Self-Assembly of an Imidazolate-Bridged Fe(III)/Cu(II) Heterometallic Cage.
Reichel, Florian; Clegg, Jack K.; Gloe, Karsten; Gloe, Kerstin; Weigand, Jan J.; Reynolds, Jason K.; Li, Chun-Guang; Aldrich-Wright, Janice R; Kepert, Cameron J.; Lindoy, Leonard F.; Yao, Hong-Chang; Li, Feng; Inorganic chemistry 53 (2014) 688–690; doi:10.1021/ic402686s

data_4337118
_publ_section_title
;
 Self-Assembly of an Imidazolate-Bridged Fe(III)/Cu(II) Heterometallic
 Cage.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              688
_journal_page_last               690
_journal_paper_doi               10.1021/ic402686s
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
;
C144 H159 Cu6 Fe8 N80, 4(H2 O), 12(Cl O4), 11(C4 H8 O2), 9(C3 H7 N O)
;
_chemical_formula_sum            'C215 H327 Cl12 Cu6 Fe8 N89 O83'
_chemical_formula_weight         6740.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.3989(6)
_cell_length_b                   21.3989(6)
_cell_length_c                   30.3895(10)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.68
_cell_volume                     13915.7(7)
_computing_cell_refinement       'SAINT (Bruker-Nonius, 2003)'
_computing_data_collection       'APEX (Bruker-Nonius, 2003)'
_computing_data_reduction
'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)'
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Altomare, et. al. 2011)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.577
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       \w+\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.577
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92340
_diffrn_reflns_point_group_measured_fraction_full 0.577
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         2.928
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2012)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       prism
_exptl_crystal_F_000             6980
_platon_squeeze_details
;
electron density included as missing anions and dixoane/dmf solvent
;
_refine_diff_density_max         1.786
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.367
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         7282
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.367
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.1195
_refine_ls_shift/su_max          0.000
_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^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3461
_refine_ls_wR_factor_ref         0.4116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             7282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402686s_si_001.cif
_cod_data_source_block           squeezed
_cod_original_cell_volume        13915.7(9)
_cod_database_code               4337118
_shelxl_version_number           2013-4