#------------------------------------------------------------------------------
#$Date: 2019-06-20 13:24:06 +0200 (jue 20 de jun de 2019) $
#$Revision: 216246 $
#$URL: svn://www.crystallography.net/cod/cif/1/55/16/1551635.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_1551635
loop_
_publ_author_name
'LIM, Jongwan'
'KIM, Gibeom'
'DO, Kyungseo'
'LEE, Seonghyun'
'RYU, Sanghoon'
'YOSHIOKA, Daisuke'
'MIKURIYA, Masahiro'
_publ_section_title
;
 Tetranuclear Nickel(II) and Cobalt(II) Complexes with
 3,5-Dimethyl-1-pyrazolylmethanolato and Acetato Bridges Having a Cubane
 Core
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              49
_journal_paper_doi               10.2116/xraystruct.31.49
_journal_volume                  31
_journal_year                    2015
_chemical_formula_moiety         'C32 H48 N8 Ni4 O12, 2(C2 H3 N)'
_chemical_formula_sum            'C36 H54 N10 Ni4 O12'
_chemical_formula_weight         1053.73
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                   11.5812(11)
_cell_length_b                   11.5812(11)
_cell_length_c                   16.580(2)
_cell_measurement_temperature    90(2)
_cell_volume                     2223.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13499
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  0.7227
_exptl_absorpt_correction_T_min  0.5816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0492P)²+0.0617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                2222
_reflns_number_total             2671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            31_49_1.txt
_cod_data_source_block           niljwe1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/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 6524 2018-11-02 12:15:13Z antanas 
;
_cod_original_sg_symbol_H-M      P4(2)/n
_cod_database_code               1551635
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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 0.245805(19) 0.390319(19) 0.193066(14) 0.01350(10) Uani 1 1 d .
O1 O 0.10438(11) 0.49282(11) 0.20042(8) 0.0174(3) Uani 1 1 d .
O2 O 0.37990(11) 0.50514(11) 0.21843(8) 0.0171(3) Uani 1 1 d .
O3 O 0.36067(12) 0.25649(10) 0.18552(8) 0.0141(3) Uani 1 1 d .
N1 N 0.28701(13) 0.39870(12) 0.07419(10) 0.0159(3) Uani 1 1 d .
N2 N 0.38701(12) 0.34025(12) 0.05889(9) 0.0159(3) Uani 1 1 d .
N3 N 0.7500 0.2500 0.13349(18) 0.0373(7) Uani 1 2 d S
C1 C 0.42634(16) 0.36262(16) -0.01563(11) 0.0186(4) Uani 1 1 d .
C2 C 0.34832(16) 0.43668(16) -0.05109(12) 0.0218(4) Uani 1 1 d .
H2A H 0.3519 0.4678 -0.1040 0.026 Uiso 1 1 calc R
C3 C 0.26284(15) 0.45673(16) 0.00680(12) 0.0180(4) Uani 1 1 d .
C4 C 0.53617(17) 0.31195(18) -0.04748(13) 0.0240(4) Uani 1 1 d .
H4A H 0.5564 0.2432 -0.0160 0.036 Uiso 0.50 1 calc PR
H4B H 0.5983 0.3691 -0.0431 0.036 Uiso 0.50 1 calc PR
H4C H 0.5257 0.2904 -0.1042 0.036 Uiso 0.50 1 calc PR
H4D H 0.5639 0.3586 -0.0929 0.036 Uiso 0.50 1 calc PR
H4E H 0.5220 0.2327 -0.0658 0.036 Uiso 0.50 1 calc PR
H4F H 0.5945 0.3114 -0.0047 0.036 Uiso 0.50 1 calc PR
C5 C 0.15721(17) 0.53014(18) 0.00184(13) 0.0264(5) Uani 1 1 d .
H5A H 0.1263 0.5427 0.0562 0.040 Uiso 0.50 1 calc PR
H5B H 0.0990 0.4913 -0.0314 0.040 Uiso 0.50 1 calc PR
H5C H 0.1769 0.6046 -0.0226 0.040 Uiso 0.50 1 calc PR
H5D H 0.1418 0.5497 -0.0547 0.040 Uiso 0.50 1 calc PR
H5E H 0.1692 0.6012 0.0329 0.040 Uiso 0.50 1 calc PR
H5F H 0.0912 0.4878 0.0241 0.040 Uiso 0.50 1 calc PR
C6 C 0.44180(16) 0.27356(15) 0.12520(12) 0.0166(4) Uani 1 1 d .
H6A H 0.4694 0.1982 0.1046 0.020 Uiso 1 1 calc R
H6B H 0.5088 0.3166 0.1469 0.020 Uiso 1 1 calc R
C7 C 0.01145(15) 0.46663(15) 0.23667(11) 0.0170(4) Uani 1 1 d .
C8 C -0.09001(17) 0.54742(17) 0.22430(13) 0.0233(4) Uani 1 1 d .
H8A H -0.1619 0.5028 0.2240 0.035 Uiso 0.50 1 calc PR
H8B H -0.0814 0.5877 0.1727 0.035 Uiso 0.50 1 calc PR
H8C H -0.0923 0.6040 0.2682 0.035 Uiso 0.50 1 calc PR
H8D H -0.0619 0.6269 0.2193 0.035 Uiso 0.50 1 calc PR
H8E H -0.1424 0.5419 0.2706 0.035 Uiso 0.50 1 calc PR
H8F H -0.1314 0.5257 0.1750 0.035 Uiso 0.50 1 calc PR
C9 C 0.7500 0.2500 0.20204(19) 0.0233(6) Uani 1 2 d S
C10 C 0.7500 0.2500 0.28994(18) 0.0255(6) Uani 1 2 d S
H10A H 0.8120 0.3002 0.3096 0.038 Uiso 0.50 1 calc PR
H10B H 0.7624 0.1712 0.3096 0.038 Uiso 0.50 1 calc PR
H10C H 0.6755 0.2786 0.3096 0.038 Uiso 0.50 1 calc 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
O1 Ni1 N1 102.73(6) . .
O1 Ni1 O3 91.64(5) . 8_656
N1 Ni1 O3 165.47(6) . 8_656
O1 Ni1 O3 166.60(5) . .
N1 Ni1 O3 79.87(5) . .
O3 Ni1 O3 86.64(6) 8_656 .
O1 Ni1 O2 102.48(5) . .
N1 Ni1 O2 89.44(6) . .
O3 Ni1 O2 85.31(5) 8_656 .
O3 Ni1 O2 90.64(5) . .
O1 Ni1 O3 90.19(5) . 2
N1 Ni1 O3 96.82(6) . 2
O3 Ni1 O3 85.13(6) 8_656 2
O3 Ni1 O3 76.43(6) . 2
O2 Ni1 O3 164.33(5) . 2
C7 O1 Ni1 125.01(12) . .
C7 O2 Ni1 127.77(12) 7_566 .
C6 O3 Ni1 126.80(12) . 7_566
C6 O3 Ni1 112.13(10) . .
Ni1 O3 Ni1 93.38(5) 7_566 .
C6 O3 Ni1 123.73(11) . 2
Ni1 O3 Ni1 91.69(5) 7_566 2
Ni1 O3 Ni1 103.15(6) . 2
C3 N1 N2 105.79(15) . .
C3 N1 Ni1 142.02(13) . .
N2 N1 Ni1 110.86(11) . .
C1 N2 N1 111.30(15) . .
C1 N2 C6 129.54(15) . .
N1 N2 C6 118.85(15) . .
N2 C1 C2 106.89(16) . .
N2 C1 C4 122.51(17) . .
C2 C1 C4 130.60(18) . .
C1 C2 C3 105.95(17) . .
C1 C2 H2A 127.0 . .
C3 C2 H2A 127.0 . .
N1 C3 C2 110.05(16) . .
N1 C3 C5 120.36(17) . .
C2 C3 C5 129.59(18) . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C1 C4 H4D 109.5 . .
H4A C4 H4D 141.1 . .
H4B C4 H4D 56.3 . .
H4C C4 H4D 56.3 . .
C1 C4 H4E 109.5 . .
H4A C4 H4E 56.3 . .
H4B C4 H4E 141.1 . .
H4C C4 H4E 56.3 . .
H4D C4 H4E 109.5 . .
C1 C4 H4F 109.5 . .
H4A C4 H4F 56.3 . .
H4B C4 H4F 56.3 . .
H4C C4 H4F 141.1 . .
H4D C4 H4F 109.5 . .
H4E C4 H4F 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C3 C5 H5D 109.5 . .
H5A C5 H5D 141.1 . .
H5B C5 H5D 56.3 . .
H5C C5 H5D 56.3 . .
C3 C5 H5E 109.5 . .
H5A C5 H5E 56.3 . .
H5B C5 H5E 141.1 . .
H5C C5 H5E 56.3 . .
H5D C5 H5E 109.5 . .
C3 C5 H5F 109.5 . .
H5A C5 H5F 56.3 . .
H5B C5 H5F 56.3 . .
H5C C5 H5F 141.1 . .
H5D C5 H5F 109.5 . .
H5E C5 H5F 109.5 . .
O3 C6 N2 108.57(14) . .
O3 C6 H6A 110.0 . .
N2 C6 H6A 110.0 . .
O3 C6 H6B 110.0 . .
N2 C6 H6B 110.0 . .
H6A C6 H6B 108.4 . .
O2 C7 O1 126.67(17) 8_656 .
O2 C7 C8 116.86(16) 8_656 .
O1 C7 C8 116.46(16) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C8 H8D 109.5 . .
H8A C8 H8D 141.1 . .
H8B C8 H8D 56.3 . .
H8C C8 H8D 56.3 . .
C7 C8 H8E 109.5 . .
H8A C8 H8E 56.3 . .
H8B C8 H8E 141.1 . .
H8C C8 H8E 56.3 . .
H8D C8 H8E 109.5 . .
C7 C8 H8F 109.5 . .
H8A C8 H8F 56.3 . .
H8B C8 H8F 56.3 . .
H8C C8 H8F 141.1 . .
H8D C8 H8F 109.5 . .
H8E C8 H8F 109.5 . .
N3 C9 C10 180.0 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0265(13) .
Ni1 N1 2.0302(17) .
Ni1 O3 2.0423(13) 8_656
Ni1 O3 2.0463(13) .
Ni1 O2 2.0874(13) .
Ni1 O3 2.1040(13) 2
O1 C7 1.269(2) .
O2 C7 1.265(2) 7_566
O3 C6 1.387(2) .
O3 Ni1 2.0423(13) 7_566
O3 Ni1 2.1040(13) 2
N1 C3 1.334(2) .
N1 N2 1.365(2) .
N2 C1 1.342(2) .
N2 C6 1.486(2) .
N3 C9 1.137(4) .
C1 C2 1.378(3) .
C1 C4 1.497(3) .
C2 C3 1.398(3) .
C2 H2A 0.9500 .
C3 C5 1.492(3) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C4 H4D 0.9800 .
C4 H4E 0.9800 .
C4 H4F 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C5 H5D 0.9800 .
C5 H5E 0.9800 .
C5 H5F 0.9800 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 O2 1.265(2) 8_656
C7 C8 1.516(2) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C8 H8D 0.9800 .
C8 H8E 0.9800 .
C8 H8F 0.9800 .
C9 C10 1.457(4) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
