4-Hydroxymethyl-10-methoxy-17,22-dioxapentacyclo[21.2.2.2^13,16^.1^3,7^.0^11,30^]triaconta-1(25),3,5,7(30),8,10,13,15,23,26,28-undecaene-2,12-dione acetone monosolvate
Hijikata, Daichi; Sasagawa, Kosuke; Yoshiwaka, Sayaka; Okamoto, Akiko; Yonezawa, Noriyuki; Acta Crystallographica Section E 68 (2012) o2598–o2599; doi:10.1107/S1600536812033521

data_2235901
_publ_section_title
;
 4-Hydroxymethyl-10-methoxy-17,22-dioxapentacyclo[21.2.2.2^13,16^.1^3,7^.0^11,30^]triaconta-1(25),3,5,7(30),8,10,13,15,23,26,28-undecaene-2,12-dione
 acetone monosolvate
;
_journal_coeditor_code           LD2069
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2598
_journal_page_last               o2599
_journal_paper_doi               10.1107/S1600536812033521
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C30 H26 O6, C3 H6 O'
_chemical_formula_moiety         'C30 H26 O6, C3 H6 O'
_chemical_formula_sum            'C33 H32 O7'
_chemical_formula_weight         540.59
_chemical_melting_point_gt       537.5
_chemical_melting_point_lt       538.8
_chemical_name_systematic
;
4-Hydroxymethyl-10-methoxy-17,22-
dioxapentacyclo[21.2.2.2^13,16^.1^3,7^.0^11,30^]triaconta-
1(25),3,5,7(30),8,10,13,15,23,26,28-undecaene-2,12-dione acetone monosolvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   15.4948(3)
_cell_length_b                   16.1272(3)
_cell_length_c                   22.4430(4)
_cell_measurement_reflns_used    92773
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      3.38
_cell_volume                     5608.23(18)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2010)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, <i>et al.</i>, 2007)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0056
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            99441
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.94
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.7590
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.193
_refine_ls_extinction_coef       0.00160(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/6(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0495P)^2^+1.7635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                4829
_reflns_number_total             5132
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ld2069.cif
_cod_data_source_block           I
_cod_database_code               2235901
_cod_database_fobs_code          2235901