Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Prof Malcolm L. H. Green' _publ_contact_author_address ; Prof Malcolm L. H. Green Inorganic Chemistry Laboratory Oxford University South Parks Road Oxford City England OX1 3QR UNITED KINGDOM ; _publ_contact_author_email 'MALCOLM.GREEN@CHEM.OX.AC.UK ' _publ_requested_journal ' Dalton Trans.' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; New derivatives of the anionic ligands [XB(C6F5)3]-, where X=CN-, NC-, SCN- and their coordination chemistry ; loop_ _publ_author_name _publ_author_address 'Vei, I. C.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK # Address for author 1 ; 'Pascu, S. I.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK # Address 2 ; 'Green, M. L. H' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK # Address 3 ; 'Green, J. C.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address 4 ; 'Shilling, R. E.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address 5 ; 'Anderson, G. D. W.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' ; 'Rees, Leigh H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' ; # Address 7 #============================================================================== # 4. TEXT _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 for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references # Add your own references - in alphabetic order ; # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # Denzo # 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. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # Azimutal absorption correction # North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. # DIFABS # Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. # RC93 # Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; data_compound1 _database_code_CSD 204648 # Local code str46 _audit_creation_method CRYSTALS_ver_12_03_99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' Enraf-nonius DIP2000 ' _computing_data_collection 'DIP2000 software ,Xpress, MAC Science, 1989' _computing_data_reduction ; 'DIP2000 software DENZO, Otwinowski & Minor, 1996' ; _computing_cell_refinement ; 'DIP2000 software DENZO, Otwinowski & Minor, 1996' ; # end_choice #========================================================================== _chemical_name_systematic ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 8.9130(5) _cell_angle_alpha 90 _cell_length_b 21.0570(15) _cell_angle_beta 97.339(5) _cell_length_c 18.7380(14) _cell_angle_gamma 90 _cell_volume 3488.0(5) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'K ' 0.1790 0.2500 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum 'C31 H24 B F15 K N O6 S' _chemical_formula_moiety 'C31 H24 B F15 K N O6 S' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 873.47 _cell_measurement_reflns_used 35534 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.66 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1762.26 _exptl_absorpt_coefficient_mu 0.34 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.90 # Sheldrick geometric definitions 0.90 0.90 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 35534 _reflns_number_total 6629 _diffrn_reflns_av_R_equivalents 0.04 # Number of reflections with Friedels Law is 6629 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7285 _diffrn_measured_fraction_theta_max 0.910 _reflns_number_gt 4777 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -0.86 _refine_diff_density_max 0.89 _reflns_threshold_expression >5.00\s(I) _refine_ls_number_reflns 4777 _refine_ls_number_parameters 508 _refine_ls_R_factor_gt 0.0884 _refine_ls_wR_factor_ref 0.0152 _refine_ls_goodness_of_fit_ref 0.9950 _refine_ls_shift/su_max 0.000390 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.33 -3.64 1.01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _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 K1 1.0000 0.0000 0.5000 0.0259 1.0000 Uani K2 0.0000 0.5000 0.5000 0.0289 1.0000 Uani C1 0.8069(3) 0.25237(11) 0.7184(1) 0.0254 1.0000 Uani C11 0.4688(3) 0.2122(1) 0.79229(11) 0.0249 1.0000 Uani C12 0.5249(2) 0.15430(11) 0.81847(11) 0.0265 1.0000 Uani C13 0.4938(3) 0.12757(11) 0.88217(12) 0.0306 1.0000 Uani C14 0.4069(3) 0.16020(11) 0.92435(11) 0.0321 1.0000 Uani C15 0.3504(3) 0.21908(11) 0.90229(12) 0.0307 1.0000 Uani C16 0.3800(3) 0.2427(1) 0.83752(11) 0.0278 1.0000 Uani C21 0.4355(3) 0.3076(1) 0.69191(11) 0.0242 1.0000 Uani C22 0.4924(3) 0.3606(1) 0.72985(12) 0.0293 1.0000 Uani C23 0.4381(3) 0.4216(1) 0.71715(14) 0.0349 1.0000 Uani C24 0.3196(3) 0.43091(11) 0.66413(15) 0.0369 1.0000 Uani C25 0.2595(3) 0.38037(13) 0.62436(13) 0.0341 1.0000 Uani C26 0.3164(2) 0.3204(1) 0.63977(12) 0.0266 1.0000 Uani C31 0.4516(3) 0.1830(1) 0.64933(12) 0.0269 1.0000 Uani C32 0.5070(3) 0.18579(11) 0.58426(12) 0.0310 1.0000 Uani C33 0.4784(3) 0.14128(12) 0.53036(13) 0.0356 1.0000 Uani C34 0.3879(3) 0.09005(11) 0.54114(13) 0.0379 1.0000 Uani C35 0.3259(3) 0.0864(1) 0.60359(13) 0.0339 1.0000 Uani C36 0.3566(3) 0.13192(11) 0.65520(11) 0.0296 1.0000 Uani C41 0.8013(3) 0.02866(11) 0.65588(12) 0.0309 1.0000 Uani C42 0.8617(3) 0.09415(11) 0.64269(12) 0.0337 1.0000 Uani C44 0.9359(3) 0.1608(1) 0.55270(13) 0.0377 1.0000 Uani C45 0.9295(3) 0.16691(11) 0.47257(14) 0.0398 1.0000 Uani C47 1.0152(3) 0.12411(11) 0.36996(12) 0.0328 1.0000 Uani C48 1.1325(3) 0.0797(1) 0.34616(11) 0.0328 1.0000 Uani C51 -0.2249(3) 0.46916(13) 0.64576(13) 0.0396 1.0000 Uani C52 -0.1153(3) 0.51847(11) 0.67720(14) 0.0379 1.0000 Uani C54 0.0165(3) 0.61017(11) 0.64986(14) 0.0373 1.0000 Uani C55 0.0521(3) 0.65233(11) 0.58912(13) 0.0357 1.0000 Uani C57 0.1757(3) 0.6554(1) 0.48562(13) 0.0379 1.0000 Uani C58 0.2562(3) 0.61542(12) 0.43658(13) 0.0373 1.0000 Uani N1 0.6767(2) 0.24172(8) 0.7173(1) 0.0280 1.0000 Uani O43 0.87109(19) 0.10124(7) 0.56771(8) 0.0325 1.0000 Uani O46 1.02337(19) 0.12020(7) 0.44655(8) 0.0328 1.0000 Uani O49 1.09066(19) 0.01649(6) 0.36232(8) 0.0301 1.0000 Uani O53 -0.08462(19) 0.56114(7) 0.62156(8) 0.0324 1.0000 Uani O56 0.13368(19) 0.61684(7) 0.54238(8) 0.0313 1.0000 Uani O59 0.15784(18) 0.56743(7) 0.40561(8) 0.0317 1.0000 Uani S1 0.98406(7) 0.26459(4) 0.71927(4) 0.0445 1.0000 Uani F12 0.61009(16) 0.11874(6) 0.77889(6) 0.0327 1.0000 Uani F13 0.54386(17) 0.06959(6) 0.90252(7) 0.0408 1.0000 Uani F14 0.37636(18) 0.13588(7) 0.98712(7) 0.0452 1.0000 Uani F15 0.26563(16) 0.25188(7) 0.94347(7) 0.0417 1.0000 Uani F16 0.31595(15) 0.29956(6) 0.81931(7) 0.0352 1.0000 Uani F22 0.60598(16) 0.35335(7) 0.78447(8) 0.0425 1.0000 Uani F23 0.4974(2) 0.47028(6) 0.75741(9) 0.0535 1.0000 Uani F24 0.26118(18) 0.48924(6) 0.65113(9) 0.0551 1.0000 Uani F25 0.14682(18) 0.39057(7) 0.57114(8) 0.0461 1.0000 Uani F26 0.24660(15) 0.27388(6) 0.59822(7) 0.0347 1.0000 Uani F32 0.59267(16) 0.23586(6) 0.56890(7) 0.0431 1.0000 Uani F33 0.53416(18) 0.14778(9) 0.46715(8) 0.0547 1.0000 Uani F34 0.3580(2) 0.04529(7) 0.48999(8) 0.0561 1.0000 Uani F35 0.23269(19) 0.03725(7) 0.61364(8) 0.0549 1.0000 Uani F36 0.28444(16) 0.12486(7) 0.71429(7) 0.0438 1.0000 Uani B1 0.5044(3) 0.23594(11) 0.71224(14) 0.0247 1.0000 Uani H411 0.7789 0.0237 0.7063 0.0600 1.0000 Uiso H412 0.6998 0.0223 0.6227 0.0600 1.0000 Uiso H421 0.9684 0.0989 0.6697 0.0600 1.0000 Uiso H422 0.7983 0.1292 0.6588 0.0600 1.0000 Uiso H441 1.0471 0.1623 0.5749 0.0600 1.0000 Uiso H442 0.8825 0.1967 0.5732 0.0600 1.0000 Uiso H451 0.9625 0.2107 0.4593 0.0499 1.0000 Uiso H452 0.8210 0.1609 0.4501 0.0499 1.0000 Uiso H471 1.0308 0.1689 0.3535 0.0600 1.0000 Uiso H472 0.9107 0.1100 0.3459 0.0600 1.0000 Uiso H481 1.2361 0.0902 0.3751 0.0600 1.0000 Uiso H482 1.1442 0.0845 0.2942 0.0600 1.0000 Uiso H511 -0.2563 0.4402 0.6844 0.0525 1.0000 Uiso H512 -0.3208 0.4902 0.6212 0.0525 1.0000 Uiso H521 -0.1607 0.5430 0.7162 0.0511 1.0000 Uiso H522 -0.0204 0.4976 0.7002 0.0511 1.0000 Uiso H541 -0.0271 0.6348 0.6878 0.0490 1.0000 Uiso H542 0.1158 0.5902 0.6734 0.0490 1.0000 Uiso H551 0.1099 0.6909 0.6080 0.0444 1.0000 Uiso H552 -0.0484 0.6677 0.5617 0.0444 1.0000 Uiso H571 0.2371 0.6927 0.5046 0.0486 1.0000 Uiso H572 0.0779 0.6737 0.4563 0.0486 1.0000 Uiso H581 0.2930 0.6420 0.3976 0.0457 1.0000 Uiso H582 0.3472 0.5954 0.4658 0.0457 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 K1 0.0368(4) 0.0190(3) 0.0233(3) -0.0004(3) 0.0087(3) -0.0022(3) K2 0.0384(4) 0.0212(3) 0.0288(4) 0.0002(3) 0.0103(3) -0.0024(3) C1 0.0337(13) 0.024(1) 0.0180(9) -0.0040(9) 0.0025(9) 0.001(1) C11 0.0236(12) 0.0278(12) 0.0238(11) -0.0005(9) 0.0044(9) -0.0062(9) C12 0.0221(12) 0.0358(13) 0.0219(11) -0.005(1) 0.0040(9) -0.000(1) C13 0.0266(13) 0.0312(12) 0.0330(13) -0.001(1) -0.000(1) 0.004(1) C14 0.0259(14) 0.0510(15) 0.0196(11) 0.005(1) 0.004(1) 0.0006(11) C15 0.0263(13) 0.0403(13) 0.0278(12) -0.008(1) 0.0123(11) 0.001(1) C16 0.0248(11) 0.0258(12) 0.0324(12) -0.0069(9) 0.003(1) 0.0007(9) C21 0.0236(12) 0.0215(11) 0.0299(12) 0.0035(8) 0.0127(11) -0.0008(9) C22 0.0264(12) 0.0292(11) 0.0352(13) -0.0008(9) 0.0148(11) -0.002(1) C23 0.0341(14) 0.0227(12) 0.0521(15) -0.005(1) 0.0219(13) -0.005(1) C24 0.0335(15) 0.0307(12) 0.0521(16) 0.0073(11) 0.0271(14) 0.0046(11) C25 0.0255(14) 0.0451(15) 0.0339(14) 0.009(1) 0.0125(11) 0.0053(11) C26 0.0239(13) 0.0287(11) 0.0293(12) 0.0009(9) 0.0117(11) -0.0032(9) C31 0.0255(13) 0.0276(11) 0.0276(11) -0.0031(9) 0.003(1) 0.0044(9) C32 0.0306(14) 0.0353(13) 0.0270(11) 0.0027(9) 0.0025(11) 0.000(1) C33 0.0364(15) 0.0458(16) 0.0255(13) -0.005(1) 0.0067(11) 0.0100(12) C34 0.0449(16) 0.0288(12) 0.0355(13) -0.011(1) -0.0126(12) 0.0088(11) C35 0.0347(15) 0.0265(12) 0.0381(14) -0.0017(9) -0.0045(11) -0.004(1) C36 0.0270(13) 0.0323(12) 0.0295(13) 0.0040(9) 0.004(1) -0.003(1) C41 0.0360(15) 0.0342(12) 0.0250(11) -0.0052(9) 0.0139(11) -0.0003(11) C42 0.0470(16) 0.0295(12) 0.0256(11) -0.007(1) 0.008(1) 0.0029(11) C44 0.0500(16) 0.0213(11) 0.0441(14) -0.001(1) 0.0155(12) 0.0067(11) C45 0.0483(17) 0.0252(12) 0.0501(15) 0.008(1) 0.0225(13) 0.0113(11) C47 0.0439(16) 0.0282(13) 0.0281(12) 0.0116(9) 0.0119(11) 0.000(1) C48 0.0443(15) 0.0328(12) 0.0239(11) 0.0045(9) 0.0141(11) -0.000(1) C51 0.0424(16) 0.0433(15) 0.0366(15) -0.0042(11) 0.0184(12) -0.0062(12) C52 0.0426(16) 0.0374(13) 0.0364(13) 0.001(1) 0.0153(12) -0.0029(11) C54 0.0457(16) 0.0292(12) 0.0369(13) -0.004(1) 0.0051(11) -0.0039(11) C55 0.0430(15) 0.0223(11) 0.0426(14) -0.004(1) 0.0092(12) 0.0005(11) C57 0.0442(16) 0.0260(12) 0.0439(14) 0.0039(11) 0.0068(12) -0.0174(11) C58 0.0406(15) 0.0381(14) 0.0352(13) -0.000(1) 0.0129(11) -0.0157(12) N1 0.0279(12) 0.026(1) 0.031(1) -0.0008(8) 0.0064(8) -0.0002(8) O43 0.043(1) 0.0241(7) 0.0320(8) -0.0020(6) 0.0123(7) -0.0017(7) O46 0.041(1) 0.0255(7) 0.0340(9) 0.0051(7) 0.0115(8) 0.0068(7) O49 0.035(1) 0.0269(9) 0.0305(8) -0.0006(6) 0.0123(7) -0.0053(6) O53 0.035(1) 0.0324(9) 0.0296(8) -0.0021(6) 0.0039(7) -0.0002(7) O56 0.0381(9) 0.0219(7) 0.0359(9) 0.0011(6) 0.0128(8) -0.0026(7) O59 0.0313(9) 0.0309(9) 0.0345(9) 0.0006(7) 0.0106(7) -0.0054(7) S1 0.0260(3) 0.0633(4) 0.0458(4) -0.0189(3) 0.0109(3) -0.0115(3) F12 0.0393(8) 0.0310(7) 0.0296(7) -0.0017(5) 0.0112(6) 0.0120(6) F13 0.0500(9) 0.0367(7) 0.0360(7) 0.0085(6) 0.0066(7) 0.0059(7) F14 0.0499(9) 0.057(1) 0.0315(8) 0.0101(6) 0.0146(6) 0.0062(7) F15 0.0453(8) 0.0504(9) 0.0329(7) -0.0063(6) 0.0187(6) 0.0084(7) F16 0.0359(8) 0.0325(7) 0.0398(7) -0.0011(6) 0.0147(6) 0.0047(6) F22 0.0363(8) 0.0414(8) 0.0486(8) -0.0164(7) 0.0006(7) -0.0013(7) F23 0.053(1) 0.0327(8) 0.0783(11) -0.0214(8) 0.0216(8) -0.0116(8) F24 0.055(1) 0.0280(8) 0.0883(12) 0.0142(7) 0.0334(9) 0.0097(7) F25 0.0422(9) 0.0492(9) 0.0481(9) 0.0149(7) 0.0103(8) 0.0173(7) F26 0.0327(8) 0.0374(7) 0.0330(8) -0.0034(6) -0.0001(6) 0.0052(6) F32 0.050(1) 0.0468(9) 0.0352(7) 0.0027(6) 0.0170(7) -0.0138(7) F33 0.0576(11) 0.0781(12) 0.0301(8) -0.0126(7) 0.0119(7) 0.0025(9) F34 0.0689(12) 0.0487(9) 0.0455(9) -0.0283(7) -0.0131(8) 0.0078(8) F35 0.0600(11) 0.0447(9) 0.056(1) -0.0005(7) -0.0098(8) -0.0232(8) F36 0.0429(9) 0.055(1) 0.0342(8) 0.0014(6) 0.0078(7) -0.0219(7) B1 0.0218(14) 0.0215(13) 0.0313(14) -0.000(1) 0.0053(11) 0.001(1) _refine_ls_extinction_method None 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 C1 . N1 . 1.180(3) yes C1 . S1 . 1.598(2) yes C11 . C12 . 1.384(3) yes C11 . C16 . 1.388(3) yes C11 . B1 . 1.650(3) yes C12 . C13 . 1.379(3) yes C12 . F12 . 1.353(2) yes C13 . C14 . 1.361(3) yes C13 . F13 . 1.339(2) yes C14 . C15 . 1.381(3) yes C14 . F14 . 1.342(2) yes C15 . C16 . 1.368(3) yes C15 . F15 . 1.339(3) yes C16 . F16 . 1.352(2) yes C21 . C22 . 1.386(3) yes C21 . C26 . 1.375(3) yes C21 . B1 . 1.654(3) yes C22 . C23 . 1.382(3) yes C22 . F22 . 1.353(3) yes C23 . C24 . 1.369(4) yes C23 . F23 . 1.340(3) yes C24 . C25 . 1.368(4) yes C24 . F24 . 1.344(3) yes C25 . C26 . 1.377(3) yes C25 . F25 . 1.339(3) yes C26 . F26 . 1.353(2) yes C31 . C32 . 1.374(3) yes C31 . C36 . 1.382(3) yes C31 . B1 . 1.647(3) yes C32 . C33 . 1.377(3) yes C32 . F32 . 1.354(3) yes C33 . C34 . 1.377(4) yes C33 . F33 . 1.349(3) yes C34 . C35 . 1.359(3) yes C34 . F34 . 1.346(3) yes C35 . C36 . 1.365(3) yes C35 . F35 . 1.355(3) yes C36 . F36 . 1.358(2) yes C41 . C42 . 1.512(3) yes C41 . O49 2_756 1.425(3) yes C41 . H411 . 0.995 no C41 . H412 . 1.039 no C42 . O43 . 1.426(3) yes C42 . H421 . 1.024 no C42 . H422 . 0.999 no C44 . C45 . 1.501(3) yes C44 . O43 . 1.423(3) yes C44 . H441 . 1.025 no C44 . H442 . 0.998 no C45 . O46 . 1.417(3) yes C45 . H451 . 1.009 no C45 . H452 . 1.013 no C47 . C48 . 1.512(3) yes C47 . O46 . 1.430(3) yes C47 . H471 . 1.008 no C47 . H472 . 1.026 no C48 . O49 . 1.425(3) yes C48 . H481 . 1.033 no C48 . H482 . 0.998 no C51 . C52 . 1.494(4) yes C51 . O59 2_566 1.423(3) yes C51 . H511 . 1.013 no C51 . H512 . 1.018 no C52 . O53 . 1.429(3) yes C52 . H521 . 1.021 no C52 . H522 . 1.001 no C54 . C55 . 1.509(3) yes C54 . O53 . 1.427(3) yes C54 . H541 . 0.999 no C54 . H542 . 1.027 no C55 . O56 . 1.420(3) yes C55 . H551 . 1.001 no C55 . H552 . 1.027 no C57 . C58 . 1.495(3) yes C57 . O56 . 1.425(3) yes C57 . H571 . 0.997 no C57 . H572 . 1.044 no C58 . O59 . 1.413(3) yes C58 . H581 . 1.007 no C58 . H582 . 1.010 no N1 . B1 . 1.531(3) 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 N1 . C1 . S1 . 178.3(2) yes C12 . C11 . C16 . 113.53(19) yes C12 . C11 . B1 . 119.08(18) yes C16 . C11 . B1 . 127.32(19) yes C11 . C12 . C13 . 124.22(19) yes C11 . C12 . F12 . 119.75(19) yes C13 . C12 . F12 . 115.9(2) yes C12 . C13 . C14 . 119.3(2) yes C12 . C13 . F13 . 121.5(2) yes C14 . C13 . F13 . 119.2(2) yes C13 . C14 . C15 . 119.46(19) yes C13 . C14 . F14 . 120.7(2) yes C15 . C14 . F14 . 119.85(19) yes C14 . C15 . C16 . 119.14(19) yes C14 . C15 . F15 . 120.10(19) yes C16 . C15 . F15 . 120.7(2) yes C11 . C16 . C15 . 124.3(2) yes C11 . C16 . F16 . 120.70(19) yes C15 . C16 . F16 . 114.98(18) yes C22 . C21 . C26 . 113.8(2) yes C22 . C21 . B1 . 121.1(2) yes C26 . C21 . B1 . 125.00(19) yes C21 . C22 . C23 . 124.4(2) yes C21 . C22 . F22 . 119.1(2) yes C23 . C22 . F22 . 116.6(2) yes C22 . C23 . C24 . 118.6(2) yes C22 . C23 . F23 . 120.6(2) yes C24 . C23 . F23 . 120.8(2) yes C23 . C24 . C25 . 119.8(2) yes C23 . C24 . F24 . 120.5(2) yes C25 . C24 . F24 . 119.8(3) yes C24 . C25 . C26 . 119.4(2) yes C24 . C25 . F25 . 119.0(2) yes C26 . C25 . F25 . 121.6(2) yes C21 . C26 . C25 . 124.1(2) yes C21 . C26 . F26 . 121.54(19) yes C25 . C26 . F26 . 114.4(2) yes C32 . C31 . C36 . 113.4(2) yes C32 . C31 . B1 . 120.26(19) yes C36 . C31 . B1 . 126.29(18) yes C31 . C32 . C33 . 124.6(2) yes C31 . C32 . F32 . 119.9(2) yes C33 . C32 . F32 . 115.49(19) yes C32 . C33 . C34 . 118.8(2) yes C32 . C33 . F33 . 121.4(2) yes C34 . C33 . F33 . 119.8(2) yes C33 . C34 . C35 . 118.8(2) yes C33 . C34 . F34 . 120.7(2) yes C35 . C34 . F34 . 120.5(2) yes C34 . C35 . C36 . 120.2(2) yes C34 . C35 . F35 . 119.2(2) yes C36 . C35 . F35 . 120.6(2) yes C31 . C36 . C35 . 124.1(2) yes C31 . C36 . F36 . 120.61(18) yes C35 . C36 . F36 . 115.3(2) yes C42 . C41 . O49 2_756 107.69(18) yes C42 . C41 . H411 . 111.7 no O49 2_756 C41 . H411 . 112.4 no C42 . C41 . H412 . 108.7 no O49 2_756 C41 . H412 . 109.57 no H411 . C41 . H412 . 106.8 no C41 . C42 . O43 . 108.86(18) yes C41 . C42 . H421 . 109.7 no O43 . C42 . H421 . 108.0 no C41 . C42 . H422 . 113.4 no O43 . C42 . H422 . 109.1 no H421 . C42 . H422 . 107.7 no C45 . C44 . O43 . 108.00(19) yes C45 . C44 . H441 . 108.4 no O43 . C44 . H441 . 110.1 no C45 . C44 . H442 . 111.2 no O43 . C44 . H442 . 111.5 no H441 . C44 . H442 . 107.6 no C44 . C45 . O46 . 109.6(2) yes C44 . C45 . H451 . 110.5 no O46 . C45 . H451 . 110.3 no C44 . C45 . H452 . 108.5 no O46 . C45 . H452 . 110.1 no H451 . C45 . H452 . 107.8 no C48 . C47 . O46 . 108.17(18) yes C48 . C47 . H471 . 111.1 no O46 . C47 . H471 . 111.7 no C48 . C47 . H472 . 108.3 no O46 . C47 . H472 . 110.61 no H471 . C47 . H472 . 106.8 no C47 . C48 . O49 . 107.79(18) yes C47 . C48 . H481 . 108.57 no O49 . C48 . H481 . 109.18 no C47 . C48 . H482 . 112.8 no O49 . C48 . H482 . 111.44 no H481 . C48 . H482 . 107.0 no C52 . C51 . O59 2_566 109.47(19) yes C52 . C51 . H511 . 111.2 no O59 2_566 C51 . H511 . 109.7 no C52 . C51 . H512 . 110.2 no O59 2_566 C51 . H512 . 109.3 no H511 . C51 . H512 . 107.0 no C51 . C52 . O53 . 109.0(2) yes C51 . C52 . H521 . 109.6 no O53 . C52 . H521 . 109.5 no C51 . C52 . H522 . 109.7 no O53 . C52 . H522 . 111.1 no H521 . C52 . H522 . 107.8 no C55 . C54 . O53 . 109.2(2) yes C55 . C54 . H541 . 111.7 no O53 . C54 . H541 . 110.9 no C55 . C54 . H542 . 108.2 no O53 . C54 . H542 . 109.4 no H541 . C54 . H542 . 107.4 no C54 . C55 . O56 . 109.23(19) yes C54 . C55 . H551 . 111.0 no O56 . C55 . H551 . 111.3 no C54 . C55 . H552 . 108.0 no O56 . C55 . H552 . 109.9 no H551 . C55 . H552 . 107.3 no C58 . C57 . O56 . 109.34(19) yes C58 . C57 . H571 . 112.2 no O56 . C57 . H571 . 111.5 no C58 . C57 . H572 . 108.6 no O56 . C57 . H572 . 108.8 no H571 . C57 . H572 . 106.3 no C57 . C58 . O59 . 109.48(19) yes C57 . C58 . H581 . 111.1 no O59 . C58 . H581 . 110.0 no C57 . C58 . H582 . 108.4 no O59 . C58 . H582 . 109.7 no H581 . C58 . H582 . 108.1 no C1 . N1 . B1 . 173.1(2) yes C42 . O43 . C44 . 111.30(17) yes C45 . O46 . C47 . 110.39(18) yes C41 2_756 O49 . C48 . 111.67(17) yes C52 . O53 . C54 . 110.75(18) yes C55 . O56 . C57 . 111.40(17) yes C51 2_566 O59 . C58 . 111.90(18) yes C11 . B1 . C21 . 112.12(16) yes C11 . B1 . C31 . 112.02(16) yes C21 . B1 . C31 . 112.86(19) yes C11 . B1 . N1 . 106.03(18) yes C21 . B1 . N1 . 106.35(16) yes C31 . B1 . N1 . 106.89(17) yes #=end data_conpound_2 _database_code_CSD 204649 # Local code str62 _audit_creation_method CRYSTALS_ver_12_03_99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 12.8240(5) _cell_angle_alpha 108.484(2) _cell_length_b 12.9440(6) _cell_angle_beta 98.684(2) _cell_length_c 13.6630(6) _cell_angle_gamma 90.807(2) _cell_volume 2121.7 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M '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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'K ' 0.1790 0.2500 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C41.50 H36 B1 F15 K1 N1 O6 ' _chemical_formula_moiety ' C41.50 H36 B1 F15 K1 N1 O6 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 979.62 _cell_measurement_reflns_used 17785 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 998.935 _exptl_absorpt_coefficient_mu 0.240 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.89 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 17785 _reflns_number_total 8022 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_measured_fraction_theta_max 0.920 _reflns_number_gt 7066 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.41 _diffrn_reflns_limit_h_min 0 _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 16 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _refine_diff_density_min -0.79 _refine_diff_density_max 1.49 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 7066 _refine_ls_number_parameters 587 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.0712 _refine_ls_goodness_of_fit_ref 1.0779 _refine_ls_shift/su_max 0.044541 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 2.67 0.641 1.83 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _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 K1 0.68044(6) -0.18749(6) 0.64091(5) 0.0411 1.0000 Uani F12 0.88756(15) -0.01442(16) 0.85406(17) 0.0454 1.0000 Uani F13 1.06532(17) -0.09088(16) 0.92009(18) 0.0481 1.0000 Uani F14 1.25631(15) -0.00104(16) 0.91254(16) 0.0430 1.0000 Uani F15 1.26359(14) 0.16958(17) 0.83701(15) 0.0421 1.0000 Uani F16 1.08454(14) 0.25223(15) 0.77593(14) 0.0362 1.0000 Uani F22 0.87075(17) -0.01633(14) 0.59133(14) 0.0402 1.0000 Uani F23 0.8694(2) -0.03088(16) 0.39358(15) 0.0516 1.0000 Uani F24 0.8782(2) 0.15373(19) 0.33712(14) 0.0571 1.0000 Uani F25 0.88982(18) 0.35257(16) 0.48636(15) 0.0467 1.0000 Uani F26 0.89743(16) 0.37041(13) 0.68567(13) 0.0367 1.0000 Uani F32 0.99198(15) 0.30362(15) 0.98875(13) 0.0384 1.0000 Uani F33 0.93805(17) 0.48825(15) 1.11392(14) 0.0436 1.0000 Uani F34 0.76630(18) 0.58846(15) 1.05277(16) 0.0465 1.0000 Uani F35 0.64905(16) 0.49446(17) 0.85973(17) 0.0490 1.0000 Uani F36 0.70140(14) 0.30830(15) 0.73143(14) 0.0386 1.0000 Uani O41 0.53249(18) -0.1512(2) 0.4833(2) 0.0461 1.0000 Uani O44 0.4710(2) -0.1314(2) 0.6784(2) 0.0480 1.0000 Uani O47 0.6241(2) -0.16793(18) 0.83383(18) 0.0395 1.0000 Uani O50 0.79076(18) -0.29894(17) 0.76950(16) 0.0362 1.0000 Uani O53 0.85933(19) -0.31363(18) 0.57969(17) 0.0385 1.0000 Uani O56 0.69947(19) -0.2846(2) 0.42726(18) 0.0417 1.0000 Uani N1 0.6905(3) 0.0496(3) 0.7346(3) 0.0475 1.0000 Uani C1 0.7663(2) 0.0999(2) 0.7532(2) 0.0237 1.0000 Uani C11 0.9767(2) 0.1232(2) 0.8113(2) 0.0239 1.0000 Uani C12 0.9784(2) 0.0360(2) 0.8490(2) 0.0292 1.0000 Uani C13 1.0703(3) -0.0061(2) 0.8835(2) 0.0323 1.0000 Uani C14 1.1662(2) 0.0390(2) 0.8803(2) 0.0293 1.0000 Uani C15 1.1697(2) 0.1261(2) 0.8428(2) 0.0298 1.0000 Uani C16 1.0767(2) 0.1656(2) 0.8100(2) 0.0258 1.0000 Uani C21 0.8799(2) 0.1778(2) 0.6495(2) 0.0260 1.0000 Uani C22 0.8753(2) 0.0791(2) 0.5696(2) 0.0316 1.0000 Uani C23 0.8749(3) 0.0685(3) 0.4660(2) 0.0366 1.0000 Uani C24 0.8799(3) 0.1609(3) 0.4377(2) 0.0381 1.0000 Uani C25 0.8859(3) 0.2615(3) 0.5134(2) 0.0341 1.0000 Uani C26 0.8880(2) 0.2681(2) 0.6165(2) 0.0290 1.0000 Uani C31 0.8499(2) 0.2954(2) 0.8513(2) 0.0236 1.0000 Uani C32 0.9064(2) 0.3472(2) 0.9506(2) 0.0271 1.0000 Uani C33 0.8803(2) 0.4441(2) 1.0185(2) 0.0295 1.0000 Uani C34 0.7938(3) 0.4948(2) 0.9882(2) 0.0332 1.0000 Uani C35 0.7353(3) 0.4470(2) 0.8905(3) 0.0332 1.0000 Uani C36 0.7636(2) 0.3504(2) 0.8258(2) 0.0292 1.0000 Uani C42 0.4274(3) -0.1304(4) 0.5033(4) 0.0575 1.0000 Uani C43 0.4328(3) -0.0669(4) 0.6149(4) 0.0558 1.0000 Uani C45 0.4767(4) -0.0740(3) 0.7875(4) 0.0559 1.0000 Uani C46 0.5170(3) -0.1485(3) 0.8477(3) 0.0507 1.0000 Uani C48 0.6670(3) -0.2410(3) 0.8858(2) 0.0409 1.0000 Uani C49 0.7818(3) -0.2499(3) 0.8764(2) 0.0394 1.0000 Uani C51 0.8978(3) -0.3129(3) 0.7553(3) 0.0457 1.0000 Uani C52 0.9002(3) -0.3761(3) 0.6443(3) 0.0465 1.0000 Uani C54 0.8477(3) -0.3752(3) 0.4716(3) 0.0413 1.0000 Uani C55 0.8050(3) -0.3054(3) 0.4090(3) 0.0439 1.0000 Uani C57 0.6445(3) -0.2317(3) 0.3603(3) 0.0479 1.0000 Uani C58 0.5336(3) -0.2221(3) 0.3801(3) 0.0499 1.0000 Uani C61 0.5335(5) 0.2736(6) 0.9195(5) 0.0913 1.0000 Uani C62 0.6035(4) 0.3096(4) 1.0192(3) 0.0580 1.0000 Uani C63 0.5864(3) 0.4048(3) 1.0976(4) 0.0526 1.0000 Uani C64 0.6533(4) 0.4358(4) 1.1932(4) 0.0698 1.0000 Uani C65 0.7360(4) 0.3764(4) 1.2156(4) 0.0719 1.0000 Uani C66 0.7515(4) 0.2836(4) 1.1379(4) 0.0673 1.0000 Uani C67 0.6877(3) 0.2491(3) 1.0424(3) 0.0504 1.0000 Uani C71 0.3410(15) 0.513(2) 0.3810(15) 0.188(7) 0.5000 Uiso C72 0.4393(9) 0.4984(11) 0.4476(8) 0.107(4) 0.5000 Uiso C73 0.5083(6) 0.4245(6) 0.4079(6) 0.0498(17) 0.5000 Uiso C74 0.6032(8) 0.4113(9) 0.4692(8) 0.087(3) 0.5000 Uiso C75 0.6232(9) 0.4732(12) 0.5706(9) 0.106(4) 0.5000 Uiso C76 0.5516(9) 0.5481(9) 0.6074(8) 0.090(3) 0.5000 Uiso C77 0.459(1) 0.5609(11) 0.5481(9) 0.114(4) 0.5000 Uiso B1 0.8715(2) 0.1765(2) 0.7688(2) 0.0227 1.0000 Uani H421 0.3852 -0.2011 0.4868 0.0726 1.0000 Uiso H422 0.3934 -0.0879 0.4589 0.0726 1.0000 Uiso H431 0.4816 -0.0003 0.6328 0.0732 1.0000 Uiso H432 0.3606 -0.0445 0.6283 0.0732 1.0000 Uiso H451 0.5260 -0.0074 0.8082 0.0719 1.0000 Uiso H452 0.4048 -0.0521 0.8026 0.0719 1.0000 Uiso H461 0.5138 -0.1132 0.9237 0.0649 1.0000 Uiso H462 0.4730 -0.2192 0.8208 0.0649 1.0000 Uiso H481 0.6594 -0.2125 0.9613 0.0502 1.0000 Uiso H482 0.6285 -0.3145 0.8527 0.0502 1.0000 Uiso H491 0.8143 -0.2960 0.9178 0.0470 1.0000 Uiso H492 0.8189 -0.1755 0.9036 0.0470 1.0000 Uiso H511 0.9323 -0.3535 0.8014 0.0550 1.0000 Uiso H512 0.9364 -0.2399 0.7736 0.0550 1.0000 Uiso H521 0.9747 -0.3923 0.6347 0.0577 1.0000 Uiso H522 0.8559 -0.4461 0.6243 0.0577 1.0000 Uiso H541 0.9180 -0.3995 0.4535 0.0473 1.0000 Uiso H542 0.7978 -0.4405 0.4561 0.0473 1.0000 Uiso H551 0.8492 -0.2351 0.4315 0.0521 1.0000 Uiso H552 0.8050 -0.3442 0.3330 0.0521 1.0000 Uiso H571 0.6792 -0.1573 0.3754 0.0581 1.0000 Uiso H572 0.6453 -0.2756 0.2856 0.0581 1.0000 Uiso H581 0.5017 -0.2958 0.3721 0.0599 1.0000 Uiso H582 0.4918 -0.1919 0.3287 0.0599 1.0000 Uiso H611 0.5578 0.2046 0.8735 0.1121 1.0000 Uiso H612 0.4600 0.2600 0.9308 0.1121 1.0000 Uiso H613 0.5343 0.3313 0.8852 0.1121 1.0000 Uiso H631 0.5265 0.4501 1.0849 0.0676 1.0000 Uiso H641 0.6408 0.5045 1.2483 0.0836 1.0000 Uiso H651 0.7827 0.3999 1.2854 0.0844 1.0000 Uiso H661 0.8118 0.2392 1.1515 0.0839 1.0000 Uiso H671 0.7013 0.1799 0.9886 0.0640 1.0000 Uiso H711 0.3006 0.5712 0.4241 0.2254 0.5000 Uiso H712 0.3601 0.5356 0.3219 0.2254 0.5000 Uiso H713 0.2964 0.4430 0.3523 0.2254 0.5000 Uiso H731 0.4916 0.3777 0.3328 0.0598 0.5000 Uiso H741 0.6540 0.3576 0.4380 0.1043 0.5000 Uiso H751 0.6880 0.4649 0.6177 0.1275 0.5000 Uiso H761 0.5679 0.5962 0.6820 0.1080 0.5000 Uiso H771 0.4089 0.6153 0.5791 0.1370 0.5000 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 K1 0.0478(4) 0.0509(4) 0.0312(3) 0.0204(3) 0.0090(3) 0.0187(3) F12 0.033(1) 0.0478(11) 0.0675(13) 0.037(1) 0.0060(9) -0.0004(8) F13 0.0490(12) 0.035(1) 0.0669(14) 0.029(1) 0.002(1) 0.0071(9) F14 0.033(1) 0.0468(11) 0.0470(11) 0.0129(9) 0.0022(9) 0.0162(8) F15 0.0249(9) 0.0626(12) 0.041(1) 0.0198(9) 0.0054(8) -0.0028(8) F16 0.036(1) 0.040(1) 0.0365(9) 0.0206(8) 0.0004(8) -0.0077(8) F22 0.0591(12) 0.0258(9) 0.0317(9) 0.0033(7) 0.0083(9) 0.0037(8) F23 0.0747(15) 0.0418(11) 0.0273(9) -0.0060(8) 0.012(1) 0.004(1) F24 0.0838(17) 0.0676(14) 0.0201(9) 0.0134(9) 0.011(1) 0.0088(12) F25 0.0672(14) 0.0465(11) 0.034(1) 0.0218(9) 0.0110(9) 0.006(1) F26 0.0558(12) 0.0254(8) 0.0275(8) 0.0063(7) 0.0076(8) 0.0000(8) F32 0.038(1) 0.043(1) 0.0242(8) 0.0006(7) -0.0051(8) 0.0126(8) F33 0.0514(12) 0.040(1) 0.0263(9) -0.0052(8) 0.0012(8) -0.0019(9) F34 0.0588(13) 0.0270(9) 0.0491(11) 0.0002(8) 0.020(1) 0.0098(8) F35 0.0434(11) 0.0442(11) 0.0600(13) 0.017(1) 0.009(1) 0.0219(9) F36 0.033(1) 0.042(1) 0.0332(9) 0.0068(8) -0.0069(8) 0.0078(8) O41 0.0306(12) 0.0646(16) 0.0459(14) 0.0279(12) -0.0069(11) -0.0010(11) O44 0.0454(14) 0.0541(15) 0.0546(15) 0.0297(13) 0.0123(12) 0.0100(12) O47 0.0527(15) 0.0368(12) 0.0381(12) 0.019(1) 0.0186(11) 0.007(1) O50 0.0433(13) 0.0349(11) 0.027(1) 0.0090(9) -0.002(1) 0.0035(9) O53 0.0480(14) 0.0314(11) 0.0337(11) 0.0085(9) 0.003(1) 0.006(1) O56 0.0444(14) 0.0544(14) 0.0322(11) 0.0234(11) 0.004(1) -0.0023(11) N1 0.0415(17) 0.0480(17) 0.0525(18) 0.0187(14) 0.0009(14) -0.0048(14) C1 0.0221(14) 0.0235(13) 0.0217(12) 0.004(1) -0.0001(11) -0.0027(11) C11 0.0288(14) 0.0237(13) 0.0172(12) 0.003(1) 0.0050(11) 0.0062(11) C12 0.0273(15) 0.0294(14) 0.0318(14) 0.0097(12) 0.0086(12) 0.0012(11) C13 0.0411(17) 0.0250(14) 0.0312(15) 0.0097(12) 0.0058(13) 0.0076(12) C14 0.0262(15) 0.0324(15) 0.0248(13) 0.0027(11) 0.0042(12) 0.0110(12) C15 0.0263(15) 0.0384(16) 0.0202(13) 0.0020(11) 0.0064(12) 0.0018(12) C16 0.0334(15) 0.0257(13) 0.0165(12) 0.004(1) 0.0047(11) -0.0014(11) C21 0.0238(14) 0.0295(14) 0.0218(13) 0.0049(11) 0.0022(11) 0.0028(11) C22 0.0327(16) 0.0310(15) 0.0266(14) 0.0044(12) 0.0018(13) 0.0040(12) C23 0.0400(18) 0.0366(17) 0.0238(14) -0.0028(12) 0.0033(13) 0.0052(13) C24 0.0413(19) 0.0512(19) 0.0205(14) 0.0092(13) 0.0058(13) 0.0068(15) C25 0.0362(17) 0.0388(16) 0.0284(15) 0.0133(13) 0.0033(13) 0.0022(13) C26 0.0326(16) 0.0287(14) 0.0241(14) 0.0065(11) 0.0039(12) 0.0040(12) C31 0.0251(14) 0.0237(13) 0.0217(12) 0.006(1) 0.0062(11) 0.001(1) C32 0.0265(14) 0.0300(14) 0.0249(13) 0.0089(11) 0.0048(12) 0.0025(11) C33 0.0350(16) 0.0258(14) 0.0249(13) 0.0038(11) 0.0068(13) -0.0062(12) C34 0.0396(17) 0.0227(14) 0.0366(16) 0.0035(12) 0.0175(14) 0.0030(12) C35 0.0322(16) 0.0296(15) 0.0429(17) 0.0168(13) 0.0101(14) 0.0114(12) C36 0.0284(15) 0.0295(14) 0.0276(14) 0.0077(11) 0.0020(12) 0.0013(11) C42 0.0345(19) 0.081(3) 0.066(3) 0.041(2) -0.0015(19) 0.0005(19) C43 0.0325(18) 0.068(3) 0.083(3) 0.046(2) 0.009(2) 0.0099(17) C45 0.058(2) 0.054(2) 0.068(3) 0.026(2) 0.031(2) 0.0184(19) C46 0.061(2) 0.054(2) 0.047(2) 0.0214(17) 0.0277(19) 0.0121(18) C48 0.059(2) 0.0378(17) 0.0290(15) 0.0159(13) 0.0057(15) -0.0043(15) C49 0.053(2) 0.0396(17) 0.0253(15) 0.0139(13) -0.0022(14) -0.0064(15) C51 0.045(2) 0.052(2) 0.0404(18) 0.0198(16) -0.0042(16) 0.0137(16) C52 0.053(2) 0.0403(18) 0.051(2) 0.0197(16) 0.0099(18) 0.0172(16) C54 0.0439(19) 0.0396(17) 0.0348(17) 0.0024(14) 0.0101(15) 0.0032(14) C55 0.043(2) 0.054(2) 0.0329(17) 0.0103(15) 0.0117(15) -0.0107(16) C57 0.063(2) 0.053(2) 0.0297(16) 0.0217(15) -0.0042(16) -0.0117(18) C58 0.049(2) 0.060(2) 0.0410(19) 0.0269(17) -0.0140(16) -0.0144(18) C61 0.074(4) 0.123(5) 0.083(4) 0.046(4) 0.009(3) -0.040(3) C62 0.056(2) 0.066(3) 0.060(2) 0.030(2) 0.017(2) -0.010(2) C63 0.054(2) 0.0396(19) 0.075(3) 0.0242(19) 0.032(2) 0.0087(17) C64 0.085(3) 0.047(2) 0.077(3) 0.012(2) 0.029(3) 0.005(2) C65 0.078(3) 0.069(3) 0.064(3) 0.018(2) 0.006(3) -0.002(3) C66 0.064(3) 0.061(3) 0.085(3) 0.029(2) 0.023(3) 0.008(2) C67 0.055(2) 0.0361(18) 0.068(3) 0.0190(18) 0.032(2) 0.0078(16) B1 0.0237(15) 0.0225(14) 0.0203(13) 0.0053(11) 0.0025(12) 0.0021(11) _refine_ls_extinction_method None 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 F12 . C12 . 1.349(3) yes F13 . C13 . 1.346(3) yes F14 . C14 . 1.344(3) yes F15 . C15 . 1.346(4) yes F16 . C16 . 1.351(3) yes F22 . C22 . 1.361(4) yes F23 . C23 . 1.345(3) yes F24 . C24 . 1.345(4) yes F25 . C25 . 1.345(4) yes F26 . C26 . 1.353(3) yes F32 . C32 . 1.350(3) yes F33 . C33 . 1.341(3) yes F34 . C34 . 1.342(3) yes F35 . C35 . 1.349(3) yes F36 . C36 . 1.351(3) yes O41 . C42 . 1.427(5) yes O41 . C58 . 1.420(5) yes O44 . C43 . 1.426(4) yes O44 . C45 . 1.428(5) yes O47 . C46 . 1.429(5) yes O47 . C48 . 1.422(4) yes O50 . C49 . 1.419(4) yes O50 . C51 . 1.421(5) yes O53 . C52 . 1.425(4) yes O53 . C54 . 1.422(4) yes O56 . C55 . 1.427(5) yes O56 . C57 . 1.421(4) yes N1 . C1 . 1.113(4) yes C1 . B1 . 1.609(4) yes C11 . C12 . 1.380(4) yes C11 . C16 . 1.392(4) yes C11 . B1 . 1.637(4) yes C12 . C13 . 1.387(4) yes C13 . C14 . 1.367(5) yes C14 . C15 . 1.381(4) yes C15 . C16 . 1.374(4) yes C21 . C22 . 1.386(4) yes C21 . C26 . 1.387(4) yes C21 . B1 . 1.655(4) yes C22 . C23 . 1.377(4) yes C23 . C24 . 1.373(5) yes C24 . C25 . 1.375(5) yes C25 . C26 . 1.380(4) yes C31 . C32 . 1.389(4) yes C31 . C36 . 1.385(4) yes C31 . B1 . 1.649(4) yes C32 . C33 . 1.384(4) yes C33 . C34 . 1.374(5) yes C34 . C35 . 1.374(5) yes C35 . C36 . 1.373(4) yes C42 . C43 . 1.476(7) yes C42 . H421 . 1.000 no C42 . H422 . 1.000 no C43 . H431 . 1.000 no C43 . H432 . 1.000 no C45 . C46 . 1.505(5) yes C45 . H451 . 1.000 no C45 . H452 . 1.000 no C46 . H461 . 1.000 no C46 . H462 . 1.000 no C48 . C49 . 1.499(5) yes C48 . H481 . 1.000 no C48 . H482 . 1.000 no C49 . H491 . 1.000 no C49 . H492 . 1.000 no C51 . C52 . 1.483(5) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . H521 . 1.000 no C52 . H522 . 1.000 no C54 . C55 . 1.486(5) yes C54 . H541 . 1.000 no C54 . H542 . 1.000 no C55 . H551 . 1.000 no C55 . H552 . 1.000 no C57 . C58 . 1.487(6) yes C57 . H571 . 1.000 no C57 . H572 . 1.000 no C58 . H581 . 1.000 no C58 . H582 . 1.000 no C61 . C62 . 1.448(7) yes C61 . H611 . 1.000 no C61 . H612 . 1.000 no C61 . H613 . 1.000 no C62 . C63 . 1.399(6) yes C62 . C67 . 1.399(6) yes C63 . C64 . 1.387(7) yes C63 . H631 . 1.000 no C64 . C65 . 1.372(7) yes C64 . H641 . 1.000 no C65 . C66 . 1.368(7) yes C65 . H651 . 1.000 no C66 . C67 . 1.368(7) yes C66 . H661 . 1.000 no C67 . H671 . 1.000 no C71 . C72 . 1.49(1) yes C71 . C75 2_666 0.715(17) yes C71 . C76 2_666 1.612(17) yes C71 . H711 . 1.000 no C71 . H712 . 1.00 no C71 . H713 . 1.00 no C71 . H751 2_666 0.469 no C72 . C73 . 1.353(8) yes C72 . C74 2_666 1.523(14) yes C72 . C75 2_666 0.920(12) yes C72 . C76 2_666 0.826(14) yes C72 . C77 . 1.338(9) yes C72 . C77 2_666 1.521(15) yes C73 . C74 . 1.415(8) yes C73 . C76 2_666 0.875(11) yes C73 . C77 2_666 0.648(12) yes C73 . H731 . 1.000 no C73 . H771 2_666 1.201 no C74 . C75 . 1.345(9) yes C74 . C77 2_666 0.913(12) yes C74 . H741 . 1.000 no C74 . H771 2_666 0.63 no C75 . C76 . 1.375(9) yes C75 . C77 2_666 1.721(15) yes C75 . H711 2_666 1.14 no C75 . H751 . 1.000 no C76 . C77 . 1.373(9) yes C76 . H731 2_666 1.24 no C76 . H761 . 1.000 no C77 . H771 . 1.00 no H711 . H751 2_666 0.650 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 C42 . O41 . C58 . 111.9(3) yes C43 . O44 . C45 . 112.4(3) yes C46 . O47 . C48 . 111.5(3) yes C49 . O50 . C51 . 111.9(2) yes C52 . O53 . C54 . 111.8(3) yes C55 . O56 . C57 . 112.9(3) yes N1 . C1 . B1 . 173.7(3) yes C12 . C11 . C16 . 113.9(3) yes C12 . C11 . B1 . 126.4(3) yes C16 . C11 . B1 . 119.7(2) yes F12 . C12 . C11 . 120.7(3) yes F12 . C12 . C13 . 115.4(3) yes C11 . C12 . C13 . 123.9(3) yes F13 . C13 . C12 . 120.3(3) yes F13 . C13 . C14 . 120.1(3) yes C12 . C13 . C14 . 119.6(3) yes F14 . C14 . C13 . 120.6(3) yes F14 . C14 . C15 . 120.2(3) yes C13 . C14 . C15 . 119.2(3) yes F15 . C15 . C14 . 119.8(3) yes F15 . C15 . C16 . 121.0(3) yes C14 . C15 . C16 . 119.2(3) yes F16 . C16 . C11 . 118.9(2) yes F16 . C16 . C15 . 116.8(3) yes C11 . C16 . C15 . 124.2(3) yes C22 . C21 . C26 . 113.6(3) yes C22 . C21 . B1 . 118.7(3) yes C26 . C21 . B1 . 127.6(2) yes F22 . C22 . C21 . 120.0(3) yes F22 . C22 . C23 . 115.4(3) yes C21 . C22 . C23 . 124.6(3) yes F23 . C23 . C22 . 120.6(3) yes F23 . C23 . C24 . 120.4(3) yes C22 . C23 . C24 . 119.0(3) yes F24 . C24 . C23 . 120.6(3) yes F24 . C24 . C25 . 120.1(3) yes C23 . C24 . C25 . 119.2(3) yes F25 . C25 . C24 . 119.7(3) yes F25 . C25 . C26 . 120.6(3) yes C24 . C25 . C26 . 119.7(3) yes F26 . C26 . C21 . 120.9(2) yes F26 . C26 . C25 . 115.3(3) yes C21 . C26 . C25 . 123.7(3) yes C32 . C31 . C36 . 113.3(3) yes C32 . C31 . B1 . 127.0(2) yes C36 . C31 . B1 . 119.5(2) yes F32 . C32 . C31 . 121.1(3) yes F32 . C32 . C33 . 114.8(2) yes C31 . C32 . C33 . 124.1(3) yes F33 . C33 . C32 . 120.5(3) yes F33 . C33 . C34 . 119.9(3) yes C32 . C33 . C34 . 119.6(3) yes F34 . C34 . C33 . 120.8(3) yes F34 . C34 . C35 . 120.6(3) yes C33 . C34 . C35 . 118.6(3) yes F35 . C35 . C34 . 119.6(3) yes F35 . C35 . C36 . 120.4(3) yes C34 . C35 . C36 . 120.0(3) yes F36 . C36 . C31 . 119.3(3) yes F36 . C36 . C35 . 116.3(3) yes C31 . C36 . C35 . 124.4(3) yes O41 . C42 . C43 . 108.5(3) yes O41 . C42 . H421 . 109.7 no C43 . C42 . H421 . 109.7 no O41 . C42 . H422 . 109.7 no C43 . C42 . H422 . 109.7 no H421 . C42 . H422 . 109.5 no O44 . C43 . C42 . 110.0(3) yes O44 . C43 . H431 . 109.3 no C42 . C43 . H431 . 109.3 no O44 . C43 . H432 . 109.3 no C42 . C43 . H432 . 109.3 no H431 . C43 . H432 . 109.5 no O44 . C45 . C46 . 108.4(3) yes O44 . C45 . H451 . 109.7 no C46 . C45 . H451 . 109.7 no O44 . C45 . H452 . 109.7 no C46 . C45 . H452 . 109.7 no H451 . C45 . H452 . 109.5 no O47 . C46 . C45 . 108.1(3) yes O47 . C46 . H461 . 109.8 no C45 . C46 . H461 . 109.8 no O47 . C46 . H462 . 109.8 no C45 . C46 . H462 . 109.8 no H461 . C46 . H462 . 109.5 no O47 . C48 . C49 . 108.9(3) yes O47 . C48 . H481 . 109.6 no C49 . C48 . H481 . 109.6 no O47 . C48 . H482 . 109.6 no C49 . C48 . H482 . 109.6 no H481 . C48 . H482 . 109.5 no O50 . C49 . C48 . 109.0(3) yes O50 . C49 . H491 . 109.6 no C48 . C49 . H491 . 109.6 no O50 . C49 . H492 . 109.6 no C48 . C49 . H492 . 109.6 no H491 . C49 . H492 . 109.5 no O50 . C51 . C52 . 108.7(3) yes O50 . C51 . H511 . 109.7 no C52 . C51 . H511 . 109.7 no O50 . C51 . H512 . 109.7 no C52 . C51 . H512 . 109.7 no H511 . C51 . H512 . 109.5 no O53 . C52 . C51 . 109.3(3) yes O53 . C52 . H521 . 109.5 no C51 . C52 . H521 . 109.5 no O53 . C52 . H522 . 109.5 no C51 . C52 . H522 . 109.5 no H521 . C52 . H522 . 109.5 no O53 . C54 . C55 . 108.9(3) yes O53 . C54 . H541 . 109.6 no C55 . C54 . H541 . 109.6 no O53 . C54 . H542 . 109.6 no C55 . C54 . H542 . 109.6 no H541 . C54 . H542 . 109.5 no O56 . C55 . C54 . 107.5(3) yes O56 . C55 . H551 . 110.0 no C54 . C55 . H551 . 110.0 no O56 . C55 . H552 . 110.0 no C54 . C55 . H552 . 110.0 no H551 . C55 . H552 . 109.5 no O56 . C57 . C58 . 108.3(3) yes O56 . C57 . H571 . 109.8 no C58 . C57 . H571 . 109.8 no O56 . C57 . H572 . 109.8 no C58 . C57 . H572 . 109.8 no H571 . C57 . H572 . 109.5 no O41 . C58 . C57 . 109.4(3) yes O41 . C58 . H581 . 109.5 no C57 . C58 . H581 . 109.5 no O41 . C58 . H582 . 109.5 no C57 . C58 . H582 . 109.5 no H581 . C58 . H582 . 109.5 no C62 . C61 . H611 . 109.5 no C62 . C61 . H612 . 109.5 no H611 . C61 . H612 . 109.5 no C62 . C61 . H613 . 109.5 no H611 . C61 . H613 . 109.5 no H612 . C61 . H613 . 109.5 no C61 . C62 . C63 . 120.6(5) yes C61 . C62 . C67 . 121.7(5) yes C63 . C62 . C67 . 117.6(4) yes C62 . C63 . C64 . 119.3(4) yes C62 . C63 . H631 . 120.4 no C64 . C63 . H631 . 120.4 no C63 . C64 . C65 . 123.0(4) yes C63 . C64 . H641 . 118.5 no C65 . C64 . H641 . 118.5 no C64 . C65 . C66 . 116.9(5) yes C64 . C65 . H651 . 121.5 no C66 . C65 . H651 . 121.6 no C65 . C66 . C67 . 122.6(5) yes C65 . C66 . H661 . 118.7 no C67 . C66 . H661 . 118.7 no C62 . C67 . C66 . 120.7(4) yes C62 . C67 . H671 . 119.7 no C66 . C67 . H671 . 119.7 no C72 . C71 . C75 2_666 27.5(13) yes C72 . C71 . C76 2_666 30.5(5) yes C75 2_666 C71 . C76 2_666 58.1(13) yes C72 . C71 . H711 . 109.5 no C75 2_666 C71 . H711 . 82.0 no C76 2_666 C71 . H711 . 140.0 no C72 . C71 . H712 . 109.5 no C75 2_666 C71 . H712 . 120.1 no C76 2_666 C71 . H712 . 92.8 no H711 . C71 . H712 . 109.6 no C72 . C71 . H713 . 109.4 no C75 2_666 C71 . H713 . 121.7 no C76 2_666 C71 . H713 . 92.6 no H711 . C71 . H713 . 109.4 no H712 . C71 . H713 . 109.5 no C72 . C71 . H751 2_666 141.2 no C75 2_666 C71 . H751 2_666 113.7 no C76 2_666 C71 . H751 2_666 171.5 no H711 . C71 . H751 2_666 31.9 no H712 . C71 . H751 2_666 90.1 no H713 . C71 . H751 2_666 94.0 no C71 . C72 . C73 . 121.3(7) yes C71 . C72 . C74 2_666 82.2(8) yes C73 . C72 . C74 2_666 156.5(7) yes C71 . C72 . C75 2_666 21.1(11) yes C73 . C72 . C75 2_666 142.4(11) yes C74 2_666 C72 . C75 2_666 61.1(8) yes C71 . C72 . C76 2_666 82.7(11) yes C73 . C72 . C76 2_666 38.6(8) yes C74 2_666 C72 . C76 2_666 164.9(13) yes C75 2_666 C72 . C76 2_666 103.8(14) yes C71 . C72 . C77 . 118.7(7) yes C73 . C72 . C77 . 120.0(6) yes C74 2_666 C72 . C77 . 36.5(5) yes C75 2_666 C72 . C77 . 97.6(10) yes C76 2_666 C72 . C77 . 158.6(11) yes C71 . C72 . C77 2_666 146.5(9) yes C73 . C72 . C77 2_666 25.2(5) yes C74 2_666 C72 . C77 2_666 131.3(9) yes C75 2_666 C72 . C77 2_666 167.4(15) yes C76 2_666 C72 . C77 2_666 63.8(9) yes C77 . C72 . C77 2_666 94.8(7) yes C72 . C73 . C74 . 122.0(6) yes C72 . C73 . C76 2_666 36.1(9) yes C74 . C73 . C76 2_666 158.1(10) yes C72 . C73 . C77 2_666 92.1(13) yes C74 . C73 . C77 2_666 30.0(11) yes C76 2_666 C73 . C77 2_666 128.1(18) yes C72 . C73 . H731 . 119.0 no C74 . C73 . H731 . 119.0 no C76 2_666 C73 . H731 . 82.9 no C77 2_666 C73 . H731 . 148.9 no C72 . C73 . H771 2_666 148.4 no C74 . C73 . H771 2_666 26.5 no C76 2_666 C73 . H771 2_666 175.0 no C77 2_666 C73 . H771 2_666 56.4 no H731 . C73 . H771 2_666 92.6 no C72 2_666 C74 . C73 . 81.5(6) yes C72 2_666 C74 . C75 . 36.8(5) yes C73 . C74 . C75 . 118.2(6) yes C72 2_666 C74 . C77 2_666 60.7(9) yes C73 . C74 . C77 2_666 20.8(9) yes C75 . C74 . C77 2_666 97.5(11) yes C72 2_666 C74 . H741 . 157.6 no C73 . C74 . H741 . 120.9 no C75 . C74 . H741 . 120.9 no C77 2_666 C74 . H741 . 141.6 no C72 2_666 C74 . H771 2_666 138.9 no C73 . C74 . H771 2_666 57.6 no C75 . C74 . H771 2_666 175.6 no C77 2_666 C74 . H771 2_666 78.2 no H741 . C74 . H771 2_666 63.3 no C71 2_666 C75 . C72 2_666 131.4(22) yes C71 2_666 C75 . C74 . 146.4(18) yes C72 2_666 C75 . C74 . 82.1(10) yes C71 2_666 C75 . C76 . 95.7(17) yes C72 2_666 C75 . C76 . 35.7(9) yes C74 . C75 . C76 . 117.8(6) yes C71 2_666 C75 . C77 2_666 178.0(23) yes C72 2_666 C75 . C77 2_666 50.4(7) yes C74 . C75 . C77 2_666 31.7(5) yes C76 . C75 . C77 2_666 86.1(6) yes C71 2_666 C75 . H711 2_666 59.8 no C72 2_666 C75 . H711 2_666 168.6 no C74 . C75 . H711 2_666 86.6 no C76 . C75 . H711 2_666 155.6 no C77 2_666 C75 . H711 2_666 118.3 no C71 2_666 C75 . H751 . 25.4 no C72 2_666 C75 . H751 . 156.8 no C74 . C75 . H751 . 121.0 no C76 . C75 . H751 . 121.1 no C77 2_666 C75 . H751 . 152.8 no H711 2_666 C75 . H751 . 34.5 no C71 2_666 C76 . C72 2_666 66.7(10) yes C71 2_666 C76 . C73 2_666 172.1(13) yes C72 2_666 C76 . C73 2_666 105.3(14) yes C71 2_666 C76 . C75 . 26.2(7) yes C72 2_666 C76 . C75 . 40.5(9) yes C73 2_666 C76 . C75 . 145.9(10) yes C71 2_666 C76 . C77 . 150.3(9) yes C72 2_666 C76 . C77 . 83.6(10) yes C73 2_666 C76 . C77 . 21.8(8) yes C75 . C76 . C77 . 124.1(7) yes C71 2_666 C76 . H731 2_666 135.1 no C72 2_666 C76 . H731 2_666 158.2 no C73 2_666 C76 . H731 2_666 52.9 no C75 . C76 . H731 2_666 161.3 no C77 . C76 . H731 2_666 74.6 no C71 2_666 C76 . H761 . 91.7 no C72 2_666 C76 . H761 . 158.3 no C73 2_666 C76 . H761 . 96.2 no C75 . C76 . H761 . 117.9 no C77 . C76 . H761 . 118.0 no H731 2_666 C76 . H761 . 43.4 no C72 . C77 . C72 2_666 85.2(7) yes C72 . C77 . C73 2_666 147.9(14) yes C72 2_666 C77 . C73 2_666 62.7(11) yes C72 . C77 . C74 2_666 82.8(10) yes C72 2_666 C77 . C74 2_666 167.9(15) yes C73 2_666 C77 . C74 2_666 129.2(19) yes C72 . C77 . C75 2_666 32.0(5) yes C72 2_666 C77 . C75 2_666 117.1(9) yes C73 2_666 C77 . C75 2_666 177.2(26) yes C74 2_666 C77 . C75 2_666 50.8(8) yes C72 . C77 . C76 . 117.8(6) yes C72 2_666 C77 . C76 . 32.6(6) yes C73 2_666 C77 . C76 . 30.1(11) yes C74 2_666 C77 . C76 . 159.4(12) yes C75 2_666 C77 . C76 . 149.8(7) yes C72 . C77 . H771 . 121.1 no C72 2_666 C77 . H771 . 153.7 no C73 2_666 C77 . H771 . 91.0 no C74 2_666 C77 . H771 . 38.4 no C75 2_666 C77 . H771 . 89.2 no C76 . C77 . H771 . 121.1 no C1 . B1 . C11 . 111.3(2) yes C1 . B1 . C21 . 104.2(2) yes C11 . B1 . C21 . 108.3(2) yes C1 . B1 . C31 . 105.0(2) yes C11 . B1 . C31 . 113.0(2) yes C21 . B1 . C31 . 114.7(2) yes C71 . H711 . C75 2_666 38.2 no C71 . H711 . H751 2_666 22.4 no C75 2_666 H711 . H751 2_666 60.5 no C73 . H731 . C76 2_666 44.2 no C71 2_666 H751 . C75 . 40.9 no C71 2_666 H751 . H711 2_666 125.8 no C75 . H751 . H711 2_666 85.0 no C73 2_666 H771 . C74 2_666 96.0 no C73 2_666 H771 . C77 . 32.6 no C74 2_666 H771 . C77 . 63.4 no #=end data_conpound_6a _database_code_CSD 204650 # Local code sip3 _audit_creation_method CRYSTALS_ver_12_03_99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 9.9080(4) _cell_angle_alpha 97.594(2) _cell_length_b 10.4020(4) _cell_angle_beta 92.383(2) _cell_length_c 12.6890(6) _cell_angle_gamma 99.853(2) _cell_volume 1274.4 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Fe ' 0.3010 0.8450 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C26 H5 B F15 Fe N O2 ' _chemical_formula_moiety ' C26 H5 B F15 Fe N O2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 714.97 _cell_measurement_reflns_used 7026 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.86 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 701.07 _exptl_absorpt_coefficient_mu 0.73 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.86 # Sheldrick geometric definitions 0.86 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 7026 _reflns_number_total 4866 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 4866 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5323 _diffrn_measured_fraction_theta_max 0.914 _reflns_number_gt 4354 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_diff_density_min -0.66 _refine_diff_density_max 0.47 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4354 _refine_ls_number_parameters 415 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0409 _refine_ls_goodness_of_fit_ref 0.9453 _refine_ls_shift/su_max 0.000793 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.99 -.104 1.45 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _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 Fe1 1.19700(3) -0.14334(3) 0.35773(2) 0.0247 1.0000 Uani N2 1.23841(18) 0.01395(17) 0.29254(14) 0.0293 1.0000 Uani C3 1.2663(2) 0.1060(2) 0.25327(16) 0.0281 1.0000 Uani B4 1.2975(2) 0.2300(2) 0.18827(17) 0.0241 1.0000 Uani C5 1.41534(19) 0.34722(19) 0.25200(15) 0.0250 1.0000 Uani C6 1.4910(2) 0.3411(2) 0.34509(16) 0.0288 1.0000 Uani F7 1.47466(15) 0.23039(15) 0.3910(1) 0.0435 1.0000 Uani C8 1.5864(2) 0.4459(2) 0.39697(16) 0.0322 1.0000 Uani F9 1.65551(14) 0.43294(17) 0.4875(1) 0.0464 1.0000 Uani C10 1.6117(2) 0.5621(2) 0.35616(17) 0.0331 1.0000 Uani F11 1.70502(14) 0.66336(15) 0.40502(12) 0.0483 1.0000 Uani C12 1.5407(2) 0.5732(2) 0.26281(17) 0.0309 1.0000 Uani C13 1.4451(2) 0.4667(2) 0.21388(15) 0.0267 1.0000 Uani F14 1.38113(13) 0.48290(12) 0.1217(1) 0.0340 1.0000 Uani F15 1.56777(15) 0.68468(13) 0.21968(12) 0.0458 1.0000 Uani C16 1.15269(18) 0.28844(18) 0.18415(15) 0.0236 1.0000 Uani C17 1.08464(19) 0.31896(19) 0.09528(15) 0.0257 1.0000 Uani F18 1.13412(12) 0.29948(13) -0.00172(9) 0.0337 1.0000 Uani C19 0.9644(2) 0.3691(2) 0.09857(16) 0.0282 1.0000 Uani F20 0.90097(13) 0.39226(14) 0.0095(1) 0.0378 1.0000 Uani C21 0.9078(2) 0.3947(2) 0.19485(18) 0.0310 1.0000 Uani F22 0.79355(13) 0.44760(15) 0.19974(12) 0.0440 1.0000 Uani C23 0.9703(2) 0.3661(2) 0.28519(16) 0.0295 1.0000 Uani C24 1.0894(2) 0.31522(19) 0.27861(15) 0.0269 1.0000 Uani F25 1.14699(13) 0.29263(13) 0.37170(9) 0.0359 1.0000 Uani F26 0.91569(14) 0.39046(15) 0.37995(11) 0.0430 1.0000 Uani C27 1.34145(19) 0.16560(19) 0.07190(15) 0.0249 1.0000 Uani C28 1.4664(2) 0.19569(19) 0.02817(16) 0.0273 1.0000 Uani F29 1.56985(12) 0.28526(13) 0.07993(11) 0.0384 1.0000 Uani C30 1.4965(2) 0.1351(2) -0.07010(17) 0.0307 1.0000 Uani F31 1.62053(14) 0.16806(14) -0.10753(11) 0.0435 1.0000 Uani C32 1.3995(2) 0.0404(2) -0.12945(16) 0.0333 1.0000 Uani F33 1.42679(16) -0.01877(15) -0.22468(11) 0.0483 1.0000 Uani C34 1.2736(2) 0.0054(2) -0.08882(17) 0.0337 1.0000 Uani C35 1.2484(2) 0.0664(2) 0.00991(17) 0.0289 1.0000 Uani F36 1.12528(12) 0.02523(13) 0.04702(11) 0.0388 1.0000 Uani F37 1.17692(16) -0.08701(15) -0.14567(12) 0.0522 1.0000 Uani C38 1.3773(2) -0.1418(2) 0.38824(16) 0.0304 1.0000 Uani O39 1.48970(17) -0.14038(19) 0.40752(14) 0.0448 1.0000 Uani C40 1.1761(2) -0.0566(2) 0.48615(19) 0.0402 1.0000 Uani O41 1.1606(2) -0.0070(3) 0.56764(17) 0.0702 1.0000 Uani C42 0.9939(2) -0.2150(3) 0.2977(2) 0.0436 1.0000 Uani C43 1.0288(3) -0.2847(3) 0.3793(2) 0.0518 1.0000 Uani C44 1.1401(3) -0.3450(2) 0.3486(2) 0.0515 1.0000 Uani C45 1.1720(2) -0.3147(2) 0.2452(2) 0.0392 1.0000 Uani C46 1.0817(2) -0.2361(2) 0.21557(17) 0.0359 1.0000 Uani H421 0.9181 -0.1680 0.2955 0.0500 1.0000 Uiso H431 0.9848 -0.2850 0.4371 0.0500 1.0000 Uiso H441 1.1827 -0.3937 0.3812 0.0500 1.0000 Uiso H451 1.2416 -0.3371 0.2052 0.0500 1.0000 Uiso H461 1.0780 -0.1996 0.1519 0.0500 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 Fe1 0.02674(15) 0.02419(15) 0.02319(14) 0.0047(1) 0.0023(1) 0.00349(11) N2 0.0303(8) 0.0259(8) 0.0329(9) 0.0073(7) 0.0014(7) 0.0066(7) C3 0.0258(9) 0.030(1) 0.0298(9) 0.0037(8) 0.0022(7) 0.0084(8) B4 0.024(1) 0.023(1) 0.025(1) 0.0044(8) 0.0014(8) 0.0040(8) C5 0.0225(8) 0.0275(9) 0.0252(9) 0.0020(7) 0.0021(7) 0.0060(7) C6 0.0296(9) 0.033(1) 0.0256(9) 0.0075(8) 0.0030(7) 0.0087(8) F7 0.0494(8) 0.0474(8) 0.0358(7) 0.0192(6) -0.0068(6) 0.0066(7) C8 0.0237(9) 0.0481(13) 0.0251(9) 0.0008(9) 0.0005(7) 0.0108(9) F9 0.0370(7) 0.072(1) 0.0291(6) 0.0029(6) -0.0093(5) 0.0115(7) C10 0.0210(9) 0.0377(11) 0.0364(11) -0.0060(9) 0.0015(8) 0.0027(8) F11 0.0331(7) 0.0501(8) 0.0517(8) -0.0109(7) -0.0069(6) -0.0043(6) C12 0.0273(9) 0.027(1) 0.0377(11) 0.0036(8) 0.0045(8) 0.0040(8) C13 0.0248(9) 0.029(1) 0.0266(9) 0.0037(8) 0.0013(7) 0.0074(8) F14 0.0364(6) 0.0315(6) 0.0346(6) 0.0105(5) -0.0063(5) 0.0051(5) F15 0.0470(8) 0.0286(7) 0.0591(9) 0.0103(6) -0.0018(6) -0.0030(6) C16 0.0217(8) 0.0218(9) 0.0267(9) 0.0013(7) 0.0029(7) 0.0033(7) C17 0.0253(9) 0.0262(9) 0.0250(9) 0.0012(7) 0.0043(7) 0.0042(8) F18 0.0346(6) 0.0465(7) 0.0238(6) 0.0054(5) 0.0044(5) 0.0170(6) C19 0.0257(9) 0.027(1) 0.030(1) -0.0001(8) -0.0039(7) 0.0044(8) F20 0.0330(6) 0.0467(8) 0.0351(6) 0.0019(6) -0.0074(5) 0.0163(6) C21 0.0215(9) 0.028(1) 0.0414(11) -0.0040(8) 0.0022(8) 0.0058(8) F22 0.0259(6) 0.0516(8) 0.0546(8) -0.0066(7) 0.0027(5) 0.0180(6) C23 0.0281(9) 0.028(1) 0.030(1) -0.0022(8) 0.0093(8) 0.0020(8) C24 0.0285(9) 0.0253(9) 0.0254(9) 0.0038(7) 0.0015(7) 0.0006(8) F25 0.0414(7) 0.0443(7) 0.0241(6) 0.0067(5) 0.0046(5) 0.0117(6) F26 0.0403(7) 0.0541(8) 0.0345(7) -0.0023(6) 0.0159(5) 0.0116(6) C27 0.0249(9) 0.0239(9) 0.0275(9) 0.0052(7) 0.0009(7) 0.0081(8) C28 0.0263(9) 0.0246(9) 0.032(1) 0.0041(8) -0.0001(7) 0.0065(8) F29 0.0251(6) 0.0419(7) 0.0428(7) -0.0043(6) 0.0057(5) -0.0022(5) C30 0.030(1) 0.031(1) 0.035(1) 0.0092(8) 0.0098(8) 0.0097(8) F31 0.0370(7) 0.0492(8) 0.0460(8) 0.0069(6) 0.0198(6) 0.0083(6) C32 0.0457(12) 0.031(1) 0.026(1) 0.0030(8) 0.0078(9) 0.015(1) F33 0.0631(9) 0.0468(8) 0.0336(7) -0.0051(6) 0.0137(6) 0.0119(7) C34 0.0391(11) 0.025(1) 0.034(1) -0.0017(8) -0.0029(9) 0.0015(9) C35 0.0238(9) 0.027(1) 0.036(1) 0.0051(8) 0.0043(8) 0.0049(8) F36 0.0276(6) 0.0395(7) 0.0441(7) -0.0008(6) 0.0048(5) -0.0035(5) F37 0.0532(8) 0.0450(8) 0.0463(8) -0.0138(6) -0.0003(7) -0.0086(7) C38 0.0371(11) 0.028(1) 0.0276(9) 0.0072(8) 0.0021(8) 0.0067(9) O39 0.0322(8) 0.0588(11) 0.0460(9) 0.0152(8) -0.0025(7) 0.0105(8) C40 0.0405(12) 0.0433(13) 0.0352(12) -0.001(1) 0.0063(9) 0.007(1) O41 0.0730(14) 0.0840(16) 0.0456(11) -0.0231(11) 0.013(1) 0.0142(12) C42 0.028(1) 0.0521(14) 0.0450(13) -0.0090(11) -0.0027(9) 0.005(1) C43 0.0470(14) 0.0619(17) 0.0344(12) 0.0034(11) 0.007(1) -0.0229(13) C44 0.0600(16) 0.0259(11) 0.0622(16) 0.0179(11) -0.0277(13) -0.0118(11) C45 0.0360(11) 0.027(1) 0.0502(13) -0.0086(9) 0.001(1) 0.0032(9) C46 0.0462(12) 0.0305(11) 0.027(1) 0.0013(8) -0.0043(9) 0.001(1) _refine_ls_extinction_coef 280.642 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' 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 Fe1 . N2 . 1.9198(18) yes Fe1 . C38 . 1.809(2) yes Fe1 . C40 . 1.793(2) yes Fe1 . C42 . 2.097(2) yes Fe1 . C43 . 2.078(2) yes Fe1 . C44 . 2.064(2) yes Fe1 . C45 . 2.103(2) yes Fe1 . C46 . 2.117(2) yes N2 . C3 . 1.135(3) yes C3 . B4 . 1.614(3) yes B4 . C5 . 1.636(3) yes B4 . C16 . 1.653(3) yes B4 . C27 . 1.646(3) yes C5 . C6 . 1.387(3) yes C5 . C13 . 1.382(3) yes C6 . F7 . 1.346(3) yes C6 . C8 . 1.385(3) yes C8 . F9 . 1.347(2) yes C8 . C10 . 1.365(3) yes C10 . F11 . 1.340(2) yes C10 . C12 . 1.381(3) yes C12 . C13 . 1.386(3) yes C12 . F15 . 1.338(3) yes C13 . F14 . 1.351(2) yes C16 . C17 . 1.390(3) yes C16 . C24 . 1.393(3) yes C17 . F18 . 1.347(2) yes C17 . C19 . 1.380(3) yes C19 . F20 . 1.340(2) yes C19 . C21 . 1.378(3) yes C21 . F22 . 1.341(2) yes C21 . C23 . 1.371(3) yes C23 . C24 . 1.375(3) yes C23 . F26 . 1.350(2) yes C24 . F25 . 1.356(2) yes C27 . C28 . 1.382(3) yes C27 . C35 . 1.390(3) yes C28 . F29 . 1.344(2) yes C28 . C30 . 1.389(3) yes C30 . F31 . 1.342(2) yes C30 . C32 . 1.371(3) yes C32 . F33 . 1.341(2) yes C32 . C34 . 1.379(3) yes C34 . C35 . 1.380(3) yes C34 . F37 . 1.344(2) yes C35 . F36 . 1.348(2) yes C38 . O39 . 1.127(3) yes C40 . O41 . 1.122(3) yes C42 . C43 . 1.404(4) yes C42 . C46 . 1.404(3) yes C42 . H421 . 0.965 no C43 . C44 . 1.404(5) yes C43 . H431 . 0.869 no C44 . C45 . 1.426(4) yes C44 . H441 . 0.848 no C45 . C46 . 1.384(4) yes C45 . H451 . 0.916 no C46 . H461 . 0.939 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 N2 . Fe1 . C38 . 91.49(8) yes N2 . Fe1 . C40 . 94.2(1) yes C38 . Fe1 . C40 . 93.0(1) yes N2 . Fe1 . C42 . 101.1(1) yes C38 . Fe1 . C42 . 159.0(1) yes C40 . Fe1 . C42 . 102.8(1) yes N2 . Fe1 . C43 . 139.36(11) yes C38 . Fe1 . C43 . 128.86(12) yes C40 . Fe1 . C43 . 88.95(11) yes C42 . Fe1 . C43 . 39.30(12) yes N2 . Fe1 . C44 . 151.6(1) yes C38 . Fe1 . C44 . 94.86(11) yes C40 . Fe1 . C44 . 113.05(12) yes C42 . Fe1 . C44 . 66.27(11) yes C43 . Fe1 . C44 . 39.61(13) yes N2 . Fe1 . C45 . 111.99(9) yes C38 . Fe1 . C45 . 94.11(9) yes C40 . Fe1 . C45 . 152.66(11) yes C42 . Fe1 . C45 . 65.60(9) yes C43 . Fe1 . C45 . 66.2(1) yes N2 . Fe1 . C46 . 88.47(8) yes C38 . Fe1 . C46 . 126.00(9) yes C40 . Fe1 . C46 . 140.9(1) yes C42 . Fe1 . C46 . 38.92(9) yes C43 . Fe1 . C46 . 65.29(9) yes C44 . Fe1 . C45 . 40.01(11) yes C44 . Fe1 . C46 . 65.53(9) yes C45 . Fe1 . C46 . 38.3(1) yes Fe1 . N2 . C3 . 178.11(17) yes N2 . C3 . B4 . 174.9(2) yes C3 . B4 . C5 . 111.55(16) yes C3 . B4 . C16 . 105.08(15) yes C5 . B4 . C16 . 107.28(15) yes C3 . B4 . C27 . 103.97(15) yes C5 . B4 . C27 . 113.94(15) yes C16 . B4 . C27 . 114.71(15) yes B4 . C5 . C6 . 126.28(18) yes B4 . C5 . C13 . 119.62(17) yes C6 . C5 . C13 . 114.10(18) yes C5 . C6 . F7 . 120.92(18) yes C5 . C6 . C8 . 123.3(2) yes F7 . C6 . C8 . 115.75(18) yes C6 . C8 . F9 . 120.0(2) yes C6 . C8 . C10 . 120.28(19) yes F9 . C8 . C10 . 119.70(19) yes C8 . C10 . F11 . 120.7(2) yes C8 . C10 . C12 . 118.92(19) yes F11 . C10 . C12 . 120.3(2) yes C10 . C12 . C13 . 119.1(2) yes C10 . C12 . F15 . 119.71(19) yes C13 . C12 . F15 . 121.17(19) yes C5 . C13 . C12 . 124.27(19) yes C5 . C13 . F14 . 119.47(17) yes C12 . C13 . F14 . 116.24(18) yes B4 . C16 . C17 . 127.29(16) yes B4 . C16 . C24 . 118.98(17) yes C17 . C16 . C24 . 113.71(17) yes C16 . C17 . F18 . 120.60(16) yes C16 . C17 . C19 . 123.84(18) yes F18 . C17 . C19 . 115.57(17) yes C17 . C19 . F20 . 121.08(18) yes C17 . C19 . C21 . 119.56(19) yes F20 . C19 . C21 . 119.36(18) yes C19 . C21 . F22 . 120.2(2) yes C19 . C21 . C23 . 119.13(19) yes F22 . C21 . C23 . 120.67(19) yes C21 . C23 . C24 . 119.61(18) yes C21 . C23 . F26 . 119.69(19) yes C24 . C23 . F26 . 120.7(2) yes C16 . C24 . C23 . 124.13(19) yes C16 . C24 . F25 . 119.70(18) yes C23 . C24 . F25 . 116.16(17) yes B4 . C27 . C28 . 126.89(17) yes B4 . C27 . C35 . 119.00(16) yes C28 . C27 . C35 . 114.06(17) yes C27 . C28 . F29 . 121.67(17) yes C27 . C28 . C30 . 123.44(18) yes F29 . C28 . C30 . 114.88(17) yes C28 . C30 . F31 . 120.41(19) yes C28 . C30 . C32 . 120.10(19) yes F31 . C30 . C32 . 119.50(19) yes C30 . C32 . F33 . 120.8(2) yes C30 . C32 . C34 . 118.80(19) yes F33 . C32 . C34 . 120.4(2) yes C32 . C34 . C35 . 119.35(19) yes C32 . C34 . F37 . 119.82(19) yes C35 . C34 . F37 . 120.8(2) yes C27 . C35 . C34 . 124.20(18) yes C27 . C35 . F36 . 119.10(18) yes C34 . C35 . F36 . 116.70(18) yes Fe1 . C38 . O39 . 179.7(2) yes Fe1 . C40 . O41 . 177.2(3) yes Fe1 . C42 . C43 . 69.64(13) yes Fe1 . C42 . C46 . 71.31(13) yes C43 . C42 . C46 . 107.4(2) yes Fe1 . C42 . H421 . 128.6 no C43 . C42 . H421 . 126.3 no C46 . C42 . H421 . 126.0 no Fe1 . C43 . C42 . 71.06(14) yes Fe1 . C43 . C44 . 69.63(13) yes C42 . C43 . C44 . 108.2(2) yes Fe1 . C43 . H431 . 124.4 no C42 . C43 . H431 . 121.4 no C44 . C43 . H431 . 130.4 no Fe1 . C44 . C43 . 70.75(15) yes Fe1 . C44 . C45 . 71.49(13) yes C43 . C44 . C45 . 107.7(2) yes Fe1 . C44 . H441 . 124.7 no C43 . C44 . H441 . 129.7 no C45 . C44 . H441 . 122.6 no Fe1 . C45 . C44 . 68.50(13) yes Fe1 . C45 . C46 . 71.39(12) yes C44 . C45 . C46 . 107.3(2) yes Fe1 . C45 . H451 . 122.72 no C44 . C45 . H451 . 128.3 no C46 . C45 . H451 . 124.3 no Fe1 . C46 . C42 . 69.76(12) yes Fe1 . C46 . C45 . 70.33(13) yes C42 . C46 . C45 . 109.4(2) yes Fe1 . C46 . H461 . 125.24 no C42 . C46 . H461 . 123.4 no C45 . C46 . H461 . 127.2 no #=end