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_4122872
_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            'C131 H180 F15 N16 O51 Rh9 S5'
_chemical_formula_weight         4166.39
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   22.6440(15)
_cell_length_b                   22.6440(15)
_cell_length_c                   20.7045(14)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.22
_cell_volume                     9193.9(11)
_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 0.999
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65825
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         1.038
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (one and two thirds triflate anions and 
 four water molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         0.654
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details
; 
 Flack x determined using 4450 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.014(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         14052
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0914P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                10373
_reflns_number_total             14052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5096914_si_001.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4122867--4122872.cif.'
_cod_original_cell_volume        9193.9(14)
_cod_database_code               4122872
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.873
_shelxl_version_number           2013-2
_shelx_res_checksum              72851
_shelx_hkl_checksum              21584