Octadecanuclear Macrocycles and Nonanuclear Bowl-Shaped Structures Based on Two Analogous Pyridyl-Substituted Imidazole-4,5-dicarboxylate Ligands.
Zhang, Ying-Ying; Shen, Xu-Yu; Weng, Lin-Hong; Jin, Guo-Xin; Journal of the American Chemical Society 136 (2014) 15521–15524; doi:10.1021/ja5096914

data_4122868
_publ_section_title
;
 Octadecanuclear Macrocycles and Nonanuclear Bowl-Shaped Structures Based
 on Two Analogous Pyridyl-Substituted Imidazole-4,5-dicarboxylate Ligands.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15521
_journal_page_last               15524
_journal_paper_doi               10.1021/ja5096914
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C274 H398 F24 N28 O104 Rh18 S8'
_chemical_formula_weight         8313.04
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                100.142(2)
_cell_angle_beta                 95.751(2)
_cell_angle_gamma                95.281(2)
_cell_formula_units_Z            1
_cell_length_a                   18.8903(19)
_cell_length_b                   19.910(2)
_cell_length_c                   24.123(3)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.31
_cell_volume                     8830.2(17)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62609
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         0.864
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one triflate anion and six methanol 
 molecules) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         3.006
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2075
_refine_ls_number_reflns         38108
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0728
_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^)+(0.2000P)^2^+0.5034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24673
_reflns_number_total             38108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5096914_si_001.cif
_cod_data_source_block           3'
_cod_depositor_comments
'Adding full bibliography for 4122867--4122872.cif.'
_cod_original_cell_volume        8829.9(16)
_cod_database_code               4122868
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.910
_shelxl_version_number           2013-4
_shelx_res_checksum              61627
_shelx_hkl_checksum              22738