Spotting a Conglomerate Is Just Halfway to Achieving a Preparative Resolution by Preferential Crystallization
Gonella, Silvia; Mahieux, Julien; Sanselme, Morgane; Coquerel, Gérard; Organic Process Research & Development 16 (2012) 286–; doi:10.1021/op200092f

data_1503630
_publ_section_title
;
 Spotting a Conglomerate Is Just Halfway to Achieving a Preparative
 Resolution by Preferential Crystallization
;
_journal_issue                   2
_journal_name_full               'Organic Process Research &amp; Development'
_journal_page_first              286
_journal_paper_doi               10.1021/op200092f
_journal_volume                  16
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H46 Br2 N2 O15'
_chemical_formula_sum            'C35 H46 Br2 N2 O15'
_chemical_formula_weight         954.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           151
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      151
_symmetry_space_group_name_Hall  'P 31 2 (0 0 4)'
_symmetry_space_group_name_H-M   'P 31 1 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-02-21T15:06:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.299(3)
_cell_length_b                   11.299(3)
_cell_length_c                   30.405(8)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     3361.7(15)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            22750
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.875
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0
_exptl_crystal_size_mid          0
_exptl_crystal_size_min          0
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4197
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          2.296
_refine_ls_shift/su_mean         0.02
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                2312
_reflns_number_total             4197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            op200092f_si_001.cif
_cod_data_source_block           th328
_cod_original_cell_volume        3361.6(14)
_cod_original_sg_symbol_Hall     'P 31 2 (004)'
_cod_database_code               1503630