10α-Hydroxy-4,9-dimethyl-13-[(4-phenylpiperazin-1-yl)methyl]-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]tetradecan-14-one
Moumou, Mohamed; Benharref, Ahmed; Oudahmane, Abdelghani; Elhakmaoui, Ahmed; Berraho, Moha; Acta Crystallographica Section E 67 (2011) o2981–o2982; doi:10.1107/S1600536811042012

data_2232388
_publ_section_title
;
 10\a-Hydroxy-4,9-dimethyl-13-[(4-phenylpiperazin-1-yl)methyl]-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]tetradecan-14-one
;
_journal_coeditor_code           LH5350
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2981
_journal_page_last               o2982
_journal_paper_doi               10.1107/S1600536811042012
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C25 H34 N2 O5'
_chemical_formula_moiety         'C25 H34 N2 O5'
_chemical_formula_sum            'C25 H34 N2 O5'
_chemical_formula_weight         442.54
_chemical_name_systematic
;
10\aHydroxy-4,9-dimethyl-13-[(4-phenylpiperazin-1-yl)methyl]-
3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]tetradecan-14-one
;
_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                   7.7666(5)
_cell_length_b                   9.6059(8)
_cell_length_c                   31.181(2)
_cell_measurement_reflns_used    10922
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.7
_cell_volume                     2326.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia,1997) and PLATON (Spek, 2009)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8 APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            10922
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0537P)^2^+0.4378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                2362
_reflns_number_total             2723
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5350.cif
_cod_data_source_block           I
_cod_original_cell_volume        2326.2(3)
_cod_database_code               2232388
_cod_database_fobs_code          2232388