#------------------------------------------------------------------------------
#$Date: 2019-11-14 09:37:35 +0200 (Thu, 14 Nov 2019) $
#$Revision: 227761 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/29/1552908.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_1552908
loop_
_publ_author_name
'Hartmann, Nathaniel J.'
'Wu, Guang'
'Hayton, Trevor W.'
_publ_section_title
;
 Synthesis and reactivity of a nickel(ii) thioperoxide complex:
 demonstration of sulfide-mediated N₂O reduction.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              6580
_journal_page_last               6588
_journal_paper_doi               10.1039/c8sc02536c
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C101 H166 K2 N4 Ni2 O18'
_chemical_formula_weight         1919.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.268(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8490(19)
_cell_length_b                   17.4488(12)
_cell_length_c                   27.016(2)
_cell_measurement_reflns_used    545
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      1.96
_cell_volume                     10593.0(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kapa Apex II'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.1559
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47795
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.392
_diffrn_reflns_theta_min         0.933
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.7063
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         21602
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1954
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0978P)²+25.2454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10228
_reflns_number_total             21602
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc02536c2.cif
_cod_data_source_block           NH_6_84_0m_a
_cod_original_cell_volume        10592.8(14)
_cod_database_code               1552908
_shelx_shelxl_version_number     2014/7
_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'
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
Ni1 Ni 0.20820(3) 0.28582(4) 0.64116(3) 0.01605(19) Uani 1 1 d . . .
Ni2 Ni 0.71628(3) 0.20910(5) 0.64904(3) 0.0187(2) Uani 1 1 d . . .
K1 K -0.01302(6) 0.31327(8) 0.43696(6) 0.0270(3) Uani 1 1 d . . .
K2 K 0.49802(7) 0.17452(9) 0.44223(6) 0.0372(4) Uani 1 1 d . . .
O1 O 0.13275(17) 0.3300(2) 0.62144(16) 0.0221(10) Uani 1 1 d . . .
O4 O 0.63866(18) 0.1715(3) 0.62798(18) 0.0269(10) Uani 1 1 d . . .
N1 N 0.2370(2) 0.3025(3) 0.71703(19) 0.0170(11) Uani 1 1 d . . .
O2 O 0.16009(17) 0.2741(2) 0.56490(16) 0.0236(10) Uani 1 1 d . . .
O5 O 0.67238(18) 0.2149(3) 0.57239(17) 0.0292(11) Uani 1 1 d . . .
O16 O 0.4333(2) 0.0377(3) 0.41339(19) 0.0368(12) Uani 1 1 d . . .
N3 N 0.7408(2) 0.1986(3) 0.7250(2) 0.0188(11) Uani 1 1 d . . .
O3 O 0.06856(18) 0.3269(3) 0.53183(18) 0.0326(12) Uani 1 1 d . . .
N2 N 0.2783(2) 0.2456(3) 0.64106(19) 0.0176(11) Uani 1 1 d . . .
O6 O 0.57767(19) 0.1736(3) 0.53780(19) 0.0362(12) Uani 1 1 d . . .
O7 O 0.0345(2) 0.1833(3) 0.4012(2) 0.0430(13) Uani 1 1 d . . .
O12 O 0.0588(2) 0.3414(3) 0.3836(2) 0.0434(13) Uani 1 1 d . . .
N4 N 0.7879(2) 0.2434(3) 0.6498(2) 0.0223(12) Uani 1 1 d . . .
O9 O -0.0843(2) 0.2813(3) 0.49198(19) 0.0419(13) Uani 1 1 d . . .
O8 O -0.0062(2) 0.1727(3) 0.4833(2) 0.0451(14) Uani 1 1 d . . .
O17 O 0.42656(19) 0.1353(3) 0.48985(19) 0.0364(12) Uani 1 1 d . . .
O15 O 0.5352(2) 0.0572(3) 0.3954(2) 0.0467(14) Uani 1 1 d . . .
O11 O 0.0028(2) 0.4645(3) 0.4128(2) 0.0469(14) Uani 1 1 d . . .
O10 O -0.0917(3) 0.4224(3) 0.4368(2) 0.0519(15) Uani 1 1 d . . .
O18 O 0.4591(3) 0.2928(3) 0.4938(2) 0.0562(16) Uani 1 1 d . . .
O14 O 0.5734(3) 0.2104(4) 0.3910(2) 0.0593(16) Uani 1 1 d . . .
O13 O 0.5409(3) 0.3213(3) 0.4496(3) 0.0695(19) Uani 1 1 d . . .
C50 C 0.7947(3) 0.2182(3) 0.7631(2) 0.0203(13) Uani 1 1 d . . .
C15 C 0.2904(2) 0.2815(3) 0.7541(2) 0.0184(13) Uani 1 1 d . . .
C38 C 0.6967(3) 0.1610(3) 0.7378(2) 0.0200(14) Uani 1 1 d . . .
C26 C 0.2701(2) 0.2263(4) 0.5860(2) 0.0195(14) Uani 1 1 d . . .
C3 C 0.1955(2) 0.3468(4) 0.7302(2) 0.0196(14) Uani 1 1 d . . .
C1 C 0.1172(3) 0.3113(3) 0.5703(3) 0.0200(14) Uani 1 1 d . . .
C46 C 0.6513(3) 0.2040(4) 0.7413(2) 0.0236(14) Uani 1 1 d . . .
C20 C 0.3314(3) 0.2479(3) 0.7381(2) 0.0197(14) Uani 1 1 d . . .
H20 H 0.3674 0.2321 0.7676 0.024 Uiso 1 1 calc R U .
C61 C 0.7837(3) 0.2531(4) 0.5956(2) 0.0279(16) Uani 1 1 d . . .
C16 C 0.3144(2) 0.2887(4) 0.8183(2) 0.0199(13) Uani 1 1 d . . .
C9 C 0.1133(3) 0.4335(4) 0.7505(2) 0.0253(15) Uani 1 1 d . . .
H9 H 0.0851 0.4631 0.7574 0.030 Uiso 1 1 calc R U .
C11 C 0.2023(3) 0.4266(4) 0.7341(2) 0.0191(14) Uani 1 1 d . . .
C10 C 0.1602(3) 0.4690(4) 0.7451(2) 0.0244(15) Uani 1 1 d . . .
H10 H 0.1642 0.5231 0.7488 0.029 Uiso 1 1 calc R U .
C12 C 0.2526(3) 0.4669(4) 0.7276(3) 0.0256(15) Uani 1 1 d . . .
H12 H 0.2859 0.4293 0.7369 0.031 Uiso 1 1 calc R U .
C34 C 0.2400(3) 0.1377(4) 0.5123(3) 0.0277(15) Uani 1 1 d . . .
H34 H 0.2281 0.0873 0.4985 0.033 Uiso 1 1 calc R U .
C21 C 0.3289(3) 0.2336(3) 0.6863(2) 0.0211(14) Uani 1 1 d . . .
C2 C 0.6263(3) 0.1861(4) 0.5766(3) 0.0267(15) Uani 1 1 d . . .
C5 C 0.1412(3) 0.2235(4) 0.7312(3) 0.0257(15) Uani 1 1 d . . .
H5 H 0.1773 0.2020 0.7289 0.031 Uiso 1 1 calc R U .
C55 C 0.8377(3) 0.2459(4) 0.7473(2) 0.0238(15) Uani 1 1 d . . .
H55 H 0.8738 0.2609 0.7771 0.029 Uiso 1 1 calc R U .
C47 C 0.6465(3) 0.2903(4) 0.7336(3) 0.0281(15) Uani 1 1 d . . .
H47 H 0.6844 0.3088 0.7331 0.034 Uiso 1 1 calc R U .
C33 C 0.2509(3) 0.1530(4) 0.5657(2) 0.0237(15) Uani 1 1 d . . .
C27 C 0.2744(2) 0.2853(4) 0.5517(2) 0.0238(15) Uani 1 1 d . . .
C4 C 0.1482(3) 0.3099(4) 0.7356(2) 0.0213(14) Uani 1 1 d . . .
C75 C 0.4113(3) 0.0116(4) 0.4503(3) 0.0375(18) Uani 1 1 d . . .
H75A H 0.4442 -0.0100 0.4832 0.045 Uiso 1 1 calc R U .
H75B H 0.3815 -0.0294 0.4331 0.045 Uiso 1 1 calc R U .
C56 C 0.8380(3) 0.2558(4) 0.6961(3) 0.0229(14) Uani 1 1 d . . .
C69 C 0.7678(3) 0.3244(4) 0.5711(2) 0.0302(17) Uani 1 1 d . . .
C8 C 0.1076(3) 0.3553(4) 0.7459(3) 0.0262(15) Uani 1 1 d . . .
H8 H 0.0752 0.3313 0.7497 0.031 Uiso 1 1 calc R U .
C31 C 0.2630(3) 0.2655(4) 0.4981(3) 0.0297(17) Uani 1 1 d . . .
H31 H 0.2672 0.3035 0.4748 0.036 Uiso 1 1 calc R U .
C35 C 0.2403(3) 0.0905(4) 0.5998(3) 0.0279(16) Uani 1 1 d . . .
H35 H 0.2570 0.1090 0.6385 0.033 Uiso 1 1 calc R U .
C22 C 0.3894(3) 0.2068(4) 0.6877(3) 0.0287(16) Uani 1 1 d . . .
C57 C 0.9005(3) 0.2791(4) 0.6997(3) 0.0266(15) Uani 1 1 d . . .
C40 C 0.7459(3) 0.0337(4) 0.7363(3) 0.0316(17) Uani 1 1 d . . .
H40 H 0.7809 0.0679 0.7442 0.038 Uiso 1 1 calc R U .
C39 C 0.6985(3) 0.0812(4) 0.7427(3) 0.0258(15) Uani 1 1 d . . .
C01O C -0.0777(3) 0.4983(4) 0.4349(3) 0.052(3) Uani 1 1 d . . .
H01A H -0.0493 0.5153 0.4718 0.062 Uiso 1 1 calc R U .
H01B H -0.1141 0.5298 0.4234 0.062 Uiso 1 1 calc R U .
C51 C 0.8159(3) 0.2144(4) 0.8265(3) 0.0265(15) Uani 1 1 d . . .
C30 C 0.2341(3) 0.4179(4) 0.5410(3) 0.0328(17) Uani 1 1 d . . .
H30A H 0.2236 0.4184 0.5017 0.049 Uiso 1 1 calc R U .
H30B H 0.2429 0.4702 0.5554 0.049 Uiso 1 1 calc R U .
H30C H 0.2006 0.3975 0.5471 0.049 Uiso 1 1 calc R U .
C14 C 0.2771(3) 0.5366(4) 0.7666(3) 0.0355(17) Uani 1 1 d . . .
H14A H 0.2475 0.5778 0.7550 0.053 Uiso 1 1 calc R U .
H14B H 0.3138 0.5549 0.7653 0.053 Uiso 1 1 calc R U .
H14C H 0.2856 0.5210 0.8041 0.053 Uiso 1 1 calc R U .
C32 C 0.2457(3) 0.1925(4) 0.4776(3) 0.0330(17) Uani 1 1 d . . .
H32 H 0.2379 0.1802 0.4409 0.040 Uiso 1 1 calc R U .
C76 C 0.3833(3) 0.0765(4) 0.4663(3) 0.0384(19) Uani 1 1 d . . .
H76A H 0.3491 0.0965 0.4337 0.046 Uiso 1 1 calc R U .
H76B H 0.3685 0.0589 0.4931 0.046 Uiso 1 1 calc R U .
C18 C 0.3245(3) 0.2075(4) 0.8415(3) 0.0369(18) Uani 1 1 d . . .
H18A H 0.3404 0.2098 0.8815 0.055 Uiso 1 1 calc R U .
H18B H 0.3530 0.1809 0.8312 0.055 Uiso 1 1 calc R U .
H18C H 0.2866 0.1796 0.8268 0.055 Uiso 1 1 calc R U .
C19 C 0.2765(3) 0.3299(4) 0.8419(3) 0.0322(17) Uani 1 1 d . . .
H19A H 0.2959 0.3265 0.8820 0.048 Uiso 1 1 calc R U .
H19B H 0.2372 0.3058 0.8281 0.048 Uiso 1 1 calc R U .
H19C H 0.2722 0.3839 0.8309 0.048 Uiso 1 1 calc R U .
C62 C 0.7905(3) 0.1891(4) 0.5666(3) 0.0342(18) Uani 1 1 d . . .
C13 C 0.2339(3) 0.4918(4) 0.6681(2) 0.0291(16) Uani 1 1 d . . .
H13A H 0.2210 0.4468 0.6442 0.044 Uiso 1 1 calc R U .
H13B H 0.2676 0.5160 0.6646 0.044 Uiso 1 1 calc R U .
H13C H 0.2009 0.5284 0.6575 0.044 Uiso 1 1 calc R U .
C7 C 0.1379(3) 0.1889(4) 0.7827(3) 0.0412(19) Uani 1 1 d . . .
H7A H 0.1732 0.2042 0.8154 0.062 Uiso 1 1 calc R U .
H7B H 0.1364 0.1328 0.7798 0.062 Uiso 1 1 calc R U .
H7C H 0.1021 0.2076 0.7854 0.062 Uiso 1 1 calc R U .
C01Z C -0.0504(3) 0.5097(4) 0.3954(3) 0.043(2) Uani 1 1 d . . .
H01C H -0.0789 0.4939 0.3582 0.051 Uiso 1 1 calc R U .
H01D H -0.0408 0.5645 0.3942 0.051 Uiso 1 1 calc R U .
C71 C 0.7543(3) 0.3927(4) 0.5986(3) 0.0339(18) Uani 1 1 d . . .
H71 H 0.7644 0.3774 0.6372 0.041 Uiso 1 1 calc R U .
C43 C 0.6538(3) 0.0457(4) 0.7524(3) 0.0366(18) Uani 1 1 d . . .
H43 H 0.6542 -0.0085 0.7556 0.044 Uiso 1 1 calc R U .
C6 C 0.0871(3) 0.1987(4) 0.6801(3) 0.0354(17) Uani 1 1 d . . .
H6A H 0.0507 0.2148 0.6829 0.053 Uiso 1 1 calc R U .
H6B H 0.0872 0.1428 0.6766 0.053 Uiso 1 1 calc R U .
H6C H 0.0886 0.2225 0.6478 0.053 Uiso 1 1 calc R U .
C45 C 0.6073(3) 0.1651(4) 0.7517(3) 0.0339(17) Uani 1 1 d . . .
H45 H 0.5761 0.1934 0.7548 0.041 Uiso 1 1 calc R U .
C17 C 0.3739(3) 0.3319(4) 0.8411(3) 0.0377(18) Uani 1 1 d . . .
H17A H 0.3681 0.3828 0.8244 0.057 Uiso 1 1 calc R U .
H17B H 0.4029 0.3032 0.8327 0.057 Uiso 1 1 calc R U .
H17C H 0.3887 0.3371 0.8809 0.057 Uiso 1 1 calc R U .
C025 C 0.0186(3) 0.1102(4) 0.4683(3) 0.042(2) Uani 1 1 d . . .
H02A H -0.0128 0.0814 0.4381 0.051 Uiso 1 1 calc R U .
H02B H 0.0379 0.0752 0.4998 0.051 Uiso 1 1 calc R U .
C37 C 0.1727(3) 0.0790(5) 0.5805(3) 0.048(2) Uani 1 1 d . . .
H37A H 0.1548 0.0618 0.5423 0.072 Uiso 1 1 calc R U .
H37B H 0.1545 0.1275 0.5835 0.072 Uiso 1 1 calc R U .
H37C H 0.1659 0.0402 0.6035 0.072 Uiso 1 1 calc R U .
C027 C 0.0642(3) 0.1406(5) 0.4497(3) 0.046(2) Uani 1 1 d . . .
H02C H 0.0932 0.1737 0.4786 0.055 Uiso 1 1 calc R U .
H02D H 0.0861 0.0975 0.4430 0.055 Uiso 1 1 calc R U .
C28 C 0.2886(3) 0.3674(4) 0.5703(3) 0.0296(16) Uani 1 1 d . . .
H28 H 0.2993 0.3694 0.6104 0.036 Uiso 1 1 calc R U .
C66 C 0.7848(3) 0.1994(6) 0.5139(3) 0.049(2) Uani 1 1 d . . .
H66 H 0.7905 0.1572 0.4945 0.059 Uiso 1 1 calc R U .
C68 C 0.7618(3) 0.3328(5) 0.5167(3) 0.045(2) Uani 1 1 d . . .
H68 H 0.7517 0.3812 0.4991 0.054 Uiso 1 1 calc R U .
C78 C 0.4553(3) 0.2520(5) 0.5380(3) 0.042(2) Uani 1 1 d . . .
H78A H 0.4457 0.2878 0.5615 0.051 Uiso 1 1 calc R U .
H78B H 0.4939 0.2272 0.5606 0.051 Uiso 1 1 calc R U .
C02C C -0.1203(4) 0.4092(5) 0.4715(3) 0.045(2) Uani 1 1 d . . .
H02E H -0.1611 0.3901 0.4496 0.054 Uiso 1 1 calc R U .
H02F H -0.1231 0.4579 0.4891 0.054 Uiso 1 1 calc R U .
C44 C 0.6092(3) 0.0864(5) 0.7576(3) 0.043(2) Uani 1 1 d . . .
H44 H 0.5799 0.0606 0.7651 0.052 Uiso 1 1 calc R U .
C02E C -0.0867(3) 0.3528(5) 0.5138(3) 0.047(2) Uani 1 1 d . . .
H02G H -0.0457 0.3719 0.5351 0.057 Uiso 1 1 calc R U .
H02H H -0.1056 0.3472 0.5393 0.057 Uiso 1 1 calc R U .
C60 C 0.9186(3) 0.3553(4) 0.7305(3) 0.0404(19) Uani 1 1 d . . .
H60A H 0.9581 0.3703 0.7341 0.061 Uiso 1 1 calc R U .
H60B H 0.9197 0.3495 0.7670 0.061 Uiso 1 1 calc R U .
H60C H 0.8896 0.3949 0.7102 0.061 Uiso 1 1 calc R U .
C02G C 0.1021(3) 0.2840(4) 0.4004(3) 0.0414(19) Uani 1 1 d . . .
H02I H 0.1224 0.2826 0.4409 0.050 Uiso 1 1 calc R U .
H02J H 0.1322 0.2952 0.3865 0.050 Uiso 1 1 calc R U .
C67 C 0.7708(3) 0.2704(6) 0.4892(3) 0.052(2) Uani 1 1 d . . .
H67 H 0.7673 0.2766 0.4530 0.062 Uiso 1 1 calc R U .
C58 C 0.9078(3) 0.2875(5) 0.6468(3) 0.0405(19) Uani 1 1 d . . .
H58A H 0.8965 0.2395 0.6261 0.061 Uiso 1 1 calc R U .
H58B H 0.9494 0.2995 0.6554 0.061 Uiso 1 1 calc R U .
H58C H 0.8822 0.3291 0.6248 0.061 Uiso 1 1 calc R U .
C74 C 0.4596(3) -0.0244(4) 0.3967(3) 0.0366(18) Uani 1 1 d . . .
H74A H 0.4285 -0.0616 0.3748 0.044 Uiso 1 1 calc R U .
H74B H 0.4891 -0.0511 0.4293 0.044 Uiso 1 1 calc R U .
C02K C -0.0545(3) 0.2273(5) 0.5335(3) 0.045(2) Uani 1 1 d . . .
H02K H -0.0788 0.2148 0.5534 0.054 Uiso 1 1 calc R U .
H02L H -0.0159 0.2483 0.5600 0.054 Uiso 1 1 calc R U .
C59 C 0.9459(3) 0.2161(5) 0.7335(3) 0.051(2) Uani 1 1 d . . .
H59A H 0.9327 0.1662 0.7158 0.076 Uiso 1 1 calc R U .
H59B H 0.9482 0.2143 0.7706 0.076 Uiso 1 1 calc R U .
H59C H 0.9852 0.2281 0.7353 0.076 Uiso 1 1 calc R U .
C41 C 0.7241(4) 0.0057(4) 0.6769(3) 0.045(2) Uani 1 1 d . . .
H41A H 0.6877 -0.0246 0.6668 0.067 Uiso 1 1 calc R U .
H41B H 0.7549 -0.0261 0.6736 0.067 Uiso 1 1 calc R U .
H41C H 0.7158 0.0500 0.6524 0.067 Uiso 1 1 calc R U .
C02N C 0.0821(4) 0.4160(4) 0.3962(4) 0.050(2) Uani 1 1 d . . .
H02M H 0.1071 0.4271 0.3767 0.060 Uiso 1 1 calc R U .
H02N H 0.1073 0.4204 0.4360 0.060 Uiso 1 1 calc R U .
C02O C 0.0740(3) 0.2086(5) 0.3793(3) 0.044(2) Uani 1 1 d . . .
H02O H 0.0519 0.2118 0.3390 0.052 Uiso 1 1 calc R U .
H02P H 0.1058 0.1698 0.3876 0.052 Uiso 1 1 calc R U .
C02P C -0.0443(4) 0.1548(5) 0.5062(3) 0.049(2) Uani 1 1 d . . .
H02Q H -0.0269 0.1137 0.5337 0.059 Uiso 1 1 calc R U .
H02R H -0.0826 0.1363 0.4776 0.059 Uiso 1 1 calc R U .
C49 C 0.6389(4) 0.3318(5) 0.7794(3) 0.051(2) Uani 1 1 d . . .
H49A H 0.6024 0.3142 0.7813 0.077 Uiso 1 1 calc R U .
H49B H 0.6363 0.3871 0.7724 0.077 Uiso 1 1 calc R U .
H49C H 0.6731 0.3211 0.8142 0.077 Uiso 1 1 calc R U .
C29 C 0.3410(3) 0.3999(5) 0.5614(4) 0.054(2) Uani 1 1 d . . .
H29A H 0.3770 0.3704 0.5831 0.081 Uiso 1 1 calc R U .
H29B H 0.3472 0.4537 0.5729 0.081 Uiso 1 1 calc R U .
H29C H 0.3324 0.3963 0.5225 0.081 Uiso 1 1 calc R U .
C48 C 0.5953(4) 0.3118(4) 0.6785(3) 0.049(2) Uani 1 1 d . . .
H48A H 0.5999 0.2842 0.6489 0.074 Uiso 1 1 calc R U .
H48B H 0.5962 0.3671 0.6725 0.074 Uiso 1 1 calc R U .
H48C H 0.5573 0.2979 0.6788 0.074 Uiso 1 1 calc R U .
C73 C 0.4893(3) 0.0065(4) 0.3635(3) 0.0412(19) Uani 1 1 d . . .
H73A H 0.5060 -0.0362 0.3503 0.049 Uiso 1 1 calc R U .
H73B H 0.4598 0.0339 0.3312 0.049 Uiso 1 1 calc R U .
C72 C 0.6877(3) 0.4121(5) 0.5718(4) 0.056(2) Uani 1 1 d . . .
H72A H 0.6760 0.4275 0.5337 0.084 Uiso 1 1 calc R U .
H72B H 0.6799 0.4543 0.5918 0.084 Uiso 1 1 calc R U .
H72C H 0.6647 0.3670 0.5728 0.084 Uiso 1 1 calc R U .
C64 C 0.7459(4) 0.0587(5) 0.5570(3) 0.053(2) Uani 1 1 d . . .
H64A H 0.7097 0.0855 0.5533 0.080 Uiso 1 1 calc R U .
H64B H 0.7492 0.0101 0.5763 0.080 Uiso 1 1 calc R U .
H64C H 0.7440 0.0486 0.5206 0.080 Uiso 1 1 calc R U .
C63 C 0.8006(3) 0.1089(5) 0.5899(3) 0.046(2) Uani 1 1 d . . .
H63 H 0.8054 0.1118 0.6285 0.055 Uiso 1 1 calc R U .
C02X C 0.0322(4) 0.4721(5) 0.3793(3) 0.050(2) Uani 1 1 d . . .
H02S H 0.0480 0.5249 0.3822 0.060 Uiso 1 1 calc R U .
H02T H 0.0041 0.4629 0.3407 0.060 Uiso 1 1 calc R U .
C65 C 0.8568(4) 0.0716(5) 0.5902(4) 0.064(3) Uani 1 1 d . . .
H65A H 0.8549 0.0732 0.5532 0.096 Uiso 1 1 calc R U .
H65B H 0.8593 0.0182 0.6022 0.096 Uiso 1 1 calc R U .
H65C H 0.8921 0.0996 0.6153 0.096 Uiso 1 1 calc R U .
C42 C 0.7676(4) -0.0337(4) 0.7765(3) 0.051(2) Uani 1 1 d . . .
H42A H 0.7750 -0.0161 0.8132 0.077 Uiso 1 1 calc R U .
H42B H 0.8045 -0.0543 0.7769 0.077 Uiso 1 1 calc R U .
H42C H 0.7371 -0.0739 0.7649 0.077 Uiso 1 1 calc R U .
C70 C 0.7902(4) 0.4640(4) 0.6011(3) 0.050(2) Uani 1 1 d . . .
H70A H 0.8326 0.4532 0.6227 0.075 Uiso 1 1 calc R U .
H70B H 0.7780 0.5056 0.6184 0.075 Uiso 1 1 calc R U .
H70C H 0.7834 0.4791 0.5640 0.075 Uiso 1 1 calc R U .
C77 C 0.4082(3) 0.1934(5) 0.5149(4) 0.057(3) Uani 1 1 d . . .
H77A H 0.3995 0.1712 0.5445 0.069 Uiso 1 1 calc R U .
H77B H 0.3713 0.2174 0.4877 0.069 Uiso 1 1 calc R U .
C84 C 0.5699(4) 0.0814(5) 0.3677(4) 0.064(3) Uani 1 1 d . . .
H84A H 0.5432 0.0976 0.3300 0.076 Uiso 1 1 calc R U .
H84B H 0.5945 0.0382 0.3653 0.076 Uiso 1 1 calc R U .
C83 C 0.6085(4) 0.1455(6) 0.3972(4) 0.071(3) Uani 1 1 d . . .
H83A H 0.6303 0.1326 0.4365 0.086 Uiso 1 1 calc R U .
H83B H 0.6380 0.1556 0.3823 0.086 Uiso 1 1 calc R U .
C36 C 0.2713(5) 0.0154(4) 0.5993(4) 0.066(3) Uani 1 1 d . . .
H36A H 0.2515 -0.0084 0.5630 0.099 Uiso 1 1 calc R U .
H36B H 0.2693 -0.0193 0.6270 0.099 Uiso 1 1 calc R U .
H36C H 0.3130 0.0256 0.6074 0.099 Uiso 1 1 calc R U .
C79 C 0.5036(7) 0.3517(5) 0.5112(4) 0.099(5) Uani 1 1 d . . .
H79A H 0.4884 0.3955 0.5248 0.119 Uiso 1 1 calc R U .
H79B H 0.5393 0.3319 0.5424 0.119 Uiso 1 1 calc R U .
C80 C 0.5213(5) 0.3794(6) 0.4714(6) 0.098(5) Uani 1 1 d . . .
H80A H 0.4872 0.4052 0.4419 0.118 Uiso 1 1 calc R U .
H80B H 0.5535 0.4176 0.4883 0.118 Uiso 1 1 calc R U .
C23A C 0.3947(4) 0.1935(6) 0.6344(4) 0.008(2) Uiso 0.5 1 d . . P
C81 C 0.5776(4) 0.3338(6) 0.4233(6) 0.092(4) Uani 1 1 d . . .
H81A H 0.5525 0.3549 0.3865 0.111 Uiso 1 1 calc R U .
H81B H 0.6065 0.3741 0.4438 0.111 Uiso 1 1 calc R U .
C52A C 0.8314(5) 0.2952(6) 0.8493(4) 0.014(2) Uiso 0.5 1 d . . P
C24A C 0.4135(5) 0.1350(7) 0.7245(5) 0.014(2) Uiso 0.5 1 d . . P
C25A C 0.4354(4) 0.2779(6) 0.7166(4) 0.012(2) Uiso 0.5 1 d . . P
C53A C 0.8735(5) 0.1602(7) 0.8499(5) 0.016(3) Uiso 0.5 1 d . . P
C82 C 0.6091(6) 0.2736(7) 0.4164(6) 0.110(5) Uani 1 1 d . . .
H82A H 0.6399 0.2577 0.4526 0.131 Uiso 1 1 calc R U .
H82B H 0.6297 0.2907 0.3940 0.131 Uiso 1 1 calc R U .
C54A C 0.7744(5) 0.1780(6) 0.8493(4) 0.014(2) Uiso 0.5 1 d . . P
C85 C 0.9803(7) 0.0090(10) 0.3303(7) 0.182(8) Uiso 1 1 d D . .
H85A H 1.0177 -0.0192 0.3412 0.273 Uiso 1 1 calc R U .
H85B H 0.9548 -0.0177 0.3442 0.273 Uiso 1 1 calc R U .
H85C H 0.9886 0.0609 0.3456 0.273 Uiso 1 1 calc R U .
C87 C 1.0036(5) 0.0048(8) 0.2561(4) 0.170(7) Uiso 1 1 d D . .
H87A H 1.0254 -0.0434 0.2711 0.204 Uiso 1 1 calc R U .
H87B H 1.0311 0.0490 0.2697 0.204 Uiso 1 1 calc R U .
C86 C 0.9486(8) 0.0136(14) 0.2679(7) 0.278(13) Uiso 1 1 d D . .
H86A H 0.9284 0.0634 0.2551 0.333 Uiso 1 1 calc R U .
H86B H 0.9198 -0.0288 0.2519 0.333 Uiso 1 1 calc R U .
C88 C 0.9703(8) 0.0035(11) 0.1930(6) 0.207(9) Uiso 1 1 d D . .
H88A H 0.9484 0.0518 0.1781 0.249 Uiso 1 1 calc R U .
H88B H 0.9427 -0.0406 0.1796 0.249 Uiso 1 1 calc R U .
C89 C 1.0253(8) -0.0054(12) 0.1804(7) 0.216(9) Uiso 1 1 d D . .
H89A H 1.0569 0.0293 0.2039 0.323 Uiso 1 1 calc R U .
H89B H 1.0142 0.0074 0.1419 0.323 Uiso 1 1 calc R U .
H89C H 1.0396 -0.0584 0.1873 0.323 Uiso 1 1 calc R U .
C23B C 0.3771(9) 0.1197(12) 0.6548(8) 0.074(6) Uiso 0.5 1 d . . P
C24B C 0.4327(9) 0.1772(12) 0.7405(8) 0.063(5) Uiso 0.5 1 d . . P
C25B C 0.4083(10) 0.2506(13) 0.6525(9) 0.081(6) Uiso 0.5 1 d . . P
C52B C 0.8756(10) 0.2587(13) 0.8624(9) 0.085(7) Uiso 0.5 1 d . . P
C53B C 0.8222(11) 0.1343(14) 0.8520(10) 0.093(7) Uiso 0.5 1 d . . P
C54B C 0.7724(10) 0.2578(14) 0.8458(9) 0.092(7) Uiso 0.5 1 d . . P
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'
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'
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_3
N2 Ni1 O1 164.78(19) .
N2 Ni1 N1 97.9(2) .
O1 Ni1 N1 96.55(19) .
N2 Ni1 O2 96.48(19) .
O1 Ni1 O2 69.35(17) .
N1 Ni1 O2 165.29(19) .
N4 Ni2 O4 164.5(2) .
N4 Ni2 N3 98.9(2) .
O4 Ni2 N3 96.2(2) .
N4 Ni2 O5 95.5(2) .
O4 Ni2 O5 69.45(18) .
N3 Ni2 O5 165.36(19) .
O3 K1 O8 75.62(16) .
O3 K1 O10 101.62(16) .
O8 K1 O10 122.26(17) .
O3 K1 O12 95.47(15) .
O8 K1 O12 118.01(17) .
O10 K1 O12 119.65(17) .
O3 K1 O11 90.93(16) .
O8 K1 O11 166.52(16) .
O10 K1 O11 60.74(17) .
O12 K1 O11 61.57(17) .
O3 K1 O9 84.00(15) .
O8 K1 O9 60.59(16) .
O10 K1 O9 61.77(16) .
O12 K1 O9 178.58(17) .
O11 K1 O9 119.72(17) .
O3 K1 O7 98.51(15) .
O8 K1 O7 59.71(16) .
O10 K1 O7 159.53(16) .
O12 K1 O7 61.49(16) .
O11 K1 O7 122.88(16) .
O9 K1 O7 117.26(16) .
O6 K2 O17 84.11(15) .
O6 K2 O13 79.59(18) .
O17 K2 O13 121.2(2) .
O6 K2 O15 101.32(16) .
O17 K2 O15 116.66(17) .
O13 K2 O15 121.9(2) .
O6 K2 O16 112.99(15) .
O17 K2 O16 59.84(15) .
O13 K2 O16 167.08(18) .
O15 K2 O16 60.34(15) .
O6 K2 O14 96.26(17) .
O17 K2 O14 177.99(18) .
O13 K2 O14 60.8(2) .
O15 K2 O14 61.33(18) .
O16 K2 O14 118.27(17) .
O6 K2 O18 77.62(16) .
O17 K2 O18 61.57(17) .
O13 K2 O18 59.8(2) .
O15 K2 O18 177.94(18) .
O16 K2 O18 118.36(18) .
O14 K2 O18 120.44(19) .
O6 K2 C52B 146.1(4) 4_565
O17 K2 C52B 77.1(4) 4_565
O13 K2 C52B 86.3(5) 4_565
O15 K2 C52B 112.3(4) 4_565
O16 K2 C52B 81.4(4) 4_565
O14 K2 C52B 103.5(5) 4_565
O18 K2 C52B 68.6(4) 4_565
C1 O1 Ni1 90.4(3) .
C2 O4 Ni2 90.0(4) .
C15 N1 C3 123.3(5) .
C15 N1 Ni1 124.8(4) .
C3 N1 Ni1 111.7(3) .
C1 O2 Ni1 89.5(3) .
C2 O5 Ni2 90.1(4) .
C75 O16 C74 110.3(5) .
C75 O16 K2 115.6(4) .
C74 O16 K2 116.5(4) .
C50 N3 C38 122.9(5) .
C50 N3 Ni2 124.5(4) .
C38 N3 Ni2 112.4(4) .
C1 O3 K1 155.1(4) .
C21 N2 C26 124.3(5) .
C21 N2 Ni1 124.4(4) .
C26 N2 Ni1 111.2(3) .
C2 O6 K2 159.1(5) .
C027 O7 C02O 111.8(6) .
C027 O7 K1 103.2(4) .
C02O O7 K1 110.4(4) .
C02G O12 C02N 113.9(6) .
C02G O12 K1 106.3(4) .
C02N O12 K1 109.2(5) .
C56 N4 C61 124.3(5) .
C56 N4 Ni2 123.8(4) .
C61 N4 Ni2 111.9(4) .
C02E O9 C02K 111.4(6) .
C02E O9 K1 101.4(5) .
C02K O9 K1 108.5(4) .
C02P O8 C025 115.4(6) .
C02P O8 K1 119.5(5) .
C025 O8 K1 121.3(4) .
C77 O17 C76 113.5(5) .
C77 O17 K2 117.8(4) .
C76 O17 K2 119.7(4) .
C73 O15 C84 112.1(7) .
C73 O15 K2 113.8(4) .
C84 O15 K2 114.6(5) .
C02X O11 C01Z 113.7(6) .
C02X O11 K1 114.1(5) .
C01Z O11 K1 113.2(4) .
C01O O10 C02C 112.9(7) .
C01O O10 K1 118.6(5) .
C02C O10 K1 116.5(4) .
C78 O18 C79 113.6(6) .
C78 O18 K2 101.7(4) .
C79 O18 K2 107.6(6) .
C82 O14 C83 110.4(9) .
C82 O14 K2 110.4(6) .
C83 O14 K2 105.8(5) .
C80 O13 C81 122.5(8) .
C80 O13 K2 121.6(6) .
C81 O13 K2 115.3(6) .
N3 C50 C55 119.8(5) .
N3 C50 C51 126.3(5) .
C55 C50 C51 113.9(5) .
N1 C15 C20 120.6(5) .
N1 C15 C16 126.4(5) .
C20 C15 C16 113.0(5) .
C46 C38 C39 121.7(6) .
C46 C38 N3 119.6(5) .
C39 C38 N3 118.6(5) .
C33 C26 C27 121.1(6) .
C33 C26 N2 119.3(5) .
C27 C26 N2 119.0(6) .
C11 C3 C4 121.8(6) .
C11 C3 N1 118.3(5) .
C4 C3 N1 119.8(5) .
O3 C1 O2 124.3(6) .
O3 C1 O1 125.0(6) .
O2 C1 O1 110.8(5) .
C38 C46 C45 118.3(6) .
C38 C46 C47 122.9(5) .
C45 C46 C47 118.7(6) .
C15 C20 C21 131.3(5) .
C15 C20 H20 114.3 .
C21 C20 H20 114.3 .
C69 C61 C62 121.4(6) .
C69 C61 N4 118.5(6) .
C62 C61 N4 119.9(6) .
C19 C16 C18 106.7(5) .
C19 C16 C17 105.1(5) .
C18 C16 C17 109.2(5) .
C19 C16 C15 119.1(5) .
C18 C16 C15 107.2(5) .
C17 C16 C15 109.2(5) .
C8 C9 C10 119.7(6) .
C8 C9 H9 120.1 .
C10 C9 H9 120.1 .
C3 C11 C10 117.5(6) .
C3 C11 C12 122.1(5) .
C10 C11 C12 120.4(6) .
C9 C10 C11 121.4(6) .
C9 C10 H10 119.3 .
C11 C10 H10 119.3 .
C11 C12 C13 111.0(5) .
C11 C12 C14 112.9(5) .
C13 C12 C14 110.3(5) .
C11 C12 H12 107.5 .
C13 C12 H12 107.5 .
C14 C12 H12 107.5 .
C33 C34 C32 122.9(7) .
C33 C34 H34 118.5 .
C32 C34 H34 118.5 .
N2 C21 C20 120.5(5) .
N2 C21 C22 126.0(5) .
C20 C21 C22 113.5(5) .
O6 C2 O5 125.0(6) .
O6 C2 O4 124.5(6) .
O5 C2 O4 110.5(5) .
C4 C5 C6 112.4(5) .
C4 C5 C7 111.5(6) .
C6 C5 C7 109.9(5) .
C4 C5 H5 107.6 .
C6 C5 H5 107.6 .
C7 C5 H5 107.6 .
C56 C55 C50 132.3(6) .
C56 C55 H55 113.8 .
C50 C55 H55 113.8 .
C49 C47 C46 113.1(6) .
C49 C47 C48 109.6(6) .
C46 C47 C48 111.0(6) .
C49 C47 H47 107.6 .
C46 C47 H47 107.6 .
C48 C47 H47 107.6 .
C34 C33 C26 118.1(6) .
C34 C33 C35 119.3(6) .
C26 C33 C35 122.6(6) .
C31 C27 C26 117.3(6) .
C31 C27 C28 119.7(6) .
C26 C27 C28 122.9(6) .
C8 C4 C3 118.0(6) .
C8 C4 C5 120.6(6) .
C3 C4 C5 121.4(5) .
O16 C75 C76 109.3(6) .
O16 C75 H75A 109.8 .
C76 C75 H75A 109.8 .
O16 C75 H75B 109.8 .
C76 C75 H75B 109.8 .
H75A C75 H75B 108.3 .
N4 C56 C55 120.3(5) .
N4 C56 C57 126.5(6) .
C55 C56 C57 113.1(5) .
C61 C69 C68 118.0(7) .
C61 C69 C71 123.3(6) .
C68 C69 C71 118.6(7) .
C9 C8 C4 121.6(6) .
C9 C8 H8 119.2 .
C4 C8 H8 119.2 .
C32 C31 C27 122.3(6) .
C32 C31 H31 118.8 .
C27 C31 H31 118.8 .
C33 C35 C36 113.1(6) .
C33 C35 C37 109.5(5) .
C36 C35 C37 111.5(7) .
C33 C35 H35 107.5 .
C36 C35 H35 107.5 .
C37 C35 H35 107.5 .
C25B C22 C24B 121.2(12) .
C25B C22 C23A 43.3(9) .
C24B C22 C23A 123.0(10) .
C25B C22 C24A 134.7(11) .
C24B C22 C24A 33.9(8) .
C23A C22 C24A 108.6(7) .
C25B C22 C21 113.9(10) .
C24B C22 C21 115.4(9) .
C23A C22 C21 119.7(6) .
C24A C22 C21 111.3(6) .
C25B C22 C25A 63.7(10) .
C24B C22 C25A 74.4(9) .
C23A C22 C25A 103.9(7) .
C24A C22 C25A 107.8(7) .
C21 C22 C25A 104.7(6) .
C25B C22 C23B 99.4(12) .
C24B C22 C23B 95.0(11) .
C23A C22 C23B 56.2(8) .
C24A C22 C23B 63.4(8) .
C21 C22 C23B 107.2(8) .
C25A C22 C23B 147.9(9) .
C58 C57 C60 107.6(6) .
C58 C57 C59 105.8(6) .
C60 C57 C59 108.9(6) .
C58 C57 C56 118.5(5) .
C60 C57 C56 108.1(5) .
C59 C57 C56 107.6(5) .
C39 C40 C42 113.4(6) .
C39 C40 C41 110.4(6) .
C42 C40 C41 110.8(6) .
C39 C40 H40 107.3 .
C42 C40 H40 107.3 .
C41 C40 H40 107.3 .
C43 C39 C38 117.7(6) .
C43 C39 C40 120.1(6) .
C38 C39 C40 122.1(6) .
O10 C01O C01Z 110.7(8) .
O10 C01O H01A 109.5 .
C01Z C01O H01A 109.5 .
O10 C01O H01B 109.5 .
C01Z C01O H01B 109.5 .
H01A C01O H01B 108.1 .
C52A C51 C53B 134.6(11) .
C52A C51 C54A 108.4(7) .
C53B C51 C54A 53.5(10) .
C52A C51 C50 108.2(6) .
C53B C51 C50 116.9(10) .
C54A C51 C50 118.9(6) .
C52A C51 C52B 44.8(9) .
C53B C51 C52B 106.3(13) .
C54A C51 C52B 124.5(10) .
C50 C51 C52B 116.1(10) .
C52A C51 C54B 60.7(10) .
C53B C51 C54B 104.0(13) .
C54A C51 C54B 53.0(10) .
C50 C51 C54B 112.5(9) .
C52B C51 C54B 99.0(13) .
C52A C51 C53A 111.0(7) .
C53B C51 C53A 52.0(10) .
C54A C51 C53A 103.7(7) .
C50 C51 C53A 106.5(6) .
C52B C51 C53A 66.5(9) .
C54B C51 C53A 140.8(10) .
C28 C30 H30A 109.5 .
C28 C30 H30B 109.5 .
H30A C30 H30B 109.5 .
C28 C30 H30C 109.5 .
H30A C30 H30C 109.5 .
H30B C30 H30C 109.5 .
C12 C14 H14A 109.5 .
C12 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C12 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
C31 C32 C34 118.0(6) .
C31 C32 H32 121.0 .
C34 C32 H32 121.0 .
O17 C76 C75 108.8(6) .
O17 C76 H76A 109.9 .
C75 C76 H76A 109.9 .
O17 C76 H76B 109.9 .
C75 C76 H76B 109.9 .
H76A C76 H76B 108.3 .
C16 C18 H18A 109.5 .
C16 C18 H18B 109.5 .
H18A C18 H18B 109.5 .
C16 C18 H18C 109.5 .
H18A C18 H18C 109.5 .
H18B C18 H18C 109.5 .
C16 C19 H19A 109.5 .
C16 C19 H19B 109.5 .
H19A C19 H19B 109.5 .
C16 C19 H19C 109.5 .
H19A C19 H19C 109.5 .
H19B C19 H19C 109.5 .
C66 C62 C61 118.9(8) .
C66 C62 C63 118.5(7) .
C61 C62 C63 122.6(6) .
C12 C13 H13A 109.5 .
C12 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
C12 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
C5 C7 H7A 109.5 .
C5 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
C5 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
O11 C01Z C01O 109.1(6) .
O11 C01Z H01C 109.9 .
C01O C01Z H01C 109.9 .
O11 C01Z H01D 109.9 .
C01O C01Z H01D 109.9 .
H01C C01Z H01D 108.3 .
C69 C71 C70 114.7(6) .
C69 C71 C72 111.3(6) .
C70 C71 C72 109.7(6) .
C69 C71 H71 106.9 .
C70 C71 H71 106.9 .
C72 C71 H71 106.9 .
C44 C43 C39 122.2(7) .
C44 C43 H43 118.9 .
C39 C43 H43 118.9 .
C5 C6 H6A 109.5 .
C5 C6 H6B 109.5 .
H6A C6 H6B 109.5 .
C5 C6 H6C 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
C44 C45 C46 120.5(7) .
C44 C45 H45 119.8 .
C46 C45 H45 119.8 .
C16 C17 H17A 109.5 .
C16 C17 H17B 109.5 .
H17A C17 H17B 109.5 .
C16 C17 H17C 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
O8 C025 C027 107.8(6) .
O8 C025 H02A 110.1 .
C027 C025 H02A 110.1 .
O8 C025 H02B 110.1 .
C027 C025 H02B 110.1 .
H02A C025 H02B 108.5 .
C35 C37 H37A 109.5 .
C35 C37 H37B 109.5 .
H37A C37 H37B 109.5 .
C35 C37 H37C 109.5 .
H37A C37 H37C 109.5 .
H37B C37 H37C 109.5 .
O7 C027 C025 108.8(6) .
O7 C027 H02C 109.9 .
C025 C027 H02C 109.9 .
O7 C027 H02D 109.9 .
C025 C027 H02D 109.9 .
H02C C027 H02D 108.3 .
C27 C28 C30 110.2(5) .
C27 C28 C29 113.2(6) .
C30 C28 C29 109.4(6) .
C27 C28 H28 108.0 .
C30 C28 H28 108.0 .
C29 C28 H28 108.0 .
C62 C66 C67 120.8(8) .
C62 C66 H66 119.6 .
C67 C66 H66 119.6 .
C67 C68 C69 120.2(8) .
C67 C68 H68 119.9 .
C69 C68 H68 119.9 .
O18 C78 C77 108.4(7) .
O18 C78 H78A 110.0 .
C77 C78 H78A 110.0 .
O18 C78 H78B 110.0 .
C77 C78 H78B 110.0 .
H78A C78 H78B 108.4 .
O10 C02C C02E 110.2(7) .
O10 C02C H02E 109.6 .
C02E C02C H02E 109.6 .
O10 C02C H02F 109.6 .
C02E C02C H02F 109.6 .
H02E C02C H02F 108.1 .
C43 C44 C45 119.5(7) .
C43 C44 H44 120.2 .
C45 C44 H44 120.2 .
O9 C02E C02C 112.6(6) .
O9 C02E H02G 109.1 .
C02C C02E H02G 109.1 .
O9 C02E H02H 109.1 .
C02C C02E H02H 109.1 .
H02G C02E H02H 107.8 .
C57 C60 H60A 109.5 .
C57 C60 H60B 109.5 .
H60A C60 H60B 109.5 .
C57 C60 H60C 109.5 .
H60A C60 H60C 109.5 .
H60B C60 H60C 109.5 .
O12 C02G C02O 110.0(6) .
O12 C02G H02I 109.7 .
C02O C02G H02I 109.7 .
O12 C02G H02J 109.7 .
C02O C02G H02J 109.7 .
H02I C02G H02J 108.2 .
C66 C67 C68 120.6(8) .
C66 C67 H67 119.7 .
C68 C67 H67 119.7 .
C57 C58 H58A 109.5 .
C57 C58 H58B 109.5 .
H58A C58 H58B 109.5 .
C57 C58 H58C 109.5 .
H58A C58 H58C 109.5 .
H58B C58 H58C 109.5 .
O16 C74 C73 109.1(6) .
O16 C74 H74A 109.9 .
C73 C74 H74A 109.9 .
O16 C74 H74B 109.9 .
C73 C74 H74B 109.9 .
H74A C74 H74B 108.3 .
O9 C02K C02P 107.8(6) .
O9 C02K H02K 110.1 .
C02P C02K H02K 110.1 .
O9 C02K H02L 110.1 .
C02P C02K H02L 110.1 .
H02K C02K H02L 108.5 .
C57 C59 H59A 109.5 .
C57 C59 H59B 109.5 .
H59A C59 H59B 109.5 .
C57 C59 H59C 109.5 .
H59A C59 H59C 109.5 .
H59B C59 H59C 109.5 .
C40 C41 H41A 109.5 .
C40 C41 H41B 109.5 .
H41A C41 H41B 109.5 .
C40 C41 H41C 109.5 .
H41A C41 H41C 109.5 .
H41B C41 H41C 109.5 .
O12 C02N C02X 109.3(6) .
O12 C02N H02M 109.8 .
C02X C02N H02M 109.8 .
O12 C02N H02N 109.8 .
C02X C02N H02N 109.8 .
H02M C02N H02N 108.3 .
O7 C02O C02G 114.3(6) .
O7 C02O H02O 108.7 .
C02G C02O H02O 108.7 .
O7 C02O H02P 108.7 .
C02G C02O H02P 108.7 .
H02O C02O H02P 107.6 .
O8 C02P C02K 108.5(7) .
O8 C02P H02Q 110.0 .
C02K C02P H02Q 110.0 .
O8 C02P H02R 110.0 .
C02K C02P H02R 110.0 .
H02Q C02P H02R 108.4 .
C47 C49 H49A 109.5 .
C47 C49 H49B 109.5 .
H49A C49 H49B 109.5 .
C47 C49 H49C 109.5 .
H49A C49 H49C 109.5 .
H49B C49 H49C 109.5 .
C28 C29 H29A 109.5 .
C28 C29 H29B 109.5 .
H29A C29 H29B 109.5 .
C28 C29 H29C 109.5 .
H29A C29 H29C 109.5 .
H29B C29 H29C 109.5 .
C47 C48 H48A 109.5 .
C47 C48 H48B 109.5 .
H48A C48 H48B 109.5 .
C47 C48 H48C 109.5 .
H48A C48 H48C 109.5 .
H48B C48 H48C 109.5 .
O15 C73 C74 109.8(7) .
O15 C73 H73A 109.7 .
C74 C73 H73A 109.7 .
O15 C73 H73B 109.7 .
C74 C73 H73B 109.7 .
H73A C73 H73B 108.2 .
C71 C72 H72A 109.5 .
C71 C72 H72B 109.5 .
H72A C72 H72B 109.5 .
C71 C72 H72C 109.5 .
H72A C72 H72C 109.5 .
H72B C72 H72C 109.5 .
C63 C64 H64A 109.5 .
C63 C64 H64B 109.5 .
H64A C64 H64B 109.5 .
C63 C64 H64C 109.5 .
H64A C64 H64C 109.5 .
H64B C64 H64C 109.5 .
C62 C63 C65 112.6(7) .
C62 C63 C64 109.7(7) .
C65 C63 C64 109.7(6) .
C62 C63 H63 108.2 .
C65 C63 H63 108.2 .
C64 C63 H63 108.2 .
O11 C02X C02N 109.8(7) .
O11 C02X H02S 109.7 .
C02N C02X H02S 109.7 .
O11 C02X H02T 109.7 .
C02N C02X H02T 109.7 .
H02S C02X H02T 108.2 .
C63 C65 H65A 109.5 .
C63 C65 H65B 109.5 .
H65A C65 H65B 109.5 .
C63 C65 H65C 109.5 .
H65A C65 H65C 109.5 .
H65B C65 H65C 109.5 .
C40 C42 H42A 109.5 .
C40 C42 H42B 109.5 .
H42A C42 H42B 109.5 .
C40 C42 H42C 109.5 .
H42A C42 H42C 109.5 .
H42B C42 H42C 109.5 .
C71 C70 H70A 109.5 .
C71 C70 H70B 109.5 .
H70A C70 H70B 109.5 .
C71 C70 H70C 109.5 .
H70A C70 H70C 109.5 .
H70B C70 H70C 109.5 .
O17 C77 C78 110.0(6) .
O17 C77 H77A 109.7 .
C78 C77 H77A 109.7 .
O17 C77 H77B 109.7 .
C78 C77 H77B 109.7 .
H77A C77 H77B 108.2 .
O15 C84 C83 110.0(8) .
O15 C84 H84A 109.7 .
C83 C84 H84A 109.7 .
O15 C84 H84B 109.7 .
C83 C84 H84B 109.7 .
H84A C84 H84B 108.2 .
O14 C83 C84 108.8(7) .
O14 C83 H83A 109.9 .
C84 C83 H83A 109.9 .
O14 C83 H83B 109.9 .
C84 C83 H83B 109.9 .
H83A C83 H83B 108.3 .
C35 C36 H36A 109.5 .
C35 C36 H36B 109.5 .
H36A C36 H36B 109.5 .
C35 C36 H36C 109.5 .
H36A C36 H36C 109.5 .
H36B C36 H36C 109.5 .
C80 C79 O18 116.3(9) .
C80 C79 H79A 108.2 .
O18 C79 H79A 108.2 .
C80 C79 H79B 108.2 .
O18 C79 H79B 108.2 .
H79A C79 H79B 107.4 .
O13 C80 C79 111.2(10) .
O13 C80 H80A 109.4 .
C79 C80 H80A 109.4 .
O13 C80 H80B 109.4 .
C79 C80 H80B 109.4 .
H80A C80 H80B 108.0 .
C25B C23A C22 64.9(13) .
C25B C23A C23B 133.0(17) .
C22 C23A C23B 68.5(9) .
C82 C81 O13 119.1(10) .
C82 C81 H81A 107.5 .
O13 C81 H81A 107.5 .
C82 C81 H81B 107.5 .
O13 C81 H81B 107.5 .
H81A C81 H81B 107.0 .
C52B C52A C51 70.4(13) .
C52B C52A C54B 121.1(17) .
C51 C52A C54B 61.5(10) .
C24B C24A C22 67.7(15) .
C24B C24A C23B 125.8(19) .
C22 C24A C23B 63.1(8) .
C25B C25A C22 52.3(9) .
C25B C25A C24B 91.8(11) .
C22 C25A C24B 48.5(7) .
C53B C53A C51 61.5(11) .
C53B C53A C52B 105.4(15) .
C51 C53A C52B 56.3(8) .
C81 C82 O14 113.0(11) .
C81 C82 H82A 109.0 .
O14 C82 H82A 109.0 .
C81 C82 H82B 109.0 .
O14 C82 H82B 109.0 .
H82A C82 H82B 107.8 .
C53B C54A C54B 124.0(17) .
C53B C54A C51 63.0(11) .
C54B C54A C51 64.8(11) .
C86 C85 H85A 109.5 .
C86 C85 H85B 109.5 .
H85A C85 H85B 109.5 .
C86 C85 H85C 109.5 .
H85A C85 H85C 109.5 .
H85B C85 H85C 109.5 .
C86 C87 C88 97.1(12) .
C86 C87 H87A 112.3 .
C88 C87 H87A 112.3 .
C86 C87 H87B 112.3 .
C88 C87 H87B 112.3 .
H87A C87 H87B 109.9 .
C85 C86 C87 97.9(12) .
C85 C86 H86A 112.2 .
C87 C86 H86A 112.2 .
C85 C86 H86B 112.2 .
C87 C86 H86B 112.2 .
H86A C86 H86B 109.8 .
C87 C88 C89 97.8(11) .
C87 C88 H88A 112.2 .
C89 C88 H88A 112.2 .
C87 C88 H88B 112.2 .
C89 C88 H88B 112.2 .
H88A C88 H88B 109.8 .
C88 C89 H89A 109.5 .
C88 C89 H89B 109.5 .
H89A C89 H89B 109.5 .
C88 C89 H89C 109.5 .
H89A C89 H89C 109.5 .
H89B C89 H89C 109.5 .
C23A C23B C22 55.3(8) .
C23A C23B C24A 99.5(12) .
C22 C23B C24A 53.5(7) .
C24A C24B C22 78.4(16) .
C24A C24B C25A 135(2) .
C22 C24B C25A 57.1(8) .
C23A C25B C22 71.8(14) .
C23A C25B C25A 130.0(19) .
C22 C25B C25A 63.9(10) .
C52A C52B C51 64.8(12) .
C52A C52B C53A 121.6(17) .
C51 C52B C53A 57.3(9) .
C52A C52B K2 120.9(15) 4_666
C51 C52B K2 172.2(13) 4_666
C53A C52B K2 116.2(11) 4_666
C54A C53B C53A 127(2) .
C54A C53B C51 63.5(11) .
C53A C53B C51 66.5(12) .
C54A C54B C52A 113.9(17) .
C54A C54B C51 62.1(11) .
C52A C54B C51 57.8(10) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 1.879(5) .
Ni1 O1 1.882(4) .
Ni1 N1 1.883(5) .
Ni1 O2 1.901(4) .
Ni2 N4 1.871(5) .
Ni2 O4 1.881(4) .
Ni2 N3 1.883(5) .
Ni2 O5 1.887(4) .
K1 O3 2.510(4) .
K1 O8 2.725(5) .
K1 O10 2.728(6) .
K1 O12 2.777(5) .
K1 O11 2.786(5) .
K1 O9 2.811(5) .
K1 O7 2.907(5) .
K2 O6 2.494(5) .
K2 O17 2.688(5) .
K2 O13 2.748(6) .
K2 O15 2.764(6) .
K2 O16 2.797(5) .
K2 O14 2.834(6) .
K2 O18 2.878(6) .
K2 C52B 3.11(2) 4_565
O1 C1 1.306(7) .
O4 C2 1.312(7) .
N1 C15 1.329(7) .
N1 C3 1.448(7) .
O2 C1 1.309(7) .
O5 C2 1.300(7) .
O16 C75 1.403(8) .
O16 C74 1.434(8) .
N3 C50 1.339(7) .
N3 C38 1.442(7) .
O3 C1 1.242(7) .
N2 C21 1.344(7) .
N2 C26 1.451(7) .
O6 C2 1.235(7) .
O7 C027 1.412(8) .
O7 C02O 1.415(9) .
O12 C02G 1.396(9) .
O12 C02N 1.406(9) .
N4 C56 1.353(7) .
N4 C61 1.433(8) .
O9 C02E 1.392(9) .
O9 C02K 1.410(8) .
O8 C02P 1.371(9) .
O8 C025 1.395(8) .
O17 C77 1.399(9) .
O17 C76 1.425(8) .
O15 C73 1.411(8) .
O15 C84 1.427(10) .
O11 C02X 1.391(9) .
O11 C01Z 1.435(8) .
O10 C01O 1.375(9) .
O10 C02C 1.417(9) .
O18 C78 1.428(9) .
O18 C79 1.434(12) .
O14 C82 1.398(11) .
O14 C83 1.394(11) .
O13 C80 1.363(12) .
O13 C81 1.391(12) .
C50 C55 1.398(8) .
C50 C51 1.563(8) .
C15 C20 1.395(8) .
C15 C16 1.579(8) .
C38 C46 1.389(8) .
C38 C39 1.399(9) .
C26 C33 1.395(9) .
C26 C27 1.420(8) .
C3 C11 1.401(9) .
C3 C4 1.403(8) .
C46 C45 1.414(9) .
C46 C47 1.519(9) .
C20 C21 1.397(8) .
C20 H20 0.9500 .
C61 C69 1.385(10) .
C61 C62 1.415(9) .
C16 C19 1.524(9) .
C16 C18 1.527(9) .
C16 C17 1.533(8) .
C9 C8 1.372(9) .
C9 C10 1.382(9) .
C9 H9 0.9500 .
C11 C10 1.411(8) .
C11 C12 1.511(9) .
C10 H10 0.9500 .
C12 C13 1.531(8) .
C12 C14 1.553(9) .
C12 H12 1.0000 .
C34 C33 1.377(8) .
C34 C32 1.387(9) .
C34 H34 0.9500 .
C21 C22 1.559(8) .
C5 C4 1.516(9) .
C5 C6 1.522(9) .
C5 C7 1.550(9) .
C5 H5 1.0000 .
C55 C56 1.398(9) .
C55 H55 0.9500 .
C47 C49 1.515(9) .
C47 C48 1.536(9) .
C47 H47 1.0000 .
C33 C35 1.519(9) .
C27 C31 1.395(9) .
C27 C28 1.510(9) .
C4 C8 1.400(8) .
C75 C76 1.487(10) .
C75 H75A 0.9900 .
C75 H75B 0.9900 .
C56 C57 1.569(8) .
C69 C68 1.419(9) .
C69 C71 1.517(10) .
C8 H8 0.9500 .
C31 C32 1.381(10) .
C31 H31 0.9500 .
C35 C36 1.524(10) .
C35 C37 1.545(10) .
C35 H35 1.0000 .
C22 C25B 1.45(2) .
C22 C24B 1.464(19) .
C22 C23A 1.519(12) .
C22 C24A 1.550(13) .
C22 C25A 1.642(13) .
C22 C23B 1.72(2) .
C57 C58 1.523(9) .
C57 C60 1.531(9) .
C57 C59 1.560(10) .
C40 C39 1.509(9) .
C40 C42 1.532(9) .
C40 C41 1.538(9) .
C40 H40 1.0000 .
C39 C43 1.390(9) .
C01O C01Z 1.500(11) .
C01O H01A 0.9900 .
C01O H01B 0.9900 .
C51 C52A 1.522(13) .
C51 C53B 1.54(2) .
C51 C54A 1.543(13) .
C51 C52B 1.58(2) .
C51 C54B 1.58(2) .
C51 C53A 1.603(12) .
C30 C28 1.524(8) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C32 H32 0.9500 .
C76 H76A 0.9900 .
C76 H76B 0.9900 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C62 C66 1.380(10) .
C62 C63 1.510(11) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C01Z H01C 0.9900 .
C01Z H01D 0.9900 .
C71 C70 1.516(9) .
C71 C72 1.533(10) .
C71 H71 1.0000 .
C43 C44 1.373(10) .
C43 H43 0.9500 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C45 C44 1.381(10) .
C45 H45 0.9500 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C025 C027 1.517(10) .
C025 H02A 0.9900 .
C025 H02B 0.9900 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C027 H02C 0.9900 .
C027 H02D 0.9900 .
C28 C29 1.529(9) .
C28 H28 1.0000 .
C66 C67 1.379(12) .
C66 H66 0.9500 .
C68 C67 1.388(11) .
C68 H68 0.9500 .
C78 C77 1.477(10) .
C78 H78A 0.9900 .
C78 H78B 0.9900 .
C02C C02E 1.469(11) .
C02C H02E 0.9900 .
C02C H02F 0.9900 .
C44 H44 0.9500 .
C02E H02G 0.9900 .
C02E H02H 0.9900 .
C60 H60A 0.9800 .
C60 H60B 0.9800 .
C60 H60C 0.9800 .
C02G C02O 1.485(10) .
C02G H02I 0.9900 .
C02G H02J 0.9900 .
C67 H67 0.9500 .
C58 H58A 0.9800 .
C58 H58B 0.9800 .
C58 H58C 0.9800 .
C74 C73 1.483(10) .
C74 H74A 0.9900 .
C74 H74B 0.9900 .
C02K C02P 1.539(11) .
C02K H02K 0.9900 .
C02K H02L 0.9900 .
C59 H59A 0.9800 .
C59 H59B 0.9800 .
C59 H59C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C02N C02X 1.490(11) .
C02N H02M 0.9900 .
C02N H02N 0.9900 .
C02O H02O 0.9900 .
C02O H02P 0.9900 .
C02P H02Q 0.9900 .
C02P H02R 0.9900 .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C73 H73A 0.9900 .
C73 H73B 0.9900 .
C72 H72A 0.9800 .
C72 H72B 0.9800 .
C72 H72C 0.9800 .
C64 C63 1.540(10) .
C64 H64A 0.9800 .
C64 H64B 0.9800 .
C64 H64C 0.9800 .
C63 C65 1.538(10) .
C63 H63 1.0000 .
C02X H02S 0.9900 .
C02X H02T 0.9900 .
C65 H65A 0.9800 .
C65 H65B 0.9800 .
C65 H65C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C70 H70A 0.9800 .
C70 H70B 0.9800 .
C70 H70C 0.9800 .
C77 H77A 0.9900 .
C77 H77B 0.9900 .
C84 C83 1.468(12) .
C84 H84A 0.9900 .
C84 H84B 0.9900 .
C83 H83A 0.9900 .
C83 H83B 0.9900 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C79 C80 1.409(15) .
C79 H79A 0.9900 .
C79 H79B 0.9900 .
C80 H80A 0.9900 .
C80 H80B 0.9900 .
C23A C25B 1.10(2) .
C23A C23B 1.54(2) .
C81 C82 1.370(14) .
C81 H81A 0.9900 .
C81 H81B 0.9900 .
C52A C52B 1.19(2) .
C52A C54B 1.57(3) .
C24A C24B 0.883(19) .
C24A C23B 1.73(2) .
C25A C25B 1.64(2) .
C25A C24B 1.88(2) .
C53A C53B 1.38(3) .
C53A C52B 1.75(3) .
C82 H82A 0.9900 .
C82 H82B 0.9900 .
C54A C53B 1.39(3) .
C54A C54B 1.39(3) .
C85 C86 1.528(13) .
C85 H85A 0.9800 .
C85 H85B 0.9800 .
C85 H85C 0.9800 .
C87 C86 1.538(13) .
C87 C88 1.546(13) .
C87 H87A 0.9900 .
C87 H87B 0.9900 .
C86 H86A 0.9900 .
C86 H86B 0.9900 .
C88 C89 1.552(13) .
C88 H88A 0.9900 .
C88 H88B 0.9900 .
C89 H89A 0.9800 .
C89 H89B 0.9800 .
C89 H89C 0.9800 .
C52B K2 3.11(2) 4_666
