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_1575099
_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_formula_moiety         'C66 H50 N6 Na4 O25 Si2'
_chemical_formula_sum            'C66 H50 N6 Na4 O25 Si2'
_chemical_formula_weight         1475.26
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2n51b7
_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            6
_cell_length_a                   12.1103(16)
_cell_length_b                   12.1103(16)
_cell_length_c                   94.10(2)
_cell_measurement_reflns_used    2799
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      47.436
_cell_measurement_theta_min      4.2415
_cell_volume                     11952(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection       'Bruker APEX5 V2024-9'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0947
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       109
_diffrn_reflns_limit_l_min       -109
_diffrn_reflns_number            19286
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        63.648
_diffrn_reflns_theta_max         63.648
_diffrn_reflns_theta_min         5.642
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.3201
_exptl_absorpt_correction_T_min  0.1581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48
(2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0013(2)
_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   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2178
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1760
_refine_ls_R_factor_gt           0.1432
_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^)+(0.0600P)^2^+120.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3130
_refine_ls_wR_factor_ref         0.3272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1279
_reflns_number_total             2178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03271g2.cif
_cod_data_source_block           cu_XR2024023_67_01_GYT_2024082_a
_cod_depositor_comments
'Adding full bibliography for 1575099--1575105.cif.'
_cod_original_cell_volume        11951(4)
_cod_database_code               1575099
_shelx_shelxl_version_number     2019/2
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              30962