A luminescent edge-interlocked prismatic heteroleptic metallocage assembled through a ligand replacement reaction.
Zhan, Shun-Ze; Li, Jing-Hong; Zhang, Guo-Hui; Liu, Xiao-Wei; Li, Mian; Zheng, Ji; Ng, Seik Weng; Li, Dan; Chemical communications (Cambridge, England) 55 (2019) 11992–11995; doi:10.1039/c9cc05236d

data_7125399
_publ_section_title
;
 A luminescent edge-interlocked prismatic heteroleptic metallocage
 assembled through a ligand replacement reaction.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11992
_journal_page_last               11995
_journal_paper_doi               10.1039/c9cc05236d
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C22 H22 N4 S3, C2 H6 O'
_chemical_formula_sum            'C24 H28 N4 O S3'
_chemical_formula_weight         484.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-08-12 deposited with the CCDC.	2019-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.1098(4)
_cell_length_b                   13.4720(2)
_cell_length_c                   5.71530(10)
_cell_measurement_reflns_used    14606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9980
_cell_measurement_theta_min      5.5010
_cell_volume                     2472.34(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.258
_diffrn_reflns_theta_min         5.511
_exptl_absorpt_coefficient_mu    2.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1092 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+2.2602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                2501
_reflns_number_total             2537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05236d2.cif
_cod_data_source_block           H2L2
_cod_database_code               7125399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.474
_shelx_estimated_absorpt_t_max   0.759
_shelx_res_checksum              89555