#------------------------------------------------------------------------------ #$Date: 2021-03-05 03:14:52 +0200 (Fri, 05 Mar 2021) $ #$Revision: 262468 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/77/7127772.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_7127772 loop_ _publ_author_name 'Yang, Xin' 'Wei, Rui' 'Shi, Yaping' 'Liu, Liu Leo' 'Wu, Yile' 'Zhao, Yufen' 'Stephan, Douglas W.' _publ_section_title ; Oxyphosphoranes as precursors to bridging phosphate-catecholate ligands. ; _journal_issue 10 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1194 _journal_page_last 1197 _journal_paper_doi 10.1039/d0cc07736d _journal_volume 57 _journal_year 2021 _chemical_formula_moiety 'C32 H42 Cl8 Ni2 O14 P2' _chemical_formula_sum 'C32 H42 Cl8 Ni2 O14 P2' _chemical_formula_weight 1113.61 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2020-08-13 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-13 deposited with the CCDC. 2021-01-04 downloaded from the CCDC. ; _cell_angle_alpha 108.4832(15) _cell_angle_beta 97.6582(16) _cell_angle_gamma 100.3215(15) _cell_formula_units_Z 1 _cell_length_a 8.9110(5) _cell_length_b 11.1675(6) _cell_length_c 11.8597(7) _cell_measurement_reflns_used 9907 _cell_measurement_temperature 103(2) _cell_measurement_theta_max 73.47 _cell_measurement_theta_min 4.30 _cell_volume 1078.12(11) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 103.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 32977 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 73.465 _diffrn_reflns_theta_min 4.014 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.897 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.5410 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1120 before and 0.0906 after correction. The Ratio of minimum to maximum transmission is 0.7179. The \l/2 correction factor is Not present. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.715 _exptl_crystal_description block _exptl_crystal_F_000 568 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: toluene and thf' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.750 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4260 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0325 _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^)+(0.0377P)^2^+1.0232P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.0856 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4183 _reflns_number_total 4260 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc07736d2.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 7127772--7127775.cif.' _cod_database_code 7127772 _shelxl_version_number 2013-2 _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 0.387 _shelx_estimated_absorpt_t_min 0.370 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B) 2.b Idealised Me refined as rotating group: C17(H17A,H17B,H17C) ; _shelx_res_file ; TITL 1 in P-1 #2 REM reset to P-1 #2 CELL 1.54178 8.911 11.1675 11.8597 108.4832 97.6582 100.3215 ZERR 1 0.0005 0.0006 0.0007 0.0015 0.0016 0.0015 LATT 1 SFAC C H Cl Ni O P UNIT 32 42 8 2 14 2 L.S. 4 0 0 PLAN 20 SIZE 0.17 0.17 0.18 TEMP -170.15 BOND fmap 2 53 acta REM REM REM WGHT 0.037700 1.023200 FVAR 0.23138 NI1 4 0.119837 0.436195 0.542997 11.00000 0.02118 0.02092 = 0.02359 0.00995 0.00790 0.00347 P2 6 -0.181776 0.425655 0.637947 11.00000 0.02074 0.01932 = 0.02271 0.00865 0.00757 0.00194 CL3 3 -0.088125 0.688518 1.022043 11.00000 0.03501 0.03899 = 0.02317 0.01134 0.00930 0.00443 CL4 3 0.270392 0.853142 0.659793 11.00000 0.03797 0.02599 = 0.03793 0.01061 0.01568 -0.00363 CL5 3 0.320599 1.045682 0.926776 11.00000 0.04500 0.02326 = 0.04421 0.00139 0.00935 -0.00659 CL6 3 0.142394 0.962747 1.109861 11.00000 0.04177 0.03195 = 0.02548 0.00035 0.00253 0.00756 O1 5 0.049250 0.605734 0.607429 11.00000 0.02535 0.01929 = 0.02211 0.00591 0.00775 0.00350 O2 5 -0.049984 0.360667 0.618511 11.00000 0.02346 0.02453 = 0.02877 0.01412 0.01031 0.00449 O3 5 0.258544 0.527930 0.454878 11.00000 0.02198 0.02477 = 0.02733 0.01287 0.00906 0.00407 O4 5 0.178480 0.262113 0.470535 11.00000 0.03250 0.02535 = 0.04322 0.01788 0.02002 0.00977 O5 5 0.292136 0.483048 0.694717 11.00000 0.02388 0.04378 = 0.02883 0.01935 0.00445 -0.00112 O6 5 -0.129626 0.542438 0.769762 11.00000 0.02940 0.02391 = 0.02401 0.00692 0.01031 -0.00187 O7 5 -0.317684 0.336588 0.668302 11.00000 0.02293 0.02389 = 0.02789 0.01321 0.00762 0.00222 C8 1 -0.018402 0.655503 0.802065 11.00000 0.02280 0.02054 = 0.02484 0.00843 0.00513 0.00296 C9 1 -0.281649 0.277846 0.758714 11.00000 0.02856 0.03172 = 0.03431 0.02166 0.00922 0.00603 AFIX 23 H9A 2 -0.232292 0.346137 0.838393 11.00000 -1.20000 H9B 2 -0.208581 0.221806 0.734466 11.00000 -1.20000 AFIX 0 C10 1 0.066153 0.687569 0.718813 11.00000 0.02213 0.01993 = 0.02385 0.00743 0.00521 0.00475 C11 1 0.114614 0.858621 0.961805 11.00000 0.02930 0.02305 = 0.02413 0.00329 0.00345 0.00659 C12 1 0.194318 0.895175 0.880201 11.00000 0.02768 0.02036 = 0.03405 0.00718 0.00508 0.00329 C13 1 0.008602 0.738122 0.922102 11.00000 0.02540 0.02658 = 0.02396 0.00967 0.00625 0.00713 C14 1 0.439423 0.573544 0.711359 11.00000 0.02303 0.03505 = 0.03703 0.01361 0.00496 -0.00051 AFIX 23 H14A 2 0.421664 0.651680 0.694315 11.00000 -1.20000 H14B 2 0.504702 0.532221 0.656588 11.00000 -1.20000 AFIX 0 C15 1 0.352665 0.125556 0.418816 11.00000 0.03214 0.03049 = 0.04209 0.01067 0.01172 0.01069 AFIX 23 H15A 2 0.444670 0.141967 0.483251 11.00000 -1.20000 H15B 2 0.373437 0.075495 0.339585 11.00000 -1.20000 AFIX 0 C16 1 0.170256 0.810462 0.761209 11.00000 0.02602 0.02276 = 0.03009 0.00969 0.00847 0.00437 C17 1 -0.431614 0.198494 0.767284 11.00000 0.03479 0.03280 = 0.04503 0.02364 0.01437 0.00444 AFIX 137 H17A 2 -0.479649 0.131499 0.687911 11.00000 -1.50000 H17B 2 -0.502573 0.255037 0.792191 11.00000 -1.50000 H17C 2 -0.410588 0.157106 0.827349 11.00000 -1.50000 AFIX 0 C18 1 0.206869 0.053577 0.444891 11.00000 0.04682 0.03172 = 0.05848 0.02257 0.02108 0.01150 AFIX 23 H18A 2 0.129908 0.001438 0.368962 11.00000 -1.20000 H18B 2 0.232467 -0.004164 0.489231 11.00000 -1.20000 AFIX 0 C19 1 0.269726 0.472421 0.809901 11.00000 0.03223 0.05146 = 0.03179 0.02484 0.00980 0.01205 AFIX 23 H19A 2 0.294936 0.392088 0.817328 11.00000 -1.20000 H19B 2 0.160707 0.471539 0.818899 11.00000 -1.20000 AFIX 0 C20 1 0.380580 0.591446 0.904086 11.00000 0.04759 0.06558 = 0.03259 0.01100 0.00720 0.02161 AFIX 23 H20A 2 0.411869 0.576252 0.980737 11.00000 -1.20000 H20B 2 0.333899 0.667745 0.921228 11.00000 -1.20000 AFIX 0 C21 1 0.517177 0.609222 0.842711 11.00000 0.03833 0.05226 = 0.03960 0.00592 -0.00062 -0.00080 AFIX 23 H21A 2 0.579233 0.700201 0.876372 11.00000 -1.20000 H21B 2 0.585767 0.550837 0.851794 11.00000 -1.20000 AFIX 0 C23 1 0.314285 0.252297 0.416913 11.00000 0.03727 0.03051 = 0.04771 0.01505 0.02374 0.01021 AFIX 23 H23A 2 0.402685 0.326801 0.464479 11.00000 -1.20000 H23B 2 0.291845 0.251279 0.332538 11.00000 -1.20000 AFIX 0 C24 1 0.147740 0.161200 0.521466 11.00000 0.05310 0.03348 = 0.06252 0.02796 0.03066 0.01422 AFIX 23 H24A 2 0.034726 0.132958 0.517518 11.00000 -1.20000 H24B 2 0.203226 0.191655 0.607182 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P-1 #2 REM R1 = 0.0325 for 4183 Fo > 4sig(Fo) and 0.0329 for all 4260 data REM 263 parameters refined using 0 restraints END WGHT 0.0376 1.0245 REM Highest difference peak 0.750, deepest hole -0.427, 1-sigma level 0.088 Q1 1 0.0945 0.1339 0.4411 11.00000 0.05 0.75 Q2 1 0.4393 0.5245 0.8791 11.00000 0.05 0.64 Q3 1 0.2310 0.1021 0.5244 11.00000 0.05 0.50 Q4 1 0.3654 0.2771 0.4992 11.00000 0.05 0.46 Q5 1 -0.1010 0.3928 0.6218 11.00000 0.05 0.41 Q6 1 -0.1763 0.6838 1.0212 11.00000 0.05 0.38 Q7 1 0.4532 0.6626 0.8576 11.00000 0.05 0.35 Q8 1 0.1101 0.5811 0.5717 11.00000 0.05 0.32 Q9 1 0.2398 0.3039 0.5356 11.00000 0.05 0.31 Q10 1 0.0896 0.5609 0.5944 11.00000 0.05 0.31 Q11 1 0.0437 0.4805 0.5803 11.00000 0.05 0.31 Q12 1 -0.0982 0.3011 0.5628 11.00000 0.05 0.30 Q13 1 -0.2052 0.3227 0.5416 11.00000 0.05 0.30 Q14 1 0.6249 0.6579 0.8204 11.00000 0.05 0.28 Q15 1 0.1625 0.3184 0.5079 11.00000 0.05 0.27 Q16 1 -0.3303 0.2231 0.7712 11.00000 0.05 0.27 Q17 1 0.5757 0.5975 0.7457 11.00000 0.05 0.27 Q18 1 0.4109 0.9938 0.9199 11.00000 0.05 0.27 Q19 1 -0.0801 0.5946 0.7822 11.00000 0.05 0.26 Q20 1 0.2232 0.8193 0.7223 11.00000 0.05 0.26 ; _shelx_res_checksum 26899 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.11984(4) 0.43620(3) 0.54300(3) 0.02123(10) Uani 1 1 d . . . . . P2 P -0.18178(5) 0.42566(5) 0.63795(4) 0.02066(12) Uani 1 1 d . . . . . Cl3 Cl -0.08812(6) 0.68852(5) 1.02204(4) 0.03252(13) Uani 1 1 d . . . . . Cl4 Cl 0.27039(6) 0.85314(5) 0.65979(5) 0.03481(14) Uani 1 1 d . . . . . Cl5 Cl 0.32060(7) 1.04568(5) 0.92678(6) 0.04200(15) Uani 1 1 d . . . . . Cl6 Cl 0.14239(7) 0.96275(5) 1.10986(5) 0.03604(14) Uani 1 1 d . . . . . O1 O 0.04925(16) 0.60573(13) 0.60743(12) 0.0225(3) Uani 1 1 d . . . . . O2 O -0.04998(15) 0.36067(13) 0.61851(13) 0.0241(3) Uani 1 1 d . . . . . O3 O 0.25854(15) 0.52793(13) 0.45488(13) 0.0236(3) Uani 1 1 d . . . . . O4 O 0.17848(18) 0.26211(14) 0.47054(15) 0.0306(3) Uani 1 1 d . . . . . O5 O 0.29214(17) 0.48305(16) 0.69472(14) 0.0318(3) Uani 1 1 d . . . . . O6 O -0.12963(17) 0.54244(14) 0.76976(13) 0.0267(3) Uani 1 1 d . . . . . O7 O -0.31768(15) 0.33659(13) 0.66830(13) 0.0241(3) Uani 1 1 d . . . . . C8 C -0.0184(2) 0.65550(19) 0.80207(18) 0.0229(4) Uani 1 1 d . . . . . C9 C -0.2816(2) 0.2778(2) 0.7587(2) 0.0289(4) Uani 1 1 d . . . . . H9A H -0.2323 0.3461 0.8384 0.035 Uiso 1 1 calc R . . . . H9B H -0.2086 0.2218 0.7345 0.035 Uiso 1 1 calc R . . . . C10 C 0.0662(2) 0.68757(18) 0.71881(18) 0.0220(4) Uani 1 1 d . . . . . C11 C 0.1146(2) 0.8586(2) 0.96180(18) 0.0269(4) Uani 1 1 d . . . . . C12 C 0.1943(2) 0.8952(2) 0.8802(2) 0.0284(4) Uani 1 1 d . . . . . C13 C 0.0086(2) 0.7381(2) 0.92210(18) 0.0249(4) Uani 1 1 d . . . . . C14 C 0.4394(2) 0.5735(2) 0.7114(2) 0.0326(5) Uani 1 1 d . . . . . H14A H 0.4217 0.6517 0.6943 0.039 Uiso 1 1 calc R . . . . H14B H 0.5047 0.5322 0.6566 0.039 Uiso 1 1 calc R . . . . C15 C 0.3527(3) 0.1256(2) 0.4188(2) 0.0345(5) Uani 1 1 d . . . . . H15A H 0.4447 0.1420 0.4833 0.041 Uiso 1 1 calc R . . . . H15B H 0.3734 0.0755 0.3396 0.041 Uiso 1 1 calc R . . . . C16 C 0.1703(2) 0.8105(2) 0.76121(19) 0.0261(4) Uani 1 1 d . . . . . C17 C -0.4316(3) 0.1985(2) 0.7673(2) 0.0349(5) Uani 1 1 d . . . . . H17A H -0.4796 0.1315 0.6879 0.052 Uiso 1 1 calc GR . . . . H17B H -0.5026 0.2550 0.7922 0.052 Uiso 1 1 calc GR . . . . H17C H -0.4106 0.1571 0.8273 0.052 Uiso 1 1 calc GR . . . . C18 C 0.2069(3) 0.0536(2) 0.4449(3) 0.0427(6) Uani 1 1 d . . . . . H18A H 0.1299 0.0014 0.3690 0.051 Uiso 1 1 calc R . . . . H18B H 0.2325 -0.0042 0.4892 0.051 Uiso 1 1 calc R . . . . C19 C 0.2697(3) 0.4724(3) 0.8099(2) 0.0353(5) Uani 1 1 d . . . . . H19A H 0.2949 0.3921 0.8173 0.042 Uiso 1 1 calc R . . . . H19B H 0.1607 0.4715 0.8189 0.042 Uiso 1 1 calc R . . . . C20 C 0.3806(3) 0.5914(3) 0.9041(2) 0.0491(7) Uani 1 1 d . . . . . H20A H 0.4119 0.5763 0.9807 0.059 Uiso 1 1 calc R . . . . H20B H 0.3339 0.6677 0.9212 0.059 Uiso 1 1 calc R . . . . C21 C 0.5172(3) 0.6092(3) 0.8427(2) 0.0483(6) Uani 1 1 d . . . . . H21A H 0.5792 0.7002 0.8764 0.058 Uiso 1 1 calc R . . . . H21B H 0.5858 0.5508 0.8518 0.058 Uiso 1 1 calc R . . . . C23 C 0.3143(3) 0.2523(2) 0.4169(2) 0.0364(5) Uani 1 1 d . . . . . H23A H 0.4027 0.3268 0.4645 0.044 Uiso 1 1 calc R . . . . H23B H 0.2918 0.2513 0.3325 0.044 Uiso 1 1 calc R . . . . C24 C 0.1477(3) 0.1612(2) 0.5215(3) 0.0445(6) Uani 1 1 d . . . . . H24A H 0.0347 0.1330 0.5175 0.053 Uiso 1 1 calc R . . . . H24B H 0.2032 0.1917 0.6072 0.053 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 0.02118(18) 0.02092(18) 0.02359(18) 0.00995(14) 0.00790(13) 0.00347(13) P2 0.0207(2) 0.0193(2) 0.0227(2) 0.00865(19) 0.00757(18) 0.00194(18) Cl3 0.0350(3) 0.0390(3) 0.0232(2) 0.0113(2) 0.00930(19) 0.0044(2) Cl4 0.0380(3) 0.0260(3) 0.0379(3) 0.0106(2) 0.0157(2) -0.0036(2) Cl5 0.0450(3) 0.0233(3) 0.0442(3) 0.0014(2) 0.0094(2) -0.0066(2) Cl6 0.0418(3) 0.0319(3) 0.0255(3) 0.0003(2) 0.0025(2) 0.0076(2) O1 0.0254(7) 0.0193(6) 0.0221(6) 0.0059(5) 0.0077(5) 0.0035(5) O2 0.0235(7) 0.0245(7) 0.0288(7) 0.0141(6) 0.0103(5) 0.0045(5) O3 0.0220(6) 0.0248(7) 0.0273(7) 0.0129(6) 0.0091(5) 0.0041(5) O4 0.0325(8) 0.0253(7) 0.0432(9) 0.0179(7) 0.0200(7) 0.0098(6) O5 0.0239(7) 0.0438(9) 0.0288(8) 0.0194(7) 0.0044(6) -0.0011(6) O6 0.0294(7) 0.0239(7) 0.0240(7) 0.0069(6) 0.0103(6) -0.0019(6) O7 0.0229(7) 0.0239(7) 0.0279(7) 0.0132(6) 0.0076(5) 0.0022(5) C8 0.0228(9) 0.0205(9) 0.0248(9) 0.0084(8) 0.0051(7) 0.0030(7) C9 0.0286(10) 0.0317(11) 0.0343(11) 0.0217(9) 0.0092(8) 0.0060(8) C10 0.0221(9) 0.0199(9) 0.0239(9) 0.0074(7) 0.0052(7) 0.0048(7) C11 0.0293(10) 0.0231(10) 0.0241(10) 0.0033(8) 0.0034(8) 0.0066(8) C12 0.0277(10) 0.0204(9) 0.0341(11) 0.0072(8) 0.0051(8) 0.0033(8) C13 0.0254(9) 0.0266(10) 0.0240(10) 0.0097(8) 0.0062(7) 0.0071(8) C14 0.0230(10) 0.0350(12) 0.0370(12) 0.0136(10) 0.0050(9) -0.0005(8) C15 0.0321(11) 0.0305(11) 0.0421(13) 0.0107(10) 0.0117(9) 0.0107(9) C16 0.0260(10) 0.0228(10) 0.0301(10) 0.0097(8) 0.0085(8) 0.0044(8) C17 0.0348(12) 0.0328(11) 0.0450(13) 0.0236(10) 0.0144(10) 0.0044(9) C18 0.0468(14) 0.0317(12) 0.0585(16) 0.0226(12) 0.0211(12) 0.0115(11) C19 0.0322(11) 0.0515(14) 0.0318(11) 0.0248(11) 0.0098(9) 0.0121(10) C20 0.0476(15) 0.0656(18) 0.0326(13) 0.0110(12) 0.0072(11) 0.0216(13) C21 0.0383(13) 0.0523(16) 0.0396(14) 0.0059(12) -0.0006(11) -0.0008(11) C23 0.0373(12) 0.0305(11) 0.0477(14) 0.0150(10) 0.0237(10) 0.0102(9) C24 0.0531(15) 0.0335(12) 0.0625(17) 0.0280(12) 0.0307(13) 0.0142(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 O1 Ni1 O1 85.28(6) 2_566 . ? O1 Ni1 O2 87.28(6) 2_566 . ? O1 Ni1 O3 84.39(5) 2_566 . ? O1 Ni1 O3 86.94(5) . . ? O1 Ni1 O4 91.37(6) 2_566 . ? O1 Ni1 O4 176.55(6) . . ? O1 Ni1 O5 93.72(6) . . ? O1 Ni1 O5 178.59(6) 2_566 . ? O2 Ni1 O1 85.17(5) . . ? O2 Ni1 O3 168.96(6) . . ? O2 Ni1 O4 93.85(6) . . ? O2 Ni1 O5 93.63(6) . . ? O3 Ni1 O5 94.57(6) . . ? O4 Ni1 O3 93.58(6) . . ? O4 Ni1 O5 89.64(7) . . ? O2 P2 O3 122.13(8) . 2_566 ? O2 P2 O6 107.95(8) . . ? O2 P2 O7 110.20(8) . . ? O3 P2 O6 110.09(8) 2_566 . ? O3 P2 O7 105.81(8) 2_566 . ? O7 P2 O6 97.97(7) . . ? Ni1 O1 Ni1 94.72(6) 2_566 . ? C10 O1 Ni1 131.18(12) . . ? C10 O1 Ni1 130.24(12) . 2_566 ? P2 O2 Ni1 117.97(8) . . ? P2 O3 Ni1 118.35(8) 2_566 . ? C23 O4 Ni1 122.28(13) . . ? C24 O4 Ni1 121.17(14) . . ? C24 O4 C23 109.06(17) . . ? C14 O5 Ni1 120.80(13) . . ? C19 O5 Ni1 126.00(13) . . ? C19 O5 C14 109.83(17) . . ? C8 O6 P2 127.47(13) . . ? C9 O7 P2 119.62(12) . . ? O6 C8 C10 122.25(17) . . ? O6 C8 C13 116.53(17) . . ? C13 C8 C10 121.22(18) . . ? O7 C9 C17 107.73(17) . . ? O1 C10 C8 121.53(17) . . ? O1 C10 C16 121.76(18) . . ? C16 C10 C8 116.71(18) . . ? C12 C11 Cl6 120.49(16) . . ? C12 C11 C13 119.38(19) . . ? C13 C11 Cl6 120.11(16) . . ? C11 C12 Cl5 119.82(16) . . ? C16 C12 Cl5 120.38(17) . . ? C16 C12 C11 119.80(19) . . ? C8 C13 Cl3 119.06(16) . . ? C8 C13 C11 120.52(19) . . ? C11 C13 Cl3 120.40(16) . . ? O5 C14 C21 105.46(19) . . ? C23 C15 C18 103.85(18) . . ? C10 C16 Cl4 117.39(16) . . ? C12 C16 Cl4 120.37(16) . . ? C12 C16 C10 122.24(19) . . ? C24 C18 C15 102.65(19) . . ? O5 C19 C20 104.7(2) . . ? C19 C20 C21 102.1(2) . . ? C14 C21 C20 103.0(2) . . ? O4 C23 C15 106.09(18) . . ? O4 C24 C18 104.58(19) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.0429(14) 2_566 ? Ni1 O1 2.0498(14) . ? Ni1 O2 2.0460(13) . ? Ni1 O3 2.0588(13) . ? Ni1 O4 2.0532(15) . ? Ni1 O5 2.0610(15) . ? P2 O2 1.4935(14) . ? P2 O3 1.4955(14) 2_566 ? P2 O6 1.6301(15) . ? P2 O7 1.5803(13) . ? Cl3 C13 1.724(2) . ? Cl4 C16 1.723(2) . ? Cl5 C12 1.722(2) . ? Cl6 C11 1.727(2) . ? O1 Ni1 2.0429(14) 2_566 ? O1 C10 1.317(2) . ? O3 P2 1.4956(14) 2_566 ? O4 C23 1.445(3) . ? O4 C24 1.440(3) . ? O5 C14 1.453(2) . ? O5 C19 1.445(3) . ? O6 C8 1.366(2) . ? O7 C9 1.454(2) . ? C8 C10 1.413(3) . ? C8 C13 1.390(3) . ? C9 C17 1.500(3) . ? C10 C16 1.407(3) . ? C11 C12 1.392(3) . ? C11 C13 1.396(3) . ? C12 C16 1.390(3) . ? C14 C21 1.512(3) . ? C15 C18 1.523(3) . ? C15 C23 1.521(3) . ? C18 C24 1.486(4) . ? C19 C20 1.511(4) . ? C20 C21 1.514(4) . ?