data_s93
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. C. Matthews
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C74 H52 Cl3 N17 Ni4 O22'
_chemical_formula_weight          1872.52
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 '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)/n
_symmetry_space_group_name_hall   '-P 2yn'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    17.5385(2)
_cell_length_b                    23.9347(3)
_cell_length_c                    19.7227(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  93.9730(10)
_cell_angle_gamma                 90.00
_cell_volume                      8259.27(19)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     19087
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             'Light Green'
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.506
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3816
_exptl_absorpt_coefficient_mu     1.077
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7975
_exptl_absorpt_correction_T_max   0.9382
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_exptl_special_details
;
 PLEASE NOTE cell_measurement_ fields are not relevant to area detector data,
 the entire data set is used to refine the cell, which is indexed from all
 observed reflections in a 10 degree phi range.
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             90353
_diffrn_reflns_av_R_equivalents   0.0818
_diffrn_reflns_av_sigmaI/netI     0.0777
_diffrn_reflns_limit_h_min        -22
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -31
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -25
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.48
_reflns_number_total              18898
_reflns_number_gt                 12451
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
' DENZO (Otwinowski and Minor, 1997)'
_computing_cell_refinement        
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction         
' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_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.
;
 
_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)+(0.1013P)²+15.3929P] 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          18898
_refine_ls_number_parameters      1093
_refine_ls_number_restraints      38
_refine_ls_R_factor_all           0.1201
_refine_ls_R_factor_gt            0.0762
_refine_ls_wR_factor_ref          0.2125
_refine_ls_wR_factor_gt           0.1911
_refine_ls_goodness_of_fit_ref    1.031
_refine_ls_restrained_S_all       1.032
_refine_ls_shift/su_max           0.009
_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 0.73552(3) -0.06609(2) 0.50647(3) 0.02897(15) Uani 1 1 d . . .
Ni2 Ni 0.82571(3) 0.05810(2) 0.40187(3) 0.02954(15) Uani 1 1 d . . .
Ni3 Ni 0.59953(4) -0.14159(3) 0.29363(3) 0.03288(16) Uani 1 1 d . . .
Ni4 Ni 0.68772(4) -0.01671(3) 0.19114(3) 0.03646(17) Uani 1 1 d . . .
C1 C 0.6901(3) -0.1530(2) 0.6168(3) 0.0419(12) Uani 1 1 d . . .
C2 C 0.6382(3) -0.1931(3) 0.6381(3) 0.0511(14) Uani 1 1 d . . .
H2 H 0.6010 -0.2085 0.6061 0.061 Uiso 1 1 calc R . .
C3 C 0.6409(4) -0.2098(3) 0.7038(3) 0.0634(18) Uani 1 1 d . . .
H3 H 0.6055 -0.2370 0.7173 0.076 Uiso 1 1 calc R . .
C4 C 0.6942(4) -0.1880(3) 0.7516(4) 0.071(2) Uani 1 1 d . . .
H4 H 0.6952 -0.1998 0.7976 0.085 Uiso 1 1 calc R . .
C5 C 0.7459(4) -0.1488(3) 0.7314(3) 0.0635(18) Uani 1 1 d . . .
H5 H 0.7830 -0.1342 0.7641 0.076 Uiso 1 1 calc R . .
C6 C 0.7451(3) -0.1302(2) 0.6642(3) 0.0475(14) Uani 1 1 d . . .
C7 C 0.8016(3) -0.0888(2) 0.6485(3) 0.0429(13) Uani 1 1 d . . .
H7 H 0.8381 -0.0787 0.6842 0.052 Uiso 1 1 calc R . .
C8 C 0.8615(3) 0.00349(19) 0.5330(2) 0.0294(10) Uani 1 1 d . . .
C9 C 0.9244(3) 0.04339(19) 0.5246(2) 0.0299(10) Uani 1 1 d . . .
C10 C 0.9874(3) 0.0528(2) 0.5698(2) 0.0350(11) Uani 1 1 d . . .
H10 H 0.9921 0.0340 0.6123 0.042 Uiso 1 1 calc R . .
C11 C 1.0429(3) 0.0898(2) 0.5523(3) 0.0382(12) Uani 1 1 d . . .
H11 H 1.0865 0.0963 0.5827 0.046 Uiso 1 1 calc R . .
C12 C 1.0355(3) 0.1175(2) 0.4906(3) 0.0357(11) Uani 1 1 d . . .
H12 H 1.0725 0.1440 0.4787 0.043 Uiso 1 1 calc R . .
C13 C 0.9721(3) 0.10544(19) 0.4464(2) 0.0310(10) Uani 1 1 d . . .
C14 C 0.9574(3) 0.1289(2) 0.3765(3) 0.0340(11) Uani 1 1 d . . .
C15 C 1.0098(3) 0.1612(2) 0.3458(3) 0.0426(12) Uani 1 1 d . . .
H15 H 1.0573 0.1705 0.3692 0.051 Uiso 1 1 calc R . .
C16 C 0.9921(3) 0.1803(2) 0.2795(3) 0.0487(14) Uani 1 1 d . . .
H16 H 1.0272 0.2028 0.2570 0.058 Uiso 1 1 calc R . .
C17 C 0.9223(3) 0.1655(2) 0.2476(3) 0.0479(14) Uani 1 1 d . . .
H17 H 0.9083 0.1777 0.2026 0.058 Uiso 1 1 calc R . .
C18 C 0.8730(3) 0.1326(2) 0.2824(3) 0.0413(12) Uani 1 1 d . . .
H18 H 0.8251 0.1227 0.2603 0.050 Uiso 1 1 calc R . .
N1 N 0.8069(2) -0.06449(17) 0.5910(2) 0.0365(9) Uani 1 1 d . . .
N2 N 0.8664(2) -0.02624(17) 0.5898(2) 0.0351(9) Uani 1 1 d . . .
N3 N 0.9185(2) 0.06980(16) 0.46387(19) 0.0302(8) Uani 1 1 d . . .
N4 N 0.8893(2) 0.11437(16) 0.3450(2) 0.0333(9) Uani 1 1 d . . .
O1 O 0.68619(19) -0.13613(14) 0.54990(16) 0.0362(8) Uani 1 1 d D . .
O2 O 0.80834(18) -0.00123(13) 0.48486(15) 0.0307(7) Uani 1 1 d . . .
C21 C 0.4962(3) -0.2259(2) 0.3572(3) 0.0470(14) Uani 1 1 d . . .
C22 C 0.4865(4) -0.2781(2) 0.3907(3) 0.0519(15) Uani 1 1 d . . .
H22 H 0.5304 -0.2982 0.4080 0.062 Uiso 1 1 calc R . .
C23 C 0.4161(5) -0.2995(3) 0.3983(3) 0.067(2) Uani 1 1 d . . .
H23 H 0.4114 -0.3345 0.4204 0.081 Uiso 1 1 calc R . .
C24 C 0.3503(4) -0.2708(4) 0.3741(4) 0.074(2) Uani 1 1 d . . .
H24 H 0.3011 -0.2859 0.3798 0.088 Uiso 1 1 calc R . .
C25 C 0.3577(4) -0.2217(3) 0.3426(3) 0.0631(18) Uani 1 1 d . . .
H25 H 0.3130 -0.2022 0.3261 0.076 Uiso 1 1 calc R . .
C26 C 0.4308(3) -0.1976(3) 0.3331(3) 0.0492(14) Uani 1 1 d . . .
C27 C 0.4307(3) -0.1438(2) 0.3021(3) 0.0450(13) Uani 1 1 d . . .
H27 H 0.3823 -0.1280 0.2888 0.054 Uiso 1 1 calc R . .
C28 C 0.5374(3) -0.0401(2) 0.2388(2) 0.0386(12) Uani 1 1 d . . .
C29 C 0.5310(3) 0.0153(2) 0.2070(3) 0.0449(13) Uani 1 1 d . . .
C30 C 0.4672(4) 0.0511(3) 0.2068(3) 0.0598(17) Uani 1 1 d . . .
H30 H 0.4218 0.0397 0.2265 0.072 Uiso 1 1 calc R . .
C31 C 0.4723(4) 0.1038(3) 0.1771(3) 0.0625(18) Uani 1 1 d . . .
H31 H 0.4308 0.1292 0.1773 0.075 Uiso 1 1 calc R . .
C32 C 0.5380(4) 0.1184(3) 0.1477(3) 0.0624(19) Uani 1 1 d . . .
H32 H 0.5417 0.1537 0.1260 0.075 Uiso 1 1 calc R . .
C33 C 0.5988(4) 0.0817(2) 0.1498(3) 0.0470(14) Uani 1 1 d . . .
C34 C 0.6739(4) 0.0939(2) 0.1247(3) 0.0560(16) Uani 1 1 d . . .
C35 C 0.6925(6) 0.1409(3) 0.0894(4) 0.081(2) Uani 1 1 d . . .
H35 H 0.6548 0.1685 0.0780 0.097 Uiso 1 1 calc R . .
C36 C 0.7655(6) 0.1477(4) 0.0710(5) 0.092(3) Uani 1 1 d . . .
H36 H 0.7791 0.1809 0.0483 0.110 Uiso 1 1 calc R . .
C37 C 0.8180(5) 0.1080(3) 0.0846(4) 0.080(2) Uani 1 1 d . . .
H37 H 0.8682 0.1124 0.0700 0.096 Uiso 1 1 calc R . .
C38 C 0.7988(4) 0.0603(3) 0.1201(3) 0.0629(17) Uani 1 1 d . . .
H38 H 0.8369 0.0328 0.1307 0.076 Uiso 1 1 calc R . .
N21 N 0.4906(2) -0.11443(18) 0.2904(2) 0.0389(10) Uani 1 1 d . . .
N22 N 0.4756(3) -0.0613(2) 0.2626(2) 0.0446(11) Uani 1 1 d . . .
N23 N 0.5948(3) 0.03190(18) 0.1799(2) 0.0427(11) Uani 1 1 d . . .
N24 N 0.7292(3) 0.0524(2) 0.1393(2) 0.0524(13) Uani 1 1 d . . .
O21 O 0.5661(2) -0.20729(15) 0.35107(18) 0.0427(9) Uani 1 1 d D . .
O22 O 0.60457(19) -0.06437(14) 0.23969(17) 0.0368(8) Uani 1 1 d . . .
C41 C 0.6131(3) 0.02715(18) 0.5181(2) 0.0288(10) Uani 1 1 d . . .
C42 C 0.5925(3) 0.0768(2) 0.5490(3) 0.0367(11) Uani 1 1 d . . .
H42 H 0.6166 0.0872 0.5918 0.044 Uiso 1 1 calc R . .
C43 C 0.5379(3) 0.1107(2) 0.5182(3) 0.0379(12) Uani 1 1 d . . .
H43 H 0.5248 0.1446 0.5395 0.045 Uiso 1 1 calc R . .
C44 C 0.5018(3) 0.0963(2) 0.4568(3) 0.0347(11) Uani 1 1 d . . .
H44 H 0.4625 0.1195 0.4366 0.042 Uiso 1 1 calc R . .
C45 C 0.5226(3) 0.0483(2) 0.4247(2) 0.0318(10) Uani 1 1 d . . .
H45 H 0.4976 0.0388 0.3821 0.038 Uiso 1 1 calc R . .
C46 C 0.5795(2) 0.01319(18) 0.4532(2) 0.0272(9) Uani 1 1 d . . .
C47 C 0.5993(2) -0.03445(19) 0.4144(2) 0.0277(10) Uani 1 1 d . . .
H47 H 0.5660 -0.0436 0.3760 0.033 Uiso 1 1 calc R . .
C48 C 0.7355(3) -0.13320(19) 0.3929(2) 0.0292(10) Uani 1 1 d . . .
C49 C 0.7536(3) -0.1764(2) 0.3421(3) 0.0348(11) Uani 1 1 d . . .
C50 C 0.8166(3) -0.2098(2) 0.3471(3) 0.0428(12) Uani 1 1 d . . .
H50 H 0.8532 -0.2067 0.3848 0.051 Uiso 1 1 calc R . .
C51 C 0.8260(3) -0.2488(2) 0.2958(3) 0.0505(15) Uani 1 1 d . . .
H51 H 0.8692 -0.2728 0.2981 0.061 Uiso 1 1 calc R . .
C52 C 0.7724(3) -0.2522(2) 0.2417(3) 0.0490(14) Uani 1 1 d . . .
H52 H 0.7785 -0.2783 0.2062 0.059 Uiso 1 1 calc R . .
C53 C 0.7100(3) -0.2173(2) 0.2394(3) 0.0405(12) Uani 1 1 d . . .
C54 C 0.6474(3) -0.2159(2) 0.1846(3) 0.0398(12) Uani 1 1 d . . .
C55 C 0.6504(4) -0.2438(2) 0.1230(3) 0.0505(14) Uani 1 1 d . . .
H55 H 0.6935 -0.2660 0.1143 0.061 Uiso 1 1 calc R . .
C56 C 0.5903(4) -0.2389(3) 0.0747(3) 0.0563(16) Uani 1 1 d . . .
H56 H 0.5911 -0.2585 0.0329 0.068 Uiso 1 1 calc R . .
C57 C 0.5282(4) -0.2050(2) 0.0871(3) 0.0539(15) Uani 1 1 d . . .
H57 H 0.4866 -0.2003 0.0542 0.065 Uiso 1 1 calc R . .
C58 C 0.5297(3) -0.1783(2) 0.1502(3) 0.0467(13) Uani 1 1 d . . .
H58 H 0.4878 -0.1550 0.1595 0.056 Uiso 1 1 calc R . .
N41 N 0.6574(2) -0.06591(15) 0.42670(18) 0.0278(8) Uani 1 1 d . . .
N42 N 0.6676(2) -0.10845(16) 0.37986(19) 0.0310(9) Uani 1 1 d . . .
N43 N 0.7021(2) -0.18012(16) 0.2886(2) 0.0323(9) Uani 1 1 d . . .
N44 N 0.5867(2) -0.18377(17) 0.1978(2) 0.0392(10) Uani 1 1 d . . .
O41 O 0.66435(18) -0.00885(14) 0.55164(16) 0.0348(8) Uani 1 1 d . . .
O42 O 0.78291(18) -0.12220(13) 0.44282(16) 0.0330(7) Uani 1 1 d . . .
C61 C 0.7040(3) 0.14626(19) 0.4254(2) 0.0340(11) Uani 1 1 d . . .
C62 C 0.6807(3) 0.1931(2) 0.4601(3) 0.0416(12) Uani 1 1 d . . .
H62 H 0.7079 0.2038 0.5014 0.050 Uiso 1 1 calc R . .
C63 C 0.6182(3) 0.2246(2) 0.4353(3) 0.0405(12) Uani 1 1 d . . .
H63 H 0.6028 0.2560 0.4604 0.049 Uiso 1 1 calc R . .
C64 C 0.5777(3) 0.2107(2) 0.3743(3) 0.0394(12) Uani 1 1 d . . .
H64 H 0.5363 0.2331 0.3564 0.047 Uiso 1 1 calc R . .
C65 C 0.5995(3) 0.1634(2) 0.3404(3) 0.0371(11) Uani 1 1 d . . .
H65 H 0.5712 0.1528 0.2997 0.045 Uiso 1 1 calc R . .
C66 C 0.6625(3) 0.1304(2) 0.3643(2) 0.0315(10) Uani 1 1 d . . .
C67 C 0.6796(3) 0.0824(2) 0.3233(2) 0.0308(10) Uani 1 1 d . . .
H67 H 0.6447 0.0743 0.2855 0.037 Uiso 1 1 calc R . .
C68 C 0.8127(3) -0.01895(19) 0.2986(2) 0.0293(10) Uani 1 1 d . . .
C69 C 0.8299(3) -0.0629(2) 0.2498(2) 0.0351(11) Uani 1 1 d . . .
C70 C 0.8932(3) -0.0973(2) 0.2559(3) 0.0491(14) Uani 1 1 d . . .
H70 H 0.9291 -0.0945 0.2941 0.059 Uiso 1 1 calc R . .
C71 C 0.9032(4) -0.1361(3) 0.2049(3) 0.0647(18) Uani 1 1 d . . .
H71 H 0.9456 -0.1609 0.2086 0.078 Uiso 1 1 calc R . .
C72 C 0.8519(4) -0.1387(3) 0.1492(3) 0.0630(18) Uani 1 1 d . . .
H72 H 0.8593 -0.1642 0.1134 0.076 Uiso 1 1 calc R . .
C73 C 0.7886(3) -0.1031(2) 0.1459(3) 0.0458(13) Uani 1 1 d . . .
C74 C 0.7277(4) -0.1011(2) 0.0902(3) 0.0512(15) Uani 1 1 d . . .
C75 C 0.7271(5) -0.1329(3) 0.0317(3) 0.069(2) Uani 1 1 d . . .
H75 H 0.7678 -0.1579 0.0243 0.083 Uiso 1 1 calc R . .
C76 C 0.6650(5) -0.1273(4) -0.0165(3) 0.083(3) Uani 1 1 d . . .
H76 H 0.6628 -0.1491 -0.0568 0.100 Uiso 1 1 calc R . .
C77 C 0.6084(5) -0.0911(3) -0.0056(3) 0.076(2) Uani 1 1 d . . .
H77 H 0.5665 -0.0869 -0.0384 0.092 Uiso 1 1 calc R . .
C78 C 0.6118(4) -0.0603(3) 0.0536(3) 0.0622(18) Uani 1 1 d . . .
H78 H 0.5711 -0.0354 0.0614 0.075 Uiso 1 1 calc R . .
N61 N 0.7376(2) 0.04959(16) 0.33305(18) 0.0291(8) Uani 1 1 d . . .
N62 N 0.7458(2) 0.00736(16) 0.28558(19) 0.0323(9) Uani 1 1 d . . .
N63 N 0.7787(2) -0.06740(16) 0.1960(2) 0.0360(9) Uani 1 1 d . . .
N64 N 0.6708(3) -0.06434(19) 0.1006(2) 0.0479(12) Uani 1 1 d . . .
O61 O 0.7648(2) 0.11702(15) 0.45037(17) 0.0400(8) Uani 1 1 d . . .
O62 O 0.86205(18) -0.00835(13) 0.34724(16) 0.0330(7) Uani 1 1 d . . .
O81 O 1.1098(4) -0.2568(4) 0.3868(3) 0.140(3) Uani 1 1 d D . .
O82 O 1.0448(5) -0.1742(2) 0.3613(5) 0.169(4) Uani 1 1 d D . .
O83 O 1.0140(4) -0.2508(4) 0.3061(3) 0.131(3) Uani 1 1 d D . .
O84 O 0.9856(3) -0.2469(2) 0.4194(2) 0.0689(13) Uani 1 1 d D . .
Cl1 Cl 1.04040(9) -0.23296(6) 0.37185(8) 0.0559(4) Uani 1 1 d D . .
O85 O 0.5929(7) -0.4002(3) 0.5898(6) 0.227(6) Uani 1 1 d D . .
O86 O 0.6101(5) -0.3169(3) 0.5357(4) 0.144(3) Uani 1 1 d D . .
O87 O 0.5439(7) -0.3213(4) 0.6285(6) 0.229(6) Uani 1 1 d D . .
O88 O 0.4882(7) -0.3626(6) 0.5343(7) 0.287(8) Uani 1 1 d D . .
Cl2 Cl 0.56157(19) -0.35066(10) 0.57187(14) 0.1108(9) Uani 1 1 d D . .
O89 O 0.8729(16) -0.3969(12) 0.6022(14) 0.60(3) Uani 1 1 d D . .
O90 O 0.8172(6) -0.4581(5) 0.5287(6) 0.228(6) Uani 1 1 d D . .
O91 O 0.9324(9) -0.4773(6) 0.5842(9) 0.331(10) Uani 1 1 d D . .
O92 O 0.9326(11) -0.4132(13) 0.5049(10) 0.51(3) Uani 1 1 d D . .
Cl3 Cl 0.8877(3) -0.43550(16) 0.5565(2) 0.1634(16) Uani 1 1 d D . .
C91 C 0.8202(7) -0.2638(7) 0.5929(7) 0.127(5) Uani 1 1 d . . .
C92 C 0.7951(13) -0.2902(10) 0.6489(9) 0.286(14) Uani 1 1 d . . .
N91 N 0.8379(6) -0.2412(5) 0.5428(8) 0.159(5) Uani 1 1 d . . .
O101 O 0.6365(3) -0.21580(18) 0.4741(2) 0.0686(13) Uani 1 1 d D . .
H101 H 0.649(4) -0.1865(12) 0.496(3) 0.103 Uiso 1 1 d D . .
H102 H 0.615(4) -0.2061(19) 0.4367(19) 0.103 Uiso 1 1 d D . .
O102 O 0.7027(3) -0.3709(3) 0.9171(2) 0.0751(14) Uani 1 1 d D . .
H103 H 0.712(4) -0.361(4) 0.9577(15) 0.113 Uiso 1 1 d D . .
H104 H 0.6550(7) -0.370(4) 0.909(3) 0.113 Uiso 1 1 d 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
Ni1 N41 2.013(4) . ?
Ni1 N1 2.015(4) . ?
Ni1 O42 2.053(3) . ?
Ni1 O2 2.073(3) . ?
Ni1 O41 2.093(3) . ?
Ni1 O1 2.096(3) . ?
Ni2 N3 1.986(4) . ?
Ni2 N61 1.996(4) . ?
Ni2 O61 2.046(3) . ?
Ni2 O62 2.047(3) . ?
Ni2 N4 2.120(4) . ?
Ni2 O2 2.204(3) . ?
Ni3 N21 2.015(4) . ?
Ni3 N43 2.030(4) . ?
Ni3 O21 2.047(4) . ?
Ni3 O22 2.137(3) . ?
Ni3 N44 2.141(4) . ?
Ni3 N42 2.160(4) . ?
Ni4 N63 2.001(4) . ?
Ni4 N23 2.002(5) . ?
Ni4 N24 2.101(5) . ?
Ni4 N64 2.122(4) . ?
Ni4 O22 2.130(3) . ?
Ni4 N62 2.139(4) . ?
C1 O1 1.377(6) . ?
C1 C2 1.406(8) . ?
C1 C6 1.407(8) . ?
C2 C3 1.355(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.448(8) . ?
C7 N1 1.284(6) . ?
C7 H7 0.9500 . ?
C8 O2 1.289(5) . ?
C8 N2 1.324(6) . ?
C8 C9 1.477(7) . ?
C9 N3 1.353(6) . ?
C9 C10 1.389(6) . ?
C10 C11 1.377(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(6) . ?
C12 H12 0.9500 . ?
C13 N3 1.332(6) . ?
C13 C14 1.494(7) . ?
C14 N4 1.353(6) . ?
C14 C15 1.374(7) . ?
C15 C16 1.400(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(8) . ?
C17 H17 0.9500 . ?
C18 N4 1.321(6) . ?
C18 H18 0.9500 . ?
N1 N2 1.390(6) . ?
C21 O21 1.318(6) . ?
C21 C26 1.388(8) . ?
C21 C22 1.429(8) . ?
C22 C23 1.356(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.339(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.429(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.425(9) . ?
C27 N21 1.298(7) . ?
C27 H27 0.9500 . ?
C28 N22 1.311(7) . ?
C28 O22 1.313(6) . ?
C28 C29 1.469(8) . ?
C29 N23 1.333(7) . ?
C29 C30 1.409(8) . ?
C30 C31 1.396(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.371(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(9) . ?
C32 H32 0.9500 . ?
C33 N23 1.335(7) . ?
C33 C34 1.469(9) . ?
C34 C35 1.373(9) . ?
C34 N24 1.403(8) . ?
C35 C36 1.364(12) . ?
C35 H35 0.9500 . ?
C36 C37 1.336(12) . ?
C36 H36 0.9500 . ?
C37 C38 1.394(9) . ?
C37 H37 0.9500 . ?
C38 N24 1.317(8) . ?
C38 H38 0.9500 . ?
N21 N22 1.404(6) . ?
C41 O41 1.381(5) . ?
C41 C42 1.396(7) . ?
C41 C46 1.412(6) . ?
C42 C43 1.365(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.370(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.375(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.428(6) . ?
C47 N41 1.277(6) . ?
C47 H47 0.9500 . ?
C48 O42 1.271(5) . ?
C48 N42 1.339(6) . ?
C48 C49 1.490(7) . ?
C49 N43 1.342(6) . ?
C49 C50 1.361(7) . ?
C50 C51 1.395(7) . ?
C50 H50 0.9500 . ?
C51 C52 1.374(8) . ?
C51 H51 0.9500 . ?
C52 C53 1.375(8) . ?
C52 H52 0.9500 . ?
C53 N43 1.332(6) . ?
C53 C54 1.486(8) . ?
C54 N44 1.352(7) . ?
C54 C55 1.392(7) . ?
C55 C56 1.376(9) . ?
C55 H55 0.9500 . ?
C56 C57 1.392(9) . ?
C56 H56 0.9500 . ?
C57 C58 1.396(8) . ?
C57 H57 0.9500 . ?
C58 N44 1.330(7) . ?
C58 H58 0.9500 . ?
N41 N42 1.394(5) . ?
C61 O61 1.341(6) . ?
C61 C62 1.391(7) . ?
C61 C66 1.416(7) . ?
C62 C63 1.391(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.396(8) . ?
C63 H63 0.9500 . ?
C64 C65 1.381(7) . ?
C64 H64 0.9500 . ?
C65 C66 1.412(7) . ?
C65 H65 0.9500 . ?
C66 C67 1.448(7) . ?
C67 N61 1.288(6) . ?
C67 H67 0.9500 . ?
C68 O62 1.272(5) . ?
C68 N62 1.341(6) . ?
C68 C69 1.471(6) . ?
C69 N63 1.346(6) . ?
C69 C70 1.381(7) . ?
C70 C71 1.389(8) . ?
C70 H70 0.9500 . ?
C71 C72 1.374(9) . ?
C71 H71 0.9500 . ?
C72 C73 1.397(9) . ?
C72 H72 0.9500 . ?
C73 N63 1.327(6) . ?
C73 C74 1.479(8) . ?
C74 N64 1.356(8) . ?
C74 C75 1.382(8) . ?
C75 C76 1.402(11) . ?
C75 H75 0.9500 . ?
C76 C77 1.346(11) . ?
C76 H76 0.9500 . ?
C77 C78 1.379(9) . ?
C77 H77 0.9500 . ?
C78 N64 1.345(8) . ?
C78 H78 0.9500 . ?
N61 N62 1.392(5) . ?
O81 Cl1 1.358(5) . ?
O82 Cl1 1.425(6) . ?
O83 Cl1 1.413(6) . ?
O84 Cl1 1.428(5) . ?
O85 Cl2 1.344(7) . ?
O86 Cl2 1.403(6) . ?
O87 Cl2 1.374(8) . ?
O88 Cl2 1.467(9) . ?
O89 Cl3 1.329(13) . ?
O90 Cl3 1.424(8) . ?
O91 Cl3 1.362(10) . ?
O92 Cl3 1.433(12) . ?
C91 N91 1.188(15) . ?
C91 C92 1.37(2) . ?
O101 H101 0.840(5) . ?
O101 H102 0.840(5) . ?
O102 H103 0.840(5) . ?
O102 H104 0.840(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
N41 Ni1 N1 175.40(16) . . ?
N41 Ni1 O42 78.80(14) . . ?
N1 Ni1 O42 105.30(15) . . ?
N41 Ni1 O2 103.48(13) . . ?
N1 Ni1 O2 78.45(14) . . ?
O42 Ni1 O2 94.75(13) . . ?
N41 Ni1 O41 86.44(14) . . ?
N1 Ni1 O41 89.41(15) . . ?
O42 Ni1 O41 165.21(13) . . ?
O2 Ni1 O41 89.51(13) . . ?
N41 Ni1 O1 92.49(14) . . ?
N1 Ni1 O1 85.83(15) . . ?
O42 Ni1 O1 85.57(13) . . ?
O2 Ni1 O1 163.80(12) . . ?
O41 Ni1 O1 94.26(13) . . ?
N3 Ni2 N61 174.85(16) . . ?
N3 Ni2 O61 92.70(14) . . ?
N61 Ni2 O61 89.05(14) . . ?
N3 Ni2 O62 99.31(14) . . ?
N61 Ni2 O62 79.49(14) . . ?
O61 Ni2 O62 166.67(14) . . ?
N3 Ni2 N4 78.31(15) . . ?
N61 Ni2 N4 96.68(15) . . ?
O61 Ni2 N4 96.94(15) . . ?
O62 Ni2 N4 91.17(14) . . ?
N3 Ni2 O2 77.48(14) . . ?
N61 Ni2 O2 107.39(14) . . ?
O61 Ni2 O2 89.62(13) . . ?
O62 Ni2 O2 87.38(12) . . ?
N4 Ni2 O2 155.17(13) . . ?
N21 Ni3 N43 170.60(16) . . ?
N21 Ni3 O21 87.59(17) . . ?
N43 Ni3 O21 88.07(15) . . ?
N21 Ni3 O22 77.14(16) . . ?
N43 Ni3 O22 107.54(14) . . ?
O21 Ni3 O22 164.34(14) . . ?
N21 Ni3 N44 94.78(16) . . ?
N43 Ni3 N44 77.42(16) . . ?
O21 Ni3 N44 96.30(15) . . ?
O22 Ni3 N44 88.49(15) . . ?
N21 Ni3 N42 112.16(15) . . ?
N43 Ni3 N42 76.21(15) . . ?
O21 Ni3 N42 90.58(15) . . ?
O22 Ni3 N42 91.99(13) . . ?
N44 Ni3 N42 152.47(16) . . ?
N63 Ni4 N23 176.05(17) . . ?
N63 Ni4 N24 101.5(2) . . ?
N23 Ni4 N24 78.2(2) . . ?
N63 Ni4 N64 77.23(18) . . ?
N23 Ni4 N64 98.84(19) . . ?
N24 Ni4 N64 92.65(17) . . ?
N63 Ni4 O22 102.85(15) . . ?
N23 Ni4 O22 77.50(17) . . ?
N24 Ni4 O22 155.65(18) . . ?
N64 Ni4 O22 91.73(15) . . ?
N63 Ni4 N62 78.00(16) . . ?
N23 Ni4 N62 105.93(16) . . ?
N24 Ni4 N62 92.99(16) . . ?
N64 Ni4 N62 155.22(18) . . ?
O22 Ni4 N62 92.99(14) . . ?
O1 C1 C2 119.7(5) . . ?
O1 C1 C6 120.6(5) . . ?
C2 C1 C6 119.7(5) . . ?
C3 C2 C1 120.4(6) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 121.2(6) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C3 C4 C5 119.1(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C6 121.7(6) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 117.9(5) . . ?
C5 C6 C7 117.3(5) . . ?
C1 C6 C7 124.8(5) . . ?
N1 C7 C6 126.2(5) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
O2 C8 N2 125.3(4) . . ?
O2 C8 C9 118.8(4) . . ?
N2 C8 C9 115.9(4) . . ?
N3 C9 C10 120.0(4) . . ?
N3 C9 C8 113.0(4) . . ?
C10 C9 C8 126.9(4) . . ?
C11 C10 C9 119.3(5) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 118.2(5) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
N3 C13 C12 121.2(4) . . ?
N3 C13 C14 113.5(4) . . ?
C12 C13 C14 125.3(4) . . ?
N4 C14 C15 122.5(5) . . ?
N4 C14 C13 114.8(4) . . ?
C15 C14 C13 122.7(4) . . ?
C14 C15 C16 119.0(5) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C17 C16 C15 118.2(5) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C16 C17 C18 118.9(5) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
N4 C18 C17 123.2(5) . . ?
N4 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
C7 N1 N2 114.5(4) . . ?
C7 N1 Ni1 130.1(4) . . ?
N2 N1 Ni1 115.0(3) . . ?
C8 N2 N1 111.4(4) . . ?
C13 N3 C9 121.1(4) . . ?
C13 N3 Ni2 119.6(3) . . ?
C9 N3 Ni2 119.2(3) . . ?
C18 N4 C14 118.2(4) . . ?
C18 N4 Ni2 128.0(3) . . ?
C14 N4 Ni2 113.5(3) . . ?
C1 O1 Ni1 129.1(3) . . ?
C8 O2 Ni1 109.8(3) . . ?
C8 O2 Ni2 111.2(3) . . ?
Ni1 O2 Ni2 138.93(15) . . ?
O21 C21 C26 123.8(5) . . ?
O21 C21 C22 118.6(6) . . ?
C26 C21 C22 117.6(5) . . ?
C23 C22 C21 121.4(7) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 120.8(7) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C23 119.1(6) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C24 C25 C26 122.1(7) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C21 C26 C27 124.3(5) . . ?
C21 C26 C25 119.1(6) . . ?
C27 C26 C25 116.5(6) . . ?
N21 C27 C26 126.1(5) . . ?
N21 C27 H27 117.0 . . ?
C26 C27 H27 117.0 . . ?
N22 C28 O22 126.0(5) . . ?
N22 C28 C29 117.5(5) . . ?
O22 C28 C29 116.6(5) . . ?
N23 C29 C30 120.5(6) . . ?
N23 C29 C28 113.5(5) . . ?
C30 C29 C28 125.9(6) . . ?
C31 C30 C29 118.4(7) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C32 C31 C30 119.3(6) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 119.6(6) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
N23 C33 C32 121.2(6) . . ?
N23 C33 C34 113.9(5) . . ?
C32 C33 C34 124.8(6) . . ?
C35 C34 N24 120.0(7) . . ?
C35 C34 C33 125.8(7) . . ?
N24 C34 C33 114.3(5) . . ?
C36 C35 C34 119.5(8) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C37 C36 C35 120.6(8) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C36 C37 C38 119.7(8) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
N24 C38 C37 121.5(7) . . ?
N24 C38 H38 119.2 . . ?
C37 C38 H38 119.2 . . ?
C27 N21 N22 115.4(5) . . ?
C27 N21 Ni3 126.7(4) . . ?
N22 N21 Ni3 117.1(3) . . ?
C28 N22 N21 110.7(4) . . ?
C29 N23 C33 121.0(5) . . ?
C29 N23 Ni4 118.8(4) . . ?
C33 N23 Ni4 120.0(4) . . ?
C38 N24 C34 118.7(5) . . ?
C38 N24 Ni4 127.7(5) . . ?
C34 N24 Ni4 113.6(4) . . ?
C21 O21 Ni3 127.9(4) . . ?
C28 O22 Ni4 113.5(3) . . ?
C28 O22 Ni3 108.7(3) . . ?
Ni4 O22 Ni3 137.72(17) . . ?
O41 C41 C42 120.1(4) . . ?
O41 C41 C46 120.3(4) . . ?
C42 C41 C46 119.6(4) . . ?
C43 C42 C41 120.4(5) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C42 C43 C44 120.8(5) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C45 119.7(5) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
C44 C45 C46 121.7(5) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 H45 119.2 . . ?
C45 C46 C41 117.7(4) . . ?
C45 C46 C47 117.4(4) . . ?
C41 C46 C47 124.9(4) . . ?
N41 C47 C46 126.1(4) . . ?
N41 C47 H47 116.9 . . ?
C46 C47 H47 116.9 . . ?
O42 C48 N42 125.6(4) . . ?
O42 C48 C49 120.4(4) . . ?
N42 C48 C49 113.9(4) . . ?
N43 C49 C50 121.2(5) . . ?
N43 C49 C48 114.3(4) . . ?
C50 C49 C48 124.6(5) . . ?
C49 C50 C51 118.4(5) . . ?
C49 C50 H50 120.8 . . ?
C51 C50 H50 120.8 . . ?
C52 C51 C50 119.6(5) . . ?
C52 C51 H51 120.2 . . ?
C50 C51 H51 120.2 . . ?
C51 C52 C53 119.4(5) . . ?
C51 C52 H52 120.3 . . ?
C53 C52 H52 120.3 . . ?
N43 C53 C52 120.2(5) . . ?
N43 C53 C54 114.0(4) . . ?
C52 C53 C54 125.8(5) . . ?
N44 C54 C55 121.3(5) . . ?
N44 C54 C53 115.2(4) . . ?
C55 C54 C53 123.5(5) . . ?
C56 C55 C54 119.3(6) . . ?
C56 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C55 C56 C57 119.9(5) . . ?
C55 C56 H56 120.0 . . ?
C57 C56 H56 120.0 . . ?
C56 C57 C58 117.2(6) . . ?
C56 C57 H57 121.4 . . ?
C58 C57 H57 121.4 . . ?
N44 C58 C57 123.4(6) . . ?
N44 C58 H58 118.3 . . ?
C57 C58 H58 118.3 . . ?
C47 N41 N42 116.2(4) . . ?
C47 N41 Ni1 129.8(3) . . ?
N42 N41 Ni1 113.9(3) . . ?
C48 N42 N41 110.4(4) . . ?
C48 N42 Ni3 115.1(3) . . ?
N41 N42 Ni3 134.5(3) . . ?
C53 N43 C49 121.3(4) . . ?
C53 N43 Ni3 118.4(3) . . ?
C49 N43 Ni3 118.8(3) . . ?
C58 N44 C54 118.9(5) . . ?
C58 N44 Ni3 127.2(4) . . ?
C54 N44 Ni3 113.7(3) . . ?
C41 O41 Ni1 126.3(3) . . ?
C48 O42 Ni1 109.8(3) . . ?
O61 C61 C62 119.5(4) . . ?
O61 C61 C66 121.5(4) . . ?
C62 C61 C66 119.0(5) . . ?
C61 C62 C63 120.9(5) . . ?
C61 C62 H62 119.5 . . ?
C63 C62 H62 119.5 . . ?
C62 C63 C64 121.1(5) . . ?
C62 C63 H63 119.5 . . ?
C64 C63 H63 119.5 . . ?
C65 C64 C63 118.1(5) . . ?
C65 C64 H64 121.0 . . ?
C63 C64 H64 121.0 . . ?
C64 C65 C66 122.4(5) . . ?
C64 C65 H65 118.8 . . ?
C66 C65 H65 118.8 . . ?
C65 C66 C61 118.5(4) . . ?
C65 C66 C67 116.5(4) . . ?
C61 C66 C67 125.0(4) . . ?
N61 C67 C66 126.3(4) . . ?
N61 C67 H67 116.9 . . ?
C66 C67 H67 116.9 . . ?
O62 C68 N62 126.3(4) . . ?
O62 C68 C69 118.5(4) . . ?
N62 C68 C69 115.3(4) . . ?
N63 C69 C70 120.6(5) . . ?
N63 C69 C68 114.7(4) . . ?
C70 C69 C68 124.7(5) . . ?
C69 C70 C71 118.5(5) . . ?
C69 C70 H70 120.8 . . ?
C71 C70 H70 120.8 . . ?
C72 C71 C70 120.0(6) . . ?
C72 C71 H71 120.0 . . ?
C70 C71 H71 120.0 . . ?
C71 C72 C73 119.0(5) . . ?
C71 C72 H72 120.5 . . ?
C73 C72 H72 120.5 . . ?
N63 C73 C72 120.1(5) . . ?
N63 C73 C74 114.0(5) . . ?
C72 C73 C74 125.8(5) . . ?
N64 C74 C75 121.4(6) . . ?
N64 C74 C73 114.2(5) . . ?
C75 C74 C73 124.4(6) . . ?
C74 C75 C76 118.3(8) . . ?
C74 C75 H75 120.9 . . ?
C76 C75 H75 120.9 . . ?
C77 C76 C75 120.1(7) . . ?
C77 C76 H76 120.0 . . ?
C75 C76 H76 120.0 . . ?
C76 C77 C78 119.3(7) . . ?
C76 C77 H77 120.3 . . ?
C78 C77 H77 120.3 . . ?
N64 C78 C77 122.1(7) . . ?
N64 C78 H78 118.9 . . ?
C77 C78 H78 118.9 . . ?
C67 N61 N62 117.3(4) . . ?
C67 N61 Ni2 127.3(3) . . ?
N62 N61 Ni2 114.9(3) . . ?
C68 N62 N61 110.0(4) . . ?
C68 N62 Ni4 113.4(3) . . ?
N61 N62 Ni4 135.7(3) . . ?
C73 N63 C69 121.6(5) . . ?
C73 N63 Ni4 120.0(4) . . ?
C69 N63 Ni4 118.4(3) . . ?
C78 N64 C74 118.8(5) . . ?
C78 N64 Ni4 126.7(4) . . ?
C74 N64 Ni4 114.5(4) . . ?
C61 O61 Ni2 128.0(3) . . ?
C68 O62 Ni2 109.3(3) . . ?
O81 Cl1 O83 107.7(5) . . ?
O81 Cl1 O82 112.9(6) . . ?
O83 Cl1 O82 100.5(6) . . ?
O81 Cl1 O84 113.1(4) . . ?
O83 Cl1 O84 109.9(3) . . ?
O82 Cl1 O84 111.9(4) . . ?
O85 Cl2 O87 110.4(8) . . ?
O85 Cl2 O86 112.9(6) . . ?
O87 Cl2 O86 107.3(5) . . ?
O85 Cl2 O88 106.8(8) . . ?
O87 Cl2 O88 105.7(9) . . ?
O86 Cl2 O88 113.3(7) . . ?
O89 Cl3 O91 111.9(14) . . ?
O89 Cl3 O90 108.7(13) . . ?
O91 Cl3 O90 109.6(9) . . ?
O89 Cl3 O92 111.4(16) . . ?
O91 Cl3 O92 103.2(13) . . ?
O90 Cl3 O92 112.0(10) . . ?
N91 C91 C92 176.3(19) . . ?
H101 O101 H102 107.3(9) . . ?
H103 O102 H104 107.0(9) . . ?
 
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
O101 H101 O1  0.840(5) 1.713(11) 2.540(5) 168(5) .
O101 H102 O21  0.840(5) 1.838(13) 2.652(6) 163(5) .
O102 H103 O61  0.840(5) 1.91(5) 2.652(5) 148(9) 2_646
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.978
_refine_diff_density_min   -1.280
_refine_diff_density_rms    0.121
