Experimental and Theoretical Study of the Transannular Intramolecular Interaction and Cage Effect in the Atrane Framework of Boratrane and 1-Methylsilatrane
Alexander A. Korlyukov; Konstantin A. Lyssenko; Mikhail Yu. Antipin; Valerii N. Kirin; Eugenii A. Chernyshev; Sergei P. Knyazev; Inorganic Chemistry 41 (2002) 5043–5051; doi:10.1021/ic010842e

data_4318652
_publ_section_title
;
 Experimental and Theoretical Study of the Transannular Intramolecular
 Interaction and Cage Effect in the Atrane Framework of Boratrane and
 1-Methylsilatrane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5043
_journal_page_last               5051
_journal_paper_doi               10.1021/ic010842e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C7 H15 N O3 Si'
_chemical_formula_sum            'C7 H15 N O3 Si'
_chemical_formula_weight         189.29
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.7400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.56630(10)
_cell_length_b                   12.0408(2)
_cell_length_c                   9.62100(10)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     876.11(2)
_computing_cell_refinement       'SMART (Bruker, 1998b)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20349
_diffrn_reflns_theta_full        47.59
_diffrn_reflns_theta_max         47.59
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1998a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         7397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0648P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                6305
_reflns_number_total             7397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010842e_2.cif
_cod_data_source_block           msabs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318652