#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/76/1517654.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_1517654
loop_
_publ_author_name
'Ying-Ying Liu'
'Jie Liu'
'Jin Yang'
'Bo Liu'
'Jian-Fang Ma'
_publ_section_title
;
 Eight coordination compounds based on a reduced Schiff base
 tetraaminodiphenol macrocyclic ligand
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              85
_journal_page_last               96
_journal_volume                  403
_journal_year                    2013
_chemical_formula_sum            'C28 H40 N4 Ni2 O9.5'
_chemical_formula_weight         702.06
_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
_cell_angle_alpha                97.378(16)
_cell_angle_beta                 105.934(14)
_cell_angle_gamma                98.935(18)
_cell_formula_units_Z            2
_cell_length_a                   10.336(4)
_cell_length_b                   12.175(6)
_cell_length_c                   12.760(5)
_cell_measurement_reflns_used    4859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1500.4(11)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14826
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis (Oxford Diffraction, 2006)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0540P)²+1.5282P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                4859
_reflns_number_total             6757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-403-85-96-8.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C28 H40 N4 Ni2 O9.50'
_cod_database_code               1517654
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
Ni1 Ni -0.06986(5) 0.01897(4) -0.11515(3) 0.02036(13) Uani 1 1 d .
Ni2 Ni 0.08633(5) 0.56331(4) 0.44179(3) 0.01985(13) Uani 1 1 d .
C1 C 0.3406(5) -0.2434(4) -0.0950(4) 0.0393(10) Uani 1 1 d .
C2 C 0.2125(4) -0.2446(3) -0.1665(3) 0.0319(9) Uani 1 1 d .
H2 H 0.1778 -0.3010 -0.2291 0.038 Uiso 1 1 calc R
C3 C 0.1323(4) -0.1655(3) -0.1495(3) 0.0266(8) Uani 1 1 d .
C4 C 0.1864(4) -0.0799(3) -0.0550(3) 0.0242(8) Uani 1 1 d .
C5 C 0.3148(4) -0.0794(3) 0.0193(3) 0.0289(8) Uani 1 1 d .
C6 C 0.3897(5) -0.1595(4) -0.0014(4) 0.0394(10) Uani 1 1 d .
H6 H 0.4751 -0.1572 0.0486 0.047 Uiso 1 1 calc R
C7 C 0.4220(6) -0.3321(5) -0.1164(4) 0.0572(14) Uani 1 1 d .
H7A H 0.5079 -0.3176 -0.0586 0.086 Uiso 1 1 calc R
H7B H 0.4390 -0.3298 -0.1864 0.086 Uiso 1 1 calc R
H7C H 0.3708 -0.4055 -0.1178 0.086 Uiso 1 1 calc R
C8 C -0.0091(4) -0.1815(3) -0.2298(3) 0.0287(8) Uani 1 1 d .
H8A H -0.0052 -0.1348 -0.2854 0.034 Uiso 1 1 calc R
H8B H -0.0378 -0.2597 -0.2672 0.034 Uiso 1 1 calc R
C9 C -0.2560(5) -0.1862(4) -0.2517(4) 0.0397(10) Uani 1 1 d .
H9A H -0.3147 -0.2216 -0.2127 0.048 Uiso 1 1 calc R
H9B H -0.2595 -0.2410 -0.3153 0.048 Uiso 1 1 calc R
C10 C -0.3086(4) -0.0844(4) -0.2910(3) 0.0379(10) Uani 1 1 d .
H10A H -0.2658 -0.0604 -0.3453 0.045 Uiso 1 1 calc R
H10B H -0.4071 -0.1047 -0.3262 0.045 Uiso 1 1 calc R
C11 C 0.3661(4) 0.0082(4) 0.1232(3) 0.0341(9) Uani 1 1 d .
H11A H 0.4593 0.0040 0.1627 0.041 Uiso 1 1 calc R
H11B H 0.3672 0.0828 0.1041 0.041 Uiso 1 1 calc R
C12 C -0.0505(4) 0.2678(3) -0.1148(3) 0.0243(8) Uani 1 1 d .
C13 C -0.0213(4) 0.3889(3) -0.0575(3) 0.0217(7) Uani 1 1 d .
C14 C -0.0008(4) 0.4118(3) 0.0567(3) 0.0230(7) Uani 1 1 d .
H14 H -0.0006 0.3520 0.0953 0.028 Uiso 1 1 calc R
C15 C 0.0191(4) 0.5203(3) 0.1140(3) 0.0221(7) Uani 1 1 d .
C16 C 0.0383(4) 0.5323(3) 0.2368(3) 0.0245(8) Uani 1 1 d .
C17 C -0.2943(5) 0.8096(4) 0.4119(3) 0.0400(11) Uani 1 1 d .
C18 C -0.3487(5) 0.7010(4) 0.4203(3) 0.0375(10) Uani 1 1 d .
H18 H -0.4436 0.6774 0.3987 0.045 Uiso 1 1 calc R
C19 C -0.2660(4) 0.6254(3) 0.4601(3) 0.0299(9) Uani 1 1 d .
C20 C -0.1230(4) 0.6608(3) 0.4943(3) 0.0242(8) Uani 1 1 d .
C21 C -0.0660(4) 0.7701(3) 0.4827(3) 0.0271(8) Uani 1 1 d .
C22 C -0.1512(5) 0.8421(4) 0.4421(3) 0.0354(9) Uani 1 1 d .
H22 H -0.1124 0.9138 0.4346 0.042 Uiso 1 1 calc R
C23 C -0.3870(6) 0.8888(5) 0.3673(5) 0.0617(15) Uani 1 1 d .
H23A H -0.3319 0.9602 0.3679 0.093 Uiso 1 1 calc R
H23B H -0.4455 0.9000 0.4130 0.093 Uiso 1 1 calc R
H23C H -0.4424 0.8565 0.2928 0.093 Uiso 1 1 calc R
C24 C 0.0867(4) 0.8061(3) 0.5144(3) 0.0311(9) Uani 1 1 d .
H24A H 0.1097 0.8838 0.5048 0.037 Uiso 1 1 calc R
H24B H 0.1259 0.8031 0.5920 0.037 Uiso 1 1 calc R
C25 C 0.2987(4) 0.7516(4) 0.4852(3) 0.0355(9) Uani 1 1 d .
H25A H 0.3367 0.8321 0.5045 0.043 Uiso 1 1 calc R
H25B H 0.3319 0.7198 0.4263 0.043 Uiso 1 1 calc R
C26 C 0.3462(4) 0.6966(4) 0.5858(4) 0.0383(10) Uani 1 1 d .
H26A H 0.4430 0.6947 0.6004 0.046 Uiso 1 1 calc R
H26B H 0.3348 0.7410 0.6503 0.046 Uiso 1 1 calc R
C27 C 0.3380(4) 0.4916(4) 0.5371(4) 0.0383(10) Uani 1 1 d .
H27A H 0.4301 0.5072 0.5883 0.046 Uiso 1 1 calc R
H27B H 0.3456 0.4941 0.4633 0.046 Uiso 1 1 calc R
C28 C 0.3799(9) 0.5541(10) 0.1430(8) 0.134(4) Uani 1 1 d .
H28A H 0.3671 0.6288 0.1662 0.202 Uiso 1 1 calc R
H28B H 0.3097 0.5193 0.0751 0.202 Uiso 1 1 calc R
H28C H 0.4684 0.5586 0.1316 0.202 Uiso 1 1 calc R
O1 O 0.1191(3) 0.0016(2) -0.02917(18) 0.0227(5) Uani 1 1 d .
O2 O -0.0347(3) 0.5966(2) 0.53809(18) 0.0225(5) Uani 1 1 d .
O3 O -0.1134(3) 0.2454(2) -0.2176(2) 0.0351(7) Uani 1 1 d .
O4 O -0.0124(3) 0.1956(2) -0.05715(18) 0.0250(6) Uani 1 1 d .
O5 O 0.1523(3) 0.5223(2) 0.29991(19) 0.0307(6) Uani 1 1 d .
O6 O -0.0594(3) 0.5475(2) 0.2748(2) 0.0312(6) Uani 1 1 d .
O7 O 0.3714(6) 0.4869(7) 0.2279(5) 0.143(3) Uani 1 1 d .
H7 H 0.3237 0.4243 0.1988 0.214 Uiso 1 1 calc R
N1 N -0.1128(3) -0.1527(3) -0.1772(3) 0.0266(7) Uani 1 1 d D
H1N H -0.111(5) -0.195(4) -0.123(3) 0.040 Uiso 1 1 d D
N2 N -0.2770(3) 0.0093(3) -0.1962(2) 0.0274(7) Uani 1 1 d D
H2N H -0.290(5) 0.074(4) -0.223(3) 0.041 Uiso 1 1 d D
N3 N 0.1483(3) 0.7330(3) 0.4464(2) 0.0269(7) Uani 1 1 d D
H3N H 0.121(5) 0.748(4) 0.383(3) 0.040 Uiso 1 1 d D
N4 N 0.2655(3) 0.5792(3) 0.5666(3) 0.0313(7) Uani 1 1 d D
H4N H 0.249(5) 0.567(4) 0.633(3) 0.047 Uiso 1 1 d D
O1W O -0.0160(4) 0.0578(2) -0.2601(2) 0.0363(7) Uani 1 1 d D
H1A H -0.052(5) 0.119(4) -0.266(4) 0.054 Uiso 1 1 d D
H1B H 0.072(4) 0.083(4) -0.236(4) 0.054 Uiso 1 1 d D
O2W O 0.2545(5) 0.1447(4) -0.1461(4) 0.0816(14) Uani 1 1 d D
H2A H 0.247(8) 0.166(6) -0.078(4) 0.122 Uiso 1 1 d D
H2B H 0.292(7) 0.196(3) -0.168(5) 0.122 Uiso 1 1 d D
O3W O 0.2781(8) 0.3595(7) -0.1663(6) 0.0578(19) Uiso 0.50 1 d PD
H3A H 0.279(6) 0.392(4) -0.108(3) 0.087 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
O1 Ni1 N1 87.84(12) . .
O1 Ni1 O1 84.65(11) . 2
N1 Ni1 O1 94.11(11) . 2
O1 Ni1 N2 169.66(12) . .
N1 Ni1 N2 84.24(13) . .
O1 Ni1 N2 89.28(11) 2 .
O1 Ni1 O4 89.66(10) . .
N1 Ni1 O4 175.36(12) . .
O1 Ni1 O4 89.55(10) 2 .
N2 Ni1 O4 98.68(12) . .
O1 Ni1 O1W 96.05(12) . .
N1 Ni1 O1W 91.42(12) . .
O1 Ni1 O1W 174.45(10) 2 .
N2 Ni1 O1W 90.79(13) . .
O4 Ni1 O1W 84.96(10) . .
O2 Ni2 O2 84.20(10) 2_566 .
O2 Ni2 N4 88.40(12) 2_566 .
O2 Ni2 N4 97.63(13) . .
O2 Ni2 N3 171.49(11) 2_566 .
O2 Ni2 N3 90.75(11) . .
N4 Ni2 N3 85.48(13) . .
O2 Ni2 O5 95.93(10) 2_566 .
O2 Ni2 O5 161.47(10) . .
N4 Ni2 O5 100.90(13) . .
N3 Ni2 O5 91.04(12) . .
O2 Ni2 O6 97.40(10) 2_566 .
O2 Ni2 O6 100.78(10) . .
N4 Ni2 O6 161.16(13) . .
N3 Ni2 O6 90.26(11) . .
O5 Ni2 O6 60.77(11) . .
O2 Ni2 C16 99.71(11) 2_566 .
O2 Ni2 C16 131.13(12) . .
N4 Ni2 C16 130.99(14) . .
N3 Ni2 C16 88.78(12) . .
O5 Ni2 C16 30.51(11) . .
O6 Ni2 C16 30.38(11) . .
O2 Ni2 Ni2 42.38(7) 2_566 2_566
O2 Ni2 Ni2 41.82(7) . 2_566
N4 Ni2 Ni2 94.08(11) . 2_566
N3 Ni2 Ni2 132.20(9) . 2_566
O5 Ni2 Ni2 135.37(8) . 2_566
O6 Ni2 Ni2 102.30(8) . 2_566
C16 Ni2 Ni2 123.96(9) . 2_566
C2 C1 C6 117.4(4) . .
C2 C1 C7 121.3(4) . .
C6 C1 C7 121.3(4) . .
C1 C2 C3 123.5(4) . .
C1 C2 H2 118.3 . .
C3 C2 H2 118.3 . .
C2 C3 C4 117.7(4) . .
C2 C3 C8 117.9(3) . .
C4 C3 C8 124.3(3) . .
O1 C4 C5 117.3(3) . .
O1 C4 C3 123.5(3) . .
C5 C4 C3 119.3(3) . .
C6 C5 C4 120.6(4) . .
C6 C5 C11 121.1(4) . .
C4 C5 C11 118.2(3) . .
C5 C6 C1 121.5(4) . .
C5 C6 H6 119.3 . .
C1 C6 H6 119.3 . .
C1 C7 H7A 109.5 . .
C1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 C3 113.7(3) . .
N1 C8 H8A 108.8 . .
C3 C8 H8A 108.8 . .
N1 C8 H8B 108.8 . .
C3 C8 H8B 108.8 . .
H8A C8 H8B 107.7 . .
N1 C9 C10 111.0(3) . .
N1 C9 H9A 109.4 . .
C10 C9 H9A 109.4 . .
N1 C9 H9B 109.4 . .
C10 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
N2 C10 C9 110.1(3) . .
N2 C10 H10A 109.6 . .
C9 C10 H10A 109.6 . .
N2 C10 H10B 109.6 . .
C9 C10 H10B 109.6 . .
H10A C10 H10B 108.2 . .
N2 C11 C5 110.9(3) 2 .
N2 C11 H11A 109.5 2 .
C5 C11 H11A 109.5 . .
N2 C11 H11B 109.5 2 .
C5 C11 H11B 109.5 . .
H11A C11 H11B 108.0 . .
O4 C12 O3 124.5(3) . .
O4 C12 C13 117.9(3) . .
O3 C12 C13 117.6(3) . .
C15 C13 C14 118.2(3) 2_565 .
C15 C13 C12 123.0(3) 2_565 .
C14 C13 C12 118.8(3) . .
C15 C14 C13 122.1(3) . .
C15 C14 H14 118.9 . .
C13 C14 H14 118.9 . .
C14 C15 C13 119.7(3) . 2_565
C14 C15 C16 116.4(3) . .
C13 C15 C16 124.0(3) 2_565 .
O6 C16 O5 120.9(3) . .
O6 C16 C15 120.5(3) . .
O5 C16 C15 118.6(3) . .
O6 C16 Ni2 62.42(18) . .
O5 C16 Ni2 58.80(17) . .
C15 C16 Ni2 175.5(3) . .
C18 C17 C22 117.7(4) . .
C18 C17 C23 121.0(5) . .
C22 C17 C23 121.3(5) . .
C17 C18 C19 122.4(4) . .
C17 C18 H18 118.8 . .
C19 C18 H18 118.8 . .
C20 C19 C18 119.2(4) . .
C20 C19 C27 123.5(3) . 2_566
C18 C19 C27 117.3(4) . 2_566
O2 C20 C19 124.0(3) . .
O2 C20 C21 117.1(3) . .
C19 C20 C21 118.9(3) . .
C22 C21 C20 120.1(4) . .
C22 C21 C24 120.9(4) . .
C20 C21 C24 119.0(3) . .
C21 C22 C17 121.6(4) . .
C21 C22 H22 119.2 . .
C17 C22 H22 119.2 . .
C17 C23 H23A 109.5 . .
C17 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C17 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N3 C24 C21 112.1(3) . .
N3 C24 H24A 109.2 . .
C21 C24 H24A 109.2 . .
N3 C24 H24B 109.2 . .
C21 C24 H24B 109.2 . .
H24A C24 H24B 107.9 . .
N3 C25 C26 110.6(3) . .
N3 C25 H25A 109.5 . .
C26 C25 H25A 109.5 . .
N3 C25 H25B 109.5 . .
C26 C25 H25B 109.5 . .
H25A C25 H25B 108.1 . .
N4 C26 C25 110.5(3) . .
N4 C26 H26A 109.6 . .
C25 C26 H26A 109.6 . .
N4 C26 H26B 109.6 . .
C25 C26 H26B 109.6 . .
H26A C26 H26B 108.1 . .
N4 C27 C19 112.4(4) . 2_566
N4 C27 H27A 109.1 . .
C19 C27 H27A 109.1 2_566 .
N4 C27 H27B 109.1 . .
C19 C27 H27B 109.1 2_566 .
H27A C27 H27B 107.8 . .
O7 C28 H28A 109.5 . .
O7 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
O7 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C4 O1 Ni1 126.6(2) . .
C4 O1 Ni1 109.5(2) . 2
Ni1 O1 Ni1 95.35(11) . 2
C20 O2 Ni2 125.6(2) . 2_566
C20 O2 Ni2 111.6(2) . .
Ni2 O2 Ni2 95.80(10) 2_566 .
C12 O4 Ni1 123.8(2) . .
C16 O5 Ni2 90.7(2) . .
C16 O6 Ni2 87.2(2) . .
C28 O7 H7 109.5 . .
C8 N1 C9 113.9(3) . .
C8 N1 Ni1 110.1(2) . .
C9 N1 Ni1 109.4(2) . .
C8 N1 H1N 106(3) . .
C9 N1 H1N 104(3) . .
Ni1 N1 H1N 113(3) . .
C10 N2 C11 113.5(3) . 2
C10 N2 Ni1 103.6(2) . .
C11 N2 Ni1 113.1(2) 2 .
C10 N2 H2N 108(3) . .
C11 N2 H2N 107(3) 2 .
Ni1 N2 H2N 111(3) . .
C25 N3 C24 114.7(3) . .
C25 N3 Ni2 103.9(2) . .
C24 N3 Ni2 113.4(2) . .
C25 N3 H3N 111(3) . .
C24 N3 H3N 105(3) . .
Ni2 N3 H3N 109(3) . .
C27 N4 C26 113.8(3) . .
C27 N4 Ni2 108.6(3) . .
C26 N4 Ni2 108.9(2) . .
C27 N4 H4N 107(3) . .
C26 N4 H4N 108(3) . .
Ni2 N4 H4N 111(3) . .
Ni1 O1W H1A 97(3) . .
Ni1 O1W H1B 104(3) . .
H1A O1W H1B 105(4) . .
H2A O2W H2B 113(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.018(3) .
Ni1 N1 2.070(3) .
Ni1 O1 2.075(2) 2
Ni1 N2 2.084(3) .
Ni1 O4 2.116(3) .
Ni1 O1W 2.159(3) .
Ni2 O2 2.006(3) 2_566
Ni2 O2 2.028(3) .
Ni2 N4 2.048(3) .
Ni2 N3 2.053(3) .
Ni2 O5 2.131(3) .
Ni2 O6 2.211(3) .
Ni2 C16 2.491(3) .
Ni2 Ni2 2.9928(12) 2_566
C1 C2 1.383(6) .
C1 C6 1.385(6) .
C1 C7 1.511(6) .
C2 C3 1.397(5) .
C2 H2 0.9300 .
C3 C4 1.407(5) .
C3 C8 1.504(5) .
C4 O1 1.354(4) .
C4 C5 1.402(5) .
C5 C6 1.379(6) .
C5 C11 1.500(5) .
C6 H6 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 N1 1.475(5) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 N1 1.484(5) .
C9 C10 1.517(6) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 N2 1.478(5) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N2 1.491(5) 2
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 O4 1.259(4) .
C12 O3 1.266(4) .
C12 C13 1.504(5) .
C13 C15 1.395(5) 2_565
C13 C14 1.398(5) .
C14 C15 1.381(5) .
C14 H14 0.9300 .
C15 C13 1.395(5) 2_565
C15 C16 1.510(4) .
C16 O6 1.261(5) .
C16 O5 1.265(5) .
C17 C18 1.383(6) .
C17 C22 1.400(6) .
C17 C23 1.517(6) .
C18 C19 1.401(5) .
C18 H18 0.9300 .
C19 C20 1.400(6) .
C19 C27 1.511(6) 2_566
C20 O2 1.345(4) .
C20 C21 1.413(5) .
C21 C22 1.385(5) .
C21 C24 1.495(6) .
C22 H22 0.9300 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 N3 1.494(5) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 N3 1.467(5) .
C25 C26 1.521(6) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 N4 1.493(5) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C27 N4 1.462(6) .
C27 C19 1.511(6) 2_566
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C28 O7 1.451(10) .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
O1 Ni1 2.075(2) 2
O2 Ni2 2.006(3) 2_566
O7 H7 0.8200 .
N1 H1N 0.91(4) .
N2 C11 1.491(5) 2
N2 H2N 0.91(4) .
N3 H3N 0.84(3) .
N4 H4N 0.94(4) .
O1W H1A 0.89(4) .
O1W H1B 0.87(4) .
O2W H2A 0.90(4) .
O2W H2B 0.81(5) .
O3W H3A 0.796(19) .
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
O1W H1A O3 0.89(4) 1.84(4) 2.688(4) 157(5) .
O1W H1B O2W 0.87(4) 1.89(4) 2.739(6) 165(5) .
N1 H1N O4 0.91(4) 2.30(4) 3.061(4) 140(4) 2
O2W H2A O1 0.90(4) 2.47(7) 2.877(5) 108(6) .
N2 H2N O3 0.91(4) 2.54(4) 3.185(5) 129(4) .
N3 H3N O3 0.84(3) 2.10(4) 2.893(4) 158(4) 2_565
O2W H2B O3W 0.81(5) 2.01(4) 2.641(9) 134(5) .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 0.8(7) . .
C7 C1 C2 C3 179.0(4) . .
C1 C2 C3 C4 0.6(6) . .
C1 C2 C3 C8 -175.9(4) . .
C2 C3 C4 O1 -180.0(3) . .
C8 C3 C4 O1 -3.8(6) . .
C2 C3 C4 C5 -1.9(5) . .
C8 C3 C4 C5 174.3(3) . .
O1 C4 C5 C6 -179.9(4) . .
C3 C4 C5 C6 2.0(6) . .
O1 C4 C5 C11 2.1(5) . .
C3 C4 C5 C11 -176.1(3) . .
C4 C5 C6 C1 -0.6(7) . .
C11 C5 C6 C1 177.4(4) . .
C2 C1 C6 C5 -0.8(7) . .
C7 C1 C6 C5 -179.0(5) . .
C2 C3 C8 N1 141.9(3) . .
C4 C3 C8 N1 -34.3(5) . .
N1 C9 C10 N2 -47.2(5) . .
C6 C5 C11 N2 -112.9(4) . 2
C4 C5 C11 N2 65.1(5) . 2
O4 C12 C13 C15 159.9(4) . 2_565
O3 C12 C13 C15 -21.0(6) . 2_565
O4 C12 C13 C14 -22.7(5) . .
O3 C12 C13 C14 156.3(4) . .
C15 C13 C14 C15 1.0(6) 2_565 .
C12 C13 C14 C15 -176.5(4) . .
C13 C14 C15 C13 -1.0(6) . 2_565
C13 C14 C15 C16 179.3(4) . .
C14 C15 C16 O6 -101.8(4) . .
C13 C15 C16 O6 78.6(5) 2_565 .
C14 C15 C16 O5 75.5(5) . .
C13 C15 C16 O5 -104.2(4) 2_565 .
C14 C15 C16 Ni2 128(3) . .
C13 C15 C16 Ni2 -51(4) 2_565 .
O2 Ni2 C16 O6 88.1(2) 2_566 .
O2 Ni2 C16 O6 -2.7(3) . .
N4 Ni2 C16 O6 -175.5(2) . .
N3 Ni2 C16 O6 -92.6(2) . .
O5 Ni2 C16 O6 173.3(3) . .
Ni2 Ni2 C16 O6 50.1(2) 2_566 .
O2 Ni2 C16 O5 -85.2(2) 2_566 .
O2 Ni2 C16 O5 -175.96(19) . .
N4 Ni2 C16 O5 11.2(3) . .
N3 Ni2 C16 O5 94.1(2) . .
O6 Ni2 C16 O5 -173.3(3) . .
Ni2 Ni2 C16 O5 -123.2(2) 2_566 .
O2 Ni2 C16 C15 -140(3) 2_566 .
O2 Ni2 C16 C15 129(3) . .
N4 Ni2 C16 C15 -44(4) . .
N3 Ni2 C16 C15 39(3) . .
O5 Ni2 C16 C15 -55(3) . .
O6 Ni2 C16 C15 132(4) . .
Ni2 Ni2 C16 C15 -178(100) 2_566 .
C22 C17 C18 C19 1.7(6) . .
C23 C17 C18 C19 179.4(4) . .
C17 C18 C19 C20 0.9(6) . .
C17 C18 C19 C27 -178.7(4) . 2_566
C18 C19 C20 O2 177.1(3) . .
C27 C19 C20 O2 -3.3(6) 2_566 .
C18 C19 C20 C21 -3.0(5) . .
C27 C19 C20 C21 176.6(4) 2_566 .
O2 C20 C21 C22 -177.6(3) . .
C19 C20 C21 C22 2.5(5) . .
O2 C20 C21 C24 2.6(5) . .
C19 C20 C21 C24 -177.3(3) . .
C20 C21 C22 C17 0.2(6) . .
C24 C21 C22 C17 179.9(4) . .
C18 C17 C22 C21 -2.3(6) . .
C23 C17 C22 C21 -179.9(4) . .
C22 C21 C24 N3 -118.4(4) . .
C20 C21 C24 N3 61.4(4) . .
N3 C25 C26 N4 46.5(5) . .
C5 C4 O1 Ni1 -177.1(2) . .
C3 C4 O1 Ni1 1.0(5) . .
C5 C4 O1 Ni1 -64.4(4) . 2
C3 C4 O1 Ni1 113.7(3) . 2
N1 Ni1 O1 C4 24.8(3) . .
O1 Ni1 O1 C4 119.1(3) 2 .
N2 Ni1 O1 C4 64.8(7) . .
O4 Ni1 O1 C4 -151.3(3) . .
O1W Ni1 O1 C4 -66.4(3) . .
N1 Ni1 O1 Ni1 -94.33(12) . 2
O1 Ni1 O1 Ni1 0.0 2 2
N2 Ni1 O1 Ni1 -54.3(6) . 2
O4 Ni1 O1 Ni1 89.58(10) . 2
O1W Ni1 O1 Ni1 174.47(10) . 2
C19 C20 O2 Ni2 2.6(5) . 2_566
C21 C20 O2 Ni2 -177.3(2) . 2_566
C19 C20 O2 Ni2 117.2(3) . .
C21 C20 O2 Ni2 -62.6(3) . .
O2 Ni2 O2 C20 -132.0(3) 2_566 .
N4 Ni2 O2 C20 140.4(3) . .
N3 Ni2 O2 C20 54.8(3) . .
O5 Ni2 O2 C20 -40.7(5) . .
O6 Ni2 O2 C20 -35.6(3) . .
C16 Ni2 O2 C20 -34.2(3) . .
Ni2 Ni2 O2 C20 -132.0(3) 2_566 .
O2 Ni2 O2 Ni2 0.0 2_566 2_566
N4 Ni2 O2 Ni2 -87.60(12) . 2_566
N3 Ni2 O2 Ni2 -173.14(11) . 2_566
O5 Ni2 O2 Ni2 91.4(3) . 2_566
O6 Ni2 O2 Ni2 96.46(11) . 2_566
C16 Ni2 O2 Ni2 97.84(14) . 2_566
O3 C12 O4 Ni1 -8.9(6) . .
C13 C12 O4 Ni1 170.1(2) . .
O1 Ni1 O4 C12 142.8(3) . .
N1 Ni1 O4 C12 85.4(14) . .
O1 Ni1 O4 C12 -132.5(3) 2 .
N2 Ni1 O4 C12 -43.3(3) . .
O1W Ni1 O4 C12 46.7(3) . .
O6 C16 O5 Ni2 -6.9(4) . .
C15 C16 O5 Ni2 175.8(3) . .
O2 Ni2 O5 C16 99.1(2) 2_566 .
O2 Ni2 O5 C16 9.6(4) . .
N4 Ni2 O5 C16 -171.4(2) . .
N3 Ni2 O5 C16 -85.8(2) . .
O6 Ni2 O5 C16 3.9(2) . .
Ni2 Ni2 O5 C16 81.2(2) 2_566 .
O5 C16 O6 Ni2 6.7(3) . .
C15 C16 O6 Ni2 -176.1(3) . .
O2 Ni2 O6 C16 -96.6(2) 2_566 .
O2 Ni2 O6 C16 178.0(2) . .
N4 Ni2 O6 C16 10.5(5) . .
N3 Ni2 O6 C16 87.1(2) . .
O5 Ni2 O6 C16 -3.9(2) . .
Ni2 Ni2 O6 C16 -139.3(2) 2_566 .
C3 C8 N1 C9 -170.2(3) . .
C3 C8 N1 Ni1 66.5(3) . .
C10 C9 N1 C8 -104.0(4) . .
C10 C9 N1 Ni1 19.7(4) . .
O1 Ni1 N1 C8 -55.0(2) . .
O1 Ni1 N1 C8 -139.5(2) 2 .
N2 Ni1 N1 C8 131.7(2) . .
O4 Ni1 N1 C8 2.5(15) . .
O1W Ni1 N1 C8 41.0(2) . .
O1 Ni1 N1 C9 179.1(3) . .
O1 Ni1 N1 C9 94.6(3) 2 .
N2 Ni1 N1 C9 5.8(3) . .
O4 Ni1 N1 C9 -123.4(13) . .
O1W Ni1 N1 C9 -84.9(3) . .
C9 C10 N2 C11 -74.2(4) . 2
C9 C10 N2 Ni1 48.8(4) . .
O1 Ni1 N2 C10 -69.9(7) . .
N1 Ni1 N2 C10 -29.7(3) . .
O1 Ni1 N2 C10 -123.9(3) 2 .
O4 Ni1 N2 C10 146.7(2) . .
O1W Ni1 N2 C10 61.7(3) . .
O1 Ni1 N2 C11 53.4(7) . 2
N1 Ni1 N2 C11 93.6(3) . 2
O1 Ni1 N2 C11 -0.6(3) 2 2
O4 Ni1 N2 C11 -90.1(3) . 2
O1W Ni1 N2 C11 -175.1(3) . 2
C26 C25 N3 C24 76.9(4) . .
C26 C25 N3 Ni2 -47.6(4) . .
C21 C24 N3 C25 -170.3(3) . .
C21 C24 N3 Ni2 -51.1(4) . .
O2 Ni2 N3 C25 72.7(9) 2_566 .
O2 Ni2 N3 C25 126.2(2) . .
N4 Ni2 N3 C25 28.6(2) . .
O5 Ni2 N3 C25 -72.3(2) . .
O6 Ni2 N3 C25 -133.0(2) . .
C16 Ni2 N3 C25 -102.7(2) . .
Ni2 Ni2 N3 C25 120.0(2) 2_566 .
O2 Ni2 N3 C24 -52.5(9) 2_566 .
O2 Ni2 N3 C24 0.9(3) . .
N4 Ni2 N3 C24 -96.7(3) . .
O5 Ni2 N3 C24 162.5(2) . .
O6 Ni2 N3 C24 101.7(3) . .
C16 Ni2 N3 C24 132.0(3) . .
Ni2 Ni2 N3 C24 -5.3(3) 2_566 .
C19 C27 N4 C26 168.9(3) 2_566 .
C19 C27 N4 Ni2 -69.6(4) 2_566 .
C25 C26 N4 C27 101.3(4) . .
C25 C26 N4 Ni2 -20.0(4) . .
O2 Ni2 N4 C27 56.7(3) 2_566 .
O2 Ni2 N4 C27 140.7(3) . .
N3 Ni2 N4 C27 -129.2(3) . .
O5 Ni2 N4 C27 -39.0(3) . .
O6 Ni2 N4 C27 -51.8(5) . .
C16 Ni2 N4 C27 -44.8(3) . .
Ni2 Ni2 N4 C27 98.8(3) 2_566 .
O2 Ni2 N4 C26 -178.8(3) 2_566 .
O2 Ni2 N4 C26 -94.9(3) . .
N3 Ni2 N4 C26 -4.7(3) . .
O5 Ni2 N4 C26 85.4(3) . .
O6 Ni2 N4 C26 72.7(5) . .
C16 Ni2 N4 C26 79.7(3) . .
Ni2 Ni2 N4 C26 -136.8(3) 2_566 .
