 
data_04src0194
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C44 H46 Cl4 N16 Ni2 O21'
_chemical_formula_weight          1394.19
 
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            Orthorhombic
_symmetry_space_group_name_H-M    Pna2(1)
_symmetry_space_group_name_hall   'P 2c -2n'
 
loop_
 _symmetry_equiv_pos_as_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                    25.809(5)
_cell_length_b                    11.899(5)
_cell_length_c                    17.357(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      5330(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6933
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.737
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2856
_exptl_absorpt_coefficient_mu     1.004
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8093
_exptl_absorpt_correction_T_max   0.9705
_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             87747
_diffrn_reflns_av_R_equivalents   0.1260
_diffrn_reflns_av_sigmaI/netI     0.0998
_diffrn_reflns_limit_h_min        -33
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          3.01
_diffrn_reflns_theta_max          27.48
_reflns_number_total              12190
_reflns_number_gt                 8263
_reflns_threshold_expression      >2σ(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 > 2σ(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)+(0.0623P)²+30.2162P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_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 H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.52(3)
_refine_ls_number_reflns          12190
_refine_ls_number_parameters      786
_refine_ls_number_restraints      823
_refine_ls_R_factor_all           0.1288
_refine_ls_R_factor_gt            0.0810
_refine_ls_wR_factor_ref          0.1905
_refine_ls_wR_factor_gt           0.1720
_refine_ls_goodness_of_fit_ref    1.069
_refine_ls_restrained_S_all       1.044
_refine_ls_shift/su_max           0.004
_refine_ls_shift/su_mean          0.001
 
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
C1 C 0.0278(4) 0.0870(8) 0.5847(6) 0.027(2) Uani 1 1 d U . .
H1 H 0.0452 0.0267 0.5598 0.032 Uiso 1 1 calc R . .
C2 C -0.0136(4) 0.0613(8) 0.6297(6) 0.026(2) Uani 1 1 d U . .
H2 H -0.0272 -0.0128 0.6326 0.031 Uiso 1 1 calc R . .
C3 C -0.0352(4) 0.1506(9) 0.6715(6) 0.032(2) Uani 1 1 d U . .
H3 H -0.0636 0.1380 0.7054 0.038 Uiso 1 1 calc R . .
C4 C -0.0147(4) 0.2568(8) 0.6629(6) 0.025(2) Uani 1 1 d U . .
H4 H -0.0284 0.3178 0.6919 0.030 Uiso 1 1 calc R . .
C5 C 0.0256(3) 0.2743(8) 0.6122(6) 0.0210(17) Uani 1 1 d U . .
C6 C 0.0508(3) 0.3843(8) 0.6031(5) 0.0183(16) Uani 1 1 d U . .
C7 C 0.0340(3) 0.4865(7) 0.6319(5) 0.0183(17) Uani 1 1 d U . .
H7 H 0.0034 0.4919 0.6620 0.022 Uiso 1 1 calc R . .
C8 C 0.0624(4) 0.5768(8) 0.6160(6) 0.025(2) Uani 1 1 d U . .
H8 H 0.0508 0.6475 0.6348 0.030 Uiso 1 1 calc R . .
C9 C 0.1080(4) 0.5737(7) 0.5734(5) 0.0173(17) Uani 1 1 d U . .
H9 H 0.1282 0.6389 0.5634 0.021 Uiso 1 1 calc R . .
C10 C 0.1217(3) 0.4693(7) 0.5469(5) 0.0154(16) Uani 1 1 d U . .
C11 C 0.1676(3) 0.4429(6) 0.4964(6) 0.0173(15) Uani 1 1 d U . .
C12 C 0.2058(4) 0.2709(8) 0.3593(5) 0.0197(18) Uani 1 1 d U . .
C13 C 0.2496(3) 0.1977(7) 0.3354(5) 0.0181(17) Uani 1 1 d U . .
C14 C 0.2609(4) 0.1613(7) 0.2651(5) 0.0219(18) Uani 1 1 d U . .
H14 H 0.2394 0.1841 0.2234 0.026 Uiso 1 1 calc R . .
C15 C 0.3032(4) 0.0904(8) 0.2498(6) 0.0250(19) Uani 1 1 d U . .
H15 H 0.3125 0.0666 0.1994 0.030 Uiso 1 1 calc R . .
C16 C 0.3301(4) 0.0587(8) 0.3154(6) 0.0278(19) Uani 1 1 d U . .
H16 H 0.3585 0.0085 0.3097 0.033 Uiso 1 1 calc R . .
C17 C 0.3182(3) 0.0957(8) 0.3884(5) 0.0206(17) Uani 1 1 d U . .
C18 C 0.3457(3) 0.0724(8) 0.4617(6) 0.0201(18) Uani 1 1 d U . .
C19 C 0.3863(4) 0.0007(9) 0.4666(6) 0.031(2) Uani 1 1 d U . .
H19 H 0.4001 -0.0337 0.4217 0.037 Uiso 1 1 calc R . .
C20 C 0.4070(4) -0.0213(9) 0.5371(6) 0.032(2) Uani 1 1 d U . .
H20 H 0.4349 -0.0731 0.5413 0.039 Uiso 1 1 calc R . .
C21 C 0.3889(3) 0.0289(8) 0.6005(7) 0.030(2) Uani 1 1 d U . .
H21 H 0.4025 0.0136 0.6503 0.035 Uiso 1 1 calc R . .
C22 C 0.3473(3) 0.1078(8) 0.5884(6) 0.026(2) Uani 1 1 d U . .
H22 H 0.3341 0.1470 0.6319 0.031 Uiso 1 1 calc R . .
C31 C 0.0268(3) 0.3930(8) 0.4067(6) 0.0207(18) Uani 1 1 d U . .
H31 H 0.0402 0.4531 0.4366 0.025 Uiso 1 1 calc R . .
C32 C -0.0127(3) 0.4154(7) 0.3546(5) 0.0203(18) Uani 1 1 d U . .
H32 H -0.0239 0.4903 0.3452 0.024 Uiso 1 1 calc R . .
C33 C -0.0346(3) 0.3286(8) 0.3179(6) 0.0246(19) Uani 1 1 d U . .
H33 H -0.0625 0.3421 0.2835 0.030 Uiso 1 1 calc R . .
C34 C -0.0178(4) 0.2221(9) 0.3288(6) 0.0250(19) Uani 1 1 d U . .
H34 H -0.0348 0.1602 0.3053 0.030 Uiso 1 1 calc R . .
C35 C 0.0252(4) 0.2069(8) 0.3754(5) 0.0182(17) Uani 1 1 d U . .
C36 C 0.0506(4) 0.0980(8) 0.3891(6) 0.0216(18) Uani 1 1 d U . .
C37 C 0.0328(4) -0.0051(8) 0.3617(6) 0.029(2) Uani 1 1 d U . .
H37 H 0.0024 -0.0092 0.3309 0.035 Uiso 1 1 calc R . .
C38 C 0.0604(3) -0.1021(8) 0.3804(6) 0.0201(18) Uani 1 1 d U . .
H38 H 0.0486 -0.1738 0.3639 0.024 Uiso 1 1 calc R . .
C39 C 0.1055(3) -0.0918(8) 0.4235(6) 0.0249(19) Uani 1 1 d U . .
H39 H 0.1255 -0.1563 0.4361 0.030 Uiso 1 1 calc R . .
C40 C 0.1205(3) 0.0123(7) 0.4476(6) 0.0187(17) Uani 1 1 d U . .
C41 C 0.1662(3) 0.0381(6) 0.4935(6) 0.0176(15) Uani 1 1 d U . .
C42 C 0.2036(4) 0.2165(8) 0.6315(5) 0.0185(17) Uani 1 1 d U . .
C43 C 0.2453(3) 0.2914(8) 0.6553(5) 0.0207(17) Uani 1 1 d U . .
C44 C 0.2559(4) 0.3286(8) 0.7314(6) 0.0249(19) Uani 1 1 d U . .
H44 H 0.2375 0.3015 0.7750 0.030 Uiso 1 1 calc R . .
C45 C 0.2945(4) 0.4062(8) 0.7368(5) 0.0245(19) Uani 1 1 d U . .
H45 H 0.3013 0.4365 0.7864 0.029 Uiso 1 1 calc R . .
C46 C 0.3234(4) 0.4433(8) 0.6788(6) 0.027(2) Uani 1 1 d U . .
H46 H 0.3501 0.4974 0.6858 0.033 Uiso 1 1 calc R . .
C47 C 0.3116(3) 0.3964(8) 0.6060(5) 0.0215(17) Uani 1 1 d U . .
C48 C 0.3401(3) 0.4260(7) 0.5355(5) 0.0173(16) Uani 1 1 d U . .
C49 C 0.3764(3) 0.5065(8) 0.5303(5) 0.0218(18) Uani 1 1 d U . .
H49 H 0.3847 0.5495 0.5748 0.026 Uiso 1 1 calc R . .
C50 C 0.4019(4) 0.5284(8) 0.4621(6) 0.026(2) Uani 1 1 d U . .
H50 H 0.4282 0.5841 0.4587 0.031 Uiso 1 1 calc R . .
C51 C 0.3869(4) 0.4640(8) 0.3978(6) 0.026(2) Uani 1 1 d U . .
H51 H 0.4028 0.4768 0.3492 0.031 Uiso 1 1 calc R . .
C52 C 0.3506(4) 0.3851(9) 0.4049(6) 0.026(2) Uani 1 1 d U . .
H52 H 0.3411 0.3421 0.3611 0.031 Uiso 1 1 calc R . .
N1 N 0.0458(3) 0.1905(6) 0.5729(4) 0.0179(14) Uani 1 1 d U . .
N2 N 0.0939(3) 0.3786(6) 0.5611(4) 0.0162(13) Uani 1 1 d U . .
N3 N 0.2071(3) 0.5112(6) 0.4994(5) 0.0230(15) Uani 1 1 d U . .
H3A H 0.2354 0.4959 0.4732 0.028 Uiso 1 1 calc R . .
H3B H 0.2054 0.5725 0.5276 0.028 Uiso 1 1 calc R . .
N4 N 0.1628(2) 0.3508(6) 0.4592(4) 0.0142(13) Uani 1 1 d U . .
N5 N 0.2099(3) 0.3114(6) 0.4279(4) 0.0175(14) Uani 1 1 d U . .
N6 N 0.1671(3) 0.2855(7) 0.3138(5) 0.0269(18) Uani 1 1 d U . .
H6A H 0.1404 0.3261 0.3287 0.032 Uiso 1 1 calc R . .
H6B H 0.1673 0.2548 0.2676 0.032 Uiso 1 1 calc R . .
N7 N 0.2780(3) 0.1664(6) 0.3996(4) 0.0212(15) Uani 1 1 d U . .
N8 N 0.3277(3) 0.1276(6) 0.5239(4) 0.0225(15) Uani 1 1 d U . .
N31 N 0.0466(3) 0.2908(6) 0.4164(4) 0.0167(13) Uani 1 1 d U . .
N32 N 0.0936(3) 0.1037(6) 0.4303(4) 0.0180(14) Uani 1 1 d U . .
N33 N 0.2083(3) -0.0254(6) 0.4915(5) 0.0242(17) Uani 1 1 d U . .
H33A H 0.2360 -0.0056 0.5179 0.029 Uiso 1 1 calc R . .
H33B H 0.2086 -0.0873 0.4639 0.029 Uiso 1 1 calc R . .
N34 N 0.1626(3) 0.1306(6) 0.5329(4) 0.0229(15) Uani 1 1 d U . .
N35 N 0.2087(3) 0.1723(6) 0.5626(4) 0.0181(14) Uani 1 1 d U . .
N36 N 0.1629(3) 0.2002(7) 0.6789(4) 0.0237(17) Uani 1 1 d U . .
H36A H 0.1370 0.1570 0.6643 0.028 Uiso 1 1 calc R . .
H36B H 0.1621 0.2328 0.7244 0.028 Uiso 1 1 calc R . .
N37 N 0.2743(3) 0.3254(6) 0.5979(4) 0.0181(14) Uani 1 1 d U . .
N38 N 0.3266(2) 0.3644(6) 0.4741(4) 0.0171(14) Uani 1 1 d U . .
Ni1 Ni 0.10293(3) 0.24214(10) 0.49517(10) 0.01781(19) Uani 1 1 d U . .
Ni2 Ni 0.26906(3) 0.24429(10) 0.49723(10) 0.01792(19) Uani 1 1 d U . .
O1 O 0.0652(3) 0.1706(5) 0.7905(4) 0.0352(18) Uani 1 1 d DU . .
O2 O 0.1356(2) 0.2573(6) 0.8465(5) 0.0328(19) Uani 1 1 d DU . .
O3 O 0.0748(3) 0.3618(5) 0.7815(4) 0.0290(16) Uani 1 1 d DU . .
O4 O 0.0527(3) 0.2825(7) 0.8991(4) 0.0388(18) Uani 1 1 d DU . .
Cl1 Cl 0.08204(10) 0.26751(19) 0.83047(15) 0.0267(5) Uani 1 1 d DU . .
O11 O 0.1367(3) 0.2450(6) 1.1519(5) 0.038(2) Uani 1 1 d DU . .
O12 O 0.0546(3) 0.2216(7) 1.0999(4) 0.0383(19) Uani 1 1 d DU . .
O13 O 0.0638(3) 0.3289(6) 1.2113(5) 0.040(2) Uani 1 1 d DU . .
O14 O 0.0769(3) 0.1360(6) 1.2167(4) 0.0327(17) Uani 1 1 d DU . .
Cl11 Cl 0.08139(10) 0.2341(2) 1.16958(14) 0.0240(5) Uani 1 1 d DU . .
O21 O 0.1215(3) -0.2059(6) 0.7274(4) 0.0370(17) Uani 1 1 d DU . .
O22 O 0.1862(3) -0.1036(6) 0.6652(4) 0.0537(19) Uani 1 1 d DU . .
O23 O 0.1106(4) -0.1511(7) 0.6000(4) 0.060(2) Uani 1 1 d DU . .
O24 O 0.1074(3) -0.0207(5) 0.6968(4) 0.0437(18) Uani 1 1 d DU . .
Cl21 Cl 0.13453(9) -0.12069(19) 0.67272(14) 0.0296(5) Uani 1 1 d DU . .
O31 O -0.0614(3) 0.4036(8) 0.7977(6) 0.091(3) Uani 1 1 d DU . .
O32 O -0.1315(4) 0.2938(6) 0.7777(5) 0.061(2) Uani 1 1 d DU . .
O33 O -0.1399(4) 0.4854(6) 0.8025(5) 0.075(3) Uani 1 1 d DU . .
O34 O -0.1157(4) 0.3634(7) 0.8991(4) 0.068(3) Uani 1 1 d DU . .
Cl31 Cl -0.11491(11) 0.3856(2) 0.81944(16) 0.0402(6) Uani 1 1 d DU . .
O51 O 0.2314(3) 0.7069(6) 0.5816(4) 0.0386(18) Uani 1 1 d . . .
O52 O 0.2788(3) 0.5950(7) 0.3776(5) 0.060(2) Uani 1 1 d . . .
O53 O 0.2575(4) 0.0397(7) 0.7404(6) 0.075(3) Uani 1 1 d . . .
O54 O 0.2150(3) -0.2192(7) 0.4003(4) 0.049(2) Uani 1 1 d . . .
O55 O 0.1852(3) 0.2929(8) 1.0061(7) 0.085(3) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 N1 1.332(12) . ?
C1 C2 1.359(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.403(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(13) . ?
C4 H4 0.9500 . ?
C5 N1 1.316(12) . ?
C5 C6 1.470(13) . ?
C6 N2 1.334(11) . ?
C6 C7 1.383(12) . ?
C7 C8 1.328(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.371(11) . ?
C9 H9 0.9500 . ?
C10 N2 1.318(11) . ?
C10 C11 1.507(12) . ?
C11 N4 1.279(10) . ?
C11 N3 1.304(10) . ?
C12 N6 1.285(12) . ?
C12 N5 1.288(11) . ?
C12 C13 1.487(12) . ?
C13 C14 1.327(13) . ?
C13 N7 1.383(12) . ?
C14 C15 1.406(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(14) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(13) . ?
C16 H16 0.9500 . ?
C17 N7 1.350(11) . ?
C17 C18 1.483(13) . ?
C18 N8 1.346(12) . ?
C18 C19 1.355(13) . ?
C19 C20 1.360(14) . ?
C19 H19 0.9500 . ?
C20 C21 1.338(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.440(13) . ?
C21 H21 0.9500 . ?
C22 N8 1.252(12) . ?
C22 H22 0.9500 . ?
C31 N31 1.329(11) . ?
C31 C32 1.389(13) . ?
C31 H31 0.9500 . ?
C32 C33 1.338(12) . ?
C32 H32 0.9500 . ?
C33 C34 1.352(13) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(13) . ?
C34 H34 0.9500 . ?
C35 N31 1.345(11) . ?
C35 C36 1.471(13) . ?
C36 N32 1.322(11) . ?
C36 C37 1.394(13) . ?
C37 C38 1.395(13) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(12) . ?
C38 H38 0.9500 . ?
C39 C40 1.364(13) . ?
C39 H39 0.9500 . ?
C40 N32 1.325(11) . ?
C40 C41 1.456(12) . ?
C41 N34 1.299(11) . ?
C41 N33 1.325(10) . ?
C42 N35 1.313(11) . ?
C42 N36 1.350(11) . ?
C42 C43 1.456(13) . ?
C43 N37 1.310(11) . ?
C43 C44 1.419(13) . ?
C44 C45 1.362(13) . ?
C44 H44 0.9500 . ?
C45 C46 1.328(14) . ?
C45 H45 0.9500 . ?
C46 C47 1.415(13) . ?
C46 H46 0.9500 . ?
C47 N37 1.288(11) . ?
C47 C48 1.472(13) . ?
C48 N38 1.339(11) . ?
C48 C49 1.342(13) . ?
C49 C50 1.380(13) . ?
C49 H49 0.9500 . ?
C50 C51 1.408(14) . ?
C50 H50 0.9500 . ?
C51 C52 1.332(13) . ?
C51 H51 0.9500 . ?
C52 N38 1.373(12) . ?
C52 H52 0.9500 . ?
N1 Ni1 2.090(8) . ?
N2 Ni1 1.999(7) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N4 N5 1.412(9) . ?
N4 Ni1 2.108(7) . ?
N5 Ni2 2.103(7) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N7 Ni2 1.946(8) . ?
N8 Ni2 2.105(7) . ?
N31 Ni1 2.079(8) . ?
N32 Ni1 2.009(7) . ?
N33 H33A 0.8800 . ?
N33 H33B 0.8800 . ?
N34 N35 1.389(10) . ?
N34 Ni1 2.136(7) . ?
N35 Ni2 2.109(7) . ?
N36 H36A 0.8800 . ?
N36 H36B 0.8800 . ?
N37 Ni2 2.001(8) . ?
N38 Ni2 2.101(7) . ?
O1 Cl1 1.414(6) . ?
O2 Cl1 1.414(6) . ?
O3 Cl1 1.420(6) . ?
O4 Cl1 1.423(6) . ?
O11 Cl11 1.466(7) . ?
O12 Cl11 1.401(6) . ?
O13 Cl11 1.415(7) . ?
O14 Cl11 1.430(6) . ?
O21 Cl21 1.429(6) . ?
O22 Cl21 1.355(6) . ?
O23 Cl21 1.451(7) . ?
O24 Cl21 1.442(6) . ?
O31 Cl31 1.448(8) . ?
O32 Cl31 1.380(7) . ?
O33 Cl31 1.381(7) . ?
O34 Cl31 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 C1 C2 124.9(9) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C1 C2 C3 116.1(9) . . ?
C1 C2 H2 122.0 . . ?
C3 C2 H2 122.0 . . ?
C4 C3 C2 119.1(9) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.8(9) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 121.1(9) . . ?
N1 C5 C6 116.4(8) . . ?
C4 C5 C6 122.4(9) . . ?
N2 C6 C7 120.2(8) . . ?
N2 C6 C5 112.4(8) . . ?
C7 C6 C5 127.4(8) . . ?
C8 C7 C6 117.7(8) . . ?
C8 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C7 C8 C9 123.7(9) . . ?
C7 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 114.9(8) . . ?
C10 C9 H9 122.6 . . ?
C8 C9 H9 122.6 . . ?
N2 C10 C9 122.6(8) . . ?
N2 C10 C11 111.4(7) . . ?
C9 C10 C11 125.9(8) . . ?
N4 C11 N3 129.1(8) . . ?
N4 C11 C10 113.3(7) . . ?
N3 C11 C10 117.5(8) . . ?
N6 C12 N5 125.6(9) . . ?
N6 C12 C13 119.9(8) . . ?
N5 C12 C13 114.5(8) . . ?
C14 C13 N7 122.5(8) . . ?
C14 C13 C12 127.8(8) . . ?
N7 C13 C12 109.6(8) . . ?
C13 C14 C15 122.6(9) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C16 C15 C14 113.4(9) . . ?
C16 C15 H15 123.3 . . ?
C14 C15 H15 123.3 . . ?
C17 C16 C15 123.9(9) . . ?
C17 C16 H16 118.1 . . ?
C15 C16 H16 118.1 . . ?
N7 C17 C16 120.2(9) . . ?
N7 C17 C18 111.1(8) . . ?
C16 C17 C18 128.6(8) . . ?
N8 C18 C19 121.6(9) . . ?
N8 C18 C17 115.6(7) . . ?
C19 C18 C17 122.8(9) . . ?
C18 C19 C20 118.8(9) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
C21 C20 C19 121.1(10) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 115.6(10) . . ?
C20 C21 H21 122.2 . . ?
C22 C21 H21 122.2 . . ?
N8 C22 C21 123.7(10) . . ?
N8 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
N31 C31 C32 122.7(9) . . ?
N31 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C33 C32 C31 118.1(8) . . ?
C33 C32 H32 121.0 . . ?
C31 C32 H32 121.0 . . ?
C32 C33 C34 121.5(9) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C33 C34 C35 117.4(9) . . ?
C33 C34 H34 121.3 . . ?
C35 C34 H34 121.3 . . ?
N31 C35 C34 122.7(9) . . ?
N31 C35 C36 112.7(8) . . ?
C34 C35 C36 124.5(8) . . ?
N32 C36 C37 120.4(8) . . ?
N32 C36 C35 114.6(8) . . ?
C37 C36 C35 124.9(8) . . ?
C36 C37 C38 118.7(9) . . ?
C36 C37 H37 120.6 . . ?
C38 C37 H37 120.6 . . ?
C39 C38 C37 118.7(9) . . ?
C39 C38 H38 120.6 . . ?
C37 C38 H38 120.6 . . ?
C40 C39 C38 118.9(8) . . ?
C40 C39 H39 120.5 . . ?
C38 C39 H39 120.5 . . ?
N32 C40 C39 121.8(9) . . ?
N32 C40 C41 112.0(8) . . ?
C39 C40 C41 126.2(8) . . ?
N34 C41 N33 123.7(8) . . ?
N34 C41 C40 114.2(7) . . ?
N33 C41 C40 121.9(8) . . ?
N35 C42 N36 125.1(9) . . ?
N35 C42 C43 115.5(8) . . ?
N36 C42 C43 119.4(8) . . ?
N37 C43 C44 120.0(9) . . ?
N37 C43 C42 113.3(8) . . ?
C44 C43 C42 126.7(8) . . ?
C45 C44 C43 114.6(9) . . ?
C45 C44 H44 122.7 . . ?
C43 C44 H44 122.7 . . ?
C46 C45 C44 125.7(9) . . ?
C46 C45 H45 117.1 . . ?
C44 C45 H45 117.1 . . ?
C45 C46 C47 115.1(9) . . ?
C45 C46 H46 122.4 . . ?
C47 C46 H46 122.4 . . ?
N37 C47 C46 121.2(9) . . ?
N37 C47 C48 116.1(8) . . ?
C46 C47 C48 122.8(8) . . ?
N38 C48 C49 121.3(9) . . ?
N38 C48 C47 113.6(7) . . ?
C49 C48 C47 125.1(9) . . ?
C48 C49 C50 121.7(9) . . ?
C48 C49 H49 119.1 . . ?
C50 C49 H49 119.1 . . ?
C49 C50 C51 116.4(9) . . ?
C49 C50 H50 121.8 . . ?
C51 C50 H50 121.8 . . ?
C52 C51 C50 120.2(9) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 N38 121.7(10) . . ?
C51 C52 H52 119.2 . . ?
N38 C52 H52 119.2 . . ?
C5 N1 C1 118.8(9) . . ?
C5 N1 Ni1 113.0(6) . . ?
C1 N1 Ni1 128.1(7) . . ?
C10 N2 C6 120.9(8) . . ?
C10 N2 Ni1 119.6(6) . . ?
C6 N2 Ni1 116.9(6) . . ?
C11 N3 H3A 120.0 . . ?
C11 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C11 N4 N5 113.2(7) . . ?
C11 N4 Ni1 116.6(6) . . ?
N5 N4 Ni1 122.8(5) . . ?
C12 N5 N4 114.1(7) . . ?
C12 N5 Ni2 116.5(6) . . ?
N4 N5 Ni2 122.1(5) . . ?
C12 N6 H6A 120.0 . . ?
C12 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C17 N7 C13 117.3(8) . . ?
C17 N7 Ni2 120.8(6) . . ?
C13 N7 Ni2 120.7(6) . . ?
C22 N8 C18 119.1(8) . . ?
C22 N8 Ni2 127.7(7) . . ?
C18 N8 Ni2 113.2(6) . . ?
C31 N31 C35 117.1(8) . . ?
C31 N31 Ni1 127.4(6) . . ?
C35 N31 Ni1 115.3(6) . . ?
C36 N32 C40 121.3(8) . . ?
C36 N32 Ni1 116.4(6) . . ?
C40 N32 Ni1 119.0(6) . . ?
C41 N33 H33A 120.0 . . ?
C41 N33 H33B 120.0 . . ?
H33A N33 H33B 120.0 . . ?
C41 N34 N35 115.9(7) . . ?
C41 N34 Ni1 114.6(6) . . ?
N35 N34 Ni1 120.7(5) . . ?
C42 N35 N34 113.3(7) . . ?
C42 N35 Ni2 113.6(6) . . ?
N34 N35 Ni2 125.3(6) . . ?
C42 N36 H36A 120.0 . . ?
C42 N36 H36B 120.0 . . ?
H36A N36 H36B 120.0 . . ?
C47 N37 C43 123.1(8) . . ?
C47 N37 Ni2 117.6(6) . . ?
C43 N37 Ni2 118.4(6) . . ?
C48 N38 C52 118.7(8) . . ?
C48 N38 Ni2 113.9(5) . . ?
C52 N38 Ni2 127.4(6) . . ?
N2 Ni1 N32 166.4(2) . . ?
N2 Ni1 N31 93.9(3) . . ?
N32 Ni1 N31 77.1(3) . . ?
N2 Ni1 N1 77.8(3) . . ?
N32 Ni1 N1 92.0(3) . . ?
N31 Ni1 N1 90.7(2) . . ?
N2 Ni1 N4 75.9(3) . . ?
N32 Ni1 N4 115.1(3) . . ?
N31 Ni1 N4 98.4(3) . . ?
N1 Ni1 N4 152.6(3) . . ?
N2 Ni1 N34 114.4(3) . . ?
N32 Ni1 N34 75.4(3) . . ?
N31 Ni1 N34 151.6(3) . . ?
N1 Ni1 N34 97.3(3) . . ?
N4 Ni1 N34 86.8(2) . . ?
N7 Ni2 N37 169.3(2) . . ?
N7 Ni2 N38 94.2(3) . . ?
N37 Ni2 N38 77.9(3) . . ?
N7 Ni2 N5 76.6(3) . . ?
N37 Ni2 N5 111.5(3) . . ?
N38 Ni2 N5 98.4(3) . . ?
N7 Ni2 N8 78.0(3) . . ?
N37 Ni2 N8 94.4(3) . . ?
N38 Ni2 N8 89.0(2) . . ?
N5 Ni2 N8 154.0(3) . . ?
N7 Ni2 N35 111.3(3) . . ?
N37 Ni2 N35 77.1(3) . . ?
N38 Ni2 N35 154.4(3) . . ?
N5 Ni2 N35 85.8(2) . . ?
N8 Ni2 N35 98.3(3) . . ?
O2 Cl1 O1 109.1(4) . . ?
O2 Cl1 O3 108.3(4) . . ?
O1 Cl1 O3 108.1(5) . . ?
O2 Cl1 O4 111.6(5) . . ?
O1 Cl1 O4 110.4(5) . . ?
O3 Cl1 O4 109.4(5) . . ?
O12 Cl11 O13 111.7(5) . . ?
O12 Cl11 O14 111.5(5) . . ?
O13 Cl11 O14 109.4(5) . . ?
O12 Cl11 O11 107.9(5) . . ?
O13 Cl11 O11 110.4(5) . . ?
O14 Cl11 O11 105.7(4) . . ?
O22 Cl21 O21 113.7(5) . . ?
O22 Cl21 O24 112.4(4) . . ?
O21 Cl21 O24 106.3(5) . . ?
O22 Cl21 O23 111.9(5) . . ?
O21 Cl21 O23 107.5(5) . . ?
O24 Cl21 O23 104.6(5) . . ?
O32 Cl31 O33 115.1(6) . . ?
O32 Cl31 O34 111.3(6) . . ?
O33 Cl31 O34 111.3(6) . . ?
O32 Cl31 O31 106.0(6) . . ?
O33 Cl31 O31 105.2(6) . . ?
O34 Cl31 O31 107.3(7) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    1.012
_refine_diff_density_min   -0.819
_refine_diff_density_rms    0.127
