Crystal structure 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>SR</i>)-13-benzyloxy-7-methoxymethoxy-11,15,18,18-tetramethyl-3-oxo-2,4-dioxatetracyclo[12.3.1.0^1,5^.0^6,11^]octadeca-14,16-dien-10-yl benzoate
Oishi, Takeshi; Fukaya, Keisuke; Yamaguchi, Yu; Sugai, Tomoya; Watanabe, Ami; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 71 (2015) 490–493; doi:10.1107/S2056989015007136

data_2240612
_publ_section_title
;
 Crystal structure 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>SR</i>)-13-benzyloxy-7-methoxymethoxy-11,15,18,18-tetramethyl-3-oxo-2,4-dioxatetracyclo[12.3.1.0^1,5^.0^6,11^]octadeca-14,16-dien-10-yl
 benzoate
;
_journal_coeditor_code           IS5396
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              490
_journal_page_last               493
_journal_paper_doi               10.1107/S2056989015007136
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C36 H42 O8'
_chemical_formula_moiety         'C36 H42 O8'
_chemical_formula_sum            'C36 H42 O8'
_chemical_formula_weight         602.69
_chemical_melting_point          465.2
_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>,13<i>SR</i>)-13-Benzyloxy-7-methoxymethoxy-11,15,18,18-tetramethyl-3-oxo-2,4-dioxatetracyclo[12.3.1.0^1,5^.0^6,11^]octadeca-14,16-dien-10-yl benzoate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                72.148(2)
_cell_angle_beta                 86.447(2)
_cell_angle_gamma                66.766(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9358(6)
_cell_length_b                   11.6121(6)
_cell_length_c                   13.6833(7)
_cell_measurement_reflns_used    9212
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.22
_cell_volume                     1516.36(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0519
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27885
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0504P)^2^+1.0416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                4078
_reflns_number_total             5346
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5396sup1.cf
_cod_data_source_block           I
_cod_database_code               2240612
_cod_database_fobs_code          2240612