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_4122958
_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(C70 H64 B2 Co2 Fe2 N26), 4(C24 H20 B), 11(C2 H3 N), H2 O'
_chemical_formula_sum            'C258 H243 B8 Co4 Fe4 N63 O'
_chemical_formula_weight         4787.74
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.612(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3435(19)
_cell_length_b                   26.718(3)
_cell_length_c                   30.650(4)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      21.80
_cell_measurement_theta_min      2.38
_cell_volume                     12524(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.1732
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            111583
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.258
_diffrn_reflns_theta_min         1.534
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2012/1'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4984
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.172
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1454
_refine_ls_number_reflns         22165
_refine_ls_number_restraints     1884
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.2063
_refine_ls_R_factor_gt           0.0943
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1435P)^2^+7.3653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2427
_refine_ls_wR_factor_ref         0.3008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9808
_reflns_number_total             22165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508280n_si_007.cif
_cod_data_source_block           wlt
_cod_database_code               4122958
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.911
_shelxl_version_number           2013-4
_shelx_res_checksum              38675
_shelx_hkl_checksum              97179