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_1568917
_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                 96.315(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2260(6)
_cell_length_b                   9.2521(5)
_cell_length_c                   26.4803(10)
_cell_measurement_reflns_used    8681
_cell_measurement_temperature    300
_cell_measurement_theta_max      28.2320
_cell_measurement_theta_min      1.5500
_cell_volume                     3464.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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 0.799
_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    -10.00  33.00   0.50    3.03    --    6.07 -99.00  30.00   86
  2  \w      8.00  37.00   0.50    3.03    --    6.07 -99.00 -30.00   58
  3  \w    -28.00  21.00   0.50    3.03    --    0.80 -80.00-178.00   98
  4  \w    -11.00  14.00   0.50    3.03    --    6.07 -99.00 -60.00   50
  5  \w     -2.00  37.00   0.50    3.03    --    6.07 -99.00  90.00   78
  6  \w     -9.00  34.00   0.50    3.03    --    6.07 -99.00 120.00   86
  7  \w     -7.00  68.00   0.50    3.03    --    0.80  37.00-180.00  150
  8  \w    -18.00   8.00   0.50    3.03    --    0.80  80.00 -55.00   52
;
_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      -0.0026803000
_diffrn_orient_matrix_UB_12      -0.0299965000
_diffrn_orient_matrix_UB_13      0.0244456000
_diffrn_orient_matrix_UB_21      -0.0272255000
_diffrn_orient_matrix_UB_22      -0.0583124000
_diffrn_orient_matrix_UB_23      -0.0111444000
_diffrn_orient_matrix_UB_31      0.0420465000
_diffrn_orient_matrix_UB_32      -0.0397211000
_diffrn_orient_matrix_UB_33      -0.0021140000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.163
_diffrn_reflns_theta_min         1.547
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-R
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.297
_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         0.681
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0956P)^2^+1.0912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4585
_reflns_number_total             8956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00838j5.cif
_cod_data_source_block           SO-B
_cod_depositor_comments
'Adding full bibliography for 1568914--1568920.cif.'
_cod_database_code               1568917
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H44Br2O3SSi2
_chemical_oxdiff_usercomment     300K-10sec
_reflns_odcompleteness_completeness 99.97
_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              40397
_shelx_hkl_checksum              67200
_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 3.228
_oxdiff_exptl_absorpt_empirical_full_min 0.539