Dehydration of Octacyanido-Bridged Ni(II)-W(IV) Framework toward Negative Thermal Expansion and Magneto-Colorimetric Switching.
Reczyński, Mateusz; Chorazy, Szymon; Nowicka, Beata; Sieklucka, Barbara; Ohkoshi, Shin-Ichi; Inorganic chemistry  (2016) –; doi:10.1021/acs.inorgchem.6b01883

data_4344935
_publ_section_title
;
 Dehydration of Octacyanido-Bridged Ni(II)-W(IV) Framework toward Negative
 Thermal Expansion and Magneto-Colorimetric Switching.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b01883
_journal_year                    2016
_chemical_formula_moiety         'C4 N4 Ni W0.50'
_chemical_formula_sum            'C4 N4 Ni W0.5'
_chemical_formula_weight         254.72
_space_group_IT_number           140
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      140
_symmetry_space_group_name_Hall  '-I 4 2c'
_symmetry_space_group_name_H-M   'I 4/m c m'
_atom_sites_solution_hydrogens   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2016-05-31T15:32:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9485(13)
_cell_length_b                   10.9485(13)
_cell_length_c                   12.7277(9)
_cell_measurement_reflns_used    6588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.325
_cell_measurement_theta_min      3.201
_cell_measurement_wavelength     0.71075
_cell_volume                     1525.7(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6588
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.325
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.96
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.062
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     25
_refine_ls_number_reflns         489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.04
_refine_ls_R_factor_gt           0.04
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+61.6213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0
_reflns_number_gt                489
_reflns_number_total             489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01883_si_003.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1525.7(4)
_cod_original_formula_sum        'C4 N4 Ni W0.50'
_cod_database_code               4344935
_shelx_estimated_absorpt_t_min   0.358
_shelx_estimated_absorpt_t_max   0.407