# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
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# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Audit and citation data items may have been added by the CCDC. 
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data_pbar1_a
_database_code_depnum_ccdc_archive 'CCDC 1511267'
_audit_update_record             
;
2016-10-24 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_audit_creation_date             2016-09-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common            NiCycP
_chemical_name_systematic        
'[Ni([(1,4,8,11-tetraazacyclotetradecan-1-yl)methylene]phosphonic acid)]n'
_chemical_formula_moiety         '0.5(C44 H100 N16 Ni4 O12 P4), 2(H2 O), 2(O)'
_chemical_formula_sum            'C22 H54 N8 Ni2 O10.01 P2'
_chemical_formula_weight         770.25
_chemical_melting_point          ?
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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3977(3)
_cell_length_b                   14.1488(4)
_cell_length_c                   22.4532(7)
_cell_angle_alpha                90.0930(10)
_cell_angle_beta                 90.5310(11)
_cell_angle_gamma                90.0970(10)
_cell_volume                     3303.05(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.7252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1595 before and 0.1133 after correction.
The Ratio of minimum to maximum transmission is 0.7726.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Purple
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            137618
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.314
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11409
_reflns_number_total             13486
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         13486
_refine_ls_number_restraints     289
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0640
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+30.4206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1443
_refine_special_details          ', Twin'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Free rotating group:
 O20(H20C,H20D), O15(H15C,H15D), O16(H16C,H16D), O18(H18C,H18D)
3.b Ternary CH refined with riding coordinates:
 N11(H11), N3(H3), N12(H12), N8(H8), N1(H1), N13(H13), N15(H15), N4(H4),
 N5(H5), N16(H16), N7(H7), N9(H9)
3.c Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C4(H4A,H4B), C25(H25A,H25B), C30(H30A,H30B), C41(H41A,H41B),
 C14(H14A,H14B), C17(H17A,H17B), C27(H27A,H27B), C5(H5A,H5B), C32(H32A,H32B),
 C26(H26A,H26B), C16(H16A,H16B), C29(H29A,H29B), C9(H9A,H9B), C23(H23A,H23B),
 C24(H24A,H24B), C19(H19A,H19B), C2(H2A,H2B), C34(H34A,H34B), C13(H13A,H13B),
 C1(H1A,H1B), C7(H7A,H7B), C10(H10A,H10B), C22(H22A,H22B), C6(H6A,H6B),
 C21(H21A,H21B), C36(H36A,H36B), C43(H43A,H43B), C37(H37A,H37B), C12(H12A,H12B),
  C39(H39A,H39B), C40(H40A,H40B), C8(H8A,H8B), C18(H18A,H18B), C38(H38A,H38B),
 C15(H15A,H15B), C28(H28A,H28B), C3(H3A,H3B), C11(H11A,H11B), C35(H35A,H35B),
 C20(H20A,H20B), C42(H42A,H42B), C44(H44A,H44B), C31(H31A,H31B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Ni3 Ni 0.64206(6) 0.78530(4) 0.36025(3) 0.01084(13) Uani 1 1 d . U . . .
Ni4 Ni 0.37784(6) 0.77116(4) 0.10026(3) 0.01140(14) Uani 1 1 d . U . . .
Ni2 Ni 0.87291(6) 0.73105(4) 0.60150(3) 0.01181(14) Uani 1 1 d . U . . .
P4 P 0.36008(12) 0.72961(9) -0.03173(5) 0.0130(3) Uani 1 1 d . U . . .
P2 P 0.84728(12) 0.78283(9) 0.47175(5) 0.0139(3) Uani 1 1 d . U . . .
P3 P 0.50777(12) 0.81544(9) 0.23989(5) 0.0143(3) Uani 1 1 d . U . . .
P1 P 1.01070(13) 0.69259(10) 0.74068(6) 0.0170(3) Uani 1 1 d . U . . .
O5 O 0.7679(3) 0.8342(2) 0.42501(15) 0.0169(7) Uani 1 1 d . U . . .
O4 O 0.7665(3) 0.7385(2) 0.52090(14) 0.0134(7) Uani 1 1 d . U . . .
O10 O 0.2728(3) 0.7565(2) 0.02048(14) 0.0134(7) Uani 1 1 d . U . . .
O7 O 0.5185(3) 0.7422(2) 0.28968(15) 0.0174(7) Uani 1 1 d . U . . .
O6 O 0.9415(4) 0.7136(3) 0.44581(15) 0.0209(8) Uani 1 1 d . U . . .
O11 O 0.2893(3) 0.6734(2) -0.07949(15) 0.0162(7) Uani 1 1 d . U . . .
O8 O 0.4852(3) 0.7723(3) 0.17925(15) 0.0195(8) Uani 1 1 d . U . . .
O9 O 0.4138(4) 0.8947(3) 0.25435(16) 0.0225(8) Uani 1 1 d . U . . .
O1 O 1.0077(3) 0.7587(3) 0.79516(15) 0.0188(8) Uani 1 1 d . U . . .
O12 O 0.4327(3) 0.8149(3) -0.05622(15) 0.0195(8) Uani 1 1 d . U . . .
O2 O 0.9393(4) 0.6010(3) 0.75198(17) 0.0256(9) Uani 1 1 d . U . . .
O3 O 0.9728(4) 0.7398(3) 0.68291(16) 0.0227(8) Uani 1 1 d . U . . .
O20 O 0.4135(4) 0.5616(3) 0.2549(2) 0.0322(10) Uani 1 1 d . U . . .
H20C H 0.3892 0.5027 0.2542 0.048 Uiso 1 1 d G . . . .
H20D H 0.3548 0.5955 0.2722 0.048 Uiso 1 1 d G . . . .
O15 O 0.6346(4) 0.9158(3) 0.76049(18) 0.0292(9) Uani 1 1 d . U . . .
H15C H 0.6057 0.9734 0.7604 0.044 Uiso 1 1 d G . . . .
H15D H 0.6138 0.8883 0.7938 0.044 Uiso 1 1 d G . . . .
N10 N 0.7396(4) 0.8677(3) 0.29579(18) 0.0176(9) Uani 1 1 d . U . . .
O19 O 1.1509(4) 0.5770(3) 0.2696(2) 0.0379(11) Uani 1 1 d . U . . .
O14 O 0.6947(5) 0.6258(3) 0.8036(2) 0.0386(11) Uani 1 1 d . U . . .
O13 O 0.6353(4) 0.8060(3) 0.86482(18) 0.0299(9) Uani 1 1 d . U . . .
N11 N 0.7715(4) 0.6795(3) 0.33973(19) 0.0201(9) Uani 1 1 d . U . . .
H11 H 0.8389 0.6803 0.3718 0.024 Uiso 1 1 calc R . . . .
O16 O 0.9016(4) 0.9400(3) 0.7647(2) 0.0330(10) Uani 1 1 d . U . . .
H16C H 0.9377 0.8848 0.7682 0.049 Uiso 1 1 d G . . . .
H16D H 0.8191 0.9329 0.7594 0.049 Uiso 1 1 d G . . . .
O18 O 1.1723(5) 0.8797(3) 0.2987(2) 0.0381(11) Uani 1 1 d . U . . .
H18C H 1.2552 0.8801 0.2936 0.057 Uiso 1 1 d G . . . .
H18D H 1.1376 0.9251 0.2780 0.057 Uiso 1 1 d G . . . .
O17 O 1.1261(4) 0.7065(3) 0.36062(18) 0.0316(10) Uani 1 1 d . U . . .
N3 N 1.0581(5) 0.5853(3) 0.8748(2) 0.0232(10) Uani 1 1 d . U . . .
H3 H 0.9911 0.5759 0.8431 0.028 Uiso 1 1 calc R . . . .
N12 N 0.5471(4) 0.7070(3) 0.4238(2) 0.0203(9) Uani 1 1 d . U . . .
H12 H 0.5981 0.7115 0.4617 0.024 Uiso 1 1 calc R . . . .
N8 N 0.7811(5) 0.6082(3) 0.6253(2) 0.0230(10) Uani 1 1 d . U . . .
H8 H 0.8056 0.5940 0.6675 0.028 Uiso 1 1 calc R . . . .
N1 N 1.2356(4) 0.8478(3) 0.85306(19) 0.0203(9) Uani 1 1 d . U . . .
H1 H 1.3054 0.8501 0.8840 0.024 Uiso 1 1 calc R . . . .
N14 N 0.5099(4) 0.6714(3) 0.06414(19) 0.0199(9) Uani 1 1 d . U . . .
N13 N 0.4763(4) 0.8858(3) 0.06471(19) 0.0215(9) Uani 1 1 d . U . . .
H13 H 0.4544 0.8887 0.0213 0.026 Uiso 1 1 calc R . . . .
N6 N 0.9647(4) 0.8575(3) 0.57349(19) 0.0209(9) Uani 1 1 d . U . . .
N15 N 0.2821(5) 0.6563(3) 0.1352(2) 0.0239(10) Uani 1 1 d . U . . .
H15 H 0.3057 0.6528 0.1784 0.029 Uiso 1 1 calc R . . . .
N4 N 1.0346(4) 0.7625(3) 0.9327(2) 0.0238(10) Uani 1 1 d . U . . .
H4 H 1.0896 0.7592 0.9694 0.029 Uiso 1 1 calc R . . . .
N5 N 0.7375(4) 0.8187(3) 0.64086(19) 0.0192(9) Uani 1 1 d . U . . .
H5 H 0.7577 0.8204 0.6845 0.023 Uiso 1 1 calc R . . . .
N16 N 0.2496(5) 0.8700(3) 0.13226(19) 0.0224(9) Uani 1 1 d . U . . .
H16 H 0.2730 0.8825 0.1749 0.027 Uiso 1 1 calc R . . . .
N7 N 1.0090(5) 0.6430(3) 0.5624(2) 0.0242(10) Uani 1 1 d . U . . .
H7 H 0.9890 0.6421 0.5188 0.029 Uiso 1 1 calc R . . . .
C33 C 0.6679(5) 0.8693(4) 0.2374(2) 0.0208(11) Uani 1 1 d . U . . .
H33A H 0.7196 0.8356 0.2072 0.025 Uiso 1 1 calc R . . . .
H33B H 0.6591 0.9357 0.2242 0.025 Uiso 1 1 calc R . . . .
N9 N 0.5172(4) 0.8942(3) 0.3848(2) 0.0225(9) Uani 1 1 d . U . . .
H9 H 0.4511 0.9009 0.3525 0.027 Uiso 1 1 calc R . . . .
N2 N 1.2579(4) 0.6706(3) 0.78948(19) 0.0218(9) Uani 1 1 d . U . . .
C4 C 1.2989(6) 0.8434(4) 0.7953(2) 0.0261(12) Uani 1 1 d . U . . .
H4A H 1.3665 0.8926 0.7930 0.031 Uiso 1 1 calc R . . . .
H4B H 1.2355 0.8549 0.7630 0.031 Uiso 1 1 calc R . . . .
C25 C 0.7635(5) 0.9660(4) 0.3185(2) 0.0218(11) Uani 1 1 d . U . . .
H25A H 0.8080 1.0025 0.2873 0.026 Uiso 1 1 calc R . . . .
H25B H 0.8221 0.9624 0.3535 0.026 Uiso 1 1 calc R . . . .
C30 C 0.5303(6) 0.6046(4) 0.4095(3) 0.0272(12) Uani 1 1 d . U . . .
H30A H 0.4721 0.5980 0.3746 0.033 Uiso 1 1 calc R . . . .
H30B H 0.4894 0.5725 0.4437 0.033 Uiso 1 1 calc R . . . .
C41 C 0.6463(5) 0.7050(4) 0.0716(2) 0.0257(12) Uani 1 1 d . U . . .
H41A H 0.7043 0.6566 0.0548 0.031 Uiso 1 1 calc R . . . .
H41B H 0.6660 0.7102 0.1147 0.031 Uiso 1 1 calc R . . . .
C14 C 0.6021(5) 0.7872(4) 0.6344(3) 0.0234(11) Uani 1 1 d . U . . .
H14A H 0.5765 0.7901 0.5918 0.028 Uiso 1 1 calc R . . . .
H14B H 0.5459 0.8308 0.6567 0.028 Uiso 1 1 calc R . . . .
C17 C 1.1049(5) 0.8527(4) 0.5832(2) 0.0256(12) Uani 1 1 d . U . . .
H17A H 1.1221 0.8437 0.6262 0.031 Uiso 1 1 calc R . . . .
H17B H 1.1434 0.9138 0.5715 0.031 Uiso 1 1 calc R . . . .
C27 C 0.8350(5) 0.7126(4) 0.2842(2) 0.0241(12) Uani 1 1 d . U . . .
H27A H 0.7785 0.6999 0.2494 0.029 Uiso 1 1 calc R . . . .
H27B H 0.9167 0.6780 0.2785 0.029 Uiso 1 1 calc R . . . .
C5 C 1.3578(5) 0.7474(4) 0.7879(2) 0.0267(12) Uani 1 1 d . U . . .
H5A H 1.4216 0.7367 0.8202 0.032 Uiso 1 1 calc R . . . .
H5B H 1.4036 0.7446 0.7495 0.032 Uiso 1 1 calc R . . . .
C32 C 0.4508(6) 0.8588(4) 0.4389(3) 0.0307(13) Uani 1 1 d . U . . .
H32A H 0.3686 0.8930 0.4440 0.037 Uiso 1 1 calc R . . . .
H32B H 0.5051 0.8709 0.4745 0.037 Uiso 1 1 calc R . . . .
C26 C 0.8613(5) 0.8170(4) 0.2892(2) 0.0233(11) Uani 1 1 d . U . . .
H26A H 0.9176 0.8295 0.3242 0.028 Uiso 1 1 calc R . . . .
H26B H 0.9061 0.8393 0.2532 0.028 Uiso 1 1 calc R . . . .
C16 C 0.9057(6) 0.9290(4) 0.6138(2) 0.0243(12) Uani 1 1 d . U . . .
H16A H 0.9231 0.9933 0.5985 0.029 Uiso 1 1 calc R . . . .
H16B H 0.9448 0.9239 0.6540 0.029 Uiso 1 1 calc R . . . .
C29 C 0.6580(6) 0.5565(4) 0.3961(3) 0.0286(13) Uani 1 1 d . U . . .
H29A H 0.7193 0.5712 0.4288 0.034 Uiso 1 1 calc R . . . .
H29B H 0.6441 0.4872 0.3960 0.034 Uiso 1 1 calc R . . . .
C9 C 0.9939(6) 0.5921(4) 0.9323(3) 0.0289(13) Uani 1 1 d . U . . .
H9A H 1.0571 0.5826 0.9650 0.035 Uiso 1 1 calc R . . . .
H9B H 0.9271 0.5424 0.9353 0.035 Uiso 1 1 calc R . . . .
C23 C 0.5791(6) 0.9854(4) 0.3926(2) 0.0232(11) Uani 1 1 d . U . . .
H23A H 0.6443 0.9808 0.4249 0.028 Uiso 1 1 calc R . . . .
H23B H 0.5141 1.0325 0.4049 0.028 Uiso 1 1 calc R . . . .
C24 C 0.6434(6) 1.0192(4) 0.3364(3) 0.0239(12) Uani 1 1 d . U . . .
H24A H 0.6662 1.0867 0.3416 0.029 Uiso 1 1 calc R . . . .
H24B H 0.5803 1.0151 0.3032 0.029 Uiso 1 1 calc R . . . .
C19 C 1.1467(6) 0.6735(5) 0.5685(3) 0.0305(13) Uani 1 1 d . U . . .
H19A H 1.2008 0.6308 0.5444 0.037 Uiso 1 1 calc R . . . .
H19B H 1.1739 0.6666 0.6107 0.037 Uiso 1 1 calc R . . . .
C2 C 1.0885(6) 0.9301(4) 0.9224(3) 0.0278(12) Uani 1 1 d . U . . .
H2A H 1.1545 0.9180 0.9535 0.033 Uiso 1 1 calc R . . . .
H2B H 1.0521 0.9935 0.9301 0.033 Uiso 1 1 calc R . . . .
C34 C 0.1421(6) 0.6596(5) 0.1314(3) 0.0296(13) Uani 1 1 d . U . . .
H34A H 0.1060 0.6023 0.1503 0.036 Uiso 1 1 calc R . . . .
H34B H 0.1153 0.6595 0.0890 0.036 Uiso 1 1 calc R . . . .
C13 C 0.5824(6) 0.6880(4) 0.6569(3) 0.0277(12) Uani 1 1 d . U . . .
H13A H 0.6177 0.6846 0.6980 0.033 Uiso 1 1 calc R . . . .
H13B H 0.4887 0.6764 0.6594 0.033 Uiso 1 1 calc R . . . .
C1 C 0.9824(6) 0.8579(4) 0.9290(3) 0.0289(13) Uani 1 1 d . U . . .
H1A H 0.9330 0.8718 0.9655 0.035 Uiso 1 1 calc R . . . .
H1B H 0.9228 0.8621 0.8945 0.035 Uiso 1 1 calc R . . . .
C7 C 1.2202(6) 0.5014(4) 0.8124(3) 0.0282(13) Uani 1 1 d . U . . .
H7A H 1.2652 0.4399 0.8098 0.034 Uiso 1 1 calc R . . . .
H7B H 1.1546 0.5026 0.7802 0.034 Uiso 1 1 calc R . . . .
C10 C 0.9332(6) 0.6879(5) 0.9378(3) 0.0328(14) Uani 1 1 d . U . . .
H10A H 0.8677 0.6964 0.9060 0.039 Uiso 1 1 calc R . . . .
H10B H 0.8899 0.6935 0.9767 0.039 Uiso 1 1 calc R . . . .
C22 C 0.9326(5) 0.8797(4) 0.5099(2) 0.0218(11) Uani 1 1 d . U . . .
H22A H 1.0131 0.8935 0.4884 0.026 Uiso 1 1 calc R . . . .
H22B H 0.8785 0.9371 0.5086 0.026 Uiso 1 1 calc R . . . .
C6 C 1.3162(6) 0.5783(4) 0.8006(2) 0.0254(12) Uani 1 1 d . U . . .
H6A H 1.3753 0.5836 0.8353 0.030 Uiso 1 1 calc R . . . .
H6B H 1.3681 0.5604 0.7656 0.030 Uiso 1 1 calc R . . . .
C21 C 0.8392(6) 0.5334(4) 0.5868(3) 0.0298(13) Uani 1 1 d . U . . .
H21A H 0.8019 0.5369 0.5461 0.036 Uiso 1 1 calc R . . . .
H21B H 0.8201 0.4702 0.6033 0.036 Uiso 1 1 calc R . . . .
C36 C 0.1120(6) 0.8403(5) 0.1306(3) 0.0307(13) Uani 1 1 d . U . . .
H36A H 0.0830 0.8356 0.0886 0.037 Uiso 1 1 calc R . . . .
H36B H 0.0594 0.8893 0.1503 0.037 Uiso 1 1 calc R . . . .
C43 C 0.3401(6) 0.5725(4) 0.1058(3) 0.0287(13) Uani 1 1 d . U . . .
H43A H 0.3023 0.5641 0.0655 0.034 Uiso 1 1 calc R . . . .
H43B H 0.3223 0.5149 0.1292 0.034 Uiso 1 1 calc R . . . .
C37 C 0.2755(6) 0.9572(4) 0.0988(3) 0.0286(13) Uani 1 1 d . U . . .
H37A H 0.2378 1.0120 0.1197 0.034 Uiso 1 1 calc R . . . .
H37B H 0.2358 0.9530 0.0586 0.034 Uiso 1 1 calc R . . . .
C12 C 0.6405(6) 0.6093(4) 0.6215(3) 0.0281(12) Uani 1 1 d . U . . .
H12A H 0.6068 0.5482 0.6361 0.034 Uiso 1 1 calc R . . . .
H12B H 0.6139 0.6159 0.5792 0.034 Uiso 1 1 calc R . . . .
C39 C 0.6166(5) 0.8849(4) 0.0702(3) 0.0273(12) Uani 1 1 d . U . . .
H39A H 0.6410 0.8877 0.1129 0.033 Uiso 1 1 calc R . . . .
H39B H 0.6518 0.9419 0.0506 0.033 Uiso 1 1 calc R . . . .
C40 C 0.6752(6) 0.7985(5) 0.0426(3) 0.0307(13) Uani 1 1 d . U . . .
H40A H 0.7698 0.8070 0.0425 0.037 Uiso 1 1 calc R . . . .
H40B H 0.6462 0.7950 0.0006 0.037 Uiso 1 1 calc R . . . .
C8 C 1.1507(6) 0.5053(4) 0.8719(3) 0.0256(12) Uani 1 1 d . U . . .
H8A H 1.1038 0.4452 0.8781 0.031 Uiso 1 1 calc R . . . .
H8B H 1.2149 0.5121 0.9045 0.031 Uiso 1 1 calc R . . . .
C18 C 1.1705(6) 0.7745(5) 0.5491(3) 0.0299(13) Uani 1 1 d . U . . .
H18A H 1.2644 0.7861 0.5512 0.036 Uiso 1 1 calc R . . . .
H18B H 1.1443 0.7799 0.5068 0.036 Uiso 1 1 calc R . . . .
C38 C 0.4176(6) 0.9698(4) 0.0936(2) 0.0271(12) Uani 1 1 d . U . . .
H38A H 0.4359 1.0270 0.0697 0.033 Uiso 1 1 calc R . . . .
H38B H 0.4560 0.9789 0.1337 0.033 Uiso 1 1 calc R . . . .
C15 C 0.7623(6) 0.9137(4) 0.6176(3) 0.0242(12) Uani 1 1 d . U . . .
H15A H 0.7241 0.9616 0.6443 0.029 Uiso 1 1 calc R . . . .
H15B H 0.7224 0.9204 0.5776 0.029 Uiso 1 1 calc R . . . .
C28 C 0.7189(6) 0.5836(4) 0.3382(3) 0.0274(12) Uani 1 1 d . U . . .
H28A H 0.7888 0.5385 0.3291 0.033 Uiso 1 1 calc R . . . .
H28B H 0.6539 0.5791 0.3058 0.033 Uiso 1 1 calc R . . . .
C3 C 1.1548(6) 0.9324(4) 0.8623(3) 0.0257(12) Uani 1 1 d . U . . .
H3A H 1.0890 0.9359 0.8303 0.031 Uiso 1 1 calc R . . . .
H3B H 1.2091 0.9897 0.8599 0.031 Uiso 1 1 calc R . . . .
C11 C 1.1847(5) 0.6699(4) 0.7318(2) 0.0253(12) Uani 1 1 d . U . . .
H11A H 1.1960 0.6076 0.7124 0.030 Uiso 1 1 calc R . . . .
H11B H 1.2212 0.7185 0.7052 0.030 Uiso 1 1 calc R . . . .
C35 C 0.0889(6) 0.7454(5) 0.1613(3) 0.0323(14) Uani 1 1 d . U . . .
H35A H 0.1261 0.7490 0.2020 0.039 Uiso 1 1 calc R . . . .
H35B H -0.0051 0.7366 0.1654 0.039 Uiso 1 1 calc R . . . .
C20 C 0.9822(6) 0.5483(4) 0.5845(3) 0.0317(13) Uani 1 1 d . U . . .
H20A H 1.0202 0.5405 0.6247 0.038 Uiso 1 1 calc R . . . .
H20B H 1.0212 0.5007 0.5578 0.038 Uiso 1 1 calc R . . . .
C42 C 0.4833(6) 0.5879(4) 0.1014(3) 0.0264(12) Uani 1 1 d . U . . .
H42A H 0.5205 0.5975 0.1417 0.032 Uiso 1 1 calc R . . . .
H42B H 0.5240 0.5314 0.0837 0.032 Uiso 1 1 calc R . . . .
C44 C 0.4802(5) 0.6497(4) 0.0001(2) 0.0212(11) Uani 1 1 d . U . . .
H44A H 0.4483 0.5839 -0.0032 0.025 Uiso 1 1 calc R . . . .
H44B H 0.5603 0.6544 -0.0232 0.025 Uiso 1 1 calc R . . . .
C31 C 0.4249(6) 0.7551(4) 0.4333(3) 0.0284(13) Uani 1 1 d . U . . .
H31A H 0.3842 0.7313 0.4701 0.034 Uiso 1 1 calc R . . . .
H31B H 0.3658 0.7429 0.3994 0.034 Uiso 1 1 calc R . . . .
Ni1 Ni 1.14481(6) 0.71745(4) 0.86185(3) 0.01132(14) Uani 1 1 d . 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
Ni3 O5 2.065(3) . ?
Ni3 O7 2.119(3) . ?
Ni3 N10 2.124(4) . ?
Ni3 N11 2.069(4) . ?
Ni3 N12 2.065(4) . ?
Ni3 N9 2.093(5) . ?
Ni4 O10 2.099(3) . ?
Ni4 O8 2.087(3) . ?
Ni4 N14 2.135(4) . ?
Ni4 N13 2.081(5) . ?
Ni4 N15 2.064(5) . ?
Ni4 N16 2.067(4) . ?
Ni2 O4 2.115(3) . ?
Ni2 O3 2.097(4) . ?
Ni2 N8 2.055(5) . ?
Ni2 N6 2.126(5) . ?
Ni2 N5 2.080(4) . ?
Ni2 N7 2.086(5) . ?
P4 O10 1.537(3) . ?
P4 O11 1.518(3) . ?
P4 O12 1.528(4) . ?
P4 C44 1.828(5) . ?
P2 O5 1.517(4) . ?
P2 O4 1.528(4) . ?
P2 O6 1.507(4) . ?
P2 C22 1.838(5) . ?
P3 O7 1.529(4) . ?
P3 O8 1.507(4) . ?
P3 O9 1.525(4) . ?
P3 C33 1.832(5) . ?
P1 O1 1.539(4) . ?
P1 O2 1.516(4) . ?
P1 O3 1.509(4) . ?
P1 C11 1.850(6) . ?
O11 Ni1 2.085(3) 1_454 ?
O1 Ni1 2.141(3) . ?
O20 H20C 0.8699 . ?
O20 H20D 0.8701 . ?
O15 H15C 0.8699 . ?
O15 H15D 0.8714 . ?
N10 C33 1.502(6) . ?
N10 C25 1.501(7) . ?
N10 C26 1.465(7) . ?
N11 H11 1.0000 . ?
N11 C27 1.492(7) . ?
N11 C28 1.461(7) . ?
O16 H16C 0.8703 . ?
O16 H16D 0.8698 . ?
O18 H18C 0.8703 . ?
O18 H18D 0.8694 . ?
N3 H3 1.0000 . ?
N3 C9 1.462(7) . ?
N3 C8 1.489(7) . ?
N3 Ni1 2.096(4) . ?
N12 H12 1.0000 . ?
N12 C30 1.494(7) . ?
N12 C31 1.459(7) . ?
N8 H8 1.0000 . ?
N8 C21 1.496(7) . ?
N8 C12 1.463(7) . ?
N1 H1 1.0000 . ?
N1 C4 1.462(7) . ?
N1 C3 1.479(7) . ?
N1 Ni1 2.081(4) . ?
N14 C41 1.503(7) . ?
N14 C42 1.476(7) . ?
N14 C44 1.500(6) . ?
N13 H13 1.0000 . ?
N13 C39 1.463(7) . ?
N13 C38 1.489(7) . ?
N6 C17 1.474(7) . ?
N6 C16 1.492(7) . ?
N6 C22 1.496(6) . ?
N15 H15 1.0000 . ?
N15 C34 1.459(7) . ?
N15 C43 1.487(7) . ?
N4 H4 1.0000 . ?
N4 C1 1.458(7) . ?
N4 C10 1.495(8) . ?
N4 Ni1 2.069(4) . ?
N5 H5 1.0000 . ?
N5 C14 1.482(7) . ?
N5 C15 1.466(7) . ?
N16 H16 1.0000 . ?
N16 C36 1.491(8) . ?
N16 C37 1.471(7) . ?
N7 H7 1.0000 . ?
N7 C19 1.499(8) . ?
N7 C20 1.458(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
N9 H9 1.0000 . ?
N9 C32 1.490(7) . ?
N9 C23 1.451(7) . ?
N2 C5 1.503(7) . ?
N2 C6 1.461(7) . ?
N2 C11 1.495(6) . ?
N2 Ni1 2.121(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.501(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.516(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C29 1.526(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C40 1.506(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.507(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.510(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.506(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.496(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C15 1.509(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C28 1.501(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.502(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.511(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.515(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.511(9) . ?
C2 C3 1.519(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.496(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.499(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.502(9) . ?
C7 C8 1.527(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.503(9) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.529(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C42 1.509(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.494(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.503(9) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
Ni1 O11 2.085(3) 1_656 ?

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
O5 Ni3 O7 175.98(14) . . ?
O5 Ni3 N10 89.64(15) . . ?
O5 Ni3 N11 89.38(16) . . ?
O5 Ni3 N12 89.75(16) . . ?
O5 Ni3 N9 87.66(16) . . ?
O7 Ni3 N10 86.40(15) . . ?
N11 Ni3 O7 90.99(16) . . ?
N11 Ni3 N10 86.01(18) . . ?
N11 Ni3 N9 177.01(18) . . ?
N12 Ni3 O7 94.20(16) . . ?
N12 Ni3 N10 179.08(18) . . ?
N12 Ni3 N11 94.66(18) . . ?
N12 Ni3 N9 84.92(18) . . ?
N9 Ni3 O7 91.99(16) . . ?
N9 Ni3 N10 94.37(18) . . ?
O10 Ni4 N14 86.75(15) . . ?
O8 Ni4 O10 174.70(14) . . ?
O8 Ni4 N14 89.17(15) . . ?
N13 Ni4 O10 90.11(15) . . ?
N13 Ni4 O8 93.46(16) . . ?
N13 Ni4 N14 92.83(19) . . ?
N15 Ni4 O10 89.97(15) . . ?
N15 Ni4 O8 86.41(16) . . ?
N15 Ni4 N14 86.42(19) . . ?
N15 Ni4 N13 179.2(2) . . ?
N15 Ni4 N16 94.9(2) . . ?
N16 Ni4 O10 91.71(16) . . ?
N16 Ni4 O8 92.45(16) . . ?
N16 Ni4 N14 177.94(18) . . ?
N16 Ni4 N13 85.81(19) . . ?
O4 Ni2 N6 86.31(15) . . ?
O3 Ni2 O4 173.48(14) . . ?
O3 Ni2 N6 89.44(16) . . ?
N8 Ni2 O4 91.48(16) . . ?
N8 Ni2 O3 92.81(16) . . ?
N8 Ni2 N6 177.74(17) . . ?
N8 Ni2 N5 94.38(19) . . ?
N8 Ni2 N7 85.6(2) . . ?
N5 Ni2 O4 88.95(15) . . ?
N5 Ni2 O3 85.83(16) . . ?
N5 Ni2 N6 86.03(18) . . ?
N5 Ni2 N7 179.74(18) . . ?
N7 Ni2 O4 91.30(15) . . ?
N7 Ni2 O3 93.91(16) . . ?
N7 Ni2 N6 94.02(19) . . ?
O10 P4 C44 105.2(2) . . ?
O11 P4 O10 112.4(2) . . ?
O11 P4 O12 113.3(2) . . ?
O11 P4 C44 106.1(2) . . ?
O12 P4 O10 112.1(2) . . ?
O12 P4 C44 107.0(2) . . ?
O5 P2 O4 113.5(2) . . ?
O5 P2 C22 102.8(2) . . ?
O4 P2 C22 103.6(2) . . ?
O6 P2 O5 113.4(2) . . ?
O6 P2 O4 112.1(2) . . ?
O6 P2 C22 110.6(2) . . ?
O7 P3 C33 104.1(2) . . ?
O8 P3 O7 113.3(2) . . ?
O8 P3 O9 113.2(2) . . ?
O8 P3 C33 105.8(2) . . ?
O9 P3 O7 112.8(2) . . ?
O9 P3 C33 106.6(2) . . ?
O1 P1 C11 102.6(2) . . ?
O2 P1 O1 111.8(2) . . ?
O2 P1 C11 110.4(3) . . ?
O3 P1 O1 114.0(2) . . ?
O3 P1 O2 113.5(2) . . ?
O3 P1 C11 103.5(2) . . ?
P2 O5 Ni3 131.6(2) . . ?
P2 O4 Ni2 110.66(18) . . ?
P4 O10 Ni4 111.62(18) . . ?
P3 O7 Ni3 113.09(19) . . ?
P4 O11 Ni1 129.1(2) . 1_454 ?
P3 O8 Ni4 147.9(2) . . ?
P1 O1 Ni1 111.75(19) . . ?
P1 O3 Ni2 147.9(2) . . ?
H20C O20 H20D 109.4 . . ?
H15C O15 H15D 109.4 . . ?
C33 N10 Ni3 111.6(3) . . ?
C25 N10 Ni3 110.8(3) . . ?
C25 N10 C33 111.1(4) . . ?
C26 N10 Ni3 102.5(3) . . ?
C26 N10 C33 110.1(4) . . ?
C26 N10 C25 110.4(4) . . ?
Ni3 N11 H11 106.6 . . ?
C27 N11 Ni3 104.6(3) . . ?
C27 N11 H11 106.6 . . ?
C28 N11 Ni3 115.7(4) . . ?
C28 N11 H11 106.6 . . ?
C28 N11 C27 116.1(4) . . ?
H16C O16 H16D 109.5 . . ?
H18C O18 H18D 109.5 . . ?
C9 N3 H3 108.4 . . ?
C9 N3 C8 112.8(4) . . ?
C9 N3 Ni1 105.4(3) . . ?
C8 N3 H3 108.4 . . ?
C8 N3 Ni1 113.2(3) . . ?
Ni1 N3 H3 108.4 . . ?
Ni3 N12 H12 107.6 . . ?
C30 N12 Ni3 115.3(3) . . ?
C30 N12 H12 107.6 . . ?
C31 N12 Ni3 105.8(3) . . ?
C31 N12 H12 107.6 . . ?
C31 N12 C30 112.6(4) . . ?
Ni2 N8 H8 107.6 . . ?
C21 N8 Ni2 104.9(3) . . ?
C21 N8 H8 107.6 . . ?
C12 N8 Ni2 116.2(4) . . ?
C12 N8 H8 107.6 . . ?
C12 N8 C21 112.5(4) . . ?
C4 N1 H1 106.7 . . ?
C4 N1 C3 114.9(4) . . ?
C4 N1 Ni1 104.8(3) . . ?
C3 N1 H1 106.7 . . ?
C3 N1 Ni1 116.4(4) . . ?
Ni1 N1 H1 106.7 . . ?
C41 N14 Ni4 111.0(3) . . ?
C42 N14 Ni4 101.0(3) . . ?
C42 N14 C41 111.7(4) . . ?
C42 N14 C44 110.0(4) . . ?
C44 N14 Ni4 111.8(3) . . ?
C44 N14 C41 110.9(4) . . ?
Ni4 N13 H13 107.4 . . ?
C39 N13 Ni4 117.0(4) . . ?
C39 N13 H13 107.4 . . ?
C39 N13 C38 112.6(4) . . ?
C38 N13 Ni4 104.5(3) . . ?
C38 N13 H13 107.4 . . ?
C17 N6 Ni2 111.2(4) . . ?
C17 N6 C16 110.8(4) . . ?
C17 N6 C22 111.2(4) . . ?
C16 N6 Ni2 101.7(3) . . ?
C16 N6 C22 110.2(4) . . ?
C22 N6 Ni2 111.3(3) . . ?
Ni4 N15 H15 107.1 . . ?
C34 N15 Ni4 115.8(4) . . ?
C34 N15 H15 107.1 . . ?
C34 N15 C43 114.2(5) . . ?
C43 N15 Ni4 105.0(3) . . ?
C43 N15 H15 107.1 . . ?
C1 N4 H4 107.5 . . ?
C1 N4 C10 113.2(5) . . ?
C1 N4 Ni1 116.7(4) . . ?
C10 N4 H4 107.5 . . ?
C10 N4 Ni1 103.8(3) . . ?
Ni1 N4 H4 107.5 . . ?
Ni2 N5 H5 107.0 . . ?
C14 N5 Ni2 115.2(3) . . ?
C14 N5 H5 107.0 . . ?
C15 N5 Ni2 105.9(3) . . ?
C15 N5 H5 107.0 . . ?
C15 N5 C14 114.2(4) . . ?
Ni4 N16 H16 107.3 . . ?
C36 N16 Ni4 115.0(3) . . ?
C36 N16 H16 107.3 . . ?
C37 N16 Ni4 105.6(3) . . ?
C37 N16 H16 107.3 . . ?
C37 N16 C36 113.8(5) . . ?
Ni2 N7 H7 106.5 . . ?
C19 N7 Ni2 116.2(4) . . ?
C19 N7 H7 106.5 . . ?
C20 N7 Ni2 105.9(4) . . ?
C20 N7 H7 106.5 . . ?
C20 N7 C19 114.7(5) . . ?
P3 C33 H33A 108.7 . . ?
P3 C33 H33B 108.7 . . ?
N10 C33 P3 114.2(3) . . ?
N10 C33 H33A 108.7 . . ?
N10 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
Ni3 N9 H9 107.6 . . ?
C32 N9 Ni3 105.1(3) . . ?
C32 N9 H9 107.6 . . ?
C23 N9 Ni3 114.3(3) . . ?
C23 N9 H9 107.6 . . ?
C23 N9 C32 114.2(5) . . ?
C5 N2 Ni1 100.4(3) . . ?
C6 N2 C5 111.3(5) . . ?
C6 N2 C11 110.5(4) . . ?
C6 N2 Ni1 112.4(3) . . ?
C11 N2 C5 109.3(4) . . ?
C11 N2 Ni1 112.5(3) . . ?
N1 C4 H4A 109.9 . . ?
N1 C4 H4B 109.9 . . ?
N1 C4 C5 108.9(4) . . ?
H4A C4 H4B 108.3 . . ?
C5 C4 H4A 109.9 . . ?
C5 C4 H4B 109.9 . . ?
N10 C25 H25A 108.6 . . ?
N10 C25 H25B 108.6 . . ?
N10 C25 C24 114.6(4) . . ?
H25A C25 H25B 107.6 . . ?
C24 C25 H25A 108.6 . . ?
C24 C25 H25B 108.6 . . ?
N12 C30 H30A 109.2 . . ?
N12 C30 H30B 109.2 . . ?
N12 C30 C29 112.1(5) . . ?
H30A C30 H30B 107.9 . . ?
C29 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
N14 C41 H41A 108.5 . . ?
N14 C41 H41B 108.5 . . ?
N14 C41 C40 114.9(4) . . ?
H41A C41 H41B 107.5 . . ?
C40 C41 H41A 108.5 . . ?
C40 C41 H41B 108.5 . . ?
N5 C14 H14A 109.2 . . ?
N5 C14 H14B 109.2 . . ?
N5 C14 C13 112.2(4) . . ?
H14A C14 H14B 107.9 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
N6 C17 H17A 108.7 . . ?
N6 C17 H17B 108.7 . . ?
N6 C17 C18 114.4(5) . . ?
H17A C17 H17B 107.6 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
N11 C27 H27A 109.9 . . ?
N11 C27 H27B 109.9 . . ?
N11 C27 C26 109.1(4) . . ?
H27A C27 H27B 108.3 . . ?
C26 C27 H27A 109.9 . . ?
C26 C27 H27B 109.9 . . ?
N2 C5 H5A 109.3 . . ?
N2 C5 H5B 109.3 . . ?
C4 C5 N2 111.6(5) . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
N9 C32 H32A 109.6 . . ?
N9 C32 H32B 109.6 . . ?
N9 C32 C31 110.3(5) . . ?
H32A C32 H32B 108.1 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
N10 C26 C27 109.4(4) . . ?
N10 C26 H26A 109.8 . . ?
N10 C26 H26B 109.8 . . ?
C27 C26 H26A 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
N6 C16 H16A 109.5 . . ?
N6 C16 H16B 109.5 . . ?
N6 C16 C15 110.5(4) . . ?
H16A C16 H16B 108.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.4 . . ?
C28 C29 C30 115.6(5) . . ?
C28 C29 H29A 108.4 . . ?
C28 C29 H29B 108.4 . . ?
N3 C9 H9A 109.9 . . ?
N3 C9 H9B 109.9 . . ?
N3 C9 C10 109.1(5) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
N9 C23 H23A 109.1 . . ?
N9 C23 H23B 109.1 . . ?
N9 C23 C24 112.4(4) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
C25 C24 H24A 108.3 . . ?
C25 C24 H24B 108.3 . . ?
C23 C24 C25 115.8(5) . . ?
C23 C24 H24A 108.3 . . ?
C23 C24 H24B 108.3 . . ?
H24A C24 H24B 107.4 . . ?
N7 C19 H19A 108.8 . . ?
N7 C19 H19B 108.8 . . ?
N7 C19 C18 113.7(5) . . ?
H19A C19 H19B 107.7 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H2A C2 H2B 107.4 . . ?
C1 C2 H2A 108.3 . . ?
C1 C2 H2B 108.3 . . ?
C1 C2 C3 116.1(5) . . ?
C3 C2 H2A 108.3 . . ?
C3 C2 H2B 108.3 . . ?
N15 C34 H34A 109.2 . . ?
N15 C34 H34B 109.2 . . ?
N15 C34 C35 112.0(5) . . ?
H34A C34 H34B 107.9 . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C14 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C12 C13 C14 117.2(5) . . ?
C12 C13 H13A 108.0 . . ?
C12 C13 H13B 108.0 . . ?
N4 C1 C2 111.1(5) . . ?
N4 C1 H1A 109.4 . . ?
N4 C1 H1B 109.4 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
H7A C7 H7B 107.3 . . ?
C6 C7 H7A 108.1 . . ?
C6 C7 H7B 108.1 . . ?
C6 C7 C8 116.7(5) . . ?
C8 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
N4 C10 C9 109.4(5) . . ?
N4 C10 H10A 109.8 . . ?
N4 C10 H10B 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
P2 C22 H22A 109.0 . . ?
P2 C22 H22B 109.0 . . ?
N6 C22 P2 113.0(4) . . ?
N6 C22 H22A 109.0 . . ?
N6 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
N2 C6 C7 113.7(5) . . ?
N2 C6 H6A 108.8 . . ?
N2 C6 H6B 108.8 . . ?
C7 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
N8 C21 H21A 109.9 . . ?
N8 C21 H21B 109.9 . . ?
N8 C21 C20 109.1(5) . . ?
H21A C21 H21B 108.3 . . ?
C20 C21 H21A 109.9 . . ?
C20 C21 H21B 109.9 . . ?
N16 C36 H36A 109.0 . . ?
N16 C36 H36B 109.0 . . ?
N16 C36 C35 113.0(5) . . ?
H36A C36 H36B 107.8 . . ?
C35 C36 H36A 109.0 . . ?
C35 C36 H36B 109.0 . . ?
N15 C43 H43A 110.0 . . ?
N15 C43 H43B 110.0 . . ?
N15 C43 C42 108.7(4) . . ?
H43A C43 H43B 108.3 . . ?
C42 C43 H43A 110.0 . . ?
C42 C43 H43B 110.0 . . ?
N16 C37 H37A 109.9 . . ?
N16 C37 H37B 109.9 . . ?
N16 C37 C38 109.0(5) . . ?
H37A C37 H37B 108.3 . . ?
C38 C37 H37A 109.9 . . ?
C38 C37 H37B 109.9 . . ?
N8 C12 C13 112.7(5) . . ?
N8 C12 H12A 109.1 . . ?
N8 C12 H12B 109.1 . . ?
C13 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N13 C39 H39A 109.1 . . ?
N13 C39 H39B 109.1 . . ?
N13 C39 C40 112.4(5) . . ?
H39A C39 H39B 107.8 . . ?
C40 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C41 C40 H40A 108.1 . . ?
C41 C40 H40B 108.1 . . ?
C39 C40 C41 117.0(5) . . ?
C39 C40 H40A 108.1 . . ?
C39 C40 H40B 108.1 . . ?
H40A C40 H40B 107.3 . . ?
N3 C8 C7 112.2(4) . . ?
N3 C8 H8A 109.2 . . ?
N3 C8 H8B 109.2 . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C17 C18 C19 118.0(5) . . ?
C17 C18 H18A 107.8 . . ?
C17 C18 H18B 107.8 . . ?
C19 C18 H18A 107.8 . . ?
C19 C18 H18B 107.8 . . ?
H18A C18 H18B 107.1 . . ?
N13 C38 C37 110.5(4) . . ?
N13 C38 H38A 109.6 . . ?
N13 C38 H38B 109.6 . . ?
C37 C38 H38A 109.6 . . ?
C37 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?
N5 C15 C16 109.1(4) . . ?
N5 C15 H15A 109.9 . . ?
N5 C15 H15B 109.9 . . ?
C16 C15 H15A 109.9 . . ?
C16 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
N11 C28 C29 112.2(5) . . ?
N11 C28 H28A 109.2 . . ?
N11 C28 H28B 109.2 . . ?
C29 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
N1 C3 C2 111.7(4) . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
P1 C11 H11A 108.9 . . ?
P1 C11 H11B 108.9 . . ?
N2 C11 P1 113.4(4) . . ?
N2 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C34 C35 C36 116.8(5) . . ?
C34 C35 H35A 108.1 . . ?
C34 C35 H35B 108.1 . . ?
C36 C35 H35A 108.1 . . ?
C36 C35 H35B 108.1 . . ?
H35A C35 H35B 107.3 . . ?
N7 C20 C21 109.4(5) . . ?
N7 C20 H20A 109.8 . . ?
N7 C20 H20B 109.8 . . ?
C21 C20 H20A 109.8 . . ?
C21 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
N14 C42 C43 109.9(4) . . ?
N14 C42 H42A 109.7 . . ?
N14 C42 H42B 109.7 . . ?
C43 C42 H42A 109.7 . . ?
C43 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
P4 C44 H44A 109.1 . . ?
P4 C44 H44B 109.1 . . ?
N14 C44 P4 112.5(3) . . ?
N14 C44 H44A 109.1 . . ?
N14 C44 H44B 109.1 . . ?
H44A C44 H44B 107.8 . . ?
N12 C31 C32 108.3(5) . . ?
N12 C31 H31A 110.0 . . ?
N12 C31 H31B 110.0 . . ?
C32 C31 H31A 110.0 . . ?
C32 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
O11 Ni1 O1 174.77(14) 1_656 . ?
O11 Ni1 N3 87.27(16) 1_656 . ?
O11 Ni1 N2 89.35(15) 1_656 . ?
N3 Ni1 O1 93.30(16) . . ?
N3 Ni1 N2 94.03(19) . . ?
N1 Ni1 O11 90.09(16) . 1_656 ?
N1 Ni1 O1 89.43(16) . . ?
N1 Ni1 N3 177.14(17) . . ?
N1 Ni1 N2 87.06(19) . . ?
N4 Ni1 O11 90.46(16) . 1_656 ?
N4 Ni1 O1 94.77(16) . . ?
N4 Ni1 N3 85.72(19) . . ?
N4 Ni1 N1 93.19(19) . . ?
N4 Ni1 N2 179.69(19) . . ?
N2 Ni1 O1 85.42(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni3 N10 C33 P3 8.2(5) . . . . ?
Ni3 N10 C25 C24 -57.7(5) . . . . ?
Ni3 N10 C26 C27 45.3(4) . . . . ?
Ni3 N11 C27 C26 40.8(5) . . . . ?
Ni3 N11 C28 C29 -57.3(5) . . . . ?
Ni3 N12 C30 C29 55.0(6) . . . . ?
Ni3 N12 C31 C32 -45.5(5) . . . . ?
Ni3 N9 C32 C31 -37.0(5) . . . . ?
Ni3 N9 C23 C24 59.9(5) . . . . ?
Ni4 N14 C41 C40 -59.0(5) . . . . ?
Ni4 N14 C42 C43 46.6(5) . . . . ?
Ni4 N14 C44 P4 10.4(5) . . . . ?
Ni4 N13 C39 C40 57.2(5) . . . . ?
Ni4 N13 C38 C37 -39.5(5) . . . . ?
Ni4 N15 C34 C35 -57.4(6) . . . . ?
Ni4 N15 C43 C42 40.2(5) . . . . ?
Ni4 N16 C36 C35 53.3(6) . . . . ?
Ni4 N16 C37 C38 -42.1(5) . . . . ?
Ni2 N8 C21 C20 42.6(5) . . . . ?
Ni2 N8 C12 C13 -55.5(6) . . . . ?
Ni2 N6 C17 C18 61.2(5) . . . . ?
Ni2 N6 C16 C15 -44.5(5) . . . . ?
Ni2 N6 C22 P2 -9.5(5) . . . . ?
Ni2 N5 C14 C13 55.1(5) . . . . ?
Ni2 N5 C15 C16 -39.4(5) . . . . ?
Ni2 N7 C19 C18 -51.9(6) . . . . ?
Ni2 N7 C20 C21 39.6(5) . . . . ?
O5 P2 O4 Ni2 -151.41(18) . . . . ?
O5 P2 C22 N6 151.7(4) . . . . ?
O4 P2 O5 Ni3 -69.4(3) . . . . ?
O4 P2 C22 N6 33.3(4) . . . . ?
O10 P4 O11 Ni1 68.7(3) . . . 1_454 ?
O10 P4 C44 N14 -31.0(5) . . . . ?
O7 P3 O8 Ni4 130.5(4) . . . . ?
O7 P3 C33 N10 -27.9(4) . . . . ?
O6 P2 O5 Ni3 60.0(3) . . . . ?
O6 P2 O4 Ni2 78.5(2) . . . . ?
O6 P2 C22 N6 -86.9(4) . . . . ?
O11 P4 O10 Ni4 151.85(18) . . . . ?
O11 P4 C44 N14 -150.4(4) . . . . ?
O8 P3 O7 Ni3 148.9(2) . . . . ?
O8 P3 C33 N10 -147.6(4) . . . . ?
O9 P3 O7 Ni3 -80.8(3) . . . . ?
O9 P3 O8 Ni4 0.4(5) . . . . ?
O9 P3 C33 N10 91.5(4) . . . . ?
O1 P1 O3 Ni2 -139.5(4) . . . . ?
O1 P1 C11 N2 31.6(5) . . . . ?
O12 P4 O10 Ni4 -79.1(2) . . . . ?
O12 P4 O11 Ni1 -59.8(3) . . . 1_454 ?
O12 P4 C44 N14 88.4(4) . . . . ?
O2 P1 O1 Ni1 78.9(3) . . . . ?
O2 P1 O3 Ni2 -9.9(6) . . . . ?
O2 P1 C11 N2 -87.8(4) . . . . ?
O3 P1 O1 Ni1 -150.7(2) . . . . ?
O3 P1 C11 N2 150.4(4) . . . . ?
N10 C25 C24 C23 71.2(6) . . . . ?
N11 C27 C26 N10 -61.3(5) . . . . ?
N3 C9 C10 N4 -59.0(6) . . . . ?
N12 C30 C29 C28 -70.8(6) . . . . ?
N8 C21 C20 N7 -57.2(6) . . . . ?
N1 C4 C5 N2 61.0(6) . . . . ?
N14 C41 C40 C39 70.1(6) . . . . ?
N13 C39 C40 C41 -66.3(6) . . . . ?
N6 C17 C18 C19 -70.4(7) . . . . ?
N6 C16 C15 N5 59.8(6) . . . . ?
N15 C34 C35 C36 70.7(7) . . . . ?
N15 C43 C42 N14 -62.1(6) . . . . ?
N5 C14 C13 C12 -69.7(6) . . . . ?
N16 C36 C35 C34 -68.9(7) . . . . ?
N16 C37 C38 N13 56.9(6) . . . . ?
N7 C19 C18 C17 62.8(7) . . . . ?
C33 P3 O7 Ni3 34.4(3) . . . . ?
C33 P3 O8 Ni4 -116.0(4) . . . . ?
C33 N10 C25 C24 67.1(5) . . . . ?
C33 N10 C26 C27 -73.6(5) . . . . ?
N9 C32 C31 N12 57.2(6) . . . . ?
N9 C23 C24 C25 -70.8(6) . . . . ?
C4 N1 C3 C2 177.9(5) . . . . ?
C25 N10 C33 P3 -116.1(4) . . . . ?
C25 N10 C26 C27 163.4(4) . . . . ?
C30 N12 C31 C32 -172.3(5) . . . . ?
C30 C29 C28 N11 72.1(6) . . . . ?
C41 N14 C42 C43 164.7(4) . . . . ?
C41 N14 C44 P4 -114.1(4) . . . . ?
C14 N5 C15 C16 -167.2(4) . . . . ?
C14 C13 C12 N8 69.7(7) . . . . ?
C17 N6 C16 C15 -162.8(5) . . . . ?
C17 N6 C22 P2 115.1(4) . . . . ?
C27 N11 C28 C29 179.6(5) . . . . ?
C5 N2 C6 C7 170.7(4) . . . . ?
C5 N2 C11 P1 -119.2(4) . . . . ?
C32 N9 C23 C24 -179.1(5) . . . . ?
C26 N10 C33 P3 121.4(4) . . . . ?
C26 N10 C25 C24 -170.5(4) . . . . ?
C16 N6 C17 C18 173.5(5) . . . . ?
C16 N6 C22 P2 -121.6(4) . . . . ?
C9 N3 C8 C7 -178.0(5) . . . . ?
C23 N9 C32 C31 -163.0(5) . . . . ?
C19 N7 C20 C21 169.2(5) . . . . ?
C34 N15 C43 C42 168.1(5) . . . . ?
C1 N4 C10 C9 171.8(5) . . . . ?
C1 C2 C3 N1 -70.5(6) . . . . ?
C10 N4 C1 C2 -178.5(5) . . . . ?
C22 P2 O5 Ni3 179.4(3) . . . . ?
C22 P2 O4 Ni2 -40.7(3) . . . . ?
C22 N6 C17 C18 -63.5(6) . . . . ?
C22 N6 C16 C15 73.6(5) . . . . ?
C6 N2 C5 C4 -162.6(4) . . . . ?
C6 N2 C11 P1 118.0(5) . . . . ?
C6 C7 C8 N3 70.1(6) . . . . ?
C21 N8 C12 C13 -176.4(5) . . . . ?
C36 N16 C37 C38 -169.2(4) . . . . ?
C43 N15 C34 C35 -179.6(5) . . . . ?
C37 N16 C36 C35 175.3(5) . . . . ?
C12 N8 C21 C20 169.8(5) . . . . ?
C39 N13 C38 C37 -167.4(5) . . . . ?
C8 N3 C9 C10 163.9(5) . . . . ?
C8 C7 C6 N2 -71.2(6) . . . . ?
C38 N13 C39 C40 178.2(5) . . . . ?
C15 N5 C14 C13 178.0(5) . . . . ?
C28 N11 C27 C26 169.6(4) . . . . ?
C3 N1 C4 C5 -170.2(5) . . . . ?
C3 C2 C1 N4 72.0(6) . . . . ?
C11 P1 O1 Ni1 -39.5(3) . . . . ?
C11 P1 O3 Ni2 109.8(5) . . . . ?
C11 N2 C5 C4 75.0(5) . . . . ?
C11 N2 C6 C7 -67.7(6) . . . . ?
C20 N7 C19 C18 -176.1(5) . . . . ?
C42 N14 C41 C40 -170.9(5) . . . . ?
C42 N14 C44 P4 121.8(4) . . . . ?
C44 P4 O10 Ni4 36.8(3) . . . . ?
C44 P4 O11 Ni1 -176.9(3) . . . 1_454 ?
C44 N14 C41 C40 65.9(6) . . . . ?
C44 N14 C42 C43 -71.7(5) . . . . ?
C31 N12 C30 C29 176.6(5) . . . . ?
Ni1 N3 C9 C10 39.9(5) . . . . ?
Ni1 N3 C8 C7 -58.4(5) . . . . ?
Ni1 N1 C4 C5 -41.2(5) . . . . ?
Ni1 N1 C3 C2 54.9(5) . . . . ?
Ni1 N4 C1 C2 -58.1(6) . . . . ?
Ni1 N4 C10 C9 44.2(5) . . . . ?
Ni1 N2 C5 C4 -43.5(5) . . . . ?
Ni1 N2 C6 C7 59.0(5) . . . . ?
Ni1 N2 C11 P1 -8.5(5) . . . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
