Spin Crossover in Tetranuclear Fe(II) Complexes, {[(tpma)Fe(μ-CN)]4}X4 (X = ClO4(-), BF4(-)).
Hietsoi, Oleksandr; Dunk, Paul W.; Stout, Heather D.; Arroyave, Alejandra; Kovnir, Kirill; Irons, Raechel E.; Kassenova, Nazira; Erkasov, Rakhmetulla; Achim, Catalina; Shatruk, Michael; Inorganic chemistry  (2014) 141202143346008–; doi:10.1021/ic502215h

data_4341792
_publ_section_title
;
 Spin Crossover in Tetranuclear Fe(II) Complexes, {[(tpma)Fe(\m-CN)]4}X4
 (X = ClO4(-), BF4(-)).
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141202143346008
_journal_paper_doi               10.1021/ic502215h
_journal_year                    2014
_chemical_formula_sum            'C78 H75 B4 F16 Fe4 N21 O'
_chemical_formula_weight         1893.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 133.0610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.482(3)
_cell_length_b                   27.585(2)
_cell_length_c                   25.201(3)
_cell_measurement_temperature    100(2)
_cell_volume                     18530(3)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.778
_diffrn_measured_fraction_theta_max 0.793
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.778
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            73254
_diffrn_reflns_point_group_measured_fraction_full 0.778
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.845
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9327
_exptl_absorpt_correction_T_min  0.6818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             7728
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         15042
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1636P)^2^+28.5883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2277
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11038
_reflns_number_total             15042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502215h_si_002.cif
_cod_data_source_block           Structure-1b-100K
_cod_database_code               4341792
_shelx_estimated_absorpt_t_min   0.682
_shelx_estimated_absorpt_t_max   0.933
_shelxl_version_number           2013-4
_shelx_res_checksum              69182
_shelx_hkl_checksum              80791