# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

 
data_a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C68 H69.69 N24.33 Ni5 O13' 
_chemical_formula_weight          1729.36 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'   0.3393   1.1124 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    19.8290(2) 
_cell_length_b                    14.3210(2) 
_cell_length_c                    28.6903(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.0550(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      8145.84(16) 
_cell_formula_units_Z             4  
_cell_measurement_temperature     120.01(10) 
_cell_measurement_reflns_used   18966
_cell_measurement_theta_min     2.2267
_cell_measurement_theta_max     74.2529 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.417 
_exptl_crystal_density_method     'not measured'   
_exptl_crystal_F_000              3589 
_exptl_absorpt_coefficient_mu     1.874  
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.15918 
_exptl_absorpt_correction_T_max   1.00000 
_exptl_absorpt_process_details    none 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120.01(10) 
_diffrn_radiation_wavelength      1.5418 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'SuperNova (Cu) X-ray Source' 
_diffrn_radiation_monochromator   mirror 
_diffrn_measurement_device_type   'SuperNova' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  none  
_diffrn_standards_number          none 
_diffrn_standards_interval_count  none 
_diffrn_standards_interval_time   none 
_diffrn_standards_decay_%         none
_diffrn_reflns_number             31793 
_diffrn_reflns_av_R_equivalents   0.0208 
_diffrn_reflns_av_sigmaI/netI     0.0222 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -34 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          2.2267 
_diffrn_reflns_theta_max          74.2529
_reflns_number_total              14315 
_reflns_number_gt                 12881 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrysAlisPro, Agilent Technologies' 
_computing_cell_refinement        'CrysAlisPro, Agilent Technologies' 
_computing_data_reduction         'CrysAlisPro, Agilent Technologies'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'CrysAlisPro, Agilent Technologies' 
_computing_publication_material   'CrysAlisPro, Agilent Technologies'
 
_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. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1416P)²+25.0388P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          14315 
_refine_ls_number_parameters      945 
_refine_ls_number_restraints      33 
_refine_ls_R_factor_all           0.0761 
_refine_ls_R_factor_gt            0.0716 
_refine_ls_wR_factor_ref          0.2165 
_refine_ls_wR_factor_gt           0.2109 
_refine_ls_goodness_of_fit_ref    1.044 
_refine_ls_restrained_S_all       1.133 
_refine_ls_shift/su_max           0.023 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni1 Ni 0.77885(3) 1.01883(5) 0.18785(3) 0.0356(2) Uani 1 1 d U . . 
Ni2 Ni 0.56296(3) 1.25168(5) 0.09287(2) 0.03203(19) Uani 1 1 d D . . 
Ni3 Ni 0.64205(4) 1.32371(5) 0.29200(2) 0.0349(2) Uani 1 1 d . B . 
Ni4 Ni 0.83457(3) 1.41858(5) 0.13997(2) 0.03352(19) Uani 1 1 d . . . 
Ni5 Ni 0.70489(3) 1.25120(4) 0.17827(2) 0.02936(19) Uani 1 1 d . . . 
O1B O 0.4857(3) 1.1562(5) 0.08639(19) 0.0237(15) Uiso 0.67 1 d PU A 1 
O3 O 1.00457(17) 0.9906(3) 0.38409(13) 0.0336(8) Uani 1 1 d . . . 
O4 O 0.59502(16) 1.4570(2) 0.30073(11) 0.0261(7) Uani 1 1 d U . . 
O5 O 0.82387(16) 1.9154(2) 0.14526(11) 0.0234(6) Uani 1 1 d . . . 
O6 O 0.67640(16) 1.3393(2) 0.36286(10) 0.0262(7) Uani 1 1 d . . . 
O7 O 0.57751(17) 1.2778(2) 0.34507(10) 0.0267(7) Uani 1 1 d . . . 
O8 O 0.87928(16) 1.4319(2) 0.07545(11) 0.0270(7) Uani 1 1 d . . . 
H8A H 0.8709 1.3830 0.0582 0.040 Uiso 1 1 d R . . 
H8B H 0.9230 1.4373 0.0786 0.040 Uiso 1 1 d R . . 
O9 O 1.07243(15) 0.9387(2) 0.32779(11) 0.0239(7) Uani 1 1 d . . . 
O10 O 0.74650(15) 1.8784(2) 0.19648(12) 0.0247(7) Uani 1 1 d . . . 
O11B O 0.3958(4) 1.2352(5) 0.0602(2) 0.0382(18) Uiso 0.67 1 d P A 1 
N1 N 0.5250(3) 1.5253(5) 0.2539(2) 0.0437(17) Uiso 0.67 1 d PDU B 1 
N2 N 0.81769(19) 1.5652(3) 0.13906(14) 0.0229(8) Uani 1 1 d . . . 
N3 N 0.54918(17) 1.2630(3) 0.16415(12) 0.0187(7) Uani 1 1 d . . . 
N4 N 0.63848(17) 1.3495(2) 0.09499(11) 0.0164(7) Uani 1 1 d . . . 
N5 N 0.83058(18) 1.1320(2) 0.16585(13) 0.0203(7) Uani 1 1 d U . . 
N6 N 0.85983(19) 0.9947(3) 0.23864(15) 0.0264(8) Uani 1 1 d . . . 
N7 N 0.70075(18) 1.0475(3) 0.13983(13) 0.0220(8) Uani 1 1 d . . . 
N8 N 0.62621(17) 1.1390(2) 0.10442(12) 0.0174(7) Uani 1 1 d . A . 
N9 N 0.68721(18) 1.1939(3) 0.28296(12) 0.0199(7) Uani 1 1 d . . . 
N10 N 0.72664(18) 1.0802(2) 0.23992(13) 0.0190(7) Uani 1 1 d . . . 
N11 N 0.71711(18) 1.3889(3) 0.25914(12) 0.0198(7) Uani 1 1 d . . . 
N12 N 0.79305(18) 1.4185(2) 0.20582(12) 0.0195(7) Uani 1 1 d . . . 
N13 N 0.58049(19) 1.2590(3) 0.51945(12) 0.0208(8) Uani 1 1 d . . . 
N14 N 0.58116(17) 1.2952(2) 0.23650(11) 0.0156(7) Uani 1 1 d . . . 
N15 N 0.85120(17) 1.2764(3) 0.14450(13) 0.0189(7) Uani 1 1 d . . . 
N16 N 0.60148(16) 1.2782(2) 0.19332(11) 0.0143(7) Uani 1 1 d . . . 
N17 N 0.74225(17) 1.4011(2) 0.10690(12) 0.0177(7) Uani 1 1 d . . . 
N18 N 0.80567(17) 1.2176(2) 0.16157(12) 0.0166(7) Uani 1 1 d . . . 
N19 N 0.67394(16) 1.1332(2) 0.13791(11) 0.0153(7) Uani 1 1 d . . . 
N20 N 0.70794(16) 1.1690(2) 0.24065(12) 0.0169(7) Uani 1 1 d . . . 
N21 N 0.69537(16) 1.3394(2) 0.11966(11) 0.0143(7) Uani 1 1 d . . . 
N22 N 0.74129(16) 1.3647(2) 0.21763(11) 0.0158(7) Uani 1 1 d . . . 
C2B C 0.4454(7) 1.5588(12) 0.2507(7) 0.033(4) Uiso 0.33 1 d PD B 2 
H2BA H 0.4452 1.5256 0.2216 0.050 Uiso 0.33 1 calc PR B 2 
H2BB H 0.4534 1.6239 0.2451 0.050 Uiso 0.33 1 calc PR B 2 
H2BC H 0.4026 1.5512 0.2653 0.050 Uiso 0.33 1 calc PR B 2 
C3 C 0.5389(4) 1.4949(5) 0.2898(3) 0.0281(15) Uiso 0.67 1 d PDU B 1 
C4 C 0.4826(4) 1.5076(5) 0.3224(3) 0.0592(18) Uani 1 1 d DU . . 
H4AA H 0.4455 1.5376 0.3065 0.089 Uiso 0.67 1 calc PR B 1 
H4AB H 0.4974 1.5457 0.3482 0.089 Uiso 0.67 1 calc PR B 1 
H4AC H 0.4684 1.4478 0.3338 0.089 Uiso 0.67 1 calc PR B 1 
H4BD H 0.4375 1.5295 0.3273 0.089 Uiso 0.33 1 d PR B 2 
H4BE H 0.5133 1.5405 0.3429 0.089 Uiso 0.33 1 d PR B 2 
H4BF H 0.4850 1.4419 0.3290 0.089 Uiso 0.33 1 d PR B 2 
C5 C 0.6950(4) 1.0133(4) 0.3759(2) 0.0514(16) Uani 1 1 d . B . 
H5 H 0.6885 1.0017 0.4074 0.062 Uiso 1 1 calc R . . 
C6 C 0.5819(3) 1.5214(5) 0.2158(2) 0.0479(14) Uani 1 1 d DU . . 
H6AA H 0.5651 1.5481 0.1872 0.072 Uiso 0.67 1 calc PR B 1 
H6AB H 0.5946 1.4576 0.2106 0.072 Uiso 0.67 1 calc PR B 1 
H6AC H 0.6206 1.5561 0.2267 0.072 Uiso 0.67 1 calc PR B 1 
H6BD H 0.5440 1.5495 0.2001 0.072 Uiso 0.33 1 d PR B 2 
H6BE H 0.5949 1.4658 0.1995 0.072 Uiso 0.33 1 d PR B 2 
H6BF H 0.6190 1.5646 0.2166 0.072 Uiso 0.33 1 d PR B 2 
C7 C 1.0054(3) 1.0882(4) 0.1314(3) 0.0491(16) Uani 1 1 d . . . 
H7 H 1.0391 1.0433 0.1291 0.059 Uiso 1 1 calc R . . 
C9 C 0.9453(3) 0.9043(4) 0.2776(2) 0.0375(12) Uani 1 1 d . . . 
H9 H 0.9687 0.8481 0.2798 0.045 Uiso 1 1 calc R . . 
C10 C 0.7181(4) 0.9406(4) 0.3473(2) 0.0481(15) Uani 1 1 d . B . 
H10 H 0.7249 0.8817 0.3601 0.058 Uiso 1 1 calc R . . 
C11 C 0.9721(3) 1.2504(4) 0.1199(2) 0.0353(12) Uani 1 1 d . . . 
H11 H 0.9812 1.3109 0.1100 0.042 Uiso 1 1 calc R B . 
C12 C 0.5876(3) 0.9305(4) 0.0344(2) 0.0454(15) Uani 1 1 d . . . 
H12 H 0.5608 0.9069 0.0102 0.055 Uiso 1 1 calc R . . 
C13 C 0.6341(4) 0.8717(4) 0.0562(3) 0.063(2) Uani 1 1 d . . . 
H13 H 0.6378 0.8103 0.0460 0.076 Uiso 1 1 calc R . . 
C14 C 0.7946(3) 1.5891(5) 0.3207(2) 0.0457(15) Uani 1 1 d . B . 
H14 H 0.7927 1.6268 0.3470 0.055 Uiso 1 1 calc R . . 
C15 C 0.6308(3) 1.5359(4) 0.0059(2) 0.0430(14) Uani 1 1 d . . . 
H15 H 0.6035 1.5657 -0.0162 0.052 Uiso 1 1 calc R . . 
C16 C 0.3782(3) 1.2680(5) 0.2143(2) 0.0397(13) Uani 1 1 d . . . 
H16 H 0.3324 1.2605 0.2080 0.048 Uiso 1 1 calc R . . 
C17 C 0.6976(3) 1.5673(4) 0.0128(2) 0.0447(14) Uani 1 1 d . B . 
H17 H 0.7130 1.6169 -0.0050 0.054 Uiso 1 1 calc R . . 
C18 C 0.7490(3) 1.5175(4) 0.31539(18) 0.0370(12) Uani 1 1 d . . . 
H18 H 0.7164 1.5056 0.3376 0.044 Uiso 1 1 calc R B . 
C19 C 1.0195(3) 1.1810(4) 0.1179(3) 0.0475(15) Uani 1 1 d . B . 
H19 H 1.0624 1.1954 0.1073 0.057 Uiso 1 1 calc R . . 
C20 C 0.8442(3) 1.6069(4) 0.2873(2) 0.0449(14) Uani 1 1 d . . . 
H20 H 0.8737 1.6565 0.2923 0.054 Uiso 1 1 calc R B . 
C21 C 0.8506(3) 1.5539(4) 0.24781(19) 0.0360(12) Uani 1 1 d . B . 
H21 H 0.8843 1.5652 0.2264 0.043 Uiso 1 1 calc R . . 
C22 C 0.5315(2) 1.2514(3) 0.48686(16) 0.0250(10) Uani 1 1 d . . . 
H22 H 0.4883 1.2361 0.4963 0.030 Uiso 1 1 calc R . . 
C23 C 0.9444(3) 1.0625(4) 0.1477(2) 0.0384(12) Uani 1 1 d . B . 
H23 H 0.9351 1.0012 0.1561 0.046 Uiso 1 1 calc R . . 
C24 C 0.6819(3) 1.1015(4) 0.35843(19) 0.0425(13) Uani 1 1 d . . . 
H24 H 0.6657 1.1489 0.3773 0.051 Uiso 1 1 calc R B . 
C25 C 0.9267(3) 1.0596(4) 0.3006(2) 0.0434(14) Uani 1 1 d . . . 
H25 H 0.9366 1.1110 0.3194 0.052 Uiso 1 1 calc R . . 
C26 C 0.6578(2) 1.2971(4) 0.45898(16) 0.0286(10) Uani 1 1 d . B . 
H26 H 0.7015 1.3127 0.4506 0.034 Uiso 1 1 calc R . . 
C27 C 0.8941(3) 0.9156(4) 0.2446(2) 0.0362(12) Uani 1 1 d . . . 
H27 H 0.8831 0.8651 0.2255 0.043 Uiso 1 1 calc R . . 
C28 C 0.6048(3) 1.4627(4) 0.03076(18) 0.0334(11) Uani 1 1 d . A . 
H28 H 0.5610 1.4416 0.0256 0.040 Uiso 1 1 calc R . . 
C29 C 0.8774(3) 1.0657(4) 0.2662(2) 0.0410(13) Uani 1 1 d . . . 
H29 H 0.8552 1.1224 0.2621 0.049 Uiso 1 1 calc R . . 
C30 C 0.6747(4) 0.9017(4) 0.0924(3) 0.063(2) Uani 1 1 d . A . 
H30 H 0.7051 0.8616 0.1072 0.075 Uiso 1 1 calc R . . 
C31 C 0.5800(2) 1.0205(4) 0.04688(17) 0.0295(10) Uani 1 1 d . . . 
H31 H 0.5488 1.0591 0.0319 0.035 Uiso 1 1 calc R . . 
C32 C 0.7308(3) 0.9545(4) 0.30080(19) 0.0358(11) Uani 1 1 d . . . 
H32 H 0.7469 0.9067 0.2821 0.043 Uiso 1 1 calc R B . 
C33 C 0.8579(2) 1.7222(3) 0.13655(18) 0.0271(10) Uani 1 1 d . . . 
H33 H 0.8921 1.7636 0.1289 0.032 Uiso 1 1 calc R . . 
C34 C 0.7474(2) 1.6901(3) 0.16437(18) 0.0279(10) Uani 1 1 d . . . 
H34 H 0.7064 1.7097 0.1763 0.034 Uiso 1 1 calc R . . 
C35 C 0.7401(3) 1.5274(4) 0.04461(19) 0.0364(12) Uani 1 1 d . . . 
H35 H 0.7844 1.5475 0.0486 0.044 Uiso 1 1 calc R B . 
C36 C 0.5423(3) 1.2655(4) 0.43965(16) 0.0284(10) Uani 1 1 d . B . 
H36 H 0.5073 1.2582 0.4180 0.034 Uiso 1 1 calc R . . 
C37 C 0.8955(2) 1.1341(3) 0.15128(18) 0.0258(9) Uani 1 1 d . . . 
C38 C 0.4229(2) 1.2562(5) 0.17864(19) 0.0382(13) Uani 1 1 d . A . 
H38 H 0.4086 1.2408 0.1486 0.046 Uiso 1 1 calc R . . 
C39 C 0.3990(2) 1.2908(3) 0.25984(17) 0.0275(10) Uani 1 1 d . A . 
H39 H 0.3666 1.2994 0.2825 0.033 Uiso 1 1 calc R . . 
C40 C 1.0173(2) 0.9684(3) 0.34322(18) 0.0271(10) Uani 1 1 d . . . 
C41 C 0.7540(2) 1.4630(3) 0.27467(16) 0.0257(9) Uani 1 1 d . B . 
C42 C 0.9611(2) 0.9772(3) 0.30698(18) 0.0282(10) Uani 1 1 d . . . 
C43 C 0.6481(2) 1.4212(3) 0.06452(15) 0.0222(9) Uani 1 1 d . . . 
C44 C 0.6686(2) 0.9956(3) 0.10628(18) 0.0296(10) Uani 1 1 d . . . 
C45 C 0.6066(2) 1.2908(3) 0.42531(15) 0.0250(9) Uani 1 1 d . . . 
C46 C 0.8032(2) 1.4812(3) 0.24147(16) 0.0257(9) Uani 1 1 d . B . 
C47 C 0.7589(2) 1.5976(3) 0.15540(18) 0.0269(10) Uani 1 1 d . . . 
H47 H 0.7245 1.5551 0.1609 0.032 Uiso 1 1 calc R . . 
C48 C 0.6427(2) 1.2798(3) 0.50512(15) 0.0254(9) Uani 1 1 d . . . 
H48 H 0.6775 1.2829 0.5273 0.030 Uiso 1 1 calc R B . 
C49 C 0.7889(2) 1.8554(3) 0.16610(17) 0.0239(9) Uani 1 1 d . . . 
C50 C 0.7181(2) 1.0442(3) 0.28314(16) 0.0243(9) Uani 1 1 d . B . 
C51 C 0.6940(2) 1.1165(3) 0.31085(16) 0.0262(9) Uani 1 1 d . B . 
C52 C 0.8654(2) 1.6273(3) 0.12959(17) 0.0251(9) Uani 1 1 d . . . 
H52 H 0.9058 1.6057 0.1177 0.030 Uiso 1 1 calc R . . 
C53 C 0.6219(2) 1.0537(3) 0.08394(16) 0.0232(9) Uani 1 1 d . A . 
C54 C 0.4920(2) 1.2689(3) 0.19041(15) 0.0216(9) Uani 1 1 d . . . 
C55 C 0.9085(2) 1.2252(3) 0.13772(18) 0.0271(10) Uani 1 1 d . B . 
C56 C 0.4658(2) 1.3007(3) 0.27191(15) 0.0233(9) Uani 1 1 d . . . 
H56 H 0.4795 1.3143 0.3023 0.028 Uiso 1 1 calc R A . 
C57 C 0.7981(2) 1.7542(3) 0.15525(17) 0.0240(9) Uani 1 1 d . . . 
C58 C 0.6210(2) 1.3049(3) 0.37469(15) 0.0254(9) Uani 1 1 d . B . 
C59 C 0.7136(2) 1.4538(3) 0.07140(15) 0.0223(9) Uani 1 1 d . A . 
C60 C 0.5125(2) 1.2893(3) 0.23611(14) 0.0172(8) Uani 1 1 d . A . 
C64 C 0.4791(4) 1.4406(6) 0.1047(3) 0.0392(18) Uani 0.67 1 d PD A 1 
H64A H 0.4477 1.4263 0.1288 0.059 Uiso 0.67 1 calc PR A 1 
H64B H 0.4607 1.4889 0.0850 0.059 Uiso 0.67 1 calc PR A 1 
H64C H 0.5208 1.4616 0.1186 0.059 Uiso 0.67 1 calc PR A 1 
C65 C 0.4233(4) 1.1649(6) 0.0757(2) 0.0288(16) Uani 0.67 1 d PU A 1 
C66 C 0.3811(5) 1.0776(7) 0.0826(3) 0.049(2) Uani 0.67 1 d P A 1 
H66A H 0.4093 1.0283 0.0946 0.073 Uiso 0.67 1 calc PR A 1 
H66B H 0.3613 1.0588 0.0533 0.073 Uiso 0.67 1 calc PR A 1 
H66C H 0.3461 1.0906 0.1043 0.073 Uiso 0.67 1 calc PR A 1 
N1B N 0.4984(5) 1.5220(8) 0.2810(4) 0.019(2) Uiso 0.33 1 d P B 2 
C1P C 0.5610(6) 1.4939(8) 0.2702(4) 0.015(2) Uiso 0.33 1 d P B 2 
C2A C 0.4579(4) 1.5619(6) 0.2317(3) 0.0321(17) Uiso 0.67 1 d PD B 1 
H2AA H 0.4326 1.5103 0.2191 0.048 Uiso 0.67 1 calc PR B 1 
H2AB H 0.4678 1.6051 0.2072 0.048 Uiso 0.67 1 calc PR B 1 
H2AC H 0.4320 1.5928 0.2550 0.048 Uiso 0.67 1 calc PR B 1 
N1A N 0.4421(8) 1.2571(10) 0.0748(5) 0.040(3) Uiso 0.33 1 d P A 2 
O2 O 0.4761(6) 1.3311(8) 0.0799(3) 0.019(2) Uiso 0.33 1 d P A 2 
O12 O 0.4908(3) 1.3595(4) 0.07773(17) 0.0204(11) Uiso 0.67 1 d PD A 1 
H12A H 0.4524(13) 1.345(2) 0.065(2) 0.031 Uiso 0.67 1 d PD C 1 
O1A O 0.4729(6) 1.1787(9) 0.0823(4) 0.019(3) Uiso 0.33 1 d P A 2 
O11A O 0.3811(8) 1.2602(11) 0.0635(5) 0.040(4) Uiso 0.33 1 d P A 2 
N23 N 0.9089(6) 1.2896(8) 0.3512(4) 0.119(3) Uiso 1 1 d D . . 
O14 O 0.8292(8) 1.3408(12) 0.4770(6) 0.204(6) Uiso 1 1 d D . . 
N24 N 0.8058(11) 1.5289(15) 0.4904(12) 0.40(2) Uiso 1 1 d D . . 
C71 C 0.8135(8) 1.4017(12) 0.5503(5) 0.130(5) Uiso 1 1 d D . . 
H71A H 0.8409 1.3495 0.5598 0.196 Uiso 1 1 calc R . . 
H71B H 0.7668 1.3859 0.5532 0.196 Uiso 1 1 calc R . . 
H71C H 0.8240 1.4544 0.5698 0.196 Uiso 1 1 calc R . . 
C74 C 0.8279(14) 1.4258(17) 0.4997(7) 0.222(11) Uiso 1 1 d D . . 
C70 C 0.8331(9) 1.2741(15) 0.3527(8) 0.186(8) Uiso 1 1 d D . . 
H70A H 0.8135 1.2859 0.3224 0.279 Uiso 1 1 calc R . . 
H70B H 0.8139 1.3158 0.3750 0.279 Uiso 1 1 calc R . . 
H70C H 0.8242 1.2107 0.3616 0.279 Uiso 1 1 calc R . . 
C73 C 0.8141(11) 1.5026(19) 0.4370(10) 0.225(11) Uiso 1 1 d D . . 
H73A H 0.8226 1.4368 0.4342 0.337 Uiso 1 1 calc R . . 
H73B H 0.8512 1.5368 0.4245 0.337 Uiso 1 1 calc R . . 
H73C H 0.7735 1.5182 0.4200 0.337 Uiso 1 1 calc R . . 
O13 O 1.0065(17) 1.313(2) 0.3324(12) 0.384(17) Uiso 1 1 d D . . 
C69 C 0.9523(16) 1.3049(16) 0.3116(9) 0.35(2) Uiso 1 1 d D . . 
C68 C 0.9593(14) 1.2783(18) 0.3908(9) 0.244(13) Uiso 1 1 d D . . 
H68A H 1.0037 1.2922 0.3799 0.365 Uiso 1 1 calc R . . 
H68B H 0.9581 1.2152 0.4020 0.365 Uiso 1 1 calc R . . 
H68C H 0.9483 1.3203 0.4156 0.365 Uiso 1 1 calc R . . 
C67 C 0.9057(16) 1.3106(19) 0.2708(11) 0.278(16) Uiso 1 1 d D . . 
H67A H 0.9311 1.3202 0.2430 0.417 Uiso 1 1 calc R . . 
H67B H 0.8751 1.3619 0.2748 0.417 Uiso 1 1 calc R . . 
H67C H 0.8805 1.2535 0.2680 0.417 Uiso 1 1 calc R . . 
C72 C 0.7920(17) 1.621(3) 0.513(2) 0.57(5) Uiso 1 1 d D . . 
H72A H 0.7903 1.6122 0.5464 0.857 Uiso 1 1 calc R . . 
H72B H 0.7496 1.6447 0.5019 0.857 Uiso 1 1 calc R . . 
H72C H 0.8274 1.6639 0.5060 0.857 Uiso 1 1 calc R . . 
 
 
_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 N5 2.025(4) . ? 
Ni1 N10 2.033(4) . ? 
Ni1 N7 2.094(4) . ? 
Ni1 O5 2.127(3) 1_545 ? 
Ni1 O10 2.127(3) 1_545 ? 
Ni1 N6 2.176(4) . ? 
Ni1 C49 2.431(4) 1_545 ? 
Ni2 N4 2.051(4) . ? 
Ni2 O1B 2.059(6) . ? 
Ni2 N8 2.067(4) . ? 
Ni2 N3 2.075(4) . ? 
Ni2 O1A 2.087(12) . ? 
Ni2 O2 2.091(10) . ? 
Ni2 O12 2.144(5) . ? 
Ni2 N13 2.147(4) 4_585 ? 
Ni2 N1A 2.445(15) . ? 
Ni3 N11 2.007(4) . ? 
Ni3 N14 2.022(3) . ? 
Ni3 N9 2.082(4) . ? 
Ni3 O7 2.112(3) . ? 
Ni3 O4 2.142(3) . ? 
Ni3 O6 2.144(3) . ? 
Ni3 C58 2.432(4) . ? 
Ni4 N17 2.061(3) . ? 
Ni4 N15 2.066(4) . ? 
Ni4 O9 2.068(3) 2_755 ? 
Ni4 N12 2.075(4) . ? 
Ni4 O8 2.076(3) . ? 
Ni4 N2 2.127(4) . ? 
Ni5 N22 2.100(3) . ? 
Ni5 N21 2.109(3) . ? 
Ni5 N18 2.119(4) . ? 
Ni5 N19 2.132(3) . ? 
Ni5 N16 2.139(3) . ? 
Ni5 N20 2.142(4) . ? 
O1B C65 1.275(10) . ? 
O3 C40 1.245(6) . ? 
O4 C1P 1.215(13) . ? 
O4 C3 1.272(8) . ? 
O5 C49 1.262(6) . ? 
O5 Ni1 2.127(3) 1_565 ? 
O6 C58 1.258(6) . ? 
O7 C58 1.260(6) . ? 
O8 H8A 0.8727 . ? 
O8 H8B 0.8731 . ? 
O9 C40 1.261(6) . ? 
O9 Ni4 2.068(3) 2_745 ? 
O10 C49 1.265(6) . ? 
O10 Ni1 2.127(3) 1_565 ? 
O11B C65 1.225(11) . ? 
N1 C3 1.147(11) . ? 
N1 C2A 1.556(9) . ? 
N1 C6 1.585(8) . ? 
N2 C52 1.329(6) . ? 
N2 C47 1.347(6) . ? 
N3 N16 1.338(5) . ? 
N3 C54 1.376(6) . ? 
N4 N21 1.329(5) . ? 
N4 C43 1.365(6) . ? 
N5 N18 1.327(5) . ? 
N5 C37 1.360(6) . ? 
N6 C27 1.330(6) . ? 
N6 C29 1.331(7) . ? 
N7 N19 1.338(5) . ? 
N7 C44 1.365(6) . ? 
N8 N19 1.339(5) . ? 
N8 C53 1.358(6) . ? 
N9 N20 1.337(5) . ? 
N9 C51 1.372(6) . ? 
N10 N20 1.325(5) . ? 
N10 C50 1.356(6) . ? 
N11 N22 1.338(5) . ? 
N11 C41 1.359(6) . ? 
N12 N22 1.331(5) . ? 
N12 C46 1.373(6) . ? 
N13 C22 1.340(6) . ? 
N13 C48 1.341(6) . ? 
N13 Ni2 2.147(4) 4_586 ? 
N14 N16 1.332(5) . ? 
N14 C60 1.363(5) . ? 
N15 N18 1.334(5) . ? 
N15 C55 1.369(6) . ? 
N17 N21 1.339(5) . ? 
N17 C59 1.381(5) . ? 
C2B N1B 1.451(18) . ? 
C2B H2BA 0.9600 . ? 
C2B H2BB 0.9600 . ? 
C2B H2BC 0.9600 . ? 
C3 C4 1.482(10) . ? 
C4 N1B 1.251(13) . ? 
C4 H4AA 0.9600 . ? 
C4 H4AB 0.9600 . ? 
C4 H4AC 0.9600 . ? 
C4 H4BD 0.9598 . ? 
C4 H4BE 0.9602 . ? 
C4 H4BF 0.9600 . ? 
C5 C24 1.382(8) . ? 
C5 C10 1.408(9) . ? 
C5 H5 0.9300 . ? 
C6 C1P 1.669(14) . ? 
C6 H6AA 0.9600 . ? 
C6 H6AB 0.9600 . ? 
C6 H6AC 0.9600 . ? 
C6 H6BD 0.9599 . ? 
C6 H6BE 0.9603 . ? 
C6 H6BF 0.9600 . ? 
C7 C23 1.357(8) . ? 
C7 C19 1.415(9) . ? 
C7 H7 0.9300 . ? 
C9 C42 1.374(8) . ? 
C9 C27 1.386(8) . ? 
C9 H9 0.9300 . ? 
C10 C32 1.375(8) . ? 
C10 H10 0.9300 . ? 
C11 C19 1.370(8) . ? 
C11 C55 1.417(7) . ? 
C11 H11 0.9300 . ? 
C12 C31 1.347(8) . ? 
C12 C13 1.390(9) . ? 
C12 H12 0.9300 . ? 
C13 C30 1.371(8) . ? 
C13 H13 0.9300 . ? 
C14 C18 1.375(8) . ? 
C14 C20 1.407(9) . ? 
C14 H14 0.9300 . ? 
C15 C28 1.374(8) . ? 
C15 C17 1.408(9) . ? 
C15 H15 0.9300 . ? 
C16 C38 1.377(8) . ? 
C16 C39 1.400(8) . ? 
C16 H16 0.9300 . ? 
C17 C35 1.357(8) . ? 
C17 H17 0.9300 . ? 
C18 C41 1.410(7) . ? 
C18 H18 0.9300 . ? 
C19 H19 0.9300 . ? 
C20 C21 1.372(8) . ? 
C20 H20 0.9300 . ? 
C21 C46 1.412(7) . ? 
C21 H21 0.9300 . ? 
C22 C36 1.390(7) . ? 
C22 H22 0.9300 . ? 
C23 C37 1.417(7) . ? 
C23 H23 0.9300 . ? 
C24 C51 1.407(7) . ? 
C24 H24 0.9300 . ? 
C25 C42 1.375(7) . ? 
C25 C29 1.379(8) . ? 
C25 H25 0.9300 . ? 
C26 C48 1.385(7) . ? 
C26 C45 1.392(7) . ? 
C26 H26 0.9300 . ? 
C27 H27 0.9300 . ? 
C28 C43 1.414(6) . ? 
C28 H28 0.9300 . ? 
C29 H29 0.9300 . ? 
C30 C44 1.408(7) . ? 
C30 H30 0.9300 . ? 
C31 C53 1.419(6) . ? 
C31 H31 0.9300 . ? 
C32 C50 1.402(7) . ? 
C32 H32 0.9300 . ? 
C33 C52 1.382(7) . ? 
C33 C57 1.388(7) . ? 
C33 H33 0.9300 . ? 
C34 C47 1.370(7) . ? 
C34 C57 1.391(7) . ? 
C34 H34 0.9300 . ? 
C35 C59 1.411(7) . ? 
C35 H35 0.9300 . ? 
C36 C45 1.395(7) . ? 
C36 H36 0.9300 . ? 
C37 C55 1.387(7) . ? 
C38 C54 1.416(7) . ? 
C38 H38 0.9300 . ? 
C39 C56 1.371(7) . ? 
C39 H39 0.9300 . ? 
C40 C42 1.515(7) . ? 
C41 C46 1.400(7) . ? 
C43 C59 1.390(7) . ? 
C44 C53 1.392(7) . ? 
C45 C58 1.498(6) . ? 
C47 H47 0.9300 . ? 
C48 H48 0.9300 . ? 
C49 C57 1.494(6) . ? 
C49 Ni1 2.431(4) 1_565 ? 
C50 C51 1.396(7) . ? 
C52 H52 0.9300 . ? 
C54 C60 1.397(6) . ? 
C56 C60 1.406(6) . ? 
C56 H56 0.9300 . ? 
C64 O12 1.418(10) . ? 
C64 H64A 0.9600 . ? 
C64 H64B 0.9600 . ? 
C64 H64C 0.9600 . ? 
C65 C66 1.519(11) . ? 
C66 H66A 0.9600 . ? 
C66 H66B 0.9600 . ? 
C66 H66C 0.9600 . ? 
N1B C1P 1.348(17) . ? 
C2A H2AA 0.9600 . ? 
C2A H2AB 0.9600 . ? 
C2A H2AC 0.9600 . ? 
N1A O11A 1.25(2) . ? 
N1A O2 1.26(2) . ? 
N1A O1A 1.29(2) . ? 
N1A H12A 1.30(5) . ? 
O2 H12A 0.65(3) . ? 
O12 H12A 0.860(11) . ? 
N23 C69 1.45(2) . ? 
N23 C68 1.508(18) . ? 
N23 C70 1.519(16) . ? 
O14 C74 1.381(17) . ? 
N24 C72 1.50(2) . ? 
N24 C74 1.561(17) . ? 
N24 C73 1.59(2) . ? 
C71 C74 1.525(18) . ? 
C71 H71A 0.9600 . ? 
C71 H71B 0.9600 . ? 
C71 H71C 0.9600 . ? 
C70 H70A 0.9600 . ? 
C70 H70B 0.9600 . ? 
C70 H70C 0.9600 . ? 
C73 H73A 0.9600 . ? 
C73 H73B 0.9600 . ? 
C73 H73C 0.9600 . ? 
O13 C69 1.23(2) . ? 
C69 C67 1.48(2) . ? 
C68 H68A 0.9600 . ? 
C68 H68B 0.9600 . ? 
C68 H68C 0.9600 . ? 
C67 H67A 0.9600 . ? 
C67 H67B 0.9600 . ? 
C67 H67C 0.9600 . ? 
C72 H72A 0.9600 . ? 
C72 H72B 0.9600 . ? 
C72 H72C 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 
N5 Ni1 N10 98.69(15) . . ? 
N5 Ni1 N7 90.62(15) . . ? 
N10 Ni1 N7 91.05(14) . . ? 
N5 Ni1 O5 99.08(14) . 1_545 ? 
N10 Ni1 O5 161.43(14) . 1_545 ? 
N7 Ni1 O5 94.12(13) . 1_545 ? 
N5 Ni1 O10 161.54(14) . 1_545 ? 
N10 Ni1 O10 99.47(13) . 1_545 ? 
N7 Ni1 O10 92.35(14) . 1_545 ? 
O5 Ni1 O10 62.54(12) 1_545 1_545 ? 
N5 Ni1 N6 87.94(15) . . ? 
N10 Ni1 N6 87.48(15) . . ? 
N7 Ni1 N6 177.76(15) . . ? 
O5 Ni1 N6 87.81(14) 1_545 . ? 
O10 Ni1 N6 89.55(14) 1_545 . ? 
N5 Ni1 C49 130.25(16) . 1_545 ? 
N10 Ni1 C49 130.52(15) . 1_545 ? 
N7 Ni1 C49 94.75(14) . 1_545 ? 
O5 Ni1 C49 31.24(14) 1_545 1_545 ? 
O10 Ni1 C49 31.32(14) 1_545 1_545 ? 
N6 Ni1 C49 87.49(15) . 1_545 ? 
N4 Ni2 O1B 176.3(2) . . ? 
N4 Ni2 N8 95.05(14) . . ? 
O1B Ni2 N8 86.8(2) . . ? 
N4 Ni2 N3 91.53(14) . . ? 
O1B Ni2 N3 91.70(18) . . ? 
N8 Ni2 N3 89.62(14) . . ? 
N4 Ni2 O1A 165.7(4) . . ? 
O1B Ni2 O1A 11.8(3) . . ? 
N8 Ni2 O1A 98.5(4) . . ? 
N3 Ni2 O1A 93.2(3) . . ? 
N4 Ni2 O2 103.4(4) . . ? 
O1B Ni2 O2 74.7(4) . . ? 
N8 Ni2 O2 161.5(4) . . ? 
N3 Ni2 O2 90.6(3) . . ? 
O1A Ni2 O2 63.0(5) . . ? 
N4 Ni2 O12 89.88(19) . . ? 
O1B Ni2 O12 88.2(3) . . ? 
N8 Ni2 O12 174.57(19) . . ? 
N3 Ni2 O12 92.53(16) . . ? 
O1A Ni2 O12 76.4(4) . . ? 
O2 Ni2 O12 13.6(3) . . ? 
N4 Ni2 N13 86.92(14) . 4_585 ? 
O1B Ni2 N13 89.88(18) . 4_585 ? 
N8 Ni2 N13 89.60(14) . 4_585 ? 
N3 Ni2 N13 178.20(14) . 4_585 ? 
O1A Ni2 N13 88.6(3) . 4_585 ? 
O2 Ni2 N13 90.6(3) . 4_585 ? 
O12 Ni2 N13 88.39(17) . 4_585 ? 
N4 Ni2 N1A 134.2(4) . . ? 
O1B Ni2 N1A 43.7(4) . . ? 
N8 Ni2 N1A 130.4(4) . . ? 
N3 Ni2 N1A 93.4(4) . . ? 
O1A Ni2 N1A 32.0(5) . . ? 
O2 Ni2 N1A 31.1(5) . . ? 
O12 Ni2 N1A 44.5(4) . . ? 
N13 Ni2 N1A 88.3(4) 4_585 . ? 
N11 Ni3 N14 99.29(14) . . ? 
N11 Ni3 N9 91.86(15) . . ? 
N14 Ni3 N9 88.47(14) . . ? 
N11 Ni3 O7 161.44(14) . . ? 
N14 Ni3 O7 98.27(13) . . ? 
N9 Ni3 O7 94.56(14) . . ? 
N11 Ni3 O4 88.20(14) . . ? 
N14 Ni3 O4 91.00(13) . . ? 
N9 Ni3 O4 179.47(14) . . ? 
O7 Ni3 O4 85.54(13) . . ? 
N11 Ni3 O6 99.87(13) . . ? 
N14 Ni3 O6 160.46(14) . . ? 
N9 Ni3 O6 94.67(13) . . ? 
O7 Ni3 O6 62.29(13) . . ? 
O4 Ni3 O6 85.84(13) . . ? 
N11 Ni3 C58 130.72(15) . . ? 
N14 Ni3 C58 129.41(15) . . ? 
N9 Ni3 C58 96.00(15) . . ? 
O7 Ni3 C58 31.20(15) . . ? 
O4 Ni3 C58 84.36(14) . . ? 
O6 Ni3 C58 31.10(15) . . ? 
N17 Ni4 N15 92.81(14) . . ? 
N17 Ni4 O9 178.71(14) . 2_755 ? 
N15 Ni4 O9 88.22(14) . 2_755 ? 
N17 Ni4 N12 93.15(14) . . ? 
N15 Ni4 N12 90.43(15) . . ? 
O9 Ni4 N12 87.62(14) 2_755 . ? 
N17 Ni4 O8 89.49(14) . . ? 
N15 Ni4 O8 94.38(14) . . ? 
O9 Ni4 O8 89.66(13) 2_755 . ? 
N12 Ni4 O8 174.40(14) . . ? 
N17 Ni4 N2 88.61(14) . . ? 
N15 Ni4 N2 177.09(15) . . ? 
O9 Ni4 N2 90.40(14) 2_755 . ? 
N12 Ni4 N2 86.95(15) . . ? 
O8 Ni4 N2 88.17(14) . . ? 
N22 Ni5 N21 89.42(13) . . ? 
N22 Ni5 N18 88.92(13) . . ? 
N21 Ni5 N18 91.53(13) . . ? 
N22 Ni5 N19 176.61(13) . . ? 
N21 Ni5 N19 91.19(13) . . ? 
N18 Ni5 N19 87.74(13) . . ? 
N22 Ni5 N16 94.17(13) . . ? 
N21 Ni5 N16 88.89(13) . . ? 
N18 Ni5 N16 176.88(13) . . ? 
N19 Ni5 N16 89.17(13) . . ? 
N22 Ni5 N20 88.40(13) . . ? 
N21 Ni5 N20 174.96(13) . . ? 
N18 Ni5 N20 92.97(13) . . ? 
N19 Ni5 N20 91.25(13) . . ? 
N16 Ni5 N20 86.74(13) . . ? 
C65 O1B Ni2 132.3(6) . . ? 
C1P O4 C3 33.5(6) . . ? 
C1P O4 Ni3 122.7(6) . . ? 
C3 O4 Ni3 137.0(4) . . ? 
C49 O5 Ni1 87.8(3) . 1_565 ? 
C58 O6 Ni3 87.2(3) . . ? 
C58 O7 Ni3 88.6(3) . . ? 
Ni4 O8 H8A 110.7 . . ? 
Ni4 O8 H8B 110.8 . . ? 
H8A O8 H8B 108.0 . . ? 
C40 O9 Ni4 131.4(3) . 2_745 ? 
C49 O10 Ni1 87.7(3) . 1_565 ? 
C3 N1 C2A 133.2(7) . . ? 
C3 N1 C6 116.3(7) . . ? 
C2A N1 C6 110.1(6) . . ? 
C52 N2 C47 117.7(4) . . ? 
C52 N2 Ni4 123.4(3) . . ? 
C47 N2 Ni4 118.2(3) . . ? 
N16 N3 C54 106.5(3) . . ? 
N16 N3 Ni2 121.0(3) . . ? 
C54 N3 Ni2 132.0(3) . . ? 
N21 N4 C43 107.2(3) . . ? 
N21 N4 Ni2 123.6(3) . . ? 
C43 N4 Ni2 127.3(3) . . ? 
N18 N5 C37 107.6(3) . . ? 
N18 N5 Ni1 125.3(3) . . ? 
C37 N5 Ni1 127.0(3) . . ? 
C27 N6 C29 116.6(4) . . ? 
C27 N6 Ni1 126.1(3) . . ? 
C29 N6 Ni1 117.3(3) . . ? 
N19 N7 C44 106.9(3) . . ? 
N19 N7 Ni1 119.7(3) . . ? 
C44 N7 Ni1 133.4(3) . . ? 
N19 N8 C53 107.1(3) . . ? 
N19 N8 Ni2 125.6(3) . . ? 
C53 N8 Ni2 126.9(3) . . ? 
N20 N9 C51 106.6(4) . . ? 
N20 N9 Ni3 119.4(3) . . ? 
C51 N9 Ni3 133.4(3) . . ? 
N20 N10 C50 108.1(4) . . ? 
N20 N10 Ni1 125.0(3) . . ? 
C50 N10 Ni1 125.5(3) . . ? 
N22 N11 C41 107.1(4) . . ? 
N22 N11 Ni3 125.4(3) . . ? 
C41 N11 Ni3 127.5(3) . . ? 
N22 N12 C46 106.9(3) . . ? 
N22 N12 Ni4 123.6(3) . . ? 
C46 N12 Ni4 128.5(3) . . ? 
C22 N13 C48 117.6(4) . . ? 
C22 N13 Ni2 123.4(3) . 4_586 ? 
C48 N13 Ni2 118.9(3) . 4_586 ? 
N16 N14 C60 107.5(3) . . ? 
N16 N14 Ni3 125.6(3) . . ? 
C60 N14 Ni3 126.9(3) . . ? 
N18 N15 C55 106.4(4) . . ? 
N18 N15 Ni4 122.5(3) . . ? 
C55 N15 Ni4 130.6(3) . . ? 
N14 N16 N3 111.5(3) . . ? 
N14 N16 Ni5 121.9(2) . . ? 
N3 N16 Ni5 125.4(3) . . ? 
N21 N17 C59 106.5(3) . . ? 
N21 N17 Ni4 124.7(3) . . ? 
C59 N17 Ni4 128.5(3) . . ? 
N5 N18 N15 111.4(3) . . ? 
N5 N18 Ni5 122.7(3) . . ? 
N15 N18 Ni5 125.9(3) . . ? 
N7 N19 N8 111.2(3) . . ? 
N7 N19 Ni5 126.5(2) . . ? 
N8 N19 Ni5 122.3(3) . . ? 
N10 N20 N9 111.2(3) . . ? 
N10 N20 Ni5 121.2(3) . . ? 
N9 N20 Ni5 127.4(3) . . ? 
N4 N21 N17 111.7(3) . . ? 
N4 N21 Ni5 123.6(3) . . ? 
N17 N21 Ni5 124.1(2) . . ? 
N12 N22 N11 111.6(3) . . ? 
N12 N22 Ni5 124.7(3) . . ? 
N11 N22 Ni5 123.6(3) . . ? 
N1B C2B H2BA 109.5 . . ? 
N1B C2B H2BB 109.5 . . ? 
H2BA C2B H2BB 109.5 . . ? 
N1B C2B H2BC 109.5 . . ? 
H2BA C2B H2BC 109.5 . . ? 
H2BB C2B H2BC 109.5 . . ? 
N1 C3 O4 125.3(8) . . ? 
N1 C3 C4 110.5(7) . . ? 
O4 C3 C4 124.2(7) . . ? 
N1B C4 C3 38.3(6) . . ? 
N1B C4 H4AA 71.1 . . ? 
C3 C4 H4AA 109.5 . . ? 
N1B C4 H4AB 124.0 . . ? 
C3 C4 H4AB 109.5 . . ? 
H4AA C4 H4AB 109.5 . . ? 
N1B C4 H4AC 123.3 . . ? 
C3 C4 H4AC 109.5 . . ? 
H4AA C4 H4AC 109.5 . . ? 
H4AB C4 H4AC 109.5 . . ? 
N1B C4 H4BD 109.5 . . ? 
C3 C4 H4BD 147.9 . . ? 
H4AA C4 H4BD 38.4 . . ? 
H4AB C4 H4BD 88.6 . . ? 
H4AC C4 H4BD 87.8 . . ? 
N1B C4 H4BE 109.4 . . ? 
C3 C4 H4BE 88.3 . . ? 
H4AA C4 H4BE 122.9 . . ? 
H4AB C4 H4BE 21.6 . . ? 
H4AC C4 H4BE 114.6 . . ? 
H4BD C4 H4BE 109.5 . . ? 
N1B C4 H4BF 109.5 . . ? 
C3 C4 H4BF 88.1 . . ? 
H4AA C4 H4BF 124.4 . . ? 
H4AB C4 H4BF 113.2 . . ? 
H4AC C4 H4BF 22.1 . . ? 
H4BD C4 H4BF 109.5 . . ? 
H4BE C4 H4BF 109.5 . . ? 
C24 C5 C10 121.7(5) . . ? 
C24 C5 H5 119.2 . . ? 
C10 C5 H5 119.2 . . ? 
N1 C6 C1P 34.2(5) . . ? 
N1 C6 H6AA 109.5 . . ? 
C1P C6 H6AA 143.6 . . ? 
N1 C6 H6AB 109.5 . . ? 
C1P C6 H6AB 89.6 . . ? 
H6AA C6 H6AB 109.5 . . ? 
N1 C6 H6AC 109.5 . . ? 
C1P C6 H6AC 91.7 . . ? 
H6AA C6 H6AC 109.5 . . ? 
H6AB C6 H6AC 109.5 . . ? 
N1 C6 H6BD 75.4 . . ? 
C1P C6 H6BD 109.5 . . ? 
H6AA C6 H6BD 34.1 . . ? 
H6AB C6 H6BD 122.0 . . ? 
H6AC C6 H6BD 123.4 . . ? 
N1 C6 H6BE 124.5 . . ? 
C1P C6 H6BE 109.5 . . ? 
H6AA C6 H6BE 90.3 . . ? 
H6AB C6 H6BE 20.3 . . ? 
H6AC C6 H6BE 111.5 . . ? 
H6BD C6 H6BE 109.5 . . ? 
N1 C6 H6BF 121.0 . . ? 
C1P C6 H6BF 109.5 . . ? 
H6AA C6 H6BF 91.0 . . ? 
H6AB C6 H6BF 114.5 . . ? 
H6AC C6 H6BF 18.8 . . ? 
H6BD C6 H6BF 109.5 . . ? 
H6BE C6 H6BF 109.5 . . ? 
C23 C7 C19 122.1(5) . . ? 
C23 C7 H7 119.0 . . ? 
C19 C7 H7 119.0 . . ? 
C42 C9 C27 119.1(5) . . ? 
C42 C9 H9 120.4 . . ? 
C27 C9 H9 120.4 . . ? 
C32 C10 C5 121.8(5) . . ? 
C32 C10 H10 119.1 . . ? 
C5 C10 H10 119.1 . . ? 
C19 C11 C55 116.5(5) . . ? 
C19 C11 H11 121.8 . . ? 
C55 C11 H11 121.8 . . ? 
C31 C12 C13 122.4(5) . . ? 
C31 C12 H12 118.8 . . ? 
C13 C12 H12 118.8 . . ? 
C30 C13 C12 121.7(5) . . ? 
C30 C13 H13 119.1 . . ? 
C12 C13 H13 119.1 . . ? 
C18 C14 C20 121.8(5) . . ? 
C18 C14 H14 119.1 . . ? 
C20 C14 H14 119.1 . . ? 
C28 C15 C17 122.1(5) . . ? 
C28 C15 H15 118.9 . . ? 
C17 C15 H15 118.9 . . ? 
C38 C16 C39 122.7(5) . . ? 
C38 C16 H16 118.7 . . ? 
C39 C16 H16 118.7 . . ? 
C35 C17 C15 122.0(5) . . ? 
C35 C17 H17 119.0 . . ? 
C15 C17 H17 119.0 . . ? 
C14 C18 C41 116.6(5) . . ? 
C14 C18 H18 121.7 . . ? 
C41 C18 H18 121.7 . . ? 
C11 C19 C7 122.1(5) . . ? 
C11 C19 H19 118.9 . . ? 
C7 C19 H19 118.9 . . ? 
C21 C20 C14 122.5(5) . . ? 
C21 C20 H20 118.7 . . ? 
C14 C20 H20 118.7 . . ? 
C20 C21 C46 116.3(5) . . ? 
C20 C21 H21 121.9 . . ? 
C46 C21 H21 121.9 . . ? 
N13 C22 C36 123.1(5) . . ? 
N13 C22 H22 118.5 . . ? 
C36 C22 H22 118.5 . . ? 
C7 C23 C37 116.4(5) . . ? 
C7 C23 H23 121.8 . . ? 
C37 C23 H23 121.8 . . ? 
C5 C24 C51 117.2(5) . . ? 
C5 C24 H24 121.4 . . ? 
C51 C24 H24 121.4 . . ? 
C42 C25 C29 119.5(5) . . ? 
C42 C25 H25 120.2 . . ? 
C29 C25 H25 120.2 . . ? 
C48 C26 C45 118.9(5) . . ? 
C48 C26 H26 120.5 . . ? 
C45 C26 H26 120.5 . . ? 
N6 C27 C9 123.6(5) . . ? 
N6 C27 H27 118.2 . . ? 
C9 C27 H27 118.2 . . ? 
C15 C28 C43 116.6(5) . . ? 
C15 C28 H28 121.7 . . ? 
C43 C28 H28 121.7 . . ? 
N6 C29 C25 123.5(5) . . ? 
N6 C29 H29 118.3 . . ? 
C25 C29 H29 118.3 . . ? 
C13 C30 C44 117.5(5) . . ? 
C13 C30 H30 121.2 . . ? 
C44 C30 H30 121.2 . . ? 
C12 C31 C53 117.0(5) . . ? 
C12 C31 H31 121.5 . . ? 
C53 C31 H31 121.5 . . ? 
C10 C32 C50 116.6(5) . . ? 
C10 C32 H32 121.7 . . ? 
C50 C32 H32 121.7 . . ? 
C52 C33 C57 118.4(4) . . ? 
C52 C33 H33 120.8 . . ? 
C57 C33 H33 120.8 . . ? 
C47 C34 C57 118.6(4) . . ? 
C47 C34 H34 120.7 . . ? 
C57 C34 H34 120.7 . . ? 
C17 C35 C59 116.7(5) . . ? 
C17 C35 H35 121.7 . . ? 
C59 C35 H35 121.7 . . ? 
C22 C36 C45 118.9(4) . . ? 
C22 C36 H36 120.5 . . ? 
C45 C36 H36 120.5 . . ? 
N5 C37 C55 106.9(4) . . ? 
N5 C37 C23 131.1(4) . . ? 
C55 C37 C23 122.0(4) . . ? 
C16 C38 C54 116.1(5) . . ? 
C16 C38 H38 122.0 . . ? 
C54 C38 H38 122.0 . . ? 
C56 C39 C16 121.7(4) . . ? 
C56 C39 H39 119.1 . . ? 
C16 C39 H39 119.1 . . ? 
O3 C40 O9 127.5(4) . . ? 
O3 C40 C42 117.8(4) . . ? 
O9 C40 C42 114.7(4) . . ? 
N11 C41 C46 107.4(4) . . ? 
N11 C41 C18 131.2(5) . . ? 
C46 C41 C18 121.4(4) . . ? 
C9 C42 C25 117.6(5) . . ? 
C9 C42 C40 121.0(4) . . ? 
C25 C42 C40 121.3(5) . . ? 
N4 C43 C59 107.7(4) . . ? 
N4 C43 C28 131.6(4) . . ? 
C59 C43 C28 120.7(4) . . ? 
N7 C44 C53 107.3(4) . . ? 
N7 C44 C30 132.7(5) . . ? 
C53 C44 C30 120.0(4) . . ? 
C26 C45 C36 118.1(4) . . ? 
C26 C45 C58 121.0(4) . . ? 
C36 C45 C58 120.8(4) . . ? 
N12 C46 C41 106.9(4) . . ? 
N12 C46 C21 131.7(5) . . ? 
C41 C46 C21 121.3(4) . . ? 
N2 C47 C34 123.1(4) . . ? 
N2 C47 H47 118.4 . . ? 
C34 C47 H47 118.4 . . ? 
N13 C48 C26 123.3(4) . . ? 
N13 C48 H48 118.3 . . ? 
C26 C48 H48 118.3 . . ? 
O5 C49 O10 121.9(4) . . ? 
O5 C49 C57 119.4(4) . . ? 
O10 C49 C57 118.8(4) . . ? 
O5 C49 Ni1 61.0(2) . 1_565 ? 
O10 C49 Ni1 61.0(2) . 1_565 ? 
C57 C49 Ni1 176.4(3) . 1_565 ? 
N10 C50 C51 106.8(4) . . ? 
N10 C50 C32 130.9(5) . . ? 
C51 C50 C32 122.3(4) . . ? 
N9 C51 C50 107.4(4) . . ? 
N9 C51 C24 132.3(5) . . ? 
C50 C51 C24 120.4(5) . . ? 
N2 C52 C33 123.3(4) . . ? 
N2 C52 H52 118.3 . . ? 
C33 C52 H52 118.3 . . ? 
N8 C53 C44 107.6(4) . . ? 
N8 C53 C31 131.1(4) . . ? 
C44 C53 C31 121.3(4) . . ? 
N3 C54 C60 107.3(4) . . ? 
N3 C54 C38 131.7(4) . . ? 
C60 C54 C38 121.0(4) . . ? 
N15 C55 C37 107.7(4) . . ? 
N15 C55 C11 131.4(5) . . ? 
C37 C55 C11 120.9(4) . . ? 
C39 C56 C60 116.8(4) . . ? 
C39 C56 H56 121.6 . . ? 
C60 C56 H56 121.6 . . ? 
C33 C57 C34 118.8(4) . . ? 
C33 C57 C49 120.7(4) . . ? 
C34 C57 C49 120.6(4) . . ? 
O6 C58 O7 121.9(4) . . ? 
O6 C58 C45 119.8(4) . . ? 
O7 C58 C45 118.2(4) . . ? 
O6 C58 Ni3 61.7(2) . . ? 
O7 C58 Ni3 60.2(2) . . ? 
C45 C58 Ni3 178.3(4) . . ? 
N17 C59 C43 107.0(4) . . ? 
N17 C59 C35 131.1(4) . . ? 
C43 C59 C35 121.9(4) . . ? 
N14 C60 C54 107.1(4) . . ? 
N14 C60 C56 131.2(4) . . ? 
C54 C60 C56 121.7(4) . . ? 
O11B C65 O1B 126.3(8) . . ? 
O11B C65 C66 118.7(7) . . ? 
O1B C65 C66 115.0(7) . . ? 
C65 C66 H66A 109.5 . . ? 
C65 C66 H66B 109.5 . . ? 
H66A C66 H66B 109.5 . . ? 
C65 C66 H66C 109.5 . . ? 
H66A C66 H66C 109.5 . . ? 
H66B C66 H66C 109.5 . . ? 
C4 N1B C1P 114.6(10) . . ? 
C4 N1B C2B 116.0(11) . . ? 
C1P N1B C2B 129.1(12) . . ? 
O4 C1P N1B 117.7(11) . . ? 
O4 C1P C6 129.2(10) . . ? 
N1B C1P C6 113.0(9) . . ? 
O11A N1A O2 121.0(14) . . ? 
O11A N1A O1A 121.7(15) . . ? 
O2 N1A O1A 117.3(14) . . ? 
O11A N1A Ni2 177.1(13) . . ? 
O2 N1A Ni2 58.8(7) . . ? 
O1A N1A Ni2 58.6(8) . . ? 
O11A N1A H12A 93.9(14) . . ? 
O2 N1A H12A 29.4(10) . . ? 
O1A N1A H12A 142.7(18) . . ? 
Ni2 N1A H12A 85.2(10) . . ? 
N1A O2 Ni2 90.1(9) . . ? 
N1A O2 H12A 78(4) . . ? 
Ni2 O2 H12A 149(4) . . ? 
C64 O12 Ni2 126.6(4) . . ? 
C64 O12 H12A 105.8(19) . . ? 
Ni2 O12 H12A 119(2) . . ? 
N1A O1A Ni2 89.4(9) . . ? 
C69 N23 C68 102.1(19) . . ? 
C69 N23 C70 130.1(19) . . ? 
C68 N23 C70 127.2(18) . . ? 
C72 N24 C74 144(4) . . ? 
C72 N24 C73 131(4) . . ? 
C74 N24 C73 84.6(15) . . ? 
C74 C71 H71A 109.5 . . ? 
C74 C71 H71B 109.5 . . ? 
H71A C71 H71B 109.5 . . ? 
C74 C71 H71C 109.5 . . ? 
H71A C71 H71C 109.5 . . ? 
H71B C71 H71C 109.5 . . ? 
O14 C74 C71 104.8(18) . . ? 
O14 C74 N24 140(2) . . ? 
C71 C74 N24 109(2) . . ? 
N23 C70 H70A 109.5 . . ? 
N23 C70 H70B 109.5 . . ? 
H70A C70 H70B 109.5 . . ? 
N23 C70 H70C 109.5 . . ? 
H70A C70 H70C 109.5 . . ? 
H70B C70 H70C 109.5 . . ? 
N24 C73 H73A 109.5 . . ? 
N24 C73 H73B 109.5 . . ? 
H73A C73 H73B 109.5 . . ? 
N24 C73 H73C 109.5 . . ? 
H73A C73 H73C 109.5 . . ? 
H73B C73 H73C 109.5 . . ? 
O13 C69 N23 99(3) . . ? 
O13 C69 C67 155(3) . . ? 
N23 C69 C67 105(3) . . ? 
N23 C68 H68A 109.5 . . ? 
N23 C68 H68B 109.5 . . ? 
H68A C68 H68B 109.5 . . ? 
N23 C68 H68C 109.5 . . ? 
H68A C68 H68C 109.5 . . ? 
H68B C68 H68C 109.5 . . ? 
C69 C67 H67A 109.5 . . ? 
C69 C67 H67B 109.5 . . ? 
H67A C67 H67B 109.5 . . ? 
C69 C67 H67C 109.5 . . ? 
H67A C67 H67C 109.5 . . ? 
H67B C67 H67C 109.5 . . ? 
N24 C72 H72A 109.5 . . ? 
N24 C72 H72B 109.5 . . ? 
H72A C72 H72B 109.5 . . ? 
N24 C72 H72C 109.5 . . ? 
H72A C72 H72C 109.5 . . ? 
H72B C72 H72C 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              64.9871 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    2.206 
_refine_diff_density_min   -1.167 
_refine_diff_density_rms    0.138 

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
         1     0.000    -0.034     0.000     570.5      -9.4
         2     1.000    -0.019     0.500     570.6      -9.4
         3     0.402     0.166     0.384      31.0      -1.7
         4     0.007     0.171     0.231       9.4      -1.2
         5     0.402     0.334     0.884      31.0      -1.7
         6     0.007     0.329     0.731       9.4      -1.2
         7     0.598     0.666     0.116      31.0      -1.2
         8     0.993     0.671     0.269       9.4      -1.4
         9     0.598     0.834     0.616      31.0      -1.5
        10     0.993     0.829     0.769       9.4      -1.3
_platon_squeeze_details
;
;
