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_7247501
_publ_section_title
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 Probing local structure of glass with orientation-dependent luminescence.
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_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         'C48 H36 O2 Si2'
_chemical_formula_sum            'C48 H36 O2 Si2'
_chemical_formula_weight         700.990
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_Int_Tables_number      1
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.306(2)
_cell_angle_beta                 91.906(2)
_cell_angle_gamma                101.613(2)
_cell_formula_units_Z            4
_cell_length_a                   11.5209(5)
_cell_length_b                   11.6461(5)
_cell_length_c                   28.3488(12)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      72.478
_cell_measurement_theta_min      3.119
_cell_volume                     3723.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223.15
_diffrn_measured_fraction_theta_full 0.9833
_diffrn_measured_fraction_theta_max 0.9829
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.9833
_diffrn_reflns_Laue_measured_fraction_max 0.9829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            157009
_diffrn_reflns_point_group_measured_fraction_full 0.9411
_diffrn_reflns_point_group_measured_fraction_max 0.9401
_diffrn_reflns_theta_full        67.6786
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         1.56
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1274 before and 0.0907 after correction.
The Ratio of minimum to maximum transmission is 0.7277.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             1477.994
_exptl_crystal_size_max          0.527
_exptl_crystal_size_mid          0.415
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.5476
_refine_diff_density_min         -0.3516
_refine_diff_density_rms         0.0512
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.252(19)
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             28.3310
_refine_ls_goodness_of_fit_ref   1.0498
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    264
_refine_ls_number_parameters     1921
_refine_ls_number_reflns         25617
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.0489
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+3.1070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.897
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              34
_reflns_limit_l_min              -34
_reflns_number_gt                25265
_reflns_number_total             25617
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cp03565d3.cif
_cod_data_source_block           cu_yt4_142_EtOH_2_0m_a
_cod_depositor_comments
'Adding full bibliography for 7247498--7247501.cif.'
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               7247501
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Si(H,H) groups
2. Restrained distances
 Si30-H343 = Si30-H344 = Si26-H317 = Si26-H318 = Si21-H229 = Si21-H230 = Si17-
 H256 = Si17-H255 = Si12-H168 = Si12-H167 = Si89-H141 = Si89-H142 = Si38-H80 =
 Si38-H79 = Si1-H53 = Si1-H54
 1.49 with sigma of 0.02
 H53-H54
 2.4 with sigma of 0.04
 H142-H141
 2.4 with sigma of 0.04
 H318-H317
 2.4 with sigma of 0.04
 H343-H344
 2.4 with sigma of 0.04
 H80-H79
 2.4 with sigma of 0.04
 H230-H229
 2.4 with sigma of 0.04
 H256-H255
 2.4 with sigma of 0.04
 H167-H168
 2.4 with sigma of 0.04
 C213-H229
 2.75 with sigma of 0.04
 H229-C215
 2.75 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C15 \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C184(H249,H250), C207(H236,H235), C96(H148,H147), C295(H338,H337), C31(H73,
 H74), C8(H60,H59), C272(H324,H323), C119(H162,H161)
4.b Aromatic/amide H refined with riding coordinates:
 C188(H247), C270(H322), C227(H264), C44(H84), C110(H155), C217(H257),
 C268(H320), C22(H67), C136(H173), C105(H154), C122(H164), C315(H352), C27(H71),
  C269(H321), C48(H85), C187(H248), C267(H319), C276(H326), C278(H327),
 C35(H77), C99(H149), C43(H83), C11(H61), C116(H160), C17(H66), C292(H336),
 C113(H158), C34(H76), C180(H253), C121(H163), C28(H72), C112(H157), C4(H56),
 C275(H325), C23(H68), C226(H263), C14(H63), C15(H64), C36(H78), C12(H62),
 C132(H172), C42(H82), C123(H165), C198(H242), C287(H332), C100(H150),
 C115(H159), C190(H246), C104(H153), C111(H156), C281(H330), C33(H75),
 C286(H331), C91(H143), C3(H55), C193(H243), C102(H151), C200(H240), C305(H345),
  C291(H335), C182(H251), C307(H347), C306(H346), C225(H262), C179(H254),
 C103(H152), C289(H334), C297(H339), C131(H171), C203(H238), C308(H348),
 C204(H237), C212(H231), C199(H241), C218(H258), C6(H58), C181(H252), C5(H57),
 C124(H166), C94(H146), C41(H81), C16(H65), C279(H328), C300(H342), C129(H169),
 C92(H144), C288(H333), C312(H349), C211(H232), C314(H351), C224(H261),
 C220(H260), C137(H174), C298(H340), C313(H350), C299(H341), C219(H259),
 C280(H329), C201(H239), C25(H70), C209(H234), C130(H170), C24(H69), C191(H245),
  C93(H145), C50(H87), C139(H176), C49(H86), C192(H244), C51(H88), C138(H175),
 C210(H233)
;
_olex2_submission_special_instructions 'No special instructions were received'