#------------------------------------------------------------------------------ #$Date: 2024-04-18 01:11:35 +0300 (Thu, 18 Apr 2024) $ #$Revision: 291261 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/14/1571459.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_1571459 loop_ _publ_author_name 'Sikdar, Nivedita' 'Laha, Subhajit' 'Jena, Rohan' 'Dey, Anupam' 'Rahimi, Faruk Ahamed' 'Maji, Tapas Kumar' _publ_section_title ; An Adsorbate Biased Dynamic 3D Porous Framework for Inverse CO2 Sieving over C2H2 ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D3SC06611H _journal_year 2024 _chemical_formula_sum 'C36 H18 Ni4 O19' _chemical_formula_weight 989.34 _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 geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-03-27 deposited with the CCDC. 2024-04-09 downloaded from the CCDC. ; _cell_angle_alpha 98.9030(10) _cell_angle_beta 96.0020(10) _cell_angle_gamma 101.5900(10) _cell_formula_units_Z 2 _cell_length_a 7.07440(10) _cell_length_b 13.6038(3) _cell_length_c 20.6602(4) _cell_measurement_reflns_used 9916 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 32.42 _cell_measurement_theta_min 2.76 _cell_volume 1905.31(6) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 114743 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.191 _diffrn_reflns_theta_min 1.999 _diffrn_source Mo _exptl_absorpt_coefficient_mu 2.028 _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.724 _exptl_crystal_description Block _exptl_crystal_F_000 996 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.065 _exptl_crystal_size_min 0.052 _refine_diff_density_max 1.715 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.242 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 534 _refine_ls_number_reflns 14547 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0410 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.1728P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1087 _refine_ls_wR_factor_ref 0.1236 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10196 _reflns_number_total 14547 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3sc06611h2.cif _cod_data_source_block Ni_NDC _cod_database_code 1571459 _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_res_file ; TITL C:\Users\91700\Desktop\Ni_NDC_3\mo_Ni_NDC_3_0m_a.res in P-1 C:\Users\91700\Desktop\Ni_NDC_3\mo_Ni_NDC_3_0m_a.res created by SHELXL-2018/3 at 11:06:08 on 27-Mar-2024 CELL 0.71073 7.0744 13.6038 20.6602 98.903 96.002 101.590 ZERR 2.0000 0.0001 0.0003 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H NI O UNIT 72 36 8 38 BOND ACTA FMAP 2 1 53 PLAN 20 0 0 LIST 4 1 TEMP 25 L.S. 10 WGHT 0.061300 0.172800 SWAT 323.759247 29.8745 FVAR 0.41190 NI1 3 -0.037800 0.644415 0.788762 11.00000 0.01347 0.01201 = 0.01387 0.00394 0.00263 0.00326 NI2 3 0.431895 0.653247 0.786737 11.00000 0.01433 0.01244 = 0.01374 0.00426 0.00441 0.00429 NI3 3 0.178554 0.438849 0.737150 11.00000 0.01428 0.01199 = 0.01523 0.00336 0.00433 0.00426 NI4 3 0.641992 0.444756 0.732762 11.00000 0.01300 0.01214 = 0.01439 0.00291 0.00208 0.00333 O1 4 0.062762 0.780536 0.761524 11.00000 0.01829 0.01546 = 0.03209 0.01008 0.00405 0.00309 O2 4 0.387133 0.798804 0.787117 11.00000 0.01957 0.01392 = 0.03374 0.00790 0.00400 0.00540 O3 4 0.217248 1.294330 0.736118 11.00000 0.01955 0.01434 = 0.03379 0.00583 0.00502 0.00556 O4 4 0.541316 1.307969 0.759396 11.00000 0.01943 0.01535 = 0.03130 0.00855 0.00335 0.00220 O5 4 0.103424 0.688969 0.881442 11.00000 0.02438 0.03088 = 0.01521 0.00310 0.00299 0.00893 O6 4 0.397028 0.650370 0.883139 11.00000 0.02386 0.02937 = 0.01474 0.00684 0.00583 0.00848 O7 4 -0.089531 0.568521 1.171826 11.00000 0.02054 0.02664 = 0.02000 0.01155 0.00843 0.00958 O8 4 0.162687 0.492912 1.182083 11.00000 0.01660 0.01624 = 0.01511 0.00613 0.00114 0.00442 O9 4 0.202834 0.428380 0.637582 11.00000 0.02440 0.03263 = 0.01441 0.00325 0.00450 0.01127 O10 4 0.502718 0.398198 0.640967 11.00000 0.02139 0.03296 = 0.01377 0.00129 0.00171 0.00616 O11 4 0.231993 0.416853 0.298605 11.00000 0.01703 0.01819 = 0.01447 0.00580 0.00088 0.00445 O12 4 0.481206 0.338190 0.303813 11.00000 0.02614 0.03047 = 0.01798 0.01174 0.01006 0.01451 O13 4 0.156027 0.585333 0.741943 11.00000 0.01572 0.01204 = 0.01573 0.00379 0.00336 0.00433 O14 4 -0.261669 0.711933 0.829457 11.00000 0.01821 0.02406 = 0.02197 -0.00013 0.00301 0.00653 O15 4 0.452665 0.505967 0.779677 11.00000 0.01381 0.01288 = 0.01515 0.00326 0.00232 0.00491 O16 4 0.870715 0.376908 0.693376 11.00000 0.01788 0.02421 = 0.02096 0.00074 0.00318 0.00610 O17 4 -0.216081 0.897495 0.800805 11.00000 0.04559 0.03160 = 0.12119 0.00234 0.02262 0.00653 O18 4 -0.258537 0.737102 0.965621 11.00000 0.18630 0.62890 = 0.43763 0.00701 0.05059 -0.01137 O19 4 0.759112 0.178170 0.689742 11.00000 0.06370 0.04545 = 0.09826 0.01245 0.03751 0.02033 C1 1 0.237860 0.830405 0.770153 11.00000 0.01869 0.01319 = 0.02063 0.00517 0.00555 0.00444 C2 1 0.269784 0.939742 0.760648 11.00000 0.01971 0.01042 = 0.02908 0.00645 0.00494 0.00333 C3 1 0.391034 1.013097 0.808541 11.00000 0.02808 0.01668 = 0.03156 0.00911 -0.00256 0.00445 AFIX 43 H3 2 0.453681 0.993704 0.844767 11.00000 -1.20000 AFIX 0 C4 1 0.422295 1.116776 0.803903 11.00000 0.02490 0.01335 = 0.03128 0.00474 -0.00237 0.00193 AFIX 43 H4 2 0.504599 1.165234 0.837035 11.00000 -1.20000 AFIX 0 C5 1 0.332529 1.146893 0.751010 11.00000 0.01921 0.01251 = 0.02669 0.00565 0.00653 0.00328 C6 1 0.210057 1.073325 0.698649 11.00000 0.02015 0.01284 = 0.02150 0.00456 0.00311 0.00328 C7 1 0.177322 0.967754 0.703861 11.00000 0.02120 0.01501 = 0.02310 0.00581 0.00461 0.00446 C8 1 0.059309 0.895454 0.650409 11.00000 0.03434 0.01660 = 0.02883 0.00440 0.00201 -0.00144 AFIX 43 H8 2 0.034986 0.826505 0.653003 11.00000 -1.20000 AFIX 0 C9 1 -0.018919 0.925259 0.595402 11.00000 0.04428 0.02758 = 0.02949 0.00284 -0.00399 -0.00196 AFIX 43 H9 2 -0.094930 0.876529 0.560995 11.00000 -1.20000 AFIX 0 C10 1 0.014344 1.028525 0.590377 11.00000 0.04894 0.03146 = 0.02659 0.00895 -0.00552 0.00724 AFIX 43 H10 2 -0.039805 1.048011 0.552711 11.00000 -1.20000 AFIX 0 C11 1 0.126155 1.101030 0.640598 11.00000 0.03712 0.02120 = 0.02524 0.00961 0.00302 0.00677 AFIX 43 H11 2 0.147444 1.169418 0.636622 11.00000 -1.20000 AFIX 0 C12 1 0.366182 1.259727 0.748851 11.00000 0.02077 0.01187 = 0.01935 0.00504 0.00687 0.00429 C13 1 0.251690 0.666698 0.909570 11.00000 0.02284 0.01715 = 0.01268 0.00320 0.00328 0.00309 C14 1 0.243264 0.651998 0.980124 11.00000 0.02141 0.02031 = 0.01375 0.00650 0.00538 0.00173 C15 1 0.278446 0.563543 0.996443 11.00000 0.02937 0.03065 = 0.01885 0.00864 0.01065 0.01557 AFIX 43 H15 2 0.334478 0.521761 0.967842 11.00000 -1.20000 AFIX 0 C16 1 0.230548 0.534850 1.056376 11.00000 0.02875 0.02465 = 0.02077 0.01170 0.00960 0.01370 AFIX 43 H16 2 0.259051 0.475297 1.067609 11.00000 -1.20000 AFIX 0 C17 1 0.142027 0.593936 1.098522 11.00000 0.01959 0.01809 = 0.01329 0.00607 0.00403 0.00360 C18 1 0.119019 0.691350 1.085674 11.00000 0.02396 0.01805 = 0.01503 0.00509 0.00533 0.00548 C19 1 0.174937 0.721675 1.026032 11.00000 0.02980 0.01830 = 0.01592 0.00534 0.00650 0.00407 C20 1 0.165101 0.820826 1.015416 11.00000 0.07202 0.02213 = 0.02650 0.01286 0.02104 0.01307 AFIX 43 H20 2 0.200536 0.841174 0.976615 11.00000 -1.20000 AFIX 0 C21 1 0.105084 0.886789 1.060642 11.00000 0.10095 0.02335 = 0.03675 0.01270 0.02655 0.02591 AFIX 43 H21 2 0.104327 0.952461 1.053298 11.00000 -1.20000 AFIX 0 C22 1 0.043877 0.856713 1.118646 11.00000 0.07850 0.02582 = 0.03732 0.00811 0.02973 0.02232 AFIX 43 H22 2 -0.000403 0.901873 1.148867 11.00000 -1.20000 AFIX 0 C23 1 0.049375 0.761745 1.130574 11.00000 0.04906 0.02348 = 0.02483 0.00676 0.01824 0.01289 AFIX 43 H23 2 0.006870 0.742348 1.168768 11.00000 -1.20000 AFIX 0 C24 1 0.065327 0.550461 1.154998 11.00000 0.01672 0.01417 = 0.01132 0.00274 0.00230 0.00150 C25 1 0.341459 0.402570 0.611053 11.00000 0.02177 0.01571 = 0.01227 0.00386 0.00205 0.00176 C26 1 0.320073 0.378508 0.536578 11.00000 0.01871 0.02119 = 0.01412 0.00346 0.00484 0.00427 C27 1 0.232997 0.438746 0.502011 11.00000 0.02856 0.02942 = 0.01659 0.00569 0.00607 0.01718 AFIX 43 H27 2 0.170950 0.485418 0.523897 11.00000 -1.20000 AFIX 0 C28 1 0.236110 0.430941 0.433106 11.00000 0.02888 0.02869 = 0.01666 0.00874 0.00573 0.01584 AFIX 43 H28 2 0.176656 0.473011 0.410314 11.00000 -1.20000 AFIX 0 C29 1 0.325435 0.362287 0.399199 11.00000 0.01836 0.01912 = 0.01344 0.00617 0.00370 0.00448 C30 1 0.405963 0.292240 0.432867 11.00000 0.02196 0.01983 = 0.01458 0.00544 0.00514 0.00681 C31 1 0.401597 0.300730 0.502710 11.00000 0.02297 0.01868 = 0.01426 0.00585 0.00368 0.00597 C32 1 0.472002 0.227982 0.535635 11.00000 0.04609 0.02883 = 0.01932 0.00913 0.00553 0.01738 AFIX 43 H32 2 0.471297 0.232978 0.581011 11.00000 -1.20000 AFIX 0 C33 1 0.540215 0.151395 0.502148 11.00000 0.06539 0.04203 = 0.03158 0.01710 0.01207 0.03522 AFIX 43 H33 2 0.584189 0.104291 0.524619 11.00000 -1.20000 AFIX 0 C34 1 0.544574 0.143105 0.434096 11.00000 0.07111 0.03830 = 0.03310 0.01526 0.02345 0.03761 AFIX 43 H34 2 0.591671 0.090479 0.411593 11.00000 -1.20000 AFIX 0 C35 1 0.480261 0.211623 0.400241 11.00000 0.04893 0.02936 = 0.01919 0.00889 0.01470 0.02055 AFIX 43 H35 2 0.485355 0.205219 0.355019 11.00000 -1.20000 AFIX 0 C36 1 0.348231 0.371199 0.328826 11.00000 0.01730 0.01515 = 0.01260 0.00500 0.00364 0.00140 HKLF 4 REM C:\Users\91700\Desktop\Ni_NDC_3\mo_Ni_NDC_3_0m_a.res in P-1 REM wR2 = 0.1236, GooF = S = 1.060, Restrained GooF = 1.060 for all data REM R1 = 0.0410 for 10196 Fo > 4sig(Fo) and 0.0709 for all 14547 data REM 534 parameters refined using 0 restraints END WGHT 0.0613 0.1728 REM Highest difference peak 1.715, deepest hole -1.064, 1-sigma level 0.242 Q1 1 0.8555 0.3290 0.5607 11.00000 0.05 0.86 Q2 1 0.4352 0.2679 0.5162 11.00000 0.05 0.74 Q3 1 0.0108 0.8663 1.0389 11.00000 0.05 0.73 Q4 1 0.1872 0.7636 1.0181 11.00000 0.05 0.71 Q5 1 0.4814 0.4951 0.8219 11.00000 0.05 0.70 Q6 1 0.2662 0.4390 0.4618 11.00000 0.05 0.68 Q7 1 0.2356 0.3969 0.5185 11.00000 0.05 0.67 Q8 1 0.2970 0.3998 0.4198 11.00000 0.05 0.65 Q9 1 0.2379 0.6002 0.9840 11.00000 0.05 0.65 Q10 1 0.3476 0.3353 0.5224 11.00000 0.05 0.65 Q11 1 0.1463 0.5969 0.6989 11.00000 0.05 0.64 Q12 1 0.0889 0.7995 0.9896 11.00000 0.05 0.64 Q13 1 0.8658 0.2772 0.5416 11.00000 0.05 0.64 Q14 1 0.0154 0.4485 0.5150 11.00000 0.05 0.63 Q15 1 0.3220 0.3974 0.5746 11.00000 0.05 0.62 Q16 1 0.4152 0.3015 0.4671 11.00000 0.05 0.62 Q17 1 -0.2409 0.7163 0.8748 11.00000 0.05 0.62 Q18 1 0.4657 0.5756 1.0024 11.00000 0.05 0.61 Q19 1 0.3025 0.4612 0.4958 11.00000 0.05 0.61 Q20 1 0.3199 0.4225 0.5195 11.00000 0.05 0.60 ; _shelx_res_checksum 36470 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 -0.03780(4) 0.64442(2) 0.78876(2) 0.01283(6) Uani 1 1 d . . . . . Ni2 Ni 0.43189(4) 0.65325(2) 0.78674(2) 0.01292(6) Uani 1 1 d . . . . . Ni3 Ni 0.17855(4) 0.43885(2) 0.73715(2) 0.01337(6) Uani 1 1 d . . . . . Ni4 Ni 0.64199(4) 0.44476(2) 0.73276(2) 0.01303(6) Uani 1 1 d . . . . . O1 O 0.0628(2) 0.78054(12) 0.76152(8) 0.0214(3) Uani 1 1 d . . . . . O2 O 0.3871(2) 0.79880(12) 0.78712(8) 0.0218(3) Uani 1 1 d . . . . . O3 O 0.2172(2) 1.29433(12) 0.73612(8) 0.0220(3) Uani 1 1 d . . . . . O4 O 0.5413(2) 1.30797(12) 0.75940(8) 0.0218(3) Uani 1 1 d . . . . . O5 O 0.1034(2) 0.68897(13) 0.88144(7) 0.0232(3) Uani 1 1 d . . . . . O6 O 0.3970(2) 0.65037(13) 0.88314(7) 0.0217(3) Uani 1 1 d . . . . . O7 O -0.0895(2) 0.56852(13) 1.17183(7) 0.0206(3) Uani 1 1 d . . . . . O8 O 0.1627(2) 0.49291(11) 1.18208(7) 0.0156(3) Uani 1 1 d . . . . . O9 O 0.2028(2) 0.42838(13) 0.63758(7) 0.0231(3) Uani 1 1 d . . . . . O10 O 0.5027(2) 0.39820(13) 0.64097(7) 0.0231(3) Uani 1 1 d . . . . . O11 O 0.2320(2) 0.41685(11) 0.29860(7) 0.0163(3) Uani 1 1 d . . . . . O12 O 0.4812(2) 0.33819(13) 0.30381(7) 0.0224(3) Uani 1 1 d . . . . . O13 O 0.1560(2) 0.58533(11) 0.74194(7) 0.0141(3) Uani 1 1 d . . . . . O14 O -0.2617(2) 0.71193(12) 0.82946(8) 0.0216(3) Uani 1 1 d . . . . . O15 O 0.4527(2) 0.50597(11) 0.77968(7) 0.0136(3) Uani 1 1 d . . . . . O16 O 0.8707(2) 0.37691(12) 0.69338(8) 0.0211(3) Uani 1 1 d . . . . . O17 O -0.2161(4) 0.89750(18) 0.80080(15) 0.0669(8) Uani 1 1 d . . . . . O18 O -0.2585(13) 0.7371(10) 0.9656(6) 0.441(8) Uani 1 1 d . . . . . O19 O 0.7591(4) 0.17817(19) 0.68974(14) 0.0661(8) Uani 1 1 d . . . . . C1 C 0.2379(3) 0.83041(16) 0.77015(10) 0.0169(4) Uani 1 1 d . . . . . C2 C 0.2698(3) 0.93974(16) 0.76065(11) 0.0193(4) Uani 1 1 d . . . . . C3 C 0.3910(4) 1.01310(18) 0.80854(12) 0.0255(5) Uani 1 1 d . . . . . H3 H 0.453681 0.993704 0.844767 0.031 Uiso 1 1 calc R U . . . C4 C 0.4223(4) 1.11678(17) 0.80390(12) 0.0239(5) Uani 1 1 d . . . . . H4 H 0.504599 1.165234 0.837035 0.029 Uiso 1 1 calc R U . . . C5 C 0.3325(3) 1.14689(16) 0.75101(11) 0.0190(4) Uani 1 1 d . . . . . C6 C 0.2101(3) 1.07333(16) 0.69865(11) 0.0180(4) Uani 1 1 d . . . . . C7 C 0.1773(3) 0.96775(16) 0.70386(11) 0.0193(4) Uani 1 1 d . . . . . C8 C 0.0593(4) 0.89545(18) 0.65041(12) 0.0277(5) Uani 1 1 d . . . . . H8 H 0.034986 0.826505 0.653003 0.033 Uiso 1 1 calc R U . . . C9 C -0.0189(5) 0.9253(2) 0.59540(13) 0.0361(6) Uani 1 1 d . . . . . H9 H -0.094930 0.876529 0.560995 0.043 Uiso 1 1 calc R U . . . C10 C 0.0143(5) 1.0285(2) 0.59038(13) 0.0363(6) Uani 1 1 d . . . . . H10 H -0.039805 1.048011 0.552711 0.044 Uiso 1 1 calc R U . . . C11 C 0.1262(4) 1.10103(19) 0.64060(12) 0.0273(5) Uani 1 1 d . . . . . H11 H 0.147444 1.169418 0.636622 0.033 Uiso 1 1 calc R U . . . C12 C 0.3662(3) 1.25973(15) 0.74885(10) 0.0167(4) Uani 1 1 d . . . . . C13 C 0.2517(3) 0.66670(16) 0.90957(10) 0.0176(4) Uani 1 1 d . . . . . C14 C 0.2433(3) 0.65200(17) 0.98012(10) 0.0183(4) Uani 1 1 d . . . . . C15 C 0.2784(4) 0.56354(19) 0.99644(11) 0.0240(5) Uani 1 1 d . . . . . H15 H 0.334478 0.521761 0.967842 0.029 Uiso 1 1 calc R U . . . C16 C 0.2305(4) 0.53485(18) 1.05638(11) 0.0223(5) Uani 1 1 d . . . . . H16 H 0.259051 0.475297 1.067609 0.027 Uiso 1 1 calc R U . . . C17 C 0.1420(3) 0.59394(16) 1.09852(10) 0.0166(4) Uani 1 1 d . . . . . C18 C 0.1190(3) 0.69135(17) 1.08567(10) 0.0185(4) Uani 1 1 d . . . . . C19 C 0.1749(4) 0.72168(17) 1.02603(10) 0.0210(4) Uani 1 1 d . . . . . C20 C 0.1651(5) 0.8208(2) 1.01542(13) 0.0379(7) Uani 1 1 d . . . . . H20 H 0.200536 0.841174 0.976615 0.045 Uiso 1 1 calc R U . . . C21 C 0.1051(6) 0.8868(2) 1.06064(14) 0.0499(9) Uani 1 1 d . . . . . H21 H 0.104327 0.952461 1.053298 0.060 Uiso 1 1 calc R U . . . C22 C 0.0439(5) 0.8567(2) 1.11865(14) 0.0438(8) Uani 1 1 d . . . . . H22 H -0.000403 0.901873 1.148867 0.053 Uiso 1 1 calc R U . . . C23 C 0.0494(4) 0.76174(19) 1.13057(12) 0.0305(6) Uani 1 1 d . . . . . H23 H 0.006870 0.742348 1.168768 0.037 Uiso 1 1 calc R U . . . C24 C 0.0653(3) 0.55046(15) 1.15500(9) 0.0143(4) Uani 1 1 d . . . . . C25 C 0.3415(3) 0.40257(16) 0.61105(10) 0.0168(4) Uani 1 1 d . . . . . C26 C 0.3201(3) 0.37851(17) 0.53658(10) 0.0178(4) Uani 1 1 d . . . . . C27 C 0.2330(4) 0.43875(19) 0.50201(10) 0.0229(5) Uani 1 1 d . . . . . H27 H 0.170950 0.485418 0.523897 0.028 Uiso 1 1 calc R U . . . C28 C 0.2361(4) 0.43094(19) 0.43311(10) 0.0227(5) Uani 1 1 d . . . . . H28 H 0.176656 0.473011 0.410314 0.027 Uiso 1 1 calc R U . . . C29 C 0.3254(3) 0.36229(16) 0.39920(10) 0.0165(4) Uani 1 1 d . . . . . C30 C 0.4060(3) 0.29224(17) 0.43287(10) 0.0180(4) Uani 1 1 d . . . . . C31 C 0.4016(3) 0.30073(17) 0.50271(10) 0.0180(4) Uani 1 1 d . . . . . C32 C 0.4720(4) 0.2280(2) 0.53564(12) 0.0295(6) Uani 1 1 d . . . . . H32 H 0.471297 0.232978 0.581011 0.035 Uiso 1 1 calc R U . . . C33 C 0.5402(5) 0.1514(2) 0.50215(13) 0.0415(8) Uani 1 1 d . . . . . H33 H 0.584189 0.104291 0.524619 0.050 Uiso 1 1 calc R U . . . C34 C 0.5446(5) 0.1431(2) 0.43410(13) 0.0417(8) Uani 1 1 d . . . . . H34 H 0.591671 0.090479 0.411593 0.050 Uiso 1 1 calc R U . . . C35 C 0.4803(4) 0.21162(19) 0.40024(12) 0.0296(6) Uani 1 1 d . . . . . H35 H 0.485355 0.205219 0.355019 0.035 Uiso 1 1 calc R U . . . C36 C 0.3482(3) 0.37120(16) 0.32883(9) 0.0149(4) Uani 1 1 d . . . . . 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 0.01347(13) 0.01201(12) 0.01387(12) 0.00394(9) 0.00263(9) 0.00326(10) Ni2 0.01433(13) 0.01244(12) 0.01374(12) 0.00426(9) 0.00441(10) 0.00429(10) Ni3 0.01428(13) 0.01199(13) 0.01523(12) 0.00336(10) 0.00433(10) 0.00426(10) Ni4 0.01300(13) 0.01214(12) 0.01439(12) 0.00291(9) 0.00208(9) 0.00333(10) O1 0.0183(8) 0.0155(7) 0.0321(9) 0.0101(6) 0.0041(7) 0.0031(6) O2 0.0196(8) 0.0139(7) 0.0337(9) 0.0079(6) 0.0040(7) 0.0054(6) O3 0.0195(8) 0.0143(7) 0.0338(9) 0.0058(6) 0.0050(7) 0.0056(6) O4 0.0194(8) 0.0154(7) 0.0313(9) 0.0085(6) 0.0034(7) 0.0022(6) O5 0.0244(9) 0.0309(9) 0.0152(7) 0.0031(6) 0.0030(6) 0.0089(7) O6 0.0239(9) 0.0294(9) 0.0147(7) 0.0068(6) 0.0058(6) 0.0085(7) O7 0.0205(8) 0.0266(8) 0.0200(7) 0.0115(6) 0.0084(6) 0.0096(7) O8 0.0166(7) 0.0162(7) 0.0151(7) 0.0061(5) 0.0011(5) 0.0044(6) O9 0.0244(9) 0.0326(9) 0.0144(7) 0.0032(6) 0.0045(6) 0.0113(7) O10 0.0214(8) 0.0330(9) 0.0138(7) 0.0013(6) 0.0017(6) 0.0062(7) O11 0.0170(7) 0.0182(7) 0.0145(7) 0.0058(5) 0.0009(5) 0.0044(6) O12 0.0261(9) 0.0305(9) 0.0180(7) 0.0117(6) 0.0101(6) 0.0145(7) O13 0.0157(7) 0.0120(7) 0.0157(7) 0.0038(5) 0.0034(5) 0.0043(6) O14 0.0182(8) 0.0241(8) 0.0220(8) -0.0001(6) 0.0030(6) 0.0065(7) O15 0.0138(7) 0.0129(7) 0.0152(6) 0.0033(5) 0.0023(5) 0.0049(5) O16 0.0179(8) 0.0242(8) 0.0210(8) 0.0007(6) 0.0032(6) 0.0061(7) O17 0.0456(15) 0.0316(12) 0.121(2) 0.0023(14) 0.0226(15) 0.0065(11) O18 0.186(9) 0.63(2) 0.438(16) 0.007(14) 0.051(10) -0.011(11) O19 0.0637(18) 0.0455(14) 0.098(2) 0.0125(14) 0.0375(16) 0.0203(13) C1 0.0187(10) 0.0132(9) 0.0206(10) 0.0052(8) 0.0056(8) 0.0044(8) C2 0.0197(11) 0.0104(9) 0.0291(11) 0.0065(8) 0.0049(9) 0.0033(8) C3 0.0281(13) 0.0167(11) 0.0316(12) 0.0091(9) -0.0026(10) 0.0045(9) C4 0.0249(12) 0.0133(10) 0.0313(12) 0.0047(9) -0.0024(9) 0.0019(9) C5 0.0192(11) 0.0125(9) 0.0267(11) 0.0057(8) 0.0065(9) 0.0033(8) C6 0.0201(11) 0.0128(9) 0.0215(10) 0.0046(8) 0.0031(8) 0.0033(8) C7 0.0212(11) 0.0150(10) 0.0231(10) 0.0058(8) 0.0046(8) 0.0045(8) C8 0.0343(14) 0.0166(11) 0.0288(12) 0.0044(9) 0.0020(10) -0.0014(10) C9 0.0443(17) 0.0276(14) 0.0295(13) 0.0028(11) -0.0040(12) -0.0020(12) C10 0.0489(18) 0.0315(14) 0.0266(13) 0.0090(11) -0.0055(12) 0.0072(13) C11 0.0371(15) 0.0212(11) 0.0252(11) 0.0096(9) 0.0030(10) 0.0068(11) C12 0.0208(11) 0.0119(9) 0.0194(10) 0.0050(7) 0.0069(8) 0.0043(8) C13 0.0228(11) 0.0171(10) 0.0127(9) 0.0032(7) 0.0033(8) 0.0031(8) C14 0.0214(11) 0.0203(10) 0.0137(9) 0.0065(8) 0.0054(8) 0.0017(9) C15 0.0294(13) 0.0307(13) 0.0188(10) 0.0086(9) 0.0107(9) 0.0156(10) C16 0.0287(13) 0.0247(11) 0.0208(10) 0.0117(9) 0.0096(9) 0.0137(10) C17 0.0196(10) 0.0181(10) 0.0133(9) 0.0061(7) 0.0040(8) 0.0036(8) C18 0.0240(11) 0.0180(10) 0.0150(9) 0.0051(8) 0.0053(8) 0.0055(9) C19 0.0298(12) 0.0183(10) 0.0159(9) 0.0053(8) 0.0065(9) 0.0041(9) C20 0.072(2) 0.0221(12) 0.0265(13) 0.0129(10) 0.0210(14) 0.0131(14) C21 0.101(3) 0.0234(14) 0.0367(15) 0.0127(12) 0.0265(17) 0.0259(17) C22 0.079(2) 0.0258(14) 0.0373(15) 0.0081(11) 0.0297(16) 0.0223(15) C23 0.0491(17) 0.0235(12) 0.0248(12) 0.0068(9) 0.0182(11) 0.0129(12) C24 0.0167(10) 0.0142(9) 0.0113(8) 0.0027(7) 0.0023(7) 0.0015(8) C25 0.0218(11) 0.0157(10) 0.0123(9) 0.0039(7) 0.0021(8) 0.0018(8) C26 0.0187(10) 0.0212(10) 0.0141(9) 0.0035(8) 0.0048(8) 0.0043(8) C27 0.0286(13) 0.0294(12) 0.0166(10) 0.0057(9) 0.0061(9) 0.0172(10) C28 0.0289(13) 0.0287(12) 0.0167(10) 0.0087(9) 0.0057(9) 0.0158(10) C29 0.0184(10) 0.0191(10) 0.0134(9) 0.0062(7) 0.0037(7) 0.0045(8) C30 0.0220(11) 0.0198(10) 0.0146(9) 0.0054(8) 0.0051(8) 0.0068(9) C31 0.0230(11) 0.0187(10) 0.0143(9) 0.0059(8) 0.0037(8) 0.0060(9) C32 0.0461(16) 0.0288(13) 0.0193(11) 0.0091(9) 0.0055(10) 0.0174(12) C33 0.065(2) 0.0420(17) 0.0316(14) 0.0171(12) 0.0121(14) 0.0352(16) C34 0.071(2) 0.0383(16) 0.0331(14) 0.0153(12) 0.0235(15) 0.0376(16) C35 0.0489(17) 0.0294(13) 0.0192(11) 0.0089(9) 0.0147(11) 0.0206(12) C36 0.0173(10) 0.0151(9) 0.0126(8) 0.0050(7) 0.0036(7) 0.0014(8) 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' 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 O13 Ni1 O5 101.87(6) . . ? O13 Ni1 O1 90.06(6) . . ? O5 Ni1 O1 93.97(7) . . ? O13 Ni1 O11 85.72(6) . 2_566 ? O5 Ni1 O11 168.19(7) . 2_566 ? O1 Ni1 O11 95.07(6) . 2_566 ? O13 Ni1 O8 94.13(6) . 2_567 ? O5 Ni1 O8 86.85(6) . 2_567 ? O1 Ni1 O8 175.48(6) . 2_567 ? O11 Ni1 O8 83.55(6) 2_566 2_567 ? O13 Ni1 O14 173.75(6) . . ? O5 Ni1 O14 83.78(6) . . ? O1 Ni1 O14 86.84(6) . . ? O11 Ni1 O14 89.14(6) 2_566 . ? O8 Ni1 O14 88.83(6) 2_567 . ? O15 Ni2 O13 81.38(6) . . ? O15 Ni2 O6 86.72(6) . . ? O13 Ni2 O6 100.06(6) . . ? O15 Ni2 O12 92.30(6) . 2_666 ? O13 Ni2 O12 89.85(6) . 2_666 ? O6 Ni2 O12 169.76(7) . 2_666 ? O15 Ni2 O2 174.46(6) . . ? O13 Ni2 O2 93.34(6) . . ? O6 Ni2 O2 95.89(7) . . ? O12 Ni2 O2 85.99(6) 2_666 . ? O15 Ni2 O14 93.23(6) . 1_655 ? O13 Ni2 O14 173.82(6) . 1_655 ? O6 Ni2 O14 82.55(6) . 1_655 ? O12 Ni2 O14 87.34(7) 2_666 1_655 ? O2 Ni2 O14 91.95(6) . 1_655 ? O15 Ni3 O13 82.08(6) . . ? O15 Ni3 O3 94.45(6) . 1_545 ? O13 Ni3 O3 176.45(6) . 1_545 ? O15 Ni3 O7 91.13(6) . 2_567 ? O13 Ni3 O7 92.83(6) . 2_567 ? O3 Ni3 O7 86.46(7) 1_545 2_567 ? O15 Ni3 O9 102.05(6) . . ? O13 Ni3 O9 89.83(6) . . ? O3 Ni3 O9 91.64(7) 1_545 . ? O7 Ni3 O9 166.79(7) 2_567 . ? O15 Ni3 O16 175.34(6) . 1_455 ? O13 Ni3 O16 93.57(6) . 1_455 ? O3 Ni3 O16 89.88(6) 1_545 1_455 ? O7 Ni3 O16 87.42(6) 2_567 1_455 ? O9 Ni3 O16 79.50(6) . 1_455 ? O15 Ni4 O10 102.92(6) . . ? O15 Ni4 O4 91.23(6) . 1_545 ? O10 Ni4 O4 92.82(7) . 1_545 ? O15 Ni4 O8 85.65(6) . 2_667 ? O10 Ni4 O8 167.28(6) . 2_667 ? O4 Ni4 O8 96.41(6) 1_545 2_667 ? O15 Ni4 O11 93.76(6) . 2_666 ? O10 Ni4 O11 86.72(6) . 2_666 ? O4 Ni4 O11 174.96(6) 1_545 2_666 ? O8 Ni4 O11 83.32(6) 2_667 2_666 ? O15 Ni4 O16 172.65(6) . . ? O10 Ni4 O16 84.15(6) . . ? O4 Ni4 O16 86.38(6) 1_545 . ? O8 Ni4 O16 87.72(6) 2_667 . ? O11 Ni4 O16 88.59(6) 2_666 . ? C1 O1 Ni1 126.94(14) . . ? C1 O2 Ni2 131.76(15) . . ? C12 O3 Ni3 132.33(15) . 1_565 ? C12 O4 Ni4 125.15(14) . 1_565 ? C13 O5 Ni1 131.51(14) . . ? C13 O6 Ni2 125.85(14) . . ? C24 O7 Ni3 126.00(14) . 2_567 ? C24 O8 Ni4 119.18(13) . 2_667 ? C24 O8 Ni1 124.81(14) . 2_567 ? Ni4 O8 Ni1 97.53(6) 2_667 2_567 ? C25 O9 Ni3 124.84(14) . . ? C25 O10 Ni4 135.83(14) . . ? C36 O11 Ni1 126.75(13) . 2_566 ? C36 O11 Ni4 117.73(13) . 2_666 ? Ni1 O11 Ni4 95.60(6) 2_566 2_666 ? C36 O12 Ni2 129.61(14) . 2_666 ? Ni1 O13 Ni3 123.47(7) . . ? Ni1 O13 Ni2 110.51(6) . . ? Ni3 O13 Ni2 97.90(6) . . ? Ni1 O14 Ni2 120.09(7) . 1_455 ? Ni4 O15 Ni3 110.45(6) . . ? Ni4 O15 Ni2 124.94(7) . . ? Ni3 O15 Ni2 98.62(6) . . ? Ni4 O16 Ni3 119.90(7) . 1_655 ? O2 C1 O1 126.8(2) . . ? O2 C1 C2 116.6(2) . . ? O1 C1 C2 116.59(19) . . ? C3 C2 C7 120.1(2) . . ? C3 C2 C1 118.3(2) . . ? C7 C2 C1 121.6(2) . . ? C2 C3 C4 121.3(2) . . ? C5 C4 C3 120.3(2) . . ? C4 C5 C6 120.6(2) . . ? C4 C5 C12 118.6(2) . . ? C6 C5 C12 120.7(2) . . ? C11 C6 C5 122.2(2) . . ? C11 C6 C7 118.9(2) . . ? C5 C6 C7 118.8(2) . . ? C8 C7 C2 123.2(2) . . ? C8 C7 C6 117.9(2) . . ? C2 C7 C6 118.8(2) . . ? C9 C8 C7 121.3(2) . . ? C8 C9 C10 120.5(2) . . ? C11 C10 C9 120.4(2) . . ? C10 C11 C6 120.9(2) . . ? O3 C12 O4 127.5(2) . . ? O3 C12 C5 116.6(2) . . ? O4 C12 C5 115.89(19) . . ? O6 C13 O5 126.03(19) . . ? O6 C13 C14 118.4(2) . . ? O5 C13 C14 115.40(19) . . ? C15 C14 C19 120.53(19) . . ? C15 C14 C13 117.87(19) . . ? C19 C14 C13 121.1(2) . . ? C14 C15 C16 120.4(2) . . ? C17 C16 C15 120.8(2) . . ? C16 C17 C18 119.92(19) . . ? C16 C17 C24 117.69(19) . . ? C18 C17 C24 122.34(19) . . ? C23 C18 C19 118.0(2) . . ? C23 C18 C17 123.28(19) . . ? C19 C18 C17 118.63(19) . . ? C20 C19 C14 122.3(2) . . ? C20 C19 C18 118.7(2) . . ? C14 C19 C18 118.9(2) . . ? C21 C20 C19 121.3(2) . . ? C20 C21 C22 120.5(3) . . ? C23 C22 C21 120.1(2) . . ? C22 C23 C18 121.3(2) . . ? O7 C24 O8 124.03(18) . . ? O7 C24 C17 118.81(19) . . ? O8 C24 C17 117.13(19) . . ? O9 C25 O10 125.84(19) . . ? O9 C25 C26 118.44(19) . . ? O10 C25 C26 115.67(19) . . ? C27 C26 C31 120.21(19) . . ? C27 C26 C25 117.79(19) . . ? C31 C26 C25 121.81(19) . . ? C26 C27 C28 120.5(2) . . ? C29 C28 C27 121.2(2) . . ? C28 C29 C30 119.93(18) . . ? C28 C29 C36 116.90(19) . . ? C30 C29 C36 122.96(18) . . ? C35 C30 C31 118.2(2) . . ? C35 C30 C29 123.50(19) . . ? C31 C30 C29 118.26(19) . . ? C32 C31 C26 122.03(19) . . ? C32 C31 C30 118.4(2) . . ? C26 C31 C30 119.54(19) . . ? C33 C32 C31 121.4(2) . . ? C32 C33 C34 120.3(2) . . ? C35 C34 C33 120.7(2) . . ? C34 C35 C30 121.2(2) . . ? O12 C36 O11 123.90(18) . . ? O12 C36 C29 118.80(19) . . ? O11 C36 C29 117.24(18) . . ? 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 O13 1.9853(14) . ? Ni1 O5 2.0073(15) . ? Ni1 O1 2.0319(16) . ? Ni1 O11 2.0966(15) 2_566 ? Ni1 O8 2.1047(15) 2_567 ? Ni1 O14 2.1639(16) . ? Ni2 O15 2.0222(14) . ? Ni2 O13 2.0376(15) . ? Ni2 O6 2.0377(15) . ? Ni2 O12 2.0422(15) 2_666 ? Ni2 O2 2.0661(15) . ? Ni2 O14 2.1914(17) 1_655 ? Ni3 O15 2.0125(15) . ? Ni3 O13 2.0189(14) . ? Ni3 O3 2.0360(16) 1_545 ? Ni3 O7 2.0552(15) 2_567 ? Ni3 O9 2.0675(15) . ? Ni3 O16 2.2103(16) 1_455 ? Ni4 O15 1.9740(14) . ? Ni4 O10 1.9888(15) . ? Ni4 O4 2.0345(16) 1_545 ? Ni4 O8 2.0694(15) 2_667 ? Ni4 O11 2.1409(15) 2_666 ? Ni4 O16 2.1852(16) . ? O1 C1 1.267(3) . ? O2 C1 1.255(3) . ? O3 C12 1.257(3) . ? O4 C12 1.259(3) . ? O5 C13 1.259(3) . ? O6 C13 1.256(3) . ? O7 C24 1.242(3) . ? O8 C24 1.293(2) . ? O9 C25 1.256(3) . ? O10 C25 1.256(3) . ? O11 C36 1.292(3) . ? O12 C36 1.246(3) . ? C1 C2 1.506(3) . ? C2 C3 1.372(3) . ? C2 C7 1.424(3) . ? C3 C4 1.403(3) . ? C4 C5 1.365(3) . ? C5 C6 1.429(3) . ? C5 C12 1.514(3) . ? C6 C11 1.419(3) . ? C6 C7 1.431(3) . ? C7 C8 1.423(3) . ? C8 C9 1.365(4) . ? C9 C10 1.399(4) . ? C10 C11 1.369(4) . ? C13 C14 1.507(3) . ? C14 C15 1.361(3) . ? C14 C19 1.426(3) . ? C15 C16 1.409(3) . ? C16 C17 1.377(3) . ? C17 C18 1.428(3) . ? C17 C24 1.491(3) . ? C18 C23 1.425(3) . ? C18 C19 1.428(3) . ? C19 C20 1.414(3) . ? C20 C21 1.355(4) . ? C21 C22 1.407(4) . ? C22 C23 1.359(4) . ? C25 C26 1.508(3) . ? C26 C27 1.361(3) . ? C26 C31 1.429(3) . ? C27 C28 1.414(3) . ? C28 C29 1.375(3) . ? C29 C30 1.434(3) . ? C29 C36 1.500(3) . ? C30 C35 1.418(3) . ? C30 C31 1.434(3) . ? C31 C32 1.423(3) . ? C32 C33 1.359(4) . ? C33 C34 1.397(4) . ? C34 C35 1.368(4) . ?