Properties of Prussian Blue Materials Manifested in Molecular Complexes: Observation of Cyanide Linkage Isomerism and Spin-Crossover Behavior in Pentanuclear Cyanide Clusters
Mikhail Shatruk; Alina Dragulescu-Andrasi; Kristen Chambers; Sebastian A. Stoian; Emile L. Bominaar; Catalina Achim; Kim R. Dunbar; Journal of the American Chemical Society 129 (2007) 6104–6116; doi:10.1021/ja066273x

data_4109405
_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
;
 Properties of Prussian Blue Materials Manifested in Molecular Complexes:
 Observation of Cyanide Linkage Isomerism and Spin-Crossover Behavior in
 Pentanuclear Cyanide Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6104
_journal_page_last               6116
_journal_paper_doi               10.1021/ja066273x
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C108 H96 Co2 Fe3 N24'
_chemical_formula_weight         2015.50
_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                 97.938(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.159(4)
_cell_length_b                   24.952(5)
_cell_length_c                   24.709(5)
_cell_measurement_reflns_used    109
_cell_measurement_temperature    110(2)
_cell_volume                     11699(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, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_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  0.1639
_diffrn_reflns_av_sigmaI/netI    0.2104
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76232
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.7457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            'burgundy red'
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.000156(10)
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         16757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+15.0000+0.0000*P+(0.0500P)^2^+0.0000sin\q/\l]
 where P = 0.33330Fo^2^ + 0.66670Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                7111
_reflns_number_total             16757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066273xsi20060829_022504.cif
_cod_data_source_block           p21_c_2
_cod_original_formula_sum        'C86.40 H76.80 Co1.60 Fe2.40 N19.20'
_cod_database_code               4109405