# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_Complex1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 N10 Ni2 O2'
_chemical_formula_sum            'C32 H26 N10 Ni2 O2'
_chemical_formula_weight         700.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4696(4)
_cell_length_b                   11.6432(5)
_cell_length_c                   13.4883(5)
_cell_angle_alpha                84.488(2)
_cell_angle_beta                 82.801(2)
_cell_angle_gamma                61.108(2)
_cell_volume                     1563.33(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4490
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      21.50

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720.0
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25635
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         28.37
_reflns_number_total             7832
_reflns_number_gt                6258
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0660P)²+0.0000P] 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         7832
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.85439(4) 0.03498(4) 0.47877(3) 0.03650(15) Uani 1 1 d . . .
Ni2 Ni 0.35826(4) 0.51640(4) 0.04573(3) 0.03911(16) Uani 1 1 d . . .
O1 O 0.4518(2) 0.6285(2) 0.01920(18) 0.0413(6) Uani 1 1 d . . .
O2 O 0.9849(2) 0.1052(2) 0.43773(16) 0.0369(6) Uani 1 1 d . . .
N1 N 0.2617(3) 0.4052(3) 0.0375(2) 0.0421(7) Uani 1 1 d . . .
N2 N 0.2831(3) 0.5817(3) -0.0883(2) 0.0418(7) Uani 1 1 d . . .
N3 N 0.4177(3) 0.4485(3) 0.1850(3) 0.0528(9) Uani 1 1 d . . .
N4 N 0.5117(4) 0.3847(4) 0.3470(3) 0.0634(10) Uani 1 1 d . . .
N5 N 0.7082(3) 0.1798(3) 0.3936(2) 0.0511(9) Uani 1 1 d . . .
N6 N 0.1805(3) 0.6604(3) 0.1184(2) 0.0520(9) Uani 1 1 d . . .
N7 N -0.0095(4) 0.7327(4) 0.2478(3) 0.0677(11) Uani 1 1 d . . .
N8 N 0.7755(3) 0.1633(3) 0.5904(2) 0.0411(7) Uani 1 1 d . . .
N9 N 0.7198(3) -0.0219(3) 0.5544(2) 0.0455(8) Uani 1 1 d . . .
N10 N 0.9149(3) -0.0945(3) 0.3663(2) 0.0458(8) Uani 1 1 d . . .
C1 C 0.2385(4) 0.3329(4) 0.1115(3) 0.0553(11) Uani 1 1 d . . .
H1 H 0.2739 0.3229 0.1721 0.066 Uiso 1 1 calc R . .
C2 C 0.1624(5) 0.2715(4) 0.1008(4) 0.0671(13) Uani 1 1 d . . .
H2 H 0.1484 0.2204 0.1535 0.081 Uiso 1 1 calc R . .
C3 C 0.1092(4) 0.2866(4) 0.0135(4) 0.0660(13) Uani 1 1 d . . .
H3 H 0.0570 0.2475 0.0058 0.079 Uiso 1 1 calc R . .
C4 C 0.1333(4) 0.3604(4) -0.0638(3) 0.0595(12) Uani 1 1 d . . .
H4 H 0.0990 0.3709 -0.1249 0.071 Uiso 1 1 calc R . .
C5 C 0.2096(4) 0.4189(4) -0.0490(3) 0.0476(10) Uani 1 1 d . . .
C6 C 0.2385(4) 0.5002(4) -0.1318(3) 0.0548(11) Uani 1 1 d . . .
H6 H 0.1555 0.5582 -0.1627 0.066 Uiso 1 1 calc R . .
C7 C 0.3413(6) 0.4159(5) -0.2108(4) 0.0899(17) Uani 1 1 d . . .
H7A H 0.3441 0.4701 -0.2684 0.135 Uiso 1 1 calc R . .
H7B H 0.3180 0.3525 -0.2294 0.135 Uiso 1 1 calc R . .
H7C H 0.4274 0.3712 -0.1851 0.135 Uiso 1 1 calc R . .
C8 C 0.2527(4) 0.6953(4) -0.1271(3) 0.0488(10) Uani 1 1 d . . .
H8 H 0.1994 0.7238 -0.1802 0.059 Uiso 1 1 calc R . .
C9 C 0.2948(4) 0.7848(4) -0.0951(3) 0.0466(10) Uani 1 1 d . . .
C10 C 0.2407(4) 0.9119(4) -0.1405(3) 0.0571(11) Uani 1 1 d . . .
H10 H 0.1781 0.9360 -0.1866 0.068 Uiso 1 1 calc R . .
C11 C 0.2785(5) 1.0004(4) -0.1183(4) 0.0691(13) Uani 1 1 d . . .
H11 H 0.2418 1.0839 -0.1490 0.083 Uiso 1 1 calc R . .
C12 C 0.3713(4) 0.9652(4) -0.0501(3) 0.0604(12) Uani 1 1 d . . .
H12 H 0.3967 1.0257 -0.0348 0.073 Uiso 1 1 calc R . .
C13 C 0.4266(4) 0.8427(4) -0.0046(3) 0.0522(10) Uani 1 1 d . . .
H13 H 0.4887 0.8222 0.0413 0.063 Uiso 1 1 calc R . .
C14 C 0.3927(4) 0.7462(4) -0.0248(3) 0.0484(10) Uani 1 1 d . . .
C15 C 0.4668(4) 0.4124(4) 0.2585(3) 0.0462(10) Uani 1 1 d . . .
C16 C 0.6194(4) 0.2730(4) 0.3673(3) 0.0443(9) Uani 1 1 d . . .
C17 C 0.0944(4) 0.6983(4) 0.1805(3) 0.0447(9) Uani 1 1 d . . .
C18 C 0.6913(4) -0.1114(4) 0.5258(3) 0.0594(12) Uani 1 1 d . . .
H18 H 0.7319 -0.1512 0.4654 0.071 Uiso 1 1 calc R . .
C19 C 0.6051(5) -0.1472(5) 0.5815(4) 0.0764(14) Uani 1 1 d . . .
H19 H 0.5883 -0.2107 0.5596 0.092 Uiso 1 1 calc R . .
C20 C 0.5440(5) -0.0883(5) 0.6698(4) 0.0848(16) Uani 1 1 d . . .
H20 H 0.4846 -0.1106 0.7088 0.102 Uiso 1 1 calc R . .
C21 C 0.5717(5) 0.0043(5) 0.6999(4) 0.0774(15) Uani 1 1 d . . .
H21 H 0.5311 0.0456 0.7598 0.093 Uiso 1 1 calc R . .
C22 C 0.6604(4) 0.0360(4) 0.6407(3) 0.0528(11) Uani 1 1 d . . .
C23 C 0.6987(5) 0.1325(4) 0.6731(3) 0.0661(13) Uani 1 1 d . . .
H23 H 0.6181 0.2129 0.6941 0.079 Uiso 1 1 calc R . .
C24 C 0.7926(7) 0.0690(6) 0.7639(3) 0.117(2) Uani 1 1 d . . .
H24A H 0.8775 -0.0009 0.7399 0.175 Uiso 1 1 calc R . .
H24B H 0.7505 0.0350 0.8155 0.175 Uiso 1 1 calc R . .
H24C H 0.8057 0.1351 0.7904 0.175 Uiso 1 1 calc R . .
C25 C 0.7698(4) 0.2752(4) 0.5832(3) 0.0490(10) Uani 1 1 d . . .
H25 H 0.7141 0.3350 0.6312 0.059 Uiso 1 1 calc R . .
C26 C 0.8429(4) 0.3185(4) 0.5062(3) 0.0470(10) Uani 1 1 d . . .
C27 C 0.8091(5) 0.4515(4) 0.5017(4) 0.0709(13) Uani 1 1 d . . .
H27 H 0.7401 0.5079 0.5458 0.085 Uiso 1 1 calc R . .
C28 C 0.8747(5) 0.5009(5) 0.4342(4) 0.0820(15) Uani 1 1 d . . .
H28 H 0.8513 0.5894 0.4332 0.098 Uiso 1 1 calc R . .
C29 C 0.9752(5) 0.4189(5) 0.3679(4) 0.0733(14) Uani 1 1 d . . .
H29 H 1.0196 0.4518 0.3212 0.088 Uiso 1 1 calc R . .
C30 C 1.0104(4) 0.2875(4) 0.3707(3) 0.0569(11) Uani 1 1 d . . .
H30 H 1.0793 0.2333 0.3256 0.068 Uiso 1 1 calc R . .
C31 C 0.9466(4) 0.2321(4) 0.4388(3) 0.0416(9) Uani 1 1 d . . .
C32 C 0.9559(4) -0.1739(4) 0.3096(3) 0.0437(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 O2 2.025(2) . ?
Ni1 N8 2.026(3) . ?
Ni1 N10 2.054(3) . ?
Ni1 N9 2.080(3) . ?
Ni1 N5 2.087(3) . ?
Ni1 O2 2.143(2) 2_756 ?
Ni2 N2 2.021(3) . ?
Ni2 N3 2.033(3) . ?
Ni2 O1 2.036(2) . ?
Ni2 N1 2.087(3) . ?
Ni2 N6 2.107(3) . ?
Ni2 O1 2.148(2) 2_665 ?
O1 C14 1.318(4) . ?
O1 Ni2 2.148(2) 2_665 ?
O2 C31 1.324(4) . ?
O2 Ni1 2.143(2) 2_756 ?
N1 C1 1.329(5) . ?
N1 C5 1.338(4) . ?
N2 C8 1.270(4) . ?
N2 C6 1.469(4) . ?
N3 C15 1.144(5) . ?
N4 C15 1.310(5) . ?
N4 C16 1.325(5) . ?
N5 C16 1.136(5) . ?
N6 C17 1.147(4) . ?
N7 C32 1.307(5) 1_465 ?
N7 C17 1.320(5) . ?
N8 C25 1.268(4) . ?
N8 C23 1.459(4) . ?
N9 C18 1.334(5) . ?
N9 C22 1.335(5) . ?
N10 C32 1.134(4) . ?
C1 C2 1.396(5) . ?
C2 C3 1.352(6) . ?
C3 C4 1.374(6) . ?
C4 C5 1.384(5) . ?
C5 C6 1.503(5) . ?
C6 C7 1.503(6) . ?
C8 C9 1.459(5) . ?
C9 C10 1.409(5) . ?
C9 C14 1.435(5) . ?
C10 C11 1.365(5) . ?
C11 C12 1.378(6) . ?
C12 C13 1.367(5) . ?
C13 C14 1.413(5) . ?
C18 C19 1.366(5) . ?
C19 C20 1.364(6) . ?
C20 C21 1.369(6) . ?
C21 C22 1.383(5) . ?
C22 C23 1.505(5) . ?
C23 C24 1.611(7) . ?
C25 C26 1.458(5) . ?
C26 C27 1.400(5) . ?
C26 C31 1.414(5) . ?
C27 C28 1.369(6) . ?
C28 C29 1.372(6) . ?
C29 C30 1.378(6) . ?
C30 C31 1.403(5) . ?
C32 N7 1.307(5) 1_645 ?

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
O2 Ni1 N8 88.05(10) . . ?
O2 Ni1 N10 97.48(10) . . ?
N8 Ni1 N10 173.88(11) . . ?
O2 Ni1 N9 166.23(11) . . ?
N8 Ni1 N9 79.57(11) . . ?
N10 Ni1 N9 95.20(12) . . ?
O2 Ni1 N5 92.95(11) . . ?
N8 Ni1 N5 86.61(12) . . ?
N10 Ni1 N5 90.46(12) . . ?
N9 Ni1 N5 92.32(12) . . ?
O2 Ni1 O2 81.94(9) . 2_756 ?
N8 Ni1 O2 92.90(10) . 2_756 ?
N10 Ni1 O2 90.49(10) . 2_756 ?
N9 Ni1 O2 92.60(10) . 2_756 ?
N5 Ni1 O2 174.88(10) . 2_756 ?
N2 Ni2 N3 174.35(12) . . ?
N2 Ni2 O1 88.49(11) . . ?
N3 Ni2 O1 96.50(11) . . ?
N2 Ni2 N1 79.29(12) . . ?
N3 Ni2 N1 95.94(13) . . ?
O1 Ni2 N1 166.88(11) . . ?
N2 Ni2 N6 90.69(12) . . ?
N3 Ni2 N6 86.14(13) . . ?
O1 Ni2 N6 96.38(11) . . ?
N1 Ni2 N6 88.59(12) . . ?
N2 Ni2 O1 93.21(11) . 2_665 ?
N3 Ni2 O1 90.19(11) . 2_665 ?
O1 Ni2 O1 81.03(10) . 2_665 ?
N1 Ni2 O1 94.79(10) . 2_665 ?
N6 Ni2 O1 175.25(10) . 2_665 ?
C14 O1 Ni2 121.1(2) . . ?
C14 O1 Ni2 119.2(2) . 2_665 ?
Ni2 O1 Ni2 98.97(10) . 2_665 ?
C31 O2 Ni1 121.3(2) . . ?
C31 O2 Ni1 120.6(2) . 2_756 ?
Ni1 O2 Ni1 98.06(9) . 2_756 ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Ni2 126.3(3) . . ?
C5 N1 Ni2 115.2(2) . . ?
C8 N2 C6 119.0(3) . . ?
C8 N2 Ni2 124.2(3) . . ?
C6 N2 Ni2 115.7(2) . . ?
C15 N3 Ni2 170.2(3) . . ?
C15 N4 C16 121.6(3) . . ?
C16 N5 Ni1 164.2(3) . . ?
C17 N6 Ni2 154.5(3) . . ?
C32 N7 C17 122.2(3) 1_465 . ?
C25 N8 C23 119.7(3) . . ?
C25 N8 Ni1 123.5(3) . . ?
C23 N8 Ni1 115.6(2) . . ?
C18 N9 C22 118.5(3) . . ?
C18 N9 Ni1 126.2(3) . . ?
C22 N9 Ni1 115.3(2) . . ?
C32 N10 Ni1 174.0(3) . . ?
N1 C1 C2 121.8(4) . . ?
C3 C2 C1 119.6(4) . . ?
C2 C3 C4 119.1(4) . . ?
C3 C4 C5 118.8(4) . . ?
N1 C5 C4 122.4(4) . . ?
N1 C5 C6 117.2(3) . . ?
C4 C5 C6 120.4(4) . . ?
N2 C6 C7 110.9(3) . . ?
N2 C6 C5 108.6(3) . . ?
C7 C6 C5 111.6(4) . . ?
N2 C8 C9 125.2(4) . . ?
C10 C9 C14 119.7(4) . . ?
C10 C9 C8 117.2(4) . . ?
C14 C9 C8 122.9(3) . . ?
C11 C10 C9 121.3(4) . . ?
C10 C11 C12 119.5(4) . . ?
C13 C12 C11 121.0(4) . . ?
C12 C13 C14 122.3(4) . . ?
O1 C14 C13 119.8(4) . . ?
O1 C14 C9 124.2(3) . . ?
C13 C14 C9 116.1(4) . . ?
N3 C15 N4 173.0(4) . . ?
N5 C16 N4 173.8(4) . . ?
N6 C17 N7 173.1(4) . . ?
N9 C18 C19 122.8(4) . . ?
C20 C19 C18 119.0(4) . . ?
C19 C20 C21 118.9(4) . . ?
C20 C21 C22 119.6(4) . . ?
N9 C22 C21 121.2(4) . . ?
N9 C22 C23 117.3(3) . . ?
C21 C22 C23 121.4(4) . . ?
N8 C23 C22 109.7(3) . . ?
N8 C23 C24 107.4(3) . . ?
C22 C23 C24 110.1(4) . . ?
N8 C25 C26 125.7(4) . . ?
C27 C26 C31 119.7(4) . . ?
C27 C26 C25 117.3(4) . . ?
C31 C26 C25 123.0(3) . . ?
C28 C27 C26 121.8(4) . . ?
C27 C28 C29 119.5(4) . . ?
C28 C29 C30 119.9(4) . . ?
C29 C30 C31 122.8(4) . . ?
O2 C31 C30 119.9(3) . . ?
O2 C31 C26 123.6(3) . . ?
C30 C31 C26 116.4(3) . . ?
N10 C32 N7 173.0(4) . 1_645 ?

_diffrn_measured_fraction_theta_max 1.00
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 1.00
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 1014355'
