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_4122867
_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            'C276 H394 F54 N18 O108 Rh18 S18'
_chemical_formula_weight         9147.53
_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                70.598(3)
_cell_angle_beta                 88.362(3)
_cell_angle_gamma                89.674(3)
_cell_formula_units_Z            1
_cell_length_a                   15.839(4)
_cell_length_b                   25.104(5)
_cell_length_c                   25.353(5)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.38
_cell_volume                     9504(4)
_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 0.979
_diffrn_measured_fraction_theta_max 0.980
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.1545
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58523
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.700
_diffrn_reflns_theta_min         0.852
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (two triflate anions, two methanol and 
 one water molecule) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         2.438
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2029
_refine_ls_number_reflns         35427
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.2000
_refine_ls_R_factor_gt           0.1237
_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^+1.0443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3392
_refine_ls_wR_factor_ref         0.3830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16383
_reflns_number_total             35427
_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        9505(4)
_cod_database_code               4122867
_shelx_estimated_absorpt_t_min   0.711
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2013-4
_shelx_res_checksum              15538
_shelx_hkl_checksum              42951