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_1548196
_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_formula_sum            'C41.5 H31 F12 N7 P2 Ru'
_chemical_formula_weight         1018.74
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.5619(2)
_cell_length_b                   25.5619(2)
_cell_length_c                   12.5769(2)
_cell_measurement_reflns_used    30668
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.9477
_cell_measurement_theta_min      2.8818
_cell_volume                     8217.88(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            64514
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.484
_diffrn_reflns_theta_min         2.888
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       needle
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.623
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         19736
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+8.7890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                17221
_reflns_number_total             19736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIF1.cif
_cod_data_source_block           delta-1
_cod_depositor_comments
;

2019-06-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        8217.88(18)
_cod_original_formula_sum        'C83 H62 F24 N14 P4 Ru2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2037.48
_cod_database_code               1548196
_shelx_estimated_absorpt_t_min   0.768
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              39406
_shelx_hkl_checksum              23284