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_4341793
_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            'C77.5 H73.5 B4 F16 Fe4 N20.75 O'
_chemical_formula_weight         1882.21
_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                 133.2530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.995(5)
_cell_length_b                   27.796(4)
_cell_length_c                   25.479(6)
_cell_measurement_temperature    209(2)
_cell_volume                     19083(6)
_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      209(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -46
_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            74204
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.831
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.9086
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             7678
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         19393
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1752P)^2^+83.9949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2795
_refine_ls_wR_factor_ref         0.3112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13365
_reflns_number_total             19393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502215h_si_003.cif
_cod_data_source_block           Structure-1b-210K
_cod_original_formula_sum        'C77.50 H73.50 B4 F16 Fe4 N20.75 O'
_cod_database_code               4341793
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.909
_shelxl_version_number           2013-4
_shelx_res_checksum              91764
_shelx_hkl_checksum              60164