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_4304015
_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         'C36 H84 Li4 N4 O6 Si4'
_chemical_formula_sum            'C36 H84 Li4 N4 O6 Si4'
_chemical_formula_weight         809.19
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                65.1620(17)
_cell_angle_beta                 76.3660(17)
_cell_angle_gamma                77.9070(18)
_cell_formula_units_Z            1
_cell_length_a                   10.5240(4)
_cell_length_b                   11.1990(3)
_cell_length_c                   11.9060(3)
_cell_measurement_reflns_used    5328
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1227.79(7)
_computing_cell_refinement       'HKL DENZO and SCALEPACK, Bruker AXS/Nonius'
_computing_data_collection       'COLLECT, Bruker AXS/Nonius'
_computing_data_reduction        'HKL DENZO and SCALEPACK, Bruker AXS/Nonius'
_computing_molecular_graphics
; 
Ortep (SHELXTL-NT v6.14, Bruker AXS)
;
_computing_publication_material  'WinGX v1.70.01 (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
' SIR-97 (A. Altomare, G. Cascarano, C. Giacovazzo et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9648
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.9530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0506P)^2^+0.8236P] 
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                4490
_reflns_number_total             5637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701267a-file001_4.cif
_cod_data_source_block           PrNNOLi_THF
_cod_original_cell_volume        1227.79(6)
_cod_database_code               4304015