A Stable Schrock-Type Hafnium-Silylene Complex
Norio Nakata; Toshiyuki Fujita; Akira Sekiguchi; Journal of the American Chemical Society 128 (2006) 16024–16025; doi:10.1021/ja067251d

data_4111243
_publ_section_title
;
 A Stable Schrock-Type Hafnium-Silylene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16024
_journal_page_last               16025
_journal_paper_doi               10.1021/ja067251d
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C35 H69 Hf P Si3'
_chemical_formula_sum            'C35 H69 Hf P Si3'
_chemical_formula_weight         783.63
_chemical_name_common            'Hf-Si complex'
_chemical_name_systematic
; 
 Hf-silylene complex
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.138(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1080(13)
_cell_length_b                   11.7660(9)
_cell_length_c                   19.6560(14)
_cell_measurement_reflns_used    8638
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.09
_cell_volume                     3896.9(5)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8638
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  0.5379
_exptl_absorpt_correction_T_min  0.4373
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.986
_refine_diff_density_min         -2.440
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.8762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                7670
_reflns_number_total             8638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067251dsi20061105_114308.cif
_cod_data_source_block           Hf-silylene
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4111243