#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/99/2219967.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_2219967
loop_
_publ_author_name
'Meng, Shuang-Ming'
'Fan, Yue-Qin'
'Guo, Yong'
_publ_section_title
catena-Poly[[(1,12,15,26-tetraaza-5,8,19,22-tetraoxa-3,4:9,10:17,18:23,24-tetrabenzocyclooctacosane-κ⁴N¹,N¹²,N¹⁵,N²⁶)nickel(II)]-μ-terephthalato-κ²O¹:O⁴]
_journal_coeditor_code           PV2108
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1431
_journal_paper_doi               10.1107/S160053680803314X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C8 H4 O4) (C36 H44 N4 O4)]'
_chemical_formula_moiety         'C44 H48 N4 Ni O8'
_chemical_formula_sum            'C44 H48 N4 Ni O8'
_chemical_formula_weight         819.57
_chemical_name_systematic
;
catena-Poly[[(1,12,15,26-tetraaza-5,8,19,22-tetraoxa-3,4:9,10:17,18:23,24-
tetrabenzocyclooctacosane-
κ⁴N¹,N¹²,N¹⁵,N²⁶)nickel(II)]-
μ-terephthalato-κ²O¹:O⁴]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.758(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.407(3)
_cell_length_b                   16.575(3)
_cell_length_c                   21.675(6)
_cell_measurement_reflns_used    9133
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4012.1(17)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       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  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37289
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.791
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9133
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0631
_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)+(0.0632P)²+2.1456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                5535
_reflns_number_total             9133
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pv2108.cif
_cod_data_source_block           I
_cod_original_cell_volume        4012.2(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2219967
_cod_database_fobs_code          2219967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ni Ni1 0.76937(4) 0.21301(2) 0.898586(19) 0.02536(13) Uani d . 1
C C1 0.5251(3) 0.0013(2) 0.84876(18) 0.0422(9) Uani d . 1
C C2 0.5463(4) -0.0627(3) 0.8114(2) 0.0660(14) Uani d . 1
H H2 0.6008 -0.0565 0.7852 0.079 Uiso calc R 1
C C3 0.4876(5) -0.1363(3) 0.8124(3) 0.0747(16) Uani d . 1
H H3 0.5032 -0.1786 0.7871 0.090 Uiso calc R 1
C C4 0.4075(4) -0.1459(3) 0.8502(2) 0.0628(13) Uani d . 1
H H4 0.3674 -0.1947 0.8505 0.075 Uiso calc R 1
C C5 0.3859(4) -0.0837(3) 0.8880(2) 0.0573(12) Uani d . 1
H H5 0.3307 -0.0902 0.9138 0.069 Uiso calc R 1
C C6 0.4457(4) -0.0118(2) 0.8878(2) 0.0479(10) Uani d . 1
C C9 0.3299(4) 0.0644(3) 0.9479(2) 0.0519(11) Uani d . 1
H H9A 0.3091 0.0169 0.9696 0.062 Uiso calc R 1
H H9B 0.2668 0.0734 0.9112 0.062 Uiso calc R 1
C C10 0.3383(4) 0.1346(3) 0.9901(2) 0.0623(13) Uani d . 1
H H10A 0.2583 0.1526 0.9920 0.075 Uiso calc R 1
H H10B 0.3779 0.1185 1.0322 0.075 Uiso calc R 1
C C11 0.4113(3) 0.2674(2) 1.00719(17) 0.0414(9) Uani d . 1
C C12 0.3125(4) 0.3033(3) 1.0236(2) 0.0643(13) Uani d . 1
H H12 0.2367 0.2809 1.0106 0.077 Uiso calc R 1
C C13 0.3278(5) 0.3727(4) 1.0595(3) 0.0872(18) Uani d . 1
H H13 0.2621 0.3977 1.0706 0.105 Uiso calc R 1
C C14 0.4397(6) 0.4046(4) 1.0786(3) 0.0852(18) Uani d . 1
H H14 0.4500 0.4506 1.1037 0.102 Uiso calc R 1
C C15 0.5377(5) 0.3695(3) 1.0612(2) 0.0641(13) Uani d . 1
H H15 0.6131 0.3923 1.0742 0.077 Uiso calc R 1
C C16 0.5245(3) 0.3001(2) 1.02442(17) 0.0395(9) Uani d . 1
C C17 0.6303(3) 0.2610(2) 1.00410(16) 0.0389(9) Uani d . 1
H H17A 0.7025 0.2758 1.0340 0.047 Uiso calc R 1
H H17B 0.6216 0.2029 1.0062 0.047 Uiso calc R 1
C C18 0.6834(4) 0.3678(2) 0.93574(19) 0.0457(10) Uani d . 1
H H18A 0.6499 0.4007 0.9649 0.055 Uiso calc R 1
H H18B 0.6541 0.3882 0.8935 0.055 Uiso calc R 1
C C19 0.8183(4) 0.3724(2) 0.95182(19) 0.0476(10) Uani d . 1
H H19A 0.8440 0.4281 0.9509 0.057 Uiso calc R 1
H H19B 0.8479 0.3512 0.9938 0.057 Uiso calc R 1
C C20 0.8686(4) 0.3707(2) 0.84692(18) 0.0435(9) Uani d . 1
H H20A 0.7875 0.3871 0.8282 0.052 Uiso calc R 1
H H20B 0.8962 0.3354 0.8171 0.052 Uiso calc R 1
C C21 0.9472(4) 0.4448(2) 0.85675(18) 0.0429(9) Uani d . 1
C C22 0.8995(5) 0.5222(2) 0.8504(2) 0.0600(12) Uani d . 1
H H22 0.8169 0.5296 0.8406 0.072 Uiso calc R 1
C C23 0.9760(6) 0.5892(3) 0.8586(3) 0.0780(17) Uani d . 1
H H23 0.9442 0.6410 0.8549 0.094 Uiso calc R 1
C C24 1.0953(6) 0.5787(3) 0.8720(3) 0.0761(16) Uani d . 1
H H24 1.1452 0.6236 0.8768 0.091 Uiso calc R 1
C C25 1.1447(5) 0.5027(3) 0.8786(2) 0.0646(13) Uani d . 1
H H25 1.2274 0.4961 0.8883 0.077 Uiso calc R 1
C C26 1.0705(4) 0.4364(2) 0.8707(2) 0.0487(10) Uani d . 1
C C27 1.2162(4) 0.3402(3) 0.8544(3) 0.0679(14) Uani d . 1
H H27A 1.2857 0.3572 0.8853 0.081 Uiso calc R 1
H H27B 1.2160 0.3694 0.8156 0.081 Uiso calc R 1
C C28 1.2233(4) 0.2533(3) 0.8431(3) 0.0801(17) Uani d . 1
H H28A 1.2944 0.2420 0.8265 0.096 Uiso calc R 1
H H28B 1.2305 0.2247 0.8827 0.096 Uiso calc R 1
C C29 1.1211(4) 0.1467(2) 0.78328(19) 0.0444(9) Uani d . 1
C C30 1.2200(4) 0.1073(3) 0.7688(2) 0.0617(13) Uani d . 1
H H30 1.2932 0.1336 0.7733 0.074 Uiso calc R 1
C C31 1.2076(5) 0.0288(3) 0.7478(2) 0.0674(14) Uani d . 1
H H31 1.2738 0.0016 0.7393 0.081 Uiso calc R 1
C C32 1.0996(5) -0.0101(3) 0.7394(2) 0.0665(13) Uani d . 1
H H32 1.0920 -0.0628 0.7243 0.080 Uiso calc R 1
C C33 1.0018(4) 0.0298(3) 0.7534(2) 0.0561(11) Uani d . 1
H H33 0.9281 0.0038 0.7470 0.067 Uiso calc R 1
C C34 1.0114(4) 0.1088(2) 0.77716(18) 0.0423(9) Uani d . 1
C C35 0.9067(3) 0.1515(2) 0.79519(17) 0.0388(9) Uani d . 1
H H35A 0.9145 0.2089 0.7883 0.047 Uiso calc R 1
H H35B 0.8338 0.1334 0.7674 0.047 Uiso calc R 1
C C36 0.8639(4) 0.0525(3) 0.8715(3) 0.0643(9) Uani d . 1
H H36A 0.8305 0.0284 0.8310 0.077 Uiso calc R 1
H H36B 0.9374 0.0239 0.8890 0.077 Uiso calc R 1
C C37 0.7792(4) 0.0404(3) 0.9134(3) 0.0643(9) Uani d . 1
H H37A 0.7457 -0.0135 0.9075 0.077 Uiso calc R 1
H H37B 0.8211 0.0453 0.9569 0.077 Uiso calc R 1
C C38 0.5845(4) 0.0823(2) 0.84676(19) 0.0474(10) Uani d . 1
H H38A 0.6153 0.0855 0.8083 0.057 Uiso calc R 1
H H38B 0.5243 0.1240 0.8449 0.057 Uiso calc R 1
C C39 0.5795(3) 0.2704(2) 0.78663(15) 0.0322(8) Uani d . 1
C C40 0.5548(3) 0.2906(2) 0.71679(15) 0.0295(7) Uani d . 1
C C41 0.4375(3) 0.2997(2) 0.68456(16) 0.0364(8) Uani d . 1
H H41 0.3755 0.2989 0.7066 0.044 Uiso calc R 1
C C42 0.4119(3) 0.3100(2) 0.61992(16) 0.0350(8) Uani d . 1
H H42 0.3326 0.3154 0.5990 0.042 Uiso calc R 1
C C43 0.5016(3) 0.3125(2) 0.58600(15) 0.0293(7) Uani d . 1
C C44 0.4709(3) 0.3139(2) 0.51426(16) 0.0335(8) Uani d . 1
C C45 0.6199(3) 0.3074(2) 0.61860(16) 0.0371(9) Uani d . 1
H H45 0.6820 0.3117 0.5969 0.044 Uiso calc R 1
C C46 0.6456(3) 0.2961(2) 0.68337(16) 0.0360(8) Uani d . 1
H H46 0.7249 0.2921 0.7046 0.043 Uiso calc R 1
O O1 0.4368(3) 0.05093(19) 0.92886(16) 0.0669(7) Uani d . 1
O O2 0.4008(3) 0.19793(19) 0.97062(16) 0.0669(7) Uani d . 1
O O3 1.1119(3) 0.35817(18) 0.87622(17) 0.0655(9) Uani d . 1
O O4 1.1251(3) 0.22632(19) 0.80180(18) 0.0706(10) Uani d . 1
O O5 0.4986(2) 0.2814(2) 0.81597(12) 0.0555(8) Uani d . 1
O O6 0.6840(2) 0.24327(14) 0.80900(10) 0.0333(6) Uani d . 1
O O7 0.3600(2) 0.31285(15) 0.49024(10) 0.0349(6) Uani d . 1
O O8 0.5516(2) 0.3137(2) 0.48444(13) 0.0710(10) Uani d . 1
N N1 0.6832(3) 0.09923(18) 0.90061(15) 0.0374(7) Uani d D 1
H H1N 0.653(3) 0.100(2) 0.9325(13) 0.045 Uiso d D 1
N N2 0.8942(3) 0.13883(19) 0.86124(13) 0.0343(7) Uani d D 1
H H2N 0.954(2) 0.153(2) 0.8863(15) 0.041 Uiso d D 1
N N3 0.8662(3) 0.32447(18) 0.90502(14) 0.0353(7) Uani d D 1
H H3N 0.9388(19) 0.317(2) 0.9209(17) 0.042 Uiso d D 1
N N4 0.6460(2) 0.28272(18) 0.93980(13) 0.0327(6) Uani d D 1
H H4N 0.582(2) 0.275(2) 0.9139(15) 0.039 Uiso d 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
O6 Ni1 O7 . 4_666 177.49(10)
O6 Ni1 N1 . . 95.97(11)
O7 Ni1 N1 4_666 . 86.54(11)
O6 Ni1 N3 . . 89.42(11)
O7 Ni1 N3 4_666 . 88.08(11)
N1 Ni1 N3 . . 174.59(12)
O6 Ni1 N4 . . 92.13(10)
O7 Ni1 N4 4_666 . 87.37(10)
N1 Ni1 N4 . . 97.09(12)
N3 Ni1 N4 . . 83.23(12)
O6 Ni1 N2 . . 90.38(10)
O7 Ni1 N2 4_666 . 90.20(10)
N1 Ni1 N2 . . 81.13(12)
N3 Ni1 N2 . . 98.32(12)
N4 Ni1 N2 . . 177.07(11)
C6 C1 C2 . . 117.0(4)
C6 C1 C38 . . 120.8(4)
C2 C1 C38 . . 122.2(4)
C1 C2 C3 . . 121.4(4)
C1 C2 H2 . . 119.3
C3 C2 H2 . . 119.3
C4 C3 C2 . . 119.8(5)
C4 C3 H3 . . 120.1
C2 C3 H3 . . 120.1
C3 C4 C5 . . 119.9(4)
C3 C4 H4 . . 120.1
C5 C4 H4 . . 120.1
C4 C5 C6 . . 120.1(5)
C4 C5 H5 . . 119.9
C6 C5 H5 . . 119.9
C5 C6 C1 . . 121.8(4)
C5 C6 O1 . . 123.3(4)
C1 C6 O1 . . 114.9(3)
O1 C9 C10 . . 111.3(3)
O1 C9 H9A . . 109.4
C10 C9 H9A . . 109.4
O1 C9 H9B . . 109.4
C10 C9 H9B . . 109.4
H9A C9 H9B . . 108.0
O2 C10 C9 . . 112.6(4)
O2 C10 H10A . . 109.1
C9 C10 H10A . . 109.1
O2 C10 H10B . . 109.1
C9 C10 H10B . . 109.1
H10A C10 H10B . . 107.8
C16 C11 C12 . . 121.8(4)
C16 C11 O2 . . 116.6(3)
C12 C11 O2 . . 121.6(4)
C13 C12 C11 . . 119.2(5)
C13 C12 H12 . . 120.4
C11 C12 H12 . . 120.4
C14 C13 C12 . . 119.8(5)
C14 C13 H13 . . 120.1
C12 C13 H13 . . 120.1
C13 C14 C15 . . 120.8(5)
C13 C14 H14 . . 119.6
C15 C14 H14 . . 119.6
C14 C15 C16 . . 120.5(5)
C14 C15 H15 . . 119.8
C16 C15 H15 . . 119.8
C11 C16 C15 . . 117.8(4)
C11 C16 C17 . . 120.7(3)
C15 C16 C17 . . 121.5(4)
N4 C17 C16 . . 115.2(3)
N4 C17 H17A . . 108.5
C16 C17 H17A . . 108.5
N4 C17 H17B . . 108.5
C16 C17 H17B . . 108.5
H17A C17 H17B . . 107.5
N4 C18 C19 . . 109.1(3)
N4 C18 H18A . . 109.9
C19 C18 H18A . . 109.9
N4 C18 H18B . . 109.9
C19 C18 H18B . . 109.9
H18A C18 H18B . . 108.3
N3 C19 C18 . . 108.5(3)
N3 C19 H19A . . 110.0
C18 C19 H19A . . 110.0
N3 C19 H19B . . 110.0
C18 C19 H19B . . 110.0
H19A C19 H19B . . 108.4
N3 C20 C21 . . 114.5(3)
N3 C20 H20A . . 108.6
C21 C20 H20A . . 108.6
N3 C20 H20B . . 108.6
C21 C20 H20B . . 108.6
H20A C20 H20B . . 107.6
C26 C21 C22 . . 118.3(4)
C26 C21 C20 . . 119.8(4)
C22 C21 C20 . . 121.8(4)
C21 C22 C23 . . 119.8(5)
C21 C22 H22 . . 120.1
C23 C22 H22 . . 120.1
C24 C23 C22 . . 120.2(5)
C24 C23 H23 . . 119.9
C22 C23 H23 . . 119.9
C23 C24 C25 . . 121.1(5)
C23 C24 H24 . . 119.5
C25 C24 H24 . . 119.5
C26 C25 C24 . . 119.2(5)
C26 C25 H25 . . 120.4
C24 C25 H25 . . 120.4
C25 C26 O3 . . 123.3(4)
C25 C26 C21 . . 121.3(4)
O3 C26 C21 . . 115.4(3)
O3 C27 C28 . . 110.2(4)
O3 C27 H27A . . 109.6
C28 C27 H27A . . 109.6
O3 C27 H27B . . 109.6
C28 C27 H27B . . 109.6
H27A C27 H27B . . 108.1
O4 C28 C27 . . 111.5(4)
O4 C28 H28A . . 109.3
C27 C28 H28A . . 109.3
O4 C28 H28B . . 109.3
C27 C28 H28B . . 109.3
H28A C28 H28B . . 108.0
O4 C29 C34 . . 116.1(3)
O4 C29 C30 . . 122.3(4)
C34 C29 C30 . . 121.5(4)
C31 C30 C29 . . 119.0(5)
C31 C30 H30 . . 120.5
C29 C30 H30 . . 120.5
C32 C31 C30 . . 121.2(4)
C32 C31 H31 . . 119.4
C30 C31 H31 . . 119.4
C31 C32 C33 . . 119.3(5)
C31 C32 H32 . . 120.4
C33 C32 H32 . . 120.4
C32 C33 C34 . . 121.4(5)
C32 C33 H33 . . 119.3
C34 C33 H33 . . 119.3
C29 C34 C33 . . 117.5(4)
C29 C34 C35 . . 120.7(4)
C33 C34 C35 . . 121.8(4)
N2 C35 C34 . . 115.0(3)
N2 C35 H35A . . 108.5
C34 C35 H35A . . 108.5
N2 C35 H35B . . 108.5
C34 C35 H35B . . 108.5
H35A C35 H35B . . 107.5
C37 C36 N2 . . 115.0(4)
C37 C36 H36A . . 108.5
N2 C36 H36A . . 108.5
C37 C36 H36B . . 108.5
N2 C36 H36B . . 108.5
H36A C36 H36B . . 107.5
N1 C37 C36 . . 110.8(4)
N1 C37 H37A . . 109.5
C36 C37 H37A . . 109.5
N1 C37 H37B . . 109.5
C36 C37 H37B . . 109.5
H37A C37 H37B . . 108.1
N1 C38 C1 . . 115.0(3)
N1 C38 H38A . . 108.5
C1 C38 H38A . . 108.5
N1 C38 H38B . . 108.5
C1 C38 H38B . . 108.5
H38A C38 H38B . . 107.5
O5 C39 O6 . . 126.5(3)
O5 C39 C40 . . 118.3(3)
O6 C39 C40 . . 115.2(3)
C46 C40 C41 . . 118.6(3)
C46 C40 C39 . . 122.0(3)
C41 C40 C39 . . 119.3(3)
C42 C41 C40 . . 120.5(3)
C42 C41 H41 . . 119.8
C40 C41 H41 . . 119.8
C43 C42 C41 . . 121.2(3)
C43 C42 H42 . . 119.4
C41 C42 H42 . . 119.4
C42 C43 C45 . . 118.5(3)
C42 C43 C44 . . 120.3(3)
C45 C43 C44 . . 121.1(3)
O8 C44 O7 . . 125.2(3)
O8 C44 C43 . . 119.8(3)
O7 C44 C43 . . 114.9(3)
C46 C45 C43 . . 120.3(3)
C46 C45 H45 . . 119.9
C43 C45 H45 . . 119.9
C40 C46 C45 . . 120.9(3)
C40 C46 H46 . . 119.6
C45 C46 H46 . . 119.6
C9 O1 C6 . . 119.8(3)
C10 O2 C11 . . 116.4(3)
C26 O3 C27 . . 118.1(3)
C28 O4 C29 . . 118.8(4)
C39 O6 Ni1 . . 132.4(2)
C44 O7 Ni1 . 4_565 130.8(2)
C37 N1 C38 . . 116.6(4)
C37 N1 Ni1 . . 105.4(3)
C38 N1 Ni1 . . 115.7(2)
C37 N1 H1N . . 106(3)
C38 N1 H1N . . 106(3)
Ni1 N1 H1N . . 106(3)
C35 N2 C36 . . 110.4(3)
C35 N2 Ni1 . . 118.8(2)
C36 N2 Ni1 . . 107.4(2)
C35 N2 H2N . . 112(3)
C36 N2 H2N . . 112(3)
Ni1 N2 H2N . . 96(3)
C19 N3 C20 . . 112.3(3)
C19 N3 Ni1 . . 104.5(2)
C20 N3 Ni1 . . 119.3(2)
C19 N3 H3N . . 106(3)
C20 N3 H3N . . 104(3)
Ni1 N3 H3N . . 110(3)
C18 N4 C17 . . 112.2(3)
C18 N4 Ni1 . . 105.4(2)
C17 N4 Ni1 . . 118.3(2)
C18 N4 H4N . . 109(3)
C17 N4 H4N . . 110(3)
Ni1 N4 H4N . . 101(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O6 . 2.049(2)
Ni1 O7 4_666 2.089(2)
Ni1 N1 . 2.131(3)
Ni1 N3 . 2.142(3)
Ni1 N4 . 2.151(3)
Ni1 N2 . 2.160(3)
C1 C6 . 1.377(6)
C1 C2 . 1.384(6)
C1 C38 . 1.508(5)
C2 C3 . 1.393(6)
C2 H2 . 0.9300
C3 C4 . 1.356(7)
C3 H3 . 0.9300
C4 C5 . 1.370(6)
C4 H4 . 0.9300
C5 C6 . 1.374(5)
C5 H5 . 0.9300
C6 O1 . 1.385(5)
C9 O1 . 1.383(5)
C9 C10 . 1.471(6)
C9 H9A . 0.9700
C9 H9B . 0.9700
C10 O2 . 1.382(5)
C10 H10A . 0.9700
C10 H10B . 0.9700
C11 C16 . 1.381(5)
C11 C12 . 1.383(6)
C11 O2 . 1.389(5)
C12 C13 . 1.380(7)
C12 H12 . 0.9300
C13 C14 . 1.366(8)
C13 H13 . 0.9300
C14 C15 . 1.380(7)
C14 H14 . 0.9300
C15 C16 . 1.389(6)
C15 H15 . 0.9300
C16 C17 . 1.512(5)
C17 N4 . 1.485(4)
C17 H17A . 0.9700
C17 H17B . 0.9700
C18 N4 . 1.481(5)
C18 C19 . 1.508(6)
C18 H18A . 0.9700
C18 H18B . 0.9700
C19 N3 . 1.478(5)
C19 H19A . 0.9700
C19 H19B . 0.9700
C20 N3 . 1.479(5)
C20 C21 . 1.510(5)
C20 H20A . 0.9700
C20 H20B . 0.9700
C21 C26 . 1.384(6)
C21 C22 . 1.390(6)
C22 C23 . 1.401(7)
C22 H22 . 0.9300
C23 C24 . 1.343(7)
C23 H23 . 0.9300
C24 C25 . 1.376(7)
C24 H24 . 0.9300
C25 C26 . 1.376(6)
C25 H25 . 0.9300
C26 O3 . 1.377(5)
C27 O3 . 1.399(5)
C27 C28 . 1.465(7)
C27 H27A . 0.9700
C27 H27B . 0.9700
C28 O4 . 1.359(5)
C28 H28A . 0.9700
C28 H28B . 0.9700
C29 O4 . 1.377(5)
C29 C34 . 1.382(6)
C29 C30 . 1.394(6)
C30 C31 . 1.376(7)
C30 H30 . 0.9300
C31 C32 . 1.369(7)
C31 H31 . 0.9300
C32 C33 . 1.383(6)
C32 H32 . 0.9300
C33 C34 . 1.402(6)
C33 H33 . 0.9300
C34 C35 . 1.506(5)
C35 N2 . 1.482(4)
C35 H35A . 0.9700
C35 H35B . 0.9700
C36 C37 . 1.469(6)
C36 N2 . 1.500(5)
C36 H36A . 0.9700
C36 H36B . 0.9700
C37 N1 . 1.450(5)
C37 H37A . 0.9700
C37 H37B . 0.9700
C38 N1 . 1.474(5)
C38 H38A . 0.9700
C38 H38B . 0.9700
C39 O5 . 1.236(4)
C39 O6 . 1.274(4)
C39 C40 . 1.519(4)
C40 C46 . 1.382(5)
C40 C41 . 1.386(4)
C41 C42 . 1.382(5)
C41 H41 . 0.9300
C42 C43 . 1.377(5)
C42 H42 . 0.9300
C43 C45 . 1.393(4)
C43 C44 . 1.523(5)
C44 O8 . 1.228(4)
C44 O7 . 1.267(4)
C45 C46 . 1.387(5)
C45 H45 . 0.9300
C46 H46 . 0.9300
O7 Ni1 4_565 2.089(2)
N1 H1N . 0.83(2)
N2 H2N . 0.81(2)
N3 H3N . 0.84(2)
N4 H4N . 0.83(2)
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
N1 H1N O1 . 0.83(2) 2.58(4) 3.101(4) 122(3)
N2 H2N O8 4_666 0.81(2) 2.26(2) 3.003(4) 152(4)
N3 H3N O3 . 0.84(2) 2.47(3) 3.044(4) 127(3)
N4 H4N O5 . 0.83(2) 2.14(3) 2.862(4) 144(4)
C10 H10A O8 4_566 0.97 2.40 3.359(6) 172
C12 H12 O8 4_566 0.93 2.60 3.508(6) 166
C28 H28B O2 1_655 0.97 2.47 3.210(7) 133
C28 H28A O5 1_655 0.97 2.47 3.342(6) 149
C35 H35A O4 . 0.97 2.38 2.761(5) 103
C37 H37B O7 4_666 0.97 2.47 2.985(6) 113
C42 H42 O7 . 0.93 2.44 2.752(4) 100
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_4
_geom_torsion
C6 C1 C2 C3 . . 1.5(7)
C38 C1 C2 C3 . . -177.8(4)
C1 C2 C3 C4 . . 0.3(8)
C2 C3 C4 C5 . . -0.9(8)
C3 C4 C5 C6 . . -0.4(8)
C4 C5 C6 C1 . . 2.3(7)
C4 C5 C6 O1 . . -173.8(4)
C2 C1 C6 C5 . . -2.8(6)
C38 C1 C6 C5 . . 176.5(4)
C2 C1 C6 O1 . . 173.6(4)
C38 C1 C6 O1 . . -7.0(6)
O1 C9 C10 O2 . . 41.1(6)
C16 C11 C12 C13 . . -1.6(7)
O2 C11 C12 C13 . . -179.3(5)
C11 C12 C13 C14 . . -0.5(9)
C12 C13 C14 C15 . . 1.7(10)
C13 C14 C15 C16 . . -0.9(9)
C12 C11 C16 C15 . . 2.4(6)
O2 C11 C16 C15 . . -179.8(4)
C12 C11 C16 C17 . . -178.1(4)
O2 C11 C16 C17 . . -0.2(6)
C14 C15 C16 C11 . . -1.1(7)
C14 C15 C16 C17 . . 179.3(5)
C11 C16 C17 N4 . . 83.3(5)
C15 C16 C17 N4 . . -97.2(5)
N4 C18 C19 N3 . . 61.8(4)
N3 C20 C21 C26 . . 71.6(5)
N3 C20 C21 C22 . . -110.4(4)
C26 C21 C22 C23 . . -0.6(7)
C20 C21 C22 C23 . . -178.6(4)
C21 C22 C23 C24 . . 0.8(8)
C22 C23 C24 C25 . . -0.9(9)
C23 C24 C25 C26 . . 0.8(8)
C24 C25 C26 O3 . . 179.8(5)
C24 C25 C26 C21 . . -0.6(7)
C22 C21 C26 C25 . . 0.5(7)
C20 C21 C26 C25 . . 178.6(4)
C22 C21 C26 O3 . . -179.9(4)
C20 C21 C26 O3 . . -1.8(6)
O3 C27 C28 O4 . . 56.8(7)
O4 C29 C30 C31 . . -177.0(4)
C34 C29 C30 C31 . . 0.2(7)
C29 C30 C31 C32 . . 1.8(7)
C30 C31 C32 C33 . . -1.4(8)
C31 C32 C33 C34 . . -1.1(7)
O4 C29 C34 C33 . . 174.9(4)
C30 C29 C34 C33 . . -2.4(6)
O4 C29 C34 C35 . . -4.8(6)
C30 C29 C34 C35 . . 177.8(4)
C32 C33 C34 C29 . . 2.9(6)
C32 C33 C34 C35 . . -177.4(4)
C29 C34 C35 N2 . . -91.4(4)
C33 C34 C35 N2 . . 88.8(5)
N2 C36 C37 N1 . . 41.6(6)
C6 C1 C38 N1 . . 76.5(5)
C2 C1 C38 N1 . . -104.2(5)
O5 C39 C40 C46 . . 166.5(4)
O6 C39 C40 C46 . . -13.6(5)
O5 C39 C40 C41 . . -16.9(5)
O6 C39 C40 C41 . . 163.0(3)
C46 C40 C41 C42 . . 3.2(5)
C39 C40 C41 C42 . . -173.5(3)
C40 C41 C42 C43 . . -0.8(6)
C41 C42 C43 C45 . . -2.5(5)
C41 C42 C43 C44 . . 172.8(3)
C42 C43 C44 O8 . . -177.9(4)
C45 C43 C44 O8 . . -2.8(6)
C42 C43 C44 O7 . . 0.2(5)
C45 C43 C44 O7 . . 175.3(3)
C42 C43 C45 C46 . . 3.2(5)
C44 C43 C45 C46 . . -172.0(3)
C41 C40 C46 C45 . . -2.4(5)
C39 C40 C46 C45 . . 174.2(3)
C43 C45 C46 C40 . . -0.8(6)
C10 C9 O1 C6 . . -178.7(4)
C5 C6 O1 C9 . . -34.0(6)
C1 C6 O1 C9 . . 149.7(4)
C9 C10 O2 C11 . . 178.9(4)
C16 C11 O2 C10 . . 131.3(4)
C12 C11 O2 C10 . . -50.8(6)
C25 C26 O3 C27 . . -36.7(7)
C21 C26 O3 C27 . . 143.7(4)
C28 C27 O3 C26 . . -160.0(4)
C27 C28 O4 C29 . . 176.2(4)
C34 C29 O4 C28 . . 140.7(5)
C30 C29 O4 C28 . . -41.9(7)
O5 C39 O6 Ni1 . . -4.2(6)
C40 C39 O6 Ni1 . . 175.8(2)
N1 Ni1 O6 C39 . . 78.3(3)
N3 Ni1 O6 C39 . . -102.3(3)
N4 Ni1 O6 C39 . . -19.1(3)
N2 Ni1 O6 C39 . . 159.4(3)
O8 C44 O7 Ni1 . 4_565 14.3(6)
C43 C44 O7 Ni1 . 4_565 -163.6(2)
C36 C37 N1 C38 . . 81.0(5)
C36 C37 N1 Ni1 . . -48.9(5)
C1 C38 N1 C37 . . 54.7(5)
C1 C38 N1 Ni1 . . 179.6(3)
O6 Ni1 N1 C37 . . 122.4(3)
O7 Ni1 N1 C37 4_666 . -57.8(3)
N4 Ni1 N1 C37 . . -144.7(3)
N2 Ni1 N1 C37 . . 32.9(3)
O6 Ni1 N1 C38 . . -8.1(3)
O7 Ni1 N1 C38 4_666 . 171.7(3)
N4 Ni1 N1 C38 . . 84.8(3)
N2 Ni1 N1 C38 . . -97.6(3)
C34 C35 N2 C36 . . -66.6(4)
C34 C35 N2 Ni1 . . 168.8(3)
C37 C36 N2 C35 . . -142.5(4)
C37 C36 N2 Ni1 . . -11.6(5)
O6 Ni1 N2 C35 . . 18.2(3)
O7 Ni1 N2 C35 4_666 . -159.3(3)
N1 Ni1 N2 C35 . . 114.2(3)
N3 Ni1 N2 C35 . . -71.2(3)
O6 Ni1 N2 C36 . . -107.9(3)
O7 Ni1 N2 C36 4_666 . 74.6(3)
N1 Ni1 N2 C36 . . -11.9(3)
N3 Ni1 N2 C36 . . 162.6(3)
C18 C19 N3 C20 . . 83.7(4)
C18 C19 N3 Ni1 . . -47.0(3)
C21 C20 N3 C19 . . 61.7(4)
C21 C20 N3 Ni1 . . -175.6(3)
O6 Ni1 N3 C19 . . 111.2(2)
O7 Ni1 N3 C19 4_666 . -68.6(2)
N4 Ni1 N3 C19 . . 19.0(2)
N2 Ni1 N3 C19 . . -158.5(2)
O6 Ni1 N3 C20 . . -15.3(3)
O7 Ni1 N3 C20 4_666 . 164.9(3)
N4 Ni1 N3 C20 . . -107.5(3)
N2 Ni1 N3 C20 . . 75.0(3)
C19 C18 N4 C17 . . 89.0(4)
C19 C18 N4 Ni1 . . -41.1(3)
C16 C17 N4 C18 . . 69.4(4)
C16 C17 N4 Ni1 . . -167.5(2)
O6 Ni1 N4 C18 . . -77.3(2)
O7 Ni1 N4 C18 4_666 . 100.2(2)
N1 Ni1 N4 C18 . . -173.6(2)
N3 Ni1 N4 C18 . . 11.9(2)
O6 Ni1 N4 C17 . . 156.3(2)
O7 Ni1 N4 C17 4_666 . -26.1(2)
N1 Ni1 N4 C17 . . 60.0(3)
N3 Ni1 N4 C17 . . -114.5(3)
