#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/62/2216230.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2216230
loop_
_publ_author_name
'Zhang, Shu-Ming'
'Du, Jian-Long'
_publ_section_title
;
 Tetraaquabis[4-(tetrazol-1-yl)benzoato-κN⁴]nickel(II)
 dihydrate
;
_journal_coeditor_code           AT2494
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3139
_journal_page_last               m3139
_journal_paper_doi               10.1107/S1600536807060138
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C8 H5 N4 O2)2 (H2 O)4], 2H2 O'
_chemical_formula_moiety         'C16 H22 N8 Ni O10'
_chemical_formula_sum            'C16 H22 N8 Ni O10'
_chemical_formula_weight         545.13
_chemical_name_systematic
;
Tetraaquabis[4-(tetrazol-1-yl)benzoato-\kN⁴]nickel(II) dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                96.90(3)
_cell_angle_beta                 94.62(3)
_cell_angle_gamma                116.00(3)
_cell_formula_units_Z            1
_cell_length_a                   7.3830(15)
_cell_length_b                   7.5819(15)
_cell_length_c                   10.712(2)
_cell_measurement_reflns_used    5360
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      3.0
_cell_volume                     529.0(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5651
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.270
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0314
_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)+(0.0235P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                2221
_reflns_number_total             2419
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            at2494.cif
_cod_data_source_block           I
_cod_database_code               2216230
_cod_database_fobs_code          2216230
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ni Ni1 0.5000 0.0000 0.5000 0.01921(10) Uani d S 1
O O2W 0.7492(2) -0.0451(3) 0.53264(13) 0.0276(3) Uani d . 1
O O3W 0.0848(2) 0.2902(2) 0.64256(16) 0.0335(3) Uani d . 1
N N1 0.5324(2) 0.1275(2) 0.68998(14) 0.0241(3) Uani d . 1
O O1W 0.6797(2) 0.2685(2) 0.45392(14) 0.0298(3) Uani d . 1
O O2 0.1970(2) 0.3646(2) 1.40415(12) 0.0319(3) Uani d . 1
N N4 0.4656(2) 0.2020(2) 0.87325(13) 0.0222(3) Uani d . 1
O O1 -0.0689(2) 0.3363(2) 1.27599(13) 0.0389(4) Uani d . 1
N N2 0.6909(3) 0.1679(3) 0.77918(15) 0.0364(4) Uani d . 1
C C1 0.3960(3) 0.1505(3) 0.75005(16) 0.0270(4) Uani d . 1
H H1A 0.2701 0.1334 0.7125 0.032 Uiso calc R 1
N N3 0.6530(3) 0.2133(3) 0.88977(16) 0.0381(4) Uani d . 1
C C8 0.1002(3) 0.3386(3) 1.29574(17) 0.0259(4) Uani d . 1
C C6 0.3882(3) 0.3152(3) 1.20129(17) 0.0289(4) Uani d . 1
H H6A 0.4567 0.3434 1.2835 0.035 Uiso calc R 1
C C4 0.1001(3) 0.2715(3) 1.06100(18) 0.0287(4) Uani d . 1
H H4A -0.0268 0.2696 1.0481 0.034 Uiso calc R 1
C C2 0.3748(3) 0.2411(3) 0.97907(16) 0.0222(4) Uani d . 1
C C5 0.1985(3) 0.3081(3) 1.18314(16) 0.0232(4) Uani d . 1
C C7 0.4783(3) 0.2814(3) 1.09967(17) 0.0284(4) Uani d . 1
H H7A 0.6064 0.2857 1.1123 0.034 Uiso calc R 1
C C3 0.1874(3) 0.2377(3) 0.95800(17) 0.0294(4) Uani d . 1
H H3A 0.1208 0.2129 0.8757 0.035 Uiso calc R 1
H H1WB 0.716(4) 0.371(4) 0.502(3) 0.043(7) Uiso d . 1
H H2WB 0.741(4) -0.138(4) 0.559(3) 0.056(9) Uiso d . 1
H H1WA 0.762(4) 0.288(4) 0.408(3) 0.059(9) Uiso d . 1
H H3WB 0.069(4) 0.372(4) 0.675(3) 0.044(8) Uiso d . 1
H H2WA 0.847(5) 0.048(5) 0.574(3) 0.059(9) Uiso d . 1
H H3WA 0.118(5) 0.321(5) 0.572(3) 0.074(10) Uiso d . 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2W Ni1 O2W 2_656 . 180.00(8) ?
O2W Ni1 O1W 2_656 . 90.81(7) ?
O2W Ni1 O1W . . 89.19(7) yes
O2W Ni1 O1W 2_656 2_656 89.19(7) ?
O2W Ni1 O1W . 2_656 90.81(7) ?
O1W Ni1 O1W . 2_656 180.0 ?
O2W Ni1 N1 2_656 2_656 92.56(7) ?
O2W Ni1 N1 . 2_656 87.44(7) ?
O1W Ni1 N1 . 2_656 88.07(7) ?
O1W Ni1 N1 2_656 2_656 91.93(7) ?
O2W Ni1 N1 2_656 . 87.44(7) ?
O2W Ni1 N1 . . 92.56(7) yes
O1W Ni1 N1 . . 91.93(7) yes
O1W Ni1 N1 2_656 . 88.07(7) ?
N1 Ni1 N1 2_656 . 180.0 ?
Ni1 O2W H2WB . . 120(2) ?
Ni1 O2W H2WA . . 115(2) ?
H2WB O2W H2WA . . 106(3) ?
H3WB O3W H3WA . . 106(3) ?
C1 N1 N2 . . 106.30(15) ?
C1 N1 Ni1 . . 128.19(13) ?
N2 N1 Ni1 . . 124.50(12) ?
Ni1 O1W H1WB . . 122.5(18) ?
Ni1 O1W H1WA . . 125(2) ?
H1WB O1W H1WA . . 106(3) ?
C1 N4 N3 . . 107.85(15) ?
C1 N4 C2 . . 131.03(16) ?
N3 N4 C2 . . 121.12(15) ?
N3 N2 N1 . . 110.27(15) ?
N1 C1 N4 . . 108.89(17) ?
N1 C1 H1A . . 125.6 ?
N4 C1 H1A . . 125.6 ?
N2 N3 N4 . . 106.69(16) ?
O1 C8 O2 . . 124.76(17) ?
O1 C8 C5 . . 118.33(17) ?
O2 C8 C5 . . 116.91(17) ?
C5 C6 C7 . . 120.97(18) ?
C5 C6 H6A . . 119.5 ?
C7 C6 H6A . . 119.5 ?
C3 C4 C5 . . 120.80(18) ?
C3 C4 H4A . . 119.6 ?
C5 C4 H4A . . 119.6 ?
C3 C2 C7 . . 121.79(17) ?
C3 C2 N4 . . 119.42(16) ?
C7 C2 N4 . . 118.79(16) ?
C6 C5 C4 . . 119.21(17) ?
C6 C5 C8 . . 119.98(17) ?
C4 C5 C8 . . 120.81(17) ?
C2 C7 C6 . . 118.51(18) ?
C2 C7 H7A . . 120.7 ?
C6 C7 H7A . . 120.7 ?
C2 C3 C4 . . 118.70(17) ?
C2 C3 H3A . . 120.6 ?
C4 C3 H3A . . 120.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O2W 2_656 2.0252(15) ?
Ni1 O2W . 2.0252(15) yes
Ni1 O1W . 2.0315(16) yes
Ni1 O1W 2_656 2.0315(16) ?
Ni1 N1 2_656 2.0927(15) ?
Ni1 N1 . 2.0927(15) yes
O2W H2WB . 0.77(3) ?
O2W H2WA . 0.80(3) ?
O3W H3WB . 0.74(3) ?
O3W H3WA . 0.84(3) ?
N1 C1 . 1.299(2) ?
N1 N2 . 1.346(2) ?
O1W H1WB . 0.80(3) ?
O1W H1WA . 0.79(3) ?
O2 C8 . 1.259(2) ?
N4 C1 . 1.323(2) ?
N4 N3 . 1.344(2) ?
N4 C2 . 1.428(2) ?
O1 C8 . 1.241(2) ?
N2 N3 . 1.281(2) ?
C1 H1A . 0.9300 ?
C8 C5 . 1.502(2) ?
C6 C5 . 1.375(3) ?
C6 C7 . 1.376(3) ?
C6 H6A . 0.9300 ?
C4 C3 . 1.375(3) ?
C4 C5 . 1.378(3) ?
C4 H4A . 0.9300 ?
C2 C3 . 1.371(3) ?
C2 C7 . 1.374(3) ?
C7 H7A . 0.9300 ?
C3 H3A . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1WA O1 1_654 0.79(3) 1.92(3) 2.704(2) 171(3)
O1W H1WB O2 2_667 0.80(3) 1.93(3) 2.724(2) 172(3)
O2W H2WB O2 2_657 0.77(3) 2.04(3) 2.771(2) 160(3)
O2W H2WA O3W 1_655 0.80(3) 1.91(3) 2.697(3) 168(3)
O3W H3WB O1 2_567 0.74(3) 2.21(3) 2.917(2) 162(3)
O3W H3WA O2 1_554 0.84(3) 1.96(3) 2.793(2) 173(3)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
O2W Ni1 N1 C1 2_656 19.06(17)
O2W Ni1 N1 C1 . -160.94(17)
O1W Ni1 N1 C1 . 109.78(17)
O1W Ni1 N1 C1 2_656 -70.22(17)
N1 Ni1 N1 C1 2_656 -11E1(10)
O2W Ni1 N1 N2 2_656 -174.01(16)
O2W Ni1 N1 N2 . 5.99(16)
O1W Ni1 N1 N2 . -83.29(16)
O1W Ni1 N1 N2 2_656 96.71(16)
N1 Ni1 N1 N2 2_656 6E1(10)
C1 N1 N2 N3 . 0.2(2)
Ni1 N1 N2 N3 . -169.14(14)
N2 N1 C1 N4 . -0.5(2)
Ni1 N1 C1 N4 . 168.30(12)
N3 N4 C1 N1 . 0.6(2)
C2 N4 C1 N1 . -178.81(17)
N1 N2 N3 N4 . 0.2(2)
C1 N4 N3 N2 . -0.5(2)
C2 N4 N3 N2 . 179.00(17)
C1 N4 C2 C3 . -3.8(3)
N3 N4 C2 C3 . 176.84(18)
C1 N4 C2 C7 . 176.2(2)
N3 N4 C2 C7 . -3.1(3)
C7 C6 C5 C4 . -1.7(3)
C7 C6 C5 C8 . 177.90(18)
C3 C4 C5 C6 . 1.5(3)
C3 C4 C5 C8 . -178.04(18)
O1 C8 C5 C6 . 178.18(18)
O2 C8 C5 C6 . -1.9(3)
O1 C8 C5 C4 . -2.3(3)
O2 C8 C5 C4 . 177.66(18)
C3 C2 C7 C6 . 1.2(3)
N4 C2 C7 C6 . -178.79(17)
C5 C6 C7 C2 . 0.3(3)
C7 C2 C3 C4 . -1.4(3)
N4 C2 C3 C4 . 178.65(18)
C5 C4 C3 C2 . 0.0(3)
