#------------------------------------------------------------------------------ #$Date: 2020-04-06 01:15:10 +0300 (Mon, 06 Apr 2020) $ #$Revision: 250393 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/33/2243347.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243347 loop_ _publ_author_name 'Gavrish, Sergey P.' 'Shova, Sergiu' 'Cazacu, Maria' 'Dascalu, Mihaela' 'Lampeka, Yaroslaw D.' _publ_section_title ; Syntheses and crystal structures of the one-dimensional coordination polymers formed by [Ni(cyclam)]^2+^ cations and 1,3-bis(3-carboxypropyl)tetramethyldisiloxane anions in different degrees of deprotonation ; _journal_coeditor_code HB7892 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 446 _journal_page_last 451 _journal_paper_doi 10.1107/S2056989020002327 _journal_volume 76 _journal_year 2020 _chemical_formula_iupac '[Ni (C10 H25 O5 Si2) (C12 H24 N4)] Cl O4' _chemical_formula_moiety 'C22 H49 N4 Ni O5 Si2 +, Cl O4 -' _chemical_formula_sum 'C22 H49 Cl N4 Ni O9 Si2' _chemical_formula_weight 663.99 _chemical_name_systematic 'catena-Poly[[[(1,4,8,11-tetraazacyclotetradecane-\k^4^N^1^,N^4^,N^8^,N^11^)nickel(II)]-\m-4-({[(3-carboxypropyl)dimethylsilyl]oxy}dimethylsilyl)butanoato-\k^2^O:O'] perchlorate]' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _cell_angle_alpha 99.309(5) _cell_angle_beta 100.343(6) _cell_angle_gamma 99.232(6) _cell_formula_units_Z 2 _cell_length_a 9.3815(7) _cell_length_b 12.9009(8) _cell_length_c 14.7604(10) _cell_measurement_reflns_used 2033 _cell_measurement_temperature 200.00(10) _cell_measurement_theta_max 24.5610 _cell_measurement_theta_min 1.6600 _cell_volume 1700.9(2) _computing_cell_refinement ; CrysAlisPro (Agilent, 2014) ; _computing_data_collection ; CrysAlisPro (Agilent, 2014) ; _computing_data_reduction ; CrysAlisPro (Agilent, 2014) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 200.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1593 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Agilent Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_unetI/netI 0.1003 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 9606 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 1.947 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.88882 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Agilent, 2014) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.296 _exptl_crystal_description block _exptl_crystal_F_000 708 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.511 _refine_diff_density_min -0.436 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 367 _refine_ls_number_reflns 9606 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0498 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1096 _refine_ls_wR_factor_ref 0.1149 _reflns_number_gt 5769 _reflns_number_total 9606 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL II in P-1 #2 II.res created by SHELXL-2018/3 at 10:58:53 on 06-Jan-2020 REM reset to P-1 #2 CELL 0.71073 9.381518 12.900864 14.76035 99.3091 100.3429 99.2316 ZERR 2 0.000698 0.000762 0.000968 0.0052 0.0059 0.0056 LATT 1 SFAC C H Cl N Ni O Si UNIT 44 98 2 8 2 18 4 DFIX 0.4 0.01 O6X O6 EADP O6X O6 SADI 0.01 Si2 O6 Si2 O6X ISOR 0.01 0.02 C12 L.S. 10 PLAN 13 SIZE 0.3 0.35 0.45 CONF HTAB O2 O5 HTAB O2 O8 HTAB N1 O2 HTAB N1 O8 HTAB N2 O2 HTAB O5 O2 HTAB N3 O5 HTAB N4 O7 htab BOND MORE -1 BOND $H fmap 2 acta MERG 0 SHEL 99 0.84 OMIT 0 1 0 OMIT 0 -1 0 OMIT -4 -3 -1 OMIT 1 -1 0 OMIT 0 -2 1 OMIT -1 -2 -2 OMIT 0 -3 2 OMIT 0 -1 2 OMIT 0 2 -1 OMIT -2 1 4 OMIT 1 2 -1 OMIT -1 -2 1 OMIT 5 -1 -7 OMIT -1 1 0 OMIT -2 1 0 OMIT 5 -10 12 OMIT 3 -3 5 OMIT 1 -4 1 OMIT 6 -1 -3 OMIT 1 0 1 OMIT -3 3 -1 OMIT -4 -3 -2 OMIT 1 2 3 OMIT -1 4 -1 OMIT -4 5 0 OMIT -5 3 -1 OMIT -1 2 0 OMIT -2 3 2 OMIT 2 -1 -2 OMIT 0 1 -2 OMIT -6 3 3 OMIT 1 2 4 OMIT -4 -3 -3 OMIT 0 1 3 OMIT 1 2 5 OMIT -4 -3 -4 OMIT 1 -1 -3 OMIT 1 -2 0 OMIT 3 1 7 OMIT 1 2 6 OMIT 4 3 5 OMIT -1 1 3 OMIT 0 -1 -3 OMIT -1 -3 4 REM REM REM WGHT 0.045120 BASF 0.28820 FVAR 5.68998 NI1 5 0.000000 0.000000 0.000000 10.50000 0.02535 0.02015 = 0.02262 -0.00397 0.00723 -0.00206 SI1 7 -0.397692 -0.559866 -0.054689 11.00000 0.11337 0.02743 = 0.09673 0.01345 0.07741 0.00561 O1 6 -0.118406 -0.154229 -0.072718 11.00000 0.04035 0.02564 = 0.02058 -0.00650 0.01128 -0.00642 O2 6 -0.082560 -0.158333 -0.216477 11.00000 0.05087 0.02063 = 0.02970 -0.00135 0.02276 -0.00381 AFIX 3 H2C 2 -0.034950 -0.196653 -0.243367 10.50000 -1.50000 AFIX 0 O3 6 -0.553465 -0.508403 -0.033234 10.50000 0.08461 0.05080 = 0.06913 0.02016 0.05601 0.01957 N1 4 0.185904 -0.023582 -0.049888 11.00000 0.03335 0.03780 = 0.04145 -0.01725 0.01600 -0.00516 AFIX 13 H1 2 0.157126 -0.087684 -0.099864 11.00000 -1.20000 AFIX 0 N2 4 -0.080920 0.072455 -0.107496 11.00000 0.05240 0.02564 = 0.03116 -0.00436 -0.00068 0.00582 AFIX 13 H2 2 -0.128011 0.014955 -0.161639 11.00000 -1.20000 AFIX 0 C1 1 0.285822 -0.049412 0.029455 11.00000 0.02842 0.06546 = 0.08107 -0.03209 -0.00588 0.01903 AFIX 23 H1A 2 0.335337 0.015969 0.073702 11.00000 -1.20000 H1B 2 0.360480 -0.083840 0.006336 11.00000 -1.20000 AFIX 0 C2 1 -0.199233 0.121903 -0.077273 11.00000 0.07199 0.04829 = 0.05825 -0.00863 -0.02230 0.02439 AFIX 23 H2B 2 -0.263674 0.135605 -0.131369 11.00000 -1.20000 H2A 2 -0.156944 0.189771 -0.034619 11.00000 -1.20000 AFIX 0 C3 1 0.028208 0.144842 -0.138755 11.00000 0.11857 0.02704 = 0.03168 0.00313 0.00647 -0.01020 AFIX 23 H3A 2 0.071451 0.206181 -0.088446 11.00000 -1.20000 H3B 2 -0.020855 0.170724 -0.191801 11.00000 -1.20000 AFIX 0 C4 1 0.150052 0.090913 -0.167139 11.00000 0.10554 0.04485 = 0.03617 -0.00905 0.03867 -0.04123 AFIX 23 H4A 2 0.104405 0.025115 -0.211911 11.00000 -1.20000 H4B 2 0.205970 0.137198 -0.199462 11.00000 -1.20000 AFIX 0 C5 1 0.257044 0.064140 -0.089318 11.00000 0.05877 0.05967 = 0.05134 -0.01818 0.03586 -0.02337 AFIX 23 H5A 2 0.339987 0.043288 -0.113487 11.00000 -1.20000 H5B 2 0.294711 0.127196 -0.039965 11.00000 -1.20000 AFIX 0 C6 1 -0.133179 -0.203463 -0.153692 11.00000 0.02553 0.02494 = 0.02288 -0.00212 0.00807 0.00018 C7 1 -0.214571 -0.317130 -0.183220 11.00000 0.05312 0.02729 = 0.02725 -0.00436 0.01816 -0.00964 AFIX 23 H7A 2 -0.303379 -0.319448 -0.229384 11.00000 -1.20000 H7B 2 -0.153320 -0.358866 -0.214036 11.00000 -1.20000 AFIX 0 C8 1 -0.257952 -0.370028 -0.106556 11.00000 0.04814 0.02523 = 0.03305 -0.00158 0.01612 -0.00125 AFIX 23 H8A 2 -0.316658 -0.327704 -0.073869 11.00000 -1.20000 H8B 2 -0.169508 -0.371782 -0.061703 11.00000 -1.20000 AFIX 0 C9 1 -0.346349 -0.484197 -0.143055 11.00000 0.05575 0.02799 = 0.05304 -0.00372 0.02226 -0.01020 AFIX 23 H9A 2 -0.289182 -0.524186 -0.179202 11.00000 -1.20000 H9B 2 -0.436249 -0.480898 -0.185840 11.00000 -1.20000 AFIX 0 C10 1 -0.227455 -0.571019 0.025784 11.00000 0.27420 0.09629 = 0.09109 0.04745 -0.02989 -0.04222 AFIX 137 H10A 2 -0.191865 -0.505635 0.071407 11.00000 -1.50000 H10B 2 -0.153386 -0.583786 -0.009580 11.00000 -1.50000 H10C 2 -0.248872 -0.629417 0.057238 11.00000 -1.50000 AFIX 0 C11 1 -0.500272 -0.695705 -0.112402 11.00000 0.07455 0.04154 = 0.19213 0.03415 0.03876 -0.00616 AFIX 137 H11A 2 -0.442542 -0.730299 -0.150911 11.00000 -1.50000 H11B 2 -0.592187 -0.690955 -0.150829 11.00000 -1.50000 H11C 2 -0.519460 -0.736539 -0.065495 11.00000 -1.50000 AFIX 0 NI2 5 0.000000 -0.500000 -0.500000 10.50000 0.02849 0.02284 = 0.02923 -0.00669 0.01254 -0.00092 SI2 7 0.353164 0.046467 -0.526792 11.00000 0.03304 0.03963 = 0.05026 0.01558 0.00903 0.00469 O4 6 0.030516 -0.329678 -0.472844 11.00000 0.04207 0.02418 = 0.03338 -0.00614 0.02116 0.00312 O5 6 -0.083960 -0.289046 -0.357608 11.00000 0.05308 0.02630 = 0.03278 -0.00607 0.02583 -0.00135 AFIX 3 H5C 2 -0.095950 -0.235276 -0.324118 10.50000 -1.50000 AFIX 0 N3 4 -0.144201 -0.520637 -0.412896 11.00000 0.09860 0.02633 = 0.07318 -0.00249 0.06431 0.00677 AFIX 13 H3 2 -0.143842 -0.449452 -0.377416 11.00000 -1.20000 AFIX 0 N4 4 0.184425 -0.487012 -0.396827 11.00000 0.05559 0.04272 = 0.08016 -0.02735 -0.01860 0.01608 AFIX 13 H4 2 0.207815 -0.412879 -0.361974 11.00000 -1.20000 AFIX 0 C12 1 -0.293748 -0.558501 -0.477055 11.00000 0.04854 0.05650 = 0.16679 -0.03322 0.06582 -0.01041 AFIX 23 H12A 2 -0.370162 -0.545605 -0.442664 11.00000 -1.20000 H12B 2 -0.309077 -0.634809 -0.501474 11.00000 -1.20000 AFIX 0 C13 1 0.302046 -0.501232 -0.443476 11.00000 0.03949 0.06155 = 0.18815 -0.04809 -0.02712 0.01449 AFIX 23 H13A 2 0.295115 -0.576820 -0.467592 11.00000 -1.20000 H13B 2 0.395995 -0.474737 -0.399517 11.00000 -1.20000 AFIX 0 C14 1 0.163510 -0.558724 -0.325564 11.00000 0.16367 0.05544 = 0.08772 0.00408 -0.05497 0.04031 AFIX 23 H14A 2 0.151266 -0.632881 -0.356424 11.00000 -1.20000 H14B 2 0.251865 -0.542354 -0.276130 11.00000 -1.20000 AFIX 0 C15 1 0.031755 -0.545422 -0.282100 11.00000 0.31341 0.06739 = 0.04893 0.01891 0.04652 0.08375 AFIX 23 H15A 2 0.035328 -0.582999 -0.230129 11.00000 -1.20000 H15B 2 0.040102 -0.470013 -0.256570 11.00000 -1.20000 AFIX 0 C16 1 -0.114536 -0.585081 -0.347389 11.00000 0.23799 0.04489 = 0.08840 0.00115 0.12246 0.01231 AFIX 23 H16A 2 -0.117774 -0.657098 -0.380421 11.00000 -1.20000 H16B 2 -0.191132 -0.588632 -0.311103 11.00000 -1.20000 AFIX 0 C20 1 0.225464 0.003450 -0.450709 11.00000 0.03362 0.03484 = 0.04143 0.00216 0.01063 0.00319 AFIX 23 H20A 2 0.276718 0.028112 -0.385648 11.00000 -1.20000 H20B 2 0.142064 0.039091 -0.460546 11.00000 -1.20000 AFIX 0 C19 1 0.166421 -0.116395 -0.466221 11.00000 0.03780 0.03072 = 0.04055 0.00349 0.01700 0.00411 AFIX 23 H19A 2 0.108087 -0.140813 -0.529665 11.00000 -1.20000 H19B 2 0.249045 -0.153188 -0.460348 11.00000 -1.20000 AFIX 0 C18 1 0.072377 -0.146302 -0.397771 11.00000 0.03250 0.01820 = 0.03574 0.00060 0.01448 0.00281 AFIX 23 H18A 2 0.132997 -0.123812 -0.334828 11.00000 -1.20000 H18B 2 -0.006193 -0.105610 -0.401545 11.00000 -1.20000 AFIX 0 C17 1 0.003585 -0.262502 -0.410826 11.00000 0.02774 0.02825 = 0.02434 0.00044 0.00278 0.00460 C21 1 0.272512 -0.009358 -0.652906 11.00000 0.07922 0.08845 = 0.04499 0.01700 0.01100 0.01732 AFIX 137 H21A 2 0.180766 0.013540 -0.670484 11.00000 -1.50000 H21B 2 0.255162 -0.086153 -0.663382 11.00000 -1.50000 H21C 2 0.339876 0.015653 -0.690111 11.00000 -1.50000 AFIX 0 C22 1 0.399714 0.193924 -0.507886 11.00000 0.08194 0.04758 = 0.11588 0.02135 0.02252 -0.01247 AFIX 137 H22A 2 0.445438 0.222461 -0.443122 11.00000 -1.50000 H22B 2 0.311213 0.221370 -0.523912 11.00000 -1.50000 H22C 2 0.466709 0.214650 -0.546789 11.00000 -1.50000 AFIX 0 PART 1 O6X 6 0.492713 -0.013138 -0.496771 10.25000 0.03654 PART 0 PART 2 O6 6 0.510429 0.021193 -0.477240 10.25000 0.03654 PART 0 CL1 3 0.382920 -0.215897 -0.210546 11.00000 0.05707 0.05989 = 0.06948 -0.01109 -0.01509 0.01390 O7 6 0.394086 -0.288347 -0.282579 11.00000 0.13696 0.16255 = 0.20241 -0.14609 0.03716 -0.01937 O8 6 0.236203 -0.232328 -0.195471 11.00000 0.07653 0.15396 = 0.14367 0.05044 0.01689 0.02628 O9 6 0.411217 -0.110169 -0.227867 11.00000 0.17624 0.07920 = 0.15796 0.01624 -0.00457 -0.00607 O10 6 0.476753 -0.216114 -0.127114 11.00000 0.11714 0.14340 = 0.11463 -0.00589 -0.05041 0.03676 HKLF 5 REM II in P-1 #2 REM wR2 = 0.1149, GooF = S = 1.013, Restrained GooF = 1.021 for all data REM R1 = 0.0498 for 5769 Fo > 4sig(Fo) and 0.0852 for all 9606 data REM 367 parameters refined using 7 restraints END WGHT 0.0619 0.0000 REM Instructions for potential hydrogen bonds HTAB O2 O5 HTAB O2 O8 HTAB N1 O2 HTAB N1 O8 HTAB N2 O2 EQIV $2 -x, -y, -z HTAB C3 O1_$2 HTAB C5 O9 HTAB C5 O1_$2 HTAB C7 O5 HTAB O5 O2 HTAB N3 O5 HTAB N4 O7 EQIV $4 -x, -y-1, -z-1 HTAB C16 O4_$4 REM Highest difference peak 0.511, deepest hole -0.436, 1-sigma level 0.074 Q1 1 0.3932 -0.3325 -0.1950 11.00000 0.05 0.51 Q2 1 -0.0020 -0.5534 -0.3008 11.00000 0.05 0.48 Q3 1 -0.2419 -0.5696 -0.4128 11.00000 0.05 0.47 Q4 1 0.2579 -0.5248 -0.3464 11.00000 0.05 0.41 Q5 1 0.5346 -0.1781 -0.2193 11.00000 0.05 0.38 Q6 1 0.3488 -0.2295 -0.3054 11.00000 0.05 0.38 Q7 1 -0.1776 -0.5854 0.0163 11.00000 0.05 0.37 Q8 1 -0.3527 -0.5466 0.0289 11.00000 0.05 0.35 Q9 1 0.4202 0.0589 -0.4328 11.00000 0.05 0.33 Q10 1 0.4197 -0.2936 -0.3054 11.00000 0.05 0.33 Q11 1 -0.4501 -0.5191 -0.0269 11.00000 0.05 0.33 Q12 1 -0.3926 -0.5159 -0.1033 11.00000 0.05 0.32 Q13 1 0.0186 -0.4821 -0.4792 11.00000 0.05 0.32 REM The information below was added by Olex2. REM REM R1 = 0.0498 for 5769 Fo > 4sig(Fo) and 0.0852 for all 12223 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.51, deepest hole -0.44 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0852 REM R1_gt = 0.0498 REM wR_ref = 0.1149 REM GOOF = 1.013 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 12223 REM Reflections_gt = 5769 REM Parameters = n/a REM Hole = -0.44 REM Peak = 0.51 REM Flack = n/a ; _cod_data_source_file hb7892sup1.cif _cod_data_source_block II _cod_database_code 2243347 _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_min 0.724 _shelx_estimated_absorpt_t_max 0.803 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni1 0.000000 0.000000 0.000000 0.0241(2) Uani d 1 . . Si Si1 -0.3977(2) -0.55987(11) -0.05469(15) 0.0729(6) Uani d 1 . . O O1 -0.1184(3) -0.1542(2) -0.0727(2) 0.0310(8) Uani d 1 . . O O2 -0.0826(3) -0.1583(2) -0.2165(2) 0.0339(8) Uani d 1 . . H H2C -0.034950 -0.196653 -0.243367 0.051 Uiso d 0.5 . . O O3 -0.5535(8) -0.5084(6) -0.0332(5) 0.061(3) Uani d 0.5 . . N N1 0.1859(4) -0.0236(3) -0.0499(3) 0.0408(11) Uani d 1 . . H H1 0.157126 -0.087684 -0.099864 0.049 Uiso calc 1 . . N N2 -0.0809(4) 0.0725(3) -0.1075(3) 0.0390(11) Uani d 1 . . H H2 -0.128011 0.014955 -0.161639 0.047 Uiso calc 1 . . C C1 0.2858(6) -0.0494(5) 0.0295(4) 0.065(2) Uani d 1 . . H H1A 0.335337 0.015969 0.073702 0.078 Uiso calc 1 . . H H1B 0.360480 -0.083840 0.006336 0.078 Uiso calc 1 . . C C2 -0.1992(7) 0.1219(4) -0.0773(4) 0.0649(19) Uani d 1 . . H H2A -0.156944 0.189771 -0.034619 0.078 Uiso calc 1 . . H H2B -0.263674 0.135605 -0.131369 0.078 Uiso calc 1 . . C C3 0.0282(7) 0.1448(4) -0.1388(4) 0.0634(18) Uani d 1 . . H H3A 0.071451 0.206181 -0.088446 0.076 Uiso calc 1 . . H H3B -0.020855 0.170724 -0.191801 0.076 Uiso calc 1 . . C C4 0.1501(7) 0.0909(4) -0.1671(4) 0.068(2) Uani d 1 . . H H4A 0.104405 0.025115 -0.211911 0.081 Uiso calc 1 . . H H4B 0.205970 0.137198 -0.199462 0.081 Uiso calc 1 . . C C5 0.2570(6) 0.0641(4) -0.0893(4) 0.0608(18) Uani d 1 . . H H5A 0.339987 0.043288 -0.113487 0.073 Uiso calc 1 . . H H5B 0.294711 0.127196 -0.039965 0.073 Uiso calc 1 . . C C6 -0.1332(4) -0.2035(3) -0.1537(3) 0.0254(11) Uani d 1 . . C C7 -0.2146(5) -0.3171(3) -0.1832(3) 0.0378(13) Uani d 1 . . H H7A -0.303379 -0.319448 -0.229384 0.045 Uiso calc 1 . . H H7B -0.153320 -0.358866 -0.214036 0.045 Uiso calc 1 . . C C8 -0.2580(5) -0.3700(3) -0.1066(3) 0.0363(12) Uani d 1 . . H H8A -0.316658 -0.327704 -0.073869 0.044 Uiso calc 1 . . H H8B -0.169508 -0.371782 -0.061703 0.044 Uiso calc 1 . . C C9 -0.3463(5) -0.4842(3) -0.1431(3) 0.0477(14) Uani d 1 . . H H9A -0.289182 -0.524186 -0.179202 0.057 Uiso calc 1 . . H H9B -0.436249 -0.480898 -0.185840 0.057 Uiso calc 1 . . C C10 -0.2275(11) -0.5710(6) 0.0258(5) 0.168(4) Uani d 1 . . H H10A -0.191865 -0.505635 0.071407 0.252 Uiso calc 1 . . H H10B -0.153386 -0.583786 -0.009580 0.252 Uiso calc 1 . . H H10C -0.248872 -0.629417 0.057238 0.252 Uiso calc 1 . . C C11 -0.5003(7) -0.6957(4) -0.1124(5) 0.102(3) Uani d 1 . . H H11A -0.442542 -0.730299 -0.150911 0.153 Uiso calc 1 . . H H11B -0.592187 -0.690955 -0.150829 0.153 Uiso calc 1 . . H H11C -0.519460 -0.736539 -0.065495 0.153 Uiso calc 1 . . Ni Ni2 0.000000 -0.500000 -0.500000 0.0281(2) Uani d 1 . . Si Si2 0.35316(15) 0.04647(10) -0.52679(11) 0.0404(4) Uani d 1 . . O O4 0.0305(3) -0.3297(2) -0.47284(19) 0.0333(8) Uani d 1 . . O O5 -0.0840(3) -0.2890(2) -0.3576(2) 0.0376(9) Uani d 1 . . H H5C -0.095950 -0.235276 -0.324118 0.056 Uiso d 0.5 . . N N3 -0.1442(6) -0.5206(3) -0.4129(4) 0.0621(15) Uani d 1 . . H H3 -0.143842 -0.449452 -0.377416 0.075 Uiso calc 1 . . N N4 0.1844(5) -0.4870(3) -0.3968(4) 0.0675(16) Uani d 1 . . H H4 0.207815 -0.412879 -0.361974 0.081 Uiso calc 1 . . C C12 -0.2937(7) -0.5585(5) -0.4771(6) 0.094(3) Uani d 1 . . H H12A -0.370162 -0.545605 -0.442664 0.113 Uiso calc 1 . . H H12B -0.309077 -0.634809 -0.501474 0.113 Uiso calc 1 . . C C13 0.3020(7) -0.5012(5) -0.4435(7) 0.111(4) Uani d 1 . . H H13A 0.295115 -0.576820 -0.467592 0.133 Uiso calc 1 . . H H13B 0.395995 -0.474737 -0.399517 0.133 Uiso calc 1 . . C C14 0.1635(10) -0.5587(5) -0.3256(6) 0.112(3) Uani d 1 . . H H14A 0.151266 -0.632881 -0.356424 0.134 Uiso calc 1 . . H H14B 0.251865 -0.542354 -0.276130 0.134 Uiso calc 1 . . C C15 0.0318(15) -0.5454(6) -0.2821(5) 0.136(4) Uani d 1 . . H H15A 0.035328 -0.582999 -0.230129 0.163 Uiso calc 1 . . H H15B 0.040102 -0.470013 -0.256570 0.163 Uiso calc 1 . . C C16 -0.1145(11) -0.5851(5) -0.3474(6) 0.116(4) Uani d 1 . . H H16A -0.117774 -0.657098 -0.380421 0.139 Uiso calc 1 . . H H16B -0.191132 -0.588632 -0.311103 0.139 Uiso calc 1 . . C C17 0.0036(5) -0.2625(3) -0.4108(3) 0.0278(11) Uani d 1 . . C C18 0.0724(5) -0.1463(3) -0.3978(3) 0.0287(12) Uani d 1 . . H H18A 0.132997 -0.123812 -0.334828 0.034 Uiso calc 1 . . H H18B -0.006193 -0.105610 -0.401545 0.034 Uiso calc 1 . . C C19 0.1664(5) -0.1164(3) -0.4662(3) 0.0359(12) Uani d 1 . . H H19A 0.108087 -0.140813 -0.529665 0.043 Uiso calc 1 . . H H19B 0.249045 -0.153188 -0.460348 0.043 Uiso calc 1 . . C C20 0.2255(5) 0.0035(3) -0.4507(3) 0.0373(13) Uani d 1 . . H H20A 0.276718 0.028112 -0.385648 0.045 Uiso calc 1 . . H H20B 0.142064 0.039091 -0.460546 0.045 Uiso calc 1 . . C C21 0.2725(6) -0.0094(4) -0.6529(4) 0.0706(18) Uani d 1 . . H H21A 0.180766 0.013540 -0.670484 0.106 Uiso calc 1 . . H H21B 0.255162 -0.086153 -0.663382 0.106 Uiso calc 1 . . H H21C 0.339876 0.015653 -0.690111 0.106 Uiso calc 1 . . C C22 0.3997(6) 0.1939(4) -0.5079(5) 0.084(2) Uani d 1 . . H H22A 0.445438 0.222461 -0.443122 0.126 Uiso calc 1 . . H H22B 0.311213 0.221370 -0.523912 0.126 Uiso calc 1 . . H H22C 0.466709 0.214650 -0.546789 0.126 Uiso calc 1 . . O O6X 0.493(3) -0.013(5) -0.497(6) 0.037(3) Uiso d 0.25 A 1 O O6 0.510(3) 0.021(4) -0.4772(12) 0.037(3) Uiso d 0.25 A 2 Cl Cl1 0.38292(17) -0.21590(12) -0.21055(12) 0.0683(5) Uani d 1 . . O O7 0.3941(6) -0.2883(5) -0.2826(4) 0.194(3) Uani d 1 . . O O8 0.2362(5) -0.2323(4) -0.1955(4) 0.1227(19) Uani d 1 . . O O9 0.4112(6) -0.1102(4) -0.2279(4) 0.147(2) Uani d 1 . . O O10 0.4768(6) -0.2161(4) -0.1271(4) 0.137(2) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.0254(4) 0.0202(4) 0.0226(5) -0.0021(4) 0.0072(4) -0.0040(3) Si1 0.1134(15) 0.0274(8) 0.0967(15) 0.0056(9) 0.0774(14) 0.0135(8) O1 0.0404(19) 0.0256(16) 0.0206(19) -0.0064(14) 0.0113(15) -0.0065(14) O2 0.051(2) 0.0206(16) 0.030(2) -0.0038(14) 0.0228(17) -0.0013(14) O3 0.085(7) 0.051(4) 0.069(8) 0.020(5) 0.056(5) 0.020(5) N1 0.033(2) 0.038(2) 0.041(3) -0.005(2) 0.016(2) -0.017(2) N2 0.052(3) 0.026(2) 0.031(3) 0.006(2) -0.001(2) -0.0044(18) C1 0.028(3) 0.065(4) 0.081(5) 0.019(3) -0.006(3) -0.032(4) C2 0.072(4) 0.048(3) 0.058(4) 0.024(3) -0.022(4) -0.009(3) C3 0.119(5) 0.027(3) 0.032(3) -0.010(3) 0.006(4) 0.003(2) C4 0.106(5) 0.045(3) 0.036(4) -0.041(3) 0.039(4) -0.009(3) C5 0.059(4) 0.060(4) 0.051(4) -0.023(3) 0.036(3) -0.018(3) C6 0.026(3) 0.025(2) 0.023(3) 0.000(2) 0.008(2) -0.002(2) C7 0.053(3) 0.027(3) 0.027(3) -0.010(2) 0.018(3) -0.004(2) C8 0.048(3) 0.025(2) 0.033(3) -0.001(2) 0.016(3) -0.002(2) C9 0.056(3) 0.028(3) 0.053(4) -0.010(2) 0.022(3) -0.004(2) C10 0.274(12) 0.096(6) 0.091(7) -0.042(7) -0.030(7) 0.047(5) C11 0.075(5) 0.042(4) 0.192(8) -0.006(3) 0.039(5) 0.034(4) Ni2 0.0285(5) 0.0228(4) 0.0292(5) -0.0009(4) 0.0125(4) -0.0067(4) Si2 0.0330(8) 0.0396(8) 0.0503(10) 0.0047(7) 0.0090(7) 0.0156(7) O4 0.0421(19) 0.0242(16) 0.0334(19) 0.0031(14) 0.0212(16) -0.0061(14) O5 0.053(2) 0.0263(17) 0.033(2) -0.0013(15) 0.0258(18) -0.0061(14) N3 0.099(4) 0.026(2) 0.073(4) 0.007(3) 0.064(3) -0.002(3) N4 0.056(3) 0.043(3) 0.080(4) 0.016(3) -0.019(3) -0.027(3) C12 0.049(4) 0.056(4) 0.167(7) -0.010(3) 0.066(5) -0.033(4) C13 0.039(4) 0.062(5) 0.188(10) 0.014(4) -0.027(5) -0.048(5) C14 0.164(8) 0.055(4) 0.088(6) 0.040(5) -0.055(6) 0.004(4) C15 0.313(15) 0.067(5) 0.049(5) 0.084(8) 0.047(8) 0.019(4) C16 0.238(11) 0.045(4) 0.088(7) 0.012(6) 0.122(7) 0.001(4) C17 0.028(3) 0.028(2) 0.024(3) 0.005(2) 0.003(2) 0.000(2) C18 0.033(3) 0.018(2) 0.036(3) 0.003(2) 0.014(2) 0.001(2) C19 0.038(3) 0.031(3) 0.041(3) 0.004(2) 0.017(3) 0.003(2) C20 0.034(3) 0.035(3) 0.041(3) 0.003(2) 0.011(3) 0.002(2) C21 0.079(4) 0.088(4) 0.045(4) 0.017(4) 0.011(3) 0.017(3) C22 0.082(5) 0.048(3) 0.116(6) -0.012(3) 0.023(4) 0.021(4) Cl1 0.0571(10) 0.0599(10) 0.0695(12) 0.0139(8) -0.0151(10) -0.0111(9) O7 0.137(5) 0.163(5) 0.202(6) -0.019(4) 0.037(4) -0.146(5) O8 0.077(3) 0.154(5) 0.144(5) 0.026(3) 0.017(3) 0.050(4) O9 0.176(6) 0.079(4) 0.158(5) -0.006(4) -0.005(5) 0.016(3) O10 0.117(4) 0.143(4) 0.115(4) 0.037(3) -0.050(4) -0.006(4) 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' Cl Cl 0.1484 0.1585 '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' Si Si 0.0817 0.0704 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Ni1 O1 . 2 180.0 ? N1 Ni1 O1 2 . 88.17(12) ? N1 Ni1 O1 2 2 91.83(12) ? N1 Ni1 O1 . 2 88.17(12) ? N1 Ni1 O1 . . 91.83(12) ? N1 Ni1 N1 2 . 180.0 ? N1 Ni1 N2 2 . 85.82(17) ? N1 Ni1 N2 . 2 85.82(17) ? N1 Ni1 N2 2 2 94.18(17) ? N1 Ni1 N2 . . 94.18(17) ? N2 Ni1 O1 . 2 87.38(12) ? N2 Ni1 O1 2 . 87.38(12) ? N2 Ni1 O1 . . 92.62(12) ? N2 Ni1 O1 2 2 92.62(12) ? N2 Ni1 N2 . 2 180.0 ? O3 Si1 O3 2_445 . 42.6(4) ? O3 Si1 C9 2_445 . 115.6(3) ? O3 Si1 C9 . . 100.2(3) ? O3 Si1 C10 . . 131.5(4) ? O3 Si1 C10 2_445 . 89.4(4) ? O3 Si1 C11 2_445 . 121.3(4) ? O3 Si1 C11 . . 95.7(3) ? C9 Si1 C10 . . 109.0(3) ? C9 Si1 C11 . . 110.1(3) ? C11 Si1 C10 . . 108.8(3) ? C6 O1 Ni1 . . 132.9(3) ? C6 O2 H2C . . 109.8 ? Si1 O3 Si1 2_445 . 137.4(4) ? O3 O3 Si1 2_445 . 63.0(6) ? O3 O3 Si1 2_445 2_445 74.4(7) ? Ni1 N1 H1 . . 107.4 ? C1 N1 Ni1 . . 105.0(3) ? C1 N1 H1 . . 107.4 ? C5 N1 Ni1 . . 116.2(3) ? C5 N1 H1 . . 107.4 ? C5 N1 C1 . . 113.1(4) ? Ni1 N2 H2 . . 106.7 ? C2 N2 Ni1 . . 105.7(3) ? C2 N2 H2 . . 106.7 ? C3 N2 Ni1 . . 116.1(3) ? C3 N2 H2 . . 106.7 ? C3 N2 C2 . . 114.2(4) ? N1 C1 H1A . . 109.7 ? N1 C1 H1B . . 109.7 ? N1 C1 C2 . 2 109.7(4) ? H1A C1 H1B . . 108.2 ? C2 C1 H1A 2 . 109.7 ? C2 C1 H1B 2 . 109.7 ? N2 C2 C1 . 2 109.8(4) ? N2 C2 H2B . . 109.7 ? N2 C2 H2A . . 109.7 ? C1 C2 H2B 2 . 109.7 ? C1 C2 H2A 2 . 109.7 ? H2B C2 H2A . . 108.2 ? N2 C3 H3A . . 109.1 ? N2 C3 H3B . . 109.1 ? N2 C3 C4 . . 112.3(4) ? H3A C3 H3B . . 107.9 ? C4 C3 H3A . . 109.1 ? C4 C3 H3B . . 109.1 ? C3 C4 H4A . . 108.1 ? C3 C4 H4B . . 108.1 ? H4A C4 H4B . . 107.3 ? C5 C4 C3 . . 116.7(4) ? C5 C4 H4A . . 108.1 ? C5 C4 H4B . . 108.1 ? N1 C5 C4 . . 111.4(4) ? N1 C5 H5A . . 109.4 ? N1 C5 H5B . . 109.4 ? C4 C5 H5A . . 109.4 ? C4 C5 H5B . . 109.4 ? H5A C5 H5B . . 108.0 ? O1 C6 O2 . . 121.4(4) ? O1 C6 C7 . . 120.8(4) ? O2 C6 C7 . . 117.7(4) ? C6 C7 H7A . . 108.3 ? C6 C7 H7B . . 108.3 ? H7A C7 H7B . . 107.4 ? C8 C7 C6 . . 116.0(4) ? C8 C7 H7A . . 108.3 ? C8 C7 H7B . . 108.3 ? C7 C8 H8A . . 109.0 ? C7 C8 H8B . . 109.0 ? C7 C8 C9 . . 112.8(4) ? H8A C8 H8B . . 107.8 ? C9 C8 H8A . . 109.0 ? C9 C8 H8B . . 109.0 ? Si1 C9 H9A . . 108.1 ? Si1 C9 H9B . . 108.1 ? C8 C9 Si1 . . 116.8(3) ? C8 C9 H9A . . 108.1 ? C8 C9 H9B . . 108.1 ? H9A C9 H9B . . 107.3 ? Si1 C10 H10A . . 109.5 ? Si1 C10 H10B . . 109.5 ? Si1 C10 H10C . . 109.5 ? H10A C10 H10B . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? Si1 C11 H11A . . 109.5 ? Si1 C11 H11B . . 109.5 ? Si1 C11 H11C . . 109.5 ? H11A C11 H11B . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? O4 Ni2 O4 . 2_544 180.00(3) ? N3 Ni2 O4 2_544 2_544 94.96(13) ? N3 Ni2 O4 . . 94.96(13) ? N3 Ni2 O4 2_544 . 85.04(13) ? N3 Ni2 O4 . 2_544 85.04(13) ? N3 Ni2 N3 2_544 . 180.0 ? N3 Ni2 N4 2_544 2_544 94.3(2) ? N3 Ni2 N4 . . 94.3(2) ? N3 Ni2 N4 . 2_544 85.7(2) ? N3 Ni2 N4 2_544 . 85.7(2) ? N4 Ni2 O4 . 2_544 91.33(14) ? N4 Ni2 O4 . . 88.67(14) ? N4 Ni2 O4 2_544 . 91.33(14) ? N4 Ni2 O4 2_544 2_544 88.67(14) ? N4 Ni2 N4 . 2_544 180.0 ? C21 Si2 C20 . . 111.6(2) ? C22 Si2 C20 . . 110.6(2) ? C22 Si2 C21 . . 109.6(3) ? O6X Si2 C20 2_654 . 113.4(14) ? O6X Si2 C20 . . 102.5(13) ? O6X Si2 C21 . . 107(3) ? O6X Si2 C21 2_654 . 107(3) ? O6X Si2 C22 . . 116(2) ? O6X Si2 C22 2_654 . 104(2) ? O6X Si2 O6X 2_654 . 13(3) ? O6X Si2 O6 . 2_654 13(3) ? O6X Si2 O6 2_654 2_654 17(2) ? O6 Si2 C20 2_654 . 111.2(17) ? O6 Si2 C20 . . 103.5(15) ? O6 Si2 C21 . . 120.4(6) ? O6 Si2 C21 2_654 . 94.3(5) ? O6 Si2 C22 . . 100.3(19) ? O6 Si2 C22 2_654 . 118.5(19) ? O6 Si2 O6 . 2_654 26.9(17) ? C17 O4 Ni2 . . 133.8(3) ? C17 O5 H5C . . 109.9 ? Ni2 N3 H3 . . 106.9 ? C12 N3 Ni2 . . 105.1(4) ? C12 N3 H3 . . 106.9 ? C16 N3 Ni2 . . 117.3(4) ? C16 N3 H3 . . 106.9 ? C16 N3 C12 . . 113.2(6) ? Ni2 N4 H4 . . 106.8 ? C13 N4 Ni2 . . 106.5(4) ? C13 N4 H4 . . 106.8 ? C13 N4 C14 . . 115.0(6) ? C14 N4 Ni2 . . 114.4(4) ? C14 N4 H4 . . 106.8 ? N3 C12 H12A . . 109.9 ? N3 C12 H12B . . 109.9 ? N3 C12 C13 . 2_544 108.8(5) ? H12A C12 H12B . . 108.3 ? C13 C12 H12A 2_544 . 109.9 ? C13 C12 H12B 2_544 . 109.9 ? N4 C13 C12 . 2_544 109.6(6) ? N4 C13 H13A . . 109.8 ? N4 C13 H13B . . 109.8 ? C12 C13 H13A 2_544 . 109.8 ? C12 C13 H13B 2_544 . 109.8 ? H13A C13 H13B . . 108.2 ? N4 C14 H14A . . 109.0 ? N4 C14 H14B . . 109.0 ? H14A C14 H14B . . 107.8 ? C15 C14 N4 . . 113.0(6) ? C15 C14 H14A . . 109.0 ? C15 C14 H14B . . 109.0 ? C14 C15 H15A . . 108.5 ? C14 C15 H15B . . 108.5 ? H15A C15 H15B . . 107.5 ? C16 C15 C14 . . 115.0(6) ? C16 C15 H15A . . 108.5 ? C16 C15 H15B . . 108.5 ? N3 C16 C15 . . 113.1(7) ? N3 C16 H16A . . 109.0 ? N3 C16 H16B . . 109.0 ? C15 C16 H16A . . 109.0 ? C15 C16 H16B . . 109.0 ? H16A C16 H16B . . 107.8 ? Si2 C20 H20A . . 108.3 ? Si2 C20 H20B . . 108.3 ? H20A C20 H20B . . 107.4 ? C19 C20 Si2 . . 115.9(3) ? C19 C20 H20A . . 108.3 ? C19 C20 H20B . . 108.3 ? C20 C19 H19A . . 109.0 ? C20 C19 H19B . . 109.0 ? H19A C19 H19B . . 107.8 ? C18 C19 C20 . . 113.1(3) ? C18 C19 H19A . . 109.0 ? C18 C19 H19B . . 109.0 ? C19 C18 H18A . . 108.1 ? C19 C18 H18B . . 108.1 ? H18A C18 H18B . . 107.3 ? C17 C18 C19 . . 116.7(3) ? C17 C18 H18A . . 108.1 ? C17 C18 H18B . . 108.1 ? O4 C17 O5 . . 121.9(4) ? O4 C17 C18 . . 120.1(4) ? O5 C17 C18 . . 118.0(3) ? Si2 C21 H21A . . 109.5 ? Si2 C21 H21B . . 109.5 ? Si2 C21 H21C . . 109.5 ? H21A C21 H21B . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? Si2 C22 H22A . . 109.5 ? Si2 C22 H22B . . 109.5 ? Si2 C22 H22C . . 109.5 ? H22A C22 H22B . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? Si2 O6X Si2 2_654 . 167(3) ? O6X O6X Si2 2_654 2_654 96(6) ? O6X O6X Si2 2_654 . 71(6) ? Si2 O6 Si2 . 2_654 153.1(17) ? O6 O6 Si2 2_654 . 78(2) ? O7 Cl1 O8 . . 110.3(3) ? O7 Cl1 O9 . . 112.0(4) ? O7 Cl1 O10 . . 114.2(4) ? O9 Cl1 O8 . . 105.3(3) ? O10 Cl1 O8 . . 107.7(4) ? O10 Cl1 O9 . . 106.8(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 O1 . 2.125(2) ? Ni1 O1 2 2.125(2) ? Ni1 N1 2 2.058(3) ? Ni1 N1 . 2.058(3) ? Ni1 N2 2 2.060(4) ? Ni1 N2 . 2.060(4) ? Si1 O3 . 1.757(8) ? Si1 O3 2_445 1.626(7) ? Si1 C9 . 1.837(5) ? Si1 C10 . 1.852(9) ? Si1 C11 . 1.845(5) ? O1 C6 . 1.232(4) ? O2 H2C . 0.8200 ? O2 C6 . 1.291(5) ? O3 O3 2_445 1.234(13) ? N1 H1 . 0.9800 ? N1 C1 . 1.481(6) ? N1 C5 . 1.475(6) ? N2 H2 . 0.9800 ? N2 C2 . 1.467(6) ? N2 C3 . 1.461(6) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C1 C2 2 1.486(7) ? C2 H2B . 0.9700 ? C2 H2A . 0.9700 ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C3 C4 . 1.516(7) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C4 C5 . 1.507(7) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 C7 . 1.496(5) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C7 C8 . 1.496(6) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C8 C9 . 1.529(5) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 H10A . 0.9600 ? C10 H10B . 0.9600 ? C10 H10C . 0.9600 ? C11 H11A . 0.9600 ? C11 H11B . 0.9600 ? C11 H11C . 0.9600 ? Ni2 O4 2_544 2.131(2) ? Ni2 O4 . 2.131(2) ? Ni2 N3 2_544 2.043(4) ? Ni2 N3 . 2.043(4) ? Ni2 N4 . 2.054(4) ? Ni2 N4 2_544 2.054(4) ? Si2 C20 . 1.864(5) ? Si2 C21 . 1.855(5) ? Si2 C22 . 1.845(5) ? Si2 O6X 2_654 1.570(19) ? Si2 O6X . 1.651(19) ? Si2 O6 2_654 1.66(2) ? Si2 O6 . 1.632(16) ? O4 C17 . 1.245(4) ? O5 H5C . 0.8199 ? O5 C17 . 1.280(5) ? N3 H3 . 0.9800 ? N3 C12 . 1.502(8) ? N3 C16 . 1.393(9) ? N4 H4 . 0.9800 ? N4 C13 . 1.422(8) ? N4 C14 . 1.527(9) ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ? C12 C13 2_544 1.502(10) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C14 C15 . 1.512(11) ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C15 C16 . 1.488(11) ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? C20 H20A . 0.9700 ? C20 H20B . 0.9700 ? C20 C19 . 1.521(5) ? C19 H19A . 0.9700 ? C19 H19B . 0.9700 ? C19 C18 . 1.512(6) ? C18 H18A . 0.9700 ? C18 H18B . 0.9700 ? C18 C17 . 1.501(5) ? C21 H21A . 0.9600 ? C21 H21B . 0.9600 ? C21 H21C . 0.9600 ? C22 H22A . 0.9600 ? C22 H22B . 0.9600 ? C22 H22C . 0.9600 ? O6X O6X 2_654 0.38(7) ? O6 O6 2_654 0.77(5) ? Cl1 O7 . 1.329(4) ? Cl1 O8 . 1.421(5) ? Cl1 O9 . 1.420(5) ? Cl1 O10 . 1.380(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O2 . 0.98 2.51 3.225(5) 130 yes N1 H1 O8 . 0.98 2.45 3.315(6) 147 yes N2 H2 O2 . 0.98 2.38 3.143(4) 134 yes N3 H3 O5 . 0.98 2.01 2.901(5) 150 yes N4 H4 O7 . 0.98 2.18 3.012(6) 142 yes O2 H2C O5 . 0.82 1.84 2.456(4) 131 yes O2 H2C O8 . 0.82 2.65 3.260(5) 133 yes O5 H5C O2 . 0.82 1.70 2.456(4) 151 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ni1 O1 C6 O2 . . . . -7.2(6) ? Ni1 O1 C6 C7 . . . . 174.5(3) ? Ni1 N1 C1 C2 . . . 2 40.9(4) ? Ni1 N1 C5 C4 . . . . -56.2(5) ? Ni1 N2 C2 C1 . . . 2 -39.8(4) ? Ni1 N2 C3 C4 . . . . 55.3(5) ? O1 C6 C7 C8 . . . . -7.7(6) ? O2 C6 C7 C8 . . . . 174.0(4) ? O3 Si1 O3 Si1 2_445 . . 2_445 -0.001(2) ? O3 Si1 C9 C8 . . . . 81.0(4) ? O3 Si1 C9 C8 2_445 . . . 39.0(5) ? N2 C3 C4 C5 . . . . -70.0(6) ? C1 N1 C5 C4 . . . . -177.7(4) ? C2 N2 C3 C4 . . . . 178.7(4) ? C3 N2 C2 C1 . . . 2 -168.7(4) ? C3 C4 C5 N1 . . . . 70.1(5) ? C5 N1 C1 C2 . . . 2 168.6(4) ? C6 C7 C8 C9 . . . . 177.5(4) ? C7 C8 C9 Si1 . . . . 176.9(4) ? C9 Si1 O3 Si1 . . . 2_445 -116.9(7) ? C9 Si1 O3 O3 . . . 2_445 -116.9(7) ? C10 Si1 O3 Si1 . . . 2_445 10.0(10) ? C10 Si1 O3 O3 . . . 2_445 10.0(10) ? C10 Si1 C9 C8 . . . . -59.7(5) ? C11 Si1 O3 Si1 . . . 2_445 131.5(8) ? C11 Si1 O3 O3 . . . 2_445 131.5(8) ? C11 Si1 C9 C8 . . . . -179.0(4) ? Ni2 O4 C17 O5 . . . . -16.3(6) ? Ni2 O4 C17 C18 . . . . 164.8(3) ? Ni2 N3 C12 C13 . . . 2_544 -39.0(6) ? Ni2 N3 C16 C15 . . . . 59.1(7) ? Ni2 N4 C13 C12 . . . 2_544 42.1(6) ? Ni2 N4 C14 C15 . . . . -52.9(7) ? Si2 C20 C19 C18 . . . . 176.0(3) ? N4 C14 C15 C16 . . . . 68.4(9) ? C12 N3 C16 C15 . . . . -178.2(6) ? C13 N4 C14 C15 . . . . -176.6(6) ? C14 N4 C13 C12 . . . 2_544 169.9(5) ? C14 C15 C16 N3 . . . . -71.7(8) ? C16 N3 C12 C13 . . . 2_544 -168.2(5) ? C20 Si2 O6X Si2 . . . 2_654 -15E1(3) ? C20 Si2 O6X O6X . . . 2_654 -15E1(3) ? C20 Si2 O6 Si2 . . . 2_654 110(7) ? C20 Si2 O6 O6 . . . 2_654 110(7) ? C20 C19 C18 C17 . . . . 177.2(4) ? C19 C18 C17 O4 . . . . 3.3(6) ? C19 C18 C17 O5 . . . . -175.7(4) ? C21 Si2 C20 C19 . . . . 52.0(4) ? C21 Si2 O6X Si2 . . . 2_654 10E1(3) ? C21 Si2 O6X O6X . . . 2_654 10E1(3) ? C21 Si2 O6 Si2 . . . 2_654 -15(9) ? C21 Si2 O6 O6 . . . 2_654 -15(9) ? C22 Si2 C20 C19 . . . . 174.3(4) ? C22 Si2 O6X Si2 . . . 2_654 -3E1(3) ? C22 Si2 O6X O6X . . . 2_654 -3E1(3) ? C22 Si2 O6 Si2 . . . 2_654 -135(8) ? C22 Si2 O6 O6 . . . 2_654 -135(8) ? O6X Si2 C20 C19 2_654 . . . -70(4) ? O6X Si2 C20 C19 . . . . -62(3) ? O6X Si2 O6X Si2 2_654 . . 2_654 -0.01(14) ? O6 Si2 C20 C19 2_654 . . . -51.9(12) ? O6 Si2 C20 C19 . . . . -79.0(15) ? O6 Si2 O6 Si2 2_654 . . 2_654 0.006(14) ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.7118(8) 2 0.2882(8) _cod_database_fobs_code 2243347