The absolute structure of ptilosarcenone 2.5-hydrate, a diterpenoid briarane from the orange sea pen <i>Ptilosarcus gurneyi</i> (Gray)
Nurco, Daniel J.; Conklin, Douglas E.; Shapiro, Nathan S.; Tran, Elaine; Acta Crystallographica Section E 67 (2011) o181–o182; doi:10.1107/S1600536810050142

data_2228723
_publ_section_title
;
 The absolute structure of ptilosarcenone 2.5-hydrate, a diterpenoid
 briarane from the orange sea pen <i>Ptilosarcus gurneyi</i> (Gray)
;
_journal_coeditor_code           HB5711
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o181
_journal_page_last               o182
_journal_paper_doi               10.1107/S1600536810050142
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '2C24 H29 Cl O8, 5H2 O'
_chemical_formula_moiety         'C24 H29 Cl O8, 2.5(H2 O)'
_chemical_formula_sum            'C24 H34 Cl O10.5'
_chemical_formula_weight         525.98
_chemical_name_common            'ptilosarcenone 2.5-hydrate'
_chemical_name_systematic
;
ptilosarcenone 2.5-hydrate
;
_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   mixed
_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            8
_cell_length_a                   9.8505(4)
_cell_length_b                   13.5256(6)
_cell_length_c                   39.3169(17)
_cell_measurement_reflns_used    9574
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.3
_cell_volume                     5238.3(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      95(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            75112
_diffrn_reflns_theta_full        28.62
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.602
_refine_ls_abs_structure_details
;
Flack (1983), 5967 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         13416
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+10.7413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                12944
_reflns_number_total             13416
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5711.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C24 H34 Cl1 O10.5'
_cod_database_code               2228723
_cod_database_fobs_code          2228723