Mixed-Valence Cobalt(II/III)‒Octacyanidotungstate(IV/V) Ferromagnet
Komori-Orisaku, Keiko; Imoto, Kenta; Koide, Yoshihiro; Ohkoshi, Shin-ichi; Crystal Growth & Design 13 (2013) 5267–; doi:10.1021/cg401011d

data_4508451
_publ_section_title
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 Mixed-Valence Cobalt(II/III)--Octacyanidotungstate(IV/V) Ferromagnet
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_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5267
_journal_paper_doi               10.1021/cg401011d
_journal_volume                  13
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C30 H22 Co3 N18 O4 W2, 3H2O'
_chemical_formula_sum            'C30 H28 Co3 N18 O7 W2'
_chemical_formula_weight         1297.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.042(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2123(5)
_cell_length_b                   24.0547(18)
_cell_length_c                   11.7186(8)
_cell_measurement_reflns_used    23583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.32
_cell_measurement_theta_min      1.83
_cell_volume                     2033.1(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'SV (Nemoto & Ohashi, 1993)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       omega_scan
_diffrn_radiation_monochromator  Si
_diffrn_radiation_source         'SPring-8 BL38B1 '
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75000
_diffrn_reflns_av_R_equivalents  0.1808
_diffrn_reflns_av_sigmaI/netI    0.1536
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46930
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         35.67
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    6.903
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.120
_refine_diff_density_min         -5.316
_refine_diff_density_rms         0.414
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5863 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_extinction_coef       0.0073(7)
_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   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         14024
_refine_ls_number_restraints     407
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1393
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2858
_reflns_number_gt                8634
_reflns_number_total             14024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401011d_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4508451