Crystal structure of (±)-(4<i>RS</i>,5<i>RS</i>,7<i>SR</i>)-4-[(1<i>RS</i>,2<i>RS</i>,3<i>RS</i>,6<i>RS</i>)-3-benzoyloxy-2-(2-hydroxyethyl)-6-methoxymethoxy-2-methylcyclohexyl]-8,10,10-trimethyl-2-oxo-1,3-dioxaspiro[4.5]dec-8-en-7-yl benzoate benzene monosolvate
Oishi, Takeshi; Yamaguchi, Yuu; Fukaya, Keisuke; Sugai, Tomoya; Watanabe, Ami; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 71 (2015) 8–11; doi:10.1107/S2056989014026048

data_2240316
_publ_section_title
;
 Crystal structure of
 (+-)-(4<i>RS</i>,5<i>RS</i>,7<i>SR</i>)-4-[(1<i>RS</i>,2<i>RS</i>,3<i>RS</i>,6<i>RS</i>)-3-benzoyloxy-2-(2-hydroxyethyl)-6-methoxymethoxy-2-methylcyclohexyl]-8,10,10-trimethyl-2-oxo-1,3-dioxaspiro[4.5]dec-8-en-7-yl
 benzoate benzene monosolvate
;
_journal_coeditor_code           IS5382
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              8
_journal_page_last               11
_journal_paper_doi               10.1107/S2056989014026048
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C36 H44 O10, C6 H6'
_chemical_formula_moiety         'C36 H44 O10, C6 H6'
_chemical_formula_sum            'C42 H50 O10'
_chemical_formula_weight         714.82
_chemical_melting_point          459.2
_chemical_name_systematic
;(+-)-(4<i>RS</i>,5<i>RS</i>,7<i>SR</i>)-4-[(1<i>RS</i>,2<i>RS</i>,3<i>RS</i>,6<i>RS</i>)-3-Benzoyloxy-2-(2-hydroxyethyl)-6-methoxymethoxy-2-methylcyclohexyl]-8,10,10-trimethyl-2-oxo-1,3-dioxaspiro[4.5]dec-8-en-7-yl
benzoate benzene monosolvate
;
_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                83.6966(19)
_cell_angle_beta                 77.488(2)
_cell_angle_gamma                77.9768(18)
_cell_formula_units_Z            2
_cell_length_a                   9.6397(6)
_cell_length_b                   13.6008(8)
_cell_length_c                   15.0461(10)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.20
_cell_volume                     1879.2(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2013)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2013)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2013)
;
_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, 2008)
;
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0434
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25389
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2013)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+1.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                5180
_reflns_number_total             6526
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5382sup1.cif
_cod_data_source_block           I
_cod_database_code               2240316
_cod_database_fobs_code          2240316
_shelx_res_checksum              23298