Turrapubesins A and B, first examples of halogenated and maleimide-bearing limonoids in nature from Turraea pubescens.
Wang, Xiao-Ning; Yin, Sheng; Fan, Cheng-Qi; Wang, Fang-Dao; Lin, Li-Ping; Ding, Jian; Yue, Jian-Min; Organic letters 8 (2006) 3845–3848; doi:10.1021/ol061466a

data_1506152
_publ_section_title
;
 Turrapubesins A and B, first examples of halogenated and
 maleimide-bearing limonoids in nature from Turraea pubescens.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              3845
_journal_page_last               3848
_journal_paper_doi               10.1021/ol061466a
_journal_volume                  8
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_sum            'C31 H39 Cl O9'
_chemical_formula_weight         591.07
_chemical_melting_point          454
_chemical_name_common            'Turrapubesin A'
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.7020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5361(10)
_cell_length_b                   11.1344(10)
_cell_length_c                   13.6933(12)
_cell_measurement_reflns_used    3217
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.000
_cell_measurement_theta_min      4.821
_cell_volume                     1521.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8668
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7689
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             628
_exptl_crystal_preparation       methanol
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.485
_exptl_crystal_size_min          0.347
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(13)
_refine_ls_extinction_coef       0.008(3)
_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   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                4073
_reflns_number_total             5363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol061466asi20060615_013213.cif
_cod_data_source_block           cd26176
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1506152