Spontaneous enrichment of one-handed helix by dissolution of quasiracemic crystals of a tetranuclear single helical complex
Shigehisa Akine; Sayaka Hotate; Takashi Matsumoto; Tatsuya Nabeshima; Chem.Commun. 47 (2011) 2925–; doi:10.1039/c0cc04998k

data_7106048
_publ_section_title
;
 Spontaneous enrichment of one-handed helix by dissolution of quasiracemic
 crystals of a tetranuclear single helical complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              2925
_journal_paper_doi               10.1039/c0cc04998k
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         C49H52.50Cl1.50LaN6O19Zn3
_chemical_formula_sum            'C49 H52.5 Cl1.5 La N6 O19 Zn3'
_chemical_formula_weight         1417.67
_chemical_name_common            (LZn3La(OAc)3(solv))_0.5CHCl3
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 93.479(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.779(7)
_cell_length_b                   8.917(2)
_cell_length_c                   42.307(10)
_cell_measurement_reflns_used    25347
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      0.96
_cell_volume                     10837(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer confocal mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.1795
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            25347
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.239
_exptl_absorpt_correction_T_max  0.9780
_exptl_absorpt_correction_T_min  0.8412
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5704
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.202
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         18160
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+189.6663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1979
_reflns_number_gt                10154
_reflns_number_total             18160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04998K.TXT
_cod_data_source_block           mat129
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C49 H52.50 Cl1.50 La N6 O19 Zn3'
_cod_database_code               7106048