Three Lactone Fused Perhydroisoxazolo[2,3-<i>a</i>]pyridines: a Conformational Study
Alvarez-Larena, A.; Piniella, J. F.; Cid, P.; de March, P.; Figueredo, M.; Font, J.; Milán, S.; Soria, A.; Acta Crystallographica Section C 51 (1995) 1314–1319; doi:10.1107/S0108270194013661

data_2003710
_publ_section_title
;
 Three Lactone Fused Perhydroisoxazolo[2,3-<i>a</i>]pyridines: a
 Conformational Study
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1314
_journal_page_last               1319
_journal_paper_doi               10.1107/S0108270194013661
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C11 H17 N O3'
_chemical_formula_weight         211.26
_chemical_name_systematic
(5aRS,11aRS,11bRS)-Decahydro-1H-oxepino[3',4':4,5]isoxazolo[2,3-a]pyridin-1-one
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.84(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0456(7)
_cell_length_b                   16.735(3)
_cell_length_c                   10.786(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.20
_cell_measurement_theta_min      10.00
_cell_volume                     1078.3(3)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994).'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70926
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1893
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.144
_refine_ls_extinction_coef       0.053(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_obs          0.0367
_refine_ls_shift/esd_max         -0.050
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^) + (0.0345P)^2^ + 0.3628P]
where P = (Fo^2^ + 2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.1005
_refine_ls_wR_factor_obs         0.0879
_reflns_number_observed          1493
_reflns_number_total             1893
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1129.cif
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2003710