#------------------------------------------------------------------------------ #$Date: 2019-11-08 04:14:57 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225335 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551201.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_1551201 loop_ _publ_author_name 'Tran, Thi V.' 'Nguyen, Yennie H.' 'Do, Loi H.' _publ_section_title ; Development of highly productive nickel--sodium phenoxyphosphine ethylene polymerization catalysts and their reaction temperature profiles ; _journal_issue 27 _journal_name_full 'Polymer Chemistry' _journal_page_first 3718 _journal_paper_doi 10.1039/C9PY00610A _journal_volume 10 _journal_year 2019 _chemical_formula_sum 'C70 H62 B F24 Na Ni O7 P2' _chemical_formula_weight 1625.64 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-04-25 deposited with the CCDC. 2019-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.5400(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.7805(17) _cell_length_b 17.3222(14) _cell_length_c 19.7901(16) _cell_measurement_reflns_used 9691 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.55 _cell_measurement_theta_min 2.42 _cell_volume 7288.4(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_unetI/netI 0.0236 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 43028 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.554 _diffrn_reflns_theta_min 1.516 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6734 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.481 _exptl_crystal_description block _exptl_crystal_F_000 3312 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _refine_diff_density_max 1.893 _refine_diff_density_min -1.533 _refine_diff_density_rms 0.102 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 944 _refine_ls_number_reflns 16670 _refine_ls_number_restraints 57 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0666 _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^)+(0.1103P)^2^+14.2674P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1861 _refine_ls_wR_factor_ref 0.2007 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14039 _reflns_number_total 16670 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 14_a.res in P2(1)/c 14_a.res created by SHELXL-2018/3 at 15:44:38 on 11-May-2018 REM Old TITL 14 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.213, Rweak 0.006, Alpha 0.043 REM 0.303 for 522 systematic absences, Orientation as input REM Formula found by SHELXT: C71 O6 B2 F23 Na P2 Br CELL 0.71073 21.7805 17.3222 19.7901 90.000 102.540 90.000 ZERR 4.000 0.0017 0.0014 0.0016 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C Ni O F Na P B H UNIT 280 4 28 96 4 8 4 248 TEMP -150.060 ACTA SIZE 0.120 0.180 0.250 L.S. 25 LIST 6 FMAP 2 PLAN 10 WGHT 0.110300 14.267400 FVAR 0.16989 0.60606 0.52759 0.59610 C1 1 0.740011 0.113333 0.389894 11.00000 0.01947 0.02178 = 0.02117 0.00019 0.00828 -0.00146 C2 1 0.761392 0.046929 0.360534 11.00000 0.02435 0.02204 = 0.02904 0.00219 0.01008 0.00348 C3 1 0.724758 0.014968 0.300882 11.00000 0.03118 0.02140 = 0.02887 -0.00252 0.01001 -0.00038 AFIX 43 H3 8 0.739666 -0.029921 0.281994 11.00000 -1.20000 AFIX 0 C4 1 0.666854 0.046015 0.267405 11.00000 0.03090 0.02551 = 0.02444 -0.00306 0.00588 -0.00410 C5 1 0.647868 0.114662 0.293695 11.00000 0.02343 0.02487 = 0.02439 0.00083 0.00555 -0.00078 AFIX 43 H5 8 0.610105 0.139125 0.270529 11.00000 -1.20000 AFIX 0 C6 1 0.683924 0.147719 0.353796 11.00000 0.02017 0.01978 = 0.02456 0.00093 0.00998 -0.00091 C7 1 0.626736 0.005937 0.205319 11.00000 0.04262 0.03482 = 0.03558 -0.01027 0.00108 -0.00491 AFIX 137 H7A 8 0.605548 0.044675 0.172250 11.00000 -1.50000 H7B 8 0.595207 -0.026257 0.220386 11.00000 -1.50000 H7C 8 0.653467 -0.026567 0.183105 11.00000 -1.50000 AFIX 0 C8 1 0.824965 0.014045 0.392812 11.00000 0.02770 0.02574 = 0.03077 -0.00201 0.00585 0.00705 AFIX 23 H8A 8 0.825387 -0.001420 0.441069 11.00000 -1.20000 H8AB 8 0.832221 -0.032842 0.367025 11.00000 -1.20000 AFIX 0 C9 1 0.876319 0.098406 0.325934 11.00000 0.04120 0.05461 = 0.02833 -0.00124 0.01661 0.00070 AFIX 23 H9A 8 0.834706 0.120412 0.304464 11.00000 -1.20000 H9AB 8 0.885953 0.056747 0.295590 11.00000 -1.20000 AFIX 0 C10 1 0.925652 0.159785 0.334132 11.00000 0.03629 0.06180 = 0.03806 0.00937 0.02015 0.00223 AFIX 23 H10A 8 0.967348 0.137947 0.355521 11.00000 -1.20000 H10B 8 0.927692 0.181564 0.288421 11.00000 -1.20000 AFIX 0 C11 1 0.949624 0.283962 0.385260 11.00000 0.03194 0.05381 = 0.05949 0.02716 0.00389 -0.00874 AFIX 23 H11A 8 0.935122 0.321038 0.347058 11.00000 -1.20000 H11B 8 0.993062 0.267876 0.384391 11.00000 -1.20000 AFIX 0 C12 1 0.947959 0.320926 0.453697 11.00000 0.03691 0.03616 = 0.07471 0.00814 0.00770 -0.00533 AFIX 23 H12A 8 0.979997 0.362340 0.463301 11.00000 -1.20000 H12B 8 0.906225 0.344965 0.450762 11.00000 -1.20000 AFIX 0 C13 1 1.021896 0.236109 0.524669 11.00000 0.02154 0.04853 = 0.04325 -0.00155 0.00566 -0.00568 AFIX 23 H13A 8 1.052030 0.275816 0.547571 11.00000 -1.20000 H13B 8 1.034066 0.220190 0.481345 11.00000 -1.20000 AFIX 0 C14 1 1.023520 0.168457 0.571066 11.00000 0.02032 0.04987 = 0.03551 -0.00822 0.00329 -0.00542 AFIX 23 H14A 8 1.066146 0.145455 0.581472 11.00000 -1.20000 H14B 8 1.013124 0.184738 0.615215 11.00000 -1.20000 AFIX 0 C15 1 0.983896 0.040467 0.571932 11.00000 0.03438 0.03803 = 0.04146 -0.00020 0.00911 0.00620 AFIX 137 H15A 8 0.951646 0.005217 0.546908 11.00000 -1.50000 H15B 8 0.977923 0.047746 0.619192 11.00000 -1.50000 H15C 8 1.025664 0.018529 0.573551 11.00000 -1.50000 AFIX 0 C16 1 0.588217 0.260172 0.358360 11.00000 0.01773 0.02345 = 0.03191 -0.00340 0.00688 -0.00008 C17 1 0.570342 0.316076 0.307219 11.00000 0.02288 0.02890 = 0.03521 0.00246 0.00178 0.00210 AFIX 43 H17 8 0.601693 0.344888 0.291603 11.00000 -1.20000 AFIX 0 C18 1 0.506789 0.330260 0.278614 11.00000 0.02516 0.04187 = 0.04929 0.00368 -0.00337 0.00671 AFIX 43 H18 8 0.494797 0.368218 0.243584 11.00000 -1.20000 AFIX 0 C19 1 0.461667 0.288118 0.302159 11.00000 0.01877 0.05280 = 0.06657 -0.00492 -0.00118 0.00384 AFIX 43 H19 8 0.418427 0.297741 0.283142 11.00000 -1.20000 AFIX 0 C20 1 0.478235 0.232163 0.352905 11.00000 0.01923 0.04216 = 0.06964 -0.00370 0.01308 -0.00387 AFIX 43 H20 8 0.446601 0.203820 0.368452 11.00000 -1.20000 AFIX 0 C21 1 0.541587 0.217731 0.380985 11.00000 0.02204 0.02739 = 0.04541 -0.00300 0.01302 -0.00102 C22 1 0.519744 0.121218 0.459479 11.00000 0.04265 0.06842 = 0.11285 0.03893 0.03746 -0.00737 AFIX 137 H22A 8 0.542428 0.087605 0.496406 11.00000 -1.50000 H22B 8 0.493679 0.089657 0.423168 11.00000 -1.50000 H22C 8 0.492857 0.156785 0.478524 11.00000 -1.50000 AFIX 0 C23 1 0.715256 0.307791 0.357242 11.00000 0.01768 0.02351 = 0.02576 0.00667 0.00243 -0.00155 C24 1 0.752636 0.285542 0.311626 11.00000 0.02464 0.03560 = 0.03032 0.00944 0.00822 -0.00087 AFIX 43 H24 8 0.751912 0.233403 0.296585 11.00000 -1.20000 AFIX 0 C25 1 0.791103 0.338857 0.287766 11.00000 0.02948 0.05339 = 0.04213 0.01824 0.01295 -0.00534 AFIX 43 H25 8 0.816167 0.323286 0.256424 11.00000 -1.20000 AFIX 0 C26 1 0.792341 0.414090 0.310082 11.00000 0.03387 0.05240 = 0.05220 0.02166 0.00586 -0.01845 AFIX 43 H26 8 0.818795 0.450257 0.294166 11.00000 -1.20000 AFIX 0 C27 1 0.755955 0.438160 0.355118 11.00000 0.04075 0.02821 = 0.04731 0.00775 -0.00316 -0.01421 AFIX 43 H27 8 0.757005 0.490528 0.369584 11.00000 -1.20000 AFIX 0 C28 1 0.717482 0.384866 0.379341 11.00000 0.02510 0.02468 = 0.03209 0.00480 -0.00235 -0.00389 C29 1 0.678223 0.480782 0.445500 11.00000 0.04981 0.02087 = 0.08036 -0.00915 0.00759 0.00444 AFIX 137 H29A 8 0.650192 0.485686 0.477877 11.00000 -1.50000 H29B 8 0.662492 0.512987 0.404701 11.00000 -1.50000 H29C 8 0.720623 0.497707 0.468191 11.00000 -1.50000 AFIX 0 C30 1 0.795439 0.192351 0.577465 11.00000 0.02444 0.03415 = 0.02163 -0.00235 0.00851 0.00604 C31 1 0.844691 0.242653 0.603698 11.00000 0.03097 0.03839 = 0.02814 -0.00754 0.00991 0.00030 AFIX 43 H31 8 0.842740 0.294355 0.587359 11.00000 -1.20000 AFIX 0 C32 1 0.897349 0.218543 0.653941 11.00000 0.02470 0.06315 = 0.03073 -0.01738 0.00775 -0.00116 AFIX 43 H32 8 0.930261 0.254050 0.671203 11.00000 -1.20000 AFIX 0 C33 1 0.901398 0.143913 0.678148 11.00000 0.02590 0.06663 = 0.02648 -0.00743 0.00375 0.01644 AFIX 43 H33 8 0.936791 0.127908 0.712341 11.00000 -1.20000 AFIX 0 C34 1 0.853178 0.091844 0.652162 11.00000 0.03896 0.04420 = 0.02794 0.00179 0.00865 0.01606 AFIX 43 H34 8 0.855742 0.040044 0.668302 11.00000 -1.20000 AFIX 0 C35 1 0.801459 0.116033 0.602643 11.00000 0.02874 0.03394 = 0.02636 -0.00147 0.00641 0.00626 AFIX 43 H35 8 0.769054 0.079953 0.585148 11.00000 -1.20000 AFIX 0 C36 1 0.724680 0.353128 0.617892 11.00000 0.05161 0.06846 = 0.07329 -0.04586 0.00092 0.01519 AFIX 137 H36A 8 0.735215 0.392727 0.586902 11.00000 -1.50000 H36B 8 0.763429 0.332911 0.647303 11.00000 -1.50000 H36C 8 0.698319 0.375863 0.647007 11.00000 -1.50000 AFIX 0 C37 1 0.661219 0.210420 0.631194 11.00000 0.06053 0.08955 = 0.04371 0.02725 0.03193 0.03274 AFIX 137 H37A 8 0.632321 0.170591 0.607766 11.00000 -1.50000 H37B 8 0.640761 0.240083 0.662291 11.00000 -1.50000 H37C 8 0.699336 0.185925 0.658067 11.00000 -1.50000 AFIX 0 C38 1 0.606239 0.319559 0.531238 11.00000 0.03391 0.05034 = 0.03578 -0.00278 0.01339 0.01395 AFIX 137 H38A 8 0.575114 0.279286 0.514235 11.00000 -1.50000 H38B 8 0.610031 0.353792 0.492930 11.00000 -1.50000 H38C 8 0.592736 0.349556 0.567412 11.00000 -1.50000 AFIX 0 C39 1 0.249312 0.212232 0.608492 11.00000 0.02263 0.02056 = 0.02105 0.00325 0.00939 -0.00060 C40 1 0.301962 0.162605 0.617354 11.00000 0.02708 0.02593 = 0.02342 0.00530 0.01108 0.00386 AFIX 43 H40 8 0.331787 0.163199 0.660223 11.00000 -1.20000 AFIX 0 C41 1 0.311529 0.113144 0.565635 11.00000 0.03567 0.02348 = 0.03504 0.00502 0.02075 0.00531 C42 1 0.268311 0.108107 0.503197 11.00000 0.04256 0.02159 = 0.03419 -0.00409 0.02177 -0.00156 AFIX 43 H42 8 0.275221 0.074417 0.467704 11.00000 -1.20000 AFIX 0 C43 1 0.214779 0.153388 0.493773 11.00000 0.03389 0.02540 = 0.02621 -0.00416 0.01249 -0.00792 C44 1 0.205391 0.204416 0.545691 11.00000 0.02377 0.02173 = 0.02339 -0.00026 0.00880 -0.00375 AFIX 43 H44 8 0.168094 0.234586 0.537997 11.00000 -1.20000 AFIX 0 C45 1 0.165987 0.148723 0.427581 11.00000 0.04174 0.03983 = 0.02953 -0.01004 0.00770 -0.01154 C46 1 0.371002 0.066763 0.574508 11.00000 0.04535 0.03563 = 0.04689 0.00922 0.02773 0.01340 C47 1 0.307239 0.328664 0.688737 11.00000 0.02221 0.02230 = 0.02161 0.00498 0.00236 0.00035 C48 1 0.356039 0.327160 0.652856 11.00000 0.02053 0.03808 = 0.02717 0.00934 0.00272 -0.00310 AFIX 43 H48 8 0.352899 0.293032 0.614680 11.00000 -1.20000 AFIX 0 C49 1 0.408998 0.374003 0.671260 11.00000 0.02654 0.06311 = 0.03486 0.01729 -0.00295 -0.01504 C50 1 0.414470 0.426021 0.725856 11.00000 0.04314 0.05441 = 0.03961 0.01320 -0.01103 -0.02729 AFIX 43 H50 8 0.450672 0.457782 0.738859 11.00000 -1.20000 AFIX 0 C51 1 0.366488 0.430381 0.760402 11.00000 0.04719 0.03076 = 0.03613 0.00656 -0.00919 -0.01160 C52 1 0.313521 0.383028 0.742543 11.00000 0.03250 0.02320 = 0.02801 0.00189 -0.00016 -0.00188 AFIX 43 H52 8 0.280950 0.387679 0.767369 11.00000 -1.20000 AFIX 0 C53 1 0.460158 0.369293 0.632256 11.00000 0.02809 0.12481 = 0.03677 0.01633 0.00246 -0.03503 C54 1 0.369421 0.485700 0.818869 11.00000 0.07390 0.03565 = 0.04909 -0.00527 -0.02065 -0.00891 C55 1 0.236409 0.222603 0.737900 11.00000 0.02139 0.01975 = 0.02011 0.00020 0.00665 0.00244 C56 1 0.279926 0.219236 0.801300 11.00000 0.02059 0.02222 = 0.02095 -0.00008 0.00531 0.00186 AFIX 43 H56 8 0.317810 0.248051 0.806915 11.00000 -1.20000 AFIX 0 C57 1 0.269296 0.174617 0.856781 11.00000 0.02562 0.02723 = 0.01967 0.00212 0.00415 0.00476 C58 1 0.214354 0.132728 0.851220 11.00000 0.03111 0.02810 = 0.01889 0.00293 0.00849 0.00050 AFIX 43 H58 8 0.207013 0.102780 0.888900 11.00000 -1.20000 AFIX 0 C59 1 0.169960 0.135704 0.788623 11.00000 0.02879 0.02605 = 0.02065 -0.00093 0.00834 -0.00231 C60 1 0.181394 0.178575 0.733357 11.00000 0.02384 0.02468 = 0.01758 0.00028 0.00486 0.00015 AFIX 43 H60 8 0.150959 0.178157 0.690939 11.00000 -1.20000 AFIX 0 C61 1 0.318272 0.173489 0.923566 11.00000 0.02934 0.03430 = 0.02256 0.00267 0.00334 0.00234 C62 1 0.107969 0.095885 0.783038 11.00000 0.03598 0.03428 = 0.02343 -0.00004 0.00837 -0.00856 C63 1 0.184011 0.332810 0.647935 11.00000 0.01848 0.02088 = 0.02089 -0.00081 0.00431 -0.00046 C64 1 0.140480 0.348292 0.689235 11.00000 0.02259 0.03024 = 0.01824 -0.00054 0.00505 0.00023 AFIX 43 H64 8 0.145270 0.323116 0.732714 11.00000 -1.20000 AFIX 0 C65 1 0.090571 0.399325 0.668487 11.00000 0.02093 0.03831 = 0.02300 -0.00470 0.00660 0.00281 C66 1 0.081261 0.437435 0.605555 11.00000 0.02224 0.03122 = 0.02676 -0.00166 0.00277 0.00704 AFIX 43 H66 8 0.046784 0.471615 0.591208 11.00000 -1.20000 AFIX 0 C67 1 0.124047 0.423934 0.564234 11.00000 0.02532 0.02403 = 0.02296 -0.00059 0.00351 0.00088 C68 1 0.174471 0.373827 0.585297 11.00000 0.02155 0.02159 = 0.02041 -0.00050 0.00655 -0.00081 AFIX 43 H68 8 0.203526 0.367097 0.556249 11.00000 -1.20000 AFIX 0 C69 1 0.043912 0.412912 0.713134 11.00000 0.02559 0.06183 = 0.02824 -0.00397 0.00919 0.01178 C70 1 0.114004 0.459092 0.493766 11.00000 0.03024 0.04078 = 0.02715 0.00943 0.00681 0.00933 NI1 2 0.729137 0.214247 0.498935 11.00000 0.01904 0.02264 = 0.02020 -0.00019 0.00634 0.00231 O1 3 0.772194 0.144216 0.448584 11.00000 0.01750 0.02740 = 0.02484 -0.00192 0.00624 0.00296 O2 3 0.875298 0.068065 0.392901 11.00000 0.02370 0.03549 = 0.03013 0.00030 0.00883 0.00496 O3 3 0.908974 0.218222 0.377283 11.00000 0.02667 0.04294 = 0.04106 0.00852 0.01251 -0.00189 O4 3 0.978736 0.113088 0.537221 11.00000 0.02245 0.03733 = 0.03478 -0.00119 -0.00016 -0.00109 O5 3 0.959530 0.267120 0.509305 11.00000 0.02474 0.03686 = 0.05109 -0.00293 0.00891 -0.00233 O6 3 0.563887 0.164401 0.430802 11.00000 0.02828 0.03679 = 0.05376 0.01114 0.02040 -0.00240 O7 3 0.680207 0.402023 0.424701 11.00000 0.03852 0.02029 = 0.04450 -0.00423 0.00724 0.00012 F1 4 0.402128 0.060258 0.640383 11.00000 0.04829 0.06757 = 0.05258 0.01345 0.01840 0.03164 F2 4 0.410562 0.097460 0.539378 11.00000 0.05015 0.06889 = 0.08744 0.03234 0.04833 0.01988 F3 4 0.360664 -0.005104 0.550760 11.00000 0.06828 0.03584 = 0.09552 -0.00659 0.03208 0.01958 F4 4 0.187355 0.118701 0.375598 11.00000 0.06835 0.13439 = 0.03917 -0.04317 0.00629 0.01105 F5 4 0.116373 0.106850 0.434042 11.00000 0.05771 0.08440 = 0.05700 0.00931 -0.00655 -0.04135 F6 4 0.141657 0.217337 0.405391 11.00000 0.08551 0.04937 = 0.04099 0.00020 -0.02061 -0.00792 EADP F7 F8 F9 F7 4 0.444989 0.328665 0.574822 11.00000 0.04653 0.17544 = 0.08187 0.02377 0.02332 -0.01921 F8 4 0.513055 0.341836 0.668897 11.00000 0.04653 0.17544 = 0.08187 0.02377 0.02332 -0.01921 F9 4 0.475991 0.439225 0.611146 11.00000 0.04653 0.17544 = 0.08187 0.02377 0.02332 -0.01921 SADI F10 F11 F11 F12 F12 F10 F10b F11b F11b F12b F12b F10b SADI C54 F10 C54 F11 C54 F12 SADI C54 F10b C54 F11b C54 F12b EADP F10 F11 F12 F10b F11b F12b Part 1 F10 4 0.378002 0.446813 0.881514 21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F11 4 0.311293 0.521524 0.821132 21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F12 4 0.411174 0.539860 0.829836 21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 Part 2 F10B 4 0.340091 0.546645 0.796503 -21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F11B 4 0.434994 0.510301 0.836290 -21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F12B 4 0.362267 0.454470 0.874842 -21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 Part 0 SADI F13 F14 F14 F15 F15 F13 F13b F14b F14b F15b F15b F13b EADP F13 F14 F15 F13b F14b F15b Part 1 F13 4 0.336793 0.247043 0.944803 31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F14 4 0.371302 0.138245 0.916737 31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F15 4 0.298321 0.142335 0.976176 31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 Part 2 F13B 4 0.353006 0.237366 0.935607 -31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F14B 4 0.357614 0.113612 0.927408 -31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F15B 4 0.290376 0.166319 0.979218 -31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 Part 0 F16 4 0.112999 0.028578 0.817301 11.00000 0.04900 0.03714 = 0.03028 0.00243 0.00815 -0.01744 F17 4 0.066222 0.139348 0.806943 11.00000 0.03355 0.05161 = 0.06076 -0.00631 0.02344 -0.00547 F18 4 0.079932 0.079635 0.716883 11.00000 0.04080 0.06269 = 0.02642 0.00059 0.00250 -0.02221 sadi F19 F20 F20 F21 F21 F19 F19b F20b F20b F21b F21b F19b EADP F19 F20 F21 F19b F20b F21b SADI C69 F19 C69 F20 C69 F21 SADI C69 F19b C69 F20b C69 F21b Part 1 F19 4 0.064478 0.395459 0.778470 41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F20 4 0.033672 0.494511 0.718359 41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F21 4 -0.012329 0.389966 0.688223 41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 Part 2 F19B 4 0.044068 0.349001 0.759035 -41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F20B 4 0.051638 0.471722 0.750131 -41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F21B 4 -0.015740 0.406725 0.674954 -41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 Part 0 F22 4 0.066519 0.506961 0.479309 11.00000 0.07516 0.10232 = 0.05704 0.04660 0.02910 0.05805 F23 4 0.098798 0.403360 0.444537 11.00000 0.10626 0.07034 = 0.02719 0.00146 0.00418 -0.01793 F24 4 0.164759 0.489556 0.479143 11.00000 0.04510 0.08515 = 0.04677 0.03449 0.00331 -0.01504 NA1 5 0.879555 0.164822 0.479730 11.00000 0.01693 0.03478 = 0.02944 -0.00116 0.00574 0.00049 P1 6 0.669962 0.236985 0.394496 11.00000 0.01606 0.01843 = 0.02224 0.00113 0.00646 0.00060 P2 6 0.682164 0.275013 0.566820 11.00000 0.03264 0.03942 = 0.02580 -0.00379 0.00952 0.01105 B1 7 0.244229 0.273732 0.670466 11.00000 0.01926 0.02116 = 0.01915 0.00146 0.00655 0.00090 HKLF 4 REM 14_a.res in P2(1)/c REM wR2 = 0.2007, GooF = S = 1.053, Restrained GooF = 1.072 for all data REM R1 = 0.0666 for 14039 Fo > 4sig(Fo) and 0.0779 for all 16670 data REM 944 parameters refined using 57 restraints END WGHT 0.1105 14.1932 REM Highest difference peak 1.893, deepest hole -1.533, 1-sigma level 0.102 Q1 1 0.4573 0.2864 0.5936 11.00000 0.05 1.89 Q2 1 0.4390 0.3776 0.5679 11.00000 0.05 1.73 Q3 1 0.0744 0.4372 0.7773 11.00000 0.05 1.62 Q4 1 0.4608 0.4128 0.5768 11.00000 0.05 1.51 Q5 1 0.0310 0.3249 0.7366 11.00000 0.05 1.46 Q6 1 0.4816 0.4609 0.6426 11.00000 0.05 1.41 Q7 1 0.3790 0.5585 0.7992 11.00000 0.05 1.39 Q8 1 0.0543 0.3681 0.7739 11.00000 0.05 1.24 Q9 1 0.3312 0.0872 0.9348 11.00000 0.05 1.04 Q10 1 0.1133 0.5472 0.5088 11.00000 0.05 1.03 ; _cod_data_source_file c9py00610a2.cif _cod_data_source_block Ni11Na _cod_depositor_comments 'Adding full bibliography for 1551200--1551201.cif.' _cod_database_code 1551201 _shelx_shelxl_version_number 2018/3 _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 0.900 _shelx_estimated_absorpt_t_max 0.950 _shelx_res_file ; TITL 14_a.res in P2(1)/c 14_a.res created by SHELXL-2018/3 at 15:44:38 on 11-May-2018 REM Old TITL 14 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.213, Rweak 0.006, Alpha 0.043 REM 0.303 for 522 systematic absences, Orientation as input REM Formula found by SHELXT: C71 O6 B2 F23 Na P2 Br CELL 0.71073 21.7805 17.3222 19.7901 90.000 102.540 90.000 ZERR 4.000 0.0017 0.0014 0.0016 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C Ni O F Na P B H UNIT 280 4 28 96 4 8 4 248 TEMP -150.060 ACTA SIZE 0.120 0.180 0.250 L.S. 25 LIST 6 FMAP 2 PLAN 10 WGHT 0.110300 14.267400 FVAR 0.16989 0.60606 0.52759 0.59610 C1 1 0.740011 0.113333 0.389894 11.00000 0.01947 0.02178 = 0.02117 0.00019 0.00828 -0.00146 C2 1 0.761392 0.046929 0.360534 11.00000 0.02435 0.02204 = 0.02904 0.00219 0.01008 0.00348 C3 1 0.724758 0.014968 0.300882 11.00000 0.03118 0.02140 = 0.02887 -0.00252 0.01001 -0.00038 AFIX 43 H3 8 0.739666 -0.029921 0.281994 11.00000 -1.20000 AFIX 0 C4 1 0.666854 0.046015 0.267405 11.00000 0.03090 0.02551 = 0.02444 -0.00306 0.00588 -0.00410 C5 1 0.647868 0.114662 0.293695 11.00000 0.02343 0.02487 = 0.02439 0.00083 0.00555 -0.00078 AFIX 43 H5 8 0.610105 0.139125 0.270529 11.00000 -1.20000 AFIX 0 C6 1 0.683924 0.147719 0.353796 11.00000 0.02017 0.01978 = 0.02456 0.00093 0.00998 -0.00091 C7 1 0.626736 0.005937 0.205319 11.00000 0.04262 0.03482 = 0.03558 -0.01027 0.00108 -0.00491 AFIX 137 H7A 8 0.605548 0.044675 0.172250 11.00000 -1.50000 H7B 8 0.595207 -0.026257 0.220386 11.00000 -1.50000 H7C 8 0.653467 -0.026567 0.183105 11.00000 -1.50000 AFIX 0 C8 1 0.824965 0.014045 0.392812 11.00000 0.02770 0.02574 = 0.03077 -0.00201 0.00585 0.00705 AFIX 23 H8A 8 0.825387 -0.001420 0.441069 11.00000 -1.20000 H8AB 8 0.832221 -0.032842 0.367025 11.00000 -1.20000 AFIX 0 C9 1 0.876319 0.098406 0.325934 11.00000 0.04120 0.05461 = 0.02833 -0.00124 0.01661 0.00070 AFIX 23 H9A 8 0.834706 0.120412 0.304464 11.00000 -1.20000 H9AB 8 0.885953 0.056747 0.295590 11.00000 -1.20000 AFIX 0 C10 1 0.925652 0.159785 0.334132 11.00000 0.03629 0.06180 = 0.03806 0.00937 0.02015 0.00223 AFIX 23 H10A 8 0.967348 0.137947 0.355521 11.00000 -1.20000 H10B 8 0.927692 0.181564 0.288421 11.00000 -1.20000 AFIX 0 C11 1 0.949624 0.283962 0.385260 11.00000 0.03194 0.05381 = 0.05949 0.02716 0.00389 -0.00874 AFIX 23 H11A 8 0.935122 0.321038 0.347058 11.00000 -1.20000 H11B 8 0.993062 0.267876 0.384391 11.00000 -1.20000 AFIX 0 C12 1 0.947959 0.320926 0.453697 11.00000 0.03691 0.03616 = 0.07471 0.00814 0.00770 -0.00533 AFIX 23 H12A 8 0.979997 0.362340 0.463301 11.00000 -1.20000 H12B 8 0.906225 0.344965 0.450762 11.00000 -1.20000 AFIX 0 C13 1 1.021896 0.236109 0.524669 11.00000 0.02154 0.04853 = 0.04325 -0.00155 0.00566 -0.00568 AFIX 23 H13A 8 1.052030 0.275816 0.547571 11.00000 -1.20000 H13B 8 1.034066 0.220190 0.481345 11.00000 -1.20000 AFIX 0 C14 1 1.023520 0.168457 0.571066 11.00000 0.02032 0.04987 = 0.03551 -0.00822 0.00329 -0.00542 AFIX 23 H14A 8 1.066146 0.145455 0.581472 11.00000 -1.20000 H14B 8 1.013124 0.184738 0.615215 11.00000 -1.20000 AFIX 0 C15 1 0.983896 0.040467 0.571932 11.00000 0.03438 0.03803 = 0.04146 -0.00020 0.00911 0.00620 AFIX 137 H15A 8 0.951646 0.005217 0.546908 11.00000 -1.50000 H15B 8 0.977923 0.047746 0.619192 11.00000 -1.50000 H15C 8 1.025664 0.018529 0.573551 11.00000 -1.50000 AFIX 0 C16 1 0.588217 0.260172 0.358360 11.00000 0.01773 0.02345 = 0.03191 -0.00340 0.00688 -0.00008 C17 1 0.570342 0.316076 0.307219 11.00000 0.02288 0.02890 = 0.03521 0.00246 0.00178 0.00210 AFIX 43 H17 8 0.601693 0.344888 0.291603 11.00000 -1.20000 AFIX 0 C18 1 0.506789 0.330260 0.278614 11.00000 0.02516 0.04187 = 0.04929 0.00368 -0.00337 0.00671 AFIX 43 H18 8 0.494797 0.368218 0.243584 11.00000 -1.20000 AFIX 0 C19 1 0.461667 0.288118 0.302159 11.00000 0.01877 0.05280 = 0.06657 -0.00492 -0.00118 0.00384 AFIX 43 H19 8 0.418427 0.297741 0.283142 11.00000 -1.20000 AFIX 0 C20 1 0.478235 0.232163 0.352905 11.00000 0.01923 0.04216 = 0.06964 -0.00370 0.01308 -0.00387 AFIX 43 H20 8 0.446601 0.203820 0.368452 11.00000 -1.20000 AFIX 0 C21 1 0.541587 0.217731 0.380985 11.00000 0.02204 0.02739 = 0.04541 -0.00300 0.01302 -0.00102 C22 1 0.519744 0.121218 0.459479 11.00000 0.04265 0.06842 = 0.11285 0.03893 0.03746 -0.00737 AFIX 137 H22A 8 0.542428 0.087605 0.496406 11.00000 -1.50000 H22B 8 0.493679 0.089657 0.423168 11.00000 -1.50000 H22C 8 0.492857 0.156785 0.478524 11.00000 -1.50000 AFIX 0 C23 1 0.715256 0.307791 0.357242 11.00000 0.01768 0.02351 = 0.02576 0.00667 0.00243 -0.00155 C24 1 0.752636 0.285542 0.311626 11.00000 0.02464 0.03560 = 0.03032 0.00944 0.00822 -0.00087 AFIX 43 H24 8 0.751912 0.233403 0.296585 11.00000 -1.20000 AFIX 0 C25 1 0.791103 0.338857 0.287766 11.00000 0.02948 0.05339 = 0.04213 0.01824 0.01295 -0.00534 AFIX 43 H25 8 0.816167 0.323286 0.256424 11.00000 -1.20000 AFIX 0 C26 1 0.792341 0.414090 0.310082 11.00000 0.03387 0.05240 = 0.05220 0.02166 0.00586 -0.01845 AFIX 43 H26 8 0.818795 0.450257 0.294166 11.00000 -1.20000 AFIX 0 C27 1 0.755955 0.438160 0.355118 11.00000 0.04075 0.02821 = 0.04731 0.00775 -0.00316 -0.01421 AFIX 43 H27 8 0.757005 0.490528 0.369584 11.00000 -1.20000 AFIX 0 C28 1 0.717482 0.384866 0.379341 11.00000 0.02510 0.02468 = 0.03209 0.00480 -0.00235 -0.00389 C29 1 0.678223 0.480782 0.445500 11.00000 0.04981 0.02087 = 0.08036 -0.00915 0.00759 0.00444 AFIX 137 H29A 8 0.650192 0.485686 0.477877 11.00000 -1.50000 H29B 8 0.662492 0.512987 0.404701 11.00000 -1.50000 H29C 8 0.720623 0.497707 0.468191 11.00000 -1.50000 AFIX 0 C30 1 0.795439 0.192351 0.577465 11.00000 0.02444 0.03415 = 0.02163 -0.00235 0.00851 0.00604 C31 1 0.844691 0.242653 0.603698 11.00000 0.03097 0.03839 = 0.02814 -0.00754 0.00991 0.00030 AFIX 43 H31 8 0.842740 0.294355 0.587359 11.00000 -1.20000 AFIX 0 C32 1 0.897349 0.218543 0.653941 11.00000 0.02470 0.06315 = 0.03073 -0.01738 0.00775 -0.00116 AFIX 43 H32 8 0.930261 0.254050 0.671203 11.00000 -1.20000 AFIX 0 C33 1 0.901398 0.143913 0.678148 11.00000 0.02590 0.06663 = 0.02648 -0.00743 0.00375 0.01644 AFIX 43 H33 8 0.936791 0.127908 0.712341 11.00000 -1.20000 AFIX 0 C34 1 0.853178 0.091844 0.652162 11.00000 0.03896 0.04420 = 0.02794 0.00179 0.00865 0.01606 AFIX 43 H34 8 0.855742 0.040044 0.668302 11.00000 -1.20000 AFIX 0 C35 1 0.801459 0.116033 0.602643 11.00000 0.02874 0.03394 = 0.02636 -0.00147 0.00641 0.00626 AFIX 43 H35 8 0.769054 0.079953 0.585148 11.00000 -1.20000 AFIX 0 C36 1 0.724680 0.353128 0.617892 11.00000 0.05161 0.06846 = 0.07329 -0.04586 0.00092 0.01519 AFIX 137 H36A 8 0.735215 0.392727 0.586902 11.00000 -1.50000 H36B 8 0.763429 0.332911 0.647303 11.00000 -1.50000 H36C 8 0.698319 0.375863 0.647007 11.00000 -1.50000 AFIX 0 C37 1 0.661219 0.210420 0.631194 11.00000 0.06053 0.08955 = 0.04371 0.02725 0.03193 0.03274 AFIX 137 H37A 8 0.632321 0.170591 0.607766 11.00000 -1.50000 H37B 8 0.640761 0.240083 0.662291 11.00000 -1.50000 H37C 8 0.699336 0.185925 0.658067 11.00000 -1.50000 AFIX 0 C38 1 0.606239 0.319559 0.531238 11.00000 0.03391 0.05034 = 0.03578 -0.00278 0.01339 0.01395 AFIX 137 H38A 8 0.575114 0.279286 0.514235 11.00000 -1.50000 H38B 8 0.610031 0.353792 0.492930 11.00000 -1.50000 H38C 8 0.592736 0.349556 0.567412 11.00000 -1.50000 AFIX 0 C39 1 0.249312 0.212232 0.608492 11.00000 0.02263 0.02056 = 0.02105 0.00325 0.00939 -0.00060 C40 1 0.301962 0.162605 0.617354 11.00000 0.02708 0.02593 = 0.02342 0.00530 0.01108 0.00386 AFIX 43 H40 8 0.331787 0.163199 0.660223 11.00000 -1.20000 AFIX 0 C41 1 0.311529 0.113144 0.565635 11.00000 0.03567 0.02348 = 0.03504 0.00502 0.02075 0.00531 C42 1 0.268311 0.108107 0.503197 11.00000 0.04256 0.02159 = 0.03419 -0.00409 0.02177 -0.00156 AFIX 43 H42 8 0.275221 0.074417 0.467704 11.00000 -1.20000 AFIX 0 C43 1 0.214779 0.153388 0.493773 11.00000 0.03389 0.02540 = 0.02621 -0.00416 0.01249 -0.00792 C44 1 0.205391 0.204416 0.545691 11.00000 0.02377 0.02173 = 0.02339 -0.00026 0.00880 -0.00375 AFIX 43 H44 8 0.168094 0.234586 0.537997 11.00000 -1.20000 AFIX 0 C45 1 0.165987 0.148723 0.427581 11.00000 0.04174 0.03983 = 0.02953 -0.01004 0.00770 -0.01154 C46 1 0.371002 0.066763 0.574508 11.00000 0.04535 0.03563 = 0.04689 0.00922 0.02773 0.01340 C47 1 0.307239 0.328664 0.688737 11.00000 0.02221 0.02230 = 0.02161 0.00498 0.00236 0.00035 C48 1 0.356039 0.327160 0.652856 11.00000 0.02053 0.03808 = 0.02717 0.00934 0.00272 -0.00310 AFIX 43 H48 8 0.352899 0.293032 0.614680 11.00000 -1.20000 AFIX 0 C49 1 0.408998 0.374003 0.671260 11.00000 0.02654 0.06311 = 0.03486 0.01729 -0.00295 -0.01504 C50 1 0.414470 0.426021 0.725856 11.00000 0.04314 0.05441 = 0.03961 0.01320 -0.01103 -0.02729 AFIX 43 H50 8 0.450672 0.457782 0.738859 11.00000 -1.20000 AFIX 0 C51 1 0.366488 0.430381 0.760402 11.00000 0.04719 0.03076 = 0.03613 0.00656 -0.00919 -0.01160 C52 1 0.313521 0.383028 0.742543 11.00000 0.03250 0.02320 = 0.02801 0.00189 -0.00016 -0.00188 AFIX 43 H52 8 0.280950 0.387679 0.767369 11.00000 -1.20000 AFIX 0 C53 1 0.460158 0.369293 0.632256 11.00000 0.02809 0.12481 = 0.03677 0.01633 0.00246 -0.03503 C54 1 0.369421 0.485700 0.818869 11.00000 0.07390 0.03565 = 0.04909 -0.00527 -0.02065 -0.00891 C55 1 0.236409 0.222603 0.737900 11.00000 0.02139 0.01975 = 0.02011 0.00020 0.00665 0.00244 C56 1 0.279926 0.219236 0.801300 11.00000 0.02059 0.02222 = 0.02095 -0.00008 0.00531 0.00186 AFIX 43 H56 8 0.317810 0.248051 0.806915 11.00000 -1.20000 AFIX 0 C57 1 0.269296 0.174617 0.856781 11.00000 0.02562 0.02723 = 0.01967 0.00212 0.00415 0.00476 C58 1 0.214354 0.132728 0.851220 11.00000 0.03111 0.02810 = 0.01889 0.00293 0.00849 0.00050 AFIX 43 H58 8 0.207013 0.102780 0.888900 11.00000 -1.20000 AFIX 0 C59 1 0.169960 0.135704 0.788623 11.00000 0.02879 0.02605 = 0.02065 -0.00093 0.00834 -0.00231 C60 1 0.181394 0.178575 0.733357 11.00000 0.02384 0.02468 = 0.01758 0.00028 0.00486 0.00015 AFIX 43 H60 8 0.150959 0.178157 0.690939 11.00000 -1.20000 AFIX 0 C61 1 0.318272 0.173489 0.923566 11.00000 0.02934 0.03430 = 0.02256 0.00267 0.00334 0.00234 C62 1 0.107969 0.095885 0.783038 11.00000 0.03598 0.03428 = 0.02343 -0.00004 0.00837 -0.00856 C63 1 0.184011 0.332810 0.647935 11.00000 0.01848 0.02088 = 0.02089 -0.00081 0.00431 -0.00046 C64 1 0.140480 0.348292 0.689235 11.00000 0.02259 0.03024 = 0.01824 -0.00054 0.00505 0.00023 AFIX 43 H64 8 0.145270 0.323116 0.732714 11.00000 -1.20000 AFIX 0 C65 1 0.090571 0.399325 0.668487 11.00000 0.02093 0.03831 = 0.02300 -0.00470 0.00660 0.00281 C66 1 0.081261 0.437435 0.605555 11.00000 0.02224 0.03122 = 0.02676 -0.00166 0.00277 0.00704 AFIX 43 H66 8 0.046784 0.471615 0.591208 11.00000 -1.20000 AFIX 0 C67 1 0.124047 0.423934 0.564234 11.00000 0.02532 0.02403 = 0.02296 -0.00059 0.00351 0.00088 C68 1 0.174471 0.373827 0.585297 11.00000 0.02155 0.02159 = 0.02041 -0.00050 0.00655 -0.00081 AFIX 43 H68 8 0.203526 0.367097 0.556249 11.00000 -1.20000 AFIX 0 C69 1 0.043912 0.412912 0.713134 11.00000 0.02559 0.06183 = 0.02824 -0.00397 0.00919 0.01178 C70 1 0.114004 0.459092 0.493766 11.00000 0.03024 0.04078 = 0.02715 0.00943 0.00681 0.00933 NI1 2 0.729137 0.214247 0.498935 11.00000 0.01904 0.02264 = 0.02020 -0.00019 0.00634 0.00231 O1 3 0.772194 0.144216 0.448584 11.00000 0.01750 0.02740 = 0.02484 -0.00192 0.00624 0.00296 O2 3 0.875298 0.068065 0.392901 11.00000 0.02370 0.03549 = 0.03013 0.00030 0.00883 0.00496 O3 3 0.908974 0.218222 0.377283 11.00000 0.02667 0.04294 = 0.04106 0.00852 0.01251 -0.00189 O4 3 0.978736 0.113088 0.537221 11.00000 0.02245 0.03733 = 0.03478 -0.00119 -0.00016 -0.00109 O5 3 0.959530 0.267120 0.509305 11.00000 0.02474 0.03686 = 0.05109 -0.00293 0.00891 -0.00233 O6 3 0.563887 0.164401 0.430802 11.00000 0.02828 0.03679 = 0.05376 0.01114 0.02040 -0.00240 O7 3 0.680207 0.402023 0.424701 11.00000 0.03852 0.02029 = 0.04450 -0.00423 0.00724 0.00012 F1 4 0.402128 0.060258 0.640383 11.00000 0.04829 0.06757 = 0.05258 0.01345 0.01840 0.03164 F2 4 0.410562 0.097460 0.539378 11.00000 0.05015 0.06889 = 0.08744 0.03234 0.04833 0.01988 F3 4 0.360664 -0.005104 0.550760 11.00000 0.06828 0.03584 = 0.09552 -0.00659 0.03208 0.01958 F4 4 0.187355 0.118701 0.375598 11.00000 0.06835 0.13439 = 0.03917 -0.04317 0.00629 0.01105 F5 4 0.116373 0.106850 0.434042 11.00000 0.05771 0.08440 = 0.05700 0.00931 -0.00655 -0.04135 F6 4 0.141657 0.217337 0.405391 11.00000 0.08551 0.04937 = 0.04099 0.00020 -0.02061 -0.00792 EADP F7 F8 F9 F7 4 0.444989 0.328665 0.574822 11.00000 0.04653 0.17544 = 0.08187 0.02377 0.02332 -0.01921 F8 4 0.513055 0.341836 0.668897 11.00000 0.04653 0.17544 = 0.08187 0.02377 0.02332 -0.01921 F9 4 0.475991 0.439225 0.611146 11.00000 0.04653 0.17544 = 0.08187 0.02377 0.02332 -0.01921 SADI F10 F11 F11 F12 F12 F10 F10b F11b F11b F12b F12b F10b SADI C54 F10 C54 F11 C54 F12 SADI C54 F10b C54 F11b C54 F12b EADP F10 F11 F12 F10b F11b F12b Part 1 F10 4 0.378002 0.446813 0.881514 21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F11 4 0.311293 0.521524 0.821132 21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F12 4 0.411174 0.539860 0.829836 21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 Part 2 F10B 4 0.340091 0.546645 0.796503 -21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F11B 4 0.434994 0.510301 0.836290 -21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 F12B 4 0.362267 0.454470 0.874842 -21.00000 0.07330 0.06418 = 0.07095 -0.02938 0.00399 -0.00247 Part 0 SADI F13 F14 F14 F15 F15 F13 F13b F14b F14b F15b F15b F13b EADP F13 F14 F15 F13b F14b F15b Part 1 F13 4 0.336793 0.247043 0.944803 31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F14 4 0.371302 0.138245 0.916737 31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F15 4 0.298321 0.142335 0.976176 31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 Part 2 F13B 4 0.353006 0.237366 0.935607 -31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F14B 4 0.357614 0.113612 0.927408 -31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 F15B 4 0.290376 0.166319 0.979218 -31.00000 0.03951 0.05405 = 0.02819 0.00031 0.00213 0.00604 Part 0 F16 4 0.112999 0.028578 0.817301 11.00000 0.04900 0.03714 = 0.03028 0.00243 0.00815 -0.01744 F17 4 0.066222 0.139348 0.806943 11.00000 0.03355 0.05161 = 0.06076 -0.00631 0.02344 -0.00547 F18 4 0.079932 0.079635 0.716883 11.00000 0.04080 0.06269 = 0.02642 0.00059 0.00250 -0.02221 sadi F19 F20 F20 F21 F21 F19 F19b F20b F20b F21b F21b F19b EADP F19 F20 F21 F19b F20b F21b SADI C69 F19 C69 F20 C69 F21 SADI C69 F19b C69 F20b C69 F21b Part 1 F19 4 0.064478 0.395459 0.778470 41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F20 4 0.033672 0.494511 0.718359 41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F21 4 -0.012329 0.389966 0.688223 41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 Part 2 F19B 4 0.044068 0.349001 0.759035 -41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F20B 4 0.051638 0.471722 0.750131 -41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 F21B 4 -0.015740 0.406725 0.674954 -41.00000 0.03987 0.08425 = 0.04540 -0.00396 0.02231 0.00736 Part 0 F22 4 0.066519 0.506961 0.479309 11.00000 0.07516 0.10232 = 0.05704 0.04660 0.02910 0.05805 F23 4 0.098798 0.403360 0.444537 11.00000 0.10626 0.07034 = 0.02719 0.00146 0.00418 -0.01793 F24 4 0.164759 0.489556 0.479143 11.00000 0.04510 0.08515 = 0.04677 0.03449 0.00331 -0.01504 NA1 5 0.879555 0.164822 0.479730 11.00000 0.01693 0.03478 = 0.02944 -0.00116 0.00574 0.00049 P1 6 0.669962 0.236985 0.394496 11.00000 0.01606 0.01843 = 0.02224 0.00113 0.00646 0.00060 P2 6 0.682164 0.275013 0.566820 11.00000 0.03264 0.03942 = 0.02580 -0.00379 0.00952 0.01105 B1 7 0.244229 0.273732 0.670466 11.00000 0.01926 0.02116 = 0.01915 0.00146 0.00655 0.00090 HKLF 4 REM 14_a.res in P2(1)/c REM wR2 = 0.2007, GooF = S = 1.053, Restrained GooF = 1.072 for all data REM R1 = 0.0666 for 14039 Fo > 4sig(Fo) and 0.0779 for all 16670 data REM 944 parameters refined using 57 restraints END WGHT 0.1105 14.1932 REM Highest difference peak 1.893, deepest hole -1.533, 1-sigma level 0.102 Q1 1 0.4573 0.2864 0.5936 11.00000 0.05 1.89 Q2 1 0.4390 0.3776 0.5679 11.00000 0.05 1.73 Q3 1 0.0744 0.4372 0.7773 11.00000 0.05 1.62 Q4 1 0.4608 0.4128 0.5768 11.00000 0.05 1.51 Q5 1 0.0310 0.3249 0.7366 11.00000 0.05 1.46 Q6 1 0.4816 0.4609 0.6426 11.00000 0.05 1.41 Q7 1 0.3790 0.5585 0.7992 11.00000 0.05 1.39 Q8 1 0.0543 0.3681 0.7739 11.00000 0.05 1.24 Q9 1 0.3312 0.0872 0.9348 11.00000 0.05 1.04 Q10 1 0.1133 0.5472 0.5088 11.00000 0.05 1.03 ; _shelx_res_checksum 59402 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.74001(12) 0.11333(16) 0.38989(14) 0.0202(5) Uani 1 1 d . . . . . C2 C 0.76139(13) 0.04693(17) 0.36053(15) 0.0245(6) Uani 1 1 d . . . . . C3 C 0.72476(14) 0.01497(17) 0.30088(16) 0.0266(6) Uani 1 1 d . . . . . H3 H 0.739666 -0.029921 0.281994 0.032 Uiso 1 1 calc R U . . . C4 C 0.66685(14) 0.04602(17) 0.26740(15) 0.0270(6) Uani 1 1 d . . . . . C5 C 0.64787(13) 0.11466(17) 0.29370(15) 0.0242(5) Uani 1 1 d . . . . . H5 H 0.610105 0.139125 0.270529 0.029 Uiso 1 1 calc R U . . . C6 C 0.68392(12) 0.14772(16) 0.35380(14) 0.0207(5) Uani 1 1 d . . . . . C7 C 0.62674(18) 0.0059(2) 0.20532(18) 0.0388(8) Uani 1 1 d . . . . . H7A H 0.605548 0.044675 0.172250 0.058 Uiso 1 1 calc R U . . . H7B H 0.595207 -0.026257 0.220386 0.058 Uiso 1 1 calc R U . . . H7C H 0.653467 -0.026567 0.183105 0.058 Uiso 1 1 calc R U . . . C8 C 0.82496(14) 0.01405(18) 0.39281(16) 0.0281(6) Uani 1 1 d . . . . . H8A H 0.825387 -0.001420 0.441069 0.034 Uiso 1 1 calc R U . . . H8AB H 0.832221 -0.032842 0.367025 0.034 Uiso 1 1 calc R U . . . C9 C 0.87632(17) 0.0984(2) 0.32593(18) 0.0400(8) Uani 1 1 d . . . . . H9A H 0.834706 0.120412 0.304464 0.048 Uiso 1 1 calc R U . . . H9AB H 0.885953 0.056747 0.295590 0.048 Uiso 1 1 calc R U . . . C10 C 0.92565(17) 0.1598(3) 0.33413(19) 0.0435(9) Uani 1 1 d . . . . . H10A H 0.967348 0.137947 0.355521 0.052 Uiso 1 1 calc R U . . . H10B H 0.927692 0.181564 0.288421 0.052 Uiso 1 1 calc R U . . . C11 C 0.94962(18) 0.2840(2) 0.3853(2) 0.0493(10) Uani 1 1 d . . . . . H11A H 0.935122 0.321038 0.347058 0.059 Uiso 1 1 calc R U . . . H11B H 0.993062 0.267876 0.384391 0.059 Uiso 1 1 calc R U . . . C12 C 0.94796(19) 0.3209(2) 0.4537(2) 0.0499(10) Uani 1 1 d . . . . . H12A H 0.979997 0.362340 0.463301 0.060 Uiso 1 1 calc R U . . . H12B H 0.906225 0.344965 0.450762 0.060 Uiso 1 1 calc R U . . . C13 C 1.02190(15) 0.2361(2) 0.5247(2) 0.0380(7) Uani 1 1 d . . . . . H13A H 1.052030 0.275816 0.547571 0.046 Uiso 1 1 calc R U . . . H13B H 1.034066 0.220190 0.481345 0.046 Uiso 1 1 calc R U . . . C14 C 1.02352(14) 0.1685(2) 0.57107(18) 0.0357(7) Uani 1 1 d . . . . . H14A H 1.066146 0.145455 0.581472 0.043 Uiso 1 1 calc R U . . . H14B H 1.013124 0.184738 0.615215 0.043 Uiso 1 1 calc R U . . . C15 C 0.98390(17) 0.0405(2) 0.57193(19) 0.0378(7) Uani 1 1 d . . . . . H15A H 0.951646 0.005217 0.546908 0.057 Uiso 1 1 calc R U . . . H15B H 0.977923 0.047746 0.619192 0.057 Uiso 1 1 calc R U . . . H15C H 1.025664 0.018529 0.573551 0.057 Uiso 1 1 calc R U . . . C16 C 0.58822(13) 0.26017(17) 0.35836(16) 0.0241(5) Uani 1 1 d . . . . . C17 C 0.57034(14) 0.31608(18) 0.30722(17) 0.0297(6) Uani 1 1 d . . . . . H17 H 0.601693 0.344888 0.291603 0.036 Uiso 1 1 calc R U . . . C18 C 0.50679(16) 0.3303(2) 0.2786(2) 0.0405(8) Uani 1 1 d . . . . . H18 H 0.494797 0.368218 0.243584 0.049 Uiso 1 1 calc R U . . . C19 C 0.46167(16) 0.2881(2) 0.3022(2) 0.0476(10) Uani 1 1 d . . . . . H19 H 0.418427 0.297741 0.283142 0.057 Uiso 1 1 calc R U . . . C20 C 0.47823(15) 0.2322(2) 0.3529(2) 0.0432(9) Uani 1 1 d . . . . . H20 H 0.446601 0.203820 0.368452 0.052 Uiso 1 1 calc R U . . . C21 C 0.54159(14) 0.21773(18) 0.38098(18) 0.0307(7) Uani 1 1 d . . . . . C22 C 0.5197(2) 0.1212(3) 0.4595(3) 0.0715(16) Uani 1 1 d . . . . . H22A H 0.542428 0.087605 0.496406 0.107 Uiso 1 1 calc R U . . . H22B H 0.493679 0.089657 0.423168 0.107 Uiso 1 1 calc R U . . . H22C H 0.492857 0.156785 0.478524 0.107 Uiso 1 1 calc R U . . . C23 C 0.71526(12) 0.30779(16) 0.35724(15) 0.0227(5) Uani 1 1 d . . . . . C24 C 0.75264(14) 0.28554(19) 0.31163(16) 0.0298(6) Uani 1 1 d . . . . . H24 H 0.751912 0.233403 0.296585 0.036 Uiso 1 1 calc R U . . . C25 C 0.79110(16) 0.3389(2) 0.28777(19) 0.0409(8) Uani 1 1 d . . . . . H25 H 0.816167 0.323286 0.256424 0.049 Uiso 1 1 calc R U . . . C26 C 0.79234(17) 0.4141(2) 0.3101(2) 0.0467(10) Uani 1 1 d . . . . . H26 H 0.818795 0.450257 0.294166 0.056 Uiso 1 1 calc R U . . . C27 C 0.75595(17) 0.4382(2) 0.3551(2) 0.0407(8) Uani 1 1 d . . . . . H27 H 0.757005 0.490528 0.369584 0.049 Uiso 1 1 calc R U . . . C28 C 0.71748(14) 0.38487(18) 0.37934(16) 0.0286(6) Uani 1 1 d . . . . . C29 C 0.6782(2) 0.4808(2) 0.4455(3) 0.0513(10) Uani 1 1 d . . . . . H29A H 0.650192 0.485686 0.477877 0.077 Uiso 1 1 calc R U . . . H29B H 0.662492 0.512987 0.404701 0.077 Uiso 1 1 calc R U . . . H29C H 0.720623 0.497707 0.468191 0.077 Uiso 1 1 calc R U . . . C30 C 0.79544(14) 0.19235(18) 0.57746(15) 0.0262(6) Uani 1 1 d . . . . . C31 C 0.84469(15) 0.2427(2) 0.60370(16) 0.0320(7) Uani 1 1 d . . . . . H31 H 0.842740 0.294355 0.587359 0.038 Uiso 1 1 calc R U . . . C32 C 0.89735(16) 0.2185(2) 0.65394(18) 0.0393(8) Uani 1 1 d . . . . . H32 H 0.930261 0.254050 0.671203 0.047 Uiso 1 1 calc R U . . . C33 C 0.90140(15) 0.1439(2) 0.67815(17) 0.0400(8) Uani 1 1 d . . . . . H33 H 0.936791 0.127908 0.712341 0.048 Uiso 1 1 calc R U . . . C34 C 0.85318(16) 0.0918(2) 0.65216(17) 0.0368(7) Uani 1 1 d . . . . . H34 H 0.855742 0.040044 0.668302 0.044 Uiso 1 1 calc R U . . . C35 C 0.80146(15) 0.11603(19) 0.60264(16) 0.0296(6) Uani 1 1 d . . . . . H35 H 0.769054 0.079953 0.585148 0.036 Uiso 1 1 calc R U . . . C36 C 0.7247(2) 0.3531(3) 0.6179(3) 0.0664(15) Uani 1 1 d . . . . . H36A H 0.735215 0.392727 0.586902 0.100 Uiso 1 1 calc R U . . . H36B H 0.763429 0.332911 0.647303 0.100 Uiso 1 1 calc R U . . . H36C H 0.698319 0.375863 0.647007 0.100 Uiso 1 1 calc R U . . . C37 C 0.6612(2) 0.2104(3) 0.6312(2) 0.0615(13) Uani 1 1 d . . . . . H37A H 0.632321 0.170591 0.607766 0.092 Uiso 1 1 calc R U . . . H37B H 0.640761 0.240083 0.662291 0.092 Uiso 1 1 calc R U . . . H37C H 0.699336 0.185925 0.658067 0.092 Uiso 1 1 calc R U . . . C38 C 0.60624(16) 0.3196(2) 0.53124(19) 0.0391(8) Uani 1 1 d . . . . . H38A H 0.575114 0.279286 0.514235 0.059 Uiso 1 1 calc R U . . . H38B H 0.610031 0.353792 0.492930 0.059 Uiso 1 1 calc R U . . . H38C H 0.592736 0.349556 0.567412 0.059 Uiso 1 1 calc R U . . . C39 C 0.24931(13) 0.21223(16) 0.60849(14) 0.0207(5) Uani 1 1 d . . . . . C40 C 0.30196(14) 0.16261(17) 0.61735(15) 0.0246(6) Uani 1 1 d . . . . . H40 H 0.331787 0.163199 0.660223 0.030 Uiso 1 1 calc R U . . . C41 C 0.31153(15) 0.11314(17) 0.56564(17) 0.0294(6) Uani 1 1 d . . . . . C42 C 0.26831(16) 0.10811(18) 0.50320(17) 0.0307(7) Uani 1 1 d . . . . . H42 H 0.275221 0.074417 0.467704 0.037 Uiso 1 1 calc R U . . . C43 C 0.21478(15) 0.15339(18) 0.49377(15) 0.0276(6) Uani 1 1 d . . . . . C44 C 0.20539(13) 0.20442(16) 0.54569(14) 0.0224(5) Uani 1 1 d . . . . . H44 H 0.168094 0.234586 0.537997 0.027 Uiso 1 1 calc R U . . . C45 C 0.16599(17) 0.1487(2) 0.42758(17) 0.0370(7) Uani 1 1 d . . . . . C46 C 0.37100(18) 0.0668(2) 0.5745(2) 0.0399(8) Uani 1 1 d . . . . . C47 C 0.30724(13) 0.32866(16) 0.68874(14) 0.0224(5) Uani 1 1 d . . . . . C48 C 0.35604(13) 0.32716(19) 0.65286(16) 0.0290(6) Uani 1 1 d . . . . . H48 H 0.352899 0.293032 0.614680 0.035 Uiso 1 1 calc R U . . . C49 C 0.40900(16) 0.3740(3) 0.67126(19) 0.0430(9) Uani 1 1 d . . . . . C50 C 0.41447(19) 0.4260(2) 0.7259(2) 0.0488(10) Uani 1 1 d . . . . . H50 H 0.450672 0.457782 0.738859 0.059 Uiso 1 1 calc R U . . . C51 C 0.36649(18) 0.4304(2) 0.76040(19) 0.0408(8) Uani 1 1 d . . . . . C52 C 0.31352(15) 0.38303(17) 0.74254(16) 0.0289(6) Uani 1 1 d . . . . . H52 H 0.280950 0.387679 0.767369 0.035 Uiso 1 1 calc R U . . . C53 C 0.46016(18) 0.3693(4) 0.6323(2) 0.0639(15) Uani 1 1 d . . . . . C54 C 0.3694(2) 0.4857(2) 0.8189(2) 0.0580(12) Uani 1 1 d D . . . . C55 C 0.23641(13) 0.22260(15) 0.73790(14) 0.0201(5) Uani 1 1 d . . . . . C56 C 0.27993(13) 0.21924(16) 0.80130(14) 0.0211(5) Uani 1 1 d . . . . . H56 H 0.317810 0.248051 0.806915 0.025 Uiso 1 1 calc R U . . . C57 C 0.26930(13) 0.17462(17) 0.85678(14) 0.0243(6) Uani 1 1 d . . . . . C58 C 0.21435(14) 0.13273(17) 0.85122(14) 0.0256(6) Uani 1 1 d . . . . . H58 H 0.207013 0.102780 0.888900 0.031 Uiso 1 1 calc R U . . . C59 C 0.16996(14) 0.13570(17) 0.78862(14) 0.0247(6) Uani 1 1 d . . . . . C60 C 0.18139(13) 0.17857(16) 0.73336(14) 0.0220(5) Uani 1 1 d . . . . . H60 H 0.150959 0.178157 0.690939 0.026 Uiso 1 1 calc R U . . . C61 C 0.31827(14) 0.17349(19) 0.92357(15) 0.0291(6) Uani 1 1 d . . . . . C62 C 0.10797(16) 0.09588(19) 0.78304(16) 0.0309(6) Uani 1 1 d . . . . . C63 C 0.18401(12) 0.33281(16) 0.64794(14) 0.0201(5) Uani 1 1 d . . . . . C64 C 0.14048(13) 0.34829(17) 0.68923(14) 0.0236(5) Uani 1 1 d . . . . . H64 H 0.145270 0.323116 0.732714 0.028 Uiso 1 1 calc R U . . . C65 C 0.09057(13) 0.39933(19) 0.66849(15) 0.0271(6) Uani 1 1 d . . . . . C66 C 0.08126(13) 0.43744(18) 0.60555(15) 0.0271(6) Uani 1 1 d . . . . . H66 H 0.046784 0.471615 0.591208 0.033 Uiso 1 1 calc R U . . . C67 C 0.12405(13) 0.42393(17) 0.56423(15) 0.0244(5) Uani 1 1 d . . . . . C68 C 0.17447(13) 0.37383(16) 0.58530(14) 0.0209(5) Uani 1 1 d . . . . . H68 H 0.203526 0.367097 0.556249 0.025 Uiso 1 1 calc R U . . . C69 C 0.04391(15) 0.4129(2) 0.71313(16) 0.0380(8) Uani 1 1 d D . . . . C70 C 0.11400(15) 0.4591(2) 0.49377(16) 0.0326(7) Uani 1 1 d . . . . . Ni1 Ni 0.72914(2) 0.21425(2) 0.49894(2) 0.02031(11) Uani 1 1 d . . . . . O1 O 0.77219(9) 0.14422(12) 0.44858(10) 0.0230(4) Uani 1 1 d . . . . . O2 O 0.87530(10) 0.06806(13) 0.39290(11) 0.0293(4) Uani 1 1 d . . . . . O3 O 0.90897(11) 0.21822(15) 0.37728(13) 0.0361(5) Uani 1 1 d . . . . . O4 O 0.97874(10) 0.11309(14) 0.53722(12) 0.0325(5) Uani 1 1 d . . . . . O5 O 0.95953(11) 0.26712(15) 0.50931(14) 0.0375(5) Uani 1 1 d . . . . . O6 O 0.56389(11) 0.16440(14) 0.43080(14) 0.0379(5) Uani 1 1 d . . . . . O7 O 0.68021(11) 0.40202(13) 0.42470(13) 0.0347(5) Uani 1 1 d . . . . . F1 F 0.40213(11) 0.06026(16) 0.64038(13) 0.0550(6) Uani 1 1 d . . . . . F2 F 0.41056(12) 0.09746(16) 0.53938(16) 0.0638(8) Uani 1 1 d . . . . . F3 F 0.36066(13) -0.00510(14) 0.55076(17) 0.0644(7) Uani 1 1 d . . . . . F4 F 0.18736(14) 0.1187(2) 0.37560(14) 0.0815(10) Uani 1 1 d . . . . . F5 F 0.11637(13) 0.10685(18) 0.43404(14) 0.0693(8) Uani 1 1 d . . . . . F6 F 0.14166(15) 0.21734(15) 0.40539(13) 0.0638(8) Uani 1 1 d . . . . . F7 F 0.44499(15) 0.3287(3) 0.57482(19) 0.0999(8) Uani 1 1 d . . . . . F8 F 0.51306(14) 0.3418(3) 0.66890(19) 0.0999(8) Uani 1 1 d . . . . . F9 F 0.47599(14) 0.4392(3) 0.61115(19) 0.0999(8) Uani 1 1 d . . . . . F10 F 0.3780(3) 0.4468(4) 0.8815(4) 0.0712(7) Uani 0.606(5) 1 d D . P A 1 F11 F 0.3113(2) 0.5215(3) 0.8211(3) 0.0712(7) Uani 0.606(5) 1 d D . P A 1 F12 F 0.4112(3) 0.5399(3) 0.8298(3) 0.0712(7) Uani 0.606(5) 1 d D . P A 1 F10B F 0.3401(4) 0.5466(4) 0.7965(4) 0.0712(7) Uani 0.394(5) 1 d D . P A 2 F11B F 0.4350(3) 0.5103(5) 0.8363(4) 0.0712(7) Uani 0.394(5) 1 d D . P A 2 F12B F 0.3623(4) 0.4545(6) 0.8748(5) 0.0712(7) Uani 0.394(5) 1 d D . P A 2 F13 F 0.3368(3) 0.2470(3) 0.9448(3) 0.0414(5) Uani 0.528(7) 1 d D . P B 1 F14 F 0.3713(2) 0.1382(4) 0.9167(2) 0.0414(5) Uani 0.528(7) 1 d D . P B 1 F15 F 0.2983(3) 0.1423(3) 0.9762(3) 0.0414(5) Uani 0.528(7) 1 d D . P B 1 F13B F 0.3530(3) 0.2374(4) 0.9356(3) 0.0414(5) Uani 0.472(7) 1 d D . P B 2 F14B F 0.3576(3) 0.1136(4) 0.9274(3) 0.0414(5) Uani 0.472(7) 1 d D . P B 2 F15B F 0.2904(3) 0.1663(4) 0.9792(3) 0.0414(5) Uani 0.472(7) 1 d D . P B 2 F16 F 0.11300(10) 0.02858(12) 0.81730(10) 0.0389(5) Uani 1 1 d . . . . . F17 F 0.06622(10) 0.13935(14) 0.80694(13) 0.0466(5) Uani 1 1 d . . . . . F18 F 0.07993(10) 0.07963(14) 0.71688(10) 0.0440(5) Uani 1 1 d . . . . . F19 F 0.06448(18) 0.3955(3) 0.7785(2) 0.0545(6) Uani 0.596(4) 1 d D . P C 1 F20 F 0.03367(19) 0.4945(3) 0.7184(2) 0.0545(6) Uani 0.596(4) 1 d D . P C 1 F21 F -0.0123(3) 0.3900(4) 0.6882(3) 0.0545(6) Uani 0.596(4) 1 d D . P C 1 F19B F 0.0441(3) 0.3490(4) 0.7590(3) 0.0545(6) Uani 0.404(4) 1 d D . P C 2 F20B F 0.0516(3) 0.4717(4) 0.7501(3) 0.0545(6) Uani 0.404(4) 1 d D . P C 2 F21B F -0.0157(4) 0.4067(5) 0.6750(4) 0.0545(6) Uani 0.404(4) 1 d D . P C 2 F22 F 0.06652(14) 0.5070(2) 0.47931(14) 0.0759(10) Uani 1 1 d . . . . . F23 F 0.09880(16) 0.40336(18) 0.44454(12) 0.0695(8) Uani 1 1 d . . . . . F24 F 0.16476(11) 0.48956(17) 0.47914(13) 0.0600(7) Uani 1 1 d . . . . . Na1 Na 0.87955(5) 0.16482(7) 0.47973(6) 0.0269(3) Uani 1 1 d . . . . . P1 P 0.66996(3) 0.23698(4) 0.39450(4) 0.01856(15) Uani 1 1 d . . . . . P2 P 0.68216(4) 0.27501(5) 0.56682(4) 0.03214(19) Uani 1 1 d . . . . . B1 B 0.24423(14) 0.27373(18) 0.67047(15) 0.0195(5) 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 0.0195(12) 0.0218(13) 0.0212(12) 0.0002(10) 0.0083(10) -0.0015(10) C2 0.0243(13) 0.0220(13) 0.0290(14) 0.0022(11) 0.0101(11) 0.0035(10) C3 0.0312(14) 0.0214(13) 0.0289(14) -0.0025(11) 0.0100(11) -0.0004(11) C4 0.0309(14) 0.0255(14) 0.0244(13) -0.0031(11) 0.0059(11) -0.0041(11) C5 0.0234(13) 0.0249(14) 0.0244(13) 0.0008(11) 0.0056(10) -0.0008(11) C6 0.0202(12) 0.0198(12) 0.0246(13) 0.0009(10) 0.0100(10) -0.0009(10) C7 0.0426(18) 0.0348(17) 0.0356(17) -0.0103(14) 0.0011(14) -0.0049(14) C8 0.0277(14) 0.0257(14) 0.0308(15) -0.0020(11) 0.0058(11) 0.0070(11) C9 0.0412(18) 0.055(2) 0.0283(16) -0.0012(15) 0.0166(14) 0.0007(16) C10 0.0363(18) 0.062(2) 0.0381(18) 0.0094(17) 0.0202(15) 0.0022(16) C11 0.0319(17) 0.054(2) 0.059(2) 0.0272(19) 0.0039(16) -0.0087(16) C12 0.0369(19) 0.036(2) 0.075(3) 0.0081(19) 0.0077(18) -0.0053(15) C13 0.0215(14) 0.049(2) 0.0432(19) -0.0016(15) 0.0057(13) -0.0057(13) C14 0.0203(13) 0.050(2) 0.0355(16) -0.0082(15) 0.0033(12) -0.0054(13) C15 0.0344(17) 0.0380(18) 0.0415(18) -0.0002(14) 0.0091(14) 0.0062(14) C16 0.0177(12) 0.0235(13) 0.0319(14) -0.0034(11) 0.0069(10) -0.0001(10) C17 0.0229(14) 0.0289(15) 0.0352(16) 0.0025(12) 0.0018(11) 0.0021(11) C18 0.0252(15) 0.0419(19) 0.049(2) 0.0037(16) -0.0034(14) 0.0067(13) C19 0.0188(15) 0.053(2) 0.067(3) -0.0049(19) -0.0012(15) 0.0038(14) C20 0.0192(14) 0.0422(19) 0.070(3) -0.0037(18) 0.0131(15) -0.0039(13) C21 0.0220(14) 0.0274(15) 0.0454(18) -0.0030(13) 0.0130(13) -0.0010(11) C22 0.043(2) 0.068(3) 0.113(4) 0.039(3) 0.037(3) -0.007(2) C23 0.0177(12) 0.0235(13) 0.0258(13) 0.0067(11) 0.0024(10) -0.0015(10) C24 0.0246(14) 0.0356(16) 0.0303(15) 0.0094(12) 0.0082(12) -0.0009(12) C25 0.0295(16) 0.053(2) 0.0421(19) 0.0182(16) 0.0129(14) -0.0053(15) C26 0.0339(17) 0.052(2) 0.052(2) 0.0217(18) 0.0059(16) -0.0185(16) C27 0.0407(18) 0.0282(16) 0.047(2) 0.0078(14) -0.0032(15) -0.0142(14) C28 0.0251(14) 0.0247(14) 0.0321(15) 0.0048(12) -0.0023(11) -0.0039(11) C29 0.050(2) 0.0209(16) 0.080(3) -0.0091(17) 0.008(2) 0.0044(15) C30 0.0244(13) 0.0342(15) 0.0216(13) -0.0024(11) 0.0085(10) 0.0060(12) C31 0.0310(15) 0.0384(17) 0.0281(15) -0.0075(13) 0.0099(12) 0.0003(13) C32 0.0247(15) 0.063(2) 0.0307(16) -0.0174(16) 0.0078(12) -0.0012(14) C33 0.0259(15) 0.067(2) 0.0265(15) -0.0074(15) 0.0037(12) 0.0164(15) C34 0.0390(17) 0.0442(19) 0.0279(15) 0.0018(13) 0.0086(13) 0.0161(15) C35 0.0287(14) 0.0339(16) 0.0264(14) -0.0015(12) 0.0064(11) 0.0063(12) C36 0.052(2) 0.068(3) 0.073(3) -0.046(3) 0.001(2) 0.015(2) C37 0.061(3) 0.090(4) 0.044(2) 0.027(2) 0.032(2) 0.033(2) C38 0.0339(17) 0.050(2) 0.0358(17) -0.0028(15) 0.0134(14) 0.0139(15) C39 0.0226(12) 0.0206(13) 0.0211(12) 0.0033(10) 0.0094(10) -0.0006(10) C40 0.0271(13) 0.0259(14) 0.0234(13) 0.0053(11) 0.0111(11) 0.0039(11) C41 0.0357(16) 0.0235(14) 0.0350(16) 0.0050(12) 0.0208(13) 0.0053(12) C42 0.0426(17) 0.0216(14) 0.0342(16) -0.0041(12) 0.0218(14) -0.0016(12) C43 0.0339(15) 0.0254(14) 0.0262(14) -0.0042(11) 0.0125(12) -0.0079(12) C44 0.0238(13) 0.0217(13) 0.0234(13) -0.0003(10) 0.0088(10) -0.0037(10) C45 0.0417(18) 0.0398(18) 0.0295(16) -0.0100(14) 0.0077(13) -0.0115(15) C46 0.0453(19) 0.0356(18) 0.047(2) 0.0092(15) 0.0277(16) 0.0134(15) C47 0.0222(12) 0.0223(13) 0.0216(12) 0.0050(10) 0.0024(10) 0.0004(10) C48 0.0205(13) 0.0381(17) 0.0272(14) 0.0093(12) 0.0027(11) -0.0031(12) C49 0.0265(15) 0.063(2) 0.0349(17) 0.0173(17) -0.0030(13) -0.0150(16) C50 0.043(2) 0.054(2) 0.0396(19) 0.0132(17) -0.0110(15) -0.0273(18) C51 0.047(2) 0.0308(17) 0.0361(17) 0.0066(14) -0.0092(15) -0.0116(15) C52 0.0325(15) 0.0232(14) 0.0280(14) 0.0019(11) -0.0002(12) -0.0019(12) C53 0.0281(17) 0.125(4) 0.037(2) 0.016(2) 0.0025(15) -0.035(2) C54 0.074(3) 0.036(2) 0.049(2) -0.0053(17) -0.021(2) -0.009(2) C55 0.0214(12) 0.0197(12) 0.0201(12) 0.0002(9) 0.0066(10) 0.0024(10) C56 0.0206(12) 0.0222(13) 0.0210(12) -0.0001(10) 0.0053(10) 0.0019(10) C57 0.0256(13) 0.0272(14) 0.0197(12) 0.0021(10) 0.0042(10) 0.0048(11) C58 0.0311(14) 0.0281(14) 0.0189(12) 0.0029(11) 0.0085(11) 0.0005(11) C59 0.0288(14) 0.0261(14) 0.0207(13) -0.0009(11) 0.0083(11) -0.0023(11) C60 0.0238(12) 0.0247(13) 0.0176(12) 0.0003(10) 0.0049(10) 0.0002(10) C61 0.0293(14) 0.0343(16) 0.0226(13) 0.0027(12) 0.0033(11) 0.0023(12) C62 0.0360(16) 0.0343(16) 0.0234(14) 0.0000(12) 0.0084(12) -0.0086(13) C63 0.0185(11) 0.0209(12) 0.0209(12) -0.0008(10) 0.0043(9) -0.0005(9) C64 0.0226(12) 0.0302(14) 0.0182(12) -0.0005(10) 0.0050(10) 0.0002(11) C65 0.0209(13) 0.0383(16) 0.0230(13) -0.0047(12) 0.0066(10) 0.0028(11) C66 0.0222(13) 0.0312(15) 0.0268(14) -0.0017(12) 0.0028(11) 0.0070(11) C67 0.0253(13) 0.0240(13) 0.0230(13) -0.0006(10) 0.0035(10) 0.0009(11) C68 0.0215(12) 0.0216(13) 0.0204(12) -0.0005(10) 0.0066(10) -0.0008(10) C69 0.0256(15) 0.062(2) 0.0282(15) -0.0040(15) 0.0092(12) 0.0118(15) C70 0.0302(15) 0.0408(18) 0.0271(15) 0.0094(13) 0.0068(12) 0.0093(13) Ni1 0.01904(18) 0.02264(19) 0.02020(18) -0.00019(13) 0.00634(13) 0.00231(12) O1 0.0175(9) 0.0274(10) 0.0248(9) -0.0019(8) 0.0062(7) 0.0030(7) O2 0.0237(10) 0.0355(12) 0.0301(11) 0.0003(9) 0.0088(8) 0.0050(9) O3 0.0267(11) 0.0429(14) 0.0411(13) 0.0085(10) 0.0125(10) -0.0019(9) O4 0.0224(10) 0.0373(12) 0.0348(11) -0.0012(9) -0.0002(8) -0.0011(9) O5 0.0247(11) 0.0369(13) 0.0511(14) -0.0029(11) 0.0089(10) -0.0023(9) O6 0.0283(11) 0.0368(13) 0.0538(15) 0.0111(11) 0.0204(10) -0.0024(9) O7 0.0385(12) 0.0203(10) 0.0445(13) -0.0042(9) 0.0072(10) 0.0001(9) F1 0.0483(13) 0.0676(16) 0.0526(14) 0.0135(12) 0.0184(11) 0.0316(12) F2 0.0501(14) 0.0689(17) 0.0874(19) 0.0323(15) 0.0483(14) 0.0199(12) F3 0.0683(17) 0.0358(12) 0.096(2) -0.0066(13) 0.0321(15) 0.0196(12) F4 0.0683(18) 0.134(3) 0.0392(13) -0.0432(17) 0.0063(12) 0.0110(18) F5 0.0577(15) 0.084(2) 0.0570(15) 0.0093(14) -0.0066(12) -0.0413(15) F6 0.086(2) 0.0494(14) 0.0410(13) 0.0002(11) -0.0206(13) -0.0079(13) F7 0.0465(9) 0.175(2) 0.0819(13) 0.0238(14) 0.0233(9) -0.0192(12) F8 0.0465(9) 0.175(2) 0.0819(13) 0.0238(14) 0.0233(9) -0.0192(12) F9 0.0465(9) 0.175(2) 0.0819(13) 0.0238(14) 0.0233(9) -0.0192(12) F10 0.073(2) 0.0642(15) 0.0710(14) -0.0294(12) 0.0040(13) -0.0025(13) F11 0.073(2) 0.0642(15) 0.0710(14) -0.0294(12) 0.0040(13) -0.0025(13) F12 0.073(2) 0.0642(15) 0.0710(14) -0.0294(12) 0.0040(13) -0.0025(13) F10B 0.073(2) 0.0642(15) 0.0710(14) -0.0294(12) 0.0040(13) -0.0025(13) F11B 0.073(2) 0.0642(15) 0.0710(14) -0.0294(12) 0.0040(13) -0.0025(13) F12B 0.073(2) 0.0642(15) 0.0710(14) -0.0294(12) 0.0040(13) -0.0025(13) F13 0.0395(11) 0.0540(14) 0.0282(8) 0.0003(8) 0.0021(7) 0.0060(9) F14 0.0395(11) 0.0540(14) 0.0282(8) 0.0003(8) 0.0021(7) 0.0060(9) F15 0.0395(11) 0.0540(14) 0.0282(8) 0.0003(8) 0.0021(7) 0.0060(9) F13B 0.0395(11) 0.0540(14) 0.0282(8) 0.0003(8) 0.0021(7) 0.0060(9) F14B 0.0395(11) 0.0540(14) 0.0282(8) 0.0003(8) 0.0021(7) 0.0060(9) F15B 0.0395(11) 0.0540(14) 0.0282(8) 0.0003(8) 0.0021(7) 0.0060(9) F16 0.0490(12) 0.0371(11) 0.0303(9) 0.0024(8) 0.0081(8) -0.0174(9) F17 0.0336(10) 0.0516(13) 0.0608(14) -0.0063(11) 0.0234(10) -0.0055(9) F18 0.0408(11) 0.0627(14) 0.0264(9) 0.0006(9) 0.0025(8) -0.0222(10) F19 0.0399(10) 0.0842(18) 0.0454(13) -0.0040(11) 0.0223(9) 0.0074(10) F20 0.0399(10) 0.0842(18) 0.0454(13) -0.0040(11) 0.0223(9) 0.0074(10) F21 0.0399(10) 0.0842(18) 0.0454(13) -0.0040(11) 0.0223(9) 0.0074(10) F19B 0.0399(10) 0.0842(18) 0.0454(13) -0.0040(11) 0.0223(9) 0.0074(10) F20B 0.0399(10) 0.0842(18) 0.0454(13) -0.0040(11) 0.0223(9) 0.0074(10) F21B 0.0399(10) 0.0842(18) 0.0454(13) -0.0040(11) 0.0223(9) 0.0074(10) F22 0.0752(18) 0.102(2) 0.0570(15) 0.0466(16) 0.0291(14) 0.0581(17) F23 0.106(2) 0.0703(18) 0.0272(11) 0.0015(11) 0.0042(13) -0.0179(16) F24 0.0451(12) 0.0851(19) 0.0468(13) 0.0345(13) 0.0033(10) -0.0150(12) Na1 0.0169(5) 0.0348(6) 0.0294(6) -0.0012(5) 0.0057(4) 0.0005(4) P1 0.0161(3) 0.0184(3) 0.0222(3) 0.0011(2) 0.0065(2) 0.0006(2) P2 0.0326(4) 0.0394(5) 0.0258(4) -0.0038(3) 0.0095(3) 0.0111(3) B1 0.0193(13) 0.0212(14) 0.0192(13) 0.0015(11) 0.0066(10) 0.0009(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' B B 0.0013 0.0007 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 C1 C6 120.5(2) O1 C1 C2 121.9(2) C6 C1 C2 117.6(2) C3 C2 C1 119.6(3) C3 C2 C8 121.1(3) C1 C2 C8 119.3(3) C2 C3 C4 122.8(3) C5 C4 C3 117.4(3) C5 C4 C7 121.9(3) C3 C4 C7 120.7(3) C4 C5 C6 120.6(3) C5 C6 C1 121.6(3) C5 C6 P1 127.9(2) C1 C6 P1 110.4(2) O2 C8 C2 112.6(2) O2 C9 C10 108.4(3) O3 C10 C9 107.5(3) O3 C11 C12 107.6(3) O5 C12 C11 112.5(3) O5 C13 C14 108.8(3) O4 C14 C13 108.6(3) C17 C16 C21 119.2(3) C17 C16 P1 122.4(2) C21 C16 P1 118.3(2) C16 C17 C18 120.8(3) C19 C18 C17 118.9(3) C18 C19 C20 121.4(3) C19 C20 C21 119.6(3) O6 C21 C20 125.3(3) O6 C21 C16 114.7(3) C20 C21 C16 120.1(3) C24 C23 C28 118.6(3) C24 C23 P1 121.2(2) C28 C23 P1 119.9(2) C23 C24 C25 120.9(3) C26 C25 C24 119.3(4) C25 C26 C27 121.4(3) C26 C27 C28 119.5(3) O7 C28 C27 124.5(3) O7 C28 C23 115.2(3) C27 C28 C23 120.3(3) C31 C30 C35 116.8(3) C31 C30 Ni1 124.2(2) C35 C30 Ni1 117.9(2) C31 C30 Na1 79.02(17) C35 C30 Na1 93.23(18) Ni1 C30 Na1 88.08(10) C30 C31 C32 121.4(3) C30 C31 Na1 74.24(17) C32 C31 Na1 97.5(2) C33 C32 C31 120.4(3) C32 C33 C34 119.6(3) C35 C34 C33 119.7(3) C34 C35 C30 122.1(3) C44 C39 C40 115.5(3) C44 C39 B1 125.5(2) C40 C39 B1 119.0(2) C41 C40 C39 122.2(3) C42 C41 C40 121.1(3) C42 C41 C46 118.2(3) C40 C41 C46 120.6(3) C43 C42 C41 118.3(3) C42 C43 C44 120.7(3) C42 C43 C45 120.3(3) C44 C43 C45 119.0(3) C39 C44 C43 122.0(3) F4 C45 F5 106.9(3) F4 C45 F6 106.0(3) F5 C45 F6 104.1(3) F4 C45 C43 113.5(3) F5 C45 C43 112.4(3) F6 C45 C43 113.2(3) F2 C46 F3 105.6(3) F2 C46 F1 107.1(3) F3 C46 F1 106.0(3) F2 C46 C41 111.4(3) F3 C46 C41 112.5(3) F1 C46 C41 113.6(3) C48 C47 C52 115.9(3) C48 C47 B1 124.5(3) C52 C47 B1 119.6(2) C49 C48 C47 122.2(3) C50 C49 C48 120.4(3) C50 C49 C53 119.4(3) C48 C49 C53 120.2(4) C51 C50 C49 118.5(3) C50 C51 C52 121.3(4) C50 C51 C54 120.9(3) C52 C51 C54 117.8(4) C51 C52 C47 121.6(3) F8 C53 F7 108.0(5) F8 C53 F9 104.1(3) F7 C53 F9 104.2(4) F8 C53 C49 113.6(3) F7 C53 C49 113.6(3) F9 C53 C49 112.4(5) F10B C54 F12B 120.8(7) F12 C54 F10 104.4(4) F12 C54 F11 106.1(4) F10 C54 F11 97.6(5) F10B C54 F11B 103.5(5) F12B C54 F11B 102.5(6) F10B C54 C51 109.4(4) F12B C54 C51 114.1(6) F12 C54 C51 120.4(5) F10 C54 C51 110.8(4) F11 C54 C51 114.6(3) F11B C54 C51 104.2(5) C56 C55 C60 115.9(2) C56 C55 B1 125.6(2) C60 C55 B1 118.6(2) C55 C56 C57 122.0(3) C58 C57 C56 120.9(3) C58 C57 C61 119.9(3) C56 C57 C61 119.2(3) C57 C58 C59 118.1(3) C60 C59 C58 120.7(3) C60 C59 C62 120.1(3) C58 C59 C62 119.2(3) C59 C60 C55 122.4(3) F13B C61 F14B 107.6(4) F15 C61 F14 109.3(3) F13B C61 F15B 105.3(4) F14B C61 F15B 105.9(4) F15 C61 F13 105.2(3) F14 C61 F13 104.5(3) F15 C61 C57 113.8(3) F13B C61 C57 114.3(3) F14B C61 C57 112.5(3) F14 C61 C57 112.3(3) F15B C61 C57 110.6(3) F13 C61 C57 111.2(3) F16 C62 F17 107.2(3) F16 C62 F18 106.2(3) F17 C62 F18 105.1(3) F16 C62 C59 112.9(3) F17 C62 C59 112.6(3) F18 C62 C59 112.2(2) C68 C63 C64 115.3(2) C68 C63 B1 120.6(2) C64 C63 B1 124.0(2) C65 C64 C63 122.1(3) C66 C65 C64 121.4(3) C66 C65 C69 117.9(3) C64 C65 C69 120.7(3) C65 C66 C67 117.6(3) C66 C67 C68 121.1(3) C66 C67 C70 120.1(3) C68 C67 C70 118.7(3) C67 C68 C63 122.4(2) F21 C69 F19 113.7(4) F20B C69 F21B 112.5(5) F20B C69 F19B 106.2(4) F21B C69 F19B 99.3(5) F21 C69 F20 100.5(4) F19 C69 F20 100.4(3) F20B C69 C65 116.9(4) F21 C69 C65 115.9(4) F19 C69 C65 114.5(3) F21B C69 C65 110.4(4) F19B C69 C65 110.1(3) F20 C69 C65 109.4(3) F22 C70 F24 111.1(3) F22 C70 F23 103.6(3) F24 C70 F23 102.3(3) F22 C70 C67 114.3(3) F24 C70 C67 114.2(3) F23 C70 C67 110.0(3) C30 Ni1 O1 85.95(10) C30 Ni1 P2 88.11(9) O1 Ni1 P2 169.94(7) C30 Ni1 P1 166.68(9) O1 Ni1 P1 83.12(6) P2 Ni1 P1 103.75(3) C30 Ni1 Na1 58.61(8) O1 Ni1 Na1 38.59(6) P2 Ni1 Na1 141.26(3) P1 Ni1 Na1 108.14(3) C1 O1 Ni1 118.59(16) C1 O1 Na1 127.21(16) Ni1 O1 Na1 109.92(9) C9 O2 C8 113.7(2) C9 O2 Na1 113.8(2) C8 O2 Na1 111.55(17) C10 O3 C11 113.6(3) C10 O3 Na1 112.2(2) C11 O3 Na1 118.6(2) C15 O4 C14 113.1(3) C15 O4 Na1 121.96(19) C14 O4 Na1 115.3(2) C12 O5 C13 114.3(3) C12 O5 Na1 106.9(2) C13 O5 Na1 111.7(2) C21 O6 C22 118.5(3) C28 O7 C29 117.1(3) O1 Na1 O4 145.80(10) O1 Na1 O2 79.68(8) O4 Na1 O2 88.24(8) O1 Na1 O3 105.67(9) O4 Na1 O3 99.49(9) O2 Na1 O3 69.14(9) O1 Na1 O5 142.73(9) O4 Na1 O5 68.71(9) O2 Na1 O5 126.20(9) O3 Na1 O5 67.96(9) O1 Na1 C30 57.91(8) O4 Na1 C30 111.80(9) O2 Na1 C30 130.30(9) O3 Na1 C30 142.15(10) O5 Na1 C30 103.50(9) O1 Na1 C31 82.42(8) O4 Na1 C31 98.09(9) O2 Na1 C31 156.29(10) O3 Na1 C31 131.34(10) O5 Na1 C31 77.10(9) C30 Na1 C31 26.74(9) O1 Na1 Ni1 31.48(5) O4 Na1 Ni1 144.59(7) O2 Na1 Ni1 111.12(6) O3 Na1 Ni1 114.87(7) O5 Na1 Ni1 115.47(7) C30 Na1 Ni1 33.32(6) C31 Na1 Ni1 52.92(6) C6 P1 C16 105.11(13) C6 P1 C23 103.75(13) C16 P1 C23 105.19(13) C6 P1 Ni1 98.27(9) C16 P1 Ni1 136.71(10) C23 P1 Ni1 103.86(9) C36 P2 C38 102.1(2) C36 P2 C37 104.0(3) C38 P2 C37 100.71(19) C36 P2 Ni1 117.46(16) C38 P2 Ni1 118.97(12) C37 P2 Ni1 111.31(16) C55 B1 C47 111.3(2) C55 B1 C39 107.0(2) C47 B1 C39 110.5(2) C55 B1 C63 109.8(2) C47 B1 C63 106.1(2) C39 B1 C63 112.3(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 O1 1.332(3) C1 C6 1.407(4) C1 C2 1.412(4) C2 C3 1.388(4) C2 C8 1.505(4) C3 C4 1.399(4) C4 C5 1.396(4) C4 C7 1.513(4) C5 C6 1.398(4) C6 P1 1.800(3) C8 O2 1.441(4) C9 O2 1.430(4) C9 C10 1.495(5) C10 O3 1.421(5) C11 O3 1.430(4) C11 C12 1.506(7) C12 O5 1.422(5) C13 O5 1.431(4) C13 C14 1.484(5) C14 O4 1.427(4) C15 O4 1.426(4) C16 C17 1.394(4) C16 C21 1.404(4) C16 P1 1.814(3) C17 C18 1.399(4) C18 C19 1.384(6) C19 C20 1.386(6) C20 C21 1.394(4) C21 O6 1.361(4) C22 O6 1.429(4) C23 C24 1.395(4) C23 C28 1.402(4) C23 P1 1.827(3) C24 C25 1.396(4) C25 C26 1.374(6) C26 C27 1.379(6) C27 C28 1.400(4) C28 O7 1.367(4) C29 O7 1.428(4) C30 C31 1.392(4) C30 C35 1.409(5) C30 Ni1 1.916(3) C30 Na1 2.977(3) C31 C32 1.408(5) C31 Na1 3.037(3) C32 C33 1.375(6) C33 C34 1.395(5) C34 C35 1.388(4) C36 P2 1.818(4) C37 P2 1.826(4) C38 P2 1.822(3) C39 C44 1.401(4) C39 C40 1.413(4) C39 B1 1.646(4) C40 C41 1.385(4) C41 C42 1.384(5) C41 C46 1.502(4) C42 C43 1.384(5) C43 C44 1.404(4) C43 C45 1.499(5) C45 F4 1.324(4) C45 F5 1.330(4) C45 F6 1.336(5) C46 F2 1.330(4) C46 F3 1.332(5) C46 F1 1.337(5) C47 C48 1.401(4) C47 C52 1.406(4) C47 B1 1.644(4) C48 C49 1.393(4) C49 C50 1.392(6) C49 C53 1.489(6) C50 C51 1.370(6) C51 C52 1.397(4) C51 C54 1.493(6) C53 F8 1.310(6) C53 F7 1.317(6) C53 F9 1.350(7) C54 F10B 1.263(8) C54 F12B 1.272(9) C54 F12 1.292(6) C54 F10 1.387(7) C54 F11 1.419(7) C54 F11B 1.458(8) C55 C56 1.400(4) C55 C60 1.407(4) C55 B1 1.641(4) C56 C57 1.402(4) C57 C58 1.383(4) C57 C61 1.508(4) C58 C59 1.397(4) C59 C60 1.389(4) C59 C62 1.499(4) C61 F15 1.327(6) C61 F13B 1.332(7) C61 F14B 1.337(6) C61 F14 1.339(6) C61 F15B 1.374(6) C61 F13 1.374(6) C62 F16 1.341(4) C62 F17 1.343(4) C62 F18 1.349(4) C63 C68 1.405(4) C63 C64 1.405(4) C63 B1 1.647(4) C64 C65 1.392(4) C65 C66 1.385(4) C65 C69 1.503(4) C66 C67 1.387(4) C67 C68 1.391(4) C67 C70 1.494(4) C69 F20B 1.244(7) C69 F21 1.280(6) C69 F19 1.309(5) C69 F21B 1.358(8) C69 F19B 1.432(7) C69 F20 1.438(6) C70 F22 1.308(4) C70 F24 1.313(4) C70 F23 1.360(4) Ni1 O1 1.9364(19) Ni1 P2 2.1346(8) Ni1 P1 2.2207(8) Ni1 Na1 3.4859(12) O1 Na1 2.313(2) O2 Na1 2.388(3) O3 Na1 2.437(3) O4 Na1 2.387(2) O5 Na1 2.465(3)