Thermal decomposition of [Co(en)3][Fe(CN)6].2H2O: Topotactic dehydration process, valence and spin exchange mechanism elucidation
Zdenek Travnicek; Radek Zboril; Miroslava Matikova-Malarova; Bohuslav Drahos; Juraj Cernak; Chemistry Central Journal 7 (2013) 28–; doi:10.1186/1752-153X-7-28

data_1547208
_publ_section_title
;
 Thermal decomposition of [Co(en)3][Fe(CN)6].2H2O: Topotactic dehydration
 process, valence and spin exchange mechanism elucidation
;
_journal_name_full               'Chemistry Central Journal'
_journal_page_first              28
_journal_paper_doi               10.1186/1752-153X-7-28
_journal_volume                  7
_journal_year                    2013
_chemical_formula_sum            'C24 H50 Co2 Fe2 N24 O'
_chemical_formula_weight         920.44
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1603(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.0448(3)
_cell_length_b                   8.4631(2)
_cell_length_c                   14.9812(3)
_cell_measurement_reflns_used    9208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.97
_cell_measurement_theta_min      2.70
_cell_volume                     1907.48(7)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9451
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.6820
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3348
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0596P)^2^+0.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                2960
_reflns_number_total             3348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            13065_2012_594_MOESM3_ESM.cif
_cod_data_source_block           r
_cod_database_code               1547208