Synthesis and Magnetic Characterization of Fe(III)-Based 9-Metallacrown-3 Complexes Which Exhibit Magnetorefrigerant Properties.
Chow, Chun Y.; Guillot, Régis; Rivière, Eric; Kampf, Jeff W.; Mallah, Talal; Pecoraro, Vincent L.; Inorganic chemistry 55 (2016) 10238–10247; doi:10.1021/acs.inorgchem.6b01404

data_4348599
_publ_section_title
;
 Synthesis and Magnetic Characterization of Fe(III)-Based 9-Metallacrown-3
 Complexes Which Exhibit Magnetorefrigerant Properties.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10238
_journal_page_last               10247
_journal_paper_doi               10.1021/acs.inorgchem.6b01404
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C45 H39 Fe4 N3 O18 + (solvent)'
_chemical_formula_sum            'C45 H39 Fe4 N3 O18'
_chemical_formula_weight         1133.19
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.44496(20)
_cell_length_b                   18.44496(20)
_cell_length_c                   31.7624(3)
_cell_measurement_reflns_used    26850
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      73.5230
_cell_measurement_theta_min      3.0690
_cell_volume                     9358.35(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            82010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.847
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    7.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       cube
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.000143(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0844P)^2^+9.8939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3943
_reflns_number_total             4218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01404_si_002.cif
_cod_data_source_block           1-OBz
_cod_original_cell_volume        9358.3(2)
_cod_database_code               4348599
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.573
_shelxl_version_number           2014/6
_shelx_res_checksum              78687
_shelx_hkl_checksum              19721
_shelx_fab_checksum              31916