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#$Date: 2021-04-05 17:52:35 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263770 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/66/7706664.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_7706664
loop_
_publ_author_name
'Podda, Enrico'
'Coles, Simon J.'
'Horton, Peter N.'
'Lickiss, Paul D.'
'Bull, Okpara S.'
'Orton, James B.'
'Pintus, Anna'
'Pugh, David'
'Carla Aragoni, M.'
'Davies, Robert P.'
_publ_section_title
;
 First example of solid-state luminescent borasiloxane-based chiral
 helices assembled through N-B bonds.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3782
_journal_page_last               3785
_journal_paper_doi               10.1039/d1dt00114k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C36 H28 B2 F2 O4 Si2'
_chemical_formula_sum            'C36 H28 B2 F2 O4 Si2'
_chemical_formula_weight         640.38
_chemical_name_systematic
'8-bis(4-fluorophenyl)-2,2,6,6-tetraphenyl- 1,3,5,7,2,6,4,8-tetraoxadisiladiborocane'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2021-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                112.478(8)
_cell_angle_beta                 108.622(6)
_cell_angle_gamma                91.091(7)
_cell_formula_units_Z            1
_cell_length_a                   8.5686(6)
_cell_length_b                   9.8331(10)
_cell_length_c                   11.3579(8)
_cell_measurement_reflns_used    1572
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.1830
_cell_measurement_theta_min      3.1750
_cell_volume                     827.02(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'WinGX, enCIFer'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    Olex-2
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4382
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         3.124
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0445P)²+0.0257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2089
_reflns_number_total             2890
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00114k2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7706663--7706667.cif.'
_cod_original_cell_volume        827.02(13)
_cod_database_code               7706664
_shelx_shelxl_version_number     2016/4
_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   0.954
_shelx_estimated_absorpt_t_max   0.977
_oxdiff_exptl_absorpt_empirical_full_min 0.915
_oxdiff_exptl_absorpt_empirical_full_max 1.052
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2875(3) 0.6785(2) 0.27996(19) 0.0253(5) Uani 1 1 d . . . . .
C2 C 0.3614(3) 0.8253(3) 0.3250(2) 0.0308(6) Uani 1 1 d . . . . .
H2 H 0.474493 0.857037 0.384551 0.037 Uiso 1 1 calc R U . . .
C3 C 0.2726(3) 0.9258(3) 0.2843(2) 0.0386(6) Uani 1 1 d . . . . .
H3 H 0.325050 1.025545 0.316290 0.046 Uiso 1 1 calc R U . . .
C4 C 0.1085(3) 0.8816(3) 0.1976(2) 0.0457(7) Uani 1 1 d . . . . .
H4 H 0.047549 0.950927 0.170603 0.055 Uiso 1 1 calc R U . . .
C5 C 0.0330(3) 0.7358(3) 0.1501(2) 0.0463(7) Uani 1 1 d . . . . .
H5 H -0.079782 0.704705 0.089907 0.056 Uiso 1 1 calc R U . . .
C6 C 0.1218(3) 0.6355(3) 0.1904(2) 0.0374(6) Uani 1 1 d . . . . .
H6 H 0.069136 0.535423 0.156487 0.045 Uiso 1 1 calc R U . . .
C7 C 0.4183(3) 0.3843(3) 0.1807(2) 0.0378(6) Uani 1 1 d . . . . .
C8 C 0.3297(3) 0.2413(3) 0.1267(2) 0.0486(7) Uani 1 1 d . . . . .
H8 H 0.258066 0.220337 0.168598 0.058 Uiso 1 1 calc R U . . .
C9 C 0.3437(4) 0.1288(3) 0.0128(3) 0.0712(10) Uani 1 1 d . . . . .
H9 H 0.282540 0.031528 -0.022826 0.085 Uiso 1 1 calc R U . . .
C10 C 0.4467(5) 0.1592(4) -0.0479(3) 0.0840(13) Uani 1 1 d . . . . .
H10 H 0.456181 0.082207 -0.126112 0.101 Uiso 1 1 calc R U . . .
C11 C 0.5357(5) 0.2980(4) 0.0020(3) 0.0825(12) Uani 1 1 d . . . . .
H11 H 0.607551 0.317492 -0.040322 0.099 Uiso 1 1 calc R U . . .
C12 C 0.5202(4) 0.4108(3) 0.1155(3) 0.0598(9) Uani 1 1 d . . . . .
H12 H 0.580496 0.507981 0.149239 0.072 Uiso 1 1 calc R U . . .
C13 C 0.8960(3) 0.6913(2) 0.56254(19) 0.0250(5) Uani 1 1 d . . . . .
C14 C 1.0382(3) 0.6877(3) 0.6644(2) 0.0336(6) Uani 1 1 d . . . . .
H14 H 1.027313 0.637306 0.718722 0.040 Uiso 1 1 calc R U . . .
C15 C 1.1946(3) 0.7562(3) 0.6878(2) 0.0410(7) Uani 1 1 d . . . . .
H15 H 1.290490 0.754412 0.757843 0.049 Uiso 1 1 calc R U . . .
C16 C 1.2069(3) 0.8261(3) 0.6076(2) 0.0377(6) Uani 1 1 d . . . . .
C17 C 1.0733(3) 0.8346(3) 0.5065(2) 0.0383(6) Uani 1 1 d . . . . .
H17 H 1.086690 0.885064 0.453002 0.046 Uiso 1 1 calc R U . . .
C18 C 0.9180(3) 0.7667(3) 0.4854(2) 0.0323(6) Uani 1 1 d . . . . .
H18 H 0.823246 0.771532 0.416157 0.039 Uiso 1 1 calc R U . . .
B1 B 0.7212(3) 0.6111(3) 0.5340(2) 0.0260(6) Uani 1 1 d . . . . .
O1 O 0.58490(17) 0.62336(17) 0.43746(14) 0.0316(4) Uani 1 1 d . . . . .
O2 O 0.29226(17) 0.46863(17) 0.39382(14) 0.0338(4) Uani 1 1 d . . . . .
SI1 Si 0.39916(7) 0.53924(7) 0.33041(5) 0.02542(19) Uani 1 1 d . . . . .
F1 F 1.36180(16) 0.89092(19) 0.62884(14) 0.0607(5) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
_geom_angle_publ_flag
C2 C1 C6 117.6(2) . . ?
C2 C1 SI1 123.15(17) . . ?
C6 C1 SI1 119.19(17) . . ?
C3 C2 C1 121.1(2) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 120.3(2) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 121.3(2) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C8 C7 C12 117.5(2) . . ?
C8 C7 SI1 122.7(2) . . ?
C12 C7 SI1 119.8(2) . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.3(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C7 121.4(3) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
C18 C13 C14 117.3(2) . . ?
C18 C13 B1 121.4(2) . . ?
C14 C13 B1 121.3(2) . . ?
C15 C14 C13 121.3(2) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
C15 C16 F1 118.1(2) . . ?
C15 C16 C17 123.7(2) . . ?
F1 C16 C17 118.2(2) . . ?
C16 C17 C18 117.4(2) . . ?
C16 C17 H17 121.3 . . ?
C18 C17 H17 121.3 . . ?
C17 C18 C13 122.1(2) . . ?
C17 C18 H18 118.9 . . ?
C13 C18 H18 118.9 . . ?
O2 B1 O1 121.7(2) 2_666 . ?
O2 B1 C13 119.2(2) 2_666 . ?
O1 B1 C13 119.1(2) . . ?
B1 O1 SI1 143.08(16) . . ?
B1 O2 SI1 151.03(16) 2_666 . ?
O2 SI1 O1 113.21(8) . . ?
O2 SI1 C1 108.57(9) . . ?
O1 SI1 C1 107.54(9) . . ?
O2 SI1 C7 107.58(10) . . ?
O1 SI1 C7 108.89(10) . . ?
C1 SI1 C7 111.08(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.392(3) . ?
C1 C6 1.399(3) . ?
C1 SI1 1.849(2) . ?
C2 C3 1.387(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.389(4) . ?
C7 C12 1.389(4) . ?
C7 SI1 1.856(2) . ?
C8 C9 1.387(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.371(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.364(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.396(3) . ?
C13 C14 1.399(3) . ?
C13 B1 1.556(3) . ?
C14 C15 1.387(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.360(3) . ?
C15 H15 0.9500 . ?
C16 F1 1.368(2) . ?
C16 C17 1.368(3) . ?
C17 C18 1.383(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
B1 O2 1.360(3) 2_666 ?
B1 O1 1.367(3) . ?
O1 SI1 1.6250(14) . ?
O2 B1 1.360(3) 2_666 ?
O2 SI1 1.6184(16) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.2(3) . . . . ?
SI1 C1 C2 C3 179.98(16) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C4 C5 C6 C1 0.6(4) . . . . ?
C2 C1 C6 C5 -1.4(3) . . . . ?
SI1 C1 C6 C5 179.75(18) . . . . ?
C12 C7 C8 C9 0.7(4) . . . . ?
SI1 C7 C8 C9 178.5(2) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C9 C10 C11 0.2(5) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C10 C11 C12 C7 1.2(5) . . . . ?
C8 C7 C12 C11 -1.2(4) . . . . ?
SI1 C7 C12 C11 -179.1(2) . . . . ?
C18 C13 C14 C15 0.0(3) . . . . ?
B1 C13 C14 C15 178.5(2) . . . . ?
C13 C14 C15 C16 -0.8(4) . . . . ?
C14 C15 C16 F1 -178.66(19) . . . . ?
C14 C15 C16 C17 1.1(4) . . . . ?
C15 C16 C17 C18 -0.5(4) . . . . ?
F1 C16 C17 C18 179.20(19) . . . . ?
C16 C17 C18 C13 -0.3(3) . . . . ?
C14 C13 C18 C17 0.6(3) . . . . ?
B1 C13 C18 C17 -177.9(2) . . . . ?
C18 C13 B1 O2 175.9(2) . . . 2_666 ?
C14 C13 B1 O2 -2.5(3) . . . 2_666 ?
C18 C13 B1 O1 -4.5(3) . . . . ?
C14 C13 B1 O1 177.1(2) . . . . ?
O2 B1 O1 SI1 -27.2(4) 2_666 . . . ?
C13 B1 O1 SI1 153.21(18) . . . . ?
B1 O2 SI1 O1 -45.8(3) 2_666 . . . ?
B1 O2 SI1 C1 -165.2(3) 2_666 . . . ?
B1 O2 SI1 C7 74.6(3) 2_666 . . . ?
B1 O1 SI1 O2 43.2(3) . . . . ?
B1 O1 SI1 C1 163.2(2) . . . . ?
B1 O1 SI1 C7 -76.4(3) . . . . ?
C2 C1 SI1 O2 125.76(17) . . . . ?
C6 C1 SI1 O2 -55.45(18) . . . . ?
C2 C1 SI1 O1 2.92(19) . . . . ?
C6 C1 SI1 O1 -178.29(16) . . . . ?
C2 C1 SI1 C7 -116.15(18) . . . . ?
C6 C1 SI1 C7 62.7(2) . . . . ?
C8 C7 SI1 O2 9.4(2) . . . . ?
C12 C7 SI1 O2 -172.9(2) . . . . ?
C8 C7 SI1 O1 132.5(2) . . . . ?
C12 C7 SI1 O1 -49.8(2) . . . . ?
C8 C7 SI1 C1 -109.3(2) . . . . ?
C12 C7 SI1 C1 68.4(2) . . . . ?
