Synthesis, Molecular Structure, Conformational Analysis, and Chemical Properties of Silicon-Containing Derivatives of Quinolizidine
Nataliya F. Lazareva; Bagrat A. Shainyan; Uwe Schilde; Nina N. Chipanina; Larisa P. Oznobikhina; Alexander I. Albanov; Erich Kleinpeter; Journal of Organic Chemistry 77 (2012) 2382–2388; doi:10.1021/jo202658n

data_4027044
_publ_contact_author_address
;
 University of Potsdam
 Institute of Chemistry
 Karl-Liebknecht-Str. 24-25
 D-14476 Potsdam
 Germany
;
_publ_contact_author_email       us@chem.uni-potsdam.de
_publ_contact_author_fax         +49-331-977-5153
_publ_contact_author_name        'Schilde, Uwe'
_publ_contact_author_phone       +49-331-977-5188
_publ_section_title
;
 Synthesis, Molecular Structure, Conformational Analysis, and Chemical
 Properties of Silicon-Containing Derivatives of Quinolizidine
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2382
_journal_page_last               2388
_journal_paper_doi               10.1021/jo202658n
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C10 H23 N O3 Si2'
_chemical_formula_sum            'C10 H23 N O3 Si2'
_chemical_formula_weight         261.47
_chemical_melting_point          442(1)
_chemical_name_systematic
; 
 (3,3,7,7-tetramethylhexahydro-1H-[1,4,2]oxazasilino
 [4,5-d][1,4,2]oxazasilin-9a-yl)methanol
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.601(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0574(5)
_cell_length_b                   11.2877(12)
_cell_length_c                   21.5246(16)
_cell_measurement_reflns_used    6028
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.81
_cell_volume                     1417.5(2)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_molecular_graphics
;
  DIAMOND (Brandenburg, 2005)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
 180 frames, exposure time per frame = 8 min
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, 1.0 \%'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1145
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8379
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       needle
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                1623
_reflns_number_total             2365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo202658n_si_002.cif
_cod_data_source_block           irk-5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '441-443' was changed to '442.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4027044