Stepwise construction of extra-large heterometallic calixarene-based cages.
Su, Kongzhao; Jiang, Feilong; Qian, Jinjie; Chen, Lian; Pang, Jiandong; Bawaked, Salem M.; Mokhtar, Mohamed; Al-Thabaiti, Shaeel A; Hong, Maochun; Inorganic chemistry 54 (2015) 3183–3188; doi:10.1021/ic502677g

data_4343125
_publ_section_title
;
 Stepwise construction of extra-large heterometallic calixarene-based
 cages.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3183
_journal_page_last               3188
_journal_paper_doi               10.1021/ic502677g
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C298 H366 Cl4 Dy4 N8 Na4 Ni24 O72 S24'
_chemical_formula_weight         8228.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   23.5399(2)
_cell_length_b                   23.5399(2)
_cell_length_c                   65.7940(4)
_cell_measurement_temperature    100(2)
_cell_volume                     31573.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            69230
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.45
_diffrn_standards_number         72305
_exptl_absorpt_coefficient_mu    4.426
_exptl_absorpt_correction_T_max  0.4714
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'hexagonal prism'
_exptl_crystal_density_diffrn    0.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       green
_exptl_crystal_F_000             8180
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.323
_refine_diff_density_min         -2.610
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         19971
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1499P)^2^+4.0372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2445
_refine_ls_wR_factor_ref         0.2571
_reflns_number_gt                14161
_reflns_number_total             19971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502677g_si_002.cif
_cod_data_source_block           d:HMONC-2
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               4343125