#------------------------------------------------------------------------------ #$Date: 2021-09-03 22:47:39 +0300 (Fri, 03 Sep 2021) $ #$Revision: 268427 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519002.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_4519002 loop_ _publ_author_name 'Lohrey, Trevor D.' 'Cusumano, Alexander Q.' 'Goddard, William A.' 'Stoltz, Brian M.' _publ_section_title ; Identifying the Imperative Role of Metal--Olefin Interactions in Catalytic C--O Reductive Elimination from Nickel(II) ; _journal_issue 16 _journal_name_full 'ACS Catalysis' _journal_page_first 10208 _journal_page_last 10222 _journal_paper_doi 10.1021/acscatal.1c02790 _journal_volume 11 _journal_year 2021 _chemical_formula_moiety 'C16 H24 I2 Ni2' _chemical_formula_sum 'C16 H24 I2 Ni2' _chemical_formula_weight 587.57 _chemical_name_common '[(COD)NiI]2' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 97.511(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.4617(17) _cell_length_b 10.686(2) _cell_length_c 10.939(3) _cell_measurement_reflns_used 3345 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.34 _cell_measurement_theta_min 2.68 _cell_volume 864.7(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SHELXT _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker AXS D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_unetI/netI 0.0403 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 13084 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 26.390 _diffrn_reflns_theta_min 2.676 _diffrn_source 'rotating anode' _exptl_absorpt_coefficient_mu 5.735 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.257 _exptl_crystal_description needle _exptl_crystal_F_000 564 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.647 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.153 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1774 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0278 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+1.1899P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0546 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1467 _reflns_number_total 1774 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c02790_si_002.cif _cod_data_source_block '[(COD)NiI]2' _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_secondary' value 'diffmap' was changed to 'difmap'. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 864.8(4) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4519002 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.007 _shelx_estimated_absorpt_t_max 0.009 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1)/n CELL 0.71073 7.4617 10.6861 10.9391 90.000 97.511 90.000 ZERR 2.00 0.0017 0.0020 0.0031 0.000 0.010 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H NI I UNIT 32 48 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 15.000 20.000 100.000 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 10 TEMP -173.15 WGHT 0.015000 1.189900 FVAR 0.12947 C1 1 0.734568 0.705508 0.723177 11.00000 0.02161 0.01670 = 0.01452 0.00132 -0.00533 -0.00220 AFIX 43 H1 2 0.689797 0.636151 0.764293 11.00000 -1.20000 AFIX 0 C2 1 0.858256 0.682606 0.644602 11.00000 0.01513 0.02143 = 0.02194 -0.00296 -0.00398 -0.00052 AFIX 43 H2 2 0.894598 0.598098 0.636756 11.00000 -1.20000 AFIX 0 C3 1 0.943139 0.778933 0.568721 11.00000 0.01653 0.02997 = 0.03313 -0.00214 -0.00244 -0.00275 AFIX 23 H3A 2 1.036514 0.825084 0.623635 11.00000 -1.20000 H3B 2 1.004828 0.734708 0.506518 11.00000 -1.20000 AFIX 0 C4 1 0.812527 0.872474 0.503049 11.00000 0.02333 0.03282 = 0.02753 0.00755 0.00168 -0.00728 AFIX 23 H4A 2 0.862454 0.903211 0.429086 11.00000 -1.20000 H4B 2 0.803283 0.944969 0.558226 11.00000 -1.20000 AFIX 0 C5 1 0.624824 0.821525 0.463630 11.00000 0.02746 0.01297 = 0.01528 0.00212 -0.00204 -0.00425 AFIX 43 H5 2 0.601286 0.784823 0.384051 11.00000 -1.20000 AFIX 0 C6 1 0.487083 0.824397 0.533829 11.00000 0.02354 0.01041 = 0.01907 -0.00134 -0.00140 0.00270 AFIX 43 H6 2 0.373837 0.793367 0.496198 11.00000 -1.20000 AFIX 0 C7 1 0.493434 0.871112 0.664363 11.00000 0.03214 0.01954 = 0.02532 -0.00488 0.00523 0.00404 AFIX 23 H7A 2 0.387277 0.837704 0.699300 11.00000 -1.20000 H7B 2 0.482872 0.963463 0.662551 11.00000 -1.20000 AFIX 0 C8 1 0.663118 0.835699 0.749478 11.00000 0.03402 0.02811 = 0.01116 -0.00737 -0.00132 0.00161 AFIX 23 H8A 2 0.636872 0.838538 0.835838 11.00000 -1.20000 H8B 2 0.758393 0.898340 0.740805 11.00000 -1.20000 AFIX 0 NI1 3 0.599869 0.642259 0.548921 11.00000 0.01626 0.01513 = 0.01495 -0.00125 0.00153 -0.00023 I1 4 0.670592 0.484798 0.376584 11.00000 0.02039 0.01877 = 0.02014 -0.00398 0.00857 -0.00247 HKLF 4 REM shelxt_a.res in P2(1)/n REM R1 = 0.0278 for 1467 Fo > 4sig(Fo) and 0.0414 for all 1774 data REM 91 parameters refined using 0 restraints END WGHT 0.0148 1.2633 REM Highest difference peak 0.647, deepest hole -0.773, 1-sigma level 0.153 Q1 1 0.5909 0.9168 0.6717 11.00000 0.05 0.65 Q2 1 0.7769 0.4822 0.4014 11.00000 0.05 0.62 Q3 1 0.9298 0.6150 0.6790 11.00000 0.05 0.57 Q4 1 0.6586 0.8825 0.8174 11.00000 0.05 0.52 Q5 1 0.7498 0.6289 0.3666 11.00000 0.05 0.52 Q6 1 0.5232 0.8798 0.5822 11.00000 0.05 0.50 Q7 1 0.7660 0.4942 0.2640 11.00000 0.05 0.50 Q8 1 0.9464 0.9520 0.3513 11.00000 0.05 0.50 Q9 1 0.5915 0.8611 0.4180 11.00000 0.05 0.49 Q10 1 0.5312 0.4206 0.2846 11.00000 0.05 0.48 Q11 1 0.3260 0.8321 0.4593 11.00000 0.05 0.47 Q12 1 1.0489 0.7976 0.5760 11.00000 0.05 0.47 Q13 1 0.6728 0.5423 0.3730 11.00000 0.05 0.47 Q14 1 1.0133 0.6380 0.6125 11.00000 0.05 0.46 Q15 1 0.5206 0.5395 0.4071 11.00000 0.05 0.46 Q16 1 0.5019 0.6850 0.4031 11.00000 0.05 0.46 Q17 1 1.0627 0.9411 0.6795 11.00000 0.05 0.46 Q18 1 0.6928 0.8453 0.4871 11.00000 0.05 0.46 Q19 1 0.9282 0.7541 0.4022 11.00000 0.05 0.45 Q20 1 0.8826 0.6578 0.8512 11.00000 0.05 0.45 ; _shelx_res_checksum 44366 _shelx_hkl_file ; -1 0 0 -0.07 0.32 1 0 0 0.47 0.55 -2 0 0 54.78 3.16 2 0 0 58.00 3.27 -3 0 0 0.30 0.95 -3 0 0 0.79 1.25 -4 0 0 203.89 3.10 -4 0 0 193.86 10.03 -4 0 0 208.68 3.03 -4 0 0 212.96 8.50 -5 0 0 0.66 0.42 -5 0 0 1.28 1.84 -5 0 0 0.21 0.40 -6 0 0 74.07 3.40 -6 0 0 79.77 3.24 -6 0 0 79.80 7.96 -6 0 0 73.69 6.24 -6 0 0 82.35 6.26 -7 0 0 0.17 1.39 -7 0 0 -2.14 1.70 -8 0 0 14.43 3.74 -8 0 0 12.07 4.63 -8 0 0 10.92 3.63 -8 0 0 11.44 2.40 -9 0 0 2.26 1.92 -9 0 0 0.48 2.25 -9 0 0 4.58 3.65 -9 0 0 -3.36 1.61 1 -1 0 200.76 3.80 1 -1 0 210.03 5.55 1 -1 0 208.81 4.32 -1 -1 0 202.94 4.10 1 1 0 205.30 4.11 -1 1 0 201.47 5.27 -1 1 0 202.38 3.92 -1 1 0 209.68 4.53 2 -1 0 43.83 3.36 2 -1 0 39.02 1.51 -2 -1 0 36.51 2.29 -2 -1 0 35.58 2.86 2 -1 0 40.23 1.48 -2 1 0 38.66 3.11 -2 1 0 38.57 1.99 -2 1 0 37.21 2.15 -3 -1 0 537.45 10.72 3 -1 0 545.17 13.04 -3 -1 0 533.86 10.37 -3 -1 0 544.24 13.61 -3 1 0 521.33 15.19 -3 1 0 528.50 14.62 -3 1 0 525.38 8.45 -3 1 0 538.48 7.80 -4 -1 0 24.88 3.30 4 -1 0 23.84 4.26 -4 -1 0 17.47 3.53 -4 -1 0 22.75 4.10 -4 1 0 17.81 1.70 -4 1 0 17.90 1.84 -4 1 0 19.40 3.53 -4 1 0 20.58 4.34 -5 -1 0 12.49 3.33 -5 -1 0 17.86 3.33 -5 -1 0 16.70 2.93 -5 1 0 19.79 1.91 -5 1 0 22.80 4.21 -5 1 0 16.17 2.24 -5 1 0 17.57 4.29 -6 -1 0 14.49 3.15 -6 -1 0 23.03 5.14 -6 -1 0 18.04 1.00 -6 -1 0 23.19 4.15 -6 -1 0 20.15 0.99 -6 1 0 10.27 4.15 -6 1 0 16.05 2.57 -6 1 0 15.73 3.74 -7 -1 0 -0.42 2.28 -7 -1 0 4.40 2.07 -7 -1 0 -0.41 0.69 -7 -1 0 -0.51 1.35 -7 1 0 2.55 1.36 -7 1 0 2.21 2.01 -7 1 0 -1.49 2.08 -8 -1 0 17.20 5.69 -8 -1 0 23.09 2.32 -8 -1 0 31.84 5.20 -8 1 0 27.00 6.56 -8 1 0 25.12 3.88 -8 1 0 27.33 5.32 -9 -1 0 19.60 4.65 -9 -1 0 29.21 3.11 -9 -1 0 15.63 5.64 -9 1 0 29.65 6.19 -9 1 0 33.09 4.87 -9 1 0 28.03 5.45 -9 1 0 15.82 7.00 0 -2 0 88.10 3.89 0 -2 0 91.67 3.39 0 2 0 87.58 3.24 1 -2 0 0.70 1.07 1 -2 0 -0.13 0.83 1 -2 0 0.32 1.05 -1 -2 0 0.70 0.58 -1 -2 0 0.71 0.33 -1 -2 0 0.27 0.89 1 2 0 0.52 0.83 -1 2 0 0.36 0.61 -1 2 0 0.36 1.07 -1 2 0 -0.04 1.01 -2 -2 0 187.33 5.42 2 -2 0 182.31 5.01 -2 -2 0 174.42 5.38 2 -2 0 177.97 7.27 2 -2 0 171.71 5.41 -2 2 0 168.87 5.91 2 2 0 174.27 5.41 -2 2 0 182.70 5.33 -2 2 0 175.37 6.90 3 -2 0 102.26 6.32 3 -2 0 93.99 3.19 3 -2 0 87.55 3.29 -3 -2 0 91.19 6.33 -3 -2 0 96.27 4.24 -3 2 0 91.51 5.75 -3 2 0 96.92 6.63 -3 2 0 95.97 4.18 -4 -2 0 29.19 4.43 -4 -2 0 24.60 2.72 4 -2 0 26.87 4.73 -4 -2 0 24.49 2.52 -4 2 0 25.17 2.74 -4 2 0 27.31 4.46 -4 2 0 30.09 5.37 -4 2 0 22.77 2.30 -5 -2 0 7.85 1.88 -5 -2 0 13.58 2.87 -5 -2 0 8.49 3.05 5 -2 0 7.52 3.19 -5 2 0 11.95 3.13 -5 2 0 14.95 2.37 -5 2 0 19.04 4.76 -5 2 0 13.60 2.58 -6 -2 0 149.54 10.20 -6 -2 0 175.27 8.52 -6 2 0 160.79 7.54 -6 2 0 159.68 9.71 -7 -2 0 55.16 8.40 -7 -2 0 52.86 4.56 -7 -2 0 47.33 5.00 -7 -2 0 57.81 1.52 -7 2 0 46.40 5.73 -7 2 0 54.90 9.08 -7 2 0 51.60 5.06 -8 -2 0 40.73 6.02 -8 -2 0 38.06 2.06 -8 -2 0 32.87 3.88 -8 -2 0 43.32 7.76 -8 2 0 39.81 6.81 -8 2 0 36.52 5.18 -8 2 0 32.76 7.65 -9 -2 0 4.44 1.07 -9 -2 0 -0.89 2.42 -9 -2 0 9.04 4.27 -9 -2 0 -0.17 1.94 -9 2 0 1.58 2.57 -9 2 0 -2.24 2.17 -9 2 0 -2.95 2.48 -9 2 0 3.74 4.28 0 -3 0 -0.79 1.04 0 -3 0 0.89 0.97 0 3 0 1.80 1.08 1 -3 0 59.30 4.18 1 -3 0 61.24 3.58 1 -3 0 59.66 4.20 -1 -3 0 63.91 2.92 1 3 0 52.29 3.76 -1 3 0 62.61 4.39 -1 3 0 58.30 3.87 2 -3 0 0.30 0.88 2 -3 0 1.72 1.26 -2 -3 0 1.03 0.60 2 -3 0 -1.26 1.11 -2 -3 0 0.03 0.89 2 3 0 0.03 0.68 -2 3 0 1.16 1.07 -2 3 0 1.07 1.36 -2 3 0 0.34 1.12 -2 3 0 1.55 1.24 -3 -3 0 242.76 7.56 3 -3 0 241.65 6.93 -3 -3 0 253.64 7.60 3 -3 0 236.45 10.25 3 -3 0 234.89 7.41 3 3 0 238.48 7.78 -3 3 0 243.03 7.56 -3 3 0 234.98 10.73 -3 3 0 228.23 11.78 -3 3 0 244.09 8.81 4 -3 0 64.24 6.05 4 -3 0 62.31 3.07 -4 -3 0 59.92 4.76 4 -3 0 63.62 3.30 -4 -3 0 65.99 4.12 -4 -3 0 65.30 3.91 -4 3 0 71.75 6.89 -4 3 0 64.92 4.16 -4 3 0 61.55 4.84 -4 3 0 69.53 5.93 -5 -3 0 200.54 7.50 -5 -3 0 203.20 10.06 5 -3 0 205.32 11.34 -5 3 0 203.70 9.07 -5 3 0 193.70 10.48 -5 3 0 208.71 12.81 -6 -3 0 2.22 1.55 6 -3 0 1.75 2.23 -6 -3 0 6.24 2.68 -6 -3 0 7.89 3.25 -6 3 0 9.59 3.43 -6 3 0 10.21 3.93 -6 3 0 8.10 2.60 -7 -3 0 58.63 5.94 -7 -3 0 67.37 7.17 -7 -3 0 58.04 1.72 -7 3 0 53.16 5.48 -7 3 0 54.98 9.70 -7 3 0 56.66 6.66 -8 -3 0 9.97 1.01 -8 -3 0 10.01 3.98 -8 -3 0 3.42 2.23 -8 3 0 11.43 4.09 -8 3 0 7.05 4.53 -8 3 0 5.86 2.95 -9 -3 0 65.99 2.39 -9 -3 0 61.62 9.61 -9 3 0 62.48 11.04 -9 3 0 73.40 8.08 -9 3 0 80.43 8.86 0 -4 0 22.87 2.55 0 -4 0 20.12 3.38 0 -4 0 22.54 3.19 0 4 0 23.39 2.16 0 4 0 22.62 2.46 1 -4 0 103.54 6.13 1 -4 0 106.79 6.01 1 -4 0 100.65 5.14 -1 -4 0 108.16 4.57 -1 4 0 103.06 5.59 -1 4 0 97.84 6.01 1 4 0 102.36 4.34 1 4 0 107.97 6.12 2 -4 0 142.67 7.10 2 -4 0 147.42 6.34 2 -4 0 157.68 8.17 -2 -4 0 146.21 4.73 -2 -4 0 151.81 6.98 -2 4 0 147.85 7.54 -2 4 0 154.14 7.97 2 4 0 148.25 6.85 -2 4 0 146.69 7.40 3 -4 0 0.90 1.08 3 -4 0 2.78 1.50 -3 -4 0 0.63 0.63 3 -4 0 3.50 2.12 -3 -4 0 0.50 0.98 -3 4 0 -0.44 1.32 -3 4 0 1.53 1.45 -3 4 0 1.99 1.76 3 4 0 0.57 1.17 -4 -4 0 0.90 1.01 -4 -4 0 -0.74 0.72 4 -4 0 0.73 1.73 4 -4 0 1.50 1.03 -4 4 0 -0.43 1.37 -4 4 0 1.31 1.54 4 4 0 -0.84 0.97 -4 4 0 2.05 1.82 5 -4 0 8.28 1.55 5 -4 0 8.75 3.43 -5 -4 0 8.69 2.56 -5 -4 0 9.33 2.29 -5 -4 0 8.69 1.96 -5 4 0 7.74 2.62 -5 4 0 10.63 3.41 -5 4 0 5.53 2.89 6 -4 0 159.90 11.90 -6 -4 0 166.85 9.77 -6 -4 0 166.62 7.19 -6 4 0 162.14 10.62 -6 4 0 158.39 9.38 -7 -4 0 3.93 2.72 7 -4 0 2.17 2.31 -7 -4 0 3.11 0.81 -7 -4 0 2.47 1.70 -7 4 0 -1.30 1.80 -7 4 0 -1.21 2.95 -7 4 0 4.60 2.44 -8 -4 0 49.89 8.08 -8 -4 0 35.89 2.19 -8 -4 0 32.68 3.27 -8 4 0 38.74 10.57 -8 4 0 35.86 6.68 0 -5 0 1.01 1.21 0 -5 0 -0.08 1.45 0 -5 0 0.62 1.30 0 5 0 0.94 0.84 0 5 0 -0.70 1.10 0 5 0 -0.04 0.95 1 -5 0 20.28 3.28 -1 -5 0 19.70 3.61 1 -5 0 19.78 3.79 -1 -5 0 21.32 3.06 1 -5 0 19.50 3.74 1 5 0 18.83 3.68 1 5 0 18.07 1.36 -1 5 0 26.68 3.97 1 5 0 20.32 2.99 -1 5 0 20.76 3.59 2 -5 0 265.90 9.37 -2 -5 0 243.44 8.75 2 -5 0 243.10 10.88 -2 5 0 259.01 11.03 -2 5 0 263.62 10.52 2 5 0 281.64 10.81 -2 5 0 242.43 10.56 3 -5 0 118.56 6.35 3 -5 0 110.81 8.05 -3 -5 0 116.68 4.57 -3 5 0 115.98 7.70 3 5 0 118.07 6.73 -3 5 0 110.97 7.51 -3 5 0 114.02 8.46 -4 -5 0 0.68 0.78 -4 -5 0 3.99 1.25 4 -5 0 -0.10 1.23 4 -5 0 4.34 1.93 4 -5 0 0.22 1.97 -4 -5 0 2.39 1.34 4 5 0 1.80 1.25 -4 5 0 1.12 1.85 -4 5 0 2.14 1.74 -4 5 0 0.78 1.63 5 -5 0 74.30 4.52 -5 -5 0 61.37 4.89 5 -5 0 67.90 7.74 -5 -5 0 67.71 5.15 5 -5 0 65.57 4.80 -5 5 0 66.98 6.42 5 5 0 66.87 5.21 -5 5 0 61.26 6.50 6 -5 0 6.29 3.08 -6 -5 0 4.42 1.88 -6 -5 0 4.34 2.31 -6 5 0 6.48 2.80 -6 5 0 4.31 2.98 -7 -5 0 4.72 2.46 -7 -5 0 -2.31 2.41 -7 -5 0 3.19 1.24 -7 5 0 1.86 2.45 -8 -5 0 1.56 1.18 -8 -5 0 2.48 1.85 -8 -5 0 -0.58 2.62 -8 5 0 3.89 4.30 -8 5 0 -5.19 1.88 -8 5 0 2.63 2.98 0 -6 0 622.02 17.67 0 -6 0 620.70 15.11 0 -6 0 618.17 15.80 0 6 0 608.89 18.78 0 6 0 617.47 14.62 0 6 0 609.40 12.20 -1 -6 0 109.79 6.01 1 -6 0 104.88 7.45 1 -6 0 109.93 6.52 1 -6 0 101.78 7.02 -1 -6 0 106.60 6.06 -1 -6 0 102.48 7.20 -1 6 0 110.05 6.56 1 6 0 108.47 2.65 1 6 0 110.70 7.69 1 6 0 108.14 5.67 -1 6 0 112.90 6.82 -2 -6 0 28.61 2.95 2 -6 0 27.75 4.87 2 -6 0 32.39 5.14 -2 -6 0 33.99 4.99 2 -6 0 37.30 3.88 -2 6 0 31.71 5.14 2 6 0 25.95 4.42 -2 6 0 38.17 4.48 -3 -6 0 49.17 3.46 3 -6 0 52.69 6.05 3 -6 0 42.22 4.82 3 -6 0 48.32 4.55 3 6 0 45.81 4.83 -3 6 0 41.07 6.21 -3 6 0 48.81 7.22 -3 6 0 54.43 5.53 4 -6 0 72.41 7.77 4 -6 0 96.55 7.04 4 -6 0 87.90 6.10 -4 6 0 81.85 8.24 4 6 0 96.26 6.62 -4 6 0 90.61 7.72 -4 6 0 79.91 7.24 5 -6 0 24.56 6.03 5 -6 0 19.67 3.65 5 -6 0 17.87 3.26 5 6 0 22.24 3.91 -5 6 0 18.48 4.40 -5 6 0 16.52 5.08 -5 6 0 26.02 5.63 6 -6 0 48.01 3.80 -6 -6 0 42.95 4.25 -6 -6 0 55.99 4.03 -6 -6 0 52.76 3.64 -6 6 0 53.22 8.08 -6 6 0 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2.31 2 3 -12 2.03 4.24 -2 3 12 -4.47 3.11 2 3 -12 5.69 2.87 2 3 -12 -1.74 2.98 1 -3 -12 5.55 3.16 -1 -3 12 1.87 3.00 1 -3 -12 -0.62 3.03 -1 3 12 -0.65 2.59 1 3 -12 -2.55 2.86 -1 3 12 -1.87 2.75 1 3 -12 -0.66 2.66 0 -3 -12 3.19 4.03 0 -3 -12 1.87 3.26 0 -3 -12 -0.88 2.93 0 -3 12 -3.50 2.26 0 3 -12 1.79 2.79 0 3 12 -1.04 2.28 -1 -3 -12 2.69 3.56 1 -3 12 7.00 3.80 -1 -3 -12 12.40 4.83 -1 -3 -12 5.88 4.40 1 -3 12 0.97 2.82 -1 3 -12 10.27 4.08 -1 3 -12 2.23 3.49 1 3 12 3.19 3.15 -2 -3 -12 -2.01 2.73 -2 -3 -12 2.59 3.97 2 -3 12 -1.13 2.98 2 -3 12 1.47 3.13 -2 3 -12 -2.38 3.04 -2 3 -12 3.33 3.61 2 3 12 1.61 2.96 2 3 12 1.60 3.11 4 -4 -12 6.64 4.54 4 -4 -12 7.25 4.84 4 -4 -12 6.37 4.65 4 4 -12 6.64 6.04 4 4 -12 1.86 3.32 -4 4 12 10.42 4.05 -4 4 12 -3.51 4.08 -4 4 12 4.58 4.32 -3 -4 12 1.53 3.26 3 -4 -12 1.21 2.91 3 -4 -12 1.11 3.62 -3 4 12 0.47 3.72 3 4 -12 -1.50 3.95 -3 4 12 5.87 3.28 3 4 -12 2.01 2.82 3 4 -12 0.37 3.11 2 -4 -12 38.41 7.95 -2 -4 12 40.72 7.98 2 -4 -12 36.33 8.06 2 4 -12 49.32 8.26 -2 4 12 55.88 10.22 2 4 -12 31.99 8.07 -2 4 12 39.94 6.75 2 4 -12 51.11 8.73 -1 -4 12 3.97 3.47 -1 -4 12 4.26 3.50 1 -4 -12 9.80 3.88 1 -4 -12 7.06 5.04 1 -4 -12 5.92 3.57 1 4 -12 11.38 4.82 -1 4 12 6.37 3.66 1 4 -12 2.76 3.66 -1 4 12 1.18 4.70 0 -4 -12 24.30 6.44 0 -4 12 33.23 6.88 0 -4 -12 43.98 9.14 0 -4 -12 11.09 3.85 0 4 -12 24.52 6.18 0 4 -12 20.57 5.83 0 4 12 23.92 6.00 1 -4 12 12.28 4.40 1 -4 12 27.28 5.91 -1 -4 -12 22.55 5.72 -1 -4 -12 16.87 5.40 -1 -4 -12 22.18 6.66 -1 4 -12 25.11 6.53 -1 4 -12 35.81 8.27 1 4 12 22.70 5.10 2 -4 12 10.70 4.78 -2 -4 -12 4.01 3.94 -2 -4 -12 3.78 4.05 -2 -4 -12 7.81 4.03 2 4 12 2.28 3.42 2 4 12 5.79 3.04 -2 4 -12 10.34 6.06 -3 -5 12 79.11 9.29 3 -5 -12 70.72 11.45 3 -5 -12 68.45 10.28 3 -5 -12 54.42 10.61 3 5 -12 74.27 10.37 3 5 -12 56.98 8.50 -3 5 12 58.42 8.83 -3 5 12 62.51 11.87 -3 5 12 79.56 11.73 3 5 -12 48.64 9.90 2 -5 -12 27.34 6.32 2 -5 -12 43.78 9.22 -2 -5 12 26.74 7.43 -2 -5 12 26.57 5.56 2 -5 -12 16.89 6.23 -2 5 12 34.09 7.44 2 5 -12 32.62 7.07 2 5 -12 35.04 7.60 2 5 -12 30.58 7.94 1 -5 -12 5.75 5.14 1 -5 -12 8.69 4.75 -1 -5 12 6.07 3.74 1 -5 -12 11.26 4.47 -1 5 12 5.17 3.33 1 5 -12 2.15 3.32 1 5 -12 3.69 4.11 -1 5 12 7.46 4.06 -1 5 12 5.85 4.81 0 -5 -12 11.64 5.89 0 -5 -12 4.27 3.43 0 -5 12 -4.51 2.93 0 5 12 4.60 3.43 0 5 -12 9.85 4.63 0 5 -12 6.72 4.87 0 5 12 11.11 5.72 0 5 12 7.81 4.08 -1 -5 -12 5.22 3.49 -1 -5 -12 0.65 3.89 1 -5 12 2.43 3.20 -1 -5 -12 -2.63 3.38 1 5 12 0.76 2.73 1 5 12 9.69 5.34 -1 5 -12 -1.14 3.05 -1 5 -12 -1.87 4.33 -2 -6 12 8.61 4.30 -2 -6 12 2.76 3.87 2 -6 -12 0.02 3.63 2 -6 -12 5.72 3.33 -2 6 12 0.95 2.66 2 6 -12 -8.96 3.15 -2 6 12 1.14 3.27 2 6 -12 1.15 4.84 -2 6 12 -0.08 3.88 1 -6 -12 10.22 5.28 -1 -6 12 10.09 4.67 1 -6 -12 10.92 4.94 -1 -6 12 4.19 3.92 1 -6 -12 12.37 5.00 1 6 -12 19.78 6.16 1 6 -12 21.15 6.72 -1 6 12 8.76 4.41 -1 6 12 12.46 4.46 -1 6 12 13.65 6.08 0 -6 -12 76.65 12.52 0 -6 12 50.81 8.59 0 -6 12 62.14 10.02 0 -6 -12 51.62 9.00 0 6 -12 64.23 10.31 0 6 12 58.58 10.32 0 6 12 53.21 11.46 0 6 12 73.67 7.92 0 6 -12 61.79 11.12 -4 0 13 -2.02 3.15 4 0 -13 -2.23 3.40 4 0 -13 -5.19 3.40 3 0 -13 16.47 6.37 -3 0 13 20.95 5.54 3 0 -13 15.29 5.37 3 0 -13 19.53 6.08 2 0 -13 -2.06 3.59 2 0 -13 -0.41 2.89 2 0 -13 -2.15 3.13 1 0 -13 25.44 6.09 1 0 -13 12.55 5.50 1 0 -13 8.11 4.35 0 0 13 -3.91 2.61 0 0 -13 -3.88 2.97 0 0 -13 -3.39 3.21 0 0 -13 -2.45 3.00 1 0 13 52.30 8.15 -1 0 -13 47.50 9.51 1 0 13 49.65 7.75 -1 0 -13 56.81 10.66 -3 -1 13 8.16 4.25 3 -1 -13 11.42 4.95 3 -1 -13 12.07 4.72 3 1 -13 5.54 5.18 3 1 -13 14.78 5.01 -3 1 13 8.56 3.97 3 1 -13 17.22 5.33 2 -1 -13 32.26 7.81 -2 -1 13 30.68 7.29 2 -1 -13 15.29 5.94 2 -1 -13 15.16 4.98 2 1 -13 26.21 6.97 -2 1 13 24.69 6.10 2 1 -13 23.18 7.10 1 -1 -13 -0.90 3.25 1 -1 -13 4.30 3.50 1 -1 -13 0.23 2.56 1 1 -13 -1.61 3.87 1 1 -13 -5.19 2.85 1 1 -13 -1.27 2.85 0 -1 -13 45.73 8.39 0 -1 -13 50.64 11.76 0 -1 -13 37.29 8.25 0 1 -13 57.93 9.57 0 1 13 60.10 8.63 0 1 -13 44.86 8.71 -1 -1 -13 4.21 3.31 -1 -1 -13 -0.42 3.73 1 -1 13 0.27 3.04 1 -1 13 -1.85 2.96 1 1 13 4.63 3.04 -1 1 -13 -0.42 3.96 -1 1 -13 -5.89 2.80 1 1 13 -0.98 2.77 3 -2 -13 45.73 9.69 3 -2 -13 27.45 6.96 -3 -2 13 38.22 7.25 3 -2 -13 37.77 7.89 3 2 -13 24.13 8.56 -3 2 13 26.98 5.93 3 2 -13 41.37 7.82 3 2 -13 33.62 6.91 2 -2 -13 5.76 3.85 -2 -2 13 1.93 3.44 2 -2 -13 -2.71 3.91 2 -2 -13 -2.83 3.21 -2 2 13 -0.92 3.11 2 2 -13 -2.22 4.04 2 2 -13 2.91 3.93 2 2 -13 -1.12 2.73 -1 -2 13 4.95 4.49 1 -2 -13 -5.21 3.47 1 -2 -13 9.51 4.41 1 -2 -13 19.02 6.20 1 2 -13 -0.06 3.94 1 2 -13 7.72 4.59 1 2 -13 17.07 6.32 0 -2 -13 9.68 5.30 0 -2 -13 14.50 5.59 0 -2 -13 14.03 6.40 0 2 -13 22.00 6.85 0 2 -13 28.18 7.03 0 2 13 28.52 7.04 -1 -2 -13 31.97 8.13 1 -2 13 16.99 5.04 -1 -2 -13 22.05 6.10 -1 2 -13 31.95 8.43 1 2 13 25.36 6.06 3 -3 -13 5.58 5.55 3 -3 -13 0.33 3.30 3 -3 -13 5.26 4.60 -3 -3 13 11.39 4.79 3 3 -13 -3.61 4.09 3 3 -13 2.58 3.53 -3 3 13 3.88 3.23 3 3 -13 8.73 4.65 -3 3 13 11.65 5.38 2 -3 -13 110.44 11.26 -2 -3 13 108.44 10.56 2 -3 -13 87.56 10.57 2 -3 -13 108.88 12.69 2 3 -13 120.80 11.78 2 3 -13 105.71 12.61 -2 3 13 101.60 9.92 2 3 -13 86.35 9.95 1 -3 -13 1.08 4.25 -1 -3 13 13.81 4.99 1 -3 -13 13.50 4.52 -1 3 13 6.82 3.56 1 3 -13 8.17 5.75 1 3 -13 2.60 3.48 1 3 -13 5.92 4.33 0 -3 13 15.38 5.03 0 -3 -13 10.71 4.91 0 -3 -13 14.64 5.79 0 -3 -13 3.81 4.17 0 -3 13 16.32 4.88 0 3 -13 9.68 4.86 0 3 -13 17.29 6.96 1 -4 -13 2.44 5.52 -1 -4 13 2.73 3.90 1 -4 -13 13.39 6.03 -1 -4 13 9.44 4.78 1 4 -13 17.39 5.81 1 4 -13 18.95 6.38 -1 4 13 9.78 4.78 -1 4 13 19.96 6.58 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 90063 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7346(6) 0.7055(4) 0.7232(4) 0.0183(10) Uani 1 1 d . . . . . H1 H 0.6898 0.6362 0.7643 0.022 Uiso 1 1 calc R U . . . C2 C 0.8583(6) 0.6826(4) 0.6446(4) 0.0201(11) Uani 1 1 d . . . . . H2 H 0.8946 0.5981 0.6368 0.024 Uiso 1 1 calc R U . . . C3 C 0.9431(6) 0.7789(5) 0.5687(5) 0.0271(12) Uani 1 1 d . . . . . H3A H 1.0365 0.8251 0.6236 0.032 Uiso 1 1 calc R U . . . H3B H 1.0048 0.7347 0.5065 0.032 Uiso 1 1 calc R U . . . C4 C 0.8125(6) 0.8725(5) 0.5030(5) 0.0280(12) Uani 1 1 d . . . . . H4A H 0.8625 0.9032 0.4291 0.034 Uiso 1 1 calc R U . . . H4B H 0.8033 0.9450 0.5582 0.034 Uiso 1 1 calc R U . . . C5 C 0.6248(6) 0.8215(4) 0.4636(4) 0.0190(10) Uani 1 1 d . . . . . H5 H 0.6013 0.7848 0.3841 0.023 Uiso 1 1 calc R U . . . C6 C 0.4871(6) 0.8244(4) 0.5338(4) 0.0180(10) Uani 1 1 d . . . . . H6 H 0.3738 0.7934 0.4962 0.022 Uiso 1 1 calc R U . . . C7 C 0.4934(7) 0.8711(5) 0.6644(5) 0.0255(11) Uani 1 1 d . . . . . H7A H 0.3873 0.8377 0.6993 0.031 Uiso 1 1 calc R U . . . H7B H 0.4829 0.9635 0.6626 0.031 Uiso 1 1 calc R U . . . C8 C 0.6631(7) 0.8357(5) 0.7495(4) 0.0248(11) Uani 1 1 d . . . . . H8A H 0.6369 0.8385 0.8358 0.030 Uiso 1 1 calc R U . . . H8B H 0.7584 0.8983 0.7408 0.030 Uiso 1 1 calc R U . . . Ni1 Ni 0.59987(8) 0.64226(5) 0.54892(6) 0.01549(14) Uani 1 1 d . . . . . I1 I 0.67059(4) 0.48480(3) 0.37658(3) 0.01924(9) 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 C1 0.022(2) 0.017(2) 0.015(3) 0.0013(19) -0.005(2) -0.0022(19) C2 0.015(2) 0.021(2) 0.022(3) -0.003(2) -0.004(2) -0.0005(19) C3 0.017(2) 0.030(3) 0.033(3) -0.002(2) -0.002(2) -0.003(2) C4 0.023(3) 0.033(3) 0.028(3) 0.008(2) 0.002(2) -0.007(2) C5 0.027(3) 0.013(2) 0.015(3) 0.0021(19) -0.002(2) -0.0042(19) C6 0.024(2) 0.010(2) 0.019(3) -0.0013(19) -0.001(2) 0.0027(18) C7 0.032(3) 0.020(3) 0.025(3) -0.005(2) 0.005(2) 0.004(2) C8 0.034(3) 0.028(3) 0.011(3) -0.007(2) -0.001(2) 0.002(2) Ni1 0.0163(3) 0.0151(3) 0.0150(3) -0.0013(2) 0.0015(2) -0.0002(2) I1 0.02039(15) 0.01877(16) 0.02014(17) -0.00398(14) 0.00857(12) -0.00247(13) 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' I I -0.4742 1.8119 '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 C2 C1 C8 124.3(4) . . ? C2 C1 Ni1 70.1(3) . . ? C8 C1 Ni1 108.6(3) . . ? C2 C1 H1 117.9 . . ? C8 C1 H1 117.9 . . ? Ni1 C1 H1 91.3 . . ? C1 C2 C3 126.2(4) . . ? C1 C2 Ni1 72.5(3) . . ? C3 C2 Ni1 106.7(3) . . ? C1 C2 H2 116.9 . . ? C3 C2 H2 116.9 . . ? Ni1 C2 H2 90.8 . . ? C4 C3 C2 114.9(4) . . ? C4 C3 H3A 108.5 . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 C5 114.4(4) . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 124.8(5) . . ? C6 C5 Ni1 70.2(3) . . ? C4 C5 Ni1 109.1(3) . . ? C6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? Ni1 C5 H5 90.8 . . ? C5 C6 C7 127.5(4) . . ? C5 C6 Ni1 72.6(3) . . ? C7 C6 Ni1 105.5(3) . . ? C5 C6 H6 116.2 . . ? C7 C6 H6 116.2 . . ? Ni1 C6 H6 92.0 . . ? C6 C7 C8 114.8(4) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C1 113.2(4) . . ? C7 C8 H8A 108.9 . . ? C1 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C1 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C2 Ni1 C6 100.28(18) . . ? C2 Ni1 C1 37.32(17) . . ? C6 Ni1 C1 85.12(18) . . ? C2 Ni1 C5 84.72(18) . . ? C6 Ni1 C5 37.19(17) . . ? C1 Ni1 C5 92.74(18) . . ? C2 Ni1 I1 103.28(13) . . ? C6 Ni1 I1 130.28(13) . . ? C1 Ni1 I1 136.36(12) . . ? C5 Ni1 I1 102.83(13) . . ? C2 Ni1 I1 129.39(14) . 3_666 ? C6 Ni1 I1 100.61(13) . 3_666 ? C1 Ni1 I1 100.11(13) . 3_666 ? C5 Ni1 I1 134.70(13) . 3_666 ? I1 Ni1 I1 97.18(2) . 3_666 ? Ni1 I1 Ni1 82.82(2) . 3_666 ? 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 C1 C2 1.363(6) . ? C1 C8 1.531(6) . ? C1 Ni1 2.145(5) . ? C1 H1 0.9500 . ? C2 C3 1.512(7) . ? C2 Ni1 2.114(4) . ? C2 H2 0.9500 . ? C3 C4 1.511(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.512(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.361(6) . ? C5 Ni1 2.149(4) . ? C5 H5 0.9500 . ? C6 C7 1.508(6) . ? C6 Ni1 2.118(4) . ? C6 H6 0.9500 . ? C7 C8 1.518(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? Ni1 I1 2.6313(8) . ? Ni1 I1 2.6476(8) 3_666 ? I1 Ni1 2.6477(8) 3_666 ?