Crystal structure, Hirshfeld surface analysis and electrostatic potential study of naturally occurring cassane-type diterpenoid Pulcherrimin C monohydrate at 100K
Kumar, Rajesh; Ogbeide, K. Osahon; Mujeeb-Ur-Rehman; Owolabi, Bodunde; Falodun, Abiodun; Choudhary, M. Iqbal; Yousuf, Sammer; Acta Crystallographica Section E 75 (2019) 119–123; doi:10.1107/S2056989018017498

data_2242813
_publ_section_title
;
 Crystal structure, Hirshfeld surface analysis and electrostatic potential
 study of naturally occurring cassane-type diterpenoid Pulcherrimin C
 monohydrate at 100K
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              119
_journal_page_last               123
_journal_paper_doi               10.1107/S2056989018017498
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C34 H36 O8, H2 O'
_chemical_formula_moiety         'C34 H36 O8, H2 O'
_chemical_formula_sum            'C34 H38 O9'
_chemical_formula_weight         590.64
_chemical_name_common            'Pulcherrimin C monohydrate'
_chemical_name_systematic
;5,6-Bis(benzoyloxy)-4a-hydroxy-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
monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8027(7)
_cell_length_b                   13.2843(8)
_cell_length_c                   19.0835(10)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      4.05
_cell_volume                     2992.1(3)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
APEX2 (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18780
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.213
_diffrn_reflns_theta_min         4.055
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.7720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.234
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1939 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5425
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0537P)^2^+0.4392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                4931
_reflns_number_total             5425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5245sup1.cif
_cod_data_source_block           I
_cod_database_code               2242813
_cod_database_fobs_code          2242813
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.926
_shelx_hkl_checksum              71450
_shelx_res_checksum              20097