.460167 0.043 Uiso calc 1
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'
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'
Na Na 0.0362 0.0249 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 NA1 O2 . . 97.78(5)
O1 NA1 F5 . 2_655 101.16(4)
O2 NA1 F5 . 2_655 80.88(4)
O1 NA1 B1 . . 100.56(5)
O2 NA1 B1 . . 107.00(5)
F5 NA1 B1 2_655 . 155.60(5)
O1 NA1 B1 . 2_655 123.38(5)
O2 NA1 B1 . 2_655 129.23(5)
F5 NA1 B1 2_655 2_655 64.36(4)
B1 NA1 B1 . 2_655 94.23(5)
O1 NA1 NA1 . 2_655 122.73(4)
O2 NA1 NA1 . 2_655 132.93(4)
F5 NA1 NA1 2_655 2_655 110.18(3)
B1 NA1 NA1 . 2_655 47.51(4)
B1 NA1 NA1 2_655 2_655 46.73(4)
O1 NA1 H2 . . 91.5(6)
O2 NA1 H2 . . 87.9(6)
F5 NA1 H2 2_655 . 164.1(6)
B1 NA1 H2 . . 22.6(6)
B1 NA1 H2 2_655 . 116.2(6)
NA1 NA1 H2 2_655 . 69.7(6)
O1 NA1 H3 . . 91.0(5)
O2 NA1 H3 . . 130.7(5)
F5 NA1 H3 2_655 . 144.5(5)
B1 NA1 H3 . . 24.2(5)
B1 NA1 H3 2_655 . 81.0(5)
NA1 NA1 H3 2_655 . 38.6(5)
H2 NA1 H3 . . 43.3(8)
C1 B1 NA1 . . 155.20(11)
C1 B1 NA1 . 2_655 109.90(9)
NA1 B1 NA1 . 2_655 85.77(5)
C1 B1 H1 . . 111.0(11)
NA1 B1 H1 . . 93.7(11)
NA1 B1 H1 2_655 . 55.7(12)
C1 B1 H2 . . 109.9(13)
NA1 B1 H2 . . 56.3(13)
NA1 B1 H2 2_655 . 140.1(13)
H1 B1 H2 . . 110.2(17)
C1 B1 H3 . . 107.0(11)
NA1 B1 H3 . . 64.1(11)
NA1 B1 H3 2_655 . 58.4(11)
H1 B1 H3 . . 111.4(16)
H2 B1 H3 . . 107.2(16)
C2 C1 C6 . . 113.31(13)
C2 C1 B1 . . 125.13(12)
C6 C1 B1 . . 121.55(13)
F1 C2 C3 . . 115.87(14)
F1 C2 C1 . . 119.98(13)
C3 C2 C1 . . 124.15(14)
F2 C3 C2 . . 121.03(15)
F2 C3 C4 . . 119.32(15)
C2 C3 C4 . . 119.64(15)
F3 C4 C5 . . 119.96(15)
F3 C4 C3 . . 121.29(16)
C5 C4 C3 . . 118.75(15)
F4 C5 C6 . . 121.25(15)
F4 C5 C4 . . 119.52(15)
C6 C5 C4 . . 119.23(14)
F5 C6 C5 . . 116.66(13)
F5 C6 C1 . . 118.44(13)
C5 C6 C1 . . 124.90(14)
C6 F5 NA1 . 2_655 124.58(8)
C7 O1 C10 . . 105.86(12)
C7 O1 NA1 . . 124.28(11)
C10 O1 NA1 . . 127.60(10)
O1 C7 C8 . . 105.75(15)
O1 C7 H4 . . 110.6
C8 C7 H4 . . 110.6
O1 C7 H5 . . 110.6
C8 C7 H5 . . 110.6
H4 C7 H5 . . 108.7
C9 C8 C7 . . 104.83(14)
C9 C8 H6 . . 110.8
C7 C8 H6 . . 110.8
C9 C8 H7 . . 110.8
C7 C8 H7 . . 110.8
H6 C8 H7 . . 108.9
C8 C9 C10 . . 104.49(14)
C8 C9 H8 . . 110.9
C10 C9 H8 . . 110.9
C8 C9 H9 . . 110.9
C10 C9 H9 . . 110.9
H8 C9 H9 . . 108.9
O1 C10 C9 . . 105.64(13)
O1 C10 H10 . . 110.6
C9 C10 H10 . . 110.6
O1 C10 H11 . . 110.6
C9 C10 H11 . . 110.6
H10 C10 H11 . . 108.7
C11 O2 C14 . . 104.91(11)
C11 O2 NA1 . . 133.50(10)
C14 O2 NA1 . . 119.96(9)
O2 C11 C12 . . 105.00(13)
O2 C11 H12 . . 110.7
C12 C11 H12 . . 110.7
O2 C11 H13 . . 110.7
C12 C11 H13 . . 110.7
H12 C11 H13 . . 108.8
C11 C12 C13 . . 104.30(14)
C11 C12 H14 . . 110.9
C13 C12 H14 . . 110.9
C11 C12 H15 . . 110.9
C13 C12 H15 . . 110.9
H14 C12 H15 . . 108.9
C14 C13 C12 . . 104.48(14)
C14 C13 H16 . . 110.9
C12 C13 H16 . . 110.9
C14 C13 H17 . . 110.9
C12 C13 H17 . . 110.9
H16 C13 H17 . . 108.9
O2 C14 C13 . . 105.39(14)
O2 C14 H18 . . 110.7
C13 C14 H18 . . 110.7
O2 C14 H19 . . 110.7
C13 C14 H19 . . 110.7
H18 C14 H19 . . 108.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
NA1 O1 . 2.2714(12)
NA1 O2 . 2.3122(12)
NA1 F5 2_655 2.6373(12)
NA1 B1 . 2.7494(18)
NA1 B1 2_655 2.7845(19)
NA1 NA1 2_655 3.7658(11)
NA1 H2 . 2.33(2)
NA1 H3 . 2.47(2)
B1 C1 . 1.614(2)
B1 NA1 2_655 2.7844(19)
B1 H1 . 1.11(2)
B1 H2 . 1.08(3)
B1 H3 . 1.13(2)
C1 C2 . 1.386(2)
C1 C6 . 1.3889(18)
C2 F1 . 1.3520(16)
C2 C3 . 1.380(2)
C3 F2 . 1.3431(18)
C3 C4 . 1.380(2)
C4 F3 . 1.3384(18)
C4 C5 . 1.380(2)
C5 F4 . 1.3486(17)
C5 C6 . 1.371(2)
C6 F5 . 1.3677(17)
F5 NA1 2_655 2.6373(12)
O1 C7 . 1.425(2)
O1 C10 . 1.433(2)
C7 C8 . 1.522(3)
C7 H4 . 0.9900
C7 H5 . 0.9900
C8 C9 . 1.511(3)
C8 H6 . 0.9900
C8 H7 . 0.9900
C9 C10 . 1.514(2)
C9 H8 . 0.9900
C9 H9 . 0.9900
C10 H10 . 0.9900
C10 H11 . 0.9900
O2 C11 . 1.4317(18)
O2 C14 . 1.440(2)
C11 C12 . 1.520(2)
C11 H12 . 0.9900
C11 H13 . 0.9900
C12 C13 . 1.522(3)
C12 H14 . 0.9900
C12 H15 . 0.9900
C13 C14 . 1.514(2)
C13 H16 . 0.9900
C13 H17 . 0.9900
C14 H18 . 0.9900
C14 H19 . 0.9900
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
NA1 B1 C1 C2 . . -45.4(3)
NA1 B1 C1 C2 2_655 . -172.01(11)
NA1 B1 C1 C6 . . 133.6(2)
NA1 B1 C1 C6 2_655 . 7.05(16)
C6 C1 C2 F1 . . 178.94(12)
B1 C1 C2 F1 . . -1.9(2)
C6 C1 C2 C3 . . -1.3(2)
B1 C1 C2 C3 . . 177.85(14)
F1 C2 C3 F2 . . -0.3(2)
C1 C2 C3 F2 . . 179.89(13)
F1 C2 C3 C4 . . -179.20(13)
C1 C2 C3 C4 . . 1.0(2)
F2 C3 C4 F3 . . 1.6(2)
C2 C3 C4 F3 . . -179.52(13)
F2 C3 C4 C5 . . -179.17(13)
C2 C3 C4 C5 . . -0.3(2)
F3 C4 C5 F4 . . -0.8(2)
C3 C4 C5 F4 . . 179.93(13)
F3 C4 C5 C6 . . 179.21(13)
C3 C4 C5 C6 . . -0.1(2)
F4 C5 C6 F5 . . 0.4(2)
C4 C5 C6 F5 . . -179.57(13)
F4 C5 C6 C1 . . 179.69(13)
C4 C5 C6 C1 . . -0.3(2)
C2 C1 C6 F5 . . -179.83(12)
B1 C1 C6 F5 . . 1.0(2)
C2 C1 C6 C5 . . 0.9(2)
B1 C1 C6 C5 . . -178.22(14)
C5 C6 F5 NA1 . 2_655 169.12(10)
C1 C6 F5 NA1 . 2_655 -10.18(17)
C10 O1 C7 C8 . . 35.26(19)
NA1 O1 C7 C8 . . -128.73(14)
O1 C7 C8 C9 . . -19.7(2)
C7 C8 C9 C10 . . -2.2(2)
C7 O1 C10 C9 . . -36.82(18)
NA1 O1 C10 C9 . . 126.48(13)
C8 C9 C10 O1 . . 23.29(19)
C14 O2 C11 C12 . . 39.54(17)
NA1 O2 C11 C12 . . -155.60(12)
O2 C11 C12 C13 . . -24.77(18)
C11 C12 C13 C14 . . 1.6(2)
C11 O2 C14 C13 . . -38.57(18)
NA1 O2 C14 C13 . . 154.06(11)
C12 C13 C14 O2 . . 21.94(19)

_cod_database_fobs_code 2243243
