Bufospirostenin A and Bufogargarizin C, Steroids with Rearranged Skeletons from the Toad Bufo bufo gargarizans.
Tian, Hai-Yan; Ruan, Li-Jun; Yu, Tong; Zheng, Qing-Fei; Chen, Nan-Hao; Wu, Rui-Bo; Zhang, Xiao-Qi; Wang, Lei; Jiang, Ren-Wang; Ye, Wen-Cai; Journal of natural products 80 (2017) 1182–1186; doi:10.1021/acs.jnatprod.6b01018

data_1545391
_publ_section_title
;
 Bufospirostenin A and Bufogargarizin C, Steroids with Rearranged
 Skeletons from the Toad Bufo bufo gargarizans.
;
_journal_issue                   4
_journal_name_full               'Journal of natural products'
_journal_page_first              1182
_journal_page_last               1186
_journal_paper_doi               10.1021/acs.jnatprod.6b01018
_journal_volume                  80
_journal_year                    2017
_chemical_formula_sum            'C24 H32 O3'
_chemical_formula_weight         368.49
_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                   8.42641(16)
_cell_length_b                   10.9379(2)
_cell_length_c                   21.7505(4)
_cell_measurement_reflns_used    4033
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.70
_cell_measurement_theta_min      4.06
_cell_volume                     2004.68(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4137
_diffrn_reflns_theta_full        62.70
_diffrn_reflns_theta_max         62.70
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71312
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_coef       0.0051(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                2637
_reflns_number_total             2806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np6b01018_si_003.cif
_cod_data_source_block           xf5
_cod_depositor_comments
;
Adding full bibliography for 1545390--1545391.cif.

2019-03-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2004.69(6)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C96 H128 O12'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1473.98
_cod_database_code               1545391