#------------------------------------------------------------------------------
#$Date: 2018-06-07 08:42:52 +0300 (Thu, 07 Jun 2018) $
#$Revision: 208163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/33/7003374.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_7003374
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 H30 N12 Ni3 O16, 4(H2 O)'
_chemical_formula_sum            'C30 H38 N12 Ni3 O20'
_chemical_formula_weight         1062.85
_chemical_name_common
;
Diaqua-di(mu-aqua)-bis(mu2-benzene-1,3,5-tricarboxylato)-
bis(mu4-1,2-bis(1,2,4-triazol-4-yl)ethane)-trinickel(ii) tetrahydrate
;
_chemical_name_systematic
;
Diaqua-di(μ-aqua)-bis(μ2-benzene-1,3,5-tricarboxylato)-
bis(μ4-1,2-bis(1,2,4-triazol-4-yl)ethane)-trinickel(II) tetrahydrate
;
_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                 114.636(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7399(9)
_cell_length_b                   8.2320(5)
_cell_length_c                   18.8439(13)
_cell_measurement_reflns_used    1698
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      19.385
_cell_measurement_theta_min      2.75
_cell_volume                     1937.4(2)
_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, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8884
_diffrn_reflns_theta_full        19.90
_diffrn_reflns_theta_max         19.90
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_correction_T_min  0.5564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1772
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0658
_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)+(0.0885P)²+18.3368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                1360
_reflns_number_total             1772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715812b.txt
_cod_data_source_block           146froz
_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_sg_symbol_H-M      P2(1)/c
_cod_database_code               7003374
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 0.26471(11) 0.38631(18) 0.55871(8) 0.0348(6) Uani 1 1 d . . .
Ni2 Ni 0.0000 0.5000 0.5000 0.0298(6) Uani 1 2 d S . .
O1 O 0.0994(7) 0.3114(9) 0.4924(4) 0.038(2) Uani 1 1 d D . .
H1A H 0.085(9) 0.214(8) 0.501(7) 0.057 Uiso 1 1 d D . .
H1B H 0.100(9) 0.306(14) 0.448(4) 0.057 Uiso 1 1 d D . .
O8 O 0.3167(8) 0.1595(11) 0.5936(5) 0.056(3) Uani 1 1 d D . .
H8A H 0.246(6) 0.108(15) 0.580(8) 0.084 Uiso 1 1 d D . .
H8B H 0.348(11) 0.164(18) 0.640(8) 0.084 Uiso 1 1 d . . .
N1 N 0.2105(7) 0.6103(10) 0.5082(4) 0.030(2) Uani 1 1 d . . .
N2 N 0.1040(7) 0.6488(10) 0.4771(5) 0.029(2) Uani 1 1 d . . .
C1 C 0.2572(9) 0.7142(13) 0.4799(6) 0.036(3) Uiso 1 1 d . . .
H1 H 0.3308 0.7158 0.4917 0.043 Uiso 1 1 calc R . .
C2 C 0.0910(8) 0.7734(13) 0.4319(6) 0.032(3) Uiso 1 1 d . . .
H2 H 0.0250 0.8248 0.4033 0.038 Uiso 1 1 calc R . .
N3 N 0.1842(6) 0.8187(10) 0.4315(5) 0.031(2) Uiso 1 1 d . . .
C3 C 0.1971(9) 0.9429(13) 0.3794(6) 0.034(3) Uiso 1 1 d . . .
H3A H 0.2559 1.0167 0.4092 0.040 Uiso 1 1 calc R . .
H3B H 0.1313 1.0068 0.3545 0.040 Uiso 1 1 calc R . .
N5 N 0.1056(7) 0.5004(11) 0.6188(5) 0.034(2) Uani 1 1 d . . .
N6 N 0.2111(7) 0.4486(11) 0.6434(5) 0.035(2) Uani 1 1 d . . .
C5 C 0.1003(9) 0.5643(13) 0.6820(6) 0.034(3) Uiso 1 1 d . . .
H5 H 0.0377 0.6077 0.6831 0.041 Uiso 1 1 calc R . .
C6 C 0.2619(9) 0.4860(13) 0.7188(7) 0.040(3) Uiso 1 1 d . . .
H6 H 0.3344 0.4646 0.7504 0.048 Uiso 1 1 calc R . .
N4 N 0.1934(7) 0.5592(10) 0.7426(5) 0.034(2) Uiso 1 1 d . . .
C4 C 0.2213(10) 0.6463(15) 0.8177(7) 0.051(3) Uiso 1 1 d . . .
H4A H 0.1827 0.7499 0.8064 0.061 Uiso 1 1 calc R . .
H4B H 0.2980 0.6713 0.8399 0.061 Uiso 1 1 calc R . .
O2 O 0.3006(6) 0.3441(9) 0.4627(4) 0.040(2) Uani 1 1 d . . .
C7 C 0.2316(9) 0.3578(13) 0.3937(7) 0.031(3) Uiso 1 1 d . . .
O3 O 0.1339(6) 0.3310(9) 0.3716(4) 0.040(2) Uiso 1 1 d . . .
O4 O 0.5858(6) 0.5319(10) 0.3851(4) 0.045(2) Uani 1 1 d . . .
C8 C 0.5146(9) 0.5840(14) 0.3216(7) 0.040(3) Uiso 1 1 d . . .
O5 O 0.5346(6) 0.6799(11) 0.2759(5) 0.061(2) Uiso 1 1 d . . .
O6 O 0.1527(7) 0.5134(10) 0.0667(5) 0.059(2) Uiso 1 1 d . . .
C9 C 0.1283(9) 0.5474(14) 0.1239(7) 0.044(3) Uiso 1 1 d . . .
O7 O 0.0388(6) 0.5868(9) 0.1174(5) 0.049(2) Uiso 1 1 d . . .
C10 C 0.2692(8) 0.4200(13) 0.3350(6) 0.033(3) Uiso 1 1 d . . .
C11 C 0.3723(8) 0.4625(12) 0.3534(6) 0.029(3) Uiso 1 1 d . . .
H11 H 0.4247 0.4401 0.4037 0.035 Uiso 1 1 calc R . .
C12 C 0.4025(8) 0.5384(13) 0.2998(6) 0.034(3) Uiso 1 1 d . . .
C13 C 0.3226(8) 0.5639(13) 0.2239(6) 0.035(3) Uiso 1 1 d . . .
H13 H 0.3411 0.6118 0.1859 0.042 Uiso 1 1 calc R . .
C14 C 0.2190(8) 0.5204(13) 0.2046(6) 0.033(3) Uiso 1 1 d . . .
C15 C 0.1904(9) 0.4458(13) 0.2591(6) 0.035(3) Uiso 1 1 d . . .
H15 H 0.1193 0.4129 0.2454 0.043 Uiso 1 1 calc R . .
O9 O 0.4876(8) 0.7009(12) 0.9737(6) 0.081(3) Uiso 1 1 d . . .
H9A H 0.5179 0.6061 0.9657 0.121 Uiso 1 1 d . . .
H9B H 0.5214 0.7884 0.9610 0.121 Uiso 1 1 d . . .
O10 O 0.4712(10) 0.4233(15) 0.8809(8) 0.121(4) Uiso 1 1 d . . .
H10A H 0.4625 0.3523 0.9144 0.181 Uiso 1 1 d . . .
H10B H 0.4631 0.3685 0.8342 0.181 Uiso 1 1 d . . .
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'
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
_geom_angle_publ_flag
O4 Ni1 O8 89.6(4) 3_666 . ?
O4 Ni1 N1 92.1(3) 3_666 . ?
O8 Ni1 N1 172.2(3) . . ?
O4 Ni1 N6 97.2(3) 3_666 . ?
O8 Ni1 N6 99.7(3) . . ?
N1 Ni1 N6 87.6(3) . . ?
O4 Ni1 O2 87.3(3) 3_666 . ?
O8 Ni1 O2 87.1(3) . . ?
N1 Ni1 O2 85.4(3) . . ?
N6 Ni1 O2 171.8(3) . . ?
O4 Ni1 O1 176.2(3) 3_666 . ?
O8 Ni1 O1 93.9(4) . . ?
N1 Ni1 O1 84.2(3) . . ?
N6 Ni1 O1 83.8(3) . . ?
O2 Ni1 O1 91.3(3) . . ?
N2 Ni2 N2 179.998(1) . 3_566 ?
N2 Ni2 N5 89.5(3) . . ?
N2 Ni2 N5 90.5(3) 3_566 . ?
N2 Ni2 N5 90.5(3) . 3_566 ?
N2 Ni2 N5 89.5(3) 3_566 3_566 ?
N5 Ni2 N5 179.998(1) . 3_566 ?
N2 Ni2 O1 95.8(3) . 3_566 ?
N2 Ni2 O1 84.2(3) 3_566 3_566 ?
N5 Ni2 O1 96.1(3) . 3_566 ?
N5 Ni2 O1 84.0(3) 3_566 3_566 ?
N2 Ni2 O1 84.2(3) . . ?
N2 Ni2 O1 95.8(3) 3_566 . ?
N5 Ni2 O1 84.0(3) . . ?
N5 Ni2 O1 96.0(3) 3_566 . ?
O1 Ni2 O1 179.997(2) 3_566 . ?
Ni2 O1 Ni1 107.6(3) . . ?
Ni2 O1 H1A 117(8) . . ?
Ni1 O1 H1A 115(8) . . ?
Ni2 O1 H1B 112(8) . . ?
Ni1 O1 H1B 98(8) . . ?
H1A O1 H1B 104(10) . . ?
Ni1 O8 H8A 98(8) . . ?
Ni1 O8 H8B 106(10) . . ?
H8A O8 H8B 109(10) . . ?
C1 N1 N2 107.0(8) . . ?
C1 N1 Ni1 128.8(7) . . ?
N2 N1 Ni1 121.4(6) . . ?
C2 N2 N1 107.2(8) . . ?
C2 N2 Ni2 133.6(7) . . ?
N1 N2 Ni2 119.0(6) . . ?
N1 C1 N3 109.9(9) . . ?
N1 C1 H1 125.1 . . ?
N3 C1 H1 125.1 . . ?
N2 C2 N3 110.7(9) . . ?
N2 C2 H2 124.6 . . ?
N3 C2 H2 124.6 . . ?
C2 N3 C1 105.2(9) . . ?
C2 N3 C3 125.2(9) . . ?
C1 N3 C3 129.0(9) . . ?
N3 C3 C4 107.4(8) . 4_575 ?
N3 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 4_575 . ?
N3 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 4_575 . ?
H3A C3 H3B 108.5 . . ?
C5 N5 N6 105.1(8) . . ?
C5 N5 Ni2 133.1(8) . . ?
N6 N5 Ni2 121.1(6) . . ?
C6 N6 N5 107.1(8) . . ?
C6 N6 Ni1 132.8(8) . . ?
N5 N6 Ni1 118.1(6) . . ?
N4 C5 N5 111.5(10) . . ?
N4 C5 H5 124.2 . . ?
N5 C5 H5 124.2 . . ?
N6 C6 N4 109.4(10) . . ?
N6 C6 H6 125.3 . . ?
N4 C6 H6 125.3 . . ?
C5 N4 C6 106.8(9) . . ?
C5 N4 C4 125.6(9) . . ?
C6 N4 C4 126.6(9) . . ?
N4 C4 C3 116.2(9) . 4_576 ?
N4 C4 H4A 108.2 . . ?
C3 C4 H4A 108.2 4_576 . ?
N4 C4 H4B 108.2 . . ?
C3 C4 H4B 108.2 4_576 . ?
H4A C4 H4B 107.4 . . ?
C7 O2 Ni1 122.2(7) . . ?
O3 C7 O2 125.0(10) . . ?
O3 C7 C10 118.0(10) . . ?
O2 C7 C10 116.9(9) . . ?
C8 O4 Ni1 127.4(7) . 3_666 ?
O4 C8 O5 123.2(10) . . ?
O4 C8 C12 119.0(10) . . ?
O5 C8 C12 117.7(11) . . ?
O7 C9 O6 125.0(11) . . ?
O7 C9 C14 120.4(10) . . ?
O6 C9 C14 114.4(10) . . ?
C11 C10 C15 120.1(10) . . ?
C11 C10 C7 123.1(10) . . ?
C15 C10 C7 116.6(9) . . ?
C10 C11 C12 121.8(10) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C13 117.5(10) . . ?
C11 C12 C8 120.6(10) . . ?
C13 C12 C8 121.8(10) . . ?
C14 C13 C12 121.1(10) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 120.5(10) . . ?
C13 C14 C9 123.7(10) . . ?
C15 C14 C9 115.8(9) . . ?
C14 C15 C10 119.0(10) . . ?
C14 C15 H15 120.5 . . ?
C10 C15 H15 120.5 . . ?
H9A O9 H9B 107.5 . . ?
H10A O10 H10B 109.9 . . ?
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 1.995(8) 3_666 ?
Ni1 O8 2.009(9) . ?
Ni1 N1 2.066(9) . ?
Ni1 N6 2.082(8) . ?
Ni1 O2 2.092(7) . ?
Ni1 O1 2.177(9) . ?
Ni2 N2 2.060(8) . ?
Ni2 N2 2.060(8) 3_566 ?
Ni2 N5 2.100(9) . ?
Ni2 N5 2.100(8) 3_566 ?
Ni2 O1 2.112(7) 3_566 ?
Ni2 O1 2.112(7) . ?
O1 H1A 0.86(5) . ?
O1 H1B 0.84(5) . ?
O8 H8A 0.98(5) . ?
O8 H8B 0.80(14) . ?
N1 C1 1.309(13) . ?
N1 N2 1.367(11) . ?
N2 C2 1.297(13) . ?
C1 N3 1.347(13) . ?
C1 H1 0.9400 . ?
C2 N3 1.337(12) . ?
C2 H2 0.9400 . ?
N3 C3 1.479(13) . ?
C3 C4 1.525(15) 4_575 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
N5 C5 1.332(13) . ?
N5 N6 1.392(12) . ?
N6 C6 1.331(13) . ?
C5 N4 1.313(12) . ?
C5 H5 0.9400 . ?
C6 N4 1.342(13) . ?
C6 H6 0.9400 . ?
N4 C4 1.487(14) . ?
C4 C3 1.525(15) 4_576 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
O2 C7 1.255(12) . ?
C7 O3 1.248(11) . ?
C7 C10 1.495(15) . ?
O4 C8 1.264(13) . ?
O4 Ni1 1.995(8) 3_666 ?
C8 O5 1.279(13) . ?
C8 C12 1.468(15) . ?
O6 C9 1.287(13) . ?
C9 O7 1.227(12) . ?
C9 C14 1.528(16) . ?
C10 C11 1.356(13) . ?
C10 C15 1.404(14) . ?
C11 C12 1.389(14) . ?
C11 H11 0.9400 . ?
C12 C13 1.410(14) . ?
C13 C14 1.362(14) . ?
C13 H13 0.9400 . ?
C14 C15 1.386(14) . ?
C15 H15 0.9400 . ?
O9 H9A 0.9270 . ?
O9 H9B 0.9400 . ?
O10 H10A 0.9042 . ?
O10 H10B 0.9527 . ?
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 O6 0.86(5) 2.22(8) 2.965(11) 144(10) 4_566
O1 H1A O7 0.86(5) 2.41(11) 2.833(11) 111(9) 2_545
O1 H1B O3 0.84(5) 1.70(6) 2.516(9) 163(12) .
O1 H1B O2 0.84(5) 2.67(11) 3.052(10) 109(9) .
O8 H8A O6 0.98(5) 1.57(6) 2.532(13) 165(13) 4_566
O8 H8B O5 0.80(14) 2.15(14) 2.789(13) 137(14) 3_666
O8 H8B O4 0.80(14) 2.77(15) 2.822(13) 85(11) 3_666
O9 H9A O10 0.93 2.09 2.830(16) 135.6 .
O9 H9B O2 0.94 2.31 2.896(12) 120.1 2_656
O9 H9B O4 0.94 2.46 3.365(12) 160.5 4_576
O10 H10A O9 0.90 1.98 2.754(16) 143.2 3_667
O10 H10B O5 0.95 2.13 3.043(16) 161.1 3_666
