A tetranuclear iridium(iii) complex with a flavin analogue as a bridging ligand in different coordination modes and exchangeable anion encapsulation in a supramolecular cage.
Kojima, Takahiko; Inui, Yuji; Miyazaki, Soushi; Shiro, Motoo; Fukuzumi, Shunichi; Chemical communications (Cambridge, England)  (2009) 6643–6645; doi:10.1039/b911033j

data_7104974
_publ_section_title
;
 A tetranuclear iridium(iii) complex with a flavin analogue as a
 bridging ligand in different coordination modes and exchangeable anion
 encapsulation in a supramolecular cage.
;
_journal_issue                   43
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6643
_journal_page_last               6645
_journal_paper_doi               10.1039/b911033j
_journal_year                    2009
_chemical_formula_moiety
'C70 H74 Cl2 Ir4 N12 O6, 4.5(C H Cl3), 2(H2 O), 2(F6 P)'
_chemical_formula_sum            'C74.5 H82.5 Cl15.5 F12 Ir4 N12 O8 P2'
_chemical_formula_weight         2882.38
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 122.6940(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   31.4226(7)
_cell_length_b                   24.4702(5)
_cell_length_c                   34.0543(8)
_cell_measurement_reflns_used    67831
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     22036.3(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku SATURN'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            92718
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    5.304
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             11096.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.81
_refine_diff_density_min         -2.01
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         25019
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.0090
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1245P)^2^+312.9670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2292
_reflns_number_gt                19654
_reflns_number_total             25019
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b911033j.txt
_cod_data_source_block           Ir-complex
_cod_original_formula_sum        'C74.5 H82.5 Cl15.5 F12 Ir4 N12 O8 P2 '
_cod_database_code               7104974
_verf_plat201_alert_2_a
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PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 16
RESPONSE: Disordered atoms heavily superimposed, see _publ_section_
exptl_refinement.
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_verf_plat242_alert_2_a
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PROBLEM: Check Low Ueq as Compared to Neighbors for C71
RESPONSE: No significant differences found, see _atom_site_U_iso_
or_equiv
;
_verf_plat431_alert_2_a
;
PROBLEM: Short Inter HL..A Contact Cl8 .. Cl21 .. 2.49 Ang.
RESPONSE: Disordered atoms belonging to different groups in the same
assembly, see _atom_site_disorder_assembly and _atom_site_
disorder_group
;
_verf_plat601_alert_2_a
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . . 1372.00 A**3
RESPONSE: Other solvent molecules not located in the final d-Fourier map.
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