#------------------------------------------------------------------------------
#$Date: 2017-01-01 03:27:10 +0200 (Sun, 01 Jan 2017) $
#$Revision: 189533 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/49/4344935.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4344935
loop_
_publ_author_name
'Reczyński, Mateusz'
'Chorazy, Szymon'
'Nowicka, Beata'
'Sieklucka, Barbara'
'Ohkoshi, Shin-Ichi'
_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       ω
_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/[σ²(Fo²)+(0.0170P)²+61.6213P] where P=(Fo²+2Fc²)/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 > 2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'-x, y, z+1/2'
'y, x, z+1/2'
'x, -y, z+1/2'
'-y, -x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'-y+1/2, -x+1/2, z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'x, -y, -z-1/2'
'-y, -x, -z-1/2'
'-x, y, -z-1/2'
'y, x, -z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, y+1/2, -z'
'y+1/2, x+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0 0 0.25 0.0142(2) Uani 1 8 d S T P
Ni1 Ni 0.31684(13) 0.18316(13) 0.5 0.0174(4) Uani 1 4 d S T P
N1 N 0.2248(6) 0.1039(6) 0.3977(4) 0.0206(13) Uani 1 1 d . . .
C1 C 0.1487(7) 0.0656(6) 0.3435(5) 0.0176(14) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 W1 C1 145.0(4) . 22_556
C1 W1 C1 140.8(4) . 23_556
C1 W1 C1 72.01(17) 22_556 23_556
C1 W1 C1 72.01(17) . 2
C1 W1 C1 140.8(4) 22_556 2
C1 W1 C1 78.4(3) 23_556 2
C1 W1 C1 78.4(3) . 24_556
C1 W1 C1 112.5(3) 22_556 24_556
C1 W1 C1 72.01(17) 23_556 24_556
C1 W1 C1 81.0(4) 2 24_556
C1 W1 C1 112.5(3) . 3
C1 W1 C1 78.4(3) 22_556 3
C1 W1 C1 81.0(4) 23_556 3
C1 W1 C1 72.01(17) 2 3
C1 W1 C1 145.0(4) 24_556 3
C1 W1 C1 81.0(4) . 21_556
C1 W1 C1 72.01(17) 22_556 21_556
C1 W1 C1 112.5(3) 23_556 21_556
C1 W1 C1 145.0(4) 2 21_556
C1 W1 C1 72.01(17) 24_556 21_556
C1 W1 C1 140.8(4) 3 21_556
C1 W1 C1 72.01(17) . 4
C1 W1 C1 81.0(4) 22_556 4
C1 W1 C1 145.0(4) 23_556 4
C1 W1 C1 112.5(3) 2 4
C1 W1 C1 140.8(4) 24_556 4
C1 W1 C1 72.01(17) 3 4
C1 W1 C1 78.4(3) 21_556 4
N1 Ni1 N1 88.8(3) 30_556 16_554
N1 Ni1 N1 90.9(3) 30_556 19_556
N1 Ni1 N1 173.9(4) 16_554 19_556
N1 Ni1 N1 173.9(4) 30_556 .
N1 Ni1 N1 90.9(3) 16_554 .
N1 Ni1 N1 88.8(3) 19_556 .
C1 N1 Ni1 166.8(6) . .
N1 C1 W1 176.3(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C1 2.141(7) .
W1 C1 2.141(7) 22_556
W1 C1 2.141(7) 23_556
W1 C1 2.141(7) 2
W1 C1 2.141(7) 24_556
W1 C1 2.141(7) 3
W1 C1 2.141(7) 21_556
W1 C1 2.141(7) 4
Ni1 N1 1.861(6) 30_556
Ni1 N1 1.861(6) 16_554
Ni1 N1 1.861(6) 19_556
Ni1 N1 1.861(6) .
N1 C1 1.160(9) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N1 Ni1 N1 C1 -116(2) 16_554
N1 Ni1 N1 C1 58(3) 19_556
