#------------------------------------------------------------------------------ #$Date: 2020-11-06 14:12:09 +0200 (Fri, 06 Nov 2020) $ #$Revision: 258830 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705317.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_7705317 loop_ _publ_author_name 'Tretiakov, Serhii' 'Damen, Johannes A. M.' 'Lutz, Martin' 'Moret, Marc-Etienne' _publ_section_title ; A dianionic C3-symmetric scorpionate: synthesis and coordination chemistry. ; _journal_issue 39 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13549 _journal_page_last 13556 _journal_paper_doi 10.1039/d0dt02601h _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C14 H27 K N O6, C34 H39 Cu N3 O3 P2, 0.5(C6 H6), C2 H3 N' _chemical_formula_sum 'C53 H72 Cu K N5 O9 P2' _chemical_formula_weight 1087.73 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2020-06-19 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.867(1) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.8978(5) _cell_length_b 13.9828(3) _cell_length_c 33.8978(7) _cell_measurement_reflns_used 51999 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.55 _cell_measurement_theta_min 1.56 _cell_volume 11027.2(4) _computing_cell_refinement Peakref _computing_data_collection Apex3 _computing_data_reduction 'Eval15, SADABS-2016/2' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution SHELXT _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_number 108621 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.493 _diffrn_reflns_theta_min 1.592 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.310 _exptl_crystal_description needle _exptl_crystal_F_000 4600 _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.049 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 679 _refine_ls_number_reflns 12649 _refine_ls_number_restraints 111 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0440 _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^)+(0.0669P)^2^+18.0984P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1222 _refine_ls_wR_factor_ref 0.1358 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9315 _reflns_number_total 12649 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02601h2.cif _cod_data_source_block l0981a _cod_depositor_comments 'Adding full bibliography for 7705312--7705317.cif.' _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 7705317 _shelx_shelxl_version_number 2018/1 _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_res_file ; TITL l0981a l0981a.res created by SHELXL-2018/1 at 13:51:25 on 13-Apr-2018 CELL 0.71073 24.89776 13.98283 33.89776 90.0 110.867 90.0 ZERR 8 0.00049 0.00026 0.00066 0.0 0.001 0.0 LATT 2 SYMM 0.5-x, y, -z SFAC C H Cu K N O P UNIT 424 576 8 8 40 72 16 TEMP -123 L.S. 15 FMAP 2 PLAN -20 ACTA BOND $H CONF EQIV $1 0.5-x, y, -z DFIX 1.40 0.01 C13 C23 C23 C33 C33 C43 C43 C33_$1 C13 C23_$1 SADI 0.02 C13 C33 C23 C43 C33 C33_$1 C23 C23_$1 FLAT 0.01 C13 > C43 DFIX 1.13 0.01 N14A C14A N14B C14B DFIX 1.44 0.01 C14A C24A C14B C24B DFIX 2.57 0.02 N14A C24A N14B C24B RIGU C13 > C24B ISOR 0.01 C13 > C24B WGHT 0.066900 18.098400 FVAR 0.07767 0.70703 CU1 3 0.528663 0.242015 0.400419 11.00000 0.02661 0.02623 = 0.01562 0.00049 0.00695 -0.00021 P11 7 0.503836 0.248005 0.303873 11.00000 0.02964 0.03179 = 0.01540 0.00137 0.00573 -0.00323 P21 7 0.544263 0.237941 0.466097 11.00000 0.03012 0.02271 = 0.01749 0.00056 0.00867 0.00057 O11 6 0.595679 0.302989 0.497299 11.00000 0.03858 0.03089 = 0.02377 0.00110 0.00624 -0.00423 O21 6 0.489539 0.265949 0.477960 11.00000 0.03629 0.03703 = 0.02131 -0.00039 0.01296 0.00261 O31 6 0.561267 0.139550 0.492140 11.00000 0.04799 0.02649 = 0.02851 0.00400 0.01773 0.00630 N11 5 0.593761 0.242212 0.375567 11.00000 0.02575 0.02861 = 0.01784 0.00094 0.00713 -0.00082 N21 5 0.482427 0.351373 0.362423 11.00000 0.02542 0.02668 = 0.02260 0.00181 0.00668 -0.00124 N31 5 0.480706 0.138443 0.359719 11.00000 0.02714 0.02642 = 0.02049 0.00041 0.00852 -0.00244 C11 1 0.579166 0.246066 0.332374 11.00000 0.03189 0.02619 = 0.01779 -0.00007 0.00841 -0.00351 C21 1 0.626430 0.245189 0.319535 11.00000 0.03496 0.02367 = 0.02588 0.00028 0.01464 -0.00266 C31 1 0.674575 0.240665 0.357700 11.00000 0.03305 0.01525 = 0.03025 -0.00127 0.01504 -0.00198 C41 1 0.734653 0.238280 0.367292 11.00000 0.03410 0.02368 = 0.04440 -0.00315 0.02020 -0.00262 AFIX 43 H41 2 0.750014 0.240413 0.345358 11.00000 -1.20000 AFIX 0 C51 1 0.770413 0.232848 0.408683 11.00000 0.02575 0.03439 = 0.04999 -0.00160 0.01241 0.00021 AFIX 43 H51 2 0.810845 0.230942 0.415416 11.00000 -1.20000 AFIX 0 C61 1 0.747952 0.230057 0.441355 11.00000 0.02989 0.03960 = 0.03628 -0.00055 0.00181 0.00026 AFIX 43 H61 2 0.773631 0.225875 0.469796 11.00000 -1.20000 AFIX 0 C71 1 0.689866 0.233228 0.433130 11.00000 0.03102 0.03403 = 0.02657 -0.00055 0.00780 -0.00155 AFIX 43 H71 2 0.675315 0.231794 0.455503 11.00000 -1.20000 AFIX 0 C81 1 0.652394 0.238642 0.390891 11.00000 0.02605 0.01957 = 0.02684 -0.00091 0.00954 -0.00189 C91 1 0.629716 0.248618 0.276080 11.00000 0.05355 0.05889 = 0.02995 0.00185 0.02433 -0.00447 AFIX 137 H91A 2 0.611039 0.191800 0.260139 11.00000 -1.50000 H91B 2 0.670089 0.250101 0.278418 11.00000 -1.50000 H91C 2 0.610159 0.306185 0.261384 11.00000 -1.50000 AFIX 0 C101 1 0.473801 0.349946 0.319823 11.00000 0.02697 0.03046 = 0.02326 0.00349 0.00461 -0.00286 C111 1 0.441609 0.427725 0.297766 11.00000 0.02604 0.03286 = 0.03001 0.01033 0.00356 -0.00287 C121 1 0.428755 0.480940 0.328990 11.00000 0.02105 0.02723 = 0.03948 0.00731 0.00509 -0.00527 C131 1 0.398134 0.566306 0.328320 11.00000 0.02454 0.02894 = 0.05847 0.01335 0.00998 0.00020 AFIX 43 H131 2 0.380085 0.599757 0.302584 11.00000 -1.20000 AFIX 0 C141 1 0.394819 0.600239 0.365341 11.00000 0.02781 0.02530 = 0.07314 0.00488 0.02039 -0.00017 AFIX 43 H141 2 0.374305 0.657697 0.365017 11.00000 -1.20000 AFIX 0 C151 1 0.421218 0.551648 0.403886 11.00000 0.02740 0.02921 = 0.05612 -0.00723 0.02042 -0.00782 AFIX 43 H151 2 0.418369 0.577137 0.429045 11.00000 -1.20000 AFIX 0 C161 1 0.451164 0.467554 0.405658 11.00000 0.02306 0.02908 = 0.03866 -0.00151 0.01136 -0.00521 AFIX 43 H161 2 0.468655 0.434876 0.431672 11.00000 -1.20000 AFIX 0 C171 1 0.455141 0.431580 0.368195 11.00000 0.01979 0.02399 = 0.03407 0.00341 0.00744 -0.00449 C181 1 0.422643 0.454459 0.251620 11.00000 0.04210 0.04787 = 0.03592 0.01663 0.00128 0.00001 AFIX 137 H18A 2 0.456415 0.460327 0.243347 11.00000 -1.50000 H18B 2 0.402125 0.515641 0.247030 11.00000 -1.50000 H18C 2 0.397087 0.404748 0.234556 11.00000 -1.50000 AFIX 0 C191 1 0.473107 0.143540 0.317428 11.00000 0.02646 0.03112 = 0.01847 -0.00105 0.00638 -0.00109 C201 1 0.440918 0.067712 0.293690 11.00000 0.02559 0.02985 = 0.02371 -0.00406 0.00509 0.00101 C211 1 0.426846 0.011721 0.323558 11.00000 0.02060 0.02740 = 0.02664 -0.00422 0.00677 0.00326 C221 1 0.395184 -0.073237 0.321050 11.00000 0.03016 0.02751 = 0.03622 -0.00757 0.00953 -0.00023 AFIX 43 H221 2 0.377599 -0.104634 0.294723 11.00000 -1.20000 AFIX 0 C231 1 0.390104 -0.110015 0.357198 11.00000 0.03185 0.02311 = 0.05235 0.00092 0.01694 -0.00083 AFIX 43 H231 2 0.368381 -0.166699 0.355566 11.00000 -1.20000 AFIX 0 C241 1 0.416563 -0.065082 0.396628 11.00000 0.03053 0.02681 = 0.03971 0.00567 0.01775 0.00601 AFIX 43 H241 2 0.413112 -0.092902 0.421183 11.00000 -1.20000 AFIX 0 C251 1 0.447231 0.018145 0.400204 11.00000 0.02352 0.02726 = 0.02727 0.00317 0.01009 0.00532 AFIX 43 H251 2 0.464549 0.048326 0.426852 11.00000 -1.20000 AFIX 0 C261 1 0.452496 0.057923 0.363493 11.00000 0.01901 0.02252 = 0.02535 -0.00067 0.00599 0.00377 C271 1 0.423195 0.044547 0.247336 11.00000 0.03906 0.04294 = 0.02376 -0.01058 0.00656 -0.00447 AFIX 137 H27A 2 0.396370 0.093401 0.230792 11.00000 -1.50000 H27B 2 0.404426 -0.018180 0.241830 11.00000 -1.50000 H27C 2 0.457274 0.043368 0.239266 11.00000 -1.50000 AFIX 0 C281 1 0.489356 0.251754 0.248275 11.00000 0.04245 0.05542 = 0.01668 0.00198 0.00581 -0.00744 AFIX 137 H28A 2 0.447713 0.250970 0.233035 11.00000 -1.50000 H28B 2 0.506773 0.195987 0.240035 11.00000 -1.50000 H28C 2 0.505650 0.310360 0.241297 11.00000 -1.50000 AFIX 0 C291 1 0.601144 0.399054 0.483520 11.00000 0.04792 0.02613 = 0.04341 0.00265 0.00526 -0.00751 AFIX 23 H29A 2 0.571088 0.440400 0.487343 11.00000 -1.20000 H29B 2 0.595870 0.398661 0.453161 11.00000 -1.20000 AFIX 0 C301 1 0.658855 0.437347 0.508499 11.00000 0.04480 0.03987 = 0.06468 -0.00433 0.01525 -0.01138 AFIX 137 H30A 2 0.665400 0.431627 0.538673 11.00000 -1.50000 H30B 2 0.661010 0.504795 0.501347 11.00000 -1.50000 H30C 2 0.688274 0.400909 0.501974 11.00000 -1.50000 AFIX 0 C311 1 0.489634 0.259462 0.520700 11.00000 0.04146 0.04413 = 0.02221 -0.00407 0.01596 -0.00508 AFIX 23 H31A 2 0.523715 0.292557 0.540548 11.00000 -1.20000 H31B 2 0.490870 0.191654 0.529382 11.00000 -1.20000 AFIX 0 C321 1 0.436195 0.305456 0.521127 11.00000 0.07512 0.10188 = 0.04286 0.01087 0.03720 0.03625 AFIX 137 H32A 2 0.435574 0.372586 0.512668 11.00000 -1.50000 H32B 2 0.434897 0.301996 0.549649 11.00000 -1.50000 H32C 2 0.402790 0.272190 0.501348 11.00000 -1.50000 AFIX 0 C331 1 0.601954 0.076955 0.484416 11.00000 0.04906 0.03356 = 0.04776 0.00804 0.02431 0.01228 AFIX 23 H33A 2 0.641543 0.098307 0.500867 11.00000 -1.20000 H33B 2 0.596806 0.078307 0.454083 11.00000 -1.20000 AFIX 0 C341 1 0.592964 -0.021669 0.497032 11.00000 0.06848 0.03290 = 0.04827 0.00643 0.02391 0.01175 AFIX 137 H34A 2 0.597365 -0.022279 0.526934 11.00000 -1.50000 H34B 2 0.621396 -0.064597 0.492575 11.00000 -1.50000 H34C 2 0.554196 -0.043250 0.479916 11.00000 -1.50000 AFIX 0 K1 4 0.321762 0.241912 0.134870 11.00000 0.02163 0.01981 = 0.04563 -0.00170 0.01662 -0.00146 O12 6 0.427819 0.227802 0.122774 11.00000 0.02053 0.06086 = 0.03197 0.00012 0.01154 0.00165 O22 6 0.386414 0.404334 0.136219 11.00000 0.04443 0.03029 = 0.05153 0.00874 0.01204 -0.01388 O32 6 0.267832 0.418159 0.115229 11.00000 0.04407 0.02426 = 0.05811 0.00257 0.00931 0.00585 O42 6 0.204903 0.255922 0.118329 11.00000 0.02013 0.04290 = 0.04366 0.00677 0.01014 0.00465 O52 6 0.254752 0.076851 0.116040 11.00000 0.03448 0.02724 = 0.04937 0.00242 0.01071 -0.00668 O62 6 0.372071 0.065117 0.134080 11.00000 0.03922 0.02996 = 0.04289 -0.00484 0.01641 0.01051 N12 5 0.328799 0.246274 0.222105 11.00000 0.04736 0.08742 = 0.04537 0.00121 0.01516 0.00353 C12 1 0.464916 0.309383 0.135377 11.00000 0.02415 0.08744 = 0.03309 0.01041 0.01100 -0.01754 AFIX 23 H12A 2 0.496044 0.304460 0.123712 11.00000 -1.20000 H12B 2 0.482672 0.311623 0.166548 11.00000 -1.20000 AFIX 0 C22 1 0.431268 0.397326 0.119686 11.00000 0.04031 0.07452 = 0.04691 0.01958 0.01063 -0.03072 AFIX 23 H22A 2 0.456715 0.453854 0.128399 11.00000 -1.20000 H22B 2 0.414712 0.396039 0.088455 11.00000 -1.20000 AFIX 0 C32 1 0.356352 0.493369 0.125470 11.00000 0.06463 0.02354 = 0.10182 0.01374 0.00053 -0.01602 AFIX 23 H32D 2 0.344337 0.504364 0.094679 11.00000 -1.20000 H32E 2 0.382049 0.546394 0.140162 11.00000 -1.20000 AFIX 0 C42 1 0.305376 0.491408 0.137950 11.00000 0.06731 0.02290 = 0.09407 -0.00800 0.00384 0.00634 AFIX 23 H42A 2 0.317238 0.479270 0.168651 11.00000 -1.20000 H42B 2 0.285465 0.553936 0.131753 11.00000 -1.20000 AFIX 0 C52 1 0.213249 0.423135 0.119807 11.00000 0.05271 0.04452 = 0.08645 -0.00045 0.02082 0.02747 AFIX 23 H52A 2 0.193776 0.483679 0.107598 11.00000 -1.20000 H52B 2 0.218219 0.421563 0.150105 11.00000 -1.20000 AFIX 0 C62 1 0.177851 0.340282 0.097582 11.00000 0.02850 0.05264 = 0.07238 0.01106 0.01062 0.01794 AFIX 23 H62A 2 0.138590 0.345222 0.098388 11.00000 -1.20000 H62B 2 0.174948 0.339202 0.067688 11.00000 -1.20000 AFIX 0 C72 1 0.171986 0.172464 0.101528 11.00000 0.01905 0.06177 = 0.07169 0.00744 0.00551 -0.01081 AFIX 23 H72A 2 0.166210 0.165680 0.071218 11.00000 -1.20000 H72B 2 0.133829 0.177054 0.104334 11.00000 -1.20000 AFIX 0 C82 1 0.203975 0.088603 0.125532 11.00000 0.03198 0.04961 = 0.08290 0.01752 0.01480 -0.01564 AFIX 23 H82A 2 0.214025 0.099182 0.156203 11.00000 -1.20000 H82B 2 0.179866 0.030424 0.117432 11.00000 -1.20000 AFIX 0 C92 1 0.286986 -0.004220 0.136735 11.00000 0.05573 0.02365 = 0.07207 0.00892 0.01351 -0.00683 AFIX 23 H92A 2 0.262383 -0.061979 0.129886 11.00000 -1.20000 H92B 2 0.301132 0.005273 0.167701 11.00000 -1.20000 AFIX 0 C102 1 0.336469 -0.016816 0.122257 11.00000 0.06662 0.02191 = 0.07721 -0.00629 0.02083 0.00838 AFIX 23 H10A 2 0.358587 -0.074637 0.135368 11.00000 -1.20000 H10B 2 0.322362 -0.024823 0.091211 11.00000 -1.20000 AFIX 0 C112 1 0.419250 0.058764 0.119608 11.00000 0.04427 0.05997 = 0.03548 -0.00386 0.01636 0.02629 AFIX 23 H11A 2 0.404912 0.059846 0.088363 11.00000 -1.20000 H11B 2 0.440129 -0.002087 0.129260 11.00000 -1.20000 AFIX 0 C122 1 0.458483 0.140510 0.136520 11.00000 0.02802 0.07854 = 0.03447 0.00059 0.01393 0.01910 AFIX 23 H12C 2 0.473970 0.138001 0.167755 11.00000 -1.20000 H12D 2 0.491164 0.137061 0.126419 11.00000 -1.20000 AFIX 0 C132 1 0.333312 0.244469 0.256433 11.00000 0.03346 0.05590 = 0.04810 0.00284 0.01722 0.00423 C142 1 0.339296 0.242410 0.300464 11.00000 0.04347 0.07863 = 0.04828 0.00219 0.02681 0.00690 AFIX 137 H14A 2 0.301130 0.243487 0.302705 11.00000 -1.50000 H14B 2 0.361272 0.298372 0.314900 11.00000 -1.50000 H14C 2 0.359542 0.183976 0.313618 11.00000 -1.50000 AFIX 0 C13 1 0.250000 0.156995 0.000000 10.50000 0.08394 0.11202 = 0.18181 0.00000 0.06231 0.00000 AFIX 43 H13 2 0.250000 0.089054 0.000000 10.50000 -1.20000 AFIX 0 C23 1 0.289667 0.204102 0.029887 11.00000 0.14130 0.13454 = 0.09566 0.00943 0.03428 0.01850 AFIX 43 H23 2 0.318495 0.170391 0.051593 11.00000 -1.20000 AFIX 0 C33 1 0.289326 0.304164 0.029651 11.00000 0.16033 0.14543 = 0.10972 -0.04304 0.02074 0.00879 AFIX 43 H33 2 0.318824 0.335221 0.051909 11.00000 -1.20000 AFIX 0 C43 1 0.250000 0.362625 0.000000 10.50000 0.11868 0.19917 = 0.11089 0.00000 0.05397 0.00000 AFIX 43 H43 2 0.250000 0.430565 0.000000 10.50000 -1.20000 AFIX 0 PART 1 N14A 5 0.752883 0.332840 0.254278 21.00000 0.08253 0.16630 = 0.26305 0.03366 0.09716 0.01228 C14A 1 0.751757 0.414306 0.256580 21.00000 0.05275 0.14473 = 0.13488 -0.01966 0.00744 0.00588 C24A 1 0.752942 0.517391 0.249206 21.00000 0.17989 0.15749 = 0.16219 -0.01177 0.04993 0.01114 AFIX 137 H24A 2 0.713717 0.542823 0.239947 21.00000 -1.50000 H24B 2 0.769352 0.529144 0.227318 21.00000 -1.50000 H24C 2 0.776550 0.549162 0.275421 21.00000 -1.50000 AFIX 0 PART 2 N14B 5 0.750864 0.576468 0.253290 -21.00000 0.11219 0.06800 = 0.09949 -0.01285 -0.01688 0.01131 C14B 1 0.752058 0.497952 0.246857 -21.00000 0.02770 0.06339 = 0.04999 0.00134 0.01600 -0.00282 C24B 1 0.755858 0.403763 0.230015 -21.00000 0.06553 0.07572 = 0.09258 -0.01396 0.00097 0.00477 AFIX 137 H24D 2 0.792869 0.397209 0.226161 -21.00000 -1.50000 H24E 2 0.724560 0.395729 0.202763 -21.00000 -1.50000 H24F 2 0.752710 0.354775 0.249754 -21.00000 -1.50000 AFIX 0 HKLF 4 REM l0981a REM R1 = 0.0440 for 9315 Fo > 4sig(Fo) and 0.0658 for all 12649 data REM 679 parameters refined using 111 restraints END WGHT 0.0671 18.0525 REM Highest difference peak 1.049, deepest hole -0.652, 1-sigma level 0.066 Q1 1 0.2500 0.4753 0.0000 10.50000 0.05 1.05 Q2 1 0.2564 0.2610 0.0393 11.00000 0.05 0.95 Q3 1 0.7633 0.2452 0.2657 11.00000 0.05 0.58 Q4 1 0.3126 0.2574 0.1113 11.00000 0.05 0.56 Q5 1 0.5359 0.2444 0.4342 11.00000 0.05 0.51 Q6 1 0.5955 0.1750 0.5002 11.00000 0.05 0.46 Q7 1 0.4418 0.4586 0.3496 11.00000 0.05 0.42 Q8 1 0.4963 0.2449 0.2739 11.00000 0.05 0.41 Q9 1 0.2836 0.3713 0.0259 11.00000 0.05 0.36 Q10 1 0.5423 0.2407 0.3208 11.00000 0.05 0.36 Q11 1 0.4807 0.3462 0.3429 11.00000 0.05 0.35 Q12 1 0.5735 0.2672 0.4808 11.00000 0.05 0.34 Q13 1 0.4400 0.0250 0.3441 11.00000 0.05 0.34 Q14 1 0.2500 0.2293 0.0000 10.50000 0.05 0.33 Q15 1 0.4823 0.1390 0.3364 11.00000 0.05 0.32 Q16 1 0.2597 0.1724 0.0240 11.00000 0.05 0.32 Q17 1 0.6572 0.2543 0.3386 11.00000 0.05 0.31 Q18 1 0.4513 0.4435 0.3864 11.00000 0.05 0.31 Q19 1 0.5837 0.2504 0.3510 11.00000 0.05 0.30 Q20 1 0.4638 0.1047 0.3040 11.00000 0.05 0.30 ; _shelx_res_checksum 55162 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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 Cu1 Cu 0.52866(2) 0.24201(2) 0.40042(2) 0.02298(9) Uani 1 1 d . . . . . P11 P 0.50384(3) 0.24801(4) 0.30387(2) 0.02623(14) Uani 1 1 d . . . . . P21 P 0.54426(3) 0.23794(4) 0.46610(2) 0.02339(13) Uani 1 1 d . . . . . O11 O 0.59568(8) 0.30299(12) 0.49730(5) 0.0324(4) Uani 1 1 d . . . . . O21 O 0.48954(8) 0.26595(12) 0.47796(5) 0.0308(4) Uani 1 1 d . . . . . O31 O 0.56127(8) 0.13955(12) 0.49214(5) 0.0332(4) Uani 1 1 d . . . . . N11 N 0.59376(8) 0.24221(13) 0.37557(6) 0.0242(4) Uani 1 1 d . . . . . N21 N 0.48243(8) 0.35137(14) 0.36242(6) 0.0254(4) Uani 1 1 d . . . . . N31 N 0.48071(8) 0.13844(13) 0.35972(6) 0.0247(4) Uani 1 1 d . . . . . C11 C 0.57917(10) 0.24607(15) 0.33237(7) 0.0254(5) Uani 1 1 d . . . . . C21 C 0.62643(11) 0.24519(15) 0.31953(8) 0.0271(5) Uani 1 1 d . . . . . C31 C 0.67458(10) 0.24066(14) 0.35770(8) 0.0252(5) Uani 1 1 d . . . . . C41 C 0.73465(11) 0.23828(16) 0.36729(9) 0.0324(5) Uani 1 1 d . . . . . H41 H 0.750014 0.240413 0.345358 0.039 Uiso 1 1 calc R U . . . C51 C 0.77041(11) 0.23285(18) 0.40868(9) 0.0370(6) Uani 1 1 d . . . . . H51 H 0.810845 0.230942 0.415416 0.044 Uiso 1 1 calc R U . . . C61 C 0.74795(11) 0.23006(19) 0.44136(9) 0.0380(6) Uani 1 1 d . . . . . H61 H 0.773631 0.225875 0.469796 0.046 Uiso 1 1 calc R U . . . C71 C 0.68987(11) 0.23323(17) 0.43313(8) 0.0312(5) Uani 1 1 d . . . . . H71 H 0.675315 0.231794 0.455503 0.037 Uiso 1 1 calc R U . . . C81 C 0.65239(10) 0.23864(15) 0.39089(7) 0.0241(4) Uani 1 1 d . . . . . C91 C 0.62972(14) 0.2486(2) 0.27608(9) 0.0449(7) Uani 1 1 d . . . . . H91A H 0.611039 0.191800 0.260139 0.067 Uiso 1 1 calc R U . . . H91B H 0.670089 0.250101 0.278418 0.067 Uiso 1 1 calc R U . . . H91C H 0.610159 0.306185 0.261384 0.067 Uiso 1 1 calc R U . . . C101 C 0.47380(10) 0.34995(17) 0.31982(7) 0.0281(5) Uani 1 1 d . . . . . C111 C 0.44161(10) 0.42773(18) 0.29777(8) 0.0314(5) Uani 1 1 d . . . . . C121 C 0.42876(10) 0.48094(17) 0.32899(8) 0.0308(5) Uani 1 1 d . . . . . C131 C 0.39813(11) 0.56631(18) 0.32832(10) 0.0386(6) Uani 1 1 d . . . . . H131 H 0.380085 0.599757 0.302584 0.046 Uiso 1 1 calc R U . . . C141 C 0.39482(11) 0.60024(18) 0.36534(10) 0.0414(7) Uani 1 1 d . . . . . H141 H 0.374305 0.657697 0.365017 0.050 Uiso 1 1 calc R U . . . C151 C 0.42122(11) 0.55165(18) 0.40389(9) 0.0361(6) Uani 1 1 d . . . . . H151 H 0.418369 0.577137 0.429045 0.043 Uiso 1 1 calc R U . . . C161 C 0.45116(10) 0.46755(17) 0.40566(8) 0.0302(5) Uani 1 1 d . . . . . H161 H 0.468655 0.434876 0.431672 0.036 Uiso 1 1 calc R U . . . C171 C 0.45514(9) 0.43158(16) 0.36820(8) 0.0265(5) Uani 1 1 d . . . . . C181 C 0.42264(13) 0.4545(2) 0.25162(9) 0.0454(7) Uani 1 1 d . . . . . H18A H 0.456415 0.460327 0.243347 0.068 Uiso 1 1 calc R U . . . H18B H 0.402125 0.515641 0.247030 0.068 Uiso 1 1 calc R U . . . H18C H 0.397087 0.404748 0.234556 0.068 Uiso 1 1 calc R U . . . C191 C 0.47311(10) 0.14354(17) 0.31743(7) 0.0258(5) Uani 1 1 d . . . . . C201 C 0.44092(10) 0.06771(17) 0.29369(7) 0.0274(5) Uani 1 1 d . . . . . C211 C 0.42685(9) 0.01172(16) 0.32356(7) 0.0253(5) Uani 1 1 d . . . . . C221 C 0.39518(11) -0.07324(17) 0.32105(8) 0.0319(5) Uani 1 1 d . . . . . H221 H 0.377599 -0.104634 0.294723 0.038 Uiso 1 1 calc R U . . . C231 C 0.39010(11) -0.11001(17) 0.35720(9) 0.0352(6) Uani 1 1 d . . . . . H231 H 0.368381 -0.166699 0.355566 0.042 Uiso 1 1 calc R U . . . C241 C 0.41656(10) -0.06508(17) 0.39663(8) 0.0309(5) Uani 1 1 d . . . . . H241 H 0.413112 -0.092902 0.421183 0.037 Uiso 1 1 calc R U . . . C251 C 0.44723(10) 0.01815(16) 0.40020(7) 0.0257(5) Uani 1 1 d . . . . . H251 H 0.464549 0.048326 0.426852 0.031 Uiso 1 1 calc R U . . . C261 C 0.45250(9) 0.05792(15) 0.36349(7) 0.0228(4) Uani 1 1 d . . . . . C271 C 0.42320(12) 0.0445(2) 0.24734(8) 0.0365(6) Uani 1 1 d . . . . . H27A H 0.396370 0.093401 0.230792 0.055 Uiso 1 1 calc R U . . . H27B H 0.404426 -0.018180 0.241830 0.055 Uiso 1 1 calc R U . . . H27C H 0.457274 0.043368 0.239266 0.055 Uiso 1 1 calc R U . . . C281 C 0.48936(13) 0.2518(2) 0.24827(8) 0.0395(6) Uani 1 1 d . . . . . H28A H 0.447713 0.250970 0.233035 0.059 Uiso 1 1 calc R U . . . H28B H 0.506773 0.195987 0.240035 0.059 Uiso 1 1 calc R U . . . H28C H 0.505650 0.310360 0.241297 0.059 Uiso 1 1 calc R U . . . C291 C 0.60114(13) 0.39905(18) 0.48352(9) 0.0421(7) Uani 1 1 d . . . . . H29A H 0.571088 0.440400 0.487343 0.051 Uiso 1 1 calc R U . . . H29B H 0.595870 0.398661 0.453161 0.051 Uiso 1 1 calc R U . . . C301 C 0.65886(13) 0.4373(2) 0.50850(11) 0.0509(8) Uani 1 1 d . . . . . H30A H 0.665400 0.431627 0.538673 0.076 Uiso 1 1 calc R U . . . H30B H 0.661010 0.504795 0.501347 0.076 Uiso 1 1 calc R U . . . H30C H 0.688274 0.400909 0.501974 0.076 Uiso 1 1 calc R U . . . C311 C 0.48963(12) 0.25946(19) 0.52070(8) 0.0347(6) Uani 1 1 d . . . . . H31A H 0.523715 0.292557 0.540548 0.042 Uiso 1 1 calc R U . . . H31B H 0.490870 0.191654 0.529382 0.042 Uiso 1 1 calc R U . . . C321 C 0.43620(17) 0.3055(3) 0.52113(11) 0.0689(11) Uani 1 1 d . . . . . H32A H 0.435574 0.372586 0.512668 0.103 Uiso 1 1 calc R U . . . H32B H 0.434897 0.301996 0.549649 0.103 Uiso 1 1 calc R U . . . H32C H 0.402790 0.272190 0.501348 0.103 Uiso 1 1 calc R U . . . C331 C 0.60195(13) 0.07695(19) 0.48442(10) 0.0415(6) Uani 1 1 d . . . . . H33A H 0.641543 0.098307 0.500867 0.050 Uiso 1 1 calc R U . . . H33B H 0.596806 0.078307 0.454083 0.050 Uiso 1 1 calc R U . . . C341 C 0.59296(15) -0.0217(2) 0.49703(10) 0.0490(7) Uani 1 1 d . . . . . H34A H 0.597365 -0.022279 0.526934 0.074 Uiso 1 1 calc R U . . . H34B H 0.621396 -0.064597 0.492575 0.074 Uiso 1 1 calc R U . . . H34C H 0.554196 -0.043250 0.479916 0.074 Uiso 1 1 calc R U . . . K1 K 0.32176(2) 0.24191(3) 0.13487(2) 0.02776(12) Uani 1 1 d . . . . . O12 O 0.42782(7) 0.22780(14) 0.12277(6) 0.0372(4) Uani 1 1 d . . . . . O22 O 0.38641(8) 0.40433(13) 0.13622(6) 0.0435(5) Uani 1 1 d . . . . . O32 O 0.26783(8) 0.41816(12) 0.11523(7) 0.0446(5) Uani 1 1 d . . . . . O42 O 0.20490(7) 0.25592(12) 0.11833(6) 0.0359(4) Uani 1 1 d . . . . . O52 O 0.25475(8) 0.07685(12) 0.11604(6) 0.0382(4) Uani 1 1 d . . . . . O62 O 0.37207(8) 0.06512(12) 0.13408(6) 0.0369(4) Uani 1 1 d . . . . . N12 N 0.32880(13) 0.2463(2) 0.22210(10) 0.0604(8) Uani 1 1 d . . . . . C12 C 0.46492(11) 0.3094(3) 0.13538(9) 0.0480(8) Uani 1 1 d . . . . . H12A H 0.496044 0.304460 0.123712 0.058 Uiso 1 1 calc R U . . . H12B H 0.482672 0.311623 0.166548 0.058 Uiso 1 1 calc R U . . . C22 C 0.43127(13) 0.3973(3) 0.11969(10) 0.0552(9) Uani 1 1 d . . . . . H22A H 0.456715 0.453854 0.128399 0.066 Uiso 1 1 calc R U . . . H22B H 0.414712 0.396039 0.088455 0.066 Uiso 1 1 calc R U . . . C32 C 0.35635(16) 0.4934(2) 0.12547(14) 0.0712(12) Uani 1 1 d . . . . . H32D H 0.344337 0.504364 0.094679 0.085 Uiso 1 1 calc R U . . . H32E H 0.382049 0.546394 0.140162 0.085 Uiso 1 1 calc R U . . . C42 C 0.30538(16) 0.4914(2) 0.13795(13) 0.0682(11) Uani 1 1 d . . . . . H42A H 0.317238 0.479270 0.168651 0.082 Uiso 1 1 calc R U . . . H42B H 0.285465 0.553936 0.131753 0.082 Uiso 1 1 calc R U . . . C52 C 0.21325(14) 0.4231(2) 0.11981(13) 0.0623(10) Uani 1 1 d . . . . . H52A H 0.193776 0.483679 0.107598 0.075 Uiso 1 1 calc R U . . . H52B H 0.218219 0.421563 0.150105 0.075 Uiso 1 1 calc R U . . . C62 C 0.17785(12) 0.3403(2) 0.09758(11) 0.0532(8) Uani 1 1 d . . . . . H62A H 0.138590 0.345222 0.098388 0.064 Uiso 1 1 calc R U . . . H62B H 0.174948 0.339202 0.067688 0.064 Uiso 1 1 calc R U . . . C72 C 0.17199(12) 0.1725(2) 0.10153(12) 0.0537(8) Uani 1 1 d . . . . . H72A H 0.166210 0.165680 0.071218 0.064 Uiso 1 1 calc R U . . . H72B H 0.133829 0.177054 0.104334 0.064 Uiso 1 1 calc R U . . . C82 C 0.20397(12) 0.0886(2) 0.12553(12) 0.0564(9) Uani 1 1 d . . . . . H82A H 0.214025 0.099182 0.156203 0.068 Uiso 1 1 calc R U . . . H82B H 0.179866 0.030424 0.117432 0.068 Uiso 1 1 calc R U . . . C92 C 0.28699(14) -0.00422(19) 0.13674(11) 0.0530(8) Uani 1 1 d . . . . . H92A H 0.262383 -0.061979 0.129886 0.064 Uiso 1 1 calc R U . . . H92B H 0.301132 0.005273 0.167701 0.064 Uiso 1 1 calc R U . . . C102 C 0.33647(15) -0.0168(2) 0.12226(12) 0.0565(9) Uani 1 1 d . . . . . H10A H 0.358587 -0.074637 0.135368 0.068 Uiso 1 1 calc R U . . . H10B H 0.322362 -0.024823 0.091211 0.068 Uiso 1 1 calc R U . . . C112 C 0.41925(13) 0.0588(2) 0.11961(9) 0.0460(7) Uani 1 1 d . . . . . H11A H 0.404912 0.059846 0.088363 0.055 Uiso 1 1 calc R U . . . H11B H 0.440129 -0.002087 0.129260 0.055 Uiso 1 1 calc R U . . . C122 C 0.45848(12) 0.1405(2) 0.13652(9) 0.0462(7) Uani 1 1 d . . . . . H12C H 0.473970 0.138001 0.167755 0.055 Uiso 1 1 calc R U . . . H12D H 0.491164 0.137061 0.126419 0.055 Uiso 1 1 calc R U . . . C132 C 0.33331(13) 0.2445(2) 0.25643(10) 0.0451(7) Uani 1 1 d . . . . . C142 C 0.33930(14) 0.2424(2) 0.30046(11) 0.0540(8) Uani 1 1 d . . . . . H14A H 0.301130 0.243487 0.302705 0.081 Uiso 1 1 calc R U . . . H14B H 0.361272 0.298372 0.314900 0.081 Uiso 1 1 calc R U . . . H14C H 0.359542 0.183976 0.313618 0.081 Uiso 1 1 calc R U . . . C13 C 0.250000 0.1570(6) 0.000000 0.122(3) Uani 1 2 d DS TU P . . H13 H 0.250000 0.089054 0.000000 0.146 Uiso 1 2 calc R U P . . C23 C 0.2897(2) 0.2041(4) 0.02989(16) 0.126(2) Uani 1 1 d D U . . . H23 H 0.318495 0.170391 0.051593 0.151 Uiso 1 1 calc R U . . . C33 C 0.2893(2) 0.3042(4) 0.02965(16) 0.146(3) Uani 1 1 d D U . . . H33 H 0.318824 0.335221 0.051909 0.175 Uiso 1 1 calc R U . . . C43 C 0.250000 0.3626(7) 0.000000 0.139(3) Uani 1 2 d DS TU P . . H43 H 0.250000 0.430565 0.000000 0.167 Uiso 1 2 calc R U P . . N14A N 0.7529(3) 0.3328(8) 0.2543(3) 0.161(4) Uani 0.707(12) 1 d D U P A 1 C14A C 0.7518(4) 0.4143(8) 0.2566(4) 0.118(4) Uani 0.707(12) 1 d D U P A 1 C24A C 0.7529(7) 0.5174(9) 0.2492(5) 0.170(6) Uani 0.707(12) 1 d D U P A 1 H24A H 0.713717 0.542823 0.239947 0.254 Uiso 0.707(12) 1 calc R U P A 1 H24B H 0.769352 0.529144 0.227318 0.254 Uiso 0.707(12) 1 calc R U P A 1 H24C H 0.776550 0.549162 0.275421 0.254 Uiso 0.707(12) 1 calc R U P A 1 N14B N 0.7509(8) 0.5765(9) 0.2533(5) 0.108(7) Uani 0.293(12) 1 d D U P A 2 C14B C 0.7521(6) 0.4980(8) 0.2469(5) 0.046(3) Uani 0.293(12) 1 d D U P A 2 C24B C 0.7559(8) 0.4038(10) 0.2300(7) 0.085(6) Uani 0.293(12) 1 d D U P A 2 H24D H 0.792869 0.397209 0.226161 0.128 Uiso 0.293(12) 1 calc R U P A 2 H24E H 0.724560 0.395729 0.202763 0.128 Uiso 0.293(12) 1 calc R U P A 2 H24F H 0.752710 0.354775 0.249754 0.128 Uiso 0.293(12) 1 calc R U P A 2 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 Cu1 0.02661(15) 0.02623(15) 0.01562(14) 0.00049(10) 0.00695(11) -0.00021(11) P11 0.0296(3) 0.0318(3) 0.0154(3) 0.0014(2) 0.0057(2) -0.0032(2) P21 0.0301(3) 0.0227(3) 0.0175(3) 0.0006(2) 0.0087(2) 0.0006(2) O11 0.0386(10) 0.0309(9) 0.0238(8) 0.0011(7) 0.0062(7) -0.0042(7) O21 0.0363(9) 0.0370(9) 0.0213(8) -0.0004(7) 0.0130(7) 0.0026(7) O31 0.0480(11) 0.0265(8) 0.0285(9) 0.0040(7) 0.0177(8) 0.0063(8) N11 0.0258(9) 0.0286(10) 0.0178(9) 0.0009(7) 0.0071(7) -0.0008(8) N21 0.0254(10) 0.0267(10) 0.0226(10) 0.0018(7) 0.0067(8) -0.0012(8) N31 0.0271(10) 0.0264(10) 0.0205(9) 0.0004(7) 0.0085(8) -0.0024(8) C11 0.0319(12) 0.0262(11) 0.0178(10) -0.0001(8) 0.0084(9) -0.0035(9) C21 0.0350(12) 0.0237(11) 0.0259(11) 0.0003(9) 0.0146(10) -0.0027(9) C31 0.0330(12) 0.0153(10) 0.0303(12) -0.0013(8) 0.0150(10) -0.0020(9) C41 0.0341(13) 0.0237(11) 0.0444(15) -0.0031(10) 0.0202(11) -0.0026(10) C51 0.0257(12) 0.0344(13) 0.0500(16) -0.0016(12) 0.0124(11) 0.0002(10) C61 0.0299(13) 0.0396(14) 0.0363(14) -0.0006(11) 0.0018(11) 0.0003(11) C71 0.0310(13) 0.0340(13) 0.0266(12) -0.0005(10) 0.0078(10) -0.0015(10) C81 0.0260(11) 0.0196(10) 0.0268(11) -0.0009(8) 0.0095(9) -0.0019(8) C91 0.0535(18) 0.0589(19) 0.0299(14) 0.0018(12) 0.0243(13) -0.0045(14) C101 0.0270(12) 0.0305(12) 0.0233(12) 0.0035(9) 0.0046(9) -0.0029(9) C111 0.0260(12) 0.0329(13) 0.0300(13) 0.0103(10) 0.0036(10) -0.0029(10) C121 0.0210(12) 0.0272(12) 0.0395(14) 0.0073(10) 0.0051(10) -0.0053(9) C131 0.0245(13) 0.0289(13) 0.0585(18) 0.0133(12) 0.0100(12) 0.0002(10) C141 0.0278(13) 0.0253(12) 0.073(2) 0.0049(13) 0.0204(13) -0.0002(10) C151 0.0274(13) 0.0292(13) 0.0561(17) -0.0072(11) 0.0204(12) -0.0078(10) C161 0.0231(12) 0.0291(12) 0.0387(14) -0.0015(10) 0.0114(10) -0.0052(9) C171 0.0198(11) 0.0240(11) 0.0341(13) 0.0034(9) 0.0074(9) -0.0045(9) C181 0.0421(16) 0.0479(17) 0.0359(15) 0.0166(12) 0.0013(12) 0.0000(13) C191 0.0265(12) 0.0311(12) 0.0185(11) -0.0011(9) 0.0064(9) -0.0011(9) C201 0.0256(12) 0.0298(12) 0.0237(11) -0.0041(9) 0.0051(9) 0.0010(9) C211 0.0206(11) 0.0274(11) 0.0266(11) -0.0042(9) 0.0068(9) 0.0033(9) C221 0.0302(13) 0.0275(12) 0.0362(14) -0.0076(10) 0.0095(11) -0.0002(10) C231 0.0319(13) 0.0231(12) 0.0523(16) 0.0009(11) 0.0169(12) -0.0008(10) C241 0.0305(13) 0.0268(12) 0.0397(14) 0.0057(10) 0.0177(11) 0.0060(10) C251 0.0235(11) 0.0273(11) 0.0273(12) 0.0032(9) 0.0101(9) 0.0053(9) C261 0.0190(11) 0.0225(10) 0.0254(11) -0.0007(8) 0.0060(9) 0.0038(8) C271 0.0391(15) 0.0429(15) 0.0238(12) -0.0106(10) 0.0066(11) -0.0045(11) C281 0.0425(15) 0.0554(17) 0.0167(11) 0.0020(11) 0.0058(10) -0.0074(12) C291 0.0479(17) 0.0261(13) 0.0434(16) 0.0026(11) 0.0053(13) -0.0075(11) C301 0.0448(17) 0.0399(16) 0.065(2) -0.0043(14) 0.0152(15) -0.0114(13) C311 0.0415(14) 0.0441(15) 0.0222(11) -0.0041(10) 0.0160(10) -0.0051(11) C321 0.075(2) 0.102(3) 0.0429(18) 0.0109(19) 0.0372(18) 0.036(2) C331 0.0491(17) 0.0336(14) 0.0478(16) 0.0080(12) 0.0243(14) 0.0123(12) C341 0.068(2) 0.0329(15) 0.0483(17) 0.0064(12) 0.0239(16) 0.0118(14) K1 0.0216(2) 0.0198(2) 0.0456(3) -0.0017(2) 0.0166(2) -0.00146(18) O12 0.0205(8) 0.0609(12) 0.0320(9) 0.0001(8) 0.0115(7) 0.0016(8) O22 0.0444(11) 0.0303(9) 0.0515(12) 0.0087(8) 0.0120(9) -0.0139(8) O32 0.0441(11) 0.0243(9) 0.0581(13) 0.0026(8) 0.0093(10) 0.0058(8) O42 0.0201(8) 0.0429(10) 0.0437(11) 0.0068(8) 0.0101(7) 0.0047(7) O52 0.0345(10) 0.0272(9) 0.0494(11) 0.0024(8) 0.0107(9) -0.0067(7) O62 0.0392(10) 0.0300(9) 0.0429(10) -0.0048(8) 0.0164(8) 0.0105(8) N12 0.0474(16) 0.087(2) 0.0454(17) 0.0012(14) 0.0152(13) 0.0035(14) C12 0.0241(13) 0.087(2) 0.0331(14) 0.0104(15) 0.0110(11) -0.0175(14) C22 0.0403(17) 0.075(2) 0.0469(17) 0.0196(16) 0.0106(14) -0.0307(16) C32 0.065(2) 0.0235(14) 0.102(3) 0.0137(16) 0.001(2) -0.0160(14) C42 0.067(2) 0.0229(14) 0.094(3) -0.0080(16) 0.004(2) 0.0063(14) C52 0.053(2) 0.0445(18) 0.086(3) -0.0004(17) 0.0208(18) 0.0275(15) C62 0.0285(15) 0.0526(18) 0.072(2) 0.0111(16) 0.0106(14) 0.0179(13) C72 0.0190(13) 0.062(2) 0.072(2) 0.0074(16) 0.0055(13) -0.0108(13) C82 0.0320(15) 0.0496(18) 0.083(2) 0.0175(17) 0.0148(15) -0.0156(13) C92 0.0557(19) 0.0236(13) 0.072(2) 0.0089(13) 0.0135(17) -0.0068(12) C102 0.067(2) 0.0219(13) 0.077(2) -0.0063(14) 0.0208(18) 0.0084(13) C112 0.0443(16) 0.0600(19) 0.0355(15) -0.0039(13) 0.0164(13) 0.0263(14) C122 0.0280(14) 0.079(2) 0.0345(15) 0.0006(14) 0.0139(12) 0.0191(14) C132 0.0335(14) 0.0559(19) 0.0481(18) 0.0028(14) 0.0172(13) 0.0042(13) C142 0.0435(17) 0.079(2) 0.0483(18) 0.0022(16) 0.0268(15) 0.0069(16) C13 0.084(5) 0.112(5) 0.182(7) 0.000 0.062(5) 0.000 C23 0.141(5) 0.135(4) 0.096(4) 0.009(3) 0.034(4) 0.019(4) C33 0.160(6) 0.145(5) 0.110(4) -0.043(4) 0.021(4) 0.009(4) C43 0.119(6) 0.199(7) 0.111(6) 0.000 0.054(5) 0.000 N14A 0.083(5) 0.166(7) 0.263(11) 0.034(7) 0.097(6) 0.012(5) C14A 0.053(4) 0.145(6) 0.135(7) -0.020(6) 0.007(5) 0.006(5) C24A 0.180(13) 0.157(8) 0.162(13) -0.012(10) 0.050(10) 0.011(10) N14B 0.112(11) 0.068(7) 0.099(11) -0.013(6) -0.017(8) 0.011(7) C14B 0.028(5) 0.063(6) 0.050(6) 0.001(5) 0.016(4) -0.003(4) C24B 0.066(9) 0.076(8) 0.093(11) -0.014(7) 0.001(9) 0.005(7) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' O O 0.0106 0.0060 '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' 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 N31 Cu1 N21 92.38(8) . . ? N31 Cu1 N11 94.54(7) . . ? N21 Cu1 N11 95.06(7) . . ? N31 Cu1 P21 121.97(5) . . ? N21 Cu1 P21 121.85(6) . . ? N11 Cu1 P21 123.28(6) . . ? C11 P11 C101 108.84(11) . . ? C11 P11 C191 108.29(10) . . ? C101 P11 C191 108.20(11) . . ? C11 P11 C281 110.53(12) . . ? C101 P11 C281 110.34(12) . . ? C191 P11 C281 110.58(12) . . ? O21 P21 O31 98.78(9) . . ? O21 P21 O11 104.13(9) . . ? O31 P21 O11 97.46(9) . . ? O21 P21 Cu1 113.79(7) . . ? O31 P21 Cu1 120.90(7) . . ? O11 P21 Cu1 118.52(7) . . ? C291 O11 P21 117.06(15) . . ? C311 O21 P21 122.47(16) . . ? C331 O31 P21 119.19(16) . . ? C81 N11 C11 104.31(19) . . ? C81 N11 Cu1 136.83(16) . . ? C11 N11 Cu1 118.86(15) . . ? C171 N21 C101 105.21(19) . . ? C171 N21 Cu1 135.75(16) . . ? C101 N21 Cu1 119.04(15) . . ? C261 N31 C191 104.88(18) . . ? C261 N31 Cu1 135.68(15) . . ? C191 N31 Cu1 119.43(15) . . ? N11 C11 C21 113.5(2) . . ? N11 C11 P11 113.94(17) . . ? C21 C11 P11 132.50(18) . . ? C11 C21 C31 104.4(2) . . ? C11 C21 C91 130.7(2) . . ? C31 C21 C91 124.9(2) . . ? C41 C31 C21 133.8(2) . . ? C41 C31 C81 119.7(2) . . ? C21 C31 C81 106.4(2) . . ? C51 C41 C31 119.0(2) . . ? C51 C41 H41 120.5 . . ? C31 C41 H41 120.5 . . ? C41 C51 C61 120.8(2) . . ? C41 C51 H51 119.6 . . ? C61 C51 H51 119.6 . . ? C71 C61 C51 121.6(2) . . ? C71 C61 H61 119.2 . . ? C51 C61 H61 119.2 . . ? C61 C71 C81 118.5(2) . . ? C61 C71 H71 120.7 . . ? C81 C71 H71 120.7 . . ? N11 C81 C71 128.4(2) . . ? N11 C81 C31 111.3(2) . . ? C71 C81 C31 120.3(2) . . ? C21 C91 H91A 109.5 . . ? C21 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C21 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N21 C101 C111 113.2(2) . . ? N21 C101 P11 113.76(16) . . ? C111 C101 P11 133.04(19) . . ? C101 C111 C121 104.3(2) . . ? C101 C111 C181 130.8(3) . . ? C121 C111 C181 124.9(2) . . ? C131 C121 C111 134.0(2) . . ? C131 C121 C171 119.3(2) . . ? C111 C121 C171 106.8(2) . . ? C141 C131 C121 119.1(3) . . ? C141 C131 H131 120.5 . . ? C121 C131 H131 120.5 . . ? C131 C141 C151 121.4(2) . . ? C131 C141 H141 119.3 . . ? C151 C141 H141 119.3 . . ? C161 C151 C141 121.1(3) . . ? C161 C151 H151 119.5 . . ? C141 C151 H151 119.5 . . ? C151 C161 C171 118.5(2) . . ? C151 C161 H161 120.8 . . ? C171 C161 H161 120.8 . . ? N21 C171 C161 128.7(2) . . ? N21 C171 C121 110.6(2) . . ? C161 C171 C121 120.7(2) . . ? C111 C181 H18A 109.5 . . ? C111 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C111 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? N31 C191 C201 113.4(2) . . ? N31 C191 P11 113.42(16) . . ? C201 C191 P11 133.11(18) . . ? C191 C201 C211 104.1(2) . . ? C191 C201 C271 131.1(2) . . ? C211 C201 C271 124.7(2) . . ? C221 C211 C201 134.1(2) . . ? C221 C211 C261 119.3(2) . . ? C201 C211 C261 106.6(2) . . ? C231 C221 C211 119.2(2) . . ? C231 C221 H221 120.4 . . ? C211 C221 H221 120.4 . . ? C221 C231 C241 121.2(2) . . ? C221 C231 H231 119.4 . . ? C241 C231 H231 119.4 . . ? C251 C241 C231 121.2(2) . . ? C251 C241 H241 119.4 . . ? C231 C241 H241 119.4 . . ? C241 C251 C261 118.7(2) . . ? C241 C251 H251 120.7 . . ? C261 C251 H251 120.7 . . ? N31 C261 C251 128.6(2) . . ? N31 C261 C211 110.9(2) . . ? C251 C261 C211 120.4(2) . . ? C201 C271 H27A 109.5 . . ? C201 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C201 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? P11 C281 H28A 109.5 . . ? P11 C281 H28B 109.5 . . ? H28A C281 H28B 109.5 . . ? P11 C281 H28C 109.5 . . ? H28A C281 H28C 109.5 . . ? H28B C281 H28C 109.5 . . ? O11 C291 C301 109.6(2) . . ? O11 C291 H29A 109.8 . . ? C301 C291 H29A 109.8 . . ? O11 C291 H29B 109.8 . . ? C301 C291 H29B 109.8 . . ? H29A C291 H29B 108.2 . . ? C291 C301 H30A 109.5 . . ? C291 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C291 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? O21 C311 C321 107.5(2) . . ? O21 C311 H31A 110.2 . . ? C321 C311 H31A 110.2 . . ? O21 C311 H31B 110.2 . . ? C321 C311 H31B 110.2 . . ? H31A C311 H31B 108.5 . . ? C311 C321 H32A 109.5 . . ? C311 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? C311 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? O31 C331 C341 109.0(2) . . ? O31 C331 H33A 109.9 . . ? C341 C331 H33A 109.9 . . ? O31 C331 H33B 109.9 . . ? C341 C331 H33B 109.9 . . ? H33A C331 H33B 108.3 . . ? C331 C341 H34A 109.5 . . ? C331 C341 H34B 109.5 . . ? H34A C341 H34B 109.5 . . ? C331 C341 H34C 109.5 . . ? H34A C341 H34C 109.5 . . ? H34B C341 H34C 109.5 . . ? O42 K1 O32 60.26(6) . . ? O42 K1 O22 120.49(6) . . ? O32 K1 O22 60.31(6) . . ? O42 K1 O62 120.44(6) . . ? O32 K1 O62 166.21(6) . . ? O22 K1 O62 117.90(6) . . ? O42 K1 O52 60.76(5) . . ? O32 K1 O52 118.83(6) . . ? O22 K1 O52 168.12(6) . . ? O62 K1 O52 59.69(6) . . ? O42 K1 O12 161.28(6) . . ? O32 K1 O12 115.21(6) . . ? O22 K1 O12 59.46(6) . . ? O62 K1 O12 59.14(6) . . ? O52 K1 O12 115.10(6) . . ? O42 K1 N12 83.25(7) . . ? O32 K1 N12 94.27(8) . . ? O22 K1 N12 98.16(8) . . ? O62 K1 N12 99.50(7) . . ? O52 K1 N12 93.71(7) . . ? O12 K1 N12 115.48(7) . . ? O42 K1 C23 87.75(11) . . ? O32 K1 C23 88.49(11) . . ? O22 K1 C23 93.62(11) . . ? O62 K1 C23 77.88(11) . . ? O52 K1 C23 74.51(11) . . ? O12 K1 C23 73.74(10) . . ? N12 K1 C23 167.69(11) . . ? O42 K1 C33 86.05(10) . . ? O32 K1 C33 67.37(10) . . ? O22 K1 C33 74.53(11) . . ? O62 K1 C33 98.85(10) . . ? O52 K1 C33 94.08(11) . . ? O12 K1 C33 75.85(10) . . ? N12 K1 C33 161.58(11) . . ? C23 K1 C33 23.45(11) . . ? O42 K1 C42 79.11(7) . . ? O32 K1 C42 22.20(7) . . ? O22 K1 C42 42.32(8) . . ? O62 K1 C42 160.20(8) . . ? O52 K1 C42 139.65(7) . . ? O12 K1 C42 101.43(8) . . ? N12 K1 C42 85.09(9) . . ? C23 K1 C42 101.47(12) . . ? C33 K1 C42 78.18(12) . . ? C122 O12 C12 111.7(2) . . ? C122 O12 K1 115.61(16) . . ? C12 O12 K1 115.99(16) . . ? C22 O22 C32 111.9(2) . . ? C22 O22 K1 118.04(17) . . ? C32 O22 K1 117.39(17) . . ? C42 O32 C52 112.1(3) . . ? C42 O32 K1 110.07(17) . . ? C52 O32 K1 114.64(17) . . ? C62 O42 C72 112.4(2) . . ? C62 O42 K1 116.09(16) . . ? C72 O42 K1 115.92(16) . . ? C82 O52 C92 111.8(2) . . ? C82 O52 K1 111.16(16) . . ? C92 O52 K1 111.16(15) . . ? C102 O62 C112 111.2(2) . . ? C102 O62 K1 118.95(16) . . ? C112 O62 K1 119.21(16) . . ? C132 N12 K1 176.7(3) . . ? O12 C12 C22 109.4(2) . . ? O12 C12 H12A 109.8 . . ? C22 C12 H12A 109.8 . . ? O12 C12 H12B 109.8 . . ? C22 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? O22 C22 C12 109.9(2) . . ? O22 C22 H22A 109.7 . . ? C12 C22 H22A 109.7 . . ? O22 C22 H22B 109.7 . . ? C12 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O22 C32 C42 109.7(3) . . ? O22 C32 H32D 109.7 . . ? C42 C32 H32D 109.7 . . ? O22 C32 H32E 109.7 . . ? C42 C32 H32E 109.7 . . ? H32D C32 H32E 108.2 . . ? O32 C42 C32 109.1(3) . . ? O32 C42 K1 47.73(12) . . ? C32 C42 K1 83.63(17) . . ? O32 C42 H42A 109.9 . . ? C32 C42 H42A 109.9 . . ? K1 C42 H42A 82.3 . . ? O32 C42 H42B 109.9 . . ? C32 C42 H42B 109.9 . . ? K1 C42 H42B 157.5 . . ? H42A C42 H42B 108.3 . . ? O32 C52 C62 108.9(3) . . ? O32 C52 H52A 109.9 . . ? C62 C52 H52A 109.9 . . ? O32 C52 H52B 109.9 . . ? C62 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? O42 C62 C52 107.8(2) . . ? O42 C62 H62A 110.1 . . ? C52 C62 H62A 110.1 . . ? O42 C62 H62B 110.1 . . ? C52 C62 H62B 110.1 . . ? H62A C62 H62B 108.5 . . ? O42 C72 C82 107.9(2) . . ? O42 C72 H72A 110.1 . . ? C82 C72 H72A 110.1 . . ? O42 C72 H72B 110.1 . . ? C82 C72 H72B 110.1 . . ? H72A C72 H72B 108.4 . . ? O52 C82 C72 108.3(2) . . ? O52 C82 H82A 110.0 . . ? C72 C82 H82A 110.0 . . ? O52 C82 H82B 110.0 . . ? C72 C82 H82B 110.0 . . ? H82A C82 H82B 108.4 . . ? O52 C92 C102 108.6(3) . . ? O52 C92 H92A 110.0 . . ? C102 C92 H92A 110.0 . . ? O52 C92 H92B 110.0 . . ? C102 C92 H92B 110.0 . . ? H92A C92 H92B 108.3 . . ? O62 C102 C92 108.6(2) . . ? O62 C102 H10A 110.0 . . ? C92 C102 H10A 110.0 . . ? O62 C102 H10B 110.0 . . ? C92 C102 H10B 110.0 . . ? H10A C102 H10B 108.4 . . ? O62 C112 C122 109.2(2) . . ? O62 C112 H11A 109.8 . . ? C122 C112 H11A 109.8 . . ? O62 C112 H11B 109.8 . . ? C122 C112 H11B 109.8 . . ? H11A C112 H11B 108.3 . . ? O12 C122 C112 109.4(2) . . ? O12 C122 H12C 109.8 . . ? C112 C122 H12C 109.8 . . ? O12 C122 H12D 109.8 . . ? C112 C122 H12D 109.8 . . ? H12C C122 H12D 108.2 . . ? N12 C132 C142 179.8(4) . . ? C132 C142 H14A 109.5 . . ? C132 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C132 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C23 C13 C23 119.8(8) . 2 ? C23 C13 H13 120.1 . . ? C23 C13 H13 120.1 2 . ? C13 C23 C33 119.7(5) . . ? C13 C23 K1 135.9(3) . . ? C33 C23 K1 81.3(2) . . ? C13 C23 H23 120.1 . . ? C33 C23 H23 120.1 . . ? K1 C23 H23 55.6 . . ? C43 C33 C23 126.4(5) . . ? C43 C33 K1 137.3(3) . . ? C23 C33 K1 75.2(2) . . ? C43 C33 H33 116.8 . . ? C23 C33 H33 116.8 . . ? K1 C33 H33 57.9 . . ? C33 C43 C33 108.0(7) 2 . ? C33 C43 H43 126.0 2 . ? C33 C43 H43 126.0 . . ? N14A C14A C24A 165.1(16) . . ? C14A C24A H24A 109.5 . . ? C14A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C14A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? N14B C14B C24B 167.0(19) . . ? C14B C24B H24D 109.5 . . ? C14B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C14B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? 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 Cu1 N31 2.0622(19) . ? Cu1 N21 2.0654(19) . ? Cu1 N11 2.0759(19) . ? Cu1 P21 2.1201(6) . ? P11 C11 1.778(2) . ? P11 C101 1.781(3) . ? P11 C191 1.783(2) . ? P11 C281 1.789(3) . ? P21 O21 1.6006(18) . ? P21 O31 1.6078(17) . ? P21 O11 1.6187(18) . ? O11 C291 1.444(3) . ? O21 C311 1.451(3) . ? O31 C331 1.432(3) . ? N11 C81 1.365(3) . ? N11 C11 1.378(3) . ? N21 C171 1.361(3) . ? N21 C101 1.382(3) . ? N31 C261 1.357(3) . ? N31 C191 1.379(3) . ? C11 C21 1.393(3) . ? C21 C31 1.418(3) . ? C21 C91 1.505(3) . ? C31 C41 1.413(3) . ? C31 C81 1.419(3) . ? C41 C51 1.370(4) . ? C41 H41 0.9500 . ? C51 C61 1.408(4) . ? C51 H51 0.9500 . ? C61 C71 1.373(4) . ? C61 H61 0.9500 . ? C71 C81 1.405(3) . ? C71 H71 0.9500 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C101 C111 1.399(3) . ? C111 C121 1.420(4) . ? C111 C181 1.511(3) . ? C121 C131 1.412(4) . ? C121 C171 1.433(3) . ? C131 C141 1.371(4) . ? C131 H131 0.9500 . ? C141 C151 1.410(4) . ? C141 H141 0.9500 . ? C151 C161 1.382(3) . ? C151 H151 0.9500 . ? C161 C171 1.402(3) . ? C161 H161 0.9500 . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C191 C201 1.398(3) . ? C201 C211 1.419(3) . ? C201 C271 1.508(3) . ? C211 C221 1.411(3) . ? C211 C261 1.429(3) . ? C221 C231 1.376(4) . ? C221 H221 0.9500 . ? C231 C241 1.410(4) . ? C231 H231 0.9500 . ? C241 C251 1.373(3) . ? C241 H241 0.9500 . ? C251 C261 1.411(3) . ? C251 H251 0.9500 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C281 H28A 0.9800 . ? C281 H28B 0.9800 . ? C281 H28C 0.9800 . ? C291 C301 1.484(4) . ? C291 H29A 0.9900 . ? C291 H29B 0.9900 . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C311 C321 1.482(4) . ? C311 H31A 0.9900 . ? C311 H31B 0.9900 . ? C321 H32A 0.9800 . ? C321 H32B 0.9800 . ? C321 H32C 0.9800 . ? C331 C341 1.484(4) . ? C331 H33A 0.9900 . ? C331 H33B 0.9900 . ? C341 H34A 0.9800 . ? C341 H34B 0.9800 . ? C341 H34C 0.9800 . ? K1 O42 2.7669(17) . ? K1 O32 2.7718(18) . ? K1 O22 2.7747(18) . ? K1 O62 2.7757(17) . ? K1 O52 2.7855(18) . ? K1 O12 2.8197(17) . ? K1 N12 2.900(3) . ? K1 C23 3.399(5) . ? K1 C33 3.476(5) . ? K1 C42 3.518(3) . ? O12 C122 1.427(3) . ? O12 C12 1.434(4) . ? O22 C22 1.420(4) . ? O22 C32 1.431(4) . ? O32 C42 1.415(4) . ? O32 C52 1.423(4) . ? O42 C62 1.415(3) . ? O42 C72 1.423(3) . ? O52 C82 1.421(4) . ? O52 C92 1.421(3) . ? O62 C102 1.416(4) . ? O62 C112 1.428(3) . ? N12 C132 1.129(4) . ? C12 C22 1.476(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C32 C42 1.474(6) . ? C32 H32D 0.9900 . ? C32 H32E 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C52 C62 1.488(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C72 C82 1.487(4) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C92 C102 1.490(5) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C102 H10A 0.9900 . ? C102 H10B 0.9900 . ? C112 C122 1.480(5) . ? C112 H11A 0.9900 . ? C112 H11B 0.9900 . ? C122 H12C 0.9900 . ? C122 H12D 0.9900 . ? C132 C142 1.446(5) . ? C142 H14A 0.9800 . ? C142 H14B 0.9800 . ? C142 H14C 0.9800 . ? C13 C23 1.313(5) . ? C13 C23 1.313(5) 2 ? C13 H13 0.9500 . ? C23 C33 1.399(7) . ? C23 H23 0.9500 . ? C33 C43 1.391(5) . ? C33 H33 0.9500 . ? C43 H43 0.9500 . ? N14A C14A 1.143(8) . ? C14A C24A 1.465(8) . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? N14B C14B 1.122(9) . ? C14B C24B 1.452(9) . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O21 P21 O11 C291 -85.3(2) . . . . ? O31 P21 O11 C291 173.65(19) . . . . ? Cu1 P21 O11 C291 42.3(2) . . . . ? O31 P21 O21 C311 44.94(19) . . . . ? O11 P21 O21 C311 -55.10(19) . . . . ? Cu1 P21 O21 C311 174.43(15) . . . . ? O21 P21 O31 C331 167.46(19) . . . . ? O11 P21 O31 C331 -86.9(2) . . . . ? Cu1 P21 O31 C331 42.8(2) . . . . ? C81 N11 C11 C21 -0.1(2) . . . . ? Cu1 N11 C11 C21 -179.62(15) . . . . ? C81 N11 C11 P11 178.37(15) . . . . ? Cu1 N11 C11 P11 -1.2(2) . . . . ? C101 P11 C11 N11 59.27(18) . . . . ? C191 P11 C11 N11 -58.14(18) . . . . ? C281 P11 C11 N11 -179.40(16) . . . . ? C101 P11 C11 C21 -122.7(2) . . . . ? C191 P11 C11 C21 119.9(2) . . . . ? C281 P11 C11 C21 -1.4(3) . . . . ? N11 C11 C21 C31 -0.2(3) . . . . ? P11 C11 C21 C31 -178.21(18) . . . . ? N11 C11 C21 C91 -179.8(2) . . . . ? P11 C11 C21 C91 2.1(4) . . . . ? C11 C21 C31 C41 -179.6(2) . . . . ? C91 C21 C31 C41 0.1(4) . . . . ? C11 C21 C31 C81 0.3(2) . . . . ? C91 C21 C31 C81 180.0(2) . . . . ? C21 C31 C41 C51 -179.4(2) . . . . ? C81 C31 C41 C51 0.8(3) . . . . ? C31 C41 C51 C61 -0.3(4) . . . . ? C41 C51 C61 C71 -0.4(4) . . . . ? C51 C61 C71 C81 0.5(4) . . . . ? C11 N11 C81 C71 -179.5(2) . . . . ? Cu1 N11 C81 C71 -0.1(4) . . . . ? C11 N11 C81 C31 0.3(2) . . . . ? Cu1 N11 C81 C31 179.70(15) . . . . ? C61 C71 C81 N11 179.8(2) . . . . ? C61 C71 C81 C31 0.1(3) . . . . ? C41 C31 C81 N11 179.51(19) . . . . ? C21 C31 C81 N11 -0.4(2) . . . . ? C41 C31 C81 C71 -0.7(3) . . . . ? C21 C31 C81 C71 179.4(2) . . . . ? C171 N21 C101 C111 0.2(3) . . . . ? Cu1 N21 C101 C111 179.66(16) . . . . ? C171 N21 C101 P11 -177.96(16) . . . . ? Cu1 N21 C101 P11 1.5(2) . . . . ? C11 P11 C101 N21 -59.56(19) . . . . ? C191 P11 C101 N21 57.91(19) . . . . ? C281 P11 C101 N21 179.00(17) . . . . ? C11 P11 C101 C111 122.8(2) . . . . ? C191 P11 C101 C111 -119.8(2) . . . . ? C281 P11 C101 C111 1.3(3) . . . . ? N21 C101 C111 C121 -0.7(3) . . . . ? P11 C101 C111 C121 177.0(2) . . . . ? N21 C101 C111 C181 179.6(2) . . . . ? P11 C101 C111 C181 -2.7(4) . . . . ? C101 C111 C121 C131 179.9(3) . . . . ? C181 C111 C121 C131 -0.3(4) . . . . ? C101 C111 C121 C171 0.8(3) . . . . ? C181 C111 C121 C171 -179.4(2) . . . . ? C111 C121 C131 C141 -178.5(3) . . . . ? C171 C121 C131 C141 0.5(3) . . . . ? C121 C131 C141 C151 -0.1(4) . . . . ? C131 C141 C151 C161 -0.4(4) . . . . ? C141 C151 C161 C171 0.4(3) . . . . ? C101 N21 C171 C161 -179.1(2) . . . . ? Cu1 N21 C171 C161 1.5(4) . . . . ? C101 N21 C171 C121 0.4(2) . . . . ? Cu1 N21 C171 C121 -178.96(16) . . . . ? C151 C161 C171 N21 179.5(2) . . . . ? C151 C161 C171 C121 0.0(3) . . . . ? C131 C121 C171 N21 180.0(2) . . . . ? C111 C121 C171 N21 -0.8(3) . . . . ? C131 C121 C171 C161 -0.5(3) . . . . ? C111 C121 C171 C161 178.8(2) . . . . ? C261 N31 C191 C201 -0.4(3) . . . . ? Cu1 N31 C191 C201 178.58(16) . . . . ? C261 N31 C191 P11 177.15(15) . . . . ? Cu1 N31 C191 P11 -3.8(2) . . . . ? C11 P11 C191 N31 61.34(19) . . . . ? C101 P11 C191 N31 -56.49(19) . . . . ? C281 P11 C191 N31 -177.43(18) . . . . ? C11 P11 C191 C201 -121.7(2) . . . . ? C101 P11 C191 C201 120.5(2) . . . . ? C281 P11 C191 C201 -0.5(3) . . . . ? N31 C191 C201 C211 0.7(3) . . . . ? P11 C191 C201 C211 -176.2(2) . . . . ? N31 C191 C201 C271 -179.2(2) . . . . ? P11 C191 C201 C271 3.9(4) . . . . ? C191 C201 C211 C221 179.4(3) . . . . ? C271 C201 C211 C221 -0.7(4) . . . . ? C191 C201 C211 C261 -0.7(2) . . . . ? C271 C201 C211 C261 179.2(2) . . . . ? C201 C211 C221 C231 179.4(2) . . . . ? C261 C211 C221 C231 -0.5(3) . . . . ? C211 C221 C231 C241 -0.9(4) . . . . ? C221 C231 C241 C251 1.5(4) . . . . ? C231 C241 C251 C261 -0.7(3) . . . . ? C191 N31 C261 C251 179.0(2) . . . . ? Cu1 N31 C261 C251 0.3(4) . . . . ? C191 N31 C261 C211 -0.1(2) . . . . ? Cu1 N31 C261 C211 -178.83(16) . . . . ? C241 C251 C261 N31 -179.7(2) . . . . ? C241 C251 C261 C211 -0.6(3) . . . . ? C221 C211 C261 N31 -179.6(2) . . . . ? C201 C211 C261 N31 0.5(3) . . . . ? C221 C211 C261 C251 1.2(3) . . . . ? C201 C211 C261 C251 -178.7(2) . . . . ? P21 O11 C291 C301 -163.1(2) . . . . ? P21 O21 C311 C321 170.9(2) . . . . ? P21 O31 C331 C341 -156.5(2) . . . . ? C122 O12 C12 C22 178.9(2) . . . . ? K1 O12 C12 C22 -45.7(3) . . . . ? C32 O22 C22 C12 173.9(3) . . . . ? K1 O22 C22 C12 -45.2(3) . . . . ? O12 C12 C22 O22 59.2(3) . . . . ? C22 O22 C32 C42 171.9(3) . . . . ? K1 O22 C32 C42 30.7(4) . . . . ? C52 O32 C42 C32 -169.3(3) . . . . ? K1 O32 C42 C32 61.8(3) . . . . ? C52 O32 C42 K1 128.9(3) . . . . ? O22 C32 C42 O32 -62.1(4) . . . . ? O22 C32 C42 K1 -21.1(3) . . . . ? C42 O32 C52 C62 -176.1(3) . . . . ? K1 O32 C52 C62 -49.7(3) . . . . ? C72 O42 C62 C52 175.4(3) . . . . ? K1 O42 C62 C52 -48.0(3) . . . . ? O32 C52 C62 O42 64.4(4) . . . . ? C62 O42 C72 C82 -179.8(3) . . . . ? K1 O42 C72 C82 43.5(3) . . . . ? C92 O52 C82 C72 -178.0(3) . . . . ? K1 O52 C82 C72 57.1(3) . . . . ? O42 C72 C82 O52 -67.7(4) . . . . ? C82 O52 C92 C102 175.0(3) . . . . ? K1 O52 C92 C102 -60.1(3) . . . . ? C112 O62 C102 C92 -177.8(2) . . . . ? K1 O62 C102 C92 -33.5(3) . . . . ? O52 C92 C102 O62 62.1(3) . . . . ? C102 O62 C112 C122 -174.0(2) . . . . ? K1 O62 C112 C122 41.8(3) . . . . ? C12 O12 C122 C112 -175.2(2) . . . . ? K1 O12 C122 C112 49.2(2) . . . . ? O62 C112 C122 O12 -58.9(3) . . . . ? C23 C13 C23 C33 0.03(14) 2 . . . ? C23 C13 C23 K1 109.9(6) 2 . . . ? C13 C23 C33 C43 -0.1(3) . . . . ? K1 C23 C33 C43 -138.6(4) . . . . ? C13 C23 C33 K1 138.5(4) . . . . ? C23 C33 C43 C33 0.03(15) . . . 2 ? K1 C33 C43 C33 -109.3(6) . . . 2 ?