Aggregation-Induced Electrochemiluminescence of Tetraphenylbenzosilole Derivatives in an Aqueous Phase System for Ultrasensitive Detection of Hexavalent Chromium.
Guo, Jinna; Feng, Weiqiang; Du, Peiyao; Zhang, Ruizhong; Liu, Jia; Liu, Yu; Wang, Zhiming; Lu, Xiaoquan; Analytical chemistry 92 (2020) 14838–14845; doi:10.1021/acs.analchem.0c03709

data_1559392
_publ_section_title
;
 Aggregation-Induced Electrochemiluminescence of Tetraphenylbenzosilole
 Derivatives in an Aqueous Phase System for Ultrasensitive Detection of
 Hexavalent Chromium.
;
_journal_issue                   21
_journal_name_full               'Analytical chemistry'
_journal_page_first              14838
_journal_page_last               14845
_journal_paper_doi               10.1021/acs.analchem.0c03709
_journal_volume                  92
_journal_year                    2020
_chemical_formula_moiety         'C34 H22 N2 Si, 2(C2 H6 O)'
_chemical_formula_sum            'C38 H34 N2 O2 Si'
_chemical_formula_weight         578.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8883(7)
_cell_length_b                   7.2668(3)
_cell_length_c                   34.9364(13)
_cell_measurement_reflns_used    9122
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.33
_cell_volume                     6318.5(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            45594
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.486
_diffrn_reflns_theta_min         2.471
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1299 before and 0.0441 after correction.
The Ratio of minimum to maximum transmission is 0.9254.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6496
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1009P)^2^+5.9039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5047
_reflns_number_total             6496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac0c03709_si_002.cif
_cod_data_source_block           191030_sisscn_0ma
_cod_depositor_comments          'Adding full bibliography for 1559392.cif.'
_cod_database_code               1559392
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C38-C37
 1.5 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.001
 O1-C36
 1.45 with sigma of 0.001
 O1-C35
 2.5 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
C35: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
O1 \\sim C36 \\sim C35: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Everything fixed:
 H1
4.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C38(H38A,H38B)
4.c Me refined with riding coordinates:
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
4.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              70
_shelx_hkl_checksum              34213
_olex2_submission_special_instructions 'No special instructions were received'