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_4344934
_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         'C8 H16 N8 Ni2 O8 W'
_chemical_formula_sum            'C8 H16 N8 Ni2 O8 W'
_chemical_formula_weight         653.56
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      87
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/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             2016-06-02T22:45:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6752(6)
_cell_length_b                   11.6752(6)
_cell_length_c                   12.8954(4)
_cell_measurement_reflns_used    8624
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.445
_cell_measurement_theta_min      3.160
_cell_measurement_wavelength     0.71075
_cell_volume                     1757.78(14)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0158
_diffrn_reflns_av_unetI/netI     0.0082
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8624
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.445
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.706
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.47
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.651
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.464
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1054
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.469
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0194
_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^)+8.8248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0332
_reflns_Friedel_coverage         0
_reflns_number_gt                1047
_reflns_number_total             1054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01883_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1757.78(19)
_cod_database_code               4344934
_shelx_estimated_absorpt_t_min   0.397
_shelx_estimated_absorpt_t_max   0.448