# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p4-sr _vrf_CHEMW03_p4-sr ; PROBLEM:The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 RESPONSE: The unit cell contains 100 methanol molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _vrf_PLAT220_p4-sr ; PROBLEM:Large Non-Solvent C Ueq(max)/Ueq(min) RESPONSE: this is related to impossibility to correctly take into account thermal motion. It is expleined by following reason: the first reason is related to the fact that crystal structure contains large value of the MeOH or H2O molecules which can not be localized. The second reason is related to disorder of some Ph cycles, however it is impossible to find correct way to resove this disorder. ; _vrf_PLAT430_p4-sr ; PROBLEM: Short Inter D...A Contact O1 .. N1 .. 2.83 Ang. RESPONSE: probably, it is the hydrogen bond H2O...N1 (H(H2O) atoms can not be localized). ; _vrf_DENSD01_p4-sr ; PROBLEM:Calculated Density less than 1.0 gcm-3 ......... 0.7695 RESPONSE: see previous Alert. ; _vrf_PLAT046_p4-sr ; PROBLEM:Calculated Density less than 1.0 gcm-3 ......... 0.7695 RESPONSE: see previous Alert. ; _vrf_PLAT910_p4-sr ; PROBLEM:Missing # of FCF Reflections Below Th(Min) ..... 22 RESPONSE: these reflections have high Delta(F^2)/esd values, therefore they are omitted. ; _vrf_PLAT043_p4-sr ; PROBLEM:Check Reported Molecular Weight ................ 3388.77 RESPONSE: The methanol molecules were not located. Hovewer, these molecules were included in brutto-formula and moiety formula. ; _vrf_PLAT044_p4-sr ; PROBLEM:Calculated and Reported Dx Differ RESPONSE: The methanol molecules were not located. Hovewer, these molecules were included in brutto-formula and moiety formula. ; _audit_creation_method SHELXL-2013 _vrf_PUBL024_GLOBAL ; PROBLEM: The number of authors is greater than 5. RESPONSE: All co-authors have made significant scientific contributions to the work reported and share responsibility and accountability for the results. ; _chemical_name_systematic ; bis[2,3,9,10,16,17,23,24-octa-phenylphthalocyanine] lutetium ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C160 H96 Lu N16,0.5(H2 O), 100(C H4 O)' _chemical_formula_sum 'C260 H497 Lu N16 O100.50' _chemical_formula_weight 5630.68 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' Lu Lu -0.4720 5.8584 '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' _space_group_crystal_system tetragonal _space_group_IT_number 85 _space_group_name_H-M_alt 'P 4/n' _space_group_name_Hall '-P 4a' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' _cell_length_a 31.3930(10) _cell_length_b 31.3930(10) _cell_length_c 10.6224(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10468.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3570 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 123312 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.917 _diffrn_reflns_theta_max 28.997 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 13919 _reflns_number_gt 10732 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 0.108 0.553 5653 1929 ' ' _platon_squeeze_details ; The unit cell contains 100 methanol molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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. ; _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+1.5741P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13919 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Lu1 Lu 0.7500 0.7500 -0.09364(2) 0.02871(7) Uani 1 4 d S T P . . N1 N 0.78419(6) 0.80210(6) 0.0321(2) 0.0290(4) Uani 1 1 d . . . . . N2 N 0.85529(6) 0.77175(6) 0.04998(19) 0.0255(4) Uani 1 1 d . . . . . C1 C 0.82785(7) 0.80388(7) 0.0457(2) 0.0252(4) Uani 1 1 d . . . . . C2 C 0.84126(7) 0.84843(7) 0.0598(2) 0.0259(5) Uani 1 1 d . . . . . C3 C 0.88115(7) 0.86715(8) 0.0696(2) 0.0283(5) Uani 1 1 d . . . . . H3A H 0.9063 0.8503 0.0680 0.034 Uiso 1 1 calc R U . . . C4 C 0.88337(8) 0.91164(8) 0.0819(3) 0.0354(5) Uani 1 1 d . . . . . C5 C 0.84568(8) 0.93641(8) 0.0799(3) 0.0357(6) Uani 1 1 d . . . . . C6 C 0.80575(8) 0.91682(7) 0.0690(2) 0.0304(5) Uani 1 1 d . . . . . H6A H 0.7804 0.9333 0.0674 0.037 Uiso 1 1 calc R U . . . C7 C 0.80419(7) 0.87283(7) 0.0607(2) 0.0251(5) Uani 1 1 d . . . . . C8 C 0.76860(7) 0.84286(7) 0.0464(2) 0.0239(4) Uani 1 1 d . . . . . C9 C 0.92627(8) 0.93082(8) 0.1071(3) 0.0407(6) Uani 1 1 d . . . . . C10 C 0.95923(10) 0.92513(10) 0.0225(4) 0.0551(8) Uani 1 1 d . . . . . H10A H 0.9546 0.9093 -0.0524 0.066 Uiso 1 1 calc R U . . . C11 C 0.99937(12) 0.94264(14) 0.0472(5) 0.0780(12) Uani 1 1 d . . . . . H11A H 1.0218 0.9391 -0.0118 0.094 Uiso 1 1 calc R U . . . C12 C 1.00634(13) 0.96504(13) 0.1568(5) 0.0854(14) Uani 1 1 d . . . . . H12A H 1.0336 0.9771 0.1730 0.102 Uiso 1 1 calc R U . . . C13 C 0.97364(12) 0.97008(11) 0.2438(5) 0.0723(12) Uani 1 1 d . . . . . H13A H 0.9786 0.9845 0.3211 0.087 Uiso 1 1 calc R U . . . C14 C 0.93370(10) 0.95368(10) 0.2160(3) 0.0525(8) Uani 1 1 d . . . . . H14A H 0.9109 0.9583 0.2733 0.063 Uiso 1 1 calc R U . . . C15 C 0.84713(9) 0.98399(9) 0.0864(3) 0.0476(7) Uani 1 1 d . . . . . C16 C 0.87409(10) 1.00749(10) 0.0091(4) 0.0597(9) Uani 1 1 d . . . . . H16A H 0.8928 0.9932 -0.0472 0.072 Uiso 1 1 calc R U . . . C17 C 0.87399(12) 1.05210(11) 0.0133(5) 0.0758(13) Uani 1 1 d . . . . . H17A H 0.8922 1.0679 -0.0406 0.091 Uiso 1 1 calc R U . . . C18 C 0.84749(13) 1.07280(11) 0.0956(6) 0.0951(18) Uani 1 1 d . . . . . H18A H 0.8480 1.1030 0.0995 0.114 Uiso 1 1 calc R U . . . C19 C 0.82015(13) 1.05042(11) 0.1728(5) 0.0817(14) Uani 1 1 d . . . . . H19A H 0.8017 1.0651 0.2288 0.098 Uiso 1 1 calc R U . . . C20 C 0.81992(10) 1.00590(10) 0.1676(4) 0.0602(9) Uani 1 1 d . . . . . H20A H 0.8010 0.9904 0.2202 0.072 Uiso 1 1 calc R U . . . N1A N 0.73700(6) 0.81090(6) -0.21899(19) 0.0270(4) Uani 1 1 d . . . . . N2A N 0.80838(6) 0.84019(6) -0.23665(18) 0.0272(4) Uani 1 1 d . . . . . C1A C 0.76625(7) 0.84317(7) -0.2319(2) 0.0240(4) Uani 1 1 d . . . . . C2A C 0.74411(7) 0.88398(7) -0.2467(2) 0.0281(5) Uani 1 1 d . . . . . C3A C 0.75847(8) 0.92586(8) -0.2569(2) 0.0327(5) Uani 1 1 d . . . . . H3AA H 0.7881 0.9321 -0.2563 0.039 Uiso 1 1 calc R U . . . C4A C 0.72844(8) 0.95855(8) -0.2680(3) 0.0359(6) Uani 1 1 d . . . . . C5A C 0.68415(8) 0.94903(8) -0.2664(3) 0.0375(6) Uani 1 1 d . . . . . C6A C 0.67044(8) 0.90671(8) -0.2568(2) 0.0334(5) Uani 1 1 d . . . . . H6AA H 0.6409 0.9001 -0.2566 0.040 Uiso 1 1 calc R U . . . C7A C 0.70058(7) 0.87471(7) -0.2474(2) 0.0292(5) Uani 1 1 d . . . . . C8A C 0.69700(7) 0.82840(7) -0.2326(2) 0.0238(4) Uani 1 1 d . . . . . C9A C 0.74442(9) 1.00274(8) -0.2865(3) 0.0462(7) Uani 1 1 d . . . . . C10A C 0.77201(12) 1.02102(10) -0.2010(4) 0.0691(11) Uani 1 1 d . . . . . H10B H 0.7811 1.0051 -0.1298 0.083 Uiso 1 1 calc R U . . . C11A C 0.78663(15) 1.06242(13) -0.2175(6) 0.108(2) Uani 1 1 d . . . . . H11B H 0.8050 1.0750 -0.1569 0.129 Uiso 1 1 calc R U . . . C12A C 0.77437(17) 1.08496(14) -0.3222(8) 0.127(3) Uani 1 1 d . . . . . H12B H 0.7841 1.1134 -0.3331 0.153 Uiso 1 1 calc R U . . . C13A C 0.74794(16) 1.06674(14) -0.4126(6) 0.104(2) Uani 1 1 d . . . . . H13B H 0.7406 1.0821 -0.4866 0.125 Uiso 1 1 calc R U . . . C14A C 0.73244(12) 1.02580(11) -0.3930(4) 0.0658(10) Uani 1 1 d . . . . . H14B H 0.7135 1.0134 -0.4525 0.079 Uiso 1 1 calc R U . . . C15A C 0.65096(9) 0.98314(8) -0.2715(3) 0.0455(7) Uani 1 1 d . . . . . C16A C 0.65308(11) 1.01878(10) -0.1950(4) 0.0587(9) Uani 1 1 d . . . . . H16B H 0.6766 1.0229 -0.1429 0.070 Uiso 1 1 d R U . . . C17A C 0.62120(13) 1.04923(11) -0.1979(5) 0.0800(13) Uani 1 1 d . . . . . H17B H 0.6233 1.0737 -0.1455 0.096 Uiso 1 1 calc R U . . . C18A C 0.58673(13) 1.04453(13) -0.2754(6) 0.0943(16) Uani 1 1 d . . . . . H18B H 0.5648 1.0654 -0.2759 0.113 Uiso 1 1 calc R U . . . C19A C 0.58394(13) 1.00928(13) -0.3529(5) 0.0849(13) Uani 1 1 d . . . . . H19B H 0.5603 1.0061 -0.4081 0.102 Uiso 1 1 calc R U . . . C20A C 0.61600(10) 0.97833(11) -0.3501(4) 0.0601(9) Uani 1 1 d . . . . . H20B H 0.6138 0.9539 -0.4022 0.072 Uiso 1 1 calc R U . . . O1 O 0.7500 0.7500 0.2245(7) 0.0394(16) Uiso 0.5 4 d S . P . . 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 Lu1 0.02181(7) 0.02181(7) 0.04251(13) 0.000 0.000 0.000 N1 0.0243(9) 0.0242(9) 0.0387(12) 0.0011(8) 0.0034(8) 0.0006(7) N2 0.0221(9) 0.0224(9) 0.0320(10) -0.0022(8) -0.0019(8) 0.0000(7) C1 0.0226(10) 0.0217(10) 0.0312(11) -0.0005(9) -0.0009(9) -0.0004(8) C2 0.0257(11) 0.0241(10) 0.0281(12) -0.0025(9) 0.0010(9) -0.0010(8) C3 0.0266(11) 0.0293(11) 0.0291(13) -0.0025(9) -0.0019(9) -0.0017(9) C4 0.0319(12) 0.0314(12) 0.0430(15) -0.0053(11) -0.0019(11) -0.0052(9) C5 0.0341(12) 0.0267(11) 0.0464(16) -0.0020(11) -0.0033(11) -0.0033(9) C6 0.0306(12) 0.0259(11) 0.0348(14) -0.0026(9) -0.0014(10) 0.0002(9) C7 0.0268(11) 0.0254(11) 0.0232(11) -0.0033(8) -0.0009(8) -0.0020(8) C8 0.0228(10) 0.0209(10) 0.0280(11) -0.0009(9) 0.0026(9) 0.0011(8) C9 0.0315(12) 0.0269(11) 0.0636(19) -0.0031(12) -0.0083(13) -0.0045(9) C10 0.0362(15) 0.0504(18) 0.079(2) -0.0043(17) 0.0015(16) -0.0105(13) C11 0.0381(18) 0.076(3) 0.120(3) -0.003(3) 0.006(2) -0.0182(18) C12 0.047(2) 0.060(2) 0.149(4) -0.009(3) -0.027(3) -0.0233(18) C13 0.054(2) 0.0505(19) 0.113(3) -0.020(2) -0.030(2) -0.0075(16) C14 0.0450(16) 0.0436(16) 0.069(2) -0.0136(15) -0.0177(15) -0.0024(13) C15 0.0348(13) 0.0284(12) 0.079(2) -0.0046(14) -0.0140(15) -0.0043(10) C16 0.0430(17) 0.0352(15) 0.101(3) 0.0096(17) -0.0114(18) -0.0075(13) C17 0.0480(19) 0.0366(17) 0.143(4) 0.017(2) -0.022(2) -0.0120(15) C18 0.054(2) 0.0254(14) 0.206(6) -0.006(2) -0.031(3) -0.0047(14) C19 0.062(2) 0.0366(17) 0.147(4) -0.030(2) -0.012(3) 0.0042(16) C20 0.0459(17) 0.0339(15) 0.101(3) -0.0178(17) -0.0079(18) 0.0001(13) N1A 0.0257(9) 0.0253(9) 0.0300(10) 0.0010(8) -0.0021(8) -0.0001(7) N2A 0.0282(10) 0.0251(9) 0.0283(10) 0.0019(8) 0.0028(8) -0.0005(7) C1A 0.0268(11) 0.0257(10) 0.0195(10) -0.0025(8) 0.0011(9) -0.0002(8) C2A 0.0269(11) 0.0257(11) 0.0317(12) 0.0042(9) -0.0002(9) 0.0008(9) C3A 0.0303(12) 0.0285(12) 0.0393(14) 0.0061(10) 0.0017(10) -0.0010(9) C4A 0.0371(13) 0.0261(11) 0.0443(15) 0.0058(11) 0.0001(11) 0.0015(10) C5A 0.0346(13) 0.0283(12) 0.0495(16) 0.0059(11) 0.0001(12) 0.0041(10) C6A 0.0280(11) 0.0304(12) 0.0417(15) 0.0034(11) 0.0002(10) 0.0027(9) C7A 0.0285(11) 0.0258(11) 0.0332(13) 0.0052(9) 0.0008(10) 0.0007(9) C8A 0.0265(11) 0.0267(11) 0.0181(10) 0.0009(8) -0.0004(8) 0.0012(8) C9A 0.0380(14) 0.0268(12) 0.074(2) 0.0122(13) -0.0021(14) 0.0006(11) C10A 0.058(2) 0.0341(16) 0.116(3) 0.0069(19) -0.021(2) -0.0041(14) C11A 0.083(3) 0.044(2) 0.196(6) 0.012(3) -0.055(4) -0.020(2) C12A 0.086(3) 0.045(2) 0.251(8) 0.058(4) -0.036(4) -0.025(2) C13A 0.080(3) 0.060(2) 0.173(5) 0.068(3) -0.018(3) -0.016(2) C14A 0.057(2) 0.0468(18) 0.093(3) 0.0274(19) -0.0093(19) -0.0057(15) C15A 0.0367(14) 0.0277(12) 0.072(2) 0.0082(13) 0.0051(14) 0.0059(11) C16A 0.0496(18) 0.0353(15) 0.091(3) -0.0045(16) 0.0091(18) 0.0080(13) C17A 0.063(2) 0.0381(18) 0.139(4) -0.009(2) 0.013(3) 0.0175(16) C18A 0.058(2) 0.049(2) 0.176(5) 0.003(3) 0.000(3) 0.0259(18) C19A 0.051(2) 0.062(2) 0.141(4) 0.009(3) -0.016(2) 0.0199(18) C20A 0.0444(17) 0.0415(17) 0.094(3) 0.0079(17) -0.0064(18) 0.0106(14) _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 Lu1 N1A 2.3653(19) 2_655 ? Lu1 N1A 2.3653(19) 3_665 ? Lu1 N1A 2.3653(19) 4_565 ? Lu1 N1A 2.3653(19) . ? Lu1 N1 2.369(2) . ? Lu1 N1 2.369(2) 4_565 ? Lu1 N1 2.369(2) 3_665 ? Lu1 N1 2.369(2) 2_655 ? N1 C1 1.380(3) . ? N1 C8 1.378(3) . ? N2 C8 1.326(3) 4_565 ? N2 C1 1.327(3) . ? C1 C2 1.468(3) . ? C2 C3 1.387(3) . ? C2 C7 1.393(3) . ? C3 C4 1.404(3) . ? C3 H3A 0.9500 . ? C4 C5 1.416(4) . ? C4 C9 1.499(3) . ? C5 C6 1.401(3) . ? C5 C15 1.496(3) . ? C6 C7 1.385(3) . ? C6 H6A 0.9500 . ? C7 C8 1.469(3) . ? C8 N2 1.326(3) 2_655 ? C9 C14 1.381(4) . ? C9 C10 1.382(5) . ? C10 C11 1.399(5) . ? C10 H10A 0.9500 . ? C11 C12 1.378(7) . ? C11 H11A 0.9500 . ? C12 C13 1.391(6) . ? C12 H12A 0.9500 . ? C13 C14 1.387(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.391(5) . ? C15 C20 1.395(5) . ? C16 C17 1.401(4) . ? C16 H16A 0.9500 . ? C17 C18 1.371(7) . ? C17 H17A 0.9500 . ? C18 C19 1.379(7) . ? C18 H18A 0.9500 . ? C19 C20 1.399(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? N1A C1A 1.374(3) . ? N1A C8A 1.378(3) . ? N2A C1A 1.327(3) . ? N2A C8A 1.326(3) 4_565 ? C1A C2A 1.466(3) . ? C2A C3A 1.394(3) . ? C2A C7A 1.397(3) . ? C3A C4A 1.399(3) . ? C3A H3AA 0.9500 . ? C4A C5A 1.422(4) . ? C4A C9A 1.488(3) . ? C5A C6A 1.400(3) . ? C5A C15A 1.495(3) . ? C6A C7A 1.384(3) . ? C6A H6AA 0.9500 . ? C7A C8A 1.467(3) . ? C8A N2A 1.326(3) 2_655 ? C9A C10A 1.381(5) . ? C9A C14A 1.394(5) . ? C10A C11A 1.389(5) . ? C10A H10B 0.9500 . ? C11A C12A 1.373(8) . ? C11A H11B 0.9500 . ? C12A C13A 1.392(8) . ? C12A H12B 0.9500 . ? C13A C14A 1.390(5) . ? C13A H13B 0.9500 . ? C14A H14B 0.9500 . ? C15A C16A 1.384(5) . ? C15A C20A 1.387(5) . ? C16A C17A 1.384(4) . ? C16A H16B 0.9304 . ? C17A C18A 1.368(7) . ? C17A H17B 0.9500 . ? C18A C19A 1.382(7) . ? C18A H18B 0.9500 . ? C19A C20A 1.399(5) . ? C19A H19B 0.9500 . ? C20A H20B 0.9500 . ? 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 N1A Lu1 N1A 71.52(5) 2_655 3_665 ? N1A Lu1 N1A 111.48(10) 2_655 4_565 ? N1A Lu1 N1A 71.52(5) 3_665 4_565 ? N1A Lu1 N1A 71.53(5) 2_655 . ? N1A Lu1 N1A 111.48(10) 3_665 . ? N1A Lu1 N1A 71.52(5) 4_565 . ? N1A Lu1 N1 143.40(6) 2_655 . ? N1A Lu1 N1 142.87(6) 3_665 . ? N1A Lu1 N1 80.33(7) 4_565 . ? N1A Lu1 N1 80.64(7) . . ? N1A Lu1 N1 142.88(6) 2_655 4_565 ? N1A Lu1 N1 80.33(7) 3_665 4_565 ? N1A Lu1 N1 80.65(7) 4_565 4_565 ? N1A Lu1 N1 143.40(6) . 4_565 ? N1 Lu1 N1 71.47(5) . 4_565 ? N1A Lu1 N1 80.33(7) 2_655 3_665 ? N1A Lu1 N1 80.65(7) 3_665 3_665 ? N1A Lu1 N1 143.40(6) 4_565 3_665 ? N1A Lu1 N1 142.88(6) . 3_665 ? N1 Lu1 N1 111.36(10) . 3_665 ? N1 Lu1 N1 71.47(5) 4_565 3_665 ? N1A Lu1 N1 80.65(7) 2_655 2_655 ? N1A Lu1 N1 143.40(6) 3_665 2_655 ? N1A Lu1 N1 142.88(6) 4_565 2_655 ? N1A Lu1 N1 80.33(7) . 2_655 ? N1 Lu1 N1 71.47(5) . 2_655 ? N1 Lu1 N1 111.36(10) 4_565 2_655 ? N1 Lu1 N1 71.47(5) 3_665 2_655 ? C1 N1 C8 107.68(18) . . ? C1 N1 Lu1 122.51(15) . . ? C8 N1 Lu1 122.84(15) . . ? C8 N2 C1 122.28(19) 4_565 . ? N2 C1 N1 128.1(2) . . ? N2 C1 C2 122.3(2) . . ? N1 C1 C2 109.51(19) . . ? C3 C2 C7 121.4(2) . . ? C3 C2 C1 132.1(2) . . ? C7 C2 C1 106.57(19) . . ? C2 C3 C4 118.2(2) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C3 C4 C5 120.2(2) . . ? C3 C4 C9 117.4(2) . . ? C5 C4 C9 122.2(2) . . ? C6 C5 C4 120.5(2) . . ? C6 C5 C15 118.0(2) . . ? C4 C5 C15 121.5(2) . . ? C7 C6 C5 118.3(2) . . ? C7 C6 H6A 120.8 . . ? C5 C6 H6A 120.8 . . ? C6 C7 C2 121.3(2) . . ? C6 C7 C8 132.2(2) . . ? C2 C7 C8 106.42(19) . . ? N2 C8 N1 128.0(2) 2_655 . ? N2 C8 C7 122.4(2) 2_655 . ? N1 C8 C7 109.63(19) . . ? C14 C9 C10 119.0(3) . . ? C14 C9 C4 120.7(3) . . ? C10 C9 C4 120.3(3) . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 118.9(4) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C9 C14 C13 121.6(4) . . ? C9 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C16 C15 C20 118.4(3) . . ? C16 C15 C5 121.4(3) . . ? C20 C15 C5 120.1(3) . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C15 C20 C19 120.9(4) . . ? C15 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C1A N1A C8A 107.73(18) . . ? C1A N1A Lu1 122.46(14) . . ? C8A N1A Lu1 122.59(15) . . ? C1A N2A C8A 122.21(19) . 4_565 ? N2A C1A N1A 128.2(2) . . ? N2A C1A C2A 122.0(2) . . ? N1A C1A C2A 109.77(19) . . ? C3A C2A C7A 120.8(2) . . ? C3A C2A C1A 132.8(2) . . ? C7A C2A C1A 106.38(19) . . ? C2A C3A C4A 118.7(2) . . ? C2A C3A H3AA 120.6 . . ? C4A C3A H3AA 120.6 . . ? C3A C4A C5A 120.2(2) . . ? C3A C4A C9A 117.9(2) . . ? C5A C4A C9A 121.8(2) . . ? C6A C5A C4A 120.0(2) . . ? C6A C5A C15A 117.9(2) . . ? C4A C5A C15A 122.0(2) . . ? C7A C6A C5A 118.9(2) . . ? C7A C6A H6AA 120.5 . . ? C5A C6A H6AA 120.5 . . ? C6A C7A C2A 121.2(2) . . ? C6A C7A C8A 132.5(2) . . ? C2A C7A C8A 106.32(19) . . ? N2A C8A N1A 128.1(2) 2_655 . ? N2A C8A C7A 122.3(2) 2_655 . ? N1A C8A C7A 109.66(19) . . ? C10A C9A C14A 119.2(3) . . ? C10A C9A C4A 120.8(3) . . ? C14A C9A C4A 120.0(3) . . ? C9A C10A C11A 120.8(4) . . ? C9A C10A H10B 119.6 . . ? C11A C10A H10B 119.6 . . ? C12A C11A C10A 119.5(5) . . ? C12A C11A H11B 120.3 . . ? C10A C11A H11B 120.3 . . ? C11A C12A C13A 120.9(4) . . ? C11A C12A H12B 119.5 . . ? C13A C12A H12B 119.5 . . ? C14A C13A C12A 119.0(4) . . ? C14A C13A H13B 120.5 . . ? C12A C13A H13B 120.5 . . ? C13A C14A C9A 120.5(4) . . ? C13A C14A H14B 119.8 . . ? C9A C14A H14B 119.8 . . ? C16A C15A C20A 118.6(3) . . ? C16A C15A C5A 121.6(3) . . ? C20A C15A C5A 119.7(3) . . ? C15A C16A C17A 120.7(4) . . ? C15A C16A H16B 120.0 . . ? C17A C16A H16B 119.3 . . ? C18A C17A C16A 120.7(4) . . ? C18A C17A H17B 119.6 . . ? C16A C17A H17B 119.6 . . ? C17A C18A C19A 119.7(3) . . ? C17A C18A H18B 120.2 . . ? C19A C18A H18B 120.2 . . ? C18A C19A C20A 119.8(4) . . ? C18A C19A H19B 120.1 . . ? C20A C19A H19B 120.1 . . ? C15A C20A C19A 120.4(4) . . ? C15A C20A H20B 119.8 . . ? C19A C20A H20B 119.8 . . ? 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 C8 N2 C1 N1 -3.0(4) 4_565 . . . ? C8 N2 C1 C2 175.0(2) 4_565 . . . ? C8 N1 C1 N2 173.6(2) . . . . ? Lu1 N1 C1 N2 -34.9(3) . . . . ? C8 N1 C1 C2 -4.6(3) . . . . ? Lu1 N1 C1 C2 146.85(16) . . . . ? N2 C1 C2 C3 5.5(4) . . . . ? N1 C1 C2 C3 -176.2(2) . . . . ? N2 C1 C2 C7 -175.3(2) . . . . ? N1 C1 C2 C7 3.1(3) . . . . ? C7 C2 C3 C4 0.6(3) . . . . ? C1 C2 C3 C4 179.8(2) . . . . ? C2 C3 C4 C5 -2.1(4) . . . . ? C2 C3 C4 C9 173.2(2) . . . . ? C3 C4 C5 C6 1.7(4) . . . . ? C9 C4 C5 C6 -173.3(3) . . . . ? C3 C4 C5 C15 -177.0(3) . . . . ? C9 C4 C5 C15 8.0(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C15 C5 C6 C7 178.9(2) . . . . ? C5 C6 C7 C2 -1.7(4) . . . . ? C5 C6 C7 C8 -178.7(2) . . . . ? C3 C2 C7 C6 1.3(3) . . . . ? C1 C2 C7 C6 -178.0(2) . . . . ? C3 C2 C7 C8 179.0(2) . . . . ? C1 C2 C7 C8 -0.4(2) . . . . ? C1 N1 C8 N2 -174.4(2) . . . 2_655 ? Lu1 N1 C8 N2 34.3(3) . . . 2_655 ? C1 N1 C8 C7 4.3(3) . . . . ? Lu1 N1 C8 C7 -146.97(15) . . . . ? C6 C7 C8 N2 -6.3(4) . . . 2_655 ? C2 C7 C8 N2 176.4(2) . . . 2_655 ? C6 C7 C8 N1 174.9(2) . . . . ? C2 C7 C8 N1 -2.4(3) . . . . ? C3 C4 C9 C14 -118.8(3) . . . . ? C5 C4 C9 C14 56.4(4) . . . . ? C3 C4 C9 C10 59.9(4) . . . . ? C5 C4 C9 C10 -124.9(3) . . . . ? C14 C9 C10 C11 -0.5(5) . . . . ? C4 C9 C10 C11 -179.2(3) . . . . ? C9 C10 C11 C12 1.0(6) . . . . ? C10 C11 C12 C13 0.5(7) . . . . ? C11 C12 C13 C14 -2.5(6) . . . . ? C10 C9 C14 C13 -1.6(5) . . . . ? C4 C9 C14 C13 177.1(3) . . . . ? C12 C13 C14 C9 3.1(6) . . . . ? C6 C5 C15 C16 -129.9(3) . . . . ? C4 C5 C15 C16 48.7(4) . . . . ? C6 C5 C15 C20 47.5(4) . . . . ? C4 C5 C15 C20 -133.8(3) . . . . ? C20 C15 C16 C17 0.3(5) . . . . ? C5 C15 C16 C17 177.8(3) . . . . ? C15 C16 C17 C18 0.9(6) . . . . ? C16 C17 C18 C19 -1.4(7) . . . . ? C17 C18 C19 C20 0.7(7) . . . . ? C16 C15 C20 C19 -1.0(5) . . . . ? C5 C15 C20 C19 -178.5(3) . . . . ? C18 C19 C20 C15 0.5(6) . . . . ? C8A N2A C1A N1A 2.0(4) 4_565 . . . ? C8A N2A C1A C2A -174.9(2) 4_565 . . . ? C8A N1A C1A N2A -173.5(2) . . . . ? Lu1 N1A C1A N2A 35.6(3) . . . . ? C8A N1A C1A C2A 3.7(3) . . . . ? Lu1 N1A C1A C2A -147.14(16) . . . . ? N2A C1A C2A C3A -6.1(4) . . . . ? N1A C1A C2A C3A 176.5(3) . . . . ? N2A C1A C2A C7A 175.0(2) . . . . ? N1A C1A C2A C7A -2.4(3) . . . . ? C7A C2A C3A C4A 0.0(4) . . . . ? C1A C2A C3A C4A -178.8(3) . . . . ? C2A C3A C4A C5A 1.1(4) . . . . ? C2A C3A C4A C9A -176.4(3) . . . . ? C3A C4A C5A C6A -1.5(4) . . . . ? C9A C4A C5A C6A 175.9(3) . . . . ? C3A C4A C5A C15A 176.9(3) . . . . ? C9A C4A C5A C15A -5.7(4) . . . . ? C4A C5A C6A C7A 0.7(4) . . . . ? C15A C5A C6A C7A -177.7(3) . . . . ? C5A C6A C7A C2A 0.4(4) . . . . ? C5A C6A C7A C8A 178.0(3) . . . . ? C3A C2A C7A C6A -0.8(4) . . . . ? C1A C2A C7A C6A 178.3(2) . . . . ? C3A C2A C7A C8A -178.9(2) . . . . ? C1A C2A C7A C8A 0.2(3) . . . . ? C1A N1A C8A N2A 174.4(2) . . . 2_655 ? Lu1 N1A C8A N2A -34.8(3) . . . 2_655 ? C1A N1A C8A C7A -3.6(3) . . . . ? Lu1 N1A C8A C7A 147.22(16) . . . . ? C6A C7A C8A N2A 6.2(4) . . . 2_655 ? C2A C7A C8A N2A -176.1(2) . . . 2_655 ? C6A C7A C8A N1A -175.7(3) . . . . ? C2A C7A C8A N1A 2.1(3) . . . . ? C3A C4A C9A C10A -57.1(4) . . . . ? C5A C4A C9A C10A 125.4(3) . . . . ? C3A C4A C9A C14A 121.3(3) . . . . ? C5A C4A C9A C14A -56.2(4) . . . . ? C14A C9A C10A C11A 2.3(6) . . . . ? C4A C9A C10A C11A -179.4(4) . . . . ? C9A C10A C11A C12A -1.8(8) . . . . ? C10A C11A C12A C13A -0.8(10) . . . . ? C11A C12A C13A C14A 2.8(10) . . . . ? C12A C13A C14A C9A -2.3(8) . . . . ? C10A C9A C14A C13A -0.2(6) . . . . ? C4A C9A C14A C13A -178.6(4) . . . . ? C6A C5A C15A C16A 130.9(3) . . . . ? C4A C5A C15A C16A -47.5(4) . . . . ? C6A C5A C15A C20A -45.9(4) . . . . ? C4A C5A C15A C20A 135.7(3) . . . . ? C20A C15A C16A C17A -0.7(5) . . . . ? C5A C15A C16A C17A -177.6(3) . . . . ? C15A C16A C17A C18A 0.7(7) . . . . ? C16A C17A C18A C19A -0.9(8) . . . . ? C17A C18A C19A C20A 1.1(8) . . . . ? C16A C15A C20A C19A 1.0(5) . . . . ? C5A C15A C20A C19A 177.9(4) . . . . ? C18A C19A C20A C15A -1.2(7) . . . . ? _refine_diff_density_max 3.656 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.101 _shelxl_version_number 2013-2 _shelx_res_file ; TITL fin R = New: P4/n CELL 0.71073 31.3930 31.3930 10.6224 90.000 90.000 90.000 ZERR 2 0.0010 0.0010 0.0007 0.000 0.000 0.000 LATT 1 SYMM 0.50000 - Y , X , Z SYMM 0.50000 - X , 0.50000 - Y , Z SYMM Y , 0.50000 - X , Z SFAC C H Lu N O UNIT 520 994 2 32 201 TEMP -173.000 L.S. 5 FMAP 2 PLAN -30 ACTA BOND $H CONF WGHT 0.069500 1.574100 FVAR 0.56209 LU1 3 0.750000 0.750000 -0.093638 10.25000 0.02181 0.02181 = 0.04251 0.00000 0.00000 0.00000 N1 4 0.784186 0.802100 0.032076 11.00000 0.02429 0.02416 = 0.03869 0.00106 0.00337 0.00057 N2 4 0.855293 0.771746 0.049976 11.00000 0.02206 0.02244 = 0.03201 -0.00220 -0.00189 -0.00002 C1 1 0.827854 0.803878 0.045735 11.00000 0.02259 0.02170 = 0.03117 -0.00054 -0.00089 -0.00037 C2 1 0.841257 0.848433 0.059782 11.00000 0.02567 0.02407 = 0.02807 -0.00246 0.00103 -0.00095 C3 1 0.881153 0.867155 0.069568 11.00000 0.02662 0.02929 = 0.02910 -0.00246 -0.00193 -0.00172 AFIX 43 H3A 2 0.906301 0.850331 0.067999 11.00000 -1.20000 AFIX 0 C4 1 0.883367 0.911640 0.081857 11.00000 0.03185 0.03145 = 0.04295 -0.00530 -0.00187 -0.00522 C5 1 0.845680 0.936405 0.079875 11.00000 0.03405 0.02666 = 0.04636 -0.00198 -0.00327 -0.00328 C6 1 0.805748 0.916821 0.069012 11.00000 0.03064 0.02586 = 0.03477 -0.00262 -0.00142 0.00019 AFIX 43 H6A 2 0.780377 0.933307 0.067364 11.00000 -1.20000 AFIX 0 C7 1 0.804195 0.872828 0.060738 11.00000 0.02676 0.02541 = 0.02323 -0.00327 -0.00087 -0.00201 C8 1 0.768596 0.842862 0.046377 11.00000 0.02284 0.02093 = 0.02802 -0.00088 0.00262 0.00112 C9 1 0.926266 0.930825 0.107083 11.00000 0.03155 0.02694 = 0.06364 -0.00315 -0.00826 -0.00450 C10 1 0.959231 0.925129 0.022548 11.00000 0.03620 0.05039 = 0.07875 -0.00428 0.00148 -0.01053 AFIX 43 H10A 2 0.954639 0.909296 -0.052450 11.00000 -1.20000 AFIX 0 C11 1 0.999369 0.942638 0.047194 11.00000 0.03809 0.07618 = 0.11972 -0.00259 0.00559 -0.01816 AFIX 43 H11A 2 1.021846 0.939070 -0.011752 11.00000 -1.20000 AFIX 0 C12 1 1.006341 0.965040 0.156805 11.00000 0.04687 0.06008 = 0.14923 -0.00898 -0.02661 -0.02327 AFIX 43 H12A 2 1.033563 0.977073 0.172972 11.00000 -1.20000 AFIX 0 C13 1 0.973637 0.970083 0.243839 11.00000 0.05387 0.05046 = 0.11264 -0.01959 -0.02981 -0.00748 AFIX 43 H13A 2 0.978564 0.984526 0.321068 11.00000 -1.20000 AFIX 0 C14 1 0.933701 0.953676 0.216032 11.00000 0.04502 0.04363 = 0.06894 -0.01361 -0.01765 -0.00237 AFIX 43 H14A 2 0.910914 0.958266 0.273295 11.00000 -1.20000 AFIX 0 C15 1 0.847133 0.983992 0.086416 11.00000 0.03482 0.02844 = 0.07947 -0.00465 -0.01402 -0.00426 C16 1 0.874094 1.007493 0.009061 11.00000 0.04299 0.03523 = 0.10076 0.00962 -0.01143 -0.00748 AFIX 43 H16A 2 0.892754 0.993155 -0.047169 11.00000 -1.20000 AFIX 0 C17 1 0.873990 1.052096 0.013293 11.00000 0.04803 0.03658 = 0.14266 0.01677 -0.02184 -0.01196 AFIX 43 H17A 2 0.892214 1.067925 -0.040648 11.00000 -1.20000 AFIX 0 C18 1 0.847491 1.072804 0.095570 11.00000 0.05361 0.02542 = 0.20628 -0.00579 -0.03069 -0.00468 AFIX 43 H18A 2 0.847956 1.103032 0.099491 11.00000 -1.20000 AFIX 0 C19 1 0.820153 1.050417 0.172774 11.00000 0.06181 0.03663 = 0.14658 -0.02992 -0.01163 0.00423 AFIX 43 H19A 2 0.801683 1.065079 0.228822 11.00000 -1.20000 AFIX 0 C20 1 0.819923 1.005902 0.167635 11.00000 0.04591 0.03389 = 0.10090 -0.01784 -0.00788 0.00011 AFIX 43 H20A 2 0.800984 0.990369 0.220155 11.00000 -1.20000 AFIX 0 N1A 4 0.736997 0.810900 -0.218990 11.00000 0.02569 0.02535 = 0.02999 0.00102 -0.00212 -0.00010 N2A 4 0.808379 0.840192 -0.236646 11.00000 0.02815 0.02511 = 0.02825 0.00188 0.00278 -0.00053 C1A 1 0.766247 0.843174 -0.231881 11.00000 0.02678 0.02575 = 0.01947 -0.00254 0.00112 -0.00022 C2A 1 0.744112 0.883985 -0.246664 11.00000 0.02688 0.02570 = 0.03174 0.00417 -0.00022 0.00076 C3A 1 0.758472 0.925858 -0.256889 11.00000 0.03029 0.02853 = 0.03929 0.00606 0.00167 -0.00104 AFIX 43 H3AA 2 0.788088 0.932069 -0.256343 11.00000 -1.20000 AFIX 0 C4A 1 0.728442 0.958552 -0.267966 11.00000 0.03715 0.02612 = 0.04432 0.00579 0.00012 0.00154 C5A 1 0.684147 0.949028 -0.266436 11.00000 0.03463 0.02830 = 0.04953 0.00587 0.00008 0.00414 C6A 1 0.670437 0.906709 -0.256765 11.00000 0.02795 0.03039 = 0.04172 0.00336 0.00021 0.00274 AFIX 43 H6AA 2 0.640911 0.900075 -0.256619 11.00000 -1.20000 AFIX 0 C7A 1 0.700580 0.874706 -0.247425 11.00000 0.02853 0.02577 = 0.03321 0.00518 0.00084 0.00074 C8A 1 0.696998 0.828399 -0.232626 11.00000 0.02653 0.02667 = 0.01815 0.00090 -0.00036 0.00118 C9A 1 0.744424 1.002739 -0.286541 11.00000 0.03795 0.02679 = 0.07380 0.01219 -0.00209 0.00057 C10A 1 0.772011 1.021024 -0.200960 11.00000 0.05755 0.03405 = 0.11577 0.00692 -0.02101 -0.00413 AFIX 43 H10B 2 0.781113 1.005099 -0.129827 11.00000 -1.20000 AFIX 0 C11A 1 0.786632 1.062417 -0.217535 11.00000 0.08291 0.04441 = 0.19602 0.01240 -0.05459 -0.02043 AFIX 43 H11B 2 0.804971 1.075022 -0.156930 11.00000 -1.20000 AFIX 0 C12A 1 0.774367 1.084960 -0.322183 11.00000 0.08640 0.04451 = 0.25057 0.05773 -0.03561 -0.02504 AFIX 43 H12B 2 0.784051 1.113393 -0.333058 11.00000 -1.20000 AFIX 0 C13A 1 0.747944 1.066737 -0.412560 11.00000 0.07968 0.05963 = 0.17316 0.06793 -0.01811 -0.01615 AFIX 43 H13B 2 0.740609 1.082058 -0.486576 11.00000 -1.20000 AFIX 0 C14A 1 0.732445 1.025801 -0.392957 11.00000 0.05740 0.04684 = 0.09304 0.02742 -0.00928 -0.00566 AFIX 43 H14B 2 0.713549 1.013446 -0.452511 11.00000 -1.20000 AFIX 0 C15A 1 0.650962 0.983145 -0.271476 11.00000 0.03669 0.02767 = 0.07216 0.00820 0.00510 0.00595 C16A 1 0.653082 1.018779 -0.194961 11.00000 0.04963 0.03532 = 0.09115 -0.00451 0.00915 0.00802 AFIX 3 H16B 2 0.676552 1.022929 -0.142901 11.00000 -1.20000 AFIX 0 C17A 1 0.621196 1.049226 -0.197870 11.00000 0.06299 0.03806 = 0.13881 -0.00857 0.01262 0.01748 AFIX 43 H17B 2 0.623282 1.073656 -0.145451 11.00000 -1.20000 AFIX 0 C18A 1 0.586728 1.044526 -0.275359 11.00000 0.05783 0.04880 = 0.17630 0.00345 0.00040 0.02593 AFIX 43 H18B 2 0.564804 1.065385 -0.275871 11.00000 -1.20000 AFIX 0 C19A 1 0.583937 1.009280 -0.352946 11.00000 0.05138 0.06225 = 0.14117 0.00893 -0.01562 0.01986 AFIX 43 H19B 2 0.560322 1.006084 -0.408067 11.00000 -1.20000 AFIX 0 C20A 1 0.615995 0.978327 -0.350055 11.00000 0.04436 0.04151 = 0.09431 0.00788 -0.00641 0.01057 AFIX 43 H20B 2 0.613801 0.953852 -0.402247 11.00000 -1.20000 AFIX 0 O1 5 0.750000 0.750000 0.224521 10.12500 0.03943 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 REM fin R = New: P4/n REM R1 = 0.0501 for 10732 Fo > 4sig(Fo) and 0.0699 for all 13919 data REM 402 parameters refined using 0 restraints END WGHT 0.0779 0.0000 REM Highest difference peak 3.656, deepest hole -1.342, 1-sigma level 0.101 Q1 1 0.7500 0.7500 -0.1774 10.25000 0.05 3.66 Q2 1 0.7500 0.7500 -0.0085 10.25000 0.05 2.36 Q3 1 0.7500 0.7500 0.3487 10.25000 0.05 2.33 Q4 1 0.7725 0.7297 0.2945 11.00000 0.05 0.70 Q5 1 0.7500 0.7500 -0.2660 10.25000 0.05 0.66 Q6 1 0.7500 0.7500 0.5020 10.25000 0.05 0.62 Q7 1 0.7742 0.7419 -0.0198 11.00000 0.05 0.53 Q8 1 0.8090 0.8404 0.0512 11.00000 0.05 0.42 Q9 1 0.8138 0.7402 -0.1665 11.00000 0.05 0.40 Q10 1 0.8026 0.8740 -0.0163 11.00000 0.05 0.39 Q11 1 0.8084 0.9160 -0.2730 11.00000 0.05 0.38 Q12 1 0.7780 0.7192 -0.0959 11.00000 0.05 0.38 Q13 1 0.7172 0.6998 -0.2205 11.00000 0.05 0.38 Q14 1 0.7789 0.7337 -0.1646 11.00000 0.05 0.37 Q15 1 0.8388 0.8486 -0.0148 11.00000 0.05 0.36 Q16 1 0.7097 0.6689 -0.1643 11.00000 0.05 0.36 Q17 1 0.7231 0.7174 -0.1109 11.00000 0.05 0.36 Q18 1 0.8831 0.7572 0.0553 11.00000 0.05 0.36 Q19 1 0.7446 0.6984 -0.1003 11.00000 0.05 0.35 Q20 1 0.7500 0.7500 0.0729 10.25000 0.05 0.34 Q21 1 0.7123 0.6892 -0.1076 11.00000 0.05 0.33 Q22 1 0.7191 0.7017 0.1033 11.00000 0.05 0.33 Q23 1 0.8069 0.8734 -0.2583 11.00000 0.05 0.32 Q24 1 0.7793 1.0691 -0.2406 11.00000 0.05 0.32 Q25 1 0.7681 1.1236 -0.2719 11.00000 0.05 0.31 Q26 1 0.7633 0.7534 -0.0938 11.00000 0.05 0.31 Q27 1 0.7877 1.1077 -0.4119 11.00000 0.05 0.31 Q28 1 0.7502 1.0734 -0.3601 11.00000 0.05 0.31 Q29 1 0.8707 1.0503 0.0909 11.00000 0.05 0.31 Q30 1 0.8076 0.8400 -0.3205 11.00000 0.05 0.30 ; _shelx_res_checksum 3350 _database_code_depnum_ccdc_archive 'CCDC 946890'