# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sm-3mp
_database_code_depnum_ccdc_archive 'CCDC 1975592'
loop_
_audit_author_name
_audit_author_address
'marappan velusamy'
;North Eastern Hill University
India
;
_audit_update_record             
;
2021-02-26 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C134 H139 B4 N13 Ni2'
_chemical_formula_weight         2092.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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'

_cell_length_a                   24.8742(10)
_cell_length_b                   17.6602(8)
_cell_length_c                   26.6397(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.624(4)
_cell_angle_gamma                90
_cell_volume                     11624.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7894
_cell_measurement_theta_min      3.3880
_cell_measurement_theta_max      25.9580

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_F_000             4440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.380
_shelx_estimated_absorpt_T_min   0.945
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.67925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_absorpt_special_details   'Sheldrick,G.M.,2015,University of gottingen'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47841
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.264
_diffrn_reflns_theta_max         30.463
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.750
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.750
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             26525
_reflns_number_gt                12160
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1049P)²+11.0078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00086(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         26525
_refine_ls_number_parameters     1387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1909
_refine_ls_R_factor_gt           0.0942
_refine_ls_wR_factor_ref         0.2901
_refine_ls_wR_factor_gt          0.2271
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
N5 N 0.1872(2) 0.7040(3) 0.8318(2) 0.0835(17) Uani 1 1 d . . . . .
N2 N 0.07042(17) 0.7177(3) 0.93175(18) 0.0593(12) Uani 1 1 d . . . . .
N9 N 0.2853(2) 0.2674(3) 0.7100(3) 0.0937(19) Uani 1 1 d . . . . .
N4 N 0.08609(18) 0.6525(3) 0.8200(2) 0.0680(13) Uani 1 1 d . . . . .
N6 N 0.18543(19) 0.7819(3) 0.9287(2) 0.0690(13) Uani 1 1 d . . . . .
N10 N 0.3920(2) 0.3366(3) 0.7058(2) 0.0713(14) Uani 1 1 d . . . . .
N12 N 0.2997(2) 0.1908(3) 0.60057(19) 0.0680(13) Uani 1 1 d . . . . .
N3 N 0.14059(19) 0.6160(3) 0.9312(2) 0.0710(14) Uani 1 1 d . . . . .
N8 N 0.3619(2) 0.1751(3) 0.71727(19) 0.0736(14) Uani 1 1 d . . . . .
N1 N 0.09854(19) 0.8148(3) 0.85466(19) 0.0659(13) Uani 1 1 d . . . . .
N11 N 0.32616(18) 0.3482(3) 0.6047(2) 0.0718(14) Uani 1 1 d . . . . .
C8 C 0.0892(3) 0.5800(3) 0.9298(3) 0.0741(18) Uani 1 1 d . . . . .
H8A H 0.088455 0.547066 0.958898 0.089 Uiso 1 1 calc R U . . .
H8B H 0.081963 0.549697 0.899428 0.089 Uiso 1 1 calc R U . . .
C29 C 0.2542(2) 0.1969(4) 0.7050(3) 0.085(2) Uani 1 1 d . . . . .
H29A H 0.222492 0.203156 0.722620 0.102 Uiso 1 1 calc R U . . .
H29B H 0.241550 0.189741 0.669480 0.102 Uiso 1 1 calc R U . . .
C9 C 0.0912(3) 0.7365(4) 0.9877(3) 0.081(2) Uani 1 1 d . . . . .
H9A H 0.115299 0.779734 0.988104 0.098 Uiso 1 1 calc R U . . .
H9B H 0.060520 0.751369 1.004818 0.098 Uiso 1 1 calc R U . . .
C6 C 0.0342(3) 0.7748(4) 0.9091(3) 0.098(2) Uani 1 1 d . . . . .
H6A H 0.017307 0.799317 0.935810 0.117 Uiso 1 1 calc R U . . .
H6B H 0.005731 0.749553 0.887304 0.117 Uiso 1 1 calc R U . . .
C13 C 0.07246(19) 0.6194(3) 0.7821(2) 0.0566(14) Uani 1 1 d . . . . .
C98 C 0.3484(2) 0.9552(3) 0.83960(19) 0.0506(12) Uani 1 1 d . . . . .
C11 C 0.1586(3) 0.6356(4) 0.9878(3) 0.089(2) Uani 1 1 d . . . . .
H11A H 0.169427 0.588681 1.005008 0.107 Uiso 1 1 calc R U . . .
H11B H 0.190609 0.667107 0.988935 0.107 Uiso 1 1 calc R U . . .
C92 C 0.45263(18) 0.9647(3) 0.85532(18) 0.0451(11) Uani 1 1 d . . . . .
C56 C 0.14951(19) 0.4947(3) 0.65715(19) 0.0486(12) Uani 1 1 d . . . . .
C68 C 0.30991(18) 0.3810(3) 0.90914(18) 0.0454(11) Uani 1 1 d . . . . .
C86 C 0.35671(18) 0.4948(3) 0.85975(19) 0.0463(11) Uani 1 1 d . . . . .
C128 C -0.09906(18) 0.5961(3) 0.79371(19) 0.0482(12) Uani 1 1 d . . . . .
C26 C 0.3165(3) 0.2608(5) 0.7737(3) 0.110(3) Uani 1 1 d . . . . .
H26A H 0.329773 0.309841 0.785916 0.131 Uiso 1 1 calc R U . . .
H26B H 0.291070 0.241934 0.795722 0.131 Uiso 1 1 calc R U . . .
C7 C 0.0478(2) 0.6405(4) 0.9305(3) 0.0729(17) Uani 1 1 d . . . . .
H7A H 0.021744 0.635383 0.900703 0.088 Uiso 1 1 calc R U . . .
H7B H 0.028694 0.633433 0.959876 0.088 Uiso 1 1 calc R U . . .
C25 C 0.3614(3) 0.2074(4) 0.7713(2) 0.0693(16) Uani 1 1 d . . . . .
H25A H 0.357884 0.166041 0.794723 0.083 Uiso 1 1 calc R U . . .
H25B H 0.395373 0.232932 0.781572 0.083 Uiso 1 1 calc R U . . .
C85 C 0.3338(2) 0.4775(3) 0.8083(2) 0.0539(13) Uani 1 1 d . . . . .
H85 H 0.313135 0.433644 0.804159 0.065 Uiso 1 1 calc R U . . .
C67 C 0.3134(2) 0.3096(3) 0.9330(2) 0.0584(14) Uani 1 1 d . . . . .
H67 H 0.346596 0.295350 0.950142 0.070 Uiso 1 1 calc R U . . .
C104 C 0.41211(19) 0.8586(3) 0.79431(19) 0.0477(12) Uani 1 1 d . . . . .
C82 C 0.3919(2) 0.6049(3) 0.8174(2) 0.0650(15) Uani 1 1 d . . . . .
H82 H 0.412335 0.649075 0.821344 0.078 Uiso 1 1 calc R U . . .
C87 C 0.4547(2) 1.0342(3) 0.8305(2) 0.0555(13) Uani 1 1 d . . . . .
H87 H 0.423243 1.051762 0.811921 0.067 Uiso 1 1 calc R U . . .
C81 C 0.3855(2) 0.5616(3) 0.8624(2) 0.0603(14) Uani 1 1 d . . . . .
H81 H 0.400949 0.579198 0.893687 0.072 Uiso 1 1 calc R U . . .
C80 C 0.34998(18) 0.4922(3) 0.96671(19) 0.0491(12) Uani 1 1 d . . . . .
C51 C 0.1159(2) 0.4331(3) 0.6557(2) 0.0607(14) Uani 1 1 d . . . . .
H51 H 0.096602 0.419261 0.625042 0.073 Uiso 1 1 calc R U . . .
C50 C 0.15735(18) 0.4945(3) 0.54959(19) 0.0468(11) Uani 1 1 d . . . . .
C45 C 0.1486(3) 0.5245(4) 0.4981(2) 0.0704(16) Uani 1 1 d . . . . .
H45 H 0.137160 0.574584 0.494653 0.084 Uiso 1 1 calc R U . . .
C102 C 0.4537(2) 0.7547(3) 0.7534(2) 0.0643(15) Uani 1 1 d . . . . .
H102 H 0.475195 0.711592 0.757930 0.077 Uiso 1 1 calc R U . . .
C103 C 0.4443(2) 0.7964(3) 0.7975(2) 0.0555(13) Uani 1 1 d . . . . .
H103 H 0.460629 0.780639 0.828991 0.067 Uiso 1 1 calc R U . . .
C79 C 0.3708(2) 0.4732(4) 1.0192(2) 0.0622(15) Uani 1 1 d . . . . .
H79 H 0.391955 0.429763 1.023962 0.075 Uiso 1 1 calc R U . . .
C110 C 0.39778(19) 0.8584(3) 0.9015(2) 0.0489(12) Uani 1 1 d . . . . .
C109 C 0.4032(2) 0.8908(3) 0.9532(2) 0.0625(15) Uani 1 1 d . . . . .
H109 H 0.412785 0.941662 0.956042 0.075 Uiso 1 1 calc R U . . .
C75 C 0.3187(2) 0.5559(3) 0.9637(2) 0.0610(14) Uani 1 1 d . . . . .
H75 H 0.303132 0.572634 0.932219 0.073 Uiso 1 1 calc R U . . .
C132 C 0.0132(2) 0.4207(3) 0.9207(2) 0.0655(16) Uani 1 1 d . . . . .
H132 H 0.025679 0.404640 0.953172 0.079 Uiso 1 1 calc R U . . .
C133 C -0.02640(19) 0.4725(3) 0.9121(2) 0.0569(14) Uani 1 1 d . . . . .
H133 H -0.041777 0.492823 0.939342 0.068 Uiso 1 1 calc R U . . .
C122 C -0.10508(17) 0.6050(3) 0.8996(2) 0.0490(12) Uani 1 1 d . . . . .
C49 C 0.1744(2) 0.4202(3) 0.5508(2) 0.0621(15) Uani 1 1 d . . . . .
H49 H 0.181116 0.395525 0.581690 0.074 Uiso 1 1 calc R U . . .
C131 C 0.0346(2) 0.3925(3) 0.8785(3) 0.0720(18) Uani 1 1 d . . . . .
H131 H 0.061666 0.356060 0.883710 0.086 Uiso 1 1 calc R U . . .
C93 C 0.3405(2) 1.0212(3) 0.8669(2) 0.0588(14) Uani 1 1 d . . . . .
H93 H 0.370180 1.043376 0.885642 0.071 Uiso 1 1 calc R U . . .
C55 C 0.1745(2) 0.5075(3) 0.7079(2) 0.0606(14) Uani 1 1 d . . . . .
H55 H 0.197374 0.549313 0.712290 0.073 Uiso 1 1 calc R U . . .
C14 C 0.0550(2) 0.5761(4) 0.7346(2) 0.0710(17) Uani 1 1 d . . . . .
H14A H 0.085927 0.565387 0.717373 0.106 Uiso 1 1 calc R U . . .
H14B H 0.029456 0.605766 0.713072 0.106 Uiso 1 1 calc R U . . .
H14C H 0.038290 0.529467 0.742963 0.106 Uiso 1 1 calc R U . . .
C123 C -0.0573(2) 0.6405(3) 0.7838(2) 0.0626(15) Uani 1 1 d . . . . .
H123 H -0.026315 0.639932 0.806909 0.075 Uiso 1 1 calc R U . . .
C94 C 0.2925(3) 1.0533(4) 0.8671(2) 0.0751(18) Uani 1 1 d . . . . .
H94 H 0.287756 1.097397 0.885129 0.090 Uiso 1 1 calc R U . . .
C48 C 0.1820(3) 0.3802(4) 0.5051(3) 0.0794(19) Uani 1 1 d . . . . .
H48 H 0.194072 0.330417 0.508257 0.095 Uiso 1 1 calc R U . . .
C91 C 0.4986(2) 0.9388(3) 0.8826(2) 0.0590(14) Uani 1 1 d . . . . .
H91 H 0.498893 0.892902 0.899695 0.071 Uiso 1 1 calc R U . . .
C124 C -0.0571(2) 0.6889(4) 0.7401(3) 0.0733(17) Uani 1 1 d . . . . .
H124 H -0.026433 0.717945 0.737256 0.088 Uiso 1 1 calc R U . . .
C120 C -0.1039(3) 0.7302(4) 0.9413(3) 0.090(2) Uani 1 1 d . . . . .
H120 H -0.100290 0.782303 0.937821 0.108 Uiso 1 1 calc R U . . .
C62 C 0.20510(19) 0.5984(3) 0.60859(18) 0.0477(11) Uani 1 1 d . . . . .
C88 C 0.4990(2) 1.0767(4) 0.8318(2) 0.0707(17) Uani 1 1 d . . . . .
H88 H 0.499031 1.123008 0.815238 0.085 Uiso 1 1 calc R U . . .
C31 C 0.4220(3) 0.3742(3) 0.7290(3) 0.0655(15) Uani 1 1 d . . . . .
C121 C -0.0997(2) 0.6833(3) 0.8973(3) 0.0669(15) Uani 1 1 d . . . . .
H121 H -0.093297 0.705877 0.867061 0.080 Uiso 1 1 calc R U . . .
C39 C 0.1014(2) 0.5984(3) 0.5970(2) 0.0568(13) Uani 1 1 d . . . . .
C105 C 0.3827(3) 0.7835(3) 0.9004(3) 0.085(2) Uani 1 1 d . . . . .
H105 H 0.377062 0.758119 0.869682 0.101 Uiso 1 1 calc R U . . .
C15 C 0.2189(3) 0.7008(4) 0.8058(3) 0.094(2) Uani 1 1 d . . . . .
C130 C 0.0176(2) 0.4158(4) 0.8272(3) 0.0719(17) Uani 1 1 d . . . . .
H130 H 0.033504 0.395484 0.800264 0.086 Uiso 1 1 calc R U . . .
C127 C -0.14060(19) 0.6047(3) 0.75460(19) 0.0529(13) Uani 1 1 d . . . . .
H127 H -0.171631 0.576172 0.756999 0.063 Uiso 1 1 calc R U . . .
C99 C 0.3928(3) 0.8774(4) 0.7419(2) 0.0706(17) Uani 1 1 d . . . . .
H99 H 0.371287 0.920346 0.736729 0.085 Uiso 1 1 calc R U . . .
C17 C 0.2177(2) 0.8221(3) 0.9402(2) 0.0635(15) Uani 1 1 d . . . . .
C90 C 0.5426(2) 0.9801(4) 0.8841(3) 0.0725(17) Uani 1 1 d . . . . .
H90 H 0.574200 0.963298 0.902792 0.087 Uiso 1 1 calc R U . . .
C32 C 0.4588(2) 0.4207(4) 0.7598(3) 0.0756(17) Uani 1 1 d . . . . .
H32A H 0.442354 0.437137 0.788801 0.113 Uiso 1 1 calc R U . . .
H32B H 0.468051 0.463994 0.740795 0.113 Uiso 1 1 calc R U . . .
H32C H 0.490999 0.392323 0.770700 0.113 Uiso 1 1 calc R U . . .
C134 C -0.04580(18) 0.4976(3) 0.8610(2) 0.0503(12) Uani 1 1 d . . . . .
C129 C -0.0219(2) 0.4676(3) 0.8196(2) 0.0642(15) Uani 1 1 d . . . . .
H129 H -0.033535 0.483978 0.786976 0.077 Uiso 1 1 calc R U . . .
C126 C -0.1413(2) 0.6524(4) 0.7109(2) 0.0669(16) Uani 1 1 d . . . . .
H126 H -0.172316 0.653505 0.687786 0.080 Uiso 1 1 calc R U . . .
C117 C -0.11670(19) 0.5787(3) 0.9500(2) 0.0569(14) Uani 1 1 d . . . . .
H117 H -0.121852 0.526985 0.953893 0.068 Uiso 1 1 calc R U . . .
C118 C -0.1208(2) 0.6257(4) 0.9938(2) 0.0668(16) Uani 1 1 d . . . . .
H118 H -0.128441 0.604357 1.024057 0.080 Uiso 1 1 calc R U . . .
C125 C -0.0997(3) 0.6946(4) 0.7025(3) 0.0731(17) Uani 1 1 d . . . . .
H125 H -0.099108 0.725018 0.674033 0.088 Uiso 1 1 calc R U . . .
C74 C 0.41252(19) 0.3994(3) 0.91743(19) 0.0501(12) Uani 1 1 d . . . . .
C101 C 0.4327(3) 0.7736(4) 0.7029(3) 0.0750(18) Uani 1 1 d . . . . .
H101 H 0.439244 0.743266 0.675764 0.090 Uiso 1 1 calc R U . . .
C65 C 0.2254(3) 0.2836(4) 0.9084(3) 0.0787(19) Uani 1 1 d . . . . .
H65 H 0.195711 0.251353 0.906948 0.094 Uiso 1 1 calc R U . . .
C40 C 0.0971(3) 0.6670(4) 0.6247(3) 0.0759(18) Uani 1 1 d . . . . .
H40 H 0.127317 0.684247 0.645295 0.091 Uiso 1 1 calc R U . . .
C5 C 0.0580(3) 0.8356(4) 0.8785(3) 0.0795(19) Uani 1 1 d . . . . .
C84 C 0.3393(3) 0.5199(3) 0.7631(2) 0.0663(15) Uani 1 1 d . . . . .
H84 H 0.322816 0.503570 0.731826 0.080 Uiso 1 1 calc R U . . .
C35 C 0.2787(2) 0.1516(4) 0.5691(2) 0.0586(14) Uani 1 1 d . . . . .
C77 C 0.3307(3) 0.5788(4) 1.0588(3) 0.078(2) Uani 1 1 d . . . . .
H77 H 0.323654 0.608189 1.086215 0.094 Uiso 1 1 calc R U . . .
C106 C 0.3755(4) 0.7438(4) 0.9466(4) 0.112(3) Uani 1 1 d . . . . .
H106 H 0.365641 0.692963 0.944035 0.134 Uiso 1 1 calc R U . . .
C66 C 0.2722(3) 0.2613(3) 0.9325(3) 0.0755(18) Uani 1 1 d . . . . .
H66 H 0.276146 0.214384 0.948313 0.091 Uiso 1 1 calc R U . . .
C89 C 0.5431(2) 1.0491(4) 0.8580(3) 0.0796(19) Uani 1 1 d . . . . .
H89 H 0.575232 1.076227 0.859284 0.095 Uiso 1 1 calc R U . . .
C36 C 0.2512(2) 0.1009(4) 0.5318(2) 0.0694(16) Uani 1 1 d . . . . .
H36A H 0.267317 0.051565 0.535448 0.104 Uiso 1 1 calc R U . . .
H36B H 0.254306 0.120007 0.498568 0.104 Uiso 1 1 calc R U . . .
H36C H 0.213635 0.097624 0.536848 0.104 Uiso 1 1 calc R U . . .
C116 C -0.14518(18) 0.4852(3) 0.84371(19) 0.0499(12) Uani 1 1 d . . . . .
C119 C -0.1133(2) 0.7015(5) 0.9900(3) 0.079(2) Uani 1 1 d . . . . .
H119 H -0.114179 0.733438 1.017657 0.095 Uiso 1 1 calc R U . . .
C78 C 0.3615(3) 0.5161(5) 1.0649(2) 0.079(2) Uani 1 1 d . . . . .
H78 H 0.376361 0.500382 1.096800 0.094 Uiso 1 1 calc R U . . .
C54 C 0.1688(3) 0.4638(4) 0.7531(2) 0.0769(19) Uani 1 1 d . . . . .
H54 H 0.187283 0.477393 0.784093 0.092 Uiso 1 1 calc R U . . .
C69 C 0.4560(2) 0.4330(4) 0.9428(2) 0.0642(15) Uani 1 1 d . . . . .
H69 H 0.452258 0.477224 0.960997 0.077 Uiso 1 1 calc R U . . .
C64 C 0.2196(2) 0.3532(4) 0.8854(2) 0.0698(17) Uani 1 1 d . . . . .
H64 H 0.186121 0.367230 0.868881 0.084 Uiso 1 1 calc R U . . .
C59 C 0.2970(3) 0.6786(5) 0.6105(3) 0.084(2) Uani 1 1 d . . . . .
H59 H 0.329526 0.704907 0.612286 0.101 Uiso 1 1 calc R U . . .
C107 C 0.3823(3) 0.7770(5) 0.9961(3) 0.091(2) Uani 1 1 d . . . . .
H107 H 0.378081 0.748463 1.024726 0.109 Uiso 1 1 calc R U . . .
C115 C -0.1939(2) 0.5060(3) 0.8531(2) 0.0598(14) Uani 1 1 d . . . . .
H115 H -0.200006 0.555359 0.863294 0.072 Uiso 1 1 calc R U . . .
C73 C 0.4202(2) 0.3319(4) 0.8911(2) 0.0681(16) Uani 1 1 d . . . . .
H73 H 0.390072 0.309012 0.873443 0.082 Uiso 1 1 calc R U . . .
C41 C 0.0524(4) 0.7067(5) 0.6222(3) 0.102(3) Uani 1 1 d . . . . .
H41 H 0.050685 0.751868 0.639834 0.122 Uiso 1 1 calc R U . . .
C57 C 0.2510(2) 0.5672(4) 0.6282(2) 0.0709(17) Uani 1 1 d . . . . .
H57 H 0.251437 0.518218 0.640942 0.085 Uiso 1 1 calc R U . . .
C63 C 0.2615(2) 0.4012(3) 0.8864(2) 0.0560(13) Uani 1 1 d . . . . .
H63 H 0.256786 0.448544 0.871291 0.067 Uiso 1 1 calc R U . . .
C76 C 0.3094(2) 0.5981(4) 1.0089(3) 0.0743(18) Uani 1 1 d . . . . .
H76 H 0.287754 0.641105 1.004640 0.089 Uiso 1 1 calc R U . . .
C52 C 0.1096(3) 0.3893(4) 0.7002(3) 0.0750(18) Uani 1 1 d . . . . .
H52 H 0.085979 0.348325 0.696558 0.090 Uiso 1 1 calc R U . . .
C60 C 0.2526(3) 0.7115(4) 0.5898(3) 0.083(2) Uani 1 1 d . . . . .
H60 H 0.252712 0.760323 0.576668 0.100 Uiso 1 1 calc R U . . .
C108 C 0.3955(2) 0.8524(5) 0.9995(2) 0.0783(19) Uani 1 1 d . . . . .
H108 H 0.399151 0.877582 1.030377 0.094 Uiso 1 1 calc R U . . .
C111 C -0.1404(2) 0.4105(3) 0.8287(3) 0.0711(17) Uani 1 1 d . . . . .
H111 H -0.106436 0.394386 0.821842 0.085 Uiso 1 1 calc R U . . .
C100 C 0.4038(3) 0.8356(4) 0.6964(2) 0.085(2) Uani 1 1 d . . . . .
H100 H 0.390804 0.852521 0.664183 0.102 Uiso 1 1 calc R U . . .
C83 C 0.3694(2) 0.5849(3) 0.7674(2) 0.0651(15) Uani 1 1 d . . . . .
H83 H 0.374883 0.614279 0.739476 0.078 Uiso 1 1 calc R U . . .
C47 C 0.1723(3) 0.4110(4) 0.4552(3) 0.084(2) Uani 1 1 d . . . . .
H47 H 0.177099 0.382479 0.426720 0.100 Uiso 1 1 calc R U . . .
C61 C 0.2074(2) 0.6710(3) 0.5886(2) 0.0681(16) Uani 1 1 d . . . . .
H61 H 0.175446 0.692519 0.573482 0.082 Uiso 1 1 calc R U . . .
C95 C 0.2512(2) 1.0188(4) 0.8399(3) 0.079(2) Uani 1 1 d . . . . .
H95 H 0.216631 1.038561 0.840305 0.095 Uiso 1 1 calc R U . . .
C33 C 0.3176(2) 0.3935(4) 0.5727(3) 0.0686(16) Uani 1 1 d . . . . .
C71 C 0.5096(3) 0.3354(5) 0.9157(3) 0.088(2) Uani 1 1 d . . . . .
H71 H 0.544001 0.314446 0.916138 0.105 Uiso 1 1 calc R U . . .
C58 C 0.2968(2) 0.6069(5) 0.6294(3) 0.086(2) Uani 1 1 d . . . . .
H58 H 0.329201 0.585231 0.643470 0.103 Uiso 1 1 calc R U . . .
C18 C 0.2596(3) 0.8733(4) 0.9555(3) 0.090(2) Uani 1 1 d . . . . .
H18A H 0.259711 0.884318 0.990824 0.135 Uiso 1 1 calc R U . . .
H18B H 0.254093 0.919265 0.936375 0.135 Uiso 1 1 calc R U . . .
H18C H 0.293692 0.851316 0.949863 0.135 Uiso 1 1 calc R U . . .
C53 C 0.1364(3) 0.4037(4) 0.7488(3) 0.0755(18) Uani 1 1 d . . . . .
H53 H 0.131625 0.372964 0.776323 0.091 Uiso 1 1 calc R U . . .
C3 C 0.0608(5) 0.9581(5) 0.8389(4) 0.125(4) Uani 1 1 d . . . . .
H3 H 0.047727 1.007328 0.834985 0.150 Uiso 1 1 calc R U . . .
C44 C 0.0568(2) 0.5731(4) 0.5679(3) 0.082(2) Uani 1 1 d . . . . .
H44 H 0.058130 0.528282 0.549686 0.099 Uiso 1 1 calc R U . . .
C96 C 0.2576(2) 0.9553(5) 0.8115(3) 0.089(2) Uani 1 1 d . . . . .
H96 H 0.227838 0.935161 0.791647 0.107 Uiso 1 1 calc R U . . .
C112 C -0.1807(3) 0.3595(4) 0.8233(3) 0.091(2) Uani 1 1 d . . . . .
H112 H -0.174923 0.309976 0.813420 0.109 Uiso 1 1 calc R U . . .
C10 C 0.1206(4) 0.6736(5) 1.0173(3) 0.097(2) Uani 1 1 d . . . . .
H10A H 0.140073 0.694028 1.047938 0.116 Uiso 1 1 calc R U . . .
H10B H 0.094486 0.637071 1.026974 0.116 Uiso 1 1 calc R U . . .
C70 C 0.5040(2) 0.4023(5) 0.9413(3) 0.083(2) Uani 1 1 d . . . . .
H70 H 0.534536 0.425929 0.957735 0.100 Uiso 1 1 calc R U . . .
C46 C 0.1557(3) 0.4844(5) 0.4520(2) 0.090(2) Uani 1 1 d . . . . .
H46 H 0.149133 0.508328 0.420786 0.108 Uiso 1 1 calc R U . . .
C23 C 0.4279(3) 0.1605(4) 0.6551(2) 0.083(2) Uani 1 1 d . . . . .
C42 C 0.0096(3) 0.6798(6) 0.5935(4) 0.117(3) Uani 1 1 d . . . . .
H42 H -0.022725 0.706490 0.591895 0.140 Uiso 1 1 calc R U . . .
C72 C 0.4678(3) 0.2994(4) 0.8903(3) 0.087(2) Uani 1 1 d . . . . .
H72 H 0.472006 0.254323 0.873085 0.105 Uiso 1 1 calc R U . . .
C97 C 0.3042(2) 0.9233(4) 0.8118(3) 0.0727(17) Uani 1 1 d . . . . .
H97 H 0.307779 0.879184 0.793384 0.087 Uiso 1 1 calc R U . . .
C113 C -0.2277(3) 0.3827(4) 0.8325(3) 0.082(2) Uani 1 1 d . . . . .
H113 H -0.257121 0.349865 0.828773 0.099 Uiso 1 1 calc R U . . .
C4 C 0.0380(3) 0.9086(5) 0.8710(4) 0.106(3) Uani 1 1 d . . . . .
H4 H 0.009089 0.924541 0.887605 0.128 Uiso 1 1 calc R U . . .
C2 C 0.1012(4) 0.9356(5) 0.8135(4) 0.101(3) Uani 1 1 d . . . . .
H2 H 0.116337 0.967099 0.790981 0.121 Uiso 1 1 calc R U . . .
C19 C 0.4209(3) 0.2365(4) 0.5800(3) 0.084(2) Uani 1 1 d . . . . .
H19 H 0.402946 0.276035 0.562132 0.100 Uiso 1 1 calc R U . . .
C1 C 0.1184(3) 0.8653(4) 0.8227(3) 0.083(2) Uani 1 1 d . . . . .
H1 H 0.146787 0.848764 0.805670 0.100 Uiso 1 1 calc R U . . .
C114 C -0.2342(2) 0.4564(4) 0.8480(3) 0.0735(18) Uani 1 1 d . . . . .
H114 H -0.268273 0.471849 0.855075 0.088 Uiso 1 1 calc R U . . .
C34 C 0.3057(3) 0.4522(4) 0.5332(3) 0.087(2) Uani 1 1 d . . . . .
H34A H 0.267293 0.459026 0.526421 0.130 Uiso 1 1 calc R U . . .
H34B H 0.319938 0.436467 0.502847 0.130 Uiso 1 1 calc R U . . .
H34C H 0.322308 0.499093 0.544749 0.130 Uiso 1 1 calc R U . . .
C22 C 0.4691(3) 0.1206(5) 0.6362(3) 0.100(3) Uani 1 1 d . . . . .
H22 H 0.486781 0.080715 0.653957 0.121 Uiso 1 1 calc R U . . .
C21 C 0.4828(3) 0.1440(6) 0.5879(4) 0.107(3) Uani 1 1 d . . . . .
H21 H 0.510552 0.117445 0.575159 0.129 Uiso 1 1 calc R U . . .
C20 C 0.4601(3) 0.2001(5) 0.5591(4) 0.102(3) Uani 1 1 d . . . . .
H20 H 0.470424 0.212588 0.527685 0.123 Uiso 1 1 calc R U . . .
C12 C 0.1755(3) 0.5598(4) 0.9125(4) 0.111(3) Uani 1 1 d . . . . .
H12A H 0.175278 0.514829 0.932725 0.167 Uiso 1 1 calc R U . . .
H12B H 0.211713 0.579342 0.914467 0.167 Uiso 1 1 calc R U . . .
H12C H 0.162755 0.548023 0.878048 0.167 Uiso 1 1 calc R U . . .
C43 C 0.0109(3) 0.6130(6) 0.5654(4) 0.109(3) Uani 1 1 d . . . . .
H43 H -0.019876 0.596526 0.545221 0.131 Uiso 1 1 calc R U . . .
C24 C 0.4138(4) 0.1461(5) 0.7101(3) 0.123(3) Uani 1 1 d . . . . .
H24A H 0.414691 0.092113 0.716775 0.148 Uiso 1 1 calc R U . . .
H24B H 0.441022 0.169993 0.733969 0.148 Uiso 1 1 calc R U . . .
C28 C 0.2813(4) 0.1291(5) 0.7232(4) 0.120(3) Uani 1 1 d . . . . .
H28A H 0.284522 0.130747 0.759812 0.143 Uiso 1 1 calc R U . . .
H28B H 0.257664 0.086985 0.712649 0.143 Uiso 1 1 calc R U . . .
C27 C 0.3305(5) 0.1126(6) 0.7100(3) 0.117(3) Uani 1 1 d . . . . .
H27A H 0.327483 0.097286 0.674850 0.141 Uiso 1 1 calc R U . . .
H27B H 0.346406 0.071162 0.730557 0.141 Uiso 1 1 calc R U . . .
C16 C 0.2604(4) 0.6945(6) 0.7729(5) 0.164(5) Uani 1 1 d . . . . .
H16A H 0.287316 0.659019 0.786801 0.246 Uiso 1 1 calc R U . . .
H16B H 0.276897 0.743110 0.769494 0.246 Uiso 1 1 calc R U . . .
H16C H 0.244782 0.677174 0.740246 0.246 Uiso 1 1 calc R U . . .
C30 C 0.2537(5) 0.3318(6) 0.6998(8) 0.282(11) Uani 1 1 d . . . . .
H30A H 0.276281 0.376012 0.703766 0.422 Uiso 1 1 calc R U . . .
H30B H 0.236216 0.329515 0.665805 0.422 Uiso 1 1 calc R U . . .
H30C H 0.226813 0.334437 0.722898 0.422 Uiso 1 1 calc R U . . .
C37 C 0.4268(3) 0.3699(5) 0.4739(3) 0.084(2) Uani 1 1 d . . . . .
N13 N 0.3862(3) 0.3561(5) 0.4780(4) 0.141(3) Uani 1 1 d . . . . .
C38 C 0.4784(3) 0.3852(6) 0.4689(3) 0.126(3) Uani 1 1 d . . . . .
H38A H 0.488739 0.431477 0.486315 0.189 Uiso 1 1 calc R U . . .
H38B H 0.482628 0.390639 0.433715 0.189 Uiso 1 1 calc R U . . .
H38C H 0.500869 0.344616 0.483070 0.189 Uiso 1 1 calc R U . . .
Ni1 Ni 0.12887(2) 0.71341(4) 0.88231(3) 0.0556(2) Uani 1 1 d . . . . .
B4 B -0.0988(2) 0.5472(3) 0.8497(2) 0.0469(13) Uani 1 1 d . . . . .
Ni2 Ni 0.34335(3) 0.25921(4) 0.65952(3) 0.0547(2) Uani 1 1 d . . . . .
B3 B 0.4026(2) 0.9096(3) 0.8474(2) 0.0446(13) Uani 1 1 d . . . . .
N7 N 0.40550(18) 0.2177(3) 0.6282(2) 0.0662(13) Uani 1 1 d . . . . .
B2 B 0.3573(2) 0.4414(3) 0.9136(2) 0.0462(13) Uani 1 1 d . . . . .
B1 B 0.1532(2) 0.5470(3) 0.6034(2) 0.0471(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
N5 C15 1.112(9) . ?
N5 Ni1 2.094(6) . ?
N2 C6 1.438(8) . ?
N2 C7 1.473(7) . ?
N2 C9 1.556(8) . ?
N2 Ni1 2.073(5) . ?
N9 C30 1.392(11) . ?
N9 C29 1.463(8) . ?
N9 C26 1.785(10) . ?
N9 Ni2 2.089(6) . ?
N4 C13 1.183(7) . ?
N4 Ni1 2.152(5) . ?
N6 C17 1.089(6) . ?
N6 Ni1 2.137(5) . ?
N10 C31 1.128(7) . ?
N10 Ni2 2.123(6) . ?
N12 C35 1.164(7) . ?
N12 Ni2 2.170(6) . ?
N3 C8 1.425(7) . ?
N3 C12 1.443(9) . ?
N3 C11 1.561(8) . ?
N3 Ni1 2.157(5) . ?
N8 C27 1.354(9) . ?
N8 C24 1.423(9) . ?
N8 C25 1.550(8) . ?
N8 Ni2 2.150(5) . ?
N1 C5 1.303(8) . ?
N1 C1 1.363(8) . ?
N1 Ni1 2.047(5) . ?
N11 C33 1.172(7) . ?
N11 Ni2 2.153(5) . ?
C8 C7 1.484(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C29 C28 1.431(11) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C9 C10 1.502(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C6 C5 1.511(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C13 C14 1.499(8) . ?
C98 C97 1.375(7) . ?
C98 C93 1.399(7) . ?
C98 B3 1.563(7) . ?
C11 C10 1.460(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C92 C91 1.362(6) . ?
C92 C87 1.397(7) . ?
C92 B3 1.575(7) . ?
C56 C51 1.370(7) . ?
C56 C55 1.439(7) . ?
C56 B1 1.715(8) . ?
C68 C63 1.332(7) . ?
C68 C67 1.410(7) . ?
C68 B2 1.583(7) . ?
C86 C81 1.377(7) . ?
C86 C85 1.454(7) . ?
C86 B2 1.715(8) . ?
C128 C123 1.352(7) . ?
C128 C127 1.388(7) . ?
C128 B4 1.723(8) . ?
C26 C25 1.469(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C85 C84 1.438(8) . ?
C85 H85 0.9300 . ?
C67 C66 1.333(8) . ?
C67 H67 0.9300 . ?
C104 C103 1.357(7) . ?
C104 C99 1.461(7) . ?
C104 B3 1.716(8) . ?
C82 C83 1.429(8) . ?
C82 C81 1.446(8) . ?
C82 H82 0.9300 . ?
C87 C88 1.330(7) . ?
C87 H87 0.9300 . ?
C81 H81 0.9300 . ?
C80 C75 1.364(7) . ?
C80 C79 1.472(7) . ?
C80 B2 1.703(7) . ?
C51 C52 1.440(8) . ?
C51 H51 0.9300 . ?
C50 C49 1.378(7) . ?
C50 C45 1.463(7) . ?
C50 B1 1.720(8) . ?
C45 C46 1.446(9) . ?
C45 H45 0.9300 . ?
C102 C101 1.424(9) . ?
C102 C103 1.430(8) . ?
C102 H102 0.9300 . ?
C103 H103 0.9300 . ?
C79 C78 1.476(8) . ?
C79 H79 0.9300 . ?
C110 C105 1.375(8) . ?
C110 C109 1.482(7) . ?
C110 B3 1.717(7) . ?
C109 C108 1.441(8) . ?
C109 H109 0.9300 . ?
C75 C76 1.459(8) . ?
C75 H75 0.9300 . ?
C132 C133 1.344(7) . ?
C132 C131 1.390(9) . ?
C132 H132 0.9300 . ?
C133 C134 1.461(7) . ?
C133 H133 0.9300 . ?
C122 C121 1.390(7) . ?
C122 C117 1.480(7) . ?
C122 B4 1.699(8) . ?
C49 C48 1.438(8) . ?
C49 H49 0.9300 . ?
C131 C130 1.444(9) . ?
C131 H131 0.9300 . ?
C93 C94 1.322(8) . ?
C93 H93 0.9300 . ?
C55 C54 1.451(8) . ?
C55 H55 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C123 C124 1.444(8) . ?
C123 H123 0.9300 . ?
C94 C95 1.332(9) . ?
C94 H94 0.9300 . ?
C48 C47 1.430(9) . ?
C48 H48 0.9300 . ?
C91 C90 1.311(8) . ?
C91 H91 0.9300 . ?
C124 C125 1.375(8) . ?
C124 H124 0.9300 . ?
C120 C119 1.436(10) . ?
C120 C121 1.449(9) . ?
C120 H120 0.9300 . ?
C62 C57 1.319(7) . ?
C62 C61 1.393(7) . ?
C62 B1 1.571(7) . ?
C88 C89 1.322(9) . ?
C88 H88 0.9300 . ?
C31 C32 1.419(9) . ?
C121 H121 0.9300 . ?
C39 C44 1.354(8) . ?
C39 C40 1.429(8) . ?
C39 B1 1.569(7) . ?
C105 C106 1.445(10) . ?
C105 H105 0.9300 . ?
C15 C16 1.433(11) . ?
C130 C129 1.340(7) . ?
C130 H130 0.9300 . ?
C127 C126 1.434(7) . ?
C127 H127 0.9300 . ?
C99 C100 1.472(9) . ?
C99 H99 0.9300 . ?
C17 C18 1.405(8) . ?
C90 C89 1.402(9) . ?
C90 H90 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C134 C129 1.414(8) . ?
C134 B4 1.583(7) . ?
C129 H129 0.9300 . ?
C126 C125 1.317(8) . ?
C126 H126 0.9300 . ?
C117 C118 1.443(8) . ?
C117 H117 0.9300 . ?
C118 C119 1.357(9) . ?
C118 H118 0.9300 . ?
C125 H125 0.9300 . ?
C74 C69 1.346(7) . ?
C74 C73 1.407(8) . ?
C74 B2 1.554(7) . ?
C101 C100 1.309(9) . ?
C101 H101 0.9300 . ?
C65 C66 1.323(9) . ?
C65 C64 1.373(9) . ?
C65 H65 0.9300 . ?
C40 C41 1.310(9) . ?
C40 H40 0.9300 . ?
C5 C4 1.389(10) . ?
C84 C83 1.369(8) . ?
C84 H84 0.9300 . ?
C35 C36 1.449(8) . ?
C77 C78 1.345(9) . ?
C77 C76 1.413(9) . ?
C77 H77 0.9300 . ?
C106 C107 1.436(11) . ?
C106 H106 0.9300 . ?
C66 H66 0.9300 . ?
C89 H89 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C116 C115 1.318(7) . ?
C116 C111 1.388(8) . ?
C116 B4 1.584(7) . ?
C119 H119 0.9300 . ?
C78 H78 0.9300 . ?
C54 C53 1.330(9) . ?
C54 H54 0.9300 . ?
C69 C70 1.316(8) . ?
C69 H69 0.9300 . ?
C64 C63 1.342(7) . ?
C64 H64 0.9300 . ?
C59 C60 1.313(10) . ?
C59 C58 1.363(10) . ?
C59 H59 0.9300 . ?
C107 C108 1.372(10) . ?
C107 H107 0.9300 . ?
C115 C114 1.328(8) . ?
C115 H115 0.9300 . ?
C73 C72 1.320(8) . ?
C73 H73 0.9300 . ?
C41 C42 1.324(12) . ?
C41 H41 0.9300 . ?
C57 C58 1.335(8) . ?
C57 H57 0.9300 . ?
C63 H63 0.9300 . ?
C76 H76 0.9300 . ?
C52 C53 1.410(9) . ?
C52 H52 0.9300 . ?
C60 C61 1.328(8) . ?
C60 H60 0.9300 . ?
C108 H108 0.9300 . ?
C111 C112 1.341(8) . ?
C111 H111 0.9300 . ?
C100 H100 0.9300 . ?
C83 H83 0.9300 . ?
C47 C46 1.361(10) . ?
C47 H47 0.9300 . ?
C61 H61 0.9300 . ?
C95 C96 1.372(10) . ?
C95 H95 0.9300 . ?
C33 C34 1.482(8) . ?
C71 C72 1.334(9) . ?
C71 C70 1.380(10) . ?
C71 H71 0.9300 . ?
C58 H58 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C53 H53 0.9300 . ?
C3 C2 1.335(14) . ?
C3 C4 1.388(13) . ?
C3 H3 0.9300 . ?
C44 C43 1.337(9) . ?
C44 H44 0.9300 . ?
C96 C97 1.288(8) . ?
C96 H96 0.9300 . ?
C112 C113 1.289(9) . ?
C112 H112 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C70 H70 0.9300 . ?
C46 H46 0.9300 . ?
C23 N7 1.324(8) . ?
C23 C22 1.386(9) . ?
C23 C24 1.563(11) . ?
C42 C43 1.398(12) . ?
C42 H42 0.9300 . ?
C72 H72 0.9300 . ?
C97 H97 0.9300 . ?
C113 C114 1.379(9) . ?
C113 H113 0.9300 . ?
C4 H4 0.9300 . ?
C2 C1 1.327(10) . ?
C2 H2 0.9300 . ?
C19 C20 1.342(9) . ?
C19 N7 1.420(9) . ?
C19 H19 0.9300 . ?
C1 H1 0.9300 . ?
C114 H114 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C22 C21 1.431(12) . ?
C22 H22 0.9300 . ?
C21 C20 1.337(11) . ?
C21 H21 0.9300 . ?
C20 H20 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C43 H43 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C28 C27 1.342(13) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C37 N13 1.057(9) . ?
C37 C38 1.332(11) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
Ni2 N7 1.981(5) . ?

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
C15 N5 Ni1 177.9(6) . . ?
C6 N2 C7 114.8(5) . . ?
C6 N2 C9 112.1(5) . . ?
C7 N2 C9 107.6(5) . . ?
C6 N2 Ni1 102.1(4) . . ?
C7 N2 Ni1 104.2(4) . . ?
C9 N2 Ni1 115.9(3) . . ?
C30 N9 C29 113.4(8) . . ?
C30 N9 C26 114.3(10) . . ?
C29 N9 C26 101.5(5) . . ?
C30 N9 Ni2 110.3(6) . . ?
C29 N9 Ni2 106.2(4) . . ?
C26 N9 Ni2 110.5(4) . . ?
C13 N4 Ni1 166.6(4) . . ?
C17 N6 Ni1 161.2(6) . . ?
C31 N10 Ni2 173.3(5) . . ?
C35 N12 Ni2 176.3(5) . . ?
C8 N3 C12 105.0(5) . . ?
C8 N3 C11 106.2(5) . . ?
C12 N3 C11 111.6(6) . . ?
C8 N3 Ni1 106.4(4) . . ?
C12 N3 Ni1 112.6(5) . . ?
C11 N3 Ni1 114.2(4) . . ?
C27 N8 C24 101.9(8) . . ?
C27 N8 C25 111.4(6) . . ?
C24 N8 C25 111.3(6) . . ?
C27 N8 Ni2 112.9(5) . . ?
C24 N8 Ni2 106.0(4) . . ?
C25 N8 Ni2 112.8(3) . . ?
C5 N1 C1 118.4(6) . . ?
C5 N1 Ni1 110.1(5) . . ?
C1 N1 Ni1 130.7(5) . . ?
C33 N11 Ni2 175.9(5) . . ?
N3 C8 C7 107.4(5) . . ?
N3 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
N3 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
C28 C29 N9 117.2(6) . . ?
C28 C29 H29A 108.0 . . ?
N9 C29 H29A 108.0 . . ?
C28 C29 H29B 108.0 . . ?
N9 C29 H29B 108.0 . . ?
H29A C29 H29B 107.2 . . ?
C10 C9 N2 115.6(5) . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
N2 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
N2 C6 C5 117.3(5) . . ?
N2 C6 H6A 108.0 . . ?
C5 C6 H6A 108.0 . . ?
N2 C6 H6B 108.0 . . ?
C5 C6 H6B 108.0 . . ?
H6A C6 H6B 107.2 . . ?
N4 C13 C14 178.9(6) . . ?
C97 C98 C93 117.9(5) . . ?
C97 C98 B3 119.0(5) . . ?
C93 C98 B3 122.1(4) . . ?
C10 C11 N3 119.4(6) . . ?
C10 C11 H11A 107.5 . . ?
N3 C11 H11A 107.5 . . ?
C10 C11 H11B 107.5 . . ?
N3 C11 H11B 107.5 . . ?
H11A C11 H11B 107.0 . . ?
C91 C92 C87 118.2(5) . . ?
C91 C92 B3 117.8(4) . . ?
C87 C92 B3 123.4(4) . . ?
C51 C56 C55 110.4(5) . . ?
C51 C56 B1 119.6(5) . . ?
C55 C56 B1 129.8(5) . . ?
C63 C68 C67 116.8(5) . . ?
C63 C68 B2 118.6(5) . . ?
C67 C68 B2 124.2(4) . . ?
C81 C86 C85 111.9(5) . . ?
C81 C86 B2 118.3(4) . . ?
C85 C86 B2 129.6(4) . . ?
C123 C128 C127 108.2(5) . . ?
C123 C128 B4 122.3(4) . . ?
C127 C128 B4 129.2(4) . . ?
C25 C26 N9 104.5(5) . . ?
C25 C26 H26A 110.8 . . ?
N9 C26 H26A 110.8 . . ?
C25 C26 H26B 110.8 . . ?
N9 C26 H26B 110.8 . . ?
H26A C26 H26B 108.9 . . ?
N2 C7 C8 113.8(5) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C26 C25 N8 111.3(5) . . ?
C26 C25 H25A 109.4 . . ?
N8 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
N8 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C84 C85 C86 128.1(5) . . ?
C84 C85 H85 116.0 . . ?
C86 C85 H85 116.0 . . ?
C66 C67 C68 124.0(6) . . ?
C66 C67 H67 118.0 . . ?
C68 C67 H67 118.0 . . ?
C103 C104 C99 111.7(5) . . ?
C103 C104 B3 120.6(4) . . ?
C99 C104 B3 127.4(4) . . ?
C83 C82 C81 125.0(5) . . ?
C83 C82 H82 117.5 . . ?
C81 C82 H82 117.5 . . ?
C88 C87 C92 123.9(5) . . ?
C88 C87 H87 118.0 . . ?
C92 C87 H87 118.0 . . ?
C86 C81 C82 121.1(5) . . ?
C86 C81 H81 119.4 . . ?
C82 C81 H81 119.4 . . ?
C75 C80 C79 112.4(5) . . ?
C75 C80 B2 120.0(5) . . ?
C79 C80 B2 127.5(5) . . ?
C56 C51 C52 121.8(5) . . ?
C56 C51 H51 119.1 . . ?
C52 C51 H51 119.1 . . ?
C49 C50 C45 112.2(5) . . ?
C49 C50 B1 122.8(5) . . ?
C45 C50 B1 124.7(4) . . ?
C46 C45 C50 126.8(6) . . ?
C46 C45 H45 116.6 . . ?
C50 C45 H45 116.6 . . ?
C101 C102 C103 125.4(5) . . ?
C101 C102 H102 117.3 . . ?
C103 C102 H102 117.3 . . ?
C104 C103 C102 121.0(5) . . ?
C104 C103 H103 119.5 . . ?
C102 C103 H103 119.5 . . ?
C80 C79 C78 126.5(6) . . ?
C80 C79 H79 116.8 . . ?
C78 C79 H79 116.8 . . ?
C105 C110 C109 112.7(5) . . ?
C105 C110 B3 122.3(5) . . ?
C109 C110 B3 124.7(4) . . ?
C108 C109 C110 127.4(5) . . ?
C108 C109 H109 116.3 . . ?
C110 C109 H109 116.3 . . ?
C80 C75 C76 121.1(6) . . ?
C80 C75 H75 119.5 . . ?
C76 C75 H75 119.5 . . ?
C133 C132 C131 116.7(6) . . ?
C133 C132 H132 121.7 . . ?
C131 C132 H132 121.7 . . ?
C132 C133 C134 121.4(6) . . ?
C132 C133 H133 119.3 . . ?
C134 C133 H133 119.3 . . ?
C121 C122 C117 112.4(5) . . ?
C121 C122 B4 123.0(5) . . ?
C117 C122 B4 124.5(4) . . ?
C50 C49 C48 121.2(5) . . ?
C50 C49 H49 119.4 . . ?
C48 C49 H49 119.4 . . ?
C132 C131 C130 124.4(5) . . ?
C132 C131 H131 117.8 . . ?
C130 C131 H131 117.8 . . ?
C94 C93 C98 122.8(6) . . ?
C94 C93 H93 118.6 . . ?
C98 C93 H93 118.6 . . ?
C56 C55 C54 128.4(5) . . ?
C56 C55 H55 115.8 . . ?
C54 C55 H55 115.8 . . ?
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 . . ?
C128 C123 C124 125.1(5) . . ?
C128 C123 H123 117.4 . . ?
C124 C123 H123 117.4 . . ?
C93 C94 C95 116.1(6) . . ?
C93 C94 H94 121.9 . . ?
C95 C94 H94 121.9 . . ?
C47 C48 C49 125.1(6) . . ?
C47 C48 H48 117.5 . . ?
C49 C48 H48 117.5 . . ?
C90 C91 C92 118.4(5) . . ?
C90 C91 H91 120.8 . . ?
C92 C91 H91 120.8 . . ?
C125 C124 C123 123.8(5) . . ?
C125 C124 H124 118.1 . . ?
C123 C124 H124 118.1 . . ?
C119 C120 C121 124.3(6) . . ?
C119 C120 H120 117.9 . . ?
C121 C120 H120 117.9 . . ?
C57 C62 C61 117.6(5) . . ?
C57 C62 B1 117.3(5) . . ?
C61 C62 B1 124.6(5) . . ?
C89 C88 C87 116.1(6) . . ?
C89 C88 H88 122.0 . . ?
C87 C88 H88 122.0 . . ?
N10 C31 C32 177.8(7) . . ?
C122 C121 C120 121.1(6) . . ?
C122 C121 H121 119.4 . . ?
C120 C121 H121 119.4 . . ?
C44 C39 C40 118.1(5) . . ?
C44 C39 B1 118.7(5) . . ?
C40 C39 B1 122.9(5) . . ?
C110 C105 C106 120.7(7) . . ?
C110 C105 H105 119.7 . . ?
C106 C105 H105 119.7 . . ?
N5 C15 C16 178.2(11) . . ?
C129 C130 C131 117.8(6) . . ?
C129 C130 H130 121.1 . . ?
C131 C130 H130 121.1 . . ?
C128 C127 C126 127.7(5) . . ?
C128 C127 H127 116.2 . . ?
C126 C127 H127 116.2 . . ?
C104 C99 C100 127.0(5) . . ?
C104 C99 H99 116.5 . . ?
C100 C99 H99 116.5 . . ?
N6 C17 C18 179.2(8) . . ?
C91 C90 C89 121.5(5) . . ?
C91 C90 H90 119.2 . . ?
C89 C90 H90 119.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C129 C134 C133 119.4(4) . . ?
C129 C134 B4 118.4(5) . . ?
C133 C134 B4 121.5(5) . . ?
C130 C129 C134 120.3(6) . . ?
C130 C129 H129 119.8 . . ?
C134 C129 H129 119.8 . . ?
C125 C126 C127 122.3(5) . . ?
C125 C126 H126 118.8 . . ?
C127 C126 H126 118.8 . . ?
C118 C117 C122 126.2(5) . . ?
C118 C117 H117 116.9 . . ?
C122 C117 H117 116.9 . . ?
C119 C118 C117 119.0(6) . . ?
C119 C118 H118 120.5 . . ?
C117 C118 H118 120.5 . . ?
C126 C125 C124 112.9(6) . . ?
C126 C125 H125 123.6 . . ?
C124 C125 H125 123.6 . . ?
C69 C74 C73 118.4(5) . . ?
C69 C74 B2 118.5(5) . . ?
C73 C74 B2 122.7(4) . . ?
C100 C101 C102 117.3(6) . . ?
C100 C101 H101 121.4 . . ?
C102 C101 H101 121.4 . . ?
C66 C65 C64 121.6(5) . . ?
C66 C65 H65 119.2 . . ?
C64 C65 H65 119.2 . . ?
C41 C40 C39 122.8(7) . . ?
C41 C40 H40 118.6 . . ?
C39 C40 H40 118.6 . . ?
N1 C5 C4 118.4(8) . . ?
N1 C5 C6 115.9(6) . . ?
C4 C5 C6 125.5(8) . . ?
C83 C84 C85 118.0(5) . . ?
C83 C84 H84 121.0 . . ?
C85 C84 H84 121.0 . . ?
N12 C35 C36 177.1(6) . . ?
C78 C77 C76 117.3(6) . . ?
C78 C77 H77 121.3 . . ?
C76 C77 H77 121.3 . . ?
C107 C106 C105 124.8(6) . . ?
C107 C106 H106 117.6 . . ?
C105 C106 H106 117.6 . . ?
C65 C66 C67 116.6(6) . . ?
C65 C66 H66 121.7 . . ?
C67 C66 H66 121.7 . . ?
C88 C89 C90 121.8(5) . . ?
C88 C89 H89 119.1 . . ?
C90 C89 H89 119.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C115 C116 C111 115.5(5) . . ?
C115 C116 B4 117.6(5) . . ?
C111 C116 B4 126.9(5) . . ?
C118 C119 C120 116.9(6) . . ?
C118 C119 H119 121.5 . . ?
C120 C119 H119 121.5 . . ?
C77 C78 C79 117.7(6) . . ?
C77 C78 H78 121.2 . . ?
C79 C78 H78 121.2 . . ?
C53 C54 C55 118.1(6) . . ?
C53 C54 H54 120.9 . . ?
C55 C54 H54 120.9 . . ?
C70 C69 C74 118.9(6) . . ?
C70 C69 H69 120.5 . . ?
C74 C69 H69 120.5 . . ?
C63 C64 C65 121.0(6) . . ?
C63 C64 H64 119.5 . . ?
C65 C64 H64 119.5 . . ?
C60 C59 C58 122.0(6) . . ?
C60 C59 H59 119.0 . . ?
C58 C59 H59 119.0 . . ?
C108 C107 C106 117.4(6) . . ?
C108 C107 H107 121.3 . . ?
C106 C107 H107 121.3 . . ?
C116 C115 C114 119.8(6) . . ?
C116 C115 H115 120.1 . . ?
C114 C115 H115 120.1 . . ?
C72 C73 C74 123.4(6) . . ?
C72 C73 H73 118.3 . . ?
C74 C73 H73 118.3 . . ?
C40 C41 C42 117.3(8) . . ?
C40 C41 H41 121.4 . . ?
C42 C41 H41 121.4 . . ?
C62 C57 C58 119.3(6) . . ?
C62 C57 H57 120.4 . . ?
C58 C57 H57 120.4 . . ?
C68 C63 C64 119.9(5) . . ?
C68 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C77 C76 C75 125.1(6) . . ?
C77 C76 H76 117.5 . . ?
C75 C76 H76 117.5 . . ?
C53 C52 C51 125.1(6) . . ?
C53 C52 H52 117.4 . . ?
C51 C52 H52 117.4 . . ?
C59 C60 C61 116.1(7) . . ?
C59 C60 H60 122.0 . . ?
C61 C60 H60 122.0 . . ?
C107 C108 C109 117.0(7) . . ?
C107 C108 H108 121.5 . . ?
C109 C108 H108 121.5 . . ?
C112 C111 C116 125.6(6) . . ?
C112 C111 H111 117.2 . . ?
C116 C111 H111 117.2 . . ?
C101 C100 C99 117.4(6) . . ?
C101 C100 H100 121.3 . . ?
C99 C100 H100 121.3 . . ?
C84 C83 C82 116.0(5) . . ?
C84 C83 H83 122.0 . . ?
C82 C83 H83 122.0 . . ?
C46 C47 C48 116.0(6) . . ?
C46 C47 H47 122.0 . . ?
C48 C47 H47 122.0 . . ?
C60 C61 C62 124.0(6) . . ?
C60 C61 H61 118.0 . . ?
C62 C61 H61 118.0 . . ?
C94 C95 C96 122.8(6) . . ?
C94 C95 H95 118.6 . . ?
C96 C95 H95 118.6 . . ?
N11 C33 C34 178.2(7) . . ?
C72 C71 C70 122.8(6) . . ?
C72 C71 H71 118.6 . . ?
C70 C71 H71 118.6 . . ?
C57 C58 C59 121.1(6) . . ?
C57 C58 H58 119.4 . . ?
C59 C58 H58 119.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C54 C53 C52 116.0(6) . . ?
C54 C53 H53 122.0 . . ?
C52 C53 H53 122.0 . . ?
C2 C3 C4 120.6(8) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C43 C44 C39 119.5(7) . . ?
C43 C44 H44 120.3 . . ?
C39 C44 H44 120.3 . . ?
C97 C96 C95 121.1(6) . . ?
C97 C96 H96 119.4 . . ?
C95 C96 H96 119.4 . . ?
C113 C112 C111 116.7(7) . . ?
C113 C112 H112 121.7 . . ?
C111 C112 H112 121.7 . . ?
C11 C10 C9 111.3(6) . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C69 C70 C71 120.8(6) . . ?
C69 C70 H70 119.6 . . ?
C71 C70 H70 119.6 . . ?
C47 C46 C45 118.6(6) . . ?
C47 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
N7 C23 C22 118.2(7) . . ?
N7 C23 C24 120.5(6) . . ?
C22 C23 C24 120.8(6) . . ?
C41 C42 C43 123.1(7) . . ?
C41 C42 H42 118.5 . . ?
C43 C42 H42 118.5 . . ?
C73 C72 C71 115.6(7) . . ?
C73 C72 H72 122.2 . . ?
C71 C72 H72 122.2 . . ?
C96 C97 C98 119.1(6) . . ?
C96 C97 H97 120.5 . . ?
C98 C97 H97 120.5 . . ?
C112 C113 C114 119.8(6) . . ?
C112 C113 H113 120.1 . . ?
C114 C113 H113 120.1 . . ?
C3 C4 C5 120.5(9) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C1 C2 C3 115.5(9) . . ?
C1 C2 H2 122.2 . . ?
C3 C2 H2 122.2 . . ?
C20 C19 N7 123.2(7) . . ?
C20 C19 H19 118.4 . . ?
N7 C19 H19 118.4 . . ?
C2 C1 N1 126.5(8) . . ?
C2 C1 H1 116.8 . . ?
N1 C1 H1 116.8 . . ?
C115 C114 C113 122.7(6) . . ?
C115 C114 H114 118.6 . . ?
C113 C114 H114 118.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C23 C22 C21 116.3(7) . . ?
C23 C22 H22 121.8 . . ?
C21 C22 H22 121.8 . . ?
C20 C21 C22 126.9(8) . . ?
C20 C21 H21 116.5 . . ?
C22 C21 H21 116.5 . . ?
C21 C20 C19 113.3(8) . . ?
C21 C20 H20 123.3 . . ?
C19 C20 H20 123.3 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C44 C43 C42 119.3(8) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
N8 C24 C23 111.8(5) . . ?
N8 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
N8 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
C27 C28 C29 120.1(10) . . ?
C27 C28 H28A 107.3 . . ?
C29 C28 H28A 107.3 . . ?
C27 C28 H28B 107.3 . . ?
C29 C28 H28B 107.3 . . ?
H28A C28 H28B 106.9 . . ?
C28 C27 N8 108.3(9) . . ?
C28 C27 H27A 110.0 . . ?
N8 C27 H27A 110.0 . . ?
C28 C27 H27B 110.0 . . ?
N8 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N9 C30 H30A 109.5 . . ?
N9 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N9 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N13 C37 C38 178.4(11) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N1 Ni1 N2 86.6(2) . . ?
N1 Ni1 N5 95.3(2) . . ?
N2 Ni1 N5 177.5(2) . . ?
N1 Ni1 N6 84.46(18) . . ?
N2 Ni1 N6 94.33(19) . . ?
N5 Ni1 N6 87.6(2) . . ?
N1 Ni1 N4 91.76(19) . . ?
N2 Ni1 N4 100.80(18) . . ?
N5 Ni1 N4 77.46(19) . . ?
N6 Ni1 N4 164.2(2) . . ?
N1 Ni1 N3 159.0(2) . . ?
N2 Ni1 N3 72.62(19) . . ?
N5 Ni1 N3 105.6(2) . . ?
N6 Ni1 N3 93.93(19) . . ?
N4 Ni1 N3 95.01(19) . . ?
C134 B4 C116 102.6(4) . . ?
C134 B4 C122 109.5(4) . . ?
C116 B4 C122 111.2(4) . . ?
C134 B4 C128 111.2(4) . . ?
C116 B4 C128 109.2(4) . . ?
C122 B4 C128 112.6(4) . . ?
N7 Ni2 N9 158.2(2) . . ?
N7 Ni2 N10 93.63(19) . . ?
N9 Ni2 N10 88.3(2) . . ?
N7 Ni2 N8 86.1(2) . . ?
N9 Ni2 N8 72.2(2) . . ?
N10 Ni2 N8 88.2(2) . . ?
N7 Ni2 N11 95.0(2) . . ?
N9 Ni2 N11 106.8(2) . . ?
N10 Ni2 N11 88.8(2) . . ?
N8 Ni2 N11 176.8(2) . . ?
N7 Ni2 N12 80.71(18) . . ?
N9 Ni2 N12 100.3(2) . . ?
N10 Ni2 N12 169.3(2) . . ?
N8 Ni2 N12 100.5(2) . . ?
N11 Ni2 N12 82.64(19) . . ?
C98 B3 C92 110.8(4) . . ?
C98 B3 C104 111.1(4) . . ?
C92 B3 C104 104.6(4) . . ?
C98 B3 C110 103.9(4) . . ?
C92 B3 C110 110.1(4) . . ?
C104 B3 C110 116.4(4) . . ?
C23 N7 C19 121.9(6) . . ?
C23 N7 Ni2 110.7(5) . . ?
C19 N7 Ni2 126.8(4) . . ?
C74 B2 C68 109.2(4) . . ?
C74 B2 C80 112.0(4) . . ?
C68 B2 C80 105.5(4) . . ?
C74 B2 C86 103.8(4) . . ?
C68 B2 C86 112.0(4) . . ?
C80 B2 C86 114.4(4) . . ?
C39 B1 C62 109.4(4) . . ?
C39 B1 C56 106.2(4) . . ?
C62 B1 C56 111.1(4) . . ?
C39 B1 C50 110.4(4) . . ?
C62 B1 C50 104.9(4) . . ?
C56 B1 C50 114.8(4) . . ?

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
C12 N3 C8 C7 -160.0(6) . . . . ?
C11 N3 C8 C7 81.6(6) . . . . ?
Ni1 N3 C8 C7 -40.4(6) . . . . ?
C30 N9 C29 C28 -169.3(11) . . . . ?
C26 N9 C29 C28 -46.2(9) . . . . ?
Ni2 N9 C29 C28 69.4(9) . . . . ?
C6 N2 C9 C10 168.8(6) . . . . ?
C7 N2 C9 C10 41.6(7) . . . . ?
Ni1 N2 C9 C10 -74.6(6) . . . . ?
C7 N2 C6 C5 -140.9(7) . . . . ?
C9 N2 C6 C5 95.9(8) . . . . ?
Ni1 N2 C6 C5 -28.8(7) . . . . ?
C8 N3 C11 C10 -48.6(8) . . . . ?
C12 N3 C11 C10 -162.5(7) . . . . ?
Ni1 N3 C11 C10 68.3(7) . . . . ?
C30 N9 C26 C25 -159.9(7) . . . . ?
C29 N9 C26 C25 77.6(7) . . . . ?
Ni2 N9 C26 C25 -34.8(6) . . . . ?
C6 N2 C7 C8 151.8(6) . . . . ?
C9 N2 C7 C8 -82.7(6) . . . . ?
Ni1 N2 C7 C8 40.9(6) . . . . ?
N3 C8 C7 N2 0.6(8) . . . . ?
N9 C26 C25 N8 -3.4(7) . . . . ?
C27 N8 C25 C26 -87.9(8) . . . . ?
C24 N8 C25 C26 159.2(7) . . . . ?
Ni2 N8 C25 C26 40.2(7) . . . . ?
C81 C86 C85 C84 1.6(8) . . . . ?
B2 C86 C85 C84 -172.4(5) . . . . ?
C63 C68 C67 C66 2.4(9) . . . . ?
B2 C68 C67 C66 174.5(6) . . . . ?
C91 C92 C87 C88 0.0(9) . . . . ?
B3 C92 C87 C88 -171.1(6) . . . . ?
C85 C86 C81 C82 -2.1(7) . . . . ?
B2 C86 C81 C82 172.7(5) . . . . ?
C83 C82 C81 C86 1.2(9) . . . . ?
C55 C56 C51 C52 -1.2(7) . . . . ?
B1 C56 C51 C52 -177.3(5) . . . . ?
C49 C50 C45 C46 0.3(9) . . . . ?
B1 C50 C45 C46 174.7(6) . . . . ?
C99 C104 C103 C102 -3.5(7) . . . . ?
B3 C104 C103 C102 -178.4(4) . . . . ?
C101 C102 C103 C104 2.0(9) . . . . ?
C75 C80 C79 C78 -1.1(7) . . . . ?
B2 C80 C79 C78 -176.5(5) . . . . ?
C105 C110 C109 C108 1.1(8) . . . . ?
B3 C110 C109 C108 174.7(5) . . . . ?
C79 C80 C75 C76 0.8(7) . . . . ?
B2 C80 C75 C76 176.6(4) . . . . ?
C131 C132 C133 C134 0.0(8) . . . . ?
C45 C50 C49 C48 0.2(8) . . . . ?
B1 C50 C49 C48 -174.4(5) . . . . ?
C133 C132 C131 C130 0.9(9) . . . . ?
C97 C98 C93 C94 0.4(9) . . . . ?
B3 C98 C93 C94 -168.4(6) . . . . ?
C51 C56 C55 C54 1.6(8) . . . . ?
B1 C56 C55 C54 177.2(5) . . . . ?
C127 C128 C123 C124 0.7(8) . . . . ?
B4 C128 C123 C124 -173.4(5) . . . . ?
C98 C93 C94 C95 0.6(9) . . . . ?
C50 C49 C48 C47 -1.0(10) . . . . ?
C87 C92 C91 C90 -0.1(9) . . . . ?
B3 C92 C91 C90 171.5(5) . . . . ?
C128 C123 C124 C125 -1.1(10) . . . . ?
C92 C87 C88 C89 0.9(10) . . . . ?
C117 C122 C121 C120 1.7(7) . . . . ?
B4 C122 C121 C120 -178.3(5) . . . . ?
C119 C120 C121 C122 0.5(9) . . . . ?
C109 C110 C105 C106 -1.9(9) . . . . ?
B3 C110 C105 C106 -175.7(6) . . . . ?
C132 C131 C130 C129 -0.7(9) . . . . ?
C123 C128 C127 C126 -0.8(8) . . . . ?
B4 C128 C127 C126 172.8(5) . . . . ?
C103 C104 C99 C100 1.7(9) . . . . ?
B3 C104 C99 C100 176.2(6) . . . . ?
C92 C91 C90 C89 -0.6(10) . . . . ?
C132 C133 C134 C129 -1.0(8) . . . . ?
C132 C133 C134 B4 169.1(5) . . . . ?
C131 C130 C129 C134 -0.4(9) . . . . ?
C133 C134 C129 C130 1.2(8) . . . . ?
B4 C134 C129 C130 -169.3(5) . . . . ?
C128 C127 C126 C125 1.3(10) . . . . ?
C121 C122 C117 C118 -1.9(7) . . . . ?
B4 C122 C117 C118 178.1(4) . . . . ?
C122 C117 C118 C119 -0.3(7) . . . . ?
C127 C126 C125 C124 -1.4(9) . . . . ?
C123 C124 C125 C126 1.4(10) . . . . ?
C103 C102 C101 C100 2.1(10) . . . . ?
C44 C39 C40 C41 -1.3(10) . . . . ?
B1 C39 C40 C41 -174.5(6) . . . . ?
C1 N1 C5 C4 -1.5(9) . . . . ?
Ni1 N1 C5 C4 169.4(5) . . . . ?
C1 N1 C5 C6 174.0(6) . . . . ?
Ni1 N1 C5 C6 -15.2(7) . . . . ?
N2 C6 C5 N1 32.4(10) . . . . ?
N2 C6 C5 C4 -152.6(7) . . . . ?
C86 C85 C84 C83 0.0(9) . . . . ?
C110 C105 C106 C107 0.7(12) . . . . ?
C64 C65 C66 C67 -0.5(11) . . . . ?
C68 C67 C66 C65 -0.9(10) . . . . ?
C87 C88 C89 C90 -1.7(10) . . . . ?
C91 C90 C89 C88 1.6(11) . . . . ?
C117 C118 C119 C120 2.6(8) . . . . ?
C121 C120 C119 C118 -2.8(9) . . . . ?
C76 C77 C78 C79 0.4(9) . . . . ?
C80 C79 C78 C77 0.5(9) . . . . ?
C56 C55 C54 C53 -0.3(9) . . . . ?
C73 C74 C69 C70 1.1(9) . . . . ?
B2 C74 C69 C70 -172.2(6) . . . . ?
C66 C65 C64 C63 0.3(11) . . . . ?
C105 C106 C107 C108 1.6(12) . . . . ?
C111 C116 C115 C114 0.1(8) . . . . ?
B4 C116 C115 C114 179.1(5) . . . . ?
C69 C74 C73 C72 0.5(10) . . . . ?
B2 C74 C73 C72 173.5(6) . . . . ?
C39 C40 C41 C42 1.6(12) . . . . ?
C61 C62 C57 C58 2.1(9) . . . . ?
B1 C62 C57 C58 174.5(6) . . . . ?
C67 C68 C63 C64 -2.5(8) . . . . ?
B2 C68 C63 C64 -175.0(5) . . . . ?
C65 C64 C63 C68 1.3(10) . . . . ?
C78 C77 C76 C75 -0.7(9) . . . . ?
C80 C75 C76 C77 0.0(9) . . . . ?
C56 C51 C52 C53 -0.3(9) . . . . ?
C58 C59 C60 C61 0.3(11) . . . . ?
C106 C107 C108 C109 -2.4(9) . . . . ?
C110 C109 C108 C107 1.2(9) . . . . ?
C115 C116 C111 C112 0.0(10) . . . . ?
B4 C116 C111 C112 -179.0(6) . . . . ?
C102 C101 C100 C99 -3.7(10) . . . . ?
C104 C99 C100 C101 2.1(11) . . . . ?
C85 C84 C83 C82 -1.0(8) . . . . ?
C81 C82 C83 C84 0.5(9) . . . . ?
C49 C48 C47 C46 1.3(11) . . . . ?
C59 C60 C61 C62 1.3(11) . . . . ?
C57 C62 C61 C60 -2.6(10) . . . . ?
B1 C62 C61 C60 -174.4(6) . . . . ?
C93 C94 C95 C96 -2.6(10) . . . . ?
C62 C57 C58 C59 -0.6(11) . . . . ?
C60 C59 C58 C57 -0.7(12) . . . . ?
C55 C54 C53 C52 -1.2(9) . . . . ?
C51 C52 C53 C54 1.6(10) . . . . ?
C40 C39 C44 C43 0.8(10) . . . . ?
B1 C39 C44 C43 174.3(7) . . . . ?
C94 C95 C96 C97 3.8(12) . . . . ?
C116 C111 C112 C113 0.6(12) . . . . ?
N3 C11 C10 C9 -43.6(9) . . . . ?
N2 C9 C10 C11 43.8(8) . . . . ?
C74 C69 C70 C71 -2.1(10) . . . . ?
C72 C71 C70 C69 1.7(12) . . . . ?
C48 C47 C46 C45 -0.8(10) . . . . ?
C50 C45 C46 C47 0.1(11) . . . . ?
C40 C41 C42 C43 -1.6(14) . . . . ?
C74 C73 C72 C71 -1.0(11) . . . . ?
C70 C71 C72 C73 -0.1(12) . . . . ?
C95 C96 C97 C98 -2.6(11) . . . . ?
C93 C98 C97 C96 0.6(9) . . . . ?
B3 C98 C97 C96 169.8(6) . . . . ?
C111 C112 C113 C114 -1.1(11) . . . . ?
C2 C3 C4 C5 2.0(13) . . . . ?
N1 C5 C4 C3 0.0(11) . . . . ?
C6 C5 C4 C3 -175.0(8) . . . . ?
C4 C3 C2 C1 -2.2(13) . . . . ?
C3 C2 C1 N1 0.6(12) . . . . ?
C5 N1 C1 C2 1.3(10) . . . . ?
Ni1 N1 C1 C2 -167.4(6) . . . . ?
C116 C115 C114 C113 -0.6(10) . . . . ?
C112 C113 C114 C115 1.2(11) . . . . ?
N7 C23 C22 C21 -1.6(11) . . . . ?
C24 C23 C22 C21 -173.0(8) . . . . ?
C23 C22 C21 C20 -0.2(13) . . . . ?
C22 C21 C20 C19 0.7(13) . . . . ?
N7 C19 C20 C21 0.5(12) . . . . ?
C39 C44 C43 C42 -0.7(12) . . . . ?
C41 C42 C43 C44 1.1(14) . . . . ?
C27 N8 C24 C23 97.0(8) . . . . ?
C25 N8 C24 C23 -144.2(7) . . . . ?
Ni2 N8 C24 C23 -21.3(9) . . . . ?
N7 C23 C24 N8 25.8(12) . . . . ?
C22 C23 C24 N8 -163.0(7) . . . . ?
N9 C29 C28 C27 -48.8(12) . . . . ?
C29 C28 C27 N8 48.0(11) . . . . ?
C24 N8 C27 C28 170.8(8) . . . . ?
C25 N8 C27 C28 52.1(9) . . . . ?
Ni2 N8 C27 C28 -75.9(8) . . . . ?
C129 C134 B4 C116 85.1(6) . . . . ?
C133 C134 B4 C116 -85.1(6) . . . . ?
C129 C134 B4 C122 -156.6(5) . . . . ?
C133 C134 B4 C122 33.1(6) . . . . ?
C129 C134 B4 C128 -31.5(6) . . . . ?
C133 C134 B4 C128 158.2(4) . . . . ?
C115 C116 B4 C134 154.7(5) . . . . ?
C111 C116 B4 C134 -26.4(7) . . . . ?
C115 C116 B4 C122 37.7(6) . . . . ?
C111 C116 B4 C122 -143.4(5) . . . . ?
C115 C116 B4 C128 -87.3(6) . . . . ?
C111 C116 B4 C128 91.7(6) . . . . ?
C121 C122 B4 C134 111.9(5) . . . . ?
C117 C122 B4 C134 -68.1(6) . . . . ?
C121 C122 B4 C116 -135.5(5) . . . . ?
C117 C122 B4 C116 44.6(6) . . . . ?
C121 C122 B4 C128 -12.4(6) . . . . ?
C117 C122 B4 C128 167.6(4) . . . . ?
C123 C128 B4 C134 -52.8(7) . . . . ?
C127 C128 B4 C134 134.5(5) . . . . ?
C123 C128 B4 C116 -165.3(5) . . . . ?
C127 C128 B4 C116 21.9(7) . . . . ?
C123 C128 B4 C122 70.6(6) . . . . ?
C127 C128 B4 C122 -102.2(6) . . . . ?
C97 C98 B3 C92 152.4(5) . . . . ?
C93 C98 B3 C92 -39.0(7) . . . . ?
C97 C98 B3 C104 36.5(7) . . . . ?
C93 C98 B3 C104 -154.8(5) . . . . ?
C97 C98 B3 C110 -89.4(6) . . . . ?
C93 C98 B3 C110 79.3(6) . . . . ?
C91 C92 B3 C98 153.1(5) . . . . ?
C87 C92 B3 C98 -35.8(7) . . . . ?
C91 C92 B3 C104 -87.2(5) . . . . ?
C87 C92 B3 C104 83.9(6) . . . . ?
C91 C92 B3 C110 38.7(6) . . . . ?
C87 C92 B3 C110 -150.2(5) . . . . ?
C103 C104 B3 C98 -156.5(5) . . . . ?
C99 C104 B3 C98 29.5(7) . . . . ?
C103 C104 B3 C92 83.9(5) . . . . ?
C99 C104 B3 C92 -90.1(6) . . . . ?
C103 C104 B3 C110 -37.9(6) . . . . ?
C99 C104 B3 C110 148.1(5) . . . . ?
C105 C110 B3 C98 99.5(6) . . . . ?
C109 C110 B3 C98 -73.5(6) . . . . ?
C105 C110 B3 C92 -141.8(5) . . . . ?
C109 C110 B3 C92 45.2(6) . . . . ?
C105 C110 B3 C104 -23.0(7) . . . . ?
C109 C110 B3 C104 164.0(4) . . . . ?
C22 C23 N7 C19 2.9(10) . . . . ?
C24 C23 N7 C19 174.3(7) . . . . ?
C22 C23 N7 Ni2 174.5(5) . . . . ?
C24 C23 N7 Ni2 -14.1(8) . . . . ?
C20 C19 N7 C23 -2.4(11) . . . . ?
C20 C19 N7 Ni2 -172.6(6) . . . . ?
C69 C74 B2 C68 -151.0(5) . . . . ?
C73 C74 B2 C68 35.9(7) . . . . ?
C69 C74 B2 C80 -34.6(7) . . . . ?
C73 C74 B2 C80 152.4(5) . . . . ?
C69 C74 B2 C86 89.4(5) . . . . ?
C73 C74 B2 C86 -83.6(6) . . . . ?
C63 C68 B2 C74 -154.2(5) . . . . ?
C67 C68 B2 C74 33.9(7) . . . . ?
C63 C68 B2 C80 85.3(6) . . . . ?
C67 C68 B2 C80 -86.6(6) . . . . ?
C63 C68 B2 C86 -39.8(6) . . . . ?
C67 C68 B2 C86 148.3(5) . . . . ?
C75 C80 B2 C74 151.1(5) . . . . ?
C79 C80 B2 C74 -33.8(7) . . . . ?
C75 C80 B2 C68 -90.2(5) . . . . ?
C79 C80 B2 C68 84.9(6) . . . . ?
C75 C80 B2 C86 33.3(6) . . . . ?
C79 C80 B2 C86 -151.6(5) . . . . ?
C81 C86 B2 C74 -79.3(5) . . . . ?
C85 C86 B2 C74 94.4(5) . . . . ?
C81 C86 B2 C68 163.0(5) . . . . ?
C85 C86 B2 C68 -23.3(7) . . . . ?
C81 C86 B2 C80 43.0(6) . . . . ?
C85 C86 B2 C80 -143.3(5) . . . . ?
C44 C39 B1 C62 146.8(6) . . . . ?
C40 C39 B1 C62 -40.0(7) . . . . ?
C44 C39 B1 C56 -93.2(6) . . . . ?
C40 C39 B1 C56 80.0(6) . . . . ?
C44 C39 B1 C50 31.8(7) . . . . ?
C40 C39 B1 C50 -155.0(5) . . . . ?
C57 C62 B1 C39 161.4(5) . . . . ?
C61 C62 B1 C39 -26.8(7) . . . . ?
C57 C62 B1 C56 44.4(7) . . . . ?
C61 C62 B1 C56 -143.8(5) . . . . ?
C57 C62 B1 C50 -80.2(6) . . . . ?
C61 C62 B1 C50 91.6(6) . . . . ?
C51 C56 B1 C39 78.0(6) . . . . ?
C55 C56 B1 C39 -97.3(6) . . . . ?
C51 C56 B1 C62 -163.1(5) . . . . ?
C55 C56 B1 C62 21.7(7) . . . . ?
C51 C56 B1 C50 -44.3(6) . . . . ?
C55 C56 B1 C50 140.4(5) . . . . ?
C49 C50 B1 C39 -140.8(5) . . . . ?
C45 C50 B1 C39 45.3(6) . . . . ?
C49 C50 B1 C62 101.4(5) . . . . ?
C45 C50 B1 C62 -72.4(6) . . . . ?
C49 C50 B1 C56 -20.8(6) . . . . ?
C45 C50 B1 C56 165.4(5) . . . . ?

_refine_diff_density_max         1.104
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.066

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MU4a
_database_code_depnum_ccdc_archive 'CCDC 1975594'
loop_
_audit_author_name
_audit_author_address
'marappan velusamy'
;North Eastern Hill University
India
;
_audit_update_record             
;
2021-04-23 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;

_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_chemical_name_systematic        
"(mu2-carbonatato)-diaqua-bis(1-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-4-methyl-1,4-diazepane-N,N',N")-di-nickel(II) diperchlorate acetone solvate dihydrate"
_chemical_name_common            
"(mu2-carbonatato)-diaqua-bis(1-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-4-methyl-1,4-diazepane-N,N',N")-di-nickel(II) diperchlorate acetone solvate dihydrate"
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H54 N6 Ni2 O7, 2(Cl O4), C3 H6 O, 2(H2 O)'
_chemical_formula_sum            'C34 H64 Cl2 N6 Ni2 O18'
_chemical_formula_weight         1033.23

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.7462(7)
_cell_length_b                   15.1861(9)
_cell_length_c                   25.9560(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4630.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    290.9(4)
_cell_measurement_reflns_used    3853
_cell_measurement_theta_min      3.985
_cell_measurement_theta_max      28.570

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_F_000             2176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.005
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      290.9(4)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 8.0640
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  23.00   0.50    3.40    --  -17.74 -99.00 120.00   96
  2  ω    -49.00  50.00   0.50    3.40    --   20.09 -77.00-150.00  198
;

_diffrn_reflns_number            13024
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.414
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 0.899
_reflns_number_total             9085
_reflns_number_gt                7600
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_max     0.793
_reflns_Friedel_fraction_full    0.793

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 
 The non-hydrogen atoms of the metal complex, the acetone solvate molecule,
 and of the two hydrate molecules were refined with anisotropic displacement
 parameters without any constraints.

 One of the two perchlorate anions was disordered over two orientations which
 refined to site occupation factors of 0.697(11) and 0.303(11), respectively.
 In this disordered anion the C-Cl bonds were restrained to have the same
 lengths (DFIX of SHELXL) and the same anisotropic displacement parameters
 were used for equivalent atoms (EADP of SHELXL). Rigid bond restraints were
 applied for the perchlorate anions (RIGU of SHELXL).

 The position of the H atoms of the aqua ligands and of the hydrate molecules
 were taken from a difference Fourier map, the O-H distances were fixed to
 0.84 Å (DFIX of SHELXL), and the distances between the H atoms of the
 hydrate molecules were restrained to 1.40 Å (DFIX of SHELXL). The H atoms
 of the aqua ligands were refined without any constraints to the bond angles.
 These H atoms were refined with a common isotropic displacement parameter
 for the atoms of the aqua ligands, and an other one for the hydrate
 molecules. 

 The H atoms of the pyridine rings and of the CH₂  were included with
 idealized geometries and their isotropic displacement parameters fixed
 to 1.2 times Ueq of the C atom they are bonded to
 (AFIX 43 and AFIX 23 of SHELXL).

 The H atoms of the methyl groups were included with their isotropic
 displacement parameters fixed to 1.5 times Ueq of the C atom they are
 bonded to and and idealized geometries with tetrahedral angles, enabling
 rotations around the X-C bonds, and C-H distances of 0.98 Å
 (AFIX 137 of SHELXL).
;

# start Validation Reply Form
_vrf_PLAT003_MU4a                
;
PROBLEM: Number of Uiso or Uij Restrained non-H Atoms ...... 10 Report
RESPONSE:
 The non-hydrogen atoms of the metal complex, the acetone solvate molecule,
 and of the two hydrate molecules were refined with anisotropic displacement
 parameters without any constraints.
 One of the two perchlorate anions was disordered over two orientations which
 refined to site occupation factors of 0.697(11) and 0.303(11), respectively.
 In this disordered anion the C-Cl bonds were restrained to have the same
 lengths (DFIX of SHELXL) and the same anisotropic displacement parameters
 were used for equivalent atoms (EADP of SHELXL). Rigid bond restraints were
 applied for the perchlorate anions (RIGU of SHELXL).
;
_vrf_PLAT171_MU4a                
;
PROBLEM: The CIF-Embedded .res File Contains EADP Records ....... 5 Report
RESPONSE: see above.
;
_vrf_PLAT172_MU4a                
;
PROBLEM: The CIF-Embedded .res File Contains DFIX Records ....... 4 Report
RESPONSE: see above and the following:
 The position of the H atoms of the aqua ligands and of the hydrate molecules
 were taken from a difference Fourier map, the O-H distances were fixed to
 0.84A (DFIX of SHELXL), and the distances between the H atoms of the
 hydrate molecules were restrained to 1.40A (DFIX of SHELXL).
;
_vrf_PLAT187_MU4a                
;
PROBLEM: The CIF-Embedded .res File Contains RIGU Records ....... 1 Report
RESPONSE:
Rigid bond restraints were applied for the perchlorate anions.
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0636P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2513 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         9085
_refine_ls_number_parameters     612
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.26579(5) 0.65047(4) 0.42049(3) 0.02735(17) Uani 1 1 d . . . . .
Ni2 Ni 0.62927(5) 0.59765(4) 0.45958(3) 0.02986(18) Uani 1 1 d . . . . .
C31 C 0.4481(4) 0.6832(3) 0.4672(2) 0.0264(11) Uani 1 1 d . . . . .
O1 O 0.4485(3) 0.6165(2) 0.43646(15) 0.0293(8) Uani 1 1 d . . . . .
O2 O 0.5427(3) 0.7060(2) 0.48721(15) 0.0331(9) Uani 1 1 d . . . . .
O3 O 0.3528(3) 0.7208(2) 0.47571(15) 0.0329(9) Uani 1 1 d . . . . .
N1 N 0.3236(4) 0.7199(3) 0.35761(19) 0.0320(11) Uani 1 1 d . . . . .
C1 C 0.3916(5) 0.7902(4) 0.3584(2) 0.0380(13) Uani 1 1 d . . . . .
H1 H 0.4103 0.8145 0.3902 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4354(6) 0.8286(4) 0.3150(3) 0.0441(15) Uani 1 1 d . . . . .
C3 C 0.4046(6) 0.7929(5) 0.2679(2) 0.0495(17) Uani 1 1 d . . . . .
C4 C 0.3299(6) 0.7212(5) 0.2657(2) 0.0463(16) Uani 1 1 d . . . . .
C5 C 0.2910(5) 0.6877(4) 0.3121(2) 0.0365(13) Uani 1 1 d . . . . .
C6 C 0.5118(7) 0.9090(5) 0.3190(3) 0.069(2) Uani 1 1 d . . . . .
H61 H 0.5169 0.9272 0.3544 0.104 Uiso 1 1 calc R U . . .
H62 H 0.4803 0.9561 0.2988 0.104 Uiso 1 1 calc R U . . .
H63 H 0.5864 0.8948 0.3064 0.104 Uiso 1 1 calc R U . . .
C7 C 0.2900(8) 0.6854(7) 0.2146(3) 0.083(3) Uani 1 1 d . . . . .
H701 H 0.3281 0.6308 0.2076 0.125 Uiso 1 1 calc R U . . .
H702 H 0.3070 0.7270 0.1879 0.125 Uiso 1 1 calc R U . . .
H703 H 0.2093 0.6755 0.2159 0.125 Uiso 1 1 calc R U . . .
O4 O 0.4435(5) 0.8284(4) 0.2232(2) 0.0710(16) Uani 1 1 d . . . . .
C8 C 0.5479(9) 0.7971(9) 0.2073(4) 0.100(4) Uani 1 1 d . . . . .
H801 H 0.6027 0.8054 0.2343 0.151 Uiso 1 1 calc R U . . .
H802 H 0.5718 0.8287 0.1772 0.151 Uiso 1 1 calc R U . . .
H803 H 0.5418 0.7356 0.1994 0.151 Uiso 1 1 calc R U . . .
C9 C 0.2054(6) 0.6143(4) 0.3144(2) 0.0439(15) Uani 1 1 d . . . . .
H901 H 0.1298 0.6385 0.3093 0.053 Uiso 1 1 calc R U . . .
H902 H 0.2201 0.5733 0.2865 0.053 Uiso 1 1 calc R U . . .
N2 N 0.2085(4) 0.5664(3) 0.36356(19) 0.0316(10) Uani 1 1 d . . . . .
C10 C 0.0944(5) 0.5356(5) 0.3799(2) 0.0426(15) Uani 1 1 d . . . . .
H101 H 0.0779 0.4794 0.3637 0.051 Uiso 1 1 calc R U . . .
H102 H 0.0372 0.5775 0.3688 0.051 Uiso 1 1 calc R U . . .
C11 C 0.0892(5) 0.5253(4) 0.4389(2) 0.0402(14) Uani 1 1 d . . . . .
H111 H 0.0307 0.5639 0.4525 0.048 Uiso 1 1 calc R U . . .
H112 H 0.0682 0.4652 0.4473 0.048 Uiso 1 1 calc R U . . .
N3 N 0.1987(4) 0.5463(3) 0.4639(2) 0.0355(11) Uani 1 1 d . . . . .
C12 C 0.2906(5) 0.4925(4) 0.3616(3) 0.0411(15) Uani 1 1 d . . . . .
H121 H 0.3673 0.5162 0.3612 0.049 Uiso 1 1 calc R U . . .
H122 H 0.2794 0.4601 0.3298 0.049 Uiso 1 1 calc R U . . .
C13 C 0.2791(5) 0.4296(4) 0.4067(3) 0.0465(16) Uani 1 1 d . . . . .
H131 H 0.2101 0.3955 0.4017 0.056 Uiso 1 1 calc R U . . .
H132 H 0.3425 0.3888 0.4055 0.056 Uiso 1 1 calc R U . . .
C14 C 0.2751(5) 0.4692(4) 0.4598(3) 0.0422(14) Uani 1 1 d . . . . .
H141 H 0.2500 0.4245 0.4840 0.051 Uiso 1 1 calc R U . . .
H142 H 0.3514 0.4869 0.4696 0.051 Uiso 1 1 calc R U . . .
C15 C 0.1795(6) 0.5685(5) 0.5184(3) 0.0508(17) Uani 1 1 d . . . . .
H151 H 0.1411 0.5205 0.5351 0.076 Uiso 1 1 calc R U . . .
H152 H 0.1334 0.6206 0.5206 0.076 Uiso 1 1 calc R U . . .
H153 H 0.2513 0.5788 0.5350 0.076 Uiso 1 1 calc R U . . .
O5 O 0.1148(3) 0.7191(2) 0.42393(11) 0.0424(10) Uani 1 1 d D . . . .
H51 H 0.0998(17) 0.7394(8) 0.45324(18) 0.050(10) Uiso 1 1 d D U . . .
H52 H 0.111(5) 0.7523(4) 0.3981(2) 0.050(10) Uiso 1 1 d D U . . .
N4 N 0.5723(4) 0.5126(3) 0.51525(19) 0.0332(11) Uani 1 1 d . . . . .
C16 C 0.4994(5) 0.5299(4) 0.5524(2) 0.0396(14) Uani 1 1 d . . . . .
H16 H 0.4739 0.5876 0.5556 0.048 Uiso 1 1 calc R U . . .
C17 C 0.4577(6) 0.4685(5) 0.5870(3) 0.0476(16) Uani 1 1 d . . . . .
C18 C 0.5042(6) 0.3853(4) 0.5828(3) 0.0516(17) Uani 1 1 d . . . . .
C19 C 0.5872(6) 0.3650(4) 0.5473(3) 0.0472(16) Uani 1 1 d . . . . .
C20 C 0.6148(5) 0.4308(4) 0.5112(3) 0.0368(14) Uani 1 1 d . . . . .
C21 C 0.3691(7) 0.4923(5) 0.6258(3) 0.063(2) Uani 1 1 d . . . . .
H211 H 0.2992 0.4627 0.6176 0.095 Uiso 1 1 calc R U . . .
H212 H 0.3571 0.5548 0.6253 0.095 Uiso 1 1 calc R U . . .
H213 H 0.3941 0.4746 0.6595 0.095 Uiso 1 1 calc R U . . .
C22 C 0.6489(7) 0.2795(4) 0.5475(4) 0.071(2) Uani 1 1 d . . . . .
H221 H 0.6405 0.2519 0.5806 0.106 Uiso 1 1 calc R U . . .
H222 H 0.7281 0.2895 0.5407 0.106 Uiso 1 1 calc R U . . .
H223 H 0.6178 0.2418 0.5213 0.106 Uiso 1 1 calc R U . . .
O6 O 0.4695(6) 0.3237(4) 0.6186(2) 0.0818(19) Uani 1 1 d . . . . .
C23 C 0.4008(9) 0.2538(6) 0.5992(4) 0.097(3) Uani 1 1 d . . . . .
H231 H 0.3223 0.2712 0.5997 0.145 Uiso 1 1 calc R U . . .
H232 H 0.4110 0.2025 0.6202 0.145 Uiso 1 1 calc R U . . .
H233 H 0.4231 0.2407 0.5644 0.145 Uiso 1 1 calc R U . . .
C24 C 0.6990(5) 0.4153(4) 0.4685(3) 0.0442(16) Uani 1 1 d . . . . .
H241 H 0.7754 0.4155 0.4827 0.053 Uiso 1 1 calc R U . . .
H242 H 0.6856 0.3576 0.4536 0.053 Uiso 1 1 calc R U . . .
N5 N 0.6917(4) 0.4826(3) 0.4272(2) 0.0377(12) Uani 1 1 d . . . . .
C25 C 0.8047(5) 0.5039(4) 0.4052(3) 0.0517(19) Uani 1 1 d . . . . .
H251 H 0.8227 0.4623 0.3780 0.062 Uiso 1 1 calc R U . . .
H252 H 0.8623 0.4984 0.4318 0.062 Uiso 1 1 calc R U . . .
C26 C 0.8063(5) 0.5980(5) 0.3834(3) 0.0471(16) Uani 1 1 d . . . . .
H261 H 0.8638 0.6322 0.4012 0.056 Uiso 1 1 calc R U . . .
H262 H 0.8268 0.5959 0.3472 0.056 Uiso 1 1 calc R U . . .
N6 N 0.6951(4) 0.6419(3) 0.3888(2) 0.0382(11) Uani 1 1 d . . . . .
C27 C 0.6109(5) 0.4569(4) 0.3868(3) 0.0462(16) Uani 1 1 d . . . . .
H271 H 0.5341 0.4612 0.4004 0.055 Uiso 1 1 calc R U . . .
H272 H 0.6244 0.3959 0.3776 0.055 Uiso 1 1 calc R U . . .
C28 C 0.6198(6) 0.5134(5) 0.3386(3) 0.0510(17) Uani 1 1 d . . . . .
H281 H 0.5567 0.4985 0.3161 0.061 Uiso 1 1 calc R U . . .
H282 H 0.6894 0.4975 0.3207 0.061 Uiso 1 1 calc R U . . .
C29 C 0.6197(5) 0.6132(4) 0.3465(3) 0.0467(16) Uani 1 1 d . . . . .
H291 H 0.6437 0.6416 0.3149 0.056 Uiso 1 1 calc R U . . .
H292 H 0.5426 0.6324 0.3539 0.056 Uiso 1 1 calc R U . . .
C30 C 0.7087(6) 0.7390(4) 0.3857(3) 0.0568(19) Uani 1 1 d . . . . .
H301 H 0.7420 0.7544 0.3531 0.085 Uiso 1 1 calc R U . . .
H302 H 0.7574 0.7588 0.4131 0.085 Uiso 1 1 calc R U . . .
H303 H 0.6355 0.7667 0.3888 0.085 Uiso 1 1 calc R U . . .
O7 O 0.7803(3) 0.6210(2) 0.49582(13) 0.0445(10) Uani 1 1 d D . . . .
H71 H 0.7953(17) 0.5974(7) 0.52429(19) 0.050(10) Uiso 1 1 d D U . . .
H72 H 0.8026(11) 0.6718(3) 0.5038(6) 0.050(10) Uiso 1 1 d D U . . .
O8 O 0.8336(4) 0.5248(2) 0.57619(15) 0.088(2) Uani 1 1 d D . . . .
H81 H 0.7977(7) 0.529(2) 0.60405(19) 0.113(19) Uiso 1 1 d D U . . .
H82 H 0.8686(7) 0.4768(3) 0.5733(13) 0.113(19) Uiso 1 1 d D U . . .
O9 O 0.5835(3) 0.6676(3) 0.65196(16) 0.0891(19) Uani 1 1 d D . . . .
H91 H 0.5378(6) 0.6726(19) 0.6767(2) 0.113(19) Uiso 1 1 d D U . . .
H92 H 0.6329(5) 0.6285(4) 0.6568(9) 0.113(19) Uiso 1 1 d D U . . .
O10 O 0.7177(7) 0.5195(5) 0.6667(4) 0.113(3) Uani 1 1 d . . . . .
C32 C 0.6918(8) 0.4520(7) 0.6883(4) 0.079(3) Uani 1 1 d . . . . .
C33 C 0.7448(8) 0.3769(5) 0.6783(4) 0.085(3) Uani 1 1 d . . . . .
H331 H 0.7757 0.3788 0.6441 0.128 Uiso 1 1 calc R U . . .
H332 H 0.6918 0.3290 0.6810 0.128 Uiso 1 1 calc R U . . .
H333 H 0.8053 0.3685 0.7027 0.128 Uiso 1 1 calc R U . . .
C34 C 0.5994(10) 0.4462(8) 0.7265(4) 0.105(4) Uani 1 1 d . . . . .
H341 H 0.5667 0.5035 0.7315 0.157 Uiso 1 1 calc R U . . .
H342 H 0.6293 0.4249 0.7585 0.157 Uiso 1 1 calc R U . . .
H343 H 0.5419 0.4065 0.7142 0.157 Uiso 1 1 calc R U . . .
Cl1 Cl 0.50934(18) 0.17230(14) 0.42790(9) 0.0699(6) Uani 1 1 d . U . . .
O11 O 0.4752(9) 0.2589(5) 0.4306(5) 0.156(4) Uani 1 1 d . U . . .
O12 O 0.4764(7) 0.1261(5) 0.4727(3) 0.104(2) Uani 1 1 d . U . . .
O13 O 0.4657(10) 0.1298(7) 0.3849(4) 0.159(4) Uani 1 1 d . U . . .
O14 O 0.6265(7) 0.1738(8) 0.4239(4) 0.150(3) Uani 1 1 d . U . . .
Cl2 Cl 0.8957(8) 0.8388(5) 0.2330(3) 0.0881(14) Uani 0.697(11) 1 d D U P A 1
O21 O 0.9095(14) 0.7718(8) 0.2701(5) 0.154(6) Uani 0.697(11) 1 d D U P A 1
O22 O 1.0059(10) 0.8663(10) 0.2181(6) 0.170(6) Uani 0.697(11) 1 d D U P A 1
O23 O 0.8356(13) 0.9104(9) 0.2529(6) 0.162(6) Uani 0.697(11) 1 d D U P A 1
O24 O 0.8386(14) 0.8053(11) 0.1895(5) 0.108(4) Uani 0.697(11) 1 d D U P A 1
Cl3 Cl 0.8919(18) 0.8213(13) 0.2398(8) 0.0881(14) Uani 0.303(11) 1 d D . P A 2
O31 O 0.811(2) 0.769(2) 0.2660(11) 0.154(6) Uani 0.303(11) 1 d D . P A 2
O32 O 1.001(2) 0.785(2) 0.2471(14) 0.170(6) Uani 0.303(11) 1 d D . P A 2
O33 O 0.890(3) 0.9078(15) 0.2589(15) 0.162(6) Uani 0.303(11) 1 d D . P A 2
O34 O 0.866(4) 0.823(3) 0.1868(9) 0.108(4) Uani 0.303(11) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N1 2.058(5) . ?
Ni1 O5 2.059(4) . ?
Ni1 O3 2.059(4) . ?
Ni1 N2 2.066(5) . ?
Ni1 N3 2.095(5) . ?
Ni1 O1 2.246(3) . ?
Ni1 C31 2.510(5) . ?
Ni2 O7 2.039(4) . ?
Ni2 N4 2.050(5) . ?
Ni2 O2 2.063(4) . ?
Ni2 N5 2.073(5) . ?
Ni2 N6 2.103(5) . ?
Ni2 O1 2.225(4) . ?
Ni2 C31 2.501(5) . ?
C31 O2 1.275(6) . ?
C31 O3 1.276(6) . ?
C31 O1 1.289(6) . ?
N1 C1 1.334(8) . ?
N1 C5 1.334(7) . ?
C1 C2 1.369(9) . ?
C1 H1 0.93 . ?
C2 C3 1.385(9) . ?
C2 C6 1.520(10) . ?
C3 O4 1.359(8) . ?
C3 C4 1.399(10) . ?
C4 C5 1.385(8) . ?
C4 C7 1.508(10) . ?
C5 C9 1.503(9) . ?
C6 H61 0.96 . ?
C6 H62 0.96 . ?
C6 H63 0.96 . ?
C7 H701 0.96 . ?
C7 H702 0.96 . ?
C7 H703 0.96 . ?
O4 C8 1.378(11) . ?
C8 H801 0.96 . ?
C8 H802 0.96 . ?
C8 H803 0.96 . ?
C9 N2 1.470(8) . ?
C9 H901 0.97 . ?
C9 H902 0.97 . ?
N2 C12 1.481(7) . ?
N2 C10 1.482(7) . ?
C10 C11 1.541(9) . ?
C10 H101 0.97 . ?
C10 H102 0.97 . ?
C11 N3 1.474(7) . ?
C11 H111 0.97 . ?
C11 H112 0.97 . ?
N3 C15 1.472(9) . ?
N3 C14 1.480(7) . ?
C12 C13 1.517(9) . ?
C12 H121 0.97 . ?
C12 H122 0.97 . ?
C13 C14 1.505(9) . ?
C13 H131 0.97 . ?
C13 H132 0.97 . ?
C14 H141 0.97 . ?
C14 H142 0.97 . ?
C15 H151 0.96 . ?
C15 H152 0.96 . ?
C15 H153 0.96 . ?
O5 H51 0.84 . ?
O5 H52 0.84 . ?
N4 C16 1.315(8) . ?
N4 C20 1.344(7) . ?
C16 C17 1.386(9) . ?
C16 H16 0.93 . ?
C17 C18 1.380(10) . ?
C17 C21 1.492(10) . ?
C18 C19 1.377(11) . ?
C18 O6 1.380(8) . ?
C19 C20 1.408(9) . ?
C19 C22 1.487(9) . ?
C20 C24 1.505(9) . ?
C21 H211 0.96 . ?
C21 H212 0.96 . ?
C21 H213 0.96 . ?
C22 H221 0.96 . ?
C22 H222 0.96 . ?
C22 H223 0.96 . ?
O6 C23 1.426(10) . ?
C23 H231 0.96 . ?
C23 H232 0.96 . ?
C23 H233 0.96 . ?
C24 N5 1.484(8) . ?
C24 H241 0.97 . ?
C24 H242 0.97 . ?
N5 C27 1.466(8) . ?
N5 C25 1.480(8) . ?
C25 C26 1.538(10) . ?
C25 H251 0.97 . ?
C25 H252 0.97 . ?
C26 N6 1.472(7) . ?
C26 H261 0.97 . ?
C26 H262 0.97 . ?
N6 C29 1.476(8) . ?
N6 C30 1.486(8) . ?
C27 C28 1.521(10) . ?
C27 H271 0.97 . ?
C27 H272 0.97 . ?
C28 C29 1.530(10) . ?
C28 H281 0.97 . ?
C28 H282 0.97 . ?
C29 H291 0.97 . ?
C29 H292 0.97 . ?
C30 H301 0.96 . ?
C30 H302 0.96 . ?
C30 H303 0.96 . ?
O7 H71 0.84 . ?
O7 H72 0.84 . ?
O8 H81 0.84 . ?
O8 H82 0.84 . ?
O9 H91 0.84 . ?
O9 H92 0.84 . ?
O10 C32 1.208(11) . ?
C32 C33 1.324(12) . ?
C32 C34 1.471(14) . ?
C33 H331 0.96 . ?
C33 H332 0.96 . ?
C33 H333 0.96 . ?
C34 H341 0.96 . ?
C34 H342 0.96 . ?
C34 H343 0.96 . ?
Cl1 O11 1.377(8) . ?
Cl1 O14 1.380(8) . ?
Cl1 O13 1.386(9) . ?
Cl1 O12 1.413(7) . ?
Cl2 O23 1.397(7) . ?
Cl2 O24 1.408(7) . ?
Cl2 O21 1.411(8) . ?
Cl2 O22 1.413(8) . ?
Cl3 O33 1.405(8) . ?
Cl3 O31 1.406(8) . ?
Cl3 O32 1.407(8) . ?
Cl3 O34 1.408(8) . ?

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
N1 Ni1 O5 93.41(16) . . ?
N1 Ni1 O3 97.04(17) . . ?
O5 Ni1 O3 97.76(14) . . ?
N1 Ni1 N2 81.8(2) . . ?
O5 Ni1 N2 93.62(16) . . ?
O3 Ni1 N2 168.61(16) . . ?
N1 Ni1 N3 159.5(2) . . ?
O5 Ni1 N3 91.99(16) . . ?
O3 Ni1 N3 101.78(18) . . ?
N2 Ni1 N3 78.2(2) . . ?
N1 Ni1 O1 87.06(16) . . ?
O5 Ni1 O1 158.66(14) . . ?
O3 Ni1 O1 61.07(13) . . ?
N2 Ni1 O1 107.54(15) . . ?
N3 Ni1 O1 94.98(16) . . ?
N1 Ni1 C31 90.00(18) . . ?
O5 Ni1 C31 127.87(15) . . ?
O3 Ni1 C31 30.44(15) . . ?
N2 Ni1 C31 138.21(17) . . ?
N3 Ni1 C31 102.17(18) . . ?
O1 Ni1 C31 30.81(14) . . ?
O7 Ni2 N4 93.94(16) . . ?
O7 Ni2 O2 97.45(14) . . ?
N4 Ni2 O2 95.53(17) . . ?
O7 Ni2 N5 91.50(16) . . ?
N4 Ni2 N5 82.6(2) . . ?
O2 Ni2 N5 170.97(16) . . ?
O7 Ni2 N6 91.55(17) . . ?
N4 Ni2 N6 159.5(2) . . ?
O2 Ni2 N6 103.31(18) . . ?
N5 Ni2 N6 77.5(2) . . ?
O7 Ni2 O1 158.80(14) . . ?
N4 Ni2 O1 87.66(16) . . ?
O2 Ni2 O1 61.38(13) . . ?
N5 Ni2 O1 109.65(16) . . ?
N6 Ni2 O1 94.28(16) . . ?
O7 Ni2 C31 127.85(16) . . ?
N4 Ni2 C31 89.63(18) . . ?
O2 Ni2 C31 30.57(15) . . ?
N5 Ni2 C31 140.41(17) . . ?
N6 Ni2 C31 102.48(18) . . ?
O1 Ni2 C31 30.96(14) . . ?
O2 C31 O3 124.9(5) . . ?
O2 C31 O1 117.6(4) . . ?
O3 C31 O1 117.6(4) . . ?
O2 C31 Ni2 55.4(2) . . ?
O3 C31 Ni2 173.0(4) . . ?
O1 C31 Ni2 62.6(2) . . ?
O2 C31 Ni1 173.9(4) . . ?
O3 C31 Ni1 54.8(3) . . ?
O1 C31 Ni1 63.2(3) . . ?
Ni2 C31 Ni1 125.8(2) . . ?
C31 O1 Ni2 86.4(3) . . ?
C31 O1 Ni1 86.0(3) . . ?
Ni2 O1 Ni1 172.40(18) . . ?
C31 O2 Ni2 94.1(3) . . ?
C31 O3 Ni1 94.7(3) . . ?
C1 N1 C5 118.7(5) . . ?
C1 N1 Ni1 126.5(4) . . ?
C5 N1 Ni1 114.8(4) . . ?
N1 C1 C2 123.5(6) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 117.5(6) . . ?
C1 C2 C6 120.5(6) . . ?
C3 C2 C6 122.0(6) . . ?
O4 C3 C2 120.7(6) . . ?
O4 C3 C4 118.9(6) . . ?
C2 C3 C4 120.3(6) . . ?
C5 C4 C3 117.2(6) . . ?
C5 C4 C7 121.9(6) . . ?
C3 C4 C7 120.8(6) . . ?
N1 C5 C4 122.7(6) . . ?
N1 C5 C9 115.4(5) . . ?
C4 C5 C9 121.8(5) . . ?
C2 C6 H61 109.5 . . ?
C2 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
C2 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
C4 C7 H701 109.5 . . ?
C4 C7 H702 109.5 . . ?
H701 C7 H702 109.5 . . ?
C4 C7 H703 109.5 . . ?
H701 C7 H703 109.5 . . ?
H702 C7 H703 109.5 . . ?
C3 O4 C8 114.7(7) . . ?
O4 C8 H801 109.5 . . ?
O4 C8 H802 109.5 . . ?
H801 C8 H802 109.5 . . ?
O4 C8 H803 109.5 . . ?
H801 C8 H803 109.5 . . ?
H802 C8 H803 109.5 . . ?
N2 C9 C5 112.6(5) . . ?
N2 C9 H901 109.1 . . ?
C5 C9 H901 109.1 . . ?
N2 C9 H902 109.1 . . ?
C5 C9 H902 109.1 . . ?
H901 C9 H902 107.8 . . ?
C9 N2 C12 111.2(5) . . ?
C9 N2 C10 112.5(5) . . ?
C12 N2 C10 111.1(5) . . ?
C9 N2 Ni1 108.9(3) . . ?
C12 N2 Ni1 106.3(3) . . ?
C10 N2 Ni1 106.6(4) . . ?
N2 C10 C11 110.6(5) . . ?
N2 C10 H101 109.5 . . ?
C11 C10 H101 109.5 . . ?
N2 C10 H102 109.5 . . ?
C11 C10 H102 109.5 . . ?
H101 C10 H102 108.1 . . ?
N3 C11 C10 112.3(5) . . ?
N3 C11 H111 109.1 . . ?
C10 C11 H111 109.1 . . ?
N3 C11 H112 109.1 . . ?
C10 C11 H112 109.1 . . ?
H111 C11 H112 107.9 . . ?
C15 N3 C11 109.7(5) . . ?
C15 N3 C14 110.0(5) . . ?
C11 N3 C14 109.0(5) . . ?
C15 N3 Ni1 113.7(4) . . ?
C11 N3 Ni1 104.8(4) . . ?
C14 N3 Ni1 109.3(3) . . ?
N2 C12 C13 113.1(5) . . ?
N2 C12 H121 109.0 . . ?
C13 C12 H121 109.0 . . ?
N2 C12 H122 109.0 . . ?
C13 C12 H122 109.0 . . ?
H121 C12 H122 107.8 . . ?
C14 C13 C12 117.2(5) . . ?
C14 C13 H131 108.0 . . ?
C12 C13 H131 108.0 . . ?
C14 C13 H132 108.0 . . ?
C12 C13 H132 108.0 . . ?
H131 C13 H132 107.2 . . ?
N3 C14 C13 113.6(5) . . ?
N3 C14 H141 108.8 . . ?
C13 C14 H141 108.8 . . ?
N3 C14 H142 108.8 . . ?
C13 C14 H142 108.8 . . ?
H141 C14 H142 107.7 . . ?
N3 C15 H151 109.5 . . ?
N3 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
N3 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
Ni1 O5 H51 114.0(12) . . ?
Ni1 O5 H52 108(3) . . ?
H51 O5 H52 119.4(13) . . ?
C16 N4 C20 119.0(5) . . ?
C16 N4 Ni2 127.1(4) . . ?
C20 N4 Ni2 113.9(4) . . ?
N4 C16 C17 124.8(6) . . ?
N4 C16 H16 117.6 . . ?
C17 C16 H16 117.6 . . ?
C18 C17 C16 115.1(6) . . ?
C18 C17 C21 123.4(7) . . ?
C16 C17 C21 121.4(6) . . ?
C19 C18 C17 122.6(6) . . ?
C19 C18 O6 120.6(6) . . ?
C17 C18 O6 116.7(7) . . ?
C18 C19 C20 116.7(6) . . ?
C18 C19 C22 122.6(7) . . ?
C20 C19 C22 120.6(7) . . ?
N4 C20 C19 121.2(6) . . ?
N4 C20 C24 116.6(5) . . ?
C19 C20 C24 122.1(5) . . ?
C17 C21 H211 109.5 . . ?
C17 C21 H212 109.5 . . ?
H211 C21 H212 109.5 . . ?
C17 C21 H213 109.5 . . ?
H211 C21 H213 109.5 . . ?
H212 C21 H213 109.5 . . ?
C19 C22 H221 109.5 . . ?
C19 C22 H222 109.5 . . ?
H221 C22 H222 109.5 . . ?
C19 C22 H223 109.5 . . ?
H221 C22 H223 109.5 . . ?
H222 C22 H223 109.5 . . ?
C18 O6 C23 115.7(6) . . ?
O6 C23 H231 109.5 . . ?
O6 C23 H232 109.5 . . ?
H231 C23 H232 109.5 . . ?
O6 C23 H233 109.5 . . ?
H231 C23 H233 109.5 . . ?
H232 C23 H233 109.5 . . ?
N5 C24 C20 112.7(4) . . ?
N5 C24 H241 109.0 . . ?
C20 C24 H241 109.0 . . ?
N5 C24 H242 109.0 . . ?
C20 C24 H242 109.0 . . ?
H241 C24 H242 107.8 . . ?
C27 N5 C25 111.3(5) . . ?
C27 N5 C24 111.7(5) . . ?
C25 N5 C24 112.1(5) . . ?
C27 N5 Ni2 106.6(3) . . ?
C25 N5 Ni2 106.8(4) . . ?
C24 N5 Ni2 107.9(4) . . ?
N5 C25 C26 110.8(5) . . ?
N5 C25 H251 109.5 . . ?
C26 C25 H251 109.5 . . ?
N5 C25 H252 109.5 . . ?
C26 C25 H252 109.5 . . ?
H251 C25 H252 108.1 . . ?
N6 C26 C25 112.0(5) . . ?
N6 C26 H261 109.2 . . ?
C25 C26 H261 109.2 . . ?
N6 C26 H262 109.2 . . ?
C25 C26 H262 109.2 . . ?
H261 C26 H262 107.9 . . ?
C26 N6 C29 109.1(5) . . ?
C26 N6 C30 110.4(5) . . ?
C29 N6 C30 108.4(5) . . ?
C26 N6 Ni2 105.4(4) . . ?
C29 N6 Ni2 109.5(4) . . ?
C30 N6 Ni2 113.9(5) . . ?
N5 C27 C28 113.2(5) . . ?
N5 C27 H271 108.9 . . ?
C28 C27 H271 108.9 . . ?
N5 C27 H272 108.9 . . ?
C28 C27 H272 108.9 . . ?
H271 C27 H272 107.8 . . ?
C27 C28 C29 116.6(6) . . ?
C27 C28 H281 108.1 . . ?
C29 C28 H281 108.1 . . ?
C27 C28 H282 108.1 . . ?
C29 C28 H282 108.1 . . ?
H281 C28 H282 107.3 . . ?
N6 C29 C28 113.1(5) . . ?
N6 C29 H291 109.0 . . ?
C28 C29 H291 109.0 . . ?
N6 C29 H292 109.0 . . ?
C28 C29 H292 109.0 . . ?
H291 C29 H292 107.8 . . ?
N6 C30 H301 109.5 . . ?
N6 C30 H302 109.5 . . ?
H301 C30 H302 109.5 . . ?
N6 C30 H303 109.5 . . ?
H301 C30 H303 109.5 . . ?
H302 C30 H303 109.5 . . ?
Ni2 O7 H71 120.9(14) . . ?
Ni2 O7 H72 123.0(9) . . ?
H71 O7 H72 96.3(14) . . ?
H81 O8 H82 112.8(8) . . ?
H91 O9 H92 113.0(8) . . ?
O10 C32 C33 121.4(10) . . ?
O10 C32 C34 123.3(10) . . ?
C33 C32 C34 115.3(10) . . ?
C32 C33 H331 109.5 . . ?
C32 C33 H332 109.5 . . ?
H331 C33 H332 109.5 . . ?
C32 C33 H333 109.5 . . ?
H331 C33 H333 109.5 . . ?
H332 C33 H333 109.5 . . ?
C32 C34 H341 109.5 . . ?
C32 C34 H342 109.5 . . ?
H341 C34 H342 109.5 . . ?
C32 C34 H343 109.5 . . ?
H341 C34 H343 109.5 . . ?
H342 C34 H343 109.5 . . ?
O11 Cl1 O14 106.1(7) . . ?
O11 Cl1 O13 112.2(7) . . ?
O14 Cl1 O13 108.4(7) . . ?
O11 Cl1 O12 110.7(7) . . ?
O14 Cl1 O12 110.1(6) . . ?
O13 Cl1 O12 109.3(5) . . ?
O23 Cl2 O24 109.7(7) . . ?
O23 Cl2 O21 111.5(7) . . ?
O24 Cl2 O21 110.0(7) . . ?
O23 Cl2 O22 109.5(8) . . ?
O24 Cl2 O22 108.9(7) . . ?
O21 Cl2 O22 107.2(7) . . ?
O33 Cl3 O31 110.2(9) . . ?
O33 Cl3 O32 109.1(9) . . ?
O31 Cl3 O32 109.2(9) . . ?
O33 Cl3 O34 109.3(9) . . ?
O31 Cl3 O34 109.7(9) . . ?
O32 Cl3 O34 109.4(9) . . ?

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
O2 C31 O1 Ni2 7.1(4) . . . . ?
O3 C31 O1 Ni2 -172.1(5) . . . . ?
Ni1 C31 O1 Ni2 -179.76(18) . . . . ?
O2 C31 O1 Ni1 -173.1(5) . . . . ?
O3 C31 O1 Ni1 7.6(4) . . . . ?
Ni2 C31 O1 Ni1 179.76(18) . . . . ?
O3 C31 O2 Ni2 171.5(5) . . . . ?
O1 C31 O2 Ni2 -7.7(5) . . . . ?
O2 C31 O3 Ni1 172.5(5) . . . . ?
O1 C31 O3 Ni1 -8.3(5) . . . . ?
C5 N1 C1 C2 -3.9(9) . . . . ?
Ni1 N1 C1 C2 173.8(5) . . . . ?
N1 C1 C2 C3 1.5(10) . . . . ?
N1 C1 C2 C6 179.6(6) . . . . ?
C1 C2 C3 O4 179.0(6) . . . . ?
C6 C2 C3 O4 1.0(11) . . . . ?
C1 C2 C3 C4 1.0(10) . . . . ?
C6 C2 C3 C4 -177.0(7) . . . . ?
O4 C3 C4 C5 -179.1(6) . . . . ?
C2 C3 C4 C5 -1.1(10) . . . . ?
O4 C3 C4 C7 -1.9(11) . . . . ?
C2 C3 C4 C7 176.1(7) . . . . ?
C1 N1 C5 C4 3.7(9) . . . . ?
Ni1 N1 C5 C4 -174.2(5) . . . . ?
C1 N1 C5 C9 -174.1(5) . . . . ?
Ni1 N1 C5 C9 7.9(7) . . . . ?
C3 C4 C5 N1 -1.3(10) . . . . ?
C7 C4 C5 N1 -178.5(7) . . . . ?
C3 C4 C5 C9 176.4(6) . . . . ?
C7 C4 C5 C9 -0.8(11) . . . . ?
C2 C3 O4 C8 86.5(10) . . . . ?
C4 C3 O4 C8 -95.5(9) . . . . ?
N1 C5 C9 N2 -24.3(7) . . . . ?
C4 C5 C9 N2 157.8(6) . . . . ?
C5 C9 N2 C12 -89.0(6) . . . . ?
C5 C9 N2 C10 145.6(5) . . . . ?
C5 C9 N2 Ni1 27.7(6) . . . . ?
C9 N2 C10 C11 -154.1(5) . . . . ?
C12 N2 C10 C11 80.5(7) . . . . ?
Ni1 N2 C10 C11 -34.8(6) . . . . ?
N2 C10 C11 N3 -1.4(8) . . . . ?
C10 C11 N3 C15 158.5(6) . . . . ?
C10 C11 N3 C14 -80.9(7) . . . . ?
C10 C11 N3 Ni1 36.1(6) . . . . ?
C9 N2 C12 C13 -167.7(5) . . . . ?
C10 N2 C12 C13 -41.5(7) . . . . ?
Ni1 N2 C12 C13 74.0(5) . . . . ?
N2 C12 C13 C14 -49.2(7) . . . . ?
C15 N3 C14 C13 167.2(5) . . . . ?
C11 N3 C14 C13 46.9(6) . . . . ?
Ni1 N3 C14 C13 -67.2(5) . . . . ?
C12 C13 C14 N3 45.3(7) . . . . ?
C20 N4 C16 C17 -3.1(9) . . . . ?
Ni2 N4 C16 C17 175.5(5) . . . . ?
N4 C16 C17 C18 4.3(9) . . . . ?
N4 C16 C17 C21 -175.8(6) . . . . ?
C16 C17 C18 C19 0.9(10) . . . . ?
C21 C17 C18 C19 -179.0(6) . . . . ?
C16 C17 C18 O6 176.5(6) . . . . ?
C21 C17 C18 O6 -3.4(10) . . . . ?
C17 C18 C19 C20 -6.6(10) . . . . ?
O6 C18 C19 C20 178.0(6) . . . . ?
C17 C18 C19 C22 171.2(7) . . . . ?
O6 C18 C19 C22 -4.3(10) . . . . ?
C16 N4 C20 C19 -3.2(8) . . . . ?
Ni2 N4 C20 C19 178.0(4) . . . . ?
C16 N4 C20 C24 -179.2(5) . . . . ?
Ni2 N4 C20 C24 2.0(6) . . . . ?
C18 C19 C20 N4 7.9(9) . . . . ?
C22 C19 C20 N4 -169.9(6) . . . . ?
C18 C19 C20 C24 -176.5(6) . . . . ?
C22 C19 C20 C24 5.7(9) . . . . ?
C19 C18 O6 C23 -73.2(10) . . . . ?
C17 C18 O6 C23 111.2(8) . . . . ?
N4 C20 C24 N5 -20.1(7) . . . . ?
C19 C20 C24 N5 164.0(5) . . . . ?
C20 C24 N5 C27 -90.0(6) . . . . ?
C20 C24 N5 C25 144.3(5) . . . . ?
C20 C24 N5 Ni2 26.9(5) . . . . ?
C27 N5 C25 C26 80.9(7) . . . . ?
C24 N5 C25 C26 -153.1(5) . . . . ?
Ni2 N5 C25 C26 -35.1(7) . . . . ?
N5 C25 C26 N6 -1.2(8) . . . . ?
C25 C26 N6 C29 -81.5(7) . . . . ?
C25 C26 N6 C30 159.4(6) . . . . ?
C25 C26 N6 Ni2 36.0(6) . . . . ?
C25 N5 C27 C28 -41.2(7) . . . . ?
C24 N5 C27 C28 -167.4(5) . . . . ?
Ni2 N5 C27 C28 74.9(5) . . . . ?
N5 C27 C28 C29 -49.4(8) . . . . ?
C26 N6 C29 C28 47.3(7) . . . . ?
C30 N6 C29 C28 167.5(6) . . . . ?
Ni2 N6 C29 C28 -67.7(6) . . . . ?
C27 C28 C29 N6 45.2(8) . . . . ?

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
O5 H51 O2 0.84 1.878(6) 2.708(5) 169.5(16) 4_466
O5 H52 O9 0.84 1.810(9) 2.642(5) 170(4) 4_466
O7 H71 O8 0.84 1.798(6) 2.623(5) 166.7(10) .
O7 H72 O3 0.84 1.814(5) 2.654(4) 177.1(15) 4_566
O8 H81 O10 0.84 1.883(11) 2.717(10) 171(3) .
O8 H82 O12 0.84 2.339(17) 3.111(8) 153(3) 4_556
O8 H82 O13 0.84 2.26(2) 2.990(10) 146(3) 4_556
O9 H91 O21 0.84 2.212(17) 3.019(15) 161(2) 4_466
O9 H91 O32 0.84 2.12(4) 2.88(3) 150.4(16) 4_466
O9 H92 O10 0.84 1.948(8) 2.773(9) 166.8(9) .

_refine_diff_density_max         0.613
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.073

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MU2a
_database_code_depnum_ccdc_archive 'CCDC 1975598'
loop_
_audit_author_name
_audit_author_address
'marappan velusamy'
;North Eastern Hill University
India
;
_audit_update_record             
;
2021-04-23 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;

_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_name_systematic        
"(mu2-carbonatato)-bis(acetonitrile)-bis[1-methyl-4-(2-pyridin-2-ylethyl)-1,4-diazepane-N,N',N"]-di-nickel(II) bis(tetraphenylborate) acetonitrile solvate (1:2)"
_chemical_name_common            
"(mu2-carbonatato)-bis(acetonitrile)-bis[1-methyl-4-(2-pyridin-2-ylethyl)-1,4-diazepane-N,N',N"]-di-nickel(II) bis(tetraphenylborate) acetonitrile solvate (1:2)"
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H48 N8 Ni2 O3, 2(C24 H20 B), 2(C2 H3 N)'
_chemical_formula_sum            'C83 H94 B2 N10 Ni2 O3'
_chemical_formula_weight         1418.72

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   31.3574(16)
_cell_length_b                   11.0783(5)
_cell_length_c                   21.4842(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7463.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    291.19(18)
_cell_measurement_reflns_used    4963
_cell_measurement_theta_min      3.607
_cell_measurement_theta_max      25.682

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             3008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.561
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      291.19(18)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1279
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -99.00  -56.00   1.0000    8.8100
omega____ theta____ kappa____ phi______ frames
    -      -20.2184  178.0000  -90.0000 43

#__ type_ start__ end____ width___ exp.time_
  2 omega  -23.00   13.00   1.0000    8.8100
omega____ theta____ kappa____ phi______ frames
    -      -20.2184   57.0000 -150.0000 36

#__ type_ start__ end____ width___ exp.time_
  3 omega  -45.00   73.00   1.0000    8.8100
omega____ theta____ kappa____ phi______ frames
    -       22.5622    0.0000  -90.0000 118

;
_diffrn_reflns_number            24457
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.127
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.786
_diffrn_reflns_point_group_measured_fraction_full 0.786
_reflns_number_total             12818
_reflns_number_gt                10349
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_max     0.573
_reflns_Friedel_fraction_full    0.573

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 
 The non-hydrogen atoms were refined with anisotropic displacement
 parameters without any constraints.

 The H atoms of the pyridine rings and of the CH₂ groups were included with
 idealized geometries and their isotropic displacement parameters fixed
 to 1.2 times Ueq of the C atom they are bonded to
 (AFIX 43 and AFIX 23 of SHELXL).

 The H atoms of the methyl groups were included with their isotropic
 displacement parameters fixed to 1.5 times Ueq of the C atom they are
 bonded to and and idealized geometries with tetrahedral angles, enabling
 rotations around the X-C bonds, and C-H distances of 0.98 Å
 (AFIX 137 of SHELXL).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0019P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12818
_refine_ls_number_parameters     907
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0708
_refine_ls_wR_factor_gt          0.0620
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
N3 N 0.46907(12) 0.2673(4) 0.51453(18) 0.0494(10) Uani 1 1 d . . . . .
C28 C 0.27910(17) 0.4564(5) 0.6609(2) 0.0645(15) Uani 1 1 d . . . . .
H281 H 0.2673 0.5210 0.6366 0.097 Uiso 1 1 calc R U . . .
H282 H 0.3077 0.4765 0.6728 0.097 Uiso 1 1 calc R U . . .
H283 H 0.2621 0.4444 0.6975 0.097 Uiso 1 1 calc R U . . .
C10 C 0.43310(18) 0.0471(5) 0.5710(3) 0.0639(15) Uani 1 1 d . . . . .
H101 H 0.4040 0.0710 0.5802 0.077 Uiso 1 1 calc R U . . .
H102 H 0.4362 -0.0370 0.5827 0.077 Uiso 1 1 calc R U . . .
C11 C 0.4405(2) 0.0586(6) 0.5032(3) 0.0741(17) Uani 1 1 d . . . . .
H111 H 0.4184 0.0142 0.4815 0.089 Uiso 1 1 calc R U . . .
H112 H 0.4676 0.0212 0.4932 0.089 Uiso 1 1 calc R U . . .
C13 C 0.47512(19) 0.3793(5) 0.4791(3) 0.0776(18) Uani 1 1 d . . . . .
H131 H 0.4917 0.4350 0.5033 0.116 Uiso 1 1 calc R U . . .
H132 H 0.4478 0.4144 0.4699 0.116 Uiso 1 1 calc R U . . .
H133 H 0.4898 0.3617 0.4409 0.116 Uiso 1 1 calc R U . . .
C9 C 0.51092(15) 0.2075(5) 0.5274(3) 0.0656(14) Uani 1 1 d . . . . .
H91 H 0.5322 0.2683 0.5372 0.079 Uiso 1 1 calc R U . . .
H92 H 0.5203 0.1641 0.4907 0.079 Uiso 1 1 calc R U . . .
C8 C 0.50661(15) 0.1189(5) 0.5826(3) 0.0659(16) Uani 1 1 d . . . . .
H81 H 0.5134 0.0379 0.5686 0.079 Uiso 1 1 calc R U . . .
H82 H 0.5269 0.1407 0.6148 0.079 Uiso 1 1 calc R U . . .
C12 C 0.44085(18) 0.1846(5) 0.4795(2) 0.0650(16) Uani 1 1 d . . . . .
H121 H 0.4498 0.1837 0.4363 0.078 Uiso 1 1 calc R U . . .
H122 H 0.4120 0.2161 0.4808 0.078 Uiso 1 1 calc R U . . .
N4 N 0.49879(12) 0.3786(4) 0.63665(19) 0.0533(10) Uani 1 1 d . . . . .
N8 N 0.26176(13) 0.4794(4) 0.50477(19) 0.0574(11) Uani 1 1 d . . . . .
C14 C 0.52190(15) 0.4518(5) 0.6512(2) 0.0521(12) Uani 1 1 d . . . . .
C15 C 0.55137(17) 0.5443(5) 0.6706(3) 0.0796(18) Uani 1 1 d . . . . .
H151 H 0.5381 0.5944 0.7015 0.119 Uiso 1 1 calc R U . . .
H152 H 0.5592 0.5927 0.6354 0.119 Uiso 1 1 calc R U . . .
H153 H 0.5764 0.5073 0.6879 0.119 Uiso 1 1 calc R U . . .
C29 C 0.23627(16) 0.5412(4) 0.4869(3) 0.0574(13) Uani 1 1 d . . . . .
C30 C 0.20232(18) 0.6193(5) 0.4647(3) 0.095(2) Uani 1 1 d . . . . .
H301 H 0.2095 0.6493 0.4241 0.142 Uiso 1 1 calc R U . . .
H302 H 0.1989 0.6859 0.4928 0.142 Uiso 1 1 calc R U . . .
H303 H 0.1762 0.5744 0.4624 0.142 Uiso 1 1 calc R U . . .
C81 C 0.4779(2) 0.7233(6) 0.5297(4) 0.0814(17) Uani 1 1 d . . . . .
N9 N 0.5085(3) 0.7439(7) 0.5567(3) 0.125(3) Uani 1 1 d . . . . .
C80 C 0.4402(3) 0.7015(6) 0.4965(3) 0.103(3) Uani 1 1 d . . . . .
H801 H 0.4179 0.6792 0.5250 0.155 Uiso 1 1 calc R U . . .
H802 H 0.4447 0.6371 0.4674 0.155 Uiso 1 1 calc R U . . .
H803 H 0.4320 0.7732 0.4745 0.155 Uiso 1 1 calc R U . . .
Ni1 Ni 0.44276(2) 0.29927(5) 0.60523(3) 0.03642(12) Uani 1 1 d . . . . .
Ni2 Ni 0.31073(2) 0.36708(4) 0.53551(3) 0.03729(12) Uani 1 1 d . . . . .
N6 N 0.27868(11) 0.2055(3) 0.52525(18) 0.0439(9) Uani 1 1 d . . . . .
N5 N 0.33572(11) 0.3673(4) 0.44436(16) 0.0433(9) Uani 1 1 d . . . . .
O1 O 0.37478(9) 0.3149(2) 0.56975(13) 0.0345(6) Uani 1 1 d . . . . .
O2 O 0.41887(8) 0.4665(2) 0.58826(12) 0.0395(7) Uani 1 1 d . . . . .
N2 N 0.46250(11) 0.1207(3) 0.60908(19) 0.0465(9) Uani 1 1 d . . . . .
O3 O 0.35106(9) 0.5025(3) 0.56149(13) 0.0420(7) Uani 1 1 d . . . . .
N1 N 0.41756(12) 0.2974(3) 0.69691(16) 0.0416(9) Uani 1 1 d . . . . .
C44 C 0.62092(14) 0.3789(4) 0.40938(19) 0.0372(10) Uani 1 1 d . . . . .
C62 C 0.07727(14) 0.3131(4) 0.79866(19) 0.0391(10) Uani 1 1 d . . . . .
C31 C 0.38180(13) 0.4298(4) 0.57340(18) 0.0329(9) Uani 1 1 d . . . . .
N7 N 0.27941(12) 0.3454(3) 0.62377(17) 0.0458(10) Uani 1 1 d . . . . .
C25 C 0.30105(16) 0.1123(4) 0.5640(2) 0.0535(13) Uani 1 1 d . . . . .
H251 H 0.2920 0.0328 0.5505 0.064 Uiso 1 1 calc R U . . .
H252 H 0.3315 0.1184 0.5566 0.064 Uiso 1 1 calc R U . . .
C67 C 0.05648(15) 0.2040(5) 0.7903(2) 0.0510(12) Uani 1 1 d . . . . .
H67 H 0.0704 0.1432 0.7684 0.061 Uiso 1 1 calc R U . . .
C56 C 0.13942(14) 0.2348(4) 0.7233(2) 0.0370(10) Uani 1 1 d . . . . .
C61 C 0.12275(14) 0.2320(4) 0.6634(2) 0.0417(11) Uani 1 1 d . . . . .
H61 H 0.1045 0.2937 0.6510 0.050 Uiso 1 1 calc R U . . .
C74 C 0.12634(13) 0.4717(4) 0.73545(18) 0.0351(9) Uani 1 1 d . . . . .
C43 C 0.67181(14) 0.2251(4) 0.34495(19) 0.0424(11) Uani 1 1 d . . . . .
B2 B 0.12589(16) 0.3415(4) 0.7727(2) 0.0362(11) Uani 1 1 d . . . . .
C52 C 0.62564(14) 0.1475(4) 0.4866(2) 0.0439(11) Uani 1 1 d . . . . .
H52 H 0.6400 0.2163 0.4998 0.053 Uiso 1 1 calc R U . . .
C51 C 0.61310(13) 0.1407(4) 0.42419(19) 0.0358(10) Uani 1 1 d . . . . .
C26 C 0.29302(18) 0.1236(5) 0.6320(2) 0.0606(14) Uani 1 1 d . . . . .
H261 H 0.3113 0.0667 0.6535 0.073 Uiso 1 1 calc R U . . .
H262 H 0.2638 0.0999 0.6401 0.073 Uiso 1 1 calc R U . . .
C59 C 0.15879(17) 0.0477(4) 0.6368(2) 0.0530(13) Uani 1 1 d . . . . .
H59 H 0.1652 -0.0130 0.6084 0.064 Uiso 1 1 calc R U . . .
B1 B 0.62383(16) 0.2482(4) 0.3736(2) 0.0350(11) Uani 1 1 d . . . . .
C45 C 0.65599(15) 0.4307(4) 0.4402(2) 0.0450(11) Uani 1 1 d . . . . .
H45 H 0.6821 0.3912 0.4380 0.054 Uiso 1 1 calc R U . . .
C79 C 0.08994(15) 0.5249(5) 0.7112(2) 0.0539(13) Uani 1 1 d . . . . .
H79 H 0.0638 0.4880 0.7185 0.065 Uiso 1 1 calc R U . . .
C68 C 0.15935(14) 0.3412(4) 0.8318(2) 0.0406(10) Uani 1 1 d . . . . .
C5 C 0.40718(16) 0.1982(4) 0.7295(2) 0.0482(11) Uani 1 1 d . . . . .
C50 C 0.59275(15) 0.0325(4) 0.4090(2) 0.0449(11) Uani 1 1 d . . . . .
H50 H 0.5842 0.0211 0.3680 0.054 Uiso 1 1 calc R U . . .
C37 C 0.60023(18) 0.2648(4) 0.2546(2) 0.0533(13) Uani 1 1 d . . . . .
H37 H 0.6289 0.2783 0.2456 0.064 Uiso 1 1 calc R U . . .
C1 C 0.40805(16) 0.4043(4) 0.7215(2) 0.0495(12) Uani 1 1 d . . . . .
H1 H 0.4163 0.4731 0.6998 0.059 Uiso 1 1 calc R U . . .
C24 C 0.23503(13) 0.3079(5) 0.6072(3) 0.0571(12) Uani 1 1 d . . . . .
H241 H 0.2179 0.3790 0.5992 0.069 Uiso 1 1 calc R U . . .
H242 H 0.2224 0.2648 0.6419 0.069 Uiso 1 1 calc R U . . .
C4 C 0.38458(17) 0.2084(5) 0.7846(2) 0.0629(14) Uani 1 1 d . . . . .
H4 H 0.3765 0.1391 0.8059 0.076 Uiso 1 1 calc R U . . .
C57 C 0.16610(16) 0.1377(4) 0.7376(2) 0.0517(12) Uani 1 1 d . . . . .
H57 H 0.1781 0.1340 0.7771 0.062 Uiso 1 1 calc R U . . .
C19 C 0.36160(18) 0.2756(6) 0.3518(2) 0.0643(15) Uani 1 1 d . . . . .
H19 H 0.3643 0.2073 0.3270 0.077 Uiso 1 1 calc R U . . .
C27 C 0.30012(18) 0.2478(5) 0.6601(2) 0.0586(14) Uani 1 1 d . . . . .
H271 H 0.2889 0.2486 0.7022 0.070 Uiso 1 1 calc R U . . .
H272 H 0.3305 0.2635 0.6624 0.070 Uiso 1 1 calc R U . . .
C34 C 0.51601(17) 0.2220(5) 0.2766(3) 0.0661(15) Uani 1 1 d . . . . .
H34 H 0.4874 0.2069 0.2849 0.079 Uiso 1 1 calc R U . . .
C20 C 0.33976(15) 0.2693(5) 0.4082(2) 0.0478(12) Uani 1 1 d . . . . .
C42 C 0.68871(17) 0.1099(5) 0.3389(3) 0.0693(16) Uani 1 1 d . . . . .
H42 H 0.6726 0.0443 0.3523 0.083 Uiso 1 1 calc R U . . .
C49 C 0.58306(16) 0.4437(4) 0.4155(2) 0.0527(12) Uani 1 1 d . . . . .
H49 H 0.5587 0.4149 0.3957 0.063 Uiso 1 1 calc R U . . .
C53 C 0.61789(16) 0.0575(4) 0.5297(2) 0.0549(12) Uani 1 1 d . . . . .
H53 H 0.6268 0.0670 0.5707 0.066 Uiso 1 1 calc R U . . .
C47 C 0.6154(2) 0.5957(5) 0.4793(2) 0.0669(16) Uani 1 1 d . . . . .
H47 H 0.6134 0.6659 0.5029 0.080 Uiso 1 1 calc R U . . .
C23 C 0.23487(14) 0.2264(5) 0.5494(2) 0.0564(13) Uani 1 1 d . . . . .
H231 H 0.2220 0.1494 0.5598 0.068 Uiso 1 1 calc R U . . .
H232 H 0.2177 0.2636 0.5171 0.068 Uiso 1 1 calc R U . . .
C46 C 0.65366(18) 0.5372(4) 0.4735(2) 0.0557(13) Uani 1 1 d . . . . .
H46 H 0.6780 0.5690 0.4920 0.067 Uiso 1 1 calc R U . . .
C73 C 0.14699(17) 0.3310(4) 0.8932(2) 0.0538(13) Uani 1 1 d . . . . .
H73 H 0.1180 0.3259 0.9022 0.065 Uiso 1 1 calc R U . . .
C60 C 0.13227(16) 0.1405(4) 0.6210(2) 0.0504(12) Uani 1 1 d . . . . .
H60 H 0.1204 0.1428 0.5813 0.060 Uiso 1 1 calc R U . . .
C32 C 0.58878(14) 0.2444(4) 0.3158(2) 0.0407(10) Uani 1 1 d . . . . .
C63 C 0.05425(16) 0.3992(5) 0.8322(2) 0.0577(13) Uani 1 1 d . . . . .
H63 H 0.0668 0.4738 0.8397 0.069 Uiso 1 1 calc R U . . .
C2 C 0.38691(19) 0.4192(5) 0.7766(2) 0.0665(15) Uani 1 1 d . . . . .
H2 H 0.3814 0.4958 0.7924 0.080 Uiso 1 1 calc R U . . .
C54 C 0.59696(17) -0.0462(5) 0.5118(2) 0.0565(13) Uani 1 1 d . . . . .
H54 H 0.5913 -0.1067 0.5406 0.068 Uiso 1 1 calc R U . . .
C58 C 0.17561(17) 0.0461(4) 0.6953(2) 0.0582(14) Uani 1 1 d . . . . .
H58 H 0.1936 -0.0166 0.7071 0.070 Uiso 1 1 calc R U . . .
C78 C 0.09063(17) 0.6305(5) 0.6766(3) 0.0669(15) Uani 1 1 d . . . . .
H78 H 0.0653 0.6613 0.6607 0.080 Uiso 1 1 calc R U . . .
C77 C 0.12782(18) 0.6897(4) 0.6655(2) 0.0591(14) Uani 1 1 d . . . . .
H77 H 0.1282 0.7617 0.6433 0.071 Uiso 1 1 calc R U . . .
C65 C -0.00584(18) 0.2696(6) 0.8450(3) 0.0730(18) Uani 1 1 d . . . . .
H65 H -0.0332 0.2555 0.8599 0.088 Uiso 1 1 calc R U . . .
C39 C 0.73728(17) 0.2976(6) 0.2960(3) 0.0717(17) Uani 1 1 d . . . . .
H39 H 0.7531 0.3625 0.2811 0.086 Uiso 1 1 calc R U . . .
C38 C 0.69749(15) 0.3169(5) 0.3217(2) 0.0532(12) Uani 1 1 d . . . . .
H38 H 0.6873 0.3957 0.3236 0.064 Uiso 1 1 calc R U . . .
C17 C 0.37380(19) 0.4829(6) 0.3693(3) 0.0749(17) Uani 1 1 d . . . . .
H17 H 0.3848 0.5569 0.3567 0.090 Uiso 1 1 calc R U . . .
C76 C 0.16422(18) 0.6404(5) 0.6877(3) 0.0708(16) Uani 1 1 d . . . . .
H76 H 0.1902 0.6779 0.6801 0.085 Uiso 1 1 calc R U . . .
C70 C 0.23222(18) 0.3491(5) 0.8730(3) 0.0710(16) Uani 1 1 d . . . . .
H70 H 0.2612 0.3564 0.8650 0.085 Uiso 1 1 calc R U . . .
C75 C 0.16293(16) 0.5347(5) 0.7218(2) 0.0623(15) Uani 1 1 d . . . . .
H75 H 0.1886 0.5039 0.7365 0.075 Uiso 1 1 calc R U . . .
C33 C 0.54561(15) 0.2223(5) 0.3245(2) 0.0548(13) Uani 1 1 d . . . . .
H33 H 0.5360 0.2069 0.3647 0.066 Uiso 1 1 calc R U . . .
C3 C 0.37419(19) 0.3183(6) 0.8077(2) 0.0705(17) Uani 1 1 d . . . . .
H3 H 0.3586 0.3247 0.8443 0.085 Uiso 1 1 calc R U . . .
C48 C 0.58011(18) 0.5495(5) 0.4499(3) 0.0657(15) Uani 1 1 d . . . . .
H48 H 0.5541 0.5892 0.4531 0.079 Uiso 1 1 calc R U . . .
C22 C 0.27617(15) 0.1661(4) 0.4598(2) 0.0528(12) Uani 1 1 d . . . . .
H221 H 0.2592 0.2239 0.4367 0.063 Uiso 1 1 calc R U . . .
H222 H 0.2616 0.0889 0.4582 0.063 Uiso 1 1 calc R U . . .
C66 C 0.01555(18) 0.1811(6) 0.8130(3) 0.0681(16) Uani 1 1 d . . . . .
H66 H 0.0029 0.1062 0.8066 0.082 Uiso 1 1 calc R U . . .
C69 C 0.20342(17) 0.3488(5) 0.8238(2) 0.0631(15) Uani 1 1 d . . . . .
H69 H 0.2141 0.3538 0.7835 0.076 Uiso 1 1 calc R U . . .
C40 C 0.75341(19) 0.1831(7) 0.2924(3) 0.085(2) Uani 1 1 d . . . . .
H40 H 0.7804 0.1697 0.2759 0.102 Uiso 1 1 calc R U . . .
C21 C 0.31948(16) 0.1536(5) 0.4282(2) 0.0561(13) Uani 1 1 d . . . . .
H211 H 0.3387 0.1129 0.4567 0.067 Uiso 1 1 calc R U . . .
H212 H 0.3162 0.1023 0.3920 0.067 Uiso 1 1 calc R U . . .
C55 C 0.58459(16) -0.0590(4) 0.4514(2) 0.0535(13) Uani 1 1 d . . . . .
H55 H 0.5707 -0.1290 0.4386 0.064 Uiso 1 1 calc R U . . .
C35 C 0.5292(2) 0.2442(5) 0.2169(3) 0.0696(17) Uani 1 1 d . . . . .
H35 H 0.5097 0.2444 0.1843 0.084 Uiso 1 1 calc R U . . .
C72 C 0.1757(2) 0.3279(5) 0.9423(3) 0.0752(18) Uani 1 1 d . . . . .
H72 H 0.1656 0.3180 0.9827 0.090 Uiso 1 1 calc R U . . .
C36 C 0.5712(2) 0.2661(5) 0.2057(2) 0.0685(17) Uani 1 1 d . . . . .
H36 H 0.5805 0.2820 0.1654 0.082 Uiso 1 1 calc R U . . .
C7 C 0.46407(19) 0.0751(5) 0.6736(3) 0.0720(17) Uani 1 1 d . . . . .
H701 H 0.4842 0.1236 0.6971 0.086 Uiso 1 1 calc R U . . .
H702 H 0.4748 -0.0071 0.6730 0.086 Uiso 1 1 calc R U . . .
C16 C 0.35205(16) 0.4723(5) 0.4242(2) 0.0564(13) Uani 1 1 d . . . . .
H16 H 0.3484 0.5408 0.4487 0.068 Uiso 1 1 calc R U . . .
C71 C 0.2185(2) 0.3390(5) 0.9325(3) 0.0725(18) Uani 1 1 d . . . . .
H71 H 0.2376 0.3395 0.9656 0.087 Uiso 1 1 calc R U . . .
C18 C 0.3789(2) 0.3826(7) 0.3335(3) 0.083(2) Uani 1 1 d . . . . .
H18 H 0.3943 0.3871 0.2966 0.099 Uiso 1 1 calc R U . . .
C64 C 0.01336(18) 0.3785(6) 0.8548(3) 0.0697(16) Uani 1 1 d . . . . .
H64 H -0.0009 0.4388 0.8765 0.084 Uiso 1 1 calc R U . . .
C6 C 0.4217(2) 0.0765(5) 0.7069(3) 0.0731(18) Uani 1 1 d . . . . .
H601 H 0.4001 0.0447 0.6789 0.088 Uiso 1 1 calc R U . . .
H62 H 0.4234 0.0225 0.7423 0.088 Uiso 1 1 calc R U . . .
C41 C 0.7293(2) 0.0890(7) 0.3132(3) 0.096(2) Uani 1 1 d . . . . .
H41 H 0.7397 0.0106 0.3105 0.115 Uiso 1 1 calc R U . . .
N10 N 0.2421(2) 0.8109(7) 0.5889(3) 0.112(2) Uani 1 1 d . . . . .
C101 C 0.2744(3) 0.7921(6) 0.6089(4) 0.0846(18) Uani 1 1 d . . . . .
C102 C 0.3164(3) 0.7692(7) 0.6346(4) 0.119(3) Uani 1 1 d . . . . .
H103 H 0.3285 0.6992 0.6150 0.179 Uiso 1 1 calc R U . . .
H104 H 0.3140 0.7553 0.6786 0.179 Uiso 1 1 calc R U . . .
H105 H 0.3344 0.8377 0.6273 0.179 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
N3 C13 1.468(6) . ?
N3 C12 1.479(6) . ?
N3 C9 1.496(6) . ?
N3 Ni1 2.145(4) . ?
C28 N7 1.465(6) . ?
C28 H281 0.9600 . ?
C28 H282 0.9600 . ?
C28 H283 0.9600 . ?
C10 N2 1.478(6) . ?
C10 C11 1.480(7) . ?
C10 H101 0.9700 . ?
C10 H102 0.9700 . ?
C11 C12 1.486(8) . ?
C11 H111 0.9700 . ?
C11 H112 0.9700 . ?
C13 H131 0.9600 . ?
C13 H132 0.9600 . ?
C13 H133 0.9600 . ?
C9 C8 1.545(7) . ?
C9 H91 0.9700 . ?
C9 H92 0.9700 . ?
C8 N2 1.496(6) . ?
C8 H81 0.9700 . ?
C8 H82 0.9700 . ?
C12 H121 0.9700 . ?
C12 H122 0.9700 . ?
N4 C14 1.132(6) . ?
N4 Ni1 2.077(4) . ?
N8 C29 1.121(6) . ?
N8 Ni2 2.083(4) . ?
C14 C15 1.441(7) . ?
C15 H151 0.9600 . ?
C15 H152 0.9600 . ?
C15 H153 0.9600 . ?
C29 C30 1.453(7) . ?
C30 H301 0.9600 . ?
C30 H302 0.9600 . ?
C30 H303 0.9600 . ?
C81 N9 1.144(8) . ?
C81 C80 1.403(9) . ?
C80 H801 0.9600 . ?
C80 H802 0.9600 . ?
C80 H803 0.9600 . ?
Ni1 O2 2.032(3) . ?
Ni1 N2 2.075(3) . ?
Ni1 N1 2.122(4) . ?
Ni1 O1 2.271(3) . ?
Ni1 C31 2.493(4) . ?
Ni2 O3 2.040(3) . ?
Ni2 N6 2.064(3) . ?
Ni2 N5 2.109(4) . ?
Ni2 N7 2.149(4) . ?
Ni2 O1 2.216(3) . ?
Ni2 C31 2.472(4) . ?
N6 C22 1.473(6) . ?
N6 C23 1.486(5) . ?
N6 C25 1.501(6) . ?
N5 C20 1.341(6) . ?
N5 C16 1.343(6) . ?
O1 C31 1.294(5) . ?
O2 C31 1.272(5) . ?
N2 C7 1.476(6) . ?
O3 C31 1.282(5) . ?
N1 C1 1.331(6) . ?
N1 C5 1.343(6) . ?
C44 C49 1.394(6) . ?
C44 C45 1.406(6) . ?
C44 B1 1.642(6) . ?
C62 C67 1.385(6) . ?
C62 C63 1.396(6) . ?
C62 B2 1.653(6) . ?
N7 C27 1.483(6) . ?
N7 C24 1.496(5) . ?
C25 C26 1.487(6) . ?
C25 H251 0.9700 . ?
C25 H252 0.9700 . ?
C67 C66 1.397(7) . ?
C67 H67 0.9300 . ?
C56 C61 1.390(6) . ?
C56 C57 1.397(6) . ?
C56 B2 1.645(6) . ?
C61 C60 1.395(6) . ?
C61 H61 0.9300 . ?
C74 C75 1.374(6) . ?
C74 C79 1.386(6) . ?
C74 B2 1.651(6) . ?
C43 C42 1.388(7) . ?
C43 C38 1.390(6) . ?
C43 B1 1.646(6) . ?
B2 C68 1.647(7) . ?
C52 C53 1.381(6) . ?
C52 C51 1.399(6) . ?
C52 H52 0.9300 . ?
C51 C50 1.397(6) . ?
C51 B1 1.647(7) . ?
C26 C27 1.519(7) . ?
C26 H261 0.9700 . ?
C26 H262 0.9700 . ?
C59 C58 1.363(7) . ?
C59 C60 1.366(6) . ?
C59 H59 0.9300 . ?
B1 C32 1.658(6) . ?
C45 C46 1.382(6) . ?
C45 H45 0.9300 . ?
C79 C78 1.386(7) . ?
C79 H79 0.9300 . ?
C68 C73 1.381(6) . ?
C68 C69 1.395(7) . ?
C5 C4 1.384(7) . ?
C5 C6 1.503(7) . ?
C50 C55 1.387(6) . ?
C50 H50 0.9300 . ?
C37 C32 1.383(6) . ?
C37 C36 1.389(7) . ?
C37 H37 0.9300 . ?
C1 C2 1.368(7) . ?
C1 H1 0.9300 . ?
C24 C23 1.535(7) . ?
C24 H241 0.9700 . ?
C24 H242 0.9700 . ?
C4 C3 1.355(8) . ?
C4 H4 0.9300 . ?
C57 C58 1.395(6) . ?
C57 H57 0.9300 . ?
C19 C18 1.363(8) . ?
C19 C20 1.392(7) . ?
C19 H19 0.9300 . ?
C27 H271 0.9700 . ?
C27 H272 0.9700 . ?
C34 C35 1.370(8) . ?
C34 C33 1.386(7) . ?
C34 H34 0.9300 . ?
C20 C21 1.494(7) . ?
C42 C41 1.406(7) . ?
C42 H42 0.9300 . ?
C49 C48 1.388(7) . ?
C49 H49 0.9300 . ?
C53 C54 1.378(7) . ?
C53 H53 0.9300 . ?
C47 C46 1.369(7) . ?
C47 C48 1.374(8) . ?
C47 H47 0.9300 . ?
C23 H231 0.9700 . ?
C23 H232 0.9700 . ?
C46 H46 0.9300 . ?
C73 C72 1.386(7) . ?
C73 H73 0.9300 . ?
C60 H60 0.9300 . ?
C32 C33 1.388(6) . ?
C63 C64 1.390(7) . ?
C63 H63 0.9300 . ?
C2 C3 1.361(8) . ?
C2 H2 0.9300 . ?
C54 C55 1.362(6) . ?
C54 H54 0.9300 . ?
C58 H58 0.9300 . ?
C78 C77 1.359(7) . ?
C78 H78 0.9300 . ?
C77 C76 1.353(7) . ?
C77 H77 0.9300 . ?
C65 C64 1.364(8) . ?
C65 C66 1.373(8) . ?
C65 H65 0.9300 . ?
C39 C40 1.367(8) . ?
C39 C38 1.381(7) . ?
C39 H39 0.9300 . ?
C38 H38 0.9300 . ?
C17 C18 1.360(8) . ?
C17 C16 1.368(7) . ?
C17 H17 0.9300 . ?
C76 C75 1.382(7) . ?
C76 H76 0.9300 . ?
C70 C71 1.352(8) . ?
C70 C69 1.391(7) . ?
C70 H70 0.9300 . ?
C75 H75 0.9300 . ?
C33 H33 0.9300 . ?
C3 H3 0.9300 . ?
C48 H48 0.9300 . ?
C22 C21 1.525(6) . ?
C22 H221 0.9700 . ?
C22 H222 0.9700 . ?
C66 H66 0.9300 . ?
C69 H69 0.9300 . ?
C40 C41 1.364(9) . ?
C40 H40 0.9300 . ?
C21 H211 0.9700 . ?
C21 H212 0.9700 . ?
C55 H55 0.9300 . ?
C35 C36 1.362(9) . ?
C35 H35 0.9300 . ?
C72 C71 1.364(8) . ?
C72 H72 0.9300 . ?
C36 H36 0.9300 . ?
C7 C6 1.510(7) . ?
C7 H701 0.9700 . ?
C7 H702 0.9700 . ?
C16 H16 0.9300 . ?
C71 H71 0.9300 . ?
C18 H18 0.9300 . ?
C64 H64 0.9300 . ?
C6 H601 0.9700 . ?
C6 H62 0.9700 . ?
C41 H41 0.9300 . ?
N10 C101 1.122(8) . ?
C101 C102 1.450(10) . ?
C102 H103 0.9600 . ?
C102 H104 0.9600 . ?
C102 H105 0.9600 . ?

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
C13 N3 C12 109.7(4) . . ?
C13 N3 C9 110.9(4) . . ?
C12 N3 C9 110.2(4) . . ?
C13 N3 Ni1 112.4(3) . . ?
C12 N3 Ni1 109.5(3) . . ?
C9 N3 Ni1 104.0(3) . . ?
N7 C28 H281 109.5 . . ?
N7 C28 H282 109.5 . . ?
H281 C28 H282 109.5 . . ?
N7 C28 H283 109.5 . . ?
H281 C28 H283 109.5 . . ?
H282 C28 H283 109.5 . . ?
N2 C10 C11 113.6(5) . . ?
N2 C10 H101 108.9 . . ?
C11 C10 H101 108.9 . . ?
N2 C10 H102 108.9 . . ?
C11 C10 H102 108.9 . . ?
H101 C10 H102 107.7 . . ?
C10 C11 C12 114.8(5) . . ?
C10 C11 H111 108.6 . . ?
C12 C11 H111 108.6 . . ?
C10 C11 H112 108.6 . . ?
C12 C11 H112 108.6 . . ?
H111 C11 H112 107.5 . . ?
N3 C13 H131 109.5 . . ?
N3 C13 H132 109.5 . . ?
H131 C13 H132 109.5 . . ?
N3 C13 H133 109.5 . . ?
H131 C13 H133 109.5 . . ?
H132 C13 H133 109.5 . . ?
N3 C9 C8 110.3(4) . . ?
N3 C9 H91 109.6 . . ?
C8 C9 H91 109.6 . . ?
N3 C9 H92 109.6 . . ?
C8 C9 H92 109.6 . . ?
H91 C9 H92 108.1 . . ?
N2 C8 C9 111.4(4) . . ?
N2 C8 H81 109.4 . . ?
C9 C8 H81 109.4 . . ?
N2 C8 H82 109.4 . . ?
C9 C8 H82 109.4 . . ?
H81 C8 H82 108.0 . . ?
N3 C12 C11 114.3(5) . . ?
N3 C12 H121 108.7 . . ?
C11 C12 H121 108.7 . . ?
N3 C12 H122 108.7 . . ?
C11 C12 H122 108.7 . . ?
H121 C12 H122 107.6 . . ?
C14 N4 Ni1 159.2(4) . . ?
C29 N8 Ni2 177.8(5) . . ?
N4 C14 C15 179.2(6) . . ?
C14 C15 H151 109.5 . . ?
C14 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
C14 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
N8 C29 C30 178.4(6) . . ?
C29 C30 H301 109.5 . . ?
C29 C30 H302 109.5 . . ?
H301 C30 H302 109.5 . . ?
C29 C30 H303 109.5 . . ?
H301 C30 H303 109.5 . . ?
H302 C30 H303 109.5 . . ?
N9 C81 C80 178.5(8) . . ?
C81 C80 H801 109.5 . . ?
C81 C80 H802 109.5 . . ?
H801 C80 H802 109.5 . . ?
C81 C80 H803 109.5 . . ?
H801 C80 H803 109.5 . . ?
H802 C80 H803 109.5 . . ?
O2 Ni1 N2 170.73(13) . . ?
O2 Ni1 N4 89.11(14) . . ?
N2 Ni1 N4 97.94(15) . . ?
O2 Ni1 N1 92.19(12) . . ?
N2 Ni1 N1 93.70(15) . . ?
N4 Ni1 N1 91.00(15) . . ?
O2 Ni1 N3 97.44(13) . . ?
N2 Ni1 N3 76.35(15) . . ?
N4 Ni1 N3 92.29(16) . . ?
N1 Ni1 N3 169.86(15) . . ?
O2 Ni1 O1 61.58(10) . . ?
N2 Ni1 O1 111.48(12) . . ?
N4 Ni1 O1 150.57(14) . . ?
N1 Ni1 O1 87.86(12) . . ?
N3 Ni1 O1 93.94(13) . . ?
O2 Ni1 C31 30.56(12) . . ?
N2 Ni1 C31 142.46(14) . . ?
N4 Ni1 C31 119.51(15) . . ?
N1 Ni1 C31 88.55(13) . . ?
N3 Ni1 C31 98.14(14) . . ?
O1 Ni1 C31 31.08(11) . . ?
O3 Ni2 N6 165.59(13) . . ?
O3 Ni2 N8 96.00(14) . . ?
N6 Ni2 N8 97.18(15) . . ?
O3 Ni2 N5 91.32(13) . . ?
N6 Ni2 N5 94.73(15) . . ?
N8 Ni2 N5 88.79(15) . . ?
O3 Ni2 N7 97.13(13) . . ?
N6 Ni2 N7 76.99(14) . . ?
N8 Ni2 N7 90.55(15) . . ?
N5 Ni2 N7 171.55(15) . . ?
O3 Ni2 O1 62.55(10) . . ?
N6 Ni2 O1 104.51(12) . . ?
N8 Ni2 O1 158.28(14) . . ?
N5 Ni2 O1 88.38(12) . . ?
N7 Ni2 O1 95.29(13) . . ?
O3 Ni2 C31 31.17(12) . . ?
N6 Ni2 C31 135.86(14) . . ?
N8 Ni2 C31 126.94(16) . . ?
N5 Ni2 C31 88.31(13) . . ?
N7 Ni2 C31 98.79(13) . . ?
O1 Ni2 C31 31.44(11) . . ?
C22 N6 C23 109.2(3) . . ?
C22 N6 C25 110.5(4) . . ?
C23 N6 C25 110.2(4) . . ?
C22 N6 Ni2 112.6(3) . . ?
C23 N6 Ni2 106.1(3) . . ?
C25 N6 Ni2 108.1(3) . . ?
C20 N5 C16 118.6(4) . . ?
C20 N5 Ni2 124.9(3) . . ?
C16 N5 Ni2 116.2(3) . . ?
C31 O1 Ni2 85.3(2) . . ?
C31 O1 Ni1 84.0(2) . . ?
Ni2 O1 Ni1 169.25(14) . . ?
C31 O2 Ni1 95.2(2) . . ?
C7 N2 C10 110.6(4) . . ?
C7 N2 C8 108.8(4) . . ?
C10 N2 C8 111.0(4) . . ?
C7 N2 Ni1 112.0(3) . . ?
C10 N2 Ni1 108.5(3) . . ?
C8 N2 Ni1 105.8(3) . . ?
C31 O3 Ni2 93.4(2) . . ?
C1 N1 C5 117.8(4) . . ?
C1 N1 Ni1 116.3(3) . . ?
C5 N1 Ni1 125.6(3) . . ?
C49 C44 C45 114.3(4) . . ?
C49 C44 B1 123.1(4) . . ?
C45 C44 B1 122.5(4) . . ?
C67 C62 C63 114.8(4) . . ?
C67 C62 B2 123.8(4) . . ?
C63 C62 B2 121.4(4) . . ?
O2 C31 O3 122.4(4) . . ?
O2 C31 O1 119.0(4) . . ?
O3 C31 O1 118.6(4) . . ?
O2 C31 Ni2 174.9(3) . . ?
O3 C31 Ni2 55.5(2) . . ?
O1 C31 Ni2 63.3(2) . . ?
O2 C31 Ni1 54.3(2) . . ?
O3 C31 Ni1 174.8(3) . . ?
O1 C31 Ni1 64.9(2) . . ?
Ni2 C31 Ni1 128.21(17) . . ?
C28 N7 C27 109.2(4) . . ?
C28 N7 C24 110.9(4) . . ?
C27 N7 C24 109.3(4) . . ?
C28 N7 Ni2 112.9(3) . . ?
C27 N7 Ni2 110.2(3) . . ?
C24 N7 Ni2 104.2(3) . . ?
C26 C25 N6 114.0(4) . . ?
C26 C25 H251 108.7 . . ?
N6 C25 H251 108.7 . . ?
C26 C25 H252 108.7 . . ?
N6 C25 H252 108.7 . . ?
H251 C25 H252 107.6 . . ?
C62 C67 C66 123.0(5) . . ?
C62 C67 H67 118.5 . . ?
C66 C67 H67 118.5 . . ?
C61 C56 C57 114.3(4) . . ?
C61 C56 B2 121.1(4) . . ?
C57 C56 B2 124.5(4) . . ?
C56 C61 C60 122.7(4) . . ?
C56 C61 H61 118.6 . . ?
C60 C61 H61 118.6 . . ?
C75 C74 C79 113.1(4) . . ?
C75 C74 B2 123.7(4) . . ?
C79 C74 B2 123.1(4) . . ?
C42 C43 C38 114.7(4) . . ?
C42 C43 B1 121.8(4) . . ?
C38 C43 B1 123.4(4) . . ?
C56 B2 C68 109.4(4) . . ?
C56 B2 C74 108.2(4) . . ?
C68 B2 C74 111.7(4) . . ?
C56 B2 C62 108.6(4) . . ?
C68 B2 C62 109.1(4) . . ?
C74 B2 C62 109.7(3) . . ?
C53 C52 C51 123.6(4) . . ?
C53 C52 H52 118.2 . . ?
C51 C52 H52 118.2 . . ?
C50 C51 C52 113.5(4) . . ?
C50 C51 B1 124.0(4) . . ?
C52 C51 B1 122.4(4) . . ?
C25 C26 C27 116.3(4) . . ?
C25 C26 H261 108.2 . . ?
C27 C26 H261 108.2 . . ?
C25 C26 H262 108.2 . . ?
C27 C26 H262 108.2 . . ?
H261 C26 H262 107.4 . . ?
C58 C59 C60 118.3(4) . . ?
C58 C59 H59 120.8 . . ?
C60 C59 H59 120.8 . . ?
C44 B1 C43 111.3(4) . . ?
C44 B1 C51 108.5(4) . . ?
C43 B1 C51 108.7(3) . . ?
C44 B1 C32 109.6(3) . . ?
C43 B1 C32 108.8(4) . . ?
C51 B1 C32 109.9(3) . . ?
C46 C45 C44 123.4(5) . . ?
C46 C45 H45 118.3 . . ?
C44 C45 H45 118.3 . . ?
C74 C79 C78 123.2(5) . . ?
C74 C79 H79 118.4 . . ?
C78 C79 H79 118.4 . . ?
C73 C68 C69 113.6(4) . . ?
C73 C68 B2 123.9(4) . . ?
C69 C68 B2 122.4(4) . . ?
N1 C5 C4 120.2(5) . . ?
N1 C5 C6 119.5(4) . . ?
C4 C5 C6 120.3(5) . . ?
C55 C50 C51 123.9(4) . . ?
C55 C50 H50 118.0 . . ?
C51 C50 H50 118.0 . . ?
C32 C37 C36 123.5(5) . . ?
C32 C37 H37 118.3 . . ?
C36 C37 H37 118.3 . . ?
N1 C1 C2 124.1(5) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
N7 C24 C23 111.1(4) . . ?
N7 C24 H241 109.4 . . ?
C23 C24 H241 109.4 . . ?
N7 C24 H242 109.4 . . ?
C23 C24 H242 109.4 . . ?
H241 C24 H242 108.0 . . ?
C3 C4 C5 120.7(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C58 C57 C56 123.0(5) . . ?
C58 C57 H57 118.5 . . ?
C56 C57 H57 118.5 . . ?
C18 C19 C20 119.4(6) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
N7 C27 C26 112.7(4) . . ?
N7 C27 H271 109.0 . . ?
C26 C27 H271 109.0 . . ?
N7 C27 H272 109.0 . . ?
C26 C27 H272 109.0 . . ?
H271 C27 H272 107.8 . . ?
C35 C34 C33 119.5(5) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
N5 C20 C19 120.7(5) . . ?
N5 C20 C21 119.1(4) . . ?
C19 C20 C21 120.2(5) . . ?
C43 C42 C41 122.3(6) . . ?
C43 C42 H42 118.9 . . ?
C41 C42 H42 118.9 . . ?
C48 C49 C44 122.8(5) . . ?
C48 C49 H49 118.6 . . ?
C44 C49 H49 118.6 . . ?
C54 C53 C52 119.9(5) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.0 . . ?
C46 C47 C48 119.1(5) . . ?
C46 C47 H47 120.4 . . ?
C48 C47 H47 120.4 . . ?
N6 C23 C24 111.7(4) . . ?
N6 C23 H231 109.3 . . ?
C24 C23 H231 109.3 . . ?
N6 C23 H232 109.3 . . ?
C24 C23 H232 109.3 . . ?
H231 C23 H232 107.9 . . ?
C47 C46 C45 119.9(5) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C68 C73 C72 123.1(5) . . ?
C68 C73 H73 118.4 . . ?
C72 C73 H73 118.4 . . ?
C59 C60 C61 121.0(4) . . ?
C59 C60 H60 119.5 . . ?
C61 C60 H60 119.5 . . ?
C37 C32 C33 114.2(4) . . ?
C37 C32 B1 122.4(4) . . ?
C33 C32 B1 123.4(4) . . ?
C64 C63 C62 123.0(5) . . ?
C64 C63 H63 118.5 . . ?
C62 C63 H63 118.5 . . ?
C3 C2 C1 117.9(5) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C55 C54 C53 119.3(5) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C59 C58 C57 120.6(5) . . ?
C59 C58 H58 119.7 . . ?
C57 C58 H58 119.7 . . ?
C77 C78 C79 121.0(5) . . ?
C77 C78 H78 119.5 . . ?
C79 C78 H78 119.5 . . ?
C76 C77 C78 117.9(5) . . ?
C76 C77 H77 121.1 . . ?
C78 C77 H77 121.1 . . ?
C64 C65 C66 119.6(5) . . ?
C64 C65 H65 120.2 . . ?
C66 C65 H65 120.2 . . ?
C40 C39 C38 120.0(6) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C38 C43 123.6(5) . . ?
C39 C38 H38 118.2 . . ?
C43 C38 H38 118.2 . . ?
C18 C17 C16 118.4(6) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C77 C76 C75 120.3(5) . . ?
C77 C76 H76 119.9 . . ?
C75 C76 H76 119.9 . . ?
C71 C70 C69 120.7(6) . . ?
C71 C70 H70 119.6 . . ?
C69 C70 H70 119.6 . . ?
C74 C75 C76 124.6(5) . . ?
C74 C75 H75 117.7 . . ?
C76 C75 H75 117.7 . . ?
C34 C33 C32 123.6(5) . . ?
C34 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
C4 C3 C2 119.2(5) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C47 C48 C49 120.4(5) . . ?
C47 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
N6 C22 C21 113.8(4) . . ?
N6 C22 H221 108.8 . . ?
C21 C22 H221 108.8 . . ?
N6 C22 H222 108.8 . . ?
C21 C22 H222 108.8 . . ?
H221 C22 H222 107.7 . . ?
C65 C66 C67 119.6(5) . . ?
C65 C66 H66 120.2 . . ?
C67 C66 H66 120.2 . . ?
C70 C69 C68 123.3(5) . . ?
C70 C69 H69 118.3 . . ?
C68 C69 H69 118.3 . . ?
C41 C40 C39 119.0(6) . . ?
C41 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C20 C21 C22 115.4(4) . . ?
C20 C21 H211 108.4 . . ?
C22 C21 H211 108.4 . . ?
C20 C21 H212 108.4 . . ?
C22 C21 H212 108.4 . . ?
H211 C21 H212 107.5 . . ?
C54 C55 C50 119.8(5) . . ?
C54 C55 H55 120.1 . . ?
C50 C55 H55 120.1 . . ?
C36 C35 C34 119.3(5) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C71 C72 C73 121.2(6) . . ?
C71 C72 H72 119.4 . . ?
C73 C72 H72 119.4 . . ?
C35 C36 C37 119.9(5) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
N2 C7 C6 114.3(5) . . ?
N2 C7 H701 108.7 . . ?
C6 C7 H701 108.7 . . ?
N2 C7 H702 108.7 . . ?
C6 C7 H702 108.7 . . ?
H701 C7 H702 107.6 . . ?
N5 C16 C17 122.9(5) . . ?
N5 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C70 C71 C72 117.9(5) . . ?
C70 C71 H71 121.1 . . ?
C72 C71 H71 121.1 . . ?
C17 C18 C19 120.0(6) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C65 C64 C63 119.9(5) . . ?
C65 C64 H64 120.0 . . ?
C63 C64 H64 120.0 . . ?
C5 C6 C7 115.4(5) . . ?
C5 C6 H601 108.4 . . ?
C7 C6 H601 108.4 . . ?
C5 C6 H62 108.4 . . ?
C7 C6 H62 108.4 . . ?
H601 C6 H62 107.5 . . ?
C40 C41 C42 120.3(6) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
N10 C101 C102 179.4(9) . . ?
C101 C102 H103 109.5 . . ?
C101 C102 H104 109.5 . . ?
H103 C102 H104 109.5 . . ?
C101 C102 H105 109.5 . . ?
H103 C102 H105 109.5 . . ?
H104 C102 H105 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C10 C11 C12 -52.9(7) . . . . ?
C13 N3 C9 C8 159.8(5) . . . . ?
C12 N3 C9 C8 -78.5(5) . . . . ?
Ni1 N3 C9 C8 38.8(5) . . . . ?
N3 C9 C8 N2 -2.0(6) . . . . ?
C13 N3 C12 C11 166.4(5) . . . . ?
C9 N3 C12 C11 44.1(6) . . . . ?
Ni1 N3 C12 C11 -69.8(5) . . . . ?
C10 C11 C12 N3 50.4(7) . . . . ?
C11 C10 N2 C7 -160.3(5) . . . . ?
C11 C10 N2 C8 -39.4(6) . . . . ?
C11 C10 N2 Ni1 76.5(5) . . . . ?
C9 C8 N2 C7 -158.0(4) . . . . ?
C9 C8 N2 C10 80.0(5) . . . . ?
C9 C8 N2 Ni1 -37.6(5) . . . . ?
Ni1 O2 C31 O3 175.2(3) . . . . ?
Ni1 O2 C31 O1 -5.2(4) . . . . ?
Ni2 O3 C31 O2 174.5(3) . . . . ?
Ni2 O3 C31 O1 -5.1(4) . . . . ?
Ni2 O1 C31 O2 -174.9(3) . . . . ?
Ni1 O1 C31 O2 4.7(3) . . . . ?
Ni2 O1 C31 O3 4.7(3) . . . . ?
Ni1 O1 C31 O3 -175.7(3) . . . . ?
Ni1 O1 C31 Ni2 179.57(13) . . . . ?
Ni2 O1 C31 Ni1 -179.57(13) . . . . ?
C22 N6 C25 C26 -161.2(4) . . . . ?
C23 N6 C25 C26 -40.4(5) . . . . ?
Ni2 N6 C25 C26 75.2(4) . . . . ?
C63 C62 C67 C66 0.3(7) . . . . ?
B2 C62 C67 C66 179.3(5) . . . . ?
C57 C56 C61 C60 -0.6(6) . . . . ?
B2 C56 C61 C60 -177.6(4) . . . . ?
C61 C56 B2 C68 -165.5(4) . . . . ?
C57 C56 B2 C68 17.8(6) . . . . ?
C61 C56 B2 C74 -43.6(5) . . . . ?
C57 C56 B2 C74 139.8(4) . . . . ?
C61 C56 B2 C62 75.4(5) . . . . ?
C57 C56 B2 C62 -101.2(5) . . . . ?
C75 C74 B2 C56 -78.2(5) . . . . ?
C79 C74 B2 C56 97.5(5) . . . . ?
C75 C74 B2 C68 42.3(6) . . . . ?
C79 C74 B2 C68 -142.0(4) . . . . ?
C75 C74 B2 C62 163.5(4) . . . . ?
C79 C74 B2 C62 -20.8(6) . . . . ?
C67 C62 B2 C56 13.2(6) . . . . ?
C63 C62 B2 C56 -167.9(4) . . . . ?
C67 C62 B2 C68 -106.0(5) . . . . ?
C63 C62 B2 C68 72.9(5) . . . . ?
C67 C62 B2 C74 131.3(4) . . . . ?
C63 C62 B2 C74 -49.8(6) . . . . ?
C53 C52 C51 C50 -1.5(6) . . . . ?
C53 C52 C51 B1 -178.5(4) . . . . ?
N6 C25 C26 C27 -51.1(6) . . . . ?
C49 C44 B1 C43 153.1(4) . . . . ?
C45 C44 B1 C43 -31.5(6) . . . . ?
C49 C44 B1 C51 -87.3(5) . . . . ?
C45 C44 B1 C51 88.1(5) . . . . ?
C49 C44 B1 C32 32.7(6) . . . . ?
C45 C44 B1 C32 -151.9(4) . . . . ?
C42 C43 B1 C44 149.8(4) . . . . ?
C38 C43 B1 C44 -34.1(6) . . . . ?
C42 C43 B1 C51 30.4(6) . . . . ?
C38 C43 B1 C51 -153.5(4) . . . . ?
C42 C43 B1 C32 -89.3(5) . . . . ?
C38 C43 B1 C32 86.8(5) . . . . ?
C50 C51 B1 C44 147.6(4) . . . . ?
C52 C51 B1 C44 -35.7(5) . . . . ?
C50 C51 B1 C43 -91.3(5) . . . . ?
C52 C51 B1 C43 85.5(5) . . . . ?
C50 C51 B1 C32 27.7(6) . . . . ?
C52 C51 B1 C32 -155.5(4) . . . . ?
C49 C44 C45 C46 -0.4(7) . . . . ?
B1 C44 C45 C46 -176.3(4) . . . . ?
C75 C74 C79 C78 0.2(7) . . . . ?
B2 C74 C79 C78 -175.9(5) . . . . ?
C56 B2 C68 C73 -124.7(5) . . . . ?
C74 B2 C68 C73 115.5(5) . . . . ?
C62 B2 C68 C73 -6.0(6) . . . . ?
C56 B2 C68 C69 53.8(6) . . . . ?
C74 B2 C68 C69 -66.0(6) . . . . ?
C62 B2 C68 C69 172.5(4) . . . . ?
C1 N1 C5 C4 4.6(7) . . . . ?
Ni1 N1 C5 C4 -169.3(4) . . . . ?
C1 N1 C5 C6 -173.2(5) . . . . ?
Ni1 N1 C5 C6 12.9(7) . . . . ?
C52 C51 C50 C55 1.5(7) . . . . ?
B1 C51 C50 C55 178.5(4) . . . . ?
C5 N1 C1 C2 -2.7(7) . . . . ?
Ni1 N1 C1 C2 171.8(4) . . . . ?
C28 N7 C24 C23 157.4(4) . . . . ?
C27 N7 C24 C23 -82.2(5) . . . . ?
Ni2 N7 C24 C23 35.6(5) . . . . ?
N1 C5 C4 C3 -2.8(8) . . . . ?
C6 C5 C4 C3 175.0(6) . . . . ?
C61 C56 C57 C58 0.5(7) . . . . ?
B2 C56 C57 C58 177.4(4) . . . . ?
C28 N7 C27 C26 166.9(4) . . . . ?
C24 N7 C27 C26 45.5(5) . . . . ?
Ni2 N7 C27 C26 -68.5(5) . . . . ?
C25 C26 C27 N7 48.1(6) . . . . ?
C16 N5 C20 C19 2.0(7) . . . . ?
Ni2 N5 C20 C19 -171.7(4) . . . . ?
C16 N5 C20 C21 -176.4(4) . . . . ?
Ni2 N5 C20 C21 9.9(6) . . . . ?
C18 C19 C20 N5 -0.1(8) . . . . ?
C18 C19 C20 C21 178.3(5) . . . . ?
C38 C43 C42 C41 2.1(8) . . . . ?
B1 C43 C42 C41 178.6(5) . . . . ?
C45 C44 C49 C48 -1.0(7) . . . . ?
B1 C44 C49 C48 174.8(5) . . . . ?
C51 C52 C53 C54 0.4(7) . . . . ?
C22 N6 C23 C24 -159.9(4) . . . . ?
C25 N6 C23 C24 78.5(5) . . . . ?
Ni2 N6 C23 C24 -38.3(5) . . . . ?
N7 C24 C23 N6 0.3(6) . . . . ?
C48 C47 C46 C45 -2.2(8) . . . . ?
C44 C45 C46 C47 2.0(7) . . . . ?
C69 C68 C73 C72 -0.3(7) . . . . ?
B2 C68 C73 C72 178.3(5) . . . . ?
C58 C59 C60 C61 0.4(7) . . . . ?
C56 C61 C60 C59 0.2(7) . . . . ?
C36 C37 C32 C33 1.4(7) . . . . ?
C36 C37 C32 B1 -177.7(4) . . . . ?
C44 B1 C32 C37 99.8(5) . . . . ?
C43 B1 C32 C37 -22.1(6) . . . . ?
C51 B1 C32 C37 -141.0(4) . . . . ?
C44 B1 C32 C33 -79.2(5) . . . . ?
C43 B1 C32 C33 158.9(4) . . . . ?
C51 B1 C32 C33 39.9(6) . . . . ?
C67 C62 C63 C64 -0.9(7) . . . . ?
B2 C62 C63 C64 -179.9(5) . . . . ?
N1 C1 C2 C3 -1.2(8) . . . . ?
C52 C53 C54 C55 0.8(7) . . . . ?
C60 C59 C58 C57 -0.4(7) . . . . ?
C56 C57 C58 C59 0.0(8) . . . . ?
C74 C79 C78 C77 -1.3(9) . . . . ?
C79 C78 C77 C76 1.9(9) . . . . ?
C40 C39 C38 C43 0.0(8) . . . . ?
C42 C43 C38 C39 -1.7(7) . . . . ?
B1 C43 C38 C39 -178.1(5) . . . . ?
C78 C77 C76 C75 -1.4(9) . . . . ?
C79 C74 C75 C76 0.2(8) . . . . ?
B2 C74 C75 C76 176.3(5) . . . . ?
C77 C76 C75 C74 0.4(9) . . . . ?
C35 C34 C33 C32 0.1(8) . . . . ?
C37 C32 C33 C34 -0.8(7) . . . . ?
B1 C32 C33 C34 178.3(5) . . . . ?
C5 C4 C3 C2 -1.2(9) . . . . ?
C1 C2 C3 C4 3.1(9) . . . . ?
C46 C47 C48 C49 0.9(8) . . . . ?
C44 C49 C48 C47 0.7(8) . . . . ?
C23 N6 C22 C21 174.4(4) . . . . ?
C25 N6 C22 C21 -64.2(5) . . . . ?
Ni2 N6 C22 C21 56.8(5) . . . . ?
C64 C65 C66 C67 -0.8(9) . . . . ?
C62 C67 C66 C65 0.5(8) . . . . ?
C71 C70 C69 C68 1.6(9) . . . . ?
C73 C68 C69 C70 -1.6(8) . . . . ?
B2 C68 C69 C70 179.8(5) . . . . ?
C38 C39 C40 C41 1.4(10) . . . . ?
N5 C20 C21 C22 37.6(6) . . . . ?
C19 C20 C21 C22 -140.8(5) . . . . ?
N6 C22 C21 C20 -77.8(5) . . . . ?
C53 C54 C55 C50 -0.7(8) . . . . ?
C51 C50 C55 C54 -0.5(8) . . . . ?
C33 C34 C35 C36 0.1(8) . . . . ?
C68 C73 C72 C71 2.2(9) . . . . ?
C34 C35 C36 C37 0.5(9) . . . . ?
C32 C37 C36 C35 -1.3(8) . . . . ?
C10 N2 C7 C6 -60.0(6) . . . . ?
C8 N2 C7 C6 177.8(4) . . . . ?
Ni1 N2 C7 C6 61.2(5) . . . . ?
C20 N5 C16 C17 -2.1(7) . . . . ?
Ni2 N5 C16 C17 172.1(4) . . . . ?
C18 C17 C16 N5 0.2(9) . . . . ?
C69 C70 C71 C72 0.3(9) . . . . ?
C73 C72 C71 C70 -2.1(9) . . . . ?
C16 C17 C18 C19 1.8(10) . . . . ?
C20 C19 C18 C17 -1.9(9) . . . . ?
C66 C65 C64 C63 0.3(9) . . . . ?
C62 C63 C64 C65 0.6(9) . . . . ?
N1 C5 C6 C7 32.6(7) . . . . ?
C4 C5 C6 C7 -145.2(5) . . . . ?
N2 C7 C6 C5 -76.7(7) . . . . ?
C39 C40 C41 C42 -0.9(11) . . . . ?
C43 C42 C41 C40 -0.9(10) . . . . ?

_refine_diff_density_max         0.313
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.042

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MU1a
_database_code_depnum_ccdc_archive 'CCDC 1975593'
loop_
_audit_author_name
_audit_author_address
'marappan velusamy'
;North Eastern Hill University
India
;
_audit_update_record             
;
2021-04-23 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;

_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_chemical_name_systematic        
"(mu2-carbonatato)-acetonitrile-aqua-bis[1-methyl-4-(2-pyridin-2-ylmethyl)-1,4-diazepane-N,N',N"]-di-nickel(II) bis(tetraphenylborate) acetonitrile solvate hydrate"
_chemical_name_common            
"(mu2-carbonatato)-acetonitrile-aqua-bis[1-methyl-4-(2-pyridin-2-ylmethyl)-1,4-diazepane-N,N',N"]-di-nickel(II) bis(tetraphenylborate) acetonitrile solvate hydrate"
_chemical_melting_point          ?
_chemical_formula_moiety         
'C27 H43 N7 Ni2 O4, 2(C24 H20 B), C2 H3 N [+ solvent]'
_chemical_formula_sum            'C77 H86 B2 N8 Ni2 O4'
_chemical_formula_weight         1326.57

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.9721(5)
_cell_length_b                   14.2148(5)
_cell_length_c                   20.9208(7)
_cell_angle_alpha                92.908(3)
_cell_angle_beta                 106.598(3)
_cell_angle_gamma                113.393(3)
_cell_volume                     3590.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    291.3(2)
_cell_measurement_reflns_used    7339
_cell_measurement_theta_min      3.4720
_cell_measurement_theta_max      27.1970

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             1404
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.578
_shelx_estimated_absorpt_T_min   0.934
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      291.3(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1279
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -22.00   23.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -      -20.3747  -99.0000   30.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   45.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184  -57.0000  -30.0000 93

#__ type_ start__ end____ width___ exp.time_
  3 omega   51.00   84.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184   57.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
  4 omega  -48.00   56.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184  -77.0000   90.0000 104

#__ type_ start__ end____ width___ exp.time_
  5 omega   54.00   96.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184  178.0000   90.0000 42

#__ type_ start__ end____ width___ exp.time_
  6 omega   -1.00   38.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184   57.0000 -120.0000 39

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00  100.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184 -178.0000    0.0000 63

#__ type_ start__ end____ width___ exp.time_
  8 omega   57.00   82.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184  178.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
  9 omega  -23.00   27.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184  -99.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
 10 omega   45.00   72.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184   57.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 11 omega   67.00   92.00   1.0000    1.6200
omega____ theta____ kappa____ phi______ frames
    -       22.7184   57.0000  120.0000 25

;
_diffrn_reflns_number            31987
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.315
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14089
_reflns_number_gt                10197
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 
 The non-hydrogen atoms of the dication and of the anions were refined
 with anisotropic displacement parameters without any constraints. The
 acetonitrile solvent molecule was refined as a rigid body
 (EADP of SHELXL).

 Besides the described ions and solvent molecule there is a cavity containing
 disordered solvent molecules. Since it was not possible to describe
 the refined peaks of residual electron density as partially occupied
 individual solvent molecules, the diffuse electron density in these
 regions was removed by the SQUEEZE routine of the PLATON program
 [A. L. Spek, Acta Cryst. C71, 9-18 (2015)]. The solvent contributions
 to the calculated structure factors for each reflection hkl is included
 in the FAB file. The SQUEEZE routine resulted in a void volume
 of 138 A³ with an electron count of 28. If this cavity is occupied by
 two solvent molecules, an occupancy of 2/3(acetonitrile + H2O) and
 1/3(H2O + H2O) would result in an average of 28 electrons. The content
 of this cavity was not included in the reported chemical formula,
 molecular weight, density, and F000. The use of SQUEEZE decreased the
 R value R1 from 0.0777 to 0.0494.

 The positions of the H atoms of the aqua ligand O4 were taken from a
 difference Fourier map, the O-H distances weres fixed to 0.84 Å
 (DFIX of SHELXL), and these H atoms were refined with a common isotropic
 displacement parameter without any constraints to the bond angles.

 The H atoms of the pyridine rings and of the CH₂ groups were included with
 idealized geometries and their isotropic displacement parameters fixed
 to 1.2 times Ueq of the C atom they are bonded to
 (AFIX 43 and AFIX 23 of SHELXL).

 The H atoms of the methyl groups were included with their isotropic
 displacement parameters fixed to 1.5 times Ueq of the C atom they are
 bonded to and and idealized geometries with tetrahedral angles, enabling
 rotations around the X-C bonds, and C-H distances of 0.98 Å
 (AFIX 137 of SHELXL).
;
# start Validation Reply Form
_vrf_PLAT171_MU1a                
;
PROBLEM: The CIF-Embedded .res File Contains EADP Records ....... 1 Report
RESPONSE:
 The non-hydrogen atoms of the dication and of the anions were refined
 with anisotropic displacement parameters without any constraints. The
 acetonitrile solvent molecule was refined as a rigid body
 (EADP of SHELXL).
;
_vrf_PLAT172_MU1a                
;
PROBLEM: The CIF-Embedded .res File Contains DFIX Records ....... 1 Report
RESPONSE:
 The positions of the H atoms of the aqua ligand O4 were taken from a
 difference Fourier map, the O-H distances weres fixed to 0.84A
 (DFIX of SHELXL), and these H atoms were refined with a common isotropic
 displacement parameter without any constraints to the bond angles.
;
_vrf_PLAT420_MU1a                
;
PROBLEM: D-H Without Acceptor O4 - H40 ....... Please Check
RESPONSE:
 The bond O4-H40 is directed to a cavity whose disordered atomic content
 has been removed by SQUEEZE.
;
_vrf_PLAT605_MU1a                
;
PROBLEM: Largest Solvent Accessible VOID in the Structure 134 A**3
RESPONSE:
 Besides the described ions and solvent molecule there is a cavity containing
 disordered solvent molecules. Since it was not possible to describe
 the refined peaks of residual electron density as partially occupied
 individual solvent molecules, the diffuse electron density in these
 regions was removed by the SQUEEZE routine of the PLATON program
 [A. L. Spek, Acta Cryst. C71, 9-18 (2015)]. The solvent contributions
 to the calculated structure factors for each reflection hkl is included
 in the FAB file. The SQUEEZE routine resulted in a void volume
 of 138 A**3 with an electron count of 28. If this cavity is occupied by
 two solvent molecules, an occupancy of 2/3(acetonitrile + H2O) and
 1/3(H2O + H2O) would result in an average of 28 electrons. The content
 of this cavity was not included in the reported chemical formula,
 molecular weight, density, and F000. The use of SQUEEZE decreased the
 R value R1 from 0.0777 to 0.0494.
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+1.2535P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14089
_refine_ls_number_parameters     837
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1228
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Ni2 Ni 1.04048(3) 0.50352(3) 0.38506(2) 0.03311(10) Uani 1 1 d . . . . .
Ni1 Ni 0.70474(3) 0.26889(3) 0.24939(2) 0.03822(10) Uani 1 1 d . . . . .
O1 O 0.87670(15) 0.38609(14) 0.30955(9) 0.0366(4) Uani 1 1 d . . . . .
O3 O 0.73938(15) 0.32252(14) 0.35014(9) 0.0382(4) Uani 1 1 d . . . . .
O2 O 0.90257(14) 0.45386(14) 0.41333(9) 0.0372(4) Uani 1 1 d . . . . .
O4 O 1.14149(16) 0.59527(16) 0.47660(10) 0.0591(6) Uani 1 1 d D . . . .
H4 H 1.1233(5) 0.5778(10) 0.51067(16) 0.098(10) Uiso 1 1 d D U . . .
H40 H 1.1986(4) 0.6522(4) 0.489(2) 0.098(10) Uiso 1 1 d D U . . .
C15 C 0.8381(2) 0.3870(2) 0.35855(14) 0.0332(6) Uani 1 1 d . . . . .
N5 N 1.07461(18) 0.37816(18) 0.40951(12) 0.0394(5) Uani 1 1 d . . . . .
N1 N 0.67942(19) 0.39291(18) 0.21494(12) 0.0424(6) Uani 1 1 d . . . . .
N7 N 1.0386(2) 0.63043(18) 0.33906(12) 0.0436(6) Uani 1 1 d . . . . .
N6 N 1.16303(19) 0.53281(18) 0.34186(12) 0.0404(5) Uani 1 1 d . . . . .
C47 C 0.7031(2) 0.6333(2) 0.41477(16) 0.0471(7) Uani 1 1 d . . . . .
H47 H 0.7732 0.6826 0.4183 0.057 Uiso 1 1 calc R U . . .
N2 N 0.7106(2) 0.2384(2) 0.15282(13) 0.0518(7) Uani 1 1 d . . . . .
C70 C 0.2553(3) 0.0475(2) 0.01422(15) 0.0479(7) Uani 1 1 d . . . . .
C38 C 0.7444(4) 1.0037(4) 0.5523(3) 0.1042(17) Uani 1 1 d . . . . .
H38 H 0.7866 1.0756 0.5643 0.125 Uiso 1 1 calc R U . . .
C52 C 0.3601(2) 0.2237(2) -0.03007(15) 0.0418(7) Uani 1 1 d . . . . .
N3 N 0.7429(2) 0.13990(19) 0.25427(14) 0.0521(7) Uani 1 1 d . . . . .
C28 C 0.7404(2) 0.8360(2) 0.36423(16) 0.0442(7) Uani 1 1 d . . . . .
C30 C 0.9410(3) 0.9238(3) 0.3879(2) 0.0620(9) Uani 1 1 d . . . . .
H30 H 1.0118 0.9547 0.4198 0.074 Uiso 1 1 calc R U . . .
C48 C 0.6907(3) 0.5353(3) 0.42714(18) 0.0550(8) Uani 1 1 d . . . . .
H48 H 0.7521 0.5207 0.4392 0.066 Uiso 1 1 calc R U . . .
C46 C 0.6162(2) 0.6619(2) 0.39727(17) 0.0460(7) Uani 1 1 d . . . . .
C17 C 0.9894(3) 0.5951(3) 0.26456(16) 0.0526(8) Uani 1 1 d . . . . .
H171 H 0.9768 0.6508 0.2441 0.063 Uiso 1 1 calc R U . . .
H172 H 0.9181 0.5359 0.2541 0.063 Uiso 1 1 calc R U . . .
C57 C 0.3813(3) 0.1719(3) -0.07890(17) 0.0577(9) Uani 1 1 d . . . . .
H57 H 0.3406 0.1000 -0.0920 0.069 Uiso 1 1 calc R U . . .
C71 C 0.3476(3) 0.0257(3) 0.02857(17) 0.0561(8) Uani 1 1 d . . . . .
H71 H 0.4133 0.0764 0.0265 0.067 Uiso 1 1 calc R U . . .
C75 C 0.1616(3) -0.0328(3) 0.01997(19) 0.0647(10) Uani 1 1 d . . . . .
H75 H 0.0980 -0.0224 0.0127 0.078 Uiso 1 1 calc R U . . .
C64 C 0.1472(3) 0.1469(3) -0.06489(17) 0.0508(8) Uani 1 1 d . . . . .
C26 C 1.0348(3) 0.2082(3) 0.43468(19) 0.0614(9) Uani 1 1 d . . . . .
H26 H 0.9929 0.1525 0.4513 0.074 Uiso 1 1 calc R U . . .
C53 C 0.4238(3) 0.3306(2) -0.01424(17) 0.0522(8) Uani 1 1 d . . . . .
H53 H 0.4134 0.3699 0.0178 0.063 Uiso 1 1 calc R U . . .
C12 C 0.6808(3) 0.4732(2) 0.25180(17) 0.0519(8) Uani 1 1 d . . . . .
H12 H 0.6764 0.4677 0.2951 0.062 Uiso 1 1 calc R U . . .
C55 C 0.5203(3) 0.3271(3) -0.09126(19) 0.0600(9) Uani 1 1 d . . . . .
H55 H 0.5731 0.3611 -0.1112 0.072 Uiso 1 1 calc R U . . .
C65 C 0.0745(3) 0.0563(3) -0.11189(18) 0.0626(9) Uani 1 1 d . . . . .
H65 H 0.0847 -0.0041 -0.1072 0.075 Uiso 1 1 calc R U . . .
C54 C 0.5025(3) 0.3820(3) -0.04401(19) 0.0605(9) Uani 1 1 d . . . . .
H54 H 0.5431 0.4540 -0.0317 0.073 Uiso 1 1 calc R U . . .
C27 C 1.0172(3) 0.2964(2) 0.43319(16) 0.0500(8) Uani 1 1 d . . . . .
H27 H 0.9628 0.2995 0.4494 0.060 Uiso 1 1 calc R U . . .
N4 N 0.5371(2) 0.1778(2) 0.22919(14) 0.0547(7) Uani 1 1 d . . . . .
C18 C 1.0595(3) 0.5644(3) 0.23279(17) 0.0603(9) Uani 1 1 d . . . . .
H181 H 1.1199 0.6276 0.2310 0.072 Uiso 1 1 calc R U . . .
H182 H 1.0148 0.5290 0.1864 0.072 Uiso 1 1 calc R U . . .
C23 C 1.1549(2) 0.3745(2) 0.38835(16) 0.0462(7) Uani 1 1 d . . . . .
C49 C 0.5910(3) 0.4609(3) 0.4220(2) 0.0809(13) Uani 1 1 d . . . . .
H49 H 0.5825 0.3948 0.4301 0.097 Uiso 1 1 calc R U . . .
C14 C 0.3270(3) 0.0756(3) 0.2017(2) 0.0679(10) Uani 1 1 d . . . . .
H141 H 0.2901 0.1141 0.1776 0.102 Uiso 1 1 calc R U . . .
H142 H 0.3105 0.0657 0.2431 0.102 Uiso 1 1 calc R U . . .
H143 H 0.3020 0.0090 0.1740 0.102 Uiso 1 1 calc R U . . .
C20 C 1.1582(3) 0.7046(2) 0.35717(17) 0.0541(8) Uani 1 1 d . . . . .
H203 H 1.1828 0.7474 0.4014 0.065 Uiso 1 1 calc R U . . .
H204 H 1.1664 0.7504 0.3243 0.065 Uiso 1 1 calc R U . . .
C58 C 0.2635(3) 0.2218(2) 0.06856(16) 0.0479(7) Uani 1 1 d . . . . .
C63 C 0.3606(3) 0.2877(3) 0.12028(17) 0.0560(8) Uani 1 1 d . . . . .
H63 H 0.4275 0.3015 0.1135 0.067 Uiso 1 1 calc R U . . .
C29 C 0.8495(3) 0.8847(2) 0.40901(19) 0.0552(8) Uani 1 1 d . . . . .
H29 H 0.8612 0.8912 0.4554 0.066 Uiso 1 1 calc R U . . .
C32 C 0.8224(3) 0.8702(3) 0.2741(2) 0.0602(9) Uani 1 1 d . . . . .
H32 H 0.8121 0.8648 0.2279 0.072 Uiso 1 1 calc R U . . .
C22 C 1.2263(3) 0.4738(2) 0.37144(19) 0.0526(8) Uani 1 1 d . . . . .
H221 H 1.2864 0.5170 0.4123 0.063 Uiso 1 1 calc R U . . .
H222 H 1.2583 0.4575 0.3394 0.063 Uiso 1 1 calc R U . . .
C33 C 0.7312(3) 0.8308(2) 0.29598(18) 0.0498(8) Uani 1 1 d . . . . .
H33 H 0.6609 0.7995 0.2635 0.060 Uiso 1 1 calc R U . . .
C19 C 1.1082(3) 0.4947(3) 0.26780(16) 0.0542(8) Uani 1 1 d . . . . .
H191 H 1.0497 0.4250 0.2597 0.065 Uiso 1 1 calc R U . . .
H192 H 1.1616 0.4905 0.2480 0.065 Uiso 1 1 calc R U . . .
C8 C 0.6824(3) 0.3991(3) 0.15171(16) 0.0535(8) Uani 1 1 d . . . . .
C56 C 0.4592(3) 0.2215(3) -0.10873(19) 0.0639(10) Uani 1 1 d . . . . .
H56 H 0.4704 0.1829 -0.1408 0.077 Uiso 1 1 calc R U . . .
C11 C 0.6886(3) 0.5636(3) 0.2283(2) 0.0669(10) Uani 1 1 d . . . . .
H11 H 0.6887 0.6180 0.2550 0.080 Uiso 1 1 calc R U . . .
C21 C 1.2321(2) 0.6467(2) 0.35856(17) 0.0473(7) Uani 1 1 d . . . . .
H211 H 1.2702 0.6675 0.3259 0.057 Uiso 1 1 calc R U . . .
H212 H 1.2872 0.6652 0.4033 0.057 Uiso 1 1 calc R U . . .
C40 C 0.5245(3) 0.7862(3) 0.33656(17) 0.0489(8) Uani 1 1 d . . . . .
C24 C 1.1760(3) 0.2875(3) 0.3875(2) 0.0621(9) Uani 1 1 d . . . . .
H24 H 1.2305 0.2856 0.3711 0.075 Uiso 1 1 calc R U . . .
C69 C 0.1268(3) 0.2344(3) -0.07594(19) 0.0668(10) Uani 1 1 d . . . . .
H69 H 0.1738 0.2976 -0.0463 0.080 Uiso 1 1 calc R U . . .
C9 C 0.6933(3) 0.4889(3) 0.1263(2) 0.0717(11) Uani 1 1 d . . . . .
H9 H 0.6989 0.4935 0.0832 0.086 Uiso 1 1 calc R U . . .
C13 C 0.4445(3) 0.1329(3) 0.21739(16) 0.0499(8) Uani 1 1 d . . . . .
C31 C 0.9272(3) 0.9170(3) 0.3204(2) 0.0648(10) Uani 1 1 d . . . . .
H31 H 0.9882 0.9438 0.3059 0.078 Uiso 1 1 calc R U . . .
C50 C 0.5028(4) 0.4845(3) 0.4045(4) 0.137(3) Uani 1 1 d . . . . .
H50 H 0.4329 0.4341 0.4005 0.164 Uiso 1 1 calc R U . . .
C72 C 0.3464(4) -0.0674(3) 0.04576(19) 0.0708(11) Uani 1 1 d . . . . .
H72 H 0.4102 -0.0779 0.0552 0.085 Uiso 1 1 calc R U . . .
C34 C 0.6596(3) 0.8439(3) 0.46677(18) 0.0530(8) Uani 1 1 d . . . . .
C45 C 0.4917(3) 0.8646(3) 0.3465(2) 0.0688(11) Uani 1 1 d . . . . .
H45 H 0.5300 0.9129 0.3869 0.083 Uiso 1 1 calc R U . . .
C66 C -0.0137(3) 0.0528(4) -0.1661(2) 0.0798(12) Uani 1 1 d . . . . .
H66 H -0.0610 -0.0096 -0.1964 0.096 Uiso 1 1 calc R U . . .
C16 C 0.9780(3) 0.6809(3) 0.3630(2) 0.0683(10) Uani 1 1 d . . . . .
H161 H 0.9830 0.7405 0.3421 0.103 Uiso 1 1 calc R U . . .
H162 H 1.0097 0.7029 0.4114 0.103 Uiso 1 1 calc R U . . .
H163 H 0.9017 0.6323 0.3511 0.103 Uiso 1 1 calc R U . . .
C62 C 0.3638(4) 0.3340(3) 0.1813(2) 0.0746(11) Uani 1 1 d . . . . .
H62 H 0.4309 0.3787 0.2138 0.090 Uiso 1 1 calc R U . . .
C60 C 0.1686(4) 0.2466(4) 0.1445(2) 0.0905(14) Uani 1 1 d . . . . .
H60 H 0.1023 0.2305 0.1526 0.109 Uiso 1 1 calc R U . . .
C73 C 0.2509(4) -0.1443(3) 0.0489(2) 0.0802(12) Uani 1 1 d . . . . .
H73 H 0.2491 -0.2074 0.0598 0.096 Uiso 1 1 calc R U . . .
C7 C 0.6632(3) 0.2988(3) 0.10985(18) 0.0698(10) Uani 1 1 d . . . . .
H701 H 0.5844 0.2570 0.0877 0.084 Uiso 1 1 calc R U . . .
H702 H 0.6970 0.3154 0.0749 0.084 Uiso 1 1 calc R U . . .
C1 C 0.7294(3) 0.0917(3) 0.3142(2) 0.0725(11) Uani 1 1 d . . . . .
H101 H 0.6555 0.0727 0.3144 0.109 Uiso 1 1 calc R U . . .
H102 H 0.7813 0.1407 0.3549 0.109 Uiso 1 1 calc R U . . .
H103 H 0.7426 0.0305 0.3120 0.109 Uiso 1 1 calc R U . . .
C59 C 0.1670(3) 0.2029(3) 0.0835(2) 0.0691(10) Uani 1 1 d . . . . .
H59 H 0.0992 0.1593 0.0512 0.083 Uiso 1 1 calc R U . . .
C74 C 0.1585(4) -0.1268(3) 0.0358(2) 0.0825(13) Uani 1 1 d . . . . .
H74 H 0.0931 -0.1784 0.0376 0.099 Uiso 1 1 calc R U . . .
C25 C 1.1151(3) 0.2036(3) 0.4114(2) 0.0694(11) Uani 1 1 d . . . . .
H25 H 1.1283 0.1444 0.4116 0.083 Uiso 1 1 calc R U . . .
C3 C 0.8747(3) 0.1979(3) 0.1902(2) 0.0773(12) Uani 1 1 d . . . . .
H301 H 0.8424 0.1336 0.1575 0.093 Uiso 1 1 calc R U . . .
H302 H 0.9536 0.2295 0.1980 0.093 Uiso 1 1 calc R U . . .
C5 C 0.6641(3) 0.0648(3) 0.19084(19) 0.0663(10) Uani 1 1 d . . . . .
H501 H 0.5938 0.0257 0.1972 0.080 Uiso 1 1 calc R U . . .
H502 H 0.6924 0.0158 0.1807 0.080 Uiso 1 1 calc R U . . .
C4 C 0.8278(3) 0.2705(3) 0.15852(18) 0.0622(9) Uani 1 1 d . . . . .
H401 H 0.8718 0.3402 0.1856 0.075 Uiso 1 1 calc R U . . .
H402 H 0.8340 0.2734 0.1136 0.075 Uiso 1 1 calc R U . . .
C2 C 0.8574(3) 0.1707(3) 0.2557(2) 0.0647(10) Uani 1 1 d . . . . .
H201 H 0.8775 0.1139 0.2660 0.078 Uiso 1 1 calc R U . . .
H202 H 0.9064 0.2305 0.2920 0.078 Uiso 1 1 calc R U . . .
C42 C 0.3744(3) 0.7272(4) 0.2275(2) 0.0885(14) Uani 1 1 d . . . . .
H42 H 0.3344 0.6793 0.1869 0.106 Uiso 1 1 calc R U . . .
C35 C 0.6222(3) 0.7933(3) 0.5164(2) 0.0717(11) Uani 1 1 d . . . . .
H35 H 0.5801 0.7214 0.5056 0.086 Uiso 1 1 calc R U . . .
B1 B 0.6340(3) 0.7820(3) 0.39080(19) 0.0452(8) Uani 1 1 d . . . . .
B2 B 0.2575(3) 0.1598(3) -0.00224(18) 0.0448(8) Uani 1 1 d . . . . .
C43 C 0.3488(4) 0.8074(4) 0.2406(3) 0.0863(14) Uani 1 1 d . . . . .
H43 H 0.2920 0.8154 0.2087 0.104 Uiso 1 1 calc R U . . .
C10 C 0.6961(3) 0.5716(3) 0.1649(2) 0.0790(12) Uani 1 1 d . . . . .
H10 H 0.7030 0.6324 0.1481 0.095 Uiso 1 1 calc R U . . .
C39 C 0.7202(3) 0.9516(3) 0.4875(2) 0.0752(11) Uani 1 1 d . . . . .
H39 H 0.7457 0.9905 0.4565 0.090 Uiso 1 1 calc R U . . .
C51 C 0.5166(3) 0.5833(3) 0.3928(3) 0.107(2) Uani 1 1 d . . . . .
H51 H 0.4547 0.5970 0.3811 0.128 Uiso 1 1 calc R U . . .
C41 C 0.4624(3) 0.7173(3) 0.2761(2) 0.0724(11) Uani 1 1 d . . . . .
H41 H 0.4788 0.6618 0.2668 0.087 Uiso 1 1 calc R U . . .
C68 C 0.0387(4) 0.2300(4) -0.1297(2) 0.0858(14) Uani 1 1 d . . . . .
H68 H 0.0272 0.2897 -0.1350 0.103 Uiso 1 1 calc R U . . .
C6 C 0.6460(3) 0.1218(3) 0.13011(19) 0.0726(11) Uani 1 1 d . . . . .
H601 H 0.6695 0.0983 0.0955 0.087 Uiso 1 1 calc R U . . .
H602 H 0.5679 0.1045 0.1103 0.087 Uiso 1 1 calc R U . . .
C67 C -0.0314(4) 0.1392(5) -0.1751(2) 0.0903(15) Uani 1 1 d . . . . .
H67 H -0.0899 0.1366 -0.2114 0.108 Uiso 1 1 calc R U . . .
C61 C 0.2650(4) 0.3123(4) 0.1927(2) 0.0901(14) Uani 1 1 d . . . . .
H61 H 0.2648 0.3426 0.2331 0.108 Uiso 1 1 calc R U . . .
C36 C 0.6441(5) 0.8436(5) 0.5804(3) 0.1035(17) Uani 1 1 d . . . . .
H36 H 0.6166 0.8057 0.6112 0.124 Uiso 1 1 calc R U . . .
C44 C 0.4062(4) 0.8751(4) 0.3001(3) 0.0874(14) Uani 1 1 d . . . . .
H44 H 0.3878 0.9291 0.3098 0.105 Uiso 1 1 calc R U . . .
C37 C 0.7050(6) 0.9474(6) 0.5986(3) 0.119(2) Uani 1 1 d . . . . .
H37 H 0.7207 0.9811 0.6421 0.142 Uiso 1 1 calc R U . . .
N8 N 0.1125(7) 0.5300(7) -0.0432(4) 0.211(2) Uani 1 1 d . . . . .
C81 C 0.1302(9) 0.4949(8) 0.0064(6) 0.211(2) Uani 1 1 d . . . . .
C82 C 0.1337(8) 0.4456(7) 0.0609(5) 0.211(2) Uani 1 1 d . . . . .
H821 H 0.0788 0.4468 0.0795 0.317 Uiso 1 1 calc R U . . .
H822 H 0.2056 0.4808 0.0949 0.317 Uiso 1 1 calc R U . . .
H823 H 0.1193 0.3746 0.0466 0.317 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ni2 O4 2.0251(19) . ?
Ni2 O2 2.0431(18) . ?
Ni2 N6 2.069(2) . ?
Ni2 N5 2.072(2) . ?
Ni2 N7 2.093(2) . ?
Ni2 O1 2.2699(19) . ?
Ni2 C15 2.518(3) . ?
Ni1 O3 2.0539(19) . ?
Ni1 N1 2.057(2) . ?
Ni1 N2 2.076(3) . ?
Ni1 N4 2.076(3) . ?
Ni1 N3 2.103(2) . ?
Ni1 O1 2.2391(19) . ?
Ni1 C15 2.490(3) . ?
O1 C15 1.289(3) . ?
O3 C15 1.270(3) . ?
O2 C15 1.284(3) . ?
O4 H4 0.84 . ?
O4 H40 0.84 . ?
N5 C27 1.336(4) . ?
N5 C23 1.336(4) . ?
N1 C12 1.334(4) . ?
N1 C8 1.341(4) . ?
N7 C16 1.475(4) . ?
N7 C17 1.479(4) . ?
N7 C20 1.498(4) . ?
N6 C21 1.478(4) . ?
N6 C19 1.479(4) . ?
N6 C22 1.482(4) . ?
C47 C48 1.381(4) . ?
C47 C46 1.388(4) . ?
C47 H47 0.9300 . ?
N2 C7 1.473(4) . ?
N2 C4 1.482(4) . ?
N2 C6 1.508(4) . ?
C70 C75 1.396(4) . ?
C70 C71 1.398(4) . ?
C70 B2 1.640(5) . ?
C38 C37 1.385(8) . ?
C38 C39 1.392(6) . ?
C38 H38 0.9300 . ?
C52 C53 1.385(4) . ?
C52 C57 1.394(4) . ?
C52 B2 1.648(4) . ?
N3 C2 1.472(4) . ?
N3 C1 1.481(4) . ?
N3 C5 1.484(4) . ?
C28 C33 1.392(4) . ?
C28 C29 1.400(4) . ?
C28 B1 1.648(5) . ?
C30 C31 1.362(5) . ?
C30 C29 1.387(5) . ?
C30 H30 0.9300 . ?
C48 C49 1.343(5) . ?
C48 H48 0.9300 . ?
C46 C51 1.369(5) . ?
C46 B1 1.643(4) . ?
C17 C18 1.508(5) . ?
C17 H171 0.9700 . ?
C17 H172 0.9700 . ?
C57 C56 1.377(5) . ?
C57 H57 0.9300 . ?
C71 C72 1.384(5) . ?
C71 H71 0.9300 . ?
C75 C74 1.379(5) . ?
C75 H75 0.9300 . ?
C64 C65 1.386(5) . ?
C64 C69 1.398(5) . ?
C64 B2 1.651(5) . ?
C26 C25 1.366(5) . ?
C26 C27 1.371(4) . ?
C26 H26 0.9300 . ?
C53 C54 1.389(4) . ?
C53 H53 0.9300 . ?
C12 C11 1.374(4) . ?
C12 H12 0.9300 . ?
C55 C54 1.365(5) . ?
C55 C56 1.366(5) . ?
C55 H55 0.9300 . ?
C65 C66 1.398(5) . ?
C65 H65 0.9300 . ?
C54 H54 0.9300 . ?
C27 H27 0.9300 . ?
N4 C13 1.135(4) . ?
C18 C19 1.517(4) . ?
C18 H181 0.9700 . ?
C18 H182 0.9700 . ?
C23 C24 1.381(4) . ?
C23 C22 1.498(4) . ?
C49 C50 1.361(5) . ?
C49 H49 0.9300 . ?
C14 C13 1.439(5) . ?
C14 H141 0.9600 . ?
C14 H142 0.9600 . ?
C14 H143 0.9600 . ?
C20 C21 1.549(4) . ?
C20 H203 0.9700 . ?
C20 H204 0.9700 . ?
C58 C63 1.392(4) . ?
C58 C59 1.397(4) . ?
C58 B2 1.648(5) . ?
C63 C62 1.386(5) . ?
C63 H63 0.9300 . ?
C29 H29 0.9300 . ?
C32 C31 1.369(5) . ?
C32 C33 1.392(4) . ?
C32 H32 0.9300 . ?
C22 H221 0.9700 . ?
C22 H222 0.9700 . ?
C33 H33 0.9300 . ?
C19 H191 0.9700 . ?
C19 H192 0.9700 . ?
C8 C9 1.376(5) . ?
C8 C7 1.520(5) . ?
C56 H56 0.9300 . ?
C11 C10 1.368(6) . ?
C11 H11 0.9300 . ?
C21 H211 0.9700 . ?
C21 H212 0.9700 . ?
C40 C41 1.372(5) . ?
C40 C45 1.390(4) . ?
C40 B1 1.650(4) . ?
C24 C25 1.376(5) . ?
C24 H24 0.9300 . ?
C69 C68 1.387(5) . ?
C69 H69 0.9300 . ?
C9 C10 1.373(6) . ?
C9 H9 0.9300 . ?
C31 H31 0.9300 . ?
C50 C51 1.384(5) . ?
C50 H50 0.9300 . ?
C72 C73 1.370(6) . ?
C72 H72 0.9300 . ?
C34 C39 1.393(5) . ?
C34 C35 1.399(5) . ?
C34 B1 1.648(5) . ?
C45 C44 1.374(5) . ?
C45 H45 0.9300 . ?
C66 C67 1.357(6) . ?
C66 H66 0.9300 . ?
C16 H161 0.9600 . ?
C16 H162 0.9600 . ?
C16 H163 0.9600 . ?
C62 C61 1.385(6) . ?
C62 H62 0.9300 . ?
C60 C61 1.354(6) . ?
C60 C59 1.380(5) . ?
C60 H60 0.9300 . ?
C73 C74 1.365(6) . ?
C73 H73 0.9300 . ?
C7 H701 0.9700 . ?
C7 H702 0.9700 . ?
C1 H101 0.9600 . ?
C1 H102 0.9600 . ?
C1 H103 0.9600 . ?
C59 H59 0.9300 . ?
C74 H74 0.9300 . ?
C25 H25 0.9300 . ?
C3 C2 1.502(5) . ?
C3 C4 1.514(5) . ?
C3 H301 0.9700 . ?
C3 H302 0.9700 . ?
C5 C6 1.555(5) . ?
C5 H501 0.9700 . ?
C5 H502 0.9700 . ?
C4 H401 0.9700 . ?
C4 H402 0.9700 . ?
C2 H201 0.9700 . ?
C2 H202 0.9700 . ?
C42 C43 1.360(6) . ?
C42 C41 1.416(5) . ?
C42 H42 0.9300 . ?
C35 C36 1.375(6) . ?
C35 H35 0.9300 . ?
C43 C44 1.346(6) . ?
C43 H43 0.9300 . ?
C10 H10 0.9300 . ?
C39 H39 0.9300 . ?
C51 H51 0.9300 . ?
C41 H41 0.9300 . ?
C68 C67 1.367(7) . ?
C68 H68 0.9300 . ?
C6 H601 0.9700 . ?
C6 H602 0.9700 . ?
C67 H67 0.9300 . ?
C61 H61 0.9300 . ?
C36 C37 1.344(8) . ?
C36 H36 0.9300 . ?
C44 H44 0.9300 . ?
C37 H37 0.9300 . ?
N8 C81 1.180(10) . ?
C81 C82 1.367(11) . ?
C82 H821 0.9600 . ?
C82 H822 0.9600 . ?
C82 H823 0.9600 . ?

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
O4 Ni2 O2 93.73(8) . . ?
O4 Ni2 N6 96.08(9) . . ?
O2 Ni2 N6 169.94(9) . . ?
O4 Ni2 N5 93.38(9) . . ?
O2 Ni2 N5 94.27(8) . . ?
N6 Ni2 N5 82.96(9) . . ?
O4 Ni2 N7 93.16(9) . . ?
O2 Ni2 N7 104.00(8) . . ?
N6 Ni2 N7 77.70(9) . . ?
N5 Ni2 N7 160.13(10) . . ?
O4 Ni2 O1 154.71(7) . . ?
O2 Ni2 O1 61.04(7) . . ?
N6 Ni2 O1 109.07(8) . . ?
N5 Ni2 O1 87.29(8) . . ?
N7 Ni2 O1 94.68(8) . . ?
O4 Ni2 C15 124.02(9) . . ?
O2 Ni2 C15 30.49(8) . . ?
N6 Ni2 C15 139.50(9) . . ?
N5 Ni2 C15 88.76(8) . . ?
N7 Ni2 C15 102.98(9) . . ?
O1 Ni2 C15 30.69(7) . . ?
O3 Ni1 N1 95.79(8) . . ?
O3 Ni1 N2 165.91(9) . . ?
N1 Ni1 N2 82.96(10) . . ?
O3 Ni1 N4 95.80(9) . . ?
N1 Ni1 N4 93.05(10) . . ?
N2 Ni1 N4 98.28(11) . . ?
O3 Ni1 N3 101.71(9) . . ?
N1 Ni1 N3 160.68(11) . . ?
N2 Ni1 N3 78.07(11) . . ?
N4 Ni1 N3 93.26(10) . . ?
O3 Ni1 O1 61.55(7) . . ?
N1 Ni1 O1 86.24(8) . . ?
N2 Ni1 O1 104.37(9) . . ?
N4 Ni1 O1 157.07(9) . . ?
N3 Ni1 O1 94.89(8) . . ?
O3 Ni1 C15 30.59(8) . . ?
N1 Ni1 C15 89.34(9) . . ?
N2 Ni1 C15 135.37(10) . . ?
N4 Ni1 C15 126.08(10) . . ?
N3 Ni1 C15 101.57(9) . . ?
O1 Ni1 C15 31.07(7) . . ?
C15 O1 Ni1 85.28(15) . . ?
C15 O1 Ni2 85.35(16) . . ?
Ni1 O1 Ni2 170.60(9) . . ?
C15 O3 Ni1 94.05(16) . . ?
C15 O2 Ni2 95.67(16) . . ?
Ni2 O4 H4 117.4(5) . . ?
Ni2 O4 H40 134(3) . . ?
H4 O4 H40 109(3) . . ?
O3 C15 O2 123.9(2) . . ?
O3 C15 O1 118.7(2) . . ?
O2 C15 O1 117.4(2) . . ?
O3 C15 Ni1 55.36(13) . . ?
O2 C15 Ni1 174.58(17) . . ?
O1 C15 Ni1 63.65(14) . . ?
O3 C15 Ni2 173.48(18) . . ?
O2 C15 Ni2 53.84(13) . . ?
O1 C15 Ni2 63.96(14) . . ?
Ni1 C15 Ni2 127.60(11) . . ?
C27 N5 C23 118.2(2) . . ?
C27 N5 Ni2 128.4(2) . . ?
C23 N5 Ni2 112.57(18) . . ?
C12 N1 C8 118.9(3) . . ?
C12 N1 Ni1 126.9(2) . . ?
C8 N1 Ni1 112.9(2) . . ?
C16 N7 C17 109.8(3) . . ?
C16 N7 C20 110.6(3) . . ?
C17 N7 C20 109.4(2) . . ?
C16 N7 Ni2 113.1(2) . . ?
C17 N7 Ni2 109.20(18) . . ?
C20 N7 Ni2 104.53(16) . . ?
C21 N6 C19 111.9(2) . . ?
C21 N6 C22 112.3(2) . . ?
C19 N6 C22 110.6(2) . . ?
C21 N6 Ni2 107.01(17) . . ?
C19 N6 Ni2 107.61(18) . . ?
C22 N6 Ni2 107.12(17) . . ?
C48 C47 C46 123.4(3) . . ?
C48 C47 H47 118.3 . . ?
C46 C47 H47 118.3 . . ?
C7 N2 C4 110.9(3) . . ?
C7 N2 C6 114.0(3) . . ?
C4 N2 C6 110.3(3) . . ?
C7 N2 Ni1 108.2(2) . . ?
C4 N2 Ni1 108.07(19) . . ?
C6 N2 Ni1 105.1(2) . . ?
C75 C70 C71 113.8(3) . . ?
C75 C70 B2 122.2(3) . . ?
C71 C70 B2 123.9(3) . . ?
C37 C38 C39 119.2(5) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C53 C52 C57 114.2(3) . . ?
C53 C52 B2 125.3(3) . . ?
C57 C52 B2 120.2(3) . . ?
C2 N3 C1 108.6(3) . . ?
C2 N3 C5 110.2(3) . . ?
C1 N3 C5 110.2(3) . . ?
C2 N3 Ni1 110.32(19) . . ?
C1 N3 Ni1 113.2(2) . . ?
C5 N3 Ni1 104.38(19) . . ?
C33 C28 C29 114.1(3) . . ?
C33 C28 B1 123.5(3) . . ?
C29 C28 B1 122.2(3) . . ?
C31 C30 C29 120.0(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C49 C48 C47 120.7(3) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C51 C46 C47 113.5(3) . . ?
C51 C46 B1 123.3(3) . . ?
C47 C46 B1 122.9(3) . . ?
N7 C17 C18 114.1(3) . . ?
N7 C17 H171 108.7 . . ?
C18 C17 H171 108.7 . . ?
N7 C17 H172 108.7 . . ?
C18 C17 H172 108.7 . . ?
H171 C17 H172 107.6 . . ?
C56 C57 C52 123.5(3) . . ?
C56 C57 H57 118.2 . . ?
C52 C57 H57 118.2 . . ?
C72 C71 C70 123.4(3) . . ?
C72 C71 H71 118.3 . . ?
C70 C71 H71 118.3 . . ?
C74 C75 C70 123.5(4) . . ?
C74 C75 H75 118.3 . . ?
C70 C75 H75 118.3 . . ?
C65 C64 C69 115.4(3) . . ?
C65 C64 B2 125.2(3) . . ?
C69 C64 B2 119.2(3) . . ?
C25 C26 C27 118.8(3) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 H26 120.6 . . ?
C52 C53 C54 123.1(3) . . ?
C52 C53 H53 118.5 . . ?
C54 C53 H53 118.5 . . ?
N1 C12 C11 122.6(3) . . ?
N1 C12 H12 118.7 . . ?
C11 C12 H12 118.7 . . ?
C54 C55 C56 118.8(3) . . ?
C54 C55 H55 120.6 . . ?
C56 C55 H55 120.6 . . ?
C64 C65 C66 122.0(4) . . ?
C64 C65 H65 119.0 . . ?
C66 C65 H65 119.0 . . ?
C55 C54 C53 120.2(3) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
N5 C27 C26 122.9(3) . . ?
N5 C27 H27 118.6 . . ?
C26 C27 H27 118.6 . . ?
C13 N4 Ni1 176.1(3) . . ?
C17 C18 C19 116.6(3) . . ?
C17 C18 H181 108.2 . . ?
C19 C18 H181 108.2 . . ?
C17 C18 H182 108.2 . . ?
C19 C18 H182 108.2 . . ?
H181 C18 H182 107.3 . . ?
N5 C23 C24 121.9(3) . . ?
N5 C23 C22 115.6(2) . . ?
C24 C23 C22 122.4(3) . . ?
C48 C49 C50 118.4(3) . . ?
C48 C49 H49 120.8 . . ?
C50 C49 H49 120.8 . . ?
C13 C14 H141 109.5 . . ?
C13 C14 H142 109.5 . . ?
H141 C14 H142 109.5 . . ?
C13 C14 H143 109.5 . . ?
H141 C14 H143 109.5 . . ?
H142 C14 H143 109.5 . . ?
N7 C20 C21 112.0(2) . . ?
N7 C20 H203 109.2 . . ?
C21 C20 H203 109.2 . . ?
N7 C20 H204 109.2 . . ?
C21 C20 H204 109.2 . . ?
H203 C20 H204 107.9 . . ?
C63 C58 C59 114.3(3) . . ?
C63 C58 B2 125.1(3) . . ?
C59 C58 B2 120.4(3) . . ?
C62 C63 C58 124.1(3) . . ?
C62 C63 H63 117.9 . . ?
C58 C63 H63 117.9 . . ?
C30 C29 C28 123.5(4) . . ?
C30 C29 H29 118.3 . . ?
C28 C29 H29 118.3 . . ?
C31 C32 C33 120.2(4) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
N6 C22 C23 112.0(2) . . ?
N6 C22 H221 109.2 . . ?
C23 C22 H221 109.2 . . ?
N6 C22 H222 109.2 . . ?
C23 C22 H222 109.2 . . ?
H221 C22 H222 107.9 . . ?
C28 C33 C32 123.0(3) . . ?
C28 C33 H33 118.5 . . ?
C32 C33 H33 118.5 . . ?
N6 C19 C18 112.9(3) . . ?
N6 C19 H191 109.0 . . ?
C18 C19 H191 109.0 . . ?
N6 C19 H192 109.0 . . ?
C18 C19 H192 109.0 . . ?
H191 C19 H192 107.8 . . ?
N1 C8 C9 120.9(3) . . ?
N1 C8 C7 115.3(3) . . ?
C9 C8 C7 123.6(3) . . ?
C55 C56 C57 120.1(3) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C10 C11 C12 118.5(4) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
N6 C21 C20 109.7(2) . . ?
N6 C21 H211 109.7 . . ?
C20 C21 H211 109.7 . . ?
N6 C21 H212 109.7 . . ?
C20 C21 H212 109.7 . . ?
H211 C21 H212 108.2 . . ?
C41 C40 C45 114.3(3) . . ?
C41 C40 B1 123.3(3) . . ?
C45 C40 B1 122.3(3) . . ?
C25 C24 C23 119.0(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C68 C69 C64 122.1(4) . . ?
C68 C69 H69 118.9 . . ?
C64 C69 H69 118.9 . . ?
C10 C9 C8 119.7(4) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N4 C13 C14 179.4(4) . . ?
C30 C31 C32 119.3(3) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C49 C50 C51 120.2(4) . . ?
C49 C50 H50 119.9 . . ?
C51 C50 H50 119.9 . . ?
C73 C72 C71 119.9(4) . . ?
C73 C72 H72 120.0 . . ?
C71 C72 H72 120.0 . . ?
C39 C34 C35 113.8(4) . . ?
C39 C34 B1 123.1(3) . . ?
C35 C34 B1 123.1(3) . . ?
C44 C45 C40 123.9(4) . . ?
C44 C45 H45 118.0 . . ?
C40 C45 H45 118.0 . . ?
C67 C66 C65 121.0(4) . . ?
C67 C66 H66 119.5 . . ?
C65 C66 H66 119.5 . . ?
N7 C16 H161 109.5 . . ?
N7 C16 H162 109.5 . . ?
H161 C16 H162 109.5 . . ?
N7 C16 H163 109.5 . . ?
H161 C16 H163 109.5 . . ?
H162 C16 H163 109.5 . . ?
C61 C62 C63 118.6(4) . . ?
C61 C62 H62 120.7 . . ?
C63 C62 H62 120.7 . . ?
C61 C60 C59 121.2(4) . . ?
C61 C60 H60 119.4 . . ?
C59 C60 H60 119.4 . . ?
C74 C73 C72 119.0(4) . . ?
C74 C73 H73 120.5 . . ?
C72 C73 H73 120.5 . . ?
N2 C7 C8 111.0(3) . . ?
N2 C7 H701 109.4 . . ?
C8 C7 H701 109.4 . . ?
N2 C7 H702 109.4 . . ?
C8 C7 H702 109.4 . . ?
H701 C7 H702 108.0 . . ?
N3 C1 H101 109.5 . . ?
N3 C1 H102 109.5 . . ?
H101 C1 H102 109.5 . . ?
N3 C1 H103 109.5 . . ?
H101 C1 H103 109.5 . . ?
H102 C1 H103 109.5 . . ?
C60 C59 C58 122.5(4) . . ?
C60 C59 H59 118.8 . . ?
C58 C59 H59 118.8 . . ?
C73 C74 C75 120.3(4) . . ?
C73 C74 H74 119.8 . . ?
C75 C74 H74 119.8 . . ?
C26 C25 C24 119.2(3) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C2 C3 C4 116.8(3) . . ?
C2 C3 H301 108.1 . . ?
C4 C3 H301 108.1 . . ?
C2 C3 H302 108.1 . . ?
C4 C3 H302 108.1 . . ?
H301 C3 H302 107.3 . . ?
N3 C5 C6 111.3(3) . . ?
N3 C5 H501 109.4 . . ?
C6 C5 H501 109.4 . . ?
N3 C5 H502 109.4 . . ?
C6 C5 H502 109.4 . . ?
H501 C5 H502 108.0 . . ?
N2 C4 C3 113.5(3) . . ?
N2 C4 H401 108.9 . . ?
C3 C4 H401 108.9 . . ?
N2 C4 H402 108.9 . . ?
C3 C4 H402 108.9 . . ?
H401 C4 H402 107.7 . . ?
N3 C2 C3 113.5(3) . . ?
N3 C2 H201 108.9 . . ?
C3 C2 H201 108.9 . . ?
N3 C2 H202 108.9 . . ?
C3 C2 H202 108.9 . . ?
H201 C2 H202 107.7 . . ?
C43 C42 C41 119.5(4) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C36 C35 C34 123.8(5) . . ?
C36 C35 H35 118.1 . . ?
C34 C35 H35 118.1 . . ?
C46 B1 C34 107.6(3) . . ?
C46 B1 C28 107.7(2) . . ?
C34 B1 C28 110.7(3) . . ?
C46 B1 C40 112.2(3) . . ?
C34 B1 C40 109.6(2) . . ?
C28 B1 C40 108.9(3) . . ?
C70 B2 C58 105.6(2) . . ?
C70 B2 C52 111.3(2) . . ?
C58 B2 C52 114.1(3) . . ?
C70 B2 C64 112.9(3) . . ?
C58 B2 C64 110.0(2) . . ?
C52 B2 C64 103.1(2) . . ?
C44 C43 C42 119.6(4) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C11 C10 C9 119.3(4) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C38 C39 C34 123.2(4) . . ?
C38 C39 H39 118.4 . . ?
C34 C39 H39 118.4 . . ?
C46 C51 C50 123.8(3) . . ?
C46 C51 H51 118.1 . . ?
C50 C51 H51 118.1 . . ?
C40 C41 C42 122.6(4) . . ?
C40 C41 H41 118.7 . . ?
C42 C41 H41 118.7 . . ?
C67 C68 C69 120.9(4) . . ?
C67 C68 H68 119.6 . . ?
C69 C68 H68 119.6 . . ?
N2 C6 C5 110.9(3) . . ?
N2 C6 H601 109.5 . . ?
C5 C6 H601 109.5 . . ?
N2 C6 H602 109.5 . . ?
C5 C6 H602 109.5 . . ?
H601 C6 H602 108.0 . . ?
C66 C67 C68 118.6(4) . . ?
C66 C67 H67 120.7 . . ?
C68 C67 H67 120.7 . . ?
C60 C61 C62 119.3(4) . . ?
C60 C61 H61 120.3 . . ?
C62 C61 H61 120.3 . . ?
C37 C36 C35 120.3(5) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C43 C44 C45 120.1(4) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C36 C37 C38 119.6(5) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
N8 C81 C82 171.3(13) . . ?
C81 C82 H821 109.5 . . ?
C81 C82 H822 109.5 . . ?
H821 C82 H822 109.5 . . ?
C81 C82 H823 109.5 . . ?
H821 C82 H823 109.5 . . ?
H822 C82 H823 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O3 C15 O2 173.5(2) . . . . ?
Ni1 O3 C15 O1 -6.5(2) . . . . ?
Ni2 O2 C15 O3 172.5(2) . . . . ?
Ni2 O2 C15 O1 -7.4(2) . . . . ?
Ni1 O1 C15 O3 6.0(2) . . . . ?
Ni2 O1 C15 O3 -173.3(2) . . . . ?
Ni1 O1 C15 O2 -174.0(2) . . . . ?
Ni2 O1 C15 O2 6.7(2) . . . . ?
Ni2 O1 C15 Ni1 -179.27(7) . . . . ?
Ni1 O1 C15 Ni2 179.27(7) . . . . ?
C46 C47 C48 C49 0.7(6) . . . . ?
C48 C47 C46 C51 -0.6(5) . . . . ?
C48 C47 C46 B1 173.1(3) . . . . ?
C16 N7 C17 C18 167.1(3) . . . . ?
C20 N7 C17 C18 45.4(3) . . . . ?
Ni2 N7 C17 C18 -68.4(3) . . . . ?
C53 C52 C57 C56 0.6(5) . . . . ?
B2 C52 C57 C56 174.4(3) . . . . ?
C75 C70 C71 C72 1.1(5) . . . . ?
B2 C70 C71 C72 176.6(3) . . . . ?
C71 C70 C75 C74 -2.3(5) . . . . ?
B2 C70 C75 C74 -177.9(3) . . . . ?
C57 C52 C53 C54 -0.4(5) . . . . ?
B2 C52 C53 C54 -173.7(3) . . . . ?
C8 N1 C12 C11 -2.0(5) . . . . ?
Ni1 N1 C12 C11 164.5(2) . . . . ?
C69 C64 C65 C66 -0.7(5) . . . . ?
B2 C64 C65 C66 -176.1(3) . . . . ?
C56 C55 C54 C53 0.3(6) . . . . ?
C52 C53 C54 C55 -0.1(6) . . . . ?
C23 N5 C27 C26 -2.1(5) . . . . ?
Ni2 N5 C27 C26 166.4(2) . . . . ?
C25 C26 C27 N5 0.4(5) . . . . ?
N7 C17 C18 C19 46.1(4) . . . . ?
C27 N5 C23 C24 3.0(5) . . . . ?
Ni2 N5 C23 C24 -167.2(3) . . . . ?
C27 N5 C23 C22 -171.9(3) . . . . ?
Ni2 N5 C23 C22 17.8(3) . . . . ?
C47 C48 C49 C50 -0.3(7) . . . . ?
C16 N7 C20 C21 158.2(3) . . . . ?
C17 N7 C20 C21 -80.7(3) . . . . ?
Ni2 N7 C20 C21 36.2(3) . . . . ?
C59 C58 C63 C62 -1.6(5) . . . . ?
B2 C58 C63 C62 -175.8(3) . . . . ?
C31 C30 C29 C28 0.8(5) . . . . ?
C33 C28 C29 C30 -0.5(4) . . . . ?
B1 C28 C29 C30 174.9(3) . . . . ?
C21 N6 C22 C23 149.0(3) . . . . ?
C19 N6 C22 C23 -85.2(3) . . . . ?
Ni2 N6 C22 C23 31.8(3) . . . . ?
N5 C23 C22 N6 -34.3(4) . . . . ?
C24 C23 C22 N6 150.8(3) . . . . ?
C29 C28 C33 C32 0.1(4) . . . . ?
B1 C28 C33 C32 -175.2(3) . . . . ?
C31 C32 C33 C28 -0.1(5) . . . . ?
C21 N6 C19 C18 -43.7(3) . . . . ?
C22 N6 C19 C18 -169.7(3) . . . . ?
Ni2 N6 C19 C18 73.6(3) . . . . ?
C17 C18 C19 N6 -48.6(4) . . . . ?
C12 N1 C8 C9 3.9(4) . . . . ?
Ni1 N1 C8 C9 -164.5(3) . . . . ?
C12 N1 C8 C7 -171.3(3) . . . . ?
Ni1 N1 C8 C7 20.4(3) . . . . ?
C54 C55 C56 C57 0.0(6) . . . . ?
C52 C57 C56 C55 -0.5(6) . . . . ?
N1 C12 C11 C10 -0.6(5) . . . . ?
C19 N6 C21 C20 81.1(3) . . . . ?
C22 N6 C21 C20 -153.8(3) . . . . ?
Ni2 N6 C21 C20 -36.6(3) . . . . ?
N7 C20 C21 N6 -0.4(4) . . . . ?
N5 C23 C24 C25 -2.3(5) . . . . ?
C22 C23 C24 C25 172.3(4) . . . . ?
C65 C64 C69 C68 1.0(5) . . . . ?
B2 C64 C69 C68 176.7(3) . . . . ?
N1 C8 C9 C10 -3.1(5) . . . . ?
C7 C8 C9 C10 171.6(4) . . . . ?
C29 C30 C31 C32 -0.8(5) . . . . ?
C33 C32 C31 C30 0.4(5) . . . . ?
C48 C49 C50 C51 -0.2(9) . . . . ?
C70 C71 C72 C73 0.5(6) . . . . ?
C41 C40 C45 C44 -1.1(5) . . . . ?
B1 C40 C45 C44 174.9(3) . . . . ?
C64 C65 C66 C67 0.4(6) . . . . ?
C58 C63 C62 C61 1.4(6) . . . . ?
C71 C72 C73 C74 -0.9(6) . . . . ?
C4 N2 C7 C8 -88.3(3) . . . . ?
C6 N2 C7 C8 146.5(3) . . . . ?
Ni1 N2 C7 C8 30.0(4) . . . . ?
N1 C8 C7 N2 -34.6(4) . . . . ?
C9 C8 C7 N2 150.4(3) . . . . ?
C61 C60 C59 C58 1.4(7) . . . . ?
C63 C58 C59 C60 0.2(5) . . . . ?
B2 C58 C59 C60 174.7(4) . . . . ?
C72 C73 C74 C75 -0.3(7) . . . . ?
C70 C75 C74 C73 2.0(6) . . . . ?
C27 C26 C25 C24 0.4(6) . . . . ?
C23 C24 C25 C26 0.5(6) . . . . ?
C2 N3 C5 C6 -80.3(3) . . . . ?
C1 N3 C5 C6 159.9(3) . . . . ?
Ni1 N3 C5 C6 38.2(3) . . . . ?
C7 N2 C4 C3 -168.7(3) . . . . ?
C6 N2 C4 C3 -41.5(4) . . . . ?
Ni1 N2 C4 C3 72.8(3) . . . . ?
C2 C3 C4 N2 -49.8(5) . . . . ?
C1 N3 C2 C3 166.9(3) . . . . ?
C5 N3 C2 C3 46.1(4) . . . . ?
Ni1 N3 C2 C3 -68.6(3) . . . . ?
C4 C3 C2 N3 47.3(5) . . . . ?
C39 C34 C35 C36 -1.1(5) . . . . ?
B1 C34 C35 C36 179.0(4) . . . . ?
C51 C46 B1 C34 86.1(5) . . . . ?
C47 C46 B1 C34 -87.1(4) . . . . ?
C51 C46 B1 C28 -154.6(4) . . . . ?
C47 C46 B1 C28 32.3(4) . . . . ?
C51 C46 B1 C40 -34.7(5) . . . . ?
C47 C46 B1 C40 152.2(3) . . . . ?
C39 C34 B1 C46 153.6(3) . . . . ?
C35 C34 B1 C46 -26.5(4) . . . . ?
C39 C34 B1 C28 36.1(4) . . . . ?
C35 C34 B1 C28 -144.0(3) . . . . ?
C39 C34 B1 C40 -84.1(4) . . . . ?
C35 C34 B1 C40 95.8(3) . . . . ?
C33 C28 B1 C46 88.8(3) . . . . ?
C29 C28 B1 C46 -86.1(3) . . . . ?
C33 C28 B1 C34 -153.8(3) . . . . ?
C29 C28 B1 C34 31.2(4) . . . . ?
C33 C28 B1 C40 -33.1(4) . . . . ?
C29 C28 B1 C40 151.9(3) . . . . ?
C41 C40 B1 C46 -39.7(4) . . . . ?
C45 C40 B1 C46 144.6(3) . . . . ?
C41 C40 B1 C34 -159.2(3) . . . . ?
C45 C40 B1 C34 25.1(4) . . . . ?
C41 C40 B1 C28 79.5(4) . . . . ?
C45 C40 B1 C28 -96.2(4) . . . . ?
C75 C70 B2 C58 74.0(4) . . . . ?
C71 C70 B2 C58 -101.2(3) . . . . ?
C75 C70 B2 C52 -161.7(3) . . . . ?
C71 C70 B2 C52 23.1(4) . . . . ?
C75 C70 B2 C64 -46.3(4) . . . . ?
C71 C70 B2 C64 138.5(3) . . . . ?
C63 C58 B2 C70 89.8(4) . . . . ?
C59 C58 B2 C70 -84.1(3) . . . . ?
C63 C58 B2 C52 -32.8(4) . . . . ?
C59 C58 B2 C52 153.3(3) . . . . ?
C63 C58 B2 C64 -148.1(3) . . . . ?
C59 C58 B2 C64 38.0(4) . . . . ?
C53 C52 B2 C70 -142.1(3) . . . . ?
C57 C52 B2 C70 44.9(4) . . . . ?
C53 C52 B2 C58 -22.8(4) . . . . ?
C57 C52 B2 C58 164.3(3) . . . . ?
C53 C52 B2 C64 96.5(4) . . . . ?
C57 C52 B2 C64 -76.5(3) . . . . ?
C65 C64 B2 C70 -17.1(4) . . . . ?
C69 C64 B2 C70 167.6(3) . . . . ?
C65 C64 B2 C58 -134.8(3) . . . . ?
C69 C64 B2 C58 49.9(4) . . . . ?
C65 C64 B2 C52 103.2(3) . . . . ?
C69 C64 B2 C52 -72.1(3) . . . . ?
C41 C42 C43 C44 -1.1(7) . . . . ?
C12 C11 C10 C9 1.4(6) . . . . ?
C8 C9 C10 C11 0.4(6) . . . . ?
C37 C38 C39 C34 -1.5(7) . . . . ?
C35 C34 C39 C38 2.0(6) . . . . ?
B1 C34 C39 C38 -178.2(4) . . . . ?
C47 C46 C51 C50 0.1(8) . . . . ?
B1 C46 C51 C50 -173.6(5) . . . . ?
C49 C50 C51 C46 0.3(10) . . . . ?
C45 C40 C41 C42 1.5(5) . . . . ?
B1 C40 C41 C42 -174.4(3) . . . . ?
C43 C42 C41 C40 -0.5(6) . . . . ?
C64 C69 C68 C67 -1.0(6) . . . . ?
C7 N2 C6 C5 -154.0(3) . . . . ?
C4 N2 C6 C5 80.5(4) . . . . ?
Ni1 N2 C6 C5 -35.7(3) . . . . ?
N3 C5 C6 N2 -2.0(4) . . . . ?
C65 C66 C67 C68 -0.4(6) . . . . ?
C69 C68 C67 C66 0.7(7) . . . . ?
C59 C60 C61 C62 -1.7(7) . . . . ?
C63 C62 C61 C60 0.3(7) . . . . ?
C34 C35 C36 C37 -0.3(7) . . . . ?
C42 C43 C44 C45 1.6(7) . . . . ?
C40 C45 C44 C43 -0.4(7) . . . . ?
C35 C36 C37 C38 0.9(9) . . . . ?
C39 C38 C37 C36 -0.1(8) . . . . ?

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
O4 H4 O2 0.84 1.770(3) 2.608(3) 175.0(7) 2_766

_refine_diff_density_max         0.478
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.051

_shelxl_version_number           2014/6



