Absolute configuration of diacetylated acrenol as its chloroform solvate
Robert A. Burrow; Ademir F. Morel; Ilmar B. Graebner; Alan J. Lough; David H. Farrar; Acta Crystallographica Section E 59 (2003) o350–o352; doi:10.1107/S1600536803003349

data_2201984
_publ_section_title
;
 Absolute configuration of diacetylated acrenol as its chloroform
 solvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o350
_journal_page_last               o352
_journal_paper_doi               10.1107/S1600536803003349
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C24 H32 O8, C H Cl3'
_chemical_formula_moiety         'C24 H32 O8, C H Cl3'
_chemical_formula_sum            'C25 H33 Cl3 O8'
_chemical_formula_weight         567.86
_chemical_name_common            'diacetylated acrenol'
_chemical_name_systematic
;
3S,5R,6S,9S,10S,13R,15R,19R-3\b,20-epoxy-3\a-hydoroxy-15,16-diacetyl-7-
pimaren-19,6\b-olide
1-(1-hydroxy-2,9-dimethyl-3-oxo-4,15-
dioxapentacyclo[11.2.2^15,13^.0^2,18^.0^7,12^]octadec-6-en-9-yl)-
2-methylcarbonyloxyethyl acetate
;
_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
_audit_creation_method           'Manual editing of cif generated by SHELXL-97'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0961(8)
_cell_length_b                   11.2954(18)
_cell_length_c                   28.684(4)
_cell_measurement_reflns_used    8481
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      4.2
_cell_volume                     2623.1(6)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\y scans and \w scans with \k offsets'
_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  0.132
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8481
_diffrn_reflns_theta_full        20.06
_diffrn_reflns_theta_max         20.06
_diffrn_reflns_theta_min         4.19
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.9249
_exptl_absorpt_correction_T_min  0.9073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
algorithm (Fox & Holmes, 1966) which effectively corrects for
absorption effects. High redundancy data were used in the scaling
program hence 'multi-scan' code word was used. No transmission
coefficients are available from the program (only scale factors
for each frame). The transmission factors in the experimental table
are calculated from the 'size' command in the SHELXL-97 input file.
Fox, G. C. & Holmes, K. C. (1966). Acta Cryst, 20, 886-891.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.202
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.17(17)
_refine_ls_extinction_coef       0.0068(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc2^\l3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0743P)^2^+2.6838P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                1863
_reflns_number_total             2410
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6019.cif
_cod_data_source_block           I
_cod_database_code               2201984
_cod_database_fobs_code          2201984