Insertion of a Spin Crossover FeIII Complex into an Oxalate-Based Layered Material: Coexistence of Spin Canting and Spin Crossover in a Hybrid Magnet
Miguel Clemente-León; Eugeno Coronado; M. Carmen Giménez-López; Alejandra Soriano-Portillo; João C. Waerenborgh; Fernando S. Delgado; Catalina Ruiz-Pérez; Inorganic Chemistry 47 (2008) 9111–9120; doi:10.1021/ic801165b

data_4306322
_publ_section_title
;
Insertion of a Spin Crossover FeIII Complex into an Oxalate-Based Layered
Material: Coexistence of Spin Canting and Spin Crossover in a Hybrid Magnet
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9111
_journal_page_last               9120
_journal_paper_doi               10.1021/ic801165b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C49 H63 Fe2 Mn2 N9 O21'
_chemical_formula_weight         1335.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.287(2)
_cell_length_b                   15.608(3)
_cell_length_c                   34.978(7)
_cell_measurement_temperature    100(2)
_cell_volume                     5563.8(19)
_computing_cell_refinement       'DENZO SNM/HKL2000 (Otwinowski, 1997)'
_computing_data_collection       'MxCube (ESRF, 2007)'
_computing_data_reduction        'Scalepack/HKL2000 (Otwinowski, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         ESRF-BM16
_diffrn_radiation_type           white-beam
_diffrn_radiation_wavelength     0.72930
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35396
_diffrn_reflns_theta_full        21.84
_diffrn_reflns_theta_max         21.84
_diffrn_reflns_theta_min         1.47
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.041
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0887
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1405P)^2^+25.6861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2464
_refine_ls_wR_factor_ref         0.2558
_reflns_number_gt                4792
_reflns_number_total             5626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801165b_si_001_1.cif
_cod_data_source_block           fesaltmncrox
_cod_original_cell_volume        5563.9(19)
_cod_database_code               4306322