#------------------------------------------------------------------------------
#$Date: 2020-03-27 01:47:23 +0200 (Fri, 27 Mar 2020) $
#$Revision: 249739 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/45/4134549.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_4134549
loop_
_publ_author_name
'Stevens, Hendrik'
'Duan, Peng-Cheng'
'Dechert, Sebastian'
'Meyer, Franc'
_publ_section_title
;
 Competing H2 versus Intramolecular C-H Activation at a Dinuclear Nickel
 Complex via Metal-Metal Cooperative Oxidative Addition.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00758
_journal_year                    2020
_chemical_formula_moiety         'C51 H43 N6 Ni2 -, 0.5(C12 H24 Na O3 +)'
_chemical_formula_sum            'C57 H55 N6 Na0.5 Ni2 O1.5'
_chemical_formula_weight         976.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 108.0510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7413(5)
_cell_length_b                   10.6411(2)
_cell_length_c                   20.9606(4)
_cell_measurement_reflns_used    71859
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.786
_cell_measurement_theta_min      1.544
_cell_volume                     5882.98(19)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2015)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71859
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.786
_diffrn_reflns_theta_min         1.544
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.9215
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       block
_exptl_crystal_F_000             2050
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         11100
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0336
_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)+(0.0423P)²+2.1589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8846
_reflns_number_total             11100
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00758_si_002.cif
_cod_data_source_block           6Na-hs281b_sq
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C57 H55 N6 Na0.50 Ni2 O1.50'
_cod_database_code               4134549
_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_min   0.726
_shelx_estimated_absorpt_t_max   0.853
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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 0.16289(2) 0.50036(2) 0.48122(2) 0.03185(7) Uani 1 1 d . . . . .
Ni2 Ni 0.29670(2) 0.65018(2) 0.46055(2) 0.04245(8) Uani 1 1 d . . . . .
N1 N 0.20892(6) 0.63295(15) 0.51935(7) 0.0385(4) Uani 1 1 d . . . . .
N2 N 0.25079(7) 0.68742(16) 0.50872(8) 0.0426(4) Uani 1 1 d . . . . .
N3 N 0.13216(6) 0.54726(14) 0.54820(7) 0.0347(3) Uani 1 1 d . . . . .
N4 N 0.12718(6) 0.34949(13) 0.46120(7) 0.0299(3) Uani 1 1 d . . . . .
N5 N 0.32880(7) 0.80541(17) 0.49913(9) 0.0504(5) Uani 1 1 d . . . . .
N6 N 0.33289(6) 0.64319(16) 0.39915(8) 0.0428(4) Uani 1 1 d . . . . .
C1 C 0.22932(8) 0.80401(19) 0.58493(10) 0.0462(5) Uani 1 1 d . . . . .
H1 H 0.229123 0.867907 0.616496 0.055 Uiso 1 1 calc R U . . .
C2 C 0.19659(8) 0.70292(18) 0.56564(9) 0.0406(5) Uani 1 1 d . . . . .
C3 C 0.26198(8) 0.79081(19) 0.54815(10) 0.0455(5) Uani 1 1 d . . . . .
C4 C 0.15358(8) 0.65919(18) 0.58719(10) 0.0438(5) Uani 1 1 d . . . . .
H4A H 0.165324 0.638834 0.635665 0.053 Uiso 1 1 calc R U . . .
H4B H 0.127513 0.725870 0.579491 0.053 Uiso 1 1 calc R U . . .
C5 C 0.08921(7) 0.50288(17) 0.55317(8) 0.0344(4) Uani 1 1 d . . . . .
C6 C 0.06479(7) 0.39915(18) 0.51511(9) 0.0346(4) Uani 1 1 d . . . . .
H6 H 0.032220 0.377983 0.517855 0.042 Uiso 1 1 calc R U . . .
C7 C 0.08368(7) 0.32474(16) 0.47395(9) 0.0315(4) Uani 1 1 d . . . . .
C8 C 0.06328(8) 0.5647(2) 0.59853(10) 0.0466(5) Uani 1 1 d . . . . .
H8A H 0.031755 0.519858 0.595294 0.070 Uiso 1 1 calc R U . . .
H8B H 0.055525 0.652338 0.584766 0.070 Uiso 1 1 calc R U . . .
H8C H 0.085716 0.562095 0.644971 0.070 Uiso 1 1 calc R U . . .
C9 C 0.05073(7) 0.21477(19) 0.44030(10) 0.0404(4) Uani 1 1 d . . . . .
H9A H 0.015664 0.243321 0.420546 0.061 Uiso 1 1 calc R U . . .
H9B H 0.051997 0.149299 0.473663 0.061 Uiso 1 1 calc R U . . .
H9C H 0.063250 0.180667 0.404962 0.061 Uiso 1 1 calc R U . . .
C10 C 0.15021(7) 0.25173(17) 0.43499(9) 0.0315(4) Uani 1 1 d . . . . .
C11 C 0.16454(7) 0.27307(17) 0.37708(9) 0.0329(4) Uani 1 1 d . . . . .
C12 C 0.18108(7) 0.17024(18) 0.34789(9) 0.0382(4) Uani 1 1 d . . . . .
H12 H 0.189796 0.182214 0.307910 0.046 Uiso 1 1 calc R U . . .
C13 C 0.18506(8) 0.05137(19) 0.37594(10) 0.0419(5) Uani 1 1 d . . . . .
H13 H 0.194402 -0.018074 0.353835 0.050 Uiso 1 1 calc R U . . .
C14 C 0.17542(8) 0.03409(18) 0.43598(10) 0.0389(4) Uani 1 1 d . . . . .
H14 H 0.179876 -0.046710 0.456252 0.047 Uiso 1 1 calc R U . . .
C15 C 0.15919(7) 0.13390(17) 0.46737(9) 0.0333(4) Uani 1 1 d . . . . .
C16 C 0.16281(7) 0.40185(18) 0.35000(9) 0.0325(4) Uani 1 1 d . . . . .
C17 C 0.15742(7) 0.42148(18) 0.28196(9) 0.0355(4) Uani 1 1 d . . . . .
H17 H 0.153091 0.351089 0.252847 0.043 Uiso 1 1 calc R U . A .
C18 C 0.15828(7) 0.54128(19) 0.25618(9) 0.0396(4) Uani 1 1 d . . . . .
H18 H 0.154882 0.552822 0.210045 0.047 Uiso 1 1 calc R U . A .
C19 C 0.16414(7) 0.64352(19) 0.29851(9) 0.0394(4) Uani 1 1 d . . . . .
H19 H 0.164688 0.726045 0.281458 0.047 Uiso 1 1 calc R U . A .
C20 C 0.16921(7) 0.62604(18) 0.36579(9) 0.0371(4) Uani 1 1 d . . . . .
H20 H 0.173175 0.697670 0.394010 0.045 Uiso 1 1 calc R U . A .
C21 C 0.16872(7) 0.50553(17) 0.39400(9) 0.0329(4) Uani 1 1 d . . . . .
C22 C 0.15477(7) 0.11448(17) 0.53587(9) 0.0344(4) Uani 1 1 d . . . . .
C23 C 0.12971(9) 0.01125(18) 0.55104(11) 0.0479(5) Uani 1 1 d . . . . .
H23 H 0.113280 -0.046480 0.516594 0.057 Uiso 1 1 calc R U . . .
C24 C 0.12838(11) -0.0087(2) 0.61607(12) 0.0581(6) Uani 1 1 d . . . . .
H24 H 0.110480 -0.078765 0.625446 0.070 Uiso 1 1 calc R U . . .
C25 C 0.15282(9) 0.0725(2) 0.66688(11) 0.0507(6) Uani 1 1 d . . . . .
H25 H 0.152240 0.058105 0.711364 0.061 Uiso 1 1 calc R U . . .
C26 C 0.17811(8) 0.1748(2) 0.65268(10) 0.0443(5) Uani 1 1 d . . . . .
H26 H 0.195364 0.230709 0.687604 0.053 Uiso 1 1 calc R U . . .
C27 C 0.17850(7) 0.19639(19) 0.58788(9) 0.0383(4) Uani 1 1 d . . . . .
H27 H 0.195318 0.268644 0.578626 0.046 Uiso 1 1 calc R U . . .
C28 C 0.30564(9) 0.8680(2) 0.54460(12) 0.0576(6) Uani 1 1 d . . . . .
H28A H 0.293990 0.953119 0.527684 0.069 Uiso 1 1 calc R U . . .
H28B H 0.330706 0.876237 0.589786 0.069 Uiso 1 1 calc R U . . .
C29 C 0.37341(9) 0.8449(2) 0.49760(11) 0.0551(6) Uani 1 1 d . . . . .
C30 C 0.39769(9) 0.7903(2) 0.45526(11) 0.0562(6) Uani 1 1 d . . . . .
H30 H 0.431384 0.817020 0.460566 0.067 Uiso 1 1 calc R U . . .
C31 C 0.37733(8) 0.7008(2) 0.40616(10) 0.0486(5) Uani 1 1 d . . . . .
C32 C 0.40100(10) 0.9501(2) 0.54332(14) 0.0702(7) Uani 1 1 d . . . . .
H32A H 0.433009 0.967999 0.534505 0.105 Uiso 1 1 calc R U . . .
H32B H 0.408010 0.924587 0.590237 0.105 Uiso 1 1 calc R U . . .
H32C H 0.379794 1.025744 0.534719 0.105 Uiso 1 1 calc R U . . .
C33 C 0.40870(9) 0.6662(3) 0.36125(12) 0.0608(6) Uani 1 1 d . . . . .
H33A H 0.444760 0.668329 0.387250 0.091 Uiso 1 1 calc R U . . .
H33B H 0.402117 0.726406 0.324150 0.091 Uiso 1 1 calc R U . . .
H33C H 0.399555 0.581476 0.343231 0.091 Uiso 1 1 calc R U . . .
C34 C 0.30937(7) 0.57739(19) 0.33822(10) 0.0415(5) Uani 1 1 d . . . . .
C35 C 0.29514(7) 0.4516(2) 0.34253(12) 0.0494(5) Uani 1 1 d . . . . .
C36 C 0.27709(9) 0.3838(2) 0.28288(15) 0.0609(7) Uani 1 1 d . . . . .
H36 H 0.268392 0.297803 0.284810 0.073 Uiso 1 1 calc R U . . .
C37 C 0.27153(9) 0.4374(3) 0.22161(15) 0.0644(7) Uani 1 1 d . . . . .
H37 H 0.260949 0.387810 0.182034 0.077 Uiso 1 1 calc R U . . .
C38 C 0.28138(8) 0.5645(2) 0.21752(12) 0.0552(6) Uani 1 1 d . . . . .
H38 H 0.275690 0.602682 0.174851 0.066 Uiso 1 1 calc R U . . .
C39 C 0.29968(8) 0.6370(2) 0.27592(10) 0.0441(5) Uani 1 1 d . . . . .
C40 C 0.29710(8) 0.3962(2) 0.40729(13) 0.0516(6) Uani 1 1 d . . . . .
C41 C 0.28929(8) 0.4726(2) 0.45785(12) 0.0493(5) Uani 1 1 d . . . . .
C42 C 0.28636(8) 0.4108(2) 0.51577(13) 0.0599(7) Uani 1 1 d . . . . .
H42 H 0.280540 0.458834 0.550873 0.072 Uiso 1 1 calc R U . . .
C43 C 0.29179(9) 0.2805(3) 0.52313(17) 0.0756(9) Uani 1 1 d . . . . .
H43 H 0.288839 0.241167 0.562437 0.091 Uiso 1 1 calc R U . . .
C44 C 0.30134(10) 0.2092(3) 0.4739(2) 0.0838(10) Uani 1 1 d . . . . .
H44 H 0.305758 0.120903 0.479403 0.101 Uiso 1 1 calc R U . . .
C45 C 0.30445(9) 0.2658(2) 0.41702(17) 0.0693(8) Uani 1 1 d . . . . .
H45 H 0.311705 0.216502 0.383345 0.083 Uiso 1 1 calc R U . . .
C46 C 0.30516(8) 0.7746(2) 0.26843(9) 0.0437(5) Uani 1 1 d . . . . .
C47 C 0.32503(10) 0.8222(2) 0.22007(11) 0.0595(6) Uani 1 1 d . . . . .
H47 H 0.337997 0.765892 0.194231 0.071 Uiso 1 1 calc R U . . .
C48 C 0.32625(12) 0.9492(3) 0.20902(13) 0.0752(8) Uani 1 1 d . . . . .
H48 H 0.339598 0.979414 0.175288 0.090 Uiso 1 1 calc R U . . .
C49 C 0.30841(12) 1.0330(3) 0.24613(15) 0.0739(8) Uani 1 1 d . . . . .
H49 H 0.309551 1.120796 0.238481 0.089 Uiso 1 1 calc R U . . .
C50 C 0.28876(10) 0.9880(2) 0.29474(12) 0.0573(6) Uani 1 1 d . . . . .
H50 H 0.276184 1.045153 0.320620 0.069 Uiso 1 1 calc R U . . .
C51 C 0.28735(8) 0.8605(2) 0.30585(10) 0.0450(5) Uani 1 1 d . . . . .
H51 H 0.273969 0.830829 0.339648 0.054 Uiso 1 1 calc R U . . .
Na1 Na 0.06264(6) 0.53982(16) 0.28436(9) 0.0490(4) Uani 0.5 1 d . . P A -1
O1 O 0.0213(5) 0.3485(9) 0.2592(6) 0.055(3) Uani 0.5 1 d D U P A -1
C61 C 0.0413(7) 0.2321(13) 0.2442(15) 0.048(2) Uani 0.5 1 d D U P A -1
H61A H 0.074628 0.214430 0.277716 0.058 Uiso 0.5 1 calc R U P A -1
H61B H 0.045679 0.235361 0.199146 0.058 Uiso 0.5 1 calc R U P A -1
C62 C 0.0034(11) 0.1320(4) 0.247(2) 0.053(3) Uani 0.5 1 d D U P A -1
H62A H 0.017371 0.075844 0.285674 0.063 Uiso 0.5 1 calc R U P A -1
H62B H -0.006017 0.080877 0.205164 0.063 Uiso 0.5 1 calc R U P A -1
C63 C -0.0423(7) 0.2036(14) 0.2531(16) 0.058(4) Uani 0.5 1 d D U P A -1
H63A H -0.074079 0.171208 0.221098 0.070 Uiso 0.5 1 calc R U P A -1
H63B H -0.044504 0.197134 0.299207 0.070 Uiso 0.5 1 calc R U P A -1
C64 C -0.0327(7) 0.3370(13) 0.2367(8) 0.051(3) Uani 0.5 1 d D U P A -1
H64A H -0.046522 0.352688 0.187863 0.061 Uiso 0.5 1 calc R U P A -1
H64B H -0.048345 0.396889 0.260600 0.061 Uiso 0.5 1 calc R U P A -1
O2 O 0.0275(2) 0.6706(5) 0.3447(3) 0.0636(15) Uani 0.5 1 d D U P A -1
C65 C 0.0566(3) 0.7504(10) 0.3936(5) 0.104(4) Uani 0.5 1 d D U P A -1
H65A H 0.082047 0.791856 0.376367 0.124 Uiso 0.5 1 calc R U P A -1
H65B H 0.075163 0.700007 0.433270 0.124 Uiso 0.5 1 calc R U P A -1
C66 C 0.0282(3) 0.8438(8) 0.4137(4) 0.079(2) Uani 0.5 1 d D U P A -1
H66A H 0.042008 0.928513 0.410464 0.095 Uiso 0.5 1 calc R U P A -1
H66B H 0.028397 0.829549 0.460491 0.095 Uiso 0.5 1 calc R U P A -1
C67 C -0.0240(3) 0.8302(8) 0.3658(4) 0.0737(18) Uani 0.5 1 d D U P A -1
H67A H -0.047449 0.796828 0.388993 0.088 Uiso 0.5 1 calc R U P A -1
H67B H -0.036999 0.912186 0.345364 0.088 Uiso 0.5 1 calc R U P A -1
C68 C -0.0191(3) 0.7408(11) 0.3141(4) 0.084(3) Uani 0.5 1 d D U P A -1
H68A H -0.048564 0.683352 0.300657 0.101 Uiso 0.5 1 calc R U P A -1
H68B H -0.017074 0.786593 0.273909 0.101 Uiso 0.5 1 calc R U P A -1
O3 O 0.01412(14) 0.6444(3) 0.18478(18) 0.0537(8) Uani 0.5 1 d D U P A -1
C69 C 0.0332(3) 0.7535(7) 0.1637(4) 0.0574(15) Uani 0.5 1 d D U P A -1
H69A H 0.058144 0.731306 0.140461 0.069 Uiso 0.5 1 calc R U P A -1
H69B H 0.050284 0.807114 0.202818 0.069 Uiso 0.5 1 calc R U P A -1
C70 C -0.0112(4) 0.8224(7) 0.1165(5) 0.091(3) Uani 0.5 1 d D U P A -1
H70A H -0.025921 0.883795 0.140814 0.109 Uiso 0.5 1 calc R U P A -1
H70B H -0.001472 0.866417 0.080756 0.109 Uiso 0.5 1 calc R U P A -1
C71 C -0.0467(3) 0.7180(7) 0.0891(3) 0.0460(15) Uani 0.5 1 d D U P A -1
H71A H -0.082202 0.748187 0.075594 0.055 Uiso 0.5 1 calc R U P A -1
H71B H -0.039945 0.680911 0.049358 0.055 Uiso 0.5 1 calc R U P A -1
C72 C -0.0379(3) 0.6245(7) 0.1434(5) 0.0578(18) Uani 0.5 1 d D U P A -1
H72A H -0.061557 0.637883 0.169736 0.069 Uiso 0.5 1 calc R U P A -1
H72B H -0.042560 0.538149 0.124930 0.069 Uiso 0.5 1 calc R U P A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
_geom_angle_publ_flag
N4 Ni1 C21 90.35(7) . . ?
N4 Ni1 N1 166.55(6) . . ?
C21 Ni1 N1 97.90(7) . . ?
N4 Ni1 N3 93.62(6) . . ?
C21 Ni1 N3 153.14(7) . . ?
N1 Ni1 N3 83.83(7) . . ?
N6 Ni2 N2 166.14(7) . . ?
N6 Ni2 C41 90.92(9) . . ?
N2 Ni2 C41 98.02(9) . . ?
N6 Ni2 N5 92.65(8) . . ?
N2 Ni2 N5 84.08(8) . . ?
C41 Ni2 N5 153.50(8) . . ?
C2 N1 N2 107.39(16) . . ?
C2 N1 Ni1 115.10(14) . . ?
N2 N1 Ni1 137.20(13) . . ?
C3 N2 N1 106.80(17) . . ?
C3 N2 Ni2 115.49(15) . . ?
N1 N2 Ni2 137.54(13) . . ?
C5 N3 C4 117.98(16) . . ?
C5 N3 Ni1 125.64(13) . . ?
C4 N3 Ni1 115.14(13) . . ?
C7 N4 C10 118.34(15) . . ?
C7 N4 Ni1 124.93(12) . . ?
C10 N4 Ni1 116.56(11) . . ?
C29 N5 C28 118.44(19) . . ?
C29 N5 Ni2 125.27(18) . . ?
C28 N5 Ni2 115.03(14) . . ?
C31 N6 C34 118.17(18) . . ?
C31 N6 Ni2 125.38(15) . . ?
C34 N6 Ni2 116.33(13) . . ?
C3 C1 C2 104.18(18) . . ?
N1 C2 C1 110.44(19) . . ?
N1 C2 C4 117.10(17) . . ?
C1 C2 C4 132.44(19) . . ?
N2 C3 C1 111.19(19) . . ?
N2 C3 C28 117.1(2) . . ?
C1 C3 C28 131.7(2) . . ?
N3 C4 C2 108.22(16) . . ?
N3 C5 C6 121.71(17) . . ?
N3 C5 C8 120.90(17) . . ?
C6 C5 C8 117.36(18) . . ?
C7 C6 C5 126.30(18) . . ?
N4 C7 C6 123.26(17) . . ?
N4 C7 C9 120.58(16) . . ?
C6 C7 C9 116.09(17) . . ?
C11 C10 C15 120.22(16) . . ?
C11 C10 N4 119.83(16) . . ?
C15 C10 N4 119.95(16) . . ?
C12 C11 C10 118.01(17) . . ?
C12 C11 C16 122.23(16) . . ?
C10 C11 C16 119.75(16) . . ?
C13 C12 C11 121.51(18) . . ?
C14 C13 C12 119.83(18) . . ?
C13 C14 C15 120.76(18) . . ?
C14 C15 C10 118.96(17) . . ?
C14 C15 C22 118.87(16) . . ?
C10 C15 C22 122.07(16) . . ?
C17 C16 C21 120.06(17) . . ?
C17 C16 C11 120.59(16) . . ?
C21 C16 C11 119.30(16) . . ?
C17 C16 Na1 71.11(11) . . ?
C21 C16 Na1 79.92(11) . . ?
C11 C16 Na1 122.23(12) . . ?
C18 C17 C16 121.57(18) . . ?
C18 C17 Na1 74.67(12) . . ?
C16 C17 Na1 81.95(11) . . ?
C19 C18 C17 119.09(17) . . ?
C19 C18 Na1 78.80(12) . . ?
C17 C18 Na1 77.76(12) . . ?
C18 C19 C20 120.18(18) . . ?
C18 C19 Na1 73.88(12) . . ?
C20 C19 Na1 81.09(12) . . ?
C19 C20 C21 122.42(18) . . ?
C19 C20 Na1 72.34(12) . . ?
C21 C20 Na1 80.12(11) . . ?
C20 C21 C16 116.68(16) . . ?
C20 C21 Ni1 116.54(14) . . ?
C16 C21 Ni1 125.59(14) . . ?
C23 C22 C27 117.71(18) . . ?
C23 C22 C15 121.72(17) . . ?
C27 C22 C15 120.46(17) . . ?
C22 C23 C24 120.8(2) . . ?
C25 C24 C23 120.4(2) . . ?
C24 C25 C26 119.4(2) . . ?
C25 C26 C27 120.3(2) . . ?
C26 C27 C22 121.34(19) . . ?
N5 C28 C3 108.09(18) . . ?
N5 C29 C30 121.7(2) . . ?
N5 C29 C32 120.9(2) . . ?
C30 C29 C32 117.4(2) . . ?
C31 C30 C29 126.3(2) . . ?
N6 C31 C30 122.9(2) . . ?
N6 C31 C33 120.4(2) . . ?
C30 C31 C33 116.6(2) . . ?
C39 C34 C35 120.93(19) . . ?
C39 C34 N6 121.04(18) . . ?
C35 C34 N6 118.02(19) . . ?
C36 C35 C34 117.7(2) . . ?
C36 C35 C40 121.5(2) . . ?
C34 C35 C40 120.8(2) . . ?
C37 C36 C35 122.0(2) . . ?
C36 C37 C38 119.8(2) . . ?
C37 C38 C39 120.5(2) . . ?
C34 C39 C38 118.6(2) . . ?
C34 C39 C46 123.24(18) . . ?
C38 C39 C46 118.1(2) . . ?
C41 C40 C45 120.7(2) . . ?
C41 C40 C35 119.71(19) . . ?
C45 C40 C35 119.5(2) . . ?
C40 C41 C42 116.4(2) . . ?
C40 C41 Ni2 123.90(17) . . ?
C42 C41 Ni2 118.32(19) . . ?
C43 C42 C41 121.8(3) . . ?
C44 C43 C42 120.3(3) . . ?
C45 C44 C43 119.6(3) . . ?
C44 C45 C40 121.1(3) . . ?
C47 C46 C51 117.5(2) . . ?
C47 C46 C39 120.9(2) . . ?
C51 C46 C39 121.50(19) . . ?
C48 C47 C46 121.2(2) . . ?
C49 C48 C47 120.8(2) . . ?
C48 C49 C50 119.1(2) . . ?
C51 C50 C49 120.2(2) . . ?
C50 C51 C46 121.2(2) . . ?
O2 Na1 O1 113.2(4) . . ?
O2 Na1 O3 88.76(17) . . ?
O1 Na1 O3 96.1(3) . . ?
O2 Na1 C18 133.13(19) . . ?
O1 Na1 C18 112.3(3) . . ?
O3 Na1 C18 97.11(12) . . ?
O2 Na1 C17 143.91(17) . . ?
O1 Na1 C17 90.1(3) . . ?
O3 Na1 C17 116.91(12) . . ?
C18 Na1 C17 27.57(6) . . ?
O2 Na1 C19 105.84(18) . . ?
O1 Na1 C19 137.8(3) . . ?
O3 Na1 C19 100.14(12) . . ?
C18 Na1 C19 27.32(6) . . ?
C17 Na1 C19 47.88(6) . . ?
O2 Na1 C20 90.73(17) . . ?
O1 Na1 C20 135.7(3) . . ?
O3 Na1 C20 122.34(12) . . ?
C18 Na1 C20 47.42(6) . . ?
C17 Na1 C20 54.65(6) . . ?
C19 Na1 C20 26.57(5) . . ?
O2 Na1 C16 121.64(15) . . ?
O1 Na1 C16 89.8(3) . . ?
O3 Na1 C16 143.61(12) . . ?
C18 Na1 C16 48.15(6) . . ?
C17 Na1 C16 26.94(5) . . ?
C19 Na1 C16 55.28(6) . . ?
C20 Na1 C16 46.28(6) . . ?
C64 O1 C61 107.0(10) . . ?
C64 O1 Na1 123.0(11) . . ?
C61 O1 Na1 127.8(9) . . ?
O1 C61 C62 106.3(9) . . ?
C61 C62 C63 105.0(4) . . ?
C64 C63 C62 104.0(10) . . ?
O1 C64 C63 104.3(11) . . ?
C65 O2 C68 104.2(6) . . ?
C65 O2 Na1 122.1(5) . . ?
C68 O2 Na1 122.7(5) . . ?
O2 C65 C66 113.8(7) . . ?
C65 C66 C67 104.2(6) . . ?
C68 C67 C66 105.3(6) . . ?
O2 C68 C67 106.2(6) . . ?
C69 O3 C72 109.6(5) . . ?
C69 O3 Na1 119.8(4) . . ?
C72 O3 Na1 130.1(4) . . ?
O3 C69 C70 107.2(6) . . ?
C71 C70 C69 101.6(6) . . ?
C72 C71 C70 106.0(6) . . ?
O3 C72 C71 105.0(6) . . ?
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
Ni1 N4 1.8646(15) . ?
Ni1 C21 1.8854(18) . ?
Ni1 N1 1.9046(16) . ?
Ni1 N3 1.9205(16) . ?
Ni2 N6 1.8630(18) . ?
Ni2 N2 1.8963(18) . ?
Ni2 C41 1.900(2) . ?
Ni2 N5 1.9310(18) . ?
N1 C2 1.349(3) . ?
N1 N2 1.376(2) . ?
N2 C3 1.353(3) . ?
N3 C5 1.316(2) . ?
N3 C4 1.462(2) . ?
N4 C7 1.341(2) . ?
N4 C10 1.418(2) . ?
N5 C29 1.317(3) . ?
N5 C28 1.464(3) . ?
N6 C31 1.343(3) . ?
N6 C34 1.425(3) . ?
C1 C3 1.366(3) . ?
C1 C2 1.385(3) . ?
C2 C4 1.476(3) . ?
C3 C28 1.484(3) . ?
C5 C6 1.407(3) . ?
C5 C8 1.509(3) . ?
C6 C7 1.388(3) . ?
C7 C9 1.517(3) . ?
C10 C11 1.408(2) . ?
C10 C15 1.411(3) . ?
C11 C12 1.399(3) . ?
C11 C16 1.478(3) . ?
C12 C13 1.385(3) . ?
C13 C14 1.377(3) . ?
C14 C15 1.395(3) . ?
C15 C22 1.493(2) . ?
C16 C17 1.403(2) . ?
C16 C21 1.415(3) . ?
C16 Na1 3.066(2) . ?
C17 C18 1.388(3) . ?
C17 Na1 2.930(2) . ?
C18 C19 1.381(3) . ?
C18 Na1 2.891(3) . ?
C19 C20 1.386(3) . ?
C19 Na1 2.952(3) . ?
C20 C21 1.414(3) . ?
C20 Na1 3.061(2) . ?
C22 C23 1.389(3) . ?
C22 C27 1.392(3) . ?
C23 C24 1.391(3) . ?
C24 C25 1.376(3) . ?
C25 C26 1.376(3) . ?
C26 C27 1.381(3) . ?
C29 C30 1.396(4) . ?
C29 C32 1.518(3) . ?
C30 C31 1.388(3) . ?
C31 C33 1.512(3) . ?
C34 C39 1.401(3) . ?
C34 C35 1.407(3) . ?
C35 C36 1.395(3) . ?
C35 C40 1.465(3) . ?
C36 C37 1.370(4) . ?
C37 C38 1.387(4) . ?
C38 C39 1.402(3) . ?
C39 C46 1.486(3) . ?
C40 C41 1.405(3) . ?
C40 C45 1.407(3) . ?
C41 C42 1.405(3) . ?
C42 C43 1.398(4) . ?
C43 C44 1.371(5) . ?
C44 C45 1.362(4) . ?
C46 C47 1.391(3) . ?
C46 C51 1.391(3) . ?
C47 C48 1.373(4) . ?
C48 C49 1.373(4) . ?
C49 C50 1.381(3) . ?
C50 C51 1.380(3) . ?
Na1 O2 2.291(6) . ?
Na1 O1 2.316(9) . ?
Na1 O3 2.380(4) . ?
O1 C64 1.430(9) . ?
O1 C61 1.431(11) . ?
C61 C62 1.510(13) . ?
C62 C63 1.519(15) . ?
C63 C64 1.503(13) . ?
O2 C65 1.382(9) . ?
O2 C68 1.458(8) . ?
C65 C66 1.411(11) . ?
C66 C67 1.493(10) . ?
C67 C68 1.479(9) . ?
O3 C69 1.404(8) . ?
O3 C72 1.451(8) . ?
C69 C70 1.511(10) . ?
C70 C71 1.477(12) . ?
C71 C72 1.475(10) . ?
