#------------------------------------------------------------------------------ #$Date: 2019-01-11 03:41:47 +0200 (Fri, 11 Jan 2019) $ #$Revision: 212972 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/04/1550436.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_1550436 loop_ _publ_author_name 'Viertl, Wolfgang' 'Pann, Johann' 'Pehn, Richard' 'Roithmeyer, Helena' 'Bendig, Marvin' 'Rodriguez-Villalon, Alba' 'Bereiter, Raphael' 'Heidescheid, Max' 'M\"uller, Thomas' 'Zhao, Xia' 'Hofer, Thomas' 'Thompson, Mark' 'Shi, Shuyang' 'Br\"uggeller, Peter' _publ_section_title ; Performance of Enhanced DuBois Type Water Reduction Catalysts (WRC) in Artificial Photosynthesis - Effects of Various Proton Relays during Catalysis ; _journal_name_full 'Faraday Discussions' _journal_paper_doi 10.1039/C8FD00162F _journal_year 2019 _chemical_formula_moiety 'C31 H35 Cl2 N Ni O4 P2, C2 H3 N' _chemical_formula_sum 'C33 H38 Cl2 N2 Ni O4 P2' _chemical_formula_weight 718.18 _chemical_name_systematic '[NiCl2(PNP-C1-Me)]' _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-10-23 deposited with the CCDC. 2019-01-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.0064(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.8814(2) _cell_length_b 18.6698(3) _cell_length_c 14.5746(2) _cell_measurement_reflns_used 9440 _cell_measurement_temperature 183(2) _cell_measurement_theta_max 26.4 _cell_measurement_theta_min 2.68 _cell_volume 3385.56(9) _computing_cell_refinement 'Bruker SAINT-V 8.34A' _computing_data_collection 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT-V 8.34A' _computing_molecular_graphics SHELXLE _computing_publication_material SHELXL-2014/7 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'Bruker Apex II' _diffrn_ambient_temperature 183(2) _diffrn_detector_area_resol_mean 10.4 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 100' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0130 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 92012 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.429 _diffrn_reflns_theta_min 2.618 _diffrn_source 'Incoatec Microfocus' _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS-2014/5' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1496 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.040 _exptl_transmission_factor_max 0.966 _exptl_transmission_factor_min 0.725 _refine_diff_density_max 0.266 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 6857 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0216 _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^)+(0.0272P)^2^+1.0998P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0537 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6269 _reflns_number_total 6968 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8fd00162f2.cif _cod_data_source_block 5a _cod_database_code 1550436 _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 0.725 _shelx_estimated_absorpt_t_max 0.966 _exptl_absorpt_special_details 'Bruker SADABS-2014/5' _shelx_res_file ; nipnp.res created by SHELXL-2014/7 TITL nipnp_0m in P2(1)/n CELL 0.71073 12.88040 18.66830 14.57360 90.0000 105.0056 90.0000 ZERR 4.00 0.00060 0.00090 0.00060 0.0000 0.0014 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N P CL NI O UNIT 124 140 4 8 8 4 16 TEMP -90.150 SIZE 0.04 0.40 0.40 OMIT -1 OMIT 3 0 3 OMIT 1 11 1 OMIT 4 6 2 OMIT -3 12 6 OMIT -4 6 8 OMIT 1 4 6 OMIT 5 3 3 OMIT -1 9 7 OMIT -5 4 5 OMIT -5 5 2 OMIT 3 3 3 OMIT -2 2 10 OMIT -4 6 7 OMIT 0 3 6 OMIT -4 4 6 OMIT -4 6 4 OMIT 5 0 3 OMIT 0 1 7 OMIT 6 9 0 OMIT 7 2 0 OMIT -5 5 5 OMIT 1 10 3 OMIT 1 2 7 OMIT -7 4 6 OMIT 6 3 0 OMIT 3 8 5 OMIT 5 14 3 OMIT -7 4 4 OMIT -9 11 7 OMIT 3 4 5 OMIT 6 4 1 OMIT -5 6 6 OMIT -7 3 5 OMIT 4 7 2 OMIT -7 0 1 OMIT 3 0 9 OMIT -10 11 10 OMIT 4 1 0 OMIT 3 18 4 OMIT -6 10 8 OMIT -7 6 5 OMIT 1 1 9 OMIT 0 5 6 OMIT 0 9 3 OMIT 0 10 0 OMIT 4 9 14 OMIT -5 3 2 OMIT 4 6 4 OMIT 6 1 6 OMIT -5 4 4 OMIT 3 7 1 OMIT -3 3 3 OMIT 5 2 4 OMIT -5 6 5 OMIT 2 6 3 OMIT -4 5 7 OMIT -7 2 3 OMIT 1 0 7 OMIT -7 6 3 OMIT -1 10 1 OMIT -2 3 7 OMIT 0 0 2 OMIT -1 1 1 OMIT 7 1 1 OMIT 5 0 1 OMIT 0 4 4 OMIT 0 2 0 OMIT -3 6 6 OMIT 2 8 1 OMIT -6 9 6 OMIT -7 8 9 OMIT 2 7 3 OMIT -2 11 2 OMIT -2 2 7 OMIT 5 1 2 OMIT 10 4 4 OMIT 7 1 2 OMIT 0 11 1 OMIT 0 6 4 OMIT -7 1 1 OMIT -2 10 4 OMIT -3 9 5 OMIT 1 4 8 OMIT 1 3 1 OMIT -7 8 5 OMIT -2 6 7 OMIT 1 9 2 OMIT -5 10 1 OMIT -1 3 7 OMIT 6 12 1 OMIT 3 7 3 OMIT -6 7 8 OMIT -4 0 8 OMIT -7 2 5 OMIT -1 10 5 OMIT 12 10 3 OMIT 1 0 1 OMIT 1 2 1 OMIT -1 4 2 OMIT 1 11 3 L.S. 4 ACTA CONF BOND BOND $H FMAP 2 PLAN 10 WGHT 0.027200 1.099800 FVAR 0.10891 NI1 6 0.838510 0.175133 0.573700 11.00000 0.01274 0.01563 = 0.01310 0.00092 0.00291 -0.00088 CL1 5 0.744203 0.118911 0.659932 11.00000 0.02006 0.02466 = 0.01730 0.00111 0.00656 -0.00480 CL2 5 0.991030 0.146818 0.675279 11.00000 0.01656 0.02548 = 0.01937 0.00354 0.00058 0.00065 P1 4 0.684968 0.212606 0.483326 11.00000 0.01384 0.01626 = 0.01513 -0.00005 0.00281 0.00028 P2 4 0.933861 0.218851 0.484633 11.00000 0.01428 0.01622 = 0.01467 -0.00003 0.00474 -0.00021 O1 7 0.746801 0.348413 0.567127 11.00000 0.03698 0.02428 = 0.04575 -0.01063 0.00577 -0.00482 O2 7 0.453820 0.218198 0.367221 11.00000 0.01792 0.02517 = 0.02705 0.00188 -0.00106 0.00265 O3 7 1.062285 0.315860 0.389568 11.00000 0.04315 0.03668 = 0.02495 -0.00361 0.02111 -0.01448 O4 7 0.889736 0.079215 0.393873 11.00000 0.02193 0.02249 = 0.03465 -0.00923 0.00760 -0.00239 N1 3 0.782098 0.300453 0.374957 11.00000 0.01859 0.02032 = 0.02232 0.00557 0.00354 0.00063 C1 1 0.678484 0.272239 0.379308 11.00000 0.01842 0.02363 = 0.01993 0.00568 0.00228 0.00018 AFIX 23 H1A 2 0.647033 0.245070 0.320318 11.00000 -1.20000 H1B 2 0.629817 0.312819 0.381825 11.00000 -1.20000 AFIX 0 C2 1 0.855206 0.243483 0.364719 11.00000 0.02102 0.02502 = 0.01525 0.00128 0.00504 0.00129 AFIX 23 H2A 2 0.903459 0.260205 0.326173 11.00000 -1.20000 H2B 2 0.814256 0.201595 0.332688 11.00000 -1.20000 AFIX 0 C3 1 0.769620 0.354756 0.300612 11.00000 0.02772 0.03653 = 0.04854 0.02507 0.00982 0.00192 AFIX 137 H3A 2 0.839893 0.375676 0.302376 11.00000 -1.50000 H3B 2 0.720999 0.392429 0.311172 11.00000 -1.50000 H3C 2 0.739605 0.332565 0.238450 11.00000 -1.50000 AFIX 0 C11 1 0.614625 0.262004 0.556790 11.00000 0.02264 0.02557 = 0.01691 -0.00018 0.00255 0.00759 C12 1 0.656163 0.328776 0.592168 11.00000 0.03121 0.02748 = 0.02233 -0.00313 -0.00093 0.00893 C13 1 0.606635 0.368841 0.649402 11.00000 0.05585 0.03522 = 0.03009 -0.00993 0.00274 0.01743 AFIX 43 H13A 2 0.634858 0.414176 0.673075 11.00000 -1.20000 AFIX 0 C14 1 0.516248 0.342122 0.671412 11.00000 0.06276 0.05597 = 0.03189 -0.00774 0.01873 0.02602 AFIX 43 H14A 2 0.481874 0.369610 0.709897 11.00000 -1.20000 AFIX 0 C15 1 0.474874 0.275881 0.638284 11.00000 0.04324 0.05928 = 0.03239 0.00297 0.02032 0.01663 AFIX 43 H15A 2 0.412590 0.258062 0.654050 11.00000 -1.20000 AFIX 0 C16 1 0.524751 0.235482 0.581848 11.00000 0.02865 0.03882 = 0.02276 0.00134 0.00998 0.00625 AFIX 43 H16A 2 0.497353 0.189513 0.560255 11.00000 -1.20000 AFIX 0 C17 1 0.783961 0.420541 0.580680 11.00000 0.05387 0.02248 = 0.04634 -0.00017 -0.00849 -0.00389 AFIX 137 H17A 2 0.841217 0.427895 0.548570 11.00000 -1.50000 H17B 2 0.811920 0.430038 0.648756 11.00000 -1.50000 H17C 2 0.724291 0.453275 0.554030 11.00000 -1.50000 AFIX 0 C21 1 0.596625 0.138982 0.431001 11.00000 0.01778 0.02042 = 0.01393 -0.00089 0.00468 -0.00178 C22 1 0.488595 0.149268 0.380530 11.00000 0.01892 0.02374 = 0.01584 0.00041 0.00558 -0.00073 C23 1 0.423254 0.090499 0.347183 11.00000 0.01770 0.03274 = 0.02139 -0.00260 0.00404 -0.00617 AFIX 43 H23A 2 0.349352 0.097410 0.316462 11.00000 -1.20000 AFIX 0 C24 1 0.465940 0.021679 0.358749 11.00000 0.02995 0.02743 = 0.02704 -0.00479 0.00747 -0.01220 AFIX 43 H24A 2 0.420843 -0.018325 0.336546 11.00000 -1.20000 AFIX 0 C25 1 0.573633 0.011163 0.402376 11.00000 0.03318 0.01965 = 0.02642 -0.00152 0.00746 -0.00219 AFIX 43 H25A 2 0.603529 -0.035633 0.407055 11.00000 -1.20000 AFIX 0 C26 1 0.637935 0.069575 0.439383 11.00000 0.02213 0.02260 = 0.01810 0.00021 0.00526 0.00060 AFIX 43 H26A 2 0.711436 0.062024 0.470988 11.00000 -1.20000 AFIX 0 C27 1 0.347087 0.230099 0.309193 11.00000 0.01802 0.03655 = 0.03225 0.00827 0.00068 0.00339 AFIX 137 H27A 2 0.335138 0.281612 0.298480 11.00000 -1.50000 H27B 2 0.294929 0.211056 0.341351 11.00000 -1.50000 H27C 2 0.338183 0.205770 0.248055 11.00000 -1.50000 AFIX 0 C31 1 1.009734 0.299229 0.531588 11.00000 0.01923 0.01757 = 0.02033 0.00006 0.00625 -0.00113 C32 1 1.066206 0.340040 0.478670 11.00000 0.02906 0.02496 = 0.02399 -0.00087 0.01244 -0.00534 C33 1 1.123977 0.400421 0.518078 11.00000 0.05036 0.03231 = 0.03836 -0.00186 0.02184 -0.01960 AFIX 43 H33A 2 1.161281 0.427754 0.481791 11.00000 -1.20000 AFIX 0 C34 1 1.127223 0.420805 0.610267 11.00000 0.05446 0.03263 = 0.04078 -0.01202 0.01699 -0.02273 AFIX 43 H34A 2 1.167161 0.461936 0.637035 11.00000 -1.20000 AFIX 0 C35 1 1.072756 0.381680 0.663402 11.00000 0.04281 0.03219 = 0.02555 -0.00917 0.01138 -0.01096 AFIX 43 H35A 2 1.075007 0.395767 0.726526 11.00000 -1.20000 AFIX 0 C36 1 1.014709 0.321621 0.623845 11.00000 0.02591 0.02452 = 0.02167 -0.00034 0.00896 -0.00396 AFIX 43 H36A 2 0.977275 0.294997 0.660720 11.00000 -1.20000 AFIX 0 C37 1 1.120397 0.353735 0.334453 11.00000 0.06948 0.06959 = 0.03799 -0.00603 0.03505 -0.03324 AFIX 137 H37A 2 1.112690 0.329139 0.273648 11.00000 -1.50000 H37B 2 1.196563 0.355658 0.368852 11.00000 -1.50000 H37C 2 1.092039 0.402546 0.322824 11.00000 -1.50000 AFIX 0 C41 1 1.032764 0.155573 0.464048 11.00000 0.02025 0.01983 = 0.01749 0.00302 0.00777 0.00314 C42 1 0.998053 0.090643 0.417430 11.00000 0.02164 0.02139 = 0.01954 0.00222 0.00826 0.00080 C43 1 1.072415 0.042695 0.397270 11.00000 0.03133 0.01929 = 0.02652 0.00274 0.01295 0.00448 AFIX 43 H43A 2 1.048932 -0.001119 0.365487 11.00000 -1.20000 AFIX 0 C44 1 1.180629 0.059675 0.424073 11.00000 0.02888 0.02455 = 0.03326 0.00807 0.01696 0.01029 AFIX 43 H44A 2 1.231164 0.027722 0.408937 11.00000 -1.20000 AFIX 0 C45 1 1.216552 0.122435 0.472576 11.00000 0.01847 0.03140 = 0.03495 0.00831 0.01015 0.00471 AFIX 43 H45A 2 1.291229 0.132909 0.491922 11.00000 -1.20000 AFIX 0 C46 1 1.142315 0.170003 0.492716 11.00000 0.02120 0.02267 = 0.02464 0.00239 0.00630 0.00089 AFIX 43 H46A 2 1.166774 0.212899 0.526490 11.00000 -1.20000 AFIX 0 C47 1 0.850969 0.014724 0.342561 11.00000 0.03118 0.02861 = 0.03493 -0.01246 0.01045 -0.00722 AFIX 137 H47A 2 0.772297 0.013618 0.327614 11.00000 -1.50000 H47B 2 0.880300 -0.026954 0.381595 11.00000 -1.50000 H47C 2 0.873870 0.013522 0.283480 11.00000 -1.50000 AFIX 0 N2 3 1.097362 0.009486 0.895231 11.00000 0.06326 0.05325 = 0.04906 -0.00219 0.01000 -0.00546 C4 1 1.025598 0.044840 0.896484 11.00000 0.04936 0.04088 = 0.02926 0.00571 0.00145 -0.01509 C5 1 0.934677 0.089578 0.898783 11.00000 0.04714 0.04937 = 0.03904 0.01280 0.00116 -0.00676 AFIX 137 H5A 2 0.959373 0.138668 0.915535 11.00000 -1.50000 H5B 2 0.899867 0.071004 0.946249 11.00000 -1.50000 H5C 2 0.883165 0.089386 0.836123 11.00000 -1.50000 AFIX 0 HKLF 4 REM nipnp_0m in P2(1)/n REM R1 = 0.0216 for 6269 Fo > 4sig(Fo) and 0.0254 for all 6857 data REM 403 parameters refined using 0 restraints END WGHT 0.0272 1.1001 REM Highest difference peak 0.266, deepest hole -0.295, 1-sigma level 0.044 Q1 1 0.9918 0.1811 0.4776 11.00000 0.05 0.27 Q2 1 1.0324 0.3179 0.5041 11.00000 0.05 0.24 Q3 1 1.0223 0.1179 0.4539 11.00000 0.05 0.22 Q4 1 0.9796 0.2669 0.5037 11.00000 0.05 0.21 Q5 1 0.6262 0.1670 0.4556 11.00000 0.05 0.21 Q6 1 0.6528 0.2418 0.5383 11.00000 0.05 0.19 Q7 1 0.6451 0.2907 0.5826 11.00000 0.05 0.19 Q8 1 0.8927 0.2331 0.4188 11.00000 0.05 0.18 Q9 1 0.5449 0.1441 0.4113 11.00000 0.05 0.18 Q10 1 0.6182 0.1041 0.4331 11.00000 0.05 0.18 ; _shelx_res_checksum 77523 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 Ni1 Ni 0.83851(2) 0.17513(2) 0.57370(2) 0.01390(5) Uani 1 1 d . . Cl1 Cl 0.74420(2) 0.11891(2) 0.65993(2) 0.02035(7) Uani 1 1 d . . Cl2 Cl 0.99103(2) 0.14682(2) 0.67528(2) 0.02122(7) Uani 1 1 d . . P1 P 0.68497(2) 0.21261(2) 0.48333(2) 0.01525(7) Uani 1 1 d . . P2 P 0.93386(2) 0.21885(2) 0.48463(2) 0.01487(7) Uani 1 1 d . . O1 O 0.74680(9) 0.34841(5) 0.56713(8) 0.0366(2) Uani 1 1 d . . O2 O 0.45382(7) 0.21820(5) 0.36722(6) 0.02465(19) Uani 1 1 d . . O3 O 1.06229(9) 0.31586(5) 0.38957(7) 0.0327(2) Uani 1 1 d . . O4 O 0.88974(7) 0.07921(5) 0.39387(7) 0.0263(2) Uani 1 1 d . . N1 N 0.78210(8) 0.30045(5) 0.37496(7) 0.0207(2) Uani 1 1 d . . C1 C 0.67848(10) 0.27224(7) 0.37931(9) 0.0212(2) Uani 1 1 d . . H1A H 0.6470 0.2451 0.3203 0.025 Uiso 1 1 calc R U H1B H 0.6298 0.3128 0.3818 0.025 Uiso 1 1 calc R U C2 C 0.85521(10) 0.24348(7) 0.36472(8) 0.0204(2) Uani 1 1 d . . H2A H 0.9035 0.2602 0.3262 0.024 Uiso 1 1 calc R U H2B H 0.8143 0.2016 0.3327 0.024 Uiso 1 1 calc R U C3 C 0.76962(12) 0.35476(8) 0.30061(12) 0.0376(4) Uani 1 1 d . . H3A H 0.8399 0.3757 0.3024 0.056 Uiso 1 1 calc R U H3B H 0.7210 0.3924 0.3112 0.056 Uiso 1 1 calc R U H3C H 0.7396 0.3326 0.2385 0.056 Uiso 1 1 calc R U C11 C 0.61463(10) 0.26200(7) 0.55679(9) 0.0222(3) Uani 1 1 d . . C12 C 0.65616(12) 0.32878(7) 0.59217(10) 0.0285(3) Uani 1 1 d . . C13 C 0.60663(14) 0.36884(9) 0.64940(11) 0.0419(4) Uani 1 1 d . . H13A H 0.6349 0.4142 0.6731 0.050 Uiso 1 1 calc R U C14 C 0.51625(16) 0.34212(10) 0.67141(12) 0.0490(5) Uani 1 1 d . . H14A H 0.4819 0.3696 0.7099 0.059 Uiso 1 1 calc R U C15 C 0.47487(14) 0.27588(10) 0.63828(11) 0.0430(4) Uani 1 1 d . . H15A H 0.4126 0.2581 0.6541 0.052 Uiso 1 1 calc R U C16 C 0.52475(11) 0.23548(8) 0.58185(9) 0.0295(3) Uani 1 1 d . . H16A H 0.4974 0.1895 0.5603 0.035 Uiso 1 1 calc R U C17 C 0.78396(15) 0.42054(8) 0.58068(12) 0.0449(4) Uani 1 1 d . . H17A H 0.8412 0.4279 0.5486 0.067 Uiso 1 1 calc R U H17B H 0.8119 0.4300 0.6488 0.067 Uiso 1 1 calc R U H17C H 0.7243 0.4533 0.5540 0.067 Uiso 1 1 calc R U C21 C 0.59663(10) 0.13898(6) 0.43100(8) 0.0173(2) Uani 1 1 d . . C22 C 0.48860(10) 0.14927(7) 0.38053(8) 0.0193(2) Uani 1 1 d . . C23 C 0.42325(10) 0.09050(7) 0.34718(9) 0.0241(3) Uani 1 1 d . . H23A H 0.3494 0.0974 0.3165 0.029 Uiso 1 1 calc R U C24 C 0.46594(11) 0.02168(7) 0.35875(10) 0.0281(3) Uani 1 1 d . . H24A H 0.4208 -0.0183 0.3365 0.034 Uiso 1 1 calc R U C25 C 0.57363(11) 0.01116(7) 0.40238(9) 0.0265(3) Uani 1 1 d . . H25A H 0.6035 -0.0356 0.4071 0.032 Uiso 1 1 calc R U C26 C 0.63793(10) 0.06958(7) 0.43938(9) 0.0209(2) Uani 1 1 d . . H26A H 0.7114 0.0620 0.4710 0.025 Uiso 1 1 calc R U C27 C 0.34709(10) 0.23010(8) 0.30919(10) 0.0300(3) Uani 1 1 d . . H27A H 0.3351 0.2816 0.2985 0.045 Uiso 1 1 calc R U H27B H 0.2949 0.2111 0.3414 0.045 Uiso 1 1 calc R U H27C H 0.3382 0.2058 0.2481 0.045 Uiso 1 1 calc R U C31 C 1.00973(10) 0.29923(6) 0.53159(8) 0.0188(2) Uani 1 1 d . . C32 C 1.06621(11) 0.34004(7) 0.47867(9) 0.0250(3) Uani 1 1 d . . C33 C 1.12398(14) 0.40042(8) 0.51808(11) 0.0384(4) Uani 1 1 d . . H33A H 1.1613 0.4278 0.4818 0.046 Uiso 1 1 calc R U C34 C 1.12722(14) 0.42080(8) 0.61027(12) 0.0418(4) Uani 1 1 d . . H34A H 1.1672 0.4619 0.6370 0.050 Uiso 1 1 calc R U C35 C 1.07276(13) 0.38168(8) 0.66340(10) 0.0330(3) Uani 1 1 d . . H35A H 1.0750 0.3958 0.7265 0.040 Uiso 1 1 calc R U C36 C 1.01471(11) 0.32162(7) 0.62385(9) 0.0235(3) Uani 1 1 d . . H36A H 0.9773 0.2950 0.6607 0.028 Uiso 1 1 calc R U C37 C 1.12040(17) 0.35374(11) 0.33445(13) 0.0551(5) Uani 1 1 d . . H37A H 1.1127 0.3291 0.2736 0.083 Uiso 1 1 calc R U H37B H 1.1966 0.3557 0.3689 0.083 Uiso 1 1 calc R U H37C H 1.0920 0.4025 0.3228 0.083 Uiso 1 1 calc R U C41 C 1.03276(10) 0.15557(6) 0.46405(8) 0.0187(2) Uani 1 1 d . . C42 C 0.99805(10) 0.09064(6) 0.41743(9) 0.0203(2) Uani 1 1 d . . C43 C 1.07241(11) 0.04269(7) 0.39727(9) 0.0247(3) Uani 1 1 d . . H43A H 1.0489 -0.0011 0.3655 0.030 Uiso 1 1 calc R U C44 C 1.18063(11) 0.05967(7) 0.42407(10) 0.0272(3) Uani 1 1 d . . H44A H 1.2312 0.0277 0.4089 0.033 Uiso 1 1 calc R U C45 C 1.21655(11) 0.12243(7) 0.47258(10) 0.0277(3) Uani 1 1 d . . H45A H 1.2912 0.1329 0.4919 0.033 Uiso 1 1 calc R U C46 C 1.14231(10) 0.17000(7) 0.49272(9) 0.0228(3) Uani 1 1 d . . H46A H 1.1668 0.2129 0.5265 0.027 Uiso 1 1 calc R U C47 C 0.85097(12) 0.01472(7) 0.34256(10) 0.0312(3) Uani 1 1 d . . H47A H 0.7723 0.0136 0.3276 0.047 Uiso 1 1 calc R U H47B H 0.8803 -0.0270 0.3816 0.047 Uiso 1 1 calc R U H47C H 0.8739 0.0135 0.2835 0.047 Uiso 1 1 calc R U N2 N 1.09736(15) 0.00949(9) 0.89523(11) 0.0560(4) Uani 1 1 d . . C4 C 1.02560(15) 0.04484(9) 0.89648(11) 0.0414(4) Uani 1 1 d . . C5 C 0.93468(14) 0.08958(10) 0.89878(12) 0.0470(4) Uani 1 1 d . . H5A H 0.9594 0.1387 0.9155 0.071 Uiso 1 1 calc R U H5B H 0.8999 0.0710 0.9462 0.071 Uiso 1 1 calc R U H5C H 0.8832 0.0894 0.8361 0.071 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 0.01274(8) 0.01563(8) 0.01310(8) 0.00092(5) 0.00291(6) -0.00088(5) Cl1 0.02006(15) 0.02466(14) 0.01730(14) 0.00111(11) 0.00656(11) -0.00480(11) Cl2 0.01656(14) 0.02548(15) 0.01937(14) 0.00354(11) 0.00058(11) 0.00065(11) P1 0.01384(14) 0.01626(14) 0.01513(14) -0.00005(11) 0.00281(11) 0.00028(11) P2 0.01428(14) 0.01622(14) 0.01467(14) -0.00003(11) 0.00474(11) -0.00021(11) O1 0.0370(6) 0.0243(5) 0.0458(6) -0.0106(4) 0.0058(5) -0.0048(4) O2 0.0179(4) 0.0252(5) 0.0270(5) 0.0019(4) -0.0011(4) 0.0027(4) O3 0.0431(6) 0.0367(5) 0.0250(5) -0.0036(4) 0.0211(5) -0.0145(5) O4 0.0219(5) 0.0225(4) 0.0347(5) -0.0092(4) 0.0076(4) -0.0024(4) N1 0.0186(5) 0.0203(5) 0.0223(5) 0.0056(4) 0.0035(4) 0.0006(4) C1 0.0184(6) 0.0236(6) 0.0199(6) 0.0057(5) 0.0023(5) 0.0002(5) C2 0.0210(6) 0.0250(6) 0.0153(5) 0.0013(5) 0.0050(5) 0.0013(5) C3 0.0277(8) 0.0365(8) 0.0485(9) 0.0251(7) 0.0098(7) 0.0019(6) C11 0.0226(6) 0.0256(6) 0.0169(6) -0.0002(5) 0.0025(5) 0.0076(5) C12 0.0312(8) 0.0275(7) 0.0223(6) -0.0031(5) -0.0009(6) 0.0089(6) C13 0.0559(11) 0.0352(8) 0.0301(8) -0.0099(6) 0.0027(7) 0.0174(7) C14 0.0628(12) 0.0560(11) 0.0319(8) -0.0077(8) 0.0187(8) 0.0260(9) C15 0.0432(9) 0.0593(11) 0.0324(8) 0.0030(7) 0.0203(7) 0.0166(8) C16 0.0287(7) 0.0388(8) 0.0228(6) 0.0013(6) 0.0100(6) 0.0063(6) C17 0.0539(10) 0.0225(7) 0.0463(9) -0.0002(6) -0.0085(8) -0.0039(7) C21 0.0178(6) 0.0204(6) 0.0139(5) -0.0009(4) 0.0047(4) -0.0018(5) C22 0.0189(6) 0.0237(6) 0.0158(6) 0.0004(5) 0.0056(5) -0.0007(5) C23 0.0177(6) 0.0327(7) 0.0214(6) -0.0026(5) 0.0040(5) -0.0062(5) C24 0.0300(7) 0.0274(7) 0.0270(7) -0.0048(5) 0.0075(6) -0.0122(6) C25 0.0332(7) 0.0196(6) 0.0264(7) -0.0015(5) 0.0075(6) -0.0022(5) C26 0.0221(6) 0.0226(6) 0.0181(6) 0.0002(5) 0.0053(5) 0.0006(5) C27 0.0180(6) 0.0365(7) 0.0323(7) 0.0083(6) 0.0007(5) 0.0034(6) C31 0.0192(6) 0.0176(5) 0.0203(6) 0.0001(5) 0.0063(5) -0.0011(5) C32 0.0291(7) 0.0250(6) 0.0240(6) -0.0009(5) 0.0124(5) -0.0053(5) C33 0.0504(10) 0.0323(8) 0.0384(8) -0.0019(6) 0.0218(7) -0.0196(7) C34 0.0545(10) 0.0326(8) 0.0408(9) -0.0120(7) 0.0170(8) -0.0227(7) C35 0.0428(9) 0.0322(7) 0.0256(7) -0.0092(6) 0.0114(6) -0.0110(6) C36 0.0259(7) 0.0245(6) 0.0217(6) -0.0003(5) 0.0090(5) -0.0040(5) C37 0.0695(13) 0.0696(12) 0.0380(9) -0.0060(9) 0.0350(9) -0.0332(10) C41 0.0203(6) 0.0198(6) 0.0175(6) 0.0030(5) 0.0078(5) 0.0031(5) C42 0.0216(6) 0.0214(6) 0.0195(6) 0.0022(5) 0.0083(5) 0.0008(5) C43 0.0313(7) 0.0193(6) 0.0265(6) 0.0027(5) 0.0130(6) 0.0045(5) C44 0.0289(7) 0.0246(6) 0.0333(7) 0.0081(5) 0.0170(6) 0.0103(5) C45 0.0185(6) 0.0314(7) 0.0350(7) 0.0083(6) 0.0102(5) 0.0047(5) C46 0.0212(6) 0.0227(6) 0.0246(6) 0.0024(5) 0.0063(5) 0.0009(5) C47 0.0312(8) 0.0286(7) 0.0349(7) -0.0125(6) 0.0104(6) -0.0072(6) N2 0.0633(11) 0.0533(9) 0.0491(9) -0.0022(7) 0.0100(8) -0.0055(9) C4 0.0494(10) 0.0409(9) 0.0293(8) 0.0057(7) 0.0014(7) -0.0151(8) C5 0.0471(10) 0.0494(10) 0.0390(9) 0.0128(7) 0.0012(7) -0.0068(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 P2 Ni1 P1 94.775(13) P2 Ni1 Cl2 86.995(12) P1 Ni1 Cl2 173.751(13) P2 Ni1 Cl1 173.980(13) P1 Ni1 Cl1 87.147(12) Cl2 Ni1 Cl1 91.699(12) C21 P1 C11 106.03(6) C21 P1 C1 102.62(5) C11 P1 C1 104.54(6) C21 P1 Ni1 112.35(4) C11 P1 Ni1 108.52(4) C1 P1 Ni1 121.56(4) C41 P2 C31 105.43(6) C41 P2 C2 104.07(6) C31 P2 C2 105.12(6) C41 P2 Ni1 112.61(4) C31 P2 Ni1 114.66(4) C2 P2 Ni1 113.96(4) C12 O1 C17 119.87(13) C22 O2 C27 117.47(10) C32 O3 C37 118.62(12) C42 O4 C47 117.18(10) C1 N1 C2 111.50(10) C1 N1 C3 110.99(10) C2 N1 C3 112.40(11) N1 C1 P1 113.83(8) N1 C1 H1A 108.8 P1 C1 H1A 108.8 N1 C1 H1B 108.8 P1 C1 H1B 108.8 H1A C1 H1B 107.7 N1 C2 P2 107.33(8) N1 C2 H2A 110.2 P2 C2 H2A 110.2 N1 C2 H2B 110.2 P2 C2 H2B 110.2 H2A C2 H2B 108.5 N1 C3 H3A 109.5 N1 C3 H3B 109.5 H3A C3 H3B 109.5 N1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C16 C11 C12 118.96(12) C16 C11 P1 123.23(10) C12 C11 P1 117.77(10) O1 C12 C13 125.04(14) O1 C12 C11 114.42(12) C13 C12 C11 120.53(15) C14 C13 C12 119.38(15) C14 C13 H13A 120.3 C12 C13 H13A 120.3 C13 C14 C15 120.97(14) C13 C14 H14A 119.5 C15 C14 H14A 119.5 C14 C15 C16 119.76(16) C14 C15 H15A 120.1 C16 C15 H15A 120.1 C15 C16 C11 120.36(15) C15 C16 H16A 119.8 C11 C16 H16A 119.8 O1 C17 H17A 109.5 O1 C17 H17B 109.5 H17A C17 H17B 109.5 O1 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C26 C21 C22 118.39(11) C26 C21 P1 118.81(9) C22 C21 P1 122.78(9) O2 C22 C23 123.31(11) O2 C22 C21 116.61(11) C23 C22 C21 120.08(11) C24 C23 C22 120.12(12) C24 C23 H23A 119.9 C22 C23 H23A 119.9 C25 C24 C23 120.35(12) C25 C24 H24A 119.8 C23 C24 H24A 119.8 C24 C25 C26 119.54(12) C24 C25 H25A 120.2 C26 C25 H25A 120.2 C25 C26 C21 121.28(12) C25 C26 H26A 119.4 C21 C26 H26A 119.4 O2 C27 H27A 109.5 O2 C27 H27B 109.5 H27A C27 H27B 109.5 O2 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C36 C31 C32 117.61(11) C36 C31 P2 119.67(9) C32 C31 P2 122.71(9) O3 C32 C33 123.08(12) O3 C32 C31 116.37(11) C33 C32 C31 120.53(12) C34 C33 C32 120.09(13) C34 C33 H33A 120.0 C32 C33 H33A 120.0 C35 C34 C33 120.40(13) C35 C34 H34A 119.8 C33 C34 H34A 119.8 C34 C35 C36 119.46(13) C34 C35 H35A 120.3 C36 C35 H35A 120.3 C35 C36 C31 121.90(12) C35 C36 H36A 119.0 C31 C36 H36A 119.0 O3 C37 H37A 109.5 O3 C37 H37B 109.5 H37A C37 H37B 109.5 O3 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C46 C41 C42 118.93(11) C46 C41 P2 121.63(9) C42 C41 P2 119.44(9) O4 C42 C43 123.99(11) O4 C42 C41 115.67(11) C43 C42 C41 120.33(12) C44 C43 C42 119.30(12) C44 C43 H43A 120.3 C42 C43 H43A 120.3 C43 C44 C45 121.14(12) C43 C44 H44A 119.4 C45 C44 H44A 119.4 C44 C45 C46 119.40(12) C44 C45 H45A 120.3 C46 C45 H45A 120.3 C41 C46 C45 120.84(12) C41 C46 H46A 119.6 C45 C46 H46A 119.6 O4 C47 H47A 109.5 O4 C47 H47B 109.5 H47A C47 H47B 109.5 O4 C47 H47C 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 N2 C4 C5 179.59(19) C4 C5 H5A 109.5 C4 C5 H5B 109.5 H5A C5 H5B 109.5 C4 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 P2 2.1645(3) Ni1 P1 2.1878(3) Ni1 Cl2 2.1964(3) Ni1 Cl1 2.2242(3) P1 C21 1.8210(12) P1 C11 1.8221(12) P1 C1 1.8651(12) P2 C41 1.8183(12) P2 C31 1.8244(12) P2 C2 1.8371(12) O1 C12 1.3606(19) O1 C17 1.4256(17) O2 C22 1.3598(15) O2 C27 1.4327(15) O3 C32 1.3633(16) O3 C37 1.4201(18) O4 C42 1.3645(15) O4 C47 1.4369(15) N1 C1 1.4513(16) N1 C2 1.4536(16) N1 C3 1.4619(17) C1 H1A 0.9900 C1 H1B 0.9900 C2 H2A 0.9900 C2 H2B 0.9900 C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C11 C16 1.3919(19) C11 C12 1.4011(19) C12 C13 1.392(2) C13 C14 1.379(3) C13 H13A 0.9500 C14 C15 1.383(3) C14 H14A 0.9500 C15 C16 1.390(2) C15 H15A 0.9500 C16 H16A 0.9500 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C21 C26 1.3940(17) C21 C22 1.4086(17) C22 C23 1.3915(17) C23 C24 1.390(2) C23 H23A 0.9500 C24 C25 1.382(2) C24 H24A 0.9500 C25 C26 1.3909(18) C25 H25A 0.9500 C26 H26A 0.9500 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C31 C36 1.3935(17) C31 C32 1.4124(17) C32 C33 1.3903(19) C33 C34 1.387(2) C33 H33A 0.9500 C34 C35 1.381(2) C34 H34A 0.9500 C35 C36 1.3875(19) C35 H35A 0.9500 C36 H36A 0.9500 C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C41 C46 1.3903(18) C41 C42 1.4048(17) C42 C43 1.3967(18) C43 C44 1.383(2) C43 H43A 0.9500 C44 C45 1.385(2) C44 H44A 0.9500 C45 C46 1.3908(18) C45 H45A 0.9500 C46 H46A 0.9500 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 N2 C4 1.140(2) C4 C5 1.446(3) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 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 C2 N1 C1 P1 62.34(12) C3 N1 C1 P1 -171.52(10) C21 P1 C1 N1 -136.67(9) C11 P1 C1 N1 112.82(10) Ni1 P1 C1 N1 -10.17(11) C1 N1 C2 P2 -92.92(10) C3 N1 C2 P2 141.72(10) C41 P2 C2 N1 -173.51(8) C31 P2 C2 N1 -62.91(9) Ni1 P2 C2 N1 63.45(9) C21 P1 C11 C16 13.45(12) C1 P1 C11 C16 121.47(11) Ni1 P1 C11 C16 -107.45(11) C21 P1 C11 C12 -168.93(10) C1 P1 C11 C12 -60.91(11) Ni1 P1 C11 C12 70.17(10) C17 O1 C12 C13 -14.7(2) C17 O1 C12 C11 166.56(12) C16 C11 C12 O1 177.14(12) P1 C11 C12 O1 -0.58(16) C16 C11 C12 C13 -1.7(2) P1 C11 C12 C13 -179.43(11) O1 C12 C13 C14 -178.49(14) C11 C12 C13 C14 0.2(2) C12 C13 C14 C15 0.7(2) C13 C14 C15 C16 -0.1(3) C14 C15 C16 C11 -1.4(2) C12 C11 C16 C15 2.3(2) P1 C11 C16 C15 179.89(11) C11 P1 C21 C26 -128.34(10) C1 P1 C21 C26 122.27(10) Ni1 P1 C21 C26 -9.95(11) C11 P1 C21 C22 53.03(11) C1 P1 C21 C22 -56.37(11) Ni1 P1 C21 C22 171.41(8) C27 O2 C22 C23 -5.27(17) C27 O2 C22 C21 174.79(11) C26 C21 C22 O2 -174.77(10) P1 C21 C22 O2 3.87(15) C26 C21 C22 C23 5.29(17) P1 C21 C22 C23 -176.07(9) O2 C22 C23 C24 176.35(12) C21 C22 C23 C24 -3.72(18) C22 C23 C24 C25 -0.7(2) C23 C24 C25 C26 3.5(2) C24 C25 C26 C21 -1.85(19) C22 C21 C26 C25 -2.54(18) P1 C21 C26 C25 178.77(10) C41 P2 C31 C36 -115.70(11) C2 P2 C31 C36 134.68(10) Ni1 P2 C31 C36 8.75(12) C41 P2 C31 C32 63.23(12) C2 P2 C31 C32 -46.39(12) Ni1 P2 C31 C32 -172.32(9) C37 O3 C32 C33 0.4(2) C37 O3 C32 C31 -178.12(15) C36 C31 C32 O3 178.33(12) P2 C31 C32 O3 -0.62(17) C36 C31 C32 C33 -0.2(2) P2 C31 C32 C33 -179.20(12) O3 C32 C33 C34 -178.01(15) C31 C32 C33 C34 0.5(2) C32 C33 C34 C35 -0.4(3) C33 C34 C35 C36 0.1(3) C34 C35 C36 C31 0.1(2) C32 C31 C36 C35 -0.1(2) P2 C31 C36 C35 178.92(11) C31 P2 C41 C46 6.76(12) C2 P2 C41 C46 117.14(11) Ni1 P2 C41 C46 -118.96(10) C31 P2 C41 C42 -172.75(9) C2 P2 C41 C42 -62.38(11) Ni1 P2 C41 C42 61.53(10) C47 O4 C42 C43 -2.06(18) C47 O4 C42 C41 177.46(11) C46 C41 C42 O4 178.16(11) P2 C41 C42 O4 -2.31(15) C46 C41 C42 C43 -2.31(18) P2 C41 C42 C43 177.22(9) O4 C42 C43 C44 179.78(12) C41 C42 C43 C44 0.29(19) C42 C43 C44 C45 1.66(19) C43 C44 C45 C46 -1.5(2) C42 C41 C46 C45 2.45(18) P2 C41 C46 C45 -177.07(10) C44 C45 C46 C41 -0.6(2)