(3<i>S</i>,5<i>R</i>,8<i>R</i>,9<i>R</i>,10<i>R</i>,13<i>S</i>,14<i>R</i>,17<i>S</i>)-Methyl 3β-acetoxy-17β-chloro-18-oxo-19,20,21,22,29,30-hexanorlupan-28-oate
Císařová, Ivana; Kvasnica, Miroslav; Sarek, Jan; Acta Crystallographica Section E 63 (2007) o3145–o3145; doi:10.1107/S1600536807026487

data_2214297
_publ_section_title
;(3<i>S</i>,5<i>R</i>,8<i>R</i>,9<i>R</i>,10<i>R</i>,13<i>S</i>,14<i>R</i>,17<i>S</i>)-Methyl
 3\b-acetoxy-17\b-chloro-18-oxo-19,20,21,22,29,30-hexanorlupan-28-oate
;
_journal_coeditor_code           LH2400
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3145
_journal_page_last               o3145
_journal_paper_doi               10.1107/S1600536807026487
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C27 H41 Cl O5'
_chemical_formula_moiety         'C27 H41 Cl O5'
_chemical_formula_sum            'C27 H41 Cl O5'
_chemical_formula_weight         481.05
_chemical_name_systematic
;
(3S,5R,8R,9R,10R,13S,14R,17S)-Methyl
3\b-acetoxy-17\b-chloro-18-oxo-19,20,21,22,29,30-hexanorlupan-28-oate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.275(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.331(3)
_cell_length_b                   6.7380(10)
_cell_length_c                   16.366(3)
_cell_measurement_reflns_used    2233
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     1242.0(4)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
;
COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)
;
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.034
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8942
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.217
_refine_ls_abs_structure_details 'Flack (1983), with 1923 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4320
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3899
_reflns_number_total             4320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2400.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2214297
_cod_database_fobs_code          2214297