9-Hydroxy-4,8-dimethyl-12-(pyrrolidin-1-ylmethyl)-3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one
Moumou, Mohamed; Benharref, Ahmed; Avignant, Daniel; Oudahmane, Abdelghani; Akssira, Mohamed; Berraho, Moha; Acta Crystallographica Section E 67 (2011) o2226–o2227; doi:10.1107/S1600536811030467

data_2231773
_publ_section_title
;
 9-Hydroxy-4,8-dimethyl-12-(pyrrolidin-1-ylmethyl)-3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one
;
_journal_coeditor_code           ZL2390
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2226
_journal_page_last               o2227
_journal_paper_doi               10.1107/S1600536811030467
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C19 H29 N O4'
_chemical_formula_moiety         'C19 H29 N O4'
_chemical_formula_sum            'C19 H29 N O4'
_chemical_formula_weight         335.43
_chemical_name_systematic
;
9-Hydroxy-4,8-dimethyl-12-(pyrrolidin-1-ylmethyl)-3,14-
dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-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                   8.1389(6)
_cell_length_b                   10.1788(7)
_cell_length_c                   21.7669(15)
_cell_measurement_reflns_used    7656
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      3.7
_cell_volume                     1803.3(2)
_computing_cell_refinement       'APEX2 and 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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7656
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.148
_refine_ls_extinction_coef       0.017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                1220
_reflns_number_total             2110
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2390.cif
_cod_data_source_block           I
_cod_database_code               2231773
_cod_database_fobs_code          2231773