10α-Hydroxy-4,9-dimethyl-13-(pipyridin-1-ylmethyl)-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) o3003–o3004; doi:10.1107/S1600536811042644

data_2232241
_publ_section_title
;
 10\a-Hydroxy-4,9-dimethyl-13-(pipyridin-1-ylmethyl)-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]tetradecan-14-one
;
_journal_coeditor_code           FJ2458
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3003
_journal_page_last               o3004
_journal_paper_doi               10.1107/S1600536811042644
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H31 N O5'
_chemical_formula_moiety         'C20 H31 N O5'
_chemical_formula_sum            'C20 H31 N O5'
_chemical_formula_weight         365.46
_chemical_name_systematic
;
10\a-Hydroxy-4,9-dimethyl-13-(pipyridin-1-ylmethyl)-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                   8.0899(5)
_cell_length_b                   10.7562(6)
_cell_length_c                   22.5093(13)
_cell_measurement_reflns_used    8987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.6
_cell_volume                     1958.7(2)
_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 publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick,2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick,2008)'
_diffrn_ambient_temperature      296(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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8978
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.159
_refine_ls_extinction_coef       0.035(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0377P)^2^+0.1661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                1707
_reflns_number_total             2291
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            fj2458.cif
_cod_data_source_block           I
_cod_database_code               2232241
_cod_database_fobs_code          2232241