5a,6,9,9a-Tetrahydro-4-hydroxy-6,9-methano-5<i>H</i>-fluoreno[2,3-<i>b</i>]furan-5-one and 5a,6,9,9a-tetrahydro-6,9-methano-4-methoxy-5<i>H</i>-fluoreno[2,3-<i>b</i>]furan-5-ol
Chinnakali, Kandasamy; Fun, Hoong-Kun; Mal, Dipakranjan; Bandopadhyay, Mousumi; Datta, Kalyani; Nigam, Gur Dayal; Acta Crystallographica Section C 55 (1999) 774–776; doi:10.1107/S0108270199001596

data_2008487
_publ_section_title
;5a,6,9,9a-Tetrahydro-4-hydroxy-6,9-methano-5<i>H</i>-fluoreno[2,3-<i>b</i>]furan-5-one
 and
 5a,6,9,9a-tetrahydro-6,9-methano-4-methoxy-5<i>H</i>-fluoreno[2,3-<i>b</i>]furan-5-ol
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              774
_journal_page_last               776
_journal_paper_doi               10.1107/S0108270199001596
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C17 H16 O3'
_chemical_formula_weight         268.30
_chemical_name_systematic
;
5,5a,6,9,9a-pentahydro-5-hydroxy-6,9-methano-4-methoxyfluoreno[ 2,3-d]furan
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.852(8)
_cell_angle_beta                 86.554(9)
_cell_angle_gamma                78.9160(10)
_cell_formula_units_Z            4
_cell_length_a                   9.83180(10)
_cell_length_b                   9.9472(2)
_cell_length_c                   14.2471(3)
_cell_measurement_reflns_used    4108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.49
_cell_volume                     1313.38(7)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PARST (Nardelli, 1995)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device       'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.109
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10634
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.25
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.142
_refine_ls_R_factor_gt           0.058
_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^)+(0.0678P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.159
_reflns_number_gt                2899
_reflns_number_total             6190
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1407.cif
_cod_data_source_block           II
_cod_original_cell_volume        1313.38(4)
_cod_database_code               2008487