#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/80/2018025.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_2018025
loop_
_publ_author_name
'Yue, Xi-Teng'
'Nie, Jin-Ju'
'Li, Yan-Tuan'
'Wu, Zhi-Yong'
'Yan, Cui-Wei'
_publ_section_title
;
 (Aqua-2κO)bis(2,2'-bipyridine-1κ²N,N'){μ-N-[3-(dimethylamino)propyl]-N'-(2-oxidophenyl)oxamidato(3{-})-1:2κ²O,O':κ⁴O'',N,N',N''}copper(II)nickel(II)
 perchlorate
;
_journal_coeditor_code           BG3135
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m115
_journal_page_last               m118
_journal_paper_doi               10.1107/S0108270111008705
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Cu Ni (C13 H16 N3 O3) (C10 H8 N2)2 (H2 O)] Cl O4'
_chemical_formula_moiety         'C33 H34 Cu N7 Ni O4 +, Cl O4 -'
_chemical_formula_sum            'C33 H34 Cl Cu N7 Ni O8'
_chemical_formula_weight         814.37
_chemical_name_systematic
;
(Aqua-2κO)bis(2,2'-bipyridine-1κ²N,N'){μ-N-
[3-(dimethylamino)propyl]-N'-(2-oxidophenyl)oxamidato(3-)-
1:2κ²O,O':κ⁴O'',N,N',N''}
copper(II)nickel(II) perchlorate
;
_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                92.261(3)
_cell_angle_beta                 109.043(3)
_cell_angle_gamma                112.911(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4692(5)
_cell_length_b                   11.8976(5)
_cell_length_c                   15.1818(7)
_cell_measurement_reflns_used    3159
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.256
_cell_measurement_theta_min      2.593
_cell_volume                     1770.51(15)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX 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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15761
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  0.8326
_exptl_absorpt_correction_T_min  0.7506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.396
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8178
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0597P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                4749
_reflns_number_total             8178
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg3135.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2018025
_cod_database_fobs_code          2018025
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
Cu Cu1 0.54940(4) 0.94857(4) 0.18183(3) 0.04840(15) Uani d . 1 . .
Ni Ni1 0.24661(4) 0.57388(4) 0.30638(3) 0.04288(14) Uani d . 1 . .
O O1 0.4933(3) 1.0777(2) 0.13145(18) 0.0584(6) Uani d . 1 . .
O O2 0.2463(2) 0.7333(2) 0.25978(16) 0.0497(6) Uani d . 1 . .
O O3 0.4338(2) 0.63997(19) 0.29168(15) 0.0434(5) Uani d . 1 . .
O O4 0.4630(3) 0.8237(3) 0.0227(2) 0.0739(8) Uani d D 1 . .
H H4A 0.474(5) 0.854(3) -0.025(2) 0.099(17) Uiso d D 1 . .
H H4B 0.470(4) 0.756(2) 0.017(3) 0.078(16) Uiso d D 1 . .
N N1 0.3811(3) 0.8913(2) 0.20327(19) 0.0436(6) Uani d . 1 . .
N N2 0.5643(2) 0.8058(2) 0.23912(19) 0.0437(6) Uani d . 1 . .
N N3 0.7501(3) 1.0436(3) 0.2046(2) 0.0546(8) Uani d . 1 . .
N N4 0.1397(3) 0.4731(2) 0.1682(2) 0.0490(7) Uani d . 1 . .
N N5 0.0459(3) 0.5237(3) 0.2946(2) 0.0568(8) Uani d . 1 . .
N N6 0.2647(3) 0.4264(3) 0.36910(19) 0.0456(7) Uani d . 1 . .
N N7 0.3371(3) 0.6570(3) 0.4491(2) 0.0547(8) Uani d . 1 . .
C C1 0.3730(4) 1.0605(3) 0.1340(2) 0.0480(8) Uani d . 1 . .
C C2 0.3049(3) 0.9596(3) 0.1739(2) 0.0447(8) Uani d . 1 . .
C C3 0.1808(4) 0.9393(3) 0.1790(3) 0.0563(9) Uani d . 1 . .
H H3 0.1396 0.8756 0.2074 0.068 Uiso calc R 1 . .
C C4 0.1180(5) 1.0141(4) 0.1415(3) 0.0764(13) Uani d . 1 . .
H H4 0.0325 0.9984 0.1425 0.092 Uiso calc R 1 . .
C C5 0.1806(5) 1.1113(4) 0.1029(3) 0.0733(13) Uani d . 1 . .
H H5 0.1368 1.1607 0.0778 0.088 Uiso calc R 1 . .
C C6 0.3075(4) 1.1369(3) 0.1008(3) 0.0628(11) Uani d . 1 . .
H H6 0.3502 1.2055 0.0770 0.075 Uiso calc R 1 . .
C C7 0.3499(3) 0.7903(3) 0.2397(2) 0.0416(8) Uani d . 1 . .
C C8 0.4579(3) 0.7399(3) 0.2587(2) 0.0391(7) Uani d . 1 . .
C C9 0.6710(3) 0.7631(3) 0.2544(3) 0.0516(9) Uani d . 1 . .
H H9A 0.6314 0.6772 0.2225 0.062 Uiso calc R 1 . .
H H9B 0.7148 0.7675 0.3217 0.062 Uiso calc R 1 . .
C C10 0.7766(4) 0.8438(3) 0.2158(3) 0.0602(10) Uani d . 1 . .
H H10A 0.8505 0.8184 0.2309 0.072 Uiso calc R 1 . .
H H10B 0.7347 0.8301 0.1472 0.072 Uiso calc R 1 . .
C C11 0.8340(3) 0.9800(3) 0.2554(3) 0.0595(10) Uani d . 1 . .
H H11A 0.8438 0.9900 0.3215 0.071 Uiso calc R 1 . .
H H11B 0.9243 1.0207 0.2533 0.071 Uiso calc R 1 . .
C C12 0.7713(4) 1.0667(4) 0.1145(3) 0.0747(12) Uani d . 1 . .
H H12A 0.7469 0.9892 0.0759 0.112 Uiso calc R 1 . .
H H12B 0.8653 1.1204 0.1281 0.112 Uiso calc R 1 . .
H H12C 0.7152 1.1056 0.0810 0.112 Uiso calc R 1 . .
C C13 0.7959(4) 1.1643(4) 0.2652(4) 0.0861(14) Uani d . 1 . .
H H13A 0.8909 1.2134 0.2783 0.129 Uiso calc R 1 . .
H H13B 0.7825 1.1507 0.3238 0.129 Uiso calc R 1 . .
H H13C 0.7442 1.2074 0.2330 0.129 Uiso calc R 1 . .
C C14 0.1933(4) 0.4464(3) 0.1097(3) 0.0585(10) Uani d . 1 . .
H H14 0.2874 0.4745 0.1308 0.070 Uiso calc R 1 . .
C C15 0.1143(5) 0.3782(4) 0.0183(3) 0.0731(12) Uani d . 1 . .
H H15 0.1542 0.3611 -0.0218 0.088 Uiso calc R 1 . .
C C16 -0.0246(6) 0.3368(4) -0.0113(4) 0.0890(17) Uani d . 1 . .
H H16 -0.0803 0.2909 -0.0723 0.107 Uiso calc R 1 . .
C C17 -0.0810(4) 0.3628(4) 0.0485(3) 0.0727(13) Uani d . 1 . .
H H17 -0.1751 0.3340 0.0290 0.087 Uiso calc R 1 . .
C C18 0.0029(3) 0.4325(3) 0.1388(3) 0.0551(10) Uani d . 1 . .
C C19 -0.0472(3) 0.4691(3) 0.2073(3) 0.0586(10) Uani d . 1 . .
C C20 -0.1815(4) 0.4509(4) 0.1846(4) 0.0859(15) Uani d . 1 . .
H H20 -0.2453 0.4127 0.1236 0.103 Uiso calc R 1 . .
C C21 -0.2191(5) 0.4885(5) 0.2510(5) 0.1000(18) Uani d . 1 . .
H H21 -0.3091 0.4764 0.2357 0.120 Uiso calc R 1 . .
C C22 -0.1271(5) 0.5441(5) 0.3401(5) 0.1016(17) Uani d . 1 . .
H H22 -0.1518 0.5706 0.3868 0.122 Uiso calc R 1 . .
C C23 0.0067(4) 0.5598(4) 0.3591(4) 0.0811(13) Uani d . 1 . .
H H23 0.0712 0.5975 0.4199 0.097 Uiso calc R 1 . .
C C24 0.2219(3) 0.3108(3) 0.3256(3) 0.0581(10) Uani d . 1 . .
H H24 0.1832 0.2922 0.2597 0.070 Uiso calc R 1 . .
C C25 0.2319(4) 0.2170(4) 0.3734(3) 0.0714(12) Uani d . 1 . .
H H25 0.1998 0.1369 0.3405 0.086 Uiso calc R 1 . .
C C26 0.2903(4) 0.2444(4) 0.4710(3) 0.0786(13) Uani d . 1 . .
H H26 0.2979 0.1827 0.5051 0.094 Uiso calc R 1 . .
C C27 0.3367(4) 0.3629(4) 0.5170(3) 0.0655(11) Uani d . 1 . .
H H27 0.3782 0.3833 0.5829 0.079 Uiso calc R 1 . .
C C28 0.3217(3) 0.4529(3) 0.4652(2) 0.0492(9) Uani d . 1 . .
C C29 0.3653(3) 0.5832(4) 0.5089(2) 0.0539(9) Uani d . 1 . .
C C30 0.4299(4) 0.6277(5) 0.6063(3) 0.0798(14) Uani d . 1 . .
H H30 0.4507 0.5764 0.6474 0.096 Uiso calc R 1 . .
C C31 0.4626(5) 0.7498(6) 0.6408(4) 0.1030(18) Uani d . 1 . .
H H31 0.5046 0.7815 0.7058 0.124 Uiso calc R 1 . .
C C32 0.4327(5) 0.8231(5) 0.5788(4) 0.0975(16) Uani d . 1 . .
H H32 0.4543 0.9055 0.6009 0.117 Uiso calc R 1 . .
C C33 0.3706(4) 0.7746(4) 0.4841(3) 0.0763(12) Uani d . 1 . .
H H33 0.3509 0.8255 0.4422 0.092 Uiso calc R 1 . .
Cl Cl1 0.0908(3) 0.8999(3) 0.47311(18) 0.0861(7) Uani d PD 0.50 A -1
O O5 0.0854(9) 0.8854(8) 0.3851(5) 0.137(3) Uani d PD 0.50 A -1
O O6 0.0175(11) 0.9659(11) 0.4820(7) 0.171(4) Uani d PD 0.50 A -1
O O7 0.2209(7) 0.9679(6) 0.5332(6) 0.124(3) Uani d PD 0.50 A -1
O O8 0.0413(9) 0.7917(6) 0.5007(5) 0.142(3) Uani d PD 0.50 A -1
Cl Cl2 0.5093(11) 0.5178(8) -0.0044(8) 0.0829(17) Uani d PD 0.50 B -2
O O9 0.4630(19) 0.3965(10) -0.0017(13) 0.261(11) Uani d PD 0.50 B -2
O O10 0.5026(8) 0.5359(9) -0.0969(5) 0.119(3) Uani d PD 0.50 B -2
O O11 0.6448(8) 0.5849(12) 0.0541(6) 0.150(4) Uani d PD 0.50 B -2
O O12 0.4342(8) 0.5725(9) 0.0201(6) 0.106(3) Uani d PD 0.50 B -2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cu1 O1 . . 82.82(11) ?
N1 Cu1 N2 . . 83.15(10) ?
O1 Cu1 N2 . . 165.95(11) ?
N1 Cu1 N3 . . 160.19(12) ?
O1 Cu1 N3 . . 96.32(11) ?
N2 Cu1 N3 . . 96.68(11) ?
O2 Ni1 O3 . . 81.98(8) ?
O2 Ni1 N7 . . 94.29(11) ?
O3 Ni1 N7 . . 91.62(10) ?
O2 Ni1 N6 . . 173.02(10) ?
O3 Ni1 N6 . . 95.87(9) ?
N7 Ni1 N6 . . 79.10(12) ?
O2 Ni1 N4 . . 90.57(10) ?
O3 Ni1 N4 . . 93.93(10) ?
N7 Ni1 N4 . . 173.09(11) ?
N6 Ni1 N4 . . 96.21(10) ?
O2 Ni1 N5 . . 87.79(10) ?
O3 Ni1 N5 . . 167.36(10) ?
N7 Ni1 N5 . . 96.55(13) ?
N6 Ni1 N5 . . 95.14(11) ?
N4 Ni1 N5 . . 78.70(13) ?
C1 O1 Cu1 . . 111.8(2) ?
C7 O2 Ni1 . . 111.3(2) ?
C8 O3 Ni1 . . 111.32(19) ?
H4A O4 H4B . . 105(4) ?
C7 N1 C2 . . 128.4(3) ?
C7 N1 Cu1 . . 116.0(2) ?
C2 N1 Cu1 . . 115.5(2) ?
C8 N2 C9 . . 118.6(3) ?
C8 N2 Cu1 . . 112.8(2) ?
C9 N2 Cu1 . . 128.4(2) ?
C13 N3 C12 . . 108.6(3) ?
C13 N3 C11 . . 108.4(3) ?
C12 N3 C11 . . 109.6(3) ?
C13 N3 Cu1 . . 105.9(2) ?
C12 N3 Cu1 . . 111.4(2) ?
C11 N3 Cu1 . . 112.7(2) ?
C14 N4 C18 . . 119.5(3) ?
C14 N4 Ni1 . . 126.1(2) ?
C18 N4 Ni1 . . 114.4(3) ?
C23 N5 C19 . . 118.3(4) ?
C23 N5 Ni1 . . 126.0(3) ?
C19 N5 Ni1 . . 114.6(3) ?
C24 N6 C28 . . 118.1(3) ?
C24 N6 Ni1 . . 127.1(2) ?
C28 N6 Ni1 . . 114.8(2) ?
C33 N7 C29 . . 119.1(3) ?
C33 N7 Ni1 . . 126.0(3) ?
C29 N7 Ni1 . . 114.8(2) ?
O1 C1 C6 . . 123.8(3) ?
O1 C1 C2 . . 119.2(3) ?
C6 C1 C2 . . 117.0(4) ?
C3 C2 N1 . . 128.2(3) ?
C3 C2 C1 . . 121.1(3) ?
N1 C2 C1 . . 110.7(3) ?
C2 C3 C4 . . 119.6(4) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C5 C4 C3 . . 120.6(4) ?
C5 C4 H4 . . 119.7 ?
C3 C4 H4 . . 119.7 ?
C4 C5 C6 . . 120.9(4) ?
C4 C5 H5 . . 119.6 ?
C6 C5 H5 . . 119.6 ?
C5 C6 C1 . . 120.7(4) ?
C5 C6 H6 . . 119.6 ?
C1 C6 H6 . . 119.6 ?
O2 C7 N1 . . 128.8(3) ?
O2 C7 C8 . . 118.6(3) ?
N1 C7 C8 . . 112.5(3) ?
O3 C8 N2 . . 128.0(3) ?
O3 C8 C7 . . 116.6(3) ?
N2 C8 C7 . . 115.4(3) ?
N2 C9 C10 . . 110.1(3) ?
N2 C9 H9A . . 109.6 ?
C10 C9 H9A . . 109.6 ?
N2 C9 H9B . . 109.6 ?
C10 C9 H9B . . 109.6 ?
H9A C9 H9B . . 108.2 ?
C11 C10 C9 . . 112.9(3) ?
C11 C10 H10A . . 109.0 ?
C9 C10 H10A . . 109.0 ?
C11 C10 H10B . . 109.0 ?
C9 C10 H10B . . 109.0 ?
H10A C10 H10B . . 107.8 ?
N3 C11 C10 . . 114.5(3) ?
N3 C11 H11A . . 108.6 ?
C10 C11 H11A . . 108.6 ?
N3 C11 H11B . . 108.6 ?
C10 C11 H11B . . 108.6 ?
H11A C11 H11B . . 107.6 ?
N3 C12 H12A . . 109.5 ?
N3 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N3 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N3 C13 H13A . . 109.5 ?
N3 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
N3 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
N4 C14 C15 . . 122.4(4) ?
N4 C14 H14 . . 118.8 ?
C15 C14 H14 . . 118.8 ?
C16 C15 C14 . . 118.0(5) ?
C16 C15 H15 . . 121.0 ?
C14 C15 H15 . . 121.0 ?
C17 C16 C15 . . 120.1(4) ?
C17 C16 H16 . . 120.0 ?
C15 C16 H16 . . 120.0 ?
C16 C17 C18 . . 119.5(4) ?
C16 C17 H17 . . 120.2 ?
C18 C17 H17 . . 120.2 ?
N4 C18 C17 . . 120.5(4) ?
N4 C18 C19 . . 115.7(3) ?
C17 C18 C19 . . 123.7(4) ?
N5 C19 C20 . . 121.0(4) ?
N5 C19 C18 . . 115.7(3) ?
C20 C19 C18 . . 123.3(4) ?
C21 C20 C19 . . 119.7(5) ?
C21 C20 H20 . . 120.1 ?
C19 C20 H20 . . 120.1 ?
C20 C21 C22 . . 120.6(5) ?
C20 C21 H21 . . 119.7 ?
C22 C21 H21 . . 119.7 ?
C21 C22 C23 . . 117.2(5) ?
C21 C22 H22 . . 121.4 ?
C23 C22 H22 . . 121.4 ?
N5 C23 C22 . . 123.2(5) ?
N5 C23 H23 . . 118.4 ?
C22 C23 H23 . . 118.4 ?
N6 C24 C25 . . 123.2(4) ?
N6 C24 H24 . . 118.4 ?
C25 C24 H24 . . 118.4 ?
C24 C25 C26 . . 118.6(4) ?
C24 C25 H25 . . 120.7 ?
C26 C25 H25 . . 120.7 ?
C27 C26 C25 . . 119.2(4) ?
C27 C26 H26 . . 120.4 ?
C25 C26 H26 . . 120.4 ?
C26 C27 C28 . . 119.5(4) ?
C26 C27 H27 . . 120.2 ?
C28 C27 H27 . . 120.2 ?
N6 C28 C27 . . 121.4(3) ?
N6 C28 C29 . . 115.1(3) ?
C27 C28 C29 . . 123.5(3) ?
N7 C29 C30 . . 121.1(4) ?
N7 C29 C28 . . 116.1(3) ?
C30 C29 C28 . . 122.8(4) ?
C31 C30 C29 . . 118.6(5) ?
C31 C30 H30 . . 120.7 ?
C29 C30 H30 . . 120.7 ?
C32 C31 C30 . . 119.3(5) ?
C32 C31 H31 . . 120.3 ?
C30 C31 H31 . . 120.3 ?
C31 C32 C33 . . 119.3(5) ?
C31 C32 H32 . . 120.3 ?
C33 C32 H32 . . 120.3 ?
N7 C33 C32 . . 122.5(5) ?
N7 C33 H33 . . 118.7 ?
C32 C33 H33 . . 118.7 ?
O5 Cl1 O8 . . 112.5(5) ?
O5 Cl1 O7 . . 110.2(5) ?
O8 Cl1 O7 . . 108.8(5) ?
O5 Cl1 O6 . . 110.0(6) ?
O8 Cl1 O6 . . 108.6(7) ?
O7 Cl1 O6 . . 106.6(6) ?
O9 Cl2 O12 . . 112.8(10) ?
O9 Cl2 O11 . . 112.9(10) ?
O12 Cl2 O11 . . 107.8(9) ?
O9 Cl2 O10 . . 110.1(10) ?
O12 Cl2 O10 . . 107.1(8) ?
O11 Cl2 O10 . . 105.7(8) ?
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
Cu1 N1 . 1.924(3) y
Cu1 O1 . 1.975(2) y
Cu1 N2 . 1.980(3) y
Cu1 N3 . 2.030(3) y
Cu1 O4 . 2.456(3) y
Ni1 O2 . 2.051(2) y
Ni1 O3 . 2.071(2) y
Ni1 N7 . 2.077(3) y
Ni1 N6 . 2.077(3) y
Ni1 N4 . 2.079(3) y
Ni1 N5 . 2.083(3) y
O1 C1 . 1.329(4) ?
O2 C7 . 1.260(4) ?
O3 C8 . 1.274(3) ?
O4 H4A . 0.85(3) ?
O4 H4B . 0.84(3) ?
N1 C7 . 1.313(4) ?
N1 C2 . 1.397(4) ?
N2 C8 . 1.305(4) ?
N2 C9 . 1.454(4) ?
N3 C13 . 1.476(5) ?
N3 C12 . 1.484(5) ?
N3 C11 . 1.491(4) ?
N4 C14 . 1.323(5) ?
N4 C18 . 1.352(4) ?
N5 C23 . 1.322(5) ?
N5 C19 . 1.338(4) ?
N6 C24 . 1.327(4) ?
N6 C28 . 1.354(4) ?
N7 C33 . 1.334(5) ?
N7 C29 . 1.339(4) ?
C1 C6 . 1.402(5) ?
C1 C2 . 1.433(5) ?
C2 C3 . 1.376(5) ?
C3 C4 . 1.380(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.371(6) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.378(6) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.528(4) ?
C9 C10 . 1.528(5) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 C11 . 1.501(5) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 C15 . 1.387(5) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.374(7) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.362(7) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.386(5) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.466(6) ?
C19 C20 . 1.388(5) ?
C20 C21 . 1.343(7) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.355(7) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.399(6) ?
C22 H22 . 0.9300 ?
C23 H23 . 0.9300 ?
C24 C25 . 1.376(5) ?
C24 H24 . 0.9300 ?
C25 C26 . 1.376(6) ?
C25 H25 . 0.9300 ?
C26 C27 . 1.362(6) ?
C26 H26 . 0.9300 ?
C27 C28 . 1.385(5) ?
C27 H27 . 0.9300 ?
C28 C29 . 1.480(5) ?
C29 C30 . 1.392(5) ?
C30 C31 . 1.384(7) ?
C30 H30 . 0.9300 ?
C31 C32 . 1.361(7) ?
C31 H31 . 0.9300 ?
C32 C33 . 1.362(6) ?
C32 H32 . 0.9300 ?
C33 H33 . 0.9300 ?
Cl1 O5 . 1.319(7) ?
Cl1 O8 . 1.336(7) ?
Cl1 O7 . 1.351(7) ?
Cl1 O6 . 1.386(7) ?
Cl2 O9 . 1.338(9) ?
Cl2 O12 . 1.389(12) ?
Cl2 O11 . 1.386(11) ?
Cl2 O10 . 1.411(12) ?
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
O4 H4A O1 2_675 0.85(3) 1.92(2) 2.763(4) 176(4)
O4 H4B O9 2_665 0.84(3) 2.23(2) 3.087(18) 167(4)
O4 H4B O12 . 0.84(3) 2.07(2) 2.871(10) 160(4)
C15 H15 O11 2_665 0.93 2.36 3.176(12) 146.4
C21 H21 O10 2_565 0.93 2.47 3.226(10) 138.8
C26 H26 O7 1_545 0.93 2.46 3.322(8) 154.0
C27 H27 O3 2_666 0.93 2.49 3.233(4) 137.5
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_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 Cu1 O1 C1 . . . . -1.9(2) ?
N2 Cu1 O1 C1 . . . . -4.4(5) ?
N3 Cu1 O1 C1 . . . . -162.0(2) ?
O3 Ni1 O2 C7 . . . . 3.6(2) ?
N7 Ni1 O2 C7 . . . . 94.7(2) ?
N4 Ni1 O2 C7 . . . . -90.3(2) ?
N5 Ni1 O2 C7 . . . . -168.9(2) ?
O2 Ni1 O3 C8 . . . . -2.7(2) ?
N7 Ni1 O3 C8 . . . . -96.8(2) ?
N6 Ni1 O3 C8 . . . . -176.0(2) ?
N4 Ni1 O3 C8 . . . . 87.4(2) ?
N5 Ni1 O3 C8 . . . . 33.6(6) ?
O1 Cu1 N1 C7 . . . . 178.6(3) ?
N2 Cu1 N1 C7 . . . . -2.1(2) ?
N3 Cu1 N1 C7 . . . . -92.7(4) ?
O1 Cu1 N1 C2 . . . . 1.3(2) ?
N2 Cu1 N1 C2 . . . . -179.3(2) ?
N3 Cu1 N1 C2 . . . . 90.0(4) ?
N1 Cu1 N2 C8 . . . . 3.2(2) ?
O1 Cu1 N2 C8 . . . . 5.8(6) ?
N3 Cu1 N2 C8 . . . . 163.3(2) ?
N1 Cu1 N2 C9 . . . . 178.4(3) ?
O1 Cu1 N2 C9 . . . . -179.1(4) ?
N3 Cu1 N2 C9 . . . . -21.6(3) ?
N1 Cu1 N3 C13 . . . . -31.6(5) ?
O1 Cu1 N3 C13 . . . . 54.7(3) ?
N2 Cu1 N3 C13 . . . . -119.9(3) ?
N1 Cu1 N3 C12 . . . . -149.6(3) ?
O1 Cu1 N3 C12 . . . . -63.3(3) ?
N2 Cu1 N3 C12 . . . . 122.1(3) ?
N1 Cu1 N3 C11 . . . . 86.7(4) ?
O1 Cu1 N3 C11 . . . . 173.0(2) ?
N2 Cu1 N3 C11 . . . . -1.6(3) ?
O2 Ni1 N4 C14 . . . . 95.7(3) ?
O3 Ni1 N4 C14 . . . . 13.7(3) ?
N6 Ni1 N4 C14 . . . . -82.7(3) ?
N5 Ni1 N4 C14 . . . . -176.7(3) ?
O2 Ni1 N4 C18 . . . . -84.7(2) ?
O3 Ni1 N4 C18 . . . . -166.7(2) ?
N6 Ni1 N4 C18 . . . . 96.9(2) ?
N5 Ni1 N4 C18 . . . . 2.9(2) ?
O2 Ni1 N5 C23 . . . . -83.9(3) ?
O3 Ni1 N5 C23 . . . . -119.8(5) ?
N7 Ni1 N5 C23 . . . . 10.1(4) ?
N6 Ni1 N5 C23 . . . . 89.7(3) ?
N4 Ni1 N5 C23 . . . . -175.0(4) ?
O2 Ni1 N5 C19 . . . . 83.4(2) ?
O3 Ni1 N5 C19 . . . . 47.5(6) ?
N7 Ni1 N5 C19 . . . . 177.5(2) ?
N6 Ni1 N5 C19 . . . . -103.0(2) ?
N4 Ni1 N5 C19 . . . . -7.6(2) ?
O3 Ni1 N6 C24 . . . . -92.3(3) ?
N7 Ni1 N6 C24 . . . . 177.2(3) ?
N4 Ni1 N6 C24 . . . . 2.4(3) ?
N5 Ni1 N6 C24 . . . . 81.5(3) ?
O3 Ni1 N6 C28 . . . . 90.8(2) ?
N7 Ni1 N6 C28 . . . . 0.3(2) ?
N4 Ni1 N6 C28 . . . . -174.6(2) ?
N5 Ni1 N6 C28 . . . . -95.4(2) ?
O2 Ni1 N7 C33 . . . . 2.4(3) ?
O3 Ni1 N7 C33 . . . . 84.4(3) ?
N6 Ni1 N7 C33 . . . . -179.9(3) ?
N5 Ni1 N7 C33 . . . . -85.9(3) ?
O2 Ni1 N7 C29 . . . . -176.2(2) ?
O3 Ni1 N7 C29 . . . . -94.1(2) ?
N6 Ni1 N7 C29 . . . . 1.6(2) ?
N5 Ni1 N7 C29 . . . . 95.6(2) ?
Cu1 O1 C1 C6 . . . . -178.6(3) ?
Cu1 O1 C1 C2 . . . . 2.2(4) ?
C7 N1 C2 C3 . . . . 2.2(6) ?
Cu1 N1 C2 C3 . . . . 179.0(3) ?
C7 N1 C2 C1 . . . . -177.3(3) ?
Cu1 N1 C2 C1 . . . . -0.5(3) ?
O1 C1 C2 C3 . . . . 179.2(3) ?
C6 C1 C2 C3 . . . . 0.0(5) ?
O1 C1 C2 N1 . . . . -1.2(4) ?
C6 C1 C2 N1 . . . . 179.6(3) ?
N1 C2 C3 C4 . . . . -176.8(3) ?
C1 C2 C3 C4 . . . . 2.7(5) ?
C2 C3 C4 C5 . . . . -2.7(6) ?
C3 C4 C5 C6 . . . . -0.2(7) ?
C4 C5 C6 C1 . . . . 3.0(6) ?
O1 C1 C6 C5 . . . . 178.0(3) ?
C2 C1 C6 C5 . . . . -2.8(5) ?
Ni1 O2 C7 N1 . . . . 175.9(3) ?
Ni1 O2 C7 C8 . . . . -4.0(4) ?
C2 N1 C7 O2 . . . . -2.5(6) ?
Cu1 N1 C7 O2 . . . . -179.3(3) ?
C2 N1 C7 C8 . . . . 177.4(3) ?
Cu1 N1 C7 C8 . . . . 0.6(4) ?
Ni1 O3 C8 N2 . . . . -178.9(3) ?
Ni1 O3 C8 C7 . . . . 1.4(3) ?
C9 N2 C8 O3 . . . . 0.9(5) ?
Cu1 N2 C8 O3 . . . . 176.6(3) ?
C9 N2 C8 C7 . . . . -179.4(3) ?
Cu1 N2 C8 C7 . . . . -3.7(3) ?
O2 C7 C8 O3 . . . . 1.8(4) ?
N1 C7 C8 O3 . . . . -178.1(3) ?
O2 C7 C8 N2 . . . . -177.9(3) ?
N1 C7 C8 N2 . . . . 2.2(4) ?
C8 N2 C9 C10 . . . . 173.0(3) ?
Cu1 N2 C9 C10 . . . . -1.9(4) ?
N2 C9 C10 C11 . . . . 54.3(4) ?
C13 N3 C11 C10 . . . . 164.4(3) ?
C12 N3 C11 C10 . . . . -77.2(4) ?
Cu1 N3 C11 C10 . . . . 47.5(4) ?
C9 C10 C11 N3 . . . . -84.5(4) ?
C18 N4 C14 C15 . . . . 0.3(5) ?
Ni1 N4 C14 C15 . . . . 179.9(3) ?
N4 C14 C15 C16 . . . . -0.5(6) ?
C14 C15 C16 C17 . . . . -0.1(6) ?
C15 C16 C17 C18 . . . . 0.8(6) ?
C14 N4 C18 C17 . . . . 0.5(5) ?
Ni1 N4 C18 C17 . . . . -179.2(3) ?
C14 N4 C18 C19 . . . . -178.5(3) ?
Ni1 N4 C18 C19 . . . . 1.9(3) ?
C16 C17 C18 N4 . . . . -1.0(5) ?
C16 C17 C18 C19 . . . . 177.9(4) ?
C23 N5 C19 C20 . . . . 0.1(5) ?
Ni1 N5 C19 C20 . . . . -168.3(3) ?
C23 N5 C19 C18 . . . . 179.3(3) ?
Ni1 N5 C19 C18 . . . . 10.9(4) ?
N4 C18 C19 N5 . . . . -8.6(4) ?
C17 C18 C19 N5 . . . . 172.5(3) ?
N4 C18 C19 C20 . . . . 170.6(3) ?
C17 C18 C19 C20 . . . . -8.3(5) ?
N5 C19 C20 C21 . . . . 0.1(6) ?
C18 C19 C20 C21 . . . . -179.1(4) ?
C19 C20 C21 C22 . . . . -0.1(8) ?
C20 C21 C22 C23 . . . . 0.0(8) ?
C19 N5 C23 C22 . . . . -0.2(6) ?
Ni1 N5 C23 C22 . . . . 166.7(4) ?
C21 C22 C23 N5 . . . . 0.2(7) ?
C28 N6 C24 C25 . . . . 0.4(5) ?
Ni1 N6 C24 C25 . . . . -176.5(3) ?
N6 C24 C25 C26 . . . . -0.6(6) ?
C24 C25 C26 C27 . . . . -0.3(6) ?
C25 C26 C27 C28 . . . . 1.4(6) ?
C24 N6 C28 C27 . . . . 0.8(5) ?
Ni1 N6 C28 C27 . . . . 178.0(3) ?
C24 N6 C28 C29 . . . . -179.2(3) ?
Ni1 N6 C28 C29 . . . . -1.9(4) ?
C26 C27 C28 N6 . . . . -1.7(5) ?
C26 C27 C28 C29 . . . . 178.3(3) ?
C33 N7 C29 C30 . . . . -0.6(5) ?
Ni1 N7 C29 C30 . . . . 178.0(3) ?
C33 N7 C29 C28 . . . . 178.3(3) ?
Ni1 N7 C29 C28 . . . . -3.1(4) ?
N6 C28 C29 N7 . . . . 3.3(4) ?
C27 C28 C29 N7 . . . . -176.6(3) ?
N6 C28 C29 C30 . . . . -177.7(3) ?
C27 C28 C29 C30 . . . . 2.3(5) ?
N7 C29 C30 C31 . . . . 1.1(6) ?
C28 C29 C30 C31 . . . . -177.7(4) ?
C29 C30 C31 C32 . . . . -0.9(7) ?
C30 C31 C32 C33 . . . . 0.3(8) ?
C29 N7 C33 C32 . . . . -0.1(6) ?
Ni1 N7 C33 C32 . . . . -178.5(4) ?
C31 C32 C33 N7 . . . . 0.2(8) ?
