# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Stephen Foley'
_publ_contact_author_email       stephen.foley@usask.ca

_publ_section_title              
;
Bis-diimidazolylidine complexes of nickel:
Investigations into nickel catalyzed coupling reactions

;

loop_
_publ_author_address
;
Department of Chemistry, University of Saskatchewan
110 Science Place, Saskatoon, Saskatchewan, Canada S7N 5C9
;
;
Department of Chemistry, University of Saskatchewan
110 Science Place, Saskatoon, Saskatchewan, Canada S7N 5C9
;
;
Saskatchewan Structural Sciences Centre, University of Saskatchewan
110 Science Place, Saskatoon, Saskatchewan, Canada S7N 5C9
;
_publ_author_name                S.R.Foley

# Attachment '- compound_4a.cif'

data_1126
_database_code_depnum_ccdc_archive 'CCDC 697184'
#TrackingRef '- compound_4a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H40 Ag4 Br4 N8'
_chemical_formula_sum            'C42 H40 Ag4 Br4 N8'
_chemical_formula_weight         1407.94

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'
Ag Ag -0.8971 1.1015 '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'
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                   9.8623(4)
_cell_length_b                   9.9754(3)
_cell_length_c                   11.6153(4)
_cell_angle_alpha                92.339(2)
_cell_angle_beta                 96.566(2)
_cell_angle_gamma                109.941(2)
_cell_volume                     1063.25(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4545
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    5.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_process_details   'Shelxtl 6.10 (Bruker-AXS, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15555
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.52
_reflns_number_total             4868
_reflns_number_gt                3940
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0824P)^2^+15.1697P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0076(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4868
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0666
_refine_ls_wR_factor_ref         0.1880
_refine_ls_wR_factor_gt          0.1752
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
Ag1 Ag 0.57073(10) 0.21097(9) 0.99118(8) 0.0491(3) Uani 1 1 d . . .
Ag2 Ag 0.26203(10) -0.02558(9) 0.94102(9) 0.0523(3) Uani 1 1 d . . .
Br1 Br 0.84981(9) 0.32006(9) 1.10057(8) 0.0302(3) Uani 1 1 d . . .
Br2 Br 0.54834(9) -0.04160(9) 0.84785(7) 0.0264(2) Uani 1 1 d . . .
N1 N 0.5898(7) 0.4172(8) 0.7964(6) 0.0245(14) Uani 1 1 d . . .
N2 N 0.4000(7) 0.3946(7) 0.8787(6) 0.0224(14) Uani 1 1 d . . .
N3 N 0.1545(7) 0.2405(7) 0.8984(5) 0.0208(13) Uani 1 1 d . . .
N4 N -0.0086(7) 0.0428(7) 0.8308(6) 0.0209(13) Uani 1 1 d . . .
C1 C 0.7245(8) 0.3618(9) 0.6445(7) 0.0213(15) Uani 1 1 d . . .
C2 C 0.6441(9) 0.2223(9) 0.5996(8) 0.0260(17) Uani 1 1 d . . .
H2 H 0.5936 0.1541 0.6488 0.031 Uiso 1 1 calc R . .
C3 C 0.6378(9) 0.1830(9) 0.4825(8) 0.0298(18) Uani 1 1 d . . .
H3 H 0.5817 0.0879 0.4518 0.036 Uiso 1 1 calc R . .
C4 C 0.7122(10) 0.2806(9) 0.4098(7) 0.0267(17) Uani 1 1 d . . .
H4 H 0.7059 0.2535 0.3294 0.032 Uiso 1 1 calc R . .
C5 C 0.7959(11) 0.4184(10) 0.4559(8) 0.0311(19) Uani 1 1 d . . .
H5 H 0.8496 0.4859 0.4077 0.037 Uiso 1 1 calc R . .
C6 C 0.8010(10) 0.4575(9) 0.5734(8) 0.0289(18) Uani 1 1 d . . .
H6 H 0.8586 0.5520 0.6047 0.035 Uiso 1 1 calc R . .
C7 C 0.7295(9) 0.4084(11) 0.7715(8) 0.0308(19) Uani 1 1 d . . .
H7A H 0.7547 0.3394 0.8208 0.037 Uiso 1 1 calc R . .
H7B H 0.8069 0.5033 0.7916 0.037 Uiso 1 1 calc R . .
C8 C 0.5226(10) 0.5070(9) 0.7440(7) 0.0272(17) Uani 1 1 d . . .
H8 H 0.5545 0.5661 0.6833 0.033 Uiso 1 1 calc R . .
C9 C 0.4038(9) 0.4935(9) 0.7966(7) 0.0265(17) Uani 1 1 d . . .
H9 H 0.3364 0.5417 0.7808 0.032 Uiso 1 1 calc R . .
C10 C 0.5143(9) 0.3468(8) 0.8792(6) 0.0216(15) Uani 1 1 d . . .
C11 C 0.2906(9) 0.3473(9) 0.9552(7) 0.0270(17) Uani 1 1 d . . .
H11A H 0.2699 0.4311 0.9864 0.032 Uiso 1 1 calc R . .
H11B H 0.3297 0.3062 1.0218 0.032 Uiso 1 1 calc R . .
C12 C 0.0381(9) 0.2759(9) 0.8500(8) 0.0288(18) Uani 1 1 d . . .
H12 H 0.0326 0.3690 0.8477 0.035 Uiso 1 1 calc R . .
C13 C -0.0667(9) 0.1503(9) 0.8062(8) 0.0261(17) Uani 1 1 d . . .
H13 H -0.1606 0.1378 0.7668 0.031 Uiso 1 1 calc R . .
C14 C 0.1271(9) 0.0966(9) 0.8869(6) 0.0212(15) Uani 1 1 d . . .
C15 C -0.0933(9) -0.1096(8) 0.7983(7) 0.0225(15) Uani 1 1 d . . .
H15A H -0.1895 -0.1338 0.8258 0.027 Uiso 1 1 calc R . .
H15B H -0.0419 -0.1689 0.8366 0.027 Uiso 1 1 calc R . .
C16 C -0.1144(8) -0.1430(8) 0.6683(7) 0.0212(15) Uani 1 1 d . . .
C17 C -0.2508(9) -0.1692(9) 0.6038(8) 0.0288(18) Uani 1 1 d . . .
H17 H -0.3300 -0.1655 0.6418 0.035 Uiso 1 1 calc R . .
C18 C -0.2704(10) -0.2007(10) 0.4836(8) 0.033(2) Uani 1 1 d . . .
H18 H -0.3629 -0.2178 0.4396 0.039 Uiso 1 1 calc R . .
C19 C -0.1553(10) -0.2073(9) 0.4282(7) 0.0288(18) Uani 1 1 d . . .
H19 H -0.1684 -0.2280 0.3462 0.035 Uiso 1 1 calc R . .
C20 C -0.0210(9) -0.1835(9) 0.4929(7) 0.0253(16) Uani 1 1 d . . .
H20 H 0.0579 -0.1889 0.4553 0.030 Uiso 1 1 calc R . .
C21 C -0.0012(9) -0.1515(8) 0.6130(7) 0.0241(16) Uani 1 1 d . . .
H21 H 0.0911 -0.1355 0.6569 0.029 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0550(6) 0.0448(5) 0.0517(5) 0.0161(4) 0.0019(4) 0.0233(4)
Ag2 0.0485(5) 0.0352(4) 0.0645(6) 0.0019(4) -0.0238(4) 0.0139(4)
Br1 0.0286(4) 0.0238(4) 0.0356(5) -0.0014(3) 0.0050(3) 0.0060(3)
Br2 0.0283(4) 0.0267(4) 0.0198(4) -0.0024(3) 0.0045(3) 0.0040(3)
N1 0.021(3) 0.029(4) 0.020(3) -0.004(3) 0.003(3) 0.005(3)
N2 0.017(3) 0.022(3) 0.022(3) -0.007(3) 0.002(2) -0.001(3)
N3 0.020(3) 0.023(3) 0.016(3) -0.005(2) 0.003(2) 0.003(3)
N4 0.020(3) 0.018(3) 0.022(3) -0.002(2) 0.006(3) 0.002(2)
C1 0.016(3) 0.025(4) 0.020(4) 0.000(3) 0.005(3) 0.003(3)
C2 0.020(4) 0.022(4) 0.030(4) 0.002(3) 0.002(3) 0.001(3)
C3 0.026(4) 0.024(4) 0.034(5) -0.007(3) -0.001(3) 0.005(3)
C4 0.034(4) 0.032(4) 0.018(4) 0.001(3) 0.003(3) 0.017(4)
C5 0.039(5) 0.030(4) 0.028(4) 0.014(4) 0.014(4) 0.014(4)
C6 0.032(4) 0.019(4) 0.032(4) -0.003(3) 0.011(4) 0.003(3)
C7 0.022(4) 0.044(5) 0.025(4) -0.002(4) 0.008(3) 0.010(4)
C8 0.035(5) 0.026(4) 0.021(4) 0.000(3) 0.004(3) 0.010(4)
C9 0.029(4) 0.024(4) 0.028(4) -0.003(3) 0.004(3) 0.012(3)
C10 0.026(4) 0.020(4) 0.014(3) -0.005(3) -0.002(3) 0.004(3)
C11 0.023(4) 0.029(4) 0.021(4) -0.005(3) 0.004(3) 0.000(3)
C12 0.025(4) 0.021(4) 0.041(5) -0.005(3) 0.011(4) 0.009(3)
C13 0.020(4) 0.024(4) 0.033(4) -0.003(3) 0.003(3) 0.008(3)
C14 0.024(4) 0.026(4) 0.014(3) 0.001(3) 0.002(3) 0.009(3)
C15 0.024(4) 0.013(3) 0.027(4) 0.000(3) 0.004(3) 0.004(3)
C16 0.022(4) 0.015(3) 0.027(4) 0.000(3) 0.004(3) 0.006(3)
C17 0.022(4) 0.028(4) 0.033(5) -0.003(3) 0.004(3) 0.005(3)
C18 0.027(4) 0.031(4) 0.033(5) -0.010(4) -0.009(4) 0.005(4)
C19 0.036(5) 0.028(4) 0.019(4) -0.003(3) 0.002(3) 0.010(4)
C20 0.030(4) 0.021(4) 0.026(4) -0.001(3) 0.008(3) 0.009(3)
C21 0.024(4) 0.019(4) 0.027(4) -0.003(3) -0.001(3) 0.007(3)

_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
Ag1 C10 2.081(8) . ?
Ag1 Br2 2.6713(12) 2_657 ?
Ag1 Br1 2.7237(13) . ?
Ag1 Br2 2.8917(12) . ?
Ag1 Ag2 2.9433(12) 2_657 ?
Ag1 Ag2 3.1239(13) . ?
Ag2 C14 2.152(8) . ?
Ag2 Br1 2.7625(12) 2_657 ?
Ag2 Br2 2.8147(12) 2_657 ?
Ag2 Ag1 2.9433(12) 2_657 ?
Br1 Ag2 2.7625(12) 2_657 ?
Br2 Ag1 2.6713(12) 2_657 ?
Br2 Ag2 2.8147(12) 2_657 ?
N1 C10 1.355(11) . ?
N1 C8 1.404(11) . ?
N1 C7 1.470(10) . ?
N2 C10 1.365(10) . ?
N2 C9 1.394(11) . ?
N2 C11 1.444(10) . ?
N3 C14 1.365(10) . ?
N3 C12 1.379(11) . ?
N3 C11 1.462(10) . ?
N4 C14 1.336(10) . ?
N4 C13 1.402(11) . ?
N4 C15 1.472(9) . ?
C1 C6 1.370(12) . ?
C1 C2 1.390(11) . ?
C1 C7 1.519(11) . ?
C2 C3 1.388(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(12) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.351(12) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.357(12) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.509(11) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C21 1.375(11) . ?
C16 C17 1.397(12) . ?
C17 C18 1.396(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.395(11) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?

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
C10 Ag1 Br2 137.4(2) . 2_657 ?
C10 Ag1 Br1 113.9(2) . . ?
Br2 Ag1 Br1 98.59(4) 2_657 . ?
C10 Ag1 Br2 106.2(2) . . ?
Br2 Ag1 Br2 88.75(3) 2_657 . ?
Br1 Ag1 Br2 106.66(4) . . ?
C10 Ag1 Ag2 152.0(2) . 2_657 ?
Br2 Ag1 Ag2 69.00(3) 2_657 2_657 ?
Br1 Ag1 Ag2 58.20(3) . 2_657 ?
Br2 Ag1 Ag2 57.67(3) . 2_657 ?
C10 Ag1 Ag2 93.3(2) . . ?
Br2 Ag1 Ag2 57.48(3) 2_657 . ?
Br1 Ag1 Ag2 152.82(4) . . ?
Br2 Ag1 Ag2 63.87(3) . . ?
Ag2 Ag1 Ag2 98.09(3) 2_657 . ?
C14 Ag2 Br1 119.1(2) . 2_657 ?
C14 Ag2 Br2 122.8(2) . 2_657 ?
Br1 Ag2 Br2 107.75(4) 2_657 2_657 ?
C14 Ag2 Ag1 176.0(2) . 2_657 ?
Br1 Ag2 Ag1 56.92(3) 2_657 2_657 ?
Br2 Ag2 Ag1 60.24(3) 2_657 2_657 ?
C14 Ag2 Ag1 102.0(2) . . ?
Br1 Ag2 Ag1 136.65(4) 2_657 . ?
Br2 Ag2 Ag1 53.15(3) 2_657 . ?
Ag1 Ag2 Ag1 81.91(3) 2_657 . ?
Ag1 Br1 Ag2 64.88(3) . 2_657 ?
Ag1 Br2 Ag2 69.36(3) 2_657 2_657 ?
Ag1 Br2 Ag1 91.25(3) 2_657 . ?
Ag2 Br2 Ag1 62.08(3) 2_657 . ?
C10 N1 C8 111.0(7) . . ?
C10 N1 C7 124.1(7) . . ?
C8 N1 C7 124.7(7) . . ?
C10 N2 C9 111.7(7) . . ?
C10 N2 C11 123.1(7) . . ?
C9 N2 C11 125.2(7) . . ?
C14 N3 C12 112.4(7) . . ?
C14 N3 C11 124.8(7) . . ?
C12 N3 C11 122.8(7) . . ?
C14 N4 C13 111.9(7) . . ?
C14 N4 C15 126.3(7) . . ?
C13 N4 C15 121.8(7) . . ?
C6 C1 C2 119.5(7) . . ?
C6 C1 C7 119.9(7) . . ?
C2 C1 C7 120.6(7) . . ?
C3 C2 C1 119.7(8) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.9(8) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 119.1(8) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 119.7(8) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 121.1(8) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N1 C7 C1 112.0(7) . . ?
N1 C7 H7A 109.2 . . ?
C1 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C1 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 N1 106.9(7) . . ?
C9 C8 H8 126.5 . . ?
N1 C8 H8 126.5 . . ?
C8 C9 N2 106.1(7) . . ?
C8 C9 H9 126.9 . . ?
N2 C9 H9 126.9 . . ?
N1 C10 N2 104.3(7) . . ?
N1 C10 Ag1 127.5(6) . . ?
N2 C10 Ag1 128.0(6) . . ?
N2 C11 N3 113.4(6) . . ?
N2 C11 H11A 108.9 . . ?
N3 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
N3 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C13 C12 N3 105.8(7) . . ?
C13 C12 H12 127.1 . . ?
N3 C12 H12 127.1 . . ?
C12 C13 N4 106.3(7) . . ?
C12 C13 H13 126.9 . . ?
N4 C13 H13 126.9 . . ?
N4 C14 N3 103.7(7) . . ?
N4 C14 Ag2 125.6(6) . . ?
N3 C14 Ag2 130.7(6) . . ?
N4 C15 C16 111.0(6) . . ?
N4 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
N4 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C21 C16 C17 119.7(8) . . ?
C21 C16 C15 120.4(7) . . ?
C17 C16 C15 119.9(7) . . ?
C18 C17 C16 119.8(8) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 120.2(8) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 119.7(8) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.2(8) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C16 C21 C20 120.5(8) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 Ag1 Ag2 C14 -24.7(3) . . . . ?
Br2 Ag1 Ag2 C14 122.3(2) 2_657 . . . ?
Br1 Ag1 Ag2 C14 153.6(2) . . . . ?
Br2 Ag1 Ag2 C14 -131.2(2) . . . . ?
Ag2 Ag1 Ag2 C14 -179.1(2) 2_657 . . . ?
C10 Ag1 Ag2 Br1 136.8(2) . . . 2_657 ?
Br2 Ag1 Ag2 Br1 -76.19(6) 2_657 . . 2_657 ?
Br1 Ag1 Ag2 Br1 -44.82(14) . . . 2_657 ?
Br2 Ag1 Ag2 Br1 30.31(6) . . . 2_657 ?
Ag2 Ag1 Ag2 Br1 -17.51(6) 2_657 . . 2_657 ?
C10 Ag1 Ag2 Br2 -147.0(2) . . . 2_657 ?
Br1 Ag1 Ag2 Br2 31.37(10) . . . 2_657 ?
Br2 Ag1 Ag2 Br2 106.50(3) . . . 2_657 ?
Ag2 Ag1 Ag2 Br2 58.67(3) 2_657 . . 2_657 ?
C10 Ag1 Ag2 Ag1 154.3(2) . . . 2_657 ?
Br2 Ag1 Ag2 Ag1 -58.67(3) 2_657 . . 2_657 ?
Br1 Ag1 Ag2 Ag1 -27.30(9) . . . 2_657 ?
Br2 Ag1 Ag2 Ag1 47.83(3) . . . 2_657 ?
Ag2 Ag1 Ag2 Ag1 0.0 2_657 . . 2_657 ?
C10 Ag1 Br1 Ag2 -149.5(2) . . . 2_657 ?
Br2 Ag1 Br1 Ag2 58.66(4) 2_657 . . 2_657 ?
Br2 Ag1 Br1 Ag2 -32.62(4) . . . 2_657 ?
Ag2 Ag1 Br1 Ag2 32.30(11) . . . 2_657 ?
C10 Ag1 Br2 Ag1 -139.5(2) . . . 2_657 ?
Br2 Ag1 Br2 Ag1 0.0 2_657 . . 2_657 ?
Br1 Ag1 Br2 Ag1 98.59(4) . . . 2_657 ?
Ag2 Ag1 Br2 Ag1 65.77(3) 2_657 . . 2_657 ?
Ag2 Ag1 Br2 Ag1 -53.97(3) . . . 2_657 ?
C10 Ag1 Br2 Ag2 154.7(2) . . . 2_657 ?
Br2 Ag1 Br2 Ag2 -65.77(3) 2_657 . . 2_657 ?
Br1 Ag1 Br2 Ag2 32.83(4) . . . 2_657 ?
Ag2 Ag1 Br2 Ag2 -119.73(3) . . . 2_657 ?
C6 C1 C2 C3 -2.4(13) . . . . ?
C7 C1 C2 C3 178.3(8) . . . . ?
C1 C2 C3 C4 0.8(13) . . . . ?
C2 C3 C4 C5 1.2(13) . . . . ?
C3 C4 C5 C6 -1.6(13) . . . . ?
C2 C1 C6 C5 2.1(13) . . . . ?
C7 C1 C6 C5 -178.7(8) . . . . ?
C4 C5 C6 C1 0.0(14) . . . . ?
C10 N1 C7 C1 124.6(8) . . . . ?
C8 N1 C7 C1 -60.3(11) . . . . ?
C6 C1 C7 N1 110.2(9) . . . . ?
C2 C1 C7 N1 -70.6(11) . . . . ?
C10 N1 C8 C9 0.8(9) . . . . ?
C7 N1 C8 C9 -174.8(7) . . . . ?
N1 C8 C9 N2 -0.7(9) . . . . ?
C10 N2 C9 C8 0.4(9) . . . . ?
C11 N2 C9 C8 -179.9(7) . . . . ?
C8 N1 C10 N2 -0.5(8) . . . . ?
C7 N1 C10 N2 175.1(7) . . . . ?
C8 N1 C10 Ag1 -175.6(5) . . . . ?
C7 N1 C10 Ag1 0.0(11) . . . . ?
C9 N2 C10 N1 0.0(8) . . . . ?
C11 N2 C10 N1 -179.6(6) . . . . ?
C9 N2 C10 Ag1 175.1(5) . . . . ?
C11 N2 C10 Ag1 -4.5(10) . . . . ?
Br2 Ag1 C10 N1 -174.9(5) 2_657 . . . ?
Br1 Ag1 C10 N1 48.6(7) . . . . ?
Br2 Ag1 C10 N1 -68.5(7) . . . . ?
Ag2 Ag1 C10 N1 -18.2(10) 2_657 . . . ?
Ag2 Ag1 C10 N1 -132.2(6) . . . . ?
Br2 Ag1 C10 N2 11.0(8) 2_657 . . . ?
Br1 Ag1 C10 N2 -125.4(6) . . . . ?
Br2 Ag1 C10 N2 117.5(6) . . . . ?
Ag2 Ag1 C10 N2 167.8(4) 2_657 . . . ?
Ag2 Ag1 C10 N2 53.8(6) . . . . ?
C10 N2 C11 N3 -101.8(9) . . . . ?
C9 N2 C11 N3 78.6(10) . . . . ?
C14 N3 C11 N2 85.8(10) . . . . ?
C12 N3 C11 N2 -94.1(9) . . . . ?
C14 N3 C12 C13 0.1(10) . . . . ?
C11 N3 C12 C13 -180.0(7) . . . . ?
N3 C12 C13 N4 0.2(9) . . . . ?
C14 N4 C13 C12 -0.4(10) . . . . ?
C15 N4 C13 C12 178.7(7) . . . . ?
C13 N4 C14 N3 0.5(9) . . . . ?
C15 N4 C14 N3 -178.6(7) . . . . ?
C13 N4 C14 Ag2 -179.1(6) . . . . ?
C15 N4 C14 Ag2 1.8(11) . . . . ?
C12 N3 C14 N4 -0.3(9) . . . . ?
C11 N3 C14 N4 179.7(7) . . . . ?
C12 N3 C14 Ag2 179.3(6) . . . . ?
C11 N3 C14 Ag2 -0.7(11) . . . . ?
Br1 Ag2 C14 N4 -1.7(7) 2_657 . . . ?
Br2 Ag2 C14 N4 -142.5(6) 2_657 . . . ?
Ag1 Ag2 C14 N4 163.9(6) . . . . ?
Br1 Ag2 C14 N3 178.8(6) 2_657 . . . ?
Br2 Ag2 C14 N3 38.1(8) 2_657 . . . ?
Ag1 Ag2 C14 N3 -15.6(7) . . . . ?
C14 N4 C15 C16 -110.6(8) . . . . ?
C13 N4 C15 C16 70.5(9) . . . . ?
N4 C15 C16 C21 74.7(9) . . . . ?
N4 C15 C16 C17 -106.9(8) . . . . ?
C21 C16 C17 C18 -1.3(13) . . . . ?
C15 C16 C17 C18 -179.7(8) . . . . ?
C16 C17 C18 C19 0.5(14) . . . . ?
C17 C18 C19 C20 0.5(14) . . . . ?
C18 C19 C20 C21 -0.7(13) . . . . ?
C17 C16 C21 C20 1.1(12) . . . . ?
C15 C16 C21 C20 179.5(7) . . . . ?
C19 C20 C21 C16 -0.1(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.208
_refine_diff_density_min         -2.679
_refine_diff_density_rms         0.243

data_1139
_database_code_depnum_ccdc_archive 'CCDC 697185'
#TrackingRef 'web_deposit_cif_file_0_StephenFoley_1312509322.697185.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C21 H20 Cl2 N4 Pd), C3 H7 N O'
_chemical_formula_sum            'C45 H47 Cl4 N9 O Pd2'
_chemical_formula_weight         1084.52

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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   30.461(2)
_cell_length_b                   7.8144(8)
_cell_length_c                   22.228(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.533(4)
_cell_angle_gamma                90.00
_cell_volume                     4557.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9735
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       chip
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.9006
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_process_details   'Shelxtl 6.10 (Bruker-AXS, 2000'
_exptl_special_details           
;
A full sphere of data was collected on the crystal in space group P1.
The crystal was a very small chip (0.10 x 0.04 x 0.01 mm) and it is not
surprising that that Rint was greater than 0.10. With an irregular
small, thin crystal, large differences in equivalent reflections can
easily occur due to absorption effects and statistical factors in the
measurement of very weak reflections. The space group was confirmed to
be C2/c by XPREP in SHEXTL with an asymmetric unit containing one molecule
of 5a and 1/2 molecule of DMF.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            25932
_diffrn_reflns_av_R_equivalents  0.1257
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4021
_reflns_number_gt                2864
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0166P)^2^+31.6858P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.00066(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4021
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.0936
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Pd1 Pd 0.113498(14) 0.24435(6) 0.49435(2) 0.02142(14) Uani 1 1 d . . .
Cl1 Cl 0.04167(5) 0.42703(17) 0.45302(7) 0.0256(3) Uani 1 1 d . . .
Cl2 Cl 0.14762(5) 0.42277(17) 0.44171(7) 0.0260(3) Uani 1 1 d . . .
N1 N 0.06432(16) 0.0928(6) 0.5729(2) 0.0232(10) Uani 1 1 d . . .
N2 N 0.08243(16) -0.0915(6) 0.5171(2) 0.0230(10) Uani 1 1 d . . .
N3 N 0.15671(15) -0.0973(5) 0.5092(2) 0.0215(10) Uani 1 1 d . . .
N4 N 0.21873(16) 0.0811(6) 0.5542(2) 0.0241(10) Uani 1 1 d . . .
C1 C 0.0877(2) 0.2324(8) 0.6847(3) 0.0293(12) Uani 1 1 d . . .
C2 C 0.1350(2) 0.1568(8) 0.7229(3) 0.0376(15) Uani 1 1 d . . .
H2 H 0.1517 0.1140 0.6997 0.045 Uiso 1 1 calc R . .
C3 C 0.1585(3) 0.1428(8) 0.7952(3) 0.0443(17) Uani 1 1 d . . .
H3 H 0.1908 0.0888 0.8212 0.053 Uiso 1 1 calc R . .
C4 C 0.1345(3) 0.2080(9) 0.8288(3) 0.0478(18) Uani 1 1 d . . .
H4 H 0.1501 0.1973 0.8781 0.057 Uiso 1 1 calc R . .
C5 C 0.0879(3) 0.2886(11) 0.7911(4) 0.060(2) Uani 1 1 d . . .
H5 H 0.0721 0.3368 0.8147 0.072 Uiso 1 1 calc R . .
C6 C 0.0641(2) 0.2993(9) 0.7192(3) 0.0431(17) Uani 1 1 d . . .
H6 H 0.0317 0.3524 0.6934 0.052 Uiso 1 1 calc R . .
C7 C 0.0618(2) 0.2515(8) 0.6064(3) 0.0312(12) Uani 1 1 d . . .
H7A H 0.0256 0.2831 0.5875 0.037 Uiso 1 1 calc R . .
H7B H 0.0783 0.3451 0.5951 0.037 Uiso 1 1 calc R . .
C8 C 0.04713(19) -0.0644(7) 0.5815(3) 0.0276(13) Uani 1 1 d . . .
H8 H 0.0304 -0.0860 0.6069 0.033 Uiso 1 1 calc R . .
C9 C 0.05866(19) -0.1811(7) 0.5468(3) 0.0260(12) Uani 1 1 d . . .
H9 H 0.0519 -0.3005 0.5434 0.031 Uiso 1 1 calc R . .
C10 C 0.08520(19) 0.0790(7) 0.5324(3) 0.0218(11) Uani 1 1 d . . .
C11 C 0.10497(19) -0.1622(7) 0.4783(3) 0.0266(13) Uani 1 1 d . . .
H11A H 0.1053 -0.2887 0.4807 0.032 Uiso 1 1 calc R . .
H11B H 0.0847 -0.1276 0.4287 0.032 Uiso 1 1 calc R . .
C12 C 0.20043(19) -0.1928(7) 0.5323(3) 0.0248(12) Uani 1 1 d . . .
H12 H 0.2025 -0.3133 0.5288 0.030 Uiso 1 1 calc R . .
C13 C 0.2397(2) -0.0820(7) 0.5609(3) 0.0275(13) Uani 1 1 d . . .
H13 H 0.2748 -0.1093 0.5816 0.033 Uiso 1 1 calc R . .
C14 C 0.16762(19) 0.0724(7) 0.5222(3) 0.0212(11) Uani 1 1 d . . .
C15 C 0.25034(19) 0.2344(8) 0.5870(3) 0.0288(12) Uani 1 1 d . . .
H15A H 0.2293 0.3383 0.5667 0.035 Uiso 1 1 calc R . .
H15B H 0.2785 0.2377 0.5769 0.035 Uiso 1 1 calc R . .
C16 C 0.27219(19) 0.2338(8) 0.6649(3) 0.0284(12) Uani 1 1 d . . .
C17 C 0.3198(2) 0.1625(8) 0.7089(3) 0.0369(15) Uani 1 1 d . . .
H17 H 0.3386 0.1130 0.6899 0.044 Uiso 1 1 calc R . .
C18 C 0.3399(3) 0.1630(9) 0.7804(3) 0.0456(17) Uani 1 1 d . . .
H18 H 0.3726 0.1150 0.8102 0.055 Uiso 1 1 calc R . .
C19 C 0.3129(3) 0.2325(10) 0.8082(3) 0.0505(18) Uani 1 1 d . . .
H19 H 0.3269 0.2311 0.8574 0.061 Uiso 1 1 calc R . .
C20 C 0.2660(3) 0.3041(9) 0.7660(4) 0.053(2) Uani 1 1 d . . .
H20 H 0.2476 0.3533 0.7857 0.063 Uiso 1 1 calc R . .
C21 C 0.2454(2) 0.3043(8) 0.6940(4) 0.0422(17) Uani 1 1 d . . .
H21 H 0.2127 0.3530 0.6645 0.051 Uiso 1 1 calc R . .
N31 N 1.0030(12) 0.8111(13) 0.7404(15) 0.038(4) Uani 0.50 1 d P A -1
O31 O 0.9821(3) 1.0104(12) 0.6551(5) 0.046(2) Uani 0.50 1 d P A -1
C31 C 0.9694(5) 0.9029(19) 0.6842(7) 0.048(4) Uani 0.50 1 d P A -1
H31 H 0.9341 0.8837 0.6660 0.058 Uiso 0.50 1 calc PR A -1
C32 C 0.9783(7) 0.664(3) 0.7586(11) 0.091(7) Uani 0.50 1 d P A -1
H32A H 0.9936 0.6573 0.8094 0.137 Uiso 0.50 1 calc PR A -1
H32B H 0.9839 0.5559 0.7412 0.137 Uiso 0.50 1 calc PR A -1
H32C H 0.9416 0.6850 0.7368 0.137 Uiso 0.50 1 calc PR A -1
C33 C 1.0525(6) 0.814(3) 0.7642(11) 0.092(7) Uani 0.50 1 d P A -1
H33A H 1.0623 0.9286 0.7570 0.138 Uiso 0.50 1 calc PR A -1
H33B H 1.0608 0.7297 0.7390 0.138 Uiso 0.50 1 calc PR A -1
H33C H 1.0710 0.7871 0.8141 0.138 Uiso 0.50 1 calc PR A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0219(2) 0.0195(2) 0.0252(2) -0.0012(2) 0.01361(16) -0.0004(2)
Cl1 0.0224(7) 0.0187(7) 0.0389(8) 0.0031(6) 0.0179(6) 0.0042(5)
Cl2 0.0306(7) 0.0209(7) 0.0343(8) 0.0044(6) 0.0222(6) 0.0000(6)
N1 0.021(2) 0.027(3) 0.024(2) -0.003(2) 0.014(2) 0.000(2)
N2 0.023(2) 0.025(3) 0.025(2) -0.005(2) 0.015(2) -0.005(2)
N3 0.022(2) 0.019(2) 0.025(2) -0.003(2) 0.014(2) -0.0001(19)
N4 0.023(2) 0.023(2) 0.028(2) -0.004(2) 0.014(2) -0.004(2)
C1 0.033(3) 0.025(3) 0.033(3) -0.009(3) 0.019(2) -0.001(3)
C2 0.035(3) 0.042(4) 0.041(4) -0.008(3) 0.023(3) 0.003(3)
C3 0.045(4) 0.035(4) 0.037(4) -0.002(3) 0.009(3) 0.002(3)
C4 0.063(5) 0.051(5) 0.028(3) -0.007(3) 0.021(3) -0.013(4)
C5 0.056(4) 0.098(7) 0.040(4) -0.014(4) 0.034(4) -0.002(4)
C6 0.035(3) 0.058(5) 0.040(4) -0.005(3) 0.022(3) 0.004(3)
C7 0.033(3) 0.033(3) 0.029(3) -0.007(3) 0.017(2) -0.001(3)
C8 0.021(3) 0.035(3) 0.027(3) 0.001(3) 0.013(2) -0.004(3)
C9 0.022(3) 0.026(3) 0.026(3) 0.001(2) 0.009(2) -0.001(2)
C10 0.018(3) 0.023(3) 0.018(3) -0.003(2) 0.005(2) 0.002(2)
C11 0.025(3) 0.026(3) 0.030(3) -0.006(2) 0.015(3) -0.005(2)
C12 0.027(3) 0.023(3) 0.028(3) 0.001(2) 0.017(3) 0.003(2)
C13 0.023(3) 0.030(3) 0.031(3) 0.005(3) 0.015(3) 0.009(3)
C14 0.026(3) 0.022(3) 0.021(3) 0.000(2) 0.016(2) 0.000(2)
C15 0.028(3) 0.025(3) 0.036(3) -0.001(3) 0.017(2) -0.006(3)
C16 0.023(3) 0.029(3) 0.033(3) -0.006(3) 0.014(2) -0.008(3)
C17 0.032(3) 0.041(4) 0.034(4) -0.008(3) 0.015(3) 0.000(3)
C18 0.040(4) 0.050(4) 0.039(4) -0.007(3) 0.015(3) 0.003(3)
C19 0.062(4) 0.057(5) 0.032(3) -0.009(4) 0.024(3) -0.016(4)
C20 0.053(4) 0.055(5) 0.060(5) -0.026(4) 0.037(4) -0.013(4)
C21 0.036(3) 0.043(4) 0.051(4) -0.013(3) 0.025(3) -0.002(3)
N31 0.046(8) 0.037(5) 0.060(16) 0.008(6) 0.047(8) 0.011(7)
O31 0.047(5) 0.051(6) 0.045(6) 0.020(5) 0.028(5) 0.005(5)
C31 0.042(8) 0.052(9) 0.051(9) 0.001(8) 0.025(7) 0.012(7)
C32 0.087(14) 0.089(14) 0.109(17) 0.051(13) 0.058(13) 0.002(12)
C33 0.038(9) 0.122(18) 0.091(14) 0.045(13) 0.015(10) 0.013(10)

_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
Pd1 C10 1.966(5) . ?
Pd1 C14 1.967(5) . ?
Pd1 Cl1 2.3721(13) . ?
Pd1 Cl2 2.3726(13) . ?
N1 C10 1.346(6) . ?
N1 C8 1.386(7) . ?
N1 C7 1.468(7) . ?
N2 C10 1.367(7) . ?
N2 C9 1.392(7) . ?
N2 C11 1.456(6) . ?
N3 C14 1.362(7) . ?
N3 C12 1.378(6) . ?
N3 C11 1.454(6) . ?
N4 C14 1.345(6) . ?
N4 C13 1.400(7) . ?
N4 C15 1.476(7) . ?
C1 C2 1.381(8) . ?
C1 C6 1.392(8) . ?
C1 C7 1.509(7) . ?
C2 C3 1.392(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.350(8) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.345(8) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.507(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C21 1.388(8) . ?
C16 C17 1.389(8) . ?
C17 C18 1.381(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.367(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.391(9) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
N31 C33 1.32(3) . ?
N31 C31 1.35(3) . ?
N31 C32 1.537(19) . ?
O31 C31 1.236(16) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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
C10 Pd1 C14 84.0(2) . . ?
C10 Pd1 Cl1 92.43(15) . . ?
C14 Pd1 Cl1 173.54(16) . . ?
C10 Pd1 Cl2 174.61(16) . . ?
C14 Pd1 Cl2 92.86(15) . . ?
Cl1 Pd1 Cl2 90.25(5) . . ?
C10 N1 C8 111.2(5) . . ?
C10 N1 C7 124.9(5) . . ?
C8 N1 C7 123.9(4) . . ?
C10 N2 C9 110.7(4) . . ?
C10 N2 C11 121.9(4) . . ?
C9 N2 C11 127.3(5) . . ?
C14 N3 C12 111.3(4) . . ?
C14 N3 C11 121.9(4) . . ?
C12 N3 C11 126.7(4) . . ?
C14 N4 C13 110.7(4) . . ?
C14 N4 C15 126.3(5) . . ?
C13 N4 C15 122.6(4) . . ?
C2 C1 C6 119.4(5) . . ?
C2 C1 C7 121.5(5) . . ?
C6 C1 C7 119.0(5) . . ?
C1 C2 C3 120.5(6) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.5(6) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.3(6) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.1(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.1(6) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
N1 C7 C1 111.7(5) . . ?
N1 C7 H7A 109.3 . . ?
C1 C7 H7A 109.3 . . ?
N1 C7 H7B 109.3 . . ?
C1 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 N1 107.1(5) . . ?
C9 C8 H8 126.4 . . ?
N1 C8 H8 126.4 . . ?
C8 C9 N2 106.2(5) . . ?
C8 C9 H9 126.9 . . ?
N2 C9 H9 126.9 . . ?
N1 C10 N2 104.7(4) . . ?
N1 C10 Pd1 134.0(4) . . ?
N2 C10 Pd1 121.3(4) . . ?
N3 C11 N2 108.2(4) . . ?
N3 C11 H11A 110.1 . . ?
N2 C11 H11A 110.1 . . ?
N3 C11 H11B 110.1 . . ?
N2 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C13 C12 N3 106.6(5) . . ?
C13 C12 H12 126.7 . . ?
N3 C12 H12 126.7 . . ?
C12 C13 N4 106.8(5) . . ?
C12 C13 H13 126.6 . . ?
N4 C13 H13 126.6 . . ?
N4 C14 N3 104.7(4) . . ?
N4 C14 Pd1 133.8(4) . . ?
N3 C14 Pd1 121.6(4) . . ?
N4 C15 C16 111.2(4) . . ?
N4 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
N4 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C21 C16 C17 118.8(5) . . ?
C21 C16 C15 120.9(5) . . ?
C17 C16 C15 120.3(5) . . ?
C18 C17 C16 120.3(6) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 120.2(6) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.7(6) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C21 119.6(6) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C16 C21 C20 120.5(6) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C33 N31 C31 122.3(13) . . ?
C33 N31 C32 121(2) . . ?
C31 N31 C32 113(2) . . ?
O31 C31 N31 123.7(15) . . ?
O31 C31 H31 118.2 . . ?
N31 C31 H31 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.9(10) . . . . ?
C7 C1 C2 C3 179.1(6) . . . . ?
C1 C2 C3 C4 -1.2(10) . . . . ?
C2 C3 C4 C5 -0.9(11) . . . . ?
C3 C4 C5 C6 2.2(12) . . . . ?
C4 C5 C6 C1 -1.5(12) . . . . ?
C2 C1 C6 C5 -0.5(10) . . . . ?
C7 C1 C6 C5 -177.8(6) . . . . ?
C10 N1 C7 C1 -122.1(5) . . . . ?
C8 N1 C7 C1 55.2(6) . . . . ?
C2 C1 C7 N1 46.0(7) . . . . ?
C6 C1 C7 N1 -136.8(6) . . . . ?
C10 N1 C8 C9 1.5(6) . . . . ?
C7 N1 C8 C9 -176.1(5) . . . . ?
N1 C8 C9 N2 -0.5(6) . . . . ?
C10 N2 C9 C8 -0.7(6) . . . . ?
C11 N2 C9 C8 175.7(5) . . . . ?
C8 N1 C10 N2 -1.9(6) . . . . ?
C7 N1 C10 N2 175.7(4) . . . . ?
C8 N1 C10 Pd1 176.2(4) . . . . ?
C7 N1 C10 Pd1 -6.2(8) . . . . ?
C9 N2 C10 N1 1.6(6) . . . . ?
C11 N2 C10 N1 -175.0(4) . . . . ?
C9 N2 C10 Pd1 -176.8(3) . . . . ?
C11 N2 C10 Pd1 6.6(7) . . . . ?
C14 Pd1 C10 N1 136.8(5) . . . . ?
Cl1 Pd1 C10 N1 -48.6(5) . . . . ?
C14 Pd1 C10 N2 -45.3(4) . . . . ?
Cl1 Pd1 C10 N2 129.2(4) . . . . ?
C14 N3 C11 N2 -49.5(6) . . . . ?
C12 N3 C11 N2 126.7(5) . . . . ?
C10 N2 C11 N3 48.2(6) . . . . ?
C9 N2 C11 N3 -127.8(5) . . . . ?
C14 N3 C12 C13 0.4(6) . . . . ?
C11 N3 C12 C13 -176.1(5) . . . . ?
N3 C12 C13 N4 -0.3(6) . . . . ?
C14 N4 C13 C12 0.0(6) . . . . ?
C15 N4 C13 C12 172.6(5) . . . . ?
C13 N4 C14 N3 0.2(5) . . . . ?
C15 N4 C14 N3 -172.0(4) . . . . ?
C13 N4 C14 Pd1 -179.1(4) . . . . ?
C15 N4 C14 Pd1 8.7(8) . . . . ?
C12 N3 C14 N4 -0.4(6) . . . . ?
C11 N3 C14 N4 176.3(4) . . . . ?
C12 N3 C14 Pd1 179.0(3) . . . . ?
C11 N3 C14 Pd1 -4.2(7) . . . . ?
C10 Pd1 C14 N4 -136.5(5) . . . . ?
Cl2 Pd1 C14 N4 47.9(5) . . . . ?
C10 Pd1 C14 N3 44.3(4) . . . . ?
Cl2 Pd1 C14 N3 -131.3(4) . . . . ?
C14 N4 C15 C16 98.4(6) . . . . ?
C13 N4 C15 C16 -72.9(6) . . . . ?
N4 C15 C16 C21 -88.2(7) . . . . ?
N4 C15 C16 C17 91.8(6) . . . . ?
C21 C16 C17 C18 -0.4(9) . . . . ?
C15 C16 C17 C18 179.6(6) . . . . ?
C16 C17 C18 C19 0.6(10) . . . . ?
C17 C18 C19 C20 -0.8(11) . . . . ?
C18 C19 C20 C21 0.7(11) . . . . ?
C17 C16 C21 C20 0.4(9) . . . . ?
C15 C16 C21 C20 -179.6(6) . . . . ?
C19 C20 C21 C16 -0.5(10) . . . . ?
C33 N31 C31 O31 -8(3) . . . . ?
C32 N31 C31 O31 -169.5(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.103

# Attachment 'web_deposit_cif_file_1_StephenFoley_1312509322.697186.cif'

data_1165
_database_code_depnum_ccdc_archive 'CCDC 697186'
#TrackingRef 'web_deposit_cif_file_1_StephenFoley_1312509322.697186.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H100 Br2 N12 Ni O4'
_chemical_formula_sum            'C70 H100 Br2 N12 Ni O4'
_chemical_formula_weight         1392.15

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'
Br Br -0.2901 2.4595 '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'
Ni Ni 0.3393 1.1124 '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'

_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                   11.8395(3)
_cell_length_b                   13.6055(4)
_cell_length_c                   13.8460(3)
_cell_angle_alpha                80.971(2)
_cell_angle_beta                 69.9533(15)
_cell_angle_gamma                73.8540(16)
_cell_volume                     2007.88(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8569
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             734
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_process_details   'Shelxtl 6.10 (Bruker-AXS, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29325
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         27.53
_reflns_number_total             9199
_reflns_number_gt                6829
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON. (Spek, 2009)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

After two DMF molecules were found with molecule 3b in the asymmetric unit,
checkCIF found a solvent accessible void of 291 A**3. The volume is
consistent with two additional DMF solvent molecules. The program SQUEEZE,
part of the PLATON system (Spek, 2009)was used to model the disordered
solvent molecules in the structure.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.4068P] where P=(Fo^2^+2Fc^2^)/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         9199
_refine_ls_number_parameters     444
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1347
_refine_ls_wR_factor_gt          0.1241
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_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 0.0000 0.0000 1.0000 0.02075(11) Uani 1 2 d S . .
Br1 Br 0.66255(3) 1.00723(2) 0.69992(2) 0.03838(11) Uani 1 1 d . . .
N1 N 0.26924(19) -0.00022(17) 0.90069(17) 0.0252(5) Uani 1 1 d . . .
N2 N 0.20403(19) -0.00234(17) 1.06463(17) 0.0244(4) Uani 1 1 d . . .
N3 N 0.0106(2) 0.09008(17) 1.16777(16) 0.0253(5) Uani 1 1 d . . .
N4 N -0.1353(2) 0.18998(17) 1.11610(17) 0.0272(5) Uani 1 1 d . . .
C1 C 0.2467(2) 0.1287(2) 0.7566(2) 0.0290(6) Uani 1 1 d . . .
C2 C 0.1263(3) 0.1868(2) 0.7715(2) 0.0362(7) Uani 1 1 d . . .
H2 H 0.0589 0.1561 0.8065 0.043 Uiso 1 1 calc R . .
C3 C 0.1034(3) 0.2890(3) 0.7360(2) 0.0410(7) Uani 1 1 d . . .
H3 H 0.0198 0.3264 0.7466 0.049 Uiso 1 1 calc R . .
C4 C 0.1982(3) 0.33991(19) 0.6850(2) 0.0384(7) Uani 1 1 d D A .
C5 C 0.3181(3) 0.2787(2) 0.6727(3) 0.0416(7) Uani 1 1 d . . .
H5 H 0.3861 0.3089 0.6387 0.050 Uiso 1 1 calc R . .
C6 C 0.3426(3) 0.1766(2) 0.7075(2) 0.0375(7) Uani 1 1 d . . .
H6 H 0.4259 0.1390 0.6977 0.045 Uiso 1 1 calc R . .
C7 C 0.2743(3) 0.0164(2) 0.7917(2) 0.0306(6) Uani 1 1 d . . .
H7A H 0.2135 -0.0153 0.7819 0.037 Uiso 1 1 calc R . .
H7B H 0.3578 -0.0180 0.7484 0.037 Uiso 1 1 calc R . .
C8 C 0.3706(3) -0.0066(2) 0.9319(2) 0.0327(6) Uani 1 1 d . . .
H8 H 0.4531 -0.0088 0.8884 0.039 Uiso 1 1 calc R . .
C9 C 0.3297(2) -0.0090(2) 1.0357(2) 0.0311(6) Uani 1 1 d . . .
H9 H 0.3775 -0.0142 1.0800 0.037 Uiso 1 1 calc R . .
C10 C 0.1655(2) 0.00093(19) 0.98258(19) 0.0235(5) Uani 1 1 d . . .
C12 C -0.0406(3) 0.1703(2) 1.2319(2) 0.0329(6) Uani 1 1 d . . .
H12 H -0.0156 0.1795 1.2874 0.040 Uiso 1 1 calc R . .
C11 C 0.1174(2) 0.0058(2) 1.1694(2) 0.0270(5) Uani 1 1 d . . .
H11A H 0.0908 -0.0591 1.1943 0.032 Uiso 1 1 calc R . .
H11B H 0.1578 0.0188 1.2163 0.032 Uiso 1 1 calc R . .
C13 C -0.1325(3) 0.2324(2) 1.1999(2) 0.0347(6) Uani 1 1 d . . .
H13 H -0.1859 0.2940 1.2291 0.042 Uiso 1 1 calc R . .
C14 C -0.0473(2) 0.10079(19) 1.0963(2) 0.0240(5) Uani 1 1 d . . .
C15 C -0.2253(3) 0.2361(2) 1.0595(2) 0.0332(6) Uani 1 1 d . . .
H15A H -0.3063 0.2211 1.0998 0.040 Uiso 1 1 calc R . .
H15B H -0.1963 0.2045 0.9928 0.040 Uiso 1 1 calc R . .
C16 C -0.2415(3) 0.3503(2) 1.0400(2) 0.0311(6) Uani 1 1 d . . .
C17 C -0.3579(3) 0.4162(2) 1.0713(3) 0.0402(7) Uani 1 1 d . . .
H17 H -0.4277 0.3889 1.1082 0.048 Uiso 1 1 calc R . .
C18 C -0.3746(3) 0.5215(2) 1.0497(3) 0.0426(8) Uani 1 1 d . . .
H18 H -0.4559 0.5645 1.0711 0.051 Uiso 1 1 calc R . .
C19 C -0.2753(3) 0.5655(2) 0.9977(2) 0.0318(6) Uani 1 1 d . . .
C20 C -0.1583(3) 0.4981(2) 0.9678(2) 0.0375(7) Uani 1 1 d . . .
H20 H -0.0880 0.5253 0.9332 0.045 Uiso 1 1 calc R . .
C21 C -0.1416(3) 0.3933(2) 0.9870(2) 0.0367(7) Uani 1 1 d . . .
H21 H -0.0608 0.3499 0.9636 0.044 Uiso 1 1 calc R . .
C22 C 0.1729(3) 0.4496(2) 0.6457(2) 0.0454(8) Uani 1 1 d D . .
C23A C 0.0357(5) 0.4825(5) 0.6484(7) 0.072(3) Uani 0.481(8) 1 d PD A 1
H23A H -0.0178 0.4704 0.7187 0.107 Uiso 0.481(8) 1 calc PR A 1
H23B H 0.0234 0.4424 0.6016 0.107 Uiso 0.481(8) 1 calc PR A 1
H23C H 0.0147 0.5556 0.6267 0.107 Uiso 0.481(8) 1 calc PR A 1
C24A C 0.2492(8) 0.4620(5) 0.5366(4) 0.092(5) Uani 0.481(8) 1 d PDU A 1
H24A H 0.2177 0.5304 0.5074 0.138 Uiso 0.481(8) 1 calc PR A 1
H24B H 0.2450 0.4097 0.4975 0.138 Uiso 0.481(8) 1 calc PR A 1
H24C H 0.3354 0.4541 0.5328 0.138 Uiso 0.481(8) 1 calc PR A 1
C25A C 0.1889(8) 0.5150(4) 0.7127(6) 0.066(3) Uani 0.481(8) 1 d PD A 1
H25A H 0.2752 0.5200 0.6894 0.099 Uiso 0.481(8) 1 calc PR A 1
H25B H 0.1676 0.4849 0.7838 0.099 Uiso 0.481(8) 1 calc PR A 1
H25C H 0.1343 0.5835 0.7097 0.099 Uiso 0.481(8) 1 calc PR A 1
C23B C 0.0794(6) 0.5164(4) 0.7268(4) 0.069(3) Uani 0.519(8) 1 d PD A 2
H23D H 0.1061 0.5052 0.7881 0.103 Uiso 0.519(8) 1 calc PR A 2
H23E H -0.0008 0.4994 0.7449 0.103 Uiso 0.519(8) 1 calc PR A 2
H23F H 0.0715 0.5884 0.7009 0.103 Uiso 0.519(8) 1 calc PR A 2
C24B C 0.1354(8) 0.4632(4) 0.5520(4) 0.076(4) Uani 0.519(8) 1 d PD A 2
H24D H 0.1263 0.5350 0.5250 0.113 Uiso 0.519(8) 1 calc PR A 2
H24E H 0.0561 0.4446 0.5693 0.113 Uiso 0.519(8) 1 calc PR A 2
H24F H 0.1987 0.4190 0.4999 0.113 Uiso 0.519(8) 1 calc PR A 2
C25B C 0.2928(5) 0.4872(5) 0.6159(7) 0.083(4) Uani 0.519(8) 1 d PD A 2
H25D H 0.2797 0.5567 0.5825 0.124 Uiso 0.519(8) 1 calc PR A 2
H25E H 0.3603 0.4410 0.5681 0.124 Uiso 0.519(8) 1 calc PR A 2
H25F H 0.3144 0.4879 0.6780 0.124 Uiso 0.519(8) 1 calc PR A 2
C26 C -0.2908(3) 0.6808(2) 0.9712(3) 0.0409(7) Uani 1 1 d . . .
C27 C -0.2019(4) 0.7180(3) 1.0066(3) 0.0532(9) Uani 1 1 d . . .
H27A H -0.1165 0.6816 0.9722 0.080 Uiso 1 1 calc R . .
H27B H -0.2207 0.7045 1.0814 0.080 Uiso 1 1 calc R . .
H27C H -0.2114 0.7919 0.9890 0.080 Uiso 1 1 calc R . .
C28 C -0.2597(6) 0.7010(3) 0.8542(4) 0.0839(16) Uani 1 1 d . . .
H28A H -0.3106 0.6710 0.8301 0.126 Uiso 1 1 calc R . .
H28B H -0.1719 0.6699 0.8210 0.126 Uiso 1 1 calc R . .
H28C H -0.2767 0.7752 0.8366 0.126 Uiso 1 1 calc R . .
C29 C -0.4219(4) 0.7416(3) 1.0238(5) 0.0822(17) Uani 1 1 d . . .
H29A H -0.4425 0.7272 1.0986 0.123 Uiso 1 1 calc R . .
H29B H -0.4806 0.7215 0.9997 0.123 Uiso 1 1 calc R . .
H29C H -0.4271 0.8150 1.0068 0.123 Uiso 1 1 calc R . .
O1 O 1.1386(3) 0.7353(2) 0.5320(3) 0.0741(8) Uani 1 1 d . . .
N5 N 0.9775(3) 0.8421(2) 0.4846(2) 0.0516(7) Uani 1 1 d . . .
C30 C 1.0952(4) 0.8117(3) 0.4836(3) 0.0560(9) Uani 1 1 d . . .
H30 H 1.1500 0.8525 0.4422 0.067 Uiso 1 1 calc R . .
C31 C 0.8904(4) 0.7799(3) 0.5395(4) 0.0713(12) Uani 1 1 d . . .
H31A H 0.9319 0.7191 0.5737 0.107 Uiso 1 1 calc R . .
H31B H 0.8598 0.7585 0.4907 0.107 Uiso 1 1 calc R . .
H31C H 0.8206 0.8200 0.5912 0.107 Uiso 1 1 calc R . .
C32 C 0.9328(5) 0.9374(3) 0.4300(3) 0.0715(13) Uani 1 1 d . . .
H32A H 0.9989 0.9741 0.4009 0.107 Uiso 1 1 calc R . .
H32B H 0.8613 0.9803 0.4780 0.107 Uiso 1 1 calc R . .
H32C H 0.9082 0.9222 0.3743 0.107 Uiso 1 1 calc R . .
O2 O 0.1794(2) 0.76526(19) 0.1862(2) 0.0527(6) Uani 1 1 d . . .
N6 N 0.3178(3) 0.6561(2) 0.2570(2) 0.0484(7) Uani 1 1 d . . .
C33 C 0.2608(3) 0.7484(3) 0.2259(3) 0.0454(8) Uani 1 1 d . . .
H33 H 0.2858 0.8059 0.2354 0.054 Uiso 1 1 calc R . .
C34 C 0.2837(4) 0.5650(3) 0.2457(4) 0.0662(11) Uani 1 1 d . . .
H34A H 0.2201 0.5491 0.3090 0.099 Uiso 1 1 calc R . .
H34B H 0.3569 0.5072 0.2331 0.099 Uiso 1 1 calc R . .
H34C H 0.2512 0.5772 0.1875 0.099 Uiso 1 1 calc R . .
C35 C 0.4047(4) 0.6467(4) 0.3123(4) 0.0799(14) Uani 1 1 d . . .
H35A H 0.4224 0.7135 0.3094 0.120 Uiso 1 1 calc R . .
H35B H 0.4817 0.5968 0.2805 0.120 Uiso 1 1 calc R . .
H35C H 0.3688 0.6235 0.3843 0.120 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0202(2) 0.0180(2) 0.0258(2) -0.00279(17) -0.01006(18) -0.00310(17)
Br1 0.03385(17) 0.0477(2) 0.03517(17) -0.00668(13) -0.01487(13) -0.00510(13)
N1 0.0229(11) 0.0234(11) 0.0278(11) -0.0026(9) -0.0061(9) -0.0051(9)
N2 0.0218(10) 0.0236(11) 0.0287(11) 0.0018(9) -0.0115(9) -0.0045(8)
N3 0.0277(11) 0.0231(11) 0.0270(11) -0.0029(8) -0.0099(9) -0.0070(9)
N4 0.0296(12) 0.0197(11) 0.0318(12) -0.0047(9) -0.0109(10) -0.0023(9)
C1 0.0289(13) 0.0324(15) 0.0266(13) -0.0043(11) -0.0092(11) -0.0074(11)
C2 0.0299(14) 0.0403(17) 0.0380(15) 0.0010(13) -0.0099(13) -0.0109(12)
C3 0.0310(15) 0.0436(18) 0.0407(17) 0.0000(14) -0.0126(13) 0.0033(13)
C4 0.0451(17) 0.0345(16) 0.0300(14) -0.0004(12) -0.0124(13) -0.0012(13)
C5 0.0356(16) 0.0369(17) 0.0487(18) 0.0105(14) -0.0114(14) -0.0130(13)
C6 0.0269(14) 0.0356(16) 0.0455(17) 0.0057(13) -0.0091(13) -0.0082(12)
C7 0.0339(15) 0.0300(15) 0.0275(13) -0.0023(11) -0.0069(12) -0.0103(12)
C8 0.0224(13) 0.0335(15) 0.0429(16) -0.0035(12) -0.0096(12) -0.0085(11)
C9 0.0241(13) 0.0304(15) 0.0419(16) 0.0005(12) -0.0158(12) -0.0065(11)
C10 0.0275(13) 0.0166(12) 0.0276(12) -0.0001(9) -0.0106(10) -0.0056(10)
C12 0.0443(16) 0.0314(15) 0.0264(13) -0.0064(11) -0.0124(12) -0.0103(12)
C11 0.0282(13) 0.0289(14) 0.0248(12) -0.0002(10) -0.0114(11) -0.0054(11)
C13 0.0412(16) 0.0253(14) 0.0361(15) -0.0114(11) -0.0105(13) -0.0024(12)
C14 0.0241(12) 0.0193(12) 0.0290(13) -0.0013(10) -0.0090(10) -0.0052(10)
C15 0.0312(14) 0.0223(14) 0.0487(17) -0.0020(12) -0.0199(13) -0.0014(11)
C16 0.0307(14) 0.0208(13) 0.0427(16) -0.0035(11) -0.0164(12) -0.0005(11)
C17 0.0243(14) 0.0268(15) 0.063(2) -0.0014(14) -0.0082(14) -0.0047(11)
C18 0.0232(14) 0.0223(15) 0.073(2) -0.0030(14) -0.0105(14) 0.0027(11)
C19 0.0318(14) 0.0223(14) 0.0421(15) 0.0005(11) -0.0151(12) -0.0053(11)
C20 0.0292(15) 0.0317(16) 0.0481(17) 0.0010(13) -0.0108(13) -0.0055(12)
C21 0.0274(14) 0.0262(15) 0.0507(18) -0.0049(13) -0.0103(13) 0.0017(11)
C22 0.058(2) 0.0319(17) 0.0384(17) 0.0017(13) -0.0158(16) -0.0003(14)
C23A 0.092(7) 0.045(5) 0.086(7) 0.022(5) -0.054(6) -0.013(5)
C24A 0.137(11) 0.044(5) 0.041(5) 0.025(4) 0.011(6) -0.002(6)
C25A 0.096(8) 0.037(4) 0.072(6) -0.006(4) -0.036(6) -0.015(4)
C23B 0.092(7) 0.039(4) 0.061(5) -0.010(3) -0.001(5) -0.019(4)
C24B 0.149(11) 0.038(4) 0.062(6) 0.014(4) -0.071(7) -0.019(5)
C25B 0.069(6) 0.054(5) 0.129(10) 0.035(6) -0.052(6) -0.016(4)
C26 0.0414(17) 0.0243(15) 0.059(2) 0.0043(13) -0.0219(15) -0.0065(13)
C27 0.058(2) 0.0293(17) 0.083(3) -0.0015(17) -0.034(2) -0.0133(15)
C28 0.150(5) 0.040(2) 0.074(3) 0.020(2) -0.062(3) -0.021(3)
C29 0.043(2) 0.0222(17) 0.171(5) -0.001(2) -0.030(3) -0.0003(15)
O1 0.075(2) 0.0563(18) 0.086(2) -0.0003(16) -0.0300(17) -0.0059(15)
N5 0.0617(19) 0.0399(16) 0.0461(16) -0.0068(13) -0.0093(15) -0.0086(14)
C30 0.059(2) 0.047(2) 0.054(2) -0.0107(17) -0.0068(19) -0.0120(18)
C31 0.062(3) 0.056(3) 0.091(3) -0.015(2) -0.014(2) -0.016(2)
C32 0.096(3) 0.063(3) 0.053(2) -0.003(2) -0.035(2) -0.002(2)
O2 0.0535(15) 0.0423(14) 0.0678(16) 0.0010(12) -0.0328(13) -0.0054(11)
N6 0.0482(16) 0.0489(18) 0.0500(16) 0.0043(13) -0.0248(14) -0.0074(13)
C33 0.0493(19) 0.0391(18) 0.0495(19) -0.0068(14) -0.0165(16) -0.0102(15)
C34 0.072(3) 0.044(2) 0.079(3) 0.014(2) -0.030(2) -0.011(2)
C35 0.070(3) 0.108(4) 0.073(3) 0.001(3) -0.047(3) -0.011(3)

_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 C10 1.894(3) 2_557 ?
Ni1 C10 1.894(3) . ?
Ni1 C14 1.899(3) 2_557 ?
Ni1 C14 1.899(3) . ?
N1 C10 1.354(3) . ?
N1 C8 1.386(3) . ?
N1 C7 1.473(3) . ?
N2 C10 1.352(3) . ?
N2 C9 1.382(3) . ?
N2 C11 1.461(3) . ?
N3 C14 1.355(3) . ?
N3 C12 1.383(3) . ?
N3 C11 1.456(3) . ?
N4 C14 1.356(3) . ?
N4 C13 1.388(4) . ?
N4 C15 1.479(3) . ?
C1 C6 1.386(4) . ?
C1 C2 1.386(4) . ?
C1 C7 1.508(4) . ?
C2 C3 1.385(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.405(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(4) . ?
C4 C22 1.490(3) . ?
C5 C6 1.380(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.349(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C12 C13 1.340(4) . ?
C12 H12 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 H13 0.9500 . ?
C15 C16 1.505(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.384(4) . ?
C16 C21 1.391(4) . ?
C17 C18 1.388(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.397(4) . ?
C19 C26 1.527(4) . ?
C20 C21 1.379(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C25A 1.470(4) . ?
C22 C24B 1.478(4) . ?
C22 C24A 1.481(4) . ?
C22 C23B 1.491(4) . ?
C22 C25B 1.543(4) . ?
C22 C23A 1.549(4) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
C26 C29 1.524(5) . ?
C26 C27 1.528(5) . ?
C26 C28 1.531(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O1 C30 1.230(5) . ?
N5 C30 1.335(5) . ?
N5 C31 1.450(5) . ?
N5 C32 1.456(5) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O2 C33 1.220(4) . ?
N6 C33 1.333(4) . ?
N6 C35 1.448(5) . ?
N6 C34 1.451(5) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

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
C10 Ni1 C10 180.0 2_557 . ?
C10 Ni1 C14 86.25(11) 2_557 2_557 ?
C10 Ni1 C14 93.75(11) . 2_557 ?
C10 Ni1 C14 93.75(11) 2_557 . ?
C10 Ni1 C14 86.25(11) . . ?
C14 Ni1 C14 180.0 2_557 . ?
C10 N1 C8 111.3(2) . . ?
C10 N1 C7 125.6(2) . . ?
C8 N1 C7 122.7(2) . . ?
C10 N2 C9 112.1(2) . . ?
C10 N2 C11 121.7(2) . . ?
C9 N2 C11 126.2(2) . . ?
C14 N3 C12 111.5(2) . . ?
C14 N3 C11 121.9(2) . . ?
C12 N3 C11 126.5(2) . . ?
C14 N4 C13 110.6(2) . . ?
C14 N4 C15 125.7(2) . . ?
C13 N4 C15 123.6(2) . . ?
C6 C1 C2 118.0(3) . . ?
C6 C1 C7 120.3(3) . . ?
C2 C1 C7 121.7(3) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 122.9(3) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 114.4(2) . . ?
C5 C4 C22 122.9(3) . . ?
C3 C4 C22 122.6(2) . . ?
C6 C5 C4 123.4(3) . . ?
C6 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
N1 C7 C1 112.3(2) . . ?
N1 C7 H7A 109.1 . . ?
C1 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
C1 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 N1 106.8(2) . . ?
C9 C8 H8 126.6 . . ?
N1 C8 H8 126.6 . . ?
C8 C9 N2 105.9(2) . . ?
C8 C9 H9 127.0 . . ?
N2 C9 H9 127.0 . . ?
N2 C10 N1 103.9(2) . . ?
N2 C10 Ni1 121.17(19) . . ?
N1 C10 Ni1 134.91(19) . . ?
C13 C12 N3 106.2(2) . . ?
C13 C12 H12 126.9 . . ?
N3 C12 H12 126.9 . . ?
N3 C11 N2 108.2(2) . . ?
N3 C11 H11A 110.1 . . ?
N2 C11 H11A 110.1 . . ?
N3 C11 H11B 110.1 . . ?
N2 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C12 C13 N4 107.3(2) . . ?
C12 C13 H13 126.3 . . ?
N4 C13 H13 126.3 . . ?
N3 C14 N4 104.3(2) . . ?
N3 C14 Ni1 121.01(18) . . ?
N4 C14 Ni1 134.7(2) . . ?
N4 C15 C16 111.9(2) . . ?
N4 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
N4 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C21 117.7(3) . . ?
C17 C16 C15 120.8(3) . . ?
C21 C16 C15 121.5(3) . . ?
C16 C17 C18 121.2(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 121.7(3) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C20 116.4(3) . . ?
C18 C19 C26 123.0(3) . . ?
C20 C19 C26 120.6(3) . . ?
C21 C20 C19 122.1(3) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
C20 C21 C16 120.9(3) . . ?
C20 C21 H21 119.6 . . ?
C16 C21 H21 119.6 . . ?
C25A C22 C24B 137.5(4) . . ?
C25A C22 C24A 112.9(3) . . ?
C24B C22 C24A 51.5(4) . . ?
C25A C22 C4 110.9(3) . . ?
C24B C22 C4 111.6(3) . . ?
C24A C22 C4 110.8(3) . . ?
C25A C22 C23B 49.4(4) . . ?
C24B C22 C23B 111.2(3) . . ?
C24A C22 C23B 137.6(4) . . ?
C4 C22 C23B 111.6(3) . . ?
C25A C22 C25B 59.3(4) . . ?
C24B C22 C25B 107.2(3) . . ?
C24A C22 C25B 58.6(4) . . ?
C4 C22 C25B 108.9(3) . . ?
C23B C22 C25B 106.0(3) . . ?
C25A C22 C23A 107.8(3) . . ?
C24B C22 C23A 57.1(4) . . ?
C24A C22 C23A 106.9(3) . . ?
C4 C22 C23A 107.5(3) . . ?
C23B C22 C23A 60.3(4) . . ?
C25B C22 C23A 143.6(4) . . ?
C22 C23A H23A 109.5 . . ?
C22 C23A H23B 109.5 . . ?
C22 C23A H23C 109.5 . . ?
C22 C24A H24A 109.5 . . ?
C22 C24A H24B 109.5 . . ?
C22 C24A H24C 109.5 . . ?
C22 C25A H25A 109.5 . . ?
C22 C25A H25B 109.5 . . ?
C22 C25A H25C 109.5 . . ?
C22 C23B H23D 109.5 . . ?
C22 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22 C24B H24D 109.5 . . ?
C22 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C22 C25B H25D 109.5 . . ?
C22 C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C22 C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C29 C26 C19 112.1(3) . . ?
C29 C26 C27 107.8(3) . . ?
C19 C26 C27 109.6(3) . . ?
C29 C26 C28 109.6(4) . . ?
C19 C26 C28 108.6(3) . . ?
C27 C26 C28 109.1(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 N5 C31 120.7(3) . . ?
C30 N5 C32 121.3(4) . . ?
C31 N5 C32 118.0(4) . . ?
O1 C30 N5 125.3(4) . . ?
O1 C30 H30 117.3 . . ?
N5 C30 H30 117.3 . . ?
N5 C31 H31A 109.5 . . ?
N5 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N5 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N5 C32 H32A 109.5 . . ?
N5 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N5 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C33 N6 C35 120.2(4) . . ?
C33 N6 C34 120.4(3) . . ?
C35 N6 C34 119.2(3) . . ?
O2 C33 N6 125.4(3) . . ?
O2 C33 H33 117.3 . . ?
N6 C33 H33 117.3 . . ?
N6 C34 H34A 109.5 . . ?
N6 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N6 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N6 C35 H35A 109.5 . . ?
N6 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N6 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.6(4) . . . . ?
C7 C1 C2 C3 -178.1(3) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C2 C3 C4 C22 179.1(3) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C22 C4 C5 C6 -179.0(3) . . . . ?
C4 C5 C6 C1 0.7(5) . . . . ?
C2 C1 C6 C5 -1.5(5) . . . . ?
C7 C1 C6 C5 178.3(3) . . . . ?
C10 N1 C7 C1 84.4(3) . . . . ?
C8 N1 C7 C1 -87.4(3) . . . . ?
C6 C1 C7 N1 95.3(3) . . . . ?
C2 C1 C7 N1 -85.0(3) . . . . ?
C10 N1 C8 C9 -0.3(3) . . . . ?
C7 N1 C8 C9 172.5(2) . . . . ?
N1 C8 C9 N2 -0.9(3) . . . . ?
C10 N2 C9 C8 1.9(3) . . . . ?
C11 N2 C9 C8 -175.1(2) . . . . ?
C9 N2 C10 N1 -2.1(3) . . . . ?
C11 N2 C10 N1 175.1(2) . . . . ?
C9 N2 C10 Ni1 175.32(18) . . . . ?
C11 N2 C10 Ni1 -7.5(3) . . . . ?
C8 N1 C10 N2 1.4(3) . . . . ?
C7 N1 C10 N2 -171.1(2) . . . . ?
C8 N1 C10 Ni1 -175.4(2) . . . . ?
C7 N1 C10 Ni1 12.0(4) . . . . ?
C14 Ni1 C10 N2 -133.8(2) 2_557 . . . ?
C14 Ni1 C10 N2 46.2(2) . . . . ?
C14 Ni1 C10 N1 42.6(3) 2_557 . . . ?
C14 Ni1 C10 N1 -137.4(3) . . . . ?
C14 N3 C12 C13 0.1(3) . . . . ?
C11 N3 C12 C13 176.9(3) . . . . ?
C14 N3 C11 N2 47.4(3) . . . . ?
C12 N3 C11 N2 -129.1(3) . . . . ?
C10 N2 C11 N3 -46.0(3) . . . . ?
C9 N2 C11 N3 130.8(3) . . . . ?
N3 C12 C13 N4 -0.7(3) . . . . ?
C14 N4 C13 C12 1.1(3) . . . . ?
C15 N4 C13 C12 179.6(3) . . . . ?
C12 N3 C14 N4 0.6(3) . . . . ?
C11 N3 C14 N4 -176.4(2) . . . . ?
C12 N3 C14 Ni1 -178.17(19) . . . . ?
C11 N3 C14 Ni1 4.9(3) . . . . ?
C13 N4 C14 N3 -1.0(3) . . . . ?
C15 N4 C14 N3 -179.4(2) . . . . ?
C13 N4 C14 Ni1 177.5(2) . . . . ?
C15 N4 C14 Ni1 -1.0(4) . . . . ?
C10 Ni1 C14 N3 135.1(2) 2_557 . . . ?
C10 Ni1 C14 N4 -43.2(3) 2_557 . . . ?
C14 N4 C15 C16 -138.3(3) . . . . ?
C13 N4 C15 C16 43.5(4) . . . . ?
N4 C15 C16 C17 -125.1(3) . . . . ?
N4 C15 C16 C21 57.3(4) . . . . ?
C21 C16 C17 C18 0.6(5) . . . . ?
C15 C16 C17 C18 -177.2(3) . . . . ?
C16 C17 C18 C19 -1.2(6) . . . . ?
C17 C18 C19 C20 0.4(5) . . . . ?
C17 C18 C19 C26 178.9(3) . . . . ?
C18 C19 C20 C21 1.2(5) . . . . ?
C26 C19 C20 C21 -177.4(3) . . . . ?
C19 C20 C21 C16 -1.9(5) . . . . ?
C17 C16 C21 C20 0.9(5) . . . . ?
C15 C16 C21 C20 178.7(3) . . . . ?
C5 C4 C22 C25A -76.7(5) . . . . ?
C3 C4 C22 C25A 104.4(5) . . . . ?
C5 C4 C22 C24B 104.9(5) . . . . ?
C3 C4 C22 C24B -74.0(5) . . . . ?
C5 C4 C22 C24A 49.4(5) . . . . ?
C3 C4 C22 C24A -129.6(5) . . . . ?
C5 C4 C22 C23B -130.0(4) . . . . ?
C3 C4 C22 C23B 51.1(5) . . . . ?
C5 C4 C22 C25B -13.3(5) . . . . ?
C3 C4 C22 C25B 167.8(4) . . . . ?
C5 C4 C22 C23A 165.8(4) . . . . ?
C3 C4 C22 C23A -13.2(5) . . . . ?
C18 C19 C26 C29 9.7(5) . . . . ?
C20 C19 C26 C29 -171.8(4) . . . . ?
C18 C19 C26 C27 129.4(4) . . . . ?
C20 C19 C26 C27 -52.1(4) . . . . ?
C18 C19 C26 C28 -111.5(4) . . . . ?
C20 C19 C26 C28 67.0(4) . . . . ?
C31 N5 C30 O1 -4.7(6) . . . . ?
C32 N5 C30 O1 175.9(4) . . . . ?
C35 N6 C33 O2 -173.9(4) . . . . ?
C34 N6 C33 O2 -0.6(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.076

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 1.000 0.500 291.6 11.4
_platon_squeeze_details          
;
;


#===========================================================================

data_350
_database_code_depnum_ccdc_archive 'CCDC 697187'
#TrackingRef '- compound_3a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H40 N8 Ni, 2(Br)'
_chemical_formula_sum            'C42 H40 Br2 N8 Ni'
_chemical_formula_weight         875.35

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'
Br Br -0.2901 2.4595 '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'
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                   9.8058(3)
_cell_length_b                   10.6250(4)
_cell_length_c                   11.2120(5)
_cell_angle_alpha                63.075(2)
_cell_angle_beta                 67.743(2)
_cell_angle_gamma                71.563(2)
_cell_volume                     948.97(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    21061
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      29.575

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             446
_exptl_absorpt_coefficient_mu    2.659
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_process_details   'Shelxtl 6.10 (Bruker-AXS, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21018
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         29.64
_reflns_number_total             5312
_reflns_number_gt                4018
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Collect (Nonius BV, 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0464P)^2^+0.5913P] where P=(Fo^2^+2Fc^2^)/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         5312
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_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 0.5000 0.5000 0.0000 0.01794(11) Uani 1 2 d S . .
Br1 Br 0.09347(3) 0.59272(3) 0.60786(3) 0.03603(10) Uani 1 1 d . . .
N1 N 0.7605(2) 0.2751(2) 0.0862(2) 0.0222(4) Uani 1 1 d . . .
N2 N 0.7883(2) 0.3761(2) -0.1336(2) 0.0214(4) Uani 1 1 d . . .
N3 N 0.6041(2) 0.4447(2) -0.2486(2) 0.0196(4) Uani 1 1 d . . .
N4 N 0.3752(2) 0.4173(2) -0.1563(2) 0.0202(4) Uani 1 1 d . . .
C1 C 0.6896(3) 0.3760(3) -0.0098(3) 0.0201(5) Uani 1 1 d . . .
C2 C 0.9006(3) 0.2153(3) 0.0220(3) 0.0283(6) Uani 1 1 d . . .
H2 H 0.9708 0.1426 0.0674 0.034 Uiso 1 1 calc R . .
C3 C 0.9190(3) 0.2789(3) -0.1162(3) 0.0265(5) Uani 1 1 d . . .
H3 H 1.0042 0.2609 -0.1873 0.032 Uiso 1 1 calc R . .
C4 C 0.7506(3) 0.4665(3) -0.2645(2) 0.0235(5) Uani 1 1 d . . .
H4A H 0.8266 0.4399 -0.3414 0.028 Uiso 1 1 calc R . .
H4B H 0.7476 0.5684 -0.2862 0.028 Uiso 1 1 calc R . .
C5 C 0.5663(3) 0.4165(3) -0.3407(3) 0.0226(5) Uani 1 1 d . . .
H5 H 0.6293 0.4101 -0.4270 0.027 Uiso 1 1 calc R . .
C6 C 0.4219(3) 0.3999(3) -0.2820(3) 0.0244(5) Uani 1 1 d . . .
H6 H 0.3629 0.3800 -0.3197 0.029 Uiso 1 1 calc R . .
C7 C 0.4862(3) 0.4477(3) -0.1353(2) 0.0189(5) Uani 1 1 d . . .
C8 C 0.6991(3) 0.2305(3) 0.2387(3) 0.0270(5) Uani 1 1 d . . .
H8A H 0.5995 0.2899 0.2607 0.032 Uiso 1 1 calc R . .
H8B H 0.7657 0.2470 0.2762 0.032 Uiso 1 1 calc R . .
C9 C 0.6842(3) 0.0743(3) 0.3081(2) 0.0225(5) Uani 1 1 d . . .
C10 C 0.5607(3) 0.0326(3) 0.3128(3) 0.0277(6) Uani 1 1 d . . .
H10 H 0.4865 0.1021 0.2707 0.033 Uiso 1 1 calc R . .
C11 C 0.5463(4) -0.1108(3) 0.3791(3) 0.0364(7) Uani 1 1 d . . .
H11 H 0.4610 -0.1394 0.3844 0.044 Uiso 1 1 calc R . .
C12 C 0.6568(4) -0.2125(3) 0.4378(3) 0.0392(7) Uani 1 1 d . . .
H12 H 0.6474 -0.3108 0.4821 0.047 Uiso 1 1 calc R . .
C13 C 0.7792(4) -0.1721(3) 0.4324(3) 0.0390(7) Uani 1 1 d . . .
H13 H 0.8544 -0.2421 0.4727 0.047 Uiso 1 1 calc R . .
C14 C 0.7929(3) -0.0288(3) 0.3681(3) 0.0316(6) Uani 1 1 d . . .
H14 H 0.8775 -0.0008 0.3650 0.038 Uiso 1 1 calc R . .
C15 C 0.2296(3) 0.3875(3) -0.0557(3) 0.0233(5) Uani 1 1 d . . .
H15A H 0.1557 0.4128 -0.1069 0.028 Uiso 1 1 calc R . .
H15B H 0.1952 0.4489 -0.0011 0.028 Uiso 1 1 calc R . .
C16 C 0.2352(3) 0.2322(3) 0.0431(3) 0.0231(5) Uani 1 1 d . . .
C17 C 0.2924(3) 0.1206(3) -0.0046(3) 0.0356(7) Uani 1 1 d . . .
H17 H 0.3347 0.1413 -0.1016 0.043 Uiso 1 1 calc R . .
C18 C 0.2882(4) -0.0201(4) 0.0876(4) 0.0471(8) Uani 1 1 d . . .
H18 H 0.3284 -0.0953 0.0535 0.057 Uiso 1 1 calc R . .
C19 C 0.2264(4) -0.0520(4) 0.2282(4) 0.0488(9) Uani 1 1 d . . .
H19 H 0.2221 -0.1486 0.2912 0.059 Uiso 1 1 calc R . .
C20 C 0.1706(4) 0.0578(4) 0.2770(3) 0.0459(8) Uani 1 1 d . . .
H20 H 0.1286 0.0362 0.3742 0.055 Uiso 1 1 calc R . .
C21 C 0.1753(3) 0.1993(4) 0.1857(3) 0.0345(6) Uani 1 1 d . . .
H21 H 0.1375 0.2739 0.2205 0.041 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0179(2) 0.0216(2) 0.0162(2) -0.00808(18) -0.00469(16) -0.00461(16)
Br1 0.02236(14) 0.0488(2) 0.03107(16) -0.01539(14) -0.00571(11) -0.00059(12)
N1 0.0232(10) 0.0229(11) 0.0205(10) -0.0057(9) -0.0077(9) -0.0059(8)
N2 0.0178(9) 0.0272(11) 0.0186(10) -0.0078(9) -0.0048(8) -0.0051(8)
N3 0.0204(9) 0.0233(11) 0.0151(9) -0.0070(8) -0.0042(8) -0.0052(8)
N4 0.0193(9) 0.0224(11) 0.0210(10) -0.0092(9) -0.0062(8) -0.0042(8)
C1 0.0224(11) 0.0213(12) 0.0190(11) -0.0069(10) -0.0062(9) -0.0076(9)
C2 0.0228(12) 0.0303(14) 0.0303(14) -0.0077(12) -0.0111(11) -0.0040(10)
C3 0.0162(11) 0.0328(15) 0.0281(14) -0.0108(12) -0.0041(10) -0.0049(10)
C4 0.0203(11) 0.0328(14) 0.0155(11) -0.0065(10) -0.0030(9) -0.0090(10)
C5 0.0268(12) 0.0255(13) 0.0187(12) -0.0104(10) -0.0078(10) -0.0038(10)
C6 0.0281(12) 0.0285(14) 0.0239(13) -0.0118(11) -0.0118(11) -0.0055(10)
C7 0.0187(11) 0.0200(12) 0.0172(11) -0.0059(9) -0.0043(9) -0.0051(9)
C8 0.0371(14) 0.0251(14) 0.0206(12) -0.0054(11) -0.0120(11) -0.0080(11)
C9 0.0241(12) 0.0258(13) 0.0150(11) -0.0066(10) -0.0055(10) -0.0029(10)
C10 0.0289(13) 0.0324(15) 0.0232(13) -0.0105(11) -0.0102(11) -0.0037(11)
C11 0.0509(18) 0.0388(17) 0.0272(14) -0.0124(13) -0.0095(13) -0.0195(14)
C12 0.068(2) 0.0245(15) 0.0238(14) -0.0082(12) -0.0108(14) -0.0105(14)
C13 0.0460(17) 0.0298(16) 0.0282(15) -0.0058(13) -0.0156(14) 0.0084(13)
C14 0.0248(13) 0.0356(16) 0.0270(14) -0.0050(12) -0.0105(11) -0.0026(11)
C15 0.0153(10) 0.0296(14) 0.0269(13) -0.0154(11) -0.0030(10) -0.0026(9)
C16 0.0148(10) 0.0291(14) 0.0274(13) -0.0122(11) -0.0047(10) -0.0056(9)
C17 0.0312(14) 0.0328(16) 0.0382(17) -0.0153(13) 0.0001(13) -0.0090(12)
C18 0.0325(16) 0.0320(17) 0.064(2) -0.0179(16) -0.0025(16) -0.0034(13)
C19 0.0355(17) 0.0356(18) 0.057(2) 0.0040(16) -0.0165(16) -0.0111(14)
C20 0.0415(17) 0.061(2) 0.0284(16) 0.0004(15) -0.0121(14) -0.0246(16)
C21 0.0290(14) 0.0502(19) 0.0292(15) -0.0182(14) -0.0039(12) -0.0137(13)

_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 C7 1.896(2) . ?
Ni1 C7 1.896(2) 2_665 ?
Ni1 C1 1.906(2) 2_665 ?
Ni1 C1 1.906(2) . ?
N1 C1 1.356(3) . ?
N1 C2 1.387(3) . ?
N1 C8 1.476(3) . ?
N2 C1 1.358(3) . ?
N2 C3 1.385(3) . ?
N2 C4 1.456(3) . ?
N3 C7 1.361(3) . ?
N3 C5 1.391(3) . ?
N3 C4 1.458(3) . ?
N4 C7 1.352(3) . ?
N4 C6 1.387(3) . ?
N4 C15 1.468(3) . ?
C2 C3 1.344(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.348(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C8 C9 1.509(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.388(3) . ?
C9 C10 1.392(4) . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(4) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.512(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.390(4) . ?
C16 C21 1.391(4) . ?
C17 C18 1.384(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.375(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.388(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?

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
C7 Ni1 C7 180.00(11) . 2_665 ?
C7 Ni1 C1 93.90(10) . 2_665 ?
C7 Ni1 C1 86.10(10) 2_665 2_665 ?
C7 Ni1 C1 86.10(10) . . ?
C7 Ni1 C1 93.90(10) 2_665 . ?
C1 Ni1 C1 180.0 2_665 . ?
C1 N1 C2 110.7(2) . . ?
C1 N1 C8 125.9(2) . . ?
C2 N1 C8 123.4(2) . . ?
C1 N2 C3 111.8(2) . . ?
C1 N2 C4 121.3(2) . . ?
C3 N2 C4 126.9(2) . . ?
C7 N3 C5 111.7(2) . . ?
C7 N3 C4 121.96(19) . . ?
C5 N3 C4 126.3(2) . . ?
C7 N4 C6 111.1(2) . . ?
C7 N4 C15 126.4(2) . . ?
C6 N4 C15 122.1(2) . . ?
N1 C1 N2 104.1(2) . . ?
N1 C1 Ni1 134.32(18) . . ?
N2 C1 Ni1 121.61(17) . . ?
C3 C2 N1 107.5(2) . . ?
C3 C2 H2 126.2 . . ?
N1 C2 H2 126.2 . . ?
C2 C3 N2 105.9(2) . . ?
C2 C3 H3 127.1 . . ?
N2 C3 H3 127.1 . . ?
N2 C4 N3 107.63(19) . . ?
N2 C4 H4A 110.2 . . ?
N3 C4 H4A 110.2 . . ?
N2 C4 H4B 110.2 . . ?
N3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
C6 C5 N3 105.7(2) . . ?
C6 C5 H5 127.2 . . ?
N3 C5 H5 127.2 . . ?
C5 C6 N4 107.4(2) . . ?
C5 C6 H6 126.3 . . ?
N4 C6 H6 126.3 . . ?
N4 C7 N3 104.06(19) . . ?
N4 C7 Ni1 134.82(18) . . ?
N3 C7 Ni1 120.95(17) . . ?
N1 C8 C9 111.5(2) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C14 C9 C10 119.4(3) . . ?
C14 C9 C8 120.5(2) . . ?
C10 C9 C8 120.1(2) . . ?
C11 C10 C9 119.8(2) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 119.9(3) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.8(3) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C9 120.6(3) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
N4 C15 C16 112.7(2) . . ?
N4 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N4 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C21 118.6(3) . . ?
C17 C16 C15 121.9(2) . . ?
C21 C16 C15 119.4(2) . . ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 119.3(3) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C21 120.7(3) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C16 120.1(3) . . ?
C20 C21 H21 119.9 . . ?
C16 C21 H21 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N2 0.4(3) . . . . ?
C8 N1 C1 N2 -178.4(2) . . . . ?
C2 N1 C1 Ni1 -179.7(2) . . . . ?
C8 N1 C1 Ni1 1.4(4) . . . . ?
C3 N2 C1 N1 -0.8(3) . . . . ?
C4 N2 C1 N1 176.9(2) . . . . ?
C3 N2 C1 Ni1 179.38(17) . . . . ?
C4 N2 C1 Ni1 -2.9(3) . . . . ?
C7 Ni1 C1 N1 -135.9(3) . . . . ?
C7 Ni1 C1 N1 44.1(3) 2_665 . . . ?
C7 Ni1 C1 N2 43.9(2) . . . . ?
C7 Ni1 C1 N2 -136.1(2) 2_665 . . . ?
C1 N1 C2 C3 0.0(3) . . . . ?
C8 N1 C2 C3 179.0(2) . . . . ?
N1 C2 C3 N2 -0.5(3) . . . . ?
C1 N2 C3 C2 0.8(3) . . . . ?
C4 N2 C3 C2 -176.7(2) . . . . ?
C1 N2 C4 N3 -49.3(3) . . . . ?
C3 N2 C4 N3 128.1(2) . . . . ?
C7 N3 C4 N2 47.5(3) . . . . ?
C5 N3 C4 N2 -131.1(2) . . . . ?
C7 N3 C5 C6 -0.7(3) . . . . ?
C4 N3 C5 C6 178.1(2) . . . . ?
N3 C5 C6 N4 -0.4(3) . . . . ?
C7 N4 C6 C5 1.3(3) . . . . ?
C15 N4 C6 C5 -171.7(2) . . . . ?
C6 N4 C7 N3 -1.7(3) . . . . ?
C15 N4 C7 N3 171.0(2) . . . . ?
C6 N4 C7 Ni1 173.5(2) . . . . ?
C15 N4 C7 Ni1 -13.8(4) . . . . ?
C5 N3 C7 N4 1.5(3) . . . . ?
C4 N3 C7 N4 -177.4(2) . . . . ?
C5 N3 C7 Ni1 -174.57(17) . . . . ?
C4 N3 C7 Ni1 6.6(3) . . . . ?
C1 Ni1 C7 N4 -40.0(3) 2_665 . . . ?
C1 Ni1 C7 N4 140.0(3) . . . . ?
C1 Ni1 C7 N3 134.5(2) 2_665 . . . ?
C1 Ni1 C7 N3 -45.5(2) . . . . ?
C1 N1 C8 C9 117.7(3) . . . . ?
C2 N1 C8 C9 -61.0(3) . . . . ?
N1 C8 C9 C14 98.4(3) . . . . ?
N1 C8 C9 C10 -81.9(3) . . . . ?
C14 C9 C10 C11 1.0(4) . . . . ?
C8 C9 C10 C11 -178.7(2) . . . . ?
C9 C10 C11 C12 -1.4(4) . . . . ?
C10 C11 C12 C13 0.9(4) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C12 C13 C14 C9 -0.5(4) . . . . ?
C10 C9 C14 C13 -0.1(4) . . . . ?
C8 C9 C14 C13 179.7(3) . . . . ?
C7 N4 C15 C16 -84.7(3) . . . . ?
C6 N4 C15 C16 87.2(3) . . . . ?
N4 C15 C16 C17 -52.9(3) . . . . ?
N4 C15 C16 C21 130.2(2) . . . . ?
C21 C16 C17 C18 0.7(4) . . . . ?
C15 C16 C17 C18 -176.2(3) . . . . ?
C16 C17 C18 C19 0.5(5) . . . . ?
C17 C18 C19 C20 -1.1(5) . . . . ?
C18 C19 C20 C21 0.5(5) . . . . ?
C19 C20 C21 C16 0.7(4) . . . . ?
C17 C16 C21 C20 -1.3(4) . . . . ?
C15 C16 C21 C20 175.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        29.64
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.121