A new norkaurane-γ-lactone from <i>Parinari sprucei</i>
Mattia, Carlo Andrea; Braca, Alessandra; De Tommasi, Nunziatina; Puliti, Raffaella; Acta Crystallographica Section C 59 (2003) o644–o646; doi:10.1107/S0108270103019814

data_2013569
_publ_section_title
;
 A new norkaurane-\g-lactone from <i>Parinari sprucei</i>
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o644
_journal_page_last               o646
_journal_paper_doi               10.1107/S0108270103019814
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         '2(C20 H28 O6), H2 O'
_chemical_formula_sum            'C40 H58 O13'
_chemical_formula_weight         746.86
_chemical_name_systematic
;
10,13,16,17-tetrahydroxy-9-methyl-15-oxo-20-nor-kauran-18-oic
acid-\g-lactone
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.627(3)
_cell_length_b                   14.7157(19)
_cell_length_c                   21.081(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291.0(5)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      27.0
_cell_volume                     3606.9(12)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction
;
Structure Determination Package (Enraf--Nonius, 1985)
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et. al., 1993)'
_diffrn_ambient_temperature      291.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method
'\w-2\q scans as suggested by peak-shape analysis'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4152
_diffrn_reflns_theta_full        74.84
_diffrn_reflns_theta_max         74.84
_diffrn_reflns_theta_min         3.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.231
_refine_ls_abs_structure_details
; The absolute configuration was chosen according to that of the known
bromine derivative of norkauren-\g-lactone (Garo et al., 1997) and is also
supported by the refined Flack parameter (Flack, 1983).
;
_refine_ls_abs_structure_Flack   0.04(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         4152
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                3553
_reflns_number_total             4152
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1027.cif
_cod_data_source_block           I
_cod_original_cell_volume        3607.0(11)
_cod_database_code               2013569
_cod_database_fobs_code          2013569