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_7040026
_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            'C65 H73 F9 Ir3 N7 O18 S3'
_chemical_formula_weight         2084.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-20 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.502(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.363(2)
_cell_length_b                   18.814(2)
_cell_length_c                   21.881(2)
_cell_measurement_reflns_used    9308
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.16
_cell_measurement_theta_min      3.20
_cell_volume                     7416.4(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35794
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        65.151
_diffrn_reflns_theta_max         65.151
_diffrn_reflns_theta_min         2.452
_exptl_absorpt_coefficient_mu    11.820
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_description       block
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one triflate anion, two methanol and 
 three water molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         8.206
_refine_diff_density_min         -5.856
_refine_diff_density_rms         0.383
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         12465
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.1245
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1886P)^2^+363.8772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3272
_refine_ls_wR_factor_ref         0.3323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11066
_reflns_number_total             12465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02460b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7040026--7040028.cif.'
_cod_original_cell_volume        7416.8(14)
_cod_database_code               7040026
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.156
_shelx_estimated_absorpt_t_max   0.270
_shelx_res_checksum              21139