#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:17:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179239 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/59/4315901.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4315901
loop_
_publ_author_name
'Jue-Chao Jiang'
'Zhao-Lian Chu'
'Wei Huang'
'Gang Wang'
'Xiao-Zeng You'
_publ_section_title
;
 Dinuclear Cadmium(II), Zinc(II), and Manganese(II), Trinuclear
 Nickel(II), and Pentanuclear Copper(II) Complexes with Novel Macrocyclic
 and Acyclic Schiff-Base Ligands Having Enantiopure or Racemic Camphoric
 Diamine Components
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5897
_journal_page_last               5911
_journal_paper_doi               10.1021/ic100349d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C48 H60 Cl4 N6 Ni3 O6, 2(N O3), 4(H2 O)'
_chemical_formula_sum            'C48 H68 Cl4 N8 Ni3 O16'
_chemical_formula_weight         1331.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.563(5)
_cell_angle_beta                 99.788(5)
_cell_angle_gamma                94.268(5)
_cell_formula_units_Z            2
_cell_length_a                   10.096(3)
_cell_length_b                   14.177(4)
_cell_length_c                   20.940(6)
_cell_measurement_reflns_used    2709
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      22.331
_cell_measurement_theta_min      2.322
_cell_volume                     2927.0(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (BRUKER 2000)'
_computing_data_reduction        'SAINT (BRUKER 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (BRUKER 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.1144
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14632
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.8395
_exptl_absorpt_correction_T_min  0.7940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         10114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0631P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                6150
_reflns_number_total             10114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100349d_si_002_11.cif
_cod_data_source_block           11
_cod_database_code               4315901
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.78833(7) 0.27792(5) 0.86085(3) 0.0328(2) Uani 1 1 d . . .
Ni2 Ni 0.71354(8) 0.06110(5) 0.76425(3) 0.0347(2) Uani 1 1 d . . .
Ni3 Ni 0.62749(8) 0.26963(5) 0.70351(4) 0.0369(2) Uani 1 1 d . . .
C1 C 0.8387(6) 0.4168(4) 0.7720(3) 0.0362(15) Uani 1 1 d . . .
C2 C 0.8980(6) 0.4355(5) 0.7185(3) 0.0413(16) Uani 1 1 d . . .
C3 C 0.9589(7) 0.5248(5) 0.7149(3) 0.0552(19) Uani 1 1 d . . .
H3 H 0.9995 0.5361 0.6794 0.066 Uiso 1 1 calc R . .
C4 C 0.9597(7) 0.5976(5) 0.7641(4) 0.058(2) Uani 1 1 d . . .
C5 C 0.8958(7) 0.5830(4) 0.8149(3) 0.0498(18) Uani 1 1 d . . .
H5 H 0.8927 0.6334 0.8463 0.060 Uiso 1 1 calc R . .
C6 C 0.8340(6) 0.4920(4) 0.8206(3) 0.0384(15) Uani 1 1 d . . .
C7 C 0.8850(6) 0.3572(5) 0.6645(3) 0.0507(18) Uani 1 1 d . . .
H7 H 0.9565 0.3298 0.6495 0.061 Uiso 1 1 calc R . .
C8 C 0.7615(6) 0.4827(4) 0.8745(3) 0.0398(16) Uani 1 1 d . . .
H8 H 0.7420 0.5384 0.8968 0.048 Uiso 1 1 calc R . .
C9 C 0.6493(6) 0.4103(4) 0.9480(3) 0.0397(15) Uani 1 1 d . . .
H9 H 0.6252 0.4755 0.9564 0.048 Uiso 1 1 calc R . .
C10 C 0.7311(6) 0.3799(4) 1.0115(3) 0.0370(15) Uani 1 1 d . . .
C11 C 0.7053(6) 0.2708(4) 1.0006(3) 0.0350(14) Uani 1 1 d . . .
C12 C 0.5572(6) 0.2522(4) 0.9694(3) 0.0453(16) Uani 1 1 d . . .
H12A H 0.5017 0.2434 1.0023 0.054 Uiso 1 1 calc R . .
H12B H 0.5425 0.1956 0.9382 0.054 Uiso 1 1 calc R . .
C13 C 0.5218(6) 0.3412(4) 0.9348(3) 0.0464(17) Uani 1 1 d . . .
H13A H 0.4932 0.3236 0.8883 0.056 Uiso 1 1 calc R . .
H13B H 0.4492 0.3704 0.9518 0.056 Uiso 1 1 calc R . .
C14 C 0.8756(6) 0.4202(4) 1.0252(3) 0.0437(16) Uani 1 1 d . . .
H14A H 0.9219 0.3963 1.0634 0.066 Uiso 1 1 calc R . .
H14B H 0.8801 0.4883 1.0323 0.066 Uiso 1 1 calc R . .
H14C H 0.9176 0.4017 0.9886 0.066 Uiso 1 1 calc R . .
C15 C 0.6647(7) 0.4196(4) 1.0690(3) 0.0532(18) Uani 1 1 d . . .
H15A H 0.7172 0.4072 1.1095 0.080 Uiso 1 1 calc R . .
H15B H 0.5749 0.3892 1.0645 0.080 Uiso 1 1 calc R . .
H15C H 0.6609 0.4870 1.0686 0.080 Uiso 1 1 calc R . .
C16 C 0.7422(7) 0.2237(4) 1.0625(3) 0.0529(18) Uani 1 1 d . . .
H16A H 0.6894 0.2461 1.0940 0.079 Uiso 1 1 calc R . .
H16B H 0.8364 0.2393 1.0800 0.079 Uiso 1 1 calc R . .
H16C H 0.7241 0.1559 1.0527 0.079 Uiso 1 1 calc R . .
C17 C 1.0799(6) 0.2732(4) 0.8485(3) 0.0394(15) Uani 1 1 d . . .
H17 H 1.1247 0.2948 0.8166 0.047 Uiso 1 1 calc R . .
C18 C 1.0822(6) 0.1760(4) 0.8701(3) 0.0342(14) Uani 1 1 d . . .
C19 C 0.9616(6) 0.1185(4) 0.8575(3) 0.0324(14) Uani 1 1 d . . .
C20 C 0.9538(6) 0.0290(4) 0.8829(3) 0.0333(14) Uani 1 1 d . . .
C21 C 1.0706(6) 0.0034(4) 0.9221(3) 0.0355(14) Uani 1 1 d . . .
H21 H 1.0680 -0.0538 0.9403 0.043 Uiso 1 1 calc R . .
C22 C 1.1869(6) 0.0618(4) 0.9333(3) 0.0376(15) Uani 1 1 d . . .
C23 C 1.1956(6) 0.1471(4) 0.9065(3) 0.0372(15) Uani 1 1 d . . .
H23 H 1.2774 0.1845 0.9131 0.045 Uiso 1 1 calc R . .
C24 C 0.8317(6) -0.0322(4) 0.8752(3) 0.0370(15) Uani 1 1 d . . .
H24 H 0.8329 -0.0819 0.9012 0.044 Uiso 1 1 calc R . .
C25 C 0.6040(6) -0.0918(4) 0.8411(3) 0.0391(15) Uani 1 1 d . . .
H25 H 0.6255 -0.1276 0.8787 0.047 Uiso 1 1 calc R . .
C26 C 0.5568(6) -0.1617(4) 0.7780(3) 0.0406(15) Uani 1 1 d . . .
C27 C 0.4697(6) -0.1008(4) 0.7325(3) 0.0454(17) Uani 1 1 d . . .
C28 C 0.3953(7) -0.0448(5) 0.7793(3) 0.0580(19) Uani 1 1 d . . .
H28A H 0.3075 -0.0776 0.7794 0.070 Uiso 1 1 calc R . .
H28B H 0.3822 0.0180 0.7660 0.070 Uiso 1 1 calc R . .
C29 C 0.4825(6) -0.0365(5) 0.8476(3) 0.0494(17) Uani 1 1 d . . .
H29A H 0.5115 0.0297 0.8633 0.059 Uiso 1 1 calc R . .
H29B H 0.4318 -0.0632 0.8780 0.059 Uiso 1 1 calc R . .
C30 C 0.4650(7) -0.2423(4) 0.7966(3) 0.058(2) Uani 1 1 d . . .
H30A H 0.4350 -0.2887 0.7594 0.087 Uiso 1 1 calc R . .
H30B H 0.3882 -0.2165 0.8108 0.087 Uiso 1 1 calc R . .
H30C H 0.5145 -0.2720 0.8313 0.087 Uiso 1 1 calc R . .
C31 C 0.6728(7) -0.2042(5) 0.7516(3) 0.0572(19) Uani 1 1 d . . .
H31A H 0.7167 -0.2430 0.7824 0.086 Uiso 1 1 calc R . .
H31B H 0.7363 -0.1540 0.7449 0.086 Uiso 1 1 calc R . .
H31C H 0.6387 -0.2426 0.7110 0.086 Uiso 1 1 calc R . .
C32 C 0.3749(7) -0.1600(5) 0.6760(3) 0.068(2) Uani 1 1 d . . .
H32A H 0.3318 -0.1185 0.6470 0.102 Uiso 1 1 calc R . .
H32B H 0.3077 -0.1972 0.6925 0.102 Uiso 1 1 calc R . .
H32C H 0.4257 -0.2016 0.6527 0.102 Uiso 1 1 calc R . .
C33 C 0.9365(6) 0.0551(5) 0.6821(3) 0.0468(17) Uani 1 1 d . . .
H33 H 1.0260 0.0809 0.6916 0.056 Uiso 1 1 calc R . .
C34 C 0.8379(6) 0.0676(4) 0.6222(3) 0.0416(16) Uani 1 1 d . . .
C35 C 0.7239(6) 0.1147(4) 0.6303(3) 0.0371(15) Uani 1 1 d . . .
C36 C 0.6258(6) 0.1230(4) 0.5748(3) 0.0388(15) Uani 1 1 d . . .
C37 C 0.6444(7) 0.0835(4) 0.5136(3) 0.0468(17) Uani 1 1 d . . .
H37 H 0.5806 0.0886 0.4768 0.056 Uiso 1 1 calc R . .
C38 C 0.7550(7) 0.0378(5) 0.5081(3) 0.0451(16) Uani 1 1 d . . .
C39 C 0.8536(6) 0.0298(5) 0.5615(3) 0.0474(17) Uani 1 1 d . . .
H39 H 0.9299 -0.0008 0.5561 0.057 Uiso 1 1 calc R . .
C40 C 0.5038(6) 0.1691(4) 0.5773(3) 0.0445(16) Uani 1 1 d . . .
H40 H 0.4370 0.1595 0.5402 0.053 Uiso 1 1 calc R . .
C41 C 0.3466(6) 0.2582(5) 0.6218(3) 0.0551(19) Uani 1 1 d . . .
H41 H 0.2889 0.2293 0.5811 0.066 Uiso 1 1 calc R . .
C42 C 0.3488(7) 0.3685(5) 0.6251(3) 0.0566(19) Uani 1 1 d . . .
C43 C 0.3841(7) 0.3985(5) 0.7004(3) 0.056(2) Uani 1 1 d . . .
C44 C 0.3012(7) 0.3233(6) 0.7275(3) 0.067(2) Uani 1 1 d . . .
H44A H 0.2143 0.3451 0.7325 0.081 Uiso 1 1 calc R . .
H44B H 0.3479 0.3107 0.7698 0.081 Uiso 1 1 calc R . .
C45 C 0.2817(7) 0.2331(5) 0.6795(3) 0.061(2) Uani 1 1 d . . .
H45A H 0.1864 0.2131 0.6653 0.073 Uiso 1 1 calc R . .
H45B H 0.3249 0.1819 0.6998 0.073 Uiso 1 1 calc R . .
C46 C 0.4409(8) 0.4130(6) 0.5852(4) 0.077(2) Uani 1 1 d . . .
H46A H 0.4181 0.3841 0.5409 0.116 Uiso 1 1 calc R . .
H46B H 0.5326 0.4034 0.6026 0.116 Uiso 1 1 calc R . .
H46C H 0.4312 0.4800 0.5866 0.116 Uiso 1 1 calc R . .
C47 C 0.2056(7) 0.3913(6) 0.5984(4) 0.082(3) Uani 1 1 d . . .
H47A H 0.2007 0.4589 0.6045 0.123 Uiso 1 1 calc R . .
H47B H 0.1432 0.3603 0.6213 0.123 Uiso 1 1 calc R . .
H47C H 0.1829 0.3691 0.5528 0.123 Uiso 1 1 calc R . .
C48 C 0.3532(8) 0.5008(5) 0.7201(4) 0.086(3) Uani 1 1 d . . .
H48A H 0.3831 0.5168 0.7662 0.129 Uiso 1 1 calc R . .
H48B H 0.2578 0.5053 0.7095 0.129 Uiso 1 1 calc R . .
H48C H 0.3996 0.5440 0.6970 0.129 Uiso 1 1 calc R . .
Cl1 Cl 1.0397(2) 0.70921(15) 0.76029(11) 0.0941(8) Uani 1 1 d . . .
Cl2 Cl 1.32816(16) 0.03268(11) 0.98662(8) 0.0488(4) Uani 1 1 d . . .
Cl3 Cl 0.77770(19) -0.01431(15) 0.43111(8) 0.0676(6) Uani 1 1 d . . .
Cl4 Cl 0.56676(15) 0.18973(10) 0.79865(7) 0.0408(4) Uani 1 1 d . . .
N1 N 0.7228(5) 0.4039(3) 0.8936(2) 0.0358(12) Uani 1 1 d . . .
N2 N 0.7879(5) 0.2315(3) 0.9518(2) 0.0324(11) Uani 1 1 d . . .
H2A H 0.7641 0.1684 0.9446 0.039 Uiso 1 1 calc R . .
H2B H 0.8744 0.2387 0.9725 0.039 Uiso 1 1 calc R . .
N3 N 0.7207(5) -0.0258(3) 0.8365(2) 0.0355(12) Uani 1 1 d . . .
N4 N 0.5606(5) -0.0319(3) 0.7058(2) 0.0405(13) Uani 1 1 d . . .
H4A H 0.5064 0.0044 0.6821 0.049 Uiso 1 1 calc R . .
H4B H 0.6004 -0.0667 0.6775 0.049 Uiso 1 1 calc R . .
N5 N 0.4797(5) 0.2223(4) 0.6264(2) 0.0439(13) Uani 1 1 d . . .
N6 N 0.5286(5) 0.3897(4) 0.7223(2) 0.0483(14) Uani 1 1 d . . .
H6A H 0.5438 0.4032 0.7660 0.058 Uiso 1 1 calc R . .
H6B H 0.5730 0.4375 0.7068 0.058 Uiso 1 1 calc R . .
N7 N 0.8206(6) 0.7159(4) 0.9661(3) 0.0490(14) Uani 1 1 d . . .
N8 N 0.7685(15) 0.8164(8) 0.5925(5) 0.141(4) Uani 1 1 d . . .
O1 O 0.7858(4) 0.3290(3) 0.77494(17) 0.0339(9) Uani 1 1 d . . .
O2 O 0.7434(4) 0.3305(3) 0.63897(18) 0.0442(11) Uani 1 1 d . . .
O3 O 0.9976(4) 0.3283(2) 0.88468(18) 0.0346(10) Uani 1 1 d . . .
O4 O 0.8532(4) 0.1508(2) 0.82434(17) 0.0345(9) Uani 1 1 d . . .
O5 O 0.8708(4) -0.0036(3) 0.72307(18) 0.0425(10) Uani 1 1 d . . .
O6 O 0.7111(4) 0.1485(3) 0.68966(18) 0.0365(10) Uani 1 1 d . . .
O7 O 0.8180(5) 0.6551(3) 1.0061(2) 0.0590(13) Uani 1 1 d . . .
O8 O 0.9254(5) 0.7674(4) 0.9673(2) 0.0658(14) Uani 1 1 d . . .
O9 O 0.7175(6) 0.7215(4) 0.9262(3) 0.0884(19) Uani 1 1 d . . .
O10 O 0.6511(9) 0.8407(7) 0.5920(4) 0.132(3) Uani 1 1 d . . .
O11 O 0.7722(12) 0.7506(8) 0.5507(5) 0.267(8) Uani 1 1 d . . .
O12 O 0.8815(8) 0.8412(4) 0.6378(3) 0.111(2) Uani 1 1 d . . .
O13 O 0.7331(8) 0.3451(6) 0.5083(4) 0.172(4) Uani 1 1 d . . .
H13C H 0.7217 0.3995 0.5264 0.258 Uiso 1 1 d R . .
H13D H 0.7950 0.3208 0.5325 0.258 Uiso 1 1 d R . .
O14 O 0.4925(10) 0.3303(7) 0.4269(4) 0.204(4) Uani 1 1 d . . .
H14D H 0.4228 0.2913 0.4233 0.306 Uiso 1 1 d R . .
H14E H 0.5427 0.3284 0.4636 0.306 Uiso 1 1 d R . .
O15 O 0.9208(12) 0.2962(13) 0.4416(7) 0.391(12) Uani 1 1 d . . .
H15D H 0.9004 0.2415 0.4202 0.587 Uiso 1 1 d R . .
H15E H 0.9965 0.3008 0.4672 0.587 Uiso 1 1 d R . .
O16 O 0.806(3) 0.5377(10) 0.5649(7) 0.66(2) Uani 1 1 d . . .
H16D H 0.8371 0.5622 0.5343 0.990 Uiso 1 1 d R . .
H16E H 0.7608 0.5785 0.5815 0.990 Uiso 1 1 d R . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 N1 87.47(17) . . ?
O1 Ni1 N2 177.08(16) . . ?
N1 Ni1 N2 89.61(18) . . ?
O1 Ni1 O4 90.68(15) . . ?
N1 Ni1 O4 178.08(16) . . ?
N2 Ni1 O4 92.24(16) . . ?
O1 Ni1 O3 87.44(15) . . ?
N1 Ni1 O3 94.59(17) . . ?
N2 Ni1 O3 92.69(16) . . ?
O4 Ni1 O3 85.85(14) . . ?
O1 Ni1 Cl4 81.05(11) . . ?
N1 Ni1 Cl4 100.87(14) . . ?
N2 Ni1 Cl4 99.62(14) . . ?
O4 Ni1 Cl4 78.31(11) . . ?
O3 Ni1 Cl4 160.23(11) . . ?
O4 Ni2 N3 87.93(17) . . ?
O4 Ni2 O6 91.79(15) . . ?
N3 Ni2 O6 178.38(18) . . ?
O4 Ni2 N4 176.60(18) . . ?
N3 Ni2 N4 90.20(19) . . ?
O6 Ni2 N4 90.16(17) . . ?
O4 Ni2 O5 89.77(15) . . ?
N3 Ni2 O5 93.58(17) . . ?
O6 Ni2 O5 84.82(15) . . ?
N4 Ni2 O5 93.19(18) . . ?
O4 Ni2 Cl4 79.68(11) . . ?
N3 Ni2 Cl4 103.53(14) . . ?
O6 Ni2 Cl4 77.98(11) . . ?
N4 Ni2 Cl4 98.01(14) . . ?
O5 Ni2 Cl4 159.43(12) . . ?
O6 Ni3 N5 88.82(18) . . ?
O6 Ni3 O1 93.39(15) . . ?
N5 Ni3 O1 173.21(19) . . ?
O6 Ni3 N6 174.9(2) . . ?
N5 Ni3 N6 90.42(19) . . ?
O1 Ni3 N6 87.93(17) . . ?
O6 Ni3 O2 89.38(16) . . ?
N5 Ni3 O2 89.53(19) . . ?
O1 Ni3 O2 84.08(15) . . ?
N6 Ni3 O2 95.61(19) . . ?
O6 Ni3 Cl4 80.53(12) . . ?
N5 Ni3 Cl4 105.95(16) . . ?
O1 Ni3 Cl4 80.75(11) . . ?
N6 Ni3 Cl4 94.88(16) . . ?
O2 Ni3 Cl4 161.20(11) . . ?
O1 C1 C2 118.9(6) . . ?
O1 C1 C6 122.0(6) . . ?
C2 C1 C6 119.0(6) . . ?
C3 C2 C1 120.7(6) . . ?
C3 C2 C7 122.0(6) . . ?
C1 C2 C7 117.1(6) . . ?
C2 C3 C4 120.1(7) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.4(7) . . ?
C5 C4 Cl1 119.6(6) . . ?
C3 C4 Cl1 120.0(6) . . ?
C4 C5 C6 120.8(7) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 118.7(6) . . ?
C1 C6 C8 123.4(6) . . ?
C5 C6 C8 117.8(6) . . ?
O2 C7 C2 109.1(5) . . ?
O2 C7 H7 125.4 . . ?
C2 C7 H7 125.4 . . ?
N1 C8 C6 125.2(6) . . ?
N1 C8 H8 117.4 . . ?
C6 C8 H8 117.4 . . ?
N1 C9 C13 111.9(5) . . ?
N1 C9 C10 112.7(5) . . ?
C13 C9 C10 103.2(5) . . ?
N1 C9 H9 109.6 . . ?
C13 C9 H9 109.6 . . ?
C10 C9 H9 109.6 . . ?
C14 C10 C11 116.4(5) . . ?
C14 C10 C15 107.3(5) . . ?
C11 C10 C15 110.0(5) . . ?
C14 C10 C9 113.2(5) . . ?
C11 C10 C9 102.5(4) . . ?
C15 C10 C9 107.0(5) . . ?
N2 C11 C16 107.7(5) . . ?
N2 C11 C12 107.9(4) . . ?
C16 C11 C12 113.9(5) . . ?
N2 C11 C10 109.7(5) . . ?
C16 C11 C10 113.3(5) . . ?
C12 C11 C10 104.3(5) . . ?
C11 C12 C13 105.9(5) . . ?
C11 C12 H12A 110.6 . . ?
C13 C12 H12A 110.6 . . ?
C11 C12 H12B 110.6 . . ?
C13 C12 H12B 110.6 . . ?
H12A C12 H12B 108.7 . . ?
C9 C13 C12 107.0(5) . . ?
C9 C13 H13A 110.3 . . ?
C12 C13 H13A 110.3 . . ?
C9 C13 H13B 110.3 . . ?
C12 C13 H13B 110.3 . . ?
H13A C13 H13B 108.6 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C17 C18 109.3(5) . . ?
O3 C17 H17 125.3 . . ?
C18 C17 H17 125.3 . . ?
C23 C18 C19 120.5(5) . . ?
C23 C18 C17 121.9(5) . . ?
C19 C18 C17 117.3(5) . . ?
O4 C19 C18 118.6(5) . . ?
O4 C19 C20 121.3(5) . . ?
C18 C19 C20 120.0(5) . . ?
C21 C20 C19 117.8(5) . . ?
C21 C20 C24 118.5(5) . . ?
C19 C20 C24 123.5(5) . . ?
C22 C21 C20 120.4(5) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 121.7(5) . . ?
C21 C22 Cl2 119.7(5) . . ?
C23 C22 Cl2 118.5(5) . . ?
C18 C23 C22 119.5(6) . . ?
C18 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
N3 C24 C20 127.0(5) . . ?
N3 C24 H24 116.5 . . ?
C20 C24 H24 116.5 . . ?
N3 C25 C29 109.9(5) . . ?
N3 C25 C26 112.5(5) . . ?
C29 C25 C26 104.4(5) . . ?
N3 C25 H25 110.0 . . ?
C29 C25 H25 110.0 . . ?
C26 C25 H25 110.0 . . ?
C31 C26 C30 108.9(5) . . ?
C31 C26 C27 116.3(5) . . ?
C30 C26 C27 109.2(5) . . ?
C31 C26 C25 113.1(5) . . ?
C30 C26 C25 106.1(5) . . ?
C27 C26 C25 102.7(5) . . ?
N4 C27 C32 109.0(5) . . ?
N4 C27 C28 108.6(5) . . ?
C32 C27 C28 113.2(6) . . ?
N4 C27 C26 109.4(5) . . ?
C32 C27 C26 113.5(5) . . ?
C28 C27 C26 102.9(5) . . ?
C27 C28 C29 107.3(5) . . ?
C27 C28 H28A 110.2 . . ?
C29 C28 H28A 110.2 . . ?
C27 C28 H28B 110.2 . . ?
C29 C28 H28B 110.2 . . ?
H28A C28 H28B 108.5 . . ?
C25 C29 C28 106.6(5) . . ?
C25 C29 H29A 110.4 . . ?
C28 C29 H29A 110.4 . . ?
C25 C29 H29B 110.4 . . ?
C28 C29 H29B 110.4 . . ?
H29A C29 H29B 108.6 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C32 H32A 109.5 . . ?
C27 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C27 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O5 C33 C34 109.5(5) . . ?
O5 C33 H33 125.3 . . ?
C34 C33 H33 125.3 . . ?
C39 C34 C35 120.4(6) . . ?
C39 C34 C33 121.6(6) . . ?
C35 C34 C33 117.9(5) . . ?
O6 C35 C34 118.7(5) . . ?
O6 C35 C36 122.4(5) . . ?
C34 C35 C36 118.9(5) . . ?
C37 C36 C35 119.3(6) . . ?
C37 C36 C40 116.9(5) . . ?
C35 C36 C40 123.7(5) . . ?
C38 C37 C36 119.9(6) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 122.1(6) . . ?
C37 C38 Cl3 120.1(5) . . ?
C39 C38 Cl3 117.8(5) . . ?
C34 C39 C38 119.4(6) . . ?
C34 C39 H39 120.3 . . ?
C38 C39 H39 120.3 . . ?
N5 C40 C36 125.5(6) . . ?
N5 C40 H40 117.2 . . ?
C36 C40 H40 117.2 . . ?
N5 C41 C45 110.2(6) . . ?
N5 C41 C42 114.5(6) . . ?
C45 C41 C42 104.3(6) . . ?
N5 C41 H41 109.2 . . ?
C45 C41 H41 109.2 . . ?
C42 C41 H41 109.2 . . ?
C46 C42 C47 107.5(6) . . ?
C46 C42 C41 114.2(6) . . ?
C47 C42 C41 107.2(6) . . ?
C46 C42 C43 115.9(7) . . ?
C47 C42 C43 110.1(6) . . ?
C41 C42 C43 101.5(6) . . ?
N6 C43 C44 109.4(6) . . ?
N6 C43 C48 109.2(6) . . ?
C44 C43 C48 113.6(7) . . ?
N6 C43 C42 108.4(5) . . ?
C44 C43 C42 102.8(6) . . ?
C48 C43 C42 113.2(6) . . ?
C43 C44 C45 107.7(6) . . ?
C43 C44 H44A 110.2 . . ?
C45 C44 H44A 110.2 . . ?
C43 C44 H44B 110.2 . . ?
C45 C44 H44B 110.2 . . ?
H44A C44 H44B 108.5 . . ?
C44 C45 C41 106.3(6) . . ?
C44 C45 H45A 110.5 . . ?
C41 C45 H45A 110.5 . . ?
C44 C45 H45B 110.5 . . ?
C41 C45 H45B 110.5 . . ?
H45A C45 H45B 108.7 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Ni3 Cl4 Ni1 84.07(5) . . ?
Ni3 Cl4 Ni2 85.20(5) . . ?
Ni1 Cl4 Ni2 85.39(5) . . ?
C8 N1 C9 116.5(5) . . ?
C8 N1 Ni1 121.5(4) . . ?
C9 N1 Ni1 121.2(4) . . ?
C11 N2 Ni1 124.3(3) . . ?
C11 N2 H2A 106.2 . . ?
Ni1 N2 H2A 106.2 . . ?
C11 N2 H2B 106.2 . . ?
Ni1 N2 H2B 106.2 . . ?
H2A N2 H2B 106.4 . . ?
C24 N3 C25 117.5(5) . . ?
C24 N3 Ni2 120.8(4) . . ?
C25 N3 Ni2 121.3(4) . . ?
C27 N4 Ni2 123.4(4) . . ?
C27 N4 H4A 106.5 . . ?
Ni2 N4 H4A 106.5 . . ?
C27 N4 H4B 106.5 . . ?
Ni2 N4 H4B 106.5 . . ?
H4A N4 H4B 106.5 . . ?
C40 N5 C41 118.0(5) . . ?
C40 N5 Ni3 121.3(4) . . ?
C41 N5 Ni3 120.2(4) . . ?
C43 N6 Ni3 125.5(4) . . ?
C43 N6 H6A 106.0 . . ?
Ni3 N6 H6A 106.0 . . ?
C43 N6 H6B 106.0 . . ?
Ni3 N6 H6B 106.0 . . ?
H6A N6 H6B 106.3 . . ?
O9 N7 O8 121.8(6) . . ?
O9 N7 O7 118.4(7) . . ?
O8 N7 O7 119.8(6) . . ?
O11 N8 O10 112.5(12) . . ?
O11 N8 O12 117.3(14) . . ?
O10 N8 O12 129.2(11) . . ?
C1 O1 Ni1 120.7(3) . . ?
C1 O1 Ni3 119.2(3) . . ?
Ni1 O1 Ni3 113.90(18) . . ?
C7 O2 Ni3 116.6(3) . . ?
C17 O3 Ni1 112.8(3) . . ?
C19 O4 Ni2 120.5(3) . . ?
C19 O4 Ni1 118.7(3) . . ?
Ni2 O4 Ni1 116.28(18) . . ?
C33 O5 Ni2 114.5(3) . . ?
C35 O6 Ni3 119.9(3) . . ?
C35 O6 Ni2 121.5(3) . . ?
Ni3 O6 Ni2 115.44(18) . . ?
H13C O13 H13D 109.5 . . ?
H14D O14 H14E 109.5 . . ?
H15D O15 H15E 113.1 . . ?
H16D O16 H16E 106.8 . . ?
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 2.000(4) . ?
Ni1 N1 2.048(5) . ?
Ni1 N2 2.075(4) . ?
Ni1 O4 2.083(4) . ?
Ni1 O3 2.138(4) . ?
Ni1 Cl4 2.5575(17) . ?
Ni2 O4 2.002(4) . ?
Ni2 N3 2.037(5) . ?
Ni2 O6 2.084(4) . ?
Ni2 N4 2.088(4) . ?
Ni2 O5 2.153(4) . ?
Ni2 Cl4 2.5594(17) . ?
Ni3 O6 1.987(4) . ?
Ni3 N5 2.026(5) . ?
Ni3 O1 2.060(4) . ?
Ni3 N6 2.075(5) . ?
Ni3 O2 2.134(4) . ?
Ni3 Cl4 2.5254(18) . ?
C1 O1 1.328(7) . ?
C1 C2 1.395(8) . ?
C1 C6 1.409(8) . ?
C2 C3 1.380(9) . ?
C2 C7 1.488(9) . ?
C3 C4 1.385(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.358(9) . ?
C4 Cl1 1.738(7) . ?
C5 C6 1.415(8) . ?
C5 H5 0.9300 . ?
C6 C8 1.457(8) . ?
C7 O2 1.447(7) . ?
C7 H7 0.9300 . ?
C8 N1 1.278(7) . ?
C8 H8 0.9300 . ?
C9 N1 1.461(7) . ?
C9 C13 1.527(8) . ?
C9 C10 1.558(8) . ?
C9 H9 0.9800 . ?
C10 C14 1.496(8) . ?
C10 C11 1.538(8) . ?
C10 C15 1.555(8) . ?
C11 N2 1.516(7) . ?
C11 C16 1.519(8) . ?
C11 C12 1.520(8) . ?
C12 C13 1.549(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O3 1.440(6) . ?
C17 C18 1.492(8) . ?
C17 H17 0.9300 . ?
C18 C23 1.376(7) . ?
C18 C19 1.385(8) . ?
C19 O4 1.330(6) . ?
C19 C20 1.425(8) . ?
C20 C21 1.410(7) . ?
C20 C24 1.430(8) . ?
C21 C22 1.357(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(8) . ?
C22 Cl2 1.757(5) . ?
C23 H23 0.9300 . ?
C24 N3 1.281(7) . ?
C24 H24 0.9300 . ?
C25 N3 1.472(7) . ?
C25 C29 1.522(8) . ?
C25 C26 1.553(8) . ?
C25 H25 0.9800 . ?
C26 C31 1.516(8) . ?
C26 C30 1.540(8) . ?
C26 C27 1.553(8) . ?
C27 N4 1.503(7) . ?
C27 C32 1.525(8) . ?
C27 C28 1.531(9) . ?
C28 C29 1.535(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 O5 1.457(7) . ?
C33 C34 1.496(8) . ?
C33 H33 0.9300 . ?
C34 C39 1.371(8) . ?
C34 C35 1.399(8) . ?
C35 O6 1.319(6) . ?
C35 C36 1.414(8) . ?
C36 C37 1.395(8) . ?
C36 C40 1.444(8) . ?
C37 C38 1.347(8) . ?
C37 H37 0.9300 . ?
C38 C39 1.384(8) . ?
C38 Cl3 1.766(6) . ?
C39 H39 0.9300 . ?
C40 N5 1.284(7) . ?
C40 H40 0.9300 . ?
C41 N5 1.463(7) . ?
C41 C45 1.529(9) . ?
C41 C42 1.557(9) . ?
C41 H41 0.9800 . ?
C42 C46 1.496(10) . ?
C42 C47 1.529(9) . ?
C42 C43 1.566(9) . ?
C43 N6 1.472(8) . ?
C43 C44 1.518(10) . ?
C43 C48 1.538(9) . ?
C44 C45 1.526(9) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 O9 1.232(6) . ?
N7 O8 1.235(7) . ?
N7 O7 1.262(7) . ?
N8 O11 1.222(11) . ?
N8 O10 1.257(13) . ?
N8 O12 1.355(12) . ?
O13 H13C 0.8499 . ?
O13 H13D 0.8499 . ?
O14 H14D 0.8500 . ?
O14 H14E 0.8500 . ?
O15 H15D 0.8500 . ?
O15 H15E 0.8500 . ?
O16 H16D 0.8499 . ?
O16 H16E 0.8501 . ?
