# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Fabrice Pointillart' ; Institut Parisien de Chimie Moleculaire, UMR CNRS 7201 UPMC Universite Paris6 , case 42, 4 place Jussieu, F-75252 Paris cedex 05, France ; K. 'Kamal Boubekeur' ; Institut Parisien de Chimie Moleculaire, UMR CNRS 7201 UPMC Universite Paris6 , case 42, 4 place Jussieu, F-75252 Paris cedex 05, France ; P. 'Patrick Herson' ; Institut Parisien de Chimie Moleculaire, UMR CNRS 7201 UPMC Universite Paris6 , case 42, 4 place Jussieu, F-75252 Paris cedex 05, France ; C. 'Cyrille Train' ; Universite Joseph Fourier BP 53, 38041 Grenoble cedex 9, France ; ? _publ_contact_author_name 'Cyrille Train' _publ_contact_author_email cyrille.train@grenoble.cnrs.fr _publ_section_title ; Barium one-dimensional coordination polymers from barium \^I^2^-diketonates and 2,2\^a-bipyrimidine derivatives ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _publ_contact_author_address ; Universite Joseph Fourier BP 53, 38041 Grenoble cedex 9, France ; _publ_contact_author_fax ? _publ_contact_author_phone ? # Check this file using the IUCr facility at: # http://journals.iucr.org/services/cif/checking/checkfull.html # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica C. The figures have been sent by mail. ; _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' # Attachment '- Data-(1).cif' data_CRYSTALS_cif1 _database_code_depnum_ccdc_archive 'CCDC 757201' #TrackingRef '- Data-(1).cif' _audit_creation_date 05-04-05 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '3091039 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.043(3) _cell_length_b 18.608(5) _cell_length_c 24.308(6) _cell_angle_alpha 90 _cell_angle_beta 100.143(17) _cell_angle_gamma 90 _cell_volume 6252(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ba -0.3244 2.2819 20.3361 3.2160 19.2970 0.2756 10.8880 20.2073 2.6959 167.2020 2.7731 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C49 H29 Ba2 F24 N14 O9' _chemical_formula_moiety 'C49 H29 Ba2 F24 N14 O9' _chemical_compound_source ? _chemical_formula_weight 1687.6 _cell_measurement_reflns_used 85 _cell_measurement_theta_min 4 _cell_measurement_theta_max 17 _cell_measurement_temperature 295(2) _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3268 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.87 # Sheldrick geometric definitions 0.87 0.87 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 295(2) _diffrn_reflns_number 40750 _reflns_number_total 14163 _diffrn_reflns_av_R_equivalents 0.085 # Number of reflections with Friedels Law is 14163 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14372 _diffrn_reflns_theta_min 2.024 _diffrn_reflns_theta_max 27.517 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 20.913 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.44 _refine_diff_density_max 2.00 _refine_ls_number_reflns 9070 _refine_ls_number_restraints 3 _refine_ls_number_parameters 884 #_refine_ls_R_factor_ref 0.0487 _refine_ls_wR_factor_ref 0.0529 _refine_ls_goodness_of_fit_ref 1.0408 #_reflns_number_all 14155 _refine_ls_R_factor_all 0.0879 _refine_ls_wR_factor_all 0.0898 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 9070 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_gt 0.0529 _refine_ls_shift/su_max 0.001298 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refU # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.571 0.551 0.326 ; # Footnote 2 _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ba1 Ba 0.64929(2) 0.300110(17) 0.166237(12) 0.0389 1.0000 Uani . . . . . . Ba2 Ba 0.87595(2) 0.245182(17) -0.092991(12) 0.0407 1.0000 Uani . . . . . . N7 N 0.8856(3) 0.2789(2) 0.02569(17) 0.0405 1.0000 Uani . . . . . . N13 N 0.4914(5) 0.4951(4) 0.0729(3) 0.0778 1.0000 Uani . . . . . . N5 N 0.6384(3) 0.2983(3) 0.04395(17) 0.0414 1.0000 Uani . . . . . . N12 N 0.5353(6) 0.4387(4) 0.5628(3) 0.0919 1.0000 Uani . . . . . . N8 N 0.7072(3) 0.2814(3) -0.03787(17) 0.0446 1.0000 Uani . . . . . . N1 N 0.5685(4) 0.2139(2) 0.2483(2) 0.0493 1.0000 Uani . . . . . . N4 N 0.4516(4) 0.2021(3) 0.30676(19) 0.0502 1.0000 Uani . . . . . . N9 N 0.5061(4) 0.3696(3) 0.4788(3) 0.0671 1.0000 Uani . . . . . . N3 N 0.4709(4) 0.3450(3) 0.3323(2) 0.0586 1.0000 Uani . . . . . . N2 N 0.5625(4) 0.3585(2) 0.2601(2) 0.0534 1.0000 Uani . . . . . . N10 N 0.3149(5) 0.3846(3) 0.4746(3) 0.0760 1.0000 Uani . . . . . . N6 N 0.8172(3) 0.2935(3) 0.10698(17) 0.0472 1.0000 Uani . . . . . . N14 N 0.3745(5) 0.5251(3) -0.0065(3) 0.0718 1.0000 Uani . . . . . . N11 N 0.3458(8) 0.4174(5) 0.5711(4) 0.1203 1.0000 Uani . . . . . . O5 O 0.6595(4) 0.4411(3) 0.1407(2) 0.0712 1.0000 Uani . . . . . . O1 O 0.7843(3) 0.2096(2) 0.21990(19) 0.0611 1.0000 Uani . . . . . . O7 O 0.9232(3) 0.3887(2) -0.07681(19) 0.0572 1.0000 Uani . . . . . . O2 O 0.7839(4) 0.3597(2) 0.24773(19) 0.0667 1.0000 Uani . . . . . . O4 O 0.5495(3) 0.1841(2) 0.11333(19) 0.0586 1.0000 Uani . . . . . . O9 O 0.7303(4) 0.1686(3) -0.1520(2) 0.0751 1.0000 Uani . . . . . . O8 O 0.7432(3) 0.3206(2) -0.16915(18) 0.0602 1.0000 Uani . . . . . . O6 O 1.0668(3) 0.2772(2) -0.0644(2) 0.0591 1.0000 Uani . . . . . . O3 O 0.4568(3) 0.3185(3) 0.1316(2) 0.0711 1.0000 Uani . . . . . . C1 C 0.4633(5) 0.1658(4) 0.1066(3) 0.0660 1.0000 Uani . . . . . . C2 C 0.5512(4) 0.3020(4) 0.0128(2) 0.0530 1.0000 Uani . . . . . . C3 C 0.2504(13) 0.4166(10) 0.5705(9) 0.1701 1.0000 Uani . . . . . . C4 C 0.9737(4) 0.2796(3) 0.0577(2) 0.0457 1.0000 Uani . . . . . . C5 C 0.8331(5) 0.3355(4) 0.2900(3) 0.0679 1.0000 Uani . . . . . . C6 C 0.8379(5) 0.2096(3) 0.2653(3) 0.0628 1.0000 Uani D . . . . . C7 C 0.5114(4) 0.2406(3) 0.2814(2) 0.0426 1.0000 Uani . . . . . . C8 C 0.7122(3) 0.2883(2) 0.01696(18) 0.0305 1.0000 Uani . . . . . . C9 C 0.5375(4) 0.2955(4) -0.0446(2) 0.0594 1.0000 Uani . . . . . . C10 C 0.6175(4) 0.2854(4) -0.0686(2) 0.0550 1.0000 Uani . . . . . . C11 C 0.3868(5) 0.2780(5) 0.1255(4) 0.0766 1.0000 Uani D . . . . . C12 C 0.8114(3) 0.2868(2) 0.05211(19) 0.0314 1.0000 Uani . . . . . . C13 C 0.5667(5) 0.1440(4) 0.2410(3) 0.0590 1.0000 Uani . . . . . . C14 C 0.4482(5) 0.1325(3) 0.2964(3) 0.0591 1.0000 Uani . . . . . . C15 C 1.2266(6) 0.3132(5) -0.0567(6) 0.1083 1.0000 Uani . . . . . . C16 C 0.5066(6) 0.0998(3) 0.2644(3) 0.0620 1.0000 Uani . . . . . . C17 C 0.9992(5) 0.4248(3) -0.0730(2) 0.0509 1.0000 Uani . . . . . . C18 C 0.9062(4) 0.2932(4) 0.1380(2) 0.0587 1.0000 Uani . . . . . . C19 C 0.9867(4) 0.2868(4) 0.1144(2) 0.0572 1.0000 Uani . . . . . . C20 C 0.8657(7) 0.2668(5) 0.3017(3) 0.0851 1.0000 Uani . . . . . . C21 C 0.5260(7) 0.4607(4) 0.3117(3) 0.0776 1.0000 Uani . . . . . . C22 C 0.7515(7) 0.4714(4) 0.1400(4) 0.0901 1.0000 Uani . . . . . . C23 C 1.1195(4) 0.3298(3) -0.0625(3) 0.0545 1.0000 Uani . . . . . . C24 C 0.8787(9) 0.1366(5) 0.2850(6) 0.1096 1.0000 Uani D . . . . . C25 C 1.0935(5) 0.4023(3) -0.0668(3) 0.0616 1.0000 Uani . . . . . . C26 C 0.5156(4) 0.3193(3) 0.2919(2) 0.0439 1.0000 Uani . . . . . . C27 C 0.8617(12) 0.3929(7) 0.3362(5) 0.1297 1.0000 Uani . . . . . . C28 C 0.2933(7) 0.3158(8) 0.1314(10) 0.1464 1.0000 Uani D . . . . . C29 C 0.4789(5) 0.4029(3) 0.5222(3) 0.0647 1.0000 Uani . . . . . . C30 C 0.4776(7) 0.4164(4) 0.3416(3) 0.0752 1.0000 Uani . . . . . . C31 C 0.3842(5) 0.2066(5) 0.1133(4) 0.0877 1.0000 Uani . . . . . . C32 C 0.6342(12) 0.1046(6) -0.2220(5) 0.1288 1.0000 Uani D . . . . . C34 C 0.9826(6) 0.5061(3) -0.0813(4) 0.0704 1.0000 Uani . . . . . . C37 C 0.5666(6) 0.4290(3) 0.2701(3) 0.0713 1.0000 Uani . . . . . . C40 C 0.6004(5) 0.3745(4) 0.4756(4) 0.0767 1.0000 Uani . . . . . . C43 C 0.6767(6) 0.1757(4) -0.1983(3) 0.0765 1.0000 Uani D . . . . . C46 C 0.4635(5) 0.5051(3) 0.0184(3) 0.0619 1.0000 Uani . . . . . . C47 C 0.6902(5) 0.3038(4) -0.2132(3) 0.0665 1.0000 Uani . . . . . . C51 C 0.6681(8) 0.3652(6) -0.2550(4) 0.0956 1.0000 Uani . . . . . . C53 C 0.6525(7) 0.2366(5) -0.2289(3) 0.0854 1.0000 Uani . . . . . . C55 C 0.4254(8) 0.5071(5) 0.1054(4) 0.0902 1.0000 Uani . . . . . . C56 C 0.3316(7) 0.5273(5) 0.0842(4) 0.0881 1.0000 Uani . . . . . . C59 C 0.3097(6) 0.5348(4) 0.0272(4) 0.0819 1.0000 Uani . . . . . . C61 C 0.3741(7) 0.4022(4) 0.5233(4) 0.0741 1.0000 Uani . . . . . . C63 C 0.6286(8) 0.4415(6) 0.5581(5) 0.1038 1.0000 Uani . . . . . . C65 C 0.6638(6) 0.4106(5) 0.5161(5) 0.0951 1.0000 Uani . . . . . . C70 C 0.4457(6) 0.0874(5) 0.0865(5) 0.1025 1.0000 Uani . . . . . . C71 C 0.2193(7) 0.3902(5) 0.4739(5) 0.0966 1.0000 Uani . . . . . . C73 C 0.1824(10) 0.4074(8) 0.5214(8) 0.1400 1.0000 Uani . . . . . . F1 F 0.3012(10) 0.3406(15) 0.1798(10) 0.3856 1.0000 Uani . . . . . . F2 F 0.2193(5) 0.2735(5) 0.1281(7) 0.2500 1.0000 Uani . . . . . . F3 F 0.5608(10) 0.1119(5) -0.2627(5) 0.2401 1.0000 Uani . . . . . . F4 F 0.6160(12) 0.0597(6) -0.1890(4) 0.2695 1.0000 Uani . . . . . . F5 F 0.9293(11) 0.1306(5) 0.3295(4) 0.2846 1.0000 Uani . . . . . . F6 F 0.2714(7) 0.3650(6) 0.0984(10) 0.2947 1.0000 Uani . . . . . . F7 F 1.2862(4) 0.3653(4) -0.0481(5) 0.1731 1.0000 Uani . . . . . . F8 F 1.2532(5) 0.2628(5) -0.0235(6) 0.2127 1.0000 Uani . . . . . . F9 F 1.2420(7) 0.2827(8) -0.1021(7) 0.2425 1.0000 Uani . . . . . . F10 F 0.9352(8) 0.3754(5) 0.3737(4) 0.2132 1.0000 Uani . . . . . . F11 F 0.6938(12) 0.0695(6) -0.2459(8) 0.2624 1.0000 Uani . . . . . . F12 F 0.8705(9) 0.4553(4) 0.3177(4) 0.2173 1.0000 Uani . . . . . . F13 F 0.8102(10) 0.0903(6) 0.2811(8) 0.2882 1.0000 Uani . . . . . . F14 F 0.9164(12) 0.1048(6) 0.2497(6) 0.2433 1.0000 Uani . . . . . . F20 F 0.7869(12) 0.3963(7) 0.3655(5) 0.2309 1.0000 Uani . . . . . . F23 F 0.9073(5) 0.5288(3) -0.0635(4) 0.1342 1.0000 Uani . . . . . . F24 F 0.9790(8) 0.5240(3) -0.1324(2) 0.1601 1.0000 Uani . . . . . . F27 F 1.0530(5) 0.5457(2) -0.0527(3) 0.1149 1.0000 Uani . . . . . . F28 F 0.6463(6) 0.4252(4) -0.2315(3) 0.1495 1.0000 Uani . . . . . . F30 F 0.4299(6) 0.0846(4) 0.0318(4) 0.1474 1.0000 Uani . . . . . . F35 F 0.5949(6) 0.3525(4) -0.2962(3) 0.1578 1.0000 Uani . . . . . . F38 F 0.5189(5) 0.0470(3) 0.1047(4) 0.1645 1.0000 Uani . . . . . . F42 F 0.7424(7) 0.3784(5) -0.2797(4) 0.1722 1.0000 Uani . . . . . . F58 F 0.3671(5) 0.0582(3) 0.1020(4) 0.1523 1.0000 Uani . . . . . . H21 H 0.4936 0.3098 0.0315 0.127(8) 1.0000 Uiso . . . . . . H31 H 0.2283 0.4204 0.6092 0.127(8) 1.0000 Uiso . . . . . . H41 H 1.0321 0.2746 0.0392 0.127(8) 1.0000 Uiso . . . . . . H91 H 0.4711 0.2982 -0.0677 0.127(8) 1.0000 Uiso . . . . . . H101 H 0.6093 0.2806 -0.1105 0.127(8) 1.0000 Uiso . . . . . . H131 H 0.6115 0.1224 0.2174 0.127(8) 1.0000 Uiso . . . . . . H141 H 0.4004 0.1023 0.3125 0.127(8) 1.0000 Uiso . . . . . . H161 H 0.5052 0.0462 0.2584 0.127(8) 1.0000 Uiso . . . . . . H181 H 0.9135 0.2983 0.1797 0.127(8) 1.0000 Uiso . . . . . . H191 H 1.0531 0.2869 0.1377 0.127(8) 1.0000 Uiso . . . . . . H201 H 0.9104 0.2571 0.3382 0.127(8) 1.0000 Uiso . . . . . . H211 H 0.5333 0.5137 0.3198 0.127(8) 1.0000 Uiso . . . . . . H251 H 1.1461 0.4395 -0.0650 0.127(8) 1.0000 Uiso . . . . . . H301 H 0.4447 0.4376 0.3717 0.127(8) 1.0000 Uiso . . . . . . H311 H 0.3196 0.1812 0.1087 0.127(8) 1.0000 Uiso . . . . . . H371 H 0.6007 0.4605 0.2459 0.127(8) 1.0000 Uiso . . . . . . H401 H 0.6249 0.3518 0.4425 0.127(8) 1.0000 Uiso . . . . . . H531 H 0.6049 0.2327 -0.2651 0.127(8) 1.0000 Uiso . . . . . . H551 H 0.4448 0.5006 0.1472 0.127(8) 1.0000 Uiso . . . . . . H561 H 0.2823 0.5357 0.1091 0.127(8) 1.0000 Uiso . . . . . . H591 H 0.2414 0.5489 0.0100 0.127(8) 1.0000 Uiso . . . . . . H631 H 0.6757 0.4684 0.5879 0.127(8) 1.0000 Uiso . . . . . . H651 H 0.7354 0.4138 0.5139 0.127(8) 1.0000 Uiso . . . . . . H711 H 0.1727 0.3805 0.4371 0.127(8) 1.0000 Uiso . . . . . . H731 H 0.1094 0.4153 0.5203 0.127(8) 1.0000 Uiso . . . . . . 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 Ba1 0.03759(14) 0.04114(16) 0.03788(14) 0.00096(12) 0.00646(10) -0.00409(12) Ba2 0.04265(15) 0.04020(17) 0.04024(15) -0.00743(13) 0.01018(11) -0.00468(13) N7 0.034(2) 0.047(2) 0.039(2) -0.0093(17) 0.0039(17) -0.0050(17) N13 0.080(4) 0.071(4) 0.077(4) 0.015(3) -0.004(3) 0.005(3) N5 0.0298(18) 0.055(3) 0.0376(19) 0.0006(19) 0.0002(15) 0.0025(18) N12 0.103(6) 0.070(4) 0.093(5) -0.023(4) -0.008(4) 0.010(4) N8 0.034(2) 0.062(3) 0.035(2) -0.0047(19) -0.0029(16) 0.0005(18) N1 0.066(3) 0.029(2) 0.057(3) 0.0041(19) 0.022(2) 0.004(2) N4 0.063(3) 0.043(2) 0.048(2) 0.004(2) 0.019(2) -0.008(2) N9 0.066(3) 0.054(3) 0.083(4) -0.007(3) 0.016(3) 0.000(3) N3 0.081(3) 0.044(3) 0.057(3) 0.007(2) 0.030(3) 0.011(2) N2 0.074(3) 0.034(2) 0.057(3) 0.001(2) 0.025(2) -0.002(2) N10 0.070(4) 0.057(3) 0.099(5) -0.009(3) 0.010(3) 0.005(3) N6 0.033(2) 0.074(3) 0.0328(19) 0.002(2) -0.0006(16) 0.001(2) N14 0.072(4) 0.049(3) 0.087(4) 0.010(3) -0.008(3) 0.003(3) N11 0.147(8) 0.120(7) 0.103(6) -0.033(5) 0.050(6) -0.002(6) O5 0.081(3) 0.056(3) 0.072(3) 0.016(2) 0.002(2) -0.004(2) O1 0.071(3) 0.048(2) 0.063(3) 0.0004(19) 0.006(2) 0.011(2) O7 0.062(2) 0.044(2) 0.065(3) -0.0083(19) 0.011(2) 0.0018(19) O2 0.078(3) 0.050(2) 0.062(3) 0.000(2) -0.018(2) -0.001(2) O4 0.048(2) 0.050(2) 0.074(3) -0.002(2) 0.0013(19) -0.0089(18) O9 0.084(3) 0.069(3) 0.064(3) 0.000(2) -0.010(3) -0.031(3) O8 0.061(2) 0.058(3) 0.058(2) -0.0073(19) -0.001(2) -0.001(2) O6 0.046(2) 0.040(2) 0.091(3) 0.003(2) 0.010(2) -0.0033(17) O3 0.046(2) 0.069(3) 0.100(4) 0.006(3) 0.015(2) 0.004(2) C1 0.064(4) 0.050(4) 0.077(4) 0.013(3) -0.007(3) -0.015(3) C2 0.036(2) 0.068(4) 0.052(3) 0.001(3) 0.000(2) 0.004(3) C3 0.141(12) 0.196(16) 0.204(17) -0.075(14) 0.113(13) -0.024(11) C4 0.032(2) 0.053(3) 0.050(3) -0.005(2) 0.003(2) -0.001(2) C5 0.071(4) 0.055(4) 0.067(4) -0.005(3) -0.014(3) -0.004(3) C6 0.065(4) 0.056(4) 0.066(4) 0.016(3) 0.006(3) 0.017(3) C7 0.051(3) 0.040(3) 0.038(2) 0.005(2) 0.011(2) 0.001(2) C8 0.031(2) 0.025(2) 0.034(2) 0.0019(16) -0.0006(17) -0.0032(16) C9 0.034(2) 0.088(5) 0.051(3) -0.001(3) -0.008(2) -0.001(3) C10 0.041(3) 0.080(4) 0.040(3) -0.004(3) -0.006(2) 0.004(3) C11 0.042(3) 0.090(6) 0.100(6) 0.016(4) 0.017(3) 0.004(3) C12 0.029(2) 0.030(2) 0.033(2) 0.0017(17) 0.0006(17) 0.0003(17) C13 0.072(4) 0.053(4) 0.056(3) 0.000(3) 0.020(3) 0.006(3) C14 0.076(4) 0.046(3) 0.056(3) -0.002(3) 0.014(3) -0.017(3) C15 0.065(5) 0.064(5) 0.204(13) 0.009(6) 0.046(6) 0.005(4) C16 0.092(5) 0.036(3) 0.058(4) 0.002(3) 0.014(3) -0.003(3) C17 0.067(4) 0.033(3) 0.051(3) -0.003(2) 0.004(3) -0.003(2) C18 0.036(3) 0.096(5) 0.041(3) -0.001(3) -0.004(2) -0.003(3) C19 0.031(2) 0.083(4) 0.052(3) 0.002(3) -0.009(2) -0.002(3) C20 0.097(6) 0.078(5) 0.065(4) 0.008(4) -0.028(4) 0.019(4) C21 0.123(7) 0.034(3) 0.083(5) 0.003(3) 0.038(5) 0.009(4) C22 0.092(6) 0.057(4) 0.120(7) 0.023(4) 0.015(5) -0.016(4) C23 0.047(3) 0.041(3) 0.076(4) 0.001(3) 0.012(3) 0.001(2) C24 0.120(8) 0.075(7) 0.129(9) 0.026(6) 0.012(7) 0.039(6) C25 0.055(3) 0.039(3) 0.089(5) 0.008(3) 0.008(3) -0.008(3) C26 0.054(3) 0.035(3) 0.044(3) 0.004(2) 0.013(2) 0.003(2) C27 0.173(13) 0.096(8) 0.093(8) -0.034(6) -0.051(8) 0.009(8) C28 0.068(6) 0.123(11) 0.26(2) -0.002(12) 0.063(10) 0.007(7) C29 0.081(4) 0.035(3) 0.076(4) -0.005(3) 0.005(4) 0.003(3) C30 0.120(6) 0.040(3) 0.075(4) 0.005(3) 0.043(4) 0.016(4) C31 0.041(3) 0.077(5) 0.141(8) 0.028(5) 0.004(4) -0.004(3) C32 0.186(13) 0.091(8) 0.091(7) -0.022(6) -0.027(8) -0.066(9) C34 0.081(5) 0.037(3) 0.090(5) -0.002(3) 0.006(4) 0.007(3) C37 0.107(6) 0.035(3) 0.079(5) 0.005(3) 0.037(4) 0.000(3) C40 0.063(4) 0.045(4) 0.119(7) -0.010(4) 0.010(4) -0.009(3) C43 0.085(5) 0.080(5) 0.059(4) -0.019(4) -0.001(4) -0.030(4) C46 0.074(4) 0.030(3) 0.073(4) 0.006(3) -0.009(3) -0.006(3) C47 0.063(4) 0.082(5) 0.051(3) -0.002(3) 0.002(3) 0.001(4) C51 0.103(7) 0.093(7) 0.078(5) 0.013(5) -0.018(5) 0.007(5) C53 0.103(6) 0.085(6) 0.055(4) -0.009(4) -0.021(4) -0.021(5) C55 0.099(6) 0.091(6) 0.075(5) 0.013(4) 0.002(5) 0.009(5) C56 0.089(6) 0.075(5) 0.098(6) 0.001(5) 0.010(5) -0.003(4) C59 0.076(5) 0.059(4) 0.104(6) 0.010(4) -0.003(5) -0.002(4) C61 0.099(6) 0.041(3) 0.087(5) -0.006(3) 0.031(5) 0.010(3) C63 0.099(7) 0.087(7) 0.113(8) -0.036(6) -0.013(6) -0.002(5) C65 0.067(5) 0.068(5) 0.142(9) -0.015(5) -0.004(5) -0.001(4) C70 0.070(5) 0.082(6) 0.139(9) 0.016(6) -0.028(6) -0.024(5) C71 0.078(5) 0.068(5) 0.148(9) -0.020(5) 0.032(6) 0.008(4) C73 0.098(8) 0.135(11) 0.196(15) -0.058(11) 0.050(9) 0.002(7) F1 0.134(10) 0.58(4) 0.47(3) -0.26(3) 0.129(14) 0.053(15) F2 0.054(3) 0.183(8) 0.53(2) 0.037(11) 0.104(7) 0.002(4) F3 0.307(14) 0.137(7) 0.203(9) -0.031(6) -0.153(10) -0.056(8) F4 0.44(2) 0.184(9) 0.147(7) 0.013(7) -0.037(10) -0.236(12) F5 0.47(2) 0.120(6) 0.175(8) -0.021(5) -0.179(11) 0.154(10) F6 0.106(6) 0.135(8) 0.65(3) 0.122(14) 0.073(11) 0.070(6) F7 0.052(3) 0.099(4) 0.363(13) 0.030(6) 0.023(5) -0.016(3) F8 0.069(4) 0.133(6) 0.414(18) 0.123(9) -0.019(6) 0.007(4) F9 0.122(7) 0.298(15) 0.330(17) -0.088(14) 0.099(9) 0.043(8) F10 0.267(11) 0.158(7) 0.150(6) -0.049(5) -0.139(8) 0.021(7) F11 0.338(19) 0.120(7) 0.350(18) -0.126(10) 0.118(16) -0.059(10) F12 0.323(14) 0.067(4) 0.198(9) -0.028(5) -0.129(9) -0.019(6) F13 0.248(13) 0.114(7) 0.47(2) 0.179(11) -0.022(15) 0.012(8) F14 0.337(17) 0.148(8) 0.242(12) -0.020(8) 0.043(12) 0.151(11) F20 0.327(17) 0.208(12) 0.147(8) -0.103(8) 0.015(10) 0.034(11) F23 0.125(5) 0.048(3) 0.236(8) -0.001(4) 0.050(5) 0.029(3) F24 0.340(12) 0.052(3) 0.080(3) 0.019(2) 0.010(5) 0.032(4) F27 0.138(5) 0.037(2) 0.153(5) -0.009(3) -0.019(4) -0.009(3) F28 0.207(8) 0.082(4) 0.134(5) 0.010(4) -0.042(5) 0.026(4) F30 0.175(7) 0.104(5) 0.146(6) -0.029(4) -0.019(5) -0.015(5) F35 0.189(7) 0.143(6) 0.106(5) 0.010(4) -0.072(5) 0.012(5) F38 0.109(5) 0.053(3) 0.303(11) 0.019(4) -0.044(5) 0.007(3) F42 0.173(7) 0.192(8) 0.154(7) 0.105(6) 0.036(6) 0.012(6) F58 0.114(5) 0.087(4) 0.252(9) 0.017(5) 0.022(5) -0.051(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.06667(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ba1 . N5 . 2.950(4) yes Ba1 . N1 . 2.939(5) yes Ba1 . N2 . 2.974(5) yes Ba1 . N6 . 2.974(4) yes Ba1 . O5 . 2.707(5) yes Ba1 . O1 . 2.695(4) yes Ba1 . O2 . 2.721(4) yes Ba1 . O4 . 2.763(4) yes Ba1 . O3 . 2.708(4) yes Ba2 . N3 4_554 2.957(5) yes Ba2 . N4 4_554 2.991(5) yes Ba2 . N10 4_554 3.124(6) yes Ba2 . N9 4_554 3.136(6) yes Ba2 . N7 . 2.931(4) yes Ba2 . N8 . 2.998(4) yes Ba2 . O7 . 2.763(4) yes Ba2 . O9 . 2.690(4) yes Ba2 . O8 . 2.768(4) yes Ba2 . O6 . 2.713(4) yes N7 . C4 . 1.341(6) yes N7 . C12 . 1.325(6) yes N13 . C46 . 1.327(9) yes N13 . C55 . 1.338(12) yes N5 . C2 . 1.323(6) yes N5 . C8 . 1.334(6) yes N12 . C29 . 1.331(10) yes N12 . C63 . 1.337(13) yes N8 . C8 . 1.328(6) yes N8 . C10 . 1.348(7) yes N1 . C7 . 1.327(7) yes N1 . C13 . 1.313(8) yes N4 . C7 . 1.335(7) yes N4 . C14 . 1.318(8) yes N9 . C29 . 1.334(9) yes N9 . C40 . 1.343(9) yes N3 . C26 . 1.345(7) yes N3 . C30 . 1.347(9) yes N2 . C26 . 1.321(7) yes N2 . C37 . 1.333(8) yes N10 . C61 . 1.361(11) yes N10 . C71 . 1.344(11) yes N6 . C12 . 1.328(6) yes N6 . C18 . 1.342(7) yes N14 . C46 . 1.343(9) yes N14 . C59 . 1.340(11) yes N11 . C3 . 1.337(17) yes N11 . C61 . 1.323(11) yes O5 . C22 . 1.412(10) yes O1 . C6 . 1.222(8) yes O7 . C17 . 1.250(7) yes O2 . C5 . 1.219(8) yes O4 . C1 . 1.240(8) yes O9 . C43 . 1.245(9) yes O8 . C47 . 1.232(8) yes O6 . C23 . 1.224(7) yes O3 . C11 . 1.226(9) yes C1 . C31 . 1.378(11) yes C1 . C70 . 1.543(12) yes C2 . C9 . 1.380(8) yes C2 . H21 . 1.006 no C3 . C73 . 1.40(2) yes C3 . H31 . 1.044 no C4 . C19 . 1.365(8) yes C4 . H41 . 1.006 no C5 . C20 . 1.372(11) yes C5 . C27 . 1.551(12) yes C6 . C20 . 1.394(11) yes C6 . C24 . 1.519(7) yes C7 . C26 . 1.485(7) yes C8 . C12 . 1.501(6) yes C9 . C10 . 1.368(8) yes C9 . H91 . 1.002 no C10 . H101 . 1.008 no C11 . C28 . 1.519(8) yes C11 . C31 . 1.361(12) yes C13 . C16 . 1.372(9) yes C13 . H131 . 1.006 no C14 . C16 . 1.367(10) yes C14 . H141 . 1.006 no C15 . C23 . 1.518(10) yes C15 . F7 . 1.273(11) yes C15 . F8 . 1.251(14) yes C15 . F9 . 1.291(17) yes C16 . H161 . 1.008 no C17 . C25 . 1.372(9) yes C17 . C34 . 1.538(8) yes C18 . C19 . 1.361(8) yes C18 . H181 . 1.004 no C19 . H191 . 1.002 no C20 . H201 . 1.008 no C21 . C30 . 1.359(10) yes C21 . C37 . 1.377(10) yes C21 . H211 . 1.008 no C23 . C25 . 1.397(9) yes C24 . F5 . 1.190(13) yes C24 . F13 . 1.282(16) yes C24 . F14 . 1.235(15) yes C25 . H251 . 1.008 no C27 . F10 . 1.292(13) yes C27 . F12 . 1.260(16) yes C27 . F20 . 1.371(19) yes C28 . F1 . 1.25(2) yes C28 . F2 . 1.295(15) yes C28 . F6 . 1.22(2) yes C29 . C61 . 1.476(11) yes C30 . H301 . 1.012 no C31 . H311 . 1.010 no C32 . C43 . 1.524(8) yes C32 . F3 . 1.304(15) yes C32 . F4 . 1.217(14) yes C32 . F11 . 1.28(2) yes C34 . F23 . 1.284(10) yes C34 . F24 . 1.277(10) yes C34 . F27 . 1.326(9) yes C37 . H371 . 1.009 no C40 . C65 . 1.379(12) yes C40 . H401 . 1.021 no C43 . C53 . 1.366(12) yes C46 . C46 2_665 1.486(15) yes C47 . C51 . 1.524(12) yes C47 . C53 . 1.385(11) yes C51 . F28 . 1.314(12) yes C51 . F35 . 1.325(10) yes C51 . F42 . 1.316(13) yes C53 . H531 . 1.008 no C55 . C56 . 1.380(13) yes C55 . H551 . 1.013 no C56 . C59 . 1.372(13) yes C56 . H561 . 1.009 no C59 . H591 . 1.012 no C63 . C65 . 1.340(15) yes C63 . H631 . 1.021 no C65 . H651 . 1.017 no C70 . F30 . 1.309(14) yes C70 . F38 . 1.287(11) yes C70 . F58 . 1.343(12) yes C71 . C73 . 1.384(17) yes C71 . H711 . 1.028 no C73 . H731 . 1.032 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N5 . Ba1 . N1 . 136.08(13) yes N5 . Ba1 . N2 . 145.19(13) yes N1 . Ba1 . N2 . 54.52(13) yes N5 . Ba1 . N6 . 54.30(11) yes N1 . Ba1 . N6 . 137.71(13) yes N2 . Ba1 . N6 . 148.59(13) yes N5 . Ba1 . O5 . 76.99(15) yes N1 . Ba1 . O5 . 136.67(15) yes N2 . Ba1 . O5 . 82.37(15) yes N6 . Ba1 . O5 . 81.41(16) yes N5 . Ba1 . O1 . 112.85(13) yes N1 . Ba1 . O1 . 69.68(14) yes N2 . Ba1 . O1 . 101.86(14) yes N6 . Ba1 . O1 . 70.03(14) yes O5 . Ba1 . O1 . 131.01(15) yes N5 . Ba1 . O2 . 130.12(14) yes N1 . Ba1 . O2 . 91.70(15) yes N2 . Ba1 . O2 . 67.60(15) yes N6 . Ba1 . O2 . 82.03(14) yes O5 . Ba1 . O2 . 73.39(15) yes N5 . Ba1 . O4 . 65.82(13) yes N1 . Ba1 . O4 . 70.42(14) yes N2 . Ba1 . O4 . 113.52(14) yes N6 . Ba1 . O4 . 97.04(14) yes O5 . Ba1 . O4 . 133.89(14) yes N5 . Ba1 . O3 . 79.42(14) yes N1 . Ba1 . O3 . 78.26(15) yes N2 . Ba1 . O3 . 70.75(16) yes N6 . Ba1 . O3 . 133.47(14) yes O5 . Ba1 . O3 . 84.03(16) yes O1 . Ba1 . O2 . 64.09(14) yes O1 . Ba1 . O4 . 89.60(13) yes O2 . Ba1 . O4 . 152.49(13) yes O1 . Ba1 . O3 . 143.93(15) yes O2 . Ba1 . O3 . 134.57(16) yes O4 . Ba1 . O3 . 63.75(14) yes N3 4_554 Ba2 . N4 4_554 54.74(13) yes N3 4_554 Ba2 . N10 4_554 94.54(16) yes N4 4_554 Ba2 . N10 4_554 148.43(16) yes N3 4_554 Ba2 . N9 4_554 70.94(16) yes N4 4_554 Ba2 . N9 4_554 114.94(14) yes N10 4_554 Ba2 . N9 4_554 50.75(16) yes N3 4_554 Ba2 . N7 . 141.04(14) yes N4 4_554 Ba2 . N7 . 140.37(13) yes N10 4_554 Ba2 . N7 . 67.49(16) yes N9 4_554 Ba2 . N7 . 71.10(15) yes N3 4_554 Ba2 . N8 . 151.61(13) yes N4 4_554 Ba2 . N8 . 135.44(13) yes N10 4_554 Ba2 . N8 . 68.13(16) yes N9 4_554 Ba2 . N8 . 109.50(14) yes N7 . Ba2 . N8 . 54.22(11) yes N3 4_554 Ba2 . O7 . 120.86(13) yes N4 4_554 Ba2 . O7 . 71.80(13) yes N10 4_554 Ba2 . O7 . 138.90(16) yes N9 4_554 Ba2 . O7 . 118.54(15) yes N7 . Ba2 . O7 . 71.66(13) yes N3 4_554 Ba2 . O9 . 75.83(17) yes N4 4_554 Ba2 . O9 . 94.90(15) yes N10 4_554 Ba2 . O9 . 67.54(17) yes N9 4_554 Ba2 . O9 . 104.49(16) yes N7 . Ba2 . O9 . 122.46(14) yes N3 4_554 Ba2 . O8 . 101.58(15) yes N4 4_554 Ba2 . O8 . 65.31(14) yes N10 4_554 Ba2 . O8 . 121.96(16) yes N9 4_554 Ba2 . O8 . 167.49(14) yes N7 . Ba2 . O8 . 117.32(13) yes N3 4_554 Ba2 . O6 . 75.50(15) yes N4 4_554 Ba2 . O6 . 70.13(15) yes N10 4_554 Ba2 . O6 . 112.61(16) yes N9 4_554 Ba2 . O6 . 63.51(14) yes N7 . Ba2 . O6 . 80.14(13) yes N8 . Ba2 . O7 . 84.70(13) yes N8 . Ba2 . O9 . 76.73(15) yes O7 . Ba2 . O9 . 136.75(15) yes N8 . Ba2 . O8 . 72.08(13) yes O7 . Ba2 . O8 . 73.81(13) yes O9 . Ba2 . O8 . 63.42(15) yes N8 . Ba2 . O6 . 131.24(13) yes O7 . Ba2 . O6 . 63.28(13) yes O9 . Ba2 . O6 . 151.23(16) yes O8 . Ba2 . O6 . 125.36(14) yes Ba2 . N7 . C4 . 116.8(3) yes Ba2 . N7 . C12 . 126.6(3) yes C4 . N7 . C12 . 116.2(4) yes C46 . N13 . C55 . 116.9(7) yes Ba1 . N5 . C2 . 117.0(3) yes Ba1 . N5 . C8 . 126.2(3) yes C2 . N5 . C8 . 116.6(4) yes C29 . N12 . C63 . 114.8(8) yes Ba2 . N8 . C8 . 124.3(3) yes Ba2 . N8 . C10 . 120.0(3) yes C8 . N8 . C10 . 115.5(4) yes Ba1 . N1 . C7 . 123.6(3) yes Ba1 . N1 . C13 . 116.7(4) yes C7 . N1 . C13 . 117.0(5) yes Ba2 4_455 N4 . C7 . 122.9(4) yes Ba2 4_455 N4 . C14 . 118.2(4) yes C7 . N4 . C14 . 116.3(5) yes Ba2 4_455 N9 . C29 . 122.4(5) yes Ba2 4_455 N9 . C40 . 119.9(5) yes C29 . N9 . C40 . 115.9(7) yes Ba2 4_455 N3 . C26 . 124.5(4) yes Ba2 4_455 N3 . C30 . 118.8(4) yes C26 . N3 . C30 . 116.5(5) yes Ba1 . N2 . C26 . 124.1(4) yes Ba1 . N2 . C37 . 119.3(4) yes C26 . N2 . C37 . 116.6(5) yes Ba2 4_455 N10 . C61 . 117.5(4) yes Ba2 4_455 N10 . C71 . 114.8(5) yes C61 . N10 . C71 . 116.5(8) yes Ba1 . N6 . C12 . 125.3(3) yes Ba1 . N6 . C18 . 117.8(3) yes C12 . N6 . C18 . 116.8(4) yes C46 . N14 . C59 . 116.1(7) yes C3 . N11 . C61 . 116.3(12) yes Ba1 . O5 . C22 . 118.4(4) yes Ba1 . O1 . C6 . 135.0(4) yes Ba2 . O7 . C17 . 135.2(4) yes Ba1 . O2 . C5 . 132.9(4) yes Ba1 . O4 . C1 . 132.8(5) yes Ba2 . O9 . C43 . 134.9(5) yes Ba2 . O8 . C47 . 133.4(5) yes Ba2 . O6 . C23 . 138.5(4) yes Ba1 . O3 . C11 . 134.0(5) yes O4 . C1 . C31 . 128.4(7) yes O4 . C1 . C70 . 113.5(7) yes C31 . C1 . C70 . 118.1(7) yes N5 . C2 . C9 . 121.5(5) yes N5 . C2 . H21 . 119.108 no C9 . C2 . H21 . 119.353 no N11 . C3 . C73 . 122.8(13) yes N11 . C3 . H31 . 116.507 no C73 . C3 . H31 . 120.590 no N7 . C4 . C19 . 122.2(5) yes N7 . C4 . H41 . 118.757 no C19 . C4 . H41 . 119.029 no O2 . C5 . C20 . 129.8(7) yes O2 . C5 . C27 . 113.1(7) yes C20 . C5 . C27 . 117.1(7) yes O1 . C6 . C20 . 129.1(6) yes O1 . C6 . C24 . 115.1(8) yes C20 . C6 . C24 . 115.7(8) yes N4 . C7 . N1 . 125.1(5) yes N4 . C7 . C26 . 117.4(5) yes N1 . C7 . C26 . 117.5(4) yes N5 . C8 . N8 . 126.8(4) yes N5 . C8 . C12 . 116.5(4) yes N8 . C8 . C12 . 116.7(4) yes C2 . C9 . C10 . 117.8(5) yes C2 . C9 . H91 . 120.902 no C10 . C9 . H91 . 121.324 no C9 . C10 . N8 . 121.9(5) yes C9 . C10 . H101 . 119.150 no N8 . C10 . H101 . 118.992 no O3 . C11 . C28 . 113.0(8) yes O3 . C11 . C31 . 128.2(7) yes C28 . C11 . C31 . 118.8(8) yes C8 . C12 . N6 . 117.1(4) yes C8 . C12 . N7 . 117.2(4) yes N6 . C12 . N7 . 125.7(4) yes N1 . C13 . C16 . 122.5(6) yes N1 . C13 . H131 . 118.325 no C16 . C13 . H131 . 119.211 no N4 . C14 . C16 . 122.7(6) yes N4 . C14 . H141 . 118.489 no C16 . C14 . H141 . 118.817 no C23 . C15 . F7 . 118.1(8) yes C23 . C15 . F8 . 113.1(9) yes F7 . C15 . F8 . 110.6(11) yes C23 . C15 . F9 . 108.8(11) yes F7 . C15 . F9 . 105.6(11) yes F8 . C15 . F9 . 98.5(11) yes C13 . C16 . C14 . 116.3(6) yes C13 . C16 . H161 . 122.091 no C14 . C16 . H161 . 121.585 no O7 . C17 . C25 . 129.7(5) yes O7 . C17 . C34 . 114.2(6) yes C25 . C17 . C34 . 115.8(6) yes N6 . C18 . C19 . 121.6(5) yes N6 . C18 . H181 . 119.168 no C19 . C18 . H181 . 119.235 no C4 . C19 . C18 . 117.5(5) yes C4 . C19 . H191 . 121.049 no C18 . C19 . H191 . 121.463 no C6 . C20 . C5 . 122.2(6) yes C6 . C20 . H201 . 118.828 no C5 . C20 . H201 . 118.928 no C30 . C21 . C37 . 116.4(6) yes C30 . C21 . H211 . 122.159 no C37 . C21 . H211 . 121.445 no C15 . C23 . O6 . 115.0(6) yes C15 . C23 . C25 . 116.5(6) yes O6 . C23 . C25 . 128.4(6) yes C6 . C24 . F5 . 120.2(11) yes C6 . C24 . F13 . 109.9(9) yes F5 . C24 . F13 . 108.9(14) yes C6 . C24 . F14 . 113.2(11) yes F5 . C24 . F14 . 109.0(12) yes F13 . C24 . F14 . 92.0(13) yes C23 . C25 . C17 . 122.5(6) yes C23 . C25 . H251 . 118.741 no C17 . C25 . H251 . 118.721 no C7 . C26 . N3 . 117.8(5) yes C7 . C26 . N2 . 117.0(5) yes N3 . C26 . N2 . 125.2(5) yes C5 . C27 . F10 . 114.3(10) yes C5 . C27 . F12 . 113.9(11) yes F10 . C27 . F12 . 111.6(12) yes C5 . C27 . F20 . 106.5(11) yes F10 . C27 . F20 . 103.6(13) yes F12 . C27 . F20 . 105.9(13) yes C11 . C28 . F1 . 108.9(16) yes C11 . C28 . F2 . 114.3(11) yes F1 . C28 . F2 . 102.6(18) yes C11 . C28 . F6 . 114.1(15) yes F1 . C28 . F6 . 108.2(17) yes F2 . C28 . F6 . 108.0(15) yes N9 . C29 . N12 . 127.0(8) yes N9 . C29 . C61 . 115.8(6) yes N12 . C29 . C61 . 117.1(7) yes C21 . C30 . N3 . 122.3(6) yes C21 . C30 . H301 . 119.068 no N3 . C30 . H301 . 118.606 no C1 . C31 . C11 . 124.9(6) yes C1 . C31 . H311 . 117.135 no C11 . C31 . H311 . 118.000 no C43 . C32 . F3 . 113.6(11) yes C43 . C32 . F4 . 117.4(10) yes F3 . C32 . F4 . 110.0(13) yes C43 . C32 . F11 . 111.8(13) yes F3 . C32 . F11 . 101.7(12) yes F4 . C32 . F11 . 100.4(15) yes C17 . C34 . F23 . 113.2(7) yes C17 . C34 . F24 . 111.4(6) yes F23 . C34 . F24 . 110.3(8) yes C17 . C34 . F27 . 113.3(6) yes F23 . C34 . F27 . 102.8(7) yes F24 . C34 . F27 . 105.2(7) yes C21 . C37 . N2 . 123.0(6) yes C21 . C37 . H371 . 118.672 no N2 . C37 . H371 . 118.303 no N9 . C40 . C65 . 120.8(8) yes N9 . C40 . H401 . 119.399 no C65 . C40 . H401 . 119.838 no C32 . C43 . O9 . 112.5(8) yes C32 . C43 . C53 . 118.1(8) yes O9 . C43 . C53 . 129.4(6) yes C46 2_665 C46 . N14 . 116.7(8) yes C46 2_665 C46 . N13 . 118.0(8) yes N14 . C46 . N13 . 125.3(7) yes O8 . C47 . C51 . 114.3(7) yes O8 . C47 . C53 . 127.6(7) yes C51 . C47 . C53 . 118.1(7) yes C47 . C51 . F28 . 112.6(8) yes C47 . C51 . F35 . 114.2(9) yes F28 . C51 . F35 . 105.6(9) yes C47 . C51 . F42 . 111.1(8) yes F28 . C51 . F42 . 107.7(10) yes F35 . C51 . F42 . 105.0(10) yes C47 . C53 . C43 . 123.5(6) yes C47 . C53 . H531 . 117.886 no C43 . C53 . H531 . 118.607 no N13 . C55 . C56 . 122.8(8) yes N13 . C55 . H551 . 118.785 no C56 . C55 . H551 . 118.443 no C55 . C56 . C59 . 115.7(9) yes C55 . C56 . H561 . 122.007 no C59 . C56 . H561 . 122.301 no C56 . C59 . N14 . 123.3(8) yes C56 . C59 . H591 . 118.166 no N14 . C59 . H591 . 118.569 no C29 . C61 . N10 . 116.3(7) yes C29 . C61 . N11 . 118.0(9) yes N10 . C61 . N11 . 125.7(9) yes N12 . C63 . C65 . 123.2(9) yes N12 . C63 . H631 . 118.616 no C65 . C63 . H631 . 118.142 no C40 . C65 . C63 . 118.2(9) yes C40 . C65 . H651 . 120.769 no C63 . C65 . H651 . 120.996 no C1 . C70 . F30 . 110.4(8) yes C1 . C70 . F38 . 111.8(7) yes F30 . C70 . F38 . 107.9(12) yes C1 . C70 . F58 . 112.8(10) yes F30 . C70 . F58 . 105.6(8) yes F38 . C70 . F58 . 108.2(9) yes N10 . C71 . C73 . 121.9(11) yes N10 . C71 . H711 . 118.594 no C73 . C71 . H711 . 119.513 no C3 . C73 . C71 . 116.0(11) yes C3 . C73 . H731 . 122.059 no C71 . C73 . H731 . 121.840 no # Attachment '- Data-(2).cif' data_CRYSTALS_cif2 _database_code_depnum_ccdc_archive 'CCDC 757202' #TrackingRef '- Data-(2).cif' _audit_creation_date 05-04-05 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '2231437 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.9876(11) _cell_length_b 12.0698(7) _cell_length_c 12.3219(7) _cell_angle_alpha 66.622(8) _cell_angle_beta 86.490(6) _cell_angle_gamma 77.145(9) _cell_volume 1594.7(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ba -0.3244 2.2819 20.3361 3.2160 19.2970 0.2756 10.8880 20.2073 2.6959 167.2020 2.7731 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C26 H14 Ba1 F12 N8 O4' _chemical_formula_moiety 'C26 H14 Ba1 F12 N8 O4' _chemical_compound_source ? _chemical_formula_weight 867.3 _cell_measurement_reflns_used 160 _cell_measurement_theta_min 4 _cell_measurement_theta_max 21 _cell_measurement_temperature 295(2) _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.87 # Sheldrick geometric definitions 0.87 0.87 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 295(2) _diffrn_reflns_number 22584 _reflns_number_total 9276 _diffrn_reflns_av_R_equivalents 0.071 # Number of reflections with Friedels Law is 9276 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9296 _diffrn_reflns_theta_min 2.029 _diffrn_reflns_theta_max 29.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.999 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -15 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.36 _refine_diff_density_max 2.66 _refine_ls_number_reflns 5821 _refine_ls_number_restraints 0 _refine_ls_number_parameters 401 #_refine_ls_R_factor_ref 0.0694 _refine_ls_wR_factor_ref 0.0777 _refine_ls_goodness_of_fit_ref 1.0595 #_reflns_number_all 9271 _refine_ls_R_factor_all 0.1062 _refine_ls_wR_factor_all 0.1091 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5821 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_gt 0.0777 _refine_ls_shift/su_max 0.000166 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refU # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.01 0.670 0.626 ; # Footnote 2 _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ba1 Ba 0.31232(3) 0.06035(4) 0.24154(4) 0.0283 1.0000 Uani . . . . . . O1 O 0.3069(4) -0.1857(5) 0.3031(5) 0.0436 1.0000 Uani . . . . . . O4 O 0.3060(5) 0.3027(5) 0.1117(5) 0.0453 1.0000 Uani . . . . . . O3 O 0.1413(5) 0.1736(6) 0.0785(6) 0.0568 1.0000 Uani . . . . . . O2 O 0.5209(5) -0.1126(5) 0.2946(6) 0.0524 1.0000 Uani . . . . . . N3 N 0.4586(5) 0.1424(5) 0.3739(5) 0.0372 1.0000 Uani . . . . . . N4 N 0.6181(5) 0.0671(5) 0.5065(5) 0.0364 1.0000 Uani . . . . . . N1 N 0.3576(5) -0.0198(6) 0.0405(5) 0.0414 1.0000 Uani . . . . . . N6 N 0.0809(5) 0.0066(6) 0.3258(7) 0.0467 1.0000 Uani . . . . . . N5 N 0.1318(6) 0.2098(7) 0.3377(7) 0.0475 1.0000 Uani . . . . . . N2 N 0.4946(6) -0.1101(7) -0.0635(7) 0.0515 1.0000 Uani . . . . . . N7 N -0.0615(7) 0.2739(8) 0.3811(9) 0.0638 1.0000 Uani . . . . . . N8 N -0.1140(6) 0.0854(9) 0.3464(10) 0.0683 1.0000 Uani . . . . . . C1 C -0.1402(8) -0.0111(13) 0.3344(14) 0.0806 1.0000 Uani . . . . . . C4 C 0.5216(5) 0.0582(6) 0.4666(5) 0.0301 1.0000 Uani . . . . . . C5 C 0.6543(6) 0.1718(7) 0.4492(6) 0.0386 1.0000 Uani . . . . . . C6 C 0.0070(10) 0.2889(12) -0.0734(11) 0.0725 1.0000 Uani . . . . . . C8 C 0.4943(7) 0.2499(7) 0.3193(7) 0.0430 1.0000 Uani . . . . . . C9 C 0.5918(8) 0.2674(7) 0.3551(7) 0.0467 1.0000 Uani . . . . . . C10 C 0.2530(7) 0.3807(7) 0.0209(7) 0.0434 1.0000 Uani . . . . . . C11 C 0.1113(7) 0.2750(9) -0.0019(7) 0.0489 1.0000 Uani . . . . . . C12 C 0.1592(8) 0.3787(9) -0.0376(8) 0.0594 1.0000 Uani . . . . . . C13 C 0.3757(6) -0.2836(6) 0.3153(7) 0.0398 1.0000 Uani . . . . . . C14 C 0.4598(6) -0.0356(6) -0.0061(6) 0.0355 1.0000 Uani . . . . . . C16 C 0.4939(6) -0.3088(7) 0.3156(8) 0.0477 1.0000 Uani . . . . . . C21 C 0.5558(6) -0.2199(7) 0.3049(7) 0.0413 1.0000 Uani . . . . . . C22 C 0.0244(6) 0.1981(7) 0.3537(6) 0.0419 1.0000 Uani . . . . . . C23 C -0.0051(6) 0.0895(8) 0.3416(7) 0.0420 1.0000 Uani . . . . . . C27 C 0.2829(7) -0.0793(9) 0.0254(7) 0.0487 1.0000 Uani . . . . . . C28 C 0.3114(9) -0.1584(10) -0.0318(9) 0.0599 1.0000 Uani . . . . . . C35 C 0.4210(9) -0.1739(11) -0.0700(10) 0.0649 1.0000 Uani . . . . . . C37 C 0.3175(8) -0.3900(8) 0.3348(11) 0.0606 1.0000 Uani . . . . . . C38 C -0.0330(11) 0.3695(11) 0.3927(12) 0.0750 1.0000 Uani . . . . . . C41 C 0.0736(10) 0.3906(10) 0.3771(10) 0.0638 1.0000 Uani . . . . . . C42 C -0.0592(8) -0.1031(10) 0.3193(12) 0.0673 1.0000 Uani . . . . . . C44 C 0.0515(7) -0.0890(9) 0.3156(11) 0.0604 1.0000 Uani . . . . . . C46 C 0.6862(7) -0.2610(9) 0.3108(9) 0.0545 1.0000 Uani . . . . . . C47 C 0.1559(8) 0.3092(9) 0.3486(9) 0.0560 1.0000 Uani . . . . . . C49 C 0.3072(9) 0.4942(9) -0.0384(9) 0.0638 1.0000 Uani . . . . . . F9 F 0.7338(7) -0.1851(7) 0.2213(7) 0.0840(19) 1.0000 Uiso . . . . . . F13 F 0.0261(9) 0.3209(10) -0.1910(10) 0.117(3) 1.0000 Uiso . . . . . . F17 F -0.0759(14) 0.3871(14) -0.0866(14) 0.168(5) 1.0000 Uiso . . . . . . F18 F 0.3377(8) 0.5335(9) 0.0400(9) 0.107(3) 1.0000 Uiso . . . . . . F19 F -0.0197(16) 0.1873(17) -0.0583(16) 0.189(6) 1.0000 Uiso . . . . . . F25 F 0.7302(9) -0.2618(9) 0.4060(9) 0.109(3) 1.0000 Uiso . . . . . . F26 F 0.7262(8) -0.3745(8) 0.3126(8) 0.099(2) 1.0000 Uiso . . . . . . F29 F 0.2387(8) 0.5937(8) -0.1163(8) 0.096(2) 1.0000 Uiso . . . . . . F33 F 0.2584(13) -0.4135(14) 0.4315(13) 0.158(5) 1.0000 Uiso . . . . . . F34 F 0.4019(9) 0.4661(9) -0.0941(9) 0.108(3) 1.0000 Uiso . . . . . . F36 F 0.2342(11) -0.3585(11) 0.2589(11) 0.136(4) 1.0000 Uiso . . . . . . F48 F 0.3805(11) -0.4924(12) 0.3437(12) 0.139(4) 1.0000 Uiso . . . . . . H11 H -0.2231 -0.0157 0.3352 0.19(3) 1.0000 Uiso . . . . . . H51 H 0.7281 0.1810 0.4752 0.19(3) 1.0000 Uiso . . . . . . H81 H 0.4478 0.3181 0.2506 0.19(3) 1.0000 Uiso . . . . . . H91 H 0.6174 0.3474 0.3144 0.19(3) 1.0000 Uiso . . . . . . H121 H 0.1244 0.4544 -0.1080 0.19(3) 1.0000 Uiso . . . . . . H161 H 0.5364 -0.3935 0.3235 0.19(3) 1.0000 Uiso . . . . . . H271 H 0.2040 -0.0660 0.0569 0.19(3) 1.0000 Uiso . . . . . . H281 H 0.2546 -0.2022 -0.0450 0.19(3) 1.0000 Uiso . . . . . . H351 H 0.4470 -0.2374 -0.1051 0.19(3) 1.0000 Uiso . . . . . . H381 H -0.0941 0.4286 0.4144 0.19(3) 1.0000 Uiso . . . . . . H411 H 0.0921 0.4641 0.3859 0.19(3) 1.0000 Uiso . . . . . . H421 H -0.0792 -0.1768 0.3123 0.19(3) 1.0000 Uiso . . . . . . H441 H 0.1137 -0.1539 0.3036 0.19(3) 1.0000 Uiso . . . . . . H471 H 0.2359 0.3233 0.3355 0.19(3) 1.0000 Uiso . . . . . . 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 Ba1 0.02801(17) 0.02855(17) 0.02887(18) -0.01127(12) 0.00150(11) -0.00754(11) O1 0.033(2) 0.034(2) 0.062(3) -0.018(2) 0.003(2) -0.0061(19) O4 0.047(3) 0.042(3) 0.042(3) -0.009(2) -0.006(2) -0.013(2) O3 0.053(3) 0.056(3) 0.054(3) -0.007(3) -0.015(3) -0.021(3) O2 0.036(3) 0.045(3) 0.081(4) -0.030(3) 0.004(3) -0.009(2) N3 0.045(3) 0.031(3) 0.032(3) -0.008(2) -0.004(2) -0.008(2) N4 0.035(3) 0.039(3) 0.034(3) -0.010(2) 0.003(2) -0.012(2) N1 0.042(3) 0.054(4) 0.035(3) -0.020(3) 0.008(2) -0.018(3) N6 0.031(3) 0.047(3) 0.066(4) -0.024(3) 0.010(3) -0.012(2) N5 0.040(3) 0.049(4) 0.060(4) -0.028(3) 0.009(3) -0.012(3) N2 0.059(4) 0.058(4) 0.058(4) -0.038(3) 0.029(3) -0.033(3) N7 0.044(4) 0.060(5) 0.090(6) -0.037(4) 0.011(4) -0.005(3) N8 0.038(3) 0.081(6) 0.108(7) -0.062(6) 0.017(4) -0.013(4) C1 0.039(4) 0.105(9) 0.134(11) -0.080(9) 0.019(6) -0.027(5) C4 0.032(3) 0.033(3) 0.027(3) -0.012(2) 0.003(2) -0.008(2) C5 0.038(3) 0.049(4) 0.031(3) -0.015(3) 0.006(3) -0.018(3) C6 0.056(5) 0.074(7) 0.075(7) -0.010(5) -0.013(5) -0.022(5) C8 0.058(4) 0.032(3) 0.035(3) -0.007(3) -0.003(3) -0.013(3) C9 0.064(5) 0.037(4) 0.038(4) -0.009(3) 0.002(3) -0.022(3) C10 0.045(4) 0.047(4) 0.036(3) -0.012(3) 0.005(3) -0.016(3) C11 0.036(3) 0.067(5) 0.038(4) -0.013(4) -0.002(3) -0.012(3) C12 0.053(5) 0.060(5) 0.049(5) -0.001(4) -0.013(4) -0.014(4) C13 0.040(3) 0.032(3) 0.047(4) -0.013(3) -0.001(3) -0.010(3) C14 0.047(4) 0.038(3) 0.025(3) -0.013(2) 0.007(3) -0.015(3) C16 0.034(3) 0.043(4) 0.066(5) -0.022(4) -0.001(3) -0.004(3) C21 0.029(3) 0.047(4) 0.045(4) -0.016(3) 0.003(3) -0.008(3) C22 0.040(3) 0.048(4) 0.036(3) -0.018(3) 0.007(3) -0.007(3) C23 0.033(3) 0.054(4) 0.040(4) -0.019(3) 0.006(3) -0.012(3) C27 0.044(4) 0.065(5) 0.044(4) -0.023(4) 0.007(3) -0.027(4) C28 0.069(6) 0.070(6) 0.061(5) -0.035(5) 0.018(4) -0.042(5) C35 0.071(6) 0.081(6) 0.078(6) -0.058(6) 0.030(5) -0.043(5) C37 0.053(5) 0.038(4) 0.089(7) -0.021(4) 0.000(5) -0.013(4) C38 0.074(7) 0.063(6) 0.092(8) -0.046(6) 0.004(6) 0.007(5) C41 0.069(6) 0.056(5) 0.074(6) -0.033(5) 0.012(5) -0.016(4) C42 0.036(4) 0.071(6) 0.110(9) -0.052(6) 0.010(5) -0.015(4) C44 0.040(4) 0.050(5) 0.103(8) -0.041(5) 0.016(4) -0.017(3) C46 0.031(3) 0.058(5) 0.062(5) -0.011(4) -0.005(3) -0.005(3) C47 0.052(5) 0.054(5) 0.072(6) -0.033(4) 0.002(4) -0.016(4) C49 0.068(6) 0.052(5) 0.054(5) 0.002(4) 0.003(4) -0.021(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1866(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C13 . 1.240(9) yes O4 . C10 . 1.236(10) yes O3 . C11 . 1.223(11) yes O2 . C21 . 1.225(10) yes N3 . C4 . 1.324(8) yes N3 . C8 . 1.356(9) yes N4 . C4 . 1.325(8) yes N4 . C5 . 1.335(9) yes N1 . C14 . 1.327(9) yes N1 . C27 . 1.329(10) yes N6 . C23 . 1.332(10) yes N6 . C44 . 1.332(11) yes N5 . C22 . 1.321(10) yes N5 . C47 . 1.352(11) yes N2 . C14 . 1.335(9) yes N2 . C35 . 1.318(11) yes N7 . C22 . 1.339(10) yes N7 . C38 . 1.335(15) yes N8 . C1 . 1.335(14) yes N8 . C23 . 1.315(10) yes C1 . C42 . 1.367(15) yes C1 . H11 . 1.007 no C4 . C4 2_656 1.508(12) yes C5 . C9 . 1.377(11) yes C5 . H51 . 1.002 no C6 . C11 . 1.514(13) yes C6 . F13 . 1.362(16) yes C6 . F17 . 1.327(19) yes C6 . F19 . 1.28(2) yes C8 . C9 . 1.362(12) yes C8 . H81 . 1.003 no C9 . H91 . 1.003 no C10 . C12 . 1.383(12) yes C10 . C49 . 1.541(12) yes C11 . C12 . 1.393(13) yes C12 . H121 . 1.003 no C13 . C16 . 1.382(10) yes C13 . C37 . 1.525(11) yes C14 . C14 2_655 1.477(13) yes C16 . C21 . 1.396(11) yes C16 . H161 . 1.004 no C21 . C46 . 1.528(10) yes C22 . C23 . 1.495(11) yes C27 . C28 . 1.372(13) yes C27 . H271 . 1.004 no C28 . C35 . 1.367(14) yes C28 . H281 . 1.005 no C35 . H351 . 1.006 no C37 . F33 . 1.312(18) yes C37 . F36 . 1.296(15) yes C37 . F48 . 1.263(15) yes C38 . C41 . 1.345(17) yes C38 . H381 . 1.007 no C41 . C47 . 1.364(14) yes C41 . H411 . 1.008 no C42 . C44 . 1.371(12) yes C42 . H421 . 1.007 no C44 . H441 . 1.005 no C46 . F9 . 1.317(12) yes C46 . F25 . 1.312(13) yes C46 . F26 . 1.339(13) yes C47 . H471 . 1.004 no C49 . F18 . 1.333(15) yes C49 . F29 . 1.334(13) yes C49 . F34 . 1.339(14) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 . N3 . C8 . 115.9(6) yes C4 . N4 . C5 . 117.1(6) yes C14 . N1 . C27 . 117.5(7) yes C23 . N6 . C44 . 115.5(7) yes C22 . N5 . C47 . 116.2(7) yes C14 . N2 . C35 . 115.8(7) yes C22 . N7 . C38 . 115.2(8) yes C1 . N8 . C23 . 116.7(8) yes N8 . C1 . C42 . 122.7(9) yes N8 . C1 . H11 . 118.594 no C42 . C1 . H11 . 118.667 no C4 2_656 C4 . N4 . 117.3(7) yes C4 2_656 C4 . N3 . 116.5(7) yes N4 . C4 . N3 . 126.2(6) yes N4 . C5 . C9 . 121.1(7) yes N4 . C5 . H51 . 119.486 no C9 . C5 . H51 . 119.415 no C11 . C6 . F13 . 113.6(10) yes C11 . C6 . F17 . 115.3(12) yes F13 . C6 . F17 . 95.7(11) yes C11 . C6 . F19 . 114.6(12) yes F13 . C6 . F19 . 94.7(13) yes F17 . C6 . F19 . 118.9(14) yes N3 . C8 . C9 . 121.7(7) yes N3 . C8 . H81 . 119.139 no C9 . C8 . H81 . 119.194 no C5 . C9 . C8 . 117.9(7) yes C5 . C9 . H91 . 121.031 no C8 . C9 . H91 . 121.108 no O4 . C10 . C12 . 130.7(8) yes O4 . C10 . C49 . 112.9(7) yes C12 . C10 . C49 . 116.3(8) yes C6 . C11 . O3 . 114.8(8) yes C6 . C11 . C12 . 115.6(8) yes O3 . C11 . C12 . 129.7(8) yes C11 . C12 . C10 . 122.1(8) yes C11 . C12 . H121 . 119.037 no C10 . C12 . H121 . 118.879 no O1 . C13 . C16 . 129.7(7) yes O1 . C13 . C37 . 113.1(7) yes C16 . C13 . C37 . 117.2(7) yes C14 2_655 C14 . N2 . 117.9(8) yes C14 2_655 C14 . N1 . 117.1(7) yes N2 . C14 . N1 . 125.0(7) yes C13 . C16 . C21 . 121.8(7) yes C13 . C16 . H161 . 118.975 no C21 . C16 . H161 . 119.180 no C16 . C21 . O2 . 129.4(7) yes C16 . C21 . C46 . 116.6(7) yes O2 . C21 . C46 . 113.9(7) yes N7 . C22 . N5 . 126.3(8) yes N7 . C22 . C23 . 116.2(7) yes N5 . C22 . C23 . 117.5(6) yes C22 . C23 . N6 . 117.2(6) yes C22 . C23 . N8 . 116.8(7) yes N6 . C23 . N8 . 126.0(8) yes N1 . C27 . C28 . 121.5(8) yes N1 . C27 . H271 . 118.973 no C28 . C27 . H271 . 119.545 no C27 . C28 . C35 . 116.2(8) yes C27 . C28 . H281 . 121.771 no C35 . C28 . H281 . 121.984 no C28 . C35 . N2 . 123.6(8) yes C28 . C35 . H351 . 118.228 no N2 . C35 . H351 . 118.144 no C13 . C37 . F33 . 110.3(10) yes C13 . C37 . F36 . 112.2(9) yes F33 . C37 . F36 . 98.8(11) yes C13 . C37 . F48 . 117.7(10) yes F33 . C37 . F48 . 105.9(12) yes F36 . C37 . F48 . 110.0(11) yes N7 . C38 . C41 . 123.2(9) yes N7 . C38 . H381 . 118.435 no C41 . C38 . H381 . 118.341 no C38 . C41 . C47 . 117.7(9) yes C38 . C41 . H411 . 121.211 no C47 . C41 . H411 . 121.043 no C1 . C42 . C44 . 115.5(9) yes C1 . C42 . H421 . 122.488 no C44 . C42 . H421 . 121.983 no C42 . C44 . N6 . 123.5(8) yes C42 . C44 . H441 . 118.242 no N6 . C44 . H441 . 118.221 no C21 . C46 . F9 . 112.0(7) yes C21 . C46 . F25 . 111.6(9) yes F9 . C46 . F25 . 105.4(8) yes C21 . C46 . F26 . 114.9(8) yes F9 . C46 . F26 . 106.6(9) yes F25 . C46 . F26 . 105.6(8) yes C41 . C47 . N5 . 121.3(9) yes C41 . C47 . H471 . 119.363 no N5 . C47 . H471 . 119.320 no C10 . C49 . F18 . 112.0(8) yes C10 . C49 . F29 . 114.9(9) yes F18 . C49 . F29 . 104.2(10) yes C10 . C49 . F34 . 110.4(9) yes F18 . C49 . F34 . 107.0(10) yes F29 . C49 . F34 . 107.8(9) yes # Attachment '- Data-(3).CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 757203' #TrackingRef '- Data-(3).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Ba1 F12 N4 O4' _chemical_formula_sum 'C22 H16 Ba1 F12 N4 O4' _chemical_formula_weight 765.3 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' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7390(10) _cell_length_b 13.3460(9) _cell_length_c 19.5040(17) _cell_angle_alpha 81.750(5) _cell_angle_beta 85.689(6) _cell_angle_gamma 72.637(5) _cell_volume 2884.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 121 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 19.59 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6472 _exptl_absorpt_correction_T_max 0.8300 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57551 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.00 _reflns_number_total 16739 _reflns_number_gt 8450 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'DIRAX/LSQ (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.4900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16739 _refine_ls_number_parameters 783 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.12805(2) 0.705842(17) 0.546818(13) 0.02981(8) Uani 1 1 d . . . F1 F -0.1363(3) 0.5910(3) 0.7536(2) 0.0944(13) Uani 1 1 d . . . F2 F -0.0374(4) 0.4349(3) 0.7845(2) 0.1114(15) Uani 1 1 d . . . F3 F -0.1321(3) 0.4738(3) 0.69133(19) 0.0973(13) Uani 1 1 d . . . F4 F 0.4318(5) 0.3453(3) 0.6046(3) 0.170(3) Uani 1 1 d . . . F5 F 0.3164(5) 0.2675(4) 0.6319(5) 0.217(4) Uani 1 1 d . . . F6 F 0.3909(6) 0.3094(5) 0.7036(3) 0.220(4) Uani 1 1 d . . . F7 F 0.3189(4) 0.8361(4) 0.31695(19) 0.1140(16) Uani 1 1 d . . . F8 F 0.2572(4) 0.9892(3) 0.3482(2) 0.1180(17) Uani 1 1 d . . . F9 F 0.4403(3) 0.9032(3) 0.3497(2) 0.0943(12) Uani 1 1 d . . . F10 F 0.4946(4) 0.8763(6) 0.6164(4) 0.209(4) Uani 1 1 d . . . F11 F 0.3382(6) 0.9076(6) 0.6686(3) 0.184(3) Uani 1 1 d . . . F12 F 0.3619(8) 1.0098(5) 0.5940(4) 0.205(4) Uani 1 1 d . . . O1 O 0.0261(3) 0.6194(2) 0.65902(18) 0.0512(9) Uani 1 1 d . . . O2 O 0.2676(3) 0.5232(2) 0.61037(17) 0.0477(8) Uani 1 1 d . . . O3 O 0.2592(3) 0.7778(3) 0.44404(17) 0.0519(9) Uani 1 1 d . . . O4 O 0.2901(3) 0.7889(3) 0.58705(18) 0.0559(9) Uani 1 1 d . . . N1 N -0.0767(3) 0.6301(2) 0.5230(2) 0.0344(9) Uani 1 1 d . . . N2 N 0.1432(3) 0.5214(3) 0.47675(18) 0.0311(8) Uani 1 1 d . . . N3 N 0.0020(3) 0.8950(3) 0.45089(19) 0.0370(9) Uani 1 1 d . . . N4 N 0.0247(3) 0.9211(2) 0.58422(18) 0.0332(8) Uani 1 1 d . . . C1 C 0.0419(4) 0.5269(4) 0.6874(2) 0.0408(11) Uani 1 1 d . . . C2 C 0.1425(5) 0.4405(3) 0.6842(3) 0.0521(14) Uani 1 1 d . . . H2 H 0.1411 0.3751 0.7092 0.062 Uiso 1 1 calc R . . C3 C 0.2450(5) 0.4466(4) 0.6458(3) 0.0448(12) Uani 1 1 d . . . C4 C -0.0667(5) 0.5067(4) 0.7295(3) 0.0535(14) Uani 1 1 d . . . C5 C 0.3472(6) 0.3442(5) 0.6484(4) 0.0644(17) Uani 1 1 d . . . C6 C 0.3114(4) 0.8480(4) 0.4370(3) 0.0466(13) Uani 1 1 d . . . C7 C 0.3512(5) 0.8898(4) 0.4887(3) 0.0561(14) Uani 1 1 d . . . H7 H 0.3893 0.9427 0.4755 0.067 Uiso 1 1 calc R . . C8 C 0.3374(4) 0.8572(4) 0.5589(3) 0.0470(13) Uani 1 1 d . . . C9 C 0.3305(5) 0.8949(5) 0.3629(3) 0.0591(15) Uani 1 1 d . . . C10 C 0.3874(6) 0.9087(6) 0.6093(4) 0.075(2) Uani 1 1 d . . . C11 C -0.0604(4) 0.5301(3) 0.5124(2) 0.0273(9) Uani 1 1 d . . . C12 C -0.1854(4) 0.6832(3) 0.5467(3) 0.0455(12) Uani 1 1 d . . . C13 C -0.2753(4) 0.6368(3) 0.5584(3) 0.0444(12) Uani 1 1 d . . . H13 H -0.3516 0.6753 0.5736 0.053 Uiso 1 1 calc R . . C14 C 0.2530(4) 0.4674(3) 0.4525(2) 0.0343(10) Uani 1 1 d . . . C15 C -0.2039(5) 0.7964(4) 0.5601(4) 0.089(3) Uani 1 1 d . . . H15A H -0.1529 0.8280 0.5282 0.133 Uiso 1 1 calc R . . H15B H -0.1837 0.7967 0.6074 0.133 Uiso 1 1 calc R . . H15C H -0.2867 0.8368 0.5532 0.133 Uiso 1 1 calc R . . C16 C 0.3483(5) 0.5221(4) 0.4411(3) 0.0592(16) Uani 1 1 d . . . H16A H 0.3738 0.5307 0.4855 0.089 Uiso 1 1 calc R . . H16B H 0.3171 0.5911 0.4145 0.089 Uiso 1 1 calc R . . H16C H 0.4159 0.4800 0.4159 0.089 Uiso 1 1 calc R . . C17 C -0.0065(4) 0.9933(3) 0.4630(2) 0.0293(9) Uani 1 1 d . . . C18 C -0.0080(5) 0.8815(3) 0.3840(2) 0.0435(12) Uani 1 1 d . . . C19 C -0.0268(5) 0.9665(3) 0.3325(2) 0.0459(12) Uani 1 1 d . . . H19 H -0.0340 0.9571 0.2863 0.055 Uiso 1 1 calc R . . C20 C 0.0351(5) 0.9350(3) 0.6506(2) 0.0427(12) Uani 1 1 d . . . C21 C 0.0031(7) 0.7717(4) 0.3686(3) 0.082(2) Uani 1 1 d . . . H21A H -0.0464 0.7402 0.4016 0.123 Uiso 1 1 calc R . . H21B H 0.0857 0.7288 0.3722 0.123 Uiso 1 1 calc R . . H21C H -0.0229 0.7752 0.3220 0.123 Uiso 1 1 calc R . . C22 C 0.0582(6) 0.8398(4) 0.7044(3) 0.0698(19) Uani 1 1 d . . . H22A H 0.1393 0.7951 0.6981 0.105 Uiso 1 1 calc R . . H22B H 0.0025 0.8004 0.6996 0.105 Uiso 1 1 calc R . . H22C H 0.0479 0.8622 0.7502 0.105 Uiso 1 1 calc R . . Ba2 Ba 0.61929(2) 0.209253(18) 0.046446(13) 0.03377(9) Uani 1 1 d . . . F13 F 0.5209(6) 0.4691(7) 0.2837(4) 0.241(4) Uani 1 1 d . . . F14 F 0.4359(7) 0.3595(5) 0.2792(3) 0.190(3) Uani 1 1 d . . . F15 F 0.3984(6) 0.4956(4) 0.2148(3) 0.166(3) Uani 1 1 d . . . F16 F 0.8496(5) 0.5052(4) 0.1286(4) 0.182(3) Uani 1 1 d . . . F17 F 0.9532(5) 0.3585(4) 0.1724(3) 0.149(2) Uani 1 1 d . . . F18 F 0.9402(5) 0.3897(5) 0.0680(3) 0.140(2) Uani 1 1 d . . . F19 F 0.7788(5) -0.1320(4) 0.2087(3) 0.174(3) Uani 1 1 d . . . F20 F 0.9518(4) -0.1708(3) 0.1721(2) 0.1155(16) Uani 1 1 d . . . F21 F 0.8374(7) -0.2398(4) 0.1371(3) 0.204(4) Uani 1 1 d . . . F22 F 0.8106(6) -0.0794(7) -0.1318(3) 0.199(4) Uani 1 1 d . . . F23 F 0.9675(7) -0.1246(7) -0.0990(4) 0.289(6) Uani 1 1 d . . . F24 F 0.9035(9) 0.0195(6) -0.1446(4) 0.242(5) Uani 1 1 d . . . O5 O 0.5459(3) 0.3082(3) 0.15776(18) 0.0550(9) Uani 1 1 d . . . O6 O 0.7751(3) 0.2959(3) 0.09184(19) 0.0553(9) Uani 1 1 d . . . O7 O 0.7536(3) 0.0253(3) 0.1103(2) 0.0623(10) Uani 1 1 d . . . O8 O 0.7712(3) 0.0856(2) -0.03666(19) 0.0599(10) Uani 1 1 d . . . N5 N 0.4175(3) 0.4053(3) 0.0214(2) 0.0386(9) Uani 1 1 d . . . N6 N 0.6346(4) 0.4118(2) -0.03355(19) 0.0402(10) Uani 1 1 d . . . N7 N 0.4962(3) 0.0434(3) 0.08396(18) 0.0368(9) Uani 1 1 d . . . N8 N 0.5029(4) 0.1230(3) -0.05168(19) 0.0432(10) Uani 1 1 d . . . C23 C 0.5756(5) 0.3707(4) 0.1888(3) 0.0519(14) Uani 1 1 d . . . C24 C 0.6794(5) 0.4020(4) 0.1779(3) 0.0612(15) Uani 1 1 d . . . H24 H 0.6883 0.4532 0.2038 0.073 Uiso 1 1 calc R . . C25 C 0.7692(5) 0.3622(4) 0.1314(3) 0.0513(13) Uani 1 1 d . . . C26 C 0.4857(8) 0.4203(7) 0.2427(4) 0.088(2) Uani 1 1 d . . . C27 C 0.8765(6) 0.4063(6) 0.1256(4) 0.0751(19) Uani 1 1 d . . . C28 C 0.8107(5) -0.0607(4) 0.0931(3) 0.0585(15) Uani 1 1 d . . . C29 C 0.8492(5) -0.0844(4) 0.0254(3) 0.0600(16) Uani 1 1 d . . . H29 H 0.8900 -0.1550 0.0196 0.072 Uiso 1 1 calc R . . C30 C 0.8303(4) -0.0100(4) -0.0327(3) 0.0517(14) Uani 1 1 d . . . C31 C 0.8456(6) -0.1528(5) 0.1510(4) 0.082(2) Uani 1 1 d . . . C32 C 0.8764(7) -0.0455(6) -0.1015(4) 0.084(2) Uani 1 1 d . . . C33 C 0.4400(4) 0.4978(3) 0.0151(2) 0.0323(10) Uani 1 1 d . . . C34 C 0.7413(5) 0.4166(4) -0.0610(3) 0.0513(14) Uani 1 1 d . . . C35 C 0.7725(5) 0.5086(4) -0.0692(3) 0.0559(15) Uani 1 1 d . . . H35 H 0.8478 0.5105 -0.0884 0.067 Uiso 1 1 calc R . . C36 C 0.3086(4) 0.4015(3) 0.0488(3) 0.0502(13) Uani 1 1 d . . . C37 C 0.8280(6) 0.3162(4) -0.0821(4) 0.097(3) Uani 1 1 d . . . H37A H 0.8389 0.2606 -0.0431 0.145 Uiso 1 1 calc R . . H37B H 0.9042 0.3286 -0.0962 0.145 Uiso 1 1 calc R . . H37C H 0.7966 0.2950 -0.1204 0.145 Uiso 1 1 calc R . . C38 C 0.2790(6) 0.2997(5) 0.0539(5) 0.096(3) Uani 1 1 d . . . H38A H 0.3010 0.2702 0.0105 0.144 Uiso 1 1 calc R . . H38B H 0.1939 0.3121 0.0634 0.144 Uiso 1 1 calc R . . H38C H 0.3228 0.2504 0.0911 0.144 Uiso 1 1 calc R . . C39 C 0.4981(4) -0.0219(3) 0.0375(2) 0.0308(10) Uani 1 1 d . . . C40 C 0.5045(5) 0.1622(4) -0.1189(3) 0.0550(15) Uani 1 1 d . . . C41 C 0.5089(5) 0.0994(4) -0.1698(2) 0.0490(13) Uani 1 1 d . . . H41 H 0.5122 0.1267 -0.2168 0.059 Uiso 1 1 calc R . . C42 C 0.4914(5) 0.0028(4) 0.1512(2) 0.0428(12) Uani 1 1 d . . . C43 C 0.5034(9) 0.2762(5) -0.1358(3) 0.115(3) Uani 1 1 d . . . H43A H 0.4250 0.3218 -0.1243 0.173 Uiso 1 1 calc R . . H43B H 0.5217 0.2910 -0.1848 0.173 Uiso 1 1 calc R . . H43C H 0.5628 0.2891 -0.1090 0.173 Uiso 1 1 calc R . . C44 C 0.4866(7) 0.0754(5) 0.2046(3) 0.078(2) Uani 1 1 d . . . H44A H 0.5670 0.0755 0.2129 0.117 Uiso 1 1 calc R . . H44B H 0.4502 0.0508 0.2474 0.117 Uiso 1 1 calc R . . H44C H 0.4396 0.1466 0.1877 0.117 Uiso 1 1 calc R . . 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 Ba1 0.04022(17) 0.02125(13) 0.03130(16) -0.00136(11) 0.00183(12) -0.01567(11) F1 0.085(3) 0.094(3) 0.112(3) -0.033(2) 0.051(2) -0.043(2) F2 0.090(3) 0.141(4) 0.085(3) 0.065(3) 0.005(2) -0.045(3) F3 0.101(3) 0.154(4) 0.076(3) -0.030(3) 0.011(2) -0.092(3) F4 0.119(4) 0.078(3) 0.231(7) 0.056(3) 0.075(4) 0.042(3) F5 0.117(4) 0.073(3) 0.455(13) -0.107(5) -0.016(6) 0.015(3) F6 0.230(7) 0.206(6) 0.102(4) -0.037(4) -0.092(4) 0.151(6) F7 0.186(5) 0.140(4) 0.048(2) -0.006(2) 0.027(3) -0.107(3) F8 0.126(4) 0.082(3) 0.094(3) 0.039(2) 0.030(3) 0.016(2) F9 0.079(3) 0.122(3) 0.086(3) 0.011(2) 0.031(2) -0.054(2) F10 0.059(3) 0.304(8) 0.305(8) -0.229(7) -0.040(4) -0.018(4) F11 0.172(5) 0.329(10) 0.147(5) -0.151(6) 0.044(4) -0.172(6) F12 0.350(10) 0.104(4) 0.202(7) -0.033(4) -0.140(7) -0.090(5) O1 0.063(2) 0.0349(18) 0.052(2) 0.0014(16) 0.0133(18) -0.0155(16) O2 0.044(2) 0.0448(19) 0.050(2) 0.0107(16) -0.0043(16) -0.0134(15) O3 0.075(3) 0.049(2) 0.044(2) -0.0087(16) 0.0130(18) -0.0378(18) O4 0.064(2) 0.069(2) 0.048(2) -0.0012(19) -0.0111(18) -0.040(2) N1 0.029(2) 0.0225(17) 0.052(2) -0.0053(16) 0.0008(17) -0.0091(15) N2 0.033(2) 0.0293(18) 0.035(2) -0.0093(16) 0.0030(16) -0.0145(15) N3 0.051(2) 0.0240(18) 0.039(2) -0.0024(16) -0.0074(18) -0.0154(16) N4 0.046(2) 0.0213(17) 0.031(2) -0.0024(15) 0.0025(17) -0.0095(15) C1 0.049(3) 0.045(3) 0.032(3) 0.002(2) -0.003(2) -0.021(2) C2 0.076(4) 0.028(2) 0.049(3) 0.011(2) 0.003(3) -0.019(2) C3 0.057(3) 0.039(3) 0.038(3) 0.004(2) -0.014(2) -0.013(2) C4 0.064(4) 0.053(3) 0.046(3) 0.005(3) -0.002(3) -0.027(3) C5 0.065(4) 0.045(3) 0.077(5) -0.005(3) -0.016(4) -0.005(3) C6 0.046(3) 0.042(3) 0.054(3) -0.003(2) 0.019(3) -0.022(2) C7 0.064(4) 0.051(3) 0.067(4) -0.011(3) 0.011(3) -0.038(3) C8 0.036(3) 0.047(3) 0.066(4) -0.016(3) -0.006(3) -0.020(2) C9 0.060(4) 0.056(3) 0.061(4) 0.002(3) 0.019(3) -0.027(3) C10 0.064(5) 0.084(5) 0.099(6) -0.042(4) -0.005(4) -0.043(4) C11 0.033(2) 0.0200(19) 0.030(2) -0.0018(17) -0.0033(18) -0.0081(16) C12 0.038(3) 0.025(2) 0.075(4) -0.013(2) 0.000(3) -0.0081(19) C13 0.031(3) 0.036(2) 0.065(3) -0.013(2) 0.011(2) -0.008(2) C14 0.033(3) 0.034(2) 0.040(3) -0.009(2) 0.003(2) -0.0141(19) C15 0.060(4) 0.034(3) 0.183(8) -0.051(4) 0.034(4) -0.022(3) C16 0.052(3) 0.056(3) 0.083(4) -0.030(3) 0.026(3) -0.032(3) C17 0.032(2) 0.024(2) 0.032(2) -0.0004(18) 0.0009(19) -0.0107(17) C18 0.070(4) 0.028(2) 0.037(3) -0.002(2) -0.014(2) -0.020(2) C19 0.072(4) 0.035(2) 0.031(3) -0.005(2) -0.009(2) -0.013(2) C20 0.067(3) 0.030(2) 0.030(3) -0.002(2) 0.001(2) -0.014(2) C21 0.169(7) 0.033(3) 0.055(4) -0.014(3) -0.041(4) -0.034(4) C22 0.131(6) 0.041(3) 0.033(3) 0.001(2) 0.005(3) -0.021(3) Ba2 0.04630(19) 0.02185(13) 0.03470(17) -0.00616(11) 0.00261(13) -0.01206(12) F13 0.171(6) 0.431(11) 0.202(6) -0.262(8) 0.068(5) -0.126(7) F14 0.258(8) 0.139(5) 0.138(5) -0.027(4) 0.144(5) -0.035(5) F15 0.165(5) 0.131(4) 0.137(5) -0.023(4) 0.054(4) 0.043(4) F16 0.141(5) 0.091(3) 0.347(10) -0.048(5) 0.006(5) -0.077(3) F17 0.134(4) 0.196(5) 0.149(5) 0.061(4) -0.084(4) -0.117(4) F18 0.118(4) 0.230(6) 0.122(4) -0.012(4) -0.003(3) -0.133(4) F19 0.138(5) 0.138(4) 0.160(5) 0.091(4) 0.027(4) 0.032(4) F20 0.091(3) 0.102(3) 0.124(4) 0.028(3) -0.031(3) 0.004(2) F21 0.366(10) 0.082(3) 0.199(6) 0.080(4) -0.160(7) -0.127(5) F22 0.199(7) 0.355(10) 0.140(5) -0.163(6) 0.073(5) -0.183(7) F23 0.223(8) 0.328(10) 0.193(7) -0.152(7) -0.016(6) 0.163(8) F24 0.433(12) 0.185(6) 0.168(6) -0.116(5) 0.219(8) -0.191(8) O5 0.059(2) 0.061(2) 0.054(2) -0.0267(19) 0.0099(18) -0.0254(19) O6 0.049(2) 0.056(2) 0.068(3) -0.019(2) 0.0067(19) -0.0246(18) O7 0.066(3) 0.045(2) 0.065(3) 0.0051(19) -0.005(2) -0.0046(19) O8 0.073(3) 0.0362(19) 0.060(2) -0.0082(17) 0.012(2) -0.0027(18) N5 0.038(2) 0.0237(18) 0.053(3) -0.0035(17) 0.0006(19) -0.0084(15) N6 0.054(3) 0.0206(17) 0.040(2) -0.0025(16) 0.0149(19) -0.0063(16) N7 0.058(3) 0.0325(19) 0.026(2) -0.0044(16) 0.0024(18) -0.0230(17) N8 0.077(3) 0.0280(19) 0.031(2) 0.0009(16) -0.007(2) -0.0253(19) C23 0.068(4) 0.049(3) 0.039(3) -0.012(3) -0.001(3) -0.015(3) C24 0.073(4) 0.054(3) 0.065(4) -0.024(3) -0.007(3) -0.023(3) C25 0.057(3) 0.042(3) 0.060(4) 0.003(3) -0.012(3) -0.022(3) C26 0.115(7) 0.088(5) 0.065(5) -0.041(4) 0.019(5) -0.025(5) C27 0.070(5) 0.090(5) 0.081(5) -0.014(4) -0.017(4) -0.042(4) C28 0.038(3) 0.043(3) 0.088(5) 0.007(3) -0.014(3) -0.005(2) C29 0.050(3) 0.027(3) 0.095(5) -0.005(3) 0.000(3) -0.001(2) C30 0.040(3) 0.040(3) 0.076(4) -0.023(3) 0.010(3) -0.010(2) C31 0.057(4) 0.048(4) 0.115(6) 0.034(4) -0.002(4) 0.000(3) C32 0.087(5) 0.064(4) 0.100(6) -0.047(4) 0.034(5) -0.015(4) C33 0.038(3) 0.024(2) 0.034(2) -0.0032(18) -0.002(2) -0.0083(18) C34 0.054(3) 0.034(3) 0.054(3) 0.001(2) 0.020(3) -0.004(2) C35 0.042(3) 0.041(3) 0.076(4) 0.006(3) 0.017(3) -0.010(2) C36 0.039(3) 0.029(2) 0.081(4) 0.001(2) 0.000(3) -0.013(2) C37 0.101(5) 0.044(3) 0.124(6) -0.011(4) 0.071(5) -0.007(3) C38 0.066(4) 0.055(4) 0.173(8) -0.007(4) 0.021(5) -0.037(3) C39 0.041(3) 0.029(2) 0.024(2) -0.0015(18) -0.0034(19) -0.0128(19) C40 0.106(5) 0.039(3) 0.030(3) 0.002(2) -0.011(3) -0.036(3) C41 0.078(4) 0.051(3) 0.024(2) 0.007(2) -0.002(2) -0.033(3) C42 0.064(3) 0.043(3) 0.030(3) -0.008(2) 0.000(2) -0.027(2) C43 0.270(11) 0.061(4) 0.039(4) 0.025(3) -0.035(5) -0.091(5) C44 0.153(7) 0.075(4) 0.025(3) -0.010(3) 0.012(3) -0.065(4) _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 Ba1 O3 2.679(3) . ? Ba1 O4 2.683(3) . ? Ba1 O2 2.686(3) . ? Ba1 O1 2.694(3) . ? Ba1 N2 2.937(3) . ? Ba1 N4 2.941(3) . ? Ba1 N1 2.961(3) . ? Ba1 N3 2.982(3) . ? F1 C4 1.303(6) . ? F2 C4 1.324(6) . ? F3 C4 1.310(6) . ? F4 C5 1.262(7) . ? F5 C5 1.271(8) . ? F6 C5 1.198(7) . ? F7 C9 1.311(6) . ? F8 C9 1.301(6) . ? F9 C9 1.330(6) . ? F10 C10 1.214(7) . ? F11 C10 1.254(8) . ? F12 C10 1.286(8) . ? O1 C1 1.243(5) . ? O2 C3 1.235(5) . ? O3 C6 1.251(5) . ? O4 C8 1.246(6) . ? N1 C11 1.335(5) . ? N1 C12 1.346(5) . ? N2 C11 1.338(5) 2_566 ? N2 C14 1.362(5) . ? N3 C17 1.340(5) . ? N3 C18 1.361(6) . ? N4 C17 1.334(5) 2_576 ? N4 C20 1.354(5) . ? C1 C2 1.388(7) . ? C1 C4 1.536(7) . ? C2 C3 1.386(7) . ? C2 H2 0.9400 . ? C3 C5 1.523(7) . ? C6 C7 1.391(7) . ? C6 C9 1.519(7) . ? C7 C8 1.388(7) . ? C7 H7 0.9400 . ? C8 C10 1.519(7) . ? C11 N2 1.338(5) 2_566 ? C11 C11 1.489(8) 2_566 ? C12 C13 1.365(6) . ? C12 C15 1.518(6) . ? C13 C14 1.380(6) 2_566 ? C13 H13 0.9400 . ? C14 C13 1.380(6) 2_566 ? C14 C16 1.497(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 N4 1.334(5) 2_576 ? C17 C17 1.505(8) 2_576 ? C18 C19 1.379(6) . ? C18 C21 1.503(6) . ? C19 C20 1.374(6) 2_576 ? C19 H19 0.9400 . ? C20 C19 1.374(6) 2_576 ? C20 C22 1.498(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? Ba2 O5 2.658(3) . ? Ba2 O8 2.666(3) . ? Ba2 O7 2.678(3) . ? Ba2 O6 2.695(3) . ? Ba2 N5 2.967(3) . ? Ba2 N7 2.968(3) . ? Ba2 N6 2.968(3) . ? Ba2 N8 2.969(4) . ? F13 C26 1.263(8) . ? F14 C26 1.249(9) . ? F15 C26 1.292(9) . ? F16 C27 1.270(8) . ? F17 C27 1.290(8) . ? F18 C27 1.310(8) . ? F19 C31 1.337(8) . ? F20 C31 1.285(8) . ? F21 C31 1.262(8) . ? F22 C32 1.227(8) . ? F23 C32 1.258(8) . ? F24 C32 1.215(8) . ? O5 C23 1.239(6) . ? O6 C25 1.240(6) . ? O7 C28 1.223(6) . ? O8 C30 1.251(5) . ? N5 C33 1.325(5) . ? N5 C36 1.361(6) . ? N6 C33 1.341(5) 2_665 ? N6 C34 1.341(6) . ? N7 C39 1.340(5) . ? N7 C42 1.349(5) . ? N8 C40 1.341(6) . ? N8 C39 1.342(5) 2_655 ? C23 C24 1.394(7) . ? C23 C26 1.509(8) . ? C24 C25 1.369(8) . ? C24 H24 0.9400 . ? C25 C27 1.532(8) . ? C28 C29 1.411(8) . ? C28 C31 1.524(8) . ? C29 C30 1.380(7) . ? C29 H29 0.9400 . ? C30 C32 1.496(8) . ? C33 N6 1.341(5) 2_665 ? C33 C33 1.500(8) 2_665 ? C34 C35 1.368(7) . ? C34 C37 1.510(7) . ? C35 C36 1.379(6) 2_665 ? C35 H35 0.9400 . ? C36 C35 1.379(6) 2_665 ? C36 C38 1.489(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 N8 1.342(5) 2_655 ? C39 C39 1.497(8) 2_655 ? C40 C41 1.377(6) . ? C40 C43 1.505(7) . ? C41 C42 1.361(6) 2_655 ? C41 H41 0.9400 . ? C42 C41 1.361(6) 2_655 ? C42 C44 1.508(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? 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 O3 Ba1 O4 64.73(11) . . ? O3 Ba1 O2 107.68(11) . . ? O4 Ba1 O2 84.09(11) . . ? O3 Ba1 O1 171.79(11) . . ? O4 Ba1 O1 109.65(11) . . ? O2 Ba1 O1 65.00(10) . . ? O3 Ba1 N2 90.69(9) . . ? O4 Ba1 N2 134.08(11) . . ? O2 Ba1 N2 66.45(10) . . ? O1 Ba1 N2 89.56(10) . . ? O3 Ba1 N4 90.42(10) . . ? O4 Ba1 N4 66.45(11) . . ? O2 Ba1 N4 134.80(10) . . ? O1 Ba1 N4 92.60(10) . . ? N2 Ba1 N4 156.63(10) . . ? O3 Ba1 N1 123.31(11) . . ? O4 Ba1 N1 170.00(10) . . ? O2 Ba1 N1 97.92(10) . . ? O1 Ba1 N1 63.01(11) . . ? N2 Ba1 N1 54.83(9) . . ? N4 Ba1 N1 106.05(9) . . ? O3 Ba1 N3 62.77(11) . . ? O4 Ba1 N3 96.52(10) . . ? O2 Ba1 N3 168.51(10) . . ? O1 Ba1 N3 124.93(10) . . ? N2 Ba1 N3 105.94(10) . . ? N4 Ba1 N3 54.58(10) . . ? N1 Ba1 N3 83.47(10) . . ? C1 O1 Ba1 133.1(3) . . ? C3 O2 Ba1 132.6(3) . . ? C6 O3 Ba1 134.0(3) . . ? C8 O4 Ba1 133.6(3) . . ? C11 N1 C12 117.2(4) . . ? C11 N1 Ba1 121.0(3) . . ? C12 N1 Ba1 117.8(3) . . ? C11 N2 C14 117.2(3) 2_566 . ? C11 N2 Ba1 121.8(3) 2_566 . ? C14 N2 Ba1 117.3(3) . . ? C17 N3 C18 116.6(4) . . ? C17 N3 Ba1 121.5(3) . . ? C18 N3 Ba1 117.7(3) . . ? C17 N4 C20 116.9(3) 2_576 . ? C17 N4 Ba1 122.1(3) 2_576 . ? C20 N4 Ba1 117.0(3) . . ? O1 C1 C2 128.6(5) . . ? O1 C1 C4 114.6(4) . . ? C2 C1 C4 116.7(4) . . ? C3 C2 C1 122.7(4) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? O2 C3 C2 129.9(5) . . ? O2 C3 C5 114.3(5) . . ? C2 C3 C5 115.7(5) . . ? F1 C4 F3 107.0(5) . . ? F1 C4 F2 105.2(5) . . ? F3 C4 F2 107.2(5) . . ? F1 C4 C1 113.0(4) . . ? F3 C4 C1 110.8(4) . . ? F2 C4 C1 113.2(5) . . ? F6 C5 F4 107.1(7) . . ? F6 C5 F5 103.0(7) . . ? F4 C5 F5 100.1(7) . . ? F6 C5 C3 116.5(6) . . ? F4 C5 C3 115.3(6) . . ? F5 C5 C3 113.0(6) . . ? O3 C6 C7 127.9(5) . . ? O3 C6 C9 115.7(5) . . ? C7 C6 C9 116.4(5) . . ? C8 C7 C6 123.2(5) . . ? C8 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? O4 C8 C7 128.6(5) . . ? O4 C8 C10 114.2(5) . . ? C7 C8 C10 117.2(5) . . ? F8 C9 F7 108.1(6) . . ? F8 C9 F9 106.9(5) . . ? F7 C9 F9 103.5(5) . . ? F8 C9 C6 111.8(5) . . ? F7 C9 C6 113.0(4) . . ? F9 C9 C6 113.0(5) . . ? F10 C10 F11 107.6(8) . . ? F10 C10 F12 106.5(7) . . ? F11 C10 F12 97.6(7) . . ? F10 C10 C8 116.1(6) . . ? F11 C10 C8 114.4(6) . . ? F12 C10 C8 112.9(7) . . ? N1 C11 N2 125.4(4) . 2_566 ? N1 C11 C11 117.6(4) . 2_566 ? N2 C11 C11 117.0(4) 2_566 2_566 ? N1 C12 C13 121.1(4) . . ? N1 C12 C15 117.4(4) . . ? C13 C12 C15 121.5(4) . . ? C12 C13 C14 119.3(4) . 2_566 ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 2_566 . ? N2 C14 C13 119.9(4) . 2_566 ? N2 C14 C16 118.5(4) . . ? C13 C14 C16 121.6(4) 2_566 . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 N3 126.2(4) 2_576 . ? N4 C17 C17 117.8(4) 2_576 2_576 ? N3 C17 C17 116.0(4) . 2_576 ? N3 C18 C19 120.3(4) . . ? N3 C18 C21 117.9(4) . . ? C19 C18 C21 121.7(4) . . ? C20 C19 C18 119.3(4) 2_576 . ? C20 C19 H19 120.3 2_576 . ? C18 C19 H19 120.3 . . ? N4 C20 C19 120.6(4) . 2_576 ? N4 C20 C22 118.0(4) . . ? C19 C20 C22 121.4(4) 2_576 . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 Ba2 O8 157.23(12) . . ? O5 Ba2 O7 98.06(11) . . ? O8 Ba2 O7 65.03(11) . . ? O5 Ba2 O6 64.64(11) . . ? O8 Ba2 O6 97.60(11) . . ? O7 Ba2 O6 85.85(12) . . ? O5 Ba2 N5 66.09(11) . . ? O8 Ba2 N5 133.66(11) . . ? O7 Ba2 N5 159.47(11) . . ? O6 Ba2 N5 97.92(10) . . ? O5 Ba2 N7 96.74(10) . . ? O8 Ba2 N7 89.72(10) . . ? O7 Ba2 N7 64.82(11) . . ? O6 Ba2 N7 143.33(11) . . ? N5 Ba2 N7 102.71(10) . . ? O5 Ba2 N6 89.41(10) . . ? O8 Ba2 N6 95.45(10) . . ? O7 Ba2 N6 142.31(12) . . ? O6 Ba2 N6 64.12(11) . . ? N5 Ba2 N6 54.33(10) . . ? N7 Ba2 N6 151.06(11) . . ? O5 Ba2 N8 134.81(11) . . ? O8 Ba2 N8 65.72(12) . . ? O7 Ba2 N8 98.23(11) . . ? O6 Ba2 N8 158.39(11) . . ? N5 Ba2 N8 85.70(10) . . ? N7 Ba2 N8 54.33(10) . . ? N6 Ba2 N8 102.34(10) . . ? C23 O5 Ba2 137.6(3) . . ? C25 O6 Ba2 135.5(3) . . ? C28 O7 Ba2 136.2(4) . . ? C30 O8 Ba2 136.0(3) . . ? C33 N5 C36 117.1(4) . . ? C33 N5 Ba2 118.6(3) . . ? C36 N5 Ba2 116.9(3) . . ? C33 N6 C34 116.4(4) 2_665 . ? C33 N6 Ba2 118.1(3) 2_665 . ? C34 N6 Ba2 118.0(3) . . ? C39 N7 C42 116.1(3) . . ? C39 N7 Ba2 118.4(3) . . ? C42 N7 Ba2 118.2(3) . . ? C40 N8 C39 116.5(4) . 2_655 ? C40 N8 Ba2 118.0(3) . . ? C39 N8 Ba2 118.3(3) 2_655 . ? O5 C23 C24 127.5(5) . . ? O5 C23 C26 115.0(6) . . ? C24 C23 C26 117.5(5) . . ? C25 C24 C23 123.6(5) . . ? C25 C24 H24 118.2 . . ? C23 C24 H24 118.2 . . ? O6 C25 C24 128.7(5) . . ? O6 C25 C27 114.7(5) . . ? C24 C25 C27 116.6(5) . . ? F14 C26 F13 106.8(8) . . ? F14 C26 F15 104.2(8) . . ? F13 C26 F15 100.4(7) . . ? F14 C26 C23 115.5(6) . . ? F13 C26 C23 116.7(7) . . ? F15 C26 C23 111.6(7) . . ? F16 C27 F17 108.1(7) . . ? F16 C27 F18 106.1(7) . . ? F17 C27 F18 102.4(7) . . ? F16 C27 C25 114.5(6) . . ? F17 C27 C25 111.9(6) . . ? F18 C27 C25 112.9(6) . . ? O7 C28 C29 127.3(5) . . ? O7 C28 C31 116.8(6) . . ? C29 C28 C31 115.9(5) . . ? C30 C29 C28 123.8(5) . . ? C30 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? O8 C30 C29 127.9(5) . . ? O8 C30 C32 113.5(6) . . ? C29 C30 C32 118.4(5) . . ? F21 C31 F20 106.6(6) . . ? F21 C31 F19 106.4(7) . . ? F20 C31 F19 102.1(7) . . ? F21 C31 C28 115.2(7) . . ? F20 C31 C28 113.8(6) . . ? F19 C31 C28 111.5(5) . . ? F24 C32 F22 104.3(9) . . ? F24 C32 F23 104.1(8) . . ? F22 C32 F23 99.0(7) . . ? F24 C32 C30 116.4(6) . . ? F22 C32 C30 116.1(7) . . ? F23 C32 C30 114.7(8) . . ? N5 C33 N6 126.0(4) . 2_665 ? N5 C33 C33 117.2(4) . 2_665 ? N6 C33 C33 116.8(4) 2_665 2_665 ? N6 C34 C35 121.7(4) . . ? N6 C34 C37 117.9(5) . . ? C35 C34 C37 120.4(5) . . ? C34 C35 C36 118.8(5) . 2_665 ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 2_665 . ? N5 C36 C35 120.0(4) . 2_665 ? N5 C36 C38 118.3(4) . . ? C35 C36 C38 121.6(5) 2_665 . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 N8 126.2(4) . 2_655 ? N7 C39 C39 117.0(4) . 2_655 ? N8 C39 C39 116.9(4) 2_655 2_655 ? N8 C40 C41 120.7(4) . . ? N8 C40 C43 117.2(4) . . ? C41 C40 C43 122.1(5) . . ? C42 C41 C40 119.3(4) 2_655 . ? C42 C41 H41 120.4 2_655 . ? C40 C41 H41 120.4 . . ? N7 C42 C41 121.2(4) . 2_655 ? N7 C42 C44 117.1(4) . . ? C41 C42 C44 121.7(4) 2_655 . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.897 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.104