Bidirectional synthesis of the central amino acid of chloptosin.
Hong, Wen-Xu; Chen, Ling-Jun; Zhong, Chun-Long; Yao, Zhu-Jun; Organic letters 8 (2006) 4919–4922; doi:10.1021/ol0620139

data_1506242
_publ_section_title
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 Bidirectional synthesis of the central amino acid of chloptosin.
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_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              4919
_journal_page_last               4922
_journal_paper_doi               10.1021/ol0620139
_journal_volume                  8
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42 H56 Cl2 N4 O12'
_chemical_formula_weight         879.81
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   27.991(7)
_cell_length_b                   27.991(7)
_cell_length_c                   20.057(7)
_cell_measurement_reflns_used    2490
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.867
_cell_measurement_theta_min      4.888
_cell_volume                     13609(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1387
_diffrn_reflns_av_sigmaI/netI    0.2041
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22864
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75094
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4194
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.467
_exptl_crystal_size_min          0.289
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(13)
_refine_ls_extinction_coef       0.0024(2)
_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   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10787
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.2038
_refine_ls_R_factor_gt           0.0963
_refine_ls_shift/su_max          0.098
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2847
_reflns_number_gt                3929
_reflns_number_total             10787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0620139si20060815_013725.cif
_cod_data_source_block           cd25192
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' 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 
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_cod_original_cell_volume        13609(6)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               1506242