Homochiral D4-symmetric metal-organic cages from stereogenic Ru(II) metalloligands for effective enantioseparation of atropisomeric molecules
Kai Wu; Kang Li; Ya-Jun Hou; Mei Pan; Lu-Yin Zhang; Ling Chen; Cheng-Yong Su; Nature Communications 7 (2016) 10487–; doi:10.1038/ncomms10487

data_1548200
_publ_section_title
;
 Homochiral D4-symmetric metal-organic cages from stereogenic Ru(II)
 metalloligands for effective enantioseparation of atropisomeric molecules
;
_journal_name_full               'Nature Communications'
_journal_page_first              10487
_journal_paper_doi               10.1038/ncomms10487
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration
;

Determined by S-BINOL as reference
;
_chemical_formula_sum            'C512 H320 N120 O8 Pd6 Ru8'
_chemical_formula_weight         9727.82
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_symmetry_space_group_name_Hall  'I 4 2'
_symmetry_space_group_name_H-M   'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.2284(4)
_cell_length_b                   32.2284(4)
_cell_length_c                   38.2801(7)
_cell_measurement_reflns_used    18410
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.1970
_cell_measurement_theta_min      3.0020
_cell_volume                     39760.4(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30e (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30e (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30e (Agilent, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            66544
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        63.687
_diffrn_reflns_theta_max         63.687
_diffrn_reflns_theta_min         3.015
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30e (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.813
_exptl_crystal_description       block
_exptl_crystal_F_000             9848
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.131(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         16396
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+72.3521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2375
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9021
_reflns_number_total             16396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIF5.cif
_cod_data_source_block           Delta-cage
_cod_original_cell_volume        39760.5(13)
_cod_database_code               1548200
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.625
_shelx_res_checksum              93832
_shelx_hkl_checksum              628
_shelx_fab_checksum              32277