# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_stahl236 _database_code_depnum_ccdc_archive 'CCDC 1949421' loop_ _audit_author_name _audit_author_address 'Ilia Guzei' ;UW Madison, Molecular Structure Laboratory United States of America ; _audit_update_record ; 2019-08-26 deposited with the CCDC. 2019-12-09 downloaded from the CCDC. ; _audit_creation_date 2018-04-18 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486) ; _shelx_SHELXL_version_number 2018/1 loop_ _audit_author_email aristov@wisc.edu iguzei@chem.wisc.edu _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C40 H34 Cu F12 N6 P2, 2(C4 H10 O)' _chemical_formula_sum 'C48 H54 Cu F12 N6 O2 P2' _chemical_formula_weight 1100.45 _chemical_melting_point ? 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' F F 0.0171 0.0103 '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' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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' _cell_length_a 21.313(6) _cell_length_b 9.951(3) _cell_length_c 24.687(6) _cell_angle_alpha 90 _cell_angle_beta 107.778(11) _cell_angle_gamma 90 _cell_volume 4986(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9792 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.125 _cell_measurement_theta_min 2.280 _shelx_estimated_absorpt_T_max 0.968 _shelx_estimated_absorpt_T_min 0.920 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_T_max 0.2612 _exptl_absorpt_correction_T_min 0.2331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Krause et al., 2015) was used for absorption correction.' _exptl_absorpt_special_details ? _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2268 _exptl_crystal_size_max 0.144 _exptl_crystal_size_mid 0.128 _exptl_crystal_size_min 0.055 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_unetI/netI 0.0186 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 112793 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 27.151 _diffrn_reflns_theta_min 1.107 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '0.5\ \w and 0.5\ \f scans' _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9758 _reflns_number_total 11042 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)' _computing_data_collection 'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)' _computing_data_reduction 'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _refine_diff_density_max 0.433 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.049 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 670 _refine_ls_number_reflns 11042 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0275 _refine_ls_restrained_S_all 1.035 _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^)+(0.0308P)^2^+3.3876P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.0725 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Same fragment restrains {C46, O2, C47A, C48A} sigma for 1-2: 0.01, 1-3: 0.02 as {C46, O2, C47, C48} 3. Others Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1) Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C42(H42A,H42B), C43(H43A,H43B), C46(H46A,H46B), C47(H47A,H47B), C47A(H47C,H47D) 4.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4A), C5(H5A), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40) 4.c Idealised Me refined as rotating group: C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,H48B, H48C), C48A(H48D,H48E,H48F) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.26312(2) 0.63019(2) 0.50785(2) 0.01084(5) Uani 1 1 d . . . . . P1 P 0.36971(2) 0.60650(4) 0.39635(2) 0.01758(8) Uani 1 1 d . . . . . P2 P 0.16599(2) 0.66204(4) 0.61921(2) 0.01518(8) Uani 1 1 d . . . . . F1 F 0.38700(5) 0.75257(10) 0.42396(5) 0.0351(2) Uani 1 1 d . . . . . F2 F 0.30705(6) 0.66640(13) 0.34983(5) 0.0491(3) Uani 1 1 d . . . . . F3 F 0.35192(5) 0.45950(10) 0.37007(4) 0.0277(2) Uani 1 1 d . . . . . F4 F 0.43147(5) 0.54518(10) 0.44435(4) 0.0332(2) Uani 1 1 d . . . . . F5 F 0.41467(7) 0.63327(12) 0.35679(5) 0.0460(3) Uani 1 1 d . . . . . F6 F 0.32496(5) 0.57847(10) 0.43731(4) 0.0303(2) Uani 1 1 d . . . . . F7 F 0.19952(5) 0.71367(9) 0.57234(4) 0.0259(2) Uani 1 1 d . . . . . F8 F 0.19616(5) 0.78871(10) 0.65796(4) 0.0327(2) Uani 1 1 d . . . . . F9 F 0.10142(5) 0.74621(11) 0.58828(5) 0.0349(2) Uani 1 1 d . . . . . F10 F 0.13344(4) 0.60981(9) 0.66562(4) 0.02251(19) Uani 1 1 d . . . . . F11 F 0.13667(5) 0.53543(10) 0.57978(4) 0.0292(2) Uani 1 1 d . . . . . F12 F 0.23145(4) 0.57889(10) 0.64968(4) 0.0275(2) Uani 1 1 d . . . . . N1 N 0.30669(6) 0.80394(12) 0.51918(5) 0.0130(2) Uani 1 1 d . . . . . H1 H 0.3345(8) 0.8179(17) 0.5491(7) 0.015(4) Uiso 1 1 d . . . . . N2 N 0.25679(6) 0.89989(12) 0.43077(5) 0.0126(2) Uani 1 1 d . . . . . H2 H 0.2597(8) 0.9566(18) 0.4081(7) 0.016(4) Uiso 1 1 d . . . . . N3 N 0.19342(5) 0.71492(11) 0.44111(5) 0.0124(2) Uani 1 1 d . . . . . N4 N 0.21999(6) 0.45664(12) 0.49383(5) 0.0138(2) Uani 1 1 d . . . . . H4 H 0.1915(9) 0.4457(19) 0.4648(8) 0.021(5) Uiso 1 1 d . . . . . N5 N 0.26759(6) 0.35206(12) 0.58051(5) 0.0133(2) Uani 1 1 d . . . . . H5 H 0.2613(8) 0.2972(18) 0.6028(7) 0.016(4) Uiso 1 1 d . . . . . N6 N 0.33003(5) 0.54363(11) 0.57616(5) 0.0121(2) Uani 1 1 d . . . . . C1 C 0.30358(6) 0.89942(13) 0.48325(6) 0.0118(3) Uani 1 1 d . . . . . C2 C 0.34919(7) 1.01615(14) 0.49533(6) 0.0130(3) Uani 1 1 d . . . . . C3 C 0.41548(7) 0.99585(15) 0.52523(6) 0.0174(3) Uani 1 1 d . . . . . H3 H 0.430780 0.908541 0.538425 0.021 Uiso 1 1 calc R . . . . C4 C 0.45906(7) 1.10318(16) 0.53569(6) 0.0212(3) Uani 1 1 d . . . . . H4A H 0.504182 1.089347 0.556161 0.025 Uiso 1 1 calc R . . . . C5 C 0.43687(8) 1.23068(15) 0.51633(6) 0.0204(3) Uani 1 1 d . . . . . H5A H 0.467028 1.303626 0.522940 0.024 Uiso 1 1 calc R . . . . C6 C 0.37068(8) 1.25211(14) 0.48728(6) 0.0188(3) Uani 1 1 d . . . . . H6 H 0.355456 1.339754 0.474540 0.023 Uiso 1 1 calc R . . . . C7 C 0.32693(7) 1.14503(14) 0.47696(6) 0.0148(3) Uani 1 1 d . . . . . H7 H 0.281632 1.159565 0.457295 0.018 Uiso 1 1 calc R . . . . C8 C 0.20263(6) 0.81789(13) 0.41229(6) 0.0122(3) Uani 1 1 d . . . . . C9 C 0.15557(7) 0.86086(13) 0.35673(6) 0.0140(3) Uani 1 1 d . . . . . C10 C 0.17499(7) 0.85744(14) 0.30792(6) 0.0176(3) Uani 1 1 d . . . . . H10 H 0.217826 0.826930 0.309738 0.021 Uiso 1 1 calc R . . . . C11 C 0.13139(8) 0.89892(16) 0.25648(6) 0.0242(3) Uani 1 1 d . . . . . H11 H 0.144483 0.897375 0.222986 0.029 Uiso 1 1 calc R . . . . C12 C 0.06887(8) 0.94253(16) 0.25387(7) 0.0264(3) Uani 1 1 d . . . . . H12 H 0.039226 0.971208 0.218604 0.032 Uiso 1 1 calc R . . . . C13 C 0.04942(8) 0.94451(17) 0.30238(7) 0.0254(3) Uani 1 1 d . . . . . H13 H 0.006289 0.973633 0.300281 0.030 Uiso 1 1 calc R . . . . C14 C 0.09255(7) 0.90421(15) 0.35403(6) 0.0189(3) Uani 1 1 d . . . . . H14 H 0.079263 0.906115 0.387412 0.023 Uiso 1 1 calc R . . . . C15 C 0.13239(7) 0.64305(13) 0.41650(6) 0.0144(3) Uani 1 1 d . . . . . C16 C 0.12378(7) 0.56695(15) 0.36761(6) 0.0191(3) Uani 1 1 d . . . . . H16 H 0.158245 0.559586 0.350826 0.023 Uiso 1 1 calc R . . . . C17 C 0.06408(8) 0.50168(16) 0.34355(7) 0.0268(3) Uani 1 1 d . . . . . H17 H 0.057472 0.450466 0.309791 0.032 Uiso 1 1 calc R . . . . C18 C 0.01410(8) 0.51080(17) 0.36849(8) 0.0285(4) Uani 1 1 d . . . . . H18 H -0.026853 0.467228 0.351477 0.034 Uiso 1 1 calc R . . . . C19 C 0.02397(7) 0.58351(16) 0.41821(7) 0.0240(3) Uani 1 1 d . . . . . H19 H -0.010072 0.588445 0.435583 0.029 Uiso 1 1 calc R . . . . C20 C 0.08355(7) 0.64951(14) 0.44294(6) 0.0178(3) Uani 1 1 d . . . . . H20 H 0.090644 0.698216 0.477393 0.021 Uiso 1 1 calc R . . . . C21 C 0.22104(7) 0.35943(13) 0.52841(6) 0.0127(3) Uani 1 1 d . . . . . C22 C 0.17261(7) 0.24774(14) 0.51440(6) 0.0145(3) Uani 1 1 d . . . . . C23 C 0.10694(7) 0.27633(15) 0.48446(7) 0.0200(3) Uani 1 1 d . . . . . H23 H 0.093963 0.365957 0.473181 0.024 Uiso 1 1 calc R . . . . C24 C 0.06078(8) 0.17361(16) 0.47124(7) 0.0240(3) Uani 1 1 d . . . . . H24 H 0.016087 0.192886 0.451073 0.029 Uiso 1 1 calc R . . . . C25 C 0.07992(8) 0.04266(16) 0.48749(7) 0.0229(3) Uani 1 1 d . . . . . H25 H 0.048143 -0.027421 0.478569 0.027 Uiso 1 1 calc R . . . . C26 C 0.14515(8) 0.01336(15) 0.51668(6) 0.0200(3) Uani 1 1 d . . . . . H26 H 0.158055 -0.076586 0.527402 0.024 Uiso 1 1 calc R . . . . C27 C 0.19137(7) 0.11571(14) 0.53012(6) 0.0161(3) Uani 1 1 d . . . . . H27 H 0.236047 0.095822 0.550129 0.019 Uiso 1 1 calc R . . . . C28 C 0.32112(6) 0.43505(13) 0.60163(6) 0.0123(3) Uani 1 1 d . . . . . C29 C 0.36817(7) 0.38373(13) 0.65583(6) 0.0135(3) Uani 1 1 d . . . . . C30 C 0.35209(7) 0.38884(14) 0.70625(6) 0.0162(3) Uani 1 1 d . . . . . H30 H 0.311691 0.428155 0.706861 0.019 Uiso 1 1 calc R . . . . C31 C 0.39523(7) 0.33636(15) 0.75565(6) 0.0189(3) Uani 1 1 d . . . . . H31 H 0.384676 0.340694 0.790318 0.023 Uiso 1 1 calc R . . . . C32 C 0.45386(8) 0.27745(15) 0.75450(6) 0.0214(3) Uani 1 1 d . . . . . H32 H 0.483031 0.240271 0.788286 0.026 Uiso 1 1 calc R . . . . C33 C 0.46997(8) 0.27270(16) 0.70425(7) 0.0229(3) Uani 1 1 d . . . . . H33 H 0.510267 0.232870 0.703672 0.027 Uiso 1 1 calc R . . . . C34 C 0.42729(7) 0.32605(15) 0.65486(6) 0.0190(3) Uani 1 1 d . . . . . H34 H 0.438362 0.323270 0.620402 0.023 Uiso 1 1 calc R . . . . C35 C 0.38776(7) 0.62200(13) 0.60444(6) 0.0128(3) Uani 1 1 d . . . . . C36 C 0.38636(7) 0.70488(14) 0.64949(6) 0.0163(3) Uani 1 1 d . . . . . H36 H 0.349121 0.705349 0.662988 0.020 Uiso 1 1 calc R . . . . C37 C 0.44020(7) 0.78693(16) 0.67442(6) 0.0216(3) Uani 1 1 d . . . . . H37 H 0.439700 0.844483 0.704992 0.026 Uiso 1 1 calc R . . . . C38 C 0.49468(7) 0.78509(16) 0.65485(7) 0.0222(3) Uani 1 1 d . . . . . H38 H 0.531426 0.841122 0.672162 0.027 Uiso 1 1 calc R . . . . C39 C 0.49569(7) 0.70181(15) 0.61011(6) 0.0192(3) Uani 1 1 d . . . . . H39 H 0.533320 0.700198 0.597151 0.023 Uiso 1 1 calc R . . . . C40 C 0.44179(7) 0.62063(14) 0.58415(6) 0.0162(3) Uani 1 1 d . . . . . H40 H 0.441913 0.564932 0.552931 0.019 Uiso 1 1 calc R . . . . O1 O 0.27895(5) 1.08481(11) 0.34957(4) 0.0208(2) Uani 1 1 d . . . . . C41 C 0.34024(10) 0.9927(2) 0.28850(9) 0.0387(4) Uani 1 1 d . . . . . H41A H 0.315340 1.047385 0.256050 0.058 Uiso 1 1 calc GR . . . . H41B H 0.318705 0.905153 0.287065 0.058 Uiso 1 1 calc GR . . . . H41C H 0.385218 0.979552 0.286904 0.058 Uiso 1 1 calc GR . . . . C42 C 0.34251(8) 1.06327(19) 0.34309(7) 0.0291(4) Uani 1 1 d . . . . . H42A H 0.369326 1.009151 0.375579 0.035 Uiso 1 1 calc R . . . . H42B H 0.364644 1.151182 0.344297 0.035 Uiso 1 1 calc R . . . . C43 C 0.24099(9) 1.18557(18) 0.31286(8) 0.0310(4) Uani 1 1 d . . . . . H43A H 0.223479 1.149711 0.273723 0.037 Uiso 1 1 calc R . . . . H43B H 0.269189 1.264068 0.311966 0.037 Uiso 1 1 calc R . . . . C44 C 0.18518(9) 1.22780(18) 0.33401(8) 0.0352(4) Uani 1 1 d . . . . . H44A H 0.156345 1.289677 0.306611 0.053 Uiso 1 1 calc GR . . . . H44B H 0.202724 1.272951 0.370828 0.053 Uiso 1 1 calc GR . . . . H44C H 0.159965 1.148424 0.338413 0.053 Uiso 1 1 calc GR . . . . C45 C 0.31251(8) 0.02372(17) 0.68191(8) 0.0292(4) Uani 1 1 d . . . . . H45A H 0.292884 -0.025612 0.646407 0.044 Uiso 1 1 calc GR . . . . H45B H 0.336227 -0.039100 0.711712 0.044 Uiso 1 1 calc GR . . . . H45C H 0.343277 0.091242 0.676043 0.044 Uiso 1 1 calc GR . . . . C46 C 0.25907(8) 0.09217(16) 0.69967(7) 0.0236(3) Uani 1 1 d D . . . . H46A H 0.226939 0.024794 0.704354 0.028 Uiso 1 1 calc R . . . . H46B H 0.278327 0.138310 0.736547 0.028 Uiso 1 1 calc R . . . . O2 O 0.22669(5) 0.18753(11) 0.65711(4) 0.0207(2) Uani 1 1 d D . . . . C47 C 0.17444(10) 0.2574(2) 0.67058(10) 0.0339(5) Uani 0.931(4) 1 d D . P A 1 H47A H 0.164046 0.340636 0.647605 0.041 Uiso 0.931(4) 1 calc R . P A 1 H47B H 0.189586 0.283659 0.711188 0.041 Uiso 0.931(4) 1 calc R . P A 1 C48 C 0.11314(11) 0.1745(3) 0.65953(13) 0.0574(9) Uani 0.931(4) 1 d D . P A 1 H48A H 0.099774 0.142364 0.620119 0.086 Uiso 0.931(4) 1 calc GR . P A 1 H48B H 0.077807 0.229413 0.665758 0.086 Uiso 0.931(4) 1 calc GR . P A 1 H48C H 0.121742 0.097400 0.685472 0.086 Uiso 0.931(4) 1 calc GR . P A 1 C47A C 0.1572(5) 0.199(2) 0.6508(7) 0.025(6) Uiso 0.069(4) 1 d D . P A 2 H47C H 0.137472 0.107763 0.648107 0.030 Uiso 0.069(4) 1 calc R . P A 2 H47D H 0.134647 0.247912 0.615350 0.030 Uiso 0.069(4) 1 calc R . P A 2 C48A C 0.1479(10) 0.272(2) 0.7009(9) 0.027(6) Uiso 0.069(4) 1 d D . P A 2 H48D H 0.172261 0.225154 0.735998 0.040 Uiso 0.069(4) 1 calc GR . P A 2 H48E H 0.100948 0.273836 0.697700 0.040 Uiso 0.069(4) 1 calc GR . P A 2 H48F H 0.164460 0.363747 0.701688 0.040 Uiso 0.069(4) 1 calc GR . 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 0.01090(8) 0.00939(8) 0.01163(8) 0.00137(6) 0.00258(6) -0.00118(6) P1 0.01941(18) 0.01710(18) 0.01893(18) 0.00034(14) 0.00986(15) 0.00147(14) P2 0.01459(17) 0.01520(17) 0.01765(18) 0.00042(14) 0.00775(14) 0.00133(13) F1 0.0394(6) 0.0180(5) 0.0565(7) -0.0084(5) 0.0273(5) -0.0053(4) F2 0.0464(7) 0.0473(7) 0.0414(7) 0.0145(5) -0.0047(5) 0.0177(6) F3 0.0342(5) 0.0257(5) 0.0243(5) -0.0096(4) 0.0103(4) -0.0032(4) F4 0.0237(5) 0.0319(5) 0.0371(6) -0.0032(4) -0.0011(4) 0.0032(4) F5 0.0661(8) 0.0391(6) 0.0537(7) 0.0021(5) 0.0493(7) -0.0038(6) F6 0.0358(5) 0.0262(5) 0.0408(6) -0.0063(4) 0.0291(5) -0.0042(4) F7 0.0320(5) 0.0253(5) 0.0280(5) 0.0084(4) 0.0203(4) 0.0062(4) F8 0.0388(6) 0.0262(5) 0.0412(6) -0.0136(4) 0.0243(5) -0.0149(4) F9 0.0233(5) 0.0382(6) 0.0450(6) 0.0142(5) 0.0130(4) 0.0156(4) F10 0.0215(4) 0.0269(5) 0.0235(4) -0.0018(4) 0.0135(4) -0.0054(4) F11 0.0386(6) 0.0266(5) 0.0234(5) -0.0080(4) 0.0108(4) -0.0075(4) F12 0.0206(5) 0.0352(5) 0.0283(5) 0.0105(4) 0.0098(4) 0.0095(4) N1 0.0123(5) 0.0136(6) 0.0111(5) 0.0008(4) 0.0008(5) -0.0009(4) N2 0.0136(6) 0.0120(5) 0.0120(5) 0.0031(4) 0.0038(4) -0.0021(4) N3 0.0107(5) 0.0118(5) 0.0142(5) 0.0000(4) 0.0029(4) -0.0014(4) N4 0.0133(6) 0.0123(6) 0.0140(6) 0.0008(4) 0.0017(5) -0.0010(4) N5 0.0151(6) 0.0120(5) 0.0135(6) 0.0033(4) 0.0055(5) -0.0011(4) N6 0.0117(5) 0.0121(5) 0.0131(5) -0.0003(4) 0.0046(4) -0.0007(4) C1 0.0109(6) 0.0121(6) 0.0134(6) -0.0010(5) 0.0053(5) 0.0006(5) C2 0.0148(6) 0.0133(6) 0.0121(6) -0.0009(5) 0.0058(5) -0.0025(5) C3 0.0165(7) 0.0160(7) 0.0193(7) -0.0014(5) 0.0047(5) -0.0012(5) C4 0.0154(7) 0.0250(8) 0.0225(7) -0.0053(6) 0.0047(6) -0.0045(6) C5 0.0239(8) 0.0189(7) 0.0211(7) -0.0062(6) 0.0112(6) -0.0111(6) C6 0.0275(8) 0.0129(6) 0.0190(7) -0.0007(5) 0.0113(6) -0.0030(6) C7 0.0165(7) 0.0150(7) 0.0137(6) -0.0002(5) 0.0055(5) -0.0008(5) C8 0.0117(6) 0.0127(6) 0.0127(6) -0.0012(5) 0.0045(5) 0.0006(5) C9 0.0150(6) 0.0120(6) 0.0133(6) 0.0015(5) 0.0019(5) -0.0022(5) C10 0.0200(7) 0.0163(7) 0.0170(7) 0.0007(5) 0.0059(6) -0.0002(5) C11 0.0347(9) 0.0227(8) 0.0135(7) 0.0008(6) 0.0047(6) 0.0006(7) C12 0.0283(8) 0.0241(8) 0.0184(7) 0.0049(6) -0.0052(6) 0.0007(7) C13 0.0175(7) 0.0258(8) 0.0291(8) 0.0073(7) 0.0015(6) 0.0032(6) C14 0.0168(7) 0.0197(7) 0.0203(7) 0.0056(6) 0.0060(6) 0.0019(6) C15 0.0113(6) 0.0119(6) 0.0177(7) 0.0038(5) 0.0009(5) -0.0005(5) C16 0.0169(7) 0.0168(7) 0.0222(7) -0.0003(6) 0.0040(6) -0.0019(6) C17 0.0237(8) 0.0220(8) 0.0283(8) -0.0058(6) -0.0017(6) -0.0065(6) C18 0.0148(7) 0.0237(8) 0.0404(10) 0.0018(7) -0.0014(7) -0.0074(6) C19 0.0124(7) 0.0215(8) 0.0372(9) 0.0078(7) 0.0064(6) 0.0002(6) C20 0.0148(7) 0.0157(7) 0.0229(7) 0.0040(6) 0.0055(6) 0.0003(5) C21 0.0121(6) 0.0115(6) 0.0161(6) -0.0008(5) 0.0065(5) 0.0007(5) C22 0.0156(7) 0.0129(6) 0.0163(6) 0.0000(5) 0.0069(5) -0.0018(5) C23 0.0164(7) 0.0159(7) 0.0265(8) 0.0026(6) 0.0051(6) 0.0003(6) C24 0.0146(7) 0.0247(8) 0.0312(8) -0.0019(7) 0.0045(6) -0.0032(6) C25 0.0230(8) 0.0184(7) 0.0297(8) -0.0051(6) 0.0117(6) -0.0091(6) C26 0.0275(8) 0.0121(7) 0.0239(7) -0.0006(6) 0.0127(6) -0.0023(6) C27 0.0183(7) 0.0145(7) 0.0171(7) 0.0008(5) 0.0077(5) -0.0002(5) C28 0.0123(6) 0.0131(6) 0.0131(6) -0.0005(5) 0.0061(5) 0.0016(5) C29 0.0155(6) 0.0105(6) 0.0139(6) 0.0024(5) 0.0034(5) -0.0006(5) C30 0.0165(7) 0.0154(7) 0.0177(7) 0.0014(5) 0.0068(5) -0.0009(5) C31 0.0248(8) 0.0173(7) 0.0144(7) 0.0023(5) 0.0058(6) -0.0036(6) C32 0.0223(7) 0.0190(7) 0.0186(7) 0.0058(6) -0.0002(6) 0.0006(6) C33 0.0180(7) 0.0230(8) 0.0265(8) 0.0048(6) 0.0053(6) 0.0058(6) C34 0.0197(7) 0.0205(7) 0.0182(7) 0.0025(6) 0.0078(6) 0.0034(6) C35 0.0117(6) 0.0126(6) 0.0126(6) 0.0031(5) 0.0013(5) 0.0007(5) C36 0.0143(7) 0.0179(7) 0.0167(7) 0.0004(5) 0.0045(5) 0.0009(5) C37 0.0190(7) 0.0235(8) 0.0202(7) -0.0074(6) 0.0030(6) -0.0018(6) C38 0.0138(7) 0.0247(8) 0.0240(8) -0.0017(6) -0.0001(6) -0.0046(6) C39 0.0119(6) 0.0228(7) 0.0231(7) 0.0022(6) 0.0056(6) 0.0001(6) C40 0.0158(7) 0.0165(7) 0.0163(7) 0.0014(5) 0.0050(5) 0.0013(5) O1 0.0219(5) 0.0234(5) 0.0188(5) 0.0039(4) 0.0091(4) -0.0023(4) C41 0.0422(11) 0.0403(11) 0.0430(11) -0.0138(9) 0.0271(9) -0.0113(9) C42 0.0236(8) 0.0371(10) 0.0304(9) -0.0066(7) 0.0140(7) -0.0071(7) C43 0.0376(10) 0.0253(8) 0.0305(9) 0.0109(7) 0.0113(7) -0.0021(7) C44 0.0400(10) 0.0252(9) 0.0395(10) 0.0093(8) 0.0107(8) 0.0087(8) C45 0.0260(8) 0.0230(8) 0.0391(10) 0.0064(7) 0.0106(7) 0.0021(7) C46 0.0265(8) 0.0218(8) 0.0219(8) 0.0067(6) 0.0067(6) 0.0002(6) O2 0.0239(5) 0.0189(5) 0.0224(5) 0.0068(4) 0.0115(4) 0.0022(4) C47 0.0395(11) 0.0251(10) 0.0462(12) 0.0114(9) 0.0266(10) 0.0111(9) C48 0.0305(12) 0.0497(15) 0.101(2) 0.0332(15) 0.0337(13) 0.0136(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 F6 2.5369(10) . ? Cu1 F7 2.5258(10) . ? Cu1 N1 1.9419(13) . ? Cu1 N3 2.0342(12) . ? Cu1 N4 1.9372(13) . ? Cu1 N6 2.0373(12) . ? P1 F1 1.6000(11) . ? P1 F2 1.5879(11) . ? P1 F3 1.5982(10) . ? P1 F4 1.5988(11) . ? P1 F5 1.5858(11) . ? P1 F6 1.6121(10) . ? P2 F7 1.6182(10) . ? P2 F8 1.5943(10) . ? P2 F9 1.5927(10) . ? P2 F10 1.5965(10) . ? P2 F11 1.5981(10) . ? P2 F12 1.5988(10) . ? N1 H1 0.806(18) . ? N1 C1 1.2876(18) . ? N2 H2 0.811(18) . ? N2 C1 1.3726(17) . ? N2 C8 1.3729(17) . ? N3 C8 1.2959(18) . ? N3 C15 1.4457(17) . ? N4 H4 0.792(19) . ? N4 C21 1.2858(18) . ? N5 H5 0.814(18) . ? N5 C21 1.3656(18) . ? N5 C28 1.3756(18) . ? N6 C28 1.2929(18) . ? N6 C35 1.4439(17) . ? C1 C2 1.4853(18) . ? C2 C3 1.395(2) . ? C2 C7 1.3943(19) . ? C3 H3 0.9500 . ? C3 C4 1.387(2) . ? C4 H4A 0.9500 . ? C4 C5 1.387(2) . ? C5 H5A 0.9500 . ? C5 C6 1.390(2) . ? C6 H6 0.9500 . ? C6 C7 1.387(2) . ? C7 H7 0.9500 . ? C8 C9 1.4934(18) . ? C9 C10 1.389(2) . ? C9 C14 1.393(2) . ? C10 H10 0.9500 . ? C10 C11 1.388(2) . ? C11 H11 0.9500 . ? C11 C12 1.384(2) . ? C12 H12 0.9500 . ? C12 C13 1.382(2) . ? C13 H13 0.9500 . ? C13 C14 1.384(2) . ? C14 H14 0.9500 . ? C15 C16 1.389(2) . ? C15 C20 1.389(2) . ? C16 H16 0.9500 . ? C16 C17 1.390(2) . ? C17 H17 0.9500 . ? C17 C18 1.386(3) . ? C18 H18 0.9500 . ? C18 C19 1.385(2) . ? C19 H19 0.9500 . ? C19 C20 1.394(2) . ? C20 H20 0.9500 . ? C21 C22 1.4841(19) . ? C22 C23 1.398(2) . ? C22 C27 1.393(2) . ? C23 H23 0.9500 . ? C23 C24 1.387(2) . ? C24 H24 0.9500 . ? C24 C25 1.388(2) . ? C25 H25 0.9500 . ? C25 C26 1.387(2) . ? C26 H26 0.9500 . ? C26 C27 1.385(2) . ? C27 H27 0.9500 . ? C28 C29 1.4958(18) . ? C29 C30 1.3890(19) . ? C29 C34 1.392(2) . ? C30 H30 0.9500 . ? C30 C31 1.386(2) . ? C31 H31 0.9500 . ? C31 C32 1.388(2) . ? C32 H32 0.9500 . ? C32 C33 1.385(2) . ? C33 H33 0.9500 . ? C33 C34 1.385(2) . ? C34 H34 0.9500 . ? C35 C36 1.392(2) . ? C35 C40 1.389(2) . ? C36 H36 0.9500 . ? C36 C37 1.389(2) . ? C37 H37 0.9500 . ? C37 C38 1.387(2) . ? C38 H38 0.9500 . ? C38 C39 1.386(2) . ? C39 H39 0.9500 . ? C39 C40 1.391(2) . ? C40 H40 0.9500 . ? O1 C42 1.4279(19) . ? O1 C43 1.426(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 C42 1.507(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.498(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C45 C46 1.503(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 O2 1.4275(18) . ? O2 C47 1.435(2) . ? O2 C47A 1.446(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.498(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C47A C48A 1.499(10) . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? 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 F7 Cu1 F6 172.15(3) . . ? N1 Cu1 F6 87.35(4) . . ? N1 Cu1 F7 86.64(4) . . ? N1 Cu1 N3 86.92(5) . . ? N1 Cu1 N6 94.26(5) . . ? N3 Cu1 F6 86.10(5) . . ? N3 Cu1 F7 88.54(4) . . ? N3 Cu1 N6 177.69(4) . . ? N4 Cu1 F6 90.80(4) . . ? N4 Cu1 F7 95.12(4) . . ? N4 Cu1 N1 177.93(5) . . ? N4 Cu1 N3 92.03(5) . . ? N4 Cu1 N6 86.85(5) . . ? N6 Cu1 F6 95.94(4) . . ? N6 Cu1 F7 89.54(4) . . ? F1 P1 F6 89.62(5) . . ? F2 P1 F1 90.03(7) . . ? F2 P1 F3 90.40(6) . . ? F2 P1 F4 178.31(7) . . ? F2 P1 F6 89.46(7) . . ? F3 P1 F1 178.62(6) . . ? F3 P1 F4 89.49(6) . . ? F3 P1 F6 89.07(5) . . ? F4 P1 F1 90.04(6) . . ? F4 P1 F6 88.85(6) . . ? F5 P1 F1 90.34(6) . . ? F5 P1 F2 91.39(8) . . ? F5 P1 F3 90.96(6) . . ? F5 P1 F4 90.29(7) . . ? F5 P1 F6 179.14(7) . . ? F8 P2 F7 89.59(6) . . ? F8 P2 F10 90.62(5) . . ? F8 P2 F11 179.00(6) . . ? F8 P2 F12 89.58(6) . . ? F9 P2 F7 89.76(6) . . ? F9 P2 F8 90.18(6) . . ? F9 P2 F10 90.81(6) . . ? F9 P2 F11 90.15(6) . . ? F9 P2 F12 179.06(6) . . ? F10 P2 F7 179.39(6) . . ? F10 P2 F11 90.32(5) . . ? F10 P2 F12 90.10(5) . . ? F11 P2 F7 89.47(5) . . ? F11 P2 F12 90.07(6) . . ? F12 P2 F7 89.33(5) . . ? P1 F6 Cu1 157.86(6) . . ? P2 F7 Cu1 141.76(5) . . ? Cu1 N1 H1 118.2(12) . . ? C1 N1 Cu1 129.50(10) . . ? C1 N1 H1 111.9(12) . . ? C1 N2 H2 117.9(12) . . ? C1 N2 C8 127.33(12) . . ? C8 N2 H2 114.7(12) . . ? C8 N3 Cu1 125.23(9) . . ? C8 N3 C15 115.34(11) . . ? C15 N3 Cu1 118.43(9) . . ? Cu1 N4 H4 118.3(14) . . ? C21 N4 Cu1 129.86(10) . . ? C21 N4 H4 110.5(14) . . ? C21 N5 H5 116.7(12) . . ? C21 N5 C28 127.20(12) . . ? C28 N5 H5 115.8(12) . . ? C28 N6 Cu1 125.89(9) . . ? C28 N6 C35 116.50(11) . . ? C35 N6 Cu1 116.72(8) . . ? N1 C1 N2 121.50(12) . . ? N1 C1 C2 123.08(12) . . ? N2 C1 C2 115.42(12) . . ? C3 C2 C1 119.22(12) . . ? C7 C2 C1 121.14(12) . . ? C7 C2 C3 119.63(13) . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 119.98(14) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4A 119.9 . . ? C3 C4 C5 120.12(14) . . ? C5 C4 H4A 119.9 . . ? C4 C5 H5A 119.9 . . ? C4 C5 C6 120.24(13) . . ? C6 C5 H5A 119.9 . . ? C5 C6 H6 120.1 . . ? C7 C6 C5 119.75(14) . . ? C7 C6 H6 120.1 . . ? C2 C7 H7 119.9 . . ? C6 C7 C2 120.26(13) . . ? C6 C7 H7 119.9 . . ? N2 C8 C9 113.31(12) . . ? N3 C8 N2 122.71(12) . . ? N3 C8 C9 123.97(12) . . ? C10 C9 C8 119.70(13) . . ? C10 C9 C14 120.30(13) . . ? C14 C9 C8 120.00(13) . . ? C9 C10 H10 120.2 . . ? C11 C10 C9 119.54(14) . . ? C11 C10 H10 120.2 . . ? C10 C11 H11 119.9 . . ? C12 C11 C10 120.13(15) . . ? C12 C11 H11 119.9 . . ? C11 C12 H12 119.9 . . ? C13 C12 C11 120.22(14) . . ? C13 C12 H12 119.9 . . ? C12 C13 H13 119.9 . . ? C12 C13 C14 120.23(15) . . ? C14 C13 H13 119.9 . . ? C9 C14 H14 120.2 . . ? C13 C14 C9 119.57(14) . . ? C13 C14 H14 120.2 . . ? C16 C15 N3 119.88(13) . . ? C20 C15 N3 119.14(13) . . ? C20 C15 C16 120.97(13) . . ? C15 C16 H16 120.4 . . ? C15 C16 C17 119.15(14) . . ? C17 C16 H16 120.4 . . ? C16 C17 H17 119.8 . . ? C18 C17 C16 120.45(15) . . ? C18 C17 H17 119.8 . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 119.91(14) . . ? C19 C18 H18 120.0 . . ? C18 C19 H19 119.8 . . ? C18 C19 C20 120.39(15) . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 119.05(15) . . ? C15 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? N4 C21 N5 121.74(13) . . ? N4 C21 C22 122.62(13) . . ? N5 C21 C22 115.64(12) . . ? C23 C22 C21 118.92(13) . . ? C27 C22 C21 121.41(13) . . ? C27 C22 C23 119.67(13) . . ? C22 C23 H23 120.1 . . ? C24 C23 C22 119.88(14) . . ? C24 C23 H23 120.1 . . ? C23 C24 H24 120.0 . . ? C23 C24 C25 119.96(14) . . ? C25 C24 H24 120.0 . . ? C24 C25 H25 119.8 . . ? C26 C25 C24 120.46(14) . . ? C26 C25 H25 119.8 . . ? C25 C26 H26 120.1 . . ? C27 C26 C25 119.77(14) . . ? C27 C26 H26 120.1 . . ? C22 C27 H27 119.9 . . ? C26 C27 C22 120.25(14) . . ? C26 C27 H27 119.9 . . ? N5 C28 C29 112.70(12) . . ? N6 C28 N5 123.05(12) . . ? N6 C28 C29 124.22(12) . . ? C30 C29 C28 120.51(12) . . ? C30 C29 C34 120.20(13) . . ? C34 C29 C28 119.24(12) . . ? C29 C30 H30 120.1 . . ? C31 C30 C29 119.72(14) . . ? C31 C30 H30 120.1 . . ? C30 C31 H31 120.0 . . ? C30 C31 C32 120.03(14) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.23(14) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 120.0 . . ? C34 C33 C32 119.97(14) . . ? C34 C33 H33 120.0 . . ? C29 C34 H34 120.1 . . ? C33 C34 C29 119.83(14) . . ? C33 C34 H34 120.1 . . ? C36 C35 N6 118.91(12) . . ? C40 C35 N6 119.87(12) . . ? C40 C35 C36 121.08(13) . . ? C35 C36 H36 120.5 . . ? C37 C36 C35 119.07(13) . . ? C37 C36 H36 120.5 . . ? C36 C37 H37 119.9 . . ? C38 C37 C36 120.24(14) . . ? C38 C37 H37 119.9 . . ? C37 C38 H38 119.9 . . ? C39 C38 C37 120.24(14) . . ? C39 C38 H38 119.9 . . ? C38 C39 H39 119.9 . . ? C38 C39 C40 120.19(14) . . ? C40 C39 H39 119.9 . . ? C35 C40 C39 119.16(13) . . ? C35 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C43 O1 C42 114.07(13) . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? O1 C42 C41 113.43(14) . . ? O1 C42 H42A 108.9 . . ? O1 C42 H42B 108.9 . . ? C41 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? O1 C43 H43A 109.8 . . ? O1 C43 H43B 109.8 . . ? O1 C43 C44 109.44(14) . . ? H43A C43 H43B 108.2 . . ? C44 C43 H43A 109.8 . . ? C44 C43 H43B 109.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? C45 C46 H46A 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? O2 C46 C45 109.02(13) . . ? O2 C46 H46A 109.9 . . ? O2 C46 H46B 109.9 . . ? C46 O2 C47 112.73(13) . . ? C46 O2 C47A 112.3(9) . . ? O2 C47 H47A 109.0 . . ? O2 C47 H47B 109.0 . . ? O2 C47 C48 112.72(18) . . ? H47A C47 H47B 107.8 . . ? C48 C47 H47A 109.0 . . ? C48 C47 H47B 109.0 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O2 C47A H47C 109.7 . . ? O2 C47A H47D 109.7 . . ? O2 C47A C48A 109.7(12) . . ? H47C C47A H47D 108.2 . . ? C48A C47A H47C 109.7 . . ? C48A C47A H47D 109.7 . . ? C47A C48A H48D 109.5 . . ? C47A C48A H48E 109.5 . . ? C47A C48A H48F 109.5 . . ? H48D C48A H48E 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2 O1 0.811(18) 2.060(18) 2.8645(16) 171.5(17) . yes N5 H5 O2 0.814(18) 2.034(18) 2.8325(16) 166.5(17) . yes 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 Cu1 N1 C1 N2 12.3(2) . . . . ? Cu1 N1 C1 C2 -168.18(10) . . . . ? Cu1 N3 C8 N2 -14.15(19) . . . . ? Cu1 N3 C8 C9 166.94(10) . . . . ? Cu1 N3 C15 C16 -98.35(13) . . . . ? Cu1 N3 C15 C20 80.51(14) . . . . ? Cu1 N4 C21 N5 -16.4(2) . . . . ? Cu1 N4 C21 C22 164.20(10) . . . . ? Cu1 N6 C28 N5 9.64(19) . . . . ? Cu1 N6 C28 C29 -172.22(10) . . . . ? Cu1 N6 C35 C36 90.96(13) . . . . ? Cu1 N6 C35 C40 -84.78(14) . . . . ? F1 P1 F6 Cu1 10.63(17) . . . . ? F2 P1 F6 Cu1 -79.40(17) . . . . ? F3 P1 F6 Cu1 -169.81(17) . . . . ? F4 P1 F6 Cu1 100.68(17) . . . . ? F8 P2 F7 Cu1 136.40(9) . . . . ? F9 P2 F7 Cu1 -133.42(9) . . . . ? F11 P2 F7 Cu1 -43.27(9) . . . . ? F12 P2 F7 Cu1 46.81(9) . . . . ? N1 C1 C2 C3 38.96(19) . . . . ? N1 C1 C2 C7 -141.52(14) . . . . ? N2 C1 C2 C3 -141.53(13) . . . . ? N2 C1 C2 C7 38.00(18) . . . . ? N2 C8 C9 C10 65.06(17) . . . . ? N2 C8 C9 C14 -114.89(14) . . . . ? N3 C8 C9 C10 -115.94(16) . . . . ? N3 C8 C9 C14 64.12(19) . . . . ? N3 C15 C16 C17 -178.12(13) . . . . ? N3 C15 C20 C19 178.06(13) . . . . ? N4 C21 C22 C23 -38.6(2) . . . . ? N4 C21 C22 C27 140.99(14) . . . . ? N5 C21 C22 C23 142.00(14) . . . . ? N5 C21 C22 C27 -38.45(19) . . . . ? N5 C28 C29 C30 -72.63(16) . . . . ? N5 C28 C29 C34 104.97(15) . . . . ? N6 C28 C29 C30 109.06(16) . . . . ? N6 C28 C29 C34 -73.35(18) . . . . ? N6 C35 C36 C37 -175.90(13) . . . . ? N6 C35 C40 C39 176.82(12) . . . . ? C1 N2 C8 N3 -9.3(2) . . . . ? C1 N2 C8 C9 169.76(12) . . . . ? C1 C2 C3 C4 178.46(13) . . . . ? C1 C2 C7 C6 -178.18(12) . . . . ? C2 C3 C4 C5 -0.2(2) . . . . ? C3 C2 C7 C6 1.3(2) . . . . ? C3 C4 C5 C6 1.2(2) . . . . ? C4 C5 C6 C7 -0.9(2) . . . . ? C5 C6 C7 C2 -0.3(2) . . . . ? C7 C2 C3 C4 -1.1(2) . . . . ? C8 N2 C1 N1 11.1(2) . . . . ? C8 N2 C1 C2 -168.42(12) . . . . ? C8 N3 C15 C16 70.85(17) . . . . ? C8 N3 C15 C20 -110.29(15) . . . . ? C8 C9 C10 C11 -179.26(13) . . . . ? C8 C9 C14 C13 179.66(14) . . . . ? C9 C10 C11 C12 -0.4(2) . . . . ? C10 C9 C14 C13 -0.3(2) . . . . ? C10 C11 C12 C13 -0.3(2) . . . . ? C11 C12 C13 C14 0.7(2) . . . . ? C12 C13 C14 C9 -0.4(2) . . . . ? C14 C9 C10 C11 0.7(2) . . . . ? C15 N3 C8 N2 177.48(12) . . . . ? C15 N3 C8 C9 -1.43(19) . . . . ? C15 C16 C17 C18 -0.9(2) . . . . ? C16 C15 C20 C19 -3.1(2) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C17 C18 C19 C20 1.0(2) . . . . ? C18 C19 C20 C15 1.0(2) . . . . ? C20 C15 C16 C17 3.0(2) . . . . ? C21 N5 C28 N6 8.4(2) . . . . ? C21 N5 C28 C29 -169.89(12) . . . . ? C21 C22 C23 C24 -179.60(14) . . . . ? C21 C22 C27 C26 179.81(13) . . . . ? C22 C23 C24 C25 -0.3(2) . . . . ? C23 C22 C27 C26 -0.6(2) . . . . ? C23 C24 C25 C26 -0.4(2) . . . . ? C24 C25 C26 C27 0.6(2) . . . . ? C25 C26 C27 C22 -0.1(2) . . . . ? C27 C22 C23 C24 0.8(2) . . . . ? C28 N5 C21 N4 -5.8(2) . . . . ? C28 N5 C21 C22 173.65(12) . . . . ? C28 N6 C35 C36 -78.87(16) . . . . ? C28 N6 C35 C40 105.39(15) . . . . ? C28 C29 C30 C31 177.64(13) . . . . ? C28 C29 C34 C33 -177.11(14) . . . . ? C29 C30 C31 C32 -0.8(2) . . . . ? C30 C29 C34 C33 0.5(2) . . . . ? C30 C31 C32 C33 1.0(2) . . . . ? C31 C32 C33 C34 -0.4(2) . . . . ? C32 C33 C34 C29 -0.3(2) . . . . ? C34 C29 C30 C31 0.1(2) . . . . ? C35 N6 C28 N5 178.41(12) . . . . ? C35 N6 C28 C29 -3.44(19) . . . . ? C35 C36 C37 C38 -0.5(2) . . . . ? C36 C35 C40 C39 1.2(2) . . . . ? C36 C37 C38 C39 0.3(2) . . . . ? C37 C38 C39 C40 0.7(2) . . . . ? C38 C39 C40 C35 -1.4(2) . . . . ? C40 C35 C36 C37 -0.2(2) . . . . ? C42 O1 C43 C44 -163.85(14) . . . . ? C43 O1 C42 C41 -71.94(19) . . . . ? C45 C46 O2 C47 179.70(15) . . . . ? C45 C46 O2 C47A 145.7(9) . . . . ? C46 O2 C47 C48 -77.6(2) . . . . ? C46 O2 C47A C48A 72.9(18) . . . . ? _shelx_res_file ; TITL stahl236.res in P2(1)/n stahl236.res created by SHELXL-2018/1 at 09:57:23 on 18-Apr-2018 REM Old TITL stahl236 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.099, Rweak 0.003, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C48 N8 F12 P2 Cu rem RTAB CuF7 Cu1 F7 rem RTAB CuF6 Cu1 F6 rem RTAB FCuF F6 Cu1 F7 CELL 0.71073 21.3126 9.951 24.687 90 107.778 90 ZERR 4 0.0058 0.0028 0.0064 0 0.011 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cu F N O P UNIT 192 216 4 48 24 8 8 L.S. 20 PLAN 5 SIZE 0.055 0.128 0.144 TEMP -173.15 HTAB N2 O1 HTAB N5 O2 BIND F7 Cu1 BIND F6 Cu1 LIST 4 CONF BOND $H more -1 fmap 2 acta 50 REM REM REM WGHT 0.030800 3.387600 FVAR 0.26559 0.93059 CU1 3 0.263123 0.630189 0.507854 11.00000 0.01090 0.00939 = 0.01163 0.00137 0.00258 -0.00118 P1 7 0.369714 0.606496 0.396352 11.00000 0.01941 0.01710 = 0.01893 0.00034 0.00986 0.00147 P2 7 0.165988 0.662044 0.619214 11.00000 0.01459 0.01520 = 0.01765 0.00042 0.00775 0.00133 F1 4 0.386997 0.752573 0.423959 11.00000 0.03936 0.01796 = 0.05650 -0.00844 0.02730 -0.00533 F2 4 0.307053 0.666397 0.349826 11.00000 0.04636 0.04732 = 0.04142 0.01447 -0.00471 0.01770 F3 4 0.351924 0.459502 0.370070 11.00000 0.03423 0.02566 = 0.02426 -0.00962 0.01032 -0.00321 F4 4 0.431465 0.545184 0.444350 11.00000 0.02368 0.03192 = 0.03714 -0.00316 -0.00109 0.00317 F5 4 0.414673 0.633267 0.356787 11.00000 0.06613 0.03906 = 0.05370 0.00209 0.04926 -0.00381 F6 4 0.324956 0.578466 0.437309 11.00000 0.03579 0.02615 = 0.04079 -0.00632 0.02910 -0.00416 F7 4 0.199523 0.713670 0.572343 11.00000 0.03197 0.02527 = 0.02799 0.00835 0.02030 0.00616 F8 4 0.196159 0.788707 0.657965 11.00000 0.03882 0.02619 = 0.04116 -0.01363 0.02433 -0.01490 F9 4 0.101418 0.746208 0.588279 11.00000 0.02325 0.03817 = 0.04500 0.01421 0.01299 0.01557 F10 4 0.133445 0.609805 0.665619 11.00000 0.02151 0.02695 = 0.02354 -0.00179 0.01350 -0.00537 F11 4 0.136668 0.535434 0.579785 11.00000 0.03864 0.02656 = 0.02336 -0.00799 0.01076 -0.00753 F12 4 0.231451 0.578887 0.649684 11.00000 0.02059 0.03517 = 0.02826 0.01052 0.00976 0.00953 N1 5 0.306688 0.803940 0.519177 11.00000 0.01229 0.01365 = 0.01112 0.00077 0.00082 -0.00094 H1 2 0.334526 0.817945 0.549092 11.00000 0.01472 N2 5 0.256790 0.899892 0.430769 11.00000 0.01362 0.01201 = 0.01201 0.00314 0.00383 -0.00210 H2 2 0.259665 0.956605 0.408076 11.00000 0.01579 N3 5 0.193425 0.714925 0.441105 11.00000 0.01071 0.01176 = 0.01420 0.00003 0.00288 -0.00137 N4 5 0.219994 0.456644 0.493830 11.00000 0.01332 0.01229 = 0.01395 0.00083 0.00165 -0.00098 H4 2 0.191542 0.445703 0.464829 11.00000 0.02101 N5 5 0.267587 0.352059 0.580510 11.00000 0.01512 0.01200 = 0.01349 0.00331 0.00554 -0.00110 H5 2 0.261264 0.297235 0.602759 11.00000 0.01575 N6 5 0.330033 0.543626 0.576162 11.00000 0.01167 0.01215 = 0.01308 -0.00031 0.00456 -0.00067 C1 1 0.303580 0.899422 0.483251 11.00000 0.01086 0.01212 = 0.01344 -0.00104 0.00533 0.00059 C2 1 0.349190 1.016152 0.495335 11.00000 0.01480 0.01327 = 0.01211 -0.00087 0.00581 -0.00251 C3 1 0.415478 0.995855 0.525230 11.00000 0.01652 0.01599 = 0.01930 -0.00142 0.00468 -0.00123 AFIX 43 H3 2 0.430780 0.908541 0.538425 11.00000 -1.20000 AFIX 0 C4 1 0.459055 1.103183 0.535693 11.00000 0.01536 0.02500 = 0.02253 -0.00534 0.00472 -0.00454 AFIX 43 H4A 2 0.504182 1.089347 0.556161 11.00000 -1.20000 AFIX 0 C5 1 0.436873 1.230681 0.516328 11.00000 0.02393 0.01889 = 0.02114 -0.00620 0.01119 -0.01109 AFIX 43 H5A 2 0.467028 1.303626 0.522940 11.00000 -1.20000 AFIX 0 C6 1 0.370680 1.252110 0.487279 11.00000 0.02749 0.01290 = 0.01895 -0.00066 0.01126 -0.00296 AFIX 43 H6 2 0.355456 1.339754 0.474540 11.00000 -1.20000 AFIX 0 C7 1 0.326932 1.145027 0.476959 11.00000 0.01651 0.01496 = 0.01368 -0.00025 0.00552 -0.00081 AFIX 43 H7 2 0.281632 1.159565 0.457295 11.00000 -1.20000 AFIX 0 C8 1 0.202627 0.817894 0.412295 11.00000 0.01171 0.01269 = 0.01268 -0.00122 0.00451 0.00065 C9 1 0.155574 0.860859 0.356729 11.00000 0.01501 0.01198 = 0.01325 0.00151 0.00189 -0.00218 C10 1 0.174994 0.857444 0.307922 11.00000 0.01995 0.01625 = 0.01695 0.00068 0.00595 -0.00020 AFIX 43 H10 2 0.217826 0.826930 0.309738 11.00000 -1.20000 AFIX 0 C11 1 0.131390 0.898923 0.256475 11.00000 0.03468 0.02273 = 0.01351 0.00076 0.00472 0.00060 AFIX 43 H11 2 0.144483 0.897375 0.222986 11.00000 -1.20000 AFIX 0 C12 1 0.068870 0.942534 0.253866 11.00000 0.02827 0.02412 = 0.01840 0.00487 -0.00517 0.00067 AFIX 43 H12 2 0.039226 0.971208 0.218604 11.00000 -1.20000 AFIX 0 C13 1 0.049420 0.944511 0.302384 11.00000 0.01752 0.02581 = 0.02914 0.00731 0.00153 0.00315 AFIX 43 H13 2 0.006289 0.973633 0.300281 11.00000 -1.20000 AFIX 0 C14 1 0.092555 0.904214 0.354026 11.00000 0.01679 0.01974 = 0.02029 0.00558 0.00599 0.00189 AFIX 43 H14 2 0.079263 0.906115 0.387412 11.00000 -1.20000 AFIX 0 C15 1 0.132393 0.643051 0.416496 11.00000 0.01135 0.01186 = 0.01772 0.00382 0.00090 -0.00054 C16 1 0.123779 0.566947 0.367610 11.00000 0.01686 0.01683 = 0.02217 -0.00034 0.00401 -0.00193 AFIX 43 H16 2 0.158245 0.559586 0.350826 11.00000 -1.20000 AFIX 0 C17 1 0.064076 0.501677 0.343551 11.00000 0.02373 0.02200 = 0.02826 -0.00580 -0.00172 -0.00645 AFIX 43 H17 2 0.057472 0.450466 0.309791 11.00000 -1.20000 AFIX 0 C18 1 0.014105 0.510803 0.368486 11.00000 0.01475 0.02367 = 0.04037 0.00180 -0.00145 -0.00740 AFIX 43 H18 2 -0.026853 0.467228 0.351477 11.00000 -1.20000 AFIX 0 C19 1 0.023967 0.583511 0.418215 11.00000 0.01242 0.02150 = 0.03720 0.00782 0.00641 0.00015 AFIX 43 H19 2 -0.010072 0.588445 0.435583 11.00000 -1.20000 AFIX 0 C20 1 0.083548 0.649512 0.442943 11.00000 0.01483 0.01566 = 0.02286 0.00404 0.00552 0.00033 AFIX 43 H20 2 0.090644 0.698216 0.477393 11.00000 -1.20000 AFIX 0 C21 1 0.221040 0.359433 0.528405 11.00000 0.01211 0.01149 = 0.01606 -0.00084 0.00652 0.00066 C22 1 0.172605 0.247736 0.514405 11.00000 0.01560 0.01290 = 0.01634 -0.00005 0.00691 -0.00176 C23 1 0.106940 0.276326 0.484457 11.00000 0.01644 0.01593 = 0.02652 0.00256 0.00508 0.00029 AFIX 43 H23 2 0.093963 0.365957 0.473181 11.00000 -1.20000 AFIX 0 C24 1 0.060784 0.173613 0.471240 11.00000 0.01456 0.02465 = 0.03124 -0.00190 0.00447 -0.00322 AFIX 43 H24 2 0.016087 0.192886 0.451073 11.00000 -1.20000 AFIX 0 C25 1 0.079923 0.042660 0.487491 11.00000 0.02303 0.01837 = 0.02972 -0.00510 0.01172 -0.00906 AFIX 43 H25 2 0.048143 -0.027421 0.478569 11.00000 -1.20000 AFIX 0 C26 1 0.145146 0.013363 0.516675 11.00000 0.02746 0.01208 = 0.02389 -0.00059 0.01273 -0.00235 AFIX 43 H26 2 0.158055 -0.076586 0.527402 11.00000 -1.20000 AFIX 0 C27 1 0.191373 0.115709 0.530119 11.00000 0.01832 0.01448 = 0.01712 0.00078 0.00768 -0.00023 AFIX 43 H27 2 0.236047 0.095822 0.550129 11.00000 -1.20000 AFIX 0 C28 1 0.321120 0.435049 0.601629 11.00000 0.01231 0.01310 = 0.01310 -0.00047 0.00607 0.00160 C29 1 0.368167 0.383731 0.655833 11.00000 0.01545 0.01046 = 0.01392 0.00236 0.00343 -0.00056 C30 1 0.352089 0.388845 0.706247 11.00000 0.01647 0.01538 = 0.01768 0.00140 0.00677 -0.00091 AFIX 43 H30 2 0.311691 0.428155 0.706861 11.00000 -1.20000 AFIX 0 C31 1 0.395229 0.336360 0.755649 11.00000 0.02477 0.01729 = 0.01438 0.00227 0.00578 -0.00357 AFIX 43 H31 2 0.384676 0.340694 0.790318 11.00000 -1.20000 AFIX 0 C32 1 0.453860 0.277451 0.754497 11.00000 0.02230 0.01898 = 0.01855 0.00575 -0.00018 0.00064 AFIX 43 H32 2 0.483031 0.240271 0.788286 11.00000 -1.20000 AFIX 0 C33 1 0.469968 0.272700 0.704254 11.00000 0.01805 0.02300 = 0.02655 0.00483 0.00527 0.00580 AFIX 43 H33 2 0.510267 0.232870 0.703672 11.00000 -1.20000 AFIX 0 C34 1 0.427293 0.326051 0.654857 11.00000 0.01972 0.02053 = 0.01821 0.00246 0.00778 0.00344 AFIX 43 H34 2 0.438362 0.323270 0.620402 11.00000 -1.20000 AFIX 0 C35 1 0.387758 0.622001 0.604445 11.00000 0.01172 0.01258 = 0.01260 0.00313 0.00126 0.00073 C36 1 0.386360 0.704885 0.649488 11.00000 0.01426 0.01787 = 0.01671 0.00041 0.00450 0.00089 AFIX 43 H36 2 0.349121 0.705349 0.662988 11.00000 -1.20000 AFIX 0 C37 1 0.440198 0.786926 0.674424 11.00000 0.01905 0.02354 = 0.02019 -0.00736 0.00303 -0.00184 AFIX 43 H37 2 0.439700 0.844483 0.704992 11.00000 -1.20000 AFIX 0 C38 1 0.494679 0.785094 0.654846 11.00000 0.01382 0.02473 = 0.02402 -0.00167 -0.00012 -0.00459 AFIX 43 H38 2 0.531426 0.841122 0.672162 11.00000 -1.20000 AFIX 0 C39 1 0.495690 0.701815 0.610112 11.00000 0.01189 0.02283 = 0.02309 0.00219 0.00558 0.00010 AFIX 43 H39 2 0.533320 0.700198 0.597151 11.00000 -1.20000 AFIX 0 C40 1 0.441788 0.620630 0.584152 11.00000 0.01584 0.01653 = 0.01634 0.00137 0.00501 0.00134 AFIX 43 H40 2 0.441913 0.564932 0.552931 11.00000 -1.20000 AFIX 0 O1 6 0.278949 1.084812 0.349572 11.00000 0.02195 0.02343 = 0.01879 0.00394 0.00906 -0.00230 C41 1 0.340245 0.992665 0.288502 11.00000 0.04222 0.04031 = 0.04302 -0.01381 0.02706 -0.01126 AFIX 137 H41A 2 0.315340 1.047385 0.256050 11.00000 -1.50000 H41B 2 0.318705 0.905153 0.287065 11.00000 -1.50000 H41C 2 0.385218 0.979552 0.286904 11.00000 -1.50000 AFIX 0 C42 1 0.342508 1.063274 0.343090 11.00000 0.02358 0.03709 = 0.03042 -0.00662 0.01403 -0.00713 AFIX 23 H42A 2 0.369326 1.009151 0.375579 11.00000 -1.20000 H42B 2 0.364644 1.151182 0.344297 11.00000 -1.20000 AFIX 0 C43 1 0.240989 1.185566 0.312865 11.00000 0.03764 0.02534 = 0.03053 0.01095 0.01130 -0.00210 AFIX 23 H43A 2 0.223479 1.149711 0.273723 11.00000 -1.20000 H43B 2 0.269189 1.264068 0.311966 11.00000 -1.20000 AFIX 0 C44 1 0.185184 1.227804 0.334006 11.00000 0.04003 0.02523 = 0.03953 0.00930 0.01073 0.00866 AFIX 137 H44A 2 0.156345 1.289677 0.306611 11.00000 -1.50000 H44B 2 0.202724 1.272951 0.370828 11.00000 -1.50000 H44C 2 0.159965 1.148424 0.338413 11.00000 -1.50000 AFIX 0 C45 1 0.312512 0.023722 0.681913 11.00000 0.02596 0.02300 = 0.03910 0.00638 0.01058 0.00212 AFIX 137 H45A 2 0.292884 -0.025612 0.646407 11.00000 -1.50000 H45B 2 0.336227 -0.039100 0.711712 11.00000 -1.50000 H45C 2 0.343277 0.091242 0.676043 11.00000 -1.50000 AFIX 0 SAME 0.01 0.02 C46 O2 C47A C48A C46 1 0.259066 0.092168 0.699665 11.00000 0.02653 0.02183 = 0.02194 0.00674 0.00673 0.00020 AFIX 23 H46A 2 0.226939 0.024794 0.704354 11.00000 -1.20000 H46B 2 0.278327 0.138310 0.736547 11.00000 -1.20000 AFIX 0 O2 6 0.226686 0.187533 0.657109 11.00000 0.02387 0.01886 = 0.02237 0.00683 0.01147 0.00224 PART 1 C47 1 0.174441 0.257392 0.670575 21.00000 0.03947 0.02514 = 0.04624 0.01136 0.02657 0.01110 AFIX 23 H47A 2 0.164046 0.340636 0.647605 21.00000 -1.20000 H47B 2 0.189586 0.283659 0.711188 21.00000 -1.20000 AFIX 0 C48 1 0.113141 0.174473 0.659525 21.00000 0.03055 0.04971 = 0.10107 0.03324 0.03367 0.01358 AFIX 137 H48A 2 0.099774 0.142364 0.620119 21.00000 -1.50000 H48B 2 0.077807 0.229413 0.665758 21.00000 -1.50000 H48C 2 0.121742 0.097400 0.685472 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C47A 1 0.157173 0.198561 0.650776 -21.00000 0.02540 AFIX 23 H47C 2 0.137472 0.107763 0.648107 -21.00000 -1.20000 H47D 2 0.134647 0.247912 0.615350 -21.00000 -1.20000 AFIX 0 C48A 1 0.147909 0.271651 0.700877 -21.00000 0.02666 AFIX 137 H48D 2 0.172261 0.225154 0.735998 -21.00000 -1.50000 H48E 2 0.100948 0.273836 0.697700 -21.00000 -1.50000 H48F 2 0.164460 0.363747 0.701688 -21.00000 -1.50000 AFIX 0 HKLF 4 REM stahl236.res in P2(1)/n REM R1 = 0.0275 for 9758 Fo > 4sig(Fo) and 0.0327 for all 11042 data REM 670 parameters refined using 4 restraints END WGHT 0.0308 3.3875 REM Highest difference peak 0.433, deepest hole -0.397, 1-sigma level 0.049 Q1 1 0.3788 0.6455 0.3330 11.00000 0.05 0.43 Q2 1 0.1798 0.8433 0.3851 11.00000 0.05 0.40 Q3 1 0.1978 0.2992 0.5220 11.00000 0.05 0.37 Q4 1 0.3251 0.9631 0.4883 11.00000 0.05 0.34 Q5 1 0.4396 0.5860 0.4180 11.00000 0.05 0.34 ; _shelx_res_checksum 3286 _olex2_submission_special_instructions 'No special instructions were received' _vrf_PLAT241_stahl236 ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of F6 Check RESPONSE: F6 has a larger thermal ellipsoid than its neighbors because it is a terminal atom of a PF~6~^-^ anion and such behavior is not unexpected. ; _vrf_PLAT242_stahl236 ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of P1 Check RESPONSE: F6 has a larger thermal ellipsoid than its neighbors because it is the center atom of a PF~6~^-^ anion and such behavior is not unexpected. ; _vrf_PLAT420_stahl236 ; PROBLEM: D-H Without Acceptor N1 --H1 Please Check RESPONSE: There are no nearby atoms that can serve as an acceptor for the N-H unit. ; _vrf_PLAT911_stahl236 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 6 Report RESPONSE: These reflections were eliminated during the data reduction phase. ;