#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/27/8102774.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_8102774
loop_
_publ_author_name
'Li-Jing Fan'
'Ying-Ying Liu'
_publ_section_title
;
 Crystal structure of hexaaquabis(hydrogen
 m-benzene-1,3,5-tricarboxylato-kO)-[m2-N,N'-bis(3-pyridylmethylamino)butane-k2N:N']dinickel(II)
 sesquihydrate, Ni2(H2O)6(C9H4O6)2(C16H22N4) · 1.5H2O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              535
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C68 H90 N8 Ni4 O39'
_chemical_formula_sum            'C68 H90 N8 Ni4 O39'
_chemical_formula_weight         1878.32
_chemical_melting_point          ?
_chemical_name_systematic
;
Poly{[tetrahydratebis(μ-benzene-1,3,5-tricarboxylato-κO)\
[μ²-N,N'-bis(3-pyridylmethylamino)butane-\
κ²N:N']bisnickel(II)] trihydrate},
{[Ni₂(C₉H₄O₆)₂(C₁₆H₂₂N₄)(H₂O)₆].1.5H₂O}
;
_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           SHELXL-97
_cell_angle_alpha                97.406(4)
_cell_angle_beta                 102.509(4)
_cell_angle_gamma                107.112(4)
_cell_formula_units_Z            1
_cell_length_a                   11.9487(6)
_cell_length_b                   12.0469(6)
_cell_length_c                   14.9025(5)
_cell_measurement_reflns_used    4436
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2188
_cell_measurement_theta_min      4.1869
_cell_volume                     1958.39(17)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis [2]'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 [4](Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 [3]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       '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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15374
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         4.20
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9010
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0590P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                4771
_reflns_number_total             9010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3073.cff
_cod_data_source_block           mm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1958.39(15)
_cod_database_code               8102774
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.3306(4) 0.4800(4) 0.3204(3) 0.0347(11) Uani 1 1 d . . .
H1 H 0.3348 0.4743 0.2585 0.042 Uiso 1 1 calc RU . .
C2 C 0.3253(5) 0.5841(4) 0.3665(3) 0.0414(12) Uani 1 1 d . . .
H2 H 0.3264 0.6474 0.3365 0.050 Uiso 1 1 calc RU . .
C3 C 0.3183(4) 0.5924(4) 0.4580(3) 0.0344(11) Uani 1 1 d . . .
H3 H 0.3147 0.6618 0.4908 0.041 Uiso 1 1 calc RU . .
C4 C 0.3240(4) 0.3962(4) 0.4499(3) 0.0256(9) Uani 1 1 d . . .
H4 H 0.3249 0.3322 0.4786 0.031 Uiso 1 1 calc RU . .
C5 C 0.3168(4) 0.4967(4) 0.5009(3) 0.0249(9) Uani 1 1 d . . .
C6 C 0.3068(4) 0.4987(4) 0.6010(3) 0.0267(9) Uani 1 1 d . . .
H6A H 0.3209 0.4294 0.6212 0.032 Uiso 1 1 calc RU . .
H6B H 0.3686 0.5687 0.6425 0.032 Uiso 1 1 calc RU . .
C7 C 0.1587(4) 0.4699(4) 0.6972(3) 0.0286(10) Uani 1 1 d . . .
H7A H 0.2126 0.5330 0.7494 0.034 Uiso 1 1 calc RU . .
H7B H 0.1754 0.3974 0.7061 0.034 Uiso 1 1 calc RU . .
C8 C 0.0282(4) 0.4538(4) 0.6972(3) 0.0312(10) Uani 1 1 d . . .
H8A H -0.0252 0.3850 0.6495 0.037 Uiso 1 1 calc RU . .
H8B H 0.0088 0.5227 0.6811 0.037 Uiso 1 1 calc RU . .
C9 C 0.0051(4) 0.4377(4) 0.7919(3) 0.0311(10) Uani 1 1 d . . .
H9A H -0.0749 0.4416 0.7915 0.037 Uiso 1 1 calc RU . .
H9B H 0.0643 0.5025 0.8404 0.037 Uiso 1 1 calc RU . .
C10 C 0.0124(4) 0.3205(4) 0.8160(3) 0.0287(10) Uani 1 1 d . . .
H10A H -0.0477 0.2550 0.7685 0.034 Uiso 1 1 calc RU . .
H10B H 0.0921 0.3157 0.8166 0.034 Uiso 1 1 calc RU . .
C11 C 0.0001(4) 0.1993(4) 0.9388(3) 0.0342(11) Uani 1 1 d . . .
H11A H 0.0691 0.1839 0.9222 0.041 Uiso 1 1 calc RU . .
H11B H -0.0725 0.1335 0.9046 0.041 Uiso 1 1 calc RU . .
C12 C 0.0161(4) 0.2075(4) 1.0428(3) 0.0303(10) Uani 1 1 d . . .
C13 C 0.1254(4) 0.2139(4) 1.0999(3) 0.0291(10) Uani 1 1 d . . .
H13 H 0.1874 0.2102 1.0724 0.035 Uiso 1 1 calc RU . .
C14 C 0.0591(4) 0.2329(4) 1.2328(3) 0.0379(11) Uani 1 1 d . . .
H14 H 0.0740 0.2427 1.2977 0.045 Uiso 1 1 calc RU . .
C15 C -0.0539(5) 0.2267(5) 1.1807(3) 0.0493(14) Uani 1 1 d . . .
H15 H -0.1141 0.2312 1.2100 0.059 Uiso 1 1 calc RU . .
C16 C -0.0762(5) 0.2137(5) 1.0847(3) 0.0447(13) Uani 1 1 d . . .
H16 H -0.1518 0.2092 1.0482 0.054 Uiso 1 1 calc RU . .
C17 C 0.2407(4) 0.0587(4) 0.4044(3) 0.0368(11) Uani 1 1 d . . .
C18 C 0.1379(4) -0.0327(4) 0.4225(3) 0.0270(9) Uani 1 1 d . . .
C19 C 0.1598(4) -0.1081(4) 0.4827(3) 0.0266(9) Uani 1 1 d . . .
H19 H 0.2395 -0.1020 0.5108 0.032 Uiso 1 1 calc RU . .
C20 C 0.0653(4) -0.1916(3) 0.5011(3) 0.0218(9) Uani 1 1 d . . .
C21 C 0.0840(4) -0.2811(4) 0.5600(2) 0.0221(9) Uani 1 1 d . . .
C22 C -0.0531(4) -0.1977(3) 0.4609(3) 0.0239(9) Uani 1 1 d . . .
H22 H -0.1171 -0.2524 0.4745 0.029 Uiso 1 1 calc R . .
C23 C -0.0781(4) -0.1232(4) 0.4004(3) 0.0263(9) Uani 1 1 d . . .
C24 C -0.2093(4) -0.1363(4) 0.3581(3) 0.0304(10) Uani 1 1 d . . .
C25 C 0.0181(4) -0.0422(4) 0.3813(3) 0.0267(9) Uani 1 1 d . . .
H25 H 0.0027 0.0068 0.3402 0.032 Uiso 1 1 calc R . .
C26 C 0.4842(4) 0.2906(4) 0.1559(3) 0.0253(9) Uani 1 1 d . . .
C27 C 0.5569(4) 0.3829(3) 0.1136(2) 0.0212(8) Uani 1 1 d . . .
C28 C 0.6253(4) 0.3519(4) 0.0555(3) 0.0234(9) Uani 1 1 d . . .
H28 H 0.6250 0.2741 0.0438 0.028 Uiso 1 1 calc RU . .
C29 C 0.6933(4) 0.4351(3) 0.0155(3) 0.0218(9) Uani 1 1 d . . .
C30 C 0.7739(4) 0.4073(4) -0.0437(3) 0.0275(10) Uani 1 1 d . . .
C31 C 0.6942(4) 0.5506(4) 0.0343(3) 0.0250(9) Uani 1 1 d . . .
H31 H 0.7396 0.6068 0.0072 0.030 Uiso 1 1 calc R . .
C32 C 0.6287(4) 0.5848(3) 0.0930(3) 0.0222(9) Uani 1 1 d . . .
C33 C 0.6392(4) 0.7134(4) 0.1134(3) 0.0290(10) Uani 1 1 d . . .
C34 C 0.5597(4) 0.5001(4) 0.1319(2) 0.0223(9) Uani 1 1 d . . .
H34 H 0.5149 0.5217 0.1706 0.027 Uiso 1 1 calc RU . .
N1 N 0.3300(3) 0.3873(3) 0.3599(2) 0.0279(8) Uani 1 1 d . . .
N2 N 0.1478(3) 0.2253(3) 1.1939(2) 0.0282(8) Uani 1 1 d . . .
N3 N 0.1840(3) 0.4994(3) 0.6075(2) 0.0223(7) Uani 1 1 d D . .
N4 N -0.0101(3) 0.3109(3) 0.9105(2) 0.0266(8) Uani 1 1 d D . .
O1 O 0.3465(3) 0.0638(4) 0.4424(3) 0.0799(13) Uani 1 1 d U . .
O2 O 0.2158(3) 0.1283(3) 0.3543(2) 0.0341(7) Uani 1 1 d U . .
O3 O -0.2278(3) -0.0639(3) 0.30813(19) 0.0331(7) Uani 1 1 d U . .
O4 O -0.2879(3) -0.2156(3) 0.3766(3) 0.0549(10) Uani 1 1 d U . .
O3W O 0.2909(3) 0.0644(3) 0.1877(2) 0.0379(7) Uani 1 1 d U . .
O5 O -0.0053(3) -0.3688(3) 0.55421(19) 0.0323(7) Uani 1 1 d U . .
O4W O 0.4732(3) 0.2178(3) 0.3644(2) 0.0335(7) Uani 1 1 d U . .
O6 O 0.1893(3) -0.2660(2) 0.60917(19) 0.0318(7) Uani 1 1 d U . .
H6 H 0.2370 -0.2052 0.6022 0.048 Uiso 1 1 calc RU . .
O5W O 0.5216(3) 0.8434(3) 0.3260(2) 0.0494(9) Uani 1 1 d U . .
O7 O 0.5002(3) 0.1908(3) 0.1496(2) 0.0381(8) Uani 1 1 d U . .
O6W O 0.4364(3) 0.8999(3) 0.1409(2) 0.0431(8) Uani 1 1 d U . .
O8 O 0.4105(3) 0.3179(2) 0.19587(19) 0.0311(7) Uani 1 1 d U . .
O7W O 0.6174(3) 1.0890(2) 0.28250(19) 0.0331(7) Uani 1 1 d U . .
O9 O 0.7541(3) 0.2999(3) -0.0802(2) 0.0351(7) Uani 1 1 d U . .
H9 H 0.6964 0.2570 -0.0658 0.053 Uiso 1 1 calc RU . .
O8W O 0.6952(3) 0.9840(3) 0.1299(2) 0.0460(8) Uani 1 1 d U . .
O10 O 0.8580(3) 0.4912(3) -0.0514(2) 0.0403(8) Uani 1 1 d U . .
O11 O 0.7108(3) 0.7834(3) 0.0790(3) 0.0520(9) Uani 1 1 d U . .
O12 O 0.5779(3) 0.7427(2) 0.1649(2) 0.0320(7) Uani 1 1 d U . .
Ni1 Ni 0.31312(5) 0.22544(5) 0.27699(3) 0.02502(15) Uani 1 1 d . . .
Ni2 Ni 0.60459(5) 0.91342(5) 0.22692(4) 0.03011(16) Uani 1 1 d . . .
H3N H 0.184(4) 0.569(2) 0.608(3) 0.036 Uiso 1 1 d DU . .
H4N H 0.040(3) 0.372(3) 0.950(3) 0.036 Uiso 1 1 d DU . .
O1W O 0.2669(5) -0.1448(5) 0.2657(5) 0.1065(16) Uani 1 1 d DU . .
H1A H 0.239(7) -0.227(3) 0.239(6) 0.160 Uiso 1 1 d DU . .
H1B H 0.329(6) -0.151(7) 0.315(5) 0.160 Uiso 1 1 d DU . .
O2W O 0.5000 1.0000 0.0000 0.162(4) Uani 1 2 d SDU . .
H2A H 0.575(8) 1.064(9) 0.031(9) 0.243 Uiso 1 1 d 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'
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
N1 C1 C2 123.3(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 118.4(4) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C2 C3 C5 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C5 C3 H3 120.2 . . ?
N1 C4 C5 122.4(4) . . ?
N1 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C3 118.2(4) . . ?
C4 C5 C6 119.3(4) . . ?
C3 C5 C6 122.5(3) . . ?
N3 C6 C5 110.8(3) . . ?
N3 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N3 C7 C8 111.9(3) . . ?
N3 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N3 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 C9 112.3(3) . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 C10 113.1(3) . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N4 C10 C9 110.3(3) . . ?
N4 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N4 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N4 C11 C12 111.4(3) . . ?
N4 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N4 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 C16 118.0(4) . . ?
C13 C12 C11 120.0(4) . . ?
C16 C12 C11 122.0(4) . . ?
N2 C13 C12 123.4(4) . . ?
N2 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
N2 C14 C15 122.7(4) . . ?
N2 C14 H14 118.6 . . ?
C15 C14 H14 118.6 . . ?
C16 C15 C14 119.0(4) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C12 119.1(4) . . ?
C15 C16 H16 120.4 . . ?
C12 C16 H16 120.4 . . ?
O1 C17 O2 123.9(4) . . ?
O1 C17 C18 118.3(4) . . ?
O2 C17 C18 117.8(4) . . ?
C25 C18 C19 119.0(4) . . ?
C25 C18 C17 120.4(4) . . ?
C19 C18 C17 120.6(4) . . ?
C20 C19 C18 121.0(4) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C22 119.0(3) . . ?
C19 C20 C21 123.0(3) . . ?
C22 C20 C21 118.0(4) . . ?
O5 C21 O6 123.2(4) . . ?
O5 C21 C20 117.7(3) . . ?
O6 C21 C20 119.0(4) . . ?
C20 C22 C23 121.3(4) . . ?
C20 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C25 C23 C22 118.6(4) . . ?
C25 C23 C24 123.1(4) . . ?
C22 C23 C24 118.3(4) . . ?
O4 C24 O3 126.2(4) . . ?
O4 C24 C23 117.4(4) . . ?
O3 C24 C23 116.4(4) . . ?
C23 C25 C18 121.1(4) . . ?
C23 C25 H25 119.5 . . ?
C18 C25 H25 119.5 . . ?
O8 C26 O7 124.2(4) . . ?
O8 C26 C27 117.2(3) . . ?
O7 C26 C27 118.6(3) . . ?
C34 C27 C28 119.0(4) . . ?
C34 C27 C26 121.4(3) . . ?
C28 C27 C26 119.7(3) . . ?
C29 C28 C27 121.0(4) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C31 C29 C28 119.0(3) . . ?
C31 C29 C30 118.0(4) . . ?
C28 C29 C30 122.9(4) . . ?
O10 C30 O9 123.6(4) . . ?
O10 C30 C29 117.6(4) . . ?
O9 C30 C29 118.8(4) . . ?
C29 C31 C32 121.4(4) . . ?
C29 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C34 C32 C31 119.0(4) . . ?
C34 C32 C33 123.0(4) . . ?
C31 C32 C33 118.0(4) . . ?
O12 C33 O11 125.3(4) . . ?
O12 C33 C32 117.4(4) . . ?
O11 C33 C32 117.2(4) . . ?
C32 C34 C27 120.7(3) . . ?
C32 C34 H34 119.7 . . ?
C27 C34 H34 119.7 . . ?
C1 N1 C4 118.1(3) . . ?
C1 N1 Ni1 119.6(3) . . ?
C4 N1 Ni1 121.7(3) . . ?
C14 N2 C13 117.8(4) . . ?
C14 N2 Ni1 120.3(3) . 1_556 ?
C13 N2 Ni1 121.9(3) . 1_556 ?
C6 N3 C7 112.4(3) . . ?
C6 N3 H3N 107(3) . . ?
C7 N3 H3N 106(3) . . ?
C11 N4 C10 112.3(3) . . ?
C11 N4 H4N 112(3) . . ?
C10 N4 H4N 107(3) . . ?
C17 O2 Ni1 130.6(3) . . ?
C24 O3 Ni2 121.6(3) . 1_445 ?
C21 O6 H6 109.5 . . ?
C26 O8 Ni1 128.5(3) . . ?
C30 O9 H9 109.5 . . ?
C33 O12 Ni2 124.7(3) . . ?
O2 Ni1 O8 177.97(11) . . ?
O2 Ni1 N2 87.53(13) . 1_554 ?
O8 Ni1 N2 92.44(13) . 1_554 ?
O2 Ni1 N1 92.65(12) . . ?
O8 Ni1 N1 89.38(12) . . ?
N2 Ni1 N1 88.73(13) 1_554 . ?
O2 Ni1 O4W 89.03(12) . . ?
O8 Ni1 O4W 90.98(12) . . ?
N2 Ni1 O4W 176.50(13) 1_554 . ?
N1 Ni1 O4W 92.06(12) . . ?
O2 Ni1 O3W 88.55(12) . . ?
O8 Ni1 O3W 89.42(11) . . ?
N2 Ni1 O3W 88.76(12) 1_554 . ?
N1 Ni1 O3W 177.17(13) . . ?
O4W Ni1 O3W 90.52(11) . . ?
O3 Ni2 O12 93.37(11) 1_665 . ?
O3 Ni2 O5W 92.09(13) 1_665 . ?
O12 Ni2 O5W 87.29(13) . . ?
O3 Ni2 O6W 176.48(13) 1_665 . ?
O12 Ni2 O6W 88.96(11) . . ?
O5W Ni2 O6W 90.65(14) . . ?
O3 Ni2 O8W 85.64(13) 1_665 . ?
O12 Ni2 O8W 92.50(12) . . ?
O5W Ni2 O8W 177.71(14) . . ?
O6W Ni2 O8W 91.63(14) . . ?
O3 Ni2 O7W 91.74(11) 1_665 . ?
O12 Ni2 O7W 174.85(11) . . ?
O5W Ni2 O7W 93.13(13) . . ?
O6W Ni2 O7W 85.90(11) . . ?
O8W Ni2 O7W 87.28(12) . . ?
H1A O1W H1B 93(2) . . ?
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
C1 N1 1.326(5) . ?
C1 C2 1.376(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(6) . ?
C2 H2 0.9300 . ?
C3 C5 1.386(6) . ?
C3 H3 0.9300 . ?
C4 N1 1.351(5) . ?
C4 C5 1.380(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.520(5) . ?
C6 N3 1.494(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.497(5) . ?
C7 C8 1.513(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.521(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.523(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N4 1.504(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N4 1.490(5) . ?
C11 C12 1.508(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.370(6) . ?
C12 C16 1.394(6) . ?
C13 N2 1.349(5) . ?
C13 H13 0.9300 . ?
C14 N2 1.332(5) . ?
C14 C15 1.380(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O1 1.248(5) . ?
C17 O2 1.249(5) . ?
C17 C18 1.489(6) . ?
C18 C25 1.395(6) . ?
C18 C19 1.395(5) . ?
C19 C20 1.378(6) . ?
C19 H19 0.9300 . ?
C20 C22 1.389(5) . ?
C20 C21 1.511(5) . ?
C21 O5 1.239(5) . ?
C21 O6 1.259(5) . ?
C22 C23 1.399(5) . ?
C22 H22 0.9300 . ?
C23 C25 1.381(6) . ?
C23 C24 1.510(6) . ?
C24 O4 1.234(5) . ?
C24 O3 1.254(5) . ?
C25 H25 0.9300 . ?
C26 O8 1.259(5) . ?
C26 O7 1.267(5) . ?
C26 C27 1.496(6) . ?
C27 C34 1.392(5) . ?
C27 C28 1.399(5) . ?
C28 C29 1.381(6) . ?
C28 H28 0.9300 . ?
C29 C31 1.379(5) . ?
C29 C30 1.517(5) . ?
C30 O10 1.236(5) . ?
C30 O9 1.268(5) . ?
C31 C32 1.394(5) . ?
C31 H31 0.9300 . ?
C32 C34 1.386(6) . ?
C32 C33 1.502(6) . ?
C33 O12 1.256(5) . ?
C33 O11 1.259(5) . ?
C34 H34 0.9300 . ?
N1 Ni1 2.100(3) . ?
N2 Ni1 2.092(3) 1_556 ?
N3 H3N 0.840(19) . ?
N4 H4N 0.84(2) . ?
O2 Ni1 2.044(3) . ?
O3 Ni2 2.023(3) 1_445 ?
O3W Ni1 2.118(3) . ?
O4W Ni1 2.102(3) . ?
O6 H6 0.8200 . ?
O5W Ni2 2.083(3) . ?
O6W Ni2 2.085(3) . ?
O8 Ni1 2.062(3) . ?
O7W Ni2 2.118(3) . ?
O9 H9 0.8200 . ?
O8W Ni2 2.107(3) . ?
O12 Ni2 2.045(3) . ?
Ni1 N2 2.092(3) 1_554 ?
Ni2 O3 2.023(3) 1_665 ?
O1W H1A 0.94(2) . ?
O1W H1B 0.96(2) . ?
O2W H2A 0.96(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
N3 H3N O6 0.840(19) 1.97(2) 2.805(4) 178(5) 1_565
N4 H4N O10 0.84(2) 1.97(2) 2.810(5) 173(4) 2_666
