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_4109401
_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 Cr2 N24 Zn3'
_chemical_formula_weight         2030.20
_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                 97.498(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.420(3)
_cell_length_b                   25.613(4)
_cell_length_c                   24.874(4)
_cell_measurement_reflns_used    174
_cell_measurement_temperature    150(2)
_cell_volume                     12267(3)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX 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  0.1471
_diffrn_reflns_av_sigmaI/netI    0.2154
_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       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75346
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.5034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       needle
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.97
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         17615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0630
_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^)+10.0000+0.0000*P+(0.0280P)^2^+0.0000sin\q/\l] 
 where P = 0.33330Fo^2^ + 0.66670Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                7315
_reflns_number_total             17615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066273xsi20060829_022413.cif
_cod_data_source_block           c:\structures\mike\ms093\work\p21_c
_cod_database_code               4109401