#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:00:07 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253809 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126455.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_7126455 loop_ _publ_author_name 'Iniesta, Ester' 'Vidal-Ferran, Anton' _publ_section_title ; Supramolecularly regulated copper-bisoxazoline catalysts for the efficient insertion of carbenoid species into hydroxyl bonds. ; _journal_issue 47 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 6364 _journal_page_last 6367 _journal_paper_doi 10.1039/d0cc00224k _journal_volume 56 _journal_year 2020 _chemical_formula_sum 'C44 H82 Cl0 Cu2 F24 N4 Na2 O15 P4' _chemical_formula_weight 1660.07 _chemical_name_common '[Cu(NaPF6.L1)]PF6' _chemical_name_systematic EI_0 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-03-04 deposited with the CCDC. 2020-04-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.9669(17) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.5906(5) _cell_length_b 25.0689(13) _cell_length_c 12.4435(6) _cell_measurement_reflns_used 9830 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.58 _cell_measurement_theta_min 2.46 _cell_volume 3299.3(3) _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 0.991 _diffrn_measured_fraction_theta_max 0.874 _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 0.0439 _diffrn_reflns_av_unetI/netI 0.0455 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.874 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 33599 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.874 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.191 _diffrn_reflns_theta_min 1.829 _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 0.885 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_correction_T_min 0.832 _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 colourless _exptl_crystal_density_diffrn 1.671 _exptl_crystal_description block _exptl_crystal_F_000 1700 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.909 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 526 _refine_ls_number_reflns 8553 _refine_ls_number_restraints 238 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0424 _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^)+(0.0346P)^2^+3.6348P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0976 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6703 _reflns_number_total 8553 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc00224k2.cif _cod_data_source_block mo_EI_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 'Monoclinic' was changed to 'monoclinic' 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 Adding full bibliography for 7126454--7126456.cif. ; _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 7126455 _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 0.917 _shelx_estimated_absorpt_t_max 0.957 _shelx_res_file ; mo_EI_0m.res created by SHELXL-2014/7 TITL mo_EI_0m in P2(1)/n CELL 0.71073 10.59060 25.06890 12.44350 90.0000 92.9669 90.0000 ZERR 2.00 0.00050 0.00130 0.00060 0.0000 0.0017 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H Cl N O F NA CU P UNIT 88 164 0 8 30 48 4 4 8 LIST 4 TEMP -173.160 SIZE 0.05 0.05 0.10 L.S. 16 BOND FMAP 2 PLAN 10 ACTA CONF WGHT 0.034600 3.634800 FVAR 0.09586 MOLE 1 CU1 8 0.463417 0.203427 0.561623 11.00000 0.01846 0.01387 = 0.01236 0.00130 -0.00126 0.00069 NA1 7 0.514471 0.122170 0.331233 11.00000 0.02006 0.01806 = 0.01528 0.00031 0.00348 0.00345 N1 4 0.516027 0.153417 0.665784 11.00000 0.01966 0.01488 = 0.01290 -0.00044 0.00073 -0.00041 N2 4 0.413274 0.260609 0.471949 11.00000 0.01760 0.01507 = 0.01495 0.00139 -0.00011 0.00074 O1 5 0.649675 0.097191 0.753066 11.00000 0.02333 0.01873 = 0.01443 0.00418 0.00135 0.00388 O2 5 0.675977 0.160686 0.497261 11.00000 0.01666 0.01960 = 0.01443 0.00065 0.00208 -0.00184 O3 5 0.729357 0.111500 0.295434 11.00000 0.01907 0.02979 = 0.01794 0.00009 0.00190 0.00936 O4 5 0.542606 0.053924 0.190207 11.00000 0.02950 0.02219 = 0.02074 -0.00024 0.00793 0.00223 O5 5 0.322255 0.093673 0.248141 11.00000 0.02621 0.02298 = 0.02016 -0.00777 -0.00064 0.00193 O6 5 0.314829 0.166186 0.406505 11.00000 0.01474 0.01574 = 0.01923 -0.00049 -0.00102 0.00243 O7 5 0.295654 0.305613 0.348003 11.00000 0.02178 0.01662 = 0.02116 0.00248 -0.00290 0.00395 C1 1 0.449046 0.139188 0.764979 11.00000 0.02133 0.01875 = 0.01037 -0.00002 0.00231 -0.00053 C2 1 0.539731 0.097451 0.817540 11.00000 0.03165 0.03004 = 0.02258 0.00967 0.00952 0.00818 AFIX 23 H2A 2 0.563610 0.107465 0.892827 11.00000 -1.20000 H2B 2 0.499491 0.061803 0.817227 11.00000 -1.20000 AFIX 0 C3 1 0.621239 0.128834 0.669256 11.00000 0.02048 0.01437 = 0.01254 -0.00115 -0.00235 -0.00241 C4 1 0.721111 0.131337 0.589265 11.00000 0.01723 0.02165 = 0.01478 0.00071 -0.00032 -0.00049 AFIX 23 H4A 2 0.797629 0.148772 0.622067 11.00000 -1.20000 H4B 2 0.744258 0.094769 0.567585 11.00000 -1.20000 AFIX 0 C5 1 0.776334 0.175979 0.430592 11.00000 0.01944 0.03595 = 0.01837 0.00746 -0.00097 -0.01164 AFIX 23 H5A 2 0.846040 0.191759 0.476194 11.00000 -1.20000 H5B 2 0.744974 0.203621 0.379029 11.00000 -1.20000 AFIX 0 C6 1 0.826441 0.129496 0.369202 11.00000 0.01580 0.05940 = 0.01684 0.00558 0.00384 0.00619 AFIX 23 H6A 2 0.901132 0.140623 0.330101 11.00000 -1.20000 H6B 2 0.852338 0.100414 0.419461 11.00000 -1.20000 AFIX 0 C7 1 0.758185 0.062357 0.242842 11.00000 0.03141 0.02563 = 0.02820 0.00705 0.01400 0.01559 AFIX 23 H7A 2 0.751625 0.032078 0.293323 11.00000 -1.20000 H7B 2 0.845355 0.063383 0.217768 11.00000 -1.20000 AFIX 0 C8 1 0.665494 0.055857 0.149629 11.00000 0.03754 0.01921 = 0.02575 -0.00123 0.01454 0.00543 AFIX 23 H8A 2 0.671860 0.086230 0.099350 11.00000 -1.20000 H8B 2 0.682941 0.022533 0.110366 11.00000 -1.20000 AFIX 0 C9 1 0.444068 0.060639 0.110067 11.00000 0.04557 0.02550 = 0.01729 -0.00862 0.00074 0.00444 AFIX 23 H9A 2 0.450333 0.033136 0.053498 11.00000 -1.20000 H9B 2 0.450303 0.096213 0.076204 11.00000 -1.20000 AFIX 0 C10 1 0.320766 0.055457 0.162947 11.00000 0.03874 0.02271 = 0.02236 -0.00887 -0.00600 0.00323 AFIX 23 H10A 2 0.249378 0.062608 0.110401 11.00000 -1.20000 H10B 2 0.311223 0.018969 0.191857 11.00000 -1.20000 AFIX 0 C11 1 0.204426 0.098596 0.296028 11.00000 0.01972 0.02389 = 0.03305 -0.00760 -0.00380 0.00316 AFIX 23 H11A 2 0.163498 0.063228 0.300766 11.00000 -1.20000 H11B 2 0.147613 0.122401 0.252319 11.00000 -1.20000 AFIX 0 C12 1 0.229452 0.121674 0.407199 11.00000 0.01947 0.01826 = 0.02892 0.00068 0.00311 -0.00120 AFIX 23 H12A 2 0.148494 0.133358 0.435892 11.00000 -1.20000 H12B 2 0.265832 0.093656 0.455573 11.00000 -1.20000 AFIX 0 C13 1 0.261649 0.211472 0.351866 11.00000 0.01551 0.01731 = 0.01539 -0.00098 -0.00137 0.00384 AFIX 23 H13A 2 0.170225 0.214088 0.364077 11.00000 -1.20000 H13B 2 0.272162 0.208352 0.273523 11.00000 -1.20000 AFIX 0 C14 1 0.329391 0.259783 0.395504 11.00000 0.01707 0.01708 = 0.01354 0.00031 0.00330 0.00201 C15 1 0.373799 0.346467 0.401903 11.00000 0.03700 0.01711 = 0.02974 0.00199 -0.00940 -0.00311 AFIX 23 H15A 2 0.320383 0.373135 0.436726 11.00000 -1.20000 H15B 2 0.426107 0.365004 0.349815 11.00000 -1.20000 AFIX 0 C16 1 0.458139 0.316649 0.486713 11.00000 0.01858 0.01320 = 0.01905 0.00027 -0.00084 0.00016 C17 1 0.320388 0.116107 0.733435 11.00000 0.02784 0.03468 = 0.02472 -0.00257 0.00438 -0.01194 AFIX 137 H17A 2 0.279918 0.103839 0.798049 11.00000 -1.50000 H17B 2 0.330190 0.085956 0.684435 11.00000 -1.50000 H17C 2 0.267740 0.143577 0.697394 11.00000 -1.50000 AFIX 0 C18 1 0.438783 0.189060 0.833978 11.00000 0.02783 0.02375 = 0.01803 -0.00555 0.00298 0.00022 AFIX 137 H18A 2 0.394602 0.180347 0.898996 11.00000 -1.50000 H18B 2 0.391444 0.216559 0.792977 11.00000 -1.50000 H18C 2 0.523701 0.202350 0.854337 11.00000 -1.50000 AFIX 0 C19 1 0.597072 0.319372 0.464499 11.00000 0.02466 0.02392 = 0.03182 0.00106 0.00491 -0.00441 AFIX 137 H19A 2 0.625821 0.356490 0.469448 11.00000 -1.50000 H19B 2 0.609775 0.305680 0.392085 11.00000 -1.50000 H19C 2 0.645631 0.297708 0.517573 11.00000 -1.50000 AFIX 0 C20 1 0.434319 0.334441 0.600887 11.00000 0.02717 0.02032 = 0.02187 -0.00325 0.00118 -0.00195 AFIX 137 H20A 2 0.460271 0.371738 0.610409 11.00000 -1.50000 H20B 2 0.483273 0.311994 0.652300 11.00000 -1.50000 H20C 2 0.344083 0.331044 0.613442 11.00000 -1.50000 AFIX 0 MOLE 2 P1A 9 0.547029 0.238430 0.139964 11.00000 0.01611 0.01768 = 0.01289 0.00295 0.00223 0.00178 F1A 6 0.501605 0.291345 0.197615 11.00000 0.04725 0.02716 = 0.02720 -0.00386 0.00951 0.01499 F2A 6 0.524274 0.204934 0.248689 11.00000 0.02851 0.03247 = 0.02103 0.01439 0.00223 0.00048 F3A 6 0.591950 0.185292 0.083044 11.00000 0.03620 0.02513 = 0.03046 -0.00803 -0.00293 0.00829 F4A 6 0.568304 0.271640 0.032767 11.00000 0.03653 0.03495 = 0.01901 0.01077 0.00869 0.00279 F5A 6 0.688612 0.249677 0.182910 11.00000 0.01707 0.03693 = 0.03076 -0.00023 -0.00080 -0.00518 F6A 6 0.404809 0.226468 0.099369 11.00000 0.01612 0.05053 = 0.02865 0.01050 -0.00420 -0.00112 MOLE 3 SIMU 0.01 P1B > F3B" DELU 0.01 P1B > F3B" P1B 9 0.500000 0.000000 0.500000 10.50000 0.01804 0.01012 = 0.01339 0.00085 0.00034 -0.00122 F1B 6 0.508496 0.062335 0.469168 11.00000 0.04423 0.01161 = 0.02501 0.00429 -0.00435 -0.00509 DFIX 1.60 0.01 P1B F2B P1B F3B P1B F2B' P1B F3B' DFIX 2.25 0.01 F1B F2B' F2B' F3B' F3B' F1B DFIX 1.60 0.01 P1B F2B" P1B F3B" DFIX 2.25 0.01 F1B F2B" F2B" F3B" F3B" F1B PART 1 10.55 F2B 6 0.356996 0.004420 0.529387 10.55000 0.02248 0.02745 = 0.05459 0.01019 0.01009 0.00326 F3B 6 0.544554 0.013478 0.620949 10.55000 0.06306 0.02407 = 0.01236 0.00032 -0.00473 -0.01513 PART 2 10.30 F2B' 6 0.597978 0.007567 0.597860 10.30000 0.04459 0.03697 = 0.01742 0.01353 -0.00917 -0.02365 F3B' 6 0.387127 0.015101 0.574178 10.30000 0.04529 0.04364 = 0.02675 0.00927 0.02295 0.02014 PART 3 10.15 F2B" 6 0.364491 -0.001682 0.437569 10.15000 0.01619 0.02040 = 0.04127 0.00739 -0.01155 -0.00107 F3B" 6 0.433545 0.018880 0.606909 10.15000 0.04680 0.02102 = 0.01952 -0.00635 0.01503 0.00000 MOLE 3 PART -1 10.50 SAME 0.005 P1A > F6A SIMU 0.01 P1C > F6C DELU 0.01 P1C > F6C P1C 9 0.492219 0.498002 0.479534 10.50000 0.01374 0.01260 = 0.02072 0.00131 0.00132 -0.00182 F1C 6 0.472884 0.530107 0.368480 10.50000 0.02369 0.03146 = 0.02302 0.01210 -0.00182 -0.00103 F2C 6 0.620728 0.530511 0.508070 10.50000 0.02312 0.03162 = 0.03519 0.00902 -0.00817 -0.01260 F3C 6 0.511436 0.465758 0.589934 10.50000 0.02864 0.03118 = 0.02416 0.01381 0.00051 -0.00012 F4C 6 0.365896 0.465718 0.449529 10.50000 0.03247 0.02812 = 0.04585 0.00807 -0.00814 -0.01659 F5C 6 0.413450 0.542418 0.538137 10.50000 0.04142 0.03698 = 0.02565 -0.00696 0.00069 0.02161 F6C 6 0.572715 0.453935 0.421159 10.50000 0.04500 0.03681 = 0.03379 -0.00780 0.00575 0.02151 MOLE 4 PART -1 10.50 DFIX 1.49 0.01 O1S C1S O1S C3S DFIX 1.52 0.01 C1S C2S C3S C4S DFIX 2.50 0.01 O1S C2S O1S C4S SIMU 0.01 O1S > C4S DELU 0.01 O1S > C4S O1S 5 0.489187 0.505158 0.031395 10.50000 0.02300 0.02998 = 0.02471 -0.00471 0.00305 0.01029 C1S 1 0.540117 0.457645 0.084347 10.50000 0.01773 0.03323 = 0.03064 -0.01382 -0.00914 0.00644 AFIX 23 H1SA 2 0.633624 0.459441 0.088820 10.50000 -1.20000 H1SB 2 0.514628 0.425723 0.041696 10.50000 -1.20000 AFIX 0 C2S 1 0.492385 0.452979 0.195464 10.50000 0.03546 0.03814 = 0.03037 -0.00694 0.00548 -0.00387 AFIX 137 H2SA 2 0.522543 0.419498 0.228349 10.50000 -1.50000 H2SB 2 0.399730 0.453294 0.191187 10.50000 -1.50000 H2SC 2 0.523723 0.483100 0.239398 10.50000 -1.50000 AFIX 0 C3S 1 0.529240 0.510206 -0.076507 10.50000 0.02359 0.03340 = 0.02877 -0.00875 0.00271 -0.00173 AFIX 23 H3SA 2 0.506063 0.477557 -0.117719 10.50000 -1.20000 H3SB 2 0.622337 0.514094 -0.075092 10.50000 -1.20000 AFIX 0 C4S 1 0.467013 0.558792 -0.131987 10.50000 0.03189 0.05984 = 0.02387 0.00103 -0.00222 0.00608 AFIX 137 H4SA 2 0.487127 0.559209 -0.207974 10.50000 -1.50000 H4SB 2 0.498957 0.591465 -0.096927 10.50000 -1.50000 H4SC 2 0.375152 0.556779 -0.126546 10.50000 -1.50000 AFIX 0 HKLF 4 REM mo_EI_0m in P2(1)/n REM R1 = 0.0424 for 6703 Fo > 4sig(Fo) and 0.0608 for all 8553 data REM 526 parameters refined using 238 restraints END WGHT 0.0346 3.6348 REM Highest difference peak 0.909, deepest hole -0.334, 1-sigma level 0.078 Q1 1 0.5798 0.2044 0.5629 11.00000 0.05 0.91 Q2 1 0.3464 0.2036 0.5622 11.00000 0.05 0.75 Q3 1 0.6988 0.2023 0.5564 11.00000 0.05 0.61 Q4 1 0.4817 0.5966 -0.1542 11.00000 0.05 0.49 Q5 1 0.4328 0.2412 0.1402 11.00000 0.05 0.42 Q6 1 0.7025 0.0586 0.1943 11.00000 0.05 0.37 Q7 1 0.4997 0.1182 0.7840 11.00000 0.05 0.36 Q8 1 0.7154 0.2973 0.0626 11.00000 0.05 0.34 Q9 1 0.6573 0.2322 0.1292 11.00000 0.05 0.34 Q10 1 0.4052 0.1480 0.6581 11.00000 0.05 0.33 ; _shelx_res_checksum 59663 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.46342(3) 0.20343(2) 0.56162(2) 0.01497(7) Uani 1 1 d . . . . . Na1 Na 0.51447(9) 0.12217(3) 0.33123(7) 0.01771(19) Uani 1 1 d . . . . . N1 N 0.51603(18) 0.15342(7) 0.66578(15) 0.0158(4) Uani 1 1 d . . . . . N2 N 0.41327(18) 0.26061(7) 0.47195(15) 0.0159(4) Uani 1 1 d . . . . . O1 O 0.64967(16) 0.09719(6) 0.75307(12) 0.0188(3) Uani 1 1 d . . . . . O2 O 0.67598(15) 0.16069(6) 0.49726(12) 0.0169(3) Uani 1 1 d . . . . . O3 O 0.72936(16) 0.11150(7) 0.29543(13) 0.0222(4) Uani 1 1 d . . . . . O4 O 0.54261(17) 0.05392(7) 0.19021(14) 0.0239(4) Uani 1 1 d . . . . . O5 O 0.32226(17) 0.09367(7) 0.24814(13) 0.0232(4) Uani 1 1 d . . . . . O6 O 0.31483(15) 0.16619(6) 0.40650(12) 0.0166(3) Uani 1 1 d . . . . . O7 O 0.29565(16) 0.30561(6) 0.34800(13) 0.0200(3) Uani 1 1 d . . . . . C1 C 0.4490(2) 0.13919(9) 0.76498(17) 0.0168(4) Uani 1 1 d . . . . . C2 C 0.5397(3) 0.09745(11) 0.8175(2) 0.0278(6) Uani 1 1 d . . . . . H2A H 0.5636 0.1075 0.8928 0.033 Uiso 1 1 calc R U . . . H2B H 0.4995 0.0618 0.8172 0.033 Uiso 1 1 calc R U . . . C3 C 0.6212(2) 0.12883(9) 0.66926(17) 0.0159(4) Uani 1 1 d . . . . . C4 C 0.7211(2) 0.13134(9) 0.58927(18) 0.0179(5) Uani 1 1 d . . . . . H4A H 0.7976 0.1488 0.6221 0.022 Uiso 1 1 calc R U . . . H4B H 0.7443 0.0948 0.5676 0.022 Uiso 1 1 calc R U . . . C5 C 0.7763(2) 0.17598(11) 0.4306(2) 0.0247(5) Uani 1 1 d . . . . . H5A H 0.8460 0.1918 0.4762 0.030 Uiso 1 1 calc R U . . . H5B H 0.7450 0.2036 0.3790 0.030 Uiso 1 1 calc R U . . . C6 C 0.8264(2) 0.12950(13) 0.3692(2) 0.0306(6) Uani 1 1 d . . . . . H6A H 0.9011 0.1406 0.3301 0.037 Uiso 1 1 calc R U . . . H6B H 0.8523 0.1004 0.4195 0.037 Uiso 1 1 calc R U . . . C7 C 0.7582(3) 0.06236(10) 0.2428(2) 0.0280(6) Uani 1 1 d . . . . . H7A H 0.7516 0.0321 0.2933 0.034 Uiso 1 1 calc R U . . . H7B H 0.8454 0.0634 0.2178 0.034 Uiso 1 1 calc R U . . . C8 C 0.6655(3) 0.05586(10) 0.1496(2) 0.0271(6) Uani 1 1 d . . . . . H8A H 0.6719 0.0862 0.0993 0.032 Uiso 1 1 calc R U . . . H8B H 0.6829 0.0225 0.1104 0.032 Uiso 1 1 calc R U . . . C9 C 0.4441(3) 0.06064(11) 0.1101(2) 0.0295(6) Uani 1 1 d . . . . . H9A H 0.4503 0.0331 0.0535 0.035 Uiso 1 1 calc R U . . . H9B H 0.4503 0.0962 0.0762 0.035 Uiso 1 1 calc R U . . . C10 C 0.3208(3) 0.05546(10) 0.1629(2) 0.0282(6) Uani 1 1 d . . . . . H10A H 0.2494 0.0626 0.1104 0.034 Uiso 1 1 calc R U . . . H10B H 0.3112 0.0190 0.1919 0.034 Uiso 1 1 calc R U . . . C11 C 0.2044(2) 0.09860(10) 0.2960(2) 0.0257(5) Uani 1 1 d . . . . . H11A H 0.1635 0.0632 0.3008 0.031 Uiso 1 1 calc R U . . . H11B H 0.1476 0.1224 0.2523 0.031 Uiso 1 1 calc R U . . . C12 C 0.2295(2) 0.12167(9) 0.4072(2) 0.0222(5) Uani 1 1 d . . . . . H12A H 0.1485 0.1334 0.4359 0.027 Uiso 1 1 calc R U . . . H12B H 0.2658 0.0937 0.4556 0.027 Uiso 1 1 calc R U . . . C13 C 0.2616(2) 0.21147(8) 0.35187(18) 0.0161(4) Uani 1 1 d . . . . . H13A H 0.1702 0.2141 0.3641 0.019 Uiso 1 1 calc R U . . . H13B H 0.2722 0.2084 0.2735 0.019 Uiso 1 1 calc R U . . . C14 C 0.3294(2) 0.25978(9) 0.39550(18) 0.0158(4) Uani 1 1 d . . . . . C15 C 0.3738(3) 0.34647(10) 0.4019(2) 0.0283(6) Uani 1 1 d . . . . . H15A H 0.3204 0.3731 0.4367 0.034 Uiso 1 1 calc R U . . . H15B H 0.4261 0.3650 0.3498 0.034 Uiso 1 1 calc R U . . . C16 C 0.4581(2) 0.31665(9) 0.48671(19) 0.0170(5) Uani 1 1 d . . . . . C17 C 0.3204(3) 0.11611(11) 0.7334(2) 0.0290(6) Uani 1 1 d . . . . . H17A H 0.2799 0.1038 0.7980 0.043 Uiso 1 1 calc R U . . . H17B H 0.3302 0.0860 0.6844 0.043 Uiso 1 1 calc R U . . . H17C H 0.2677 0.1436 0.6974 0.043 Uiso 1 1 calc R U . . . C18 C 0.4388(3) 0.18906(10) 0.83398(19) 0.0231(5) Uani 1 1 d . . . . . H18A H 0.3946 0.1803 0.8990 0.035 Uiso 1 1 calc R U . . . H18B H 0.3914 0.2166 0.7930 0.035 Uiso 1 1 calc R U . . . H18C H 0.5237 0.2023 0.8543 0.035 Uiso 1 1 calc R U . . . C19 C 0.5971(2) 0.31937(10) 0.4645(2) 0.0267(6) Uani 1 1 d . . . . . H19A H 0.6258 0.3565 0.4694 0.040 Uiso 1 1 calc R U . . . H19B H 0.6098 0.3057 0.3921 0.040 Uiso 1 1 calc R U . . . H19C H 0.6456 0.2977 0.5176 0.040 Uiso 1 1 calc R U . . . C20 C 0.4343(3) 0.33444(10) 0.60089(19) 0.0231(5) Uani 1 1 d . . . . . H20A H 0.4603 0.3717 0.6104 0.035 Uiso 1 1 calc R U . . . H20B H 0.4833 0.3120 0.6523 0.035 Uiso 1 1 calc R U . . . H20C H 0.3441 0.3310 0.6134 0.035 Uiso 1 1 calc R U . . . P1A P 0.54703(6) 0.23843(2) 0.13996(5) 0.01551(12) Uani 1 1 d D . . . . F1A F 0.50160(16) 0.29134(6) 0.19761(12) 0.0336(4) Uani 1 1 d D . . . . F2A F 0.52427(14) 0.20493(6) 0.24869(11) 0.0273(3) Uani 1 1 d D . . . . F3A F 0.59195(15) 0.18529(6) 0.08304(12) 0.0308(4) Uani 1 1 d D . . . . F4A F 0.56830(15) 0.27164(6) 0.03277(11) 0.0299(4) Uani 1 1 d D . . . . F5A F 0.68861(13) 0.24968(6) 0.18291(12) 0.0283(3) Uani 1 1 d D . . . . F6A F 0.40481(13) 0.22647(7) 0.09937(12) 0.0320(4) Uani 1 1 d D . . . . P1B P 0.5000 0.0000 0.5000 0.01386(16) Uani 1 2 d DS U P . . F1B F 0.50850(15) 0.06233(5) 0.46917(11) 0.0272(3) Uani 1 1 d D U . . . F2B F 0.3570(4) 0.00442(17) 0.5294(4) 0.0346(11) Uani 0.55 1 d D U P A 1 F3B F 0.5446(5) 0.01348(19) 0.6209(3) 0.0334(11) Uani 0.55 1 d D U P A 1 F2B' F 0.5980(7) 0.0076(4) 0.5979(6) 0.033(3) Uani 0.3 1 d D U P A 2 F3B' F 0.3871(7) 0.0151(4) 0.5742(7) 0.038(2) Uani 0.3 1 d D U P A 2 F2B" F 0.3645(9) -0.0017(5) 0.4376(11) 0.026(3) Uani 0.15 1 d D U P A 3 F3B" F 0.4335(14) 0.0189(5) 0.6069(7) 0.029(3) Uani 0.15 1 d D U P A 3 P1C P 0.4922(3) 0.49800(11) 0.47953(12) 0.0157(4) Uani 0.5 1 d D U P B -1 F1C F 0.4729(5) 0.53011(19) 0.3685(3) 0.0262(10) Uani 0.5 1 d D U P B -1 F2C F 0.6207(4) 0.5305(2) 0.5081(3) 0.0303(11) Uani 0.5 1 d D U P B -1 F3C F 0.5114(5) 0.46576(19) 0.5899(3) 0.0280(10) Uani 0.5 1 d D U P B -1 F4C F 0.3659(5) 0.4657(2) 0.4495(4) 0.0358(12) Uani 0.5 1 d D U P B -1 F5C F 0.4135(5) 0.5424(2) 0.5381(3) 0.0347(12) Uani 0.5 1 d D U P B -1 F6C F 0.5727(5) 0.4539(2) 0.4212(3) 0.0384(12) Uani 0.5 1 d D U P B -1 O1S O 0.4892(4) 0.50516(18) 0.0314(3) 0.0258(9) Uani 0.5 1 d D U P C -1 C1S C 0.5401(6) 0.4576(2) 0.0843(5) 0.0276(12) Uani 0.5 1 d D U P C -1 H1SA H 0.6336 0.4594 0.0888 0.033 Uiso 0.5 1 calc R U P C -1 H1SB H 0.5146 0.4257 0.0417 0.033 Uiso 0.5 1 calc R U P C -1 C2S C 0.4924(6) 0.4530(2) 0.1955(4) 0.0345(13) Uani 0.5 1 d D U P C -1 H2SA H 0.5225 0.4195 0.2283 0.052 Uiso 0.5 1 calc R U P C -1 H2SB H 0.3997 0.4533 0.1912 0.052 Uiso 0.5 1 calc R U P C -1 H2SC H 0.5237 0.4831 0.2394 0.052 Uiso 0.5 1 calc R U P C -1 C3S C 0.5292(6) 0.5102(3) -0.0765(4) 0.0285(14) Uani 0.5 1 d D U P C -1 H3SA H 0.5061 0.4776 -0.1177 0.034 Uiso 0.5 1 calc R U P C -1 H3SB H 0.6223 0.5141 -0.0751 0.034 Uiso 0.5 1 calc R U P C -1 C4S C 0.4670(7) 0.5588(3) -0.1320(5) 0.0387(16) Uani 0.5 1 d D U P C -1 H4SA H 0.4871 0.5592 -0.2080 0.058 Uiso 0.5 1 calc R U P C -1 H4SB H 0.4990 0.5915 -0.0969 0.058 Uiso 0.5 1 calc R U P C -1 H4SC H 0.3752 0.5568 -0.1265 0.058 Uiso 0.5 1 calc R U P C -1 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 0.01846(14) 0.01387(13) 0.01236(13) 0.00130(10) -0.00126(10) 0.00069(11) Na1 0.0201(5) 0.0181(4) 0.0153(4) 0.0003(3) 0.0035(4) 0.0035(4) N1 0.0197(10) 0.0149(9) 0.0129(9) -0.0004(7) 0.0007(7) -0.0004(7) N2 0.0176(10) 0.0151(9) 0.0150(9) 0.0014(7) -0.0001(8) 0.0007(7) O1 0.0233(9) 0.0187(8) 0.0144(8) 0.0042(6) 0.0013(7) 0.0039(7) O2 0.0167(8) 0.0196(8) 0.0144(8) 0.0006(6) 0.0021(6) -0.0018(6) O3 0.0191(9) 0.0298(9) 0.0179(8) 0.0001(7) 0.0019(7) 0.0094(7) O4 0.0295(10) 0.0222(8) 0.0207(9) -0.0002(7) 0.0079(7) 0.0022(7) O5 0.0262(10) 0.0230(8) 0.0202(9) -0.0078(7) -0.0006(7) 0.0019(7) O6 0.0147(8) 0.0157(7) 0.0192(8) -0.0005(6) -0.0010(6) 0.0024(6) O7 0.0218(9) 0.0166(8) 0.0212(8) 0.0025(6) -0.0029(7) 0.0040(6) C1 0.0213(12) 0.0188(11) 0.0104(10) 0.0000(8) 0.0023(9) -0.0005(9) C2 0.0317(15) 0.0300(13) 0.0226(13) 0.0097(11) 0.0095(11) 0.0082(11) C3 0.0205(12) 0.0144(10) 0.0125(10) -0.0012(8) -0.0024(9) -0.0024(8) C4 0.0172(11) 0.0217(11) 0.0148(11) 0.0007(9) -0.0003(9) -0.0005(9) C5 0.0194(12) 0.0359(14) 0.0184(12) 0.0075(10) -0.0010(10) -0.0116(11) C6 0.0158(12) 0.0594(19) 0.0168(12) 0.0056(12) 0.0038(10) 0.0062(12) C7 0.0314(15) 0.0256(12) 0.0282(14) 0.0071(11) 0.0140(11) 0.0156(11) C8 0.0375(16) 0.0192(11) 0.0257(13) -0.0012(10) 0.0145(11) 0.0054(11) C9 0.0456(17) 0.0255(13) 0.0173(12) -0.0086(10) 0.0007(11) 0.0044(12) C10 0.0387(16) 0.0227(12) 0.0224(13) -0.0089(10) -0.0060(11) 0.0032(11) C11 0.0197(13) 0.0239(12) 0.0331(14) -0.0076(11) -0.0038(11) 0.0032(10) C12 0.0195(12) 0.0183(11) 0.0289(13) 0.0007(10) 0.0031(10) -0.0012(9) C13 0.0155(11) 0.0173(11) 0.0154(11) -0.0010(8) -0.0014(9) 0.0038(8) C14 0.0171(11) 0.0171(10) 0.0135(10) 0.0003(8) 0.0033(9) 0.0020(8) C15 0.0370(16) 0.0171(11) 0.0297(14) 0.0020(10) -0.0094(12) -0.0031(10) C16 0.0186(12) 0.0132(10) 0.0190(11) 0.0003(8) -0.0008(9) 0.0002(8) C17 0.0278(14) 0.0347(14) 0.0247(13) -0.0026(11) 0.0044(11) -0.0119(11) C18 0.0278(13) 0.0238(12) 0.0180(12) -0.0056(9) 0.0030(10) 0.0002(10) C19 0.0247(14) 0.0239(12) 0.0318(14) 0.0011(11) 0.0049(11) -0.0044(10) C20 0.0272(13) 0.0203(11) 0.0219(12) -0.0032(9) 0.0012(10) -0.0019(10) P1A 0.0161(3) 0.0177(3) 0.0129(3) 0.0029(2) 0.0022(2) 0.0018(2) F1A 0.0473(10) 0.0272(8) 0.0272(8) -0.0039(6) 0.0095(7) 0.0150(7) F2A 0.0285(8) 0.0325(8) 0.0210(7) 0.0144(6) 0.0022(6) 0.0005(6) F3A 0.0362(9) 0.0251(8) 0.0305(8) -0.0080(6) -0.0029(7) 0.0083(7) F4A 0.0365(9) 0.0350(8) 0.0190(7) 0.0108(6) 0.0087(6) 0.0028(7) F5A 0.0171(7) 0.0369(8) 0.0308(8) -0.0002(7) -0.0008(6) -0.0052(6) F6A 0.0161(7) 0.0505(10) 0.0287(8) 0.0105(7) -0.0042(6) -0.0011(7) P1B 0.0180(4) 0.0101(3) 0.0134(4) 0.0008(3) 0.0003(3) -0.0012(3) F1B 0.0442(9) 0.0116(6) 0.0250(8) 0.0043(6) -0.0043(7) -0.0051(6) F2B 0.0225(17) 0.0275(19) 0.055(3) 0.010(2) 0.0101(18) 0.0033(13) F3B 0.063(3) 0.0241(16) 0.0124(16) 0.0003(13) -0.0047(18) -0.015(2) F2B' 0.045(5) 0.037(5) 0.017(4) 0.014(4) -0.009(4) -0.024(5) F3B' 0.045(5) 0.044(5) 0.027(4) 0.009(4) 0.023(4) 0.020(4) F2B" 0.016(5) 0.020(5) 0.041(7) 0.007(6) -0.012(5) -0.001(4) F3B" 0.047(7) 0.021(5) 0.020(5) -0.006(4) 0.015(5) 0.000(5) P1C 0.0137(8) 0.0126(6) 0.0207(13) 0.0013(10) 0.0013(11) -0.0018(5) F1C 0.024(2) 0.0315(19) 0.023(2) 0.0121(19) -0.002(2) -0.0010(14) F2C 0.0231(19) 0.032(2) 0.035(3) 0.009(2) -0.0082(19) -0.0126(15) F3C 0.029(2) 0.031(2) 0.024(2) 0.014(2) 0.001(2) -0.0001(15) F4C 0.032(2) 0.028(2) 0.046(3) 0.008(2) -0.008(2) -0.0166(16) F5C 0.041(2) 0.037(2) 0.026(3) -0.007(2) 0.001(2) 0.0216(17) F6C 0.045(3) 0.037(2) 0.034(3) -0.008(2) 0.006(2) 0.0215(18) O1S 0.023(2) 0.030(2) 0.025(3) -0.0047(19) 0.003(2) 0.0103(16) C1S 0.018(3) 0.033(3) 0.031(3) -0.014(2) -0.009(3) 0.006(2) C2S 0.035(3) 0.038(3) 0.030(3) -0.007(2) 0.005(3) -0.004(3) C3S 0.024(3) 0.033(3) 0.029(4) -0.009(2) 0.003(3) -0.002(2) C4S 0.032(3) 0.060(5) 0.024(4) 0.001(3) -0.002(3) 0.006(3) 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' Cl Cl 0.1484 0.1585 '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' Cu Cu 0.3201 1.2651 '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 N1 Cu1 N2 172.19(8) . . ? N1 Cu1 Na1 97.00(6) . . ? N2 Cu1 Na1 90.48(6) . . ? F1B Na1 F2A 157.55(7) . . ? F1B Na1 O5 94.25(7) . . ? F2A Na1 O5 97.75(7) . . ? F1B Na1 O3 97.59(7) . . ? F2A Na1 O3 87.25(6) . . ? O5 Na1 O3 134.94(7) . . ? F1B Na1 O4 95.04(6) . . ? F2A Na1 O4 107.09(6) . . ? O5 Na1 O4 67.13(6) . . ? O3 Na1 O4 68.61(6) . . ? F1B Na1 O6 87.33(6) . . ? F2A Na1 O6 80.56(6) . . ? O5 Na1 O6 65.49(6) . . ? O3 Na1 O6 157.94(7) . . ? O4 Na1 O6 132.61(7) . . ? F1B Na1 O2 73.14(5) . . ? F2A Na1 O2 88.77(6) . . ? O5 Na1 O2 156.59(6) . . ? O3 Na1 O2 67.52(6) . . ? O4 Na1 O2 132.24(6) . . ? O6 Na1 O2 93.74(5) . . ? F1B Na1 Cu1 76.15(4) . . ? F2A Na1 Cu1 81.82(4) . . ? O5 Na1 Cu1 111.25(5) . . ? O3 Na1 Cu1 113.78(5) . . ? O4 Na1 Cu1 171.01(5) . . ? O6 Na1 Cu1 46.48(4) . . ? O2 Na1 Cu1 47.27(4) . . ? C3 N1 C1 107.93(18) . . ? C3 N1 Cu1 125.32(16) . . ? C1 N1 Cu1 126.49(15) . . ? C14 N2 C16 108.32(18) . . ? C14 N2 Cu1 126.84(16) . . ? C16 N2 Cu1 124.60(15) . . ? C3 O1 C2 105.99(18) . . ? C4 O2 C5 112.06(18) . . ? C4 O2 Na1 125.83(13) . . ? C5 O2 Na1 96.24(12) . . ? C6 O3 C7 113.86(19) . . ? C6 O3 Na1 121.14(14) . . ? C7 O3 Na1 114.45(15) . . ? C9 O4 C8 113.64(19) . . ? C9 O4 Na1 107.77(14) . . ? C8 O4 Na1 111.95(14) . . ? C11 O5 C10 113.25(19) . . ? C11 O5 Na1 123.47(14) . . ? C10 O5 Na1 120.48(15) . . ? C13 O6 C12 112.86(17) . . ? C13 O6 Na1 118.35(13) . . ? C12 O6 Na1 101.31(13) . . ? C14 O7 C15 105.59(17) . . ? N1 C1 C17 109.61(18) . . ? N1 C1 C18 108.63(18) . . ? C17 C1 C18 111.7(2) . . ? N1 C1 C2 101.53(18) . . ? C17 C1 C2 112.5(2) . . ? C18 C1 C2 112.2(2) . . ? O1 C2 C1 105.61(18) . . ? N1 C3 O1 118.5(2) . . ? N1 C3 C4 127.4(2) . . ? O1 C3 C4 114.10(19) . . ? O2 C4 C3 109.79(18) . . ? O2 C5 C6 112.2(2) . . ? O3 C6 C5 108.2(2) . . ? O3 C7 C8 107.57(19) . . ? O4 C8 C7 107.8(2) . . ? O4 C9 C10 107.9(2) . . ? O5 C10 C9 106.9(2) . . ? O5 C11 C12 107.6(2) . . ? O6 C12 C11 111.9(2) . . ? O6 C13 C14 107.57(17) . . ? N2 C14 O7 118.7(2) . . ? N2 C14 C13 126.2(2) . . ? O7 C14 C13 115.13(19) . . ? O7 C15 C16 105.63(18) . . ? N2 C16 C19 109.07(18) . . ? N2 C16 C20 108.89(19) . . ? C19 C16 C20 111.5(2) . . ? N2 C16 C15 101.71(18) . . ? C19 C16 C15 112.8(2) . . ? C20 C16 C15 112.3(2) . . ? F5A P1A F6A 178.73(9) . . ? F5A P1A F3A 89.98(8) . . ? F6A P1A F3A 90.05(9) . . ? F5A P1A F1A 90.14(9) . . ? F6A P1A F1A 89.82(9) . . ? F3A P1A F1A 179.57(10) . . ? F5A P1A F4A 90.97(8) . . ? F6A P1A F4A 90.30(8) . . ? F3A P1A F4A 90.36(8) . . ? F1A P1A F4A 90.06(8) . . ? F5A P1A F2A 89.41(8) . . ? F6A P1A F2A 89.32(8) . . ? F3A P1A F2A 89.92(8) . . ? F1A P1A F2A 89.66(8) . . ? F4A P1A F2A 179.53(9) . . ? P1A F2A Na1 147.66(9) . . ? F2B' P1B F2B' 180.0 . 3_656 ? F2B P1B F2B 180.0 . 3_656 ? F2B P1B F3B 90.4(2) . . ? F2B P1B F3B 89.6(2) 3_656 . ? F2B P1B F3B 89.6(2) . 3_656 ? F2B P1B F3B 90.4(2) 3_656 3_656 ? F3B P1B F3B 180.0 . 3_656 ? F2B' P1B F3B' 89.6(3) . 3_656 ? F2B' P1B F3B' 90.4(3) 3_656 3_656 ? F2B' P1B F3B' 90.4(3) . . ? F2B' P1B F3B' 89.6(3) 3_656 . ? F3B' P1B F3B' 180.0 3_656 . ? F2B" P1B F2B" 180.0 . 3_656 ? F2B" P1B F3B" 89.4(5) . . ? F2B" P1B F3B" 90.6(5) 3_656 . ? F2B" P1B F3B" 90.6(5) . 3_656 ? F2B" P1B F3B" 89.4(5) 3_656 3_656 ? F3B" P1B F3B" 180.0 . 3_656 ? P1B F1B Na1 145.05(9) . . ? F5C P1C F4C 90.5(3) . . ? F5C P1C F6C 179.3(4) . . ? F4C P1C F6C 90.2(3) . . ? F5C P1C F3C 90.4(3) . . ? F4C P1C F3C 90.7(3) . . ? F6C P1C F3C 89.6(3) . . ? F5C P1C F1C 89.8(3) . . ? F4C P1C F1C 89.1(3) . . ? F6C P1C F1C 90.1(3) . . ? F3C P1C F1C 179.7(3) . . ? F5C P1C F2C 90.1(3) . . ? F4C P1C F2C 179.1(3) . . ? F6C P1C F2C 89.2(3) . . ? F3C P1C F2C 89.9(2) . . ? F1C P1C F2C 90.3(2) . . ? C3S O1S C1S 112.1(4) . . ? O1S C1S C2S 110.3(4) . . ? O1S C3S C4S 110.5(4) . . ? 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 N1 1.8674(18) . ? Cu1 N2 1.8764(18) . ? Cu1 Na1 3.5807(9) . ? Na1 F1B 2.2828(16) . ? Na1 F2A 2.3198(16) . ? Na1 O5 2.3464(19) . ? Na1 O3 2.3567(19) . ? Na1 O4 2.4798(19) . ? Na1 O6 2.6020(18) . ? Na1 O2 2.7857(18) . ? N1 C3 1.272(3) . ? N1 C1 1.498(3) . ? N2 C14 1.268(3) . ? N2 C16 1.491(3) . ? O1 C3 1.332(3) . ? O1 C2 1.448(3) . ? O2 C4 1.423(3) . ? O2 C5 1.434(3) . ? O3 C6 1.416(3) . ? O3 C7 1.435(3) . ? O4 C9 1.416(3) . ? O4 C8 1.421(3) . ? O5 C11 1.416(3) . ? O5 C10 1.428(3) . ? O6 C13 1.424(3) . ? O6 C12 1.437(3) . ? O7 C14 1.332(3) . ? O7 C15 1.458(3) . ? C1 C17 1.513(3) . ? C1 C18 1.524(3) . ? C1 C2 1.543(3) . ? C3 C4 1.491(3) . ? C5 C6 1.505(4) . ? C7 C8 1.489(4) . ? C9 C10 1.498(4) . ? C11 C12 1.510(3) . ? C13 C14 1.495(3) . ? C15 C16 1.540(3) . ? C16 C19 1.513(3) . ? C16 C20 1.523(3) . ? P1A F5A 1.5907(15) . ? P1A F6A 1.5922(15) . ? P1A F3A 1.5929(15) . ? P1A F1A 1.5942(15) . ? P1A F4A 1.5982(14) . ? P1A F2A 1.6209(14) . ? P1B F2B' 1.570(6) . ? P1B F2B' 1.570(6) 3_656 ? P1B F2B 1.580(4) . ? P1B F2B 1.580(4) 3_656 ? P1B F3B 1.590(4) . ? P1B F3B 1.590(4) 3_656 ? P1B F3B' 1.593(6) 3_656 ? P1B F3B' 1.593(6) . ? P1B F2B" 1.597(7) . ? P1B F2B" 1.597(7) 3_656 ? P1B F3B" 1.608(8) . ? P1B F3B" 1.608(8) 3_656 ? P1C F5C 1.591(4) . ? P1C F4C 1.591(4) . ? P1C F6C 1.593(4) . ? P1C F3C 1.598(3) . ? P1C F1C 1.603(3) . ? P1C F2C 1.610(3) . ? O1S C3S 1.434(6) . ? O1S C1S 1.452(6) . ? C1S C2S 1.501(6) . ? C3S C4S 1.532(7) . ? 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 Na1 Cu1 N1 C3 53.02(19) . . . . ? Na1 Cu1 N1 C1 -133.50(17) . . . . ? Na1 Cu1 N2 C14 52.6(2) . . . . ? Na1 Cu1 N2 C16 -133.78(17) . . . . ? C3 N1 C1 C17 -123.6(2) . . . . ? Cu1 N1 C1 C17 62.0(2) . . . . ? C3 N1 C1 C18 114.1(2) . . . . ? Cu1 N1 C1 C18 -60.3(2) . . . . ? C3 N1 C1 C2 -4.4(2) . . . . ? Cu1 N1 C1 C2 -178.78(16) . . . . ? C3 O1 C2 C1 -6.3(2) . . . . ? N1 C1 C2 O1 6.4(2) . . . . ? C17 C1 C2 O1 123.5(2) . . . . ? C18 C1 C2 O1 -109.5(2) . . . . ? C1 N1 C3 O1 0.6(3) . . . . ? Cu1 N1 C3 O1 175.04(15) . . . . ? C1 N1 C3 C4 -178.8(2) . . . . ? Cu1 N1 C3 C4 -4.3(3) . . . . ? C2 O1 C3 N1 3.9(3) . . . . ? C2 O1 C3 C4 -176.7(2) . . . . ? C5 O2 C4 C3 165.20(19) . . . . ? Na1 O2 C4 C3 -78.9(2) . . . . ? N1 C3 C4 O2 -7.6(3) . . . . ? O1 C3 C4 O2 173.00(18) . . . . ? C4 O2 C5 C6 73.3(2) . . . . ? Na1 O2 C5 C6 -59.52(19) . . . . ? C7 O3 C6 C5 -171.2(2) . . . . ? Na1 O3 C6 C5 -28.5(3) . . . . ? O2 C5 C6 O3 65.6(3) . . . . ? C6 O3 C7 C8 -165.7(2) . . . . ? Na1 O3 C7 C8 49.0(2) . . . . ? C9 O4 C8 C7 165.7(2) . . . . ? Na1 O4 C8 C7 43.3(2) . . . . ? O3 C7 C8 O4 -60.6(2) . . . . ? C8 O4 C9 C10 177.66(19) . . . . ? Na1 O4 C9 C10 -57.7(2) . . . . ? C11 O5 C10 C9 171.7(2) . . . . ? Na1 O5 C10 C9 -26.6(3) . . . . ? O4 C9 C10 O5 55.8(3) . . . . ? C10 O5 C11 C12 158.0(2) . . . . ? Na1 O5 C11 C12 -3.0(3) . . . . ? C13 O6 C12 C11 67.8(2) . . . . ? Na1 O6 C12 C11 -59.8(2) . . . . ? O5 C11 C12 O6 45.8(3) . . . . ? C12 O6 C13 C14 155.60(18) . . . . ? Na1 O6 C13 C14 -86.40(18) . . . . ? C16 N2 C14 O7 -2.1(3) . . . . ? Cu1 N2 C14 O7 172.40(15) . . . . ? C16 N2 C14 C13 178.3(2) . . . . ? Cu1 N2 C14 C13 -7.3(3) . . . . ? C15 O7 C14 N2 1.0(3) . . . . ? C15 O7 C14 C13 -179.3(2) . . . . ? O6 C13 C14 N2 -4.1(3) . . . . ? O6 C13 C14 O7 176.23(18) . . . . ? C14 O7 C15 C16 0.5(3) . . . . ? C14 N2 C16 C19 -117.3(2) . . . . ? Cu1 N2 C16 C19 68.1(2) . . . . ? C14 N2 C16 C20 120.8(2) . . . . ? Cu1 N2 C16 C20 -53.8(2) . . . . ? C14 N2 C16 C15 2.1(2) . . . . ? Cu1 N2 C16 C15 -172.52(16) . . . . ? O7 C15 C16 N2 -1.5(2) . . . . ? O7 C15 C16 C19 115.2(2) . . . . ? O7 C15 C16 C20 -117.8(2) . . . . ? F5A P1A F2A Na1 -98.76(17) . . . . ? F6A P1A F2A Na1 81.26(18) . . . . ? F3A P1A F2A Na1 -8.79(18) . . . . ? F1A P1A F2A Na1 171.09(17) . . . . ? F2B' P1B F1B Na1 140.3(4) . . . . ? F2B' P1B F1B Na1 -39.7(4) 3_656 . . . ? F2B P1B F1B Na1 -105.1(2) . . . . ? F2B P1B F1B Na1 74.9(2) 3_656 . . . ? F3B P1B F1B Na1 164.5(2) . . . . ? F3B P1B F1B Na1 -15.5(2) 3_656 . . . ? F3B' P1B F1B Na1 50.7(4) 3_656 . . . ? F3B' P1B F1B Na1 -129.3(4) . . . . ? F2B" P1B F1B Na1 -62.5(6) . . . . ? F2B" P1B F1B Na1 117.5(6) 3_656 . . . ? F3B" P1B F1B Na1 -152.0(6) . . . . ? F3B" P1B F1B Na1 28.0(6) 3_656 . . . ? C3S O1S C1S C2S -178.1(5) . . . . ? C1S O1S C3S C4S 176.4(6) . . . . ?