Photoinduced crystal melting with luminescence evolution based on conformational isomerisation.
Komura, Mao; Sotome, Hikaru; Miyasaka, Hiroshi; Ogawa, Takuji; Tani, Yosuke; Chemical science 14 (2023) 5302–5308; doi:10.1039/d3sc00838j

data_1568919
_publ_section_title
;
 Photoinduced crystal melting with luminescence evolution based on
 conformational isomerisation.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5302
_journal_page_last               5308
_journal_paper_doi               10.1039/d3sc00838j
_journal_volume                  14
_journal_year                    2023
_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             2023-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.355(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2236(6)
_cell_length_b                   9.2423(4)
_cell_length_c                   26.4876(9)
_cell_measurement_reflns_used    8355
_cell_measurement_temperature    300
_cell_measurement_theta_max      28.4430
_cell_measurement_theta_min      1.5420
_cell_volume                     3460.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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      300
_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 0.803
_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    -21.00  15.00   0.50    3.81    --    0.96  80.00 -55.00   72
  2  \w      6.00  36.00   0.50    3.81    --    6.23 -99.00 -90.00   60
  3  \w      3.00  35.00   0.50    3.81    --    6.23 -99.00 120.00   64
  4  \w    -10.00  37.00   0.50    3.81    --    6.23 -99.00  30.00   94
  5  \w    -11.00  36.00   0.50    3.81    --    6.23 -99.00 -30.00   94
  6  \w    -41.00  23.00   0.50    3.81    --    0.96 -80.00-178.00  128
  7  \w     -6.00  67.00   0.50    3.81    --    0.96  37.00  30.00  146
;
_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      0.0027353000
_diffrn_orient_matrix_UB_12      -0.0301031000
_diffrn_orient_matrix_UB_13      -0.0244226000
_diffrn_orient_matrix_UB_21      0.0272489000
_diffrn_orient_matrix_UB_22      -0.0583151000
_diffrn_orient_matrix_UB_23      0.0111878000
_diffrn_orient_matrix_UB_31      -0.0420453000
_diffrn_orient_matrix_UB_32      -0.0397758000
_diffrn_orient_matrix_UB_33      0.0021028000
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            41026
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.198
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-R
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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    1.299
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         9014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1248
_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^)+(0.0948P)^2^+1.3573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4531
_reflns_number_total             9014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00838j5.cif
_cod_data_source_block           SO-C
_cod_depositor_comments
'Adding full bibliography for 1568914--1568920.cif.'
_cod_database_code               1568919
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H44Br2O3SSi2
_chemical_oxdiff_usercomment     300K-20sec
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.240
_reflns_odcompleteness_completeness 99.95
_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:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
2.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              10047
_shelx_hkl_checksum              95767
_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 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.575