#------------------------------------------------------------------------------
#$Date: 2016-02-13 13:50:18 +0100 (Sat 13 de Feb de 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/76/7117650.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_7117650
loop_
_publ_author_name
'Jesus Ferrando-Soria'
'Oscar Fabelo'
'Maria Castellano'
'Joan Cano'
'Stephen Fordham'
'Hong-Cai Zhou'
_publ_section_title
;
 Multielectron oxidation in a ferromagnetically coupled dinickel(II)
 triple mesocate
;
_journal_name_full               Chem.Commun.
_journal_page_first              13381
_journal_paper_doi               10.1039/C5cc03544A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C51 H47 K2 N18 Ni2 O12'
_chemical_formula_weight         1299.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-23 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.536(3)
_cell_length_b                   28.635(6)
_cell_length_c                   15.794(3)
_cell_measurement_temperature    100(2)
_cell_volume                     5668(2)
_computing_cell_refinement       'SAINT  (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT  (Bruker, 2004)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57546
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2676
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.276
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         11146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1393P)²+17.7053P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2414
_reflns_number_gt                7857
_reflns_number_total             11146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03544a3.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        5667(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7117650
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 -0.04095(5) 0.12806(2) 0.80692(4) 0.0192(2) Uani 1 1 d . . .
Ni2 Ni 0.02467(5) 0.36713(2) 0.79161(4) 0.0217(2) Uani 1 1 d . . .
K1 K 0.12471(13) 0.23032(10) 1.13539(13) 0.0840(8) Uani 1 1 d . . .
K2 K 0.33593(10) 0.23459(5) 0.59893(8) 0.0304(3) Uani 1 1 d . . .
C1 C -0.2076(4) 0.0523(2) 0.8533(3) 0.0273(12) Uani 1 1 d . . .
H1 H -0.1524 0.0353 0.8789 0.033 Uiso 1 1 calc R . .
C2 C -0.3115(5) 0.0361(2) 0.8574(4) 0.0336(14) Uani 1 1 d . . .
H2 H -0.3240 0.0081 0.8851 0.040 Uiso 1 1 calc R . .
C3 C -0.3709(5) 0.0991(2) 0.7822(4) 0.0352(14) Uani 1 1 d . . .
H3 H -0.4266 0.1162 0.7575 0.042 Uiso 1 1 calc R . .
C4 C -0.2669(4) 0.1156(2) 0.7757(3) 0.0270(12) Uani 1 1 d . . .
C5 C -0.2404(4) 0.1592(2) 0.7271(3) 0.0247(12) Uani 1 1 d . . .
C6 C -0.1027(4) 0.20657(19) 0.6756(3) 0.0217(11) Uani 1 1 d . . .
C7 C -0.0417(4) 0.20088(19) 0.6034(3) 0.0250(12) Uani 1 1 d . . .
H7 H -0.0309 0.1712 0.5811 0.030 Uiso 1 1 calc R . .
C8 C 0.0030(4) 0.2397(2) 0.5650(3) 0.0269(12) Uani 1 1 d . . .
H8 H 0.0432 0.2358 0.5169 0.032 Uiso 1 1 calc R . .
C9 C -0.0118(5) 0.28458(19) 0.5977(3) 0.0265(12) Uani 1 1 d . . .
H9 H 0.0195 0.3103 0.5723 0.032 Uiso 1 1 calc R . .
C10 C -0.0740(4) 0.29037(19) 0.6687(3) 0.0240(11) Uani 1 1 d . . .
C11 C -0.1207(4) 0.25154(19) 0.7056(3) 0.0228(11) Uani 1 1 d . . .
H11 H -0.1649 0.2557 0.7513 0.027 Uiso 1 1 calc R . .
C12 C -0.1781(6) 0.3550(3) 0.7001(5) 0.050(2) Uani 1 1 d . . .
C13 C -0.1874(5) 0.4006(2) 0.7485(4) 0.0325(14) Uani 1 1 d . . .
C14 C -0.2827(5) 0.4243(2) 0.7532(4) 0.0394(16) Uani 1 1 d . . .
H14 H -0.3431 0.4120 0.7258 0.047 Uiso 1 1 calc R . .
C15 C -0.2020(5) 0.4807(2) 0.8326(4) 0.0382(15) Uani 1 1 d . . .
H15 H -0.2039 0.5090 0.8613 0.046 Uiso 1 1 calc R . .
C16 C -0.1065(5) 0.4570(2) 0.8292(4) 0.0343(14) Uani 1 1 d . . .
H16 H -0.0459 0.4697 0.8554 0.041 Uiso 1 1 calc R . .
C17 C 0.0756(5) 0.0480(2) 0.9050(4) 0.0291(12) Uani 1 1 d . . .
H17 H 0.0808 0.0324 0.8536 0.035 Uiso 1 1 calc R . .
C18 C 0.1188(6) 0.0279(2) 0.9778(4) 0.0447(17) Uani 1 1 d . . .
H18 H 0.1514 -0.0012 0.9743 0.054 Uiso 1 1 calc R . .
C19 C 0.0671(7) 0.0906(2) 1.0541(4) 0.0473(19) Uani 1 1 d . . .
H19 H 0.0634 0.1064 1.1054 0.057 Uiso 1 1 calc R . .
C20 C 0.0233(5) 0.11073(19) 0.9826(3) 0.0259(12) Uani 1 1 d . . .
C21 C -0.0308(4) 0.15815(19) 0.9847(3) 0.0229(11) Uani 1 1 d . . .
C22 C -0.1294(4) 0.21351(19) 0.9093(3) 0.0221(11) Uani 1 1 d . . .
C23 C -0.2400(4) 0.2193(2) 0.9006(3) 0.0261(12) Uani 1 1 d . . .
H23 H -0.2849 0.1934 0.9002 0.031 Uiso 1 1 calc R . .
C24 C -0.2820(4) 0.2638(2) 0.8926(3) 0.0272(12) Uani 1 1 d . . .
H24 H -0.3555 0.2674 0.8872 0.033 Uiso 1 1 calc R . .
C25 C -0.2172(4) 0.3030(2) 0.8925(3) 0.0267(12) Uani 1 1 d . . .
H25 H -0.2471 0.3326 0.8859 0.032 Uiso 1 1 calc R . .
C26 C -0.1068(4) 0.29789(19) 0.9024(3) 0.0217(11) Uani 1 1 d . . .
C27 C -0.0640(4) 0.25342(18) 0.9111(3) 0.0214(11) Uani 1 1 d . . .
H27 H 0.0094 0.2499 0.9183 0.026 Uiso 1 1 calc R . .
C28 C 0.0139(4) 0.3451(2) 0.9725(3) 0.0257(12) Uani 1 1 d . . .
C29 C 0.0997(4) 0.38150(19) 0.9664(3) 0.0241(11) Uani 1 1 d . . .
C30 C 0.1658(5) 0.3925(2) 1.0358(4) 0.0289(12) Uani 1 1 d . . .
H30 H 0.1535 0.3783 1.0876 0.035 Uiso 1 1 calc R . .
C31 C 0.2621(6) 0.4406(3) 0.9545(4) 0.0467(18) Uani 1 1 d . . .
H31 H 0.3182 0.4615 0.9481 0.056 Uiso 1 1 calc R . .
C32 C 0.1985(5) 0.4296(2) 0.8838(4) 0.0372(15) Uani 1 1 d . . .
H32 H 0.2137 0.4427 0.8315 0.045 Uiso 1 1 calc R . .
C33 C -0.0335(4) 0.04812(19) 0.6729(4) 0.0269(12) Uani 1 1 d . . .
H33 H -0.0919 0.0348 0.6988 0.032 Uiso 1 1 calc R . .
C34 C 0.0029(5) 0.0289(2) 0.5992(4) 0.0308(13) Uani 1 1 d . . .
H34 H -0.0318 0.0028 0.5767 0.037 Uiso 1 1 calc R . .
C35 C 0.1322(5) 0.0838(2) 0.5953(4) 0.0288(12) Uani 1 1 d . . .
H35 H 0.1902 0.0973 0.5692 0.035 Uiso 1 1 calc R . .
C36 C 0.0972(4) 0.10310(18) 0.6697(3) 0.0210(11) Uani 1 1 d . . .
C37 C 0.1503(4) 0.14472(18) 0.7105(3) 0.0198(10) Uani 1 1 d . . .
C38 C 0.1496(4) 0.19772(18) 0.8222(3) 0.0188(10) Uani 1 1 d . . .
C39 C 0.1978(4) 0.19573(18) 0.9028(3) 0.0213(11) Uani 1 1 d . . .
H39 H 0.2044 0.1672 0.9307 0.026 Uiso 1 1 calc R . .
C40 C 0.2361(4) 0.2366(2) 0.9419(3) 0.0241(11) Uani 1 1 d . . .
C41 C 0.2235(4) 0.27967(19) 0.9010(3) 0.0226(11) Uani 1 1 d . . .
H41 H 0.2477 0.3069 0.9272 0.027 Uiso 1 1 calc R . .
C42 C 0.1743(4) 0.28160(18) 0.8206(3) 0.0203(10) Uani 1 1 d . . .
C43 C 0.1404(4) 0.24073(18) 0.7816(3) 0.0213(11) Uani 1 1 d . . .
H43 H 0.1107 0.2420 0.7271 0.026 Uiso 1 1 calc R . .
C44 C 0.2179(4) 0.33342(19) 0.7141(4) 0.0259(12) Uani 1 1 d . . .
C45 C 0.1882(5) 0.3765(2) 0.6652(4) 0.0293(13) Uani 1 1 d . . .
C46 C 0.2441(6) 0.3907(2) 0.5953(4) 0.0430(16) Uani 1 1 d . . .
H46 H 0.3024 0.3731 0.5788 0.052 Uiso 1 1 calc R . .
C47 C 0.1329(7) 0.4519(3) 0.5772(5) 0.054(2) Uani 1 1 d . . .
H47 H 0.1109 0.4785 0.5476 0.065 Uiso 1 1 calc R . .
C48 C 0.0766(6) 0.4385(2) 0.6463(4) 0.0424(16) Uani 1 1 d . . .
H48 H 0.0183 0.4563 0.6620 0.051 Uiso 1 1 calc R . .
N1 N -0.1858(3) 0.09207(16) 0.8130(3) 0.0234(10) Uani 1 1 d . . .
N2 N -0.3937(4) 0.0591(2) 0.8232(4) 0.0405(13) Uani 1 1 d . . .
N3 N -0.1371(3) 0.16642(15) 0.7215(3) 0.0206(9) Uani 1 1 d . . .
N4 N -0.0993(4) 0.41605(16) 0.7889(3) 0.0262(10) Uani 1 1 d . . .
N5 N -0.2912(4) 0.46455(19) 0.7963(3) 0.0400(13) Uani 1 1 d . . .
N6 N -0.0848(4) 0.33512(16) 0.7077(3) 0.0259(10) Uani 1 1 d . . .
N7 N 0.0269(3) 0.08916(15) 0.9075(3) 0.0226(9) Uani 1 1 d . . .
N8 N 0.1150(7) 0.0490(2) 1.0527(4) 0.069(2) Uani 1 1 d . . .
N9 N -0.0809(3) 0.16849(15) 0.9118(3) 0.0212(9) Uani 1 1 d . . .
N10 N 0.1157(4) 0.40031(15) 0.8900(3) 0.0252(10) Uani 1 1 d . . .
N11 N 0.2464(4) 0.42283(19) 1.0303(3) 0.0384(13) Uani 1 1 d . . .
N12 N -0.0351(3) 0.33625(15) 0.8999(3) 0.0210(9) Uani 1 1 d . . .
N13 N 0.0130(3) 0.08544(15) 0.7079(3) 0.0213(9) Uani 1 1 d . . .
N14 N 0.0857(4) 0.04622(18) 0.5592(3) 0.0333(11) Uani 1 1 d . . .
N15 N 0.1063(3) 0.15738(15) 0.7812(3) 0.0203(9) Uani 1 1 d . . .
N16 N 0.1027(4) 0.40073(17) 0.6916(3) 0.0285(10) Uani 1 1 d . . .
N17 N 0.2174(5) 0.4287(2) 0.5505(4) 0.0534(16) Uani 1 1 d . . .
N18 N 0.1556(3) 0.32447(16) 0.7771(3) 0.0225(9) Uani 1 1 d . . .
O1 O -0.3163(3) 0.18225(15) 0.6951(3) 0.0311(9) Uani 1 1 d . . .
O2 O -0.2575(6) 0.3424(3) 0.6563(6) 0.122(4) Uani 1 1 d . . .
O3 O -0.0253(3) 0.18102(14) 1.0520(2) 0.0276(9) Uani 1 1 d . . .
O4 O -0.0019(4) 0.32669(16) 1.0438(3) 0.0389(11) Uani 1 1 d . . .
O5 O 0.2303(3) 0.16224(13) 0.6743(2) 0.0259(8) Uani 1 1 d . . .
O6 O 0.2976(3) 0.31044(15) 0.6908(3) 0.0365(10) Uani 1 1 d . . .
C1M C -0.0522(5) 0.2863(3) 1.3039(4) 0.0383(15) Uani 1 1 d . . .
H1M1 H -0.0941 0.2602 1.3221 0.046 Uiso 1 1 calc R . .
H1M2 H -0.0970 0.3133 1.2981 0.046 Uiso 1 1 calc R . .
H1M3 H 0.0038 0.2923 1.3451 0.046 Uiso 1 1 calc R . .
C2M C -0.1096(10) 0.4667(4) 1.0324(6) 0.085(3) Uani 1 1 d . . .
H2M1 H -0.1848 0.4682 1.0198 0.103 Uiso 1 1 calc R . .
H2M2 H -0.0814 0.4380 1.0111 0.103 Uiso 1 1 calc R . .
H2M3 H -0.0747 0.4926 1.0061 0.103 Uiso 1 1 calc R . .
C3M C 0.4777(8) 0.3578(4) 0.8236(6) 0.075(3) Uani 1 1 d . . .
H3M1 H 0.4511 0.3289 0.8457 0.090 Uiso 1 1 calc R . .
H3M2 H 0.4294 0.3826 0.8366 0.090 Uiso 1 1 calc R . .
H3M3 H 0.5466 0.3643 0.8489 0.090 Uiso 1 1 calc R . .
O1M O -0.0086(6) 0.2761(3) 1.2274(4) 0.091(2) Uani 1 1 d . . .
O2M O -0.0916(6) 0.4688(2) 1.1213(4) 0.083(2) Uani 1 1 d . . .
O3M O 0.4863(8) 0.3542(5) 0.7378(5) 0.179(6) Uani 1 1 d . . .
O1W O -0.0790(4) 0.38256(18) 1.1655(3) 0.0462(12) Uani 1 1 d . . .
O2W O 0.2331(8) 0.5174(3) 0.7475(5) 0.111(3) Uani 1 1 d . . .
O3W O 0.1305(16) 0.5877(6) 0.5063(15) 0.367(17) Uani 1 1 d . . .
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'
K K 0.2009 0.2494 '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'
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
N15 Ni1 N9 99.44(17) . .
N15 Ni1 N1 169.96(17) . .
N9 Ni1 N1 90.53(17) . .
N15 Ni1 N3 99.27(17) . .
N9 Ni1 N3 94.24(17) . .
N1 Ni1 N3 78.64(18) . .
N15 Ni1 N7 91.03(17) . .
N9 Ni1 N7 78.20(17) . .
N1 Ni1 N7 92.20(17) . .
N3 Ni1 N7 168.15(17) . .
N15 Ni1 N13 77.59(17) . .
N9 Ni1 N13 174.42(17) . .
N1 Ni1 N13 92.58(17) . .
N3 Ni1 N13 90.92(16) . .
N7 Ni1 N13 97.04(17) . .
N18 Ni2 N12 98.32(17) . .
N18 Ni2 N4 170.66(18) . .
N12 Ni2 N4 91.02(17) . .
N18 Ni2 N6 100.40(18) . .
N12 Ni2 N6 95.17(18) . .
N4 Ni2 N6 78.82(18) . .
N18 Ni2 N16 78.50(18) . .
N12 Ni2 N16 172.58(18) . .
N4 Ni2 N16 92.20(18) . .
N6 Ni2 N16 92.01(19) . .
N18 Ni2 N10 86.15(18) . .
N12 Ni2 N10 77.71(17) . .
N4 Ni2 N10 95.71(18) . .
N6 Ni2 N10 171.04(19) . .
N16 Ni2 N10 95.31(18) . .
O2 K1 O1M 135.5(3) 4_666 .
O2 K1 O3 91.70(17) 4_666 .
O1M K1 O3 95.0(2) . .
O2 K1 O1 122.80(16) 4_666 4_666
O1M K1 O1 61.5(2) . 4_666
O3 K1 O1 145.50(15) . 4_666
O2 K1 C11 63.21(15) 4_666 4_666
O1M K1 C11 110.71(19) . 4_666
O3 K1 C11 152.45(15) . 4_666
O1 K1 C11 60.64(13) 4_666 4_666
O2 K1 C40 84.8(2) 4_666 .
O1M K1 C40 139.6(2) . .
O3 K1 C40 83.41(13) . .
O1 K1 C40 98.42(15) 4_666 .
C11 K1 C40 83.13(13) 4_666 .
O2 K1 O3M 70.2(2) 4_666 4_566
O1M K1 O3M 75.5(3) . 4_566
O3 K1 O3M 59.89(19) . 4_566
O1 K1 O3M 127.9(2) 4_666 4_566
C11 K1 O3M 116.09(18) 4_666 4_566
C40 K1 O3M 133.7(2) . 4_566
O2 K1 K2 141.13(14) 4_666 4_566
O1M K1 K2 47.51(15) . 4_566
O3 K1 K2 53.66(9) . 4_566
O1 K1 K2 93.29(11) 4_666 4_566
C11 K1 K2 153.76(12) 4_666 4_566
C40 K1 K2 105.26(11) . 4_566
O3M K1 K2 76.36(13) 4_566 4_566
O6 K2 O5 106.42(13) . .
O6 K2 O1M 80.0(2) . 4_665
O5 K2 O1M 86.40(15) . 4_665
O6 K2 O4 144.31(14) . 4_665
O5 K2 O4 91.38(13) . 4_665
O1M K2 O4 70.3(2) 4_665 4_665
O6 K2 O3 66.57(12) . 4_665
O5 K2 O3 167.93(12) . 4_665
O1M K2 O3 82.72(15) 4_665 4_665
O4 K2 O3 89.86(13) 4_665 4_665
O6 K2 C27 119.21(14) . 4_665
O5 K2 C27 132.34(13) . 4_665
O1M K2 C27 113.17(17) 4_665 4_665
O4 K2 C27 59.43(13) 4_665 4_665
O3 K2 C27 57.75(12) 4_665 4_665
O6 K2 C26 141.33(14) . 4_665
O5 K2 C26 108.13(13) . 4_665
O1M K2 C26 118.8(2) 4_665 4_665
O4 K2 C26 50.87(12) 4_665 4_665
O3 K2 C26 81.84(12) 4_665 4_665
C27 K2 C26 24.22(13) 4_665 4_665
O6 K2 C22 98.83(14) . 4_665
O5 K2 C22 142.20(13) . 4_665
O1M K2 C22 126.02(15) 4_665 4_665
O4 K2 C22 83.68(13) 4_665 4_665
O3 K2 C22 49.86(12) 4_665 4_665
C27 K2 C22 24.34(13) 4_665 4_665
C26 K2 C22 42.50(13) 4_665 4_665
O6 K2 C25 136.88(14) . 4_665
O5 K2 C25 95.18(12) . 4_665
O1M K2 C25 139.4(2) 4_665 4_665
O4 K2 C25 69.04(13) 4_665 4_665
O3 K2 C25 96.47(12) 4_665 4_665
C27 K2 C25 41.52(13) 4_665 4_665
C26 K2 C25 23.52(12) 4_665 4_665
C22 K2 C25 48.12(13) 4_665 4_665
O6 K2 C23 97.52(14) . 4_665
O5 K2 C23 123.28(13) . 4_665
O1M K2 C23 149.06(16) 4_665 4_665
O4 K2 C23 97.95(13) 4_665 4_665
O3 K2 C23 68.36(12) 4_665 4_665
C27 K2 C23 41.57(12) 4_665 4_665
C26 K2 C23 48.27(13) 4_665 4_665
C22 K2 C23 23.34(12) 4_665 4_665
C25 K2 C23 40.50(14) 4_665 4_665
O6 K2 K1 83.47(11) . 4_665
O5 K2 K1 127.15(9) . 4_665
O1M K2 K1 43.34(12) 4_665 4_665
O4 K2 K1 61.40(11) 4_665 4_665
O3 K2 K1 44.31(8) 4_665 4_665
C27 K2 K1 73.84(10) 4_665 4_665
C26 K2 K1 89.25(10) 4_665 4_665
C22 K2 K1 82.72(10) 4_665 4_665
C25 K2 K1 112.52(10) 4_665 4_665
C23 K2 K1 105.76(10) 4_665 4_665
N1 C1 C2 120.8(5) . .
N2 C2 C1 122.5(6) . .
N2 C3 C4 122.3(6) . .
N1 C4 C3 119.7(6) . .
N1 C4 C5 117.7(5) . .
C3 C4 C5 122.6(5) . .
O1 C5 N3 128.9(6) . .
O1 C5 C4 117.8(5) . .
N3 C5 C4 113.2(5) . .
C11 C6 C7 118.8(5) . .
C11 C6 N3 121.1(5) . .
C7 C6 N3 119.9(5) . .
C8 C7 C6 119.8(5) . .
C7 C8 C9 121.0(5) . .
C10 C9 C8 119.3(5) . .
C11 C10 C9 119.5(5) . .
C11 C10 N6 119.3(5) . .
C9 C10 N6 121.0(5) . .
C10 C11 C6 121.5(5) . .
C10 C11 K1 98.3(3) . 4_565
C6 C11 K1 100.9(3) . 4_565
O2 C12 N6 128.6(6) . .
O2 C12 C13 117.1(6) . .
N6 C12 C13 114.2(6) . .
N4 C13 C14 121.2(5) . .
N4 C13 C12 116.9(5) . .
C14 C13 C12 121.9(5) . .
N5 C14 C13 122.0(6) . .
N5 C15 C16 122.3(6) . .
N4 C16 C15 121.3(6) . .
N7 C17 C18 120.9(5) . .
N8 C18 C17 121.9(6) . .
N8 C19 C20 122.2(6) . .
N7 C20 C19 120.9(5) . .
N7 C20 C21 117.2(5) . .
C19 C20 C21 121.9(5) . .
O3 C21 N9 129.4(5) . .
O3 C21 C20 118.2(5) . .
N9 C21 C20 112.4(4) . .
C23 C22 C27 118.8(5) . .
C23 C22 N9 122.0(5) . .
C27 C22 N9 119.1(5) . .
C23 C22 K2 83.4(3) . 4_566
C27 C22 K2 73.3(3) . 4_566
N9 C22 K2 116.0(3) . 4_566
C24 C23 C22 119.4(5) . .
C24 C23 K2 80.1(3) . 4_566
C22 C23 K2 73.3(3) . 4_566
C23 C24 C25 121.7(5) . .
C24 C25 C26 119.5(5) . .
C24 C25 K2 81.1(3) . 4_566
C26 C25 K2 72.4(3) . 4_566
C27 C26 C25 119.2(5) . .
C27 C26 N12 118.0(4) . .
C25 C26 N12 122.8(5) . .
C27 C26 K2 75.2(3) . 4_566
C25 C26 K2 84.0(3) . 4_566
N12 C26 K2 113.2(3) . 4_566
C26 C27 C22 121.3(5) . .
C26 C27 K2 80.6(3) . 4_566
C22 C27 K2 82.3(3) . 4_566
O4 C28 N12 128.2(5) . .
O4 C28 C29 118.5(5) . .
N12 C28 C29 113.4(5) . .
N10 C29 C30 121.1(5) . .
N10 C29 C28 117.5(5) . .
C30 C29 C28 121.2(5) . .
N11 C30 C29 122.1(5) . .
N11 C31 C32 123.0(6) . .
N10 C32 C31 120.7(6) . .
N13 C33 C34 121.5(5) . .
N14 C34 C33 122.3(5) . .
N14 C35 C36 122.5(5) . .
N13 C36 C35 120.6(5) . .
N13 C36 C37 117.0(5) . .
C35 C36 C37 122.4(5) . .
O5 C37 N15 129.0(5) . .
O5 C37 C36 117.8(5) . .
N15 C37 C36 113.2(4) . .
C43 C38 C39 119.0(5) . .
C43 C38 N15 118.8(4) . .
C39 C38 N15 122.1(5) . .
C38 C39 C40 120.2(5) . .
C41 C40 C39 120.0(5) . .
C41 C40 K1 114.7(4) . .
C39 C40 K1 102.0(3) . .
C42 C41 C40 119.7(5) . .
C43 C42 C41 119.6(5) . .
C43 C42 N18 118.0(5) . .
C41 C42 N18 122.4(5) . .
C42 C43 C38 121.5(5) . .
O6 C44 N18 127.9(5) . .
O6 C44 C45 117.9(5) . .
N18 C44 C45 114.2(5) . .
N16 C45 C46 121.2(5) . .
N16 C45 C44 116.8(5) . .
C46 C45 C44 121.9(5) . .
N17 C46 C45 122.4(6) . .
N17 C47 C48 122.9(6) . .
N16 C48 C47 122.1(6) . .
C1 N1 C4 118.3(5) . .
C1 N1 Ni1 129.1(4) . .
C4 N1 Ni1 112.4(4) . .
C2 N2 C3 116.3(5) . .
C5 N3 C6 118.0(4) . .
C5 N3 Ni1 115.1(4) . .
C6 N3 Ni1 124.8(3) . .
C13 N4 C16 116.8(5) . .
C13 N4 Ni2 113.1(4) . .
C16 N4 Ni2 129.6(4) . .
C15 N5 C14 116.1(5) . .
C12 N6 C10 116.6(5) . .
C12 N6 Ni2 116.0(4) . .
C10 N6 Ni2 126.6(3) . .
C17 N7 C20 117.5(5) . .
C17 N7 Ni1 128.7(4) . .
C20 N7 Ni1 113.7(4) . .
C18 N8 C19 116.5(6) . .
C21 N9 C22 114.6(4) . .
C21 N9 Ni1 116.4(4) . .
C22 N9 Ni1 126.1(3) . .
C32 N10 C29 116.9(5) . .
C32 N10 Ni2 128.8(4) . .
C29 N10 Ni2 112.8(4) . .
C31 N11 C30 116.1(5) . .
C28 N12 C26 114.0(4) . .
C28 N12 Ni2 117.8(4) . .
C26 N12 Ni2 126.4(3) . .
C36 N13 C33 117.4(5) . .
C36 N13 Ni1 113.0(3) . .
C33 N13 Ni1 128.9(4) . .
C34 N14 C35 115.7(5) . .
C37 N15 C38 116.6(4) . .
C37 N15 Ni1 116.8(3) . .
C38 N15 Ni1 124.7(3) . .
C48 N16 C45 115.8(5) . .
C48 N16 Ni2 131.2(4) . .
C45 N16 Ni2 112.6(4) . .
C47 N17 C46 115.5(6) . .
C44 N18 C42 116.3(4) . .
C44 N18 Ni2 117.5(4) . .
C42 N18 Ni2 125.3(3) . .
C5 O1 K1 143.7(4) . 4_565
C12 O2 K1 138.8(7) . 4_565
C21 O3 K1 136.0(3) . .
C21 O3 K2 126.7(3) . 4_566
K1 O3 K2 82.03(11) . 4_566
C28 O4 K2 131.4(3) . 4_566
C37 O5 K2 152.6(3) . .
C44 O6 K2 137.8(4) . .
C1M O1M K1 151.3(5) . .
C1M O1M K2 112.1(5) . 4_566
K1 O1M K2 89.15(19) . 4_566
C3M O3M K1 125.3(10) . 4_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N15 2.077(4) .
Ni1 N9 2.092(4) .
Ni1 N1 2.093(4) .
Ni1 N3 2.096(4) .
Ni1 N7 2.102(4) .
Ni1 N13 2.109(4) .
Ni2 N18 2.063(4) .
Ni2 N12 2.083(4) .
Ni2 N4 2.091(5) .
Ni2 N6 2.094(5) .
Ni2 N16 2.112(5) .
Ni2 N10 2.128(5) .
K1 O2 2.569(8) 4_666
K1 O1M 2.599(6) .
K1 O3 2.671(4) .
K1 O1 2.769(5) 4_666
K1 C11 3.391(5) 4_666
K1 C40 3.398(6) .
K1 O3M 3.412(15) 4_566
K1 K2 3.786(2) 4_566
K2 O6 2.663(4) .
K2 O5 2.747(4) .
K2 O1M 2.792(7) 4_665
K2 O4 2.839(4) 4_665
K2 O3 3.079(4) 4_665
K2 C27 3.269(5) 4_665
K2 C26 3.336(5) 4_665
K2 C22 3.382(5) 4_665
K2 C25 3.480(6) 4_665
K2 C23 3.508(5) 4_665
K2 K1 3.786(2) 4_665
C1 N1 1.335(7) .
C1 C2 1.385(8) .
C2 N2 1.325(8) .
C3 N2 1.350(9) .
C3 C4 1.393(8) .
C4 N1 1.343(7) .
C4 C5 1.508(8) .
C5 O1 1.252(7) .
C5 N3 1.317(7) .
C6 C11 1.393(7) .
C6 C7 1.399(8) .
C6 N3 1.432(7) .
C7 C8 1.392(8) .
C8 C9 1.398(8) .
C9 C10 1.392(8) .
C10 C11 1.392(8) .
C10 N6 1.430(7) .
C11 K1 3.391(5) 4_565
C12 O2 1.250(8) .
C12 N6 1.303(8) .
C12 C13 1.519(8) .
C13 N4 1.336(7) .
C13 C14 1.378(8) .
C14 N5 1.344(8) .
C15 N5 1.326(8) .
C15 C16 1.378(9) .
C16 N4 1.337(7) .
C17 N7 1.330(7) .
C17 C18 1.382(8) .
C18 N8 1.331(9) .
C19 N8 1.335(9) .
C19 C20 1.370(8) .
C20 N7 1.339(7) .
C20 C21 1.519(8) .
C21 O3 1.249(6) .
C21 N9 1.330(7) .
C22 C23 1.399(7) .
C22 C27 1.406(7) .
C22 N9 1.425(7) .
C22 K2 3.382(5) 4_566
C23 C24 1.383(8) .
C23 K2 3.508(5) 4_566
C24 C25 1.387(8) .
C25 C26 1.396(7) .
C25 K2 3.480(6) 4_566
C26 C27 1.387(7) .
C26 N12 1.421(7) .
C26 K2 3.336(5) 4_566
C27 K2 3.269(5) 4_566
C28 O4 1.263(7) .
C28 N12 1.311(7) .
C28 C29 1.504(8) .
C29 N10 1.341(7) .
C29 C30 1.393(8) .
C30 N11 1.336(8) .
C31 N11 1.321(8) .
C31 C32 1.391(9) .
C32 N10 1.340(8) .
C33 N13 1.330(7) .
C33 C34 1.376(8) .
C34 N14 1.327(8) .
C35 N14 1.344(7) .
C35 C36 1.380(8) .
C36 N13 1.330(7) .
C36 C37 1.502(7) .
C37 O5 1.271(6) .
C37 N15 1.310(7) .
C38 C43 1.392(7) .
C38 C39 1.396(7) .
C38 N15 1.425(6) .
C39 C40 1.402(7) .
C40 C41 1.399(8) .
C41 C42 1.398(7) .
C42 C43 1.384(7) .
C42 N18 1.424(7) .
C44 O6 1.260(7) .
C44 N18 1.306(7) .
C44 C45 1.497(8) .
C45 N16 1.351(8) .
C45 C46 1.385(9) .
C46 N17 1.336(9) .
C47 N17 1.328(10) .
C47 C48 1.370(10) .
C48 N16 1.333(8) .
O1 K1 2.769(5) 4_565
O2 K1 2.569(8) 4_565
O3 K2 3.079(4) 4_566
O4 K2 2.839(4) 4_566
C1M O1M 1.371(8) .
C2M O2M 1.418(11) .
C3M O3M 1.365(12) .
O1M K2 2.792(7) 4_566
O3M K1 3.412(15) 4_665
