Crystal structure of (1S,2R,4R,9S,11S,12R)-9α-hydroxy-4,8-dimethyl-12-[(thiomorpholin-4-yl)methyl]-3,14-dioxatricyclo[9.3.0.02,4]tetradec-7-en-13-one
Benharref, Ahmed; Akssira, Mohamed; El Ammari, Lahcen; Saadi, Mohamed; Berraho, Moha; Acta Crystallographica Section E Crystallographic Communications 71 (2015) o140–; doi:10.1107/S205698901500170X

data_2019833
_publ_section_title
;
 Crystal structure of
 (1S,2R,4R,9S,11S,12R)-9\a-hydroxy-4,8-dimethyl-12-[(thiomorpholin-4-yl)methyl]-3,14-dioxatricyclo[9.3.0.02,4]tetradec-7-en-13-one
;
_journal_coeditor_code           HB7355
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              o140
_journal_paper_doi               10.1107/S205698901500170X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C19 H29 N O4 S'
_chemical_formula_moiety         'C19 H29 N O4 S'
_chemical_formula_sum            'C19 H29 N O4 S'
_chemical_formula_weight         367.49
_chemical_name_systematic
(1<i>S</i>,2<i>R</i>,4<i>R</i>,9<i>S</i>,11<i>S</i>,12<i>R</i>)-9\a-Hydroxy-4,8-dimethyl-12-[(thiomorpholin-4-yl)methyl]-3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 101.659(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.920(2)
_cell_length_b                   6.7919(13)
_cell_length_c                   12.144(3)
_cell_measurement_reflns_used    3940
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.68
_cell_volume                     962.9(3)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12288
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.180
_refine_ls_abs_structure_details
;
Flack & Bernardinelli (2000)
;
_refine_ls_abs_structure_Flack   0.04(7)
_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     229
_refine_ls_number_reflns         3940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0458P)^2^+0.1195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                3749
_reflns_number_total             3940
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7355sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2019833
_cod_database_fobs_code          2019833