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_1575103
_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
'C93 H93 N6 Na4 O30 Si2, 4(C2 H6 O), C H4 O [2(C4 H10 O),0.3(C H4 O)]'
_chemical_formula_sum            'C110.6 H139.3 N6 Na4 O38.05 Si2'
_chemical_formula_weight         2309.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2n51gc
_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                 95.130(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.459(4)
_cell_length_b                   18.6423(18)
_cell_length_c                   33.242(4)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.106
_cell_measurement_theta_min      2.667
_cell_volume                     24972(5)
_computing_cell_refinement       'SAINT V8.41'
_computing_data_collection       'Bruker BIS 8.5.0.27'
_computing_data_reduction        'SAINT V8.41'
_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 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.1351
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            107052
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        61.896
_diffrn_reflns_theta_max         61.896
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.062
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             9770
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.093
_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     1319
_refine_ls_number_reflns         18438
_refine_ls_number_restraints     755
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.2424
_refine_ls_R_factor_gt           0.1768
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+320.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3603
_refine_ls_wR_factor_ref         0.3869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8215
_reflns_number_total             18438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03271g2.cif
_cod_data_source_block           cu_XR2024023_89_01_GYT_2024110_a_sq_sq
_cod_depositor_comments
'Adding full bibliography for 1575099--1575105.cif.'
_cod_original_cell_volume        24972(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C110.60 H139.30 N6 Na4 O38.05 Si2'
_cod_database_code               1575103
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.816
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              85418
_shelx_fab_checksum              44955