#------------------------------------------------------------------------------ #$Date: 2016-05-12 06:02:26 +0300 (Thu, 12 May 2016) $ #$Revision: 182887 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/51/7225190.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_7225190 loop_ _publ_author_name 'Beldon, Patrick' 'Henke, Sebastian' 'Monserrat, Bartomeu' 'Tominaka, Satoshi' 'Stock, Norbert' 'Cheetham, Tony' _publ_section_title ; Transition metal coordination complexes of chrysazin ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C5CE00792E _journal_year 2016 _chemical_formula_moiety 'C126 H114 N6 Ni12 O54' _chemical_formula_sum 'C144 H156 N12 Ni12 O60' _chemical_formula_weight 3719.32 _chemical_name_systematic 'dodeca(acetato)-hexa(chrysazinato)-hexa(N,N-dimethylformamide)-tetra-cobalt(II) N,N-dimethylformamide solvate' _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens geom _audit_creation_date 2016-03-17 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _audit_update_record ; 2016-04-20 deposited with the CCDC. 2016-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 28.6809(7) _cell_length_b 28.6809(7) _cell_length_c 15.8967(4) _cell_measurement_reflns_used 13246 _cell_measurement_temperature 120.10(14) _cell_measurement_theta_max 70.8420 _cell_measurement_theta_min 4.5080 _cell_volume 11324.6(5) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.10(14) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1183 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.9998 _diffrn_measured_fraction_theta_max 0.9941 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0300452000 _diffrn_orient_matrix_UB_12 -0.0619515000 _diffrn_orient_matrix_UB_13 0.0039501000 _diffrn_orient_matrix_UB_21 0.0396946000 _diffrn_orient_matrix_UB_22 -0.0008731000 _diffrn_orient_matrix_UB_23 -0.0644751000 _diffrn_orient_matrix_UB_31 0.0369773000 _diffrn_orient_matrix_UB_32 0.0026244000 _diffrn_orient_matrix_UB_33 0.0723068000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_unetI/netI 0.0154 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 29190 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.154 _diffrn_reflns_theta_min 3.301 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.397 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.636 _exptl_crystal_description prism _exptl_crystal_F_000 5760 _exptl_crystal_size_max 0.1868 _exptl_crystal_size_mid 0.1394 _exptl_crystal_size_min 0.0789 _platon_squeeze_details ; ; _refine_diff_density_max 0.302 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 302 _refine_ls_number_reflns 4851 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0291 _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^)+(0.0482P)^2^+13.7597P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.0847 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4425 _reflns_number_total 4851 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5ce00792e2.cif _cod_data_source_block NiChrys-1 _cod_original_cell_volume 11324.6(6) _cod_database_code 7225190 _shelxl_version_number 2014/6 _chemical_oxdiff_formula 'Ni12 C141 H149 N11 O59' _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. ; _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C19(H19) 2.b Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B, H21C) ; _shelx_res_file ; TITL NiChrys-1 in R-3 #148 CELL 1.54184 28.680945 28.680945 15.896672 90 90 120 ZERR 3 0.00068 0.00068 0.000438 0 0 0 LATT 3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H N O Ni UNIT 432 468 36 180 36 L.S. 4 0 0 PLAN 20 REM reset to R-3 #148 BOND fmap 2 53 acta MORE -1 CONF REM C:/Users/pjb76/Desktop/Dropbox/Research%20outlines/Cambridge/Chrysazi REM n%20high-throughput/Chrysazin%20paper/CIFs/Post-review/NiChrys-1-/NiChrys- REM 1.hkl WGHT 0.048200 13.759700 FVAR 1.03381 NI1 5 0.680026 0.130401 0.339652 11.00000 0.02848 0.02346 = 0.03322 -0.00103 -0.00149 0.01449 NI2 5 0.777961 0.239213 0.355228 11.00000 0.02562 0.02484 = 0.03326 -0.00194 0.00033 0.01374 O1 4 0.713113 0.189618 0.427345 11.00000 0.02892 0.02588 = 0.03299 -0.00188 -0.00085 0.01354 O2 4 0.610955 0.110042 0.402213 11.00000 0.03093 0.02444 = 0.03029 0.00227 0.00108 0.01451 O3 4 0.504736 0.081610 0.377678 11.00000 0.02868 0.02366 = 0.03684 0.00380 0.00443 0.01124 O4 4 0.579244 0.080158 0.731986 11.00000 0.08493 0.06310 = 0.03653 0.01440 0.00195 0.00899 O5 4 0.652726 0.173828 0.270052 11.00000 0.02593 0.02370 = 0.03369 0.00207 0.00145 0.01282 O6 4 0.727324 0.254343 0.281327 11.00000 0.02521 0.02549 = 0.03958 0.00086 0.00045 0.01272 O7 4 0.642888 0.069826 0.257730 11.00000 0.03387 0.02900 = 0.03879 -0.00577 -0.00389 0.01767 O8 4 0.564828 0.068191 0.234762 11.00000 0.02992 0.02690 = 0.03608 -0.00110 -0.00024 0.01327 O9 4 0.694598 0.080969 0.416030 11.00000 0.03790 0.02744 = 0.04601 -0.00096 -0.00954 0.01833 N1 3 0.745165 0.081967 0.526399 11.00000 0.03736 0.03780 = 0.04151 0.00365 -0.00431 0.01839 C1 1 0.701570 0.178828 0.507494 11.00000 0.03589 0.03198 = 0.03393 -0.00321 -0.00145 0.02112 C2 1 0.742074 0.206258 0.568673 11.00000 0.03612 0.05460 = 0.04090 -0.01131 -0.00356 0.02147 AFIX 43 H2 2 0.776115 0.232807 0.551410 11.00000 -1.20000 AFIX 0 C3 1 0.732460 0.194711 0.653108 11.00000 0.04750 0.07730 = 0.03894 -0.01321 -0.00999 0.03101 AFIX 43 H3 2 0.760229 0.212974 0.691547 11.00000 -1.20000 AFIX 0 C4 1 0.682019 0.156281 0.681606 11.00000 0.06298 0.06201 = 0.03271 -0.00251 -0.00364 0.03251 AFIX 43 H4 2 0.676262 0.147831 0.738533 11.00000 -1.20000 AFIX 0 C5 1 0.640498 0.130712 0.624961 11.00000 0.05210 0.03696 = 0.03382 0.00135 -0.00040 0.02200 C6 1 0.648994 0.140477 0.536771 11.00000 0.04127 0.02614 = 0.03348 0.00123 -0.00041 0.01855 C7 1 0.603096 0.112599 0.480216 11.00000 0.03769 0.01978 = 0.03499 0.00379 0.00313 0.01519 C8 1 0.548344 0.086266 0.511428 11.00000 0.03984 0.02120 = 0.03385 0.00263 0.00559 0.01308 C9 1 0.539673 0.072787 0.598665 11.00000 0.05117 0.02575 = 0.03660 0.00348 0.00854 0.01461 C10 1 0.585886 0.092641 0.657202 11.00000 0.06386 0.03524 = 0.03301 0.00595 0.00465 0.01782 C11 1 0.488639 0.040819 0.630281 11.00000 0.06153 0.02967 = 0.03988 0.00753 0.01747 0.01710 AFIX 43 H11 2 0.483818 0.031933 0.687109 11.00000 -1.20000 AFIX 0 C12 1 0.444202 0.021772 0.577128 11.00000 0.04556 0.02543 = 0.05164 0.00837 0.02060 0.01303 AFIX 43 H12 2 0.409760 -0.000201 0.598409 11.00000 -1.20000 AFIX 0 C13 1 0.451097 0.035319 0.493609 11.00000 0.03635 0.02291 = 0.05202 0.00427 0.00973 0.01294 AFIX 43 H13 2 0.420922 0.022190 0.459156 11.00000 -1.20000 AFIX 0 C14 1 0.502657 0.068668 0.457883 11.00000 0.03661 0.02070 = 0.03849 0.00354 0.00863 0.01394 C15 1 0.679515 0.225125 0.259621 11.00000 0.02637 0.02603 = 0.03276 0.00230 0.00324 0.01402 C16 1 0.651159 0.250928 0.217511 11.00000 0.03157 0.03123 = 0.05950 0.01219 -0.00080 0.01450 AFIX 137 H16A 2 0.632502 0.259741 0.259054 11.00000 -1.50000 H16B 2 0.625786 0.226362 0.177313 11.00000 -1.50000 H16C 2 0.677079 0.283161 0.189270 11.00000 -1.50000 AFIX 0 C17 1 0.599330 0.054308 0.219284 11.00000 0.03475 0.02679 = 0.03205 0.00128 0.00210 0.01507 C18 1 0.586687 0.014880 0.148075 11.00000 0.04802 0.05883 = 0.04292 -0.01776 -0.00834 0.03117 AFIX 137 H18A 2 0.619652 0.020146 0.123902 11.00000 -1.50000 H18B 2 0.566171 0.020651 0.105850 11.00000 -1.50000 H18C 2 0.566204 -0.021214 0.169218 11.00000 -1.50000 AFIX 0 C19 1 0.738684 0.099517 0.453180 11.00000 0.03808 0.03284 = 0.03648 -0.00096 -0.00089 0.02227 AFIX 43 H19 2 0.768875 0.127501 0.427556 11.00000 -1.20000 AFIX 0 C20 1 0.797597 0.106347 0.567141 11.00000 0.03993 0.05821 = 0.04111 0.00163 -0.00717 0.02163 AFIX 137 H20A 2 0.824387 0.132375 0.530058 11.00000 -1.50000 H20B 2 0.806371 0.078944 0.580146 11.00000 -1.50000 H20C 2 0.796615 0.123804 0.618093 11.00000 -1.50000 AFIX 0 C21 1 0.700313 0.040446 0.573553 11.00000 0.04689 0.05616 = 0.06748 0.02387 -0.00841 0.01285 AFIX 137 H21A 2 0.692181 0.056492 0.620124 11.00000 -1.50000 H21B 2 0.709676 0.014731 0.594172 11.00000 -1.50000 H21C 2 0.669388 0.022628 0.537578 11.00000 -1.50000 AFIX 0 HKLF 4 REM NiChrys-1 in R-3 #148 REM R1 = 0.0291 for 4425 Fo > 4sig(Fo) and 0.0319 for all 4851 data REM 302 parameters refined using 0 restraints END WGHT 0.0482 13.7596 REM Highest difference peak 0.302, deepest hole -0.284, 1-sigma level 0.055 Q1 1 0.6274 0.1146 0.2318 11.00000 0.05 0.30 Q2 1 0.5464 0.0768 0.5512 11.00000 0.05 0.24 Q3 1 0.6480 0.1521 0.4083 11.00000 0.05 0.23 Q4 1 0.5545 0.0865 0.6273 11.00000 0.05 0.23 Q5 1 0.6455 0.1349 0.5792 11.00000 0.05 0.22 Q6 1 0.5239 0.0764 0.4811 11.00000 0.05 0.21 Q7 1 0.6569 0.1787 0.5922 11.00000 0.05 0.21 Q8 1 0.6263 0.1289 0.5130 11.00000 0.05 0.21 Q9 1 0.5465 -0.0051 0.1370 11.00000 0.05 0.20 Q10 1 0.7435 0.0609 0.4854 11.00000 0.05 0.20 Q11 1 0.4721 0.0474 0.4812 11.00000 0.05 0.20 Q12 1 0.4525 0.0314 0.5283 11.00000 0.05 0.19 Q13 1 0.6184 0.1893 0.1064 11.00000 0.05 0.18 Q14 1 0.6962 0.0806 0.3627 11.00000 0.05 0.18 Q15 1 0.7104 0.0038 0.5606 11.00000 0.05 0.17 Q16 1 0.7204 0.1849 0.5396 11.00000 0.05 0.17 Q17 1 0.5661 0.0949 0.7163 11.00000 0.05 0.17 Q18 1 0.6880 0.0153 0.6200 11.00000 0.05 0.17 Q19 1 0.6735 0.1638 0.5214 11.00000 0.05 0.17 Q20 1 0.7937 0.0483 0.5587 11.00000 0.05 0.17 ; _shelx_res_checksum 16700 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 Ni1 Ni 0.68003(2) 0.13040(2) 0.33965(2) 0.02772(9) Uani 1 1 d . . Ni2 Ni 0.77796(2) 0.23921(2) 0.35523(2) 0.02740(9) Uani 1 1 d . . O1 O 0.71311(5) 0.18962(5) 0.42734(7) 0.0293(3) Uani 1 1 d . . O2 O 0.61096(5) 0.11004(4) 0.40221(7) 0.0283(2) Uani 1 1 d . . O3 O 0.50474(5) 0.08161(5) 0.37768(8) 0.0305(3) Uani 1 1 d . . O4 O 0.57924(8) 0.08016(8) 0.73199(10) 0.0740(6) Uani 1 1 d . . O5 O 0.65273(4) 0.17383(4) 0.27005(7) 0.0276(2) Uani 1 1 d . . O6 O 0.72732(5) 0.25434(5) 0.28133(8) 0.0301(3) Uani 1 1 d . . O7 O 0.64289(5) 0.06983(5) 0.25773(8) 0.0330(3) Uani 1 1 d . . O8 O 0.56483(5) 0.06819(5) 0.23476(8) 0.0314(3) Uani 1 1 d . . O9 O 0.69460(5) 0.08097(5) 0.41603(8) 0.0362(3) Uani 1 1 d . . N1 N 0.74517(7) 0.08197(7) 0.52640(11) 0.0391(4) Uani 1 1 d . . C1 C 0.70157(7) 0.17883(7) 0.50749(11) 0.0321(4) Uani 1 1 d . . C2 C 0.74207(8) 0.20626(9) 0.56867(13) 0.0444(5) Uani 1 1 d . . H2 H 0.7761 0.2328 0.5514 0.053 Uiso 1 1 calc R U C3 C 0.73246(9) 0.19471(11) 0.65311(14) 0.0547(6) Uani 1 1 d . . H3 H 0.7602 0.2130 0.6915 0.066 Uiso 1 1 calc R U C4 C 0.68202(10) 0.15628(10) 0.68161(13) 0.0520(5) Uani 1 1 d . . H4 H 0.6763 0.1478 0.7385 0.062 Uiso 1 1 calc R U C5 C 0.64050(9) 0.13071(8) 0.62496(12) 0.0411(4) Uani 1 1 d . . C6 C 0.64899(8) 0.14048(7) 0.53677(11) 0.0329(4) Uani 1 1 d . . C7 C 0.60310(7) 0.11260(6) 0.48022(11) 0.0305(4) Uani 1 1 d . . C8 C 0.54834(8) 0.08627(7) 0.51143(11) 0.0326(4) Uani 1 1 d . . C9 C 0.53967(9) 0.07279(7) 0.59867(12) 0.0399(4) Uani 1 1 d . . C10 C 0.58589(10) 0.09264(8) 0.65720(13) 0.0471(5) Uani 1 1 d . . C11 C 0.48864(9) 0.04082(8) 0.63028(13) 0.0462(5) Uani 1 1 d . . H11 H 0.4838 0.0319 0.6871 0.055 Uiso 1 1 calc R U C12 C 0.44420(9) 0.02177(7) 0.57713(13) 0.0430(5) Uani 1 1 d . . H12 H 0.4098 -0.0002 0.5984 0.052 Uiso 1 1 calc R U C13 C 0.45110(8) 0.03532(7) 0.49361(13) 0.0379(4) Uani 1 1 d . . H13 H 0.4209 0.0222 0.4592 0.046 Uiso 1 1 calc R U C14 C 0.50266(7) 0.06867(7) 0.45788(12) 0.0321(4) Uani 1 1 d . . C15 C 0.67952(7) 0.22512(7) 0.25962(10) 0.0280(3) Uani 1 1 d . . C16 C 0.65116(8) 0.25093(8) 0.21751(14) 0.0413(4) Uani 1 1 d . . H16A H 0.6325 0.2597 0.2591 0.062 Uiso 1 1 calc R U H16B H 0.6258 0.2264 0.1773 0.062 Uiso 1 1 calc R U H16C H 0.6771 0.2832 0.1893 0.062 Uiso 1 1 calc R U C17 C 0.59933(7) 0.05431(7) 0.21928(11) 0.0313(4) Uani 1 1 d . . C18 C 0.58669(9) 0.01488(10) 0.14808(14) 0.0479(5) Uani 1 1 d . . H18A H 0.6197 0.0201 0.1239 0.072 Uiso 1 1 calc R U H18B H 0.5662 0.0207 0.1058 0.072 Uiso 1 1 calc R U H18C H 0.5662 -0.0212 0.1692 0.072 Uiso 1 1 calc R U C19 C 0.73868(8) 0.09952(7) 0.45318(11) 0.0338(4) Uani 1 1 d . . H19 H 0.7689 0.1275 0.4276 0.041 Uiso 1 1 calc R U C20 C 0.79760(8) 0.10635(10) 0.56714(13) 0.0477(5) Uani 1 1 d . . H20A H 0.8244 0.1324 0.5301 0.072 Uiso 1 1 calc R U H20B H 0.8064 0.0789 0.5801 0.072 Uiso 1 1 calc R U H20C H 0.7966 0.1238 0.6181 0.072 Uiso 1 1 calc R U C21 C 0.70031(10) 0.04045(10) 0.57355(17) 0.0626(7) Uani 1 1 d . . H21A H 0.6922 0.0565 0.6201 0.094 Uiso 1 1 calc R U H21B H 0.7097 0.0147 0.5942 0.094 Uiso 1 1 calc R U H21C H 0.6694 0.0226 0.5376 0.094 Uiso 1 1 calc R U 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 0.02848(16) 0.02346(15) 0.03322(17) -0.00103(11) -0.00149(11) 0.01449(12) Ni2 0.02562(15) 0.02484(15) 0.03326(17) -0.00194(11) 0.00033(11) 0.01374(12) O1 0.0289(6) 0.0259(6) 0.0330(6) -0.0019(5) -0.0008(5) 0.0135(5) O2 0.0309(6) 0.0244(6) 0.0303(6) 0.0023(4) 0.0011(5) 0.0145(5) O3 0.0287(6) 0.0237(6) 0.0368(6) 0.0038(5) 0.0044(5) 0.0112(5) O4 0.0849(13) 0.0631(11) 0.0365(8) 0.0144(8) 0.0019(8) 0.0090(10) O5 0.0259(6) 0.0237(5) 0.0337(6) 0.0021(4) 0.0015(5) 0.0128(5) O6 0.0252(6) 0.0255(6) 0.0396(7) 0.0009(5) 0.0005(5) 0.0127(5) O7 0.0339(6) 0.0290(6) 0.0388(7) -0.0058(5) -0.0039(5) 0.0177(5) O8 0.0299(6) 0.0269(6) 0.0361(6) -0.0011(5) -0.0002(5) 0.0133(5) O9 0.0379(7) 0.0274(6) 0.0460(7) -0.0010(5) -0.0095(6) 0.0183(5) N1 0.0374(8) 0.0378(8) 0.0415(9) 0.0037(7) -0.0043(7) 0.0184(7) C1 0.0359(9) 0.0320(9) 0.0339(9) -0.0032(7) -0.0015(7) 0.0211(8) C2 0.0361(10) 0.0546(12) 0.0409(11) -0.0113(9) -0.0036(8) 0.0215(9) C3 0.0475(12) 0.0773(16) 0.0389(11) -0.0132(11) -0.0100(9) 0.0310(12) C4 0.0630(14) 0.0620(14) 0.0327(10) -0.0025(9) -0.0036(9) 0.0325(12) C5 0.0521(12) 0.0370(10) 0.0338(10) 0.0013(8) -0.0004(8) 0.0220(9) C6 0.0413(10) 0.0261(8) 0.0335(9) 0.0012(7) -0.0004(7) 0.0186(8) C7 0.0377(9) 0.0198(7) 0.0350(9) 0.0038(6) 0.0031(7) 0.0152(7) C8 0.0398(10) 0.0212(8) 0.0339(9) 0.0026(6) 0.0056(7) 0.0131(7) C9 0.0512(11) 0.0258(9) 0.0366(10) 0.0035(7) 0.0085(8) 0.0146(8) C10 0.0639(14) 0.0352(10) 0.0330(10) 0.0059(8) 0.0046(9) 0.0178(10) C11 0.0615(13) 0.0297(9) 0.0399(11) 0.0075(8) 0.0175(10) 0.0171(9) C12 0.0456(11) 0.0254(9) 0.0516(12) 0.0084(8) 0.0206(9) 0.0130(8) C13 0.0363(10) 0.0229(8) 0.0520(11) 0.0043(8) 0.0097(8) 0.0129(7) C14 0.0366(9) 0.0207(8) 0.0385(9) 0.0035(7) 0.0086(7) 0.0139(7) C15 0.0264(8) 0.0260(8) 0.0328(9) 0.0023(6) 0.0032(6) 0.0140(7) C16 0.0316(9) 0.0312(9) 0.0595(12) 0.0122(9) -0.0008(8) 0.0145(8) C17 0.0348(9) 0.0268(8) 0.0320(9) 0.0013(7) 0.0021(7) 0.0151(7) C18 0.0480(12) 0.0588(13) 0.0429(11) -0.0178(10) -0.0083(9) 0.0312(11) C19 0.0381(9) 0.0328(9) 0.0365(9) -0.0010(7) -0.0009(8) 0.0223(8) C20 0.0399(11) 0.0582(13) 0.0411(11) 0.0016(9) -0.0072(8) 0.0216(10) C21 0.0469(13) 0.0562(14) 0.0675(16) 0.0239(12) -0.0084(11) 0.0129(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 4 -9 9 0.0395 4.0086 -8.9942 8.9978 0.4723 -0.4132 0.7752 -9 16 5 0.0723 -8.9891 15.9985 4.9939 -0.7013 -0.6928 0.0707 9 -10 -9 0.0435 8.9847 -10.0022 -8.9934 0.3142 0.9452 -0.3443 8 -18 1 0.0670 7.9967 -17.9951 1.0037 0.8785 0.2684 0.3210 -14 5 -7 0.0644 -14.0021 4.9989 -6.9980 0.0834 -0.1090 -1.0106 -7 18 -1 0.0757 -6.9971 17.9948 -1.0037 -0.9085 -0.2287 -0.2841 14 -4 6 0.0807 14.0009 -3.9997 5.9983 -0.1492 0.1725 0.9409 2 9 -8 0.0425 1.9900 8.9931 -7.9982 -0.6485 0.5868 -0.4811 -6 4 -10 0.0359 -6.0092 3.9961 -9.9963 -0.1065 0.4025 -0.9345 6 -3 10 0.0594 6.0093 -2.9965 9.9961 0.0446 -0.4033 0.9371 -9 -3 -8 0.0550 -9.0059 -2.9998 -7.9957 0.4248 0.1607 -0.9190 -15 3 -6 0.0674 -15.0006 3.0003 -5.9981 0.2411 -0.2113 -0.9805 -4 9 -9 0.0395 -4.0086 8.9942 -8.9978 -0.4723 0.4132 -0.7752 4 6 9 0.0702 4.0095 6.0004 8.9945 -0.4567 -0.4260 0.8144 -10 4 9 0.0545 -9.9846 4.0046 8.9947 0.0874 -0.9798 0.2917 1 -10 8 0.0338 1.0086 -9.9935 7.9985 0.6204 -0.4669 0.5894 -5 -8 7 0.0384 -4.9899 -7.9931 6.9984 0.6727 -0.6423 0.3005 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 O1 Ni1 Ni2 42.83(3) . . O1 Ni1 O3 82.66(5) . 18_545 O1 Ni1 O5 91.30(5) . . O1 Ni1 O9 90.01(5) . . O2 Ni1 Ni2 122.28(3) . . O2 Ni1 O1 83.37(5) . . O2 Ni1 O3 164.49(5) . 18_545 O2 Ni1 O5 80.08(5) . . O2 Ni1 O9 91.03(5) . . O3 Ni1 Ni2 42.36(3) 18_545 . O3 Ni1 O5 93.53(5) 18_545 . O5 Ni1 Ni2 81.84(3) . . O7 Ni1 Ni2 140.88(4) . . O7 Ni1 O1 176.18(5) . . O7 Ni1 O2 92.87(5) . . O7 Ni1 O3 101.16(5) . 18_545 O7 Ni1 O5 88.71(5) . . O7 Ni1 O9 89.38(5) . . O9 Ni1 Ni2 105.16(4) . . O9 Ni1 O3 95.67(5) . 18_545 O9 Ni1 O5 170.79(5) . . O1 Ni2 Ni1 42.61(3) . . O1 Ni2 O5 110.59(5) . 18_545 O1 Ni2 O6 88.54(5) . . O2 Ni2 Ni1 125.80(3) 18_545 . O2 Ni2 O1 168.28(5) 18_545 . O2 Ni2 O5 79.58(5) 18_545 18_545 O2 Ni2 O6 86.21(5) 18_545 . O3 Ni2 Ni1 43.56(3) 18_545 . O3 Ni2 O1 83.59(5) 18_545 . O3 Ni2 O2 85.93(5) 18_545 18_545 O3 Ni2 O5 165.28(5) 18_545 18_545 O3 Ni2 O6 89.86(5) 18_545 . O3 Ni2 O8 95.49(5) 18_545 18_545 O5 Ni2 Ni1 148.11(3) 18_545 . O6 Ni2 Ni1 77.34(3) . . O6 Ni2 O5 86.66(4) . 18_545 O8 Ni2 Ni1 107.17(4) 18_545 . O8 Ni2 O1 92.88(5) 18_545 . O8 Ni2 O2 93.31(5) 18_545 18_545 O8 Ni2 O5 87.95(5) 18_545 18_545 O8 Ni2 O6 174.59(5) 18_545 . Ni1 O1 Ni2 94.56(5) . . C1 O1 Ni1 120.78(11) . . C1 O1 Ni2 138.13(11) . . Ni1 O2 Ni2 98.87(5) . 17 C7 O2 Ni1 129.78(11) . . C7 O2 Ni2 123.05(11) . 17 Ni2 O3 Ni1 94.08(5) 17 17 C14 O3 Ni1 123.94(11) . 17 C14 O3 Ni2 125.58(11) . 17 Ni1 O5 Ni2 94.56(5) . 17 C15 O5 Ni1 124.27(10) . . C15 O5 Ni2 126.69(10) . 17 C15 O6 Ni2 131.75(11) . . C17 O7 Ni1 128.93(11) . . C17 O8 Ni2 127.86(11) . 17 C19 O9 Ni1 119.73(12) . . C19 N1 C20 121.25(17) . . C19 N1 C21 122.25(17) . . C21 N1 C20 116.34(17) . . O1 C1 C2 119.71(17) . . O1 C1 C6 122.81(16) . . C2 C1 C6 117.48(17) . . C3 C2 C1 121.8(2) . . C2 C3 C4 120.9(2) . . C5 C4 C3 119.4(2) . . C4 C5 C6 121.4(2) . . C4 C5 C10 118.71(19) . . C6 C5 C10 119.88(18) . . C1 C6 C7 122.48(16) . . C5 C6 C1 118.83(17) . . C5 C6 C7 118.64(17) . . O2 C7 C6 119.75(16) . . O2 C7 C8 118.84(16) . . C8 C7 C6 121.39(16) . . C9 C8 C7 118.08(17) . . C14 C8 C7 123.02(16) . . C14 C8 C9 118.62(17) . . C8 C9 C10 120.34(18) . . C11 C9 C8 121.2(2) . . C11 C9 C10 118.43(18) . . O4 C10 C5 120.1(2) . . O4 C10 C9 121.2(2) . . C9 C10 C5 118.62(17) . . C9 C11 C12 119.97(19) . . C13 C12 C11 120.18(18) . . C12 C13 C14 122.3(2) . . O3 C14 C8 124.90(15) . . O3 C14 C13 117.49(17) . . C13 C14 C8 117.61(17) . . O5 C15 C16 117.40(15) . . O6 C15 O5 124.13(15) . . O6 C15 C16 118.47(15) . . O7 C17 O8 126.27(16) . . O7 C17 C18 117.00(16) . . O8 C17 C18 116.73(16) . . O9 C19 N1 124.16(18) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 Ni2 2.9874(4) . Ni1 O1 2.0289(12) . Ni1 O2 2.0243(12) . Ni1 O3 2.0638(12) 18_545 Ni1 O5 2.0890(11) . Ni1 O7 1.9996(12) . Ni1 O9 2.0619(12) . Ni2 O1 2.0375(12) . Ni2 O2 2.0308(12) 18_545 Ni2 O3 2.0181(12) 18_545 Ni2 O5 2.1040(11) 18_545 Ni2 O6 2.0755(12) . Ni2 O8 2.0226(12) 18_545 O1 C1 1.314(2) . O2 Ni2 2.0306(12) 17 O2 C7 1.269(2) . O3 Ni1 2.0637(12) 17 O3 Ni2 2.0181(12) 17 O3 C14 1.321(2) . O4 C10 1.229(3) . O5 Ni2 2.1039(11) 17 O5 C15 1.285(2) . O6 C15 1.246(2) . O7 C17 1.255(2) . O8 Ni2 2.0222(12) 17 O8 C17 1.262(2) . O9 C19 1.248(2) . N1 C19 1.318(2) . N1 C20 1.455(2) . N1 C21 1.450(3) . C1 C2 1.414(3) . C1 C6 1.429(3) . C2 C3 1.377(3) . C3 C4 1.385(3) . C4 C5 1.376(3) . C5 C6 1.427(3) . C5 C10 1.483(3) . C6 C7 1.459(3) . C7 C8 1.448(3) . C8 C9 1.428(3) . C8 C14 1.426(3) . C9 C10 1.481(3) . C9 C11 1.376(3) . C11 C12 1.393(3) . C12 C13 1.370(3) . C13 C14 1.418(2) . C15 C16 1.503(2) . C17 C18 1.510(3) . 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 _geom_torsion_site_symmetry_1 Ni1 O1 C1 C2 142.85(15) . Ni1 O1 C1 C6 -37.9(2) . Ni1 O2 C7 C6 9.7(2) . Ni1 O2 C7 C8 -168.59(11) . Ni1 O3 C14 C8 -124.76(15) 17 Ni1 O3 C14 C13 54.43(19) 17 Ni1 O5 C15 O6 8.7(2) . Ni1 O5 C15 C16 -172.11(12) . Ni1 O7 C17 O8 -12.7(3) . Ni1 O7 C17 C18 167.79(14) . Ni1 O9 C19 N1 149.66(15) . Ni2 O1 C1 C2 -0.6(3) . Ni2 O1 C1 C6 178.67(12) . Ni2 O2 C7 C6 -131.66(13) 17 Ni2 O2 C7 C8 50.03(19) 17 Ni2 O3 C14 C8 1.2(2) 17 Ni2 O3 C14 C13 -179.62(11) 17 Ni2 O5 C15 O6 137.58(14) 17 Ni2 O5 C15 C16 -43.2(2) 17 Ni2 O6 C15 O5 -11.2(3) . Ni2 O6 C15 C16 169.61(13) . Ni2 O8 C17 O7 11.0(3) 17 Ni2 O8 C17 C18 -169.54(13) 17 O1 C1 C2 C3 -177.25(19) . O1 C1 C6 C5 178.87(16) . O1 C1 C6 C7 -3.8(3) . O2 C7 C8 C9 158.36(15) . O2 C7 C8 C14 -15.4(2) . C1 C2 C3 C4 -1.4(4) . C1 C6 C7 O2 19.6(2) . C1 C6 C7 C8 -162.11(16) . C2 C1 C6 C5 -1.9(3) . C2 C1 C6 C7 175.43(17) . C2 C3 C4 C5 -2.4(4) . C3 C4 C5 C6 3.9(3) . C3 C4 C5 C10 -175.6(2) . C4 C5 C6 C1 -1.8(3) . C4 C5 C6 C7 -179.17(19) . C4 C5 C10 O4 -7.4(3) . C4 C5 C10 C9 169.1(2) . C5 C6 C7 O2 -163.07(16) . C5 C6 C7 C8 15.2(2) . C6 C1 C2 C3 3.5(3) . C6 C5 C10 O4 173.1(2) . C6 C5 C10 C9 -10.4(3) . C6 C7 C8 C9 -19.9(2) . C6 C7 C8 C14 166.30(16) . C7 C8 C9 C10 9.1(3) . C7 C8 C9 C11 -170.23(17) . C7 C8 C14 O3 -11.5(3) . C7 C8 C14 C13 169.28(15) . C8 C9 C10 O4 -177.9(2) . C8 C9 C10 C5 5.6(3) . C8 C9 C11 C12 -1.1(3) . C9 C8 C14 O3 174.72(16) . C9 C8 C14 C13 -4.5(2) . C9 C11 C12 C13 -0.8(3) . C10 C5 C6 C1 177.71(17) . C10 C5 C6 C7 0.3(3) . C10 C9 C11 C12 179.50(19) . C11 C9 C10 O4 1.5(3) . C11 C9 C10 C5 -175.01(19) . C11 C12 C13 C14 0.0(3) . C12 C13 C14 O3 -176.57(16) . C12 C13 C14 C8 2.7(3) . C14 C8 C9 C10 -176.83(17) . C14 C8 C9 C11 3.8(3) . C20 N1 C19 O9 -178.52(18) . C21 N1 C19 O9 -3.2(3) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 867 202 'DMF, about 5 molecules' 2 0.333 0.667 1.167 864 202 'DMF, about 5 molecules' 3 0.667 0.333 0.833 864 202 'DMF, about 5 molecules'