Tuberostemoamide hemihydrate
Zhang, Rong-Rong; Ma, Zhi-Guo; Li, Guo-Qiang; But, Paul Pui-Hay; Jiang, Ren-Wang; Acta Crystallographica Section E 67 (2011) o3056–; doi:10.1107/S1600536811043340

data_2232542
_publ_section_title
;
 Tuberostemoamide hemihydrate
;
_journal_coeditor_code           ZS2152
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3056
_journal_paper_doi               10.1107/S1600536811043340
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C17 H23 N O4, 0.5H2 O'
_chemical_formula_moiety         'C17 H23 N O4, 0.5(H2 O)'
_chemical_formula_sum            'C17 H24 N O4.5'
_chemical_formula_weight         314.37
_chemical_name_common            'tuberostemoamide hemihydrate'
_chemical_name_systematic
;
(1'<i>S</i>,2<i>R</i>,2'<i>R</i>,3'<i>S</i>,6'<i>R</i>)-3'-ethyl-4-methyl-
5<i>H</i>-5'-oxa-10'-azaspiro[furan-2,4'-tricyclo[8.3.0.0^2,6^]tridecane]-
5,11'-dione hemihydrate
;
_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            8
_cell_length_a                   8.6412(2)
_cell_length_b                   10.7998(2)
_cell_length_c                   36.1685(7)
_cell_measurement_reflns_used    4774
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      62.53
_cell_measurement_theta_min      3.66
_cell_volume                     3375.36(12)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XP (Bruker, 1998)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S Ultra CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8573
_diffrn_reflns_theta_full        62.62
_diffrn_reflns_theta_max         62.62
_diffrn_reflns_theta_min         4.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.240
_refine_ls_abs_structure_details 'Flack (1983), 1743 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0913P)^2^+0.4948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                4514
_reflns_number_total             4837
_reflns_threshold_expression     I>2\(I)
_cod_data_source_file            zs2152.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C17 H24 N1 O4.5'
_cod_database_code               2232542
_cod_database_fobs_code          2232542