data_2005src1629hklf4

_exptl_special_details
;
 The crystal was twinned (180deg about -1 0 0 direct axis)
 at 41.4%
;

 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. I. R. Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C43 H35 Br2 Cl9 Fe2 N4 Ni'
_chemical_formula_weight          1257.03
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 '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'
 'Br'  'Br'  -0.2901   2.4595
 '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                    12.605(9)
_cell_length_b                    12.979(10)
_cell_length_c                    16.011(12)
_cell_angle_alpha                 89.829(3)
_cell_angle_beta                  86.600(4)
_cell_angle_gamma                 64.693(4)
_cell_volume                      2363.1(31)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     9819
_cell_measurement_theta_min       0.998
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.767
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1248
_exptl_absorpt_coefficient_mu     3.237
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4983
_exptl_absorpt_correction_T_max   0.6424
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             35380
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.1581
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          4.85
_diffrn_reflns_theta_max          27.14
_reflns_number_total              35386
_reflns_number_gt                 20134
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_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)+(0.0802P)²+47.4232P] 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_number_reflns          35386
_refine_ls_number_parameters      551
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2071
_refine_ls_R_factor_gt            0.1109
_refine_ls_wR_factor_ref          0.2874
_refine_ls_wR_factor_gt           0.2258
_refine_ls_goodness_of_fit_ref    1.097
_refine_ls_restrained_S_all       1.097
_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 0.44716(9) -0.00522(10) 0.25267(6) 0.0166(2) Uani 1 1 d . . .
Br1 Br 0.25180(8) 0.09182(8) 0.34655(5) 0.0261(2) Uani 1 1 d . . .
Br2 Br 0.39291(8) -0.14480(8) 0.16735(5) 0.0220(2) Uani 1 1 d . . .
C1 C 0.2645(8) 0.1600(7) 0.1457(5) 0.0232(19) Uani 1 1 d . . .
H1 H 0.2107 0.1552 0.1879 0.028 Uiso 1 1 calc R . .
C2 C 0.2191(8) 0.2244(8) 0.0773(5) 0.026(2) Uani 1 1 d . . .
H2 H 0.1368 0.2679 0.0744 0.032 Uiso 1 1 calc R . .
C3 C 0.2987(9) 0.2235(9) 0.0120(5) 0.031(2) Uani 1 1 d . . .
H3 H 0.2716 0.2631 -0.0381 0.037 Uiso 1 1 calc R . .
C4 C 0.4172(9) 0.1637(8) 0.0222(5) 0.025(2) Uani 1 1 d . . .
H4 H 0.4725 0.1634 -0.0209 0.031 Uiso 1 1 calc R . .
C5 C 0.4569(7) 0.1043(8) 0.0939(5) 0.022(2) Uani 1 1 d . . .
C6 C 0.5800(8) 0.0382(8) 0.1089(5) 0.0212(19) Uani 1 1 d . . .
C7 C 0.6675(8) 0.0603(8) 0.0652(5) 0.026(2) Uani 1 1 d . . .
H7 H 0.6484 0.1158 0.0230 0.032 Uiso 1 1 calc R . .
C8 C 0.7826(8) -0.0013(9) 0.0857(6) 0.031(2) Uani 1 1 d . . .
H8 H 0.8434 0.0147 0.0596 0.038 Uiso 1 1 calc R . .
C9 C 0.8088(8) -0.0845(8) 0.1429(5) 0.027(2) Uani 1 1 d . . .
H9 H 0.8881 -0.1274 0.1562 0.033 Uiso 1 1 calc R . .
C10 C 0.7189(7) -0.1074(8) 0.1827(5) 0.0214(19) Uani 1 1 d . . .
C11 C 0.7474(7) -0.2021(8) 0.2392(5) 0.023(2) Uani 1 1 d . . .
C12 C 0.7029(9) -0.2862(8) 0.2411(6) 0.029(2) Uani 1 1 d . . .
H12 H 0.6479 -0.2911 0.2051 0.034 Uiso 1 1 calc R . .
C13 C 0.7554(8) -0.3606(8) 0.3060(6) 0.034(2) Uani 1 1 d . . .
H13 H 0.7409 -0.4244 0.3214 0.041 Uiso 1 1 calc R . .
C14 C 0.8319(9) -0.3262(9) 0.3441(6) 0.035(2) Uani 1 1 d . . .
H14 H 0.8769 -0.3618 0.3902 0.043 Uiso 1 1 calc R . .
C15 C 0.8314(8) -0.2287(8) 0.3026(6) 0.030(2) Uani 1 1 d . . .
H15 H 0.8773 -0.1891 0.3143 0.037 Uiso 1 1 calc R . .
C16 C 0.9326(11) -0.4622(11) 0.1109(7) 0.053(3) Uani 1 1 d . . .
H16 H 0.8825 -0.4718 0.0726 0.063 Uiso 1 1 calc R . .
C17 C 0.9772(11) -0.5300(11) 0.1812(8) 0.058(3) Uani 1 1 d . . .
H17 H 0.9608 -0.5917 0.1992 0.069 Uiso 1 1 calc R . .
C18 C 1.0502(10) -0.4899(10) 0.2199(7) 0.050(3) Uani 1 1 d . . .
H18 H 1.0917 -0.5206 0.2683 0.061 Uiso 1 1 calc R . .
C19 C 1.0519(8) -0.3966(10) 0.1751(6) 0.039(3) Uani 1 1 d . . .
H19 H 1.0953 -0.3546 0.1874 0.047 Uiso 1 1 calc R . .
C20 C 0.9761(8) -0.3768(9) 0.1076(6) 0.036(2) Uani 1 1 d . . .
H20 H 0.9582 -0.3179 0.0680 0.044 Uiso 1 1 calc R . .
N1 N 0.3773(6) 0.1047(6) 0.1566(4) 0.0187(16) Uani 1 1 d . . .
N2 N 0.6053(6) -0.0428(6) 0.1680(4) 0.0175(15) Uani 1 1 d . . .
Fe1 Fe 0.88278(11) -0.36401(12) 0.22026(8) 0.0282(3) Uani 1 1 d . . .
C21 C 0.4609(8) -0.1930(7) 0.3667(5) 0.0204(19) Uani 1 1 d . . .
H21 H 0.4123 -0.2048 0.3284 0.025 Uiso 1 1 calc R . .
C22 C 0.4884(8) -0.2588(8) 0.4370(5) 0.023(2) Uani 1 1 d . . .
H22 H 0.4588 -0.3141 0.4470 0.028 Uiso 1 1 calc R . .
C23 C 0.5601(8) -0.2422(7) 0.4926(5) 0.025(2) Uani 1 1 d . . .
H23 H 0.5820 -0.2875 0.5408 0.030 Uiso 1 1 calc R . .
C24 C 0.5991(8) -0.1599(8) 0.4772(5) 0.023(2) Uani 1 1 d . . .
H24 H 0.6466 -0.1464 0.5157 0.028 Uiso 1 1 calc R . .
C25 C 0.5691(7) -0.0958(8) 0.4051(5) 0.0201(19) Uani 1 1 d . . .
C26 C 0.6046(7) -0.0053(7) 0.3846(5) 0.0169(18) Uani 1 1 d . . .
C27 C 0.6987(7) 0.0005(7) 0.4229(5) 0.0202(18) Uani 1 1 d . . .
H27 H 0.7374 -0.0516 0.4649 0.024 Uiso 1 1 calc R . .
C28 C 0.7341(8) 0.0832(8) 0.3984(6) 0.028(2) Uani 1 1 d . . .
H28 H 0.8003 0.0866 0.4215 0.034 Uiso 1 1 calc R . .
C29 C 0.6737(8) 0.1601(8) 0.3410(5) 0.026(2) Uani 1 1 d . . .
H29 H 0.6984 0.2166 0.3226 0.031 Uiso 1 1 calc R . .
C30 C 0.5746(7) 0.1555(7) 0.3090(5) 0.0203(19) Uani 1 1 d . . .
C31 C 0.5036(8) 0.2443(7) 0.2522(5) 0.0176(19) Uani 1 1 d . . .
C32 C 0.5511(8) 0.2913(8) 0.1880(5) 0.026(2) Uani 1 1 d . . .
H32 H 0.6319 0.2725 0.1753 0.031 Uiso 1 1 calc R . .
C33 C 0.4548(10) 0.3717(9) 0.1464(5) 0.033(2) Uani 1 1 d . . .
H33 H 0.4605 0.4141 0.0993 0.040 Uiso 1 1 calc R . .
C34 C 0.3507(8) 0.3781(7) 0.1859(5) 0.0232(19) Uani 1 1 d . . .
H34 H 0.2734 0.4278 0.1721 0.028 Uiso 1 1 calc R . .
C35 C 0.3806(8) 0.2975(8) 0.2501(5) 0.025(2) Uani 1 1 d . . .
H35 H 0.3266 0.2819 0.2859 0.030 Uiso 1 1 calc R . .
C36 C 0.5377(11) 0.4966(9) 0.3110(6) 0.040(3) Uani 1 1 d . . .
H36 H 0.6185 0.4742 0.2953 0.048 Uiso 1 1 calc R . .
C37 C 0.4459(12) 0.5740(9) 0.2687(7) 0.049(3) Uani 1 1 d . . .
H37 H 0.4510 0.6139 0.2199 0.059 Uiso 1 1 calc R . .
C38 C 0.3409(12) 0.5815(10) 0.3140(7) 0.055(3) Uani 1 1 d . . .
H38 H 0.2628 0.6300 0.3010 0.066 Uiso 1 1 calc R . .
C39 C 0.3722(11) 0.5058(10) 0.3805(7) 0.047(3) Uani 1 1 d . . .
H39 H 0.3197 0.4911 0.4184 0.057 Uiso 1 1 calc R . .
C40 C 0.4958(10) 0.4554(9) 0.3806(6) 0.039(3) Uani 1 1 d . . .
H40 H 0.5420 0.4033 0.4201 0.047 Uiso 1 1 calc R . .
N21 N 0.4989(6) -0.1143(6) 0.3502(4) 0.0176(15) Uani 1 1 d . . .
N22 N 0.5424(6) 0.0706(6) 0.3284(4) 0.0168(15) Uani 1 1 d . . .
Fe21 Fe 0.44301(12) 0.41772(11) 0.26986(7) 0.0242(3) Uani 1 1 d . . .
C41 C 0.2439(9) -0.3884(9) -0.0060(6) 0.039(3) Uani 1 1 d . . .
H41 H 0.1980 -0.4168 0.0332 0.047 Uiso 1 1 calc R . .
Cl41 Cl 0.3170(3) -0.3305(3) 0.05183(18) 0.0550(8) Uani 1 1 d . . .
Cl42 Cl 0.1465(3) -0.2851(3) -0.0697(2) 0.0665(9) Uani 1 1 d . . .
Cl43 Cl 0.3458(3) -0.5056(3) -0.07098(18) 0.0590(8) Uani 1 1 d . . .
C51 C 0.0883(9) -0.0154(9) 0.2177(6) 0.038(3) Uani 1 1 d . . .
H51 H 0.1646 -0.0110 0.2249 0.046 Uiso 1 1 calc R . .
Cl51 Cl 0.0824(3) -0.0516(4) 0.11248(18) 0.0755(12) Uani 1 1 d . . .
Cl52 Cl 0.0782(3) -0.1179(3) 0.2823(2) 0.0778(11) Uani 1 1 d . . .
Cl53 Cl -0.0289(3) 0.1183(3) 0.2434(2) 0.0673(9) Uani 1 1 d . . .
C61 C -0.0297(10) 0.2766(10) 0.4315(7) 0.044(3) Uani 1 1 d . . .
H61 H 0.0245 0.2223 0.3872 0.053 Uiso 1 1 calc R . .
Cl61 Cl -0.0301(4) 0.2009(4) 0.5224(2) 0.0931(13) Uani 1 1 d . . .
Cl62 Cl 0.0162(4) 0.3828(3) 0.4494(3) 0.0903(13) Uani 1 1 d . . .
Cl63 Cl -0.1726(3) 0.3380(3) 0.3970(2) 0.0645(9) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ni1 N21 2.047(7) . ?
Ni1 N1 2.062(7) . ?
Ni1 N2 2.214(6) . ?
Ni1 N22 2.253(6) . ?
Ni1 Br2 2.6078(14) . ?
Ni1 Br1 2.6135(15) . ?
C1 N1 1.312(11) . ?
C1 C2 1.373(12) . ?
C1 H1 0.9500 . ?
C2 C3 1.403(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(12) . ?
C4 H4 0.9500 . ?
C5 N1 1.376(10) . ?
C5 C6 1.451(12) . ?
C6 N2 1.359(10) . ?
C6 C7 1.402(11) . ?
C7 C8 1.383(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.357(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.406(11) . ?
C9 H9 0.9500 . ?
C10 N2 1.349(11) . ?
C10 C11 1.453(12) . ?
C11 C12 1.424(12) . ?
C11 C15 1.444(12) . ?
C11 Fe1 2.073(9) . ?
C12 C13 1.407(13) . ?
C12 Fe1 2.056(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(13) . ?
C13 Fe1 2.035(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.425(14) . ?
C14 Fe1 2.042(9) . ?
C14 H14 0.9500 . ?
C15 Fe1 2.045(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.416(16) . ?
C16 C20 1.432(14) . ?
C16 Fe1 2.070(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.406(16) . ?
C17 Fe1 2.043(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.413(16) . ?
C18 Fe1 2.043(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.435(13) . ?
C19 Fe1 2.073(9) . ?
C19 H19 0.9500 . ?
C20 Fe1 2.062(9) . ?
C20 H20 0.9500 . ?
C21 N21 1.320(10) . ?
C21 C22 1.379(11) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.370(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(11) . ?
C24 H24 0.9500 . ?
C25 N21 1.374(10) . ?
C25 C26 1.455(11) . ?
C26 N22 1.346(10) . ?
C26 C27 1.397(11) . ?
C27 C28 1.375(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.361(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.402(11) . ?
C29 H29 0.9500 . ?
C30 N22 1.355(10) . ?
C30 C31 1.472(12) . ?
C31 C35 1.404(13) . ?
C31 C32 1.422(11) . ?
C31 Fe21 2.059(8) . ?
C32 C33 1.419(14) . ?
C32 Fe21 2.039(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.391(13) . ?
C33 Fe21 2.046(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.413(12) . ?
C34 Fe21 2.031(8) . ?
C34 H34 0.9500 . ?
C35 Fe21 2.058(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.379(16) . ?
C36 C40 1.405(13) . ?
C36 Fe21 2.012(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.436(17) . ?
C37 Fe21 2.044(10) . ?
C37 H37 0.9500 . ?
C38 C39 1.402(16) . ?
C38 Fe21 2.058(11) . ?
C38 H38 0.9500 . ?
C39 C40 1.409(16) . ?
C39 Fe21 2.047(10) . ?
C39 H39 0.9500 . ?
C40 Fe21 2.060(9) . ?
C40 H40 0.9500 . ?
C41 Cl41 1.723(10) . ?
C41 Cl42 1.754(11) . ?
C41 Cl43 1.796(11) . ?
C41 H41 1.0000 . ?
C51 Cl52 1.726(11) . ?
C51 Cl53 1.762(11) . ?
C51 Cl51 1.764(10) . ?
C51 H51 1.0000 . ?
C61 Cl62 1.738(10) . ?
C61 Cl63 1.753(11) . ?
C61 Cl61 1.754(11) . ?
C61 H61 1.0000 . ?
 
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
N21 Ni1 N1 173.7(2) . . ?
N21 Ni1 N2 107.1(3) . . ?
N1 Ni1 N2 78.4(3) . . ?
N21 Ni1 N22 77.6(2) . . ?
N1 Ni1 N22 106.7(2) . . ?
N2 Ni1 N22 79.6(2) . . ?
N21 Ni1 Br2 92.42(17) . . ?
N1 Ni1 Br2 84.43(17) . . ?
N2 Ni1 Br2 91.26(15) . . ?
N22 Ni1 Br2 163.66(18) . . ?
N21 Ni1 Br1 83.24(19) . . ?
N1 Ni1 Br1 91.86(19) . . ?
N2 Ni1 Br1 165.66(19) . . ?
N22 Ni1 Br1 93.36(17) . . ?
Br2 Ni1 Br1 98.33(5) . . ?
N1 C1 C2 124.3(8) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C1 C2 C3 117.6(8) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 118.3(8) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C3 C4 C5 121.1(8) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
N1 C5 C4 119.7(8) . . ?
N1 C5 C6 115.9(7) . . ?
C4 C5 C6 124.4(8) . . ?
N2 C6 C7 122.2(8) . . ?
N2 C6 C5 117.2(7) . . ?
C7 C6 C5 120.6(8) . . ?
C8 C7 C6 117.9(8) . . ?
C8 C7 H7 121.1 . . ?
C6 C7 H7 121.1 . . ?
C9 C8 C7 120.1(8) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.2(9) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
N2 C10 C9 120.5(8) . . ?
N2 C10 C11 119.1(7) . . ?
C9 C10 C11 120.4(8) . . ?
C12 C11 C15 107.9(8) . . ?
C12 C11 C10 127.6(7) . . ?
C15 C11 C10 124.5(7) . . ?
C12 C11 Fe1 69.2(5) . . ?
C15 C11 Fe1 68.4(5) . . ?
C10 C11 Fe1 126.3(6) . . ?
C13 C12 C11 107.4(8) . . ?
C13 C12 Fe1 69.1(5) . . ?
C11 C12 Fe1 70.5(5) . . ?
C13 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
Fe1 C12 H12 125.7 . . ?
C14 C13 C12 109.5(8) . . ?
C14 C13 Fe1 70.3(5) . . ?
C12 C13 Fe1 70.7(5) . . ?
C14 C13 H13 125.3 . . ?
C12 C13 H13 125.3 . . ?
Fe1 C13 H13 125.3 . . ?
C13 C14 C15 108.7(9) . . ?
C13 C14 Fe1 69.7(5) . . ?
C15 C14 Fe1 69.7(5) . . ?
C13 C14 H14 125.7 . . ?
C15 C14 H14 125.7 . . ?
Fe1 C14 H14 126.5 . . ?
C14 C15 C11 106.5(8) . . ?
C14 C15 Fe1 69.5(6) . . ?
C11 C15 Fe1 70.5(5) . . ?
C14 C15 H15 126.8 . . ?
C11 C15 H15 126.8 . . ?
Fe1 C15 H15 124.8 . . ?
C17 C16 C20 108.0(10) . . ?
C17 C16 Fe1 68.8(6) . . ?
C20 C16 Fe1 69.4(6) . . ?
C17 C16 H16 126.0 . . ?
C20 C16 H16 126.0 . . ?
Fe1 C16 H16 127.3 . . ?
C16 C17 C18 108.1(11) . . ?
C16 C17 Fe1 70.9(7) . . ?
C18 C17 Fe1 69.9(7) . . ?
C16 C17 H17 125.9 . . ?
C18 C17 H17 125.9 . . ?
Fe1 C17 H17 124.9 . . ?
C19 C18 C17 109.1(11) . . ?
C19 C18 Fe1 71.1(6) . . ?
C17 C18 Fe1 69.9(7) . . ?
C19 C18 H18 125.4 . . ?
C17 C18 H18 125.4 . . ?
Fe1 C18 H18 125.2 . . ?
C18 C19 C20 107.4(9) . . ?
C18 C19 Fe1 68.8(6) . . ?
C20 C19 Fe1 69.3(5) . . ?
C18 C19 H19 126.3 . . ?
C20 C19 H19 126.3 . . ?
Fe1 C19 H19 127.2 . . ?
C16 C20 C19 107.3(10) . . ?
C16 C20 Fe1 70.0(5) . . ?
C19 C20 Fe1 70.1(5) . . ?
C16 C20 H20 126.3 . . ?
C19 C20 H20 126.3 . . ?
Fe1 C20 H20 125.1 . . ?
C1 N1 C5 118.9(7) . . ?
C1 N1 Ni1 124.8(5) . . ?
C5 N1 Ni1 115.6(6) . . ?
C10 N2 C6 118.9(7) . . ?
C10 N2 Ni1 128.2(5) . . ?
C6 N2 Ni1 109.6(6) . . ?
C13 Fe1 C17 107.0(4) . . ?
C13 Fe1 C18 121.0(4) . . ?
C17 Fe1 C18 40.2(5) . . ?
C13 Fe1 C14 40.0(4) . . ?
C17 Fe1 C14 119.7(5) . . ?
C18 Fe1 C14 104.4(4) . . ?
C13 Fe1 C15 68.3(4) . . ?
C17 Fe1 C15 154.8(5) . . ?
C18 Fe1 C15 119.4(4) . . ?
C14 Fe1 C15 40.8(4) . . ?
C13 Fe1 C12 40.2(4) . . ?
C17 Fe1 C12 124.5(4) . . ?
C18 Fe1 C12 158.3(4) . . ?
C14 Fe1 C12 67.8(4) . . ?
C15 Fe1 C12 68.9(4) . . ?
C13 Fe1 C20 161.1(4) . . ?
C17 Fe1 C20 68.3(5) . . ?
C18 Fe1 C20 68.0(4) . . ?
C14 Fe1 C20 158.5(4) . . ?
C15 Fe1 C20 123.9(4) . . ?
C12 Fe1 C20 126.3(4) . . ?
C13 Fe1 C19 156.4(4) . . ?
C17 Fe1 C19 67.8(5) . . ?
C18 Fe1 C19 40.2(4) . . ?
C14 Fe1 C19 120.9(4) . . ?
C15 Fe1 C19 106.0(4) . . ?
C12 Fe1 C19 161.2(4) . . ?
C20 Fe1 C19 40.6(4) . . ?
C13 Fe1 C16 124.2(4) . . ?
C17 Fe1 C16 40.3(5) . . ?
C18 Fe1 C16 67.5(5) . . ?
C14 Fe1 C16 156.9(4) . . ?
C15 Fe1 C16 162.1(5) . . ?
C12 Fe1 C16 111.3(4) . . ?
C20 Fe1 C16 40.5(4) . . ?
C19 Fe1 C16 67.7(4) . . ?
C13 Fe1 C11 67.5(4) . . ?
C17 Fe1 C11 162.0(4) . . ?
C18 Fe1 C11 157.5(4) . . ?
C14 Fe1 C11 67.9(4) . . ?
C15 Fe1 C11 41.0(3) . . ?
C12 Fe1 C11 40.4(3) . . ?
C20 Fe1 C11 111.0(4) . . ?
C19 Fe1 C11 124.2(4) . . ?
C16 Fe1 C11 127.5(5) . . ?
N21 C21 C22 123.2(7) . . ?
N21 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C21 C22 C23 118.4(7) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 119.3(8) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.1(7) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
N21 C25 C24 119.8(7) . . ?
N21 C25 C26 116.4(7) . . ?
C24 C25 C26 123.8(7) . . ?
N22 C26 C27 122.9(7) . . ?
N22 C26 C25 116.9(7) . . ?
C27 C26 C25 120.2(8) . . ?
C28 C27 C26 118.6(8) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
C29 C28 C27 119.5(7) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 119.5(8) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
N22 C30 C29 121.8(8) . . ?
N22 C30 C31 118.7(7) . . ?
C29 C30 C31 119.4(7) . . ?
C35 C31 C32 107.8(8) . . ?
C35 C31 C30 127.9(7) . . ?
C32 C31 C30 124.4(8) . . ?
C35 C31 Fe21 70.0(5) . . ?
C32 C31 Fe21 68.9(5) . . ?
C30 C31 Fe21 126.5(5) . . ?
C33 C32 C31 107.0(8) . . ?
C33 C32 Fe21 69.9(5) . . ?
C31 C32 Fe21 70.4(5) . . ?
C33 C32 H32 126.5 . . ?
C31 C32 H32 126.5 . . ?
Fe21 C32 H32 124.8 . . ?
C34 C33 C32 108.8(8) . . ?
C34 C33 Fe21 69.5(5) . . ?
C32 C33 Fe21 69.4(5) . . ?
C34 C33 H33 125.6 . . ?
C32 C33 H33 125.6 . . ?
Fe21 C33 H33 127.1 . . ?
C33 C34 C35 107.8(8) . . ?
C33 C34 Fe21 70.6(5) . . ?
C35 C34 Fe21 70.8(4) . . ?
C33 C34 H34 126.1 . . ?
C35 C34 H34 126.1 . . ?
Fe21 C34 H34 124.1 . . ?
C31 C35 C34 108.5(7) . . ?
C31 C35 Fe21 70.1(4) . . ?
C34 C35 Fe21 68.8(4) . . ?
C31 C35 H35 125.8 . . ?
C34 C35 H35 125.8 . . ?
Fe21 C35 H35 126.9 . . ?
C37 C36 C40 110.9(11) . . ?
C37 C36 Fe21 71.4(6) . . ?
C40 C36 Fe21 71.7(5) . . ?
C37 C36 H36 124.5 . . ?
C40 C36 H36 124.5 . . ?
Fe21 C36 H36 124.0 . . ?
C36 C37 C38 105.4(10) . . ?
C36 C37 Fe21 68.9(6) . . ?
C38 C37 Fe21 70.1(6) . . ?
C36 C37 H37 127.3 . . ?
C38 C37 H37 127.3 . . ?
Fe21 C37 H37 125.4 . . ?
C39 C38 C37 109.1(11) . . ?
C39 C38 Fe21 69.6(7) . . ?
C37 C38 Fe21 69.0(6) . . ?
C39 C38 H38 125.5 . . ?
C37 C38 H38 125.5 . . ?
Fe21 C38 H38 127.6 . . ?
C38 C39 C40 107.4(10) . . ?
C38 C39 Fe21 70.5(6) . . ?
C40 C39 Fe21 70.4(6) . . ?
C38 C39 H39 126.3 . . ?
C40 C39 H39 126.3 . . ?
Fe21 C39 H39 124.4 . . ?
C36 C40 C39 107.1(10) . . ?
C36 C40 Fe21 68.0(5) . . ?
C39 C40 Fe21 69.5(6) . . ?
C36 C40 H40 126.5 . . ?
C39 C40 H40 126.5 . . ?
Fe21 C40 H40 127.6 . . ?
C21 N21 C25 119.2(7) . . ?
C21 N21 Ni1 124.0(5) . . ?
C25 N21 Ni1 116.5(5) . . ?
C26 N22 C30 117.4(6) . . ?
C26 N22 Ni1 109.3(5) . . ?
C30 N22 Ni1 129.4(5) . . ?
C36 Fe21 C34 155.5(4) . . ?
C36 Fe21 C32 107.1(4) . . ?
C34 Fe21 C32 68.3(3) . . ?
C36 Fe21 C37 39.7(4) . . ?
C34 Fe21 C37 120.2(4) . . ?
C32 Fe21 C37 120.4(4) . . ?
C36 Fe21 C33 121.0(4) . . ?
C34 Fe21 C33 39.9(4) . . ?
C32 Fe21 C33 40.7(4) . . ?
C37 Fe21 C33 104.8(4) . . ?
C36 Fe21 C39 67.7(4) . . ?
C34 Fe21 C39 124.6(4) . . ?
C32 Fe21 C39 160.0(4) . . ?
C37 Fe21 C39 68.8(4) . . ?
C33 Fe21 C39 158.8(5) . . ?
C36 Fe21 C35 162.2(4) . . ?
C34 Fe21 C35 40.4(3) . . ?
C32 Fe21 C35 67.7(4) . . ?
C37 Fe21 C35 157.8(5) . . ?
C33 Fe21 C35 67.0(3) . . ?
C39 Fe21 C35 110.9(4) . . ?
C36 Fe21 C31 125.2(4) . . ?
C34 Fe21 C31 68.0(3) . . ?
C32 Fe21 C31 40.6(3) . . ?
C37 Fe21 C31 158.2(4) . . ?
C33 Fe21 C31 67.6(4) . . ?
C39 Fe21 C31 125.4(4) . . ?
C35 Fe21 C31 39.9(4) . . ?
C36 Fe21 C38 66.8(5) . . ?
C34 Fe21 C38 107.8(4) . . ?
C32 Fe21 C38 157.7(4) . . ?
C37 Fe21 C38 41.0(5) . . ?
C33 Fe21 C38 122.3(5) . . ?
C39 Fe21 C38 39.9(4) . . ?
C35 Fe21 C38 124.5(5) . . ?
C31 Fe21 C38 160.2(4) . . ?
C36 Fe21 C40 40.3(4) . . ?
C34 Fe21 C40 161.8(4) . . ?
C32 Fe21 C40 123.5(4) . . ?
C37 Fe21 C40 68.0(4) . . ?
C33 Fe21 C40 157.9(4) . . ?
C39 Fe21 C40 40.1(5) . . ?
C35 Fe21 C40 127.1(4) . . ?
C31 Fe21 C40 111.0(4) . . ?
C38 Fe21 C40 66.7(5) . . ?
Cl41 C41 Cl42 110.4(6) . . ?
Cl41 C41 Cl43 110.8(6) . . ?
Cl42 C41 Cl43 108.9(5) . . ?
Cl41 C41 H41 108.9 . . ?
Cl42 C41 H41 108.9 . . ?
Cl43 C41 H41 108.9 . . ?
Cl52 C51 Cl53 110.0(6) . . ?
Cl52 C51 Cl51 109.7(5) . . ?
Cl53 C51 Cl51 109.2(6) . . ?
Cl52 C51 H51 109.3 . . ?
Cl53 C51 H51 109.3 . . ?
Cl51 C51 H51 109.3 . . ?
Cl62 C61 Cl63 109.5(7) . . ?
Cl62 C61 Cl61 111.8(6) . . ?
Cl63 C61 Cl61 108.4(6) . . ?
Cl62 C61 H61 109.0 . . ?
Cl63 C61 H61 109.0 . . ?
Cl61 C61 H61 109.0 . . ?
 
_diffrn_measured_fraction_theta_max    0.892
_diffrn_reflns_theta_full              27.14
_diffrn_measured_fraction_theta_full   0.892
_refine_diff_density_max    1.550
_refine_diff_density_min   -1.543
_refine_diff_density_rms    0.248
