Synthesis, Structures, and Kinetics of Mixed-Donor Amido-Amino-Siloxo Ligands from Symmetrical Diamidosilyl Ether Ligands via a Retro-Brook Rearrangement
Farzad Haftbaradaran; Angela M. Kuchison; Michael J. Katz; Gabriele Schatte; Daniel B. Leznoff; Inorganic Chemistry 47 (2008) 812–822; doi:10.1021/ic701267a

data_4304012
_publ_contact_author_address
; 
 Department of Chemistry
 8888 University Drive
 Simon Fraser University
 Burnaby, British Columbia
 Canada   V5A 1S6
;
_publ_contact_author_email       dleznoff@sfu.ca
_publ_contact_author_fax         604-291-3765
_publ_contact_author_name        'Daniel B. Leznoff'
_publ_contact_author_phone       604-291-4887
_publ_section_title
;
Synthesis, Structures, and Kinetics of Mixed-Donor Amido-Amino-Siloxo
Ligands from Symmetrical Diamidosilyl Ether Ligands via a Retro-Brook
Rearrangement
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              812
_journal_page_last               822
_journal_paper_doi               10.1021/ic701267a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C40 H76 Li2 N2 O4 Si2'
_chemical_formula_sum            'C40 H76 Li2 N2 O4 Si2'
_chemical_formula_weight         719.09
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.4130(2)
_cell_length_b                   12.3350(4)
_cell_length_c                   19.0520(5)
_cell_measurement_reflns_used    18440
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      1.00
_cell_volume                     4562.2(2)
_computing_molecular_graphics    ' Ortep (SHELXTL-NT v6.14, Bruker AXS)'
_computing_publication_material  'WinGX v1.64-05 (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    ' SIR-97 (A. Altomare, G. Cascarano et al.)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'KappaCCD (BruKer AXS-Nonius, FR540C)'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_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            24357
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9798
_exptl_absorpt_correction_T_min  0.9775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       0.0037(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc w=1/[\s^2^(Fo^2^)+(0.1461P)^2^+2.5871P] 
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2186
_reflns_number_gt                2921
_reflns_number_total             3391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701267a-file001_1.cif
_cod_data_source_block           iPr2PhNNOLi_Et2O
_cod_database_code               4304012