A large spin-crossover [Fe4L4]8+ tetrahedral cage
Li Li; Naoto Saigo; Yingjie Zhang; Daniel J. Fanna; Nicholas D. Shepherd; Jack K. Clegg; Rongkun Zheng; Shinya Hayami; Leonard F. Lindoy; Janice R. Aldrich-Wright; Chun-Guang Li; Jason K. Reynolds; David G. Harman; Feng Li; Journal of Materials Chemistry C 3 (2015) 7878–7882; doi:10.1039/C5TC00991J

data_7234364
_publ_section_title
;
 A large spin-crossover [Fe4L4]8+ tetrahedral cage
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              7878
_journal_page_last               7882
_journal_paper_doi               10.1039/C5TC00991J
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C156 H132 Fe4 N36, 8(B F4), 16(C2 H3 N)'
_chemical_formula_sum            'C188 H180 B8 F32 Fe4 N52'
_chemical_formula_weight         4085.71
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   31.590(5)
_cell_length_b                   31.590(5)
_cell_length_c                   18.320(4)
_cell_measurement_reflns_used    139384
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      0.744
_cell_volume                     15833(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)'
_computing_publication_material  'enCIFer 1.0 (CCDC, 2003)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Altomare et. al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.692
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monocromated synchrotron'
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.692
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            139384
_diffrn_reflns_point_group_measured_fraction_full 0.692
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         21.967
_diffrn_reflns_theta_min         0.744
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.4272
_exptl_absorpt_correction_T_min  0.3657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       prism
_exptl_crystal_F_000             6312
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2204
_refine_ls_number_reflns         25723
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0961
_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^)+(0.1718P)^2^+30.1663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2485
_refine_ls_wR_factor_ref         0.2580
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.692
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                23244
_reflns_number_total             25723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2015-3-7878.cif
_cod_data_source_block           1
_cod_original_cell_volume        15833(6)
_cod_database_code               7234364