First example of solid-state luminescent borasiloxane-based chiral helices assembled through N-B bonds.
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.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3782–3785; doi:10.1039/d1dt00114k

data_7706666
_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_absolute_configuration ad
_chemical_formula_moiety         '0.5(C108 H76 B4 F4 N4 O8 S2 Si4)'
_chemical_formula_sum            'C54 H38 B2 F2 N2 O4 S Si2'
_chemical_formula_weight         926.72
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2021-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8634(2)
_cell_length_b                   13.8634(2)
_cell_length_c                   23.7340(4)
_cell_measurement_reflns_used    17298
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1250
_cell_measurement_theta_min      2.0730
_cell_volume                     4561.53(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -101.00  15.00   1.00   62.00    --  -11.20 -38.00 -60.00  116
  2  \w   -101.00  15.00   1.00   62.00    --  -11.20 -38.00 -30.00  116
  3  \w   -101.00 -30.00   1.00   62.00    --  -11.20 -38.00   0.00   71
  4  \w    -31.00  60.00   1.00   62.00    --  -11.20  19.00 -90.00   91
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0063257000
_diffrn_orient_matrix_UB_12      0.0150796000
_diffrn_orient_matrix_UB_13      0.0283311000
_diffrn_orient_matrix_UB_21      0.0470779000
_diffrn_orient_matrix_UB_22      0.0200022000
_diffrn_orient_matrix_UB_23      -0.0000427000
_diffrn_orient_matrix_UB_31      -0.0189887000
_diffrn_orient_matrix_UB_32      0.0445966000
_diffrn_orient_matrix_UB_33      -0.0095510000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.701
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and ether'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1704 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5236
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0368
_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/[\s^2^(Fo^2^)+(0.0394P)^2^+0.9850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4550
_reflns_number_total             5236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00114k2.cif
_cod_data_source_block           Compound_4_2019ncs0237_1b
_cod_depositor_comments
'Adding full bibliography for 7706663--7706667.cif.'
_cod_original_cell_volume        4561.53(15)
_cod_database_code               7706666
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H38B2F2N2O4SSi2'
_chemical_oxdiff_usercomment     93FR
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.989
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S21-C28 \\sim S21B-C28B
 with sigma of 0.02
 C27-C28 \\sim C27-C28B
 with sigma of 0.02
 C28-C29 \\sim C28B-C29B
 with sigma of 0.02
 S21-C27 \\sim S21B-C27
 with sigma of 0.04
 S21-C29 \\sim S21B-C29B
 with sigma of 0.04
 C27-C29 \\sim C27-C29B
 with sigma of 0.04
 C28B-C29B \\sim C28B_$1-C30B
 with sigma of 0.02
 C30B-C28B \\sim C29B-C28B_$1
 with sigma of 0.02
 C29B-S21B \\sim S21B-C30B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C28) = Uanis(C28B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C28B)=1-FVAR(1)
 Sof(S21B)=Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30B)=0.5*(1-FVAR(2))
 Sof(S21)=0.5*FVAR(2)
 Sof(C28)=Sof(C29)=Sof(H29)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C23(H23), C24(H24),
  C25(H25), C29(H29), C29B(H29B), C30B(H30B)
;
_shelx_res_checksum              81678
_shelx_hkl_checksum              13594
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 93FR
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.923
_oxdiff_exptl_absorpt_empirical_full_min 0.413