#------------------------------------------------------------------------------
#$Date: 2023-08-12 01:57:53 +0300 (Sat, 12 Aug 2023) $
#$Revision: 285634 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/37/7713738.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_7713738
loop_
_publ_author_name
'Yadav, Abhishek Kumar'
'Rajak, Richa'
'Ghule, Vikas'
'Dharavath, Srinivas'
_publ_section_title
;
 Energetic coordination compounds: self-assembled from the nitrogen-rich
 energetic C-C bonded pyrazole and triazole
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02410E
_journal_year                    2023
_chemical_formula_moiety         '0.5(C10 H16 N16 Ni2 O14), 2(C3 H7 N O)'
_chemical_formula_sum            'C11 H22 N10 Ni O9'
_chemical_formula_weight         497.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2023-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                68.215(2)
_cell_angle_beta                 87.615(2)
_cell_angle_gamma                85.471(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6407(7)
_cell_length_b                   12.0947(7)
_cell_length_c                   15.6754(9)
_cell_measurement_reflns_used    8183
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.23
_cell_volume                     2042.8(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43296
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.230
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6710
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1121 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.8998.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7235
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0672P)²+8.5078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5600
_reflns_number_total             7235
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02410e2.cif
_cod_data_source_block           12octc_o_0m
_cod_database_code               7713738
_shelx_shelxl_version_number     2018/3
_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_max   0.871
_shelx_estimated_absorpt_t_min   0.822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Ni01-H1A \\sim Ni01-H1B
 with sigma of 0.02
 Ni02-H9A \\sim Ni02-H9B
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B), O9(H9A,H9B)
3.b Rotating group:
 O2(H2A,H2B), O10(H10A,H10B), O3(H3A,H3B), O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 N14(H14), N5(H5), C1(H1), C6(H6), C22(H22), C14(H14A), C19(H19), C13(H13)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni01 Ni 0.92422(5) -0.07562(5) 0.62402(4) 0.01383(17) Uani 1 1 d D . . . .
Ni02 Ni 0.42133(5) 0.63865(5) -0.09842(4) 0.01529(17) Uani 1 1 d D . . . .
O2 O 0.8291(3) -0.1727(3) 0.5690(2) 0.0171(7) Uani 1 1 d . . . . .
H2A H 0.788526 -0.124638 0.524298 0.026 Uiso 1 1 d R U . . .
H2B H 0.779173 -0.210586 0.608718 0.026 Uiso 1 1 d R U . . .
O7 O 1.2527(3) 0.3163(3) 0.0220(2) 0.0219(8) Uani 1 1 d . . . . .
O10 O 0.3345(3) 0.5151(3) -0.1335(2) 0.0195(8) Uani 1 1 d . . . . .
H10A H 0.275954 0.550577 -0.165670 0.029 Uiso 1 1 d R U . . .
H10B H 0.306388 0.464306 -0.085061 0.029 Uiso 1 1 d R U . . .
O1 O 0.7888(3) -0.0582(3) 0.7118(2) 0.0225(8) Uani 1 1 d G . . . .
H1A H 0.720295 -0.037966 0.692273 0.034 Uiso 1 1 d DG U . . .
H1B H 0.781418 -0.113773 0.763909 0.034 Uiso 1 1 d DG U . . .
O14 O 0.7576(3) -0.0389(3) 0.3903(2) 0.0202(8) Uani 1 1 d . . . . .
O3 O 1.0214(3) 0.0108(3) 0.6874(2) 0.0217(8) Uani 1 1 d . . . . .
H3A H 0.999513 0.084555 0.668228 0.032 Uiso 1 1 d R U . . .
H3B H 1.091314 0.009176 0.669418 0.032 Uiso 1 1 d R U . . .
O13 O 0.6026(3) 0.0050(3) 0.4574(2) 0.0251(9) Uani 1 1 d . . . . .
O9 O 0.2786(3) 0.7632(4) -0.1325(2) 0.0293(9) Uani 1 1 d G . . . .
H9A H 0.231242 0.782435 -0.096852 0.044 Uiso 1 1 d DG U . . .
H9B H 0.263853 0.815049 -0.185572 0.044 Uiso 1 1 d DG U . . .
O6 O 1.0907(3) 0.4235(3) 0.0152(2) 0.0300(10) Uani 1 1 d . . . . .
O12 O 0.1669(3) 0.4253(3) 0.2979(2) 0.0276(9) Uani 1 1 d . . . . .
O4 O 0.6160(3) 0.3449(3) 0.4738(3) 0.0322(10) Uani 1 1 d . . . . .
O8 O 0.5121(3) 0.7616(3) -0.0649(3) 0.0275(9) Uani 1 1 d . . . . .
H8A H 0.485458 0.765362 -0.014601 0.041 Uiso 1 1 d R U . . .
H8B H 0.581797 0.734645 -0.053364 0.041 Uiso 1 1 d R U . . .
N1 N 0.8730(3) 0.0804(3) 0.5214(3) 0.0139(8) Uani 1 1 d . . . . .
N6 N 1.0173(3) 0.2319(4) 0.2732(3) 0.0154(9) Uani 1 1 d . . . . .
N2 N 0.9277(3) 0.1256(3) 0.4374(3) 0.0139(8) Uani 1 1 d . . . . .
N12 N 0.5203(3) 0.2811(3) 0.2320(3) 0.0155(9) Uani 1 1 d . . . . .
O5 O 0.6793(3) 0.4108(3) 0.3333(2) 0.0285(9) Uani 1 1 d . . . . .
N9 N 0.3678(3) 0.5577(4) 0.0330(3) 0.0177(9) Uani 1 1 d . . . . .
N10 N 0.4254(3) 0.4620(4) 0.0979(3) 0.0160(9) Uani 1 1 d . . . . .
N7 N 1.1421(3) 0.2712(4) 0.1458(3) 0.0182(9) Uani 1 1 d . . . . .
N3 N 0.6857(3) 0.3394(4) 0.4134(3) 0.0189(9) Uani 1 1 d . . . . .
N15 N 0.6474(3) 0.1200(4) 0.3125(3) 0.0181(9) Uani 1 1 d . . . . .
O15 O 0.5771(3) 0.0511(4) 0.6839(3) 0.0368(10) Uani 1 1 d . . . . .
O11 O 0.0911(3) 0.5840(4) 0.1928(3) 0.0384(11) Uani 1 1 d . . . . .
N14 N 0.4601(3) 0.1803(4) 0.3706(3) 0.0182(9) Uani 1 1 d . . . . .
H14 H 0.458988 0.125965 0.426555 0.022 Uiso 1 1 calc R U . . .
N16 N 0.6677(3) 0.0284(4) 0.3888(3) 0.0182(9) Uani 1 1 d . . . . .
N5 N 0.9590(3) 0.3881(4) 0.1566(3) 0.0180(9) Uani 1 1 d . . . . .
H5 H 0.957096 0.444003 0.101234 0.022 Uiso 1 1 calc R U . . .
N13 N 0.3743(3) 0.2678(4) 0.3339(3) 0.0179(9) Uani 1 1 d . . . . .
N8 N 1.1599(3) 0.3396(4) 0.0595(3) 0.0193(9) Uani 1 1 d . . . . .
N4 N 0.8776(3) 0.3797(4) 0.2246(3) 0.0182(9) Uani 1 1 d . . . . .
N11 N 0.1683(4) 0.5042(4) 0.2207(3) 0.0234(10) Uani 1 1 d . . . . .
O18 O 0.1038(4) 0.8244(4) -0.0449(3) 0.0511(13) Uani 1 1 d . . . . .
C3 C 0.8691(4) 0.2258(4) 0.3852(3) 0.0153(10) Uani 1 1 d . . . . .
N20 N -0.0765(4) 0.8911(4) -0.0190(3) 0.0312(11) Uani 1 1 d . . . . .
C8 C 0.3621(4) 0.4279(4) 0.1756(3) 0.0163(10) Uani 1 1 d . . . . .
C5 C 1.0418(4) 0.2991(4) 0.1866(3) 0.0171(10) Uani 1 1 d . . . . .
C10 C 0.5460(4) 0.1889(4) 0.3091(3) 0.0161(10) Uani 1 1 d . . . . .
C4 C 0.9179(4) 0.2840(4) 0.2930(3) 0.0154(10) Uani 1 1 d . . . . .
C1 C 0.7819(4) 0.1531(4) 0.5215(3) 0.0180(11) Uani 1 1 d . . . . .
H1 H 0.729315 0.142209 0.571498 0.022 Uiso 1 1 calc R U . . .
N17 N 1.1087(4) 0.3970(4) 0.5732(3) 0.0353(12) Uani 1 1 d . . . . .
C2 C 0.7746(4) 0.2480(4) 0.4373(3) 0.0162(10) Uani 1 1 d . . . . .
C9 C 0.4145(4) 0.3258(4) 0.2501(3) 0.0164(10) Uani 1 1 d . . . . .
O16 O 0.9904(4) 0.2475(4) 0.6423(4) 0.0555(14) Uani 1 1 d . . . . .
N19 N 0.3876(4) 0.6758(4) 0.2484(4) 0.0360(12) Uani 1 1 d . . . . .
C6 C 0.2696(4) 0.5833(5) 0.0712(3) 0.0210(11) Uani 1 1 d . . . . .
H6 H 0.213953 0.646364 0.041550 0.025 Uiso 1 1 calc R U . . .
C7 C 0.2619(4) 0.5030(4) 0.1612(3) 0.0188(11) Uani 1 1 d . . . . .
O17 O 0.4377(5) 0.7827(5) 0.0979(3) 0.0617(14) Uani 1 1 d . . . . .
N18 N 0.4118(5) 0.1234(5) 0.7324(5) 0.0513(16) Uani 1 1 d . . . . .
C22 C 0.0130(5) 0.8836(5) -0.0720(4) 0.0335(14) Uani 1 1 d . . . . .
H22 H 0.006254 0.927537 -0.136153 0.040 Uiso 1 1 calc R U . . .
C17 C 0.4132(6) 0.5710(5) 0.3282(4) 0.0378(15) Uani 1 1 d . . . . .
H17A H 0.350944 0.517053 0.339623 0.057 Uiso 1 1 calc R U . . .
H17B H 0.420470 0.593728 0.381517 0.057 Uiso 1 1 calc R U . . .
H17C H 0.485840 0.530447 0.318145 0.057 Uiso 1 1 calc R U . . .
C16 C 1.1850(6) 0.4565(6) 0.4956(4) 0.0446(17) Uani 1 1 d . . . . .
H16A H 1.262412 0.455744 0.518230 0.067 Uiso 1 1 calc R U . . .
H16B H 1.154941 0.539188 0.463851 0.067 Uiso 1 1 calc R U . . .
H16C H 1.188786 0.414328 0.452765 0.067 Uiso 1 1 calc R U . . .
C14 C 1.0552(5) 0.3026(6) 0.5776(5) 0.0410(16) Uani 1 1 d . . . . .
H14A H 1.066798 0.274849 0.528411 0.049 Uiso 1 1 calc R U . . .
C19 C 0.4539(6) 0.6969(6) 0.1724(5) 0.0453(17) Uani 1 1 d . . . . .
H19 H 0.518257 0.642112 0.175611 0.054 Uiso 1 1 calc R U . . .
C20 C -0.0737(6) 0.8235(6) 0.0795(4) 0.0399(15) Uani 1 1 d . . . . .
H20A H -0.133088 0.765629 0.096296 0.060 Uiso 1 1 calc R U . . .
H20B H -0.088457 0.878071 0.112425 0.060 Uiso 1 1 calc R U . . .
H20C H 0.002212 0.781110 0.096023 0.060 Uiso 1 1 calc R U . . .
C13 C 0.5050(6) 0.0444(7) 0.7415(5) 0.0483(18) Uani 1 1 d . . . . .
H13 H 0.513196 -0.021203 0.798310 0.058 Uiso 1 1 calc R U . . .
C21 C -0.1809(5) 0.9638(6) -0.0563(5) 0.0445(17) Uani 1 1 d . . . . .
H21A H -0.193334 1.026446 -0.030608 0.067 Uiso 1 1 calc R U . . .
H21B H -0.246641 0.913707 -0.040226 0.067 Uiso 1 1 calc R U . . .
H21C H -0.173343 1.000569 -0.123298 0.067 Uiso 1 1 calc R U . . .
C15 C 1.0958(6) 0.4459(7) 0.6457(5) 0.0486(18) Uani 1 1 d . . . . .
H15A H 1.171363 0.444065 0.671652 0.073 Uiso 1 1 calc R U . . .
H15B H 1.044419 0.397853 0.694116 0.073 Uiso 1 1 calc R U . . .
H15C H 1.062842 0.528434 0.619991 0.073 Uiso 1 1 calc R U . . .
C18 C 0.2865(6) 0.7501(7) 0.2487(6) 0.060(2) Uani 1 1 d . . . . .
H18A H 0.242684 0.765963 0.192886 0.089 Uiso 1 1 calc R U . . .
H18B H 0.308450 0.825735 0.250690 0.089 Uiso 1 1 calc R U . . .
H18C H 0.238859 0.709895 0.302790 0.089 Uiso 1 1 calc R U . . .
C11 C 0.3975(7) 0.2276(7) 0.6474(8) 0.086(3) Uani 1 1 d . . . . .
H11A H 0.464682 0.229895 0.607063 0.129 Uiso 1 1 calc R U . . .
H11B H 0.390471 0.300242 0.661535 0.129 Uiso 1 1 calc R U . . .
H11C H 0.327816 0.222518 0.616402 0.129 Uiso 1 1 calc R U . . .
C12 C 0.3269(9) 0.1012(12) 0.8047(10) 0.128(6) Uani 1 1 d . . . . .
H12A H 0.257067 0.076456 0.785995 0.192 Uiso 1 1 calc R U . . .
H12B H 0.308322 0.174235 0.817273 0.192 Uiso 1 1 calc R U . . .
H12C H 0.357281 0.037775 0.860369 0.192 Uiso 1 1 calc R U . . .
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'
Ni Ni 0.3393 1.1124 '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'
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
_geom_angle_publ_flag
O2 Ni01 O1 93.03(14) . . ?
O2 Ni01 O3 175.98(13) . . ?
O2 Ni01 N2 88.46(14) . 2_756 ?
O1 Ni01 O3 86.09(14) . . ?
N1 Ni01 O2 91.16(14) . . ?
N1 Ni01 O1 92.84(14) . . ?
N1 Ni01 O3 92.80(15) . . ?
N1 Ni01 N6 177.74(15) . 2_756 ?
N1 Ni01 N2 99.94(15) . 2_756 ?
N6 Ni01 O2 90.22(15) 2_756 . ?
N6 Ni01 O1 88.86(14) 2_756 . ?
N6 Ni01 O3 85.84(15) 2_756 . ?
N6 Ni01 N2 78.31(15) 2_756 2_756 ?
N2 Ni01 O1 167.10(14) 2_756 . ?
N2 Ni01 O3 91.54(15) 2_756 . ?
O10 Ni02 O8 178.61(14) . . ?
O9 Ni02 O10 91.96(15) . . ?
O9 Ni02 O8 89.07(16) . . ?
N12 Ni02 O10 91.43(14) 2_665 . ?
N12 Ni02 O9 87.72(14) 2_665 . ?
N12 Ni02 O8 87.67(15) 2_665 . ?
N12 Ni02 N10 78.18(15) 2_665 2_665 ?
N9 Ni02 O10 88.70(15) . . ?
N9 Ni02 O9 93.63(15) . . ?
N9 Ni02 O8 92.18(16) . . ?
N9 Ni02 N12 178.63(16) . 2_665 ?
N9 Ni02 N10 100.47(16) . 2_665 ?
N10 Ni02 O10 88.70(14) 2_665 . ?
N10 Ni02 O9 165.90(14) 2_665 . ?
N10 Ni02 O8 90.08(15) 2_665 . ?
Ni01 O2 H2A 109.8 . . ?
Ni01 O2 H2B 109.8 . . ?
H2A O2 H2B 104.1 . . ?
Ni02 O10 H10A 109.6 . . ?
Ni02 O10 H10B 109.5 . . ?
H10A O10 H10B 104.4 . . ?
Ni01 O1 H1A 121.1 . . ?
Ni01 O1 H1B 118.9 . . ?
H1A O1 H1B 104.5 . . ?
Ni01 O3 H3A 109.4 . . ?
Ni01 O3 H3B 109.3 . . ?
H3A O3 H3B 104.5 . . ?
Ni02 O9 H9A 128.6 . . ?
Ni02 O9 H9B 125.8 . . ?
H9A O9 H9B 104.6 . . ?
Ni02 O8 H8A 109.2 . . ?
Ni02 O8 H8B 109.3 . . ?
H8A O8 H8B 104.5 . . ?
N2 N1 Ni01 124.4(3) . . ?
C1 N1 Ni01 127.3(3) . . ?
C1 N1 N2 108.3(4) . . ?
C5 N6 Ni01 140.2(3) . 2_756 ?
C5 N6 C4 104.6(4) . . ?
C4 N6 Ni01 115.0(3) . 2_756 ?
N1 N2 Ni01 135.6(3) . 2_756 ?
C3 N2 Ni01 115.5(3) . 2_756 ?
C3 N2 N1 108.9(4) . . ?
C10 N12 Ni02 141.0(3) . 2_665 ?
C10 N12 C9 104.0(4) . . ?
C9 N12 Ni02 114.6(3) . 2_665 ?
N10 N9 Ni02 125.0(3) . . ?
C6 N9 Ni02 126.9(3) . . ?
C6 N9 N10 108.0(4) . . ?
N9 N10 Ni02 134.5(3) . 2_665 ?
C8 N10 Ni02 116.7(3) . 2_665 ?
C8 N10 N9 108.7(4) . . ?
N8 N7 C5 116.1(4) . . ?
O4 N3 C2 118.6(4) . . ?
O5 N3 O4 122.3(4) . . ?
O5 N3 C2 119.1(4) . . ?
N16 N15 C10 116.8(4) . . ?
N13 N14 H14 124.7 . . ?
C10 N14 H14 124.7 . . ?
C10 N14 N13 110.5(4) . . ?
O14 N16 N15 117.0(4) . . ?
O13 N16 O14 120.1(4) . . ?
O13 N16 N15 122.9(4) . . ?
N4 N5 H5 124.7 . . ?
C5 N5 H5 124.7 . . ?
C5 N5 N4 110.5(4) . . ?
C9 N13 N14 102.4(4) . . ?
O7 N8 N7 116.6(4) . . ?
O6 N8 O7 120.5(4) . . ?
O6 N8 N7 122.9(4) . . ?
C4 N4 N5 102.1(4) . . ?
O12 N11 C7 118.8(4) . . ?
O11 N11 O12 123.0(4) . . ?
O11 N11 C7 118.2(4) . . ?
N2 C3 C4 114.8(4) . . ?
N2 C3 C2 108.2(4) . . ?
C2 C3 C4 136.9(4) . . ?
C22 N20 C20 120.5(5) . . ?
C22 N20 C21 121.8(5) . . ?
C21 N20 C20 117.7(5) . . ?
N10 C8 C9 113.9(4) . . ?
N10 C8 C7 108.4(4) . . ?
C7 C8 C9 137.7(4) . . ?
N6 C5 N7 119.2(4) . . ?
N6 C5 N5 108.4(4) . . ?
N5 C5 N7 132.4(4) . . ?
N12 C10 N15 118.9(4) . . ?
N12 C10 N14 109.1(4) . . ?
N14 C10 N15 132.0(4) . . ?
N6 C4 C3 116.3(4) . . ?
N4 C4 N6 114.3(4) . . ?
N4 C4 C3 129.4(4) . . ?
N1 C1 H1 125.1 . . ?
N1 C1 C2 109.7(4) . . ?
C2 C1 H1 125.1 . . ?
C14 N17 C16 121.4(5) . . ?
C14 N17 C15 121.6(5) . . ?
C15 N17 C16 117.0(5) . . ?
N3 C2 C3 130.6(4) . . ?
C1 C2 N3 124.4(4) . . ?
C1 C2 C3 104.9(4) . . ?
N12 C9 C8 116.4(4) . . ?
N13 C9 N12 114.0(4) . . ?
N13 C9 C8 129.6(4) . . ?
C19 N19 C17 119.5(6) . . ?
C19 N19 C18 121.2(6) . . ?
C18 N19 C17 119.1(6) . . ?
N9 C6 H6 125.4 . . ?
N9 C6 C7 109.2(4) . . ?
C7 C6 H6 125.4 . . ?
C8 C7 N11 130.5(4) . . ?
C6 C7 N11 123.8(4) . . ?
C6 C7 C8 105.7(4) . . ?
C13 N18 C11 119.3(6) . . ?
C13 N18 C12 119.9(8) . . ?
C12 N18 C11 120.8(8) . . ?
O18 C22 N20 125.2(6) . . ?
O18 C22 H22 117.4 . . ?
N20 C22 H22 117.4 . . ?
N19 C17 H17A 109.5 . . ?
N19 C17 H17B 109.5 . . ?
N19 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N17 C16 H16A 109.5 . . ?
N17 C16 H16B 109.5 . . ?
N17 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N17 C14 H14A 117.9 . . ?
O16 C14 N17 124.2(6) . . ?
O16 C14 H14A 117.9 . . ?
N19 C19 H19 117.3 . . ?
O17 C19 N19 125.3(7) . . ?
O17 C19 H19 117.3 . . ?
N20 C20 H20A 109.5 . . ?
N20 C20 H20B 109.5 . . ?
N20 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O15 C13 N18 125.2(7) . . ?
O15 C13 H13 117.4 . . ?
N18 C13 H13 117.4 . . ?
N20 C21 H21A 109.5 . . ?
N20 C21 H21B 109.5 . . ?
N20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N17 C15 H15A 109.5 . . ?
N17 C15 H15B 109.5 . . ?
N17 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N19 C18 H18A 109.5 . . ?
N19 C18 H18B 109.5 . . ?
N19 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N18 C11 H11A 109.5 . . ?
N18 C11 H11B 109.5 . . ?
N18 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N18 C12 H12A 109.5 . . ?
N18 C12 H12B 109.5 . . ?
N18 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni01 O2 2.093(3) . ?
Ni01 O1 2.098(3) . ?
Ni01 O3 2.100(4) . ?
Ni01 N1 2.038(4) . ?
Ni01 N6 2.064(4) 2_756 ?
Ni01 N2 2.095(4) 2_756 ?
Ni02 O10 2.109(4) . ?
Ni02 O9 2.097(4) . ?
Ni02 O8 2.117(4) . ?
Ni02 N12 2.065(4) 2_665 ?
Ni02 N9 2.021(4) . ?
Ni02 N10 2.077(4) 2_665 ?
O2 H2A 0.8571 . ?
O2 H2B 0.8576 . ?
O7 N8 1.271(5) . ?
O10 H10A 0.8515 . ?
O10 H10B 0.8516 . ?
O1 H1A 0.8499 . ?
O1 H1B 0.8501 . ?
O14 N16 1.269(5) . ?
O3 H3A 0.8503 . ?
O3 H3B 0.8508 . ?
O13 N16 1.246(5) . ?
O9 H9A 0.8492 . ?
O9 H9B 0.8494 . ?
O6 N8 1.247(5) . ?
O12 N11 1.232(5) . ?
O4 N3 1.239(5) . ?
O8 H8A 0.8506 . ?
O8 H8B 0.8507 . ?
N1 N2 1.374(5) . ?
N1 C1 1.324(6) . ?
N6 C5 1.330(6) . ?
N6 C4 1.354(6) . ?
N2 C3 1.336(6) . ?
N12 C10 1.332(6) . ?
N12 C9 1.367(6) . ?
O5 N3 1.233(5) . ?
N9 N10 1.373(5) . ?
N9 C6 1.336(6) . ?
N10 C8 1.340(6) . ?
N7 N8 1.315(5) . ?
N7 C5 1.387(6) . ?
N3 C2 1.407(6) . ?
N15 N16 1.309(5) . ?
N15 C10 1.381(6) . ?
O15 C13 1.190(8) . ?
O11 N11 1.230(5) . ?
N14 H14 0.8800 . ?
N14 N13 1.371(5) . ?
N14 C10 1.342(6) . ?
N5 H5 0.8800 . ?
N5 N4 1.376(5) . ?
N5 C5 1.345(6) . ?
N13 C9 1.324(6) . ?
N4 C4 1.321(6) . ?
N11 C7 1.407(6) . ?
O18 C22 1.226(7) . ?
C3 C4 1.465(6) . ?
C3 C2 1.410(7) . ?
N20 C22 1.325(7) . ?
N20 C20 1.454(7) . ?
N20 C21 1.449(7) . ?
C8 C9 1.460(7) . ?
C8 C7 1.393(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.391(7) . ?
N17 C16 1.465(7) . ?
N17 C14 1.322(8) . ?
N17 C15 1.461(8) . ?
O16 C14 1.246(8) . ?
N19 C17 1.434(8) . ?
N19 C19 1.345(8) . ?
N19 C18 1.424(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(7) . ?
O17 C19 1.251(8) . ?
N18 C13 1.364(9) . ?
N18 C11 1.460(11) . ?
N18 C12 1.434(11) . ?
C22 H22 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C14 H14A 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C13 H13 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni01 N1 N2 Ni01 -3.3(6) . . . 2_756 ?
Ni01 N1 N2 C3 177.3(3) . . . . ?
Ni01 N1 C1 C2 -177.9(3) . . . . ?
Ni01 N6 C5 N7 -7.6(8) 2_756 . . . ?
Ni01 N6 C5 N5 174.4(4) 2_756 . . . ?
Ni01 N6 C4 N4 -175.9(3) 2_756 . . . ?
Ni01 N6 C4 C3 2.8(5) 2_756 . . . ?
Ni01 N2 C3 C4 0.5(5) 2_756 . . . ?
Ni01 N2 C3 C2 -178.5(3) 2_756 . . . ?
Ni02 N12 C10 N15 5.5(8) 2_665 . . . ?
Ni02 N12 C10 N14 -172.6(4) 2_665 . . . ?
Ni02 N12 C9 N13 175.2(3) 2_665 . . . ?
Ni02 N12 C9 C8 -4.2(6) 2_665 . . . ?
Ni02 N9 N10 Ni02 0.6(6) . . . 2_665 ?
Ni02 N9 N10 C8 -176.7(3) . . . . ?
Ni02 N9 C6 C7 176.5(3) . . . . ?
Ni02 N10 C8 C9 1.9(5) 2_665 . . . ?
Ni02 N10 C8 C7 -178.2(3) 2_665 . . . ?
O12 N11 C7 C8 -3.6(9) . . . . ?
O12 N11 C7 C6 176.3(5) . . . . ?
O4 N3 C2 C3 -174.7(5) . . . . ?
O4 N3 C2 C1 8.8(7) . . . . ?
N1 N2 C3 C4 -179.9(4) . . . . ?
N1 N2 C3 C2 1.1(5) . . . . ?
N1 C1 C2 N3 177.8(4) . . . . ?
N1 C1 C2 C3 0.6(6) . . . . ?
N2 N1 C1 C2 0.0(5) . . . . ?
N2 C3 C4 N6 -2.2(6) . . . . ?
N2 C3 C4 N4 176.2(5) . . . . ?
N2 C3 C2 N3 -178.0(5) . . . . ?
N2 C3 C2 C1 -1.0(5) . . . . ?
O5 N3 C2 C3 5.5(8) . . . . ?
O5 N3 C2 C1 -170.9(5) . . . . ?
N9 N10 C8 C9 179.8(4) . . . . ?
N9 N10 C8 C7 -0.3(6) . . . . ?
N9 C6 C7 N11 -179.3(5) . . . . ?
N9 C6 C7 C8 0.6(6) . . . . ?
N10 N9 C6 C7 -0.8(6) . . . . ?
N10 C8 C9 N12 1.5(6) . . . . ?
N10 C8 C9 N13 -177.7(5) . . . . ?
N10 C8 C7 N11 179.7(5) . . . . ?
N10 C8 C7 C6 -0.2(6) . . . . ?
O11 N11 C7 C8 176.8(5) . . . . ?
O11 N11 C7 C6 -3.3(8) . . . . ?
N14 N13 C9 N12 -0.5(6) . . . . ?
N14 N13 C9 C8 178.7(5) . . . . ?
N16 N15 C10 N12 -178.2(4) . . . . ?
N16 N15 C10 N14 -0.5(8) . . . . ?
N5 N4 C4 N6 -0.3(5) . . . . ?
N5 N4 C4 C3 -178.7(5) . . . . ?
N13 N14 C10 N12 0.5(6) . . . . ?
N13 N14 C10 N15 -177.3(5) . . . . ?
N8 N7 C5 N6 178.6(4) . . . . ?
N8 N7 C5 N5 -4.0(8) . . . . ?
N4 N5 C5 N6 -0.3(6) . . . . ?
N4 N5 C5 N7 -177.9(5) . . . . ?
C5 N6 C4 N4 0.1(6) . . . . ?
C5 N6 C4 C3 178.8(4) . . . . ?
C5 N7 N8 O7 178.6(4) . . . . ?
C5 N7 N8 O6 -1.3(7) . . . . ?
C5 N5 N4 C4 0.3(5) . . . . ?
C10 N12 C9 N13 0.8(6) . . . . ?
C10 N12 C9 C8 -178.6(4) . . . . ?
C10 N15 N16 O14 176.3(4) . . . . ?
C10 N15 N16 O13 -2.7(7) . . . . ?
C10 N14 N13 C9 0.0(5) . . . . ?
C4 N6 C5 N7 178.1(4) . . . . ?
C4 N6 C5 N5 0.1(5) . . . . ?
C4 C3 C2 N3 3.3(10) . . . . ?
C4 C3 C2 C1 -179.7(6) . . . . ?
C1 N1 N2 Ni01 178.8(4) . . . 2_756 ?
C1 N1 N2 C3 -0.7(5) . . . . ?
C2 C3 C4 N6 176.5(5) . . . . ?
C2 C3 C4 N4 -5.1(10) . . . . ?
C9 N12 C10 N15 177.4(4) . . . . ?
C9 N12 C10 N14 -0.7(5) . . . . ?
C9 C8 C7 N11 -0.4(11) . . . . ?
C9 C8 C7 C6 179.7(6) . . . . ?
C6 N9 N10 Ni02 178.0(4) . . . 2_665 ?
C6 N9 N10 C8 0.7(5) . . . . ?
C7 C8 C9 N12 -178.4(6) . . . . ?
C7 C8 C9 N13 2.4(10) . . . . ?
C17 N19 C19 O17 177.4(6) . . . . ?
C16 N17 C14 O16 179.1(6) . . . . ?
C20 N20 C22 O18 -1.9(10) . . . . ?
C21 N20 C22 O18 179.6(6) . . . . ?
C15 N17 C14 O16 -0.1(10) . . . . ?
C18 N19 C19 O17 2.8(10) . . . . ?
C11 N18 C13 O15 -1.8(11) . . . . ?
C12 N18 C13 O15 175.9(7) . . . . ?
