#------------------------------------------------------------------------------
#$Date: 2019-11-23 01:08:39 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231731 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/63/4346343.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_4346343
loop_
_publ_author_name
'Myers, Thomas W.'
'Chavez, David E.'
'Hanson, Susan K.'
'Scharff, R. Jason'
'Scott, Brian L.'
'Veauthier, Jacqueline M.'
'Wu, Ruilian'
_publ_section_title
;
 Independent Control of Optical and Explosive Properties:
 Pyrazole-Tetrazine Complexes of First Row Transition Metals.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8077
_journal_page_last               8086
_journal_paper_doi               10.1021/acs.inorgchem.5b01313
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C28 H27 N26.5 Ni O6'
_chemical_formula_weight         889.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.593(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.004(5)
_cell_length_b                   12.044(3)
_cell_length_c                   32.076(8)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.84
_cell_measurement_theta_min      2.48
_cell_volume                     8327(3)
_computing_cell_refinement       cell_now
_computing_data_collection       'bruker apex'
_computing_data_reduction        'bruker saint'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            42595
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.136
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             3652
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         8281
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0732P)²+39.4315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                6685
_reflns_number_total             8281
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01313_si_002.cif
_cod_data_source_block           twm13
_cod_original_cell_volume        8328(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C28 H27 N26.50 Ni O6'
_cod_database_code               4346343
_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   0.842
_shelx_estimated_absorpt_t_max   0.909
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.82648(2) 0.52430(3) 0.37479(2) 0.02321(13) Uani 1 1 d . . . . .
O1 O 0.45792(13) 0.4918(3) 0.29905(13) 0.0731(10) Uani 1 1 d . . . . .
O2 O 0.36500(10) 0.43275(19) 0.28092(8) 0.0341(5) Uani 1 1 d . . . . .
O3 O 0.43628(14) 0.3252(3) 0.31509(10) 0.0642(9) Uani 1 1 d . . . A 1
O4 O 0.66534(13) 1.1149(2) 0.38412(9) 0.0470(7) Uani 1 1 d . . . . .
O5 O 0.67853(14) 1.27752(19) 0.35872(7) 0.0425(6) Uani 1 1 d . . . . .
O6 O 0.67864(19) 1.2538(3) 0.42474(8) 0.0725(11) Uani 1 1 d . . . . .
N1 N 0.58948(13) 0.4866(3) 0.29989(9) 0.0380(7) Uani 1 1 d . . . . .
H1A H 0.6007 0.4864 0.2751 0.046 Uiso 1 1 calc R U . . .
H1B H 0.5501 0.4794 0.3011 0.046 Uiso 1 1 calc R U . . .
N2 N 0.69158(12) 0.5087(2) 0.33222(8) 0.0233(5) Uani 1 1 d . . . . .
N3 N 0.73219(11) 0.50517(19) 0.36876(7) 0.0196(5) Uani 1 1 d . . . . .
N4 N 0.65288(13) 0.5030(2) 0.40811(9) 0.0328(6) Uani 1 1 d . . . . .
N5 N 0.61115(13) 0.5067(3) 0.37252(9) 0.0376(7) Uani 1 1 d . . . . .
N6 N 0.75749(12) 0.4820(2) 0.44132(8) 0.0245(5) Uani 1 1 d . . . . .
N7 N 0.81775(12) 0.4938(2) 0.43698(8) 0.0292(6) Uani 1 1 d . . . . .
N8 N 0.7165(2) 0.9111(3) 0.36355(11) 0.0659(12) Uani 1 1 d . . . . .
H8A H 0.6814 0.8744 0.3565 0.079 Uiso 1 1 calc R U . . .
H8B H 0.7164 0.9842 0.3637 0.079 Uiso 1 1 calc R U . . .
N9 N 0.76556(12) 0.7451(2) 0.37273(8) 0.0263(6) Uani 1 1 d . . . . .
N10 N 0.81886(11) 0.6928(2) 0.38106(7) 0.0233(5) Uani 1 1 d . . . . .
N11 N 0.8769(2) 0.8567(4) 0.39397(13) 0.0555(11) Uani 0.9 1 d . . P B 1
N12 N 0.8233(5) 0.9147(7) 0.3841(2) 0.071(3) Uani 0.85 1 d . . P B 1
N13 N 0.91796(15) 0.5725(4) 0.38889(17) 0.0391(13) Uani 0.9 1 d D . P B 1
N14 N 0.92609(19) 0.6895(6) 0.39657(14) 0.0513(16) Uani 0.9 1 d D . P B 1
N11B N 0.851(2) 0.400(5) 0.3616(17) 0.027(14) Uiso 0.06 1 d . . P B 2
N12B N 0.8342(15) 0.908(4) 0.3941(11) 0.021(7) Uiso 0.14 1 d . . P B 2
N13B N 0.9192(18) 0.575(3) 0.376(2) 0.06(3) Uiso 0.07 1 d D . P B 2
N14B N 0.9196(9) 0.6494(19) 0.3946(7) 0.021(5) Uiso 0.18 1 d D . P B 2
N15 N 0.82402(12) 0.7373(2) 0.23042(8) 0.0261(6) Uani 1 1 d . . . . .
H15A H 0.8270 0.7997 0.2450 0.031 Uiso 1 1 calc R U . . .
H15B H 0.8236 0.7386 0.2029 0.031 Uiso 1 1 calc R U . . .
N16 N 0.82095(11) 0.6433(2) 0.29211(7) 0.0208(5) Uani 1 1 d . . . . .
N17 N 0.82255(11) 0.54589(19) 0.31064(7) 0.0207(5) Uani 1 1 d . . . . .
N18 N 0.81375(13) 0.4523(2) 0.24523(8) 0.0293(6) Uani 1 1 d . . . . .
N19 N 0.81193(13) 0.5480(2) 0.22543(8) 0.0285(6) Uani 1 1 d . . . . .
N20 N 0.82882(12) 0.3552(2) 0.30997(8) 0.0264(6) Uani 1 1 d . . . . .
N21 N 0.83245(17) 0.3609(3) 0.35306(10) 0.0339(7) Uani 1 1 d . . . . .
N22 N 0.42000(13) 0.4156(3) 0.29903(9) 0.0343(6) Uani 1 1 d . . . . .
N23 N 0.67427(12) 1.2154(2) 0.38883(8) 0.0273(6) Uani 1 1 d . . . . .
N24 N 0.8200(2) 0.7685(4) 0.47359(13) 0.0758(13) Uani 1 1 d . . . . .
N25 N 0.5129(4) 0.6918(8) 0.4758(3) 0.076(3) Uiso 0.5 1 d . . P . .
N26 N 0.5967(2) 0.7878(5) 0.33567(15) 0.0817(16) Uani 1 1 d . . . . .
N27 N 0.9552(2) 0.5016(5) 0.29072(14) 0.0714(16) Uani 0.914(7) 1 d . . P C 1
N27A N 0.9506(13) 0.622(3) 0.2836(11) 0.036(10) Uani 0.086(7) 1 d . . P C 2
C1 C 0.63166(14) 0.4978(3) 0.33522(10) 0.0281(7) Uani 1 1 d . . . . .
C2 C 0.71181(14) 0.4933(2) 0.40459(9) 0.0223(6) Uani 1 1 d . . . . .
C3 C 0.6951(2) 0.4365(4) 0.49770(11) 0.0494(10) Uani 1 1 d . . . . .
H3A H 0.6597 0.4452 0.4740 0.074 Uiso 1 1 calc R U . . .
H3B H 0.6953 0.3611 0.5092 0.074 Uiso 1 1 calc R U . . .
H3C H 0.6919 0.4903 0.5201 0.074 Uiso 1 1 calc R U . . .
C4 C 0.75357(17) 0.4562(3) 0.48237(10) 0.0311(7) Uani 1 1 d . . . . .
C5 C 0.81297(18) 0.4526(3) 0.50449(10) 0.0410(9) Uani 1 1 d . . . . .
H5B H 0.8260 0.4370 0.5340 0.049 Uiso 1 1 calc R U . . .
C6 C 0.85139(18) 0.4761(4) 0.47586(11) 0.0454(10) Uani 1 1 d . . . . .
C7 C 0.9201(2) 0.4850(6) 0.48504(14) 0.092(2) Uani 1 1 d . . . . .
H7A H 0.9362 0.4691 0.5152 0.138 Uiso 1 1 calc R U . . .
H7B H 0.9373 0.4315 0.4675 0.138 Uiso 1 1 calc R U . . .
H7C H 0.9322 0.5603 0.4785 0.138 Uiso 1 1 calc R U . . .
C8 C 0.7692(2) 0.8570(3) 0.37381(11) 0.0429(9) Uani 1 1 d . . . . .
C9 C 0.87184(18) 0.7498(3) 0.39025(10) 0.0424(9) Uani 1 1 d D . . . .
C10 C 0.9813(4) 0.3968(8) 0.3840(3) 0.048(2) Uani 0.627(14) 1 d . . P B 1
H10A H 1.0257 0.3800 0.3878 0.071 Uiso 0.627(14) 1 calc R U P B 1
H10B H 0.9633 0.3536 0.4044 0.071 Uiso 0.627(14) 1 calc R U P B 1
H10C H 0.9604 0.3773 0.3550 0.071 Uiso 0.627(14) 1 calc R U P B 1
C11 C 0.9730(4) 0.5164(9) 0.3912(3) 0.036(2) Uani 0.627(14) 1 d D . P B 1
C12 C 1.0190(4) 0.5971(10) 0.4027(2) 0.0363(19) Uani 0.627(14) 1 d D . P B 1
H12A H 1.0625 0.5847 0.4074 0.044 Uiso 0.627(14) 1 calc R U P B 1
C13 C 0.9909(4) 0.6968(10) 0.4061(2) 0.031(2) Uani 0.627(14) 1 d D . P B 1
C14 C 1.0169(3) 0.8095(7) 0.4158(2) 0.047(2) Uani 0.627(14) 1 d . . P B 1
H14A H 0.9830 0.8624 0.4157 0.071 Uiso 0.627(14) 1 calc R U P B 1
H14B H 1.0444 0.8094 0.4439 0.071 Uiso 0.627(14) 1 calc R U P B 1
H14C H 1.0405 0.8313 0.3943 0.071 Uiso 0.627(14) 1 calc R U P B 1
C10B C 0.9965(6) 0.4542(17) 0.3986(4) 0.045(4) Uani 0.373(14) 1 d . . P B 2
H10D H 0.9590 0.4092 0.3898 0.067 Uiso 0.373(14) 1 calc R U P B 2
H10E H 1.0238 0.4442 0.3783 0.067 Uiso 0.373(14) 1 calc R U P B 2
H10F H 1.0182 0.4308 0.4270 0.067 Uiso 0.373(14) 1 calc R U P B 2
C11B C 0.9794(6) 0.5700(19) 0.3999(4) 0.035(4) Uani 0.373(14) 1 d D . P B 2
C12B C 1.0163(7) 0.661(2) 0.4103(5) 0.038(4) Uani 0.373(14) 1 d D . P B 2
H12B H 1.0604 0.6595 0.4175 0.046 Uiso 0.373(14) 1 calc R U P B 2
C13B C 0.9799(6) 0.7542(15) 0.4087(4) 0.035(3) Uani 0.373(14) 1 d D . P B 2
C14B C 0.9964(7) 0.8760(14) 0.4190(5) 0.064(4) Uiso 0.373(14) 1 d . . P B 2
H14D H 0.9584 0.9206 0.4142 0.097 Uiso 0.373(14) 1 calc R U P B 2
H14E H 1.0178 0.8825 0.4488 0.097 Uiso 0.373(14) 1 calc R U P B 2
H14F H 1.0237 0.9028 0.4005 0.097 Uiso 0.373(14) 1 calc R U P B 2
C15 C 0.82015(13) 0.6417(2) 0.24983(9) 0.0215(6) Uani 1 1 d . . . . .
C16 C 0.82250(13) 0.4548(2) 0.28741(9) 0.0228(6) Uani 1 1 d . . . . .
C17 C 0.8387(2) 0.2269(4) 0.41176(14) 0.0594(13) Uani 1 1 d . . . . .
H17A H 0.8407 0.1460 0.4150 0.089 Uiso 1 1 calc R U . . .
H17B H 0.8758 0.2602 0.4293 0.089 Uiso 1 1 calc R U . . .
H17C H 0.8017 0.2550 0.4209 0.089 Uiso 1 1 calc R U . . .
C18 C 0.83551(17) 0.2564(3) 0.36644(12) 0.0408(9) Uani 1 1 d . . . . .
C19 C 0.83437(16) 0.1845(3) 0.33255(12) 0.0386(8) Uani 1 1 d . . . . .
H19B H 0.8362 0.1057 0.3341 0.046 Uiso 1 1 calc R U . . .
C20 C 0.83012(14) 0.2472(3) 0.29657(11) 0.0298(7) Uani 1 1 d . . . . .
C21 C 0.82775(16) 0.2129(3) 0.25187(12) 0.0369(8) Uani 1 1 d . . . . .
H21A H 0.8247 0.2790 0.2337 0.055 Uiso 1 1 calc R U . . .
H21B H 0.8655 0.1717 0.2500 0.055 Uiso 1 1 calc R U . . .
H21C H 0.7914 0.1655 0.2423 0.055 Uiso 1 1 calc R U . . .
C22 C 0.8414(3) 0.7231(5) 0.55433(14) 0.0713(15) Uani 1 1 d . . . . .
C23 C 0.8291(2) 0.7484(4) 0.50897(14) 0.0603(12) Uani 1 1 d . . . . .
C24 C 0.4957(4) 0.6444(9) 0.4442(4) 0.071(3) Uani 0.5 1 d . . P . .
C25 C 0.4774(4) 0.5919(7) 0.3994(4) 0.060(2) Uani 0.5 1 d . . P . .
C26 C 0.4987(4) 0.7340(9) 0.2734(3) 0.078(4) Uani 0.538(10) 1 d . . P D 1
C26A C 0.4995(5) 0.6977(14) 0.3480(6) 0.120(8) Uani 0.462(10) 1 d . . P D 2
C27 C 0.5507(4) 0.7559(9) 0.3086(3) 0.061(3) Uani 0.538(10) 1 d . . P D 1
C27A C 0.5583(6) 0.7576(9) 0.3393(5) 0.059(3) Uani 0.462(10) 1 d . . P D 2
C28 C 1.0436(2) 0.6529(5) 0.30473(15) 0.0598(15) Uani 0.914(7) 1 d . . P C 1
C28A C 1.0683(16) 0.530(3) 0.3103(11) 0.023(8) Uani 0.086(7) 1 d . . P C 2
C29 C 0.9947(2) 0.5675(6) 0.29793(14) 0.0720(15) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
N11B Ni1 N10 161.5(19) .
N10 Ni1 N13 78.15(15) .
N11B Ni1 N3 104.0(18) .
N10 Ni1 N3 91.11(9) .
N13 Ni1 N3 167.53(16) .
N11B Ni1 N17 79.2(19) .
N10 Ni1 N17 89.15(9) .
N13 Ni1 N17 91.53(16) .
N3 Ni1 N17 94.66(9) .
N11B Ni1 N7 100.3(19) .
N10 Ni1 N7 93.21(10) .
N13 Ni1 N7 96.55(17) .
N3 Ni1 N7 77.53(10) .
N17 Ni1 N7 171.88(10) .
N11B Ni1 N21 14.7(18) .
N10 Ni1 N21 166.41(10) .
N13 Ni1 N21 102.33(17) .
N3 Ni1 N21 89.60(12) .
N17 Ni1 N21 77.27(10) .
N7 Ni1 N21 100.19(11) .
N11B Ni1 N13B 84.9(19) .
N10 Ni1 N13B 78.9(6) .
N3 Ni1 N13B 168.9(13) .
N17 Ni1 N13B 80.4(19) .
N7 Ni1 N13B 107.7(19) .
N21 Ni1 N13B 98.9(6) .
C1 N1 H1A 120.0 .
C1 N1 H1B 120.0 .
H1A N1 H1B 120.0 .
N3 N2 C1 115.5(2) .
C2 N3 N2 119.1(2) .
C2 N3 Ni1 116.24(19) .
N2 N3 Ni1 124.61(18) .
N5 N4 C2 116.9(3) .
N4 N5 C1 117.5(3) .
N7 N6 C4 111.7(3) .
N7 N6 C2 117.0(2) .
C4 N6 C2 131.3(3) .
C6 N7 N6 104.8(3) .
C6 N7 Ni1 141.9(2) .
N6 N7 Ni1 113.26(18) .
C8 N8 H8A 120.0 .
C8 N8 H8B 120.0 .
H8A N8 H8B 120.0 .
N10 N9 C8 115.3(3) .
N9 N10 C9 120.3(3) .
N9 N10 Ni1 122.89(19) .
C9 N10 Ni1 116.5(3) .
C9 N11 N12 115.9(5) .
N11 N12 C8 118.2(6) .
C11 N13 N14 113.2(6) .
C11 N13 Ni1 133.3(6) .
N14 N13 Ni1 113.4(3) .
C9 N14 C13 144.5(7) .
C9 N14 N13 114.7(3) .
C13 N14 N13 100.7(7) .
N21 N11B Ni1 124(6) .
N21 N11B N20 48(4) .
Ni1 N11B N20 119(3) .
N21 N11B C18 38(4) .
Ni1 N11B C18 141(3) .
N20 N11B C18 76(2) .
N14B N13B C11B 81(3) .
N14B N13B Ni1 99(3) .
C11B N13B Ni1 144(5) .
N13B N14B C9 131(3) .
N13B N14B C11B 58(2) .
C9 N14B C11B 166.9(17) .
N13B N14B C13B 130(3) .
C9 N14B C13B 86.0(12) .
C11B N14B C13B 81.1(11) .
C15 N15 H15A 120.0 .
C15 N15 H15B 120.0 .
H15A N15 H15B 120.0 .
N17 N16 C15 115.7(2) .
N16 N17 C16 119.2(2) .
N16 N17 Ni1 123.87(18) .
C16 N17 Ni1 116.89(19) .
N19 N18 C16 117.2(3) .
N18 N19 C15 117.4(2) .
N21 N20 C20 111.3(3) .
N21 N20 C16 117.4(3) .
C20 N20 C16 131.3(3) .
N21 N20 N11B 20.3(18) .
C20 N20 N11B 125.5(19) .
C16 N20 N11B 102.1(19) .
N11B N21 C18 125(5) .
N11B N21 N20 112(5) .
C18 N21 N20 105.5(3) .
N11B N21 Ni1 41(5) .
C18 N21 Ni1 141.6(3) .
N20 N21 Ni1 112.8(2) .
O3 N22 O1 121.1(3) .
O3 N22 O2 121.0(3) .
O1 N22 O2 117.8(3) .
O6 N23 O4 117.8(3) .
O6 N23 O5 120.0(3) .
O4 N23 O5 122.2(3) .
N1 C1 N2 118.6(3) .
N1 C1 N5 117.5(3) .
N2 C1 N5 123.7(3) .
N3 C2 N4 124.8(3) .
N3 C2 N6 115.6(3) .
N4 C2 N6 119.2(3) .
C4 C3 H3A 109.5 .
C4 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
C4 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C5 C4 N6 105.6(3) .
C5 C4 C3 129.0(3) .
N6 C4 C3 125.4(3) .
C4 C5 C6 107.3(3) .
C4 C5 H5B 126.4 .
C6 C5 H5B 126.4 .
N7 C6 C5 110.6(3) .
N7 C6 C7 121.7(3) .
C5 C6 C7 127.7(3) .
C6 C7 H7A 109.5 .
C6 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
C6 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
N8 C8 N9 116.4(4) .
N8 C8 N12 119.5(5) .
N9 C8 N12 124.1(5) .
N8 C8 N12B 126.4(14) .
N9 C8 N12B 116.5(14) .
N11 C9 N10 125.9(4) .
N11 C9 N14 117.0(4) .
N10 C9 N14 117.0(4) .
N10 C9 N14B 99.2(8) .
C11 C10 H10A 109.5 .
C11 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
C11 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
N13 C11 C12 104.8(7) .
N13 C11 C10 127.3(8) .
C12 C11 C10 127.9(8) .
C13 C12 C11 108.5(7) .
C13 C12 H12A 125.8 .
C11 C12 H12A 125.8 .
C12 C13 N14 112.7(7) .
C12 C13 C14 131.4(8) .
N14 C13 C14 115.9(9) .
C13 C14 H14A 109.5 .
C13 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C13 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
C11B C10B H10D 109.5 .
C11B C10B H10E 109.5 .
H10D C10B H10E 109.5 .
C11B C10B H10F 109.5 .
H10D C10B H10F 109.5 .
H10E C10B H10F 109.5 .
C12B C11B N13B 124(2) .
C12B C11B C10B 129.4(14) .
N13B C11B C10B 104.8(18) .
C12B C11B N14B 89.1(14) .
N13B C11B N14B 40.9(12) .
C10B C11B N14B 141.4(15) .
C11B C12B C13B 109.5(13) .
C11B C12B H12B 125.3 .
C13B C12B H12B 125.3 .
C12B C13B C14B 131.7(13) .
C12B C13B N14B 80.3(11) .
C14B C13B N14B 147.9(13) .
C13B C14B H14D 109.5 .
C13B C14B H14E 109.5 .
H14D C14B H14E 109.5 .
C13B C14B H14F 109.5 .
H14D C14B H14F 109.5 .
H14E C14B H14F 109.5 .
N15 C15 N16 118.1(3) .
N15 C15 N19 117.7(3) .
N16 C15 N19 124.1(3) .
N17 C16 N18 125.1(3) .
N17 C16 N20 115.6(3) .
N18 C16 N20 119.2(3) .
C18 C17 H17A 109.5 .
C18 C17 H17B 109.5 .
H17A C17 H17B 109.5 .
C18 C17 H17C 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
N21 C18 C19 110.3(3) .
N21 C18 C17 122.2(4) .
C19 C18 C17 127.4(3) .
N21 C18 N11B 17.4(17) .
C19 C18 N11B 121.0(18) .
C17 C18 N11B 110.2(18) .
C20 C19 C18 107.7(3) .
C20 C19 H19B 126.2 .
C18 C19 H19B 126.2 .
C19 C20 N20 105.2(3) .
C19 C20 C21 130.2(3) .
N20 C20 C21 124.6(3) .
C20 C21 H21A 109.5 .
C20 C21 H21B 109.5 .
H21A C21 H21B 109.5 .
C20 C21 H21C 109.5 .
H21A C21 H21C 109.5 .
H21B C21 H21C 109.5 .
N24 C23 C22 179.4(6) .
N25 C24 C25 172.7(10) .
C27 C26 C26 125.8(10) 2_655
N26 C27 C26 171.3(11) .
N26 C27A C26A 173.6(16) .
N27 C29 C28 177.0(6) .
N27A C29 C28A 159(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N11B 1.67(6) .
Ni1 N10 2.050(3) .
Ni1 N13 2.056(4) .
Ni1 N3 2.057(2) .
Ni1 N17 2.059(2) .
Ni1 N7 2.075(3) .
Ni1 N21 2.101(4) .
Ni1 N13B 2.12(5) .
O1 N22 1.240(4) .
O2 N22 1.250(3) .
O3 N22 1.228(4) .
O4 N23 1.231(3) .
O5 N23 1.240(3) .
O6 N23 1.227(4) .
N1 C1 1.320(4) .
N1 H1A 0.8800 .
N1 H1B 0.8800 .
N2 N3 1.324(3) .
N2 C1 1.347(4) .
N3 C2 1.323(4) .
N4 N5 1.314(4) .
N4 C2 1.329(4) .
N5 C1 1.365(4) .
N6 N7 1.368(4) .
N6 C4 1.373(4) .
N6 C2 1.393(4) .
N7 C6 1.333(4) .
N8 C8 1.313(6) .
N8 H8A 0.8800 .
N8 H8B 0.8800 .
N9 N10 1.310(4) .
N9 C8 1.350(4) .
N10 C9 1.334(4) .
N11 C9 1.296(6) .
N11 N12 1.351(10) .
N12 C8 1.361(9) .
N13 C11 1.376(10) .
N13 N14 1.436(7) .
N14 C9 1.377(7) .
N14 C13 1.401(9) .
N11B N21 0.64(5) .
N11B N20 1.72(5) .
N11B C18 1.77(6) .
N12B C8 1.57(4) .
N13B N14B 1.07(3) .
N13B C11B 1.39(3) .
N14B C9 1.59(2) .
N14B C11B 1.61(3) .
N14B C13B 1.82(3) .
N15 C15 1.320(4) .
N15 H15A 0.8800 .
N15 H15B 0.8800 .
N16 N17 1.313(3) .
N16 C15 1.353(4) .
N17 C16 1.326(4) .
N18 N19 1.313(4) .
N18 C16 1.328(4) .
N19 C15 1.365(4) .
N20 N21 1.370(4) .
N20 C20 1.372(4) .
N20 C16 1.394(4) .
N21 C18 1.326(5) .
N24 C23 1.138(6) .
N25 C24 1.157(14) .
N26 C27A 0.948(11) .
N26 C27 1.255(11) .
N27 C29 1.165(7) .
N27A C29 1.18(3) .
C3 C4 1.485(5) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.357(5) .
C5 C6 1.396(5) .
C5 H5B 0.9500 .
C6 C7 1.485(6) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C10 C11 1.476(11) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.399(11) .
C12 C13 1.365(11) .
C12 H12A 0.9500 .
C13 C14 1.481(11) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C10B C11B 1.45(2) .
C10B H10D 0.9800 .
C10B H10E 0.9800 .
C10B H10F 0.9800 .
C11B C12B 1.36(2) .
C12B C13B 1.379(19) .
C12B H12B 0.9500 .
C13B C14B 1.53(2) .
C14B H14D 0.9800 .
C14B H14E 0.9800 .
C14B H14F 0.9800 .
C17 C18 1.484(5) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 C19 1.387(6) .
C19 C20 1.367(5) .
C19 H19B 0.9500 .
C20 C21 1.483(5) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 C23 1.458(6) .
C24 C25 1.549(17) .
C26 C27 1.460(13) .
C26 C26 1.52(2) 2_655
C26A C27A 1.556(17) .
C28 C29 1.472(7) .
C28A C29 1.65(3) .
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
C1 N2 N3 C2 -1.0(4)
C1 N2 N3 Ni1 -178.0(2)
C2 N4 N5 C1 1.5(4)
C4 N6 N7 C6 -0.5(4)
C2 N6 N7 C6 -178.3(3)
C4 N6 N7 Ni1 176.8(2)
C2 N6 N7 Ni1 -0.9(3)
C8 N9 N10 C9 0.7(4)
C8 N9 N10 Ni1 -172.8(2)
C9 N11 N12 C8 3.9(9)
C11 N13 N14 C9 173.7(6)
Ni1 N13 N14 C9 -4.4(5)
C11 N13 N14 C13 -3.3(7)
Ni1 N13 N14 C13 178.6(4)
N10 Ni1 N11B N21 -133(5)
N3 Ni1 N11B N21 11(8)
N17 Ni1 N11B N21 -81(7)
N7 Ni1 N11B N21 91(7)
N13B Ni1 N11B N21 -162(8)
N10 Ni1 N11B N20 -76(7)
N3 Ni1 N11B N20 68(3)
N17 Ni1 N11B N20 -25(3)
N7 Ni1 N11B N20 147(3)
N21 Ni1 N11B N20 56(6)
N13B Ni1 N11B N20 -106(4)
N10 Ni1 N11B C18 179.7(6)
N3 Ni1 N11B C18 -36(5)
N17 Ni1 N11B C18 -128(5)
N7 Ni1 N11B C18 43(5)
N21 Ni1 N11B C18 -47(5)
N13B Ni1 N11B C18 150(6)
C11B N13B N14B C9 169(3)
Ni1 N13B N14B C9 -48(6)
Ni1 N13B N14B C11B 143(5)
C11B N13B N14B C13B 42(6)
Ni1 N13B N14B C13B -175(2)
C15 N16 N17 C16 -0.8(4)
C15 N16 N17 Ni1 178.26(19)
C16 N18 N19 C15 1.0(4)
Ni1 N11B N20 N21 -111(7)
C18 N11B N20 N21 30(4)
N21 N11B N20 C20 -50(6)
Ni1 N11B N20 C20 -161(2)
C18 N11B N20 C20 -21(3)
N21 N11B N20 C16 141(5)
Ni1 N11B N20 C16 29(3)
C18 N11B N20 C16 170.3(10)
Ni1 N11B N21 C18 -131(4)
N20 N11B N21 C18 129(5)
Ni1 N11B N21 N20 100(6)
C18 N11B N21 N20 -129(5)
N20 N11B N21 Ni1 -100(6)
C18 N11B N21 Ni1 131(4)
C20 N20 N21 N11B 138(6)
C16 N20 N21 N11B -44(6)
C20 N20 N21 C18 -0.5(4)
C16 N20 N21 C18 177.4(3)
N11B N20 N21 C18 -138(6)
C20 N20 N21 Ni1 -177.3(2)
C16 N20 N21 Ni1 0.6(4)
N11B N20 N21 Ni1 45(6)
N3 N2 C1 N1 -171.7(3)
N3 N2 C1 N5 14.0(4)
N4 N5 C1 N1 171.2(3)
N4 N5 C1 N2 -14.4(5)
N2 N3 C2 N4 -11.9(4)
Ni1 N3 C2 N4 165.3(2)
N2 N3 C2 N6 175.4(2)
Ni1 N3 C2 N6 -7.4(3)
N5 N4 C2 N3 11.5(5)
N5 N4 C2 N6 -176.0(3)
N7 N6 C2 N3 5.5(4)
C4 N6 C2 N3 -171.7(3)
N7 N6 C2 N4 -167.7(3)
C4 N6 C2 N4 15.1(5)
N7 N6 C4 C5 0.5(4)
C2 N6 C4 C5 177.8(3)
N7 N6 C4 C3 -179.2(3)
C2 N6 C4 C3 -1.9(5)
N6 C4 C5 C6 -0.2(4)
C3 C4 C5 C6 179.5(4)
N6 N7 C6 C5 0.4(4)
Ni1 N7 C6 C5 -175.7(3)
N6 N7 C6 C7 -178.0(5)
Ni1 N7 C6 C7 5.9(8)
C4 C5 C6 N7 -0.1(5)
C4 C5 C6 C7 178.2(5)
N10 N9 C8 N8 176.8(3)
N10 N9 C8 N12 -2.2(6)
N10 N9 C8 N12B -12.7(15)
N11 N12 C8 N8 -179.1(5)
N11 N12 C8 N9 -0.2(9)
N12 N11 C9 N10 -5.8(7)
N12 N11 C9 N14 174.6(5)
N9 N10 C9 N11 3.5(5)
Ni1 N10 C9 N11 177.4(3)
N9 N10 C9 N14 -176.9(3)
Ni1 N10 C9 N14 -3.0(4)
N9 N10 C9 N14B -176.9(9)
Ni1 N10 C9 N14B -3.0(9)
C13 N14 C9 N11 -0.5(10)
N13 N14 C9 N11 -175.5(4)
C13 N14 C9 N10 179.8(7)
N13 N14 C9 N10 4.8(5)
N13B N14B C9 N10 41(6)
C11B N14B C9 N10 173(7)
C13B N14B C9 N10 -177.4(7)
N14 N13 C11 C12 2.8(9)
Ni1 N13 C11 C12 -179.6(5)
N14 N13 C11 C10 -178.4(7)
Ni1 N13 C11 C10 -0.8(13)
N13 C11 C12 C13 -1.1(9)
C10 C11 C12 C13 -179.9(8)
C11 C12 C13 N14 -1.0(9)
C11 C12 C13 C14 -177.6(8)
C9 N14 C13 C12 -172.8(6)
N13 N14 C13 C12 2.5(7)
C9 N14 C13 C14 4.4(11)
N13 N14 C13 C14 179.7(5)
N14B N13B C11B C12B -37(6)
Ni1 N13B C11B C12B -130(2)
N14B N13B C11B C10B 158(3)
Ni1 N13B C11B C10B 66(4)
Ni1 N13B C11B N14B -92(6)
N13B N14B C11B C12B 150(5)
C9 N14B C11B C12B 11(8)
C13B N14B C11B C12B 0.7(10)
C9 N14B C11B N13B -139(9)
C13B N14B C11B N13B -149(5)
N13B N14B C11B C10B -35(6)
C9 N14B C11B C10B -174(6)
C13B N14B C11B C10B 176.5(16)
N13B C11B C12B C13B 22(4)
C10B C11B C12B C13B -177.6(12)
N14B C11B C12B C13B -1.0(14)
C11B C12B C13B C14B 177.3(12)
C11B C12B C13B N14B 0.9(13)
N13B N14B C13B C12B -36(5)
C9 N14B C13B C12B -178.5(12)
C11B N14B C13B C12B -0.7(10)
N13B N14B C13B C14B 149(5)
C9 N14B C13B C14B 7(3)
C11B N14B C13B C14B -175.6(19)
N17 N16 C15 N15 -174.2(3)
N17 N16 C15 N19 9.8(4)
N18 N19 C15 N15 174.0(3)
N18 N19 C15 N16 -10.0(4)
N16 N17 C16 N18 -8.2(4)
Ni1 N17 C16 N18 172.7(2)
N16 N17 C16 N20 175.5(2)
Ni1 N17 C16 N20 -3.6(3)
N19 N18 C16 N17 8.0(5)
N19 N18 C16 N20 -175.8(3)
N21 N20 C16 N17 2.0(4)
C20 N20 C16 N17 179.4(3)
N11B N20 C16 N17 -12.4(19)
N21 N20 C16 N18 -174.6(3)
C20 N20 C16 N18 2.8(5)
N11B N20 C16 N18 171.1(19)
N11B N21 C18 C19 -131(6)
N20 N21 C18 C19 0.5(4)
Ni1 N21 C18 C19 175.8(3)
N11B N21 C18 C17 50(6)
N20 N21 C18 C17 -178.7(3)
Ni1 N21 C18 C17 -3.4(7)
N20 N21 C18 N11B 132(6)
Ni1 N21 C18 N11B -53(6)
Ni1 N11B C18 N21 82(7)
N20 N11B C18 N21 -36(5)
N21 N11B C18 C19 56(7)
Ni1 N11B C18 C19 138(4)
N20 N11B C18 C19 19(2)
N21 N11B C18 C17 -137(5)
Ni1 N11B C18 C17 -54(6)
N20 N11B C18 C17 -172.9(9)
N21 C18 C19 C20 -0.3(4)
C17 C18 C19 C20 178.9(4)
N11B C18 C19 C20 -16(2)
C18 C19 C20 N20 0.0(4)
C18 C19 C20 C21 179.5(3)
N21 N20 C20 C19 0.3(4)
C16 N20 C20 C19 -177.2(3)
N11B N20 C20 C19 17(2)
N21 N20 C20 C21 -179.2(3)
C16 N20 C20 C21 3.2(5)
N11B N20 C20 C21 -163(2)
