Bis(dimethylsilyl)amide Complexes of the Alkaline-Earth Metals Stabilized by β-Si−H Agostic Interactions: Synthesis, Characterization, and Catalytic Activity
Sarazin, Yann; Roşca, Dragoş; Poirier, Valentin; Roisnel, Thierry; Silvestru, Anca; Maron, Laurent; Carpentier, Jean-François; Organometallics 29 (2010) 6569–; doi:10.1021/om100908q

data_4067228
_publ_section_title
;
 Bis(dimethylsilyl)amide Complexes of the Alkaline-Earth Metals Stabilized
 by \b-Si&#x2212;H Agostic Interactions: Synthesis, Characterization, and
 Catalytic Activity
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6569
_journal_paper_doi               10.1021/om100908q
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H112 K4 N4 O10 Si4, C6  H6'
_chemical_formula_sum            'C64 H118 K4 N4 O10 Si4'
_chemical_formula_weight         1372.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2010-05-12T18:22:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.9280(10)
_cell_angle_beta                 102.538(2)
_cell_angle_gamma                107.5100(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4506(3)
_cell_length_b                   14.7067(4)
_cell_length_c                   16.7604(6)
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.32
_cell_measurement_wavelength     0.71073
_cell_volume                     1986.74(12)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SAINT (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999))'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33195
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+1.0583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.116
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                7751
_reflns_number_total             8928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100908q_si_001.cif
_cod_data_source_block           job_complex8
_cod_original_cell_volume        1986.74(11)
_cod_database_code               4067228