Oligosilanyl-Bridged Biscarbazoles: Structure, Synthesis, and Spectroscopic Properties
Feng, Siyang; Zhou, Zhikuan; Xiang, Xiaoshuang; Feng, Hongjie; Qu, Zhirong; Lu, Hua; ACS Omega  (2020) –; doi:10.1021/acsomega.0c02559

data_4517865
_publ_section_title
;
 Oligosilanyl-Bridged Biscarbazoles: Structure, Synthesis, and
 Spectroscopic Properties
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c02559
_journal_year                    2020
_chemical_formula_moiety         'C28 H26 N2 Si'
_chemical_formula_sum            'C28 H26 N2 Si'
_chemical_formula_weight         418.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                67.242(2)
_cell_angle_beta                 89.579(2)
_cell_angle_gamma                77.246(2)
_cell_formula_units_Z            4
_cell_length_a                   12.2392(12)
_cell_length_b                   12.9941(13)
_cell_length_c                   16.2298(17)
_cell_measurement_reflns_used    3740
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.60
_cell_volume                     2312.7(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.938
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19914
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.610
_diffrn_reflns_theta_min         1.712
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0471 before and 0.0316 after correction. The Ratio of minimum to maximum transmission is 0.9169. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         11142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0584P)^2^+0.4243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7186
_reflns_number_total             11142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02559_si_002.cif
_cod_data_source_block           mo190304d
_cod_database_code               4517865
_shelx_shelxl_version_number     2014/7
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C17(H17),
 C18(H18), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31),
  C32(H32), C33(H33), C36(H36), C38(H38), C39(H39), C45(H45), C46(H46),
 C48(H48), C51(H51), C52(H52), C53(H53), C54(H54)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C56(H56A,
 H56B,H56C)
;
_shelx_res_checksum              22404
_shelx_hkl_checksum              33133
_olex2_submission_special_instructions 'No special instructions were received'