#------------------------------------------------------------------------------ #$Date: 2020-10-06 12:01:28 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257560 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705181.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_7705181 loop_ _publ_author_name 'Xu, Dandan' 'Huang, Qianqian' 'Xu, Xinxin' 'Sang, Xiaoguang' _publ_section_title ; NiMOF-derived oxygen vacancy rich NiO with excellent capacitance and ORR/OER activities as a cathode material for Zn-based hybrid batteries. ; _journal_issue 35 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12441 _journal_page_last 12449 _journal_paper_doi 10.1039/d0dt01153c _journal_volume 49 _journal_year 2020 _chemical_formula_moiety '0.5(C50 H48 N4 Ni4 O22 S4), 2(H2 O)' _chemical_formula_sum 'C25 H28 N2 Ni2 O13 S2' _chemical_formula_weight 746.03 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-08-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-12 deposited with the CCDC. 2020-08-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.198(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.3634(7) _cell_length_b 10.5517(3) _cell_length_c 16.4604(6) _cell_measurement_reflns_used 15561 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32.4130 _cell_measurement_theta_min 3.7010 _cell_volume 3212.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.938 _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.938 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 5888 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.938 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.629 _diffrn_reflns_theta_min 3.653 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _refine_diff_density_max 2.803 _refine_diff_density_min -3.177 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 215 _refine_ls_number_reflns 5888 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0600 _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/[\s^2^(Fo^2^)+(0.0504P)^2^+25.1720P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1751 _refine_ls_wR_factor_ref 0.1774 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5059 _reflns_number_total 5888 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01153c2.cif _cod_data_source_block NiMOF _cod_depositor_comments 'Adding full bibliography for 7705181.cif.' _cod_database_code 7705181 _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 0.54 _shelx_estimated_absorpt_t_min 0.21 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.685 0.315 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 3. Restrained distances O6-H6 0.85 with sigma of 0.02 4. Rigid bond restraints O0AA, O1AA with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints O0AA \\sim O1AA: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 6. Others Fixed Sof: H13A(0.5) H13B(0.5) O0AA(0.5) H0AA(0.5) H0AB(0.5) O1AA(0.5) H1AA(0.5) H1AB(0.5) 7.a Riding coordinates: O0AA(H0AA,H0AB), O1AA(H1AA,H1AB) 7.b Rotating group: O5(H5A,H5B) 7.c Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C18(H18A,H18B) 7.d Aromatic/amide H refined with riding coordinates: C2(H2), C10(H10), C7(H7), C11(H11), C3(H3), C8(H8) ; _shelx_res_file ; TITL 82a in C2/c 82a_tw.res created by SHELXL-2018/3 at 17:31:12 on 11-Aug-2020 rem DFIX 1.95 H1Aa H0Aa CELL 0.71073 19.3634 10.5517 16.4604 90 107.198 90 ZERR 4 0.0007 0.0003 0.0006 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N Ni O S UNIT 100 112 8 8 52 8 DFIX 0.85 O6 H6 DELU O0AA O1AA SIMU O0AA O1AA L.S. 10 PLAN 2 LIST 8 BOND fmap 2 acta OMIT -10 0 6 OMIT -14 0 6 OMIT -9 5 6 OMIT -14 4 6 OMIT -16 4 6 OMIT -10 4 6 OMIT -17 5 6 OMIT -16 8 6 OMIT -20 4 6 OMIT -15 5 6 OMIT 8 2 17 OMIT -12 8 6 OMIT -17 1 6 OMIT 16 0 8 OMIT -19 1 6 OMIT 5 1 17 OMIT -1 5 6 OMIT -3 3 6 OMIT -11 1 6 OMIT -21 3 6 REM REM REM WGHT 0.050400 25.172001 BASF 0.31454 FVAR 3.71812 NI1 4 0.005502 0.619802 0.142524 11.00000 0.00989 0.01769 = 0.01411 -0.00068 0.00424 0.00143 S1 6 -0.235924 0.823913 0.239018 11.00000 0.02275 0.05611 = 0.02514 0.01257 0.01320 0.02285 O6 5 0.000000 0.511736 0.250000 10.50000 0.01375 0.01774 = 0.02007 0.00000 0.00669 0.00000 O1 5 -0.081342 0.719855 0.148964 11.00000 0.01978 0.03906 = 0.02372 0.00686 0.01157 0.01671 N1 3 0.006541 0.735847 0.041039 11.00000 0.02447 0.02517 = 0.01512 0.00062 0.00753 0.00067 O5 5 -0.065709 0.494026 0.060903 11.00000 0.02832 0.03220 = 0.02861 -0.00662 0.00584 -0.00676 AFIX 7 H5A 2 -0.110788 0.497693 0.066588 11.00000 -1.50000 H5B 2 -0.054064 0.411577 0.073702 11.00000 -1.50000 AFIX 0 O3 5 -0.377337 0.916418 0.248355 11.00000 0.03114 0.06646 = 0.03419 0.01613 0.01752 0.02786 C5 1 -0.109843 0.746700 0.205714 11.00000 0.01094 0.02042 = 0.02116 0.00069 0.00546 0.00494 C4 1 -0.298787 0.909402 0.164225 11.00000 0.01489 0.03864 = 0.02473 0.00439 0.00545 0.01325 C2 1 -0.209549 0.873808 0.100718 11.00000 0.02649 0.08172 = 0.02828 0.02261 0.01471 0.03329 AFIX 43 H2 2 -0.187693 0.876311 0.057463 11.00000 -1.20000 AFIX 0 C13 1 0.000000 0.892316 -0.250000 10.50000 0.07543 0.02473 = 0.02245 0.00000 0.01845 0.00000 AFIX 23 H13A 2 -0.042376 0.838250 -0.262815 10.50000 -1.20000 H13B 2 0.042374 0.838244 -0.237186 10.50000 -1.20000 AFIX 0 C1 1 -0.180284 0.814254 0.176035 11.00000 0.01523 0.03231 = 0.02273 0.00305 0.00714 0.01040 C10 1 0.068544 0.860623 -0.036241 11.00000 0.04923 0.04105 = 0.03873 0.00466 0.02494 -0.01156 AFIX 43 H10 2 0.112273 0.890925 -0.041031 11.00000 -1.20000 AFIX 0 C9 1 0.004088 0.893405 -0.096312 11.00000 0.06706 0.02164 = 0.02218 -0.00212 0.02082 -0.00082 C7 1 -0.055740 0.767881 -0.016628 11.00000 0.02917 0.03462 = 0.02065 0.00518 0.00601 0.00419 AFIX 43 H7 2 -0.098771 0.736610 -0.010335 11.00000 -1.20000 AFIX 0 C11 1 0.067293 0.782222 0.031105 11.00000 0.02842 0.03683 = 0.02840 0.00375 0.01142 -0.00389 AFIX 43 H11 2 0.110904 0.761294 0.070979 11.00000 -1.20000 AFIX 0 C18 1 0.002750 0.973259 -0.172631 11.00000 0.09594 0.02701 = 0.02236 0.00120 0.02408 -0.00166 AFIX 23 H18A 2 0.045599 1.026202 -0.159222 11.00000 -1.20000 H18B 2 -0.039163 1.028465 -0.185837 11.00000 -1.20000 AFIX 0 C3 1 -0.276145 0.931229 0.094750 11.00000 0.02220 0.07547 = 0.03642 0.02634 0.01391 0.02749 AFIX 43 H3 2 -0.302057 0.979098 0.048285 11.00000 -1.20000 AFIX 0 C8 1 -0.058594 0.845394 -0.084968 11.00000 0.05032 0.03840 = 0.02320 0.00779 0.00869 0.00900 AFIX 43 H8 2 -0.103016 0.865364 -0.123577 11.00000 -1.20000 AFIX 0 O2 5 -0.086461 0.725103 0.283206 11.00000 0.02126 0.03853 = 0.01850 0.00212 0.00603 0.01636 C6 1 -0.367663 0.948221 0.179304 11.00000 0.01667 0.03549 = 0.02681 0.00092 0.00682 0.01112 O4 5 -0.412307 1.009696 0.120658 11.00000 0.01809 0.03564 = 0.02562 0.00282 0.00880 0.01384 H6 2 -0.039738 0.473071 0.245808 11.00000 0.05362 PART 1 O0AA 5 -0.189268 0.361262 0.080495 10.50000 0.12116 0.22630 = 0.05599 -0.00489 0.04360 -0.03040 AFIX 3 H0AA 2 -0.224458 0.318362 0.049635 10.50000 -1.50000 H0AB 2 -0.165318 0.308712 0.117285 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O1AA 5 -0.202273 0.467112 0.092385 10.50000 0.08334 0.29267 = 0.04176 0.02931 0.00233 -0.07922 AFIX 3 H1AA 2 -0.201483 0.430012 0.138465 10.50000 -1.50000 H1AB 2 -0.242403 0.506322 0.077785 10.50000 -1.50000 AFIX 0 HKLF 5 REM 82a in C2/c REM wR2 = 0.1774, GooF = S = 1.170, Restrained GooF = 1.170 for all data REM R1 = 0.0600 for 5059 Fo > 4sig(Fo) and 0.0643 for all 5524 data REM 215 parameters refined using 7 restraints END WGHT 0.0504 25.1656 REM Highest difference peak 2.803, deepest hole -3.177, 1-sigma level 0.162 Q1 1 -0.0045 0.6213 0.0122 11.00000 0.05 2.80 Q2 1 0.0005 0.3817 0.2933 11.00000 0.05 1.82 ; _shelx_res_checksum 68301 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.00550(2) 0.61980(4) 0.14252(3) 0.01374(12) Uani 1 1 d . . . . . S1 S -0.23592(6) 0.82391(13) 0.23902(7) 0.0333(3) Uani 1 1 d . . . . . O6 O 0.000000 0.5117(3) 0.250000 0.0168(6) Uani 1 2 d DS T P . . O1 O -0.08134(15) 0.7199(3) 0.14896(18) 0.0264(6) Uani 1 1 d . . . . . N1 N 0.00654(18) 0.7358(3) 0.04104(19) 0.0212(6) Uani 1 1 d . . . . . O5 O -0.06571(17) 0.4940(3) 0.0609(2) 0.0303(6) Uani 1 1 d . . . . . H5A H -0.110788 0.497693 0.066588 0.045 Uiso 1 1 d GR . . . . H5B H -0.054064 0.411577 0.073702 0.045 Uiso 1 1 d GR . . . . O3 O -0.37734(19) 0.9164(4) 0.2484(2) 0.0422(9) Uani 1 1 d . . . . . C5 C -0.10984(17) 0.7467(3) 0.2057(2) 0.0174(6) Uani 1 1 d . . . . . C4 C -0.2988(2) 0.9094(4) 0.1642(3) 0.0262(8) Uani 1 1 d . . . . . C2 C -0.2095(3) 0.8738(6) 0.1007(3) 0.0441(14) Uani 1 1 d . . . . . H2 H -0.187693 0.876311 0.057463 0.053 Uiso 1 1 calc R . . . . C13 C 0.000000 0.8923(6) -0.250000 0.0400(17) Uani 1 2 d S T P . . H13A H -0.042376 0.838250 -0.262815 0.048 Uiso 0.5 1 calc R . . . . H13B H 0.042374 0.838244 -0.237186 0.048 Uiso 0.5 1 calc R . . . . C1 C -0.18028(19) 0.8143(4) 0.1760(2) 0.0231(7) Uani 1 1 d . . . . . C10 C 0.0685(3) 0.8606(5) -0.0362(3) 0.0404(11) Uani 1 1 d . . . . . H10 H 0.112273 0.890925 -0.041031 0.049 Uiso 1 1 calc R . . . . C9 C 0.0041(3) 0.8934(4) -0.0963(3) 0.0353(10) Uani 1 1 d . . . . . C7 C -0.0557(2) 0.7679(4) -0.0166(3) 0.0284(8) Uani 1 1 d . . . . . H7 H -0.098771 0.736610 -0.010335 0.034 Uiso 1 1 calc R . . . . C11 C 0.0673(2) 0.7822(4) 0.0311(3) 0.0306(8) Uani 1 1 d . . . . . H11 H 0.110904 0.761294 0.070979 0.037 Uiso 1 1 calc R . . . . C18 C 0.0027(4) 0.9733(5) -0.1726(3) 0.0470(14) Uani 1 1 d . . . . . H18A H 0.045599 1.026202 -0.159222 0.056 Uiso 1 1 calc R . . . . H18B H -0.039163 1.028465 -0.185837 0.056 Uiso 1 1 calc R . . . . C3 C -0.2761(2) 0.9312(6) 0.0947(3) 0.0436(13) Uani 1 1 d . . . . . H3 H -0.302057 0.979098 0.048285 0.052 Uiso 1 1 calc R . . . . C8 C -0.0586(3) 0.8454(5) -0.0850(3) 0.0378(10) Uani 1 1 d . . . . . H8 H -0.103016 0.865364 -0.123577 0.045 Uiso 1 1 calc R . . . . O2 O -0.08646(15) 0.7251(3) 0.28321(17) 0.0261(6) Uani 1 1 d . . . . . C6 C -0.3677(2) 0.9482(4) 0.1793(3) 0.0262(8) Uani 1 1 d . . . . . O4 O -0.41231(15) 1.0097(3) 0.12066(18) 0.0259(6) Uani 1 1 d . . . . . H6 H -0.040(2) 0.473(6) 0.246(4) 0.054(19) Uiso 1 1 d D . . . . O0AA O -0.1893(13) 0.361(2) 0.0805(12) 0.131(9) Uani 0.5 1 d . U . A 1 H0AA H -0.224458 0.318362 0.049635 0.196 Uiso 0.5 1 d R . . A 1 H0AB H -0.165318 0.308712 0.117285 0.196 Uiso 0.5 1 d R . . A 1 O1AA O -0.2023(10) 0.467(3) 0.0924(10) 0.143(10) Uani 0.5 1 d . U . B 2 H1AA H -0.201483 0.430012 0.138465 0.214 Uiso 0.5 1 d R . . B 2 H1AB H -0.242403 0.506322 0.077785 0.214 Uiso 0.5 1 d R . . B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00989(18) 0.0177(2) 0.01411(19) -0.00068(14) 0.00424(14) 0.00143(14) S1 0.0228(5) 0.0561(7) 0.0251(5) 0.0126(4) 0.0132(4) 0.0228(5) O6 0.0138(14) 0.0177(15) 0.0201(15) 0.000 0.0067(12) 0.000 O1 0.0198(12) 0.0391(16) 0.0237(13) 0.0069(11) 0.0116(10) 0.0167(11) N1 0.0245(15) 0.0252(14) 0.0151(13) 0.0006(10) 0.0075(11) 0.0007(11) O5 0.0283(14) 0.0322(15) 0.0286(15) -0.0066(12) 0.0058(12) -0.0068(12) O3 0.0311(16) 0.066(2) 0.0342(17) 0.0161(17) 0.0175(14) 0.0279(17) C5 0.0109(13) 0.0204(14) 0.0212(15) 0.0007(11) 0.0055(11) 0.0049(11) C4 0.0149(15) 0.039(2) 0.0247(17) 0.0044(15) 0.0055(13) 0.0133(14) C2 0.026(2) 0.082(4) 0.028(2) 0.023(2) 0.0147(17) 0.033(2) C13 0.075(5) 0.025(3) 0.022(3) 0.000 0.018(3) 0.000 C1 0.0152(14) 0.0323(18) 0.0227(16) 0.0030(14) 0.0071(13) 0.0104(13) C10 0.049(3) 0.041(2) 0.039(3) 0.005(2) 0.025(2) -0.012(2) C9 0.067(3) 0.0216(17) 0.0222(17) -0.0021(14) 0.021(2) -0.0008(19) C7 0.0292(19) 0.035(2) 0.0206(17) 0.0052(15) 0.0060(15) 0.0042(16) C11 0.0284(19) 0.037(2) 0.0284(19) 0.0037(16) 0.0114(16) -0.0039(16) C18 0.096(5) 0.027(2) 0.0224(19) 0.0012(16) 0.024(3) -0.002(2) C3 0.0222(19) 0.075(4) 0.036(2) 0.026(2) 0.0139(18) 0.027(2) C8 0.050(3) 0.038(2) 0.0232(19) 0.0078(17) 0.0087(19) 0.009(2) O2 0.0213(12) 0.0385(15) 0.0185(12) 0.0021(11) 0.0060(10) 0.0164(11) C6 0.0167(15) 0.035(2) 0.0268(18) 0.0009(15) 0.0068(13) 0.0111(14) O4 0.0181(12) 0.0356(15) 0.0256(13) 0.0028(11) 0.0088(10) 0.0138(11) O0AA 0.121(14) 0.23(3) 0.056(8) -0.005(13) 0.044(9) -0.030(18) O1AA 0.083(11) 0.29(3) 0.042(7) 0.029(13) 0.002(7) -0.079(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O6 89.39(10) . . ? O1 Ni1 N1 86.56(12) . . ? O1 Ni1 O5 87.95(13) . . ? O1 Ni1 O4 172.86(12) . 3_545 ? N1 Ni1 O6 175.61(11) . . ? N1 Ni1 O5 91.08(13) . . ? N1 Ni1 O4 90.01(12) . 3_545 ? O5 Ni1 O6 90.48(11) . . ? O2 Ni1 O6 90.70(10) 2 . ? O2 Ni1 O1 101.01(13) 2 . ? O2 Ni1 N1 88.40(12) 2 . ? O2 Ni1 O5 170.97(13) 2 . ? O2 Ni1 O4 85.14(13) 2 3_545 ? O4 Ni1 O6 94.19(10) 3_545 . ? O4 Ni1 O5 85.84(13) 3_545 . ? C1 S1 C4 92.12(19) . . ? Ni1 O6 Ni1 115.39(16) . 2 ? C5 O1 Ni1 135.9(2) . . ? C7 N1 Ni1 119.9(3) . . ? C11 N1 Ni1 122.4(3) . . ? C11 N1 C7 117.7(4) . . ? O1 C5 C1 115.3(3) . . ? O2 C5 O1 128.2(3) . . ? O2 C5 C1 116.5(3) . . ? C3 C4 S1 110.9(3) . . ? C3 C4 C6 128.5(4) . . ? C6 C4 S1 120.6(3) . . ? C1 C2 C3 113.1(4) . . ? C18 C13 C18 111.7(5) . 2_554 ? C5 C1 S1 120.8(3) . . ? C2 C1 S1 111.1(3) . . ? C2 C1 C5 128.1(3) . . ? C9 C10 C11 119.5(5) . . ? C10 C9 C18 121.6(5) . . ? C8 C9 C10 117.0(4) . . ? C8 C9 C18 121.3(5) . . ? N1 C7 C8 122.6(4) . . ? N1 C11 C10 122.9(4) . . ? C9 C18 C13 111.8(4) . . ? C4 C3 C2 112.7(4) . . ? C9 C8 C7 120.3(5) . . ? C5 O2 Ni1 135.0(2) . 2 ? O3 C6 C4 117.5(3) . . ? O3 C6 O4 125.3(4) . . ? O4 C6 C4 117.3(4) . . ? C6 O4 Ni1 122.5(2) . 3_455 ? 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 O6 2.1337(19) . ? Ni1 O1 2.015(3) . ? Ni1 N1 2.076(3) . ? Ni1 O5 2.091(3) . ? Ni1 O2 2.013(3) 2 ? Ni1 O4 2.086(3) 3_545 ? S1 C4 1.710(4) . ? S1 C1 1.705(4) . ? O1 C5 1.250(4) . ? N1 C7 1.339(5) . ? N1 C11 1.328(5) . ? O3 C6 1.251(5) . ? C5 C1 1.488(5) . ? C5 O2 1.242(4) . ? C4 C3 1.360(6) . ? C4 C6 1.485(5) . ? C2 C1 1.356(6) . ? C2 C3 1.402(6) . ? C13 C18 1.521(6) . ? C13 C18 1.521(6) 2_554 ? C10 C9 1.388(8) . ? C10 C11 1.389(6) . ? C9 C18 1.507(6) . ? C9 C8 1.378(8) . ? C7 C8 1.379(6) . ? C6 O4 1.267(5) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.685 2 0.315