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_4109407
_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                 97.255(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.485(14)
_cell_length_b                   25.326(18)
_cell_length_c                   25.145(20)
_cell_measurement_reflns_used    107
_cell_measurement_temperature    298(2)
_cell_volume                     12309(16)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.2009
_diffrn_reflns_av_sigmaI/netI    0.4926
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47425
_diffrn_reflns_theta_full        23.47
_diffrn_reflns_theta_max         23.47
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.9077
_exptl_absorpt_correction_T_min  0.7472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            'burgundy red'
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.685
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         17339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.685
_refine_ls_R_factor_all          0.2575
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_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+(0.0000P)^2^+0.0000sin\q/\l] 
 where P = 0.33330Fo^2^ + 0.66670Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.3095
_reflns_number_gt                4819
_reflns_number_total             17339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066273xsi20060829_022531.cif
_cod_data_source_block           z:\x-ray\ms117\work\final\p21_c
_cod_database_code               4109407