Spontaneous racemic resolution ‒ towards control of molecular recognition nature
Białońska, Agata; Ciunik, Zbigniew; CrystEngComm 15 (2013) 6448–; doi:10.1039/c3ce40778k

data_7210338
_publ_section_title
;
 Spontaneous racemic resolution -- towards control of molecular
 recognition nature
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6448
_journal_paper_doi               10.1039/c3ce40778k
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C23 H27 N2 O4, C11 H9 N6 O8, 5(C H4 O)'
_chemical_formula_sum            'C36.5 H46 N6 O14.5'
_chemical_formula_weight         800.79
_chemical_name_systematic
;
brucinium N-(3,5-dinitrobenzoyl)-L-asparaginate methanol 5-solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                73.21(2)
_cell_angle_beta                 79.37(2)
_cell_angle_gamma                80.53(3)
_cell_formula_units_Z            2
_cell_length_a                   7.924(2)
_cell_length_b                   12.140(3)
_cell_length_c                   20.495(3)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.87
_cell_volume                     1842.1(7)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
SIR2004 (Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori G.,
Spagna, R., J. Appl. Cryst. 2005. 38, 381-388.)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.1776
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17188
_diffrn_reflns_point_group_measured_fraction_full 0.724
_diffrn_reflns_point_group_measured_fraction_max 0.646
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.799
_diffrn_reflns_theta_min         2.875
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       plate
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
Flack x determined using 1261 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         12418
_refine_ls_number_restraints     497
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.1573
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0524P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.417
_reflns_Friedel_fraction_full    0.453
_reflns_Friedel_fraction_max     0.380
_reflns_number_gt                5490
_reflns_number_total             12418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce40778k.txt
_cod_data_source_block           BDNBLN
_cod_original_cell_volume        1842.1(8)
_cod_original_formula_sum        'C36.50 H46 N6 O14.50'
_cod_database_code               7210338
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.996