#------------------------------------------------------------------------------
#$Date: 2021-03-03 10:49:53 +0200 (Wed, 03 Mar 2021) $
#$Revision: 262385 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/07/1560778.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_1560778
loop_
_publ_author_name
'Belal Ahmed'
'Hongil Jo'
'Sung Won Yoon'
'Kwang Yong Choi'
'Kang Min Ok'
_publ_section_title
;
 A series of oxyfluoride chains containing asymmetric basic building units
 of both early- and late-transition metal cations
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              140
_journal_page_last               145
_journal_paper_doi               10.1016/j.jssc.2018.08.021
_journal_volume                  267
_journal_year                    2018
_chemical_formula_moiety         'C12 H16 F4 N8 Ni O2 W'
_chemical_formula_sum            'C12 H16 F4 N8 Ni O2 W'
_chemical_formula_weight         622.89
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.61(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.239(3)
_cell_length_b                   12.290(3)
_cell_length_c                   15.440(4)
_cell_measurement_reflns_used    6407
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.6
_cell_measurement_wavelength     0.71073
_cell_volume                     1930.0(9)
_computing_cell_refinement       'SAINT V7.68A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'Bruker APEX2 software'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.011479
_diffrn_orient_matrix_UB_12      0.00521
_diffrn_orient_matrix_UB_13      0.06512
_diffrn_orient_matrix_UB_21      0.109088
_diffrn_orient_matrix_UB_22      0.084522
_diffrn_orient_matrix_UB_23      0.001578
_diffrn_orient_matrix_UB_31      -0.065315
_diffrn_orient_matrix_UB_32      0.095436
_diffrn_orient_matrix_UB_33      0.00279
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20100
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         2.599
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    6.994
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.724
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00489(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0303
_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)+(0.0303P)²+7.8817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.069
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0
_reflns_number_gt                1936
_reflns_number_total             2401
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2018-267-140.cif
_cod_data_source_block           4
_cod_original_cell_volume        1929.9(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1560778
_shelx_estimated_absorpt_t_min   0.33
_shelx_estimated_absorpt_t_max   0.359
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.25 0.75 0 0.0394(2) Uani 1 2 d S . P . .
W1 W 0 0.5 0 0.05148(14) Uani 1 2 d S . P . .
C1 C 0.2781(7) 0.8593(6) 0.2597(4) 0.079(2) Uani 1 1 d . . . . .
H1 H 0.31803 0.903943 0.303586 0.095 Uiso 1 1 calc R U . . .
C2 C 0.1887(7) 0.7825(7) 0.2688(4) 0.082(2) Uani 1 1 d . . . . .
H2 H 0.153961 0.76363 0.319761 0.099 Uiso 1 1 calc R U . . .
C3 C 0.1575(5) 0.7358(5) 0.1855(3) 0.0581(13) Uani 1 1 d . . . . .
H3 H 0.098374 0.679165 0.171996 0.07 Uiso 1 1 calc R U . . .
C4 C 0.5096(6) 0.5152(4) 0.1223(4) 0.0588(14) Uani 1 1 d . . . . .
H4 H 0.525306 0.449628 0.151808 0.071 Uiso 1 1 calc R U . . .
C5 C 0.5972(6) 0.5919(5) 0.1097(5) 0.085(2) Uani 1 1 d . . . . .
H5 H 0.687037 0.590289 0.127857 0.102 Uiso 1 1 calc R U . . .
C6 C 0.5288(5) 0.6736(4) 0.0647(4) 0.0627(15) Uani 1 1 d . . . . .
H6 H 0.566525 0.73754 0.047178 0.075 Uiso 1 1 calc R U . . .
N1 N 0.2263(4) 0.7859(3) 0.1299(2) 0.0444(9) Uani 1 1 d . . . . .
N2 N 0.2996(4) 0.8603(4) 0.1767(3) 0.0584(11) Uani 1 1 d . . . . .
H2A H 0.353965 0.903427 0.155496 0.07 Uiso 1 1 calc R U . . .
N3 N 0.4040(4) 0.6506(3) 0.0493(2) 0.0415(8) Uani 1 1 d . . . . .
N4 N 0.3928(4) 0.5524(3) 0.0833(3) 0.0599(11) Uani 1 1 d . . . . .
H4A H 0.320217 0.516644 0.080821 0.072 Uiso 1 1 calc R U . . .
O1 O -0.0169(4) 0.5212(3) 0.1167(2) 0.0677(14) Uani 0.65(5) 1 d . . P . .
O2 O 0.1424(3) 0.4074(3) 0.0307(2) 0.0750(15) Uani 0.35(5) 1 d . . P . .
F1 F -0.0169(4) 0.5212(3) 0.1167(2) 0.0677(14) Uani 0.35(5) 1 d . . P . .
F2 F 0.1424(3) 0.4074(3) 0.0307(2) 0.0750(15) Uani 0.65(5) 1 d . . P . .
F3 F 0.1188(3) 0.6207(2) 0.00257(17) 0.0576(7) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0513(5) 0.0352(4) 0.0301(4) 0.0005(3) -0.0017(3) 0.0168(3)
W1 0.03646(17) 0.03033(15) 0.0841(3) 0.01293(12) -0.00813(12) -0.01109(10)
C1 0.069(4) 0.123(6) 0.042(3) -0.028(3) -0.009(3) 0.033(4)
C2 0.089(5) 0.123(6) 0.039(3) 0.017(3) 0.020(3) 0.042(4)
C3 0.060(3) 0.064(3) 0.052(3) 0.016(2) 0.011(2) 0.015(2)
C4 0.068(4) 0.047(3) 0.058(3) 0.015(2) -0.006(3) 0.022(2)
C5 0.042(3) 0.056(3) 0.147(6) -0.015(4) -0.026(3) 0.009(3)
C6 0.041(3) 0.030(2) 0.116(5) 0.011(3) 0.010(3) 0.0015(19)
N1 0.056(2) 0.0424(19) 0.0339(18) -0.0027(15) 0.0003(16) 0.0183(17)
N2 0.058(3) 0.067(3) 0.049(2) -0.013(2) -0.0030(19) 0.011(2)
N3 0.050(2) 0.0326(17) 0.0402(19) 0.0028(14) -0.0024(16) 0.0105(15)
N4 0.047(2) 0.047(2) 0.086(3) 0.017(2) 0.008(2) 0.0022(18)
O1 0.078(3) 0.077(3) 0.048(2) 0.0045(16) 0.0071(17) 0.0008(19)
O2 0.068(2) 0.074(2) 0.083(3) 0.0232(19) 0.0068(18) 0.0376(18)
F1 0.078(3) 0.077(3) 0.048(2) 0.0045(16) 0.0071(17) 0.0008(19)
F2 0.068(2) 0.074(2) 0.083(3) 0.0232(19) 0.0068(18) 0.0376(18)
F3 0.0636(19) 0.0515(17) 0.0557(16) 0.0085(13) -0.0012(14) 0.0068(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N3 Ni1 N3 180 . 7_565
N3 Ni1 F3 89.52(13) . 7_565
N3 Ni1 F3 90.48(13) 7_565 7_565
N3 Ni1 F3 90.48(13) . .
N3 Ni1 F3 89.52(13) 7_565 .
F3 Ni1 F3 180 7_565 .
N3 Ni1 N1 86.53(14) . .
N3 Ni1 N1 93.47(14) 7_565 .
F3 Ni1 N1 90.21(14) 7_565 .
F3 Ni1 N1 89.79(14) . .
N3 Ni1 N1 93.47(14) . 7_565
N3 Ni1 N1 86.53(14) 7_565 7_565
F3 Ni1 N1 89.79(14) 7_565 7_565
F3 Ni1 N1 90.21(14) . 7_565
N1 Ni1 N1 180 . 7_565
O1 W1 O1 180 . 5_565
O1 W1 O2 90.20(17) . 5_565
O1 W1 O2 89.80(17) 5_565 5_565
O1 W1 O2 89.80(17) . .
O1 W1 O2 90.20(17) 5_565 .
O2 W1 O2 180 5_565 .
O1 W1 F3 90.08(15) . .
O1 W1 F3 89.92(15) 5_565 .
O2 W1 F3 90.48(16) 5_565 .
O2 W1 F3 89.52(16) . .
O1 W1 F3 89.92(15) . 5_565
O1 W1 F3 90.08(15) 5_565 5_565
O2 W1 F3 89.52(16) 5_565 5_565
O2 W1 F3 90.48(16) . 5_565
F3 W1 F3 180 . 5_565
N2 C1 C2 107.6(5) . .
N2 C1 H1 126.2 . .
C2 C1 H1 126.2 . .
C1 C2 C3 106.2(5) . .
C1 C2 H2 126.9 . .
C3 C2 H2 126.9 . .
N1 C3 C2 108.6(6) . .
N1 C3 H3 125.7 . .
C2 C3 H3 125.7 . .
C5 C4 N4 105.7(4) . .
C5 C4 H4 127.1 . .
N4 C4 H4 127.1 . .
C4 C5 C6 106.2(5) . .
C4 C5 H5 126.9 . .
C6 C5 H5 126.9 . .
N3 C6 C5 111.6(5) . .
N3 C6 H6 124.2 . .
C5 C6 H6 124.2 . .
C3 N1 N2 105.9(4) . .
C3 N1 Ni1 130.7(4) . .
N2 N1 Ni1 122.7(3) . .
C1 N2 N1 111.7(5) . .
C1 N2 H2A 124.2 . .
N1 N2 H2A 124.2 . .
C6 N3 N4 104.7(4) . .
C6 N3 Ni1 128.9(3) . .
N4 N3 Ni1 125.8(3) . .
N3 N4 C4 111.7(4) . .
N3 N4 H4A 124.1 . .
C4 N4 H4A 124.1 . .
W1 F3 Ni1 177.50(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3 2.070(3) .
Ni1 N3 2.070(3) 7_565
Ni1 F3 2.084(3) 7_565
Ni1 F3 2.084(3) .
Ni1 N1 2.095(3) .
Ni1 N1 2.095(3) 7_565
W1 O1 1.849(4) .
W1 O1 1.849(4) 5_565
W1 O2 1.867(3) 5_565
W1 O2 1.867(3) .
W1 F3 1.916(3) .
W1 F3 1.916(3) 5_565
C1 N2 1.325(7) .
C1 C2 1.332(10) .
C1 H1 0.93 .
C2 C3 1.411(8) .
C2 H2 0.93 .
C3 N1 1.324(6) .
C3 H3 0.93 .
C4 C5 1.331(8) .
C4 N4 1.356(7) .
C4 H4 0.93 .
C5 C6 1.367(7) .
C5 H5 0.93 .
C6 N3 1.303(6) .
C6 H6 0.93 .
N1 N2 1.340(6) .
N2 H2A 0.86 .
N3 N4 1.326(5) .
N4 H4A 0.86 .
