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_7134483
_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            'C16 H20 O4 Si2'
_chemical_formula_weight         332.50
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
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_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
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.7010
_cell_measurement_theta_min      1.5040
_cell_volume                     1676.60(10)
_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    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  '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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'PILATUS3 X CdTe 1M'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.414
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23065
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        14.383
_diffrn_reflns_theta_max         14.996
_diffrn_reflns_theta_min         1.479
_diffrn_source                   'SPring-8 BL02B1 beamline'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.3905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2718
_reflns_number_total             3406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01499a2.cif
_cod_data_source_block           43_Si01_autored_a
_cod_depositor_comments
'Adding full bibliography for 7134482--7134483.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7134483
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.999
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              72234
_shelx_hkl_checksum              50234