Thermochromic and Photoresponsive Cyanometalate Fe/Co Squares: Toward Control of the Electron Transfer Temperature.
Zhang, Yuan-Zhu; Ferko, Philip; Siretanu, Diana; Ababei, Rodica; Rath, Nigam P.; Shaw, Michael J.; Clérac, Rodolphe; Mathonière, Corine; Holmes, Stephen M.; Journal of the American Chemical Society  (2014) 141119160917008–; doi:10.1021/ja508280n

data_4122955
_publ_section_title
;
 Thermochromic and Photoresponsive Cyanometalate Fe/Co Squares: Toward
 Control of the Electron Transfer Temperature.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141119160917008
_journal_paper_doi               10.1021/ja508280n
_journal_year                    2014
_chemical_formula_moiety         '2(C15 H16 B Fe N9), 2(C8 H20 N), 9(H2 O)'
_chemical_formula_sum            'C46 H90 B2 Fe2 N20 O9'
_chemical_formula_weight         1200.69
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.3752(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.71650(10)
_cell_length_b                   17.1804(2)
_cell_length_c                   18.7380(3)
_cell_measurement_temperature    120(2)
_cell_volume                     3122.57(7)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'Diamond 2.0'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44771
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7151
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+3.9224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5590
_reflns_number_total             7151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508280n_si_001.cif
_cod_data_source_block           k09027
_cod_database_code               4122955
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2014-3
_shelx_res_checksum              62148
_shelx_hkl_checksum              90266