4-Hydroxy-4,6a,6b,9,9,12a,14b-heptamethylperhydropicen-3-one hemihydrate isolated from <i>Adiantum incisum</i>
Hussain, Altaf; Siddiqui, Hamid Latif; Zia-ur-Rehman, Muhammad; Elsegood, Mark R. J.; M. Khan, Khalid; Acta Crystallographica Section E 64 (2008) o264–o264; doi:10.1107/S1600536807064021

data_2216941
_publ_section_title
;
 4-Hydroxy-4,6a,6b,9,9,12a,14b-heptamethylperhydropicen-3-one
 hemihydrate isolated from <i>Adiantum incisum</i>
;
_journal_coeditor_code           BT2638
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o264
_journal_page_last               o264
_journal_paper_doi               10.1107/S1600536807064021
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C29 H48 O2, 0.5H2 O'
_chemical_formula_moiety         'C29 H48 O2, 0.5(H2 O)'
_chemical_formula_sum            'C29 H49 O2.5'
_chemical_formula_weight         437.68
_chemical_name_systematic
;
4-Hydroxy-4,6a,6b,9,9,12a,14b-heptamethylperhydropicen-3-one hemihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 114.725(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4432(4)
_cell_length_b                   57.477(8)
_cell_length_c                   7.2226(6)
_cell_measurement_reflns_used    10245
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2429.6(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Hooft,  1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick,  2000)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type  'Bruker--Nonius Kappa CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.1117
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            12411
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         4.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick,  2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         3758
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0174P)^2^+4.4271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                2285
_reflns_number_total             3758
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2638.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-21
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C29 H49 O2.50'
_cod_database_code               2216941
_cod_database_fobs_code          2216941