(1<i>S</i>,2<i>R</i>,3<i>R</i>,6<i>R</i>,7<i>S</i>,8<i>R</i>,10<i>S</i>,11<i>S</i>)-13-{[4-(4-Chlorophenyl)piperazin-1-yl]methyl}-10-hydroxy-4,9-dimethyl-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]pentadecan-14-one
Moumou, Mohamed; Benharref, Ahmed; El Ammari, Lahcen; Adil, Mina; Berraho, Moha; Acta Crystallographica Section E 68 (2012) o1147–o1148; doi:10.1107/S1600536812011816

data_2234115
_publ_section_title
;
 (1<i>S</i>,2<i>R</i>,3<i>R</i>,6<i>R</i>,7<i>S</i>,8<i>R</i>,10<i>S</i>,11<i>S</i>)-13-{[4-(4-Chlorophenyl)piperazin-1-yl]methyl}-10-hydroxy-4,9-dimethyl-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]pentadecan-14-one
;
_journal_coeditor_code           BT5834
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1147
_journal_page_last               o1148
_journal_paper_doi               10.1107/S1600536812011816
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C25 H33 Cl N2 O5'
_chemical_formula_moiety         'C25 H33 Cl N2 O5'
_chemical_formula_sum            'C25 H33 Cl N2 O5'
_chemical_formula_weight         476.98
_chemical_name_systematic
;
(1<i>S</i>,2<i>R</i>,3<i>R</i>,6<i>R</i>,7<i>S</i>,8<i>R</i>,
10<i>S</i>,11<i>S</i>)-13-{[4-(4-Chlorophenyl)piperazin-1-yl]methyl}-
10-hydroxy-4,9-dimethyl-3,8,15-
trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]pentadecan-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                   8.0138(3)
_cell_length_b                   10.7218(5)
_cell_length_c                   28.0174(13)
_cell_measurement_reflns_used    13518
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.4
_cell_volume                     2407.32(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
'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      296(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire1 long nozzle'
_diffrn_measurement_method       '\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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13518
_diffrn_reflns_theta_full        25.22
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       patelet
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.212
_refine_ls_abs_structure_details 'Flack (1983), 1836 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.3159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                3315
_reflns_number_total             4328
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5834.cif
_cod_data_source_block           I
_cod_database_code               2234115
_cod_database_fobs_code          2234115