Stepwise Construction of Discrete Heterometallic Coordination Cages Based on Self-Sorting Strategy.
Li, Hao; Han, Ying-Feng; Lin, Yue-Jian; Guo, Zi-Wei; Jin, Guo-Xin; Journal of the American Chemical Society 136 (2014) 2982–; doi:10.1021/ja412667t

data_4120669
_publ_section_title
;
 Stepwise Construction of Discrete Heterometallic Coordination Cages Based
 on Self-Sorting Strategy.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2982
_journal_paper_doi               10.1021/ja412667t
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C192 H348 Cu4 F24 Ir8 N16 O114 S8'
_chemical_formula_weight         7209.08
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.111(6)
_cell_length_b                   34.111(6)
_cell_length_c                   22.396(4)
_cell_measurement_reflns_used    9146
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.39
_cell_volume                     26059(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            189030
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_min         0.844
_exptl_absorpt_coefficient_mu    4.566
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             14400
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one OTf- anion, nineteen water and 
 twelve methanol molecules) which could not be refined or 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit them. 
;
_refine_diff_density_max         2.015
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
; 
 Flack x determined using 8965 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         30094
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+94.8475P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                23063
_reflns_number_total             30094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja412667t_si_001.cif
_cod_data_source_block           HCC-2
_cod_original_cell_volume        26059(10)
_cod_database_code               4120669
_shelx_estimated_absorpt_t_min   0.588
_shelx_estimated_absorpt_t_max   0.741
_shelxl_version_number           2013-2