data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. Craig Matthews
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C18 H28 Cl2 N18 Ni O16'
_chemical_formula_weight          882.19
 
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            triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    11.1391(6)
_cell_length_b                    12.8788(6)
_cell_length_c                    14.1662(6)
_cell_angle_alpha                 63.891(3)
_cell_angle_beta                  68.400(3)
_cell_angle_gamma                 74.367(3)
_cell_volume                      1682.62(14)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     7316
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.741
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              904
_exptl_absorpt_coefficient_mu     0.835
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8643
_exptl_absorpt_correction_T_max   0.9362
_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             31370
_diffrn_reflns_av_R_equivalents   0.0555
_diffrn_reflns_av_sigmaI/netI     0.0530
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.48
_reflns_number_total              7687
_reflns_number_gt                 5825
_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)+(0.0548P)²+0.8413P] 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          7687
_refine_ls_number_parameters      518
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.0702
_refine_ls_R_factor_gt            0.0448
_refine_ls_wR_factor_ref          0.1079
_refine_ls_wR_factor_gt           0.0986
_refine_ls_goodness_of_fit_ref    1.018
_refine_ls_restrained_S_all       1.018
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ni1 Ni 0.76782(3) 0.18504(3) 0.19692(2) 0.01899(10) Uani 1 1 d . . .
C1 C 0.9039(2) 0.3598(2) 0.00066(19) 0.0206(5) Uani 1 1 d . . .
C2 C 0.7762(2) 0.3737(2) -0.0170(2) 0.0206(5) Uani 1 1 d . . .
C3 C 0.7484(3) 0.4453(2) -0.1160(2) 0.0243(6) Uani 1 1 d . . .
H3 H 0.8096 0.4925 -0.1764 0.029 Uiso 1 1 calc R . .
C4 C 0.6293(3) 0.4446(2) -0.1223(2) 0.0252(6) Uani 1 1 d . . .
H4 H 0.6044 0.4920 -0.1875 0.030 Uiso 1 1 calc R . .
C5 C 0.5451(2) 0.3725(2) -0.0307(2) 0.0212(5) Uani 1 1 d . . .
C6 C 0.4169(3) 0.3622(2) -0.0324(2) 0.0247(6) Uani 1 1 d . . .
N1 N 0.9224(2) 0.27043(17) 0.08706(16) 0.0205(4) Uani 1 1 d . . .
N2 N 0.9892(2) 0.43358(19) -0.06999(17) 0.0291(5) Uani 1 1 d . . .
H2A H 1.0656 0.4238 -0.0600 0.035 Uiso 1 1 calc R . .
H2B H 0.9695 0.4924 -0.1269 0.035 Uiso 1 1 calc R . .
N3 N 0.69069(19) 0.30777(17) 0.06954(16) 0.0195(4) Uani 1 1 d . . .
N4 N 0.5741(2) 0.30685(17) 0.06385(16) 0.0210(4) Uani 1 1 d . . .
N5 N 0.3305(2) 0.3079(2) 0.06243(18) 0.0332(6) Uani 1 1 d . . .
H5A H 0.2543 0.3005 0.0623 0.040 Uiso 1 1 calc R . .
H5B H 0.3502 0.2797 0.1247 0.040 Uiso 1 1 calc R . .
N6 N 0.3993(2) 0.4069(2) -0.12842(18) 0.0353(6) Uani 1 1 d . . .
O1 O 1.04328(17) 0.26468(15) 0.10077(14) 0.0238(4) Uani 1 1 d . . .
H1 H 1.0774 0.1949 0.1221 0.036 Uiso 1 1 calc R . .
O2 O 0.2762(2) 0.3851(2) -0.11840(16) 0.0457(6) Uani 1 1 d . . .
H2 H 0.2597 0.4216 -0.1790 0.069 Uiso 1 1 calc R . .
C11 C 0.8982(2) -0.0494(2) 0.28283(19) 0.0212(5) Uani 1 1 d . . .
C12 C 0.8651(2) -0.0458(2) 0.18881(19) 0.0215(5) Uani 1 1 d . . .
C13 C 0.8853(3) -0.1412(2) 0.1603(2) 0.0246(6) Uani 1 1 d . . .
H13 H 0.9191 -0.2165 0.2031 0.029 Uiso 1 1 calc R . .
C14 C 0.8547(3) -0.1227(2) 0.0685(2) 0.0263(6) Uani 1 1 d . . .
H14 H 0.8643 -0.1852 0.0466 0.032 Uiso 1 1 calc R . .
C15 C 0.8087(2) -0.0087(2) 0.0076(2) 0.0225(5) Uani 1 1 d . . .
C16 C 0.7817(3) 0.0261(2) -0.0982(2) 0.0256(6) Uani 1 1 d . . .
N11 N 0.8653(2) 0.04931(17) 0.29671(16) 0.0207(4) Uani 1 1 d . . .
N12 N 0.9596(2) -0.14546(18) 0.34215(17) 0.0274(5) Uani 1 1 d . . .
H12A H 0.9815 -0.1459 0.3960 0.033 Uiso 1 1 calc R . .
H12B H 0.9785 -0.2088 0.3276 0.033 Uiso 1 1 calc R . .
N13 N 0.8131(2) 0.05897(17) 0.13155(16) 0.0197(4) Uani 1 1 d . . .
N14 N 0.7852(2) 0.07927(17) 0.04058(16) 0.0217(5) Uani 1 1 d . . .
N15 N 0.7151(3) 0.1319(2) -0.1371(2) 0.0381(6) Uani 1 1 d . . .
H15A H 0.6988 0.1560 -0.2003 0.046 Uiso 1 1 calc R . .
H15B H 0.6879 0.1772 -0.0995 0.046 Uiso 1 1 calc R . .
N16 N 0.8260(2) -0.04695(19) -0.14663(17) 0.0249(5) Uani 1 1 d . . .
O11 O 0.91326(17) 0.04376(15) 0.37841(14) 0.0248(4) Uani 1 1 d . . .
H11 H 0.8571 0.0788 0.4169 0.037 Uiso 1 1 calc R . .
O12 O 0.79350(19) 0.00209(16) -0.24593(14) 0.0305(4) Uani 1 1 d . . .
H12 H 0.8259 -0.0434 -0.2795 0.046 Uiso 1 1 calc R . .
C21 C 0.5889(2) 0.2868(2) 0.35054(19) 0.0200(5) Uani 1 1 d . . .
C22 C 0.5208(2) 0.1943(2) 0.36377(19) 0.0196(5) Uani 1 1 d . . .
C23 C 0.3985(2) 0.1701(2) 0.4360(2) 0.0220(5) Uani 1 1 d . . .
H23 H 0.3493 0.2162 0.4780 0.026 Uiso 1 1 calc R . .
C24 C 0.3510(3) 0.0774(2) 0.4447(2) 0.0223(5) Uani 1 1 d . . .
H24 H 0.2670 0.0582 0.4918 0.027 Uiso 1 1 calc R . .
C25 C 0.4307(2) 0.0122(2) 0.38194(19) 0.0200(5) Uani 1 1 d . . .
C26 C 0.3924(2) -0.0937(2) 0.38974(19) 0.0210(5) Uani 1 1 d . . .
N21 N 0.7071(2) 0.28708(17) 0.28718(16) 0.0203(4) Uani 1 1 d . . .
N22 N 0.5283(2) 0.35989(18) 0.40212(17) 0.0259(5) Uani 1 1 d . . .
H22A H 0.5692 0.4141 0.3943 0.031 Uiso 1 1 calc R . .
H22B H 0.4473 0.3539 0.4440 0.031 Uiso 1 1 calc R . .
N23 N 0.5898(2) 0.13274(16) 0.30136(16) 0.0195(4) Uani 1 1 d . . .
N24 N 0.5460(2) 0.04042(17) 0.31039(16) 0.0209(4) Uani 1 1 d . . .
N25 N 0.4744(2) -0.14998(19) 0.32482(18) 0.0292(5) Uani 1 1 d . . .
H25A H 0.4554 -0.2145 0.3296 0.035 Uiso 1 1 calc R . .
H25B H 0.5469 -0.1222 0.2777 0.035 Uiso 1 1 calc R . .
N26 N 0.2836(2) -0.12624(17) 0.46162(17) 0.0234(5) Uani 1 1 d . . .
O21 O 0.76544(17) 0.37650(14) 0.27853(15) 0.0268(4) Uani 1 1 d . . .
H21 H 0.8454 0.3549 0.2710 0.040 Uiso 1 1 calc R . .
O22 O 0.26497(19) -0.22925(15) 0.45893(15) 0.0295(4) Uani 1 1 d . . .
H22 H 0.1915 -0.2481 0.5011 0.044 Uiso 1 1 calc R . .
O31 O 1.02213(18) 0.35912(15) 0.26522(14) 0.0287(4) Uani 1 1 d . . .
O32 O 1.00134(18) 0.21112(16) 0.44040(14) 0.0297(4) Uani 1 1 d . . .
O33 O 1.18177(18) 0.19538(16) 0.29365(14) 0.0296(4) Uani 1 1 d . . .
O34 O 1.16317(19) 0.33505(16) 0.36384(16) 0.0338(5) Uani 1 1 d . . .
Cl31 Cl 1.09283(6) 0.27544(5) 0.34115(5) 0.02248(14) Uani 1 1 d . . .
O35 O 0.6459(2) 0.51277(19) 0.44896(18) 0.0455(6) Uani 1 1 d . . .
O36 O 0.8143(2) 0.59024(17) 0.28698(15) 0.0389(5) Uani 1 1 d . . .
O37 O 0.8610(3) 0.4796(2) 0.45387(19) 0.0598(7) Uani 1 1 d . . .
O38 O 0.7427(2) 0.66733(18) 0.42282(18) 0.0420(5) Uani 1 1 d . . .
Cl35 Cl 0.76542(7) 0.56269(5) 0.40252(5) 0.02819(16) Uani 1 1 d . . .
O1W O 1.0888(3) 0.6357(2) 0.3160(2) 0.0459(6) Uani 1 1 d D . .
H1WA H 1.046(3) 0.583(3) 0.364(3) 0.071(15) Uiso 1 1 d D . .
H1WB H 1.152(3) 0.634(3) 0.333(3) 0.063(13) Uiso 1 1 d D . .
O2W O 0.6135(3) 0.34967(19) 0.69386(18) 0.0454(6) Uani 1 1 d D . .
H2WA H 0.619(4) 0.386(3) 0.6279(15) 0.075(14) Uiso 1 1 d D . .
H2WB H 0.545(3) 0.379(3) 0.729(2) 0.075(14) 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 N1 2.034(2) . ?
Ni1 N11 2.041(2) . ?
Ni1 N21 2.045(2) . ?
Ni1 N23 2.064(2) . ?
Ni1 N13 2.070(2) . ?
Ni1 N3 2.096(2) . ?
C1 N1 1.297(3) . ?
C1 N2 1.326(3) . ?
C1 C2 1.484(3) . ?
C2 N3 1.339(3) . ?
C2 C3 1.393(3) . ?
C3 C4 1.365(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(4) . ?
C4 H4 0.9500 . ?
C5 N4 1.336(3) . ?
C5 C6 1.480(4) . ?
C6 N6 1.291(3) . ?
C6 N5 1.343(3) . ?
N1 O1 1.408(3) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N3 N4 1.334(3) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 O2 1.417(3) . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
C11 N11 1.306(3) . ?
C11 N12 1.325(3) . ?
C11 C12 1.487(3) . ?
C12 N13 1.333(3) . ?
C12 C13 1.394(3) . ?
C13 C14 1.370(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.403(3) . ?
C14 H14 0.9500 . ?
C15 N14 1.337(3) . ?
C15 C16 1.484(3) . ?
C16 N16 1.292(3) . ?
C16 N15 1.344(3) . ?
N11 O11 1.412(3) . ?
N12 H12A 0.8800 . ?
N12 H12B 0.8800 . ?
N13 N14 1.334(3) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?
N16 O12 1.406(3) . ?
O11 H11 0.8400 . ?
O12 H12 0.8400 . ?
C21 N21 1.292(3) . ?
C21 N22 1.332(3) . ?
C21 C22 1.489(3) . ?
C22 N23 1.338(3) . ?
C22 C23 1.386(3) . ?
C23 C24 1.372(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.400(3) . ?
C24 H24 0.9500 . ?
C25 N24 1.333(3) . ?
C25 C26 1.483(3) . ?
C26 N26 1.293(3) . ?
C26 N25 1.348(3) . ?
N21 O21 1.409(3) . ?
N22 H22A 0.8800 . ?
N22 H22B 0.8800 . ?
N23 N24 1.342(3) . ?
N25 H25A 0.8800 . ?
N25 H25B 0.8800 . ?
N26 O22 1.415(3) . ?
O21 H21 0.8400 . ?
O22 H22 0.8400 . ?
O31 Cl31 1.4438(18) . ?
O32 Cl31 1.4410(18) . ?
O33 Cl31 1.4377(18) . ?
O34 Cl31 1.4259(19) . ?
O35 Cl35 1.436(2) . ?
O36 Cl35 1.428(2) . ?
O37 Cl35 1.442(2) . ?
O38 Cl35 1.4376(19) . ?
O1W H1WA 0.826(18) . ?
O1W H1WB 0.823(17) . ?
O2W H2WA 0.826(18) . ?
O2W H2WB 0.839(18) . ?
 
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 N11 98.15(8) . . ?
N1 Ni1 N21 95.29(8) . . ?
N11 Ni1 N21 97.27(8) . . ?
N1 Ni1 N23 168.08(8) . . ?
N11 Ni1 N23 91.97(8) . . ?
N21 Ni1 N23 77.09(8) . . ?
N1 Ni1 N13 93.98(8) . . ?
N11 Ni1 N13 76.88(8) . . ?
N21 Ni1 N13 169.68(8) . . ?
N23 Ni1 N13 94.46(8) . . ?
N1 Ni1 N3 77.27(8) . . ?
N11 Ni1 N3 167.55(8) . . ?
N21 Ni1 N3 94.69(8) . . ?
N23 Ni1 N3 94.05(8) . . ?
N13 Ni1 N3 91.78(8) . . ?
N1 C1 N2 125.3(2) . . ?
N1 C1 C2 114.3(2) . . ?
N2 C1 C2 120.4(2) . . ?
N3 C2 C3 122.4(2) . . ?
N3 C2 C1 114.1(2) . . ?
C3 C2 C1 123.5(2) . . ?
C4 C3 C2 117.1(2) . . ?
C4 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?
C3 C4 C5 118.2(2) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
N4 C5 C4 123.1(2) . . ?
N4 C5 C6 115.3(2) . . ?
C4 C5 C6 121.6(2) . . ?
N6 C6 N5 125.6(2) . . ?
N6 C6 C5 115.2(2) . . ?
N5 C6 C5 119.2(2) . . ?
C1 N1 O1 111.23(19) . . ?
C1 N1 Ni1 118.30(17) . . ?
O1 N1 Ni1 128.82(14) . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
N4 N3 C2 120.8(2) . . ?
N4 N3 Ni1 123.27(15) . . ?
C2 N3 Ni1 114.73(16) . . ?
N3 N4 C5 118.4(2) . . ?
C6 N5 H5A 120.0 . . ?
C6 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C6 N6 O2 109.1(2) . . ?
N1 O1 H1 109.5 . . ?
N6 O2 H2 109.5 . . ?
N11 C11 N12 125.4(2) . . ?
N11 C11 C12 113.9(2) . . ?
N12 C11 C12 120.7(2) . . ?
N13 C12 C13 121.5(2) . . ?
N13 C12 C11 113.9(2) . . ?
C13 C12 C11 124.7(2) . . ?
C14 C13 C12 117.7(2) . . ?
C14 C13 H13 121.2 . . ?
C12 C13 H13 121.2 . . ?
C13 C14 C15 118.0(2) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
N14 C15 C14 122.3(2) . . ?
N14 C15 C16 113.8(2) . . ?
C14 C15 C16 123.9(2) . . ?
N16 C16 N15 125.0(2) . . ?
N16 C16 C15 117.4(2) . . ?
N15 C16 C15 117.6(2) . . ?
C11 N11 O11 110.79(19) . . ?
C11 N11 Ni1 118.49(16) . . ?
O11 N11 Ni1 130.59(14) . . ?
C11 N12 H12A 120.0 . . ?
C11 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
C12 N13 N14 121.7(2) . . ?
C12 N13 Ni1 116.21(16) . . ?
N14 N13 Ni1 122.02(15) . . ?
N13 N14 C15 118.7(2) . . ?
C16 N15 H15A 120.0 . . ?
C16 N15 H15B 120.0 . . ?
H15A N15 H15B 120.0 . . ?
C16 N16 O12 109.1(2) . . ?
N11 O11 H11 109.5 . . ?
N16 O12 H12 109.5 . . ?
N21 C21 N22 125.6(2) . . ?
N21 C21 C22 114.0(2) . . ?
N22 C21 C22 120.4(2) . . ?
N23 C22 C23 121.9(2) . . ?
N23 C22 C21 114.0(2) . . ?
C23 C22 C21 124.0(2) . . ?
C24 C23 C22 117.8(2) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
C23 C24 C25 117.7(2) . . ?
C23 C24 H24 121.1 . . ?
C25 C24 H24 121.1 . . ?
N24 C25 C24 122.8(2) . . ?
N24 C25 C26 114.9(2) . . ?
C24 C25 C26 122.2(2) . . ?
N26 C26 N25 125.3(2) . . ?
N26 C26 C25 116.5(2) . . ?
N25 C26 C25 118.1(2) . . ?
C21 N21 O21 110.92(19) . . ?
C21 N21 Ni1 118.04(16) . . ?
O21 N21 Ni1 129.98(15) . . ?
C21 N22 H22A 120.0 . . ?
C21 N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 . . ?
C22 N23 N24 121.1(2) . . ?
C22 N23 Ni1 115.86(16) . . ?
N24 N23 Ni1 123.04(15) . . ?
C25 N24 N23 118.5(2) . . ?
C26 N25 H25A 120.0 . . ?
C26 N25 H25B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
C26 N26 O22 108.40(19) . . ?
N21 O21 H21 109.5 . . ?
N26 O22 H22 109.5 . . ?
O34 Cl31 O33 109.80(12) . . ?
O34 Cl31 O32 110.68(11) . . ?
O33 Cl31 O32 108.78(11) . . ?
O34 Cl31 O31 109.44(11) . . ?
O33 Cl31 O31 109.40(11) . . ?
O32 Cl31 O31 108.72(11) . . ?
O36 Cl35 O35 111.50(13) . . ?
O36 Cl35 O38 109.13(12) . . ?
O35 Cl35 O38 109.04(12) . . ?
O36 Cl35 O37 108.62(14) . . ?
O35 Cl35 O37 108.75(15) . . ?
O38 Cl35 O37 109.78(15) . . ?
H1WA O1W H1WB 110(3) . . ?
H2WA O2W H2WB 107(3) . . ?
 
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
N2 H2A O2  0.88 2.18 2.960(3) 148.1 1_655
N2 H2B O31  0.88 2.04 2.893(3) 162.3 2_765
N5 H5A O1  0.88 2.34 3.203(3) 168.4 1_455
N5 H5B O33  0.88 2.44 2.949(3) 117.6 1_455
O1 H1 N16  0.84 1.87 2.701(3) 170.4 2_755
O2 H2 O36  0.84 2.06 2.784(3) 144.0 2_665
O2 H2 O21  0.84 2.34 2.944(3) 128.7 2_665
N12 H12A O32  0.88 2.15 2.981(3) 156.5 2_756
N12 H12B O1W  0.88 2.09 2.914(3) 155.8 1_545
N15 H15A O2W  0.88 2.42 3.042(3) 128.0 1_554
O11 H11 N26  0.84 2.05 2.877(3) 166.8 2_656
O12 H12 O33  0.84 2.08 2.828(3) 148.2 2_755
N22 H22B O38  0.88 2.24 3.111(3) 168.7 2_666
N22 H22B O35  0.88 2.55 3.037(3) 115.8 2_666
N25 H25A O2W  0.88 2.27 3.129(3) 165.6 2_656
O21 H21 O31  0.84 1.95 2.749(3) 157.5 .
O22 H22 O32  0.84 2.00 2.774(3) 152.1 2_656
O1W H1WA O37  0.826(18) 2.38(2) 3.153(4) 155(3) .
O1W H1WB O2W  0.823(17) 2.55(2) 3.321(4) 157(3) 2_766
O2W H2WA O35  0.826(18) 2.29(2) 3.107(3) 169(4) .
O2W H2WB N6  0.839(18) 2.18(2) 2.973(3) 157(3) 1_556
 
_diffrn_measured_fraction_theta_max    0.995
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    0.676
_refine_diff_density_min   -0.521
_refine_diff_density_rms    0.075
