(1<i>R</i>,3<i>S</i>,4<i>R</i>,4a<i>S</i>,7<i>R</i>,7a<i>S</i>,10<i>R</i>,12a<i>R</i>)-3-Azido-4,7,10-trimethyl-1,10-epidioxyperhydropyrano[4,3-<i>j</i>][1,2]benzodioxepine
Xie, Lijun; Zhai, Xin; Zuo, Jian; Zhao, Yanfang; Gong, Ping; Acta Crystallographica Section E 66 (2010) o1839–; doi:10.1107/S1600536810024566

data_2226533
_publ_section_title
;
 (1<i>R</i>,3<i>S</i>,4<i>R</i>,4a<i>S</i>,7<i>R</i>,7a<i>S</i>,10<i>R</i>,12a<i>R</i>)-3-Azido-4,7,10-trimethyl-1,10-epidioxyperhydropyrano[4,3-<i>j</i>][1,2]benzodioxepine
;
_journal_coeditor_code           IM2212
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1839
_journal_paper_doi               10.1107/S1600536810024566
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C15 H23 N3 O4'
_chemical_formula_moiety         'C15 H23 N3 O4'
_chemical_formula_sum            'C15 H23 N3 O4'
_chemical_formula_weight         309.36
_chemical_name_systematic
;
(1<i>R</i>,3<i>S</i>,4<i>R</i>,4a<i>S</i>,7<i>R</i>,7a<i>S</i>,10<i>R</i>,
12a<i>R</i>)-3-Azido-4,7,10-trimethyl-1,10-epidioxyperhydropyrano[4,3-
<i>j</i>][1,2]benzodioxepine
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9938(9)
_cell_length_b                   11.2070(10)
_cell_length_c                   17.984(2)
_cell_measurement_reflns_used    2309
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.347
_cell_measurement_theta_min      2.265
_cell_volume                     1611.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7585
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9654
_exptl_absorpt_correction_T_min  0.9548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.123
_refine_diff_density_min         -0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         1657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0312P)^2^+0.4488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                1130
_reflns_number_total             1657
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2212.cif
_cod_data_source_block           I
_cod_database_code               2226533
_cod_database_fobs_code          2226533