Construction of helicates based on six-coordinated silicon centres.
Guan, Yu-Tao; Ji, Heng; Yang, Ju; Yu, Sai-Sai; Liu, Ming; Chemical science 16 (2025) 14448–14454; doi:10.1039/d5sc03271g

data_1575100
_publ_section_title
;
 Construction of helicates based on six-coordinated silicon centres.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              14448
_journal_page_last               14454
_journal_paper_doi               10.1039/d5sc03271g
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C81 H57 N6 Na4 O19.5 Si2 [4(C4 H10 O), 3.5 (C2H3N)]'
_chemical_formula_sum            'C105 H107.5 N9.5 Na4 O23.5 Si2'
_chemical_formula_weight         2026.64
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2n51c8
_audit_creation_method
;FinalCif V113 by Daniel Kratzert, Freiburg 2025,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-07-08 deposited with the CCDC.	2025-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.0214(19)
_cell_length_b                   12.0214(19)
_cell_length_c                   46.609(12)
_cell_measurement_reflns_used    5903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      40.4175
_cell_measurement_theta_min      4.2465
_cell_volume                     5833(2)
_computing_cell_refinement       'SAINT V8.41'
_computing_data_collection       'Bruker APEX5 V2024-9'
_computing_data_reduction        'SAINT V8.41'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (G. Sheldrick)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1314
_diffrn_reflns_av_unetI/netI     0.1496
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            25946
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        50.391
_diffrn_reflns_theta_max         50.391
_diffrn_reflns_theta_min         4.246
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.987
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         7758
_refine_ls_number_restraints     592
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.2075
_refine_ls_R_factor_gt           0.0940
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2320
_refine_ls_wR_factor_ref         0.2719
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                2405
_reflns_number_total             7758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03271g2.cif
_cod_data_source_block           cu_xr2024023_88_01_gyt_2024110_sq
_cod_depositor_comments
'Adding full bibliography for 1575099--1575105.cif.'
_cod_original_formula_sum        'C105 H107.50 N9.50 Na4 O23.50 Si2'
_cod_database_code               1575100
_shelx_shelxl_version_number     2019/2
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              13667
_shelx_fab_checksum              64482