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_7112108
_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_formula_moiety         'C72 H72 Fe9 N48 O24 W6'
_chemical_formula_sum            'C90 H168 Fe9 N48 O42 W6'
_chemical_formula_weight         4200.24
_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             2013-11-28T21:18:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.6570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3480(4)
_cell_length_b                   19.0770(3)
_cell_length_c                   32.3450(5)
_cell_measurement_reflns_used    89741
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     16022.0(4)
_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 (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0219031
_diffrn_orient_matrix_UB_12      0.0411763
_diffrn_orient_matrix_UB_13      0.0001638
_diffrn_orient_matrix_UB_21      -0.0315444
_diffrn_orient_matrix_UB_22      0.0297715
_diffrn_orient_matrix_UB_23      -0.013589
_diffrn_orient_matrix_UB_31      0.002892
_diffrn_orient_matrix_UB_32      0.0128762
_diffrn_orient_matrix_UB_33      0.030896
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            57634
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         1.325
_exptl_absorpt_coefficient_mu    5.153
_exptl_absorpt_correction_T_max  0.4573
_exptl_absorpt_correction_T_min  0.3070
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8004
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.284
_refine_diff_density_min         -3.839
_refine_diff_density_rms         0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    307.679
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         18205
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+162.8645P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1747
_reflns_number_gt                14691
_reflns_number_total             18205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48029a.txt
_cod_data_source_block           1_LT
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7112108