Crystal structure of methyl (3<i>RS</i>,4<i>SR</i>,4a<i>RS</i>,11a<i>RS</i>,11b<i>SR</i>)-5-oxo-3,4,4a,5,7,8,9,10,11,11a-decahydro-3,11b-epoxyazepino[2,1-<i>a</i>]isoindole-4-carboxylate
Toze, Flavien A. A.; Poplevin, Dmitry S.; Zubkov, Fedor I.; Nikitina, Eugeniya V.; Porras, Ciara; Khrustalev, Victor N.; Acta Crystallographica Section E 71 (2015) o729–o730; doi:10.1107/S2056989015016679

data_2241112
_publ_section_title
;
 Crystal structure of methyl
 (3<i>RS</i>,4<i>SR</i>,4a<i>RS</i>,11a<i>RS</i>,11b<i>SR</i>)-5-oxo-3,4,4a,5,7,8,9,10,11,11a-decahydro-3,11b-epoxyazepino[2,1-<i>a</i>]isoindole-4-carboxylate
;
_journal_coeditor_code           TK5384
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o729
_journal_page_last               o730
_journal_paper_doi               10.1107/S2056989015016679
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C15 H19 N O4'
_chemical_formula_moiety         'C15 H19 N O4'
_chemical_formula_sum            'C15 H19 N O4'
_chemical_formula_weight         277.31
_chemical_name_systematic
;Methyl
(3<i>RS</i>,4<i>SR</i>,4a<i>RS</i>,11a<i>RS</i>,11b<i>SR</i>)-5-oxo-3,4,4a,5,7,8,9,10,11,11a-decahydro-3,11b-epoxyazepino[2,1-<i>a</i>]isoindole-4-carboxylate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                103.857(2)
_cell_angle_beta                 94.745(2)
_cell_angle_gamma                106.620(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5460(8)
_cell_length_b                   9.6984(10)
_cell_length_c                   10.2894(10)
_cell_measurement_reflns_used    4971
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.28
_cell_volume                     691.24(12)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9699
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.066
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0765P)^2^+0.153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                2613
_reflns_number_total             3268
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5384sup1.cif
_cod_data_source_block           I
_cod_database_code               2241112
_cod_database_fobs_code          2241112
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.976
_shelx_hkl_checksum              67320
_shelx_res_checksum              55211
_shelxl_version_number           2014/6