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_7706667
_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 H72 B4 F8 N4 O8 S2 Si4)'
_chemical_formula_sum            'C54 H36 B2 F4 N2 O4 S Si2'
_chemical_formula_weight         962.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-08
_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            8
_cell_length_a                   19.62160(10)
_cell_length_b                   19.62160(10)
_cell_length_c                   23.8883(2)
_cell_measurement_reflns_used    39435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2080
_cell_measurement_theta_min      3.6780
_cell_volume                     9197.17(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_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                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -69.00 -43.00   0.50    0.50    --    0.00  20.00   0.00   52
  2  \w     39.00  66.00   0.50    0.50    --    0.00  20.00   0.00   54
  3  \w    -11.00  85.00   0.50    0.50    --    0.00  30.00  90.00  192
  4  \w    -16.00   9.00   0.50    0.50    --    5.00   8.00 -93.00   50
  5  \w   -100.00 -60.00   0.50    2.00    --  -90.00   8.00 -93.00   80
  6  \w   -111.00 -81.00   0.50    2.00    --  -90.00  59.00  81.74   60
  7  \w   -163.00-127.00   0.50    2.00    --  -90.00  59.00  81.74   72
  8  \w    -66.00 -40.00   0.50    2.00    --  -90.00  59.00  81.74   52
  9  \w    -45.00 -19.00   0.50    2.00    --  -90.00  47.00 155.24   52
 10  \w    -80.00 -50.00   0.50    2.00    --  -90.00  47.00 155.24   60
 11  \w   -163.00-134.00   0.50    2.00    --  -90.00  59.00 101.39   58
 12  \w   -168.00  -2.00   0.50    2.00    --  -90.00  53.00 -63.33  332
 13  \w   -179.00 -23.00   0.50    2.00    --  -90.00  59.00  25.76  312
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112736000
_diffrn_orient_matrix_UB_12      0.0197905000
_diffrn_orient_matrix_UB_13      0.0617148000
_diffrn_orient_matrix_UB_21      0.0006449000
_diffrn_orient_matrix_UB_22      0.0758819000
_diffrn_orient_matrix_UB_23      -0.0163273000
_diffrn_orient_matrix_UB_31      -0.0777691000
_diffrn_orient_matrix_UB_32      -0.0022850000
_diffrn_orient_matrix_UB_33      -0.0090854000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49836
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.252
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             3968
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and ether'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 7254 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         16155
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0693P)^2^+0.6345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                15953
_reflns_number_total             16155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00114k2.cif
_cod_data_source_block           Compound_5_2019ncs0025_2b
_cod_depositor_comments
'Adding full bibliography for 7706663--7706667.cif.'
_cod_original_cell_volume        9197.17(12)
_cod_database_code               7706667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H36 B2 F4N2 O4 S Si2'
_chemical_oxdiff_usercomment     A2_EP93F2R
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.740
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5919(13)
 0.4081(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 S101-C108 \\sim S301-C308
 with sigma of 0.02
 S101-C111 \\sim S301-C311
 with sigma of 0.02
 C112-C111 \\sim C112-C311
 with sigma of 0.02
 C107-C108 \\sim C107-C308
 with sigma of 0.02
 C108-C109 \\sim C308-C309
 with sigma of 0.02
 C111-C110 \\sim C311-C310
 with sigma of 0.02
 C110-C109 \\sim C310-C309
 with sigma of 0.02
 S101-C112 \\sim S301-C112
 with sigma of 0.04
 S101-C107 \\sim S301-C107
 with sigma of 0.04
 S101-C110 \\sim S301-C310
 with sigma of 0.04
 S101-C109 \\sim S301-C309
 with sigma of 0.04
 C112-C110 \\sim C112-C310
 with sigma of 0.04
 C107-C109 \\sim C107-C309
 with sigma of 0.04
 C108-C111 \\sim C308-C311
 with sigma of 0.04
 C108-C110 \\sim C308-C310
 with sigma of 0.04
 C111-C109 \\sim C311-C309
 with sigma of 0.04
 S41-C51 \\sim S241-C251
 with sigma of 0.02
 S41-C48 \\sim S241-C248
 with sigma of 0.02
 C47-C48 \\sim C47-C248
 with sigma of 0.02
 C52-C51 \\sim C52-C251
 with sigma of 0.02
 C51-C50 \\sim C251-C250
 with sigma of 0.02
 C48-C49 \\sim C248-C249
 with sigma of 0.02
 C50-C49 \\sim C250-C249
 with sigma of 0.02
 S41-C47 \\sim S241-C47
 with sigma of 0.04
 S41-C52 \\sim S241-C52
 with sigma of 0.04
 S41-C50 \\sim S241-C250
 with sigma of 0.04
 S41-C49 \\sim S241-C249
 with sigma of 0.04
 C47-C49 \\sim C47-C249
 with sigma of 0.04
 C52-C50 \\sim C52-C250
 with sigma of 0.04
 C51-C48 \\sim C251-C248
 with sigma of 0.04
 C51-C49 \\sim C251-C249
 with sigma of 0.04
 C48-C50 \\sim C248-C250
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
S101 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim S301 \\sim C308 \\sim
C309 \\sim C310 \\sim C311: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
S41 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim S241 \\sim C248 \\sim C249
\\sim C250 \\sim C251: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C308) = Uanis(C108)
Uanis(C111) = Uanis(C311)
Uanis(C248) = Uanis(C48)
Uanis(C51) = Uanis(C251)
5. Rigid body (RIGU) restrains
 S101, C108, C109, C110, C111, S301, C308, C309, C310, C311
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S41, C48, C49, C50, C51, S241, C248, C249, C250, C251
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(S301)=Sof(C308)=Sof(C309)=Sof(H309)=Sof(C310)=Sof(H310)=Sof(C311)=1-FVAR(1)
 Sof(S101)=Sof(C108)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(H110)=Sof(C111)=FVAR(1)
 Sof(S241)=Sof(C248)=Sof(C249)=Sof(H249)=Sof(C250)=Sof(H250)=Sof(C251)=1-FVAR(2)
 Sof(S41)=Sof(C48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C10(H10), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C41(H41), C43(H43), C44(H44), C45(H45), C54(H54),
  C55(H55), C56(H56), C58(H58), C62(H62), C64(H64), C66(H66), C68(H68),
 C70(H70), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80),
  C81(H81), C82(H82), C83(H83), C84(H84), C86(H86), C87(H87), C88(H88),
 C89(H89), C90(H90), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
 C101(H101), C103(H103), C104(H104), C105(H105), C114(H114), C115(H115),
 C116(H116), C118(H118), C49(H49), C50(H50), C109(H109), C110(H110), C249(H249),
  C250(H250), C309(H309), C310(H310)
;
_shelx_res_checksum              57433
_shelx_hkl_checksum              62248
_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 A2_EP93F2R
_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 3.010
_oxdiff_exptl_absorpt_empirical_full_min 0.737