Room-temperature phosphorescence of a supercooled liquid: kinetic stabilisation by desymmetrisation
Komura, Mao; Ogawa, Takuji; Tani, Yosuke; Chemical Science  (2021) –; doi:10.1039/D1SC03800A

data_1564610
_publ_section_title
;
 Room-temperature phosphorescence of a supercooled liquid: kinetic
 stabilisation by desymmetrisation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03800A
_journal_year                    2021
_chemical_formula_moiety         'C28 H44 Br2 O3 S Si2'
_chemical_formula_sum            'C28 H44 Br2 O3 S Si2'
_chemical_formula_weight         676.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-12 deposited with the CCDC.	2021-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.165(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1498(4)
_cell_length_b                   9.2174(3)
_cell_length_c                   25.7482(8)
_cell_measurement_reflns_used    14745
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.2860
_cell_measurement_theta_min      1.5840
_cell_volume                     3344.56(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.838
_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    -62.00 -36.00   0.50    1.30    --   12.33 -19.00  90.00   52
  2  \w    -18.00   8.00   0.50    1.30    --   12.33 -19.00  90.00   52
  3  \w    -37.00  34.00   0.50    1.30    --   12.33 -57.00 -60.00  142
  4  \w     14.00  41.00   0.50    1.30    --   12.33-119.00  46.00   54
  5  \w     32.00  83.00   0.50    1.30    --   12.33-155.00-110.00  102
  6  \w     -4.00  36.00   0.50    1.30    --   12.33 -99.00  30.00   80
  7  \w    -21.00  16.00   0.50    1.30    --   -7.17 -57.00  90.00   74
  8  \w    -81.00 -28.00   0.50    1.30    --   -7.17 -57.00  90.00  106
  9  \w    -80.00  16.00   0.50    1.30    --   -7.17 -57.00   0.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0273392000
_diffrn_orient_matrix_UB_12      -0.0015292000
_diffrn_orient_matrix_UB_13      0.0244604000
_diffrn_orient_matrix_UB_21      0.0045734000
_diffrn_orient_matrix_UB_22      -0.0763916000
_diffrn_orient_matrix_UB_23      -0.0020543000
_diffrn_orient_matrix_UB_31      0.0420097000
_diffrn_orient_matrix_UB_32      0.0093221000
_diffrn_orient_matrix_UB_33      -0.0127312000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            39231
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.564
_diffrn_reflns_theta_min         1.710
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-R
_exptl_absorpt_coefficient_mu    2.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
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    1.344
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         8607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+3.9682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6023
_reflns_number_total             8607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03800a3.cif
_cod_data_source_block           mk322_-150
_cod_database_code               1564610
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H44Br2O3SSi2
_chemical_oxdiff_usercomment     123K
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C14(H14), C11(H11), C16(H16), C12(H12), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C4(H4)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C21(H21A,H21B,
 H21C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C17(H17A,
 H17B,H17C), C28(H28A,H28B,H28C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C),
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              59096
_shelx_hkl_checksum              13040
_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 2.176
_oxdiff_exptl_absorpt_empirical_full_min 0.389