# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_[Cu3]
_database_code_depnum_ccdc_archive 'CCDC 1403544'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         "C28 H21 Cl3 Cu3 N15 O2', 'Cl', 'O3"
_chemical_formula_sum            'C28 H31 Cl4 Cu3 N15 O5'
_chemical_formula_weight         990.10

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   11.665(3)
_cell_length_b                   6.7814(15)
_cell_length_c                   48.532(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.167(4)
_cell_angle_gamma                90
_cell_volume                     3828.8(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3383
_cell_measurement_theta_min      2.5245
_cell_measurement_theta_max      24.7675

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_F_000             1996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.990
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6916
_exptl_absorpt_correction_T_max  0.9613
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            19936
_diffrn_reflns_av_unetI/netI     0.1252
_diffrn_reflns_av_R_equivalents  0.1354
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         0.841
_diffrn_reflns_theta_max         25.629
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7165
_reflns_number_gt                4935
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1407P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7165
_refine_ls_number_parameters     496
_refine_ls_number_restraints     534
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0907
_refine_ls_wR_factor_ref         0.2438
_refine_ls_wR_factor_gt          0.2248
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      0.988
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.61866(8) 1.06495(15) 0.16175(2) 0.0190(3) Uani 1 1 d . U . . .
Cu2 Cu 0.53935(9) 0.80010(15) 0.06982(2) 0.0192(3) Uani 1 1 d . U . . .
Cu3 Cu 0.24133(8) 0.81124(16) 0.13307(2) 0.0220(3) Uani 1 1 d . U . . .
Cl1 Cl 0.68643(16) 0.7197(3) 0.18235(4) 0.0165(4) Uani 1 1 d . U . . .
Cl2 Cl 0.61497(17) 0.4659(3) 0.08344(4) 0.0185(4) Uani 1 1 d . U . . .
Cl3 Cl 0.19496(18) 1.1573(3) 0.10707(5) 0.0284(5) Uani 1 1 d . U . . .
Cl4 Cl 0.0926(3) 0.4527(5) 0.24077(7) 0.0628(9) Uani 1 1 d . . . . .
O1 O 0.5413(5) 0.4162(8) 0.14540(12) 0.0220(13) Uani 1 1 d . . . . .
O2 O 0.3012(5) 0.4652(9) 0.14902(13) 0.0267(14) Uani 1 1 d . . . . .
N1 N 0.6504(6) 1.1878(10) 0.20003(15) 0.0219(15) Uani 1 1 d . U . . .
N2 N 0.7631(5) 1.2465(10) 0.20370(13) 0.0163(14) Uani 1 1 d . U . . .
N3 N 0.7732(6) 1.1672(10) 0.15926(14) 0.0198(14) Uani 1 1 d . U . . .
N4 N 0.6441(6) 1.0025(11) 0.12288(14) 0.0224(15) Uani 1 1 d . U . . .
N5 N 0.5606(6) 0.9163(11) 0.10723(14) 0.0207(14) Uani 1 1 d . U . . .
N6 N 0.6564(6) 0.8604(11) 0.04176(14) 0.0229(15) Uani 1 1 d . U . . .
N7 N 0.6109(6) 0.8228(10) 0.01504(14) 0.0207(14) Uani 1 1 d . U . . .
N8 N 0.4498(6) 0.7395(10) 0.03516(14) 0.0198(14) Uani 1 1 d . U . . .
N9 N 0.3856(6) 0.7583(11) 0.08335(14) 0.0208(14) Uani 1 1 d . U . . .
N10 N 0.3717(6) 0.8000(10) 0.10984(13) 0.0205(14) Uani 1 1 d . U . . .
N11 N 0.0833(6) 0.7013(11) 0.12060(15) 0.0229(15) Uani 1 1 d . U . . .
N12 N 0.0080(5) 0.7267(10) 0.14138(14) 0.0166(14) Uani 1 1 d . U . . .
N13 N 0.1611(6) 0.8505(9) 0.16640(15) 0.0176(14) Uani 1 1 d . U . . .
N14 N 0.3652(6) 0.9250(10) 0.15812(14) 0.0199(14) Uani 1 1 d . U . . .
N15 N 0.4669(6) 0.9539(10) 0.14839(13) 0.0165(13) Uani 1 1 d . U . . .
C1 C 0.6108(7) 1.2083(12) 0.22584(17) 0.0208(17) Uani 1 1 d . U . . .
H1 H 0.5350 1.1766 0.2303 0.025 Uiso 1 1 calc R U . . .
C2 C 0.6962(7) 1.2815(13) 0.24464(17) 0.0219(18) Uani 1 1 d . U . . .
H2 H 0.6899 1.3108 0.2636 0.026 Uiso 1 1 calc R U . . .
C3 C 0.7915(7) 1.3022(12) 0.22977(15) 0.0162(16) Uani 1 1 d . U . . .
H3 H 0.8648 1.3481 0.2368 0.019 Uiso 1 1 calc R U . . .
C4 C 0.8297(7) 1.2420(11) 0.18100(16) 0.0143(15) Uani 1 1 d . U . . .
C5 C 0.9451(7) 1.3016(12) 0.18125(19) 0.0215(18) Uani 1 1 d . U . . .
H5 H 0.9857 1.3568 0.1971 0.026 Uiso 1 1 calc R U . . .
C6 C 0.9950(7) 1.2729(11) 0.15632(17) 0.0171(16) Uani 1 1 d . U . . .
H6 H 1.0734 1.3071 0.1549 0.021 Uiso 1 1 calc R U . . .
C7 C 0.9327(7) 1.1958(12) 0.13366(19) 0.0221(18) Uani 1 1 d . U . . .
H7 H 0.9679 1.1804 0.1167 0.027 Uiso 1 1 calc R U . . .
C8 C 0.8206(7) 1.1411(13) 0.13529(18) 0.0235(18) Uani 1 1 d . U . . .
C9 C 0.7416(7) 1.0518(12) 0.11405(18) 0.0209(17) Uani 1 1 d . U . . .
H9 H 0.7603 1.0322 0.0955 0.025 Uiso 1 1 calc R U . . .
C10 C 0.7672(8) 0.9099(15) 0.0380(2) 0.034(2) Uani 1 1 d . U . . .
H10 H 0.8223 0.9454 0.0525 0.040 Uiso 1 1 calc R U . . .
C11 C 0.7903(8) 0.9023(15) 0.01005(19) 0.031(2) Uani 1 1 d . U . . .
H11 H 0.8611 0.9305 0.0024 0.037 Uiso 1 1 calc R U . . .
C12 C 0.6896(7) 0.8457(12) -0.00385(18) 0.0210(17) Uani 1 1 d . U . . .
H12 H 0.6772 0.8261 -0.0232 0.025 Uiso 1 1 calc R U . . .
C13 C 0.4974(7) 0.7562(12) 0.01184(17) 0.0175(16) Uani 1 1 d . U . . .
C14 C 0.4391(8) 0.7080(13) -0.01313(16) 0.0232(18) Uani 1 1 d . U . . .
H14 H 0.4727 0.7194 -0.0303 0.028 Uiso 1 1 calc R U . . .
C15 C 0.3280(7) 0.6421(13) -0.01099(17) 0.0231(18) Uani 1 1 d . U . . .
H15 H 0.2840 0.6048 -0.0274 0.028 Uiso 1 1 calc R U . . .
C16 C 0.2780(8) 0.6277(14) 0.01380(19) 0.029(2) Uani 1 1 d . U . . .
H16 H 0.2014 0.5812 0.0144 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3408(7) 0.6815(13) 0.03742(18) 0.0224(18) Uani 1 1 d . U . . .
C18 C 0.3079(8) 0.6939(14) 0.06615(18) 0.028(2) Uani 1 1 d . U . . .
H18 H 0.2340 0.6565 0.0713 0.033 Uiso 1 1 calc R U . . .
C19 C 0.0129(7) 0.6366(13) 0.09834(18) 0.0234(18) Uani 1 1 d . U . . .
H19 H 0.0384 0.6057 0.0807 0.028 Uiso 1 1 calc R U . . .
C20 C -0.0986(7) 0.6231(13) 0.10513(18) 0.0211(18) Uani 1 1 d . U . . .
H20 H -0.1629 0.5815 0.0934 0.025 Uiso 1 1 calc R U . . .
C21 C -0.0992(7) 0.6817(12) 0.13226(18) 0.0204(17) Uani 1 1 d . U . . .
H21 H -0.1649 0.6888 0.1427 0.025 Uiso 1 1 calc R U . . .
C22 C 0.0518(7) 0.7975(11) 0.16708(16) 0.0152(15) Uani 1 1 d . U . . .
C23 C -0.0085(7) 0.8196(11) 0.19041(17) 0.0168(16) Uani 1 1 d . U . . .
H23 H -0.0866 0.7808 0.1907 0.020 Uiso 1 1 calc R U . . .
C24 C 0.0516(7) 0.9017(12) 0.21337(17) 0.0179(17) Uani 1 1 d . U . . .
H24 H 0.0149 0.9204 0.2300 0.021 Uiso 1 1 calc R U . . .
C25 C 0.1658(7) 0.9564(11) 0.21176(18) 0.0183(16) Uani 1 1 d . U . . .
H25 H 0.2073 1.0140 0.2273 0.022 Uiso 1 1 calc R U . . .
C26 C 0.2182(7) 0.9274(13) 0.18786(17) 0.0212(17) Uani 1 1 d . U . . .
C27 C 0.3385(7) 0.9725(13) 0.18272(17) 0.0212(18) Uani 1 1 d . U . . .
H27 H 0.3913 1.0309 0.1961 0.025 Uiso 1 1 calc R U . . .
C28 C 0.4676(6) 0.8891(11) 0.12161(16) 0.0138(15) Uani 1 1 d . U . . .
O1S O 0.3973(6) 0.2052(10) 0.06640(12) 0.0307(15) Uani 1 1 d . . . . .
O2S O 0.2899(9) 0.4134(12) 0.20669(15) 0.064(3) Uani 1 1 d . . . . .
O3S O 0.4785(6) 0.6344(12) 0.22445(15) 0.046(2) 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
Cu1 N3 1.944(7) . ?
Cu1 N4 1.977(7) . ?
Cu1 N15 1.989(7) . ?
Cu1 N1 2.045(7) . ?
Cu1 Cl1 2.644(2) . ?
Cu2 N8 1.958(7) . ?
Cu2 N9 1.975(7) . ?
Cu2 N5 1.978(7) . ?
Cu2 N6 2.039(7) . ?
Cu2 Cl2 2.503(2) . ?
Cu3 N13 1.945(7) . ?
Cu3 N10 1.959(7) . ?
Cu3 N14 1.977(7) . ?
Cu3 N11 2.039(7) . ?
Cu3 Cl3 2.700(3) . ?
N1 N2 1.372(9) . ?
N1 C1 1.373(11) . ?
N2 C3 1.339(10) . ?
N2 C4 1.394(10) . ?
N3 C4 1.305(10) . ?
N3 C8 1.335(11) . ?
N4 C9 1.287(10) . ?
N4 N5 1.327(10) . ?
N5 C28 1.345(10) . ?
N6 C10 1.361(12) . ?
N6 N7 1.389(10) . ?
N7 C12 1.353(11) . ?
N7 C13 1.398(11) . ?
N8 C13 1.301(10) . ?
N8 C17 1.343(11) . ?
N9 C18 1.264(11) . ?
N9 N10 1.337(9) . ?
N10 C28 1.360(10) . ?
N11 C19 1.381(11) . ?
N11 N12 1.395(9) . ?
N12 C21 1.331(10) . ?
N12 C22 1.398(10) . ?
N13 C26 1.303(11) . ?
N13 C22 1.328(10) . ?
N14 C27 1.296(11) . ?
N14 N15 1.322(9) . ?
N15 C28 1.373(10) . ?
C1 C2 1.392(12) . ?
C1 H1 0.9500 . ?
C2 C3 1.376(12) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.405(11) . ?
C5 C6 1.394(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.367(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.463(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.366(13) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.385(11) . ?
C14 C15 1.382(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.364(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.475(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.368(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.376(12) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.384(11) . ?
C23 C24 1.389(12) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.364(12) . ?
C25 H25 0.9500 . ?
C26 C27 1.475(12) . ?
C27 H27 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N4 79.2(3) . . ?
N3 Cu1 N15 157.3(3) . . ?
N4 Cu1 N15 78.5(3) . . ?
N3 Cu1 N1 78.7(3) . . ?
N4 Cu1 N1 157.5(3) . . ?
N15 Cu1 N1 123.3(3) . . ?
N3 Cu1 Cl1 94.9(2) . . ?
N4 Cu1 Cl1 96.3(2) . . ?
N15 Cu1 Cl1 91.29(19) . . ?
N1 Cu1 Cl1 89.3(2) . . ?
N8 Cu2 N9 79.3(3) . . ?
N8 Cu2 N5 153.6(3) . . ?
N9 Cu2 N5 78.9(3) . . ?
N8 Cu2 N6 79.0(3) . . ?
N9 Cu2 N6 156.8(3) . . ?
N5 Cu2 N6 119.2(3) . . ?
N8 Cu2 Cl2 101.1(2) . . ?
N9 Cu2 Cl2 95.4(2) . . ?
N5 Cu2 Cl2 95.7(2) . . ?
N6 Cu2 Cl2 96.8(2) . . ?
N13 Cu3 N10 157.6(3) . . ?
N13 Cu3 N14 79.0(3) . . ?
N10 Cu3 N14 78.8(3) . . ?
N13 Cu3 N11 79.5(3) . . ?
N10 Cu3 N11 122.5(3) . . ?
N14 Cu3 N11 158.5(3) . . ?
N13 Cu3 Cl3 100.2(2) . . ?
N10 Cu3 Cl3 84.4(2) . . ?
N14 Cu3 Cl3 93.5(2) . . ?
N11 Cu3 Cl3 91.9(2) . . ?
N2 N1 C1 103.6(6) . . ?
N2 N1 Cu1 110.2(5) . . ?
C1 N1 Cu1 145.0(6) . . ?
C3 N2 N1 111.9(6) . . ?
C3 N2 C4 129.7(7) . . ?
N1 N2 C4 118.3(6) . . ?
C4 N3 C8 122.6(8) . . ?
C4 N3 Cu1 120.3(6) . . ?
C8 N3 Cu1 116.8(6) . . ?
C9 N4 N5 123.6(7) . . ?
C9 N4 Cu1 117.4(6) . . ?
N5 N4 Cu1 119.0(5) . . ?
N4 N5 C28 110.5(7) . . ?
N4 N5 Cu2 137.6(5) . . ?
C28 N5 Cu2 111.7(5) . . ?
C10 N6 N7 102.8(7) . . ?
C10 N6 Cu2 145.9(6) . . ?
N7 N6 Cu2 111.0(5) . . ?
C12 N7 N6 112.3(7) . . ?
C12 N7 C13 130.3(7) . . ?
N6 N7 C13 117.2(7) . . ?
C13 N8 C17 124.2(8) . . ?
C13 N8 Cu2 119.6(6) . . ?
C17 N8 Cu2 116.1(5) . . ?
C18 N9 N10 125.2(8) . . ?
C18 N9 Cu2 117.0(6) . . ?
N10 N9 Cu2 117.7(6) . . ?
N9 N10 C28 110.1(7) . . ?
N9 N10 Cu3 135.6(6) . . ?
C28 N10 Cu3 113.0(5) . . ?
C19 N11 N12 103.6(6) . . ?
C19 N11 Cu3 145.3(6) . . ?
N12 N11 Cu3 110.1(5) . . ?
C21 N12 N11 110.9(7) . . ?
C21 N12 C22 130.4(7) . . ?
N11 N12 C22 118.6(6) . . ?
C26 N13 C22 121.6(7) . . ?
C26 N13 Cu3 118.1(6) . . ?
C22 N13 Cu3 120.3(6) . . ?
C27 N14 N15 125.1(7) . . ?
C27 N14 Cu3 116.7(6) . . ?
N15 N14 Cu3 118.2(5) . . ?
N14 N15 C28 111.0(6) . . ?
N14 N15 Cu1 137.7(5) . . ?
C28 N15 Cu1 111.3(5) . . ?
N1 C1 C2 111.2(8) . . ?
N1 C1 H1 124.4 . . ?
C2 C1 H1 124.4 . . ?
C3 C2 C1 105.0(7) . . ?
C3 C2 H2 127.5 . . ?
C1 C2 H2 127.5 . . ?
N2 C3 C2 108.2(7) . . ?
N2 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
N3 C4 N2 111.7(7) . . ?
N3 C4 C5 123.1(8) . . ?
N2 C4 C5 125.2(7) . . ?
C6 C5 C4 114.4(8) . . ?
C6 C5 H5 122.8 . . ?
C4 C5 H5 122.8 . . ?
C7 C6 C5 121.1(8) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C8 C7 C6 120.6(8) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
N3 C8 C7 118.2(8) . . ?
N3 C8 C9 112.9(7) . . ?
C7 C8 C9 128.9(8) . . ?
N4 C9 C8 113.5(7) . . ?
N4 C9 H9 123.2 . . ?
C8 C9 H9 123.2 . . ?
N6 C10 C11 111.9(9) . . ?
N6 C10 H10 124.1 . . ?
C11 C10 H10 124.1 . . ?
C12 C11 C10 105.6(8) . . ?
C12 C11 H11 127.2 . . ?
C10 C11 H11 127.2 . . ?
N7 C12 C11 107.4(8) . . ?
N7 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
N8 C13 C14 121.8(8) . . ?
N8 C13 N7 113.1(7) . . ?
C14 C13 N7 125.1(7) . . ?
C15 C14 C13 114.4(8) . . ?
C15 C14 H14 122.8 . . ?
C13 C14 H14 122.8 . . ?
C16 C15 C14 123.2(8) . . ?
C16 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C17 C16 C15 118.6(9) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
N8 C17 C16 117.6(8) . . ?
N8 C17 C18 111.9(7) . . ?
C16 C17 C18 130.5(8) . . ?
N9 C18 C17 114.9(8) . . ?
N9 C18 H18 122.6 . . ?
C17 C18 H18 122.6 . . ?
C20 C19 N11 110.8(8) . . ?
C20 C19 H19 124.6 . . ?
N11 C19 H19 124.6 . . ?
C19 C20 C21 106.4(8) . . ?
C19 C20 H20 126.8 . . ?
C21 C20 H20 126.8 . . ?
N12 C21 C20 108.3(7) . . ?
N12 C21 H21 125.8 . . ?
C20 C21 H21 125.8 . . ?
N13 C22 C23 122.5(8) . . ?
N13 C22 N12 111.1(7) . . ?
C23 C22 N12 126.4(7) . . ?
C22 C23 C24 116.3(7) . . ?
C22 C23 H23 121.8 . . ?
C24 C23 H23 121.8 . . ?
C23 C24 C25 119.4(7) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 120.0(8) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N13 C26 C25 120.1(8) . . ?
N13 C26 C27 112.6(7) . . ?
C25 C26 C27 127.2(8) . . ?
N14 C27 C26 113.6(7) . . ?
N14 C27 H27 123.2 . . ?
C26 C27 H27 123.2 . . ?
N5 C28 N10 120.9(7) . . ?
N5 C28 N15 120.5(7) . . ?
N10 C28 N15 118.6(7) . . ?

_refine_diff_density_max         3.245
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.221

_shelxl_version_number           2013-4


####################################################################### 
# 
# 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_[Ni3]
_database_code_depnum_ccdc_archive 'CCDC 1403545'
_audit_update_record             
;
2015-05-28 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         "C33 H36 N15 Ni3 O6', 'B4 F16', 'C H4 O"
_chemical_formula_sum            'C34 H47 B4 F16 N15 Ni3 O7'
_chemical_formula_weight         1301.23

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0521(8)
_cell_length_b                   11.4299(9)
_cell_length_c                   22.6136(18)
_cell_angle_alpha                77.6660(10)
_cell_angle_beta                 83.379(2)
_cell_angle_gamma                83.524(2)
_cell_volume                     2510.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3126
_cell_measurement_theta_min      2.3255
_cell_measurement_theta_max      25.37

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.235
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_T_max  0.8865
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            14336
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         0.926
_diffrn_reflns_theta_max         26.035
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             9666
_reflns_number_gt                7159
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1083P)²+12.2786P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9666
_refine_ls_number_parameters     719
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.2276
_refine_ls_wR_factor_gt          0.2075
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.96968(8) 0.42994(7) 0.71336(4) 0.0239(2) Uani 1 1 d . . . . .
Ni2 Ni 0.61919(8) 0.20608(7) 0.84947(4) 0.0240(2) Uani 1 1 d . . . . .
Ni3 Ni 0.73942(8) 0.13032(7) 0.63984(4) 0.0242(2) Uani 1 1 d . . . . .
O1 O 0.8350(5) 0.5710(4) 0.6731(2) 0.0343(11) Uani 1 1 d . . . . .
O2 O 1.1186(5) 0.2922(5) 0.7431(3) 0.0469(14) Uani 1 1 d . . . . .
O3 O 0.4746(5) 0.3442(4) 0.8215(2) 0.0356(11) Uani 1 1 d . . . . .
O4 O 0.7687(5) 0.0770(4) 0.8903(2) 0.0312(11) Uani 1 1 d . . . . .
O5 O 0.5897(5) 0.2621(5) 0.6108(3) 0.0532(16) Uani 1 1 d . . . . .
O6 O 0.8828(5) -0.0138(4) 0.6684(2) 0.0328(11) Uani 1 1 d . . . . .
N1 N 1.1286(6) 0.5254(5) 0.6634(3) 0.0324(13) Uani 1 1 d . . . . .
N2 N 1.1730(6) 0.6010(5) 0.6960(3) 0.0323(13) Uani 1 1 d . . . . .
N3 N 1.0102(6) 0.5319(5) 0.7697(3) 0.0303(13) Uani 1 1 d . . . . .
N4 N 0.8408(5) 0.3783(5) 0.7875(2) 0.0255(12) Uani 1 1 d . . . . .
N5 N 0.7623(5) 0.2902(5) 0.7883(2) 0.0247(12) Uani 1 1 d . . . . .
N6 N 0.5548(6) 0.2293(5) 0.9405(3) 0.0328(13) Uani 1 1 d . . . . .
N7 N 0.4483(6) 0.1618(5) 0.9645(3) 0.0316(13) Uani 1 1 d . . . . .
N8 N 0.4779(5) 0.0920(5) 0.8769(2) 0.0261(12) Uani 1 1 d . . . . .
N9 N 0.6196(5) 0.1300(5) 0.7759(2) 0.0260(12) Uani 1 1 d . . . . .
N10 N 0.7043(5) 0.1649(5) 0.7262(2) 0.0260(12) Uani 1 1 d . . . . .
N11 N 0.6487(6) 0.0062(5) 0.6024(3) 0.0352(14) Uani 1 1 d . . . . .
N12 N 0.7061(6) 0.0042(5) 0.5441(3) 0.0352(14) Uani 1 1 d . . . . .
N13 N 0.8330(6) 0.1475(5) 0.5560(3) 0.0296(13) Uani 1 1 d . . . . .
N14 N 0.8685(5) 0.2544(5) 0.6389(3) 0.0255(12) Uani 1 1 d . . . . .
N15 N 0.8701(5) 0.3016(5) 0.6888(3) 0.0278(12) Uani 1 1 d . . . . .
C1 C 1.2121(7) 0.5340(6) 0.6133(3) 0.0350(16) Uani 1 1 d . . . . .
H1 H 1.2053 0.4936 0.5813 0.042 Uiso 1 1 calc R U . . .
C2 C 1.3121(8) 0.6102(7) 0.6133(4) 0.0423(19) Uani 1 1 d . . . . .
H2 H 1.3848 0.6291 0.5832 0.051 Uiso 1 1 calc R U . . .
C3 C 1.2822(8) 0.6510(6) 0.6658(4) 0.0386(18) Uani 1 1 d . . . . .
H3 H 1.3306 0.7059 0.6790 0.046 Uiso 1 1 calc R U . . .
C4 C 1.1051(7) 0.6065(6) 0.7538(3) 0.0315(16) Uani 1 1 d . . . . .
C5 C 1.1318(8) 0.6817(6) 0.7907(4) 0.0388(18) Uani 1 1 d . . . . .
H5 H 1.2010 0.7346 0.7792 0.047 Uiso 1 1 calc R U . . .
C6 C 1.0524(8) 0.6754(6) 0.8450(4) 0.0412(19) Uani 1 1 d . . . . .
H6 H 1.0663 0.7267 0.8713 0.049 Uiso 1 1 calc R U . . .
C7 C 0.9532(8) 0.5970(7) 0.8626(4) 0.0405(18) Uani 1 1 d . . . . .
H7 H 0.8995 0.5933 0.9002 0.049 Uiso 1 1 calc R U . . .
C8 C 0.9354(7) 0.5239(6) 0.8229(3) 0.0316(15) Uani 1 1 d . . . . .
C9 C 0.8392(7) 0.4321(6) 0.8318(3) 0.0289(15) Uani 1 1 d . . . . .
H9 H 0.7803 0.4141 0.8678 0.035 Uiso 1 1 calc R U . . .
C10 C 0.5724(7) 0.2890(7) 0.9825(3) 0.0347(16) Uani 1 1 d . . . . .
H10 H 0.6397 0.3429 0.9788 0.042 Uiso 1 1 calc R U . . .
C11 C 0.4781(8) 0.2625(7) 1.0338(3) 0.0395(18) Uani 1 1 d . . . . .
H11 H 0.4699 0.2935 1.0699 0.047 Uiso 1 1 calc R U . . .
C12 C 0.4012(7) 0.1821(7) 1.0199(3) 0.0373(18) Uani 1 1 d . . . . .
H12 H 0.3277 0.1470 1.0450 0.045 Uiso 1 1 calc R U . . .
C13 C 0.4033(7) 0.0878(6) 0.9300(3) 0.0296(15) Uani 1 1 d . . . . .
C14 C 0.2969(7) 0.0173(7) 0.9476(3) 0.0367(17) Uani 1 1 d . . . . .
H14 H 0.2450 0.0150 0.9856 0.044 Uiso 1 1 calc R U . . .
C15 C 0.2702(7) -0.0495(7) 0.9070(3) 0.0344(16) Uani 1 1 d . . . . .
H15 H 0.1979 -0.0992 0.9175 0.041 Uiso 1 1 calc R U . . .
C16 C 0.3455(7) -0.0467(6) 0.8512(3) 0.0306(15) Uani 1 1 d . . . . .
H16 H 0.3262 -0.0933 0.8236 0.037 Uiso 1 1 calc R U . . .
C17 C 0.4505(6) 0.0275(6) 0.8375(3) 0.0259(14) Uani 1 1 d . . . . .
C18 C 0.5378(6) 0.0505(6) 0.7799(3) 0.0231(13) Uani 1 1 d . . . . .
H18 H 0.5334 0.0090 0.7481 0.028 Uiso 1 1 calc R U . . .
C19 C 0.5641(8) -0.0790(7) 0.6144(4) 0.046(2) Uani 1 1 d . . . . .
H19 H 0.5094 -0.0990 0.6516 0.056 Uiso 1 1 calc R U . . .
C20 C 0.5660(9) -0.1354(8) 0.5653(4) 0.056(2) Uani 1 1 d . . . . .
H20 H 0.5137 -0.1980 0.5627 0.067 Uiso 1 1 calc R U . . .
C21 C 0.6587(9) -0.0819(8) 0.5217(4) 0.049(2) Uani 1 1 d . . . . .
H21 H 0.6848 -0.1016 0.4830 0.059 Uiso 1 1 calc R U . . .
C22 C 0.8052(7) 0.0825(6) 0.5181(3) 0.0302(15) Uani 1 1 d . . . . .
C23 C 0.8689(8) 0.0925(7) 0.4598(3) 0.0388(18) Uani 1 1 d . . . . .
H23 H 0.8479 0.0457 0.4327 0.047 Uiso 1 1 calc R U . . .
C24 C 0.9640(8) 0.1736(7) 0.4434(3) 0.0387(18) Uani 1 1 d . . . . .
H24 H 1.0094 0.1841 0.4036 0.046 Uiso 1 1 calc R U . . .
C25 C 0.9952(8) 0.2403(7) 0.4831(3) 0.0361(17) Uani 1 1 d . . . . .
H25 H 1.0620 0.2955 0.4712 0.043 Uiso 1 1 calc R U . . .
C26 C 0.9278(7) 0.2253(6) 0.5404(3) 0.0315(15) Uani 1 1 d . . . . .
C27 C 0.9450(7) 0.2869(6) 0.5896(3) 0.0280(14) Uani 1 1 d . . . . .
H27 H 1.0072 0.3456 0.5854 0.034 Uiso 1 1 calc R U . . .
C28 C 0.7796(6) 0.2522(5) 0.7347(3) 0.0206(13) Uani 1 1 d . . . . .
C29 C 1.1577(13) 0.2559(9) 0.8022(6) 0.090(4) Uani 1 1 d . . . . .
H29A H 1.1432 0.3244 0.8226 0.135 Uiso 1 1 calc R U . . .
H29B H 1.2532 0.2264 0.8004 0.135 Uiso 1 1 calc R U . . .
H29C H 1.1041 0.1915 0.8249 0.135 Uiso 1 1 calc R U . . .
C30 C 0.4655(11) 0.4192(9) 0.7626(4) 0.062(3) Uani 1 1 d . . . . .
H30A H 0.5259 0.3836 0.7327 0.093 Uiso 1 1 calc R U . . .
H30B H 0.4916 0.4991 0.7630 0.093 Uiso 1 1 calc R U . . .
H30C H 0.3729 0.4263 0.7519 0.093 Uiso 1 1 calc R U . . .
C31 C 0.8570(8) 0.0007(7) 0.8563(4) 0.0426(19) Uani 1 1 d . . . . .
H31A H 0.8048 -0.0565 0.8445 0.064 Uiso 1 1 calc R U . . .
H31B H 0.9266 -0.0434 0.8817 0.064 Uiso 1 1 calc R U . . .
H31C H 0.8996 0.0504 0.8198 0.064 Uiso 1 1 calc R U . . .
C32 C 0.4546(9) 0.2639(10) 0.6284(5) 0.075(3) Uani 1 1 d . . . . .
H32A H 0.4074 0.2493 0.5954 0.112 Uiso 1 1 calc R U . . .
H32B H 0.4212 0.3426 0.6375 0.112 Uiso 1 1 calc R U . . .
H32C H 0.4385 0.2010 0.6647 0.112 Uiso 1 1 calc R U . . .
C33 C 0.8444(8) -0.1205(7) 0.7081(4) 0.0423(18) Uani 1 1 d . . . . .
H33A H 0.7958 -0.1007 0.7453 0.063 Uiso 1 1 calc R U . . .
H33B H 0.9249 -0.1747 0.7183 0.063 Uiso 1 1 calc R U . . .
H33C H 0.7860 -0.1600 0.6881 0.063 Uiso 1 1 calc R U . . .
F1 F 0.9283(7) 0.1569(6) 0.9561(3) 0.0840(19) Uani 1 1 d . . . . .
F2 F 1.0106(8) 0.2024(6) 1.0341(3) 0.103(3) Uani 1 1 d . . . . .
F3 F 0.9021(7) 0.3461(6) 0.9701(3) 0.100(2) Uani 1 1 d . . . . .
F4 F 1.1041(7) 0.2630(7) 0.9433(4) 0.108(3) Uani 1 1 d . . . . .
F5 F 0.2070(6) 0.0866(5) 0.6256(2) 0.0641(15) Uani 1 1 d . . . . .
F6 F 0.0887(5) 0.0619(6) 0.7160(3) 0.0709(17) Uani 1 1 d . . . . .
F7 F 0.1903(8) -0.0932(5) 0.6810(3) 0.097(2) Uani 1 1 d . . . . .
F8 F 0.3086(6) 0.0322(10) 0.7113(3) 0.135(4) Uani 1 1 d . . . . .
F9 F 0.6623(7) 0.4395(5) 0.5190(2) 0.0677(16) Uani 1 1 d . . . . .
F10 F 0.6555(7) 0.5374(7) 0.5957(3) 0.087(2) Uani 1 1 d . . . . .
F11 F 0.6377(15) 0.6400(6) 0.5024(4) 0.196(6) Uani 1 1 d . . . . .
F12 F 0.8247(8) 0.5460(8) 0.5266(6) 0.169(5) Uani 1 1 d . . . . .
F13 F 0.6280(5) 0.7873(5) 0.8222(2) 0.0583(13) Uani 1 1 d . . . . .
F14 F 0.5494(12) 0.6087(7) 0.8435(3) 0.146(4) Uani 1 1 d . . . . .
F15 F 0.6724(7) 0.6607(6) 0.7572(3) 0.093(2) Uani 1 1 d . . . . .
F16 F 0.4723(7) 0.7553(7) 0.7666(4) 0.122(3) Uani 1 1 d . . . . .
B1 B 0.9858(9) 0.2433(8) 0.9761(4) 0.0349(18) Uani 1 1 d . . . . .
B2 B 0.2066(9) 0.0244(8) 0.6840(4) 0.0380(19) Uani 1 1 d . . . . .
B3 B 0.6944(13) 0.5422(9) 0.5360(5) 0.054(3) Uani 1 1 d . . . . .
B4 B 0.5760(13) 0.7023(10) 0.7986(5) 0.056(3) Uani 1 1 d . . . . .
O1S O 0.2843(6) 0.4248(5) 0.8970(3) 0.0541(16) Uani 1 1 d . . . . .
H1S H 0.2505 0.3629 0.9172 0.081 Uiso 1 1 calc R U . . .
C1S C 0.2876(11) 0.5080(9) 0.9352(5) 0.067(3) Uani 1 1 d . . . . .
H1S1 H 0.3287 0.4671 0.9722 0.101 Uiso 1 1 calc R U . . .
H1S2 H 0.1957 0.5406 0.9459 0.101 Uiso 1 1 calc R U . . .
H1S3 H 0.3407 0.5737 0.9136 0.101 Uiso 1 1 calc R U . . .


_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 N3 2.002(6) . ?
Ni1 N4 2.021(5) . ?
Ni1 N15 2.066(6) . ?
Ni1 O2 2.102(5) . ?
Ni1 O1 2.104(5) . ?
Ni1 N1 2.114(6) . ?
Ni2 N8 1.992(5) . ?
Ni2 N9 2.034(5) . ?
Ni2 N5 2.047(5) . ?
Ni2 O3 2.067(5) . ?
Ni2 O4 2.128(5) . ?
Ni2 N6 2.148(6) . ?
Ni3 N13 1.997(6) . ?
Ni3 N14 2.022(5) . ?
Ni3 N10 2.057(5) . ?
Ni3 O5 2.063(5) . ?
Ni3 O6 2.105(5) . ?
Ni3 N11 2.132(6) . ?
O2 C29 1.400(12) . ?
O3 C30 1.427(10) . ?
O4 C31 1.448(8) . ?
O5 C32 1.370(11) . ?
O6 C33 1.414(9) . ?
N1 C1 1.322(9) . ?
N1 N2 1.389(8) . ?
N2 C3 1.341(10) . ?
N2 C4 1.413(10) . ?
N3 C4 1.319(9) . ?
N3 C8 1.334(9) . ?
N4 C9 1.280(8) . ?
N4 N5 1.344(7) . ?
N5 C28 1.359(8) . ?
N6 C10 1.321(9) . ?
N6 N7 1.381(8) . ?
N7 C12 1.346(9) . ?
N7 C13 1.407(9) . ?
N8 C13 1.334(8) . ?
N8 C17 1.341(9) . ?
N9 C18 1.276(8) . ?
N9 N10 1.347(7) . ?
N10 C28 1.376(8) . ?
N11 C19 1.329(9) . ?
N11 N12 1.380(9) . ?
N12 C21 1.352(10) . ?
N12 C22 1.407(9) . ?
N13 C22 1.319(9) . ?
N13 C26 1.343(9) . ?
N14 C27 1.288(8) . ?
N14 N15 1.355(8) . ?
N15 C28 1.368(8) . ?
C1 C2 1.402(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.356(11) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.384(10) . ?
C5 C6 1.379(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.472(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.412(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.371(11) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.383(10) . ?
C14 C15 1.378(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.474(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.394(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.369(13) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.384(10) . ?
C23 C24 1.372(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.376(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.474(9) . ?
C27 H27 0.9500 . ?
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 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
F1 B1 1.376(10) . ?
F2 B1 1.336(10) . ?
F3 B1 1.357(10) . ?
F4 B1 1.342(10) . ?
F5 B2 1.361(10) . ?
F6 B2 1.390(10) . ?
F7 B2 1.389(11) . ?
F8 B2 1.276(11) . ?
F9 B3 1.391(11) . ?
F10 B3 1.352(12) . ?
F11 B3 1.320(13) . ?
F12 B3 1.307(14) . ?
F13 B4 1.379(12) . ?
F14 B4 1.335(12) . ?
F15 B4 1.386(11) . ?
F16 B4 1.350(14) . ?
O1S C1S 1.419(11) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N4 77.6(2) . . ?
N3 Ni1 N15 154.5(2) . . ?
N4 Ni1 N15 76.9(2) . . ?
N3 Ni1 O2 93.4(2) . . ?
N4 Ni1 O2 92.9(2) . . ?
N15 Ni1 O2 87.7(2) . . ?
N3 Ni1 O1 89.6(2) . . ?
N4 Ni1 O1 94.1(2) . . ?
N15 Ni1 O1 92.3(2) . . ?
O2 Ni1 O1 172.9(2) . . ?
N3 Ni1 N1 77.2(2) . . ?
N4 Ni1 N1 154.7(2) . . ?
N15 Ni1 N1 128.3(2) . . ?
O2 Ni1 N1 86.4(2) . . ?
O1 Ni1 N1 88.0(2) . . ?
N8 Ni2 N9 77.8(2) . . ?
N8 Ni2 N5 154.4(2) . . ?
N9 Ni2 N5 76.5(2) . . ?
N8 Ni2 O3 90.6(2) . . ?
N9 Ni2 O3 94.8(2) . . ?
N5 Ni2 O3 90.9(2) . . ?
N8 Ni2 O4 91.6(2) . . ?
N9 Ni2 O4 94.4(2) . . ?
N5 Ni2 O4 90.9(2) . . ?
O3 Ni2 O4 170.84(19) . . ?
N8 Ni2 N6 76.7(2) . . ?
N9 Ni2 N6 154.5(2) . . ?
N5 Ni2 N6 128.9(2) . . ?
O3 Ni2 N6 86.6(2) . . ?
O4 Ni2 N6 85.2(2) . . ?
N13 Ni3 N14 77.7(2) . . ?
N13 Ni3 N10 154.6(2) . . ?
N14 Ni3 N10 76.9(2) . . ?
N13 Ni3 O5 91.8(2) . . ?
N14 Ni3 O5 91.7(2) . . ?
N10 Ni3 O5 90.3(2) . . ?
N13 Ni3 O6 88.4(2) . . ?
N14 Ni3 O6 92.6(2) . . ?
N10 Ni3 O6 91.4(2) . . ?
O5 Ni3 O6 175.6(2) . . ?
N13 Ni3 N11 77.2(2) . . ?
N14 Ni3 N11 154.9(2) . . ?
N10 Ni3 N11 128.2(2) . . ?
O5 Ni3 N11 89.7(2) . . ?
O6 Ni3 N11 86.0(2) . . ?
C29 O2 Ni1 126.6(6) . . ?
C30 O3 Ni2 128.5(5) . . ?
C31 O4 Ni2 122.3(4) . . ?
C32 O5 Ni3 128.0(6) . . ?
C33 O6 Ni3 121.2(4) . . ?
C1 N1 N2 104.8(6) . . ?
C1 N1 Ni1 143.4(5) . . ?
N2 N1 Ni1 111.4(4) . . ?
C3 N2 N1 110.0(6) . . ?
C3 N2 C4 132.2(6) . . ?
N1 N2 C4 117.7(6) . . ?
C4 N3 C8 121.6(6) . . ?
C4 N3 Ni1 120.8(5) . . ?
C8 N3 Ni1 117.6(5) . . ?
C9 N4 N5 123.4(6) . . ?
C9 N4 Ni1 117.4(5) . . ?
N5 N4 Ni1 119.3(4) . . ?
N4 N5 C28 111.4(5) . . ?
N4 N5 Ni2 135.1(4) . . ?
C28 N5 Ni2 113.5(4) . . ?
C10 N6 N7 105.3(6) . . ?
C10 N6 Ni2 144.3(5) . . ?
N7 N6 Ni2 110.3(4) . . ?
C12 N7 N6 110.7(6) . . ?
C12 N7 C13 129.9(6) . . ?
N6 N7 C13 119.4(5) . . ?
C13 N8 C17 120.4(6) . . ?
C13 N8 Ni2 121.8(5) . . ?
C17 N8 Ni2 117.5(4) . . ?
C18 N9 N10 123.5(6) . . ?
C18 N9 Ni2 117.1(4) . . ?
N10 N9 Ni2 119.5(4) . . ?
N9 N10 C28 110.6(5) . . ?
N9 N10 Ni3 136.5(4) . . ?
C28 N10 Ni3 112.7(4) . . ?
C19 N11 N12 104.7(6) . . ?
C19 N11 Ni3 144.7(6) . . ?
N12 N11 Ni3 110.3(4) . . ?
C21 N12 N11 111.1(6) . . ?
C21 N12 C22 129.6(7) . . ?
N11 N12 C22 119.2(6) . . ?
C22 N13 C26 121.3(6) . . ?
C22 N13 Ni3 121.2(5) . . ?
C26 N13 Ni3 117.4(4) . . ?
C27 N14 N15 122.5(5) . . ?
C27 N14 Ni3 117.9(4) . . ?
N15 N14 Ni3 119.5(4) . . ?
N14 N15 C28 111.0(5) . . ?
N14 N15 Ni1 137.0(4) . . ?
C28 N15 Ni1 112.0(4) . . ?
N1 C1 C2 111.6(7) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C3 C2 C1 104.7(7) . . ?
C3 C2 H2 127.6 . . ?
C1 C2 H2 127.6 . . ?
N2 C3 C2 108.9(6) . . ?
N2 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
N3 C4 C5 122.2(7) . . ?
N3 C4 N2 112.8(6) . . ?
C5 C4 N2 125.0(7) . . ?
C6 C5 C4 116.2(7) . . ?
C6 C5 H5 121.9 . . ?
C4 C5 H5 121.9 . . ?
C5 C6 C7 122.2(7) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C6 C7 C8 117.3(8) . . ?
C6 C7 H7 121.3 . . ?
C8 C7 H7 121.3 . . ?
N3 C8 C7 120.4(7) . . ?
N3 C8 C9 112.1(6) . . ?
C7 C8 C9 127.5(7) . . ?
N4 C9 C8 115.2(6) . . ?
N4 C9 H9 122.4 . . ?
C8 C9 H9 122.4 . . ?
N6 C10 C11 111.2(7) . . ?
N6 C10 H10 124.4 . . ?
C11 C10 H10 124.4 . . ?
C12 C11 C10 104.8(6) . . ?
C12 C11 H11 127.6 . . ?
C10 C11 H11 127.6 . . ?
N7 C12 C11 107.9(6) . . ?
N7 C12 H12 126.0 . . ?
C11 C12 H12 126.0 . . ?
N8 C13 C14 122.9(7) . . ?
N8 C13 N7 111.4(6) . . ?
C14 C13 N7 125.7(6) . . ?
C15 C14 C13 116.4(6) . . ?
C15 C14 H14 121.8 . . ?
C13 C14 H14 121.8 . . ?
C14 C15 C16 122.2(7) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C17 117.0(7) . . ?
C15 C16 H16 121.5 . . ?
C17 C16 H16 121.5 . . ?
N8 C17 C16 121.1(6) . . ?
N8 C17 C18 112.3(6) . . ?
C16 C17 C18 126.5(6) . . ?
N9 C18 C17 115.3(6) . . ?
N9 C18 H18 122.4 . . ?
C17 C18 H18 122.4 . . ?
N11 C19 C20 111.3(8) . . ?
N11 C19 H19 124.3 . . ?
C20 C19 H19 124.3 . . ?
C21 C20 C19 105.8(7) . . ?
C21 C20 H20 127.1 . . ?
C19 C20 H20 127.1 . . ?
N12 C21 C20 107.0(7) . . ?
N12 C21 H21 126.5 . . ?
C20 C21 H21 126.5 . . ?
N13 C22 C23 122.3(7) . . ?
N13 C22 N12 112.1(6) . . ?
C23 C22 N12 125.6(6) . . ?
C24 C23 C22 116.5(7) . . ?
C24 C23 H23 121.8 . . ?
C22 C23 H23 121.8 . . ?
C23 C24 C25 121.5(7) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 118.7(7) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
N13 C26 C25 119.6(7) . . ?
N13 C26 C27 112.7(6) . . ?
C25 C26 C27 127.7(7) . . ?
N14 C27 C26 114.2(6) . . ?
N14 C27 H27 122.9 . . ?
C26 C27 H27 122.9 . . ?
N5 C28 N15 120.4(5) . . ?
N5 C28 N10 119.9(5) . . ?
N15 C28 N10 119.8(5) . . ?
O2 C29 H29A 109.5 . . ?
O2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O3 C30 H30A 109.5 . . ?
O3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O4 C31 H31A 109.5 . . ?
O4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O5 C32 H32A 109.5 . . ?
O5 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O5 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O6 C33 H33A 109.5 . . ?
O6 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O6 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
F2 B1 F4 107.6(8) . . ?
F2 B1 F3 111.0(8) . . ?
F4 B1 F3 110.5(8) . . ?
F2 B1 F1 109.2(7) . . ?
F4 B1 F1 108.9(7) . . ?
F3 B1 F1 109.7(7) . . ?
F8 B2 F5 115.7(8) . . ?
F8 B2 F7 112.7(9) . . ?
F5 B2 F7 104.8(7) . . ?
F8 B2 F6 110.5(8) . . ?
F5 B2 F6 107.9(7) . . ?
F7 B2 F6 104.4(7) . . ?
F12 B3 F11 108.0(11) . . ?
F12 B3 F10 109.2(10) . . ?
F11 B3 F10 110.7(10) . . ?
F12 B3 F9 108.2(9) . . ?
F11 B3 F9 110.8(9) . . ?
F10 B3 F9 109.9(8) . . ?
F14 B4 F16 116.3(11) . . ?
F14 B4 F13 108.9(9) . . ?
F16 B4 F13 109.1(8) . . ?
F14 B4 F15 107.3(9) . . ?
F16 B4 F15 105.9(9) . . ?
F13 B4 F15 109.0(9) . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

_refine_diff_density_max         1.975
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.159

_shelxl_version_number           2013-4



