Synthesis of 4-Silacyclohexan-1-ones and (4-Silacyclohexan-1-yl)amines Containing the Silicon Protecting Groups MOP (4-Methoxyphenyl), DMOP (2,4-Dimethoxyphenyl), or TMOP (2,4,6-Trimethoxyphenyl): Versatile Si- and C-Functional Building Blocks for Synthesis
Fischer, Markus; Burschka, Christian; Tacke, Reinhold; Organometallics 33 (2014) 1020–; doi:10.1021/om401208y

data_4082388
_publ_section_title
;
 Synthesis of 4-Silacyclohexan-1-ones and (4-Silacyclohexan-1-yl)amines
 Containing the Silicon Protecting Groups MOP (4-Methoxyphenyl), DMOP
 (2,4-Dimethoxyphenyl), or TMOP (2,4,6-Trimethoxyphenyl): Versatile Si-
 and C-Functional Building Blocks for Synthesis
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1020
_journal_paper_doi               10.1021/om401208y
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C19 H22 O3 Si'
_chemical_formula_sum            'C19 H22 O3 Si'
_chemical_formula_weight         326.46
_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                 97.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.134(3)
_cell_length_b                   7.9793(16)
_cell_length_c                   15.193(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      5.75
_cell_volume                     1818.7(6)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  Stoe-IPDS_image_plate
_diffrn_measurement_method       'omega scan'
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25201
_diffrn_reflns_theta_full        29.08
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0569P)^2^+0.2644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                3943
_reflns_number_total             4754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401208y_si_002.cif
_cod_data_source_block           fis09f_27
_cod_original_cell_volume        1818.6(6)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4082388