Hydrogen-bridged bis(silylene) complexes of ruthenium and iron: synthesis, structures and multi-centre bonding interactions at the M‒Si‒H‒Si four-membered ring
Hashimoto, Hisako; Komura, Katsuto; Ishizaki, Takatoshi; Odagiri, Yuto; Tobita, Hiromi; Dalton Trans.  (2017) –; doi:10.1039/C7DT00505A

data_7042522
_publ_section_title
;
 Hydrogen-bridged bis(silylene) complexes of ruthenium and iron:
 synthesis, structures and multi-centre bonding interactions at the
 M--Si--H--Si four-membered ring
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00505A
_journal_year                    2017
_chemical_formula_sum            'C21 H40 Fe O Si2'
_chemical_formula_weight         420.56
_chemical_name_systematic        'hydroge-bridged bis(silylene)iron complex'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-31 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                98.2428(15)
_cell_angle_beta                 92.326(3)
_cell_angle_gamma                114.276(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3327(4)
_cell_length_b                   9.4416(7)
_cell_length_c                   16.9080(12)
_cell_measurement_reflns_used    14544
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     1192.74(14)
_computing_cell_refinement       PROECSS-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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15181
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_correction_T_min  0.8253
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.7419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                4944
_reflns_number_total             5394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00505a2.cif
_cod_data_source_block           kk025
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7042522