Large Orbital Magnetic Moment Measured in the [TpFe(III)(CN)3](-) Precursor of Photomagnetic Molecular Prussian Blue Analogues.
Jafri, Sadaf Fatima; Koumousi, Evangelia S.; Sainctavit, Philippe; Juhin, Amélie; Schuler, Vivien; Bun U, Oana; Mitcov, Dmitri; Dechambenoit, Pierre; Mathonière, Corine; Clérac, Rodolphe; Otero, Edwige; Ohresser, Philippe; Cartier Dit Moulin, Christophe; Arrio, Marie-Anne; Inorganic chemistry 55 (2016) 6980–6987; doi:10.1021/acs.inorgchem.6b00664

data_4347830
_publ_section_title
;
 Large Orbital Magnetic Moment Measured in the [TpFe(III)(CN)3](-)
 Precursor of Photomagnetic Molecular Prussian Blue Analogues.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6980
_journal_page_last               6987
_journal_paper_doi               10.1021/acs.inorgchem.6b00664
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C16 H36 N, C12 H10 B Fe N9, 3(H2 O)'
_chemical_formula_sum            'C28 H52 B Fe N10 O3'
_chemical_formula_weight         643.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                87.2840(10)
_cell_angle_beta                 76.7360(10)
_cell_angle_gamma                60.8650(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1956(4)
_cell_length_b                   11.2191(4)
_cell_length_c                   15.9740(6)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.55
_cell_volume                     1700.91(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Autostructure (Bruker)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II Quasar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41492
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         2.547
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6952
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1140P)^2^+2.4558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5867
_reflns_number_total             6952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00664_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4347830
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              90450
_shelx_hkl_checksum              86098