8-Methyltricyclo[9.3.0.0^3,7^]tetradec-3-ene-5,10-dione and 7,12-dihydroxy-9,12-dimethyltetracyclo[8.2.1.0^1,5^.0^7,11^]tridecan-13-one methanol solvate
Umehara, Misao; Hosomi, Hiroyuki; Ohba, Shigeru; Acta Crystallographica Section C 55 (1999) IUC9900068–; doi:10.1107/S0108270199099175

data_2008716
_publ_section_title
;
 8-Methyltricyclo[9.3.0.0^3,7^]tetradec-3-ene-5,10-dione and
 7,12-dihydroxy-9,12-dimethyltetracyclo[8.2.1.0^1,5^.0^7,11^]tridecan-13-one
 methanol solvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900068
_journal_paper_doi               10.1107/S0108270199099175
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C15 H22 O3, C1 H4 O1'
_chemical_formula_sum            'C16 H26 O4'
_chemical_formula_weight         282.38
_chemical_name_common
;
7,12-dihydroxy-9,12-dimethyltetracyclo[8.2.1.0^1,5^.0^7,11^]tridecan-
13-one monomethanol solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.096(2)
_cell_length_b                   8.4340(10)
_cell_length_c                   25.0950(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     3085.9(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1998)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            3678
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        10.7
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.316
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00269|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                2730
_reflns_number_total             3545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0136.cif
_cod_data_source_block           IUC9900068-2
_cod_original_cell_volume        3086.1(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C16 H26 O4 '
_cod_database_code               2008716