Equilibrium between Tetra-, Penta-, and Hexacoordinate Imine and Enamine Chelates of Silicon: Crystal Structure and Variable-Temperature NMR
Wagler, Jörg; Böhme, Uwe; Brendler, Erica; Roewer, Gerhard; Organometallics 24 (2005) 1348–; doi:10.1021/om049115s

data_4075681
_publ_contact_author
;Wagler, J\"org 
 Institut f\"ur Anorganische Chemie  
 Technische Universit\"at Bergakademie Freiberg
 Leipziger Str. 29 
 09596 Freiberg 
 Bundesrepublik Deutschland
;
_publ_section_title
;
 Equilibrium between Tetra-, Penta-, and Hexacoordinate Imine and Enamine
 Chelates of Silicon:&#x00A0; Crystal Structure and Variable-Temperature
 NMR
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1348
_journal_paper_doi               10.1021/om049115s
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C24 H24 N2 O2 Si'
_chemical_formula_sum            'C24 H24 N2 O2 Si'
_chemical_formula_weight         400.54
_chemical_melting_point          374
_chemical_name_common            (Salme*)(Salme*-H)SiPh
_chemical_name_systematic
; 
 (N,O)-N-Methyl-o-oxyacetophenoneiminato-(N',O')-N'-methyl-N'-1-(2-oxyphenyl)-
 vinylaminatophenylsilicon
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.385(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8530(10)
_cell_length_b                   17.0160(10)
_cell_length_c                   14.010(2)
_cell_measurement_reflns_used    218
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      20.889
_cell_measurement_theta_min      3.604
_cell_volume                     2075.9(4)
_computing_cell_refinement       'Dirax/lsq (Duisenb. & Schr., 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenb. & Schr., 1990-2000)'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23039
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.9439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.6427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                2107
_reflns_number_total             2877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049115ssi20041116_105720.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '374 K' was changed to '374' - the
value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075681