Solvent-induced on/off switching of intramolecular electron transfer in a cyanide-bridged trigonal bipyramidal complex.
Wei, Rong-Jia; Nakahara, Ryohei; Cameron, Jamie M.; Newton, Graham N.; Shiga, Takuya; Sagayama, Hajime; Kumai, Reiji; Murakami, Youichi; Oshio, Hiroki; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17104–17107; doi:10.1039/c6dt03416k

data_7040969
_publ_section_title
;
 Solvent-induced on/off switching of intramolecular electron transfer in a
 cyanide-bridged trigonal bipyramidal complex.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17104
_journal_page_last               17107
_journal_paper_doi               10.1039/c6dt03416k
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_sum            'C126 H145 Cl Co3 Fe2 N25 O9'
_chemical_formula_weight         2477.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.991(9)
_cell_length_b                   18.555(10)
_cell_length_c                   38.04(2)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.92
_cell_measurement_theta_min      2.20
_cell_volume                     11993(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.1613
_diffrn_reflns_av_sigmaI/netI    0.1410
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            111656
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.8098
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
    Approximately 12.5 % of the unit cell volume comprises a large region of disordered solvent that could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 497.4 electrons per unit cell which were assigned to 5 EtOH molecules per cluster. 
;
_refine_diff_density_max         0.785
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         21113
_refine_ls_number_restraints     1575
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.1655
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1937P)^2^+179.7088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4035
_refine_ls_wR_factor_ref         0.4256
_reflns_number_gt                13143
_reflns_number_total             21113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03416k2.cif
_cod_data_source_block           1de
_cod_depositor_comments
'Adding full bibliography for 7040967--7040969.cif.'
_cod_database_code               7040969