A nonanuclear triangular macrocycle and a linear heptanuclear heterometallic complex based on a 2-substituted imidazole-4,5-dicarboxylate ligand.
Lin, Yue-Jian; Shan, Wei-Long; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12680–12684; doi:10.1039/c6dt02460b

data_7040028
_publ_section_title
;
 A nonanuclear triangular macrocycle and a linear heptanuclear
 heterometallic complex based on a 2-substituted
 imidazole-4,5-dicarboxylate ligand.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12680
_journal_page_last               12684
_journal_paper_doi               10.1039/c6dt02460b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C156.5 H215 F13.5 N13.5 O53 Rh9 S4.5'
_chemical_formula_weight         4460.37
_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
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.727(2)
_cell_angle_beta                 91.725(2)
_cell_angle_gamma                107.527(2)
_cell_formula_units_Z            2
_cell_length_a                   16.2720(8)
_cell_length_b                   23.9463(11)
_cell_length_c                   26.2849(12)
_cell_measurement_reflns_used    9494
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.39
_cell_measurement_theta_min      2.54
_cell_volume                     9759.6(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      150(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            151833
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         2.535
_exptl_absorpt_coefficient_mu    7.223
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             4542
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (one triflate anion and a half, two 
 diethyl ether, five methanol and six water molecules) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         2.948
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2018
_refine_ls_number_reflns         34721
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.004
_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^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2675
_refine_ls_wR_factor_ref         0.2913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24266
_reflns_number_total             34721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02460b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7040026--7040028.cif.'
_cod_original_formula_sum        'C156.50 H215 F13.50 N13.50 O53 Rh9 S4.50'
_cod_database_code               7040028
_shelx_estimated_absorpt_t_min   0.265
_shelx_estimated_absorpt_t_max   0.478
_shelxl_version_number           2013-2
_shelx_res_checksum              67772