#------------------------------------------------------------------------------
#$Date: 2023-03-14 01:59:07 +0200 (Tue, 14 Mar 2023) $
#$Revision: 281852 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/26/7712601.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_7712601
loop_
_publ_author_name
'Deng, Yan-Ling'
'Chen, An-Na'
'Li, Wei'
'Xin, Shu-Sheng'
'Pan, Chun-Yang'
_publ_section_title
;
 Exploration of the oxygen reduction reaction activity of four transition
 metal borates: synthesis, structure and characterization.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00196b
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.04(C112 H98 B4 K4 N16 Ni8 O48)'
_chemical_formula_sum            'C4.48 H3.92 B0.16 K0.16 N0.64 Ni0.32 O1.92'
_chemical_formula_weight         124.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-10 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.1050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            25
_cell_length_a                   9.6192(2)
_cell_length_b                   33.4680(7)
_cell_length_c                   10.6609(3)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.20
_cell_volume                     3107.89(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            62596
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         2.416
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0109
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0775 after correction.
The Ratio of minimum to maximum transmission is 0.3949.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 4976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12666
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0472
_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)+(0.0520P)²+1.2841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                11674
_reflns_number_total             12666
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00196b2.cif
_cod_data_source_block           d4
_cod_database_code               7712601
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C34(H34), C2(H2), C7(H7), C6(H6), C31(H31), C3(H3), C30(H30), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C50(H50), C15(H15), C19(H19), C44(H44), C46(H46),
 C52(H52), C21(H21), C13(H13), C10(H10), C37(H37), C51(H51), C42(H42), C9(H9),
 C11(H11), C45(H45), C38(H38), C48(H48), C53(H53), C54(H54), C39(H39), C28(H28),
  C22(H22), C55(H55), C43(H43), C26(H26), C24(H24), C27(H27), C56(H56),
 C49(H49), C23(H23), C41(H41), C18(H18), C17(H17), C20(H20), C47(H47), C12(H12),
  C40(H40)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.16622(9) 0.34299(2) 0.50373(8) 0.02521(18) Uani 1 1 d . . . . .
Ni3 Ni 0.50585(10) 0.59481(3) 1.00354(9) 0.02495(17) Uani 1 1 d . . . . .
Ni4 Ni 0.80377(10) 0.69803(2) 0.82164(9) 0.02638(19) Uani 1 1 d . . . . .
Ni2 Ni 0.10322(10) 0.44363(3) 0.28303(10) 0.0309(2) Uani 1 1 d . . . . .
K2 K -0.01305(19) 0.58271(5) 0.5439(2) 0.0419(4) Uani 1 1 d . . . . .
K1 K 0.27370(17) 0.32705(4) 1.00081(17) 0.0321(3) Uani 1 1 d . . . . .
O6 O 0.2011(6) 0.38909(15) 0.8231(5) 0.0405(12) Uani 1 1 d . . . . .
O17 O 0.6976(5) 0.59739(15) 1.1836(5) 0.0328(10) Uani 1 1 d . . . . .
O15 O 0.6388(5) 0.60271(13) 0.8889(5) 0.0259(9) Uani 1 1 d . . . . .
O14 O 0.3329(5) 0.59833(16) 0.8107(5) 0.0313(10) Uani 1 1 d . . . . .
O7 O -0.1000(5) 0.40950(14) 0.2513(5) 0.0282(10) Uani 1 1 d . . . . .
O5 O 0.0307(5) 0.34647(15) 0.6771(4) 0.0284(9) Uani 1 1 d . . . . .
O9 O 0.0308(6) 0.33931(18) 0.0697(5) 0.0399(12) Uani 1 1 d . . . . .
O1 O -0.4183(5) 0.33982(19) 0.0886(5) 0.0426(12) Uani 1 1 d . . . . .
O10 O 0.1381(6) 0.39413(16) 0.1918(5) 0.0369(11) Uani 1 1 d . . . . .
O2 O -0.3483(5) 0.34512(17) 0.3151(5) 0.0335(10) Uani 1 1 d . . . . .
O12 O 0.0400(7) 0.50215(14) 0.5886(6) 0.0402(12) Uani 1 1 d . . . . .
O13 O 0.2789(6) 0.59504(19) 0.5862(5) 0.0427(13) Uani 1 1 d . . . . .
O16 O 0.5673(5) 0.65607(13) 0.9962(5) 0.0254(9) Uani 1 1 d . . . . .
O4 O -0.1074(5) 0.40339(13) 0.4856(5) 0.0259(9) Uani 1 1 d . . . . .
O8 O 0.1238(5) 0.41003(14) 0.4636(5) 0.0269(10) Uani 1 1 d . . . . .
O23 O 0.7471(5) 0.74016(14) 0.9285(5) 0.0308(10) Uani 1 1 d . . . . .
O21 O 0.7475(6) 0.59412(16) 0.6082(6) 0.0384(12) Uani 1 1 d . . . . .
O20 O 0.8070(5) 0.66286(14) 0.9908(5) 0.0274(10) Uani 1 1 d . . . . .
O24 O 0.7304(6) 0.75415(14) 1.1262(5) 0.0352(11) Uani 1 1 d . . . . .
O11 O 0.0478(6) 0.48586(15) 0.3880(6) 0.0375(12) Uani 1 1 d . . . . .
O19 O 0.5929(5) 0.66403(13) 0.7705(4) 0.0244(9) Uani 1 1 d . . . . .
O22 O 0.8435(5) 0.65010(14) 0.7270(5) 0.0321(10) Uani 1 1 d . . . . .
O3 O -0.0461(5) 0.34903(14) 0.3745(4) 0.0262(9) Uani 1 1 d . . . . .
O18 O 0.8543(8) 0.63896(19) 1.3430(6) 0.065(2) Uani 1 1 d . . . . .
N2 N -0.2965(6) 0.35299(16) 0.6108(6) 0.0298(12) Uani 1 1 d . . . . .
N6 N 0.3689(7) 0.60307(17) 1.1033(6) 0.0320(13) Uani 1 1 d . . . . .
N5 N 0.4953(7) 0.53398(17) 0.9996(6) 0.0306(12) Uani 1 1 d . . . . .
N4 N 0.3281(7) 0.46421(18) 0.3484(7) 0.0345(13) Uani 1 1 d . . . . .
N8 N 1.0320(7) 0.71610(18) 0.9028(7) 0.0341(13) Uani 1 1 d . . . . .
N1 N -0.1788(6) 0.28216(17) 0.5091(6) 0.0298(12) Uani 1 1 d . . . . .
N7 N 0.7445(7) 0.73419(17) 0.6506(6) 0.0306(12) Uani 1 1 d . . . . .
N3 N 0.0211(7) 0.4769(2) 0.1018(8) 0.0481(19) Uani 1 1 d . . . . .
C16 C -0.4750(9) 0.3696(2) 0.7506(9) 0.0424(19) Uani 1 1 d . . . . .
H16 H -0.536759 0.375155 0.798302 0.051 Uiso 1 1 calc R . . . .
C14 C -0.2558(8) 0.3401(2) 0.7397(7) 0.0326(14) Uani 1 1 d . . . . .
H14 H -0.163515 0.325194 0.783356 0.039 Uiso 1 1 calc R . . . .
C50 C 0.7364(9) 0.8003(2) 0.5652(8) 0.0383(17) Uani 1 1 d . . . . .
H50 H 0.752668 0.828061 0.584184 0.046 Uiso 1 1 calc R . . . .
C5 C 0.0882(8) 0.3814(2) 0.7142(7) 0.0287(14) Uani 1 1 d . . . . .
C15 C -0.3425(9) 0.3474(3) 0.8124(7) 0.0406(17) Uani 1 1 d . . . . .
H15 H -0.311188 0.337336 0.903654 0.049 Uiso 1 1 calc R . . . .
C34 C 0.6787(8) 0.6674(2) 1.1310(7) 0.0296(14) Uani 1 1 d . . . . .
H34 H 0.632866 0.686651 1.174598 0.035 Uiso 1 1 calc R . . . .
C19 C 0.4189(8) 0.4451(3) 0.3023(8) 0.0385(17) Uani 1 1 d . . . . .
H19 H 0.377982 0.423551 0.239275 0.046 Uiso 1 1 calc R . . . .
C1 C -0.3217(7) 0.3425(2) 0.2090(7) 0.0320(13) Uani 1 1 d . . . . .
C2 C -0.1520(7) 0.3415(2) 0.2315(6) 0.0316(14) Uani 1 1 d . . . . .
H2 H -0.127395 0.315693 0.198266 0.038 Uiso 1 1 calc R . . . .
C44 C 0.1908(11) 0.6174(3) 1.2448(10) 0.048(2) Uani 1 1 d . . . . .
H44 H 0.129462 0.622592 1.293133 0.057 Uiso 1 1 calc R . . . .
C46 C 0.4126(9) 0.5904(3) 1.2341(8) 0.0402(17) Uani 1 1 d . . . . .
H46 H 0.506839 0.576330 1.277950 0.048 Uiso 1 1 calc R . . . .
C52 C 1.1143(9) 0.7091(3) 0.8283(8) 0.0427(19) Uani 1 1 d . . . . .
H52 H 1.065800 0.695768 0.741793 0.051 Uiso 1 1 calc R . . . .
C7 C 0.1238(8) 0.43636(19) 0.5693(7) 0.0274(14) Uani 1 1 d . . . . .
H7 H 0.228265 0.437684 0.647985 0.033 Uiso 1 1 calc R . . . .
C21 C 0.6307(9) 0.4873(3) 0.4351(10) 0.047(2) Uani 1 1 d . . . . .
H21 H 0.735859 0.494407 0.467790 0.057 Uiso 1 1 calc R . . . .
C13 C -0.3145(9) 0.2634(2) 0.4549(9) 0.0392(17) Uani 1 1 d . . . . .
H13 H -0.404907 0.279272 0.421869 0.047 Uiso 1 1 calc R . . . .
C10 C -0.0572(9) 0.2183(2) 0.5499(8) 0.0375(16) Uani 1 1 d . . . . .
H10 H 0.035355 0.203317 0.584680 0.045 Uiso 1 1 calc R . . . .
C37 C 0.3610(10) 0.5148(2) 0.9403(8) 0.0414(18) Uani 1 1 d . . . . .
H37 H 0.269247 0.530185 0.902604 0.050 Uiso 1 1 calc R . . . .
C51 C 0.7638(9) 0.7737(2) 0.6703(8) 0.0367(16) Uani 1 1 d . . . . .
H51 H 0.798388 0.783768 0.761942 0.044 Uiso 1 1 calc R . . . .
C42 C 0.2389(9) 0.6229(2) 1.0448(9) 0.0394(17) Uani 1 1 d . . . . .
H42 H 0.208049 0.632436 0.952910 0.047 Uiso 1 1 calc R . . . .
C9 C -0.0535(8) 0.2596(2) 0.5571(8) 0.0339(15) Uani 1 1 d . . . . .
H9 H 0.043665 0.272471 0.598533 0.041 Uiso 1 1 calc R . . . .
C11 C -0.1960(10) 0.1995(2) 0.4919(9) 0.0455(19) Uani 1 1 d . . . . .
H11 H -0.201920 0.171238 0.483874 0.055 Uiso 1 1 calc R . . . .
C8 C 0.0671(8) 0.4787(2) 0.5113(8) 0.0339(16) Uani 1 1 d . . . . .
C33 C 0.7503(9) 0.6314(2) 1.2287(7) 0.0388(17) Uani 1 1 d . . . . .
C45 C 0.3257(10) 0.5970(3) 1.3074(8) 0.0454(18) Uani 1 1 d . . . . .
H45 H 0.359236 0.587449 1.399606 0.054 Uiso 1 1 calc R . . . .
C6 C 0.0110(8) 0.4166(2) 0.6146(7) 0.0290(14) Uani 1 1 d . . . . .
H6 H -0.030640 0.436551 0.659750 0.035 Uiso 1 1 calc R . . . .
C36 C 0.7549(7) 0.7312(2) 1.0465(7) 0.0286(14) Uani 1 1 d . . . . .
C38 C 0.3500(11) 0.4738(2) 0.9317(8) 0.046(2) Uani 1 1 d . . . . .
H38 H 0.252928 0.461173 0.885486 0.055 Uiso 1 1 calc R . . . .
C48 C 0.6627(11) 0.7461(3) 0.4095(9) 0.049(2) Uani 1 1 d . . . . .
H48 H 0.625509 0.735692 0.318067 0.059 Uiso 1 1 calc R . . . .
C53 C 1.2649(10) 0.7205(3) 0.8733(10) 0.056(2) Uani 1 1 d . . . . .
H53 H 1.318764 0.715700 0.817902 0.068 Uiso 1 1 calc R . . . .
C54 C 1.3368(9) 0.7391(3) 1.0006(11) 0.056(2) Uani 1 1 d . . . . .
H54 H 1.441120 0.747224 1.034445 0.067 Uiso 1 1 calc R . . . .
C39 C 0.4824(13) 0.4514(2) 0.9913(10) 0.052(2) Uani 1 1 d . . . . .
H39 H 0.478112 0.423012 0.988832 0.062 Uiso 1 1 calc R . . . .
C28 C 0.0108(11) 0.5162(3) 0.1062(12) 0.070(3) Uani 1 1 d . . . . .
H28 H 0.047900 0.528825 0.194250 0.084 Uiso 1 1 calc R . . . .
C22 C 0.5355(11) 0.5078(3) 0.4771(10) 0.055(2) Uani 1 1 d . . . . .
H22 H 0.572081 0.530445 0.535702 0.066 Uiso 1 1 calc R . . . .
C55 C 1.2557(10) 0.7457(3) 1.0766(12) 0.061(3) Uani 1 1 d . . . . .
H55 H 1.303630 0.758182 1.164772 0.073 Uiso 1 1 calc R . . . .
C43 C 0.1449(11) 0.6305(3) 1.1109(11) 0.054(2) Uani 1 1 d . . . . .
H43 H 0.050749 0.644433 1.064690 0.064 Uiso 1 1 calc R . . . .
C26 C -0.1037(17) 0.5239(6) -0.1351(16) 0.112(7) Uani 1 1 d . . . . .
H26 H -0.140877 0.540250 -0.215527 0.134 Uiso 1 1 calc R . . . .
C25 C -0.104(3) 0.4825(6) -0.1458(14) 0.159(10) Uani 1 1 d . . . . .
H25A H -0.052285 0.475556 -0.205931 0.191 Uiso 1 1 calc R . . . .
H25B H -0.211794 0.473646 -0.194158 0.191 Uiso 1 1 calc R . . . .
C24 C -0.034(2) 0.4602(5) -0.0233(12) 0.110(6) Uani 1 1 d . . . . .
H24 H -0.026365 0.432025 -0.029980 0.132 Uiso 1 1 calc R . . . .
C27 C -0.0509(12) 0.5398(4) -0.0105(16) 0.084(4) Uani 1 1 d . . . . .
H27 H -0.055363 0.567960 -0.000912 0.101 Uiso 1 1 calc R . . . .
C31 C 0.5841(8) 0.6320(2) 0.6782(7) 0.0260(13) Uani 1 1 d . . . . .
H31 H 0.501231 0.637359 0.583777 0.031 Uiso 1 1 calc R . . . .
C32 C 0.7386(8) 0.6244(2) 0.6701(7) 0.0295(14) Uani 1 1 d . . . . .
C3 C -0.1167(7) 0.3767(2) 0.1601(7) 0.0299(14) Uani 1 1 d . . . . .
H3 H -0.205524 0.381689 0.068713 0.036 Uiso 1 1 calc R . . . .
C4 C 0.0293(8) 0.3690(2) 0.1383(7) 0.0317(15) Uani 1 1 d . . . . .
C30 C 0.5419(8) 0.5966(2) 0.7438(7) 0.0293(14) Uani 1 1 d . . . . .
H30 H 0.570559 0.571140 0.711666 0.035 Uiso 1 1 calc R . . . .
C29 C 0.3698(7) 0.5964(2) 0.7098(7) 0.0283(13) Uani 1 1 d . . . . .
C35 C 0.8008(8) 0.6880(2) 1.0989(7) 0.0294(14) Uani 1 1 d . . . . .
H35 H 0.901827 0.687752 1.182078 0.035 Uiso 1 1 calc R . . . .
C56 C 1.1022(9) 0.7341(3) 1.0251(10) 0.047(2) Uani 1 1 d . . . . .
H56 H 1.046319 0.739178 1.078550 0.056 Uiso 1 1 calc R . . . .
C49 C 0.6852(10) 0.7865(3) 0.4321(9) 0.046(2) Uani 1 1 d . . . . .
H49 H 0.665627 0.804357 0.357376 0.055 Uiso 1 1 calc R . . . .
C23 C 0.3837(10) 0.4951(3) 0.4330(10) 0.0462(19) Uani 1 1 d . . . . .
H23 H 0.318409 0.509046 0.464431 0.055 Uiso 1 1 calc R . . . .
C41 C 0.6231(9) 0.5120(2) 1.0577(9) 0.0411(18) Uani 1 1 d . . . . .
H41 H 0.718950 0.525215 1.102900 0.049 Uiso 1 1 calc R . . . .
C18 C -0.4262(9) 0.3742(2) 0.5522(8) 0.0372(16) Uani 1 1 d . . . . .
H18 H -0.457960 0.383322 0.459754 0.045 Uiso 1 1 calc R . . . .
C17 C -0.5150(10) 0.3832(3) 0.6203(10) 0.048(2) Uani 1 1 d . . . . .
H17 H -0.604759 0.399027 0.576072 0.058 Uiso 1 1 calc R . . . .
C20 C 0.5706(9) 0.4557(2) 0.3435(9) 0.0419(18) Uani 1 1 d . . . . .
H20 H 0.633152 0.441552 0.309447 0.050 Uiso 1 1 calc R . . . .
C47 C 0.6948(9) 0.7207(2) 0.5206(8) 0.0392(17) Uani 1 1 d . . . . .
H47 H 0.680998 0.692772 0.504192 0.047 Uiso 1 1 calc R . . . .
C12 C -0.3306(10) 0.2230(3) 0.4442(10) 0.049(2) Uani 1 1 d . . . . .
H12 H -0.429353 0.210932 0.405810 0.059 Uiso 1 1 calc R . . . .
C40 C 0.6209(11) 0.4709(3) 1.0546(10) 0.050(2) Uani 1 1 d . . . . .
H40 H 0.713964 0.456235 1.095566 0.060 Uiso 1 1 calc R . . . .
B1 B -0.0327(9) 0.3927(2) 0.3926(8) 0.0265(14) Uani 1 1 d . . . . .
B2 B 0.6498(9) 0.6462(2) 0.9111(8) 0.0247(14) 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'
B B 0.0013 0.0007 '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'
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'
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 Ni1 O2 170.97(19) . . ?
O5 Ni1 O4 81.11(19) . . ?
O5 Ni1 O3 91.76(17) . . ?
O5 Ni1 N2 92.2(2) . . ?
O5 Ni1 N1 94.3(2) . . ?
O2 Ni1 O4 91.6(2) . . ?
O2 Ni1 O3 80.48(17) . . ?
O2 Ni1 N2 94.1(2) . . ?
O2 Ni1 N1 91.5(2) . . ?
O4 Ni1 O3 67.49(17) . . ?
N2 Ni1 O4 98.30(19) . . ?
N2 Ni1 O3 164.4(2) . . ?
N1 Ni1 O4 166.0(2) . . ?
N1 Ni1 O3 99.6(2) . . ?
N1 Ni1 N2 95.1(2) . . ?
O17 Ni3 O15 90.66(18) . . ?
O17 Ni3 O14 170.44(19) . . ?
O17 Ni3 O16 80.76(19) . . ?
O17 Ni3 N6 91.7(2) . . ?
O17 Ni3 N5 94.6(2) . . ?
O15 Ni3 O16 67.55(17) . . ?
O14 Ni3 O15 81.07(18) . . ?
O14 Ni3 O16 91.59(19) . . ?
O14 Ni3 N6 95.0(2) . . ?
O14 Ni3 N5 91.4(2) . . ?
N6 Ni3 O15 164.7(2) . . ?
N6 Ni3 O16 98.0(2) . . ?
N6 Ni3 N5 96.3(2) . . ?
N5 Ni3 O15 98.6(2) . . ?
N5 Ni3 O16 165.1(2) . . ?
O23 Ni4 O20 79.66(18) . . ?
O23 Ni4 O19 93.44(18) . . ?
O23 Ni4 N8 93.0(2) . . ?
O23 Ni4 N7 92.8(2) . . ?
O20 Ni4 O19 66.66(16) . . ?
O22 Ni4 O23 171.08(19) . . ?
O22 Ni4 O20 92.64(19) . . ?
O22 Ni4 O19 79.26(18) . . ?
O22 Ni4 N8 92.8(2) . . ?
O22 Ni4 N7 93.7(2) . . ?
N8 Ni4 O20 100.0(2) . . ?
N8 Ni4 O19 163.8(2) . . ?
N7 Ni4 O20 165.6(2) . . ?
N7 Ni4 O19 101.9(2) . . ?
N7 Ni4 N8 92.6(2) . . ?
O7 Ni2 O8 66.45(17) . . ?
O10 Ni2 O7 79.35(19) . . ?
O10 Ni2 O8 91.78(19) . . ?
O10 Ni2 N4 94.1(2) . . ?
O10 Ni2 N3 93.9(3) . . ?
O11 Ni2 O7 91.3(2) . . ?
O11 Ni2 O10 169.2(2) . . ?
O11 Ni2 O8 79.39(19) . . ?
O11 Ni2 N4 93.7(2) . . ?
O11 Ni2 N3 93.2(3) . . ?
N4 Ni2 O7 165.0(2) . . ?
N4 Ni2 O8 100.6(2) . . ?
N3 Ni2 O7 100.1(2) . . ?
N3 Ni2 O8 164.2(2) . . ?
N3 Ni2 N4 93.7(3) . . ?
O14 K2 C32 101.79(15) . 1_455 ?
O12 K2 O14 87.80(16) . . ?
O12 K2 C32 115.59(17) . 1_455 ?
O12 K2 C29 87.77(17) . . ?
O13 K2 O14 41.15(13) . . ?
O13 K2 O12 91.02(19) . . ?
O13 K2 O21 152.00(18) . 1_455 ?
O13 K2 O18 97.7(2) . 1_454 ?
O13 K2 C32 135.49(19) . 1_455 ?
O13 K2 C29 19.61(15) . . ?
O21 K2 O14 114.00(15) 1_455 . ?
O21 K2 O12 102.16(17) 1_455 . ?
O21 K2 O18 86.4(2) 1_455 1_454 ?
O21 K2 C32 17.60(16) 1_455 1_455 ?
O21 K2 C29 135.09(17) 1_455 . ?
O18 K2 O14 121.33(16) 1_454 . ?
O18 K2 O12 143.5(2) 1_454 . ?
O18 K2 C32 81.9(2) 1_454 1_455 ?
O18 K2 C29 111.17(19) 1_454 . ?
C29 K2 O14 21.68(13) . . ?
C29 K2 C32 121.14(18) . 1_455 ?
O6 K1 O5 42.09(14) . . ?
O6 K1 O9 94.37(18) . 1_556 ?
O6 K1 O1 92.30(18) . 1_656 ?
O6 K1 O23 152.72(15) . 2_647 ?
O6 K1 O24 112.80(16) . 2_647 ?
O6 K1 C5 20.08(15) . . ?
O6 K1 C36 132.34(17) . 2_647 ?
O5 K1 C5 22.21(14) . . ?
O9 K1 O5 86.86(14) 1_556 . ?
O9 K1 O23 85.63(16) 1_556 2_647 ?
O9 K1 O24 114.88(17) 1_556 2_647 ?
O9 K1 C5 88.76(17) 1_556 . ?
O9 K1 C36 99.38(18) 1_556 2_647 ?
O1 K1 O5 120.61(14) 1_656 . ?
O1 K1 O9 143.30(17) 1_656 1_556 ?
O1 K1 O23 103.95(17) 1_656 2_647 ?
O1 K1 O24 95.35(18) 1_656 2_647 ?
O1 K1 C5 107.92(17) 1_656 . ?
O1 K1 C36 102.48(18) 1_656 2_647 ?
O23 K1 O5 110.84(13) 2_647 . ?
O23 K1 C5 133.04(15) 2_647 . ?
O23 K1 C36 22.95(15) 2_647 2_647 ?
O24 K1 O5 78.86(14) 2_647 . ?
O24 K1 O23 44.86(13) 2_647 2_647 ?
O24 K1 C5 98.08(16) 2_647 . ?
O24 K1 C36 22.12(16) 2_647 2_647 ?
C36 K1 O5 93.23(15) 2_647 . ?
C36 K1 C5 114.77(17) 2_647 . ?
C5 O6 K1 111.3(4) . . ?
C33 O17 Ni3 117.3(5) . . ?
C30 O15 Ni3 109.0(4) . . ?
C30 O15 B2 106.4(5) . . ?
B2 O15 Ni3 92.9(4) . . ?
Ni3 O14 K2 159.6(2) . . ?
C29 O14 Ni3 116.9(4) . . ?
C29 O14 K2 78.9(4) . . ?
C3 O7 Ni2 110.2(4) . . ?
C3 O7 B1 106.1(5) . . ?
B1 O7 Ni2 93.7(4) . . ?
Ni1 O5 K1 156.9(2) . . ?
C5 O5 Ni1 116.8(4) . . ?
C5 O5 K1 80.6(4) . . ?
C4 O9 K1 120.0(5) . 1_554 ?
C1 O1 K1 126.7(4) . 1_454 ?
C4 O10 Ni2 118.9(5) . . ?
C1 O2 Ni1 117.8(4) . . ?
C8 O12 K2 125.5(5) . . ?
C29 O13 K2 113.7(4) . . ?
C34 O16 Ni3 108.4(4) . . ?
C34 O16 B2 107.9(5) . . ?
B2 O16 Ni3 92.1(4) . . ?
C6 O4 Ni1 109.9(4) . . ?
C6 O4 B1 107.5(5) . . ?
B1 O4 Ni1 93.1(4) . . ?
C7 O8 Ni2 110.5(4) . . ?
C7 O8 B1 107.6(5) . . ?
B1 O8 Ni2 93.4(4) . . ?
Ni4 O23 K1 150.3(2) . 2_657 ?
C36 O23 Ni4 118.5(4) . . ?
C36 O23 K1 87.9(4) . 2_657 ?
C32 O21 K2 121.0(5) . 1_655 ?
C35 O20 Ni4 111.1(4) . . ?
C35 O20 B2 107.3(5) . . ?
B2 O20 Ni4 94.4(4) . . ?
C36 O24 K1 100.2(4) . 2_657 ?
C8 O11 Ni2 119.1(4) . . ?
C31 O19 Ni4 109.8(4) . . ?
C31 O19 B2 106.4(5) . . ?
B2 O19 Ni4 93.0(4) . . ?
C32 O22 Ni4 119.9(4) . . ?
C2 O3 Ni1 109.2(3) . . ?
C2 O3 B1 107.0(5) . . ?
B1 O3 Ni1 92.9(4) . . ?
C33 O18 K2 123.3(5) . 1_656 ?
C14 N2 Ni1 122.7(5) . . ?
C14 N2 C18 117.5(6) . . ?
C18 N2 Ni1 119.7(5) . . ?
C46 N6 Ni3 120.9(5) . . ?
C42 N6 Ni3 121.2(5) . . ?
C42 N6 C46 117.8(7) . . ?
C37 N5 Ni3 121.2(5) . . ?
C37 N5 C41 118.0(7) . . ?
C41 N5 Ni3 120.9(5) . . ?
C19 N4 Ni2 117.8(5) . . ?
C23 N4 Ni2 123.1(5) . . ?
C23 N4 C19 119.1(7) . . ?
C52 N8 Ni4 118.8(5) . . ?
C56 N8 Ni4 123.1(5) . . ?
C56 N8 C52 118.1(7) . . ?
C13 N1 Ni1 120.9(5) . . ?
C9 N1 Ni1 121.5(5) . . ?
C9 N1 C13 117.4(6) . . ?
C51 N7 Ni4 118.3(5) . . ?
C47 N7 Ni4 124.2(5) . . ?
C47 N7 C51 117.4(6) . . ?
C28 N3 Ni2 120.4(7) . . ?
C28 N3 C24 116.7(9) . . ?
C24 N3 Ni2 122.7(8) . . ?
C17 C16 C15 118.3(7) . . ?
N2 C14 C15 122.6(7) . . ?
C51 C50 C49 119.3(7) . . ?
O6 C5 K1 48.6(3) . . ?
O6 C5 O5 124.8(6) . . ?
O6 C5 C6 117.5(6) . . ?
O5 C5 K1 77.2(4) . . ?
O5 C5 C6 117.7(6) . . ?
C6 C5 K1 162.6(4) . . ?
C16 C15 C14 119.0(7) . . ?
O16 C34 C33 113.6(5) . . ?
O16 C34 C35 102.4(5) . . ?
C35 C34 C33 109.8(6) . . ?
N4 C19 C20 122.0(8) . . ?
O1 C1 O2 126.2(6) . . ?
O1 C1 C2 116.2(6) . . ?
O2 C1 C2 117.6(6) . . ?
O3 C2 C1 112.6(5) . . ?
O3 C2 C3 100.7(5) . . ?
C3 C2 C1 110.6(6) . . ?
C45 C44 C43 119.2(7) . . ?
N6 C46 C45 122.6(7) . . ?
N8 C52 C53 122.6(8) . . ?
O8 C7 C8 111.5(6) . . ?
O8 C7 C6 102.8(5) . . ?
C6 C7 C8 110.3(6) . . ?
C22 C21 C20 118.5(7) . . ?
N1 C13 C12 123.9(8) . . ?
C11 C10 C9 118.9(7) . . ?
N5 C37 C38 122.7(8) . . ?
N7 C51 C50 123.3(7) . . ?
N6 C42 C43 123.1(8) . . ?
N1 C9 C10 123.2(7) . . ?
C10 C11 C12 118.6(7) . . ?
O12 C8 O11 125.9(6) . . ?
O12 C8 C7 116.8(7) . . ?
O11 C8 C7 117.3(6) . . ?
O17 C33 C34 117.1(6) . . ?
O18 C33 O17 126.2(7) . . ?
O18 C33 C34 116.8(7) . . ?
C44 C45 C46 118.7(8) . . ?
O4 C6 C5 112.2(5) . . ?
O4 C6 C7 102.4(5) . . ?
C7 C6 C5 110.5(5) . . ?
O23 C36 K1 69.2(4) . 2_657 ?
O23 C36 C35 118.0(6) . . ?
O24 C36 K1 57.6(4) . 2_657 ?
O24 C36 O23 125.9(6) . . ?
O24 C36 C35 116.2(6) . . ?
C35 C36 K1 167.1(4) . 2_657 ?
C37 C38 C39 118.8(8) . . ?
C49 C48 C47 119.5(8) . . ?
C52 C53 C54 118.8(9) . . ?
C55 C54 C53 118.9(8) . . ?
C40 C39 C38 118.6(8) . . ?
N3 C28 C27 123.3(12) . . ?
C21 C22 C23 119.2(8) . . ?
C54 C55 C56 120.0(9) . . ?
C44 C43 C42 118.6(8) . . ?
C27 C26 C25 118.2(11) . . ?
C26 C25 C24 118.2(17) . . ?
N3 C24 C25 122.5(14) . . ?
C26 C27 C28 120.8(13) . . ?
O19 C31 C32 112.6(5) . . ?
O19 C31 C30 102.5(5) . . ?
C30 C31 C32 110.3(5) . . ?
O21 C32 K2 41.4(3) . 1_655 ?
O21 C32 O22 126.3(6) . . ?
O21 C32 C31 117.0(6) . . ?
O22 C32 K2 85.4(4) . 1_655 ?
O22 C32 C31 116.7(6) . . ?
C31 C32 K2 156.8(5) . 1_655 ?
O7 C3 C2 103.8(5) . . ?
O7 C3 C4 112.6(5) . . ?
C2 C3 C4 111.0(6) . . ?
O9 C4 O10 125.5(7) . . ?
O9 C4 C3 117.6(6) . . ?
O10 C4 C3 116.9(6) . . ?
O15 C30 C31 101.9(5) . . ?
O15 C30 C29 113.3(5) . . ?
C31 C30 C29 111.6(6) . . ?
O14 C29 K2 79.4(4) . . ?
O14 C29 C30 117.4(6) . . ?
O13 C29 K2 46.7(3) . . ?
O13 C29 O14 125.5(6) . . ?
O13 C29 C30 117.1(6) . . ?
C30 C29 K2 162.1(4) . . ?
O20 C35 C34 102.3(5) . . ?
O20 C35 C36 111.0(5) . . ?
C34 C35 C36 112.1(6) . . ?
N8 C56 C55 121.6(9) . . ?
C50 C49 C48 118.4(7) . . ?
N4 C23 C22 121.8(8) . . ?
N5 C41 C40 122.5(8) . . ?
N2 C18 C17 122.5(7) . . ?
C16 C17 C18 120.0(8) . . ?
C19 C20 C21 119.2(8) . . ?
N7 C47 C48 122.1(8) . . ?
C13 C12 C11 117.9(7) . . ?
C41 C40 C39 119.3(8) . . ?
O7 B1 O4 117.5(6) . . ?
O7 B1 O8 106.4(5) . . ?
O8 B1 O4 103.7(5) . . ?
O3 B1 O7 105.5(6) . . ?
O3 B1 O4 106.5(5) . . ?
O3 B1 O8 117.8(6) . . ?
O15 B2 O16 107.5(5) . . ?
O15 B2 O20 116.6(5) . . ?
O15 B2 O19 105.3(5) . . ?
O16 B2 O20 104.2(5) . . ?
O16 B2 O19 117.8(6) . . ?
O19 B2 O20 106.0(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O5 2.012(4) . ?
Ni1 O2 2.032(4) . ?
Ni1 O4 2.130(4) . ?
Ni1 O3 2.150(4) . ?
Ni1 N2 2.049(6) . ?
Ni1 N1 2.042(6) . ?
Ni3 O17 2.022(5) . ?
Ni3 O15 2.128(4) . ?
Ni3 O14 2.026(5) . ?
Ni3 O16 2.145(4) . ?
Ni3 N6 2.032(6) . ?
Ni3 N5 2.038(6) . ?
Ni4 O23 2.027(5) . ?
Ni4 O20 2.143(5) . ?
Ni4 O19 2.184(4) . ?
Ni4 O22 2.016(5) . ?
Ni4 N8 2.079(6) . ?
Ni4 N7 2.057(6) . ?
Ni2 O7 2.164(5) . ?
Ni2 O10 2.020(5) . ?
Ni2 O8 2.165(5) . ?
Ni2 O11 2.010(5) . ?
Ni2 N4 2.088(6) . ?
Ni2 N3 2.074(6) . ?
K2 O14 3.377(5) . ?
K2 O12 2.748(5) . ?
K2 O13 2.681(5) . ?
K2 O21 2.695(5) 1_455 ?
K2 O18 2.728(6) 1_454 ?
K2 C32 3.491(7) 1_455 ?
K2 C29 3.372(7) . ?
K1 O6 2.695(5) . ?
K1 O5 3.309(4) . ?
K1 O9 2.761(5) 1_556 ?
K1 O1 2.736(5) 1_656 ?
K1 O23 3.032(5) 2_647 ?
K1 O24 2.782(5) 2_647 ?
K1 C5 3.348(7) . ?
K1 C36 3.242(7) 2_647 ?
O6 C5 1.234(8) . ?
O17 C33 1.257(9) . ?
O15 C30 1.442(8) . ?
O15 B2 1.471(9) . ?
O14 C29 1.269(8) . ?
O7 C3 1.429(8) . ?
O7 B1 1.475(9) . ?
O5 C5 1.283(8) . ?
O9 C4 1.239(9) . ?
O1 C1 1.227(8) . ?
O10 C4 1.273(9) . ?
O2 C1 1.265(8) . ?
O12 C8 1.244(9) . ?
O13 C29 1.235(8) . ?
O16 C34 1.432(8) . ?
O16 B2 1.474(9) . ?
O4 C6 1.433(8) . ?
O4 B1 1.494(9) . ?
O8 C7 1.430(8) . ?
O8 B1 1.486(9) . ?
O23 C36 1.265(8) . ?
O21 C32 1.231(8) . ?
O20 C35 1.448(8) . ?
O20 B2 1.493(9) . ?
O24 C36 1.240(8) . ?
O11 C8 1.270(9) . ?
O19 C31 1.432(7) . ?
O19 B2 1.485(9) . ?
O22 C32 1.268(9) . ?
O3 C2 1.451(7) . ?
O3 B1 1.474(9) . ?
O18 C33 1.231(9) . ?
N2 C14 1.331(9) . ?
N2 C18 1.338(9) . ?
N6 C46 1.343(9) . ?
N6 C42 1.316(10) . ?
N5 C37 1.337(10) . ?
N5 C41 1.338(10) . ?
N4 C19 1.333(10) . ?
N4 C23 1.327(11) . ?
N8 C52 1.358(10) . ?
N8 C56 1.331(10) . ?
N1 C13 1.338(9) . ?
N1 C9 1.327(9) . ?
N7 C51 1.340(10) . ?
N7 C47 1.338(9) . ?
N3 C28 1.322(13) . ?
N3 C24 1.332(16) . ?
C16 C15 1.377(12) . ?
C16 C17 1.354(12) . ?
C14 C15 1.380(10) . ?
C50 C51 1.365(11) . ?
C50 C49 1.370(12) . ?
C5 C6 1.548(9) . ?
C34 C33 1.548(10) . ?
C34 C35 1.521(10) . ?
C19 C20 1.380(10) . ?
C1 C2 1.546(9) . ?
C2 C3 1.517(10) . ?
C44 C45 1.365(13) . ?
C44 C43 1.374(13) . ?
C46 C45 1.383(11) . ?
C52 C53 1.373(11) . ?
C7 C8 1.549(9) . ?
C7 C6 1.514(9) . ?
C21 C22 1.364(13) . ?
C21 C20 1.387(12) . ?
C13 C12 1.361(11) . ?
C10 C9 1.384(10) . ?
C10 C11 1.364(11) . ?
C37 C38 1.378(11) . ?
C42 C43 1.386(11) . ?
C11 C12 1.412(12) . ?
C36 C35 1.545(9) . ?
C38 C39 1.379(14) . ?
C48 C49 1.373(12) . ?
C48 C47 1.383(11) . ?
C53 C54 1.384(14) . ?
C54 C55 1.360(14) . ?
C39 C40 1.377(14) . ?
C28 C27 1.377(14) . ?
C22 C23 1.397(12) . ?
C55 C56 1.395(11) . ?
C26 C25 1.39(3) . ?
C26 C27 1.32(2) . ?
C25 C24 1.403(15) . ?
C31 C32 1.546(9) . ?
C31 C30 1.517(10) . ?
C3 C4 1.539(9) . ?
C30 C29 1.537(9) . ?
C41 C40 1.373(11) . ?
C18 C17 1.369(11) . ?
