A Stable Silylene with a σ<sup>2</sup>, π- Butadiene Ligand.
Dong, Zhaowen; Reinhold, Crispin R. W.; Schmidtmann, Marc; Müller, Thomas; Journal of the American Chemical Society 139 (2017) 7117–7123; doi:10.1021/jacs.7b03566

data_4131299
_publ_section_title
;
 A Stable Silylene with a \s<sup>2</sup>, \p- Butadiene Ligand.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7117
_journal_page_last               7123
_journal_paper_doi               10.1021/jacs.7b03566
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_structural     'SiC4(C6H5)2(Si(CH3)3)2Hf(C5H5)2 *C4H8O'
_chemical_formula_sum            'C36 H46 Hf O Si3'
_chemical_formula_weight         757.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.2487(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.330(3)
_cell_length_b                   7.9638(6)
_cell_length_c                   10.8208(8)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.73
_cell_measurement_theta_min      2.61
_cell_volume                     3383.8(4)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            84101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         1.885
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.077
_refine_diff_density_min         -3.114
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 6185 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         14867
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0200P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14078
_reflns_number_total             14867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03566_si_002.cif
_cod_data_source_block           dzw104
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4131299
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.566
_shelx_estimated_absorpt_t_max   0.856
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              79516
_shelx_hkl_checksum              12295