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_7247498
_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_absolute_configuration unk
_chemical_formula_moiety         '1(C48 H36 O2 Si2)'
_chemical_formula_sum            'C48 H35.787 O2 Si2'
_chemical_formula_weight         700.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-22
_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                90
_cell_angle_beta                 90.5504(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   11.19827(2)
_cell_length_b                   27.60749(6)
_cell_length_c                   18.08478(4)
_cell_measurement_reflns_used    210534
_cell_measurement_temperature    223
_cell_measurement_theta_max      71.5840
_cell_measurement_theta_min      4.0250
_cell_volume                     5590.76(2)
_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 0.9802
_diffrn_measured_fraction_theta_max 0.9796
_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    -43.00 134.00   0.50    1.04    --   45.50  13.00-131.00  354
  2  \w      9.00 188.00   0.50    4.17    --   98.30  13.00-131.00  358
  3  \w      9.00 188.00   0.50    4.17    --   98.30 -13.00  56.00  358
  4  \w    -43.00  75.00   0.50    1.04    --   45.50 -57.00   0.00  236
  5  \w    -43.00 134.00   0.50    1.04    --   45.50 -13.00  56.00  354
  6  \w      4.00 134.00   0.50    1.04    --   45.50  82.00  30.00  260
  7  \w     16.00 134.00   0.50    1.04    --   45.50  57.00-150.00  236
  8  \w      7.00 134.00   0.50    1.04    --   45.50  77.00   0.00  254
  9  \w     16.00 134.00   0.50    1.04    --   45.50  57.00 -60.00  236
 10  \w    -43.00  75.00   0.50    1.04    --   45.50 -57.00-180.00  236
 11  \w      4.00 134.00   0.50    1.04    --   45.50  82.00 -60.00  260
 12  \w      7.00 134.00   0.50    1.04    --   45.50  38.00-120.00  254
 13  \w     59.00 188.00   0.50    4.17    --   98.30  77.00-120.00  258
 14  \w     56.00 188.00   0.50    4.17    --   98.30  82.00 -90.00  264
 15  \w     56.00 188.00   0.50    4.17    --   98.30  82.00 -91.53  264
 16  \w     56.00 188.00   0.50    4.17    --   98.30  82.00-120.00  264
 17  \w     56.00 188.00   0.50    4.17    --   98.30  82.00 -30.00  264
 18  \w      9.00 130.00   0.50    4.17    --   98.30 -61.00-120.00  242
 19  \w     59.00 188.00   0.50    4.17    --   98.30  76.00  17.86  258
 20  \w      9.00 138.00   0.50    4.17    --   98.30 -77.00 -60.00  258
 21  \w     59.00 188.00   0.50    4.17    --   98.30  77.00 -30.00  258
 22  \w     59.00 188.00   0.50    4.17    --   98.30  77.00   0.00  258
 23  \w     56.00 188.00   0.50    4.17    --   98.30  81.00 -70.17  264
 24  \w     58.00 188.00   0.50    4.17    --   98.30  78.00 -96.40  260
 25  \w     59.00 188.00   0.50    4.17    --   98.30  77.00 -60.00  258
 26  \w     59.00 188.00   0.50    4.17    --   98.30  77.00 -90.00  258
 27  \w     56.00 188.00   0.50    4.17    --   98.30  82.00 -60.00  264
 28  \w     67.00 188.00   0.50    4.17    --   98.30  61.00-120.00  242
 29  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00-120.00  264
 30  \w     59.00 188.00   0.50    4.17    --   98.30  77.00  30.00  258
 31  \w     56.00 188.00   0.50    4.17    --   98.30  82.00   0.00  264
 32  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00 -60.00  264
 33  \w     58.00 188.00   0.50    4.17    --   98.30  78.00 -18.13  260
 34  \w     16.00 134.00   0.50    1.04    --   45.50  57.00  30.00  236
 35  \w      4.00 134.00   0.50    1.04    --   45.50  82.00   0.00  260
 36  \w     16.00 134.00   0.50    1.04    --   45.50  57.00   0.00  236
 37  \w    -43.00  87.00   0.50    1.04    --   45.50 -82.00 120.00  260
 38  \w    -43.00  87.00   0.50    1.04    --   45.50 -82.00   0.00  260
 39  \w      4.00 134.00   0.50    1.04    --   45.50  82.00-150.00  260
 40  \w      4.00 134.00   0.50    1.04    --   45.50  82.00  90.00  260
 41  \w      7.00 134.00   0.50    1.04    --   45.50  77.00  60.00  254
 42  \w    -43.00  87.00   0.50    1.04    --   45.50 -82.00-180.00  260
 43  \w      7.00 134.00   0.50    1.04    --   45.50  77.00-180.00  254
 44  \w      7.00 134.00   0.50    1.04    --   45.50  77.00 120.00  254
 45  \w      4.00 134.00   0.50    1.04    --   45.50  82.00-180.00  260
 46  \w     56.00 188.00   0.50    4.17    --   98.30  82.00 120.00  264
 47  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00  60.00  264
 48  \w     56.00 188.00   0.50    4.17    --   98.30  82.00-180.00  264
 49  \w     52.00 188.00   0.50    4.17    --   98.30  30.00 150.00  272
 50  \w     56.00 188.00   0.50    4.17    --   98.30  82.00  30.00  264
 51  \w     56.00 188.00   0.50    4.17    --   98.30  82.00-150.00  264
 52  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00 150.00  264
 53  \w     59.00 188.00   0.50    4.17    --   98.30  77.00  60.00  258
 54  \w     59.00 188.00   0.50    4.17    --   98.30  76.00-155.46  258
 55  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00   0.00  264
 56  \w     56.00 188.00   0.50    4.17    --   98.30  82.00  90.00  264
 57  \w     59.00 188.00   0.50    4.17    --   98.30  77.00-150.00  258
 58  \w     61.00 188.00   0.50    4.17    --   98.30  73.00 175.39  254
 59  \w     59.00 188.00   0.50    4.17    --   98.30  77.00 150.00  258
 60  \w     56.00 188.00   0.50    4.17    --   98.30  82.00 150.00  264
 61  \w     56.00 188.00   0.50    4.17    --   98.30  82.00  60.00  264
 62  \w     59.00 188.00   0.50    4.17    --   98.30  77.00  90.00  258
 63  \w     59.00 188.00   0.50    4.17    --   98.30  77.00 120.00  258
 64  \w     59.00 188.00   0.50    4.17    --   98.30  77.00-180.00  258
 65  \w     60.00 188.00   0.50    4.17    --   98.30  75.00  85.86  256
 66  \w     57.00 188.00   0.50    4.17    --   98.30  79.00  73.18  262
 67  \w     67.00 188.00   0.50    4.17    --   98.30  61.00 150.00  242
 68  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00-180.00  264
 69  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00  90.00  264
 70  \w    -43.00 134.00   0.50    1.04    --   45.50 -13.00  56.00  354
 71  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00-120.00  354
 72  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00 -60.00  354
 73  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00-180.00  354
 74  \w    -43.00 134.00   0.50    1.04    --   45.50  13.00-131.00  354
 75  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00 -90.00  354
 76  \w    -43.00 134.00   0.50    1.04    --   45.50 -13.00  56.00  354
 77  \w    -43.00 134.00   0.50    1.04    --   45.50  13.00-131.00  354
 78  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00 -30.00  354
 79  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00   0.00  354
 80  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00  30.00  354
 81  \w    -43.00 134.00   0.50    1.04    --   45.50  19.00-150.00  354
 82  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00 120.00  264
 83  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00  30.00  264
 84  \w     63.00 188.00   0.50    4.17    --   98.30  70.00 110.40  250
 85  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00 -30.00  264
 86  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00 -90.00  264
 87  \w      9.00 141.00   0.50    4.17    --   98.30 -82.00-150.00  264
 88  \w      9.00 130.00   0.50    4.17    --   98.30 -61.00 -90.00  242
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1335812000
_diffrn_orient_matrix_UB_12      0.0074620000
_diffrn_orient_matrix_UB_13      -0.0161551000
_diffrn_orient_matrix_UB_21      -0.0255743000
_diffrn_orient_matrix_UB_22      -0.0057437000
_diffrn_orient_matrix_UB_23      -0.0833940000
_diffrn_orient_matrix_UB_31      -0.0207870000
_diffrn_orient_matrix_UB_32      0.0549945000
_diffrn_orient_matrix_UB_33      -0.0065333000
_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  0.0864
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            427146
_diffrn_reflns_theta_full        71.9060
_diffrn_reflns_theta_max         71.91
_diffrn_reflns_theta_min         3.95
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45427
_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 yellow'
_exptl_crystal_density_diffrn    1.2487
_exptl_crystal_description       block
_exptl_crystal_F_000             2215.6823
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.3426
_refine_diff_density_min         -0.3567
_refine_diff_density_rms         0.0296
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.008(9)
_refine_ls_d_res_high            0.8110
_refine_ls_d_res_low             11.1978
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0446
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    212
_refine_ls_number_parameters     1576
_refine_ls_number_reflns         21511
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.0391
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0647P)^2^+0.5791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.963
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              33
_reflns_limit_k_min              -32
_reflns_limit_l_max              22
_reflns_limit_l_min              -22
_reflns_number_gt                20973
_reflns_number_total             21511
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cp03565d3.cif
_cod_data_source_block           yt4_142_190125
_cod_depositor_comments
'Adding full bibliography for 7247498--7247501.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7247498
_chemical_oxdiff_formula         C48H36O2Si2
_reflns_odcompleteness_completeness 99.94
_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. Restrained distances
 Si4-H4a = Si4-H4b = Si1-H1a = Si1-H1b = Si3-H7da = Si3-H0ea = Si2-H9da = Si2-
 H8da
 1.415 with sigma of 0.02
 H5fa-Si6 = Si6-H6fa
 1.415 with sigma of 0.02
 H4fa-Si5 = Si5-H3fa
 1.415 with sigma of 0.02
 Si1a-C33
 1.89 with sigma of 0.003
 C3da-Si1a
 1.89 with sigma of 0.006
 O12-C7da
 2.36 with sigma of 0.002
 C8da-C51
 2.38 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
C7ca \\sim C6ca \\sim C5ca \\sim C0da \\sim C9ca \\sim C8ca \\sim C1da \\sim
Si0a: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C7da \\sim C6da \\sim C5da \\sim C4da \\sim C2da \\sim C3da \\sim Si1a \\sim
C8da: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Si0a) \\sim Ueq, Uanis(C5ca) \\sim Ueq, Uanis(C0da) \\sim Ueq,
Uanis(C9ca) \\sim Ueq, Uanis(C8ca) \\sim Ueq, Uanis(C7ca) \\sim Ueq,
Uanis(C6ca) \\sim Ueq, Uanis(C1da) \\sim Ueq, Uanis(Si1a) \\sim Ueq,
Uanis(C3da) \\sim Ueq, Uanis(C2da) \\sim Ueq, Uanis(C4da) \\sim Ueq,
Uanis(C5da) \\sim Ueq, Uanis(C6da) \\sim Ueq, Uanis(C7da) \\sim Ueq,
Uanis(C8da) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(Si1a)=Sof(C3da)=Sof(C2da)=Sof(H7ea)=Sof(C4da)=Sof(H8ea)=Sof(C5da)=
 Sof(H9ea)=Sof(C6da)=Sof(H0fa)=Sof(C7da)=Sof(C8da)=Sof(H1fa)=Sof(H2fa)=1-FVAR(1)
 Sof(Si5)=Sof(C69)=Sof(C104)=Sof(Ho)=Sof(C4ca)=Sof(H7ca)=Sof(C3ca)=Sof(H6da)=
 Sof(C2ca)=Sof(H4da)=Sof(C119)=Sof(C138)=Sof(Hz)=Sof(H0aa)=Sof(H3fa)=Sof(H4fa)=
 FVAR(1)
 Sof(Si0a)=Sof(C5ca)=Sof(C0da)=Sof(H4ea)=Sof(C9ca)=Sof(H3ea)=Sof(C8ca)=
 Sof(H2ea)=Sof(C7ca)=Sof(H1ea)=Sof(C6ca)=Sof(C1da)=Sof(H5ea)=Sof(H6ea)=1-FVAR(2)
 Sof(Si6)=Sof(C61)=Sof(C106)=Sof(C114)=Sof(Ht)=Sof(C6ba)=Sof(H4ca)=Sof(C5ba)=
 Sof(H2da)=Sof(C153)=Sof(H5aa)=Sof(C108)=Sof(Hp)=Sof(Hq)=Sof(H5fa)=Sof(H6fa)=
 FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C38(H38a,H38b), C54(H54a,H54b), C59(Hb,Hc), C108(Hp,Hq), C124(Hw,Hx), C138(Hz,
 H0aa), C1da(H5ea,H6ea), C8da(H1fa,H2fa)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C30(H30), C35(H35), C40(H40), C45(H45), C48(H), C52(H52), C56(H56),
 C57(H57), C58(Ha), C60(H60), C62(Hd), C65(H65), C67(He), C71(H71), C73(Hf),
 C75(Hg), C77(H77), C79(H79), C82(Hh), C84(Hi), C86(Hj), C87(H87), C89(H89),
 C91(H91), C93(Hk), C94(Hl), C99(Hm), C102(Hn), C104(Ho), C112(Hr), C113(Hs),
 C114(Ht), C115(H115), C117(Hu), C118(H118), C120(Hv), C123(H123), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C131(H131), C132(Hy),
 C133(H133), C141(H1aa), C143(H2aa), C145(H3aa), C149(H4aa), C150(H150),
 C152(H152), C153(H5aa), C155(H6aa), C156(H7aa), C6(H8aa), C7(H9aa), C8(H0ba),
 C4aa(H1ba), C1aa(H2ba), C2aa(H3ba), C5aa(H4ba), C0aa(H5ba), C6aa(H6ba),
 C3aa(H7ba), C9ba(H8ba), C8aa(H9ba), C3ba(H0ca), C9aa(H1ca), C0ba(H2ca),
 C7aa(H3ca), C6ba(H4ca), C0ca(H5ca), C7ba(H6ca), C4ca(H7ca), C1ca(H8ca),
 C12(H9ca), C4ba(H0da), C2ba(H1da), C5ba(H2da), C8ba(H3da), C2ca(H4da),
 C1ba(H5da), C3ca(H6da), C7ca(H1ea), C8ca(H2ea), C9ca(H3ea), C0da(H4ea),
 C2da(H7ea), C4da(H8ea), C5da(H9ea), C6da(H0fa)
5.c Fitted hexagon refined as free rotating group:
 C5ca(C6ca,C7ca,C8ca,C9ca,C0da), C7da(C3da,C2da,C4da,C5da,C6da)
;
_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 1.982
_oxdiff_exptl_absorpt_empirical_full_min 0.525