A Three-Pronged Attack To Investigate the Electronic Structure of a Family of Ferromagnetic Fe4Ln2 Cyclic Coordination Clusters: A Combined Magnetic Susceptibility, High-Field/High-Frequency Electron Paramagnetic Resonance, and (57)Fe Mössbauer Study.
Schmidt, Sebastian F. M.; Koo, Changhyun; Mereacre, Valeriu; Park, Jaena; Heermann, Dieter W.; Kataev, Vladislav; Anson, Christopher E.; Prodius, Denis; Novitchi, Ghenadie; Klingeler, Rüdiger; Powell, Annie K.; Inorganic chemistry 56 (2017) 4796–4806; doi:10.1021/acs.inorgchem.6b02682

data_4345817
_publ_section_title
;
 A Three-Pronged Attack To Investigate the Electronic Structure of a
 Family of Ferromagnetic Fe4Ln2 Cyclic Coordination Clusters: A Combined
 Magnetic Susceptibility, High-Field/High-Frequency Electron Paramagnetic
 Resonance, and (57)Fe M\"ossbauer Study.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4796
_journal_page_last               4806
_journal_paper_doi               10.1021/acs.inorgchem.6b02682
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C39 H79 Fe4 Ho2 N25 O18, 4(C2 H6 O)'
_chemical_formula_sum            'C47 H103 Fe4 Ho2 N25 O22'
_chemical_formula_weight         1923.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.053(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2509(8)
_cell_length_b                   17.3887(11)
_cell_length_c                   22.622(2)
_cell_measurement_reflns_used    20424
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      1.49
_cell_volume                     3957.6(5)
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector, \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1144
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.123
_refine_diff_density_min         -3.029
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7799
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5425
_reflns_number_total             7799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02682_si_007.cif
_cod_data_source_block           42pivho
_cod_original_cell_volume        3957.6(6)
_cod_database_code               4345817
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.481
_shelx_res_checksum              123
_shelx_hkl_checksum              1753