Exclusive macrocyclization through multiple Si–O bond formations from diol and dichlorosilane
Iwamoto, Takahiro; Amano, Sota; Maeda, Kousuke; Shibama, Natsuki; Sekiguchi, Wakana; Kazama, Yuki; Nakamura, Yasuyuki; Sugamata, Koh; Imoto, Hiroaki; Naka, Kensuke; Ishii, Youichi; Chemical Communications 61 (2025) 8180–8183; doi:10.1039/D5CC01499A

data_7134482
_publ_section_title
;
 Exclusive macrocyclization through multiple Si--O bond formations from
 diol and dichlorosilane
;
_journal_issue                   45
_journal_name_full               'Chemical Communications'
_journal_page_first              8180
_journal_page_last               8183
_journal_paper_doi               10.1039/D5CC01499A
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C56 H56 O8 Si4'
_chemical_formula_weight         969.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2025-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.8118(5)
_cell_length_b                   24.8118(5)
_cell_length_c                   5.1576(2)
_cell_measurement_reflns_used    7021
_cell_measurement_temperature    100(2)
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_cell_volume                     3175.15(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics
'Olex2 1.3-ac4 (Dolomanov et al., 2009)''Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material
'Olex2 1.3-ac4 (Dolomanov et al., 2009)''Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'PILATUS3 X CdTe 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.4139
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            60564
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        14.379
_diffrn_reflns_theta_max         14.986
_diffrn_reflns_theta_min         1.511
_diffrn_source                   'SPring-8 BL02B1 beamline'
_exptl_absorpt_coefficient_mu    0.042
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0448P)^2^+0.6589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2777
_reflns_number_total             3253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01499a2.cif
_cod_data_source_block           29_MK-3-108-B2_a_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__exptl_absorpt_correction_t_min' was replaced with
'_exptl_absorpt_correction_T_min'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 

 Adding full bibliography for 7134482--7134483.cif.
;
_cod_original_cell_volume        3175.15(18)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7134482
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   1.000
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              6330
_shelx_hkl_checksum              26956