Probing local structure of glass with orientation-dependent luminescence.
Tokoro, Yuichiro; Nakagawa, Tetsuya; Yamamoto, Shin-Ichi; Koizumi, Toshio; Oyama, Toshiyuki; Physical chemistry chemical physics : PCCP 25 (2023) 28113–28118; doi:10.1039/d3cp03565d

data_7247499
_publ_section_title
;
 Probing local structure of glass with orientation-dependent luminescence.
;
_journal_issue                   41
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              28113
_journal_page_last               28118
_journal_paper_doi               10.1039/d3cp03565d
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C40 H32 O2 Si2'
_chemical_formula_sum            'C40 H32 O2 Si2'
_chemical_formula_weight         600.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                110.8110(10)
_cell_angle_beta                 104.5240(10)
_cell_angle_gamma                95.2830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.45340(10)
_cell_length_b                   12.10100(10)
_cell_length_c                   13.64410(10)
_cell_measurement_reflns_used    23098
_cell_measurement_temperature    223
_cell_measurement_theta_max      71.1640
_cell_measurement_theta_min      4.2120
_cell_volume                     1530.15(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9813
_diffrn_measured_fraction_theta_max 0.9800
_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    -13.00 104.00   0.50    0.50    --   45.20  22.00 -82.00  234
  2  \w     22.00 134.00   0.50    0.50    --   98.30 -22.00 111.00  224
  3  \w    154.00 187.00   0.50    0.50    --   98.30  22.00 -82.00   66
  4  \w     56.00 114.00   0.50    0.50    --   98.30  22.00 -82.00  116
  5  \w     37.00  63.00   0.50    0.50    --   45.20  82.00-120.00   52
  6  \w    -44.00  84.00   0.50    0.50    --   45.20 -77.00 -90.00  256
  7  \w     62.00 108.00   0.50    0.50    --   45.20 -22.00 111.00   92
  8  \w    -44.00  -9.00   0.50    0.50    --   45.20 -22.00 111.00   70
  9  \w      4.00  30.00   0.50    0.50    --   45.20  82.00-120.00   52
 10  \w      6.00  42.00   0.50    0.50    --   45.20 -22.00 111.00   72
 11  \w      6.00  56.00   0.50    0.50    --   48.00  81.00  39.74  100
 12  \w     64.00 137.00   0.50    0.50    --   48.00  68.00 -24.29  146
 13  \w     16.00  60.00   0.50    0.50    --   48.00  68.00 -24.29   88
 14  \w     57.00 102.00   0.50    0.50    --   48.00  81.00  39.74   90
 15  \w     15.00  91.00   0.50    0.50    --   56.00  82.00-139.41  152
 16  \w    114.00 140.00   0.50    0.50    --   56.00  82.00-139.41   52
 17  \w     19.00  50.00   0.50    0.50    --   60.00  80.00  70.74   62
 18  \w     71.00 148.00   0.50    0.50    --   60.00  80.00  70.74  154
 19  \w    116.00 142.00   0.50    0.50    --   64.00  82.00 101.25   52
 20  \w     23.00  68.00   0.50    0.50    --   64.00  82.00 134.05   90
 21  \w     22.00  53.00   0.50    0.50    --   64.00  82.00 101.25   62
 22  \w    119.00 146.00   0.50    0.50    --   64.00  82.00 134.05   54
 23  \w     87.00 159.00   0.50    0.50    --   72.00  82.00-102.39  144
 24  \w     30.00  72.00   0.50    0.50    --   72.00  82.00-102.39   84
 25  \w     30.00  55.00   0.50    0.50    --   72.00  81.00 -16.13   50
 26  \w     34.00  68.00   0.50    0.50    --   76.00  81.00 157.59   68
 27  \w     34.00  87.00   0.50    0.50    --   76.00  81.00 -65.19  106
 28  \w    140.00 165.00   0.50    0.50    --   76.00  81.00 -65.19   50
 29  \w    125.00 151.00   0.50    0.50    --   76.00  81.00  19.97   52
 30  \w     35.00  61.00   0.50    0.50    --   76.00  81.00  19.97   52
 31  \w     35.00  63.00   0.50    0.50    --   76.00  81.00-159.66   56
 32  \w    128.00 164.00   0.50    0.50    --   76.00  81.00 157.59   72
 33  \w     38.00  66.00   0.50    0.50    --   80.00  81.00  64.34   56
 34  \w     58.00 186.00   0.50    0.50    --   98.30  79.00-129.02  256
 35  \w    131.00 156.00   0.50    0.50    --   98.30  82.00 -90.00   50
 36  \w    105.00 136.00   0.50    0.50    --   98.30  82.00 120.00   62
 37  \w     56.00  96.00   0.50    0.50    --   98.30  82.00 -90.00   80
 38  \w     56.00  84.00   0.50    0.50    --   98.30  82.00 120.00   56
 39  \w    140.00 188.00   0.50    0.50    --   98.30  82.00-180.00   96
 40  \w     56.00 118.00   0.50    0.50    --   98.30  82.00-180.00  124
 41  \w     46.00 139.00   0.50    0.50    --   98.30 -82.00-120.00  186
 42  \w    101.00 186.00   0.50    0.50    --   98.30  82.00 -60.00  170
 43  \w    152.00 186.00   0.50    0.50    --   98.30  82.00  90.00   68
 44  \w     59.00 122.00   0.50    0.50    --   98.30  77.00  30.00  126
 45  \w    107.00 140.00   0.50    0.50    --   98.30 -30.00 -90.00   66
 46  \w     56.00 107.00   0.50    0.50    --   98.30  82.00  90.00  102
 47  \w     60.00  96.00   0.50    0.50    --   98.30  82.00 -60.00   72
 48  \w     50.00  97.00   0.50    0.50    --   98.30 -30.00 -90.00   94
 49  \w      9.00  38.00   0.50    0.50    --   98.30 -30.00 -90.00   58
 50  \w    124.00 150.00   0.50    0.50    --   98.30  82.00   0.00   52
 51  \w    131.00 156.00   0.50    0.50    --   98.30  82.00 150.00   50
 52  \w     59.00 128.00   0.50    0.50    --   98.30  82.00 150.00  138
 53  \w     58.00 115.00   0.50    0.50    --   98.30  82.00   0.00  114
 54  \w    104.00 188.00   0.50    0.50    --   98.30  61.00  90.00  168
 55  \w     55.00 140.00   0.50    0.50    --   98.30 -82.00  90.00  170
 56  \w     59.00 138.00   0.50    0.50    --   98.30  77.00-150.00  158
 57  \w     12.00  50.00   0.50    0.50    --   98.30 -82.00  90.00   76
 58  \w     86.00 126.00   0.50    0.50    --   98.30  61.00 -60.00   80
 59  \w     68.00 187.00   0.50    0.50    --   98.30  61.00   0.00  238
 60  \w     80.00 182.00   0.50    0.50    --   98.30  61.00 150.00  204
 61  \w    152.00 177.00   0.50    0.50    --   98.30  82.00  60.00   50
 62  \w    104.00 129.00   0.50    0.50    --   98.30  82.00 -90.00   50
 63  \w     57.00 140.00   0.50    0.50    --   98.30  82.00  60.00  166
 64  \w    150.00 178.00   0.50    0.50    --   98.30  61.00  60.00   56
 65  \w     52.00 141.00   0.50    0.50    --   98.30 -82.00  30.00  178
 66  \w     69.00 120.00   0.50    0.50    --   98.30 -82.00 -90.00  102
 67  \w     13.00  38.00   0.50    0.50    --   98.30 -82.00  30.00   50
 68  \w    109.00 142.00   0.50    0.50    --   98.30  82.00 -30.00   66
 69  \w     56.00  81.00   0.50    0.50    --   98.30  82.00 -30.00   50
 70  \w     15.00  59.00   0.50    0.50    --   98.30 -82.00 -90.00   88
 71  \w     81.00 136.00   0.50    0.50    --   98.30  61.00  60.00  110
 72  \w     32.00 124.00   0.50    0.50    --   98.30 -82.00 150.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0403316000
_diffrn_orient_matrix_UB_12      0.1022742000
_diffrn_orient_matrix_UB_13      -0.0359314000
_diffrn_orient_matrix_UB_21      0.1419681000
_diffrn_orient_matrix_UB_22      0.0288272000
_diffrn_orient_matrix_UB_23      -0.0094518000
_diffrn_orient_matrix_UB_31      -0.0486151000
_diffrn_orient_matrix_UB_32      -0.0896252000
_diffrn_orient_matrix_UB_33      -0.1212520000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37126
_diffrn_reflns_theta_full        71.7458
_diffrn_reflns_theta_max         71.75
_diffrn_reflns_theta_min         3.99
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'transparent green'
_exptl_crystal_density_diffrn    1.3040
_exptl_crystal_description       block
_exptl_crystal_F_000             634.6922
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.4353
_refine_diff_density_min         -0.5562
_refine_diff_density_rms         0.0425
_refine_ls_d_res_high            0.8118
_refine_ls_d_res_low             11.0825
_refine_ls_goodness_of_fit_ref   1.0412
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0412
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.5043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5385
_reflns_number_total             5873
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cp03565d3.cif
_cod_data_source_block           yt5_010_190218
_cod_depositor_comments
'Adding full bibliography for 7247498--7247501.cif.'
_cod_database_code               7247499
_chemical_oxdiff_formula         C40H32O2Si2
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C37(H37a,H37b)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C2aa(H2aa), C13(H13), C1aa(H1aa), C32(H32), C41(H41), C31(H31),
 C28(H28), C5aa(H5aa), C4aa(H4aa), C14(H14), C3aa(H3aa), C36(H36), C4(H4),
 C2(H2), C1(H1), C6aa(H6aa), C18(H18), C7aa(H7aa), C17(H17), C12(H12), C20(H20),
  C0aa(H0aa), C3(H3)
;
_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 1.533
_oxdiff_exptl_absorpt_empirical_full_min 0.792