Crystal structure and Hirshfeld surface analysis of the naturally occurring cassane-type diterpenoid, 6β-cinnamoyl-7β-hydroxyvouacapen-5α-ol
Ogbeide, K. Osahon; Kumar, Rajesh; Mujeeb-Ur-Rehman; Owolabi, Bodunde; Falodun, Abiodun; Choudhary, M. Iqbal; Yousuf, Sammer; Acta Crystallographica Section E 74 (2018) 385–389; doi:10.1107/S2056989018002499

data_2242398
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of the naturally
 occurring cassane-type diterpenoid,
 6\b-cinnamoyl-7\b-hydroxyvouacapen-5\a-ol
;
_journal_coeditor_code           IS5486
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              385
_journal_page_last               389
_journal_paper_doi               10.1107/S2056989018002499
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C29 H36 O5'
_chemical_formula_moiety         'C29 H36 O5'
_chemical_formula_sum            'C29 H36 O5'
_chemical_formula_weight         464.58
_chemical_name_systematic
'(4a<i>R</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>)-4a,6-Dihydroxy-4,4,7,11b-tetramethyl-1,2,3,4,4a,5,6,6a,7,11,11a,11b-dodecahydrophenanthro[3,2-<i>b</i>]furan-5-yl 3-phenylprop-2-enoate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 94.9300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1129(3)
_cell_length_b                   7.8973(2)
_cell_length_c                   12.9253(3)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      3.43
_cell_volume                     1231.85(5)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
APEX2 (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and SHELXTL (Sheldrick,
2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21754
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.253
_diffrn_reflns_theta_min         3.432
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       Plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.207
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4526
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.2131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                4183
_reflns_number_total             4526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5486sup1.cif
_cod_data_source_block           I
_cod_database_code               2242398
_cod_database_fobs_code          2242398
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              43257
_shelx_res_checksum              8659