#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/61/2226170.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_2226170
loop_
_publ_author_name
'Derikvand, Zohreh'
'Olmstead, Marilyn M.'
_publ_section_title
;
 Bis(9-aminoacridinium)
 bis(pyridine-2,6-dicarboxylato-κ³O²,N,O⁶)nickelate(II)
 trihydrate
;
_journal_coeditor_code           HY2305
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m642
_journal_page_last               m643
_journal_paper_doi               10.1107/S1600536810016776
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C13 H11 N2)2 [Ni (C7 H3 N O4)2], 3H2 O'
_chemical_formula_moiety
'2(C13 H11 N2 +), C14 H6 N2 Ni O8 2-, 3(H2 O)'
_chemical_formula_sum            'C40 H34 N6 Ni O11'
_chemical_formula_weight         833.44
_chemical_name_systematic
;
Bis(9-aminoacridinium) bis(pyridine-2,6-dicarboxylato-
κ³O²,N,O⁶)nickelate(II) trihydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.288(2)
_cell_angle_beta                 103.609(2)
_cell_angle_gamma                105.482(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7939(10)
_cell_length_b                   13.3335(12)
_cell_length_c                   13.9370(13)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.9
_cell_volume                     1795.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al.,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and 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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29993
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0406P)²+0.6602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                10951
_reflns_number_total             11816
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2305.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               2226170
_cod_database_fobs_code          2226170
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.359601(12) 0.243203(9) 0.083985(9) 0.01101(3) Uani d . 1 . .
O O1 0.24161(7) 0.20633(6) 0.18019(5) 0.01602(13) Uani d . 1 . .
O O2 0.09729(8) 0.06546(6) 0.20554(6) 0.01894(14) Uani d . 1 . .
O O3 0.47436(8) 0.07283(6) -0.14184(5) 0.01698(13) Uani d . 1 . .
O O4 0.45471(7) 0.21101(5) -0.02971(5) 0.01462(12) Uani d . 1 . .
O O5 0.54671(7) 0.27912(6) 0.20078(5) 0.01500(12) Uani d . 1 . .
O O6 0.73195(8) 0.42266(7) 0.30005(6) 0.02066(15) Uani d . 1 . .
O O7 0.14490(7) 0.42729(6) -0.04067(5) 0.01533(13) Uani d . 1 . .
O O8 0.20247(7) 0.28295(5) -0.01471(5) 0.01506(12) Uani d . 1 . .
N N1 0.28850(8) 0.08335(6) 0.03374(6) 0.01215(13) Uani d . 1 . .
N N2 0.43332(8) 0.40357(6) 0.11994(6) 0.01076(13) Uani d . 1 . .
C C1 0.17544(10) 0.10551(8) 0.16048(7) 0.01420(16) Uani d . 1 . .
C C2 0.20048(9) 0.02963(7) 0.07382(7) 0.01305(15) Uani d . 1 . .
C C3 0.14477(10) -0.08340(8) 0.03748(8) 0.01671(17) Uani d . 1 . .
H H3 0.0808(16) -0.1233(13) 0.0667(12) 0.026(4) Uiso d . 1 . .
C C4 0.18596(11) -0.13846(8) -0.03952(8) 0.01748(17) Uani d . 1 . .
H H4 0.1504(15) -0.2174(13) -0.0647(12) 0.023(4) Uiso d . 1 . .
C C5 0.27985(10) -0.08048(8) -0.07890(7) 0.01533(16) Uani d . 1 . .
H H5 0.3120(16) -0.1156(13) -0.1310(12) 0.024(4) Uiso d . 1 . .
C C6 0.32823(9) 0.03235(7) -0.04062(7) 0.01215(15) Uani d . 1 . .
C C7 0.42722(9) 0.11096(7) -0.07411(7) 0.01279(15) Uani d . 1 . .
C C8 0.61936(10) 0.37940(8) 0.23293(7) 0.01360(15) Uani d . 1 . .
C C9 0.55891(9) 0.45375(7) 0.18393(7) 0.01160(15) Uani d . 1 . .
C C10 0.62363(9) 0.56455(8) 0.20244(7) 0.01367(15) Uani d . 1 . .
H H10 0.7148(16) 0.5980(13) 0.2491(12) 0.025(4) Uiso d . 1 . .
C C11 0.55385(10) 0.62207(7) 0.15184(7) 0.01395(16) Uani d . 1 . .
H H11 0.5949(15) 0.6953(12) 0.1617(11) 0.019(3) Uiso d . 1 . .
C C12 0.42193(9) 0.56827(7) 0.08503(7) 0.01255(15) Uani d . 1 . .
H H12 0.3741(15) 0.6076(12) 0.0478(11) 0.019(3) Uiso d . 1 . .
C C13 0.36452(9) 0.45752(7) 0.07089(7) 0.01066(14) Uani d . 1 . .
C C14 0.22569(9) 0.38391(7) -0.00075(7) 0.01211(15) Uani d . 1 . .
N N3 1.01535(9) 0.30800(7) 0.73932(6) 0.01601(15) Uani d . 1 . .
H H3A 1.0262(18) 0.2447(15) 0.7348(13) 0.035(4) Uiso d . 1 . .
H H3B 1.0349(16) 0.3518(14) 0.8016(13) 0.028(4) Uiso d . 1 . .
N N4 0.85905(8) 0.38995(6) 0.47807(6) 0.01216(13) Uani d . 1 . .
H H4A 0.8176(17) 0.4019(13) 0.4211(13) 0.029(4) Uiso d . 1 . .
C C15 0.96750(9) 0.33591(7) 0.65564(7) 0.01238(15) Uani d . 1 . .
C C16 0.92971(9) 0.43231(7) 0.66353(7) 0.01277(15) Uani d . 1 . .
C C17 0.94175(10) 0.50324(8) 0.75957(7) 0.01699(17) Uani d . 1 . .
H H17 0.9776(15) 0.4885(12) 0.8207(12) 0.022(4) Uiso d . 1 . .
C C18 0.89975(11) 0.59228(8) 0.76344(8) 0.01865(18) Uani d . 1 . .
H H18 0.9081(15) 0.6410(12) 0.8279(12) 0.023(4) Uiso d . 1 . .
C C19 0.84486(10) 0.61508(8) 0.67144(8) 0.01701(17) Uani d . 1 . .
H H19 0.8169(17) 0.6750(13) 0.6743(13) 0.029(4) Uiso d . 1 . .
C C20 0.83206(10) 0.54841(8) 0.57722(8) 0.01467(16) Uani d . 1 . .
H H20 0.7949(15) 0.5620(12) 0.5123(12) 0.024(4) Uiso d . 1 . .
C C21 0.87392(9) 0.45595(7) 0.57219(7) 0.01210(15) Uani d . 1 . .
C C22 0.89545(9) 0.29898(7) 0.46724(7) 0.01138(14) Uani d . 1 . .
C C23 0.87734(9) 0.23509(8) 0.36660(7) 0.01369(15) Uani d . 1 . .
H H23 0.8404(15) 0.2582(12) 0.3080(11) 0.019(3) Uiso d . 1 . .
C C24 0.91252(10) 0.14290(8) 0.35392(7) 0.01527(16) Uani d . 1 . .
H H24 0.9000(16) 0.1003(13) 0.2858(12) 0.027(4) Uiso d . 1 . .
C C25 0.96692(9) 0.11129(8) 0.44075(8) 0.01504(16) Uani d . 1 . .
H H25 0.9882(15) 0.0445(12) 0.4304(11) 0.021(4) Uiso d . 1 . .
C C26 0.98706(9) 0.17326(8) 0.53888(7) 0.01362(15) Uani d . 1 . .
H H26 1.0261(15) 0.1520(12) 0.5973(11) 0.020(3) Uiso d . 1 . .
C C27 0.95095(9) 0.26932(7) 0.55488(7) 0.01163(15) Uani d . 1 . .
N N5 0.54540(8) 0.10654(7) 0.29830(6) 0.01346(14) Uani d . 1 . .
H H5B 0.5307(17) 0.1587(14) 0.2716(12) 0.028(4) Uiso d . 1 . .
H H5A 0.5530(17) 0.0488(14) 0.2569(13) 0.032(4) Uiso d . 1 . .
N N6 0.66618(8) 0.17508(7) 0.61591(6) 0.01321(14) Uani d . 1 . .
H H6A 0.6815(18) 0.1842(14) 0.6793(14) 0.035(4) Uiso d . 1 . .
C C28 0.58088(9) 0.12538(7) 0.39986(7) 0.01094(14) Uani d . 1 . .
C C29 0.63617(9) 0.05563(7) 0.44931(7) 0.01157(14) Uani d . 1 . .
C C30 0.65177(9) -0.04016(7) 0.39368(7) 0.01397(15) Uani d . 1 . .
H H30 0.6252(15) -0.0608(12) 0.3218(12) 0.020(3) Uiso d . 1 . .
C C31 0.70392(10) -0.10461(8) 0.44482(8) 0.01636(17) Uani d . 1 . .
H H31 0.7130(15) -0.1690(13) 0.4074(12) 0.021(3) Uiso d . 1 . .
C C32 0.74404(9) -0.07552(8) 0.55373(8) 0.01687(17) Uani d . 1 . .
H H32 0.7815(15) -0.1210(12) 0.5896(12) 0.023(4) Uiso d . 1 . .
C C33 0.73293(9) 0.01756(8) 0.61017(8) 0.01544(16) Uani d . 1 . .
H H33 0.7632(16) 0.0396(13) 0.6863(12) 0.027(4) Uiso d . 1 . .
C C34 0.67789(9) 0.08377(7) 0.55852(7) 0.01229(15) Uani d . 1 . .
C C35 0.60723(9) 0.23954(7) 0.57198(7) 0.01228(15) Uani d . 1 . .
C C36 0.58907(10) 0.32831(8) 0.63673(7) 0.01603(17) Uani d . 1 . .
H H36 0.6224(16) 0.3430(13) 0.7095(13) 0.027(4) Uiso d . 1 . .
C C37 0.52273(11) 0.38982(8) 0.59321(8) 0.01782(17) Uani d . 1 . .
H H37 0.5095(16) 0.4525(13) 0.6367(12) 0.026(4) Uiso d . 1 . .
C C38 0.47143(10) 0.36511(8) 0.48487(8) 0.01641(17) Uani d . 1 . .
H H38 0.4195(15) 0.4061(12) 0.4546(11) 0.021(4) Uiso d . 1 . .
C C39 0.49140(9) 0.28085(7) 0.42143(7) 0.01346(15) Uani d . 1 . .
H H39 0.4518(14) 0.2641(12) 0.3479(11) 0.017(3) Uiso d . 1 . .
C C40 0.56196(9) 0.21681(7) 0.46364(7) 0.01130(14) Uani d . 1 . .
O O1W 0.11651(8) 0.63289(6) 0.02097(6) 0.01961(14) Uani d . 1 . .
H H1A 0.132(2) 0.5745(16) 0.0089(15) 0.045(5) Uiso d . 1 . .
H H1B 0.0366(19) 0.6155(14) 0.0272(13) 0.033(4) Uiso d . 1 . .
O O2W -0.08266(9) -0.12483(7) 0.21495(6) 0.02072(15) Uani d . 1 . .
H H2A -0.1191(18) -0.1637(15) 0.1557(14) 0.033(4) Uiso d . 1 . .
H H2B -0.031(2) -0.0729(16) 0.2114(15) 0.041(5) Uiso d . 1 . .
O O3W 0.68638(9) 0.20630(7) 0.81693(6) 0.02351(16) Uani d . 1 . .
H H3C 0.628(2) 0.1734(16) 0.8358(14) 0.039(5) Uiso d . 1 . .
H H3D 0.7472(19) 0.2544(15) 0.8698(14) 0.035(4) 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
N1 Ni1 N2 . . 173.93(3) ?
N1 Ni1 O1 . . 78.42(3) ?
N2 Ni1 O1 . . 107.10(3) ?
N1 Ni1 O4 . . 78.42(3) ?
N2 Ni1 O4 . . 96.15(3) ?
O1 Ni1 O4 . . 156.71(3) ?
N1 Ni1 O5 . . 104.16(3) ?
N2 Ni1 O5 . . 78.28(3) ?
O1 Ni1 O5 . . 94.00(3) ?
O4 Ni1 O5 . . 89.26(3) ?
N1 Ni1 O8 . . 100.69(3) ?
N2 Ni1 O8 . . 76.88(3) ?
O1 Ni1 O8 . . 92.00(3) ?
O4 Ni1 O8 . . 94.68(3) ?
O5 Ni1 O8 . . 155.12(3) ?
C1 O1 Ni1 . . 115.38(6) ?
C7 O4 Ni1 . . 114.59(6) ?
C8 O5 Ni1 . . 114.08(6) ?
C14 O8 Ni1 . . 114.13(6) ?
C2 N1 C6 . . 122.34(8) ?
C2 N1 Ni1 . . 118.90(6) ?
C6 N1 Ni1 . . 118.75(6) ?
C9 N2 C13 . . 121.37(8) ?
C9 N2 Ni1 . . 118.02(6) ?
C13 N2 Ni1 . . 120.08(6) ?
O2 C1 O1 . . 126.47(9) ?
O2 C1 C2 . . 118.90(8) ?
O1 C1 C2 . . 114.61(8) ?
N1 C2 C3 . . 120.31(8) ?
N1 C2 C1 . . 112.49(8) ?
C3 C2 C1 . . 127.18(8) ?
C2 C3 C4 . . 118.28(9) ?
C2 C3 H3 . . 120.8(9) ?
C4 C3 H3 . . 120.9(9) ?
C5 C4 C3 . . 120.26(9) ?
C5 C4 H4 . . 119.9(9) ?
C3 C4 H4 . . 119.8(9) ?
C6 C5 C4 . . 118.08(9) ?
C6 C5 H5 . . 119.2(9) ?
C4 C5 H5 . . 122.7(9) ?
N1 C6 C5 . . 120.68(8) ?
N1 C6 C7 . . 112.46(8) ?
C5 C6 C7 . . 126.86(8) ?
O3 C7 O4 . . 125.73(9) ?
O3 C7 C6 . . 118.52(8) ?
O4 C7 C6 . . 115.76(8) ?
O6 C8 O5 . . 127.62(9) ?
O6 C8 C9 . . 117.00(8) ?
O5 C8 C9 . . 115.38(8) ?
N2 C9 C10 . . 121.18(8) ?
N2 C9 C8 . . 113.61(8) ?
C10 C9 C8 . . 125.21(8) ?
C9 C10 C11 . . 118.31(8) ?
C9 C10 H10 . . 118.8(9) ?
C11 C10 H10 . . 122.9(9) ?
C10 C11 C12 . . 119.83(8) ?
C10 C11 H11 . . 120.2(9) ?
C12 C11 H11 . . 120.0(9) ?
C13 C12 C11 . . 118.26(8) ?
C13 C12 H12 . . 121.7(9) ?
C11 C12 H12 . . 120.0(9) ?
N2 C13 C12 . . 121.04(8) ?
N2 C13 C14 . . 112.51(7) ?
C12 C13 C14 . . 126.41(8) ?
O7 C14 O8 . . 125.99(9) ?
O7 C14 C13 . . 118.26(8) ?
O8 C14 C13 . . 115.75(8) ?
C15 N3 H3A . . 121.6(12) ?
C15 N3 H3B . . 121.1(11) ?
H3A N3 H3B . . 117.2(15) ?
C22 N4 C21 . . 122.33(8) ?
C22 N4 H4A . . 117.4(11) ?
C21 N4 H4A . . 120.0(11) ?
N3 C15 C27 . . 120.41(8) ?
N3 C15 C16 . . 121.15(8) ?
C27 C15 C16 . . 118.44(8) ?
C21 C16 C17 . . 118.21(8) ?
C21 C16 C15 . . 119.03(8) ?
C17 C16 C15 . . 122.73(8) ?
C18 C17 C16 . . 120.87(9) ?
C18 C17 H17 . . 119.7(9) ?
C16 C17 H17 . . 119.4(9) ?
C17 C18 C19 . . 120.21(9) ?
C17 C18 H18 . . 121.5(9) ?
C19 C18 H18 . . 118.3(9) ?
C20 C19 C18 . . 120.50(9) ?
C20 C19 H19 . . 119.5(10) ?
C18 C19 H19 . . 120.0(10) ?
C19 C20 C21 . . 119.82(9) ?
C19 C20 H20 . . 122.5(9) ?
C21 C20 H20 . . 117.6(9) ?
N4 C21 C16 . . 120.52(8) ?
N4 C21 C20 . . 119.08(8) ?
C16 C21 C20 . . 120.40(8) ?
N4 C22 C27 . . 120.54(8) ?
N4 C22 C23 . . 118.77(8) ?
C27 C22 C23 . . 120.69(8) ?
C24 C23 C22 . . 119.72(8) ?
C24 C23 H23 . . 121.5(9) ?
C22 C23 H23 . . 118.8(9) ?
C23 C24 C25 . . 120.38(9) ?
C23 C24 H24 . . 119.2(10) ?
C25 C24 H24 . . 120.4(10) ?
C26 C25 C24 . . 120.59(9) ?
C26 C25 H25 . . 120.0(9) ?
C24 C25 H25 . . 119.4(9) ?
C25 C26 C27 . . 120.51(8) ?
C25 C26 H26 . . 119.9(9) ?
C27 C26 H26 . . 119.6(9) ?
C22 C27 C26 . . 118.10(8) ?
C22 C27 C15 . . 119.12(8) ?
C26 C27 C15 . . 122.79(8) ?
C28 N5 H5B . . 119.4(10) ?
C28 N5 H5A . . 121.4(11) ?
H5B N5 H5A . . 117.9(15) ?
C35 N6 C34 . . 122.20(8) ?
C35 N6 H6A . . 118.9(12) ?
C34 N6 H6A . . 117.8(12) ?
N5 C28 C29 . . 121.91(8) ?
N5 C28 C40 . . 119.80(8) ?
C29 C28 C40 . . 118.29(8) ?
C34 C29 C30 . . 118.18(8) ?
C34 C29 C28 . . 118.75(8) ?
C30 C29 C28 . . 123.06(8) ?
C31 C30 C29 . . 120.68(9) ?
C31 C30 H30 . . 119.1(9) ?
C29 C30 H30 . . 120.2(9) ?
C30 C31 C32 . . 120.25(9) ?
C30 C31 H31 . . 120.4(9) ?
C32 C31 H31 . . 119.3(9) ?
C33 C32 C31 . . 120.72(9) ?
C33 C32 H32 . . 119.3(9) ?
C31 C32 H32 . . 120.0(9) ?
C32 C33 C34 . . 119.59(9) ?
C32 C33 H33 . . 121.2(9) ?
C34 C33 H33 . . 119.2(9) ?
N6 C34 C33 . . 118.67(8) ?
N6 C34 C29 . . 120.76(8) ?
C33 C34 C29 . . 120.56(9) ?
N6 C35 C40 . . 120.56(8) ?
N6 C35 C36 . . 118.90(8) ?
C40 C35 C36 . . 120.52(8) ?
C37 C36 C35 . . 119.41(9) ?
C37 C36 H36 . . 121.7(10) ?
C35 C36 H36 . . 118.9(10) ?
C36 C37 C38 . . 120.74(9) ?
C36 C37 H37 . . 120.9(9) ?
C38 C37 H37 . . 118.3(9) ?
C39 C38 C37 . . 120.27(9) ?
C39 C38 H38 . . 119.4(9) ?
C37 C38 H38 . . 120.3(9) ?
C38 C39 C40 . . 120.57(9) ?
C38 C39 H39 . . 118.2(8) ?
C40 C39 H39 . . 121.1(8) ?
C35 C40 C39 . . 118.39(8) ?
C35 C40 C28 . . 119.18(8) ?
C39 C40 C28 . . 122.30(8) ?
H1A O1W H1B . . 104.2(17) ?
H2A O2W H2B . . 105.1(18) ?
H3C O3W H3D . . 108.3(17) ?
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 N1 . 1.9648(8) ?
Ni1 N2 . 1.9760(8) ?
Ni1 O1 . 2.1003(7) ?
Ni1 O4 . 2.1120(7) ?
Ni1 O5 . 2.1360(7) ?
Ni1 O8 . 2.1776(7) ?
O1 C1 . 1.2770(12) ?
O2 C1 . 1.2420(12) ?
O3 C7 . 1.2523(11) ?
O4 C7 . 1.2655(11) ?
O5 C8 . 1.2741(12) ?
O6 C8 . 1.2434(12) ?
O7 C14 . 1.2580(11) ?
O8 C14 . 1.2642(11) ?
N1 C2 . 1.3359(12) ?
N1 C6 . 1.3361(11) ?
N2 C9 . 1.3318(12) ?
N2 C13 . 1.3385(11) ?
C1 C2 . 1.5280(13) ?
C2 C3 . 1.3919(13) ?
C3 C4 . 1.3970(14) ?
C3 H3 . 0.977(16) ?
C4 C5 . 1.3963(14) ?
C4 H4 . 0.971(16) ?
C5 C6 . 1.3888(12) ?
C5 H5 . 0.963(16) ?
C6 C7 . 1.5176(13) ?
C8 C9 . 1.5162(12) ?
C9 C10 . 1.3925(13) ?
C10 C11 . 1.3934(13) ?
C10 H10 . 0.965(16) ?
C11 C12 . 1.3984(13) ?
C11 H11 . 0.923(15) ?
C12 C13 . 1.3906(12) ?
C12 H12 . 0.971(15) ?
C13 C14 . 1.5164(12) ?
N3 C15 . 1.3301(12) ?
N3 H3A . 0.873(18) ?
N3 H3B . 0.878(17) ?
N4 C22 . 1.3612(11) ?
N4 C21 . 1.3620(12) ?
N4 H4A . 0.884(17) ?
C15 C27 . 1.4349(12) ?
C15 C16 . 1.4392(13) ?
C16 C21 . 1.4121(12) ?
C16 C17 . 1.4201(13) ?
C17 C18 . 1.3746(14) ?
C17 H17 . 0.934(15) ?
C18 C19 . 1.4115(15) ?
C18 H18 . 0.959(15) ?
C19 C20 . 1.3732(14) ?
C19 H19 . 0.923(17) ?
C20 C21 . 1.4158(12) ?
C20 H20 . 0.974(15) ?
C22 C27 . 1.4124(12) ?
C22 C23 . 1.4158(12) ?
C23 C24 . 1.3692(13) ?
C23 H23 . 0.969(15) ?
C24 C25 . 1.4148(13) ?
C24 H24 . 0.955(16) ?
C25 C26 . 1.3725(13) ?
C25 H25 . 0.968(15) ?
C26 C27 . 1.4240(12) ?
C26 H26 . 0.960(15) ?
N5 C28 . 1.3249(11) ?
N5 H5B . 0.889(17) ?
N5 H5A . 0.894(17) ?
N6 C35 . 1.3606(12) ?
N6 C34 . 1.3613(12) ?
N6 H6A . 0.836(18) ?
C28 C29 . 1.4393(12) ?
C28 C40 . 1.4405(12) ?
C29 C34 . 1.4157(12) ?
C29 C30 . 1.4197(12) ?
C30 C31 . 1.3760(13) ?
C30 H30 . 0.930(15) ?
C31 C32 . 1.4116(14) ?
C31 H31 . 0.947(15) ?
C32 C33 . 1.3717(14) ?
C32 H32 . 0.973(15) ?
C33 C34 . 1.4141(13) ?
C33 H33 . 0.985(16) ?
C35 C40 . 1.4104(12) ?
C35 C36 . 1.4163(13) ?
C36 C37 . 1.3691(14) ?
C36 H36 . 0.950(16) ?
C37 C38 . 1.4116(14) ?
C37 H37 . 0.987(16) ?
C38 C39 . 1.3736(13) ?
C38 H38 . 0.970(15) ?
C39 C40 . 1.4161(12) ?
C39 H39 . 0.963(14) ?
O1W H1A . 0.83(2) ?
O1W H1B . 0.861(19) ?
O2W H2A . 0.813(19) ?
O2W H2B . 0.79(2) ?
O3W H3C . 0.79(2) ?
O3W H3D . 0.856(19) ?
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
_geom_hbond_publ_flag
N3 H3A O2W 2_656 0.873(18) 2.053(18) 2.8793(12) 157.6(16) y
N3 H3B O7 1_656 0.878(17) 2.109(17) 2.9337(11) 156.1(15) y
N4 H4A O6 . 0.884(17) 1.838(17) 2.7214(11) 178.1(16) y
N5 H5A O3 2_655 0.894(17) 1.925(17) 2.7945(11) 163.9(16) y
N5 H5B O5 . 0.889(17) 2.046(17) 2.9096(11) 163.6(15) y
N6 H6A O3W . 0.836(18) 1.863(18) 2.6903(11) 170.3(18) y
O1W H1A O7 . 0.83(2) 1.99(2) 2.8138(11) 171(2) y
O1W H1B O7 2_565 0.861(19) 1.955(19) 2.8161(11) 178.7(17) y
O2W H2A O8 2 0.813(19) 2.067(19) 2.8717(11) 170.1(17) y
O2W H2B O2 . 0.79(2) 2.02(2) 2.8033(11) 177(2) y
O3W H3C O3 1_556 0.79(2) 1.97(2) 2.7595(11) 169.8(19) y
O3W H3D O1W 2_666 0.856(19) 1.879(19) 2.7328(11) 175.4(17) y
C30 H30 O3 2_655 0.931(16) 2.437(16) 3.3386(12) 163(14) y
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 Ni1 O1 C1 . . . . -3.81(7) ?
N2 Ni1 O1 C1 . . . . 173.57(7) ?
O4 Ni1 O1 C1 . . . . -10.03(12) ?
O5 Ni1 O1 C1 . . . . -107.47(7) ?
O8 Ni1 O1 C1 . . . . 96.69(7) ?
N1 Ni1 O4 C7 . . . . -1.21(7) ?
N2 Ni1 O4 C7 . . . . -178.46(7) ?
O1 Ni1 O4 C7 . . . . 5.00(12) ?
O5 Ni1 O4 C7 . . . . 103.41(7) ?
O8 Ni1 O4 C7 . . . . -101.19(7) ?
N1 Ni1 O5 C8 . . . . 170.05(6) ?
N2 Ni1 O5 C8 . . . . -4.26(6) ?
O1 Ni1 O5 C8 . . . . -110.90(6) ?
O4 Ni1 O5 C8 . . . . 92.18(6) ?
O8 Ni1 O5 C8 . . . . -7.38(11) ?
N1 Ni1 O8 C14 . . . . -177.64(6) ?
N2 Ni1 O8 C14 . . . . -3.33(6) ?
O1 Ni1 O8 C14 . . . . 103.77(7) ?
O4 Ni1 O8 C14 . . . . -98.56(7) ?
O5 Ni1 O8 C14 . . . . -0.19(11) ?
O1 Ni1 N1 C2 . . . . 3.91(7) ?
O4 Ni1 N1 C2 . . . . -178.59(7) ?
O5 Ni1 N1 C2 . . . . 95.16(7) ?
O8 Ni1 N1 C2 . . . . -85.94(7) ?
O1 Ni1 N1 C6 . . . . -177.21(7) ?
O4 Ni1 N1 C6 . . . . 0.29(7) ?
O5 Ni1 N1 C6 . . . . -85.96(7) ?
O8 Ni1 N1 C6 . . . . 92.93(7) ?
O1 Ni1 N2 C9 . . . . 97.94(7) ?
O4 Ni1 N2 C9 . . . . -80.63(7) ?
O5 Ni1 N2 C9 . . . . 7.33(6) ?
O8 Ni1 N2 C9 . . . . -174.02(7) ?
O1 Ni1 N2 C13 . . . . -90.26(7) ?
O4 Ni1 N2 C13 . . . . 91.17(7) ?
O5 Ni1 N2 C13 . . . . 179.13(7) ?
O8 Ni1 N2 C13 . . . . -2.22(6) ?
Ni1 O1 C1 O2 . . . . -178.27(8) ?
Ni1 O1 C1 C2 . . . . 3.09(10) ?
C6 N1 C2 C3 . . . . -0.99(14) ?
Ni1 N1 C2 C3 . . . . 177.85(7) ?
C6 N1 C2 C1 . . . . 177.73(8) ?
Ni1 N1 C2 C1 . . . . -3.44(10) ?
O2 C1 C2 N1 . . . . -178.73(9) ?
O1 C1 C2 N1 . . . . 0.02(12) ?
O2 C1 C2 C3 . . . . -0.13(15) ?
O1 C1 C2 C3 . . . . 178.62(9) ?
N1 C2 C3 C4 . . . . 1.59(15) ?
C1 C2 C3 C4 . . . . -176.92(9) ?
C2 C3 C4 C5 . . . . -0.51(15) ?
C3 C4 C5 C6 . . . . -1.13(15) ?
C2 N1 C6 C5 . . . . -0.74(14) ?
Ni1 N1 C6 C5 . . . . -179.58(7) ?
C2 N1 C6 C7 . . . . 179.35(8) ?
Ni1 N1 C6 C7 . . . . 0.52(10) ?
C4 C5 C6 N1 . . . . 1.78(14) ?
C4 C5 C6 C7 . . . . -178.33(9) ?
Ni1 O4 C7 O3 . . . . -178.14(8) ?
Ni1 O4 C7 C6 . . . . 1.82(10) ?
N1 C6 C7 O3 . . . . 178.38(8) ?
C5 C6 C7 O3 . . . . -1.52(14) ?
N1 C6 C7 O4 . . . . -1.58(12) ?
C5 C6 C7 O4 . . . . 178.52(9) ?
Ni1 O5 C8 O6 . . . . 179.89(8) ?
Ni1 O5 C8 C9 . . . . 0.92(10) ?
C13 N2 C9 C10 . . . . 0.07(13) ?
Ni1 N2 C9 C10 . . . . 171.76(7) ?
C13 N2 C9 C8 . . . . 179.37(8) ?
Ni1 N2 C9 C8 . . . . -8.94(10) ?
O6 C8 C9 N2 . . . . -174.13(8) ?
O5 C8 C9 N2 . . . . 4.96(12) ?
O6 C8 C9 C10 . . . . 5.13(14) ?
O5 C8 C9 C10 . . . . -175.78(9) ?
N2 C9 C10 C11 . . . . -0.28(13) ?
C8 C9 C10 C11 . . . . -179.49(8) ?
C9 C10 C11 C12 . . . . 0.39(14) ?
C10 C11 C12 C13 . . . . -0.31(13) ?
C9 N2 C13 C12 . . . . 0.02(13) ?
Ni1 N2 C13 C12 . . . . -171.51(7) ?
C9 N2 C13 C14 . . . . 178.01(8) ?
Ni1 N2 C13 C14 . . . . 6.49(10) ?
C11 C12 C13 N2 . . . . 0.10(13) ?
C11 C12 C13 C14 . . . . -177.60(8) ?
Ni1 O8 C14 O7 . . . . -172.58(7) ?
Ni1 O8 C14 C13 . . . . 7.53(10) ?
N2 C13 C14 O7 . . . . 170.84(8) ?
C12 C13 C14 O7 . . . . -11.29(14) ?
N2 C13 C14 O8 . . . . -9.27(11) ?
C12 C13 C14 O8 . . . . 168.60(9) ?
N3 C15 C16 C21 . . . . -177.27(9) ?
C27 C15 C16 C21 . . . . 2.02(13) ?
N3 C15 C16 C17 . . . . 0.48(14) ?
C27 C15 C16 C17 . . . . 179.76(9) ?
C21 C16 C17 C18 . . . . 0.23(14) ?
C15 C16 C17 C18 . . . . -177.54(9) ?
C16 C17 C18 C19 . . . . -0.57(16) ?
C17 C18 C19 C20 . . . . 0.39(16) ?
C18 C19 C20 C21 . . . . 0.13(15) ?
C22 N4 C21 C16 . . . . 0.55(13) ?
C22 N4 C21 C20 . . . . -179.16(8) ?
C17 C16 C21 N4 . . . . -179.41(8) ?
C15 C16 C21 N4 . . . . -1.56(13) ?
C17 C16 C21 C20 . . . . 0.30(13) ?
C15 C16 C21 C20 . . . . 178.15(8) ?
C19 C20 C21 N4 . . . . 179.24(9) ?
C19 C20 C21 C16 . . . . -0.48(14) ?
C21 N4 C22 C27 . . . . -0.01(13) ?
C21 N4 C22 C23 . . . . -179.65(8) ?
N4 C22 C23 C24 . . . . -179.61(8) ?
C27 C22 C23 C24 . . . . 0.74(13) ?
C22 C23 C24 C25 . . . . -0.06(14) ?
C23 C24 C25 C26 . . . . -0.96(14) ?
C24 C25 C26 C27 . . . . 1.28(14) ?
N4 C22 C27 C26 . . . . 179.94(8) ?
C23 C22 C27 C26 . . . . -0.42(13) ?
N4 C22 C27 C15 . . . . 0.51(13) ?
C23 C22 C27 C15 . . . . -179.85(8) ?
C25 C26 C27 C22 . . . . -0.60(13) ?
C25 C26 C27 C15 . . . . 178.82(9) ?
N3 C15 C27 C22 . . . . 177.79(8) ?
C16 C15 C27 C22 . . . . -1.50(12) ?
N3 C15 C27 C26 . . . . -1.62(14) ?
C16 C15 C27 C26 . . . . 179.09(8) ?
N5 C28 C29 C34 . . . . 176.98(8) ?
C40 C28 C29 C34 . . . . -4.17(12) ?
N5 C28 C29 C30 . . . . -2.62(14) ?
C40 C28 C29 C30 . . . . 176.22(8) ?
C34 C29 C30 C31 . . . . 1.09(13) ?
C28 C29 C30 C31 . . . . -179.30(9) ?
C29 C30 C31 C32 . . . . -0.67(14) ?
C30 C31 C32 C33 . . . . -0.61(14) ?
C31 C32 C33 C34 . . . . 1.41(14) ?
C35 N6 C34 C33 . . . . -176.15(8) ?
C35 N6 C34 C29 . . . . 4.00(13) ?
C32 C33 C34 N6 . . . . 179.19(8) ?
C32 C33 C34 C29 . . . . -0.96(13) ?
C30 C29 C34 N6 . . . . 179.57(8) ?
C28 C29 C34 N6 . . . . -0.06(13) ?
C30 C29 C34 C33 . . . . -0.28(13) ?
C28 C29 C34 C33 . . . . -179.91(8) ?
C34 N6 C35 C40 . . . . -3.45(13) ?
C34 N6 C35 C36 . . . . 175.03(8) ?
N6 C35 C36 C37 . . . . -176.16(9) ?
C40 C35 C36 C37 . . . . 2.32(14) ?
C35 C36 C37 C38 . . . . 0.56(15) ?
C36 C37 C38 C39 . . . . -2.15(15) ?
C37 C38 C39 C40 . . . . 0.84(15) ?
N6 C35 C40 C39 . . . . 174.90(8) ?
C36 C35 C40 C39 . . . . -3.55(13) ?
N6 C35 C40 C28 . . . . -1.02(13) ?
C36 C35 C40 C28 . . . . -179.47(8) ?
C38 C39 C40 C35 . . . . 1.97(13) ?
C38 C39 C40 C28 . . . . 177.75(9) ?
N5 C28 C40 C35 . . . . -176.42(8) ?
C29 C28 C40 C35 . . . . 4.71(12) ?
N5 C28 C40 C39 . . . . 7.83(13) ?
C29 C28 C40 C39 . . . . -171.04(8) ?
