#------------------------------------------------------------------------------
#$Date: 2019-10-28 17:10:15 +0100 (Mon 28 de Oct de 2019) $
#$Revision: 220226 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/51/4515106.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_4515106
loop_
_publ_author_name
'Liu, Guo-Cheng'
'Lu, Xue'
'Li, Xiao-Wu'
'Wang, Xiu-Li'
'Xu, Na'
'Li, Yan'
'Lin, Hong-Yan'
'Chen, Yong-Qiang'
_publ_section_title
;
 Metal/Carboxylate-Induced Versatile Structures of Nine 0D → 3D
 Complexes with Different Fluorescent and Electrochemical Behaviors
;
_journal_issue                   17
_journal_name_full               'ACS Omega'
_journal_page_first              17366
_journal_paper_doi               10.1021/acsomega.9b02124
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C41 H28 N8 Ni2 O11 S2, C4 H9 N O, 5(H2 O)'
_chemical_formula_sum            'C45 H47 N9 Ni2 O17 S2'
_chemical_formula_weight         1167.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.854(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0807(4)
_cell_length_b                   24.8681(11)
_cell_length_c                   20.3417(9)
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.20
_cell_volume                     5038.7(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29730
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.353
_diffrn_reflns_theta_min         1.303
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9234
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0722P)²+7.3285P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6589
_reflns_number_total             9234
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao9b02124_si_001.cif
_cod_data_source_block           6
_cod_database_code               4515106
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.860
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ni1 Ni 0.52448(5) 0.75230(2) 0.64932(2) 0.02089(15) Uani 1 1 d . .
Ni2 Ni -0.26054(4) 0.25788(2) 0.98647(2) 0.01934(14) Uani 1 1 d . .
S1 S 0.02791(14) 0.50917(5) 0.85030(7) 0.0442(3) Uani 1 1 d . .
S2 S 0.23990(14) 0.00170(5) 0.80212(6) 0.0460(3) Uani 1 1 d . .
O1 O 0.1918(4) 0.51888(16) 0.7476(2) 0.0673(12) Uani 1 1 d . .
O2 O -0.1863(5) 0.54242(16) 0.9909(2) 0.0716(13) Uani 1 1 d . .
O3 O 0.0637(5) 0.01503(17) 0.9027(2) 0.0809(10) Uani 1 1 d . .
O4 O 0.4480(5) 0.03572(17) 0.6594(2) 0.0809(10) Uani 1 1 d . .
O5 O 0.5120(3) 0.76582(12) 0.75119(13) 0.0261(6) Uani 1 1 d . .
O6 O 0.7064(3) 0.74297(13) 0.72386(13) 0.0320(7) Uani 1 1 d . .
O7 O 1.1108(3) 0.74654(13) 0.92008(13) 0.0308(7) Uani 1 1 d . .
O8 O 1.0573(2) 0.72640(12) 1.01772(12) 0.0244(6) Uani 1 1 d . .
O9 O 0.6028(2) 0.76190(11) 1.06479(11) 0.0181(4) Uani 1 1 d . .
O10 O 0.4318(2) 0.76116(12) 0.98024(12) 0.0256(6) Uani 1 1 d . .
O11 O 0.3314(2) 0.76504(11) 0.61032(11) 0.0181(4) Uani 1 1 d . .
H11 H 0.2718 0.7748 0.6389 0.022 Uiso 1 1 calc R U
N1 N 0.4737(3) 0.67232(15) 0.66181(16) 0.0284(8) Uani 1 1 d . .
N2 N 0.2503(4) 0.60680(16) 0.7609(2) 0.0427(10) Uani 1 1 d . .
H2C H 0.2372 0.6355 0.7826 0.051 Uiso 1 1 calc R U
N3 N -0.1695(4) 0.46364(16) 0.9369(2) 0.0400(10) Uani 1 1 d . .
H3C H -0.1366 0.4489 0.9047 0.048 Uiso 1 1 calc R U
N4 N -0.2962(3) 0.33979(14) 0.99985(16) 0.0264(8) Uani 1 1 d . .
N5 N -0.2147(3) 0.17674(15) 0.97559(17) 0.0278(8) Uani 1 1 d . .
N6 N 0.0052(4) 0.10279(16) 0.8820(2) 0.0415(10) Uani 1 1 d . .
H6 H 0.0185 0.1299 0.8577 0.050 Uiso 1 1 calc R U
N7 N 0.4185(4) -0.04519(18) 0.7028(2) 0.0501(11) Uani 1 1 d . .
H7 H 0.3750 -0.0620 0.7296 0.060 Uiso 1 1 calc R U
N8 N 0.5602(3) -0.16621(15) 0.64095(16) 0.0293(8) Uani 1 1 d . .
C1 C 0.5095(5) 0.6316(2) 0.6253(2) 0.0387(11) Uani 1 1 d . .
H1 H 0.5677 0.6384 0.5950 0.046 Uiso 1 1 calc R U
C2 C 0.4631(5) 0.5804(2) 0.6311(3) 0.0483(13) Uani 1 1 d . .
H2 H 0.4898 0.5531 0.6047 0.058 Uiso 1 1 calc R U
C3 C 0.3773(5) 0.5691(2) 0.6757(3) 0.0460(12) Uani 1 1 d . .
H3 H 0.3462 0.5343 0.6804 0.055 Uiso 1 1 calc R U
C4 C 0.3383(4) 0.61136(19) 0.7135(2) 0.0344(10) Uani 1 1 d . .
C5 C 0.3898(4) 0.66152(18) 0.7048(2) 0.0320(10) Uani 1 1 d . .
H5 H 0.3647 0.6896 0.7304 0.038 Uiso 1 1 calc R U
C6 C 0.1845(5) 0.5622(2) 0.7757(3) 0.0433(12) Uani 1 1 d . .
C7 C 0.1000(5) 0.5677(2) 0.8284(2) 0.0394(11) Uani 1 1 d . .
C8 C 0.0634(5) 0.6105(2) 0.8634(2) 0.0459(13) Uani 1 1 d . .
H8 H 0.0927 0.6455 0.8581 0.055 Uiso 1 1 calc R U
C9 C -0.0225(5) 0.5961(2) 0.9080(2) 0.0456(13) Uani 1 1 d . .
H9 H -0.0565 0.6206 0.9358 0.055 Uiso 1 1 calc R U
C10 C -0.0517(5) 0.5425(2) 0.9066(2) 0.0388(11) Uani 1 1 d . .
C11 C -0.1419(5) 0.5165(2) 0.9483(2) 0.0413(12) Uani 1 1 d . .
C12 C -0.2465(4) 0.43051(19) 0.9725(2) 0.0344(10) Uani 1 1 d . .
C13 C -0.3417(5) 0.4494(2) 1.0098(3) 0.0508(14) Uani 1 1 d . .
H13 H -0.3592 0.4860 1.0125 0.061 Uiso 1 1 calc R U
C14 C -0.4089(5) 0.4124(2) 1.0425(3) 0.0551(15) Uani 1 1 d . .
H14 H -0.4715 0.4241 1.0685 0.066 Uiso 1 1 calc R U
C15 C -0.3845(5) 0.3587(2) 1.0371(2) 0.0390(11) Uani 1 1 d . .
H15 H -0.4306 0.3345 1.0601 0.047 Uiso 1 1 calc R U
C16 C -0.2297(4) 0.37536(18) 0.9684(2) 0.0303(10) Uani 1 1 d . .
H16 H -0.1687 0.3625 0.9423 0.036 Uiso 1 1 calc R U
C17 C -0.2522(5) 0.1387(2) 1.0155(2) 0.0426(12) Uani 1 1 d . .
H17 H -0.3090 0.1480 1.0457 0.051 Uiso 1 1 calc R U
C18 C -0.2094(5) 0.0862(2) 1.0132(3) 0.0525(14) Uani 1 1 d . .
H18 H -0.2381 0.0607 1.0413 0.063 Uiso 1 1 calc R U
C19 C -0.1236(5) 0.0713(2) 0.9693(3) 0.0485(13) Uani 1 1 d . .
H19 H -0.0944 0.0360 0.9672 0.058 Uiso 1 1 calc R U
C20 C -0.0829(4) 0.11074(18) 0.9285(2) 0.0334(10) Uani 1 1 d . .
C21 C -0.1323(4) 0.16252(18) 0.9331(2) 0.0309(10) Uani 1 1 d . .
H21 H -0.1066 0.1887 0.9050 0.037 Uiso 1 1 calc R U
C22 C 0.0715(5) 0.0566(2) 0.8715(2) 0.0442(12) Uani 1 1 d . .
C23 C 0.1573(5) 0.0597(2) 0.8187(2) 0.0410(12) Uani 1 1 d . .
C24 C 0.1827(5) 0.1005(2) 0.7779(3) 0.0475(13) Uani 1 1 d . .
H24 H 0.1466 0.1348 0.7794 0.057 Uiso 1 1 calc R U
C25 C 0.2683(5) 0.0855(2) 0.7336(3) 0.0457(12) Uani 1 1 d . .
H25 H 0.2959 0.1089 0.7028 0.055 Uiso 1 1 calc R U
C26 C 0.3080(5) 0.0330(2) 0.7397(2) 0.0413(12) Uani 1 1 d . .
C27 C 0.3984(5) 0.0083(2) 0.6976(2) 0.0439(12) Uani 1 1 d . .
C28 C 0.5031(5) -0.0769(2) 0.6689(2) 0.0368(11) Uani 1 1 d . .
C29 C 0.6086(5) -0.0561(2) 0.6401(3) 0.0515(14) Uani 1 1 d . .
H29 H 0.6261 -0.0194 0.6405 0.062 Uiso 1 1 calc R U
C30 C 0.6856(6) -0.0916(2) 0.6111(3) 0.0595(16) Uani 1 1 d . .
H30 H 0.7545 -0.0788 0.5897 0.071 Uiso 1 1 calc R U
C31 C 0.6620(5) -0.1460(2) 0.6133(2) 0.0441(12) Uani 1 1 d . .
H31 H 0.7183 -0.1694 0.5950 0.053 Uiso 1 1 calc R U
C32 C 0.4825(4) -0.13144(19) 0.6675(2) 0.0330(10) Uani 1 1 d . .
H32 H 0.4106 -0.1449 0.6860 0.040 Uiso 1 1 calc R U
C33 C 0.6348(4) 0.75398(17) 0.76778(19) 0.0258(9) Uani 1 1 d . .
C34 C 0.6912(4) 0.75217(17) 0.84051(18) 0.0230(9) Uani 1 1 d . .
C35 C 0.8282(4) 0.74524(16) 0.86267(18) 0.0226(9) Uani 1 1 d . .
H35 H 0.8873 0.7416 0.8321 0.027 Uiso 1 1 calc R U
C36 C 0.8766(4) 0.74382(16) 0.93090(18) 0.0215(8) Uani 1 1 d . .
C37 C 0.7878(4) 0.74972(17) 0.97648(18) 0.0228(9) Uani 1 1 d . .
H37 H 0.8200 0.7492 1.0218 0.027 Uiso 1 1 calc R U
C38 C 0.6518(4) 0.75643(16) 0.95468(18) 0.0204(8) Uani 1 1 d . .
C39 C 0.6039(4) 0.75753(17) 0.88696(18) 0.0233(9) Uani 1 1 d . .
H39 H 0.5125 0.7619 0.8724 0.028 Uiso 1 1 calc R U
C40 C 1.0229(4) 0.73807(17) 0.95723(19) 0.0228(9) Uani 1 1 d . .
C41 C 0.5544(4) 0.76046(15) 1.00452(18) 0.0187(8) Uani 1 1 d . .
O1W O -0.2181(7) 0.2181(2) 0.6917(3) 0.128(3) Uani 1 1 d . .
H1A H -0.1956 0.2336 0.6570 0.153 Uiso 1 1 d R U
H1B H -0.2154 0.2417 0.7231 0.153 Uiso 1 1 d R U
O2W O 0.0642(6) 0.21201(19) 0.8293(4) 0.130(3) Uani 1 1 d . .
H2A H 0.1247 0.2257 0.8084 0.156 Uiso 1 1 d R U
H2B H 0.0932 0.2142 0.8713 0.156 Uiso 1 1 d R U
O3W O -0.1546(5) 0.2850(2) 0.8118(2) 0.0889(15) Uani 1 1 d . .
H3A H -0.0863 0.2643 0.8236 0.107 Uiso 1 1 d R U
H3B H -0.1345 0.3089 0.7847 0.107 Uiso 1 1 d R U
O4W O -0.3338(8) 0.3578(4) 0.6940(3) 0.180(3) Uani 1 1 d . .
H4A H -0.3724 0.3310 0.7116 0.216 Uiso 1 1 d R U
H4B H -0.3971 0.3748 0.6683 0.216 Uiso 1 1 d R U
O5W O -0.1117(9) 0.3921(3) 0.8205(4) 0.177(4) Uani 1 1 d . .
H5A H -0.0651 0.4202 0.8128 0.213 Uiso 1 1 d R U
H5B H -0.0657 0.3757 0.8540 0.213 Uiso 1 1 d R U
C42 C 0.6231(10) 0.9145(5) 0.9037(5) 0.157(6) Uani 1 1 d D .
C43 C 0.7277(12) 0.8957(4) 0.8083(4) 0.188(7) Uani 1 1 d D .
H43A H 0.6444 0.8892 0.7900 0.226 Uiso 1 1 calc R U
H43B H 0.7786 0.8680 0.8018 0.226 Uiso 1 1 calc R U
H43C H 0.7571 0.9246 0.7902 0.226 Uiso 1 1 calc R U
C44 C 0.8634(10) 0.9019(5) 0.9189(6) 0.248(10) Uani 1 1 d D .
H44A H 0.9031 0.9334 0.9181 0.297 Uiso 1 1 calc R U
H44B H 0.9119 0.8772 0.9027 0.297 Uiso 1 1 calc R U
H44C H 0.8554 0.8937 0.9602 0.297 Uiso 1 1 calc R U
C45 C 0.6350(16) 0.9263(7) 0.9764(5) 0.309(13) Uani 1 1 d D .
H45A H 0.6382 0.9613 0.9826 0.370 Uiso 1 1 calc R U
H45B H 0.7089 0.9116 0.9974 0.370 Uiso 1 1 calc R U
H45C H 0.5651 0.9130 0.9918 0.370 Uiso 1 1 calc R U
N9 N 0.7327(7) 0.9043(3) 0.8794(4) 0.125(3) Uani 1 1 d D .
O12 O 0.5127(9) 0.9170(5) 0.8713(7) 0.281(8) Uani 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'
S S 0.1246 0.1234 '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
O11 Ni1 O9 99.93(10) . 4_575
O11 Ni1 N8 89.05(12) . 1_565
O9 Ni1 N8 90.31(12) 4_575 1_565
O11 Ni1 N1 87.55(12) . .
O9 Ni1 N1 94.14(12) 4_575 .
N8 Ni1 N1 174.80(13) 1_565 .
O11 Ni1 O5 99.27(10) . .
O9 Ni1 O5 160.68(10) 4_575 .
N8 Ni1 O5 87.85(12) 1_565 .
N1 Ni1 O5 88.83(12) . .
O11 Ni1 O6 160.09(10) . .
O9 Ni1 O6 99.98(10) 4_575 .
N8 Ni1 O6 91.31(13) 1_565 .
N1 Ni1 O6 90.55(13) . .
O5 Ni1 O6 60.86(10) . .
O11 Ni2 O10 99.11(10) 2_546 3_567
O11 Ni2 N5 91.89(12) 2_546 .
O10 Ni2 N5 91.35(13) 3_567 .
O11 Ni2 N4 89.95(12) 2_546 .
O10 Ni2 N4 90.68(12) 3_567 .
N5 Ni2 N4 177.02(13) . .
O11 Ni2 O8 98.42(10) 2_546 3_667
O10 Ni2 O8 162.42(10) 3_567 3_667
N5 Ni2 O8 86.70(12) . 3_667
N4 Ni2 O8 90.71(12) . 3_667
O11 Ni2 O7 158.91(10) 2_546 3_667
O10 Ni2 O7 101.81(10) 3_567 3_667
N5 Ni2 O7 84.91(12) . 3_667
N4 Ni2 O7 92.54(12) . 3_667
O8 Ni2 O7 60.63(9) 3_667 3_667
C10 S1 C7 91.4(2) . .
C26 S2 C23 91.5(2) . .
C33 O5 Ni1 91.2(2) . .
C33 O6 Ni1 87.6(2) . .
C40 O7 Ni2 85.8(2) . 3_667
C40 O8 Ni2 92.3(2) . 3_667
C41 O9 Ni1 133.0(2) . 4_576
C41 O10 Ni2 135.1(2) . 3_567
Ni2 O11 Ni1 123.54(12) 2_556 .
Ni2 O11 H11 118.2 2_556 .
Ni1 O11 H11 118.2 . .
C5 N1 C1 117.7(4) . .
C5 N1 Ni1 117.7(3) . .
C1 N1 Ni1 124.3(3) . .
C6 N2 C4 126.9(4) . .
C6 N2 H2C 116.5 . .
C4 N2 H2C 116.5 . .
C11 N3 C12 126.4(4) . .
C11 N3 H3C 116.8 . .
C12 N3 H3C 116.8 . .
C16 N4 C15 117.7(4) . .
C16 N4 Ni2 118.4(3) . .
C15 N4 Ni2 123.9(3) . .
C21 N5 C17 117.9(4) . .
C21 N5 Ni2 119.6(3) . .
C17 N5 Ni2 122.0(3) . .
C22 N6 C20 126.9(4) . .
C22 N6 H6 116.6 . .
C20 N6 H6 116.6 . .
C27 N7 C28 127.4(4) . .
C27 N7 H7 116.3 . .
C28 N7 H7 116.3 . .
C32 N8 C31 117.4(4) . .
C32 N8 Ni1 118.7(3) . 1_545
C31 N8 Ni1 123.7(3) . 1_545
N1 C1 C2 122.1(4) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C1 C2 C3 120.3(5) . .
C1 C2 H2 119.8 . .
C3 C2 H2 119.8 . .
C2 C3 C4 118.0(5) . .
C2 C3 H3 121.0 . .
C4 C3 H3 121.0 . .
C5 C4 C3 118.0(4) . .
C5 C4 N2 116.8(4) . .
C3 C4 N2 125.2(4) . .
N1 C5 C4 123.9(4) . .
N1 C5 H5 118.1 . .
C4 C5 H5 118.1 . .
O1 C6 N2 123.3(5) . .
O1 C6 C7 120.3(5) . .
N2 C6 C7 116.4(5) . .
C8 C7 C6 133.3(5) . .
C8 C7 S1 111.5(4) . .
C6 C7 S1 115.2(4) . .
C7 C8 C9 112.7(5) . .
C7 C8 H8 123.6 . .
C9 C8 H8 123.6 . .
C10 C9 C8 113.0(5) . .
C10 C9 H9 123.5 . .
C8 C9 H9 123.5 . .
C9 C10 C11 124.2(5) . .
C9 C10 S1 111.4(4) . .
C11 C10 S1 124.4(4) . .
O2 C11 N3 123.1(4) . .
O2 C11 C10 120.0(5) . .
N3 C11 C10 116.8(4) . .
C16 C12 C13 117.9(4) . .
C16 C12 N3 117.8(4) . .
C13 C12 N3 124.3(4) . .
C14 C13 C12 118.0(5) . .
C14 C13 H13 121.0 . .
C12 C13 H13 121.0 . .
C15 C14 C13 120.5(5) . .
C15 C14 H14 119.7 . .
C13 C14 H14 119.7 . .
N4 C15 C14 122.1(5) . .
N4 C15 H15 118.9 . .
C14 C15 H15 118.9 . .
N4 C16 C12 123.6(4) . .
N4 C16 H16 118.2 . .
C12 C16 H16 118.2 . .
N5 C17 C18 122.0(5) . .
N5 C17 H17 119.0 . .
C18 C17 H17 119.0 . .
C17 C18 C19 120.3(5) . .
C17 C18 H18 119.8 . .
C19 C18 H18 119.8 . .
C18 C19 C20 117.9(5) . .
C18 C19 H19 121.1 . .
C20 C19 H19 121.1 . .
C19 C20 C21 118.2(4) . .
C19 C20 N6 125.3(4) . .
C21 C20 N6 116.5(4) . .
N5 C21 C20 123.7(4) . .
N5 C21 H21 118.2 . .
C20 C21 H21 118.2 . .
O3 C22 N6 124.0(5) . .
O3 C22 C23 120.8(5) . .
N6 C22 C23 115.2(4) . .
C24 C23 C22 131.9(5) . .
C24 C23 S2 111.3(4) . .
C22 C23 S2 116.8(4) . .
C23 C24 C25 112.9(5) . .
C23 C24 H24 123.6 . .
C25 C24 H24 123.6 . .
C26 C25 C24 113.6(5) . .
C26 C25 H25 123.2 . .
C24 C25 H25 123.2 . .
C25 C26 C27 122.9(5) . .
C25 C26 S2 110.8(4) . .
C27 C26 S2 126.3(4) . .
O4 C27 N7 122.6(5) . .
O4 C27 C26 119.7(5) . .
N7 C27 C26 117.6(4) . .
C32 C28 C29 118.7(5) . .
C32 C28 N7 117.5(4) . .
C29 C28 N7 123.7(5) . .
C30 C29 C28 117.7(5) . .
C30 C29 H29 121.1 . .
C28 C29 H29 121.1 . .
C29 C30 C31 120.5(5) . .
C29 C30 H30 119.7 . .
C31 C30 H30 119.7 . .
N8 C31 C30 122.0(5) . .
N8 C31 H31 119.0 . .
C30 C31 H31 119.0 . .
N8 C32 C28 123.6(4) . .
N8 C32 H32 118.2 . .
C28 C32 H32 118.2 . .
O6 C33 O5 120.3(4) . .
O6 C33 C34 121.3(3) . .
O5 C33 C34 118.5(3) . .
C39 C34 C35 119.3(3) . .
C39 C34 C33 118.8(3) . .
C35 C34 C33 121.9(3) . .
C34 C35 C36 120.0(3) . .
C34 C35 H35 120.0 . .
C36 C35 H35 120.0 . .
C37 C36 C35 119.7(3) . .
C37 C36 C40 118.1(3) . .
C35 C36 C40 122.1(3) . .
C38 C37 C36 120.4(3) . .
C38 C37 H37 119.8 . .
C36 C37 H37 119.8 . .
C37 C38 C39 119.7(3) . .
C37 C38 C41 120.3(3) . .
C39 C38 C41 120.0(3) . .
C38 C39 C34 120.8(3) . .
C38 C39 H39 119.6 . .
C34 C39 H39 119.6 . .
O8 C40 O7 120.6(3) . .
O8 C40 C36 118.6(3) . .
O7 C40 C36 120.8(3) . .
O9 C41 O10 126.7(3) . .
O9 C41 C38 117.5(3) . .
O10 C41 C38 115.8(3) . .
H1A O1W H1B 108.6 . .
H2A O2W H2B 107.9 . .
H3A O3W H3B 109.5 . .
H4A O4W H4B 106.6 . .
H5A O5W H5B 106.3 . .
O12 C42 N9 124.6(8) . .
O12 C42 C45 117.3(8) . .
N9 C42 C45 118.1(8) . .
N9 C43 H43A 109.5 . .
N9 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
N9 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
N9 C44 H44A 109.5 . .
N9 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
N9 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C42 C45 H45A 109.5 . .
C42 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C42 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C42 N9 C44 123.6(7) . .
C42 N9 C43 120.3(6) . .
C44 N9 C43 116.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O11 2.011(2) .
Ni1 O9 2.030(2) 4_575
Ni1 N8 2.070(4) 1_565
Ni1 N1 2.079(4) .
Ni1 O5 2.122(3) .
Ni1 O6 2.205(3) .
Ni2 O11 1.996(2) 2_546
Ni2 O10 2.006(3) 3_567
Ni2 N5 2.089(4) .
Ni2 N4 2.093(4) .
Ni2 O8 2.100(3) 3_667
Ni2 O7 2.241(3) 3_667
S1 C10 1.711(5) .
S1 C7 1.716(5) .
S2 C26 1.719(5) .
S2 C23 1.725(5) .
O1 C6 1.227(6) .
O2 C11 1.218(6) .
O3 C22 1.223(6) .
O4 C27 1.198(6) .
O5 C33 1.266(5) .
O6 C33 1.263(5) .
O7 C40 1.267(5) .
O8 C40 1.260(5) .
O9 C41 1.248(4) .
O10 C41 1.258(4) .
O11 H11 0.9300 .
N1 C5 1.334(5) .
N1 C1 1.338(6) .
N2 C6 1.351(6) .
N2 C4 1.411(6) .
N2 H2C 0.8600 .
N3 C11 1.357(6) .
N3 C12 1.407(6) .
N3 H3C 0.8600 .
N4 C16 1.331(5) .
N4 C15 1.340(5) .
N5 C21 1.335(5) .
N5 C17 1.338(6) .
N6 C22 1.362(6) .
N6 C20 1.407(6) .
N6 H6 0.8600 .
N7 C27 1.348(6) .
N7 C28 1.415(6) .
N7 H7 0.8600 .
N8 C32 1.335(6) .
N8 C31 1.343(5) .
C1 C2 1.369(7) .
C1 H1 0.9300 .
C2 C3 1.375(7) .
C2 H2 0.9300 .
C3 C4 1.395(7) .
C3 H3 0.9300 .
C4 C5 1.373(6) .
C5 H5 0.9300 .
C6 C7 1.474(7) .
C7 C8 1.363(7) .
C8 C9 1.394(7) .
C8 H8 0.9300 .
C9 C10 1.367(7) .
C9 H9 0.9300 .
C10 C11 1.482(7) .
C12 C16 1.386(6) .
C12 C13 1.394(6) .
C13 C14 1.374(7) .
C13 H13 0.9300 .
C14 C15 1.366(7) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C18 1.379(7) .
C17 H17 0.9300 .
C18 C19 1.386(7) .
C18 H18 0.9300 .
C19 C20 1.387(7) .
C19 H19 0.9300 .
C20 C21 1.389(6) .
C21 H21 0.9300 .
C22 C23 1.480(7) .
C23 C24 1.359(7) .
C24 C25 1.391(7) .
C24 H24 0.9300 .
C25 C26 1.365(7) .
C25 H25 0.9300 .
C26 C27 1.477(7) .
C28 C32 1.372(7) .
C28 C29 1.391(7) .
C29 C30 1.367(7) .
C29 H29 0.9300 .
C30 C31 1.375(7) .
C30 H30 0.9300 .
C31 H31 0.9300 .
C32 H32 0.9300 .
C33 C34 1.502(5) .
C34 C39 1.393(5) .
C34 C35 1.396(5) .
C35 C36 1.399(5) .
C35 H35 0.9300 .
C36 C37 1.393(5) .
C36 C40 1.496(5) .
C37 C38 1.385(5) .
C37 H37 0.9300 .
C38 C39 1.388(5) .
C38 C41 1.519(5) .
C39 H39 0.9300 .
O1W H1A 0.8637 .
O1W H1B 0.8638 .
O2W H2A 0.8657 .
O2W H2B 0.8609 .
O3W H3A 0.8623 .
O3W H3B 0.8566 .
O4W H4A 0.8763 .
O4W H4B 0.8701 .
O5W H5A 0.8697 .
O5W H5B 0.8660 .
C42 O12 1.206(7) .
C42 N9 1.303(7) .
C42 C45 1.493(8) .
C43 N9 1.454(7) .
C43 H43A 0.8800 .
C43 H43B 0.8800 .
C43 H43C 0.8800 .
C44 N9 1.436(7) .
C44 H44A 0.8800 .
C44 H44B 0.8800 .
C44 H44C 0.8800 .
C45 H45A 0.8800 .
C45 H45B 0.8800 .
C45 H45C 0.8800 .
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
N2 H2C O1W 0.86 2.14 2.966(6) 162 2_556
N3 H3C O5W 0.86 2.26 3.088(8) 161 .
N6 H6 O2W 0.86 2.19 3.013(6) 160 .
O11 H11 O3W 0.93 1.68 2.607(4) 173 2_556
O1W H1A O7 0.86 1.93 2.756(5) 161 2_646
O1W H1B O3W 0.86 2.11 2.943(8) 162 .
O2W H2A O6 0.87 1.96 2.807(5) 164 2_646
O3W H3A O2W 0.86 1.99 2.836(7) 167 .
O3W H3B O5W 0.86 2.19 2.701(9) 118 .
O4W H4A O5 0.88 2.35 3.212(9) 170 2_546
O4W H4B O12 0.87 1.68 2.539(14) 169 2_546
O5W H5A S1 0.87 2.48 3.249(7) 149 .
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
C5 N1 C1 C2 -0.1(7) .
Ni1 N1 C1 C2 -173.7(4) .
N1 C1 C2 C3 -0.3(8) .
C1 C2 C3 C4 0.9(8) .
C2 C3 C4 C5 -1.1(7) .
C2 C3 C4 N2 179.5(5) .
C6 N2 C4 C5 177.4(5) .
C6 N2 C4 C3 -3.2(8) .
C1 N1 C5 C4 -0.1(6) .
Ni1 N1 C5 C4 173.8(3) .
C3 C4 C5 N1 0.8(7) .
N2 C4 C5 N1 -179.8(4) .
C4 N2 C6 O1 -1.6(8) .
C4 N2 C6 C7 178.9(4) .
O1 C6 C7 C8 -173.2(6) .
N2 C6 C7 C8 6.3(8) .
O1 C6 C7 S1 5.2(7) .
N2 C6 C7 S1 -175.3(4) .
C10 S1 C7 C8 0.1(4) .
C10 S1 C7 C6 -178.6(4) .
C6 C7 C8 C9 178.5(5) .
S1 C7 C8 C9 0.1(6) .
C7 C8 C9 C10 -0.3(7) .
C8 C9 C10 C11 -179.2(5) .
C8 C9 C10 S1 0.3(6) .
C7 S1 C10 C9 -0.2(4) .
C7 S1 C10 C11 179.3(4) .
C12 N3 C11 O2 -2.6(8) .
C12 N3 C11 C10 176.6(4) .
C9 C10 C11 O2 -6.3(8) .
S1 C10 C11 O2 174.3(4) .
C9 C10 C11 N3 174.5(5) .
S1 C10 C11 N3 -4.9(7) .
C11 N3 C12 C16 -160.0(5) .
C11 N3 C12 C13 22.2(8) .
C16 C12 C13 C14 2.7(8) .
N3 C12 C13 C14 -179.5(5) .
C12 C13 C14 C15 -1.4(9) .
C16 N4 C15 C14 1.2(7) .
Ni2 N4 C15 C14 -177.3(4) .
C13 C14 C15 N4 -0.6(9) .
C15 N4 C16 C12 0.3(6) .
Ni2 N4 C16 C12 178.9(3) .
C13 C12 C16 N4 -2.3(7) .
N3 C12 C16 N4 179.8(4) .
C21 N5 C17 C18 -0.6(7) .
Ni2 N5 C17 C18 -172.6(4) .
N5 C17 C18 C19 0.7(8) .
C17 C18 C19 C20 0.3(8) .
C18 C19 C20 C21 -1.3(7) .
C18 C19 C20 N6 178.9(5) .
C22 N6 C20 C19 -4.2(8) .
C22 N6 C20 C21 176.0(5) .
C17 N5 C21 C20 -0.5(6) .
Ni2 N5 C21 C20 171.7(3) .
C19 C20 C21 N5 1.5(7) .
N6 C20 C21 N5 -178.7(4) .
C20 N6 C22 O3 -0.8(9) .
C20 N6 C22 C23 179.6(4) .
O3 C22 C23 C24 -179.8(6) .
N6 C22 C23 C24 -0.2(9) .
O3 C22 C23 S2 2.0(7) .
N6 C22 C23 S2 -178.3(4) .
C26 S2 C23 C24 -0.2(4) .
C26 S2 C23 C22 178.3(4) .
C22 C23 C24 C25 -178.4(5) .
S2 C23 C24 C25 -0.2(6) .
C23 C24 C25 C26 0.6(7) .
C24 C25 C26 C27 179.8(5) .
C24 C25 C26 S2 -0.8(6) .
C23 S2 C26 C25 0.6(4) .
C23 S2 C26 C27 180.0(5) .
C28 N7 C27 O4 3.8(9) .
C28 N7 C27 C26 -178.2(5) .
C25 C26 C27 O4 5.6(8) .
S2 C26 C27 O4 -173.8(5) .
C25 C26 C27 N7 -172.5(5) .
S2 C26 C27 N7 8.1(7) .
C27 N7 C28 C32 -163.0(5) .
C27 N7 C28 C29 20.0(8) .
C32 C28 C29 C30 0.7(8) .
N7 C28 C29 C30 177.6(5) .
C28 C29 C30 C31 -2.7(9) .
C32 N8 C31 C30 -0.9(7) .
Ni1 N8 C31 C30 -177.3(4) 1_545
C29 C30 C31 N8 3.0(9) .
C31 N8 C32 C28 -1.3(6) .
Ni1 N8 C32 C28 175.3(3) 1_545
C29 C28 C32 N8 1.4(7) .
N7 C28 C32 N8 -175.7(4) .
Ni1 O6 C33 O5 -2.8(4) .
Ni1 O6 C33 C34 175.8(4) .
Ni1 O5 C33 O6 2.9(4) .
Ni1 O5 C33 C34 -175.8(3) .
O6 C33 C34 C39 -171.4(4) .
O5 C33 C34 C39 7.2(6) .
O6 C33 C34 C35 8.5(6) .
O5 C33 C34 C35 -172.9(4) .
C39 C34 C35 C36 -0.1(6) .
C33 C34 C35 C36 180.0(4) .
C34 C35 C36 C37 -0.4(6) .
C34 C35 C36 C40 -178.2(4) .
C35 C36 C37 C38 0.7(6) .
C40 C36 C37 C38 178.5(4) .
C36 C37 C38 C39 -0.3(6) .
C36 C37 C38 C41 177.4(4) .
C37 C38 C39 C34 -0.2(6) .
C41 C38 C39 C34 -178.0(4) .
C35 C34 C39 C38 0.5(6) .
C33 C34 C39 C38 -179.6(4) .
Ni2 O8 C40 O7 8.2(4) 3_667
Ni2 O8 C40 C36 -169.4(3) 3_667
Ni2 O7 C40 O8 -7.7(4) 3_667
Ni2 O7 C40 C36 169.8(4) 3_667
C37 C36 C40 O8 16.1(6) .
C35 C36 C40 O8 -166.1(4) .
C37 C36 C40 O7 -161.5(4) .
C35 C36 C40 O7 16.3(6) .
Ni1 O9 C41 O10 17.6(6) 4_576
Ni1 O9 C41 C38 -161.2(3) 4_576
Ni2 O10 C41 O9 -23.0(6) 3_567
Ni2 O10 C41 C38 155.8(3) 3_567
C37 C38 C41 O9 5.7(6) .
C39 C38 C41 O9 -176.6(4) .
C37 C38 C41 O10 -173.3(4) .
C39 C38 C41 O10 4.4(6) .
O12 C42 N9 C44 179.4(13) .
C45 C42 N9 C44 2.4(18) .
O12 C42 N9 C43 1(2) .
C45 C42 N9 C43 -176.3(11) .
