#------------------------------------------------------------------------------
#$Date: 2018-06-07 08:42:52 +0300 (Thu, 07 Jun 2018) $
#$Revision: 208163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/33/7003373.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_7003373
loop_
_publ_author_name
'Habib, Hesham A.'
'Sanchiz, Joaquin'
'Janiak, Christoph'
_publ_section_title
;
 Mixed-ligand coordination polymers from
 1,2-bis(1,2,4-triazol-4-yl)ethane and benzene-1,3,5-tricarboxylate:
 Trinuclear nickel or zinc secondary building units for
 three-dimensional networks with crystal-to-crystal transformation upon
 dehydration
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              1734
_journal_page_last               1744
_journal_paper_doi               10.1039/b715812b
_journal_year                    2008
_chemical_formula_moiety         'C30 H26 N12 Ni3 O14, 22(O)'
_chemical_formula_sum            'C30 H26 N12 Ni3 O36'
_chemical_formula_weight         1306.76
_chemical_name_common
;
Di(mu-aqua)-bis(mu3-benzene-1,3,5-tricarboxylato)-bis(mu4-1,2-
bis(1,2,4-triazol-4-yl)ethane)-trinickel(ii) hydrate
;
_chemical_name_systematic
;
Di(μ-aqua)-bis(μ3-benzene-1,3,5-tricarboxylato)-
bis(μ4-1,2-bis(1,2,4-triazol-4-yl)ethane)-trinickel(II) hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 111.2920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9111(2)
_cell_length_b                   13.5328(2)
_cell_length_c                   17.7634(3)
_cell_measurement_reflns_used    7244
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      34.066
_cell_measurement_theta_min      3.845
_cell_volume                     3115.81(9)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'ω 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16511
_diffrn_reflns_theta_full        25.65
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.9428
_exptl_absorpt_correction_T_min  0.8193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0398
_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)+(0.0647P)²+3.5335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                5066
_reflns_number_total             5855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715812b.txt
_cod_data_source_block           m146
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-07

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3115.81(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7003373
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.26145(2) -0.01711(2) 0.077238(18) 0.01130(11) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.0000 0.0000 0.01061(12) Uani 1 2 d S . .
O1 O 0.12030(12) -0.09969(13) 0.03378(11) 0.0133(4) Uani 1 1 d . . .
H1A H 0.140(2) -0.139(2) -0.0021(19) 0.020 Uiso 1 1 d . . .
H1B H 0.136(2) -0.135(2) 0.077(2) 0.020 Uiso 1 1 d . . .
C1 C 0.22768(19) 0.1101(2) -0.07528(16) 0.0208(6) Uani 1 1 d . . .
H1 H 0.2978 0.1145 -0.0685 0.025 Uiso 1 1 calc R . .
N1 N 0.19197(15) 0.06689(16) -0.02523(13) 0.0158(4) Uani 1 1 d . . .
N2 N 0.08590(15) 0.07649(15) -0.05636(13) 0.0152(4) Uani 1 1 d . . .
C2 C 0.0620(2) 0.1249(2) -0.12421(16) 0.0206(6) Uani 1 1 d . . .
H2 H -0.0054 0.1415 -0.1582 0.025 Uiso 1 1 calc R . .
N3 N 0.14838(17) 0.14770(17) -0.13856(14) 0.0228(5) Uani 1 1 d . . .
C3 C 0.1542(2) 0.2014(2) -0.20878(18) 0.0287(7) Uani 1 1 d . . .
H3A H 0.1002 0.1776 -0.2582 0.034 Uiso 1 1 calc R . .
H3B H 0.2213 0.1893 -0.2135 0.034 Uiso 1 1 calc R . .
C4 C 0.1404(2) 0.1891(2) 0.30122(18) 0.0275(6) Uani 1 1 d . . .
H4A H 0.1975 0.1642 0.3483 0.033 Uiso 1 1 calc R . .
H4B H 0.0758 0.1775 0.3102 0.033 Uiso 1 1 calc R . .
N4 N 0.13809(17) 0.13688(17) 0.22826(14) 0.0217(5) Uani 1 1 d . . .
C5 C 0.0543(2) 0.1157(2) 0.16267(16) 0.0203(5) Uani 1 1 d . . .
H5 H -0.0138 0.1318 0.1565 0.024 Uiso 1 1 calc R . .
N5 N 0.08124(15) 0.06955(15) 0.10885(12) 0.0148(4) Uani 1 1 d . . .
N6 N 0.18722(15) 0.06040(16) 0.14084(13) 0.0160(4) Uani 1 1 d . . .
C6 C 0.2192(2) 0.1015(2) 0.21213(16) 0.0207(6) Uani 1 1 d . . .
H6 H 0.2885 0.1057 0.2471 0.025 Uiso 1 1 calc R . .
C10 C 0.32926(19) -0.18450(19) -0.10578(16) 0.0183(5) Uani 1 1 d . . .
C11 C 0.42984(19) -0.15254(19) -0.09100(16) 0.0194(5) Uani 1 1 d . . .
H11 H 0.4625 -0.1095 -0.0477 0.023 Uiso 1 1 calc R . .
C12 C 0.48162(19) -0.18421(19) -0.14024(16) 0.0188(5) Uani 1 1 d . . .
C13 C 0.43345(19) -0.24738(19) -0.20475(16) 0.0195(5) Uani 1 1 d . . .
H13 H 0.4701 -0.2718 -0.2361 0.023 Uiso 1 1 calc R . .
C14 C 0.33081(19) -0.2744(2) -0.22287(16) 0.0191(5) Uani 1 1 d . . .
C15 C 0.27953(19) -0.24249(19) -0.17296(16) 0.0190(5) Uani 1 1 d . . .
H15 H 0.2103 -0.2605 -0.1850 0.023 Uiso 1 1 calc R . .
C7 C 0.27430(18) -0.15330(19) -0.05061(16) 0.0172(5) Uani 1 1 d . . .
O2 O 0.32333(13) -0.10222(13) 0.00992(11) 0.0186(4) Uani 1 1 d . . .
O3 O 0.18107(14) -0.18025(15) -0.06966(12) 0.0253(4) Uani 1 1 d . . .
C8 C 0.59080(19) -0.1500(2) -0.12280(17) 0.0217(6) Uani 1 1 d . . .
O4 O 0.60564(13) -0.05855(13) -0.11238(12) 0.0210(4) Uani 1 1 d . . .
O5 O 0.65725(17) -0.21264(18) -0.1187(2) 0.0604(9) Uani 1 1 d . . .
C9 C 0.27401(19) -0.3333(2) -0.29673(16) 0.0188(5) Uani 1 1 d . . .
O6 O 0.32427(13) -0.39064(14) -0.32428(11) 0.0197(4) Uani 1 1 d . . .
O7 O 0.17701(13) -0.31960(15) -0.32810(12) 0.0247(4) Uani 1 1 d . . .
O11 O 0.0023(3) -0.3975(3) -0.0001(2) 0.0738(9) Uani 1 1 d . . .
O12 O 0.1141(4) -0.3762(3) 0.1625(3) 0.1116(17) Uani 1 1 d . . .
O13 O -0.0058(4) -0.0112(3) 0.2800(3) 0.0926(15) Uani 0.90 1 d P . .
O14 O 0.4380(3) 0.0998(5) -0.1299(3) 0.131(2) Uani 1 1 d . . .
O15 O 0.1163(5) -0.1260(3) 0.4040(4) 0.137(2) Uani 1 1 d . . .
O16 O 0.8238(4) -0.3225(4) -0.1149(3) 0.0679(14) Uani 0.60 1 d P . .
O17 O 0.4756(5) 0.0150(4) 0.3060(3) 0.140(2) Uani 1 1 d . . .
O18 O 0.7076(7) -0.4834(5) -0.2141(5) 0.111(3) Uani 0.60 1 d P . .
O19 O 0.4198(5) 0.1968(6) 0.3691(5) 0.176(3) Uani 0.90 1 d P . .
O20 O 0.8207(8) -0.3081(7) -0.0055(7) 0.067(3) Uani 0.30 1 d P . .
O21 O 0.6572(10) -0.3701(10) -0.2245(8) 0.100(5) Uani 0.30 1 d P . .
O22A O 0.3977(11) 0.1118(11) 0.5421(9) 0.098(4) Uiso 0.30 1 d P . .
O22B O 0.3460(9) 0.1571(10) 0.4837(8) 0.082(3) Uiso 0.30 1 d P . .
O23 O 0.2750(9) -0.0038(8) 0.4452(11) 0.343(8) Uani 1 1 d . . .
O24 O 0.5481(12) 0.0626(11) 0.5606(9) 0.200(7) Uani 0.50 1 d P . .
O25A O 0.6956(15) -0.5397(15) -0.1383(12) 0.057(5) Uiso 0.15 1 d P . .
O25B O 0.743(3) -0.510(3) -0.166(3) 0.117(12) Uiso 0.15 1 d P . .
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
_geom_angle_publ_flag
O4 Ni1 O2 86.20(7) 3_655 . ?
O4 Ni1 N1 94.41(8) 3_655 . ?
O2 Ni1 N1 87.51(8) . . ?
O4 Ni1 O6 89.21(7) 3_655 4_556 ?
O2 Ni1 O6 90.93(7) . 4_556 ?
N1 Ni1 O6 175.95(8) . 4_556 ?
O4 Ni1 N6 99.06(8) 3_655 . ?
O2 Ni1 N6 174.73(7) . . ?
N1 Ni1 N6 92.03(8) . . ?
O6 Ni1 N6 89.17(8) 4_556 . ?
O4 Ni1 O1 177.00(8) 3_655 . ?
O2 Ni1 O1 91.19(7) . . ?
N1 Ni1 O1 83.99(7) . . ?
O6 Ni1 O1 92.32(7) 4_556 . ?
N6 Ni1 O1 83.54(7) . . ?
O1 Ni2 O1 180.0 3 . ?
O1 Ni2 N5 94.83(7) 3 . ?
O1 Ni2 N5 85.17(7) . . ?
O1 Ni2 N5 85.17(7) 3 3 ?
O1 Ni2 N5 94.83(7) . 3 ?
N5 Ni2 N5 180.0 . 3 ?
O1 Ni2 N2 94.67(7) 3 . ?
O1 Ni2 N2 85.34(7) . . ?
N5 Ni2 N2 90.52(8) . . ?
N5 Ni2 N2 89.49(8) 3 . ?
O1 Ni2 N2 85.33(7) 3 3 ?
O1 Ni2 N2 94.66(7) . 3 ?
N5 Ni2 N2 89.49(8) . 3 ?
N5 Ni2 N2 90.51(8) 3 3 ?
N2 Ni2 N2 180.0 . 3 ?
Ni2 O1 Ni1 107.71(8) . . ?
Ni2 O1 H1A 125.1(18) . . ?
Ni1 O1 H1A 94.9(18) . . ?
Ni2 O1 H1B 123(2) . . ?
Ni1 O1 H1B 94(2) . . ?
H1A O1 H1B 104(3) . . ?
N1 C1 N3 109.7(2) . . ?
N1 C1 H1 125.2 . . ?
N3 C1 H1 125.2 . . ?
C1 N1 N2 107.5(2) . . ?
C1 N1 Ni1 132.52(17) . . ?
N2 N1 Ni1 119.66(15) . . ?
C2 N2 N1 107.1(2) . . ?
C2 N2 Ni2 133.87(17) . . ?
N1 N2 Ni2 118.36(15) . . ?
N2 C2 N3 110.1(2) . . ?
N2 C2 H2 125.0 . . ?
N3 C2 H2 125.0 . . ?
C2 N3 C1 105.6(2) . . ?
C2 N3 C3 126.8(2) . . ?
C1 N3 C3 127.5(2) . . ?
N3 C3 C4 109.6(2) . 4_565 ?
N3 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 4_565 . ?
N3 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 4_565 . ?
H3A C3 H3B 108.2 . . ?
N4 C4 C3 109.3(2) . 4_566 ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 4_566 . ?
N4 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 4_566 . ?
H4A C4 H4B 108.3 . . ?
C5 N4 C6 105.6(2) . . ?
C5 N4 C4 127.0(2) . . ?
C6 N4 C4 127.4(2) . . ?
N5 C5 N4 110.3(2) . . ?
N5 C5 H5 124.8 . . ?
N4 C5 H5 124.8 . . ?
C5 N5 N6 106.8(2) . . ?
C5 N5 Ni2 134.01(17) . . ?
N6 N5 Ni2 118.78(15) . . ?
C6 N6 N5 107.3(2) . . ?
C6 N6 Ni1 133.13(17) . . ?
N5 N6 Ni1 119.38(15) . . ?
N6 C6 N4 109.9(2) . . ?
N6 C6 H6 125.0 . . ?
N4 C6 H6 125.0 . . ?
C15 C10 C11 119.4(2) . . ?
C15 C10 C7 120.4(2) . . ?
C11 C10 C7 120.1(2) . . ?
C12 C11 C10 120.0(2) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.3(2) . . ?
C11 C12 C8 119.3(2) . . ?
C13 C12 C8 120.4(2) . . ?
C12 C13 C14 119.9(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 C9 119.7(2) . . ?
C13 C14 C9 120.9(2) . . ?
C10 C15 C14 120.9(2) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O2 C7 O3 125.0(2) . . ?
O2 C7 C10 117.8(2) . . ?
O3 C7 C10 117.2(2) . . ?
C7 O2 Ni1 126.52(15) . . ?
O5 C8 O4 125.9(2) . . ?
O5 C8 C12 118.5(2) . . ?
O4 C8 C12 115.6(2) . . ?
C8 O4 Ni1 129.22(17) . 3_655 ?
O6 C9 O7 124.8(2) . . ?
O6 C9 C14 118.7(2) . . ?
O7 C9 C14 116.5(2) . . ?
C9 O6 Ni1 125.34(16) . 4 ?
O25B O18 O25A 37(3) . . ?
O25B O18 O21 123(3) . . ?
O25A O18 O21 111.2(11) . . ?
O25B O25A O18 31(2) . . ?
O18 O25B O25A 112(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.0046(17) 3_655 ?
Ni1 O2 2.0603(17) . ?
Ni1 N1 2.064(2) . ?
Ni1 O6 2.0669(18) 4_556 ?
Ni1 N6 2.071(2) . ?
Ni1 O1 2.1446(16) . ?
Ni2 O1 2.0618(16) 3 ?
Ni2 O1 2.0619(16) . ?
Ni2 N5 2.077(2) . ?
Ni2 N5 2.077(2) 3 ?
Ni2 N2 2.091(2) . ?
Ni2 N2 2.091(2) 3 ?
O1 H1A 0.94(3) . ?
O1 H1B 0.86(3) . ?
C1 N1 1.304(3) . ?
C1 N3 1.356(3) . ?
C1 H1 0.9400 . ?
N1 N2 1.381(3) . ?
N2 C2 1.304(3) . ?
C2 N3 1.351(3) . ?
C2 H2 0.9400 . ?
N3 C3 1.471(3) . ?
C3 C4 1.514(4) 4_565 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.466(3) . ?
C4 C3 1.514(4) 4_566 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
N4 C5 1.346(3) . ?
N4 C6 1.349(3) . ?
C5 N5 1.305(3) . ?
C5 H5 0.9400 . ?
N5 N6 1.380(3) . ?
N6 C6 1.304(3) . ?
C6 H6 0.9400 . ?
C10 C15 1.385(4) . ?
C10 C11 1.395(3) . ?
C10 C7 1.506(3) . ?
C11 C12 1.388(4) . ?
C11 H11 0.9400 . ?
C12 C13 1.391(4) . ?
C12 C8 1.508(3) . ?
C13 C14 1.394(3) . ?
C13 H13 0.9400 . ?
C14 C15 1.393(4) . ?
C14 C9 1.493(4) . ?
C15 H15 0.9400 . ?
C7 O2 1.252(3) . ?
C7 O3 1.269(3) . ?
C8 O5 1.237(4) . ?
C8 O4 1.257(3) . ?
O4 Ni1 2.0045(17) 3_655 ?
C9 O6 1.256(3) . ?
C9 O7 1.273(3) . ?
O6 Ni1 2.0669(18) 4 ?
O18 O25B 0.89(4) . ?
O18 O25A 1.61(2) . ?
O18 O21 1.667(14) . ?
O22A O22B 1.194(17) . ?
O25A O25B 1.04(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O3 0.94(3) 1.61(3) 2.531(2) 166(3) .
O1 H1A O2 0.94(3) 2.53(3) 3.005(2) 111(2) .
O1 H1B O7 0.86(3) 1.69(4) 2.536(3) 168(3) 4_556
O1 H1B O6 0.86(3) 2.59(3) 3.038(2) 113(2) 4_556
