Crystal structures of (±)-(1<i>SR</i>,5<i>SR</i>,6<i>SR</i>,7<i>SR</i>,10<i>SR</i>,11<i>SR</i>,13<i>RS</i>,14<i>SR</i>)-13-hydroxy-7-methoxymethoxy-11,15,18,18-tetramethyl-3-oxo-2,4-dioxatetracyclo[12.3.1.0^1,5^.0^6,11^]octadec-15-en-10-yl benzoate, its 13-epimer and 13-one derivative
Oishi, Takeshi; Fukaya, Keisuke; Yamaguchi, Yu; Sugai, Tomoya; Watanabe, Ami; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 71 (2015) 466–472; doi:10.1107/S2056989015006854

data_2240566
_publ_section_title
;
 Crystal structures of
 (+-)-(1<i>SR</i>,5<i>SR</i>,6<i>SR</i>,7<i>SR</i>,10<i>SR</i>,11<i>SR</i>,13<i>RS</i>,14<i>SR</i>)-13-hydroxy-7-methoxymethoxy-11,15,18,18-tetramethyl-3-oxo-2,4-dioxatetracyclo[12.3.1.0^1,5^.0^6,11^]octadec-15-en-10-yl
 benzoate, its 13-epimer and 13-one derivative
;
_journal_coeditor_code           IS5395
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              466
_journal_page_last               472
_journal_paper_doi               10.1107/S2056989015006854
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C29 H36 O8'
_chemical_formula_moiety         'C29 H36 O8'
_chemical_formula_sum            'C29 H36 O8'
_chemical_formula_weight         512.59
_chemical_melting_point          512.2
_chemical_name_systematic
'(+-)-(1<i>SR</i>,5<i>SR</i>,6<i>SR</i>,7<i>SR</i>,10<i>SR</i>,11<i>SR</i>,14<i>SR</i>)-7-Methoxymethoxy-11,15,18,18-tetramethyl-3,13-dioxo-2,4-dioxatetracyclo[12.3.1.0^1,5^.0^6,11^]octadec-15-en-10-yl benzoate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.387(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2416(8)
_cell_length_b                   13.1779(8)
_cell_length_c                   15.2428(8)
_cell_measurement_reflns_used    6186
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.83
_cell_volume                     2509.0(3)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
<i>publCif</i> (Westrip, 2010) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2013</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90.0
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22512
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+2.2049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                3050
_reflns_number_total             4395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5395sup1.cif
_cod_data_source_block           C
_cod_database_code               2240566
_cod_database_fobs_code          2240566
_shelx_res_checksum              45243