#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:37:31 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185292 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/49/7224903.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_7224903
loop_
_publ_author_name
'Wang, Zhi'
'Jagličić, Zvonko'
'Han, Lu-Lu'
'Zhuang, Gui-Lin'
'Luo, Geng-Geng'
'Zeng, Su-Yuan'
'Tung, Chen-Ho'
'Sun, Di'
_publ_section_title
;
 Octanuclear Ni(ii) cubes based on halogen-substituted pyrazolates:
 synthesis, structure, electrochemistry and magnetism
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3462
_journal_paper_doi               10.1039/C6CE00528D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C56 H78 Cl12 N28 Ni8 O6'
_chemical_formula_weight         2134.54
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.786(2)
_cell_length_b                   11.786
_cell_length_c                   29.019(6)
_cell_measurement_temperature    298(2)
_cell_volume                     4031.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18247
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1816
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+8.7494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                1457
_reflns_number_total             1816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00528d2.cif
_cod_data_source_block           p1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7224903--7224905.cif.
;
_cod_original_cell_volume        4031.3(12)
_cod_database_code               7224903
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-x-1/2, y-1/2, z-1/2'
'x, y, -z'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.56571(4) 0.33240(4) 0.448656(15) 0.02424(17) Uani 1 1 d .
Cl1 Cl 0.95919(12) 0.30839(14) 0.32305(6) 0.0857(5) Uani 1 1 d .
Cl2 Cl 0.74362(15) -0.11603(12) 0.5000 0.0551(5) Uani 1 2 d S
O1 O 0.6556(3) 0.4310(3) 0.5000 0.0243(8) Uani 1 2 d S
H1 H 0.714(5) 0.409(4) 0.5000 0.021(16) Uiso 1 2 d S
O2 O 0.5000 0.5000 0.43078(17) 0.0266(11) Uani 1 4 d S
H2 H 0.5000 0.5000 0.4076 0.032 Uiso 1 4 d SR
N1 N 0.6981(3) 0.3503(3) 0.40368(10) 0.0312(7) Uani 1 1 d .
N2 N 0.7414(3) 0.4574(3) 0.40338(11) 0.0319(7) Uani 1 1 d .
N3 N 0.6190(3) 0.1840(2) 0.47668(10) 0.0313(7) Uani 1 1 d .
C1 C 0.7648(4) 0.2859(4) 0.37664(14) 0.0423(10) Uani 1 1 d .
H1A H 0.7543 0.2090 0.3707 0.051 Uiso 1 1 calc R
C2 C 0.8500(3) 0.3509(4) 0.35931(16) 0.0438(11) Uani 1 1 d .
C3 C 0.8329(3) 0.4580(4) 0.37625(14) 0.0407(10) Uani 1 1 d .
H3 H 0.8778 0.5209 0.3699 0.049 Uiso 1 1 calc R
C4 C 0.6586(3) 0.0835(3) 0.46224(15) 0.0377(9) Uani 1 1 d .
H4 H 0.6671 0.0617 0.4316 0.045 Uiso 1 1 calc R
C5 C 0.6847(5) 0.0181(4) 0.5000 0.0350(13) Uani 1 2 d S
N5 N 0.5000 0.5000 0.2739(5) 0.159(4) Uani 1 4 d SU
H5 H 0.5000 0.5000 0.2438 0.191 Uiso 1 4 d SR
C8 C 0.373(2) 0.536(2) 0.2814(6) 0.162(4) Uani 0.50 1 d PU
H8A H 0.3477 0.5229 0.3124 0.195 Uiso 0.50 1 d PR
H8B H 0.3229 0.5002 0.2598 0.195 Uiso 0.50 1 d PR
C8A C 0.435(3) 0.586(2) 0.3024(6) 0.166(4) Uani 0.50 1 d PU
H8AA H 0.4864 0.6195 0.3242 0.199 Uiso 0.50 1 d PR
H8C H 0.3742 0.5507 0.3189 0.199 Uiso 0.50 1 d PR
C9 C 0.3887(10) 0.6823(10) 0.2706(3) 0.173(4) Uani 1 1 d U
H9B H 0.3185 0.7231 0.2732 0.260 Uiso 1 1 d R
H8AB H 0.4425 0.7126 0.2922 0.260 Uiso 1 1 d R
H9A H 0.4179 0.6901 0.2399 0.260 Uiso 1 1 d R
N4 N 0.5000 0.5000 0.1728(5) 0.108(4) Uani 1 4 d S
C6 C 0.5000 0.5000 0.1334(5) 0.085(4) Uani 1 4 d S
C7 C 0.5000 0.5000 0.0842(5) 0.128(6) Uani 1 4 d S
H7A H 0.4235 0.4858 0.0745 0.153 Uiso 0.25 1 d PR
H7C H 0.5463 0.4407 0.0715 0.153 Uiso 0.25 1 d PR
H7B H 0.5218 0.5720 0.0715 0.153 Uiso 0.25 1 d PR
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
N2 Ni1 N3 94.88(12) 7_565 .
N2 Ni1 N1 96.38(12) 7_565 .
N3 Ni1 N1 96.22(12) . .
N2 Ni1 O1 169.60(13) 7_565 .
N3 Ni1 O1 92.02(12) . .
N1 Ni1 O1 90.59(12) . .
N2 Ni1 O1 90.68(12) 7_565 10_566
N3 Ni1 O1 90.42(12) . 10_566
N1 Ni1 O1 169.85(13) . 10_566
O1 Ni1 O1 81.48(15) . 10_566
N2 Ni1 O2 90.61(12) 7_565 .
N3 Ni1 O2 169.98(15) . .
N1 Ni1 O2 91.48(12) . .
O1 Ni1 O2 81.48(13) . .
O1 Ni1 O2 81.12(13) 10_566 .
N2 Ni1 Ni1 130.38(9) 7_565 12_556
N3 Ni1 Ni1 66.37(9) . 12_556
N1 Ni1 Ni1 129.65(9) . 12_556
O1 Ni1 Ni1 46.55(6) . 12_556
O1 Ni1 Ni1 46.94(6) 10_566 12_556
O2 Ni1 Ni1 103.74(12) . 12_556
Ni1 O1 Ni1 86.91(12) . 12_556
Ni1 O1 Ni1 87.27(5) . 2_655
Ni1 O1 Ni1 153.06(19) 12_556 2_655
Ni1 O1 Ni1 153.06(19) . 15_656
Ni1 O1 Ni1 87.27(5) 12_556 15_656
Ni1 O1 Ni1 86.12(12) 2_655 15_656
Ni1 O2 Ni1 86.77(6) 7_565 4_665
Ni1 O2 Ni1 86.77(6) 7_565 .
Ni1 O2 Ni1 152.5(2) 4_665 .
Ni1 O2 Ni1 152.5(2) 7_565 2_655
Ni1 O2 Ni1 86.77(6) 4_665 2_655
Ni1 O2 Ni1 86.77(6) . 2_655
C1 N1 N2 107.5(3) . .
C1 N1 Ni1 139.5(3) . .
N2 N1 Ni1 112.7(2) . .
C3 N2 N1 108.1(3) . .
C3 N2 Ni1 136.5(3) . 2_655
N1 N2 Ni1 114.8(2) . 2_655
C4 N3 N3 108.2(2) . 12_556
C4 N3 Ni1 138.1(3) . .
N3 N3 Ni1 113.63(9) 12_556 .
N1 C1 C2 109.2(4) . .
C1 C2 C3 106.1(4) . .
C1 C2 Cl1 127.5(3) . .
C3 C2 Cl1 126.3(3) . .
N2 C3 C2 109.0(4) . .
N3 C4 C5 108.9(4) . .
C4 C5 C4 105.7(5) 12_556 .
C4 C5 Cl2 127.1(2) 12_556 .
C4 C5 Cl2 127.1(2) . .
C8A N5 C8A 72.7(8) 2_655 .
C8A N5 C8A 114.0(17) 2_655 7_565
C8A N5 C8A 72.7(8) . 7_565
C8A N5 C8A 72.7(8) 2_655 4_665
C8A N5 C8A 114.0(17) . 4_665
C8A N5 C8A 72.7(8) 7_565 4_665
C8A N5 C8 115.2(15) . 2_655
C8A N5 C8 125.9(15) 7_565 2_655
C8A N5 C8 54.8(14) 4_665 2_655
C8A N5 C8 125.9(15) 2_655 7_565
C8A N5 C8 54.8(14) . 7_565
C8A N5 C8 115.2(15) 4_665 7_565
C8 N5 C8 164.1(19) 2_655 7_565
C8A N5 C8 54.8(14) 2_655 .
C8A N5 C8 115.2(15) 7_565 .
C8A N5 C8 125.9(15) 4_665 .
C8 N5 C8 88.9(3) 2_655 .
C8 N5 C8 88.9(3) 7_565 .
C8A N5 C8 115.2(15) 2_655 4_665
C8A N5 C8 125.9(15) . 4_665
C8A N5 C8 54.8(14) 7_565 4_665
C8 N5 C8 88.9(3) 2_655 4_665
C8 N5 C8 88.9(3) 7_565 4_665
C8 N5 C8 164.1(19) . 4_665
C8A C8 C8A 89(2) . 2_655
C8A C8 N5 65.8(18) . .
C8A C8 N5 60.4(15) 2_655 .
C8A C8 C9 61.0(15) . .
C8A C8 C9 149.1(19) 2_655 .
N5 C8 C9 98.0(13) . .
C8A C8 C9 143(2) . 2_655
C8A C8 C9 54.2(10) 2_655 2_655
N5 C8 C9 93.1(13) . 2_655
C9 C8 C9 155.6(14) . 2_655
C8 C8A C8 120(3) . 7_565
C8 C8A N5 71.7(18) . .
C8 C8A N5 64.8(14) 7_565 .
C8 C8A C9 80(2) . .
C8 C8A C9 78.1(19) 7_565 .
N5 C8A C9 110.0(13) . .
C8 C8A C8A 52(2) . 2_655
C8 C8A C8A 117.1(15) 7_565 2_655
N5 C8A C8A 53.6(4) . 2_655
C9 C8A C8A 132(2) . 2_655
C8 C8A C8A 125.3(19) . 7_565
N5 C8A C8A 53.6(4) . 7_565
C9 C8A C8A 117(3) . 7_565
C8A C8A C8A 90.000(8) 2_655 7_565
C8A C9 C8 47.6(14) . 7_565
C8 C9 C8 74.5(15) . 7_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.028(3) 7_565
Ni1 N3 2.029(3) .
Ni1 N1 2.045(3) .
Ni1 O1 2.166(2) .
Ni1 O1 2.182(2) 10_566
Ni1 O2 2.1842(12) .
Ni1 Ni1 2.9799(11) 12_556
Cl1 C2 1.736(4) .
Cl2 C5 1.726(5) .
O1 Ni1 2.166(2) 12_556
O1 Ni1 2.182(2) 2_655
O1 Ni1 2.182(2) 15_656
O2 Ni1 2.1842(13) 7_565
O2 Ni1 2.1842(12) 4_665
O2 Ni1 2.1842(13) 2_655
N1 C1 1.345(5) .
N1 N2 1.361(4) .
N2 C3 1.336(5) .
N2 Ni1 2.028(3) 2_655
N3 C4 1.340(5) .
N3 N3 1.353(6) 12_556
C1 C2 1.359(6) .
C2 C3 1.370(6) .
C4 C5 1.375(5) .
C5 C4 1.375(5) 12_556
N5 C8A 1.51(2) 2_655
N5 C8A 1.51(2) .
N5 C8A 1.51(2) 7_565
N5 C8A 1.51(2) 4_665
N5 C8 1.58(2) 2_655
N5 C8 1.58(2) 7_565
N5 C8 1.58(2) .
N5 C8 1.58(2) 4_665
C8 C8A 1.12(3) .
C8 C8A 1.42(3) 2_655
C8 C9 1.76(3) .
C8 C9 1.88(3) 2_655
C8A C8 1.42(3) 7_565
C8A C9 1.562(19) .
C8A C8A 1.79(3) 2_655
C8A C8A 1.79(3) 7_565
C9 C8 1.88(3) 7_565
N4 C6 1.143(15) .
C6 C7 1.429(19) .
