New Steroids with a Rearranged Skeleton as (h)P300 Inhibitors from the Sponge Theonella swinhoei.
Gong, Jun; Sun, Peng; Jiang, Nan; Riccio, Raffaele; Lauro, Gianluigi; Bifulco, Giuseppe; Li, Tie-Jun; Gerwick, William H; Zhang, Wen; Organic letters 16 (2014) 2224–2227; doi:10.1021/ol5007345

data_1514222
_publ_section_title
;
 New Steroids with a Rearranged Skeleton as (h)P300 Inhibitors from the
 Sponge Theonella swinhoei.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              2224
_journal_page_last               2227
_journal_paper_doi               10.1021/ol5007345
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C29 H46 O3'
_chemical_formula_weight         442.66
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   26.5740(4)
_cell_length_b                   26.5740(4)
_cell_length_c                   6.56120(10)
_cell_measurement_reflns_used    3810
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      59.81
_cell_measurement_theta_min      5.77
_cell_volume                     4012.62(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            30446
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.975
_diffrn_reflns_theta_min         5.767
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
;
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
; 
 Flack x determined using 1068 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1685P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2327
_reflns_Friedel_coverage         0.626
_reflns_Friedel_fraction_full    0.766
_reflns_Friedel_fraction_max     0.740
_reflns_number_gt                3475
_reflns_number_total             4407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5007345_si_001.cif
_cod_data_source_block           cu_dm13654_0m
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-8800/cifs/1514222.cif.
;
_cod_original_cell_volume        4012.62(14)
_cod_database_code               1514222
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2013-4
_shelx_res_checksum              44647
_shelx_hkl_checksum              54900