Si- and C-Functional Organosilicon Building Blocks for Synthesis Based on 4-Silacyclohexan-1-ones Containing the Silicon Protecting Groups MOP (4-Methoxyphenyl), DMOP (2,6-Dimethoxyphenyl), or TMOP (2,4,6-Trimethoxyphenyl).
Geyer, Marcel; Karlsson, Olle; Baus, Johannes A.; Wellner, Eric; Tacke, Reinhold; The Journal of organic chemistry 80 (2015) 5804–5811; doi:10.1021/acs.joc.5b00774

data_4031004
_publ_section_title
;
 Si- and C-Functional Organosilicon Building Blocks for Synthesis Based on
 4-Silacyclohexan-1-ones Containing the Silicon Protecting Groups MOP
 (4-Methoxyphenyl), DMOP (2,6-Dimethoxyphenyl), or TMOP
 (2,4,6-Trimethoxyphenyl).
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5804
_journal_page_last               5811
_journal_paper_doi               10.1021/acs.joc.5b00774
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C15 H23 N O2 Si'
_chemical_formula_sum            'C15 H23 N O2 Si'
_chemical_formula_weight         277.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.026(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.440(7)
_cell_length_b                   9.281(3)
_cell_length_c                   18.624(8)
_cell_measurement_reflns_used    4400
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.32
_cell_volume                     3031(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP & POV-Ray'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16592
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.300
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+5.0089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2435
_reflns_number_total             2991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b00774_si_001.cif
_cod_data_source_block           GEY03B
_cod_depositor_comments
'Adding full bibliography for 4031004--4031005.cif.'
_cod_database_code               4031004
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.964
_shelxl_version_number           2013-4
_shelx_res_checksum              14304
_shelx_hkl_checksum              58231