Crystal structure of (3<i>S</i>*,4<i>S</i>*,4a<i>S</i>*,5<i>R</i>*,6<i>R</i>*,6a<i>S</i>*,7<i>R</i>*,11a<i>S</i>*,11b<i>R</i>*)-5,6-bis(benzoyloxy)-3,4a-dihydroxy-4,7,11b-trimethyl-1,2,3,4,4a,5,6,6a,7,11,11a,11b-dodecahydrophenanthro[3,2-<i>b</i>]furan-4-carboxylic acid methanol monosolvate
Siddiqui, Sadaf; Erharuyi, Osayemwenre; Falodun, Abiodun; Choudhary, M. Iqbal; Yousuf, Sammer; Acta Crystallographica Section E 71 (2015) o739–o740; doi:10.1107/S2056989015016461

data_2241076
_publ_section_title
;
 Crystal structure of
 (3<i>S</i>*,4<i>S</i>*,4a<i>S</i>*,5<i>R</i>*,6<i>R</i>*,6a<i>S</i>*,7<i>R</i>*,11a<i>S</i>*,11b<i>R</i>*)-5,6-bis(benzoyloxy)-3,4a-dihydroxy-4,7,11b-trimethyl-1,2,3,4,4a,5,6,6a,7,11,11a,11b-dodecahydrophenanthro[3,2-<i>b</i>]furan-4-carboxylic
 acid methanol monosolvate
;
_journal_coeditor_code           IS5414
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o739
_journal_page_last               o740
_journal_paper_doi               10.1107/S2056989015016461
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C34 H36 O9, C H4 O'
_chemical_formula_moiety         'C34 H36 O9, C H4 O'
_chemical_formula_sum            'C35 H40 O10'
_chemical_formula_weight         620.67
_chemical_name_systematic
;(3<i>S</i>*,4<i>S</i>*,4a<i>S</i>*,5<i>R</i>*,6<i>R</i>*,6a<i>S</i>*,7<i>R</i>*,11a<i>S</i>*,11b<i>R</i>*)-5,6-Bis(benzoyloxy)-3,4a-dihydroxy-4,7,11b-trimethyl-1,2,3,4,4a,5,6,6a,7,11,11a,11b-dodecahydrophenanthro[3,2-<i>b</i>]furan-4-carboxylic
acid methanol monosolvate
;
_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           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                   11.7943(6)
_cell_length_b                   13.5934(7)
_cell_length_c                   19.2988(11)
_cell_measurement_reflns_used    2827
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.28
_cell_volume                     3094.1(3)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL  (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD area-detector
;
_diffrn_measurement_method       '\w scan'
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18238
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         3916
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.1739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                2882
_reflns_number_total             3916
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is5414sup1.cif
_cod_data_source_block           I
_cod_database_code               2241076
_cod_database_fobs_code          2241076