#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:19:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180257 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/43/7114353.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_7114353
loop_
_publ_author_name
'Ponomarova, Vira V.'
'Komarchuk, Vasiliy V.'
'Boldog, Ishtvan'
'Chernega, Alexander N.'
'Sieler, Joachim'
'Domasevitch, Konstantin V.'
_publ_section_title
;
 Mixed-anion complexes with a bipyrazolyl ligand. A new entry to a realm
 of three-dimensional five-connected coordination topologiesElectronic
 supplementary information (ESI) available: crystal structure
 determination and refinement details for 1â€“4. See
 http://www.rsc.org/suppdata/cc/b1/b110599j/
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              436
_journal_paper_doi               10.1039/b110599j
_journal_year                    2002
_chemical_formula_sum            'C40 H62 N18 Ni2 O13 S'
_chemical_formula_weight         1152.56
_chemical_name_systematic
;
Tetrakis(3,3',5,5'-Tetramethyl-4,4'-bipyrazolyl) Sulfato Dinitrato
Dinickel(II), trihydrate
;
_space_group_IT_number           128
_symmetry_cell_setting           tetragonal
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6542(13)
_cell_length_b                   13.6542(13)
_cell_length_c                   16.477(2)
_cell_measurement_temperature    223(2)
_cell_volume                     3071.9(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'SMART CCD Siemens'
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8138
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.713
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0169(66)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.370
_refine_ls_goodness_of_fit_obs   1.370
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1021
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      3.410
_refine_ls_restrained_S_obs      1.368
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_obs          0.0801
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0120P)²+14.8433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3476
_refine_ls_wR_factor_obs         0.1836
_reflns_number_observed          1021
_reflns_number_total             1129
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b110599j.txt
_cod_data_source_block           c1026
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+14.8433P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+14.8433P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3071.9(5)
_cod_original_sg_symbol_H-M      P4/mnc
_cod_database_code               7114353
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.0000 0.0000 0.30168(9) 0.0362(6) Uani 1 d S
O1 O 0.0000 0.0000 0.1732(6) 0.075(3) Uani 1 d S
S1 S 0.0291(7) 0.0475(6) 0.5000 0.029(2) Uani 0.25 d SP
O2 O 0.0000 0.0000 0.4281(5) 0.044(2) Uani 1 d S
O3 O 0.1445(11) 0.0320(18) 0.5000 0.076(7) Uani 0.50 d SP
N1 N 0.0869(4) 0.1267(4) 0.3040(3) 0.0381(13) Uani 1 d .
N2 N 0.0551(4) 0.2035(4) 0.3494(3) 0.0390(13) Uani 1 d .
H2A H 0.0091(4) 0.1983(4) 0.3874(3) 0.047 Uiso 1 d R
C1 C 0.1011(5) 0.2873(5) 0.3314(4) 0.043(2) Uani 1 d .
C2 C 0.1666(5) 0.2655(5) 0.2702(4) 0.040(2) Uani 1 d .
C3 C 0.1561(5) 0.1650(5) 0.2556(4) 0.0435(15) Uani 1 d .
C4 C 0.2145(8) 0.1047(7) 0.1986(7) 0.077(3) Uani 1 d .
H4A H 0.1929(8) 0.0384(7) 0.2000(7) 0.093 Uiso 1 d R
H4B H 0.2059(8) 0.1304(7) 0.1457(7) 0.093 Uiso 1 d R
H4C H 0.2820(8) 0.1077(7) 0.2129(7) 0.093 Uiso 1 d R
C5 C 0.0786(8) 0.3813(6) 0.3736(7) 0.077(3) Uani 1 d .
H5A H 0.0295(8) 0.3705(6) 0.4134(7) 0.092 Uiso 1 d R
H5B H 0.1362(8) 0.4062(6) 0.3986(7) 0.092 Uiso 1 d R
H5C H 0.0553(8) 0.4274(6) 0.3350(7) 0.092 Uiso 1 d R
O4 O -0.2034(15) -0.0705(12) 0.5000 0.011(4) Uiso 0.25 d SP
N3 N 0.3194(38) 0.4568(35) 0.5000 0.098(16) Uiso 0.25 d SPD
N3A N 0.2061(28) 0.5930(28) 0.5000 0.131(23) Uiso 0.25 d SPD
O8 O 0.3389(29) 0.4208(29) 0.5661(18) 0.115(11) Uiso 0.25 d PD
O6 O 0.1192(25) 0.5836(33) 0.5000 0.102(13) Uiso 0.25 d SPD
O7 O 0.2420(42) 0.6734(29) 0.5000 0.180(30) Uiso 0.25 d SPD
O5 O 0.2575(26) 0.5219(29) 0.5000 0.177(15) Uiso 0.50 d SPD
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'
S S 0.1246 0.1234 '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
O2 Ni1 N1 88.9(2) . .
O2 Ni1 N1 88.9(2) . 4
N1 Ni1 N1 89.981(6) . 4
O2 Ni1 N1 88.9(2) . 2
N1 Ni1 N1 177.9(3) . 2
N1 Ni1 N1 89.981(6) 4 2
O2 Ni1 N1 88.9(2) . 3
N1 Ni1 N1 89.981(6) . 3
N1 Ni1 N1 177.9(3) 4 3
N1 Ni1 N1 89.981(6) 2 3
O2 Ni1 O1 180.0 . .
N1 Ni1 O1 91.1(2) . .
N1 Ni1 O1 91.1(2) 4 .
N1 Ni1 O1 91.1(2) 2 .
N1 Ni1 O1 91.1(2) 3 .
S1 S1 S1 90.0 11_556 3
S1 S1 O2 67.5(2) 11_556 .
S1 S1 O2 67.5(2) 3 .
S1 S1 O2 67.5(2) 11_556 9_556
S1 S1 O2 67.5(2) 3 9_556
O2 S1 O2 114.6(6) . 9_556
S1 S1 S1 45.000(3) 11_556 9_556
S1 S1 S1 45.000(1) 3 9_556
O2 S1 S1 57.3(3) . 9_556
O2 S1 S1 57.3(3) 9_556 9_556
S1 S1 O3 161.3(13) 11_556 3
S1 S1 O3 71.3(12) 3 3
O2 S1 O3 103.9(6) . 3
O2 S1 O3 103.9(6) 9_556 3
S1 S1 O3 116.3(12) 9_556 3
S1 S1 O3 68.8(13) 11_556 .
S1 S1 O3 158.8(13) 3 .
O2 S1 O3 102.6(7) . .
O2 S1 O3 102.6(7) 9_556 .
S1 S1 O3 113.8(13) 9_556 .
O3 S1 O3 129.8(7) 3 .
S1 O2 S1 44.9(4) . 11_556
S1 O2 S1 44.9(4) . 3
S1 O2 S1 65.4(6) 11_556 3
S1 O2 S1 65.4(6) . 9_556
S1 O2 S1 44.9(4) 11_556 9_556
S1 O2 S1 44.9(4) 3 9_556
S1 O2 Ni1 147.3(3) . .
S1 O2 Ni1 147.3(3) 11_556 .
S1 O2 Ni1 147.3(3) 3 .
S1 O2 Ni1 147.3(3) 9_556 .
O4 O3 S1 179.1(23) 9_556 11_556
O4 O3 S1 139.2(25) 9_556 .
S1 O3 S1 39.8(7) 11_556 .
C3 N1 N2 104.5(5) . .
C3 N1 Ni1 135.1(5) . .
N2 N1 Ni1 117.7(4) . .
C1 N2 N1 112.8(5) . .
N2 C1 C2 106.4(6) . .
N2 C1 C5 122.3(6) . .
C2 C1 C5 131.3(7) . .
C1 C2 C3 105.7(6) . .
C1 C2 C2 127.1(6) . 8
C3 C2 C2 127.2(6) . 8
N1 C3 C2 110.6(6) . .
N1 C3 C4 122.6(7) . .
C2 C3 C4 126.7(6) . .
O8 N3 O8 125.6(51) 10_556 .
O8 N3 O5 116.2(27) 10_556 .
O8 N3 O5 116.2(27) . .
O6 N3A O5 119.7(21) . .
O6 N3A O7 120.2(21) . .
O5 N3A O7 120.1(21) . .
N3A O5 N3 172.3(44) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.084(8) .
Ni1 N1 2.098(5) .
Ni1 N1 2.098(5) 4
Ni1 N1 2.098(5) 2
Ni1 N1 2.098(5) 3
Ni1 O1 2.118(10) .
S1 S1 1.075(11) 11_556
S1 S1 1.075(11) 3
S1 O2 1.407(8) .
S1 O2 1.407(8) 9_556
S1 S1 1.52(2) 9_556
S1 O3 1.57(2) 3
S1 O3 1.59(2) .
O2 S1 1.407(8) 11_556
O2 S1 1.407(8) 3
O2 S1 1.407(8) 9_556
O3 O4 0.96(2) 9_556
O3 S1 1.57(2) 11_556
N1 C3 1.343(8) .
N1 N2 1.360(7) .
N2 C1 1.338(9) .
C1 C2 1.380(10) .
C1 C5 1.492(11) .
C2 C3 1.401(10) .
C2 C2 1.470(13) 8
C3 C4 1.481(11) .
O4 O3 0.96(2) 9_556
N3 O8 1.22(2) 10_556
N3 O8 1.22(2) .
N3 O5 1.23(2) .
N3A O6 1.19(2) .
N3A O5 1.20(2) .
N3A O7 1.20(2) .
