#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/71/2017192.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_2017192
loop_
_publ_author_name
'Atria, Ana María'
'Corsini, Gino'
'González, Lissette'
'Garland, Maria Teresa'
'Baggio, Ricardo'
_publ_section_title
;
 Two polymeric nickel(II) complexes with aromatic
 benzene-1,2,4,5-tetracarboxylate and pyridine-2,5-dicarboxylate
 linkers
;
_journal_coeditor_code           LN3133
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m250
_journal_page_last               m254
_journal_paper_doi               10.1107/S0108270109021404
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni2 (C7 H3 N O4)2 (C5 H14 N2)3] , 8H2 O'
_chemical_formula_moiety         'C29 H48 N8 Ni2 O8 , 8H2 O'
_chemical_formula_sum            'C29 H64 N8 Ni2 O16'
_chemical_formula_weight         898.30
_chemical_name_systematic
;
catena-poly[[[bis(2,2-methylpropane-1,3-amine-
κ²N,N')nickel(II)]-μ-pyridine-2,5-dicarboxylato-
κ³O⁵:N,O²-[(2,2-methylpropane-1,3-amine-
κ²N,N')nickel(II)]-μ-pyridine-2,5-dicarboxylato-
κ³N,O²:O⁵]octahydrate]
;
_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                105.25(3)
_cell_angle_beta                 98.02(2)
_cell_angle_gamma                111.25(3)
_cell_formula_units_Z            2
_cell_length_a                   12.269(3)
_cell_length_b                   13.622(3)
_cell_length_c                   15.171(4)
_cell_measurement_reflns_used    6745
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      1.90
_cell_volume                     2200.8(12)
_computing_cell_refinement       'SAINT-NT (Bruker, 2002)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL-NT (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker SMART? CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.038
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18893
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            light_green
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         9619
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1169P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1917
_reflns_number_gt                6322
_reflns_number_total             9619
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ln3133.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017192
_cod_database_fobs_code          2017192
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 0.5000 1.0000 0.5000 0.0474(2) Uani d S 1 . .
Ni Ni2 0.0000 0.0000 0.0000 0.0493(2) Uani d S 1 . .
Ni Ni3 0.53879(4) 0.48684(4) 0.25151(3) 0.04313(16) Uani d . 1 . .
C C11 0.2278(4) 0.9174(5) 0.4843(5) 0.110(2) Uani d DU 1 . .
H H11A 0.1519 0.9001 0.4412 0.132 Uiso calc R 1 . .
H H11B 0.2321 0.9677 0.5446 0.132 Uiso calc R 1 . .
C C21 0.2216(4) 0.8128(4) 0.4981(3) 0.0728(12) Uani d DU 1 . .
C C31 0.3240(4) 0.8214(6) 0.5656(5) 0.114(2) Uani d DU 1 . .
H H31A 0.3289 0.8693 0.6273 0.137 Uiso calc R 1 . .
H H31B 0.3068 0.7476 0.5695 0.137 Uiso calc R 1 . .
C C41 0.2059(6) 0.7275(5) 0.4029(4) 0.129(2) Uani d DU 1 . .
H H41A 0.2022 0.7598 0.3540 0.194 Uiso calc R 1 . .
H H41B 0.1323 0.6618 0.3886 0.194 Uiso calc R 1 . .
H H41C 0.2734 0.7075 0.4064 0.194 Uiso calc R 1 . .
C C51 0.1089(5) 0.7611(7) 0.5320(6) 0.158(3) Uani d DU 1 . .
H H51A 0.0416 0.7672 0.4971 0.237 Uiso calc R 1 . .
H H51B 0.1243 0.8001 0.5982 0.237 Uiso calc R 1 . .
H H51C 0.0905 0.6835 0.5218 0.237 Uiso calc R 1 . .
N N11 0.3248(3) 0.9781(3) 0.4490(3) 0.0694(10) Uani d D 1 . .
H H11C 0.3262 1.0467 0.4587 0.083 Uiso calc R 1 . .
H H11D 0.3041 0.9436 0.3859 0.083 Uiso calc R 1 . .
N N21 0.4415(3) 0.8636(3) 0.5476(3) 0.0598(9) Uani d D 1 . .
H H21C 0.4458 0.8060 0.5048 0.072 Uiso calc R 1 . .
H H21D 0.4966 0.8813 0.6016 0.072 Uiso calc R 1 . .
C C12 0.1212(4) -0.1630(3) 0.0135(4) 0.0700(12) Uani d DU 1 . .
H H12A 0.1990 -0.1666 0.0269 0.084 Uiso calc R 1 . .
H H12B 0.0775 -0.2127 -0.0508 0.084 Uiso calc R 1 . .
C C22 0.0523(4) -0.2050(3) 0.0790(3) 0.0726(12) Uani d DU 1 . .
C C32 -0.0740(4) -0.2122(3) 0.0554(4) 0.0703(12) Uani d DU 1 . .
H H32A -0.1123 -0.2581 -0.0106 0.084 Uiso calc R 1 . .
H H32B -0.1193 -0.2505 0.0930 0.084 Uiso calc R 1 . .
C C42 0.1152(5) -0.1298(6) 0.1825(3) 0.113(2) Uani d DU 1 . .
H H42A 0.1150 -0.0574 0.1916 0.169 Uiso calc R 1 . .
H H42B 0.1973 -0.1219 0.1976 0.169 Uiso calc R 1 . .
H H42C 0.0728 -0.1630 0.2232 0.169 Uiso calc R 1 . .
C C52 0.0451(6) -0.3229(4) 0.0680(5) 0.119(2) Uani d DU 1 . .
H H52A 0.0288 -0.3643 0.0022 0.179 Uiso calc R 1 . .
H H52B -0.0188 -0.3611 0.0931 0.179 Uiso calc R 1 . .
H H52C 0.1207 -0.3169 0.1018 0.179 Uiso calc R 1 . .
N N12 0.1419(3) -0.0491(3) 0.0187(3) 0.0614(9) Uani d D 1 . .
H H12C 0.1826 -0.0338 -0.0244 0.074 Uiso calc R 1 . .
H H12D 0.1925 -0.0036 0.0759 0.074 Uiso calc R 1 . .
N N22 -0.0846(3) -0.1058(3) 0.0706(3) 0.0627(9) Uani d D 1 . .
H H22C -0.0560 -0.0668 0.1331 0.075 Uiso calc R 1 . .
H H22D -0.1641 -0.1214 0.0552 0.075 Uiso calc R 1 . .
C C23 0.7925(4) 0.4348(4) 0.2547(3) 0.0683(11) Uani d DU 1 . .
C C13" 0.7867(12) 0.5169(12) 0.2105(11) 0.100(5) Uani d PDU 0.528(7) A 1
H H13A 0.8674 0.5767 0.2291 0.120 Uiso calc PR 0.528(7) A 1
H H13B 0.7670 0.4807 0.1425 0.120 Uiso calc PR 0.528(7) A 1
C C33" 0.6774(7) 0.3400(7) 0.2414(7) 0.082(3) Uani d PDU 0.528(7) A 1
H H33A 0.6401 0.3023 0.1740 0.098 Uiso calc PR 0.528(7) A 1
H H33B 0.6952 0.2872 0.2663 0.098 Uiso calc PR 0.528(7) A 1
C C43" 0.8419(10) 0.4940(10) 0.3629(4) 0.107(4) Uani d PDU 0.528(7) A 1
H H43A 0.7926 0.5308 0.3858 0.160 Uiso calc PR 0.528(7) A 1
H H43B 0.9238 0.5485 0.3773 0.160 Uiso calc PR 0.528(7) A 1
H H43C 0.8398 0.4397 0.3928 0.160 Uiso calc PR 0.528(7) A 1
C C53" 0.8884(14) 0.3903(19) 0.2362(16) 0.131(7) Uani d PDU 0.528(7) A 1
H H53A 0.8612 0.3369 0.1732 0.196 Uiso calc PR 0.528(7) A 1
H H53B 0.9009 0.3547 0.2811 0.196 Uiso calc PR 0.528(7) A 1
H H53C 0.9631 0.4514 0.2426 0.196 Uiso calc PR 0.528(7) A 1
C C13' 0.8102(7) 0.5487(9) 0.2553(12) 0.080(4) Uani d PDU 0.472(7) A 2
H H13C 0.8558 0.6008 0.3185 0.096 Uiso calc PR 0.472(7) A 2
H H13D 0.8604 0.5675 0.2130 0.096 Uiso calc PR 0.472(7) A 2
C C33' 0.7189(5) 0.3965(10) 0.3154(7) 0.070(3) Uani d PDU 0.472(7) A 2
H H33C 0.7516 0.4543 0.3774 0.084 Uiso calc PR 0.472(7) A 2
H H33D 0.7275 0.3309 0.3227 0.084 Uiso calc PR 0.472(7) A 2
C C43' 0.7372(10) 0.3549(8) 0.1512(4) 0.087(3) Uani d PDU 0.472(7) A 2
H H43D 0.6531 0.3398 0.1325 0.131 Uiso calc PR 0.472(7) A 2
H H43E 0.7450 0.2861 0.1458 0.131 Uiso calc PR 0.472(7) A 2
H H43F 0.7792 0.3892 0.1109 0.131 Uiso calc PR 0.472(7) A 2
C C53' 0.9201(11) 0.441(2) 0.2845(15) 0.105(5) Uani d PDU 0.472(7) A 2
H H53D 0.9439 0.4600 0.3520 0.158 Uiso calc PR 0.472(7) A 2
H H53E 0.9761 0.4966 0.2658 0.158 Uiso calc PR 0.472(7) A 2
H H53F 0.9200 0.3692 0.2545 0.158 Uiso calc PR 0.472(7) A 2
N N13 0.7037(3) 0.5685(3) 0.2290(3) 0.0590(8) Uani d D 1 . .
H H13G 0.6889 0.5914 0.1800 0.071 Uiso calc PR 0.528(7) A 1
H H13H 0.7447 0.6308 0.2802 0.071 Uiso calc PR 0.528(7) A 1
H H13I 0.7261 0.6419 0.2593 0.071 Uiso d PR 0.472(7) A 2
H H13J 0.6896 0.5585 0.1668 0.071 Uiso d PR 0.472(7) A 2
N N23 0.5900(3) 0.3683(3) 0.2855(2) 0.0579(8) Uani d D 1 . .
H H23G 0.6206 0.3932 0.3487 0.069 Uiso calc PR 0.528(7) A 1
H H23H 0.5226 0.3048 0.2707 0.069 Uiso calc PR 0.528(7) A 1
H H23I 0.5556 0.3051 0.2348 0.069 Uiso d PR 0.472(7) A 2
H H23J 0.5571 0.3529 0.3324 0.069 Uiso d PR 0.472(7) A 2
C C14 0.3787(3) 0.4777(3) 0.3734(2) 0.0425(8) Uani d . 1 A .
N N24 0.3803(3) 0.4206(2) 0.28696(19) 0.0427(7) Uani d . 1 . .
C C34 0.2822(3) 0.3301(3) 0.2339(2) 0.0448(8) Uani d . 1 A .
H H34 0.2834 0.2905 0.1741 0.054 Uiso calc R 1 . .
C C44 0.1805(3) 0.2927(3) 0.2629(2) 0.0433(8) Uani d . 1 . .
C C54 0.1781(3) 0.3549(3) 0.3515(3) 0.0527(9) Uani d . 1 A .
H H54 0.1084 0.3319 0.3724 0.063 Uiso calc R 1 . .
C C64 0.2785(3) 0.4498(3) 0.4077(3) 0.0525(9) Uani d . 1 . .
H H64 0.2783 0.4931 0.4664 0.063 Uiso calc R 1 A .
C C74 0.4960(3) 0.5767(3) 0.4324(2) 0.0455(8) Uani d . 1 . .
C C84 0.0768(3) 0.1840(3) 0.2003(3) 0.0511(9) Uani d . 1 A .
O O14 0.5818(2) 0.5884(2) 0.39442(17) 0.0492(6) Uani d . 1 A .
O O24 0.4987(2) 0.6362(2) 0.51062(17) 0.0564(7) Uani d . 1 A .
O O34 0.0932(2) 0.1374(2) 0.1229(2) 0.0655(8) Uani d . 1 . .
O O44 -0.0113(3) 0.1505(3) 0.2299(2) 0.0802(10) Uani d . 1 . .
C C15 0.4217(3) 0.5531(3) 0.1140(2) 0.0470(8) Uani d . 1 A .
N N25 0.4787(3) 0.5941(2) 0.20644(19) 0.0452(7) Uani d . 1 . .
C C35 0.4891(3) 0.6947(3) 0.2576(2) 0.0480(8) Uani d . 1 A .
H H35 0.5295 0.7230 0.3215 0.058 Uiso calc R 1 . .
C C45 0.4436(4) 0.7596(3) 0.2217(3) 0.0523(9) Uani d . 1 . .
C C55 0.3869(4) 0.7171(4) 0.1272(3) 0.0686(12) Uani d . 1 A .
H H55 0.3565 0.7582 0.0994 0.082 Uiso calc R 1 . .
C C65 0.3748(4) 0.6124(4) 0.0728(3) 0.0653(11) Uani d . 1 . .
H H65 0.3350 0.5828 0.0087 0.078 Uiso calc R 1 A .
C C75 0.4143(3) 0.4381(3) 0.0606(3) 0.0492(8) Uani d . 1 . .
C C85 0.4576(4) 0.8713(3) 0.2877(3) 0.0594(10) Uani d . 1 A .
O O15 0.4644(2) 0.3942(2) 0.10753(17) 0.0495(6) Uani d . 1 A .
O O25 0.3604(2) 0.3933(2) -0.02580(17) 0.0631(8) Uani d . 1 A .
O O35 0.4935(3) 0.8881(3) 0.3746(2) 0.0716(8) Uani d . 1 . .
O O45 0.4301(4) 0.9348(3) 0.2541(2) 0.0934(12) Uani d . 1 . .
O O1W 0.2874(4) 0.1899(4) 0.8222(3) 0.1322(18) Uani d . 1 . .
O O2W 0.6800(3) 0.8342(3) 0.6318(2) 0.0779(9) Uani d . 1 . .
O O3W 0.6088(4) 0.8852(3) 0.7944(3) 0.1130(13) Uani d . 1 . .
O O4W 0.6150(5) 0.8356(3) 0.9608(3) 0.1285(16) Uani d . 1 . .
O O5W 0.1007(5) 0.1392(4) 0.6761(4) 0.1458(19) Uani d . 1 . .
O O6W 0.9254(3) 0.9186(3) 0.6268(2) 0.0927(11) Uani d . 1 . .
O O7WA 0.1872(12) 0.2494(8) 0.5574(9) 0.098(3) Uani d P 0.60 . .
O O7WB 0.2144(19) 0.2054(13) 0.5488(15) 0.108(6) Uani d P 0.40 . .
O O8WA 0.7454(9) 0.0318(9) 0.1592(8) 0.095(3) Uiso d P 0.40 . .
O O8WB 0.7536(16) 0.0159(15) 0.2079(14) 0.082(5) Uiso d P 0.20 . .
O O8WC 0.5439(15) -0.0230(15) 0.0975(12) 0.081(5) Uiso d P 0.20 . .
O O8WD 0.440(3) -0.096(3) -0.002(2) 0.081(9) Uiso d P 0.10 . .
O O8WE 0.540(3) 0.036(3) 0.156(2) 0.072(8) Uiso d P 0.10 . .
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
N11 Ni1 N11 . 2_676 180.0000(10) ?
N11 Ni1 O35 . 2_676 88.17(15) ?
N11 Ni1 O35 2_676 2_676 91.83(15) ?
N11 Ni1 O35 . . 91.83(15) ?
N11 Ni1 O35 2_676 . 88.17(15) ?
O35 Ni1 O35 2_676 . 180.0000(10) ?
N11 Ni1 N21 . 2_676 87.73(13) ?
N11 Ni1 N21 2_676 2_676 92.27(13) ?
O35 Ni1 N21 2_676 2_676 86.77(14) ?
O35 Ni1 N21 . 2_676 93.23(14) ?
N11 Ni1 N21 . . 92.27(13) ?
N11 Ni1 N21 2_676 . 87.73(13) ?
O35 Ni1 N21 2_676 . 93.23(14) ?
O35 Ni1 N21 . . 86.77(14) ?
N21 Ni1 N21 2_676 . 180.0000(10) ?
O34 Ni2 O34 . 2 180.0(2) ?
O34 Ni2 N22 . 2 85.95(13) ?
O34 Ni2 N22 2 2 94.05(13) ?
O34 Ni2 N22 . . 94.05(13) ?
O34 Ni2 N22 2 . 85.95(13) ?
N22 Ni2 N22 2 . 180.00(16) ?
O34 Ni2 N12 . 2 90.71(13) ?
O34 Ni2 N12 2 2 89.29(13) ?
N22 Ni2 N12 2 2 87.43(13) ?
N22 Ni2 N12 . 2 92.57(13) ?
O34 Ni2 N12 . . 89.29(13) ?
O34 Ni2 N12 2 . 90.71(13) ?
N22 Ni2 N12 2 . 92.57(13) ?
N22 Ni2 N12 . . 87.43(13) ?
N12 Ni2 N12 2 . 180.0(2) ?
N24 Ni3 N13 . . 173.68(12) ?
N24 Ni3 N25 . . 89.51(12) ?
N13 Ni3 N25 . . 88.89(13) ?
N24 Ni3 N23 . . 89.68(12) ?
N13 Ni3 N23 . . 92.43(13) ?
N25 Ni3 N23 . . 175.03(12) ?
N24 Ni3 O15 . . 94.21(11) ?
N13 Ni3 O15 . . 91.52(13) ?
N25 Ni3 O15 . . 79.76(11) ?
N23 Ni3 O15 . . 95.41(12) ?
N24 Ni3 O14 . . 77.88(11) ?
N13 Ni3 O14 . . 96.03(13) ?
N25 Ni3 O14 . . 90.93(11) ?
N23 Ni3 O14 . . 93.69(12) ?
O15 Ni3 O14 . . 167.91(10) ?
N11 C11 C21 . . 119.1(4) ?
N11 C11 H11A . . 107.6 ?
C21 C11 H11A . . 107.6 ?
N11 C11 H11B . . 107.6 ?
C21 C11 H11B . . 107.6 ?
H11A C11 H11B . . 107.0 ?
C31 C21 C11 . . 116.6(5) ?
C31 C21 C41 . . 107.8(5) ?
C11 C21 C41 . . 109.4(5) ?
C31 C21 C51 . . 106.5(4) ?
C11 C21 C51 . . 109.7(4) ?
C41 C21 C51 . . 106.4(5) ?
N21 C31 C21 . . 117.6(4) ?
N21 C31 H31A . . 107.9 ?
C21 C31 H31A . . 107.9 ?
N21 C31 H31B . . 107.9 ?
C21 C31 H31B . . 107.9 ?
H31A C31 H31B . . 107.2 ?
C21 C41 H41A . . 109.5 ?
C21 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
C21 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
C21 C51 H51A . . 109.5 ?
C21 C51 H51B . . 109.5 ?
H51A C51 H51B . . 109.5 ?
C21 C51 H51C . . 109.5 ?
H51A C51 H51C . . 109.5 ?
H51B C51 H51C . . 109.5 ?
C11 N11 Ni1 . . 120.7(3) ?
C11 N11 H11C . . 107.2 ?
Ni1 N11 H11C . . 107.2 ?
C11 N11 H11D . . 107.2 ?
Ni1 N11 H11D . . 107.2 ?
H11C N11 H11D . . 106.8 ?
C31 N21 Ni1 . . 121.9(3) ?
C31 N21 H21C . . 106.8 ?
Ni1 N21 H21C . . 106.8 ?
C31 N21 H21D . . 106.8 ?
Ni1 N21 H21D . . 106.8 ?
H21C N21 H21D . . 106.7 ?
N12 C12 C22 . . 115.0(4) ?
N12 C12 H12A . . 108.5 ?
C22 C12 H12A . . 108.5 ?
N12 C12 H12B . . 108.5 ?
C22 C12 H12B . . 108.5 ?
H12A C12 H12B . . 107.5 ?
C12 C22 C32 . . 111.0(4) ?
C12 C22 C42 . . 111.7(4) ?
C32 C22 C42 . . 108.8(4) ?
C12 C22 C52 . . 107.9(4) ?
C32 C22 C52 . . 108.9(4) ?
C42 C22 C52 . . 108.5(5) ?
N22 C32 C22 . . 116.3(3) ?
N22 C32 H32A . . 108.2 ?
C22 C32 H32A . . 108.2 ?
N22 C32 H32B . . 108.2 ?
C22 C32 H32B . . 108.2 ?
H32A C32 H32B . . 107.4 ?
C22 C42 H42A . . 109.5 ?
C22 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C22 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
C22 C52 H52A . . 109.5 ?
C22 C52 H52B . . 109.5 ?
H52A C52 H52B . . 109.5 ?
C22 C52 H52C . . 109.5 ?
H52A C52 H52C . . 109.5 ?
H52B C52 H52C . . 109.5 ?
C12 N12 Ni2 . . 122.2(3) ?
C12 N12 H12C . . 106.8 ?
Ni2 N12 H12C . . 106.8 ?
C12 N12 H12D . . 106.8 ?
Ni2 N12 H12D . . 106.8 ?
H12C N12 H12D . . 106.6 ?
C32 N22 Ni2 . . 119.4(3) ?
C32 N22 H22C . . 107.5 ?
Ni2 N22 H22C . . 107.5 ?
C32 N22 H22D . . 107.5 ?
Ni2 N22 H22D . . 107.5 ?
H22C N22 H22D . . 107.0 ?
C13" C23 C33" . . 116.8(8) ?
C33' C23 C13' . . 113.3(8) ?
C13" C23 C53" . . 116.0(12) ?
C33" C23 C53" . . 108.9(10) ?
C33' C23 C53' . . 111.7(11) ?
C13' C23 C53' . . 105.8(11) ?
C33' C23 C43' . . 111.4(7) ?
C13' C23 C43' . . 107.6(8) ?
C53' C23 C43' . . 106.6(8) ?
C13" C23 C43" . . 108.9(8) ?
C33" C23 C43" . . 105.1(6) ?
C53" C23 C43" . . 99.1(10) ?
N13 C13" C23 . . 119.6(7) ?
N23 C33" C23 . . 115.7(5) ?
N13 C13' C23 . . 118.3(7) ?
C23 C33' N23 . . 117.3(5) ?
C13" N13 Ni3 . . 123.1(6) ?
C13' N13 Ni3 . . 124.5(5) ?
C33" N23 Ni3 . . 117.8(5) ?
C33' N23 Ni3 . . 118.1(5) ?
N24 C14 C64 . . 123.2(3) ?
N24 C14 C74 . . 116.0(3) ?
C64 C14 C74 . . 120.9(3) ?
C34 N24 C14 . . 118.7(3) ?
C34 N24 Ni3 . . 126.7(2) ?
C14 N24 Ni3 . . 114.6(2) ?
N24 C34 C44 . . 122.7(3) ?
N24 C34 H34 . . 118.6 ?
C44 C34 H34 . . 118.6 ?
C34 C44 C54 . . 118.2(3) ?
C34 C44 C84 . . 118.7(3) ?
C54 C44 C84 . . 123.0(3) ?
C64 C54 C44 . . 120.2(3) ?
C64 C54 H54 . . 119.9 ?
C44 C54 H54 . . 119.9 ?
C14 C64 C54 . . 116.9(3) ?
C14 C64 H64 . . 121.6 ?
C54 C64 H64 . . 121.6 ?
O24 C74 O14 . . 127.0(3) ?
O24 C74 C14 . . 119.1(3) ?
O14 C74 C14 . . 113.9(3) ?
O44 C84 O34 . . 127.4(4) ?
O44 C84 C44 . . 117.1(4) ?
O34 C84 C44 . . 115.5(3) ?
C74 O14 Ni3 . . 116.7(2) ?
C84 O34 Ni2 . . 139.8(3) ?
N25 C15 C65 . . 121.1(3) ?
N25 C15 C75 . . 115.0(3) ?
C65 C15 C75 . . 124.0(3) ?
C35 N25 C15 . . 118.3(3) ?
C35 N25 Ni3 . . 128.2(2) ?
C15 N25 Ni3 . . 113.4(2) ?
N25 C35 C45 . . 124.2(3) ?
N25 C35 H35 . . 117.9 ?
C45 C35 H35 . . 117.9 ?
C55 C45 C35 . . 116.6(4) ?
C55 C45 C85 . . 124.0(4) ?
C35 C45 C85 . . 119.4(3) ?
C45 C55 C65 . . 120.1(4) ?
C45 C55 H55 . . 120.0 ?
C65 C55 H55 . . 120.0 ?
C15 C65 C55 . . 119.7(4) ?
C15 C65 H65 . . 120.2 ?
C55 C65 H65 . . 120.2 ?
O25 C75 O15 . . 124.3(4) ?
O25 C75 C15 . . 118.7(4) ?
O15 C75 C15 . . 117.0(3) ?
O45 C85 O35 . . 125.8(4) ?
O45 C85 C45 . . 119.3(4) ?
O35 C85 C45 . . 114.9(4) ?
C75 O15 Ni3 . . 114.7(2) ?
C85 O35 Ni1 . . 135.6(3) ?
O8WE O8WC O8WD . . 127(3) ?
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 N11 . 2.064(3) ?
Ni1 N11 2_676 2.064(3) ?
Ni1 O35 2_676 2.073(3) ?
Ni1 O35 . 2.073(3) ?
Ni1 N21 2_676 2.091(3) ?
Ni1 N21 . 2.091(3) ?
Ni2 O34 . 2.076(3) ?
Ni2 O34 2 2.076(3) ?
Ni2 N22 2 2.083(3) ?
Ni2 N22 . 2.083(3) ?
Ni2 N12 2 2.089(3) ?
Ni2 N12 . 2.089(3) ?
Ni3 N24 . 2.040(3) ?
Ni3 N13 . 2.052(3) ?
Ni3 N25 . 2.076(3) ?
Ni3 N23 . 2.086(3) ?
Ni3 O15 . 2.087(3) ?
Ni3 O14 . 2.113(3) ?
C11 N11 . 1.444(4) ?
C11 C21 . 1.470(6) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C21 C31 . 1.454(6) ?
C21 C41 . 1.534(4) ?
C21 C51 . 1.534(7) ?
C31 N21 . 1.441(4) ?
C31 H31A . 0.9700 ?
C31 H31B . 0.9700 ?
C41 H41A . 0.9600 ?
C41 H41B . 0.9600 ?
C41 H41C . 0.9600 ?
C51 H51A . 0.9600 ?
C51 H51B . 0.9600 ?
C51 H51C . 0.9600 ?
N11 H11C . 0.9000 ?
N11 H11D . 0.9000 ?
N21 H21C . 0.9000 ?
N21 H21D . 0.9000 ?
C12 N12 . 1.457(4) ?
C12 C22 . 1.488(5) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C22 C32 . 1.502(5) ?
C22 C42 . 1.534(4) ?
C22 C52 . 1.539(4) ?
C32 N22 . 1.463(3) ?
C32 H32A . 0.9700 ?
C32 H32B . 0.9700 ?
C42 H42A . 0.9600 ?
C42 H42B . 0.9600 ?
C42 H42C . 0.9600 ?
C52 H52A . 0.9600 ?
C52 H52B . 0.9600 ?
C52 H52C . 0.9600 ?
N12 H12C . 0.9000 ?
N12 H12D . 0.9000 ?
N22 H22C . 0.9000 ?
N22 H22D . 0.9000 ?
C23 C33' . 1.443(7) ?
C23 C13" . 1.464(9) ?
C23 C33" . 1.471(8) ?
C23 C13' . 1.483(9) ?
C23 C53" . 1.533(4) ?
C23 C53' . 1.534(4) ?
C23 C43' . 1.542(4) ?
C23 C43" . 1.544(4) ?
C13" N13 . 1.450(4) ?
C13" H13A . 0.9700 ?
C13" H13B . 0.9700 ?
C33" N23 . 1.453(4) ?
C33" H33A . 0.9700 ?
C33" H33B . 0.9700 ?
C43" H43A . 0.9600 ?
C43" H43B . 0.9600 ?
C43" H43C . 0.9600 ?
C53" H53A . 0.9600 ?
C53" H53B . 0.9600 ?
C53" H53C . 0.9600 ?
C13' N13 . 1.451(4) ?
C13' H13C . 0.9700 ?
C13' H13D . 0.9700 ?
C33' N23 . 1.456(4) ?
C33' H33C . 0.9700 ?
C33' H33D . 0.9700 ?
C43' H43D . 0.9600 ?
C43' H43E . 0.9600 ?
C43' H43F . 0.9600 ?
C53' H53D . 0.9600 ?
C53' H53E . 0.9600 ?
C53' H53F . 0.9600 ?
N13 H13G . 0.9000 ?
N13 H13H . 0.9000 ?
N13 H13I . 0.8999 ?
N13 H13J . 0.9001 ?
N23 H23G . 0.9000 ?
N23 H23H . 0.9000 ?
N23 H23I . 0.9000 ?
N23 H23J . 0.9000 ?
C14 N24 . 1.344(4) ?
C14 C64 . 1.368(5) ?
C14 C74 . 1.514(5) ?
N24 C34 . 1.323(4) ?
C34 C44 . 1.349(5) ?
C34 H34 . 0.9300 ?
C44 C54 . 1.398(5) ?
C44 C84 . 1.507(5) ?
C54 C64 . 1.374(5) ?
C54 H54 . 0.9300 ?
C64 H64 . 0.9300 ?
C74 O24 . 1.237(4) ?
C74 O14 . 1.250(4) ?
C84 O44 . 1.210(5) ?
C84 O34 . 1.259(5) ?
C15 N25 . 1.342(4) ?
C15 C65 . 1.370(6) ?
C15 C75 . 1.526(5) ?
N25 C35 . 1.335(4) ?
C35 C45 . 1.385(5) ?
C35 H35 . 0.9300 ?
C45 C55 . 1.366(5) ?
C45 C85 . 1.520(5) ?
C55 C65 . 1.388(6) ?
C55 H55 . 0.9300 ?
C65 H65 . 0.9300 ?
C75 O25 . 1.254(4) ?
C75 O15 . 1.268(5) ?
C85 O45 . 1.231(5) ?
C85 O35 . 1.261(5) ?
O7WA O7WB . 0.776(18) ?
O8WA O8WB . 0.826(18) ?
O8WC O8WE . 1.05(3) ?
O8WC O8WD . 1.62(4) ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1W O5W 2.696(7) . . no
O1W O25 2.838(5) . 1_556 no
O2W O3W 2.730(6) . . no
O2W O6W 2.825(5) . . no
O2W O24 2.739(5) . . no
O3W O4W 2.781(7) . . no
O4W O15 2.766(5) . 2_666 no
O5W O7WA 2.725(8) . . no
O5W O7WB 2.685(8) . . no
O5W O6W 2.809(6) . 1_445 no
O6W O44 2.807(5) . 2_666 no
O6W O7WA 2.876(8) . 2_666 no
O6W O7WB 2.672(8) . 2_666 no
O7WA O14 2.730(6) . 2_666 no
O7WB O14 2.822(6) . 2_666 no
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
N11 H11C O2W 2_676 0.90 2.39 3.127(6) 139
N12 H12D O3W 2_666 0.90 2.56 3.423(6) 160
N13 H13G O25 2_665 0.90 2.42 3.297(4) 165
N13 H13H O7WA 2_666 0.90 2.40 3.256(4) 159
N23 H23H O3W 2_666 0.90 2.33 3.196(6) 160
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
N11 C11 C21 C31 . . . . 61.3(8) ?
N11 C11 C21 C41 . . . . -61.3(7) ?
N11 C11 C21 C51 . . . . -177.7(6) ?
C11 C21 C31 N21 . . . . -59.8(8) ?
C41 C21 C31 N21 . . . . 63.6(7) ?
C51 C21 C31 N21 . . . . 177.4(6) ?
C21 C11 N11 Ni1 . . . . -43.2(7) ?
O35 Ni1 N11 C11 2_676 . . . -71.7(4) ?
O35 Ni1 N11 C11 . . . . 108.3(4) ?
N21 Ni1 N11 C11 2_676 . . . -158.6(4) ?
N21 Ni1 N11 C11 . . . . 21.4(4) ?
C21 C31 N21 Ni1 . . . . 42.0(7) ?
N11 Ni1 N21 C31 . . . . -21.4(4) ?
N11 Ni1 N21 C31 2_676 . . . 158.6(4) ?
O35 Ni1 N21 C31 2_676 . . . 66.9(4) ?
O35 Ni1 N21 C31 . . . . -113.1(4) ?
N12 C12 C22 C32 . . . . 63.8(5) ?
N12 C12 C22 C42 . . . . -57.8(5) ?
N12 C12 C22 C52 . . . . -176.9(4) ?
C12 C22 C32 N22 . . . . -66.8(5) ?
C42 C22 C32 N22 . . . . 56.4(6) ?
C52 C22 C32 N22 . . . . 174.5(4) ?
C22 C12 N12 Ni2 . . . . -55.8(5) ?
O34 Ni2 N12 C12 . . . . 130.7(3) ?
O34 Ni2 N12 C12 2 . . . -49.3(3) ?
N22 Ni2 N12 C12 2 . . . -143.4(3) ?
N22 Ni2 N12 C12 . . . . 36.6(3) ?
C22 C32 N22 Ni2 . . . . 58.7(5) ?
O34 Ni2 N22 C32 . . . . -126.0(3) ?
O34 Ni2 N22 C32 2 . . . 54.0(3) ?
N12 Ni2 N22 C32 2 . . . 143.1(3) ?
N12 Ni2 N22 C32 . . . . -36.9(3) ?
C64 C14 N24 C34 . . . . -3.1(5) ?
C74 C14 N24 C34 . . . . 176.8(3) ?
C64 C14 N24 Ni3 . . . . 176.4(3) ?
C74 C14 N24 Ni3 . . . . -3.6(4) ?
N25 Ni3 N24 C34 . . . . 94.7(3) ?
N23 Ni3 N24 C34 . . . . -80.4(3) ?
O15 Ni3 N24 C34 . . . . 15.0(3) ?
O14 Ni3 N24 C34 . . . . -174.2(3) ?
N25 Ni3 N24 C14 . . . . -84.8(3) ?
N23 Ni3 N24 C14 . . . . 100.1(3) ?
O15 Ni3 N24 C14 . . . . -164.5(2) ?
O14 Ni3 N24 C14 . . . . 6.3(2) ?
C14 N24 C34 C44 . . . . 0.1(5) ?
Ni3 N24 C34 C44 . . . . -179.4(3) ?
N24 C34 C44 C54 . . . . 2.2(6) ?
N24 C34 C44 C84 . . . . -175.5(3) ?
C34 C44 C54 C64 . . . . -1.6(6) ?
C84 C44 C54 C64 . . . . 176.0(4) ?
N24 C14 C64 C54 . . . . 3.6(6) ?
C74 C14 C64 C54 . . . . -176.4(3) ?
C44 C54 C64 C14 . . . . -1.1(6) ?
N24 C14 C74 O24 . . . . 176.3(3) ?
C64 C14 C74 O24 . . . . -3.7(5) ?
N24 C14 C74 O14 . . . . -4.0(5) ?
C64 C14 C74 O14 . . . . 176.0(3) ?
C34 C44 C84 O44 . . . . 177.1(4) ?
C54 C44 C84 O44 . . . . -0.4(6) ?
C34 C44 C84 O34 . . . . -1.8(5) ?
C54 C44 C84 O34 . . . . -179.3(4) ?
O24 C74 O14 Ni3 . . . . -170.8(3) ?
C14 C74 O14 Ni3 . . . . 9.5(4) ?
N24 Ni3 O14 C74 . . . . -9.0(3) ?
N13 Ni3 O14 C74 . . . . 169.2(3) ?
N25 Ni3 O14 C74 . . . . 80.3(3) ?
N23 Ni3 O14 C74 . . . . -97.9(3) ?
O15 Ni3 O14 C74 . . . . 40.9(6) ?
O44 C84 O34 Ni2 . . . . 5.7(8) ?
C44 C84 O34 Ni2 . . . . -175.5(3) ?
N22 Ni2 O34 C84 2 . . . 139.9(5) ?
N22 Ni2 O34 C84 . . . . -40.1(5) ?
N12 Ni2 O34 C84 2 . . . 52.5(5) ?
N12 Ni2 O34 C84 . . . . -127.5(5) ?
C65 C15 N25 C35 . . . . -0.3(5) ?
C75 C15 N25 C35 . . . . 179.7(3) ?
C65 C15 N25 Ni3 . . . . 179.1(3) ?
C75 C15 N25 Ni3 . . . . -1.0(4) ?
N24 Ni3 N25 C35 . . . . 86.8(3) ?
O15 Ni3 N25 C35 . . . . -178.8(3) ?
O14 Ni3 N25 C35 . . . . 9.0(3) ?
N24 Ni3 N25 C15 . . . . -92.4(3) ?
N13 Ni3 N25 C15 . . . . 93.7(3) ?
O15 Ni3 N25 C15 . . . . 2.0(2) ?
O14 Ni3 N25 C15 . . . . -170.2(2) ?
C15 N25 C35 C45 . . . . 0.7(5) ?
Ni3 N25 C35 C45 . . . . -178.5(3) ?
N25 C35 C45 C55 . . . . -1.3(6) ?
N25 C35 C45 C85 . . . . 178.1(4) ?
C35 C45 C55 C65 . . . . 1.5(7) ?
C85 C45 C55 C65 . . . . -177.9(4) ?
N25 C15 C65 C55 . . . . 0.5(7) ?
C75 C15 C65 C55 . . . . -179.5(4) ?
C45 C55 C65 C15 . . . . -1.1(7) ?
N25 C15 C75 O25 . . . . 178.7(3) ?
C65 C15 C75 O25 . . . . -1.3(6) ?
N25 C15 C75 O15 . . . . -1.6(5) ?
C65 C15 C75 O15 . . . . 178.4(4) ?
C55 C45 C85 O45 . . . . -9.1(7) ?
C35 C45 C85 O45 . . . . 171.5(4) ?
C55 C45 C85 O35 . . . . 168.4(4) ?
C35 C45 C85 O35 . . . . -10.9(6) ?
O25 C75 O15 Ni3 . . . . -177.0(3) ?
C15 C75 O15 Ni3 . . . . 3.3(4) ?
N24 Ni3 O15 C75 . . . . 85.8(3) ?
N13 Ni3 O15 C75 . . . . -91.6(3) ?
N25 Ni3 O15 C75 . . . . -3.0(2) ?
N23 Ni3 O15 C75 . . . . 175.9(2) ?
O14 Ni3 O15 C75 . . . . 37.2(6) ?
O45 C85 O35 Ni1 . . . . 12.0(8) ?
C45 C85 O35 Ni1 . . . . -165.4(3) ?
N11 Ni1 O35 C85 . . . . 45.5(4) ?
N11 Ni1 O35 C85 2_676 . . . -134.5(4) ?
N21 Ni1 O35 C85 2_676 . . . -42.4(4) ?
N21 Ni1 O35 C85 . . . . 137.6(4) ?
