# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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
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data_cyw0116-2_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H54 Cl10 N16 Ni5 O2, 2(C2 H8 N)'
_chemical_formula_sum            'C62 H70 Cl10 N18 Ni5 O2'
_chemical_formula_weight         1747.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   15.7038(12)
_cell_length_b                   9.9564(7)
_cell_length_c                   23.8274(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4680(10)
_cell_angle_gamma                90.00
_cell_volume                     3718.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5211
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      26.79

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1788
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26250
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         27.14
_reflns_number_total             8215
_reflns_number_gt                6016
_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 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. 

The hydrogen atoms of the hydroxyl groups were located on the difference Fourier maps

Check-cif alerts

420_ALERT_2_B D-H Without Acceptor O1 - H1' ?

No suitable acceptors were found at reasonable orientation

;

_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^)+(0.0409P)^2^+1.8268P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8215
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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 1.0000 0.0000 0.02262(13) Uani 1 2 d S . .
Ni2 Ni 0.26995(2) 0.98284(4) -0.002924(17) 0.02516(10) Uani 1 1 d . . .
Ni3 Ni 0.34642(2) 0.99804(4) 0.110890(17) 0.02349(10) Uani 1 1 d . . .
Cl4 Cl 0.49715(4) 0.75676(7) 0.01206(3) 0.02787(17) Uani 1 1 d . . .
Cl5 Cl 0.20665(4) 1.09378(7) 0.07739(3) 0.02857(17) Uani 1 1 d . . .
Cl6 Cl 0.28395(5) 0.79395(7) 0.06815(3) 0.02869(17) Uani 1 1 d . . .
Cl7 Cl 0.39272(5) 1.21085(7) 0.14405(3) 0.03065(18) Uani 1 1 d . . .
Cl8 Cl 0.26263(5) 1.17685(8) -0.06062(4) 0.03628(19) Uani 1 1 d . . .
N5 N 0.46260(15) 0.8839(2) 0.12644(11) 0.0259(6) Uani 1 1 d . . .
N6 N 0.33068(15) 0.8383(2) -0.05509(11) 0.0257(6) Uani 1 1 d . . .
N7 N 0.16535(16) 0.9029(3) -0.04318(12) 0.0336(6) Uani 1 1 d . . .
N1 N 0.65888(15) 1.0997(3) 0.24714(11) 0.0291(6) Uani 1 1 d . . .
N4 N 0.56249(14) 1.0263(2) 0.08864(11) 0.0238(5) Uani 1 1 d . . .
N3 N 0.56288(15) 0.9865(2) 0.18768(11) 0.0273(6) Uani 1 1 d . . .
N2 N 0.66782(15) 1.1296(2) 0.15153(11) 0.0269(6) Uani 1 1 d . . .
N8 N 0.32454(16) 0.9286(3) 0.18866(11) 0.0308(6) Uani 1 1 d . . .
C1 C 0.73246(19) 1.1892(3) 0.25966(14) 0.0314(7) Uani 1 1 d . . .
H1A H 0.7221 1.2439 0.2922 0.038 Uiso 1 1 calc R . .
H1B H 0.7392 1.2488 0.2280 0.038 Uiso 1 1 calc R . .
C9 C 0.8132(2) 1.1089(3) 0.27105(15) 0.0339(8) Uani 1 1 d . . .
C15 C 0.62987(18) 1.0720(3) 0.19452(13) 0.0271(7) Uani 1 1 d . . .
C25 C 0.1772(2) 0.7872(3) -0.07055(14) 0.0326(7) Uani 1 1 d . . .
C17 C 0.63144(18) 1.1039(3) 0.10137(13) 0.0238(6) Uani 1 1 d . . .
C23 C 0.2604(2) 0.9691(4) 0.21997(16) 0.0405(9) Uani 1 1 d . . .
H23 H 0.2223 1.0339 0.2056 0.049 Uiso 1 1 calc R . .
C16 C 0.53308(18) 0.9688(3) 0.13523(13) 0.0241(6) Uani 1 1 d . . .
C19 C 0.3794(2) 0.8367(3) 0.20993(14) 0.0320(7) Uani 1 1 d . . .
C18 C 0.4465(2) 0.7883(3) 0.17196(14) 0.0308(7) Uani 1 1 d . . .
H18A H 0.4993 0.7730 0.1943 0.037 Uiso 1 1 calc R . .
H18B H 0.4284 0.7031 0.1555 0.037 Uiso 1 1 calc R . .
C24 C 0.26617(19) 0.7331(3) -0.06753(14) 0.0311(7) Uani 1 1 d . . .
H24A H 0.2715 0.6646 -0.0386 0.037 Uiso 1 1 calc R . .
H24B H 0.2771 0.6910 -0.1031 0.037 Uiso 1 1 calc R . .
C2 C 0.6255(2) 1.0298(3) 0.29514(14) 0.0341(8) Uani 1 1 d . . .
H2A H 0.6724 1.0115 0.3224 0.041 Uiso 1 1 calc R . .
H2B H 0.6021 0.9442 0.2824 0.041 Uiso 1 1 calc R . .
C22 C 0.2498(3) 0.9169(4) 0.27271(16) 0.0513(10) Uani 1 1 d . . .
H22 H 0.2047 0.9452 0.2933 0.062 Uiso 1 1 calc R . .
C28 C 0.0183(2) 0.9008(5) -0.07347(19) 0.0616(12) Uani 1 1 d . . .
H28 H -0.0346 0.9430 -0.0750 0.074 Uiso 1 1 calc R . .
C4 C 0.4783(2) 1.1316(4) 0.29711(17) 0.0470(9) Uani 1 1 d . . .
H4 H 0.4674 1.1047 0.2600 0.056 Uiso 1 1 calc R . .
C20 C 0.3725(2) 0.7824(4) 0.26279(16) 0.0450(9) Uani 1 1 d . . .
H20 H 0.4119 0.7192 0.2768 0.054 Uiso 1 1 calc R . .
C5 C 0.4155(3) 1.1965(4) 0.3251(2) 0.0593(12) Uani 1 1 d . . .
H5 H 0.3627 1.2128 0.3066 0.071 Uiso 1 1 calc R . .
C14 C 0.8527(2) 1.0481(4) 0.22663(18) 0.0457(9) Uani 1 1 d . . .
H14 H 0.8308 1.0625 0.1900 0.055 Uiso 1 1 calc R . .
C21 C 0.3068(3) 0.8226(4) 0.29455(17) 0.0546(11) Uani 1 1 d . . .
H21 H 0.3009 0.7867 0.3301 0.066 Uiso 1 1 calc R . .
C13 C 0.9233(3) 0.9675(4) 0.2358(2) 0.0623(13) Uani 1 1 d . . .
H13 H 0.9494 0.9289 0.2057 0.075 Uiso 1 1 calc R . .
C29 C 0.0874(2) 0.9579(4) -0.04542(17) 0.0492(10) Uani 1 1 d . . .
H29 H 0.0800 1.0390 -0.0270 0.059 Uiso 1 1 calc R . .
C26 C 0.1092(2) 0.7225(4) -0.09847(16) 0.0496(10) Uani 1 1 d . . .
H26 H 0.1176 0.6411 -0.1165 0.060 Uiso 1 1 calc R . .
C3 C 0.5572(2) 1.1066(3) 0.32403(15) 0.0364(8) Uani 1 1 d . . .
C12 C 0.9547(3) 0.9447(4) 0.2898(2) 0.0662(14) Uani 1 1 d . . .
H12 H 1.0017 0.8887 0.2961 0.079 Uiso 1 1 calc R . .
C10 C 0.8476(2) 1.0890(4) 0.32548(17) 0.0503(10) Uani 1 1 d . . .
H10 H 0.8241 1.1321 0.3555 0.060 Uiso 1 1 calc R . .
C6 C 0.4303(3) 1.2367(5) 0.3796(2) 0.0741(15) Uani 1 1 d . . .
H6 H 0.3881 1.2816 0.3980 0.089 Uiso 1 1 calc R . .
C8 C 0.5723(3) 1.1476(4) 0.37947(18) 0.0544(11) Uani 1 1 d . . .
H8 H 0.6253 1.1329 0.3980 0.065 Uiso 1 1 calc R . .
C7 C 0.5078(3) 1.2106(5) 0.4072(2) 0.0759(15) Uani 1 1 d . . .
H7 H 0.5174 1.2352 0.4447 0.091 Uiso 1 1 calc R . .
C27 C 0.0288(2) 0.7792(5) -0.09953(18) 0.0627(13) Uani 1 1 d . . .
H27 H -0.0175 0.7357 -0.1176 0.075 Uiso 1 1 calc R . .
C11 C 0.9182(3) 1.0029(5) 0.3348(2) 0.0670(15) Uani 1 1 d . . .
H11 H 0.9400 0.9855 0.3713 0.080 Uiso 1 1 calc R . .
O1 O 0.38437(13) 1.0347(2) 0.03252(9) 0.0228(5) Uani 1 1 d . . .
N9 N 0.29595(18) 0.3747(3) 0.04391(13) 0.0449(8) Uiso 1 1 d . . .
H9A H 0.3058 0.3235 0.0747 0.054 Uiso 1 1 calc R . .
H9B H 0.2953 0.3202 0.0138 0.054 Uiso 1 1 calc R . .
C33 C 0.3666(3) 0.4699(4) 0.04053(19) 0.0590(11) Uiso 1 1 d . . .
H33A H 0.3668 0.5053 0.0030 0.089 Uiso 1 1 calc R . .
H33B H 0.4196 0.4248 0.0498 0.089 Uiso 1 1 calc R . .
H33C H 0.3596 0.5422 0.0665 0.089 Uiso 1 1 calc R . .
C34 C 0.2113(3) 0.4371(4) 0.04629(19) 0.0599(11) Uiso 1 1 d . . .
H34A H 0.2118 0.4984 0.0774 0.090 Uiso 1 1 calc R . .
H34B H 0.1693 0.3686 0.0511 0.090 Uiso 1 1 calc R . .
H34C H 0.1976 0.4849 0.0119 0.090 Uiso 1 1 calc R . .
H1 H 0.386(2) 1.103(3) 0.0270(15) 0.031(11) Uiso 1 1 d . . .

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 0.0167(3) 0.0219(3) 0.0299(3) -0.0003(2) 0.0071(2) -0.0004(2)
Ni2 0.01653(19) 0.0274(2) 0.0319(2) -0.00294(16) 0.00417(16) -0.00192(15)
Ni3 0.01844(19) 0.0246(2) 0.0281(2) -0.00066(15) 0.00648(15) -0.00185(15)
Cl4 0.0245(4) 0.0226(4) 0.0372(5) -0.0001(3) 0.0081(3) 0.0001(3)
Cl5 0.0180(3) 0.0305(4) 0.0378(5) -0.0053(3) 0.0060(3) 0.0006(3)
Cl6 0.0267(4) 0.0250(4) 0.0352(4) -0.0015(3) 0.0085(3) -0.0046(3)
Cl7 0.0267(4) 0.0293(4) 0.0361(5) -0.0069(3) 0.0036(3) -0.0030(3)
Cl8 0.0313(4) 0.0363(4) 0.0409(5) 0.0051(4) -0.0006(4) 0.0029(3)
N5 0.0201(12) 0.0270(13) 0.0312(15) 0.0060(11) 0.0073(11) -0.0008(10)
N6 0.0214(13) 0.0251(13) 0.0314(15) -0.0021(10) 0.0082(11) -0.0052(10)
N7 0.0214(13) 0.0415(17) 0.0382(17) -0.0057(13) 0.0041(12) -0.0040(11)
N1 0.0200(13) 0.0394(15) 0.0278(15) 0.0020(11) 0.0016(11) -0.0033(11)
N4 0.0171(12) 0.0222(13) 0.0326(15) 0.0003(10) 0.0059(10) 0.0014(9)
N3 0.0197(13) 0.0299(14) 0.0326(16) 0.0029(11) 0.0041(11) 0.0001(10)
N2 0.0226(13) 0.0294(14) 0.0290(15) 0.0010(11) 0.0043(11) -0.0002(10)
N8 0.0265(14) 0.0318(15) 0.0350(16) 0.0001(12) 0.0097(12) -0.0059(11)
C1 0.0263(16) 0.0345(18) 0.0329(19) -0.0018(14) -0.0018(14) -0.0007(13)
C9 0.0269(17) 0.0342(18) 0.040(2) 0.0021(14) 0.0013(15) -0.0076(13)
C15 0.0207(15) 0.0278(16) 0.0329(19) 0.0014(13) 0.0024(13) 0.0054(12)
C25 0.0276(17) 0.0388(19) 0.0317(19) -0.0016(14) 0.0056(14) -0.0114(14)
C17 0.0194(14) 0.0236(15) 0.0289(18) -0.0018(12) 0.0052(12) 0.0045(11)
C23 0.0356(19) 0.043(2) 0.044(2) 0.0026(16) 0.0158(17) -0.0001(15)
C16 0.0178(14) 0.0238(15) 0.0308(18) 0.0018(12) 0.0036(12) 0.0047(11)
C19 0.0275(17) 0.0315(17) 0.038(2) 0.0062(14) 0.0053(14) -0.0083(13)
C18 0.0309(17) 0.0265(16) 0.0356(19) 0.0058(13) 0.0077(14) -0.0033(13)
C24 0.0311(17) 0.0294(17) 0.0337(19) -0.0023(13) 0.0081(14) -0.0099(13)
C2 0.0281(17) 0.043(2) 0.0309(19) 0.0069(14) 0.0015(14) -0.0008(14)
C22 0.052(2) 0.058(3) 0.046(2) 0.0058(19) 0.030(2) 0.0012(19)
C28 0.0225(19) 0.097(4) 0.065(3) -0.015(3) -0.0012(19) -0.003(2)
C4 0.035(2) 0.057(2) 0.049(3) -0.0065(18) 0.0052(18) 0.0003(17)
C20 0.051(2) 0.044(2) 0.042(2) 0.0131(16) 0.0133(18) -0.0010(17)
C5 0.033(2) 0.060(3) 0.085(4) -0.013(2) 0.012(2) 0.0005(18)
C14 0.0321(19) 0.049(2) 0.055(3) -0.0037(18) -0.0007(17) 0.0023(16)
C21 0.065(3) 0.059(3) 0.043(2) 0.0168(19) 0.025(2) -0.001(2)
C13 0.036(2) 0.054(3) 0.097(4) -0.005(2) 0.003(2) 0.0080(19)
C29 0.0246(18) 0.068(3) 0.055(3) -0.012(2) 0.0010(17) 0.0037(17)
C26 0.045(2) 0.059(3) 0.045(2) -0.0164(19) 0.0030(18) -0.0207(19)
C3 0.0296(18) 0.0389(19) 0.041(2) 0.0004(15) 0.0081(15) -0.0054(14)
C12 0.036(2) 0.051(3) 0.109(4) 0.024(3) -0.008(3) 0.0027(19)
C10 0.035(2) 0.067(3) 0.047(3) 0.015(2) -0.0044(18) -0.0097(18)
C6 0.051(3) 0.068(3) 0.107(5) -0.028(3) 0.038(3) -0.005(2)
C8 0.052(2) 0.062(3) 0.049(3) -0.016(2) 0.000(2) -0.002(2)
C7 0.085(4) 0.083(4) 0.063(3) -0.036(3) 0.026(3) -0.013(3)
C27 0.027(2) 0.104(4) 0.056(3) -0.016(3) -0.0048(19) -0.022(2)
C11 0.042(2) 0.084(3) 0.072(3) 0.045(3) -0.022(2) -0.020(2)
O1 0.0193(11) 0.0215(12) 0.0281(12) -0.0005(9) 0.0053(8) -0.0002(9)

_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 O1 2.046(2) . ?
Ni1 O1 2.046(2) 3_675 ?
Ni1 N4 2.289(3) . ?
Ni1 N4 2.289(3) 3_675 ?
Ni1 Cl4 2.4395(7) 3_675 ?
Ni1 Cl4 2.4395(7) . ?
Ni2 O1 2.006(2) . ?
Ni2 N7 2.015(3) . ?
Ni2 N6 2.161(2) . ?
Ni2 Cl8 2.3696(9) . ?
Ni2 Cl5 2.4700(8) . ?
Ni2 Cl6 2.5315(9) . ?
Ni2 Ni3 2.9027(6) . ?
Ni3 N8 2.026(3) . ?
Ni3 O1 2.027(2) . ?
Ni3 N5 2.162(2) . ?
Ni3 Cl7 2.3607(8) . ?
Ni3 Cl6 2.4510(8) . ?
Ni3 Cl5 2.4802(8) . ?
N5 C16 1.398(4) . ?
N5 C18 1.477(4) . ?
N6 C17 1.407(4) 3_675 ?
N6 C24 1.475(4) . ?
N7 C29 1.339(4) . ?
N7 C25 1.342(4) . ?
N1 C15 1.336(4) . ?
N1 C2 1.463(4) . ?
N1 C1 1.476(4) . ?
N4 C17 1.350(4) . ?
N4 C16 1.355(4) . ?
N3 C16 1.319(4) . ?
N3 C15 1.356(4) . ?
N2 C17 1.318(4) . ?
N2 C15 1.344(4) . ?
N8 C19 1.336(4) . ?
N8 C23 1.351(4) . ?
C1 C9 1.509(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C9 C10 1.389(5) . ?
C9 C14 1.397(5) . ?
C25 C26 1.382(5) . ?
C25 C24 1.496(4) . ?
C17 N6 1.407(4) 3_675 ?
C23 C22 1.379(5) . ?
C23 H23 0.9300 . ?
C19 C20 1.381(5) . ?
C19 C18 1.508(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C2 C3 1.516(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C22 C21 1.377(6) . ?
C22 H22 0.9300 . ?
C28 C29 1.364(5) . ?
C28 C27 1.375(6) . ?
C28 H28 0.9300 . ?
C4 C3 1.382(5) . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
C20 C21 1.376(5) . ?
C20 H20 0.9300 . ?
C5 C6 1.366(7) . ?
C5 H5 0.9300 . ?
C14 C13 1.375(5) . ?
C14 H14 0.9300 . ?
C21 H21 0.9300 . ?
C13 C12 1.367(7) . ?
C13 H13 0.9300 . ?
C29 H29 0.9300 . ?
C26 C27 1.382(6) . ?
C26 H26 0.9300 . ?
C3 C8 1.389(5) . ?
C12 C11 1.376(7) . ?
C12 H12 0.9300 . ?
C10 C11 1.409(6) . ?
C10 H10 0.9300 . ?
C6 C7 1.373(7) . ?
C6 H6 0.9300 . ?
C8 C7 1.391(6) . ?
C8 H8 0.9300 . ?
C7 H7 0.9300 . ?
C27 H27 0.9300 . ?
C11 H11 0.9300 . ?
O1 H1 0.69(3) . ?
N9 C33 1.465(5) . ?
N9 C34 1.471(5) . ?
N9 H9A 0.9000 . ?
N9 H9B 0.9000 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

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
O1 Ni1 O1 180.00(11) . 3_675 ?
O1 Ni1 N4 88.40(8) . . ?
O1 Ni1 N4 91.60(8) 3_675 . ?
O1 Ni1 N4 91.60(8) . 3_675 ?
O1 Ni1 N4 88.40(8) 3_675 3_675 ?
N4 Ni1 N4 180.00(11) . 3_675 ?
O1 Ni1 Cl4 84.27(7) . 3_675 ?
O1 Ni1 Cl4 95.73(7) 3_675 3_675 ?
N4 Ni1 Cl4 89.15(6) . 3_675 ?
N4 Ni1 Cl4 90.85(6) 3_675 3_675 ?
O1 Ni1 Cl4 95.73(7) . . ?
O1 Ni1 Cl4 84.27(7) 3_675 . ?
N4 Ni1 Cl4 90.85(6) . . ?
N4 Ni1 Cl4 89.15(6) 3_675 . ?
Cl4 Ni1 Cl4 180.0 3_675 . ?
O1 Ni2 N7 170.23(10) . . ?
O1 Ni2 N6 89.90(9) . . ?
N7 Ni2 N6 80.71(10) . . ?
O1 Ni2 Cl8 92.60(7) . . ?
N7 Ni2 Cl8 92.08(8) . . ?
N6 Ni2 Cl8 102.53(7) . . ?
O1 Ni2 Cl5 87.19(6) . . ?
N7 Ni2 Cl5 101.00(8) . . ?
N6 Ni2 Cl5 162.90(7) . . ?
Cl8 Ni2 Cl5 94.43(3) . . ?
O1 Ni2 Cl6 82.54(7) . . ?
N7 Ni2 Cl6 93.46(8) . . ?
N6 Ni2 Cl6 82.32(7) . . ?
Cl8 Ni2 Cl6 173.18(3) . . ?
Cl5 Ni2 Cl6 80.60(3) . . ?
O1 Ni2 Ni3 44.27(6) . . ?
N7 Ni2 Ni3 138.12(8) . . ?
N6 Ni2 Ni3 113.58(7) . . ?
Cl8 Ni2 Ni3 120.16(3) . . ?
Cl5 Ni2 Ni3 54.26(2) . . ?
Cl6 Ni2 Ni3 53.09(2) . . ?
N8 Ni3 O1 168.30(10) . . ?
N8 Ni3 N5 81.50(10) . . ?
O1 Ni3 N5 87.73(9) . . ?
N8 Ni3 Cl7 93.78(8) . . ?
O1 Ni3 Cl7 92.58(7) . . ?
N5 Ni3 Cl7 100.06(7) . . ?
N8 Ni3 Cl6 90.66(8) . . ?
O1 Ni3 Cl6 84.20(7) . . ?
N5 Ni3 Cl6 87.02(7) . . ?
Cl7 Ni3 Cl6 172.13(3) . . ?
N8 Ni3 Cl5 103.27(8) . . ?
O1 Ni3 Cl5 86.46(6) . . ?
N5 Ni3 Cl5 168.03(7) . . ?
Cl7 Ni3 Cl5 90.65(3) . . ?
Cl6 Ni3 Cl5 81.99(3) . . ?
N8 Ni3 Ni2 138.86(7) . . ?
O1 Ni3 Ni2 43.69(6) . . ?
N5 Ni3 Ni2 115.46(7) . . ?
Cl7 Ni3 Ni2 117.46(3) . . ?
Cl6 Ni3 Ni2 55.67(2) . . ?
Cl5 Ni3 Ni2 53.94(2) . . ?
Ni2 Cl5 Ni3 71.80(2) . . ?
Ni3 Cl6 Ni2 71.24(2) . . ?
C16 N5 C18 116.7(3) . . ?
C16 N5 Ni3 111.10(17) . . ?
C18 N5 Ni3 106.52(17) . . ?
C17 N6 C24 116.8(2) 3_675 . ?
C17 N6 Ni2 113.60(17) 3_675 . ?
C24 N6 Ni2 105.49(17) . . ?
C29 N7 C25 119.0(3) . . ?
C29 N7 Ni2 125.0(2) . . ?
C25 N7 Ni2 116.0(2) . . ?
C15 N1 C2 121.2(3) . . ?
C15 N1 C1 122.2(3) . . ?
C2 N1 C1 116.3(3) . . ?
C17 N4 C16 111.5(3) . . ?
C17 N4 Ni1 124.5(2) . . ?
C16 N4 Ni1 124.01(19) . . ?
C16 N3 C15 115.2(3) . . ?
C17 N2 C15 114.8(3) . . ?
C19 N8 C23 118.7(3) . . ?
C19 N8 Ni3 116.1(2) . . ?
C23 N8 Ni3 125.2(2) . . ?
N1 C1 C9 110.8(3) . . ?
N1 C1 H1A 109.5 . . ?
C9 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C9 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C10 C9 C14 118.7(3) . . ?
C10 C9 C1 121.2(3) . . ?
C14 C9 C1 120.0(3) . . ?
N1 C15 N2 119.0(3) . . ?
N1 C15 N3 117.4(3) . . ?
N2 C15 N3 123.6(3) . . ?
N7 C25 C26 120.6(3) . . ?
N7 C25 C24 116.2(3) . . ?
C26 C25 C24 123.2(3) . . ?
N2 C17 N4 127.8(3) . . ?
N2 C17 N6 116.8(3) . 3_675 ?
N4 C17 N6 115.4(3) . 3_675 ?
N8 C23 C22 121.7(3) . . ?
N8 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
N3 C16 N4 126.9(3) . . ?
N3 C16 N5 117.0(3) . . ?
N4 C16 N5 116.0(3) . . ?
N8 C19 C20 122.0(3) . . ?
N8 C19 C18 116.7(3) . . ?
C20 C19 C18 121.2(3) . . ?
N5 C18 C19 113.0(2) . . ?
N5 C18 H18A 109.0 . . ?
C19 C18 H18A 109.0 . . ?
N5 C18 H18B 109.0 . . ?
C19 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
N6 C24 C25 112.5(3) . . ?
N6 C24 H24A 109.1 . . ?
C25 C24 H24A 109.1 . . ?
N6 C24 H24B 109.1 . . ?
C25 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
N1 C2 C3 114.4(3) . . ?
N1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
N1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C21 C22 C23 119.3(3) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C29 C28 C27 118.4(4) . . ?
C29 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C21 C20 C19 119.4(4) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C13 C14 C9 121.5(4) . . ?
C13 C14 H14 119.2 . . ?
C9 C14 H14 119.2 . . ?
C20 C21 C22 118.8(4) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
N7 C29 C28 123.2(4) . . ?
N7 C29 H29 118.4 . . ?
C28 C29 H29 118.4 . . ?
C25 C26 C27 119.8(4) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C4 C3 C8 119.0(3) . . ?
C4 C3 C2 121.3(3) . . ?
C8 C3 C2 119.7(3) . . ?
C13 C12 C11 121.4(4) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C9 C10 C11 119.5(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C5 C6 C7 119.6(4) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C3 C8 C7 119.8(4) . . ?
C3 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C6 C7 C8 120.5(4) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C28 C27 C26 119.0(4) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
Ni2 O1 Ni3 92.05(8) . . ?
Ni2 O1 Ni1 126.16(11) . . ?
Ni3 O1 Ni1 129.46(11) . . ?
Ni2 O1 H1 102(3) . . ?
Ni3 O1 H1 112(3) . . ?
Ni1 O1 H1 93(3) . . ?
C33 N9 C34 114.7(3) . . ?
C33 N9 H9A 108.6 . . ?
C34 N9 H9A 108.6 . . ?
C33 N9 H9B 108.6 . . ?
C34 N9 H9B 108.6 . . ?
H9A N9 H9B 107.6 . . ?
N9 C33 H33A 109.5 . . ?
N9 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N9 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N9 C34 H34A 109.5 . . ?
N9 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N9 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.14
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.082
_database_code_depnum_ccdc_archive 'CCDC 947250'
#######################################################################
#
#                 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.
#
#  This CIF is provided on the understanding that it is used for bona
#  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
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_lcj231-2_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H74 Br10 N16 Ni6 O4'
_chemical_formula_weight         2306.56

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'
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

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

_cell_length_a                   11.9623(7)
_cell_length_b                   13.3874(8)
_cell_length_c                   14.2964(9)
_cell_angle_alpha                65.3520(10)
_cell_angle_beta                 72.9400(10)
_cell_angle_gamma                75.1400(10)
_cell_volume                     1965.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7872
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      29.40

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      not_measrued
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1132
_exptl_absorpt_coefficient_mu    6.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5580
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
Before absorption correction R(int) = 0.1087.
After absorption correction R(int) = 0.0291.
;

_diffrn_ambient_temperature      150(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22895
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9051
_reflns_number_gt                7427
_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 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. 

The hydrogen atoms of the hydroxyl groups were located on the difference Fourier maps

Check-cif alerts

232_ALERT_2_B Hirshfeld Test Diff (M-X) Br1 - Ni1 = 13.02 su
232_ALERT_2_B Hirshfeld Test Diff (M-X) Br1 - Ni2 = 15.43 su

Br1 is very weakly coordinated, and the Hirshfeld test does not really apply and this effect is not uncommon anyway in metal complexes.

420_ALERT_2_B D-H Without Acceptor O1 - H1' ?

No suitable acceptors were found at reasonable orientation

;

_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^)+(0.0204P)^2^+0.0000P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9051
_refine_ls_number_parameters     472
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0506
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br2 Br 1.34895(2) 0.82207(2) 0.43462(2) 0.01989(6) Uani 1 1 d . . .
Br1 Br 1.25666(2) 0.65605(2) 0.70547(2) 0.02127(6) Uani 1 1 d . . .
Br4 Br 0.98592(2) 0.63517(2) 0.673533(19) 0.01865(6) Uani 1 1 d . . .
Ni2 Ni 1.25064(3) 0.89049(3) 0.59195(2) 0.01674(7) Uani 1 1 d . . .
Ni1 Ni 1.16666(3) 0.72628(3) 0.53621(2) 0.01538(7) Uani 1 1 d . . .
Ni3 Ni 1.04159(3) 0.76956(3) 0.73777(2) 0.01562(7) Uani 1 1 d . . .
Br7 Br 1.20824(2) 1.09286(2) 0.48943(2) 0.01925(6) Uani 1 1 d . . .
Br3 Br 1.13798(2) 0.89566(2) 0.77443(2) 0.02091(6) Uani 1 1 d . . .
O1 O 1.10356(16) 0.85225(15) 0.58601(14) 0.0156(4) Uani 1 1 d . . .
O2 O 1.40906(15) 0.89937(14) 0.60825(14) 0.0218(4) Uani 1 1 d . . .
N2 N 1.06188(19) 0.78590(17) 0.41880(16) 0.0161(5) Uani 1 1 d . . .
N8 N 1.15605(18) 0.84846(17) 0.24132(16) 0.0179(5) Uani 1 1 d . . .
N5 N 0.89994(18) 1.03294(16) 0.65972(15) 0.0165(4) Uani 1 1 d . . .
N4 N 0.86123(19) 0.85194(18) 0.74266(17) 0.0175(5) Uani 1 1 d . . .
N1 N 1.22350(19) 0.60087(16) 0.48317(16) 0.0177(5) Uani 1 1 d . . .
N6 N 0.79187(19) 0.96831(17) 0.83779(16) 0.0196(5) Uani 1 1 d . . .
N3 N 0.9746(2) 0.69264(17) 0.89072(16) 0.0197(5) Uani 1 1 d . . .
C5 C 1.3198(2) 0.5230(2) 0.5015(2) 0.0230(6) Uani 1 1 d . . .
H5 H 1.3660 0.5261 0.5421 0.028 Uiso 1 1 calc R . .
C9 C 1.1591(2) 0.5980(2) 0.42205(19) 0.0189(6) Uani 1 1 d . . .
C13 C 0.8496(2) 0.9577(2) 0.74699(19) 0.0169(5) Uani 1 1 d . . .
C10 C 1.0500(2) 0.6852(2) 0.40636(19) 0.0186(5) Uani 1 1 d . . .
H10A H 1.0370 0.7053 0.3365 0.022 Uiso 1 1 calc R . .
H10B H 0.9816 0.6545 0.4572 0.022 Uiso 1 1 calc R . .
C19 C 1.0392(3) 0.6366(2) 0.9653(2) 0.0265(6) Uani 1 1 d . . .
H19 H 1.1213 0.6275 0.9450 0.032 Uiso 1 1 calc R . .
C11 C 1.1075(2) 0.8717(2) 0.32776(19) 0.0172(5) Uani 1 1 d . . .
C1 C 1.4260(3) 0.9752(2) 0.6509(2) 0.0256(6) Uani 1 1 d . . .
H1A H 1.3503 1.0121 0.6782 0.031 Uiso 1 1 calc R . .
H1B H 1.4718 1.0312 0.5967 0.031 Uiso 1 1 calc R . .
N7 N 0.7382(2) 1.08559(17) 0.92928(16) 0.0218(5) Uani 1 1 d . . .
C12 C 0.7932(2) 1.0680(2) 0.8391(2) 0.0197(6) Uani 1 1 d . . .
C4 C 1.5004(2) 0.8032(2) 0.6328(2) 0.0237(6) Uani 1 1 d . . .
H4A H 1.5743 0.8174 0.5819 0.028 Uiso 1 1 calc R . .
H4B H 1.4768 0.7386 0.6337 0.028 Uiso 1 1 calc R . .
C15 C 0.8564(2) 0.7081(2) 0.9196(2) 0.0221(6) Uani 1 1 d . . .
C14 C 0.7910(2) 0.7711(2) 0.8312(2) 0.0222(6) Uani 1 1 d . . .
H14A H 0.7754 0.7192 0.8071 0.027 Uiso 1 1 calc R . .
H14B H 0.7157 0.8100 0.8566 0.027 Uiso 1 1 calc R . .
C8 C 1.1870(3) 0.5165(2) 0.3803(2) 0.0272(6) Uani 1 1 d . . .
H8 H 1.1409 0.5162 0.3381 0.033 Uiso 1 1 calc R . .
C6 C 1.3523(3) 0.4396(2) 0.4627(2) 0.0302(7) Uani 1 1 d . . .
H6 H 1.4190 0.3868 0.4770 0.036 Uiso 1 1 calc R . .
C16 C 0.7990(3) 0.6653(2) 1.0246(2) 0.0340(7) Uani 1 1 d . . .
H16 H 0.7168 0.6758 1.0436 0.041 Uiso 1 1 calc R . .
C7 C 1.2838(3) 0.4354(2) 0.4017(2) 0.0328(7) Uani 1 1 d . . .
H7 H 1.3029 0.3787 0.3756 0.039 Uiso 1 1 calc R . .
C2 C 1.4916(3) 0.9039(3) 0.7381(3) 0.0424(9) Uani 1 1 d . . .
H2A H 1.4448 0.9075 0.8050 0.051 Uiso 1 1 calc R . .
H2B H 1.5663 0.9287 0.7240 0.051 Uiso 1 1 calc R . .
C17 C 0.8659(3) 0.6070(2) 1.1001(2) 0.0396(8) Uani 1 1 d . . .
H17 H 0.8292 0.5775 1.1707 0.048 Uiso 1 1 calc R . .
C18 C 0.9877(3) 0.5925(2) 1.0702(2) 0.0358(8) Uani 1 1 d . . .
H18 H 1.0342 0.5536 1.1202 0.043 Uiso 1 1 calc R . .
C3 C 1.5124(3) 0.7861(2) 0.7403(2) 0.0407(8) Uani 1 1 d . . .
H3A H 1.5907 0.7482 0.7521 0.049 Uiso 1 1 calc R . .
H3B H 1.4537 0.7434 0.7949 0.049 Uiso 1 1 calc R . .
C27 C 0.6565(2) 1.0122(2) 1.0098(2) 0.0244(6) Uani 1 1 d . . .
H27A H 0.6285 0.9760 0.9767 0.029 Uiso 1 1 calc R . .
H27B H 0.5885 1.0574 1.0373 0.029 Uiso 1 1 calc R . .
C21 C 0.6651(2) 1.2857(2) 0.9070(2) 0.0241(6) Uani 1 1 d . . .
C28 C 0.7076(2) 0.9237(2) 1.1010(2) 0.0219(6) Uani 1 1 d . . .
C20 C 0.7531(2) 1.1810(2) 0.9457(2) 0.0239(6) Uani 1 1 d . . .
H20A H 0.8325 1.1978 0.9102 0.029 Uiso 1 1 calc R . .
H20B H 0.7464 1.1610 1.0204 0.029 Uiso 1 1 calc R . .
C29 C 0.6314(3) 0.8609(2) 1.1877(2) 0.0280(6) Uani 1 1 d . . .
H29 H 0.5510 0.8747 1.1881 0.034 Uiso 1 1 calc R . .
C26 C 0.5877(3) 1.2955(2) 0.8473(2) 0.0298(7) Uani 1 1 d . . .
H26 H 0.5875 1.2358 0.8301 0.036 Uiso 1 1 calc R . .
C33 C 0.8259(3) 0.9016(2) 1.1021(2) 0.0343(7) Uani 1 1 d . . .
H33 H 0.8785 0.9421 1.0447 0.041 Uiso 1 1 calc R . .
C22 C 0.6649(3) 1.3765(2) 0.9301(3) 0.0386(8) Uani 1 1 d . . .
H22 H 0.7165 1.3714 0.9700 0.046 Uiso 1 1 calc R . .
C30 C 0.6727(3) 0.7786(2) 1.2729(2) 0.0359(7) Uani 1 1 d . . .
H30 H 0.6203 0.7372 1.3299 0.043 Uiso 1 1 calc R . .
C25 C 0.5103(3) 1.3934(3) 0.8127(2) 0.0371(8) Uani 1 1 d . . .
H25 H 0.4580 1.3987 0.7733 0.045 Uiso 1 1 calc R . .
C31 C 0.7910(3) 0.7575(3) 1.2737(2) 0.0386(8) Uani 1 1 d . . .
H31 H 0.8193 0.7022 1.3312 0.046 Uiso 1 1 calc R . .
C24 C 0.5109(3) 1.4824(3) 0.8366(3) 0.0436(9) Uani 1 1 d . . .
H24 H 0.4587 1.5479 0.8139 0.052 Uiso 1 1 calc R . .
C32 C 0.8674(3) 0.8192(3) 1.1881(3) 0.0447(9) Uani 1 1 d . . .
H32 H 0.9477 0.8054 1.1881 0.054 Uiso 1 1 calc R . .
C23 C 0.5891(3) 1.4742(3) 0.8944(3) 0.0493(10) Uani 1 1 d . . .
H23 H 0.5907 1.5350 0.9095 0.059 Uiso 1 1 calc R . .
H4' H 0.851(2) 0.856(2) 0.689(2) 0.015(7) Uiso 1 1 d . . .
H2' H 1.001(3) 0.812(2) 0.452(2) 0.036(9) Uiso 1 1 d . . .
H1' H 1.067(3) 0.901(2) 0.560(2) 0.031(10) Uiso 1 1 d . . .

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
Br2 0.01746(13) 0.02335(13) 0.01958(13) -0.00911(11) -0.00037(10) -0.00643(10)
Br1 0.02022(14) 0.02215(13) 0.02029(13) -0.00501(11) -0.00837(11) -0.00156(10)
Br4 0.02329(14) 0.01847(12) 0.01505(12) -0.00416(10) -0.00350(10) -0.00882(10)
Ni2 0.01557(17) 0.01889(16) 0.01750(17) -0.00712(14) -0.00409(13) -0.00417(13)
Ni1 0.01786(17) 0.01596(16) 0.01347(16) -0.00547(13) -0.00368(13) -0.00403(13)
Ni3 0.01765(17) 0.01674(16) 0.01201(16) -0.00377(13) -0.00283(13) -0.00494(13)
Br7 0.01776(13) 0.01910(13) 0.01920(13) -0.00467(10) -0.00406(10) -0.00409(10)
Br3 0.02481(14) 0.02385(13) 0.01807(13) -0.00906(11) -0.00529(11) -0.00726(11)
O1 0.0166(9) 0.0136(9) 0.0158(9) -0.0034(8) -0.0057(8) -0.0018(8)
O2 0.0177(9) 0.0215(9) 0.0311(11) -0.0130(8) -0.0085(8) -0.0013(8)
N2 0.0162(11) 0.0182(11) 0.0137(11) -0.0052(9) -0.0027(9) -0.0039(9)
N8 0.0189(11) 0.0203(11) 0.0139(11) -0.0063(9) -0.0021(9) -0.0035(9)
N5 0.0166(11) 0.0162(10) 0.0136(10) -0.0035(9) -0.0030(9) -0.0009(9)
N4 0.0204(12) 0.0196(11) 0.0115(11) -0.0046(9) -0.0016(9) -0.0056(9)
N1 0.0196(11) 0.0172(10) 0.0157(11) -0.0049(9) -0.0022(9) -0.0060(9)
N6 0.0207(12) 0.0199(11) 0.0163(11) -0.0050(9) -0.0032(9) -0.0038(9)
N3 0.0275(13) 0.0176(11) 0.0149(11) -0.0037(9) -0.0052(10) -0.0076(9)
C5 0.0250(15) 0.0241(14) 0.0196(14) -0.0080(12) -0.0053(12) -0.0030(12)
C9 0.0222(14) 0.0179(13) 0.0154(13) -0.0028(11) -0.0027(11) -0.0082(11)
C13 0.0138(12) 0.0185(13) 0.0177(13) -0.0048(11) -0.0060(10) -0.0018(10)
C10 0.0229(14) 0.0206(13) 0.0153(13) -0.0051(11) -0.0053(11) -0.0096(11)
C19 0.0392(18) 0.0228(14) 0.0174(14) -0.0027(12) -0.0109(13) -0.0073(13)
C11 0.0132(12) 0.0205(13) 0.0165(13) -0.0054(11) -0.0062(10) 0.0009(10)
C1 0.0268(15) 0.0235(14) 0.0352(16) -0.0143(13) -0.0112(13) -0.0069(12)
N7 0.0270(13) 0.0229(12) 0.0137(11) -0.0082(10) -0.0001(10) -0.0031(10)
C12 0.0188(14) 0.0219(13) 0.0167(13) -0.0060(11) -0.0054(11) -0.0006(11)
C4 0.0172(14) 0.0221(14) 0.0346(16) -0.0133(13) -0.0076(12) -0.0009(11)
C15 0.0300(16) 0.0168(13) 0.0168(13) -0.0034(11) 0.0000(12) -0.0097(11)
C14 0.0202(14) 0.0232(14) 0.0223(14) -0.0075(12) 0.0003(11) -0.0087(11)
C8 0.0343(17) 0.0274(15) 0.0270(15) -0.0144(13) -0.0044(13) -0.0113(13)
C6 0.0334(17) 0.0237(15) 0.0266(16) -0.0083(13) -0.0036(13) 0.0022(13)
C16 0.0419(19) 0.0282(16) 0.0240(16) -0.0066(13) 0.0057(14) -0.0119(14)
C7 0.046(2) 0.0252(15) 0.0286(16) -0.0154(13) -0.0034(15) -0.0047(14)
C2 0.064(2) 0.0358(18) 0.0379(19) -0.0186(16) -0.0266(18) 0.0019(16)
C17 0.069(3) 0.0289(16) 0.0123(14) -0.0029(13) 0.0054(15) -0.0171(16)
C18 0.060(2) 0.0272(16) 0.0192(15) -0.0024(13) -0.0136(15) -0.0093(15)
C3 0.058(2) 0.0277(16) 0.0401(19) -0.0082(15) -0.0275(17) -0.0001(15)
C27 0.0228(15) 0.0311(15) 0.0170(13) -0.0094(12) 0.0002(11) -0.0045(12)
C21 0.0236(15) 0.0257(14) 0.0195(14) -0.0074(12) -0.0015(12) -0.0034(12)
C28 0.0265(15) 0.0224(14) 0.0188(14) -0.0100(12) -0.0032(12) -0.0048(11)
C20 0.0277(15) 0.0288(15) 0.0164(13) -0.0108(12) -0.0034(12) -0.0035(12)
C29 0.0240(15) 0.0285(15) 0.0282(16) -0.0065(13) -0.0024(13) -0.0091(12)
C26 0.0286(16) 0.0286(15) 0.0324(17) -0.0104(14) -0.0093(14) -0.0033(13)
C33 0.0272(16) 0.0415(18) 0.0233(16) 0.0013(14) -0.0018(13) -0.0144(14)
C22 0.048(2) 0.0317(17) 0.044(2) -0.0178(15) -0.0214(17) 0.0001(15)
C30 0.0385(19) 0.0331(17) 0.0258(16) -0.0009(14) -0.0002(14) -0.0136(14)
C25 0.0262(17) 0.0423(19) 0.0373(18) -0.0045(15) -0.0134(14) -0.0058(14)
C31 0.041(2) 0.0419(18) 0.0238(16) 0.0030(14) -0.0132(15) -0.0097(15)
C24 0.041(2) 0.0297(17) 0.051(2) -0.0075(16) -0.0164(17) 0.0037(15)
C32 0.0309(18) 0.053(2) 0.0368(19) 0.0019(17) -0.0126(15) -0.0107(16)
C23 0.062(3) 0.0303(18) 0.062(2) -0.0215(18) -0.025(2) 0.0034(17)

_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
Br2 Ni1 2.5557(4) . ?
Br2 Ni2 2.6258(4) . ?
Br1 Ni1 2.6477(4) . ?
Br1 Ni3 2.6503(4) . ?
Br1 Ni2 2.8624(4) . ?
Br4 Ni3 2.6220(4) . ?
Br4 Ni1 2.6232(4) . ?
Ni2 O1 1.9876(18) . ?
Ni2 O2 2.0142(18) . ?
Ni2 Br7 2.4829(4) . ?
Ni2 Br3 2.5820(4) . ?
Ni1 O1 1.9885(17) . ?
Ni1 N1 2.007(2) . ?
Ni1 N2 2.152(2) . ?
Ni3 O1 1.9890(18) . ?
Ni3 N3 2.000(2) . ?
Ni3 N4 2.152(2) . ?
Ni3 Br3 2.5584(4) . ?
O1 H1' 0.70(3) . ?
O2 C4 1.449(3) . ?
O2 C1 1.461(3) . ?
N2 C11 1.403(3) . ?
N2 C10 1.477(3) . ?
N2 H2' 0.82(3) . ?
N8 C11 1.329(3) . ?
N8 C12 1.345(3) 2_776 ?
N5 C13 1.325(3) . ?
N5 C11 1.339(3) 2_776 ?
N4 C13 1.412(3) . ?
N4 C14 1.476(3) . ?
N4 H4' 0.79(3) . ?
N1 C9 1.340(3) . ?
N1 C5 1.347(3) . ?
N6 C13 1.327(3) . ?
N6 C12 1.347(3) . ?
N3 C15 1.339(3) . ?
N3 C19 1.347(3) . ?
C5 C6 1.368(4) . ?
C5 H5 0.9300 . ?
C9 C8 1.378(3) . ?
C9 C10 1.513(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C19 C18 1.372(4) . ?
C19 H19 0.9300 . ?
C11 N5 1.339(3) 2_776 ?
C1 C2 1.510(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N7 C12 1.351(3) . ?
N7 C20 1.453(3) . ?
N7 C27 1.460(3) . ?
C12 N8 1.345(3) 2_776 ?
C4 C3 1.502(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C15 C16 1.390(4) . ?
C15 C14 1.507(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C8 C7 1.378(4) . ?
C8 H8 0.9300 . ?
C6 C7 1.384(4) . ?
C6 H6 0.9300 . ?
C16 C17 1.378(4) . ?
C16 H16 0.9300 . ?
C7 H7 0.9300 . ?
C2 C3 1.520(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C17 C18 1.379(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C27 C28 1.512(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C21 C26 1.381(4) . ?
C21 C22 1.386(4) . ?
C21 C20 1.522(4) . ?
C28 C33 1.372(4) . ?
C28 C29 1.391(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C29 C30 1.376(4) . ?
C29 H29 0.9300 . ?
C26 C25 1.387(4) . ?
C26 H26 0.9300 . ?
C33 C32 1.386(4) . ?
C33 H33 0.9300 . ?
C22 C23 1.379(4) . ?
C22 H22 0.9300 . ?
C30 C31 1.373(4) . ?
C30 H30 0.9300 . ?
C25 C24 1.371(4) . ?
C25 H25 0.9300 . ?
C31 C32 1.379(4) . ?
C31 H31 0.9300 . ?
C24 C23 1.377(5) . ?
C24 H24 0.9300 . ?
C32 H32 0.9300 . ?
C23 H23 0.9300 . ?

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
Ni1 Br2 Ni2 73.172(12) . . ?
Ni1 Br1 Ni3 70.269(12) . . ?
Ni1 Br1 Ni2 68.063(11) . . ?
Ni3 Br1 Ni2 67.548(11) . . ?
Ni3 Br4 Ni1 71.082(12) . . ?
O1 Ni2 O2 169.66(7) . . ?
O1 Ni2 Br7 96.28(5) . . ?
O2 Ni2 Br7 93.88(5) . . ?
O1 Ni2 Br3 85.67(5) . . ?
O2 Ni2 Br3 94.97(5) . . ?
Br7 Ni2 Br3 97.183(13) . . ?
O1 Ni2 Br2 84.57(5) . . ?
O2 Ni2 Br2 92.00(5) . . ?
Br7 Ni2 Br2 98.799(14) . . ?
Br3 Ni2 Br2 162.076(16) . . ?
O1 Ni2 Br1 72.89(5) . . ?
O2 Ni2 Br1 96.96(5) . . ?
Br7 Ni2 Br1 169.155(16) . . ?
Br3 Ni2 Br1 81.823(12) . . ?
Br2 Ni2 Br1 80.952(12) . . ?
O1 Ni1 N1 177.30(8) . . ?
O1 Ni1 N2 95.81(8) . . ?
N1 Ni1 N2 81.66(8) . . ?
O1 Ni1 Br2 86.46(5) . . ?
N1 Ni1 Br2 95.01(6) . . ?
N2 Ni1 Br2 102.16(6) . . ?
O1 Ni1 Br4 85.54(5) . . ?
N1 Ni1 Br4 93.37(6) . . ?
N2 Ni1 Br4 87.56(6) . . ?
Br2 Ni1 Br4 167.986(16) . . ?
O1 Ni1 Br1 78.12(5) . . ?
N1 Ni1 Br1 104.22(6) . . ?
N2 Ni1 Br1 169.17(6) . . ?
Br2 Ni1 Br1 86.537(13) . . ?
Br4 Ni1 Br1 83.062(13) . . ?
O1 Ni3 N3 177.46(8) . . ?
O1 Ni3 N4 96.85(8) . . ?
N3 Ni3 N4 81.12(9) . . ?
O1 Ni3 Br3 86.29(5) . . ?
N3 Ni3 Br3 92.65(6) . . ?
N4 Ni3 Br3 102.75(6) . . ?
O1 Ni3 Br4 85.56(5) . . ?
N3 Ni3 Br4 95.85(6) . . ?
N4 Ni3 Br4 87.07(6) . . ?
Br3 Ni3 Br4 167.918(16) . . ?
O1 Ni3 Br1 78.04(5) . . ?
N3 Ni3 Br1 104.21(6) . . ?
N4 Ni3 Br1 169.17(6) . . ?
Br3 Ni3 Br1 86.568(14) . . ?
Br4 Ni3 Br1 83.033(13) . . ?
Ni3 Br3 Ni2 73.336(12) . . ?
Ni2 O1 Ni1 101.95(8) . . ?
Ni2 O1 Ni3 101.06(8) . . ?
Ni1 O1 Ni3 100.09(8) . . ?
Ni2 O1 H1' 110(3) . . ?
Ni1 O1 H1' 123(3) . . ?
Ni3 O1 H1' 117(3) . . ?
C4 O2 C1 106.91(19) . . ?
C4 O2 Ni2 122.50(15) . . ?
C1 O2 Ni2 123.56(15) . . ?
C11 N2 C10 117.4(2) . . ?
C11 N2 Ni1 112.02(16) . . ?
C10 N2 Ni1 105.05(14) . . ?
C11 N2 H2' 110(2) . . ?
C10 N2 H2' 113(2) . . ?
Ni1 N2 H2' 98(2) . . ?
C11 N8 C12 113.1(2) . 2_776 ?
C13 N5 C11 111.8(2) . 2_776 ?
C13 N4 C14 117.2(2) . . ?
C13 N4 Ni3 110.64(16) . . ?
C14 N4 Ni3 104.59(15) . . ?
C13 N4 H4' 112.2(19) . . ?
C14 N4 H4' 109(2) . . ?
Ni3 N4 H4' 101.4(19) . . ?
C9 N1 C5 118.4(2) . . ?
C9 N1 Ni1 115.28(16) . . ?
C5 N1 Ni1 126.26(18) . . ?
C13 N6 C12 112.8(2) . . ?
C15 N3 C19 119.2(2) . . ?
C15 N3 Ni3 115.69(17) . . ?
C19 N3 Ni3 124.80(19) . . ?
N1 C5 C6 122.6(3) . . ?
N1 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
N1 C9 C8 121.9(2) . . ?
N1 C9 C10 116.4(2) . . ?
C8 C9 C10 121.6(2) . . ?
N5 C13 N6 128.5(2) . . ?
N5 C13 N4 115.3(2) . . ?
N6 C13 N4 116.2(2) . . ?
N2 C10 C9 111.6(2) . . ?
N2 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
N3 C19 C18 122.1(3) . . ?
N3 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
N8 C11 N5 127.8(2) . 2_776 ?
N8 C11 N2 117.2(2) . . ?
N5 C11 N2 114.9(2) 2_776 . ?
O2 C1 C2 105.9(2) . . ?
O2 C1 H1A 110.5 . . ?
C2 C1 H1A 110.5 . . ?
O2 C1 H1B 110.5 . . ?
C2 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
C12 N7 C20 121.1(2) . . ?
C12 N7 C27 120.3(2) . . ?
C20 N7 C27 118.5(2) . . ?
N8 C12 N6 125.8(2) 2_776 . ?
N8 C12 N7 117.2(2) 2_776 . ?
N6 C12 N7 117.0(2) . . ?
O2 C4 C3 104.0(2) . . ?
O2 C4 H4A 111.0 . . ?
C3 C4 H4A 111.0 . . ?
O2 C4 H4B 111.0 . . ?
C3 C4 H4B 111.0 . . ?
H4A C4 H4B 109.0 . . ?
N3 C15 C16 121.3(3) . . ?
N3 C15 C14 115.8(2) . . ?
C16 C15 C14 122.9(3) . . ?
N4 C14 C15 110.6(2) . . ?
N4 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C7 C8 C9 119.2(3) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C5 C6 C7 118.7(3) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C17 C16 C15 118.9(3) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C8 C7 C6 119.1(3) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C1 C2 C3 105.8(2) . . ?
C1 C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C16 C17 C18 119.6(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 118.8(3) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C4 C3 C2 103.4(2) . . ?
C4 C3 H3A 111.1 . . ?
C2 C3 H3A 111.1 . . ?
C4 C3 H3B 111.1 . . ?
C2 C3 H3B 111.1 . . ?
H3A C3 H3B 109.0 . . ?
N7 C27 C28 115.2(2) . . ?
N7 C27 H27A 108.5 . . ?
C28 C27 H27A 108.5 . . ?
N7 C27 H27B 108.5 . . ?
C28 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C26 C21 C22 118.5(3) . . ?
C26 C21 C20 123.1(2) . . ?
C22 C21 C20 118.4(3) . . ?
C33 C28 C29 118.3(3) . . ?
C33 C28 C27 123.2(2) . . ?
C29 C28 C27 118.6(2) . . ?
N7 C20 C21 114.9(2) . . ?
N7 C20 H20A 108.5 . . ?
C21 C20 H20A 108.5 . . ?
N7 C20 H20B 108.5 . . ?
C21 C20 H20B 108.6 . . ?
H20A C20 H20B 107.5 . . ?
C30 C29 C28 121.3(3) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C21 C26 C25 120.8(3) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C33 C32 120.5(3) . . ?
C28 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C23 C22 C21 120.6(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C31 C30 C29 120.1(3) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C30 C31 C32 119.2(3) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C31 C32 C33 120.7(3) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 947251'