# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 1044662'
_audit_update_record             
;
2015-01-21 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H80 Cl2 N4 Ni2'
_chemical_formula_weight         1189.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   16.1963(11)
_cell_length_b                   12.2535(8)
_cell_length_c                   16.3252(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6890(10)
_cell_angle_gamma                90.00
_cell_volume                     3229.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    4285
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.08

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1260
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8482
_exptl_absorpt_correction_T_max  0.9197
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(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 scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20255
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         26.04
_reflns_number_total             6341
_reflns_number_gt                4646
_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)+(0.0548P)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         6341
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1033
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
C1 C 0.08677(14) 0.06547(18) 0.25052(12) 0.0250(5) Uani 1 1 d . . .
C2 C 0.10837(14) 0.08128(18) 0.33902(13) 0.0260(5) Uani 1 1 d . . .
C3 C 0.06936(16) 0.0655(2) 0.40994(13) 0.0339(6) Uani 1 1 d . . .
H3 H 0.0141 0.0390 0.4078 0.041 Uiso 1 1 calc R . .
C4 C 0.11357(17) 0.0898(2) 0.48604(14) 0.0372(6) Uani 1 1 d . . .
H4 H 0.0870 0.0786 0.5351 0.045 Uiso 1 1 calc R . .
C5 C 0.19302(16) 0.12893(18) 0.49196(13) 0.0340(6) Uani 1 1 d . . .
H5 H 0.2205 0.1433 0.5445 0.041 Uiso 1 1 calc R . .
C6 C 0.23447(15) 0.14804(17) 0.42021(13) 0.0283(5) Uani 1 1 d . . .
C7 C 0.19050(14) 0.12247(17) 0.34556(13) 0.0250(5) Uani 1 1 d . . .
C8 C 0.31506(16) 0.1913(2) 0.41516(14) 0.0359(6) Uani 1 1 d . . .
H8 H 0.3481 0.2093 0.4640 0.043 Uiso 1 1 calc R . .
C9 C 0.34561(16) 0.2072(2) 0.34027(15) 0.0387(6) Uani 1 1 d . . .
H9 H 0.3996 0.2372 0.3387 0.046 Uiso 1 1 calc R . .
C10 C 0.30048(15) 0.18109(19) 0.26552(14) 0.0314(6) Uani 1 1 d . . .
H10 H 0.3235 0.1932 0.2146 0.038 Uiso 1 1 calc R . .
C11 C 0.22266(14) 0.13779(17) 0.26764(13) 0.0239(5) Uani 1 1 d . . .
C12 C 0.15674(14) 0.10052(17) 0.20702(12) 0.0229(5) Uani 1 1 d . . .
C13 C -0.05777(14) 0.0284(2) 0.24076(13) 0.0308(6) Uani 1 1 d . . .
C14 C -0.09942(15) 0.1255(2) 0.25837(14) 0.0347(6) Uani 1 1 d . . .
C15 C -0.17632(16) 0.1162(2) 0.29019(16) 0.0452(7) Uani 1 1 d . . .
H15 H -0.2053 0.1806 0.3031 0.054 Uiso 1 1 calc R . .
C16 C -0.21156(17) 0.0158(2) 0.30340(17) 0.0473(7) Uani 1 1 d . . .
H16 H -0.2642 0.0113 0.3249 0.057 Uiso 1 1 calc R . .
C17 C -0.16988(16) -0.0777(2) 0.28516(15) 0.0416(6) Uani 1 1 d . . .
H17 H -0.1945 -0.1466 0.2943 0.050 Uiso 1 1 calc R . .
C18 C -0.09231(15) -0.0741(2) 0.25360(14) 0.0341(6) Uani 1 1 d . . .
C19 C -0.06500(17) 0.2379(2) 0.24016(15) 0.0390(6) Uani 1 1 d . . .
H19 H -0.0051 0.2286 0.2311 0.047 Uiso 1 1 calc R . .
C20 C -0.0703(2) 0.3184(3) 0.31165(18) 0.0628(9) Uani 1 1 d . . .
H20A H -0.0432 0.3871 0.2987 0.094 Uiso 1 1 calc R . .
H20B H -0.0424 0.2871 0.3618 0.094 Uiso 1 1 calc R . .
H20C H -0.1285 0.3324 0.3201 0.094 Uiso 1 1 calc R . .
C21 C -0.10821(19) 0.2839(2) 0.16125(17) 0.0543(8) Uani 1 1 d . . .
H21A H -0.1003 0.2341 0.1156 0.081 Uiso 1 1 calc R . .
H21B H -0.0846 0.3554 0.1498 0.081 Uiso 1 1 calc R . .
H21C H -0.1675 0.2918 0.1677 0.081 Uiso 1 1 calc R . .
C22 C -0.04656(16) -0.1788(2) 0.23723(16) 0.0401(6) Uani 1 1 d . . .
H22 H -0.0007 -0.1595 0.2024 0.048 Uiso 1 1 calc R . .
C23 C -0.0068(2) -0.2264(3) 0.31723(18) 0.0635(9) Uani 1 1 d . . .
H23A H 0.0319 -0.1733 0.3437 0.095 Uiso 1 1 calc R . .
H23B H 0.0231 -0.2934 0.3054 0.095 Uiso 1 1 calc R . .
H23C H -0.0500 -0.2433 0.3540 0.095 Uiso 1 1 calc R . .
C24 C -0.1006(2) -0.2632(3) 0.1902(2) 0.0722(10) Uani 1 1 d . . .
H24A H -0.1407 -0.2928 0.2261 0.108 Uiso 1 1 calc R . .
H24B H -0.0657 -0.3223 0.1721 0.108 Uiso 1 1 calc R . .
H24C H -0.1302 -0.2287 0.1422 0.108 Uiso 1 1 calc R . .
C25 C 0.20483(15) 0.15762(18) 0.08157(12) 0.0276(5) Uani 1 1 d . . .
C26 C 0.19494(16) 0.27128(19) 0.07323(13) 0.0328(6) Uani 1 1 d . . .
C27 C 0.25570(19) 0.3286(2) 0.03562(15) 0.0446(7) Uani 1 1 d . . .
H27 H 0.2515 0.4057 0.0311 0.054 Uiso 1 1 calc R . .
C28 C 0.32139(19) 0.2764(2) 0.00497(16) 0.0500(8) Uani 1 1 d . . .
H28 H 0.3626 0.3174 -0.0196 0.060 Uiso 1 1 calc R . .
C29 C 0.32749(18) 0.1643(2) 0.00986(15) 0.0436(7) Uani 1 1 d . . .
H29 H 0.3725 0.1287 -0.0128 0.052 Uiso 1 1 calc R . .
C30 C 0.26921(16) 0.10193(19) 0.04714(14) 0.0324(6) Uani 1 1 d . . .
C31 C 0.12074(17) 0.3305(2) 0.10367(15) 0.0405(6) Uani 1 1 d . . .
H31 H 0.0792 0.2741 0.1169 0.049 Uiso 1 1 calc R . .
C32 C 0.1441(2) 0.3952(2) 0.18193(16) 0.0521(8) Uani 1 1 d . . .
H32A H 0.1655 0.3453 0.2255 0.078 Uiso 1 1 calc R . .
H32B H 0.0950 0.4329 0.1991 0.078 Uiso 1 1 calc R . .
H32C H 0.1868 0.4489 0.1715 0.078 Uiso 1 1 calc R . .
C33 C 0.0790(2) 0.4063(2) 0.03787(18) 0.0596(9) Uani 1 1 d . . .
H33A H 0.1183 0.4626 0.0237 0.089 Uiso 1 1 calc R . .
H33B H 0.0305 0.4408 0.0591 0.089 Uiso 1 1 calc R . .
H33C H 0.0614 0.3637 -0.0113 0.089 Uiso 1 1 calc R . .
C34 C 0.27484(17) -0.02138(19) 0.04761(16) 0.0392(6) Uani 1 1 d . . .
H34 H 0.2321 -0.0498 0.0830 0.047 Uiso 1 1 calc R . .
C35 C 0.3589(2) -0.0622(3) 0.0830(2) 0.0679(10) Uani 1 1 d . . .
H35A H 0.4012 -0.0422 0.0461 0.102 Uiso 1 1 calc R . .
H35B H 0.3573 -0.1418 0.0887 0.102 Uiso 1 1 calc R . .
H35C H 0.3725 -0.0290 0.1370 0.102 Uiso 1 1 calc R . .
C36 C 0.2546(2) -0.0648(2) -0.03851(19) 0.0695(10) Uani 1 1 d . . .
H36A H 0.1984 -0.0424 -0.0584 0.104 Uiso 1 1 calc R . .
H36B H 0.2580 -0.1447 -0.0378 0.104 Uiso 1 1 calc R . .
H36C H 0.2943 -0.0356 -0.0750 0.104 Uiso 1 1 calc R . .
Cl1 Cl 0.01338(5) -0.12846(5) 0.02565(4) 0.0470(2) Uani 1 1 d . . .
N1 N 0.01974(12) 0.03755(15) 0.20458(11) 0.0269(4) Uani 1 1 d . . .
N2 N 0.14558(11) 0.09996(14) 0.12667(10) 0.0251(4) Uani 1 1 d . . .
Ni1 Ni 0.039357(19) 0.03589(2) 0.088642(16) 0.02789(11) 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
C1 N1 1.313(3) . ?
C1 C12 1.451(3) . ?
C1 C2 1.471(3) . ?
C2 C3 1.377(3) . ?
C2 C7 1.419(3) . ?
C3 C4 1.414(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.416(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(3) . ?
C6 C8 1.417(3) . ?
C7 C11 1.426(3) . ?
C8 C9 1.370(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.407(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.371(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.468(3) . ?
C12 N2 1.310(3) . ?
C13 C18 1.399(3) . ?
C13 C14 1.409(3) . ?
C13 N1 1.435(3) . ?
C14 C15 1.393(3) . ?
C14 C19 1.524(4) . ?
C15 C16 1.381(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.375(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.397(3) . ?
C17 H17 0.9500 . ?
C18 C22 1.515(4) . ?
C19 C21 1.523(4) . ?
C19 C20 1.536(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.521(4) . ?
C22 C23 1.524(4) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.402(3) . ?
C25 C26 1.407(3) . ?
C25 N2 1.441(3) . ?
C26 C27 1.392(3) . ?
C26 C31 1.522(3) . ?
C27 C28 1.370(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(3) . ?
C29 H29 0.9500 . ?
C30 C34 1.514(3) . ?
C31 C32 1.524(3) . ?
C31 C33 1.534(4) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.514(4) . ?
C34 C35 1.520(4) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
Cl1 Ni1 2.2846(7) . ?
Cl1 Ni1 2.2886(7) 3 ?
N1 Ni1 1.9447(17) . ?
N2 Ni1 1.9460(19) . ?
Ni1 Cl1 2.2886(7) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C12 116.10(18) . . ?
N1 C1 C2 135.6(2) . . ?
C12 C1 C2 108.01(19) . . ?
C3 C2 C7 118.6(2) . . ?
C3 C2 C1 135.9(2) . . ?
C7 C2 C1 105.49(18) . . ?
C2 C3 C4 118.4(2) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 122.8(2) . . ?
C5 C4 H4 118.6 . . ?
C3 C4 H4 118.6 . . ?
C4 C5 C6 120.4(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 116.3(2) . . ?
C7 C6 C8 116.1(2) . . ?
C5 C6 C8 127.7(2) . . ?
C6 C7 C2 123.6(2) . . ?
C6 C7 C11 123.5(2) . . ?
C2 C7 C11 112.85(19) . . ?
C9 C8 C6 120.4(2) . . ?
C9 C8 H8 119.8 . . ?
C6 C8 H8 119.8 . . ?
C8 C9 C10 122.8(2) . . ?
C8 C9 H9 118.6 . . ?
C10 C9 H9 118.6 . . ?
C11 C10 C9 118.7(2) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C7 118.5(2) . . ?
C10 C11 C12 136.3(2) . . ?
C7 C11 C12 105.19(19) . . ?
N2 C12 C1 116.1(2) . . ?
N2 C12 C11 135.2(2) . . ?
C1 C12 C11 108.44(17) . . ?
C18 C13 C14 121.6(2) . . ?
C18 C13 N1 120.4(2) . . ?
C14 C13 N1 117.9(2) . . ?
C15 C14 C13 117.7(2) . . ?
C15 C14 C19 120.0(2) . . ?
C13 C14 C19 122.3(2) . . ?
C16 C15 C14 121.7(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C15 119.5(3) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 121.7(3) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C17 C18 C13 117.8(2) . . ?
C17 C18 C22 120.4(2) . . ?
C13 C18 C22 121.8(2) . . ?
C21 C19 C14 110.4(2) . . ?
C21 C19 C20 110.8(2) . . ?
C14 C19 C20 112.8(2) . . ?
C21 C19 H19 107.5 . . ?
C14 C19 H19 107.5 . . ?
C20 C19 H19 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 C24 113.2(2) . . ?
C18 C22 C23 110.6(2) . . ?
C24 C22 C23 110.9(3) . . ?
C18 C22 H22 107.3 . . ?
C24 C22 H22 107.3 . . ?
C23 C22 H22 107.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 121.7(2) . . ?
C30 C25 N2 121.0(2) . . ?
C26 C25 N2 117.3(2) . . ?
C27 C26 C25 117.6(2) . . ?
C27 C26 C31 120.6(2) . . ?
C25 C26 C31 121.8(2) . . ?
C28 C27 C26 121.6(2) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 119.8(2) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 121.6(3) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C29 C30 C25 117.5(2) . . ?
C29 C30 C34 120.5(2) . . ?
C25 C30 C34 122.0(2) . . ?
C26 C31 C32 111.9(2) . . ?
C26 C31 C33 112.0(2) . . ?
C32 C31 C33 109.7(2) . . ?
C26 C31 H31 107.7 . . ?
C32 C31 H31 107.7 . . ?
C33 C31 H31 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 C36 109.8(2) . . ?
C30 C34 C35 112.5(2) . . ?
C36 C34 C35 110.9(2) . . ?
C30 C34 H34 107.8 . . ?
C36 C34 H34 107.8 . . ?
C35 C34 H34 107.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Ni1 Cl1 Ni1 88.44(2) . 3 ?
C1 N1 C13 119.69(18) . . ?
C1 N1 Ni1 111.43(15) . . ?
C13 N1 Ni1 128.16(14) . . ?
C12 N2 C25 117.77(18) . . ?
C12 N2 Ni1 111.57(15) . . ?
C25 N2 Ni1 130.01(14) . . ?
N1 Ni1 N2 84.02(7) . . ?
N1 Ni1 Cl1 114.11(6) . . ?
N2 Ni1 Cl1 128.66(6) . . ?
N1 Ni1 Cl1 135.11(6) . 3 ?
N2 Ni1 Cl1 108.75(6) . 3 ?
Cl1 Ni1 Cl1 91.56(2) . 3 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.060
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_3
_database_code_depnum_ccdc_archive 'CCDC 1044663'
_audit_update_record             
;
2015-01-21 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64.50 H63 Cl N2 Ni P'
_chemical_formula_weight         991.30

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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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                   11.2339(15)
_cell_length_b                   13.5323(18)
_cell_length_c                   19.012(3)
_cell_angle_alpha                72.179(2)
_cell_angle_beta                 88.564(2)
_cell_angle_gamma                84.990(2)
_cell_volume                     2741.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    3564
_cell_measurement_theta_min      0.93
_cell_measurement_theta_max      25.02

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9073
_exptl_absorpt_correction_T_max  0.9240
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(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 scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13430
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         25.10
_reflns_number_total             9520
_reflns_number_gt                6909
_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)+(0.0724P)²+7.9198P] 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         9520
_refine_ls_number_parameters     577
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.1895
_refine_ls_wR_factor_gt          0.1714
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.004

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7629(4) 0.2884(4) 0.1098(3) 0.0271(10) Uani 1 1 d . . .
C2 C 0.7216(4) 0.3668(4) 0.0408(3) 0.0284(10) Uani 1 1 d . . .
C3 C 0.7124(4) 0.3721(4) -0.0318(3) 0.0360(12) Uani 1 1 d . . .
H3 H 0.7357 0.3130 -0.0475 0.043 Uiso 1 1 calc R . .
C4 C 0.6677(5) 0.4666(4) -0.0831(3) 0.0411(13) Uani 1 1 d . . .
H4 H 0.6609 0.4698 -0.1335 0.049 Uiso 1 1 calc R . .
C5 C 0.6340(5) 0.5534(4) -0.0634(3) 0.0423(13) Uani 1 1 d . . .
H5 H 0.6035 0.6152 -0.0997 0.051 Uiso 1 1 calc R . .
C6 C 0.6440(4) 0.5522(4) 0.0108(3) 0.0342(11) Uani 1 1 d . . .
C7 C 0.6857(4) 0.4585(4) 0.0610(3) 0.0288(10) Uani 1 1 d . . .
C8 C 0.6171(4) 0.6367(4) 0.0398(3) 0.0418(13) Uani 1 1 d . . .
H8 H 0.5878 0.7027 0.0078 0.050 Uiso 1 1 calc R . .
C9 C 0.6330(5) 0.6239(4) 0.1135(3) 0.0424(13) Uani 1 1 d . . .
H9 H 0.6141 0.6817 0.1314 0.051 Uiso 1 1 calc R . .
C10 C 0.6763(4) 0.5284(4) 0.1632(3) 0.0368(12) Uani 1 1 d . . .
H10 H 0.6873 0.5213 0.2139 0.044 Uiso 1 1 calc R . .
C11 C 0.7025(4) 0.4448(4) 0.1366(3) 0.0295(11) Uani 1 1 d . . .
C12 C 0.7517(4) 0.3360(3) 0.1691(3) 0.0252(10) Uani 1 1 d . . .
C13 C 0.8529(4) 0.1544(3) 0.0674(2) 0.0249(10) Uani 1 1 d . . .
C14 C 0.9586(4) 0.1875(4) 0.0307(3) 0.0301(11) Uani 1 1 d . . .
C15 C 0.9882(5) 0.1604(4) -0.0332(3) 0.0398(12) Uani 1 1 d . . .
H15 H 1.0591 0.1826 -0.0593 0.048 Uiso 1 1 calc R . .
C16 C 0.9161(5) 0.1019(4) -0.0588(3) 0.0451(14) Uani 1 1 d . . .
H16 H 0.9355 0.0867 -0.1035 0.054 Uiso 1 1 calc R . .
C17 C 0.8154(5) 0.0652(4) -0.0197(3) 0.0391(12) Uani 1 1 d . . .
H17 H 0.7679 0.0228 -0.0372 0.047 Uiso 1 1 calc R . .
C18 C 0.7821(4) 0.0889(4) 0.0446(3) 0.0304(11) Uani 1 1 d . . .
C19 C 0.8066(4) 0.3286(3) 0.2898(3) 0.0304(11) Uani 1 1 d . . .
C20 C 0.9152(5) 0.3712(4) 0.2931(3) 0.0354(12) Uani 1 1 d . . .
C21 C 0.9249(5) 0.4221(4) 0.3459(3) 0.0478(14) Uani 1 1 d . . .
H21 H 0.9967 0.4528 0.3489 0.057 Uiso 1 1 calc R . .
C22 C 0.8337(6) 0.4290(5) 0.3937(3) 0.0573(17) Uani 1 1 d . . .
H22 H 0.8428 0.4644 0.4292 0.069 Uiso 1 1 calc R . .
C23 C 0.7294(6) 0.3851(5) 0.3906(3) 0.0549(16) Uani 1 1 d . . .
H23 H 0.6668 0.3906 0.4240 0.066 Uiso 1 1 calc R . .
C24 C 0.7130(5) 0.3321(4) 0.3391(3) 0.0405(13) Uani 1 1 d . . .
C25 C 1.0426(4) 0.2498(4) 0.0587(3) 0.0348(11) Uani 1 1 d . . .
H25 H 1.0082 0.2591 0.1056 0.042 Uiso 1 1 calc R . .
C26 C 1.0516(5) 0.3569(4) 0.0042(4) 0.0523(15) Uani 1 1 d . . .
H26A H 1.0863 0.3502 -0.0421 0.078 Uiso 1 1 calc R . .
H26B H 1.1027 0.3964 0.0249 0.078 Uiso 1 1 calc R . .
H26C H 0.9717 0.3936 -0.0054 0.078 Uiso 1 1 calc R . .
C27 C 1.1662(5) 0.1912(4) 0.0767(3) 0.0432(13) Uani 1 1 d . . .
H27A H 1.1582 0.1222 0.1121 0.065 Uiso 1 1 calc R . .
H27B H 1.2162 0.2305 0.0982 0.065 Uiso 1 1 calc R . .
H27C H 1.2034 0.1835 0.0313 0.065 Uiso 1 1 calc R . .
C28 C 0.6724(4) 0.0483(4) 0.0881(3) 0.0329(11) Uani 1 1 d . . .
H28 H 0.6852 0.0459 0.1405 0.039 Uiso 1 1 calc R . .
C29 C 0.5616(5) 0.1217(4) 0.0597(3) 0.0462(14) Uani 1 1 d . . .
H29A H 0.5721 0.1899 0.0654 0.069 Uiso 1 1 calc R . .
H29B H 0.4917 0.0930 0.0879 0.069 Uiso 1 1 calc R . .
H29C H 0.5498 0.1293 0.0073 0.069 Uiso 1 1 calc R . .
C30 C 0.6518(5) -0.0622(4) 0.0882(3) 0.0471(14) Uani 1 1 d . . .
H30A H 0.5856 -0.0878 0.1214 0.071 Uiso 1 1 calc R . .
H30B H 0.7245 -0.1083 0.1051 0.071 Uiso 1 1 calc R . .
H30C H 0.6322 -0.0613 0.0380 0.071 Uiso 1 1 calc R . .
C31 C 1.0161(5) 0.3685(4) 0.2393(3) 0.0378(12) Uani 1 1 d . . .
H31 H 1.0016 0.3133 0.2164 0.045 Uiso 1 1 calc R . .
C32 C 1.1395(5) 0.3406(5) 0.2754(4) 0.0584(17) Uani 1 1 d . . .
H32A H 1.1583 0.3949 0.2966 0.088 Uiso 1 1 calc R . .
H32B H 1.1995 0.3353 0.2381 0.088 Uiso 1 1 calc R . .
H32C H 1.1400 0.2737 0.3145 0.088 Uiso 1 1 calc R . .
C33 C 1.0165(6) 0.4703(5) 0.1775(4) 0.0649(19) Uani 1 1 d . . .
H33A H 0.9389 0.4860 0.1523 0.097 Uiso 1 1 calc R . .
H33B H 1.0796 0.4644 0.1421 0.097 Uiso 1 1 calc R . .
H33C H 1.0312 0.5263 0.1979 0.097 Uiso 1 1 calc R . .
C34 C 0.5969(5) 0.2836(5) 0.3371(3) 0.0495(15) Uani 1 1 d . . .
H34 H 0.6122 0.2327 0.3087 0.059 Uiso 1 1 calc R . .
C35 C 0.4976(6) 0.3638(6) 0.2973(4) 0.073(2) Uani 1 1 d . . .
H35A H 0.4912 0.4224 0.3176 0.110 Uiso 1 1 calc R . .
H35B H 0.4217 0.3315 0.3041 0.110 Uiso 1 1 calc R . .
H35C H 0.5162 0.3890 0.2444 0.110 Uiso 1 1 calc R . .
C36 C 0.5537(6) 0.2235(5) 0.4139(4) 0.0661(19) Uani 1 1 d . . .
H36A H 0.6169 0.1712 0.4393 0.099 Uiso 1 1 calc R . .
H36B H 0.4826 0.1889 0.4091 0.099 Uiso 1 1 calc R . .
H36C H 0.5337 0.2720 0.4424 0.099 Uiso 1 1 calc R . .
C37 C 0.7784(4) -0.1163(4) 0.2761(3) 0.0305(11) Uani 1 1 d . . .
C38 C 0.8882(5) -0.1392(4) 0.2471(3) 0.0354(12) Uani 1 1 d . . .
H38 H 0.9485 -0.0921 0.2397 0.043 Uiso 1 1 calc R . .
C39 C 0.9102(5) -0.2308(4) 0.2286(3) 0.0451(14) Uani 1 1 d . . .
H39 H 0.9851 -0.2457 0.2081 0.054 Uiso 1 1 calc R . .
C40 C 0.8240(6) -0.2998(4) 0.2401(3) 0.0524(15) Uani 1 1 d . . .
H40 H 0.8402 -0.3635 0.2290 0.063 Uiso 1 1 calc R . .
C41 C 0.7148(6) -0.2772(5) 0.2674(3) 0.0540(16) Uani 1 1 d . . .
H41 H 0.6547 -0.3244 0.2738 0.065 Uiso 1 1 calc R . .
C42 C 0.6910(5) -0.1857(4) 0.2859(3) 0.0431(13) Uani 1 1 d . . .
H42 H 0.6150 -0.1708 0.3052 0.052 Uiso 1 1 calc R . .
C43 C 0.8100(4) -0.0439(4) 0.4004(3) 0.0310(11) Uani 1 1 d . . .
C44 C 0.8343(5) -0.1481(4) 0.4400(3) 0.0480(14) Uani 1 1 d . . .
H44 H 0.8254 -0.2001 0.4169 0.058 Uiso 1 1 calc R . .
C45 C 0.8719(6) -0.1771(5) 0.5133(3) 0.0646(18) Uani 1 1 d . . .
H45 H 0.8903 -0.2485 0.5398 0.078 Uiso 1 1 calc R . .
C46 C 0.8821(6) -0.1015(6) 0.5472(3) 0.0598(18) Uani 1 1 d . . .
H46 H 0.9054 -0.1211 0.5976 0.072 Uiso 1 1 calc R . .
C47 C 0.8588(5) 0.0008(5) 0.5087(3) 0.0493(15) Uani 1 1 d . . .
H47 H 0.8672 0.0523 0.5324 0.059 Uiso 1 1 calc R . .
C48 C 0.8231(4) 0.0310(4) 0.4354(3) 0.0373(12) Uani 1 1 d . . .
H48 H 0.8075 0.1028 0.4091 0.045 Uiso 1 1 calc R . .
C49 C 0.5956(4) 0.0214(4) 0.3149(3) 0.0319(11) Uani 1 1 d . . .
C50 C 0.5355(5) -0.0281(5) 0.3781(3) 0.0467(14) Uani 1 1 d . . .
H50 H 0.5781 -0.0751 0.4191 0.056 Uiso 1 1 calc R . .
C51 C 0.4124(6) -0.0091(6) 0.3819(4) 0.0641(18) Uani 1 1 d . . .
H51 H 0.3708 -0.0431 0.4255 0.077 Uiso 1 1 calc R . .
C52 C 0.3509(5) 0.0585(6) 0.3228(4) 0.068(2) Uani 1 1 d . . .
H52 H 0.2667 0.0713 0.3256 0.081 Uiso 1 1 calc R . .
C53 C 0.4100(5) 0.1076(5) 0.2602(4) 0.0564(17) Uani 1 1 d . . .
H53 H 0.3666 0.1538 0.2192 0.068 Uiso 1 1 calc R . .
C54 C 0.5328(5) 0.0906(4) 0.2557(3) 0.0419(13) Uani 1 1 d . . .
H54 H 0.5739 0.1262 0.2123 0.050 Uiso 1 1 calc R . .
C60 C 0.1231(16) 0.7287(14) 0.3848(10) 0.236(8) Uiso 1 1 d . . .
H60A H 0.0917 0.6608 0.3930 0.354 Uiso 1 1 calc R . .
H60B H 0.0566 0.7827 0.3777 0.354 Uiso 1 1 calc R . .
H60C H 0.1703 0.7272 0.4278 0.354 Uiso 1 1 calc R . .
C61 C 0.1982(7) 0.7515(7) 0.3196(4) 0.125(4) Uiso 1 1 d G . .
C62 C 0.2128(7) 0.6577(6) 0.3036(5) 0.148(4) Uiso 1 1 d G . .
H62 H 0.1724 0.5999 0.3321 0.177 Uiso 1 1 calc R . .
C63 C 0.2866(8) 0.6484(6) 0.2458(5) 0.170(5) Uiso 1 1 d G . .
H63 H 0.2966 0.5842 0.2348 0.204 Uiso 1 1 calc R . .
C64 C 0.3458(7) 0.7329(8) 0.2040(4) 0.166(5) Uiso 1 1 d G . .
H64 H 0.3962 0.7266 0.1645 0.200 Uiso 1 1 calc R . .
C65 C 0.3312(8) 0.8268(7) 0.2201(5) 0.175(6) Uiso 1 1 d G . .
H65 H 0.3716 0.8846 0.1915 0.210 Uiso 1 1 calc R . .
C66 C 0.2574(8) 0.8361(5) 0.2779(5) 0.147(4) Uiso 1 1 d G . .
H66 H 0.2474 0.9002 0.2889 0.176 Uiso 1 1 calc R . .
Cl1 Cl 1.04155(11) 0.07870(10) 0.26596(7) 0.0401(3) Uani 1 1 d . . .
N1 N 0.8153(3) 0.1930(3) 0.1279(2) 0.0248(8) Uani 1 1 d . . .
N2 N 0.7953(3) 0.2787(3) 0.2332(2) 0.0244(8) Uani 1 1 d . . .
Ni1 Ni 0.85364(5) 0.13752(4) 0.23331(3) 0.02491(17) Uani 1 1 d . . .
P1 P 0.75798(11) 0.00060(9) 0.30544(7) 0.0266(3) Uani 1 1 d . . .
C67 C 0.5689(8) 0.4599(7) 0.5534(5) 0.088(2) Uiso 1 1 d D . .
C68 C 0.6113(12) 0.5356(11) 0.5236(8) 0.059(3) Uiso 0.50 1 d P . .
C69 C 0.3940(13) 0.3769(11) 0.5347(8) 0.158(5) Uiso 1 1 d D . .
C70 C 0.4994(14) 0.3847(13) 0.5709(10) 0.091(5) Uiso 0.50 1 d PD . .
C71 C 0.4610(14) 0.4436(13) 0.5189(9) 0.085(5) Uiso 0.50 1 d PD . .


_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
C1 N1 1.318(6) . ?
C1 C12 1.458(6) . ?
C1 C2 1.468(6) . ?
C2 C3 1.366(7) . ?
C2 C7 1.431(6) . ?
C3 C4 1.410(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.359(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.412(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(7) . ?
C6 C8 1.421(7) . ?
C7 C11 1.406(7) . ?
C8 C9 1.373(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.402(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.474(6) . ?
C12 N2 1.309(6) . ?
C13 C18 1.408(6) . ?
C13 C14 1.399(7) . ?
C13 N1 1.443(5) . ?
C14 C15 1.397(7) . ?
C14 C25 1.525(7) . ?
C15 C16 1.373(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(7) . ?
C17 H17 0.9500 . ?
C18 C28 1.513(7) . ?
C19 C24 1.399(7) . ?
C19 C20 1.406(7) . ?
C19 N2 1.446(6) . ?
C20 C21 1.391(7) . ?
C20 C31 1.512(7) . ?
C21 C22 1.368(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.371(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.403(7) . ?
C23 H23 0.9500 . ?
C24 C34 1.516(8) . ?
C25 C26 1.512(7) . ?
C25 C27 1.529(7) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.522(7) . ?
C28 C30 1.533(7) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.513(8) . ?
C31 C32 1.528(8) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.524(9) . ?
C34 C36 1.528(8) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.388(7) . ?
C37 C42 1.388(7) . ?
C37 P1 1.826(5) . ?
C38 C39 1.389(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.371(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.367(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.390(7) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.386(7) . ?
C43 C48 1.392(7) . ?
C43 P1 1.813(5) . ?
C44 C45 1.394(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.378(9) . ?
C45 H45 0.9500 . ?
C46 C47 1.359(9) . ?
C46 H46 0.9500 . ?
C47 C48 1.385(7) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.376(7) . ?
C49 C54 1.386(7) . ?
C49 P1 1.834(5) . ?
C50 C51 1.388(8) . ?
C50 H50 0.9500 . ?
C51 C52 1.370(10) . ?
C51 H51 0.9500 . ?
C52 C53 1.361(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.384(8) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C60 C61 1.450(17) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C62 C63 1.3900 . ?
C62 H62 0.9500 . ?
C63 C64 1.3900 . ?
C63 H63 0.9500 . ?
C64 C65 1.3900 . ?
C64 H64 0.9500 . ?
C65 C66 1.3900 . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
Cl1 Ni1 2.2237(13) . ?
N1 Ni1 1.957(4) . ?
N2 Ni1 1.965(3) . ?
Ni1 P1 2.2775(14) . ?
C67 C68 1.146(14) . ?
C67 C70 1.295(14) . ?
C67 C71 1.457(14) . ?
C67 C71 1.598(19) 2_666 ?
C68 C71 1.117(18) 2_666 ?
C68 C69 1.350(18) 2_666 ?
C69 C71 1.189(19) . ?
C69 C68 1.350(18) 2_666 ?
C69 C70 1.411(15) . ?
C70 C71 1.13(2) . ?
C71 C68 1.117(18) 2_666 ?
C71 C67 1.598(19) 2_666 ?
C71 C71 1.77(3) 2_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C12 115.6(4) . . ?
N1 C1 C2 135.6(4) . . ?
C12 C1 C2 108.4(4) . . ?
C3 C2 C7 117.9(4) . . ?
C3 C2 C1 137.0(4) . . ?
C7 C2 C1 105.1(4) . . ?
C2 C3 C4 119.0(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 122.6(5) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C4 C5 C6 120.4(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 116.5(5) . . ?
C7 C6 C8 116.1(5) . . ?
C5 C6 C8 127.4(5) . . ?
C6 C7 C11 123.6(4) . . ?
C6 C7 C2 123.4(5) . . ?
C11 C7 C2 113.0(4) . . ?
C9 C8 C6 120.7(5) . . ?
C9 C8 H8 119.6 . . ?
C6 C8 H8 119.6 . . ?
C8 C9 C10 122.1(5) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
C11 C10 C9 118.4(5) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C10 C11 C7 119.1(4) . . ?
C10 C11 C12 134.8(5) . . ?
C7 C11 C12 106.0(4) . . ?
N2 C12 C1 115.9(4) . . ?
N2 C12 C11 136.3(4) . . ?
C1 C12 C11 107.5(4) . . ?
C18 C13 C14 121.6(4) . . ?
C18 C13 N1 120.4(4) . . ?
C14 C13 N1 118.0(4) . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 C25 119.5(4) . . ?
C13 C14 C25 122.4(4) . . ?
C16 C15 C14 120.9(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 120.2(5) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C18 121.4(5) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C13 117.5(5) . . ?
C17 C18 C28 121.8(4) . . ?
C13 C18 C28 120.7(4) . . ?
C24 C19 C20 122.3(4) . . ?
C24 C19 N2 120.6(4) . . ?
C20 C19 N2 117.1(4) . . ?
C21 C20 C19 117.2(5) . . ?
C21 C20 C31 120.3(5) . . ?
C19 C20 C31 122.4(4) . . ?
C22 C21 C20 121.8(5) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C23 C22 C21 120.1(5) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 121.5(5) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C19 C24 C23 117.0(5) . . ?
C19 C24 C34 122.6(5) . . ?
C23 C24 C34 120.4(5) . . ?
C26 C25 C27 110.9(4) . . ?
C26 C25 C14 111.3(4) . . ?
C27 C25 C14 111.3(4) . . ?
C26 C25 H25 107.7 . . ?
C27 C25 H25 107.7 . . ?
C14 C25 H25 107.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C18 C28 C29 111.1(4) . . ?
C18 C28 C30 112.7(4) . . ?
C29 C28 C30 110.2(4) . . ?
C18 C28 H28 107.6 . . ?
C29 C28 H28 107.6 . . ?
C30 C28 H28 107.6 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C20 C31 C33 111.6(5) . . ?
C20 C31 C32 113.9(4) . . ?
C33 C31 C32 109.4(5) . . ?
C20 C31 H31 107.2 . . ?
C33 C31 H31 107.2 . . ?
C32 C31 H31 107.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C24 112.3(5) . . ?
C35 C34 C36 109.4(5) . . ?
C24 C34 C36 113.0(5) . . ?
C35 C34 H34 107.3 . . ?
C24 C34 H34 107.3 . . ?
C36 C34 H34 107.3 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C42 119.1(4) . . ?
C38 C37 P1 118.4(4) . . ?
C42 C37 P1 122.4(4) . . ?
C37 C38 C39 120.3(5) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C40 C39 C38 120.0(5) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C41 120.2(5) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 H40 119.9 . . ?
C40 C41 C42 120.5(5) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C37 C42 C41 119.8(5) . . ?
C37 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C44 C43 C48 118.7(5) . . ?
C44 C43 P1 123.5(4) . . ?
C48 C43 P1 117.8(4) . . ?
C43 C44 C45 120.6(5) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C46 C45 C44 119.6(6) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C47 C46 C45 120.3(6) . . ?
C47 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C46 C47 C48 120.8(6) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C47 C48 C43 120.0(5) . . ?
C47 C48 H48 120.0 . . ?
C43 C48 H48 120.0 . . ?
C50 C49 C54 119.7(5) . . ?
C50 C49 P1 122.6(4) . . ?
C54 C49 P1 117.8(4) . . ?
C49 C50 C51 119.8(6) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C52 C51 C50 120.1(6) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C53 C52 C51 120.3(6) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C52 C53 C54 120.5(6) . . ?
C52 C53 H53 119.8 . . ?
C54 C53 H53 119.8 . . ?
C53 C54 C49 119.6(5) . . ?
C53 C54 H54 120.2 . . ?
C49 C54 H54 120.2 . . ?
C61 C60 H60A 109.4 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 C60 103.7(10) . . ?
C66 C61 C60 136.2(10) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C64 C63 C62 120.0 . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C65 C64 C63 120.0 . . ?
C65 C64 H64 120.0 . . ?
C63 C64 H64 120.0 . . ?
C64 C65 C66 120.0 . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C66 C61 120.0 . . ?
C65 C66 H66 120.0 . . ?
C61 C66 H66 120.0 . . ?
C1 N1 C13 116.1(4) . . ?
C1 N1 Ni1 112.6(3) . . ?
C13 N1 Ni1 130.3(3) . . ?
C12 N2 C19 117.8(4) . . ?
C12 N2 Ni1 112.5(3) . . ?
C19 N2 Ni1 129.2(3) . . ?
N1 Ni1 N2 83.04(15) . . ?
N1 Ni1 Cl1 118.33(11) . . ?
N2 Ni1 Cl1 119.53(11) . . ?
N1 Ni1 P1 119.36(11) . . ?
N2 Ni1 P1 118.45(11) . . ?
Cl1 Ni1 P1 99.54(5) . . ?
C43 P1 C49 103.2(2) . . ?
C43 P1 C37 103.6(2) . . ?
C49 P1 C37 104.1(2) . . ?
C43 P1 Ni1 113.11(16) . . ?
C49 P1 Ni1 117.11(17) . . ?
C37 P1 Ni1 114.21(16) . . ?
C68 C67 C70 163.1(14) . . ?
C68 C67 C71 115.1(12) . . ?
C70 C67 C71 48.1(10) . . ?
C68 C67 C71 44.3(9) . 2_666 ?
C70 C67 C71 118.8(12) . 2_666 ?
C71 C67 C71 70.7(12) . 2_666 ?
C71 C68 C67 89.9(14) 2_666 . ?
C71 C68 C69 56.7(12) 2_666 2_666 ?
C67 C68 C69 146.6(15) . 2_666 ?
C71 C69 C68 51.7(11) . 2_666 ?
C71 C69 C70 50.6(11) . . ?
C68 C69 C70 102.4(14) 2_666 . ?
C71 C70 C67 73.5(12) . . ?
C71 C70 C69 54.4(11) . . ?
C67 C70 C69 127.9(15) . . ?
C68 C71 C70 146.5(19) 2_666 . ?
C68 C71 C69 71.6(13) 2_666 . ?
C70 C71 C69 74.9(13) . . ?
C68 C71 C67 155.1(18) 2_666 . ?
C70 C71 C67 58.4(10) . . ?
C69 C71 C67 133.3(16) . . ?
C68 C71 C67 45.8(10) 2_666 2_666 ?
C70 C71 C67 167.7(16) . 2_666 ?
C69 C71 C67 117.4(14) . 2_666 ?
C67 C71 C67 109.3(12) . 2_666 ?
C68 C71 C71 96.7(17) 2_666 2_666 ?
C70 C71 C71 116.8(16) . 2_666 ?
C69 C71 C71 168(2) . 2_666 ?
C67 C71 C71 58.4(9) . 2_666 ?
C67 C71 C71 50.9(9) 2_666 2_666 ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.087
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Complex_4
_database_code_depnum_ccdc_archive 'CCDC 1044664'
_audit_update_record             
;
2015-01-21 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H46 Al Br2 N2 Ni'
_chemical_formula_weight         776.28

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'
Al Al 0.0645 0.0514 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   13.7598(11)
_cell_length_b                   18.9444(15)
_cell_length_c                   14.2281(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3708.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    4531
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.98

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5980
_exptl_absorpt_correction_T_max  0.6850
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(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 scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22125
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.04
_reflns_number_total             3661
_reflns_number_gt                2837
_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)+(0.0503P)²+0.8671P] 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         3661
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Al1 Al 0.5000 0.15060(6) 0.2500 0.0348(3) Uani 1 2 d S . .
C1 C 0.44935(17) 0.46808(13) 0.23208(16) 0.0222(5) Uani 1 1 d . . .
C2 C 0.42019(19) 0.54167(13) 0.21813(17) 0.0250(6) Uani 1 1 d . . .
C3 C 0.3395(2) 0.57561(15) 0.18307(19) 0.0321(6) Uani 1 1 d . . .
H3 H 0.2854 0.5495 0.1603 0.038 Uiso 1 1 calc R . .
C4 C 0.3390(2) 0.64988(16) 0.1818(2) 0.0401(7) Uani 1 1 d . . .
H4 H 0.2835 0.6735 0.1576 0.048 Uiso 1 1 calc R . .
C5 C 0.4157(2) 0.68960(15) 0.2144(2) 0.0389(7) Uani 1 1 d . . .
H5 H 0.4118 0.7397 0.2129 0.047 Uiso 1 1 calc R . .
C6 C 0.5000 0.65676(19) 0.2500 0.0313(9) Uani 1 2 d S . .
C7 C 0.5000 0.58287(19) 0.2500 0.0268(8) Uani 1 2 d S . .
C8 C 0.31111(18) 0.39928(13) 0.19002(18) 0.0256(6) Uani 1 1 d . . .
C9 C 0.23376(18) 0.41873(13) 0.24894(19) 0.0298(6) Uani 1 1 d . . .
C10 C 0.1400(2) 0.40735(17) 0.2143(2) 0.0409(7) Uani 1 1 d . . .
H10 H 0.0857 0.4202 0.2519 0.049 Uiso 1 1 calc R . .
C11 C 0.1244(2) 0.37804(17) 0.1271(3) 0.0476(8) Uani 1 1 d . . .
H11 H 0.0599 0.3717 0.1050 0.057 Uiso 1 1 calc R . .
C12 C 0.2015(2) 0.35780(15) 0.0718(2) 0.0401(7) Uani 1 1 d . . .
H12 H 0.1895 0.3371 0.0121 0.048 Uiso 1 1 calc R . .
C13 C 0.29691(18) 0.36721(13) 0.10188(19) 0.0289(6) Uani 1 1 d . . .
C14 C 0.2485(2) 0.44697(15) 0.3473(2) 0.0363(7) Uani 1 1 d . . .
H14 H 0.3156 0.4672 0.3507 0.044 Uiso 1 1 calc R . .
C15 C 0.2423(4) 0.3874(2) 0.4183(2) 0.0866(15) Uani 1 1 d . . .
H15A H 0.1777 0.3657 0.4150 0.130 Uiso 1 1 calc R . .
H15B H 0.2531 0.4062 0.4816 0.130 Uiso 1 1 calc R . .
H15C H 0.2919 0.3519 0.4041 0.130 Uiso 1 1 calc R . .
C16 C 0.1779(3) 0.5046(2) 0.3746(3) 0.0687(11) Uani 1 1 d . . .
H16A H 0.1931 0.5214 0.4380 0.103 Uiso 1 1 calc R . .
H16B H 0.1115 0.4859 0.3734 0.103 Uiso 1 1 calc R . .
H16C H 0.1832 0.5439 0.3300 0.103 Uiso 1 1 calc R . .
C17 C 0.3839(2) 0.34686(15) 0.04275(19) 0.0349(7) Uani 1 1 d . . .
H17 H 0.4357 0.3308 0.0871 0.042 Uiso 1 1 calc R . .
C18 C 0.4246(3) 0.41004(17) -0.0106(2) 0.0525(9) Uani 1 1 d . . .
H18A H 0.4851 0.3964 -0.0422 0.079 Uiso 1 1 calc R . .
H18B H 0.4378 0.4486 0.0336 0.079 Uiso 1 1 calc R . .
H18C H 0.3772 0.4258 -0.0575 0.079 Uiso 1 1 calc R . .
C19 C 0.3640(3) 0.2854(2) -0.0246(3) 0.0602(10) Uani 1 1 d . . .
H19A H 0.3207 0.3012 -0.0750 0.090 Uiso 1 1 calc R . .
H19B H 0.3331 0.2466 0.0100 0.090 Uiso 1 1 calc R . .
H19C H 0.4254 0.2689 -0.0517 0.090 Uiso 1 1 calc R . .
C20 C 0.4459(2) 0.10353(17) 0.1402(2) 0.0512(8) Uani 1 1 d . . .
H20A H 0.4987 0.0843 0.1019 0.077 Uiso 1 1 calc R . .
H20B H 0.4085 0.1375 0.1030 0.077 Uiso 1 1 calc R . .
H20C H 0.4031 0.0651 0.1606 0.077 Uiso 1 1 calc R . .
Br1 Br 0.38304(2) 0.236566(16) 0.30327(2) 0.04251(12) Uani 1 1 d . . .
N1 N 0.40956(14) 0.40649(11) 0.22169(14) 0.0227(5) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.32845(2) 0.2500 0.02578(14) Uani 1 2 d S . .


_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
Al1 C20 1.947(3) . ?
Al1 C20 1.947(3) 4_655 ?
Al1 Br1 2.4118(8) 4_655 ?
Al1 Br1 2.4118(8) . ?
C1 N1 1.297(3) . ?
C1 C2 1.464(3) . ?
C1 C1 1.484(5) 4_655 ?
C2 C3 1.377(4) . ?
C2 C7 1.421(3) . ?
C3 C4 1.407(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.410(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.400(5) . ?
C6 C5 1.410(3) 4_655 ?
C7 C2 1.421(3) 4_655 ?
C8 C9 1.404(3) . ?
C8 C13 1.407(4) . ?
C8 N1 1.434(3) . ?
C9 C10 1.397(4) . ?
C9 C14 1.512(4) . ?
C10 C11 1.376(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.513(4) . ?
C14 C16 1.513(4) . ?
C14 C15 1.517(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.524(4) . ?
C17 C19 1.533(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Br1 Ni1 2.4889(4) . ?
N1 Ni1 1.974(2) . ?
Ni1 N1 1.974(2) 4_655 ?
Ni1 Br1 2.4889(4) 4_655 ?

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
C20 Al1 C20 125.5(2) . 4_655 ?
C20 Al1 Br1 108.21(11) . 4_655 ?
C20 Al1 Br1 107.82(10) 4_655 4_655 ?
C20 Al1 Br1 107.82(10) . . ?
C20 Al1 Br1 108.21(11) 4_655 . ?
Br1 Al1 Br1 95.05(4) 4_655 . ?
N1 C1 C2 136.5(2) . . ?
N1 C1 C1 115.82(14) . 4_655 ?
C2 C1 C1 107.69(14) . 4_655 ?
C3 C2 C7 118.8(3) . . ?
C3 C2 C1 135.6(2) . . ?
C7 C2 C1 105.5(2) . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 122.6(3) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 116.18(19) . . ?
C7 C6 C5 116.18(19) . 4_655 ?
C5 C6 C5 127.6(4) . 4_655 ?
C6 C7 C2 123.30(16) . . ?
C6 C7 C2 123.30(16) . 4_655 ?
C2 C7 C2 113.4(3) . 4_655 ?
C9 C8 C13 122.7(2) . . ?
C9 C8 N1 120.2(2) . . ?
C13 C8 N1 116.9(2) . . ?
C10 C9 C8 116.7(3) . . ?
C10 C9 C14 120.3(2) . . ?
C8 C9 C14 122.9(2) . . ?
C11 C10 C9 121.6(3) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 117.4(3) . . ?
C12 C13 C17 122.8(2) . . ?
C8 C13 C17 119.7(2) . . ?
C9 C14 C16 114.0(3) . . ?
C9 C14 C15 110.2(3) . . ?
C16 C14 C15 109.2(3) . . ?
C9 C14 H14 107.7 . . ?
C16 C14 H14 107.7 . . ?
C15 C14 H14 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C18 111.6(2) . . ?
C13 C17 C19 113.6(2) . . ?
C18 C17 C19 110.6(3) . . ?
C13 C17 H17 106.9 . . ?
C18 C17 H17 106.9 . . ?
C19 C17 H17 106.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Al1 C20 H20A 109.5 . . ?
Al1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Al1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Al1 Br1 Ni1 86.85(2) . . ?
C1 N1 C8 121.3(2) . . ?
C1 N1 Ni1 112.60(16) . . ?
C8 N1 Ni1 126.03(16) . . ?
N1 Ni1 N1 83.00(12) 4_655 . ?
N1 Ni1 Br1 100.27(6) 4_655 4_655 ?
N1 Ni1 Br1 150.38(6) . 4_655 ?
N1 Ni1 Br1 150.38(6) 4_655 . ?
N1 Ni1 Br1 100.27(6) . . ?
Br1 Ni1 Br1 91.24(2) 4_655 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.075


