Trigonal-Bipyramidal Metal Cyanide Complexes: A Versatile Platform for the Systematic Assessment of the Magnetic Properties of Prussian Blue Materials
Kristen E. Funck; Matthew G. Hilfiger; Curtis P. Berlinguette; Michael Shatruk; Wolfgang Wernsdorfer; Kim R. Dunbar; Inorganic Chemistry 48 (2009) 3438–3452; doi:10.1021/ic801990g

data_4301940
_publ_contact_author_address
; 
Department of Chemistry
Texas A&M University
PO Box 30012 
College Station 
Texas 77842-3012 
USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         (979)8457177
_publ_contact_author_name        'Dunbar, Kim R.'
_publ_contact_author_phone       (979)8625235
_publ_section_title
;
Trigonal-Bipyramidal Metal Cyanide Complexes: A Versatile Platform for the
Systematic Assessment of the Magnetic Properties of Prussian Blue Materials
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3438
_journal_page_last               3452
_journal_paper_doi               10.1021/ic801990g
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C122 H147 Cl3 Co3 Fe2 Mn1.5 N24 O26.5'
_chemical_formula_weight         2850.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.07(3)
_cell_angle_beta                 107.88(3)
_cell_angle_gamma                91.15(3)
_cell_formula_units_Z            2
_cell_length_a                   17.681(4)
_cell_length_b                   20.615(4)
_cell_length_c                   23.986(5)
_cell_measurement_temperature    173(2)
_cell_volume                     7987(4)
_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-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker SMART CCD area-dectector'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_sigmaI/netI    0.2609
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65813
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.9388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2961
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.849
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.0143(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1639
_refine_ls_number_reflns         33789
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.2793
_refine_ls_R_factor_gt           0.1311
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3375
_refine_ls_wR_factor_ref         0.4204
_reflns_number_gt                12223
_reflns_number_total             33789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801990g_si_003.cif
_cod_data_source_block
d:\mydocu~1\science\curren~1\tbpfor~1\struct~1\typeb
_cod_original_cell_volume        7987(3)
_cod_original_formula_sum        'C122 H147 Cl3 Co3 Fe2 Mn1.50 N24 O26.50'
_cod_database_code               4301940