The role of main group elements in shaping the properties of linearly-fused heterohexaarenes.
Espineira-Gutierrez, Adrian; Caro-Noakes, Ines; Zhang, Min; Mas-Torrent, Marta; Regulska, Elzbieta; Romero-Nieto, Carlos; Chemical communications (Cambridge, England) 61 (2025) 15590–15593; doi:10.1039/d5cc03235k

data_7134982
_publ_section_title
;
 The role of main group elements in shaping the properties of
 linearly-fused heterohexaarenes.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15590
_journal_page_last               15593
_journal_paper_doi               10.1039/d5cc03235k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C46 H52 Si2'
_chemical_formula_sum            'C46 H52 Si2'
_chemical_formula_weight         661.05
_chemical_name_systematic        Disila-hexaarene
_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             2024-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-28 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.407(10)
_cell_angle_beta                 81.941(10)
_cell_angle_gamma                74.764(8)
_cell_formula_units_Z            4
_cell_length_a                   9.869(6)
_cell_length_b                   12.442(7)
_cell_length_c                   32.249(19)
_cell_measurement_temperature    296.15
_cell_volume                     3764(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.1138
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            20144
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        22.464
_diffrn_reflns_theta_max         22.464
_diffrn_reflns_theta_min         1.705
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.7959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.8297.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       'Evaporation from chloroform'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         9659
_refine_ls_number_restraints     1331
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1791
_refine_ls_R_factor_gt           0.1091
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2711
_refine_ls_wR_factor_ref         0.3603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5070
_reflns_number_total             9659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03235k2.cif
_cod_data_source_block           elz
_cod_depositor_comments          'Adding full bibliography for 7134982.cif.'
_cod_database_code               7134982
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.969
_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
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Same fragment restrains
{C76_1, C59_1, Si3_1, C67_1, Si4_1, C68_1, Si4_1, C69_1, Si3_1, C70_1, C71_1,
C72_1, C73_1, C74_1, C75_1, C64_1, C65_1, C66_1, C60_1, C61_1, C63_1, C62_1,
C57_1, C58_1, C47_1, C48_1, C49_1, C50_1, C51_1, C56_1, C55_1, C54_1, C53_1,
C52_1, C81_1, C82_1, C83_1, C84_1, C77_1, C78_1, C79_1, C80_1, C85_1, C86_1,
C87_1, C88_1, C89_1, C90_1, C91_1, C92_1, C67_1, C68_1, C69_1, C70_1, C71_1,
C72_1, C73_1, C74_1, C75_1, C76_1, C64_1, C65_1, C66_1, C60_1, C61_1, C63_1,
C62_1, C57_1, C58_1, C59_1, C47_1, C48_1, C49_1, C50_1, C51_1, C52_1, C53_1,
C54_1, C55_1, C56_1, C85_1, C86_1, C87_1, C88_1, C89_1, C90_1, C91_1, C92_1,
C81_1, C82_1, C83_1, C84_1, C77_1, C78_1, C79_1, C80_1} sigma for 1-2: 0.02,
1-3: 0.04
as in
{C1_1, C1K_1, Si1_1, C2_1, Si2_1, C3_1, Si3_1, C4_1, Si4_1, C5_1, C6_1, C7_1,
C8_1, C9_1, C10_1, C11_1, C12_1, C13_1, C14_1, C15_1, C16_1, C17_1, C18_1,
C19_1, C20_1, C21_1, C22_1, C23_1, C24_1, C25_1, C26_1, C27_1, C28_1, C29_1,
C30_1, C31_1, C32_1, C33_1, C34_1, C35_1, C36_1, C37_1, C38_1, C39_1, C41_1,
C42_1, C43_1, C44_1, C45_1, C46_1, C47_1, C48_1, C49_1, C50_1, C51_1, C52_1,
C53_1, C54_1, C55_1, C56_1, C57_1, C58_1, C59_1, C60_1, C61_1, C62_1, C63_1,
C64_1, C65_1, C66_1, C67_1, C68_1, C69_1, C70_1, C71_1, C72_1, C73_1, C74_1,
C75_1, C76_1, C77_1, C78_1, C79_1, C80_1, C81_1, C82_1, C83_1, C84_1, C85_1,
C86_1, C87_1, C88_1, C89_1, C90_1, C91_1, C92_1}
4.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C77(H77A,H77B), C78(H78A,H78B),
  C79(H79A,H79B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C85(H85A,
 H85B), C86(H86A,H86B), C87(H87A,H87B), C89(H89A,H89B), C90(H90A,H90B),
 C91(H91A,H91B)
4.b Aromatic/amide H refined with riding coordinates:
 C1K(H1K), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C13(H13), C16(H16),
 C17(H17), C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C48(H48),
  C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C59(H59), C62(H62),
 C63(H63), C66(H66), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74)
4.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C42(H42A,H42B,H42C), C46(H46A,H46B,
 H46C), C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C), C92(H92A,
 H92B,H92C)
;
_shelx_res_checksum              97526
_olex2_exptl_crystal_mounting_method 'In the oil'
_olex2_submission_original_sample_id AE265
_olex2_submission_special_instructions 'No special instructions were received'