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_4075682
_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         'C33 H35 N3 O3 Si, 0.5(C8 H10)'
_chemical_formula_sum            'C37 H40 N3 O3 Si'
_chemical_formula_weight         602.81
_chemical_melting_point          381
_chemical_name_common            (Salme*)3SiPh*1/2p-Xylene
_chemical_name_systematic
; 
 Tris-(2-oxyacetophenone-N-methyliminato)phenylsilane p-Xylene solvate 
;
_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                 101.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.889(2)
_cell_length_b                   21.871(4)
_cell_length_c                   12.464(3)
_cell_measurement_reflns_used    114
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      19.769
_cell_measurement_theta_min      5.381
_cell_volume                     3170.8(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54176
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0330P)^2^+3.0872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                4199
_reflns_number_total             5567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049115ssi20041116_105720.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '381 K' was changed to '381' - 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_cell_volume        3170.8(11)
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075682