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_4304013
_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         'C22 H36 N2 O Si2'
_chemical_formula_sum            'C22 H36 N2 O Si2'
_chemical_formula_weight         400.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.129(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4320(3)
_cell_length_b                   15.8940(7)
_cell_length_c                   8.3240(8)
_cell_measurement_reflns_used    5030
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2434.9(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8159
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.9689
_exptl_absorpt_correction_T_min  0.9614
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      1.093
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0436P)^2^+1.3415P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                3664
_reflns_number_total             4968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701267a-file001_2.cif
_cod_data_source_block           Me3PhenNON
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304013