#------------------------------------------------------------------------------ #$Date: 2018-01-13 00:25:15 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/43/4514360.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_4514360 loop_ _publ_author_name 'Pei, Lixia' 'Liu, Fengshou' 'Liao, Heng' 'Gao, Jie' 'Zhong, Liu' 'Gao, Haiyang' 'Wu, Qing' _publ_section_title ; Synthesis of Polyethylenes with Controlled Branching with \a-Diimine Nickel Catalysts and Revisiting Formation of Long-Chain Branching ; _journal_name_full 'ACS Catalysis' _journal_page_first 1104 _journal_paper_doi 10.1021/acscatal.7b03282 _journal_year 2018 _chemical_formula_moiety 'C48 H36 Br2 N2 Ni, 4(C H2 Cl2)' _chemical_formula_sum 'C52 H44 Br2 Cl8 N2 Ni' _chemical_formula_weight 1199.02 _space_group_crystal_system orthorhombic _space_group_IT_number 45 _space_group_name_Hall 'I 2 -2c' _space_group_name_H-M_alt 'I b a 2' _symmetry_space_group_name_Hall 'I 2 -2c' _symmetry_space_group_name_H-M 'I b a 2' _atom_sites_solution_hydrogens geom _audit_creation_date 2016-10-15 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.752(6) _cell_length_b 10.970(3) _cell_length_c 22.093(5) _cell_measurement_reflns_used 5144 _cell_measurement_temperature 173.15 _cell_measurement_theta_max 24.97 _cell_measurement_theta_min 2.47 _cell_volume 5999(3) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 173.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0549 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 13046 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.021 _diffrn_reflns_theta_min 1.843 _exptl_absorpt_coefficient_mu 2.044 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.511050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0864 before and 0.0441 after correction. The Ratio of minimum to maximum transmission is 0.5111. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.328 _exptl_crystal_description block _exptl_crystal_F_000 2416 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.385 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.065 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.042(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 296 _refine_ls_number_reflns 4181 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0346 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.0890 _reflns_Friedel_coverage 0.945 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.992 _reflns_number_gt 3323 _reflns_number_total 4181 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs7b03282_si_002.cif _cod_data_source_block 1_sq _cod_original_cell_volume 5999(2) _cod_database_code 4514360 _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 0.619 _shelx_estimated_absorpt_t_min 0.440 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.958(17) 0.042(17) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3.a Secondary CH2 refined with riding coordinates: C26(H26A,H26B), C27(H27A,H27B) 3.b Me refined with riding coordinates: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C) 3.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C12(H12), C14(H14), C23(H23), C24(H24), C25(H25) ; _shelx_res_file ; 1_sq.res created by SHELXL-2014/7 TITL 1 in Iba2 CELL 0.71073 24.752 10.9698 22.0933 90 90 90 ZERR 4 0.0058 0.0026 0.0052 0 0 0 LATT -2 SYMM -X,-Y,+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,+Z SFAC C H Br Cl N Ni UNIT 208 176 8 32 8 4 L.S. 10 0 42 PLAN 20 SIZE 0.48 0.28 0.26 TEMP -100 BOND MORE -1 BOND $H CONF ABIN fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 6 2 OMIT 4 1 -3 REM REM REM WGHT 0.047100 BASF 0.04161 FVAR 0.16146 NI1 6 0.000000 1.000000 0.110956 10.50000 0.01858 0.04509 = 0.02789 0.00000 0.00000 0.00395 BR1 3 0.025117 0.821803 0.161708 11.00000 0.03710 0.04192 = 0.04164 0.00469 -0.00185 0.00068 CL1 4 -0.035285 0.663535 0.374190 11.00000 0.10013 0.08142 = 0.07986 0.00849 0.02093 0.01808 CL2 4 0.074492 0.688850 0.334063 11.00000 0.09515 0.07594 = 0.11955 0.00416 0.01883 0.00174 CL3 4 -0.197360 1.299819 0.196031 11.00000 0.12125 0.06116 = 0.13351 0.01527 -0.02246 0.00494 CL4 4 -0.218239 1.052469 0.233311 11.00000 0.05665 0.07892 = 0.07871 0.00405 -0.00422 -0.00314 N1 5 -0.053887 1.000885 0.041776 11.00000 0.01485 0.02267 = 0.03423 -0.00041 -0.00107 -0.00105 C1 1 -0.112357 0.720579 0.124159 11.00000 0.01903 0.03323 = 0.06127 0.00376 -0.01174 -0.00729 C2 1 -0.134147 0.771450 0.179028 11.00000 0.04145 0.03994 = 0.05432 0.00429 -0.00692 -0.00102 AFIX 43 H2 2 -0.148481 0.851783 0.179343 11.00000 -1.20000 AFIX 0 C3 1 -0.133979 0.703241 0.230383 11.00000 0.08186 0.05514 = 0.06208 0.01160 -0.01265 -0.01083 AFIX 43 H3 2 -0.149804 0.736119 0.265993 11.00000 -1.20000 AFIX 0 C4 1 -0.111358 0.586312 0.232791 11.00000 0.08867 0.05284 = 0.08993 0.03169 -0.02308 -0.01394 AFIX 43 H4 2 -0.111959 0.541297 0.269519 11.00000 -1.20000 AFIX 0 C5 1 -0.088687 0.537837 0.182663 11.00000 0.05234 0.03751 = 0.09916 0.01421 -0.02019 -0.00450 AFIX 43 H5 2 -0.072776 0.459154 0.184873 11.00000 -1.20000 AFIX 0 C6 1 -0.088045 0.602780 0.125718 11.00000 0.02607 0.02130 = 0.07950 0.00530 -0.01692 -0.00279 C7 1 -0.066142 0.549409 0.074307 11.00000 0.02702 0.03145 = 0.10895 -0.00634 -0.00230 0.00035 AFIX 43 H7 2 -0.050662 0.470253 0.076176 11.00000 -1.20000 AFIX 0 C8 1 -0.067201 0.613819 0.019796 11.00000 0.03292 0.03747 = 0.11579 -0.02312 0.01237 0.00075 AFIX 43 H8 2 -0.052096 0.579107 -0.015778 11.00000 -1.20000 AFIX 0 C9 1 -0.090721 0.730136 0.017913 11.00000 0.02791 0.03505 = 0.05568 -0.00737 0.00587 -0.00301 AFIX 43 H9 2 -0.091318 0.773194 -0.019389 11.00000 -1.20000 AFIX 0 C10 1 -0.112952 0.783804 0.068410 11.00000 0.01777 0.03679 = 0.05820 -0.00172 0.00178 -0.00980 C11 1 -0.140154 0.905360 0.063274 11.00000 0.02378 0.02842 = 0.04112 -0.00038 0.00003 0.00148 C12 1 -0.195636 0.915717 0.071282 11.00000 0.01827 0.03904 = 0.05452 -0.00114 -0.00252 -0.00474 AFIX 43 H12 2 -0.215650 0.845638 0.082920 11.00000 -1.20000 AFIX 0 C13 1 -0.222821 1.025303 0.062818 11.00000 0.01962 0.04121 = 0.05376 -0.00098 0.00017 0.00145 C14 1 -0.192566 1.126817 0.045561 11.00000 0.02566 0.03192 = 0.04173 0.00105 -0.00265 0.00643 AFIX 43 H14 2 -0.210856 1.201813 0.039046 11.00000 -1.20000 AFIX 0 C15 1 -0.137655 1.123357 0.037569 11.00000 0.02965 0.02688 = 0.03151 -0.00241 -0.00129 0.00309 C16 1 -0.111841 1.010331 0.046776 11.00000 0.02067 0.02669 = 0.02935 -0.00041 0.00294 0.00079 C17 1 -0.284415 1.035149 0.071561 11.00000 0.02930 0.05708 = 0.08621 0.00529 0.00583 0.00040 AFIX 33 H17A 2 -0.296017 1.119045 0.063601 11.00000 -1.50000 H17B 2 -0.302674 0.979751 0.043408 11.00000 -1.50000 H17C 2 -0.293737 1.012912 0.113233 11.00000 -1.50000 AFIX 0 C18 1 -0.106744 1.234893 0.020815 11.00000 0.03502 0.03125 = 0.05326 0.00722 -0.00033 -0.00095 AFIX 33 H18A 2 -0.068316 1.214693 0.017142 11.00000 -1.50000 H18B 2 -0.120049 1.266310 -0.017941 11.00000 -1.50000 H18C 2 -0.111532 1.297046 0.052222 11.00000 -1.50000 AFIX 0 C19 1 -0.030584 1.003548 -0.008924 11.00000 0.01725 0.02025 = 0.03396 -0.00261 -0.00113 0.00072 C20 1 -0.047987 1.009580 -0.072534 11.00000 0.02598 0.02483 = 0.03594 -0.00130 -0.00343 0.00120 C21 1 0.000000 1.000000 -0.108316 10.50000 0.03554 0.02573 = 0.03083 0.00000 0.00000 0.00001 C22 1 0.000000 1.000000 -0.171127 10.50000 0.03991 0.03030 = 0.03382 0.00000 0.00000 0.00642 C23 1 -0.051192 1.013265 -0.199493 11.00000 0.04100 0.05486 = 0.03093 0.00142 -0.00813 0.00350 AFIX 43 H23 2 -0.053554 1.016190 -0.242386 11.00000 -1.20000 AFIX 0 C24 1 -0.097027 1.021827 -0.165293 11.00000 0.03746 0.04850 = 0.04044 -0.00460 -0.01484 0.00579 AFIX 43 H24 2 -0.130699 1.030504 -0.185473 11.00000 -1.20000 AFIX 0 C25 1 -0.096767 1.018430 -0.101940 11.00000 0.03178 0.03986 = 0.03316 -0.00321 -0.00533 0.00071 AFIX 43 H25 2 -0.129603 1.022161 -0.079754 11.00000 -1.20000 AFIX 0 C26 1 0.006450 0.677647 0.312703 11.00000 0.10023 0.04811 = 0.06885 -0.00744 0.00223 -0.00606 AFIX 23 H26A 2 -0.003844 0.751229 0.289463 11.00000 -1.20000 H26B 2 0.001723 0.605983 0.285987 11.00000 -1.20000 AFIX 0 C27 1 -0.170323 1.156876 0.208356 11.00000 0.03690 0.08692 = 0.07144 0.00316 -0.00405 0.00518 AFIX 23 H27A 2 -0.141174 1.163140 0.238880 11.00000 -1.20000 H27B 2 -0.154065 1.126724 0.170251 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in Iba2 REM R1 = 0.0346 for 3323 Fo > 4sig(Fo) and 0.0543 for all 4181 data REM 296 parameters refined using 1 restraints END WGHT 0.0471 0.0000 REM Highest difference peak 0.385, deepest hole -0.326, 1-sigma level 0.065 Q1 1 0.0488 0.8200 0.1301 11.00000 0.05 0.39 Q2 1 0.0410 0.8415 0.1999 11.00000 0.05 0.38 Q3 1 0.0725 0.6248 0.3003 11.00000 0.05 0.36 Q4 1 0.0002 0.8223 0.1962 11.00000 0.05 0.31 Q5 1 0.0254 0.9039 0.1850 11.00000 0.05 0.30 Q6 1 -0.1211 0.8086 0.1162 11.00000 0.05 0.30 Q7 1 -0.0267 0.9985 -0.0872 11.00000 0.05 0.30 Q8 1 0.0077 1.0491 0.0851 11.00000 0.05 0.30 Q9 1 0.0035 0.9208 0.1439 11.00000 0.05 0.29 Q10 1 0.0188 0.9931 0.1325 11.00000 0.05 0.28 Q11 1 -0.2697 1.0368 0.0788 11.00000 0.05 0.28 Q12 1 -0.0569 0.5131 0.0223 11.00000 0.05 0.28 Q13 1 0.0184 0.7771 0.1996 11.00000 0.05 0.27 Q14 1 0.0000 0.5000 0.1294 10.50000 0.05 0.26 Q15 1 -0.0414 1.0241 -0.0390 11.00000 0.05 0.26 Q16 1 0.0000 1.0000 -0.2727 10.50000 0.05 0.26 Q17 1 -0.1213 0.7997 0.1644 11.00000 0.05 0.25 Q18 1 -0.2199 1.1203 0.2606 11.00000 0.05 0.25 Q19 1 0.0268 0.8869 0.1268 11.00000 0.05 0.25 Q20 1 -0.0523 0.4397 0.0715 11.00000 0.05 0.25 ; _shelx_res_checksum 43497 _shelx_hkl_file ; 0 -2 0 46.24 3.03 0 -4 0 2461.58 126.62 0 -6 0 2965.19 152.75 0 -8 0 54.26 6.66 0 -10 0 381.12 22.62 0 -12 0 72.76 10.17 0 -1 -1 0.36 0.52 0 -1 1 -0.54 0.32 0 1 -1 -0.16 0.37 0 1 -1 0.77 0.47 0 -3 -1 -0.23 1.35 0 -3 1 1.36 0.74 0 3 -1 1.22 0.92 0 3 -1 -1.86 1.21 0 -5 1 -2.64 2.00 0 -5 -1 -1.61 2.24 0 -7 -1 -7.13 3.31 0 -7 1 2.12 3.36 0 -9 -1 4.66 5.10 0 -9 1 0.29 4.95 0 -11 -1 -4.64 6.78 0 -11 1 -13.78 6.53 0 -13 -1 -16.45 8.76 0 0 -2 2444.17 126.04 0 2 -2 1345.15 74.41 0 2 -2 1356.77 62.84 0 -2 -2 1404.70 71.27 0 -2 2 1429.40 71.28 0 4 -2 189.86 11.56 0 -4 -2 218.86 11.32 0 4 -2 194.92 9.95 0 -6 2 61.98 5.13 0 -6 -2 76.06 6.24 0 -8 -2 1054.86 55.76 0 -10 -2 76.58 8.86 0 -10 2 53.55 7.50 0 -12 -2 5.91 8.19 0 -1 -3 0.57 1.05 0 1 -3 0.59 0.92 0 1 -3 1.34 0.86 0 3 -3 0.13 1.22 0 -3 3 1.02 1.26 0 3 -3 2.12 1.41 0 -3 -3 -1.69 1.56 0 -5 -3 -1.42 2.46 0 5 -3 1.29 2.11 0 -5 3 0.46 2.08 0 5 -3 -2.56 2.05 0 -7 3 -3.47 1.92 0 7 -3 -4.95 2.97 0 -7 -3 -3.21 3.28 0 -9 3 -4.75 2.95 0 -9 -3 -4.61 5.03 0 -11 -3 -0.29 7.10 0 -11 3 -3.74 4.51 0 -13 -3 -13.05 8.80 0 2 -4 2381.29 125.17 0 2 -4 2342.62 110.40 0 -2 -4 2584.66 125.22 0 4 -4 116.23 7.22 0 -4 4 116.24 7.10 0 -4 -4 115.25 7.33 0 4 -4 128.37 6.57 0 6 -4 1303.86 60.01 0 -6 -4 1348.21 68.10 0 6 -4 1284.86 70.78 0 -6 4 1290.71 67.94 0 -8 4 570.09 29.82 0 -8 -4 537.82 29.88 0 8 -4 528.37 26.36 0 -10 -4 73.24 8.21 0 -10 4 46.21 7.15 0 -12 -4 69.07 9.99 0 -1 -5 -0.41 1.26 0 1 -5 -0.98 1.17 0 -1 -5 0.37 0.76 0 1 -5 -0.09 0.99 0 3 -5 0.30 1.52 0 -3 -5 -1.45 1.65 0 5 -5 -0.87 1.93 0 5 -5 -0.63 2.33 0 -5 -5 -0.21 2.56 0 -5 5 -1.86 2.21 0 7 -5 -0.88 3.13 0 -7 -5 -1.67 3.61 0 -7 5 2.87 3.13 0 7 -5 0.68 2.73 0 -9 -5 -5.03 4.78 0 -9 5 -5.32 5.22 0 -11 -5 -7.06 7.12 0 -13 -5 -9.73 7.84 0 0 -6 7695.10 387.84 0 0 -6 7437.22 342.07 0 2 -6 4726.26 219.80 0 -2 -6 5093.24 219.83 0 2 -6 4775.64 249.15 0 -2 -6 4837.71 249.22 0 -4 6 154.86 8.69 0 4 -6 140.64 8.82 0 4 -6 138.35 7.88 0 -4 -6 160.99 9.12 0 6 -6 602.52 28.04 0 -6 -6 545.85 31.67 0 6 -6 571.90 32.67 0 -6 6 650.97 31.60 0 -8 -6 197.21 12.96 0 -8 6 229.11 12.73 0 8 -6 170.04 12.37 0 8 -6 191.80 11.40 0 -10 -6 26.59 6.92 0 -12 -6 42.67 9.37 0 -1 -7 -0.50 1.54 0 1 -7 -1.13 1.18 0 -1 -7 -0.01 0.65 0 1 -7 -0.05 1.35 0 3 -7 -2.82 1.61 0 3 -7 -2.83 1.86 0 -3 -7 2.00 2.03 0 5 -7 0.42 2.63 0 5 -7 -1.32 2.02 0 -5 7 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12 6 2 -0.65 0.96 14 6 2 0.74 -1.13 16 6 2 -0.22 0.35 18 6 2 -0.39 0.03 20 6 2 0.66 0.60 22 6 2 -0.64 -1.31 24 6 2 0.67 1.10 26 6 2 -0.81 -0.30 1 7 2 -0.59 0.00 3 7 2 0.99 0.32 5 7 2 -0.73 -0.27 7 7 2 0.46 -1.08 9 7 2 -0.34 2.21 11 7 2 -0.13 -0.99 13 7 2 0.95 -1.36 15 7 2 -1.37 2.06 17 7 2 1.07 -0.83 19 7 2 -0.40 -0.69 21 7 2 -0.36 1.98 23 7 2 0.97 -2.94 25 7 2 -1.02 2.59 0 8 2 -1.67 -3.67 2 8 2 1.71 3.37 4 8 2 -1.72 -2.74 6 8 2 1.03 2.15 8 8 2 -0.18 -1.90 10 8 2 0.40 1.97 12 8 2 -1.50 -2.12 14 8 2 2.09 1.97 16 8 2 -1.75 -1.33 18 8 2 1.06 0.67 20 8 2 -0.31 -0.50 22 8 2 -0.34 0.42 24 8 2 0.51 0.06 1 9 2 0.03 -0.01 3 9 2 -0.19 -0.43 5 9 2 0.48 1.18 7 9 2 -0.42 -1.36 9 9 2 0.04 1.01 11 9 2 -0.24 -0.57 13 9 2 0.98 0.13 15 9 2 -0.91 0.03 17 9 2 -0.17 0.27 19 9 2 0.84 -0.58 21 9 2 -0.48 0.33 0 10 2 -4.35 0.87 2 10 2 3.23 -1.45 4 10 2 -0.81 2.53 6 10 2 -0.82 -2.95 8 10 2 0.66 2.67 10 10 2 0.19 -2.45 12 10 2 0.34 1.83 14 10 2 -2.69 -0.12 16 10 2 4.57 -1.34 18 10 2 -4.04 0.95 20 10 2 2.09 0.38 1 11 2 1.33 -0.41 3 11 2 -2.91 1.07 5 11 2 2.23 -1.43 7 11 2 -0.41 1.60 9 11 2 -0.87 -1.73 11 11 2 0.81 1.92 13 11 2 0.00 -1.58 15 11 2 -0.24 0.06 17 11 2 -0.28 1.45 0 12 2 -2.22 -1.30 2 12 2 1.39 1.67 4 12 2 -0.01 -1.55 6 12 2 -0.81 -0.21 8 12 2 0.92 1.95 10 12 2 -0.56 -1.74 12 12 2 0.01 0.07 1 13 2 0.69 -0.30 3 13 2 -1.37 0.33 5 13 2 0.92 0.19 7 13 2 -0.10 -0.39 2 1 1 -7.82 1.50 4 1 1 15.72 -5.78 6 1 1 -21.02 10.58 8 1 1 20.91 -12.25 10 1 1 -16.01 10.31 12 1 1 8.90 -6.36 14 1 1 -1.32 1.29 16 1 1 -5.18 3.67 18 1 1 8.36 -6.08 20 1 1 -7.59 5.05 22 1 1 4.63 -2.46 24 1 1 -1.56 0.38 26 1 1 -0.52 0.66 28 1 1 1.00 -0.71 1 2 1 -21.40 9.98 3 2 1 10.69 -2.80 5 2 1 1.50 -4.88 7 2 1 -6.41 7.03 9 2 1 3.77 -4.01 11 2 1 0.57 0.10 13 2 1 -2.39 1.87 15 2 1 1.90 -1.87 17 2 1 -0.93 0.87 19 2 1 0.29 0.26 21 2 1 0.45 -0.98 23 2 1 -1.60 1.26 25 2 1 2.31 -1.28 27 2 1 -1.82 1.13 29 2 1 0.73 -0.85 2 3 1 8.57 -3.30 4 3 1 -11.93 4.90 6 3 1 8.76 -3.80 8 3 1 -3.04 1.17 10 3 1 -0.15 0.63 12 3 1 0.16 -0.66 14 3 1 0.09 0.08 16 3 1 1.23 -0.39 18 3 1 -2.98 1.72 20 3 1 2.97 -2.70 22 3 1 -0.83 2.06 24 3 1 -1.47 -0.18 26 3 1 2.17 -1.34 28 3 1 -1.39 1.40 1 4 1 8.74 -6.33 3 4 1 -5.99 4.14 5 4 1 1.72 -0.65 7 4 1 2.78 -2.48 9 4 1 -5.71 3.88 11 4 1 5.67 -3.42 13 4 1 -3.39 1.98 15 4 1 0.55 -0.15 17 4 1 1.68 -1.63 19 4 1 -2.25 2.20 21 4 1 1.12 -1.03 23 4 1 -0.08 -0.38 25 4 1 0.28 0.56 27 4 1 -0.70 -0.05 29 4 1 0.41 -0.07 2 5 1 -0.58 0.22 4 5 1 0.85 -0.36 6 5 1 -0.51 0.07 8 5 1 -0.83 0.90 12 5 1 -2.19 1.68 14 5 1 1.47 -1.07 16 5 1 -2.06 1.44 18 5 1 3.15 -2.34 20 5 1 -2.87 2.34 22 5 1 1.66 -1.48 24 5 1 -0.93 0.90 26 5 1 0.79 -0.97 28 5 1 -0.75 1.18 1 6 1 -7.65 5.46 3 6 1 3.71 -2.99 5 6 1 1.59 -0.64 7 6 1 -4.56 2.94 9 6 1 4.16 -2.78 11 6 1 -2.21 1.20 13 6 1 -0.06 0.61 15 6 1 1.93 -1.81 17 6 1 -1.51 1.13 19 6 1 -1.62 1.65 21 6 1 4.73 -4.39 23 6 1 -5.20 4.71 25 6 1 3.33 -2.75 27 6 1 -1.19 0.76 2 7 1 3.75 -3.10 4 7 1 -3.38 2.99 6 7 1 -0.56 -0.24 8 7 1 3.31 -1.81 10 7 1 -2.39 1.53 12 7 1 0.37 -0.40 14 7 1 0.33 -0.23 16 7 1 -0.54 0.68 18 7 1 1.31 -1.20 20 7 1 -2.35 1.51 22 7 1 2.95 -1.45 24 7 1 -2.42 0.98 26 7 1 0.95 -0.23 1 8 1 -5.31 4.00 3 8 1 2.11 -1.56 5 8 1 0.58 -0.44 7 8 1 -0.30 0.37 9 8 1 -0.88 0.12 11 8 1 0.19 0.63 13 8 1 1.32 -1.73 15 8 1 -1.36 1.97 17 8 1 -0.07 -1.52 19 8 1 1.91 0.50 21 8 1 -3.13 0.94 23 8 1 2.59 -1.65 2 9 1 3.43 -1.81 4 9 1 -3.56 1.73 6 9 1 0.10 0.24 8 9 1 3.41 -2.12 10 9 1 -4.02 2.44 12 9 1 2.55 -1.81 14 9 1 -0.77 0.95 16 9 1 -1.23 0.41 18 9 1 3.45 -2.18 20 9 1 -4.82 3.37 22 9 1 4.30 -3.08 1 10 1 1.51 -1.98 3 10 1 -4.19 3.42 5 10 1 6.68 -4.51 7 10 1 -5.58 3.43 9 10 1 1.64 -0.84 11 10 1 1.04 -0.87 13 10 1 -0.94 1.09 15 10 1 0.42 -1.40 17 10 1 -1.08 2.39 19 10 1 1.62 -2.74 2 11 1 2.70 -2.24 4 11 1 -2.55 1.91 6 11 1 -0.01 0.44 8 11 1 1.54 -1.72 10 11 1 -0.10 0.41 12 11 1 -2.28 1.74 14 11 1 2.91 -2.61 16 11 1 -1.73 2.03 1 12 1 -3.71 3.35 3 12 1 2.61 -1.64 5 12 1 -1.85 0.42 7 12 1 2.50 -1.26 9 12 1 -3.50 2.77 11 12 1 3.09 -2.67 13 12 1 -1.53 1.12 2 13 1 -3.02 2.27 4 13 1 4.21 -3.38 6 13 1 -3.53 3.18 8 13 1 1.86 -2.00 6 0 0 -27.89 0.14 8 0 0 -12.85 0.06 10 0 0 9.49 -0.03 12 0 0 3.58 0.06 14 0 0 -10.25 -0.15 16 0 0 11.47 0.08 18 0 0 -10.43 0.01 20 0 0 7.42 0.04 22 0 0 -4.02 -0.03 24 0 0 2.55 -0.07 26 0 0 -2.73 0.06 1 1 0 -27.43 0.63 3 1 0 60.88 0.27 5 1 0 -53.91 -0.83 7 1 0 25.51 0.54 9 1 0 -2.60 -0.03 11 1 0 -4.93 -0.18 13 1 0 2.44 0.11 15 1 0 1.84 -0.01 17 1 0 -4.62 0.00 19 1 0 5.76 0.00 21 1 0 -4.68 -0.01 23 1 0 2.53 -0.04 25 1 0 -1.84 0.07 27 1 0 2.01 0.04 0 2 0 -44.28 -0.01 2 2 0 40.01 -2.09 4 2 0 -27.41 2.06 6 2 0 10.08 -0.62 8 2 0 4.85 -0.27 10 2 0 -12.85 0.18 12 2 0 13.47 0.11 14 2 0 -8.84 -0.13 16 2 0 3.30 0.08 18 2 0 -0.03 -0.09 20 2 0 -1.09 0.00 22 2 0 0.53 0.12 24 2 0 0.79 -0.02 26 2 0 -0.22 -0.19 28 2 0 -2.35 0.14 1 3 0 -1.96 0.91 3 3 0 2.81 -0.26 5 3 0 0.47 -0.23 7 3 0 -3.07 0.20 9 3 0 2.52 0.01 11 3 0 -0.67 -0.09 13 3 0 0.17 0.04 15 3 0 -1.79 0.03 17 3 0 3.26 -0.04 19 3 0 -2.38 0.04 21 3 0 0.27 -0.05 23 3 0 1.09 -0.05 25 3 0 -1.16 0.18 27 3 0 -0.18 -0.16 29 3 0 1.91 0.03 0 4 0 2.71 0.00 2 4 0 -1.74 0.01 4 4 0 -0.17 -0.15 6 4 0 2.33 0.21 8 4 0 -5.06 -0.08 10 4 0 6.82 -0.04 12 4 0 -5.26 0.02 14 4 0 0.68 0.00 16 4 0 3.97 0.03 18 4 0 -5.40 -0.08 20 4 0 2.96 0.04 22 4 0 0.31 0.06 24 4 0 -1.57 -0.08 26 4 0 1.26 0.00 28 4 0 -0.52 0.04 1 5 0 2.26 0.23 3 5 0 -5.37 0.10 5 5 0 5.63 -0.23 7 5 0 -4.39 0.05 9 5 0 3.64 0.07 11 5 0 -3.22 0.00 13 5 0 2.00 -0.03 15 5 0 0.03 -0.05 17 5 0 -1.98 0.07 19 5 0 2.29 0.04 21 5 0 0.44 -0.08 23 5 0 -4.44 -0.02 25 5 0 5.67 0.06 27 5 0 -3.30 0.01 0 6 0 -1.46 0.00 2 6 0 1.33 0.09 4 6 0 -0.49 -0.06 6 6 0 -0.86 -0.06 8 6 0 1.16 0.13 10 6 0 0.08 -0.08 12 6 0 -1.30 0.01 14 6 0 1.10 0.02 16 6 0 -0.08 -0.03 18 6 0 -0.15 0.01 20 6 0 -0.76 0.02 22 6 0 1.54 -0.01 24 6 0 -1.19 -0.04 26 6 0 0.20 0.04 1 7 0 -0.32 -0.13 5 7 0 -0.08 0.09 7 7 0 1.04 -0.05 9 7 0 -2.02 -0.03 11 7 0 0.77 0.04 13 7 0 1.70 0.01 15 7 0 -2.45 -0.06 17 7 0 1.16 0.05 19 7 0 0.46 0.02 21 7 0 -1.93 -0.06 23 7 0 3.17 0.02 25 7 0 -2.95 0.05 0 8 0 3.09 0.00 2 8 0 -2.75 -0.11 4 8 0 2.11 -0.01 6 8 0 -1.91 0.14 8 8 0 2.17 -0.05 10 8 0 -2.27 -0.05 12 8 0 1.90 -0.08 14 8 0 -1.24 0.21 16 8 0 0.45 -0.07 18 8 0 -0.07 -0.13 20 8 0 0.52 0.05 22 8 0 -0.97 0.12 24 8 0 0.52 -0.10 1 9 0 0.03 0.05 3 9 0 0.27 0.00 5 9 0 -0.83 0.00 7 9 0 1.02 -0.04 9 9 0 -0.88 0.02 11 9 0 0.53 0.05 13 9 0 -0.02 -0.01 15 9 0 -0.10 -0.11 17 9 0 -0.39 0.08 19 9 0 0.70 0.06 21 9 0 -0.34 -0.09 0 10 0 -2.07 -0.01 2 10 0 2.41 0.03 4 10 0 -2.97 0.04 6 10 0 3.02 -0.07 8 10 0 -2.82 -0.01 10 10 0 2.85 0.07 12 10 0 -2.00 -0.01 14 10 0 -0.60 -0.08 16 10 0 2.77 0.09 18 10 0 -2.18 0.00 20 10 0 0.12 -0.06 1 11 0 0.96 -0.08 3 11 0 -2.20 0.06 5 11 0 2.17 -0.01 7 11 0 -1.43 -0.05 9 11 0 0.94 0.07 11 11 0 -1.32 -0.03 13 11 0 1.62 -0.01 15 11 0 -0.38 0.01 17 11 0 -1.45 0.00 0 12 0 0.64 0.01 2 12 0 -1.46 -0.12 4 12 0 2.17 0.09 6 12 0 -0.88 -0.01 8 12 0 -1.02 0.04 10 12 0 1.32 -0.09 12 12 0 0.00 0.01 14 12 0 -1.30 0.09 1 13 0 0.56 0.01 3 13 0 -0.90 0.00 5 13 0 0.19 0.01 7 13 0 0.43 -0.06 10 5 1 2.25 -1.84 22 6 4 -0.89 0.95 16 11 7 -0.75 -0.11 21 9 8 -0.89 -1.89 2 0 0 -256.47 0.37 4 0 0 131.59 -0.42 28 0 0 3.40 0.10 30 0 0 -3.54 -0.16 29 1 0 -1.08 -0.11 30 2 0 3.49 0.05 3 7 0 0.32 0.01 23 9 0 -0.21 -0.01 9 13 0 -0.39 0.07 30 1 1 -0.26 -0.04 30 3 1 0.21 -0.36 18 11 1 0.26 -0.90 30 0 2 0.61 3.25 23 9 2 -0.03 0.26 14 12 2 0.27 1.15 9 13 2 -0.32 0.11 29 4 3 -0.02 -0.70 26 7 3 0.63 -1.30 8 13 3 -1.43 -1.43 0 0 4 -193.46 -102.34 30 2 4 -3.36 2.44 30 1 5 1.31 0.00 28 5 5 0.22 -0.37 27 6 5 0.07 0.12 30 0 6 -0.17 -1.40 29 3 6 1.33 0.47 24 8 6 0.38 -1.30 5 13 6 -1.62 -2.25 4 13 7 -0.51 1.21 28 4 8 -0.15 0.24 27 5 8 -0.06 -0.91 26 6 8 1.25 -0.62 1 13 8 -1.53 0.64 28 3 9 0.56 2.23 28 2 10 -1.29 -0.73 22 8 10 -0.11 -0.15 28 1 11 0.33 0.39 7 12 11 1.87 0.98 26 4 12 -0.46 0.55 25 5 12 0.48 -0.33 24 6 12 1.34 0.46 16 10 12 0.30 0.91 4 12 12 -0.39 0.63 26 3 13 0.37 -0.50 22 7 13 -1.08 0.84 18 9 13 -1.42 -1.56 15 10 13 -0.48 -0.13 1 12 13 3.03 3.47 26 2 14 -1.06 -0.90 21 7 14 -2.42 -0.97 17 9 14 -0.15 0.15 9 11 14 1.57 -0.29 20 7 15 -1.98 -0.17 6 11 15 -0.75 -0.57 19 7 16 0.82 -0.10 10 10 16 1.00 0.04 1 11 16 -0.24 0.10 3 11 16 0.72 -0.24 24 1 17 -0.98 -0.77 18 7 17 0.68 -1.67 23 1 18 1.36 -1.82 17 7 18 -0.74 0.44 11 9 18 -0.76 1.34 4 10 18 0.69 1.33 22 1 19 0.29 -1.16 13 8 19 -0.13 0.29 8 9 19 -1.00 -2.22 21 1 20 0.72 1.17 16 6 20 0.41 0.63 5 9 20 0.11 -1.49 19 2 21 1.55 -0.20 16 5 21 0.16 1.23 12 7 21 -1.14 -0.78 18 0 22 1.81 -0.14 17 3 22 0.16 -1.58 16 4 22 1.23 1.25 12 6 22 0.09 0.46 9 7 22 0.96 1.04 0 8 22 1.10 0.32 2 8 22 -0.78 -0.12 12 5 23 0.69 -0.46 4 7 23 2.11 0.66 14 2 24 0.27 1.47 13 3 24 0.02 -0.01 12 4 24 0.81 -0.05 9 5 24 -0.59 0.82 6 6 24 -0.46 0.61 12 1 25 -0.72 -0.44 10 3 25 -0.03 -1.29 9 4 25 0.49 0.25 6 5 25 2.21 -0.31 10 0 26 1.37 -1.03 9 1 26 -0.96 0.61 8 2 26 -1.76 -0.27 7 3 26 0.99 1.26 0 4 26 -1.26 1.34 2 4 26 1.18 -1.25 4 4 26 -0.96 1.06 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 50315) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.250 -0.010 0.390 271 74 ' ' 2 0.750 -0.023 0.390 271 74 ' ' 3 0.250 -0.022 0.890 271 74 ' ' 4 0.750 -0.010 0.890 271 74 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 2 0 0 1.645 4 0 0 3.292 0 0 4 3.689 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL 1 I b a 2 R = 0.05 CELL 24.7520 10.9700 22.0930 90.00 90.00 90.00 SPGR Iba2 # Solvent Accessible Volume = 1123.1 # Electrons Found in S.A.V. = 294.9 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.712 0.745 0.404 ! 2.57 eA-3 C102 0.191 0.291 0.390 ! 2.17 eA-3 C103 0.729 0.857 0.388 ! 2.16 eA-3 C104 0.307 0.971 0.389 ! 2.04 eA-3 C105 0.243 0.234 0.384 ! 2.02 eA-3 C106 0.741 0.190 0.390 ! 1.89 eA-3 C107 0.238 0.374 0.402 ! 1.87 eA-3 C108 0.300 0.085 0.386 ! 1.86 eA-3 C109 0.760 0.536 0.397 ! 1.82 eA-3 C110 0.262 0.078 0.391 ! 1.78 eA-3 Q111 0.500 0.506 0.109 ! 1.11 eA-3 Q112 0.525 0.699 0.163 ! 1.03 eA-3 Q113 0.683 0.685 0.469 ! 0.59 eA-3 C114 0.651 0.188 0.392 ! 0.57 eA-3 Q115 0.845 0.420 0.371 ! 0.56 eA-3 Q116 0.757 0.579 0.469 ! 0.54 eA-3 C117 0.790 0.919 0.380 ! 0.54 eA-3 Q118 0.593 0.814 0.346 ! 0.52 eA-3 C119 0.778 0.025 0.447 ! 0.52 eA-3 C120 0.180 0.617 0.343 ! 0.50 eA-3 ) ; _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, 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 Ni1 Ni 0.0000 1.0000 0.11096(4) 0.0305(2) Uani 1 2 d S T P Br1 Br 0.02512(2) 0.82180(4) 0.16171(3) 0.04022(15) Uani 1 1 d . . . Cl1 Cl -0.03528(9) 0.6635(2) 0.37419(11) 0.0871(7) Uani 1 1 d . . . Cl2 Cl 0.07449(11) 0.6889(2) 0.33406(14) 0.0969(8) Uani 1 1 d . . . Cl3 Cl -0.19736(12) 1.2998(2) 0.19603(15) 0.1053(8) Uani 1 1 d . . . Cl4 Cl -0.21824(7) 1.05247(19) 0.23331(10) 0.0714(5) Uani 1 1 d . . . N1 N -0.05389(14) 1.0009(4) 0.04178(19) 0.0239(8) Uani 1 1 d . . . C1 C -0.1124(2) 0.7206(5) 0.1242(3) 0.0378(14) Uani 1 1 d . . . C2 C -0.1341(2) 0.7715(5) 0.1790(3) 0.0452(15) Uani 1 1 d . . . H2 H -0.1485 0.8518 0.1793 0.054 Uiso 1 1 calc R . . C3 C -0.1340(3) 0.7032(6) 0.2304(4) 0.066(2) Uani 1 1 d . . . H3 H -0.1498 0.7361 0.2660 0.080 Uiso 1 1 calc R . . C4 C -0.1114(3) 0.5863(7) 0.2328(4) 0.077(2) Uani 1 1 d . . . H4 H -0.1120 0.5413 0.2695 0.093 Uiso 1 1 calc R . . C5 C -0.0887(3) 0.5378(6) 0.1827(4) 0.063(2) Uani 1 1 d . . . H5 H -0.0728 0.4592 0.1849 0.076 Uiso 1 1 calc R . . C6 C -0.0880(2) 0.6028(5) 0.1257(3) 0.0423(16) Uani 1 1 d . . . C7 C -0.0661(2) 0.5494(6) 0.0743(4) 0.0558(19) Uani 1 1 d . . . H7 H -0.0507 0.4703 0.0762 0.067 Uiso 1 1 calc R . . C8 C -0.0672(2) 0.6138(6) 0.0198(4) 0.062(2) Uani 1 1 d . . . H8 H -0.0521 0.5791 -0.0158 0.074 Uiso 1 1 calc R . . C9 C -0.0907(2) 0.7301(5) 0.0179(3) 0.0395(13) Uani 1 1 d . . . H9 H -0.0913 0.7732 -0.0194 0.047 Uiso 1 1 calc R . . C10 C -0.1130(2) 0.7838(5) 0.0684(3) 0.0376(14) Uani 1 1 d . . . C11 C -0.1402(2) 0.9054(5) 0.0633(2) 0.0311(12) Uani 1 1 d . . . C12 C -0.19564(19) 0.9157(5) 0.0713(3) 0.0373(13) Uani 1 1 d . . . H12 H -0.2157 0.8456 0.0829 0.045 Uiso 1 1 calc R . . C13 C -0.2228(2) 1.0253(5) 0.0628(3) 0.0382(13) Uani 1 1 d . . . C14 C -0.1926(2) 1.1268(5) 0.0456(2) 0.0331(12) Uani 1 1 d . . . H14 H -0.2109 1.2018 0.0390 0.040 Uiso 1 1 calc R . . C15 C -0.1377(2) 1.1234(4) 0.0376(2) 0.0293(11) Uani 1 1 d . . . C16 C -0.11184(18) 1.0103(4) 0.0468(2) 0.0256(10) Uani 1 1 d . . . C17 C -0.2844(2) 1.0351(6) 0.0716(4) 0.0575(19) Uani 1 1 d . . . H17A H -0.2960 1.1190 0.0636 0.086 Uiso 1 1 calc R . . H17B H -0.3027 0.9798 0.0434 0.086 Uiso 1 1 calc R . . H17C H -0.2937 1.0129 0.1132 0.086 Uiso 1 1 calc R . . C18 C -0.1067(2) 1.2349(5) 0.0208(3) 0.0398(13) Uani 1 1 d . . . H18A H -0.0683 1.2147 0.0171 0.060 Uiso 1 1 calc R . . H18B H -0.1200 1.2663 -0.0179 0.060 Uiso 1 1 calc R . . H18C H -0.1115 1.2970 0.0522 0.060 Uiso 1 1 calc R . . C19 C -0.03058(17) 1.0035(5) -0.0089(2) 0.0238(10) Uani 1 1 d . . . C20 C -0.0480(2) 1.0096(5) -0.0725(3) 0.0289(12) Uani 1 1 d . . . C21 C 0.0000 1.0000 -0.1083(3) 0.0307(17) Uani 1 2 d S T P C22 C 0.0000 1.0000 -0.1711(4) 0.0347(18) Uani 1 2 d S T P C23 C -0.0512(2) 1.0133(6) -0.1995(3) 0.0423(15) Uani 1 1 d . . . H23 H -0.0536 1.0162 -0.2424 0.051 Uiso 1 1 calc R . . C24 C -0.0970(2) 1.0218(5) -0.1653(3) 0.0421(14) Uani 1 1 d . . . H24 H -0.1307 1.0305 -0.1855 0.051 Uiso 1 1 calc R . . C25 C -0.0968(2) 1.0184(5) -0.1019(2) 0.0349(13) Uani 1 1 d . . . H25 H -0.1296 1.0222 -0.0798 0.042 Uiso 1 1 calc R . . C26 C 0.0065(4) 0.6776(6) 0.3127(4) 0.072(2) Uani 1 1 d . . . H26A H -0.0038 0.7512 0.2895 0.087 Uiso 1 1 calc R . . H26B H 0.0017 0.6060 0.2860 0.087 Uiso 1 1 calc R . . C27 C -0.1703(3) 1.1569(6) 0.2084(4) 0.0651(19) Uani 1 1 d . . . H27A H -0.1412 1.1631 0.2389 0.078 Uiso 1 1 calc R . . H27B H -0.1541 1.1267 0.1703 0.078 Uiso 1 1 calc R . . 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 0.0186(4) 0.0451(5) 0.0279(4) 0.000 0.000 0.0039(4) Br1 0.0371(3) 0.0419(3) 0.0416(3) 0.0047(3) -0.0018(3) 0.0007(2) Cl1 0.1001(16) 0.0814(15) 0.0799(15) 0.0085(11) 0.0209(12) 0.0181(11) Cl2 0.0952(16) 0.0759(14) 0.120(2) 0.0042(13) 0.0188(16) 0.0017(12) Cl3 0.121(2) 0.0612(13) 0.134(2) 0.0153(13) -0.0225(18) 0.0049(12) Cl4 0.0567(11) 0.0789(13) 0.0787(13) 0.0040(10) -0.0042(10) -0.0031(9) N1 0.0149(18) 0.023(2) 0.034(2) -0.0004(18) -0.0011(16) -0.0011(17) C1 0.019(3) 0.033(3) 0.061(4) 0.004(3) -0.012(2) -0.007(2) C2 0.041(3) 0.040(3) 0.054(4) 0.004(3) -0.007(3) -0.001(3) C3 0.082(5) 0.055(5) 0.062(4) 0.012(4) -0.013(4) -0.011(4) C4 0.089(6) 0.053(5) 0.090(6) 0.032(5) -0.023(5) -0.014(4) C5 0.052(4) 0.038(4) 0.099(6) 0.014(4) -0.020(4) -0.004(3) C6 0.026(3) 0.021(3) 0.079(5) 0.005(3) -0.017(3) -0.003(2) C7 0.027(3) 0.031(3) 0.109(6) -0.006(4) -0.002(3) 0.000(3) C8 0.033(3) 0.037(4) 0.116(7) -0.023(4) 0.012(4) 0.001(3) C9 0.028(3) 0.035(3) 0.056(4) -0.007(3) 0.006(3) -0.003(2) C10 0.018(3) 0.037(3) 0.058(4) -0.002(3) 0.002(3) -0.010(2) C11 0.024(3) 0.028(3) 0.041(3) 0.000(2) 0.000(2) 0.001(2) C12 0.018(3) 0.039(3) 0.055(4) -0.001(3) -0.003(2) -0.005(2) C13 0.020(3) 0.041(3) 0.054(4) -0.001(3) 0.000(2) 0.001(2) C14 0.026(3) 0.032(3) 0.042(3) 0.001(2) -0.003(2) 0.006(2) C15 0.030(3) 0.027(3) 0.032(3) -0.002(2) -0.001(2) 0.003(2) C16 0.021(2) 0.027(3) 0.029(3) 0.000(2) 0.0029(19) 0.001(2) C17 0.029(3) 0.057(4) 0.086(5) 0.005(4) 0.006(3) 0.000(3) C18 0.035(3) 0.031(3) 0.053(3) 0.007(3) 0.000(3) -0.001(2) C19 0.017(2) 0.020(3) 0.034(3) -0.003(2) -0.0011(19) 0.001(2) C20 0.026(3) 0.025(3) 0.036(3) -0.001(3) -0.003(2) 0.001(2) C21 0.036(4) 0.026(4) 0.031(4) 0.000 0.000 0.000(4) C22 0.040(5) 0.030(4) 0.034(5) 0.000 0.000 0.006(4) C23 0.041(3) 0.055(4) 0.031(3) 0.001(3) -0.008(3) 0.003(3) C24 0.037(3) 0.049(3) 0.040(3) -0.005(3) -0.015(3) 0.006(3) C25 0.032(3) 0.040(4) 0.033(3) -0.003(3) -0.005(2) 0.001(3) C26 0.100(6) 0.048(4) 0.069(5) -0.007(3) 0.002(5) -0.006(4) C27 0.037(3) 0.087(5) 0.071(5) 0.003(4) -0.004(3) 0.005(3) 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' Br Br -0.2901 2.4595 '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' 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 Br1 Ni1 Br1 122.67(6) . 2_575 N1 Ni1 Br1 100.52(11) . 2_575 N1 Ni1 Br1 122.70(11) . . N1 Ni1 Br1 100.52(11) 2_575 . N1 Ni1 Br1 122.70(11) 2_575 2_575 N1 Ni1 N1 82.2(2) . 2_575 C16 N1 Ni1 126.6(3) . . C19 N1 Ni1 111.6(3) . . C19 N1 C16 121.4(4) . . C6 C1 C2 119.3(5) . . C10 C1 C2 122.7(5) . . C10 C1 C6 118.0(6) . . C1 C2 H2 120.4 . . C3 C2 C1 119.2(6) . . C3 C2 H2 120.4 . . C2 C3 H3 118.8 . . C2 C3 C4 122.5(8) . . C4 C3 H3 118.8 . . C3 C4 H4 120.1 . . C5 C4 C3 119.7(8) . . C5 C4 H4 120.1 . . C4 C5 H5 119.2 . . C4 C5 C6 121.6(6) . . C6 C5 H5 119.2 . . C1 C6 C5 117.6(6) . . C7 C6 C1 121.8(6) . . C7 C6 C5 120.6(6) . . C6 C7 H7 120.5 . . C6 C7 C8 119.0(6) . . C8 C7 H7 120.5 . . C7 C8 H8 120.2 . . C7 C8 C9 119.6(7) . . C9 C8 H8 120.2 . . C8 C9 H9 119.0 . . C10 C9 C8 122.1(6) . . C10 C9 H9 119.0 . . C1 C10 C11 120.5(5) . . C9 C10 C1 119.5(5) . . C9 C10 C11 119.9(5) . . C12 C11 C10 120.5(5) . . C12 C11 C16 117.5(5) . . C16 C11 C10 121.9(4) . . C11 C12 H12 118.9 . . C11 C12 C13 122.1(5) . . C13 C12 H12 118.9 . . C12 C13 C14 117.9(4) . . C12 C13 C17 121.5(5) . . C14 C13 C17 120.6(5) . . C13 C14 H14 118.5 . . C15 C14 C13 123.0(5) . . C15 C14 H14 118.5 . . C14 C15 C16 117.1(4) . . C14 C15 C18 121.2(5) . . C16 C15 C18 121.7(4) . . C11 C16 N1 117.4(4) . . C11 C16 C15 122.4(4) . . C15 C16 N1 120.2(4) . . C13 C17 H17A 109.5 . . C13 C17 H17B 109.5 . . C13 C17 H17C 109.5 . . H17A C17 H17B 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . C15 C18 H18A 109.5 . . C15 C18 H18B 109.5 . . C15 C18 H18C 109.5 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . N1 C19 C19 117.1(3) . 2_575 N1 C19 C20 135.7(4) . . C20 C19 C19 107.1(3) . 2_575 C21 C20 C19 106.3(4) . . C25 C20 C19 135.4(5) . . C25 C20 C21 118.2(5) . . C20 C21 C20 112.9(6) 2_575 . C22 C21 C20 123.5(3) . . C22 C21 C20 123.5(3) . 2_575 C21 C22 C23 116.2(4) . . C21 C22 C23 116.2(4) . 2_575 C23 C22 C23 127.7(8) . 2_575 C22 C23 H23 119.9 . . C24 C23 C22 120.2(6) . . C24 C23 H23 119.9 . . C23 C24 H24 118.4 . . C23 C24 C25 123.2(6) . . C25 C24 H24 118.4 . . C20 C25 C24 118.6(6) . . C20 C25 H25 120.7 . . C24 C25 H25 120.7 . . Cl1 C26 Cl2 111.8(5) . . Cl1 C26 H26A 109.2 . . Cl1 C26 H26B 109.2 . . Cl2 C26 H26A 109.2 . . Cl2 C26 H26B 109.2 . . H26A C26 H26B 107.9 . . Cl3 C27 Cl4 112.6(4) . . Cl3 C27 H27A 109.1 . . Cl3 C27 H27B 109.1 . . Cl4 C27 H27A 109.1 . . Cl4 C27 H27B 109.1 . . H27A C27 H27B 107.8 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 Br1 2.3377(8) 2_575 Ni1 Br1 2.3377(8) . Ni1 N1 2.029(4) 2_575 Ni1 N1 2.029(4) . Cl1 C26 1.714(9) . Cl2 C26 1.753(10) . Cl3 C27 1.726(7) . Cl4 C27 1.738(7) . N1 C16 1.442(6) . N1 C19 1.260(6) . C1 C2 1.439(8) . C1 C6 1.426(7) . C1 C10 1.414(8) . C2 H2 0.9500 . C2 C3 1.359(9) . C3 H3 0.9500 . C3 C4 1.401(10) . C4 H4 0.9500 . C4 C5 1.351(11) . C5 H5 0.9500 . C5 C6 1.446(10) . C6 C7 1.388(9) . C7 H7 0.9500 . C7 C8 1.397(11) . C8 H8 0.9500 . C8 C9 1.403(8) . C9 H9 0.9500 . C9 C10 1.376(8) . C10 C11 1.498(7) . C11 C12 1.389(7) . C11 C16 1.396(7) . C12 H12 0.9500 . C12 C13 1.390(7) . C13 C14 1.395(8) . C13 C17 1.541(7) . C14 H14 0.9500 . C14 C15 1.371(7) . C15 C16 1.410(7) . C15 C18 1.490(7) . C17 H17A 0.9800 . C17 H17B 0.9800 . C17 H17C 0.9800 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . C19 C19 1.516(8) 2_575 C19 C20 1.471(7) . C20 C21 1.431(6) . C20 C25 1.375(7) . C21 C20 1.431(6) 2_575 C21 C22 1.388(9) . C22 C23 1.421(7) . C22 C23 1.421(7) 2_575 C23 H23 0.9500 . C23 C24 1.366(9) . C24 H24 0.9500 . C24 C25 1.400(8) . C25 H25 0.9500 . C26 H26A 0.9900 . C26 H26B 0.9900 . C27 H27A 0.9900 . C27 H27B 0.9900 . 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 _geom_torsion_site_symmetry_4 Ni1 N1 C16 C11 -78.3(5) . . Ni1 N1 C16 C15 99.2(5) . . Ni1 N1 C19 C19 4.2(7) . 2_575 Ni1 N1 C19 C20 -177.4(5) . . N1 C19 C20 C21 -175.6(5) . . N1 C19 C20 C25 2.4(11) . . C1 C2 C3 C4 2.6(11) . . C1 C6 C7 C8 1.1(8) . . C1 C10 C11 C12 -64.6(7) . . C1 C10 C11 C16 119.4(6) . . C2 C1 C6 C5 2.6(8) . . C2 C1 C6 C7 -179.7(5) . . C2 C1 C10 C9 179.1(5) . . C2 C1 C10 C11 -4.2(8) . . C2 C3 C4 C5 0.0(12) . . C3 C4 C5 C6 -1.3(11) . . C4 C5 C6 C1 -0.1(9) . . C4 C5 C6 C7 -177.8(6) . . C5 C6 C7 C8 178.7(6) . . C6 C1 C2 C3 -3.9(8) . . C6 C1 C10 C9 0.5(7) . . C6 C1 C10 C11 177.2(4) . . C6 C7 C8 C9 -0.6(9) . . C7 C8 C9 C10 0.1(9) . . C8 C9 C10 C1 -0.1(8) . . C8 C9 C10 C11 -176.8(5) . . C9 C10 C11 C12 112.0(6) . . C9 C10 C11 C16 -64.0(7) . . C10 C1 C2 C3 177.5(6) . . C10 C1 C6 C5 -178.7(5) . . C10 C1 C6 C7 -1.0(8) . . C10 C11 C12 C13 -175.5(5) . . C10 C11 C16 N1 -7.3(7) . . C10 C11 C16 C15 175.3(5) . . C11 C12 C13 C14 0.2(8) . . C11 C12 C13 C17 179.7(6) . . C12 C11 C16 N1 176.6(5) . . C12 C11 C16 C15 -0.8(8) . . C12 C13 C14 C15 -1.0(9) . . C13 C14 C15 C16 0.9(8) . . C13 C14 C15 C18 -178.2(5) . . C14 C15 C16 N1 -177.3(4) . . C14 C15 C16 C11 0.0(7) . . C16 N1 C19 C19 178.3(5) . 2_575 C16 N1 C19 C20 -3.3(9) . . C16 C11 C12 C13 0.6(8) . . C17 C13 C14 C15 179.5(6) . . C18 C15 C16 N1 1.8(7) . . C18 C15 C16 C11 179.1(5) . . C19 N1 C16 C11 108.5(6) . . C19 N1 C16 C15 -74.0(6) . . C19 C19 C20 C21 2.9(6) 2_575 . C19 C19 C20 C25 -179.1(6) 2_575 . C19 C20 C21 C20 -1.1(2) . 2_575 C19 C20 C21 C22 178.9(2) . . C19 C20 C25 C24 -180.0(5) . . C20 C21 C22 C23 -178.5(4) . 2_575 C20 C21 C22 C23 -178.5(4) 2_575 . C20 C21 C22 C23 1.5(4) 2_575 2_575 C20 C21 C22 C23 1.5(4) . . C21 C20 C25 C24 -2.1(8) . . C21 C22 C23 C24 -1.8(7) . . C22 C23 C24 C25 0.1(9) . . C23 C22 C23 C24 178.2(7) 2_575 . C23 C24 C25 C20 1.9(10) . . C25 C20 C21 C20 -179.5(6) . 2_575 C25 C20 C21 C22 0.5(6) . . loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.958(17) 2 0.042(17)