Charge transfer phase transition with reversed thermal hysteresis loop in the mixed-valence Fe9[W(CN)8]6.xMeOH cluster
Szymon Chorazy; Robert Podgajny; Wojciech Nogas; Wojciech Nitek; Marcin Koziel; Michal Rams; Ewa Juszynska-Galazka; Jan Zukrowski; Czeslaw Kapusta; Koji Nakabayashi; Takashi Fujimoto; Shin-ichi Ohkoshi; Barbara Sieklucka; Chem.Commun. 50 (2014) 3484–; doi:10.1039/C3CC48029A

data_7112107
_publ_section_title
;
 Charge transfer phase transition with reversed thermal hysteresis loop in
 the mixed-valence Fe9[W(CN)8]6.xMeOH cluster
;
_journal_name_full               Chem.Commun.
_journal_page_first              3484
_journal_paper_doi               10.1039/C3CC48029A
_journal_volume                  50
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C80 H40 Fe9 N48 O34 W6'
_chemical_formula_sum            'C84.5 H145.5 Fe9 N48 O36.5 W6'
_chemical_formula_weight         4024.01
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-11-28T21:59:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 113.6570(11)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   28.8360(5)
_cell_length_b                   19.5840(5)
_cell_length_c                   32.8010(5)
_cell_measurement_reflns_used    170635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     16966.9(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0365911
_diffrn_orient_matrix_UB_12      -0.0010691
_diffrn_orient_matrix_UB_13      0.0207098
_diffrn_orient_matrix_UB_21      0.0075367
_diffrn_orient_matrix_UB_22      0.0352644
_diffrn_orient_matrix_UB_23      -0.0185389
_diffrn_orient_matrix_UB_31      -0.00614
_diffrn_orient_matrix_UB_32      0.0369151
_diffrn_orient_matrix_UB_33      0.0183097
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1347
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            180401
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         30.037
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.86
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7612
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.006
_refine_diff_density_min         -2.65
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       0.000008(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         24774
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+4.1628P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                17790
_reflns_number_total             24774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48029a.txt
_cod_data_source_block           1_HT
_cod_original_cell_volume        16967.0(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7112107
_shelx_estimated_absorpt_t_min   0.323
_shelx_estimated_absorpt_t_max   0.475