#------------------------------------------------------------------------------ #$Date: 2020-04-30 01:07:27 +0300 (Thu, 30 Apr 2020) $ #$Revision: 251292 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126456.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_7126456 loop_ _publ_author_name 'Vidal-Ferran, Anton' 'Iniesta, Ester' _publ_section_title ; Supramolecularly regulated copper-bisoxazoline catalysts for the efficient insertion of carbenoid species into hydroxyl bonds ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC00224K _journal_year 2020 _chemical_formula_sum 'C24 H44 Cu F12 N2 Na O9 P2' _chemical_formula_weight 881.08 _chemical_name_common '[Cu(NaPF6.L2)]PF6' _chemical_name_systematic EI200 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-03-04 deposited with the CCDC. 2020-04-29 downloaded from the CCDC. ; _cell_angle_alpha 64.708(2) _cell_angle_beta 87.283(2) _cell_angle_gamma 73.184(2) _cell_formula_units_Z 2 _cell_length_a 11.2430(9) _cell_length_b 12.5262(10) _cell_length_c 14.6345(10) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.16 _cell_measurement_theta_min 2.33 _cell_volume 1776.8(2) _computing_cell_refinement 'Bruker APEX3 v2015.9-0' _computing_data_collection 'Bruker APEX3 v2015.9-0' _computing_data_reduction 'Bruker SAINT V8.35A' _computing_molecular_graphics ; SHELXle: C.B. Huebschle, G.M. Sheldrick & B. Dittrich J.Appl.Cryst. (2011) 44, 1281-1284. ; _computing_publication_material 'XCIF, SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT V2014/4 (Sheldrick 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.946 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 16935 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.353 _diffrn_reflns_theta_min 1.545 _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_current 0.6 _diffrn_source_power 50 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_source_type 'Bruker APEX DUO' _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.647 _exptl_crystal_description PLATE _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.941 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 492 _refine_ls_number_reflns 8406 _refine_ls_number_restraints 111 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0500 _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^)+(0.0649P)^2^+1.0998P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1226 _refine_ls_wR_factor_ref 0.1377 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6247 _reflns_number_total 8406 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc00224k2.cif _cod_data_source_block mo_EI200_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. data item '_symmetry_cell_setting' value 'Triclinic' was changed to 'triclinic' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 7126456 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.852 _shelx_estimated_absorpt_t_max 0.960 _shelx_res_file ; mo_EI200_0m.res created by SHELXL-2014/7 TITL mo_EI200_0m in P-1 CELL 0.71073 11.24300 12.52620 14.63450 64.7084 87.2827 73.1842 ZERR 2.00 0.00090 0.00100 0.00100 0.0020 0.0022 0.0022 LATT 1 SFAC C H N O F NA P CU UNIT 48 88 4 18 24 2 4 2 ACTA CONF TEMP -173.150 SIZE 0.05 0.10 0.20 L.S. 20 BOND $H LIST 6 FMAP 2 PLAN 20 WGHT 0.064900 1.099800 FVAR 0.12732 0.66981 MOLE 1 CU1A 8 0.240305 0.689719 0.702586 11.00000 0.02326 0.03068 = 0.01801 -0.01173 0.00436 -0.01207 NA1A 6 0.182627 0.301780 0.782192 11.00000 0.02572 0.02386 = 0.01740 -0.00946 -0.00003 -0.00321 O1A 4 0.434172 0.758142 0.455528 11.00000 0.04900 0.05017 = 0.03645 -0.02813 0.02401 -0.02787 O2A 4 0.038330 0.613656 0.945933 11.00000 0.03067 0.03288 = 0.02634 -0.02044 0.01214 -0.01715 O3A 4 0.087911 0.541580 0.732437 11.00000 0.01916 0.03799 = 0.02383 -0.02036 0.00279 -0.00959 O4A 4 0.139878 0.433215 0.599114 11.00000 0.02430 0.01697 = 0.01864 -0.00804 0.00280 -0.00621 O5A 4 0.309509 0.203881 0.680176 11.00000 0.02708 0.01857 = 0.01546 -0.00643 -0.00016 -0.00564 O6A 4 0.266766 0.076059 0.877014 11.00000 0.02521 0.02599 = 0.01874 -0.00915 0.00017 -0.00144 O7A 4 0.168438 0.234034 0.965415 11.00000 0.02835 0.03144 = 0.02380 -0.01623 0.00137 -0.01146 O8A 4 0.359627 0.322522 0.868478 11.00000 0.02895 0.05699 = 0.02764 -0.00067 -0.00191 -0.01639 N1A 3 0.299001 0.754335 0.573308 11.00000 0.02838 0.03560 = 0.02136 -0.01573 0.00444 -0.01674 N2A 3 0.171040 0.661093 0.827474 11.00000 0.02495 0.02671 = 0.01858 -0.01192 0.00279 -0.01143 C1A 1 0.395952 0.697093 0.545518 11.00000 0.03084 0.03685 = 0.03421 -0.02435 0.01269 -0.02236 C2A 1 0.352823 0.884411 0.415468 11.00000 0.05145 0.05249 = 0.02559 -0.01618 0.01429 -0.02081 AFIX 23 H2AA 2 0.314918 0.910540 0.346698 11.00000 -1.20000 H2AB 2 0.399572 0.941780 0.412000 11.00000 -1.20000 AFIX 0 C3A 1 0.251460 0.882344 0.491122 11.00000 0.03710 0.03763 = 0.01793 -0.01158 0.00486 -0.01931 C4A 1 0.245104 0.974957 0.533800 11.00000 0.03987 0.03710 = 0.03102 -0.01346 0.00397 -0.01703 AFIX 137 H4AA 2 0.219360 1.058948 0.478843 11.00000 -1.50000 H4AB 2 0.327439 0.958486 0.565278 11.00000 -1.50000 H4AC 2 0.184413 0.967179 0.584811 11.00000 -1.50000 AFIX 0 C5A 1 0.124226 0.899780 0.445907 11.00000 0.04370 0.05137 = 0.02381 -0.01271 -0.00557 -0.01928 AFIX 137 H5AA 2 0.091656 0.984534 0.392987 11.00000 -1.50000 H5AB 2 0.066732 0.884728 0.499285 11.00000 -1.50000 H5AC 2 0.132380 0.841301 0.416341 11.00000 -1.50000 AFIX 0 C6A 1 0.194357 0.714211 0.897360 11.00000 0.03317 0.03236 = 0.02062 -0.01679 0.00821 -0.01940 C7A 1 0.332433 0.675268 0.928213 11.00000 0.03689 0.06829 = 0.03661 -0.03464 0.00898 -0.02721 AFIX 137 H7AA 2 0.345256 0.704760 0.978058 11.00000 -1.50000 H7AB 2 0.376086 0.710981 0.868324 11.00000 -1.50000 H7AC 2 0.365339 0.584853 0.958231 11.00000 -1.50000 AFIX 0 C8A 1 0.137278 0.853574 0.843447 11.00000 0.06623 0.03187 = 0.02996 -0.01409 0.00796 -0.02608 AFIX 137 H8AA 2 0.147161 0.890390 0.888669 11.00000 -1.50000 H8AB 2 0.048359 0.873272 0.824800 11.00000 -1.50000 H8AC 2 0.179469 0.887022 0.782069 11.00000 -1.50000 AFIX 0 C9A 1 0.122074 0.655724 0.987024 11.00000 0.02898 0.02784 = 0.02303 -0.01534 0.00393 -0.01309 AFIX 23 H9AA 2 0.179227 0.585399 1.044019 11.00000 -1.20000 H9AB 2 0.074306 0.717215 1.011081 11.00000 -1.20000 AFIX 0 rem O9A 4 0.412033 0.511615 0.684396 11.00000 0.02541 0.05388 = rem 0.08989 0.02726 0.01122 -0.00961 C10A 1 0.082730 0.614165 0.859357 11.00000 0.02198 0.02230 = 0.02060 -0.01186 0.00180 -0.00337 C11A 1 0.020176 0.557770 0.811962 11.00000 0.02450 0.03789 = 0.03303 -0.02486 0.01126 -0.01698 AFIX 23 H11A 2 0.015166 0.476742 0.863813 11.00000 -1.20000 H11B 2 -0.065817 0.612083 0.784867 11.00000 -1.20000 AFIX 0 C12A 1 0.011692 0.589729 0.639561 11.00000 0.02348 0.02306 = 0.02504 -0.01129 -0.00201 -0.00445 AFIX 23 H12A 2 -0.027961 0.679891 0.614875 11.00000 -1.20000 H12B 2 -0.054795 0.549261 0.650427 11.00000 -1.20000 AFIX 0 C13A 1 0.094760 0.563848 0.563785 11.00000 0.02684 0.01647 = 0.01963 -0.00506 -0.00251 -0.00613 AFIX 23 H13A 2 0.047496 0.602298 0.496506 11.00000 -1.20000 H13B 2 0.165291 0.598327 0.557235 11.00000 -1.20000 AFIX 0 C14A 1 0.233074 0.397228 0.539354 11.00000 0.02289 0.02420 = 0.01840 -0.00862 0.00148 -0.00658 AFIX 23 H14A 2 0.308710 0.419055 0.547001 11.00000 -1.20000 H14B 2 0.201540 0.440344 0.466784 11.00000 -1.20000 AFIX 0 C15A 1 0.263130 0.260856 0.575855 11.00000 0.02861 0.02506 = 0.01606 -0.01054 0.00029 -0.00492 AFIX 23 H15A 2 0.187398 0.239001 0.568518 11.00000 -1.20000 H15B 2 0.326818 0.232136 0.535656 11.00000 -1.20000 AFIX 0 C16A 1 0.334163 0.073377 0.723218 11.00000 0.03316 0.01973 = 0.02214 -0.01020 0.00165 -0.00237 AFIX 23 H16A 2 0.402802 0.037138 0.690433 11.00000 -1.20000 H16B 2 0.258991 0.052684 0.712503 11.00000 -1.20000 AFIX 0 C17A 1 0.369957 0.022173 0.834206 11.00000 0.02896 0.02233 = 0.02410 -0.00878 0.00270 -0.00124 AFIX 23 H17A 2 0.388952 -0.068979 0.866285 11.00000 -1.20000 H17B 2 0.444820 0.043114 0.845235 11.00000 -1.20000 AFIX 0 C18A 1 0.283818 0.026802 0.984150 11.00000 0.03387 0.02731 = 0.01975 -0.00575 -0.00278 -0.00366 AFIX 23 H18A 2 0.365287 0.028748 1.005157 11.00000 -1.20000 H18B 2 0.281821 -0.060000 1.015695 11.00000 -1.20000 AFIX 0 C19A 1 0.178500 0.106109 1.016837 11.00000 0.03599 0.03169 = 0.01996 -0.01144 0.00410 -0.00994 AFIX 23 H19A 2 0.098971 0.093864 1.003784 11.00000 -1.20000 H19B 2 0.192159 0.078740 1.090769 11.00000 -1.20000 AFIX 0 C20A 1 0.238806 0.281064 1.009995 11.00000 0.04010 0.05200 = 0.03112 -0.02493 0.00094 -0.02070 AFIX 23 H20A 2 0.245654 0.233702 1.084684 11.00000 -1.20000 H20B 2 0.192681 0.368355 0.993341 11.00000 -1.20000 AFIX 0 C21A 1 0.366379 0.274657 0.975959 11.00000 0.03690 0.04598 = 0.03140 -0.00812 -0.00812 -0.01673 AFIX 23 H21A 2 0.403267 0.323456 0.998145 11.00000 -1.20000 H21B 2 0.420263 0.187760 1.006675 11.00000 -1.20000 AFIX 0 part 1 21.0000 SIMU 0.01 O9A > C23' DELU 0.01 O9A > C23' ISOR 0.005 O9A > C23' O9A 4 0.410290 0.505130 0.674263 21.00000 0.02649 0.04978 = 0.03712 0.00097 0.00389 -0.01569 C22A 1 0.479727 0.338361 0.841262 21.00000 0.02822 0.04319 = 0.03215 -0.01074 -0.00499 -0.01361 AFIX 23 H22A 2 0.546196 0.259868 0.878975 21.00000 -1.20000 H22B 2 0.493429 0.402551 0.858361 21.00000 -1.20000 AFIX 0 C23A 1 0.483105 0.376291 0.730526 21.00000 0.02589 0.04489 = 0.03839 -0.00856 -0.00150 -0.00809 AFIX 23 H23A 2 0.570539 0.365153 0.712849 21.00000 -1.20000 H23B 2 0.448946 0.323300 0.711562 21.00000 -1.20000 AFIX 0 same o9a > c23a part 2 -21.0000 O9' 4 0.416671 0.523454 0.706840 -21.00000 0.02748 0.02922 = 0.03556 -0.00729 0.00271 -0.00995 C22' 1 0.476906 0.310103 0.817666 -21.00000 0.02925 0.03474 = 0.03727 -0.01573 0.00399 -0.00994 AFIX 23 H22C 2 0.465499 0.300318 0.755306 -21.00000 -1.20000 H22D 2 0.545515 0.238994 0.863579 -21.00000 -1.20000 AFIX 0 C23' 1 0.501164 0.429318 0.793591 -21.00000 0.02859 0.03891 = 0.03773 -0.01114 -0.00066 -0.01349 AFIX 23 H23C 2 0.486694 0.449743 0.852282 -21.00000 -1.20000 H23D 2 0.588702 0.423737 0.777682 -21.00000 -1.20000 AFIX 0 part 0 C25A 1 0.472589 0.568241 0.603924 11.00000 0.03630 0.03939 = 0.06913 -0.02803 0.02433 -0.01999 AFIX 23 H25A 2 0.498829 0.528643 0.557453 11.00000 -1.20000 H25B 2 0.548626 0.567079 0.636251 11.00000 -1.20000 AFIX 0 MOLE 2 P1B 7 -0.121234 0.237571 0.780098 11.00000 0.02782 0.02803 = 0.01910 -0.00924 0.00001 -0.01173 F1B 5 -0.031020 0.309219 0.795097 11.00000 0.03282 0.04045 = 0.03766 -0.01928 0.00505 -0.02093 F2B 5 -0.053744 0.119649 0.880103 11.00000 0.06263 0.04854 = 0.05578 0.01726 -0.02640 -0.02754 F3B 5 -0.210255 0.166653 0.765332 11.00000 0.05638 0.05455 = 0.04652 -0.02332 -0.00283 -0.03292 F4B 5 -0.186815 0.354360 0.680035 11.00000 0.05016 0.05319 = 0.03781 0.01147 -0.01599 -0.02046 F5B 5 -0.218387 0.284092 0.846283 11.00000 0.04053 0.09516 = 0.06366 -0.06115 0.02438 -0.03595 F6B 5 -0.020440 0.190148 0.715268 11.00000 0.05011 0.09916 = 0.08565 -0.07527 0.02205 -0.02627 MOLE 3 P1C 7 0.637010 0.744230 0.723385 11.00000 0.02261 0.03078 = 0.02159 -0.01020 -0.00005 -0.00285 F1C 5 0.524696 0.686740 0.737498 11.00000 0.03170 0.06955 = 0.03595 -0.02078 0.00496 -0.02295 F2C 5 0.569465 0.853504 0.617126 11.00000 0.03988 0.05402 = 0.02926 -0.00176 -0.00911 -0.00013 F3C 5 0.750242 0.801534 0.709390 11.00000 0.04115 0.03783 = 0.04677 -0.00963 -0.00398 -0.01788 F4C 5 0.705068 0.634947 0.829295 11.00000 0.03558 0.02836 = 0.02506 -0.00924 -0.00402 -0.00410 F5C 5 0.567715 0.824875 0.781126 11.00000 0.05110 0.04297 = 0.04630 -0.02557 -0.00365 0.01154 F6C 5 0.706909 0.663392 0.666348 11.00000 0.03956 0.05326 = 0.03393 -0.02826 0.00698 -0.01028 HKLF 4 REM mo_EI200_0m in P-1 REM R1 = 0.0500 for 6247 Fo > 4sig(Fo) and 0.0736 for all 8406 data REM 492 parameters refined using 111 restraints END WGHT 0.0649 1.0998 REM Highest difference peak 0.941, deepest hole -0.804, 1-sigma level 0.098 Q1 1 0.3095 0.7075 0.6765 11.00000 0.05 0.94 Q2 1 0.1752 0.6636 0.7263 11.00000 0.05 0.92 Q3 1 0.3162 0.6531 0.6929 11.00000 0.05 0.68 Q4 1 0.7032 0.7763 0.7129 11.00000 0.05 0.58 Q5 1 0.2931 0.2036 1.0434 11.00000 0.05 0.53 Q6 1 0.2828 0.3406 0.9773 11.00000 0.05 0.53 Q7 1 0.5671 0.7267 0.7413 11.00000 0.05 0.52 Q8 1 0.3434 0.7345 0.5659 11.00000 0.05 0.49 Q9 1 0.4225 0.4598 0.6480 11.00000 0.05 0.49 Q10 1 0.1947 0.7297 0.6494 11.00000 0.05 0.47 Q11 1 -0.0555 0.1369 0.7596 11.00000 0.05 0.47 Q12 1 0.2760 0.5659 0.7501 11.00000 0.05 0.47 Q13 1 -0.0752 0.1199 0.8243 11.00000 0.05 0.45 Q14 1 0.8144 0.8185 0.6943 11.00000 0.05 0.42 Q15 1 -0.1217 0.1642 0.8999 11.00000 0.05 0.42 Q16 1 0.0548 0.3096 0.7806 11.00000 0.05 0.42 Q17 1 0.2058 0.8168 0.6537 11.00000 0.05 0.41 Q18 1 0.2980 0.9034 0.4481 11.00000 0.05 0.41 Q19 1 0.1778 0.9925 0.5469 11.00000 0.05 0.40 Q20 1 0.1603 0.6858 0.9419 11.00000 0.05 0.40 ; _shelx_res_checksum 7635 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1A Cu 0.24030(3) 0.68972(3) 0.70259(3) 0.02269(11) Uani 1 1 d . . . . . Na1A Na 0.18263(10) 0.30178(11) 0.78219(8) 0.0230(2) Uani 1 1 d . . . . . O1A O 0.4342(2) 0.7581(2) 0.45553(18) 0.0394(6) Uani 1 1 d . . . . . O2A O 0.03833(18) 0.6137(2) 0.94593(15) 0.0257(4) Uani 1 1 d . . . . . O3A O 0.08791(17) 0.5416(2) 0.73244(15) 0.0242(4) Uani 1 1 d . . . . . O4A O 0.13988(17) 0.43322(17) 0.59911(14) 0.0199(4) Uani 1 1 d . . . . . O5A O 0.30951(17) 0.20388(18) 0.68018(14) 0.0209(4) Uani 1 1 d . . . . . O6A O 0.26677(18) 0.07606(19) 0.87701(14) 0.0249(4) Uani 1 1 d . . . . . O7A O 0.16844(18) 0.2340(2) 0.96542(15) 0.0257(4) Uani 1 1 d . . . . . O8A O 0.3596(2) 0.3225(3) 0.86848(17) 0.0433(6) Uani 1 1 d . . . . . N1A N 0.2990(2) 0.7543(2) 0.57331(18) 0.0256(5) Uani 1 1 d . . . . . N2A N 0.1710(2) 0.6611(2) 0.82747(17) 0.0218(5) Uani 1 1 d . . . . . C1A C 0.3960(3) 0.6971(3) 0.5455(2) 0.0282(7) Uani 1 1 d . . . . . C2A C 0.3528(3) 0.8844(4) 0.4155(3) 0.0426(9) Uani 1 1 d . . . . . H2AA H 0.3149 0.9105 0.3467 0.051 Uiso 1 1 calc R U . . . H2AB H 0.3996 0.9418 0.4120 0.051 Uiso 1 1 calc R U . . . C3A C 0.2515(3) 0.8823(3) 0.4911(2) 0.0292(7) Uani 1 1 d . . . . . C4A C 0.2451(3) 0.9750(3) 0.5338(3) 0.0352(7) Uani 1 1 d . . . . . H4AA H 0.2194 1.0589 0.4788 0.053 Uiso 1 1 calc R U . . . H4AB H 0.3274 0.9585 0.5653 0.053 Uiso 1 1 calc R U . . . H4AC H 0.1844 0.9672 0.5848 0.053 Uiso 1 1 calc R U . . . C5A C 0.1242(3) 0.8998(4) 0.4459(2) 0.0394(8) Uani 1 1 d . . . . . H5AA H 0.0917 0.9845 0.3930 0.059 Uiso 1 1 calc R U . . . H5AB H 0.0667 0.8847 0.4993 0.059 Uiso 1 1 calc R U . . . H5AC H 0.1324 0.8413 0.4163 0.059 Uiso 1 1 calc R U . . . C6A C 0.1944(3) 0.7142(3) 0.8974(2) 0.0247(6) Uani 1 1 d . . . . . C7A C 0.3324(3) 0.6753(4) 0.9282(3) 0.0404(9) Uani 1 1 d . . . . . H7AA H 0.3453 0.7048 0.9781 0.061 Uiso 1 1 calc R U . . . H7AB H 0.3761 0.7110 0.8683 0.061 Uiso 1 1 calc R U . . . H7AC H 0.3653 0.5849 0.9582 0.061 Uiso 1 1 calc R U . . . C8A C 0.1373(4) 0.8536(3) 0.8434(3) 0.0399(8) Uani 1 1 d . . . . . H8AA H 0.1472 0.8904 0.8887 0.060 Uiso 1 1 calc R U . . . H8AB H 0.0484 0.8733 0.8248 0.060 Uiso 1 1 calc R U . . . H8AC H 0.1795 0.8870 0.7821 0.060 Uiso 1 1 calc R U . . . C9A C 0.1221(3) 0.6557(3) 0.9870(2) 0.0240(6) Uani 1 1 d . . . . . H9AA H 0.1792 0.5854 1.0440 0.029 Uiso 1 1 calc R U . . . H9AB H 0.0743 0.7172 1.0111 0.029 Uiso 1 1 calc R U . . . C10A C 0.0827(2) 0.6142(3) 0.8594(2) 0.0214(6) Uani 1 1 d . . . . . C11A C 0.0202(3) 0.5578(3) 0.8120(2) 0.0268(6) Uani 1 1 d . . . . . H11A H 0.0152 0.4767 0.8638 0.032 Uiso 1 1 calc R U . . . H11B H -0.0658 0.6121 0.7849 0.032 Uiso 1 1 calc R U . . . C12A C 0.0117(3) 0.5897(3) 0.6396(2) 0.0240(6) Uani 1 1 d . . . . . H12A H -0.0280 0.6799 0.6149 0.029 Uiso 1 1 calc R U . . . H12B H -0.0548 0.5493 0.6504 0.029 Uiso 1 1 calc R U . . . C13A C 0.0948(3) 0.5638(2) 0.5638(2) 0.0219(6) Uani 1 1 d . . . . . H13A H 0.0475 0.6023 0.4965 0.026 Uiso 1 1 calc R U . . . H13B H 0.1653 0.5983 0.5572 0.026 Uiso 1 1 calc R U . . . C14A C 0.2331(2) 0.3972(3) 0.5394(2) 0.0221(6) Uani 1 1 d . . . . . H14A H 0.3087 0.4191 0.5470 0.027 Uiso 1 1 calc R U . . . H14B H 0.2015 0.4403 0.4668 0.027 Uiso 1 1 calc R U . . . C15A C 0.2631(3) 0.2609(3) 0.5759(2) 0.0233(6) Uani 1 1 d . . . . . H15A H 0.1874 0.2390 0.5685 0.028 Uiso 1 1 calc R U . . . H15B H 0.3268 0.2321 0.5357 0.028 Uiso 1 1 calc R U . . . C16A C 0.3342(3) 0.0734(3) 0.7232(2) 0.0259(6) Uani 1 1 d . . . . . H16A H 0.4028 0.0371 0.6904 0.031 Uiso 1 1 calc R U . . . H16B H 0.2590 0.0527 0.7125 0.031 Uiso 1 1 calc R U . . . C17A C 0.3700(3) 0.0222(3) 0.8342(2) 0.0271(6) Uani 1 1 d . . . . . H17A H 0.3890 -0.0690 0.8663 0.033 Uiso 1 1 calc R U . . . H17B H 0.4448 0.0431 0.8452 0.033 Uiso 1 1 calc R U . . . C18A C 0.2838(3) 0.0268(3) 0.9842(2) 0.0297(7) Uani 1 1 d . . . . . H18A H 0.3653 0.0287 1.0052 0.036 Uiso 1 1 calc R U . . . H18B H 0.2818 -0.0600 1.0157 0.036 Uiso 1 1 calc R U . . . C19A C 0.1785(3) 0.1061(3) 1.0168(2) 0.0292(7) Uani 1 1 d . . . . . H19A H 0.0990 0.0939 1.0038 0.035 Uiso 1 1 calc R U . . . H19B H 0.1922 0.0787 1.0908 0.035 Uiso 1 1 calc R U . . . C20A C 0.2388(3) 0.2811(4) 1.0100(3) 0.0368(8) Uani 1 1 d . . . . . H20A H 0.2457 0.2337 1.0847 0.044 Uiso 1 1 calc R U . . . H20B H 0.1927 0.3684 0.9933 0.044 Uiso 1 1 calc R U . . . C21A C 0.3664(3) 0.2747(4) 0.9760(3) 0.0398(8) Uani 1 1 d . . . . . H21A H 0.4033 0.3235 0.9981 0.048 Uiso 1 1 calc R U . . . H21B H 0.4203 0.1878 1.0067 0.048 Uiso 1 1 calc R U . . . O9A O 0.4103(5) 0.5051(5) 0.6743(4) 0.0441(13) Uani 0.670(7) 1 d D U P A 1 C22A C 0.4797(6) 0.3384(6) 0.8413(4) 0.0356(14) Uani 0.670(7) 1 d D U P A 1 H22A H 0.5462 0.2599 0.8790 0.043 Uiso 0.670(7) 1 calc R U P A 1 H22B H 0.4934 0.4026 0.8584 0.043 Uiso 0.670(7) 1 calc R U P A 1 C23A C 0.4831(4) 0.3763(5) 0.7305(4) 0.0403(13) Uani 0.670(7) 1 d D U P A 1 H23A H 0.5705 0.3652 0.7128 0.048 Uiso 0.670(7) 1 calc R U P A 1 H23B H 0.4489 0.3233 0.7116 0.048 Uiso 0.670(7) 1 calc R U P A 1 O9' O 0.4167(10) 0.5235(8) 0.7068(7) 0.033(2) Uani 0.330(7) 1 d D U P A 2 C22' C 0.4769(13) 0.3101(10) 0.8177(10) 0.034(2) Uani 0.330(7) 1 d D U P A 2 H22C H 0.4655 0.3003 0.7553 0.040 Uiso 0.330(7) 1 calc R U P A 2 H22D H 0.5455 0.2390 0.8636 0.040 Uiso 0.330(7) 1 calc R U P A 2 C23' C 0.5012(9) 0.4293(9) 0.7936(8) 0.036(2) Uani 0.330(7) 1 d D U P A 2 H23C H 0.4867 0.4497 0.8523 0.043 Uiso 0.330(7) 1 calc R U P A 2 H23D H 0.5887 0.4237 0.7777 0.043 Uiso 0.330(7) 1 calc R U P A 2 C25A C 0.4726(3) 0.5682(3) 0.6039(3) 0.0453(9) Uani 1 1 d . . . . . H25A H 0.4988 0.5286 0.5575 0.054 Uiso 1 1 calc R U . A 1 H25B H 0.5486 0.5671 0.6363 0.054 Uiso 1 1 calc R U . A 1 P1B P -0.12123(7) 0.23757(7) 0.78010(6) 0.02446(17) Uani 1 1 d . . . . . F1B F -0.03102(16) 0.30922(18) 0.79510(14) 0.0338(4) Uani 1 1 d . . . . . F2B F -0.0537(2) 0.1196(2) 0.88010(19) 0.0665(8) Uani 1 1 d . . . . . F3B F -0.2103(2) 0.1667(2) 0.76533(16) 0.0478(5) Uani 1 1 d . . . . . F4B F -0.1868(2) 0.3544(2) 0.68003(16) 0.0565(6) Uani 1 1 d . . . . . F5B F -0.21839(19) 0.2841(2) 0.84628(18) 0.0537(6) Uani 1 1 d . . . . . F6B F -0.0204(2) 0.1901(3) 0.7153(2) 0.0650(8) Uani 1 1 d . . . . . P1C P 0.63701(7) 0.74423(8) 0.72338(6) 0.02653(18) Uani 1 1 d . . . . . F1C F 0.52470(17) 0.6867(2) 0.73750(15) 0.0447(5) Uani 1 1 d . . . . . F2C F 0.56947(18) 0.8535(2) 0.61713(15) 0.0498(6) Uani 1 1 d . . . . . F3C F 0.75024(18) 0.80153(19) 0.70939(16) 0.0434(5) Uani 1 1 d . . . . . F4C F 0.70507(16) 0.63495(17) 0.82930(13) 0.0315(4) Uani 1 1 d . . . . . F5C F 0.5677(2) 0.8249(2) 0.78113(17) 0.0502(6) Uani 1 1 d . . . . . F6C F 0.70691(17) 0.6634(2) 0.66635(15) 0.0398(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 Cu1A 0.02326(17) 0.0307(2) 0.01801(17) -0.01173(15) 0.00436(12) -0.01207(14) Na1A 0.0257(5) 0.0239(6) 0.0174(5) -0.0095(5) 0.0000(4) -0.0032(4) O1A 0.0490(14) 0.0502(16) 0.0364(13) -0.0281(12) 0.0240(11) -0.0279(12) O2A 0.0307(10) 0.0329(12) 0.0263(10) -0.0204(10) 0.0121(8) -0.0171(9) O3A 0.0192(9) 0.0380(12) 0.0238(10) -0.0204(9) 0.0028(7) -0.0096(8) O4A 0.0243(9) 0.0170(10) 0.0186(9) -0.0080(8) 0.0028(7) -0.0062(7) O5A 0.0271(9) 0.0186(10) 0.0155(9) -0.0064(8) -0.0002(7) -0.0056(8) O6A 0.0252(9) 0.0260(11) 0.0187(9) -0.0091(9) 0.0002(8) -0.0014(8) O7A 0.0283(10) 0.0314(12) 0.0238(10) -0.0162(9) 0.0014(8) -0.0115(9) O8A 0.0289(11) 0.0570(17) 0.0276(12) -0.0007(11) -0.0019(9) -0.0164(11) N1A 0.0284(12) 0.0356(15) 0.0214(12) -0.0157(11) 0.0044(10) -0.0167(11) N2A 0.0249(11) 0.0267(13) 0.0186(11) -0.0119(10) 0.0028(9) -0.0114(10) C1A 0.0308(15) 0.0369(18) 0.0342(16) -0.0243(15) 0.0127(12) -0.0224(13) C2A 0.051(2) 0.052(2) 0.0256(16) -0.0162(16) 0.0143(15) -0.0208(18) C3A 0.0371(16) 0.0376(18) 0.0179(13) -0.0116(13) 0.0049(12) -0.0193(14) C4A 0.0399(17) 0.0371(19) 0.0310(16) -0.0135(15) 0.0040(13) -0.0170(15) C5A 0.0437(18) 0.051(2) 0.0238(15) -0.0127(16) -0.0056(14) -0.0193(16) C6A 0.0332(14) 0.0324(17) 0.0206(13) -0.0168(13) 0.0082(11) -0.0194(12) C7A 0.0369(17) 0.068(3) 0.0366(18) -0.0346(19) 0.0090(14) -0.0272(17) C8A 0.066(2) 0.0319(19) 0.0300(17) -0.0141(15) 0.0080(16) -0.0261(17) C9A 0.0290(14) 0.0278(16) 0.0230(13) -0.0153(12) 0.0039(11) -0.0131(12) C10A 0.0220(12) 0.0223(14) 0.0206(13) -0.0119(12) 0.0018(10) -0.0034(10) C11A 0.0245(13) 0.0379(18) 0.0330(16) -0.0249(15) 0.0113(12) -0.0170(12) C12A 0.0235(13) 0.0231(15) 0.0250(14) -0.0113(12) -0.0020(11) -0.0045(11) C13A 0.0268(13) 0.0165(13) 0.0196(13) -0.0051(11) -0.0025(10) -0.0061(11) C14A 0.0229(13) 0.0242(15) 0.0184(12) -0.0086(11) 0.0015(10) -0.0066(11) C15A 0.0286(14) 0.0251(15) 0.0161(12) -0.0105(11) 0.0003(10) -0.0049(11) C16A 0.0332(15) 0.0197(14) 0.0221(14) -0.0102(12) 0.0017(11) -0.0024(12) C17A 0.0290(14) 0.0223(15) 0.0241(14) -0.0088(12) 0.0027(11) -0.0012(11) C18A 0.0339(15) 0.0273(16) 0.0197(14) -0.0058(12) -0.0028(12) -0.0037(12) C19A 0.0360(16) 0.0317(17) 0.0200(13) -0.0114(13) 0.0041(12) -0.0099(13) C20A 0.0401(17) 0.052(2) 0.0311(17) -0.0249(17) 0.0009(14) -0.0207(16) C21A 0.0369(17) 0.046(2) 0.0314(17) -0.0081(16) -0.0081(14) -0.0167(15) O9A 0.0265(17) 0.050(2) 0.037(2) 0.0010(18) 0.0039(18) -0.0157(16) C22A 0.028(2) 0.043(3) 0.032(2) -0.011(2) -0.0050(19) -0.014(2) C23A 0.0259(19) 0.045(2) 0.038(2) -0.0086(19) -0.0015(17) -0.0081(17) O9' 0.027(3) 0.029(3) 0.036(3) -0.007(2) 0.003(3) -0.010(2) C22' 0.029(3) 0.035(3) 0.037(4) -0.016(3) 0.004(3) -0.010(3) C23' 0.029(3) 0.039(3) 0.038(3) -0.011(3) -0.001(3) -0.013(2) C25A 0.0363(18) 0.039(2) 0.069(3) -0.028(2) 0.0243(18) -0.0200(15) P1B 0.0278(4) 0.0280(4) 0.0191(3) -0.0092(3) 0.0000(3) -0.0117(3) F1B 0.0328(9) 0.0404(11) 0.0377(10) -0.0193(9) 0.0051(8) -0.0209(8) F2B 0.0626(14) 0.0485(14) 0.0558(15) 0.0173(12) -0.0264(12) -0.0275(12) F3B 0.0564(13) 0.0546(14) 0.0465(12) -0.0233(11) -0.0028(10) -0.0329(11) F4B 0.0502(12) 0.0532(14) 0.0378(12) 0.0115(10) -0.0160(10) -0.0205(10) F5B 0.0405(11) 0.0952(19) 0.0637(15) -0.0612(15) 0.0244(10) -0.0360(12) F6B 0.0501(13) 0.099(2) 0.0856(19) -0.0753(18) 0.0220(12) -0.0263(13) P1C 0.0226(3) 0.0308(4) 0.0216(4) -0.0102(3) -0.0001(3) -0.0028(3) F1C 0.0317(10) 0.0696(16) 0.0360(11) -0.0208(11) 0.0050(8) -0.0230(10) F2C 0.0399(11) 0.0540(14) 0.0293(10) -0.0018(10) -0.0091(8) -0.0001(10) F3C 0.0411(11) 0.0378(12) 0.0468(12) -0.0096(10) -0.0040(9) -0.0179(9) F4C 0.0356(9) 0.0284(10) 0.0251(9) -0.0092(8) -0.0040(7) -0.0041(7) F5C 0.0511(12) 0.0430(13) 0.0463(13) -0.0256(11) -0.0036(10) 0.0115(10) F6C 0.0396(10) 0.0533(13) 0.0339(10) -0.0283(10) 0.0070(8) -0.0103(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cu Cu 0.3201 1.2651 '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 N2A Cu1A N1A 167.56(11) . . ? N2A Cu1A O9' 114.6(2) . . ? N1A Cu1A O9' 75.9(2) . . ? F1B Na1A O4A 90.28(7) . . ? F1B Na1A O7A 78.87(7) . . ? O4A Na1A O7A 159.65(8) . . ? F1B Na1A O6A 95.95(8) . . ? O4A Na1A O6A 130.61(8) . . ? O7A Na1A O6A 68.26(7) . . ? F1B Na1A O5A 119.62(8) . . ? O4A Na1A O5A 67.19(7) . . ? O7A Na1A O5A 133.16(8) . . ? O6A Na1A O5A 67.30(7) . . ? F1B Na1A O8A 141.13(9) . . ? O4A Na1A O8A 115.62(8) . . ? O7A Na1A O8A 67.04(7) . . ? O6A Na1A O8A 88.53(8) . . ? O5A Na1A O8A 97.75(8) . . ? F1B Na1A O3A 82.07(7) . . ? O4A Na1A O3A 65.64(7) . . ? O7A Na1A O3A 95.58(7) . . ? O6A Na1A O3A 163.74(8) . . ? O5A Na1A O3A 127.62(8) . . ? O8A Na1A O3A 83.19(8) . . ? C1A O1A C2A 106.4(2) . . ? C10A O2A C9A 105.9(2) . . ? C11A O3A C12A 113.4(2) . . ? C11A O3A Na1A 109.38(18) . . ? C12A O3A Na1A 104.45(16) . . ? C13A O4A C14A 112.3(2) . . ? C13A O4A Na1A 119.04(15) . . ? C14A O4A Na1A 114.38(15) . . ? C16A O5A C15A 111.6(2) . . ? C16A O5A Na1A 113.86(16) . . ? C15A O5A Na1A 113.66(15) . . ? C18A O6A C17A 113.1(2) . . ? C18A O6A Na1A 117.33(18) . . ? C17A O6A Na1A 113.69(17) . . ? C19A O7A C20A 117.4(2) . . ? C19A O7A Na1A 111.98(16) . . ? C20A O7A Na1A 114.13(18) . . ? C21A O8A C22A 105.3(3) . . ? C21A O8A C22' 119.1(6) . . ? C21A O8A Na1A 117.17(19) . . ? C22A O8A Na1A 134.6(3) . . ? C22' O8A Na1A 113.4(5) . . ? C1A N1A C3A 108.1(2) . . ? C1A N1A Cu1A 124.4(2) . . ? C3A N1A Cu1A 127.25(19) . . ? C10A N2A C6A 107.6(2) . . ? C10A N2A Cu1A 127.1(2) . . ? C6A N2A Cu1A 124.32(18) . . ? N1A C1A O1A 118.2(3) . . ? N1A C1A C25A 126.2(3) . . ? O1A C1A C25A 115.6(3) . . ? O1A C2A C3A 104.9(3) . . ? O1A C2A H2AA 110.8 . . ? C3A C2A H2AA 110.8 . . ? O1A C2A H2AB 110.8 . . ? C3A C2A H2AB 110.8 . . ? H2AA C2A H2AB 108.9 . . ? N1A C3A C4A 109.5(2) . . ? N1A C3A C5A 109.2(3) . . ? C4A C3A C5A 111.6(3) . . ? N1A C3A C2A 102.0(3) . . ? C4A C3A C2A 111.6(3) . . ? C5A C3A C2A 112.5(3) . . ? C3A C4A H4AA 109.5 . . ? C3A C4A H4AB 109.5 . . ? H4AA C4A H4AB 109.5 . . ? C3A C4A H4AC 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C3A C5A H5AA 109.5 . . ? C3A C5A H5AB 109.5 . . ? H5AA C5A H5AB 109.5 . . ? C3A C5A H5AC 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? N2A C6A C7A 110.6(2) . . ? N2A C6A C8A 107.6(2) . . ? C7A C6A C8A 113.1(3) . . ? N2A C6A C9A 101.5(2) . . ? C7A C6A C9A 111.8(3) . . ? C8A C6A C9A 111.5(3) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C6A C8A H8AA 109.5 . . ? C6A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C6A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? O2A C9A C6A 104.0(2) . . ? O2A C9A H9AA 110.9 . . ? C6A C9A H9AA 110.9 . . ? O2A C9A H9AB 110.9 . . ? C6A C9A H9AB 110.9 . . ? H9AA C9A H9AB 109.0 . . ? N2A C10A O2A 117.6(3) . . ? N2A C10A C11A 127.9(3) . . ? O2A C10A C11A 114.4(2) . . ? O3A C11A C10A 110.1(2) . . ? O3A C11A H11A 109.6 . . ? C10A C11A H11A 109.6 . . ? O3A C11A H11B 109.6 . . ? C10A C11A H11B 109.6 . . ? H11A C11A H11B 108.2 . . ? O3A C12A C13A 107.4(2) . . ? O3A C12A H12A 110.2 . . ? C13A C12A H12A 110.2 . . ? O3A C12A H12B 110.2 . . ? C13A C12A H12B 110.2 . . ? H12A C12A H12B 108.5 . . ? O4A C13A C12A 107.5(2) . . ? O4A C13A H13A 110.2 . . ? C12A C13A H13A 110.2 . . ? O4A C13A H13B 110.2 . . ? C12A C13A H13B 110.2 . . ? H13A C13A H13B 108.5 . . ? O4A C14A C15A 107.6(2) . . ? O4A C14A H14A 110.2 . . ? C15A C14A H14A 110.2 . . ? O4A C14A H14B 110.2 . . ? C15A C14A H14B 110.2 . . ? H14A C14A H14B 108.5 . . ? O5A C15A C14A 107.6(2) . . ? O5A C15A H15A 110.2 . . ? C14A C15A H15A 110.2 . . ? O5A C15A H15B 110.2 . . ? C14A C15A H15B 110.2 . . ? H15A C15A H15B 108.5 . . ? O5A C16A C17A 108.3(2) . . ? O5A C16A H16A 110.0 . . ? C17A C16A H16A 110.0 . . ? O5A C16A H16B 110.0 . . ? C17A C16A H16B 110.0 . . ? H16A C16A H16B 108.4 . . ? O6A C17A C16A 107.2(2) . . ? O6A C17A H17A 110.3 . . ? C16A C17A H17A 110.3 . . ? O6A C17A H17B 110.3 . . ? C16A C17A H17B 110.3 . . ? H17A C17A H17B 108.5 . . ? O6A C18A C19A 107.1(2) . . ? O6A C18A H18A 110.3 . . ? C19A C18A H18A 110.3 . . ? O6A C18A H18B 110.3 . . ? C19A C18A H18B 110.3 . . ? H18A C18A H18B 108.5 . . ? O7A C19A C18A 112.8(3) . . ? O7A C19A H19A 109.0 . . ? C18A C19A H19A 109.0 . . ? O7A C19A H19B 109.0 . . ? C18A C19A H19B 109.0 . . ? H19A C19A H19B 107.8 . . ? O7A C20A C21A 114.0(3) . . ? O7A C20A H20A 108.7 . . ? C21A C20A H20A 108.7 . . ? O7A C20A H20B 108.7 . . ? C21A C20A H20B 108.7 . . ? H20A C20A H20B 107.6 . . ? O8A C21A C20A 109.3(3) . . ? O8A C21A H21A 109.8 . . ? C20A C21A H21A 109.8 . . ? O8A C21A H21B 109.8 . . ? C20A C21A H21B 109.8 . . ? H21A C21A H21B 108.3 . . ? C25A O9A C23A 111.9(4) . . ? O8A C22A C23A 108.0(4) . . ? O8A C22A H22A 110.1 . . ? C23A C22A H22A 110.1 . . ? O8A C22A H22B 110.1 . . ? C23A C22A H22B 110.1 . . ? H22A C22A H22B 108.4 . . ? O9A C23A C22A 110.4(5) . . ? O9A C23A H23A 109.6 . . ? C22A C23A H23A 109.6 . . ? O9A C23A H23B 109.6 . . ? C22A C23A H23B 109.6 . . ? H23A C23A H23B 108.1 . . ? C23' O9' C25A 116.8(8) . . ? C23' O9' Cu1A 127.8(8) . . ? C25A O9' Cu1A 108.0(5) . . ? O8A C22' C23' 102.2(9) . . ? O8A C22' H22C 111.3 . . ? C23' C22' H22C 111.3 . . ? O8A C22' H22D 111.3 . . ? C23' C22' H22D 111.3 . . ? H22C C22' H22D 109.2 . . ? O9' C23' C22' 107.4(9) . . ? O9' C23' H23C 110.2 . . ? C22' C23' H23C 110.2 . . ? O9' C23' H23D 110.2 . . ? C22' C23' H23D 110.2 . . ? H23C C23' H23D 108.5 . . ? O9A C25A C1A 111.1(3) . . ? C1A C25A O9' 105.3(4) . . ? O9A C25A H25A 109.4 . . ? C1A C25A H25A 109.4 . . ? O9A C25A H25B 109.4 . . ? C1A C25A H25B 109.4 . . ? H25A C25A H25B 108.0 . . ? F4B P1B F5B 91.49(14) . . ? F4B P1B F2B 179.29(16) . . ? F5B P1B F2B 89.20(15) . . ? F4B P1B F6B 89.45(15) . . ? F5B P1B F6B 178.54(13) . . ? F2B P1B F6B 89.86(16) . . ? F4B P1B F3B 89.58(12) . . ? F5B P1B F3B 89.50(12) . . ? F2B P1B F3B 90.62(13) . . ? F6B P1B F3B 91.64(13) . . ? F4B P1B F1B 90.47(12) . . ? F5B P1B F1B 90.53(11) . . ? F2B P1B F1B 89.33(12) . . ? F6B P1B F1B 88.33(12) . . ? F3B P1B F1B 179.94(17) . . ? P1B F1B Na1A 137.85(11) . . ? F1C P1C F6C 90.10(12) . . ? F1C P1C F5C 90.11(13) . . ? F6C P1C F5C 179.61(11) . . ? F1C P1C F4C 90.06(11) . . ? F6C P1C F4C 89.92(10) . . ? F5C P1C F4C 89.75(10) . . ? F1C P1C F3C 179.80(15) . . ? F6C P1C F3C 89.79(12) . . ? F5C P1C F3C 90.01(13) . . ? F4C P1C F3C 89.78(11) . . ? F1C P1C F2C 90.11(12) . . ? F6C P1C F2C 89.88(12) . . ? F5C P1C F2C 90.45(12) . . ? F4C P1C F2C 179.74(12) . . ? F3C P1C F2C 90.06(12) . . ? 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 Cu1A N2A 1.882(2) . ? Cu1A N1A 1.885(2) . ? Cu1A O9' 2.405(10) . ? Na1A F1B 2.378(2) . ? Na1A O4A 2.453(2) . ? Na1A O7A 2.455(2) . ? Na1A O6A 2.457(2) . ? Na1A O5A 2.473(2) . ? Na1A O8A 2.538(3) . ? Na1A O3A 2.653(2) . ? O1A C1A 1.334(4) . ? O1A C2A 1.450(5) . ? O2A C10A 1.338(3) . ? O2A C9A 1.462(3) . ? O3A C11A 1.416(3) . ? O3A C12A 1.434(3) . ? O4A C13A 1.423(3) . ? O4A C14A 1.429(3) . ? O5A C16A 1.421(3) . ? O5A C15A 1.429(3) . ? O6A C18A 1.417(3) . ? O6A C17A 1.426(3) . ? O7A C19A 1.421(4) . ? O7A C20A 1.430(4) . ? O8A C21A 1.421(4) . ? O8A C22A 1.434(7) . ? O8A C22' 1.484(13) . ? N1A C1A 1.274(4) . ? N1A C3A 1.490(4) . ? N2A C10A 1.268(4) . ? N2A C6A 1.505(4) . ? C1A C25A 1.471(5) . ? C2A C3A 1.549(4) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.519(5) . ? C3A C5A 1.522(4) . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? C6A C7A 1.514(4) . ? C6A C8A 1.518(5) . ? C6A C9A 1.530(4) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C10A C11A 1.492(4) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C13A 1.497(4) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.490(4) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.495(4) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A C19A 1.513(4) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A C21A 1.487(5) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? O9A C25A 1.316(6) . ? O9A C23A 1.455(7) . ? C22A C23A 1.483(7) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? O9' C23' 1.446(11) . ? O9' C25A 1.540(11) . ? C22' C23' 1.485(13) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? P1B F4B 1.574(2) . ? P1B F5B 1.576(2) . ? P1B F2B 1.584(2) . ? P1B F6B 1.590(2) . ? P1B F3B 1.593(2) . ? P1B F1B 1.6120(19) . ? P1C F1C 1.591(2) . ? P1C F6C 1.594(2) . ? P1C F5C 1.598(2) . ? P1C F4C 1.5985(18) . ? P1C F3C 1.599(2) . ? P1C F2C 1.600(2) . ? 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 N2A Cu1A N1A C1A 146.0(4) . . . . ? O9' Cu1A N1A C1A -3.3(3) . . . . ? N2A Cu1A N1A C3A -26.8(6) . . . . ? O9' Cu1A N1A C3A -176.0(4) . . . . ? N1A Cu1A N2A C10A 121.0(5) . . . . ? O9' Cu1A N2A C10A -92.0(4) . . . . ? N1A Cu1A N2A C6A -45.9(6) . . . . ? O9' Cu1A N2A C6A 101.1(4) . . . . ? C3A N1A C1A O1A 0.5(4) . . . . ? Cu1A N1A C1A O1A -173.4(2) . . . . ? C3A N1A C1A C25A 179.9(3) . . . . ? Cu1A N1A C1A C25A 6.0(5) . . . . ? C2A O1A C1A N1A 4.2(4) . . . . ? C2A O1A C1A C25A -175.2(3) . . . . ? C1A O1A C2A C3A -6.7(3) . . . . ? C1A N1A C3A C4A -122.9(3) . . . . ? Cu1A N1A C3A C4A 50.8(3) . . . . ? C1A N1A C3A C5A 114.6(3) . . . . ? Cu1A N1A C3A C5A -71.7(3) . . . . ? C1A N1A C3A C2A -4.6(3) . . . . ? Cu1A N1A C3A C2A 169.1(2) . . . . ? O1A C2A C3A N1A 6.7(3) . . . . ? O1A C2A C3A C4A 123.5(3) . . . . ? O1A C2A C3A C5A -110.2(3) . . . . ? C10A N2A C6A C7A 132.7(3) . . . . ? Cu1A N2A C6A C7A -58.3(3) . . . . ? C10A N2A C6A C8A -103.4(3) . . . . ? Cu1A N2A C6A C8A 65.7(3) . . . . ? C10A N2A C6A C9A 13.8(3) . . . . ? Cu1A N2A C6A C9A -177.11(18) . . . . ? C10A O2A C9A C6A 15.9(3) . . . . ? N2A C6A C9A O2A -17.5(3) . . . . ? C7A C6A C9A O2A -135.5(3) . . . . ? C8A C6A C9A O2A 96.8(3) . . . . ? C6A N2A C10A O2A -4.4(3) . . . . ? Cu1A N2A C10A O2A -173.10(19) . . . . ? C6A N2A C10A C11A 175.6(3) . . . . ? Cu1A N2A C10A C11A 7.0(4) . . . . ? C9A O2A C10A N2A -7.8(3) . . . . ? C9A O2A C10A C11A 172.2(2) . . . . ? C12A O3A C11A C10A -130.0(3) . . . . ? Na1A O3A C11A C10A 113.9(2) . . . . ? N2A C10A C11A O3A 10.8(4) . . . . ? O2A C10A C11A O3A -169.1(2) . . . . ? C11A O3A C12A C13A -178.8(2) . . . . ? Na1A O3A C12A C13A -59.8(2) . . . . ? C14A O4A C13A C12A -172.4(2) . . . . ? Na1A O4A C13A C12A -34.8(3) . . . . ? O3A C12A C13A O4A 65.0(3) . . . . ? C13A O4A C14A C15A -173.9(2) . . . . ? Na1A O4A C14A C15A 46.4(2) . . . . ? C16A O5A C15A C14A 176.7(2) . . . . ? Na1A O5A C15A C14A 46.3(3) . . . . ? O4A C14A C15A O5A -60.6(3) . . . . ? C15A O5A C16A C17A -174.5(2) . . . . ? Na1A O5A C16A C17A -44.2(3) . . . . ? C18A O6A C17A C16A 174.6(3) . . . . ? Na1A O6A C17A C16A -48.3(3) . . . . ? O5A C16A C17A O6A 60.7(3) . . . . ? C17A O6A C18A C19A 170.8(3) . . . . ? Na1A O6A C18A C19A 35.4(3) . . . . ? C20A O7A C19A C18A -89.3(3) . . . . ? Na1A O7A C19A C18A 45.6(3) . . . . ? O6A C18A C19A O7A -53.6(3) . . . . ? C19A O7A C20A C21A 89.7(3) . . . . ? Na1A O7A C20A C21A -44.3(3) . . . . ? C22A O8A C21A C20A 167.6(4) . . . . ? C22' O8A C21A C20A -171.7(6) . . . . ? Na1A O8A C21A C20A -28.8(4) . . . . ? O7A C20A C21A O8A 48.0(4) . . . . ? C21A O8A C22A C23A 174.4(4) . . . . ? Na1A O8A C22A C23A 15.1(7) . . . . ? C25A O9A C23A C22A 130.8(6) . . . . ? O8A C22A C23A O9A 75.1(6) . . . . ? C21A O8A C22' C23' -93.6(8) . . . . ? Na1A O8A C22' C23' 122.2(7) . . . . ? C25A O9' C23' C22' -104.0(10) . . . . ? Cu1A O9' C23' C22' 110.0(10) . . . . ? O8A C22' C23' O9' -76.4(10) . . . . ? C23A O9A C25A C1A 178.0(4) . . . . ? N1A C1A C25A O9A 19.8(6) . . . . ? O1A C1A C25A O9A -160.9(4) . . . . ? N1A C1A C25A O9' -4.4(6) . . . . ? O1A C1A C25A O9' 174.9(5) . . . . ? C23' O9' C25A C1A -150.9(8) . . . . ? Cu1A O9' C25A C1A 1.4(6) . . . . ? F4B P1B F1B Na1A -108.37(18) . . . . ? F5B P1B F1B Na1A 160.14(18) . . . . ? F2B P1B F1B Na1A 70.95(19) . . . . ? F6B P1B F1B Na1A -18.94(19) . . . . ?