A hydrogen-bridged bis(silylene) complex as a platform for small molecule activation <i>via</i> adjacent metal-ligand cooperation.
Hashimoto, Hisako; Matsuo, Satomi; Odagiri, Yuto; Tobita, Hiromi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 915–919; doi:10.1039/d4dt03226h

data_7717665
_publ_section_title
;
 A hydrogen-bridged bis(silylene) complex as a platform for small molecule
 activation <i>via</i> adjacent metal-ligand cooperation.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              915
_journal_page_last               919
_journal_paper_doi               10.1039/d4dt03226h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C29 H48 O3 Si2 W'
_chemical_formula_sum            'C29 H48 O3 Si2 W'
_chemical_formula_weight         684.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-11-18 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1114(6)
_cell_length_b                   10.5152(5)
_cell_length_c                   16.3940(5)
_cell_measurement_reflns_used    36306
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      1.72
_cell_volume                     2949.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics    'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'
_computing_publication_material  'Yadokari-XG2009(Wakita, Nemoto et al.,2009)'
_computing_structure_refinement
;
'SHELXL-97 (Sheldrick, 1997)', 'SHELXL-2018/3 (Sheldrick, 2018)'
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24264
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.404
_diffrn_reflns_theta_min         2.301
_exptl_absorpt_coefficient_mu    4.025
_exptl_absorpt_correction_T_max  0.5652
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 2486 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6660
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0139P)^2^+9.2217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                6054
_reflns_number_total             6660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03226h2.cif
_cod_data_source_block           matsuo02
_cod_depositor_comments
'Adding full bibliography for 7717662--7717666.cif.'
_cod_database_code               7717665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.500
_shelx_estimated_absorpt_t_max   0.565
_shelx_res_checksum              53122
_shelx_hkl_checksum              66301