4a-Hydroxy-3,3,6,6-tetramethyl-9-[6-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1<i>H</i>-xanthen-9-yl)pyridin-2-yl]-2,3,4,4a,5,6,7,8,9,9a-decahydro-1<i>H</i>-xanthene-1,8-dione ethanol hemisolvate hemihydrate
Mohamed, Shaaban K.; Abdelhamid, Antar A.; Khalilov, Ali N.; Gurbanov, Atash V.; Ng, Seik Weng; Acta Crystallographica Section E 67 (2011) o850–o851; doi:10.1107/S1600536811008658

data_2229706
_publ_section_title
;
 4a-Hydroxy-3,3,6,6-tetramethyl-9-[6-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1<i>H</i>-xanthen-9-yl)pyridin-2-yl]-2,3,4,4a,5,6,7,8,9,9a-decahydro-1<i>H</i>-xanthene-1,8-dione
 ethanol hemisolvate hemihydrate
;
_journal_coeditor_code           IM2271
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o850
_journal_page_last               o851
_journal_paper_doi               10.1107/S1600536811008658
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C39 H47 N O7, 0.5C2 H6 O, 0.5H2 O'
_chemical_formula_moiety         'C39 H47 N O7, 0.5(C2 H6 O), 0.5(H2 O)'
_chemical_formula_sum            'C40 H51 N O8'
_chemical_formula_weight         673.82
_chemical_name_systematic
;
4a-Hydroxy-3,3,6,6-tetramethyl-9-[6-(3,3,6,6-tetramethyl-1,8-dioxo-
2,3,4,5,6,7,8,9-octahydro-1<i>H</i>-xanthen-9-yl)pyridin-2-yl]-
2,3,4,4a,5,6,7,8,9,9a-decahydro-1<i>H</i>-xanthene-1,8-dione
ethanol hemisolvate hemihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.113(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9739(5)
_cell_length_b                   16.3416(4)
_cell_length_c                   15.3412(4)
_cell_measurement_reflns_used    7177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.5
_cell_volume                     3683.56(18)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32212
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8332
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1170P)^2^+4.4589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2466
_reflns_number_gt                5349
_reflns_number_total             8332
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2271.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2229706
_cod_database_fobs_code          2229706