#------------------------------------------------------------------------------ #$Date: 2019-07-08 10:23:07 +0300 (Mon, 08 Jul 2019) $ #$Revision: 216814 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552005.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1552005 loop_ _publ_author_name 'Arnab Rit' 'Jesus Campos' 'Haoyu Niu' 'Simon Aldridge' _publ_section_title ; A stable heavier group 14 analogue of vinylidene ; _journal_name_full 'Nature Chemistry' _journal_page_first 1022 _journal_page_last 1026 _journal_paper_doi 10.1038/nchem.2597 _journal_volume 8 _journal_year 2016 _chemical_formula_sum 'C63 H94 B2 Ge2 N6' _chemical_formula_weight 1102.24 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.8587(2) _cell_length_b 19.0488(2) _cell_length_c 19.5197(2) _cell_measurement_reflns_used 31197 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 73.0852 _cell_measurement_theta_min 3.2390 _cell_volume 6268.52(12) _computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)' _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_data_reduction 'CrysAlisPro, (Agilent, 2011)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_unetI/netI 0.0183 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 53657 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.242 _diffrn_reflns_theta_min 3.242 _exptl_absorpt_coefficient_mu 1.482 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_meas . _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 2352 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.421 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.449(15) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 696 _refine_ls_number_reflns 12415 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.883 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0290 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.7753P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.0992 _reflns_Friedel_coverage 0.826 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 12190 _reflns_number_total 12415 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nchem.2597-s6.cif _cod_data_source_block 089arjc15_a _cod_database_code 1552005 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; 089arjc15_a.res created by SHELXL-2014/7 TITL 089arjc15_a.res in P2(1)2(1)2(1) CELL 1.54184 16.8587 19.0488 19.5197 90.000 90.000 90.000 ZERR 4.000 0.0002 0.0002 0.0002 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H B N Ge UNIT 252 376 8 24 8 omit 0 4 2 ! 238.12 11.57 15.42 0.009 4. omit -2 3 6 ! 477.02 148.47 11.14 0.033 2. omit 2 3 6 ! 489.41 150.61 11.06 0.033 2. omit 2 4 0 ! 106.09 8.71 10.84 0.008 4. omit 0 2 3 ! 142.47 28.57 10.75 0.014 5. omit 2 0 7 ! 174.05 36.22 10.54 0.016 2. temp -123 L.S. 10 twin -1 0 0 0 -1 0 0 0 -1 ACTA BOND $H FMAP 2 PLAN 20 eadp ge1 ge1b eadp ge2 ge2b WGHT 0.100000 0.775320 BASF 0.44920 FVAR 0.26779 0.92105 PART 1 GE1 5 0.775285 0.776230 0.692487 21.00000 0.01624 0.01569 = 0.01782 -0.00014 -0.00097 0.00037 GE2 5 0.714778 0.675674 0.751128 21.00000 0.01900 0.01574 = 0.02236 0.00255 -0.00279 0.00029 PART 2 GE1B 5 0.766779 0.740335 0.666376 -21.00000 0.01624 0.01569 = 0.01782 -0.00014 -0.00097 0.00037 GE2B 5 0.727169 0.717411 0.783773 -21.00000 0.01900 0.01574 = 0.02236 0.00255 -0.00279 0.00029 PART 0 N1 4 0.692361 0.882985 0.593413 11.00000 0.01811 0.02010 = 0.02599 0.00665 0.00041 -0.00120 N2 4 0.610199 0.788753 0.604881 11.00000 0.01605 0.02039 = 0.02542 0.00531 0.00019 0.00202 N3 4 0.857918 0.578140 0.789982 11.00000 0.02758 0.03087 = 0.02444 0.00073 -0.00726 0.00712 N4 4 0.786362 0.605492 0.884147 11.00000 0.03325 0.02492 = 0.02569 0.00290 -0.00337 0.00635 N5 4 0.718620 0.874122 0.814272 11.00000 0.03512 0.02353 = 0.02277 -0.00164 0.00095 -0.00031 N6 4 0.844457 0.876735 0.795315 11.00000 0.03503 0.02436 = 0.02784 -0.00246 -0.00446 -0.00424 B1 3 0.683203 0.818250 0.632227 11.00000 0.01901 0.02139 = 0.02368 0.00546 0.00206 0.00297 B2 3 0.790648 0.618287 0.811816 11.00000 0.03070 0.02161 = 0.02699 -0.00035 -0.00396 0.00119 C1 1 0.627883 0.889709 0.548350 11.00000 0.02094 0.02339 = 0.02475 0.00767 -0.00163 0.00492 AFIX 43 H1 2 0.619350 0.928088 0.518156 11.00000 -1.20000 AFIX 0 C2 1 0.580072 0.833587 0.554431 11.00000 0.02040 0.02269 = 0.02644 0.00468 -0.00121 0.00378 AFIX 43 H2 2 0.533207 0.825622 0.528549 11.00000 -1.20000 AFIX 0 C3 1 0.761129 0.926502 0.585894 11.00000 0.01845 0.02695 = 0.02287 0.00753 0.00145 -0.00108 C4 1 0.826418 0.900499 0.547668 11.00000 0.01975 0.02808 = 0.02635 0.00759 0.00075 -0.00019 C5 1 0.893176 0.943537 0.540430 11.00000 0.02144 0.03456 = 0.02933 0.00516 0.00179 -0.00267 AFIX 43 H5 2 0.937887 0.926719 0.515769 11.00000 -1.20000 AFIX 0 C6 1 0.895152 1.010408 0.568690 11.00000 0.02359 0.03831 = 0.02976 0.00428 0.00084 -0.00895 AFIX 43 H6 2 0.941033 1.038846 0.563378 11.00000 -1.20000 AFIX 0 C7 1 0.830247 1.035740 0.604657 11.00000 0.03040 0.03062 = 0.02829 -0.00003 -0.00018 -0.00783 AFIX 43 H7 2 0.831830 1.081805 0.623259 11.00000 -1.20000 AFIX 0 C8 1 0.762460 0.994438 0.613949 11.00000 0.02531 0.02778 = 0.02473 0.00484 0.00133 -0.00190 C9 1 0.823581 0.829688 0.512682 11.00000 0.02499 0.02468 = 0.03165 0.00323 0.00712 0.00333 AFIX 13 H9 2 0.787699 0.798774 0.540139 11.00000 -1.20000 AFIX 0 C10 1 0.787709 0.836690 0.441023 11.00000 0.03163 0.03487 = 0.03454 -0.00474 -0.00034 0.00357 AFIX 137 H10A 2 0.736144 0.860222 0.444166 11.00000 -1.50000 H10B 2 0.780670 0.789925 0.420998 11.00000 -1.50000 H10C 2 0.823331 0.864407 0.411998 11.00000 -1.50000 AFIX 0 C11 1 0.904641 0.794070 0.509387 11.00000 0.03102 0.03583 = 0.03969 0.00384 0.00704 0.00948 AFIX 137 H11A 2 0.939278 0.820245 0.478190 11.00000 -1.50000 H11B 2 0.898355 0.745897 0.492622 11.00000 -1.50000 H11C 2 0.928310 0.793211 0.555235 11.00000 -1.50000 AFIX 0 C12 1 0.691743 1.025890 0.651006 11.00000 0.03103 0.02545 = 0.03497 -0.00089 0.00622 -0.00352 AFIX 13 H12 2 0.649661 0.989108 0.654891 11.00000 -1.20000 AFIX 0 C13 1 0.713392 1.050976 0.723399 11.00000 0.05009 0.03964 = 0.03507 -0.00811 0.01000 0.00135 AFIX 137 H13A 2 0.738252 1.012415 0.748766 11.00000 -1.50000 H13B 2 0.665234 1.066079 0.747345 11.00000 -1.50000 H13C 2 0.750506 1.090444 0.720282 11.00000 -1.50000 AFIX 0 C14 1 0.658354 1.087575 0.609936 11.00000 0.03728 0.03282 = 0.05287 0.00417 0.00686 0.00305 AFIX 137 H14A 2 0.699295 1.123728 0.604884 11.00000 -1.50000 H14B 2 0.612540 1.107351 0.634071 11.00000 -1.50000 H14C 2 0.641836 1.071162 0.564542 11.00000 -1.50000 AFIX 0 C15 1 0.579530 0.718274 0.610639 11.00000 0.01674 0.02241 = 0.02932 0.00605 -0.00340 0.00056 C16 1 0.520934 0.702708 0.659679 11.00000 0.02023 0.02822 = 0.02747 0.00753 -0.00409 -0.00397 C17 1 0.494888 0.633143 0.664283 11.00000 0.02217 0.03085 = 0.03646 0.01118 -0.00489 -0.00687 AFIX 43 H17 2 0.455773 0.621305 0.697358 11.00000 -1.20000 AFIX 0 C18 1 0.524379 0.581402 0.622213 11.00000 0.02866 0.02305 = 0.05023 0.00995 -0.00950 -0.00598 AFIX 43 H18 2 0.505967 0.534494 0.626724 11.00000 -1.20000 AFIX 0 C19 1 0.580651 0.597676 0.573523 11.00000 0.02711 0.02293 = 0.04350 0.00139 -0.00487 0.00287 AFIX 43 H19 2 0.600533 0.561825 0.544372 11.00000 -1.20000 AFIX 0 C20 1 0.608875 0.666490 0.566519 11.00000 0.02158 0.02451 = 0.03163 0.00303 -0.00525 0.00479 C21 1 0.486705 0.759530 0.704954 11.00000 0.02511 0.03567 = 0.02846 0.00169 0.00432 -0.00786 AFIX 13 H21 2 0.530453 0.793301 0.715481 11.00000 -1.20000 AFIX 0 C22 1 0.454182 0.732743 0.773383 11.00000 0.04467 0.04959 = 0.03623 0.00696 0.01363 -0.00193 AFIX 137 H22A 2 0.404743 0.706940 0.765423 11.00000 -1.50000 H22B 2 0.443813 0.772653 0.803772 11.00000 -1.50000 H22C 2 0.493177 0.701493 0.794745 11.00000 -1.50000 AFIX 0 C23 1 0.421400 0.800502 0.668253 11.00000 0.03686 0.04076 = 0.04129 -0.00716 0.00407 0.00905 AFIX 137 H23A 2 0.441918 0.818838 0.624821 11.00000 -1.50000 H23B 2 0.404030 0.839620 0.697206 11.00000 -1.50000 H23C 2 0.376364 0.769326 0.659193 11.00000 -1.50000 AFIX 0 C24 1 0.671496 0.682260 0.513163 11.00000 0.03047 0.02683 = 0.03627 -0.00219 0.00464 0.00192 AFIX 13 H24 2 0.680215 0.734185 0.512721 11.00000 -1.20000 AFIX 0 C25 1 0.750682 0.647135 0.531914 11.00000 0.02859 0.03643 = 0.04320 -0.00684 0.00156 0.00480 AFIX 137 H25A 2 0.769513 0.665614 0.575856 11.00000 -1.50000 H25B 2 0.789983 0.657124 0.496229 11.00000 -1.50000 H25C 2 0.743023 0.596277 0.535609 11.00000 -1.50000 AFIX 0 C26 1 0.643105 0.660382 0.441108 11.00000 0.04745 0.03675 = 0.03620 -0.00181 0.00250 0.00288 AFIX 137 H26A 2 0.639966 0.609080 0.438504 11.00000 -1.50000 H26B 2 0.680711 0.677610 0.406713 11.00000 -1.50000 H26C 2 0.590605 0.680562 0.432343 11.00000 -1.50000 AFIX 0 C27 1 0.888740 0.542049 0.846430 11.00000 0.03107 0.02837 = 0.03325 -0.00200 -0.01036 0.00758 AFIX 43 H27 2 0.932404 0.510552 0.845142 11.00000 -1.20000 AFIX 0 C28 1 0.847304 0.558717 0.902383 11.00000 0.04114 0.02330 = 0.02826 0.00087 -0.01108 0.00587 AFIX 43 H28 2 0.857376 0.541709 0.947299 11.00000 -1.20000 AFIX 0 C29 1 0.879593 0.560869 0.721014 11.00000 0.02910 0.03780 = 0.02895 -0.00326 -0.00918 0.01227 C30 1 0.840532 0.503489 0.689598 11.00000 0.03388 0.04434 = 0.03733 -0.01316 -0.01029 0.01233 C31 1 0.861210 0.487623 0.621448 11.00000 0.04298 0.06028 = 0.03787 -0.01865 -0.00868 0.00999 AFIX 43 H31 2 0.836066 0.449527 0.598757 11.00000 -1.20000 AFIX 0 C32 1 0.917761 0.526887 0.587098 11.00000 0.05380 0.06284 = 0.03094 -0.01036 -0.00618 0.02061 AFIX 43 H32 2 0.930923 0.515360 0.541131 11.00000 -1.20000 AFIX 0 C33 1 0.955442 0.582813 0.618900 11.00000 0.04122 0.04661 = 0.03228 0.00217 0.00074 0.01817 AFIX 43 H33 2 0.993544 0.609499 0.594251 11.00000 -1.20000 AFIX 0 C34 1 0.937979 0.600431 0.686971 11.00000 0.03127 0.03752 = 0.02787 0.00020 -0.00337 0.01493 C35 1 0.777415 0.460760 0.724910 11.00000 0.03348 0.05099 = 0.04996 -0.01701 -0.01035 0.00240 AFIX 13 H35 2 0.765864 0.483929 0.769786 11.00000 -1.20000 AFIX 0 C36 1 0.806059 0.385347 0.740387 11.00000 0.04878 0.05343 = 0.06958 0.00320 -0.00723 0.00954 AFIX 137 H36A 2 0.817357 0.360968 0.697266 11.00000 -1.50000 H36B 2 0.764636 0.359973 0.765437 11.00000 -1.50000 H36C 2 0.854350 0.387275 0.768272 11.00000 -1.50000 AFIX 0 C37 1 0.699711 0.458072 0.684477 11.00000 0.03929 0.03987 = 0.09034 -0.00526 -0.02386 -0.00222 AFIX 137 H37A 2 0.679428 0.505838 0.678081 11.00000 -1.50000 H37B 2 0.660648 0.430169 0.709793 11.00000 -1.50000 H37C 2 0.709293 0.436487 0.639661 11.00000 -1.50000 AFIX 0 C38 1 0.982310 0.658923 0.722673 11.00000 0.03743 0.03050 = 0.03742 0.00736 -0.00235 0.00950 AFIX 13 H38 2 0.944081 0.683460 0.753674 11.00000 -1.20000 AFIX 0 C39 1 1.016667 0.713720 0.673417 11.00000 0.04795 0.04344 = 0.04892 0.01254 0.00361 0.00667 AFIX 137 H39A 2 1.059224 0.692389 0.646281 11.00000 -1.50000 H39B 2 1.037995 0.753262 0.699728 11.00000 -1.50000 H39C 2 0.974750 0.730542 0.642751 11.00000 -1.50000 AFIX 0 C40 1 1.049680 0.629239 0.767304 11.00000 0.05060 0.03679 = 0.05538 0.00999 -0.02251 -0.00062 AFIX 137 H40A 2 1.027517 0.596913 0.801349 11.00000 -1.50000 H40B 2 1.076848 0.667862 0.790742 11.00000 -1.50000 H40C 2 1.087574 0.604039 0.738239 11.00000 -1.50000 AFIX 0 C41 1 0.725773 0.627302 0.931122 11.00000 0.04613 0.02199 = 0.02802 0.00614 0.00098 0.00670 C42 1 0.744034 0.677600 0.980737 11.00000 0.06161 0.02919 = 0.02844 0.00590 0.00323 0.00125 C43 1 0.682506 0.700539 1.023459 11.00000 0.08720 0.03610 = 0.03225 0.00292 0.01428 0.00959 AFIX 43 H43 2 0.693295 0.734668 1.057702 11.00000 -1.20000 AFIX 0 C44 1 0.607455 0.674818 1.016830 11.00000 0.07603 0.04491 = 0.04197 0.01446 0.02645 0.00962 AFIX 43 H44 2 0.566686 0.691487 1.046227 11.00000 -1.20000 AFIX 0 C45 1 0.589926 0.624654 0.967726 11.00000 0.04924 0.04044 = 0.04755 0.01607 0.01718 0.00591 AFIX 43 H45 2 0.537210 0.607569 0.963519 11.00000 -1.20000 AFIX 0 C46 1 0.649236 0.598917 0.924244 11.00000 0.03827 0.03140 = 0.04130 0.02064 0.00769 0.00768 C47 1 0.826967 0.710203 0.985459 11.00000 0.07023 0.03621 = 0.02642 -0.00389 -0.00655 -0.00535 AFIX 13 H47 2 0.863202 0.683341 0.954508 11.00000 -1.20000 AFIX 0 C48 1 0.860955 0.707684 1.057734 11.00000 0.10211 0.05632 = 0.03963 0.01075 -0.02346 -0.01536 AFIX 137 H48A 2 0.826826 0.734689 1.088674 11.00000 -1.50000 H48B 2 0.914398 0.727922 1.057730 11.00000 -1.50000 H48C 2 0.863503 0.658821 1.073290 11.00000 -1.50000 AFIX 0 C49 1 0.823252 0.786304 0.960087 11.00000 0.08032 0.04094 = 0.03996 0.00676 -0.00237 -0.00900 AFIX 137 H49A 2 0.809110 0.786853 0.911392 11.00000 -1.50000 H49B 2 0.875128 0.808614 0.966342 11.00000 -1.50000 H49C 2 0.783143 0.812087 0.986307 11.00000 -1.50000 AFIX 0 C50 1 0.631997 0.541530 0.873062 11.00000 0.03219 0.03740 = 0.04547 0.01257 -0.00261 -0.00180 AFIX 13 H50 2 0.661652 0.553499 0.830259 11.00000 -1.20000 AFIX 0 C51 1 0.665051 0.471385 0.898881 11.00000 0.04438 0.03199 = 0.04726 0.00533 -0.00079 0.00040 AFIX 137 H51A 2 0.721473 0.476747 0.909774 11.00000 -1.50000 H51B 2 0.658651 0.435580 0.863257 11.00000 -1.50000 H51C 2 0.636162 0.456987 0.940120 11.00000 -1.50000 AFIX 0 C52 1 0.545070 0.532884 0.853112 11.00000 0.03886 0.05166 = 0.07397 0.01453 -0.00847 -0.00778 AFIX 137 H52A 2 0.514353 0.518474 0.893350 11.00000 -1.50000 H52B 2 0.540460 0.496991 0.817365 11.00000 -1.50000 H52C 2 0.524545 0.577630 0.835805 11.00000 -1.50000 AFIX 0 C53 1 0.776187 0.845753 0.773949 11.00000 0.03041 0.02132 = 0.02111 0.00023 0.00055 -0.00259 C54 1 0.828667 0.924464 0.848024 11.00000 0.05026 0.02837 = 0.02694 -0.00648 -0.00527 -0.00718 C55 1 0.750328 0.922890 0.859571 11.00000 0.05089 0.02362 = 0.02962 -0.00606 -0.00240 -0.00242 C56 1 0.889876 0.968955 0.882373 11.00000 0.06273 0.03533 = 0.03804 -0.00573 -0.01043 -0.02073 AFIX 137 H56A 2 0.865732 1.013244 0.897131 11.00000 -1.50000 H56B 2 0.933073 0.978750 0.850165 11.00000 -1.50000 H56C 2 0.910969 0.944053 0.922350 11.00000 -1.50000 AFIX 0 C57 1 0.705759 0.964837 0.911821 11.00000 0.06616 0.03743 = 0.04500 -0.01526 0.00943 -0.00260 AFIX 137 H57A 2 0.741799 0.998454 0.933627 11.00000 -1.50000 H57B 2 0.683894 0.933234 0.946647 11.00000 -1.50000 H57C 2 0.662422 0.990270 0.889378 11.00000 -1.50000 AFIX 0 C58 1 0.923014 0.858356 0.766919 11.00000 0.02588 0.03458 = 0.04175 -0.00117 -0.00789 -0.00479 AFIX 13 H58 2 0.913994 0.818360 0.734663 11.00000 -1.20000 AFIX 0 C59 1 0.978720 0.830640 0.823101 11.00000 0.03897 0.04772 = 0.04420 0.00457 -0.01540 -0.00185 AFIX 137 H59A 2 0.990868 0.868545 0.855384 11.00000 -1.50000 H59B 2 1.027978 0.813713 0.802176 11.00000 -1.50000 H59C 2 0.952825 0.791993 0.847556 11.00000 -1.50000 AFIX 0 C60 1 0.958176 0.917262 0.724578 11.00000 0.03558 0.04756 = 0.05075 0.01083 -0.00194 -0.00988 AFIX 137 H60A 2 0.918391 0.934453 0.692044 11.00000 -1.50000 H60B 2 1.004435 0.899783 0.699410 11.00000 -1.50000 H60C 2 0.974456 0.955667 0.754880 11.00000 -1.50000 AFIX 0 C61 1 0.634979 0.850440 0.811390 11.00000 0.03303 0.02945 = 0.03230 -0.00341 0.00410 0.00045 AFIX 13 H61 2 0.632482 0.811940 0.776630 11.00000 -1.20000 AFIX 0 C62 1 0.609232 0.819050 0.878836 11.00000 0.04942 0.05470 = 0.03504 0.00247 0.00799 -0.00464 AFIX 137 H62A 2 0.647423 0.783063 0.892952 11.00000 -1.50000 H62B 2 0.556677 0.797727 0.873610 11.00000 -1.50000 H62C 2 0.606882 0.855984 0.913727 11.00000 -1.50000 AFIX 0 C63 1 0.580458 0.908743 0.786082 11.00000 0.03903 0.03463 = 0.05577 -0.00501 0.00478 0.00672 AFIX 137 H63A 2 0.588924 0.951058 0.813686 11.00000 -1.50000 H63B 2 0.525099 0.893661 0.790327 11.00000 -1.50000 H63C 2 0.592289 0.919004 0.737958 11.00000 -1.50000 AFIX 0 H1B 2 0.637745 0.683523 0.790549 11.00000 0.03762 H2B 2 0.692953 0.626844 0.703028 11.00000 0.03886 HKLF 4 REM 089arjc15_a.res in P2(1)2(1)2(1) REM R1 = 0.0290 for 12190 Fo > 4sig(Fo) and 0.0297 for all 12415 data REM 696 parameters refined using 0 restraints END WGHT 0.0463 2.5458 REM Highest difference peak 0.421, deepest hole -0.449, 1-sigma level 0.046 Q1 1 0.7154 0.8523 0.8656 11.00000 0.05 0.42 Q2 1 0.8343 0.8419 0.8344 11.00000 0.05 0.41 Q3 1 0.9008 0.8205 0.7958 11.00000 0.05 0.38 Q4 1 0.7257 0.6385 0.4857 11.00000 0.05 0.35 Q5 1 0.7649 0.8145 0.8320 11.00000 0.05 0.34 Q6 1 0.8855 0.6969 1.0026 11.00000 0.05 0.33 Q7 1 0.9019 0.7793 1.0186 11.00000 0.05 0.32 Q8 1 0.6819 0.5165 0.6946 11.00000 0.05 0.31 Q9 1 0.7929 0.6785 0.9955 11.00000 0.05 0.29 Q10 1 0.9202 0.8778 0.7261 11.00000 0.05 0.28 Q11 1 0.7652 0.6406 0.9533 11.00000 0.05 0.28 Q12 1 0.5975 0.6632 0.4129 11.00000 0.05 0.27 Q13 1 0.7245 0.9959 0.7328 11.00000 0.05 0.26 Q14 1 0.6805 0.6241 0.9572 11.00000 0.05 0.26 Q15 1 0.6603 0.6786 1.0562 11.00000 0.05 0.25 Q16 1 0.9261 0.6485 1.0492 11.00000 0.05 0.24 Q17 1 0.8414 0.5384 0.6944 11.00000 0.05 0.24 Q18 1 0.7455 0.7076 1.0568 11.00000 0.05 0.24 Q19 1 0.6058 0.8326 0.9486 11.00000 0.05 0.23 Q20 1 0.5778 0.8803 0.8292 11.00000 0.05 0.23 ; _shelx_res_checksum 28672 _shelx_hkl_file ; 0 0 2 2514.46 35.96 0 0 3 1.00 0.36 0 0 4 187.74 4.15 0 0 -4 182.38 4.79 0 0 5 2.57 0.66 0 0 -5 2.07 0.85 0 0 -5 2.42 0.72 0 0 -6 1029.58 18.53 0 0 -6 1009.78 17.54 0 0 6 1032.48 17.06 0 0 7 2.68 0.70 0 0 -7 1.08 1.44 0 0 -7 2.90 0.86 0 0 -7 2.74 1.18 0 0 -8 36.03 2.92 0 0 -8 37.07 2.44 0 0 -8 37.24 3.49 0 0 -9 0.58 0.71 0 0 -9 -0.34 1.33 0 0 -9 -1.02 2.46 0 0 -10 216.87 9.20 0 0 -10 209.56 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9.57 -2 10 -13 389.27 9.19 2 -10 -13 379.98 9.34 2 -10 -13 378.77 9.34 -2 10 -14 13.97 1.90 -2 10 -14 15.83 1.88 -2 10 -14 14.29 1.93 2 -10 -14 16.63 2.16 2 -10 -14 16.01 1.88 2 -10 -14 14.46 1.56 2 -10 -14 17.90 2.14 2 -10 -15 402.57 9.30 2 -10 -15 399.26 8.79 2 -10 -15 423.73 9.61 2 -10 -15 395.55 9.84 -2 10 -15 394.35 9.59 -2 10 -15 378.30 9.18 2 -10 -15 405.99 9.77 2 -10 -16 16.36 1.97 2 -10 -16 16.47 2.01 2 -10 -16 16.51 1.49 -2 10 -16 12.89 1.64 -2 10 -16 15.16 1.99 2 -10 -16 10.68 1.77 -2 10 -17 220.18 6.21 2 -10 -17 239.34 6.80 -2 10 -17 239.07 6.70 2 -10 -17 243.55 6.70 2 -10 -18 9.98 1.55 -2 10 -18 10.75 1.57 2 -10 -18 6.07 1.44 -2 10 -18 10.23 1.36 2 -10 -19 216.91 5.68 2 -10 -19 217.40 5.82 -2 10 -19 199.32 5.21 2 -10 -20 22.85 1.70 -2 10 -20 22.51 1.36 2 -10 -20 24.61 1.71 -2 10 -20 24.75 1.80 2 -10 -21 58.48 2.26 -2 10 -21 61.78 2.31 2 11 -21 19.40 1.17 -2 -11 -20 20.51 1.14 2 11 -20 18.09 1.16 2 11 -20 21.88 1.53 -2 -11 -20 22.70 1.32 -2 -11 -19 0.73 0.68 -2 -11 -19 2.11 0.83 -2 -11 -19 -0.29 0.63 2 11 -19 3.32 1.14 2 11 -19 1.90 0.75 -2 -11 -18 9.42 1.18 -2 -11 -18 10.84 1.34 2 11 -18 12.78 1.35 -2 -11 -18 12.47 1.63 -2 -11 -18 10.37 1.23 2 11 -18 12.47 1.77 -2 -11 -17 5.15 1.09 -2 -11 -17 6.59 1.22 -2 -11 -17 6.43 1.43 -2 -11 -17 8.65 1.23 2 11 -17 6.74 1.67 -2 -11 -16 148.15 4.81 -2 -11 -16 154.43 4.95 -2 -11 -16 147.63 5.19 2 11 -16 156.25 5.35 -2 -11 -16 141.27 4.64 -2 -11 -15 66.19 3.23 -2 -11 -15 61.12 3.32 -2 -11 -15 60.18 3.06 -2 -11 -15 56.61 2.94 2 11 -15 60.96 3.38 2 11 -15 64.34 3.35 2 11 -14 93.15 4.16 -2 -11 -14 82.81 3.55 -2 -11 -14 81.99 3.59 2 11 -14 87.63 3.90 -2 -11 -14 84.15 3.91 2 11 -13 103.91 4.35 -2 -11 -13 102.04 4.19 2 11 -13 105.85 4.20 -2 -11 -13 95.18 3.89 -2 -11 -13 92.25 3.77 -2 -11 -12 68.56 3.19 -2 -11 -12 74.22 3.48 -2 -11 -12 74.03 3.22 2 11 -12 83.37 3.80 2 -11 12 77.44 6.72 -2 -11 -12 68.87 3.28 2 11 -12 77.73 3.53 -2 -11 -12 73.25 3.65 -2 -11 -12 72.78 6.70 -2 -11 -11 494.55 10.34 -2 -11 -11 521.72 10.27 -2 -11 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262.89 11.06 2 -11 4 287.37 12.08 2 -11 3 29.09 3.99 -2 -11 -3 25.70 2.95 -2 -11 -3 26.33 2.74 -2 -11 -3 28.42 3.02 2 -11 3 26.45 3.49 2 -11 2 11.42 2.50 -2 -11 -2 6.82 1.40 -2 -11 -2 9.82 1.92 2 -11 2 12.75 3.03 -2 -11 -1 114.52 5.58 -2 -11 -1 121.07 6.44 2 -11 1 115.31 7.26 2 -11 1 116.50 6.46 2 -11 0 29.39 3.34 -2 -11 0 25.55 3.20 2 -11 0 29.98 3.87 -2 -11 0 25.37 2.55 -2 -11 1 120.62 6.91 2 -11 -1 118.31 7.02 2 -11 -1 116.98 5.94 2 -11 -2 6.46 1.37 -2 -11 2 7.18 2.25 2 -11 -2 10.60 2.53 2 -11 -3 26.33 3.32 2 -11 -3 20.91 2.33 -2 -11 3 29.60 3.80 2 -11 -4 267.02 10.18 2 -11 -4 262.77 9.24 -2 -11 4 261.65 11.32 2 -11 -5 106.02 5.97 -2 -11 5 107.40 7.29 2 -11 -5 103.66 6.06 -2 -11 6 166.29 9.38 2 -11 -6 164.39 7.99 -2 -11 7 72.48 6.41 2 -11 -7 76.65 3.16 2 -11 -7 81.10 2.94 2 -11 -7 65.78 5.29 2 -11 -7 77.63 3.12 2 -11 -8 22.15 1.80 2 -11 -8 17.62 1.71 -2 11 -8 23.01 1.79 2 -11 -8 22.98 1.54 -2 -11 8 19.18 1.50 2 -11 -8 19.67 3.14 -2 -11 8 18.62 3.78 2 -11 -8 20.21 1.64 2 -11 -8 18.02 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0.88 -2 -12 -16 3.25 1.23 2 12 -16 2.15 1.42 -2 -12 -16 3.02 1.08 -2 -12 -15 131.20 4.78 -2 -12 -15 136.75 4.68 -2 -12 -15 132.38 4.54 -2 -12 -15 130.67 4.40 2 12 -15 134.68 5.01 -2 -12 -14 97.08 3.92 2 12 -14 102.78 4.14 -2 -12 -14 97.01 3.79 -2 -12 -14 92.70 3.97 2 12 -14 98.49 4.28 -2 -12 -13 51.09 2.93 -2 -12 -13 50.00 2.70 2 12 -13 56.50 3.25 2 12 -13 53.24 3.03 -2 -12 -13 53.81 2.96 -2 -12 -12 297.75 7.39 2 12 -12 301.75 7.66 -2 -12 -12 301.44 7.60 -2 -12 -12 307.93 7.31 -2 -12 -12 299.45 7.66 2 12 -12 298.60 7.93 -2 -12 -11 9.80 1.44 -2 -12 -11 7.75 1.32 -2 -12 -11 10.56 1.39 -2 -12 -11 8.85 1.35 -2 -12 -11 8.85 2.21 2 -12 11 11.78 3.21 -2 -12 -11 7.67 1.30 2 12 -11 9.33 1.43 2 -12 10 614.51 12.48 2 -12 10 685.73 22.02 -2 -12 -10 630.10 12.30 2 -12 10 651.77 21.35 -2 -12 -10 595.09 11.99 2 12 -10 620.37 12.11 -2 -12 -10 630.91 11.78 -2 -12 -10 598.31 12.31 -2 -12 -10 644.21 20.64 -2 -12 -10 597.63 11.92 2 -12 9 30.79 4.41 -2 -12 -9 27.82 1.97 2 12 -9 29.45 1.99 2 -12 9 27.39 2.11 -2 -12 -9 29.27 1.81 -2 -12 -9 30.43 2.10 2 -12 9 33.69 4.75 -2 -12 -9 28.80 1.92 -2 -12 -9 21.96 3.61 -2 -12 -8 514.50 17.60 2 -12 8 545.07 11.24 2 -12 8 590.39 19.91 -2 -12 -8 522.96 10.56 -2 -12 -8 534.68 10.07 -2 -12 -8 541.21 10.69 2 12 -8 528.22 10.32 2 -12 8 559.50 19.24 -2 -12 -8 503.88 10.26 -2 -12 -7 3.47 0.73 -2 -12 -7 5.62 2.07 -2 -12 -7 2.35 0.65 2 -12 7 3.07 1.07 2 -12 7 3.98 2.33 -2 -12 -7 4.01 0.94 2 12 -7 3.54 0.72 2 -12 7 5.05 2.57 2 -12 6 54.13 5.59 -2 -12 -6 58.29 2.57 2 -12 6 53.69 5.98 -2 -12 -6 53.13 5.05 2 -12 6 53.54 2.79 -2 -12 -5 2.64 1.43 2 -12 5 2.44 2.09 2 -12 5 2.67 2.10 -2 -12 -5 2.73 0.89 2 -12 5 3.13 0.91 2 -12 4 21.65 3.86 2 -12 4 20.94 3.37 -2 -12 -4 20.18 2.75 2 -12 3 377.01 13.78 -2 -12 -3 397.97 12.57 -2 -12 -3 399.37 12.35 2 -12 3 402.94 14.98 2 -12 2 28.46 3.60 -2 -12 -2 27.67 2.92 -2 -12 -2 26.98 3.08 2 -12 2 26.08 4.00 -2 -12 -2 24.70 3.01 2 -12 1 593.07 16.93 -2 -12 -1 631.31 15.32 -2 -12 -1 601.60 16.67 2 -12 1 599.52 18.49 -2 -12 0 2.10 1.55 2 -12 0 1.34 1.27 2 -12 0 4.26 2.01 2 -12 -1 630.30 16.12 -2 -12 1 587.26 17.40 2 -12 -1 588.88 17.91 -2 -12 2 20.85 3.33 2 -12 -2 18.57 2.99 -2 -12 3 400.64 14.47 2 -12 -3 388.25 13.51 -2 -12 4 20.33 3.47 2 -12 -4 24.24 3.27 -2 -12 5 1.32 0.79 -2 -12 5 1.19 1.71 2 -12 -5 3.76 1.05 2 -12 -5 2.15 1.10 -2 -12 6 53.46 5.59 2 -12 -6 55.73 2.80 -2 12 -6 53.07 2.33 2 -12 -6 56.62 4.67 2 -12 -6 50.58 2.63 -2 -12 6 53.42 2.61 2 -12 -6 54.04 2.40 2 -12 -7 6.95 1.05 2 -12 -7 5.68 1.31 2 -12 -7 6.37 1.37 2 -12 -7 4.97 0.95 -2 12 -7 4.73 0.86 2 -12 -7 5.56 1.87 -2 -12 7 2.55 0.79 -2 -12 7 4.86 2.10 -2 -12 8 551.12 19.36 2 -12 -8 524.44 10.45 2 -12 -8 536.43 11.29 2 -12 -8 544.92 11.19 2 -12 -8 535.45 17.09 -2 -12 8 546.78 10.94 2 -12 -8 565.50 10.76 -2 12 -8 554.88 10.86 2 -12 -9 30.41 2.06 2 -12 -9 28.07 1.83 2 -12 -9 24.83 2.10 -2 12 -9 31.00 2.11 -2 -12 9 26.00 1.86 -2 -12 9 29.34 4.45 2 -12 -9 28.68 2.20 2 -12 -9 30.26 3.98 2 -12 -10 614.77 12.75 -2 -12 10 607.96 11.93 2 -12 -10 626.24 12.18 -2 12 -10 641.42 12.49 2 -12 -10 594.83 11.68 2 -12 -10 620.60 12.45 2 -12 -10 610.77 19.55 -2 12 -11 8.69 1.44 2 -12 -11 10.66 3.07 2 -12 -11 7.06 1.46 -2 -12 11 5.77 2.37 2 -12 -11 5.36 1.25 2 -12 -11 5.55 1.01 2 -12 -11 8.15 1.56 2 -12 -12 299.63 7.63 -2 12 -12 314.51 7.95 2 -12 -12 317.82 7.71 2 -12 -12 292.40 8.01 2 -12 -12 298.33 7.06 -2 12 -13 51.49 3.00 -2 12 -13 56.92 3.18 2 -12 -13 50.01 3.10 2 -12 -13 53.41 2.51 2 -12 -13 54.38 2.93 2 -12 -13 53.49 2.92 2 -12 -14 92.35 4.14 2 -12 -14 101.22 3.97 -2 12 -14 95.04 4.01 2 -12 -14 98.51 3.42 2 -12 -14 100.44 3.84 -2 12 -14 102.33 4.25 2 -12 -15 131.06 4.93 -2 12 -15 132.71 4.71 2 -12 -15 143.40 4.98 -2 12 -15 143.15 5.01 2 -12 -15 144.54 4.83 -2 12 -16 5.29 1.54 2 -12 -16 3.74 1.28 2 -12 -16 1.01 1.49 -2 12 -16 2.98 1.16 -2 12 -17 202.93 5.53 2 -12 -17 216.35 5.90 2 -12 -17 198.60 5.80 -2 12 -17 214.32 5.92 2 -12 -18 4.03 1.13 2 -12 -18 1.32 1.11 -2 12 -18 2.55 1.04 -2 12 -18 -0.07 0.86 2 -12 -19 50.51 2.29 2 -12 -19 52.68 2.37 -2 12 -19 50.75 2.07 2 -12 -20 76.44 2.46 2 -12 -20 78.38 2.48 2 13 -20 14.25 0.96 -2 -13 -19 39.68 1.70 2 13 -19 41.34 1.91 2 13 -18 25.83 1.41 -2 -13 -18 29.74 1.69 2 13 -18 27.14 1.84 -2 -13 -18 30.58 1.57 -2 -13 -17 11.52 1.30 -2 -13 -17 12.08 1.26 2 13 -17 11.19 1.53 -2 -13 -17 12.21 1.15 -2 -13 -16 49.18 2.50 -2 -13 -16 48.84 2.55 2 13 -16 53.13 2.94 -2 -13 -16 49.78 2.36 2 13 -15 30.22 2.39 -2 -13 -15 24.78 2.01 -2 -13 -15 25.67 2.01 -2 -13 -15 29.36 1.98 -2 -13 -15 26.25 2.00 -2 -13 -14 101.28 3.75 2 13 -14 107.04 4.43 -2 -13 -14 101.78 3.97 -2 -13 -14 98.71 3.95 -2 -13 -13 35.47 2.44 -2 -13 -13 34.93 2.37 2 13 -13 35.53 2.66 -2 -13 -13 35.86 2.24 2 13 -13 31.81 2.37 -2 -13 -12 192.69 5.54 2 13 -12 212.04 6.34 2 13 -12 193.09 5.78 -2 -13 -12 189.29 5.70 -2 -13 -12 199.66 5.91 2 13 -11 6.29 0.94 -2 -13 -11 7.24 1.21 -2 -13 -11 5.28 1.25 -2 -13 -11 5.79 1.04 -2 -13 -11 7.14 1.35 2 13 -11 7.32 1.32 2 -13 11 7.54 1.16 -2 -13 -10 83.69 3.46 2 13 -10 91.03 3.56 -2 -13 -10 87.12 3.33 2 -13 10 84.43 3.78 -2 -13 -10 82.93 6.88 2 -13 10 94.48 7.97 -2 -13 -10 83.40 3.62 -2 -13 -9 38.73 2.29 2 -13 9 35.66 4.89 -2 -13 -9 39.63 2.14 2 -13 9 37.44 2.56 2 -13 9 45.77 5.59 -2 -13 -9 38.06 2.42 2 13 -9 38.35 2.25 -2 -13 -9 39.49 4.86 -2 -13 -9 38.74 2.31 2 -13 8 38.44 5.09 -2 -13 -8 36.20 2.16 2 -13 8 33.46 4.76 -2 -13 -8 31.01 4.10 -2 -13 -8 32.87 2.19 -2 -13 -8 34.49 1.91 2 13 -8 34.34 2.01 -2 -13 -8 33.28 2.09 2 -13 8 32.76 2.40 -2 -13 -7 47.98 4.98 2 -13 7 49.08 2.86 -2 -13 -7 44.94 2.26 2 -13 7 53.73 5.79 -2 -13 -7 45.72 2.51 2 -13 7 48.94 5.69 -2 -13 -6 166.05 4.90 -2 -13 -6 160.78 8.74 2 -13 6 166.24 9.97 2 -13 6 176.17 10.44 2 -13 6 175.03 5.53 2 -13 5 14.94 3.61 -2 -13 -5 12.66 2.73 2 -13 5 9.86 1.43 -2 -13 -5 8.22 1.11 -2 -13 -5 10.50 1.29 2 -13 5 8.42 2.57 2 -13 4 397.48 15.89 2 -13 4 414.28 9.26 -2 -13 -4 381.26 8.40 -2 -13 -4 404.65 13.33 2 -13 4 402.39 14.95 -2 -13 -3 16.13 2.51 2 -13 3 15.50 1.66 2 -13 3 12.28 3.17 2 -13 3 14.33 3.02 -2 -13 -3 14.16 1.40 2 -13 2 23.11 3.35 -2 -13 -2 23.73 1.75 2 -13 2 22.20 1.85 -2 -13 -2 18.58 2.74 -2 -13 -2 23.91 2.96 2 -13 2 23.10 3.89 -2 -13 -1 16.99 2.76 2 -13 1 19.35 1.75 2 -13 1 18.41 2.94 -2 -13 -1 18.90 1.62 -2 -13 -1 19.31 3.15 2 -13 1 22.88 3.81 2 -13 0 396.23 13.20 2 -13 0 403.38 8.87 -2 -13 0 413.99 8.88 2 -13 0 391.93 14.86 -2 -13 0 400.51 13.88 -2 -13 1 18.56 1.68 2 -13 -1 16.67 1.50 2 -13 -1 18.97 2.53 -2 -13 1 15.62 2.84 2 -13 -1 14.06 2.95 -2 -13 2 20.75 3.49 2 -13 -2 22.90 1.71 2 -13 -2 21.42 3.54 -2 -13 2 26.19 1.92 2 -13 -3 15.12 1.41 -2 -13 3 14.24 1.47 -2 -13 3 11.84 2.82 2 -13 -3 15.50 1.23 2 -13 -3 13.94 2.69 -2 -13 4 415.39 9.10 -2 -13 4 380.95 15.10 2 -13 -4 412.51 14.12 2 -13 -4 403.78 8.19 -2 -13 5 9.82 1.31 -2 -13 5 8.47 2.73 2 -13 -5 11.27 1.21 -2 -13 6 175.42 5.31 2 -13 -6 178.49 5.44 -2 13 -6 169.91 4.69 -2 -13 6 172.55 10.27 2 -13 -6 178.35 4.86 2 -13 -7 47.95 2.48 2 -13 -7 51.68 4.65 2 -13 -7 51.34 2.48 -2 -13 7 49.87 5.56 2 -13 -7 48.01 2.88 -2 -13 7 47.87 2.68 -2 13 -7 46.18 2.37 -2 -13 8 34.52 2.30 2 -13 -8 36.02 2.56 2 -13 -8 34.76 2.15 2 -13 -8 37.34 2.55 2 -13 -8 34.84 2.10 2 -13 -8 33.34 4.03 -2 -13 8 32.42 4.69 -2 13 -8 34.38 2.12 2 -13 -9 38.35 2.77 -2 -13 9 38.07 2.36 2 -13 -9 39.22 2.26 -2 -13 9 42.25 5.43 2 -13 -9 40.76 2.69 -2 13 -9 38.61 2.40 2 -13 -9 45.13 2.52 2 -13 -9 41.12 4.62 2 -13 -10 87.54 3.99 2 -13 -10 89.38 3.46 2 -13 -10 89.70 3.59 2 -13 -10 92.73 6.99 -2 13 -10 86.66 3.66 2 -13 -10 88.06 3.90 -2 -13 10 92.85 7.71 -2 -13 10 87.64 3.53 -2 13 -11 6.65 1.45 2 -13 -11 3.72 1.57 2 -13 -11 6.72 1.39 2 -13 -11 6.83 1.14 2 -13 -11 6.41 1.45 2 -13 -12 190.38 6.16 2 -13 -12 192.56 5.35 2 -13 -12 196.05 5.80 -2 13 -12 209.05 6.11 2 -13 -13 38.63 2.80 -2 13 -13 37.00 2.67 2 -13 -13 34.16 2.41 -2 13 -13 34.63 2.51 2 -13 -13 37.38 2.13 -2 13 -14 97.58 4.07 -2 13 -14 111.04 4.30 2 -13 -14 104.87 3.50 2 -13 -14 99.51 4.25 2 -13 -14 101.97 3.99 -2 13 -15 28.35 2.20 -2 13 -15 26.73 2.16 2 -13 -15 26.77 2.13 2 -13 -15 28.21 2.24 2 -13 -15 28.17 2.40 2 -13 -16 52.71 2.88 -2 13 -16 51.44 2.84 -2 13 -16 47.59 2.60 2 -13 -16 54.53 2.84 2 -13 -17 11.67 1.43 -2 13 -17 10.82 1.47 -2 13 -17 10.63 1.30 2 -13 -17 13.52 1.63 2 -13 -18 30.49 1.95 2 -13 -18 32.03 1.87 -2 13 -19 35.90 1.79 -2 13 -19 36.67 1.61 2 14 -19 5.15 0.76 2 14 -18 11.66 1.16 -2 -14 -18 10.65 1.00 -2 -14 -18 12.18 0.92 -2 -14 -17 32.66 1.74 -2 -14 -17 32.44 1.84 2 14 -17 29.69 1.51 2 14 -17 34.74 2.05 -2 -14 -16 13.55 1.39 2 14 -16 11.57 1.55 -2 -14 -16 13.19 1.33 -2 -14 -15 49.05 2.61 -2 -14 -15 52.16 2.60 2 14 -15 51.92 2.86 -2 -14 -14 141.27 4.30 -2 -14 -14 132.75 4.50 2 14 -14 148.63 5.04 -2 -14 -13 40.10 2.56 -2 -14 -13 43.99 2.41 2 14 -13 38.68 2.81 2 14 -12 255.12 6.82 2 14 -12 280.47 7.62 -2 -14 -12 278.99 6.72 -2 -14 -12 272.21 7.13 2 14 -11 109.21 4.03 -2 -14 -11 109.82 3.80 2 -14 11 112.54 3.99 2 14 -11 108.53 3.59 -2 -14 -11 108.06 4.23 -2 -14 -11 113.84 4.01 2 -14 10 285.28 7.24 2 14 -10 281.26 6.98 -2 -14 -10 288.83 6.74 -2 -14 -10 285.54 7.37 2 -14 9 166.18 5.74 -2 -14 -9 186.07 4.89 -2 -14 -9 181.22 5.54 2 14 -9 177.58 5.07 2 14 -8 717.38 13.08 -2 -14 -8 706.06 13.83 2 -14 8 763.87 23.81 2 -14 8 709.43 14.58 -2 -14 -8 728.07 12.87 2 -14 8 780.63 24.43 -2 -14 -8 683.96 20.81 2 -14 7 7.72 2.52 -2 -14 -7 7.84 1.35 -2 -14 -7 7.17 1.92 2 -14 7 9.33 1.61 2 -14 7 9.35 3.16 2 -14 6 326.55 14.36 -2 -14 -6 309.19 7.53 2 -14 6 308.79 8.25 2 -14 6 327.10 15.05 -2 -14 -6 298.14 12.16 -2 -14 -5 59.27 2.83 2 -14 5 57.47 3.21 2 -14 5 62.35 6.49 -2 -14 -5 56.75 2.73 2 -14 5 54.15 5.65 2 -14 4 135.87 4.92 2 -14 4 127.53 9.08 2 -14 4 131.14 8.57 -2 -14 -4 124.33 4.26 2 -14 3 15.72 3.37 -2 -14 -3 16.14 1.56 2 -14 3 15.79 3.24 2 -14 3 16.29 1.80 2 -14 2 58.06 3.06 -2 -14 -2 57.36 2.86 2 -14 2 52.11 5.02 2 -14 2 54.64 5.87 -2 -14 -1 26.03 2.00 -2 -14 -1 30.36 3.65 2 -14 1 23.76 3.34 2 -14 1 27.00 4.10 -2 -14 -1 22.28 3.37 2 -14 1 24.95 2.02 2 -14 0 63.77 5.96 -2 -14 0 60.78 5.19 2 -14 0 62.07 3.04 -2 -14 0 57.08 5.47 2 -14 0 65.98 5.22 -2 -14 0 68.50 3.13 2 -14 -1 22.82 3.67 -2 -14 1 22.15 3.41 -2 -14 1 25.29 2.03 -2 -14 1 26.85 4.04 2 -14 -1 22.85 1.89 2 -14 -2 51.90 2.22 -2 -14 2 52.16 5.20 2 -14 -2 54.46 2.76 2 -14 -2 50.86 5.21 -2 -14 2 55.21 2.89 2 -14 -3 15.16 1.46 2 -14 -3 20.24 3.42 -2 -14 3 17.38 1.73 -2 -14 3 14.04 3.14 2 -14 -3 17.52 1.38 2 -14 -4 127.89 3.90 2 -14 -4 124.88 4.16 -2 -14 4 131.12 8.74 -2 -14 4 137.72 4.74 2 -14 -5 63.43 2.73 2 -14 -5 61.59 2.65 -2 -14 5 64.48 3.21 -2 -14 5 69.53 6.45 -2 -14 6 319.88 7.99 -2 -14 6 318.43 14.47 2 -14 -6 306.44 7.09 -2 -14 7 9.05 1.47 -2 14 -7 8.49 1.13 2 -14 -7 10.58 1.40 2 -14 -7 10.60 1.35 2 -14 -8 693.00 13.26 2 -14 -8 696.71 14.03 -2 14 -8 716.82 13.30 2 -14 -8 707.78 13.28 -2 -14 8 703.76 13.90 -2 14 -9 178.42 5.32 2 -14 -9 169.04 5.10 2 -14 -9 174.80 5.80 2 -14 -9 174.49 5.23 -2 -14 9 178.37 5.53 -2 14 -10 281.06 7.18 2 -14 -10 279.63 7.68 -2 -14 10 281.89 7.18 2 -14 -10 269.66 6.83 2 -14 -10 287.88 7.10 2 -14 -11 110.90 4.57 2 -14 -11 112.44 4.17 -2 14 -11 110.48 4.20 2 -14 -11 105.58 3.83 2 -14 -12 266.51 6.57 2 -14 -12 268.88 7.50 -2 14 -12 276.14 7.17 2 -14 -12 278.10 7.04 2 -14 -13 36.52 2.40 2 -14 -13 39.54 2.81 -2 14 -13 36.88 2.60 -2 14 -13 35.11 2.43 2 -14 -13 35.89 2.08 2 -14 -14 135.24 3.99 -2 14 -14 137.25 4.65 2 -14 -14 133.94 4.78 -2 14 -14 130.41 4.62 2 -14 -14 140.08 4.53 2 -14 -15 54.66 2.70 2 -14 -15 53.96 2.80 -2 14 -15 46.81 2.61 -2 14 -15 51.66 2.76 2 -14 -15 55.22 2.96 2 -14 -16 11.80 1.44 2 -14 -16 16.08 1.75 -2 14 -16 13.12 1.42 -2 14 -16 13.54 1.56 -2 14 -17 30.10 1.81 2 -14 -17 35.47 1.97 -2 14 -18 11.37 0.99 2 -14 -18 13.62 1.19 2 -14 -19 5.27 0.70 -2 14 -19 5.92 0.73 2 15 -18 36.21 1.67 -2 -15 -18 36.93 1.49 -2 -15 -17 41.90 1.75 2 15 -17 42.34 2.02 -2 -15 -17 43.86 1.90 2 15 -16 28.34 1.86 -2 -15 -16 27.93 1.74 -2 -15 -16 28.40 1.65 -2 -15 -15 48.03 2.36 -2 -15 -15 49.32 2.45 2 15 -15 49.28 2.61 -2 -15 -14 64.73 2.92 2 15 -14 66.35 3.19 2 15 -13 106.92 4.28 -2 -15 -13 106.27 3.96 2 15 -12 123.42 4.76 -2 -15 -12 135.28 4.65 2 15 -11 107.86 3.57 2 -15 11 109.62 3.96 -2 -15 -11 108.84 4.18 2 15 -10 25.57 1.82 -2 -15 -10 28.68 1.81 -2 -15 -10 23.40 2.08 2 -15 10 25.67 2.03 2 15 -9 24.87 1.75 -2 -15 -9 23.32 1.60 2 -15 9 23.82 2.02 -2 -15 -9 22.98 2.09 2 -15 8 32.03 2.66 -2 -15 -8 36.49 2.49 -2 -15 -7 218.34 6.24 2 -15 7 214.65 6.84 2 -15 6 61.98 3.59 2 -15 6 62.31 6.13 -2 -15 -6 60.62 3.08 2 -15 6 64.62 7.02 -2 -15 -5 176.60 5.36 -2 -15 -5 171.87 5.22 2 -15 5 192.08 11.50 2 -15 5 177.54 6.05 2 -15 5 175.10 10.27 -2 -15 -4 128.16 4.47 2 -15 4 134.72 8.64 2 -15 4 137.45 9.62 -2 -15 -4 131.17 4.48 2 -15 4 134.25 5.11 2 -15 3 28.06 4.35 2 -15 3 28.90 2.37 -2 -15 -3 28.29 2.14 2 -15 3 24.06 3.62 2 -15 2 47.27 4.91 -2 -15 -2 46.44 2.71 2 -15 2 45.73 2.88 2 -15 2 50.57 5.82 -2 -15 -1 34.45 2.38 2 -15 1 33.71 2.50 2 -15 1 30.04 3.81 2 -15 1 27.79 4.21 -2 -15 0 169.28 9.50 -2 -15 0 176.46 5.60 2 -15 0 175.79 5.62 2 -15 0 173.67 10.27 -2 -15 0 162.54 8.81 -2 -15 1 37.13 4.83 -2 -15 1 39.41 2.57 2 -15 -1 37.62 2.51 -2 -15 1 35.35 4.23 2 -15 -1 29.82 4.39 2 -15 -2 45.89 5.13 -2 -15 2 38.75 4.64 -2 -15 2 48.19 2.93 -2 -15 2 50.50 5.56 2 -15 -2 45.51 2.65 -2 -15 3 27.43 3.99 2 -15 -3 29.93 2.12 -2 -15 3 27.71 4.22 2 -15 -3 30.15 1.80 -2 -15 3 30.54 2.41 2 -15 -4 138.70 4.50 -2 -15 4 122.55 8.60 2 -15 -4 139.21 4.14 2 -15 -4 131.66 4.43 -2 -15 4 132.54 9.33 -2 -15 4 139.37 5.05 2 -15 -5 177.12 5.12 -2 -15 5 178.23 5.85 -2 -15 5 179.96 11.04 -2 -15 5 181.08 10.67 2 -15 -5 179.38 4.95 2 -15 -6 64.47 3.07 -2 -15 6 74.41 7.37 -2 -15 6 63.12 6.51 -2 -15 6 63.89 3.36 2 -15 -6 63.02 2.81 2 -15 -7 218.99 6.11 2 -15 -7 228.57 5.95 -2 -15 7 225.53 6.67 -2 15 -7 233.38 5.82 -2 15 -8 34.50 2.08 2 -15 -8 32.51 2.13 -2 -15 8 33.25 2.47 2 -15 -8 33.53 2.24 2 -15 -9 24.65 1.94 -2 15 -9 23.57 1.83 2 -15 -9 24.78 1.97 -2 -15 9 20.95 1.99 -2 -15 10 26.11 2.02 2 -15 -10 26.68 1.95 2 -15 -10 25.79 2.02 -2 15 -10 23.97 1.92 2 -15 -11 111.01 3.88 -2 -15 11 106.33 3.89 2 -15 -11 111.54 4.05 -2 15 -11 109.59 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10.53 1.57 4 -12 -13 11.48 1.74 -4 12 -13 9.12 1.59 -4 12 -13 9.95 1.74 4 -12 -13 8.67 1.71 4 -12 -14 71.53 3.42 4 -12 -14 75.69 3.80 -4 12 -14 74.18 3.69 -4 12 -14 69.68 3.28 4 -12 -14 69.64 3.36 4 -12 -14 72.01 3.40 4 -12 -15 75.82 3.42 4 -12 -15 70.48 3.63 4 -12 -15 69.05 3.21 -4 12 -15 69.55 3.13 4 -12 -15 74.32 3.45 -4 12 -15 81.29 3.71 4 -12 -16 20.51 1.79 4 -12 -16 20.05 1.86 4 -12 -16 19.96 1.69 -4 12 -16 18.93 1.58 4 -12 -16 21.99 2.21 -4 12 -16 19.37 2.04 4 -12 -17 101.78 3.65 4 -12 -17 105.65 3.98 -4 12 -17 99.96 3.26 -4 12 -17 98.31 3.79 4 -12 -18 10.38 1.48 -4 12 -18 6.14 0.79 4 -12 -18 9.59 1.18 -4 12 -18 8.11 1.19 4 -12 -19 63.52 2.39 4 -12 -19 68.39 2.62 -4 12 -20 34.11 1.57 -4 -13 -19 10.15 0.81 4 13 -19 11.28 1.02 4 13 -18 125.55 3.68 -4 -13 -18 124.99 3.45 -4 -13 -17 4.10 0.79 -4 -13 -17 3.62 0.93 4 13 -17 4.03 1.13 -4 -13 -16 53.78 2.43 -4 -13 -16 56.79 2.67 4 13 -16 61.16 2.95 -4 -13 -16 59.76 2.79 -4 -13 -15 6.44 1.03 -4 -13 -15 8.75 1.35 -4 -13 -15 7.48 1.40 4 13 -15 6.75 1.43 -4 -13 -14 174.42 5.47 -4 -13 -14 173.33 5.22 4 13 -14 188.17 5.68 -4 -13 -13 10.94 1.66 -4 -13 -13 10.79 1.40 4 13 -13 12.05 1.80 4 13 -12 130.57 4.78 -4 -13 -12 134.31 4.79 -4 -13 -12 123.64 4.26 -4 -13 -12 122.22 4.65 -4 -13 -11 77.08 3.59 -4 -13 -11 72.21 3.51 4 -13 11 77.95 3.53 4 13 -11 81.08 3.71 4 13 -11 79.93 3.04 -4 -13 -10 79.65 3.62 4 13 -10 74.52 3.03 4 -13 10 70.49 3.47 -4 -13 -10 70.57 3.37 4 13 -9 115.62 4.01 -4 -13 -9 128.53 4.53 -4 -13 -9 117.24 8.29 4 -13 9 126.72 4.73 -4 -13 -9 119.52 4.35 4 -13 9 123.02 8.98 -4 -13 -8 83.73 3.59 -4 -13 -8 87.97 7.09 4 -13 8 87.18 7.56 -4 -13 -8 81.51 3.40 4 -13 8 81.99 3.80 4 -13 7 23.07 2.14 4 -13 7 21.41 4.18 -4 -13 -7 22.12 3.56 -4 -13 -7 21.45 1.65 -4 -13 -7 22.88 1.87 -4 -13 -6 120.98 7.88 4 -13 6 123.44 9.05 -4 -13 -6 125.08 4.20 4 -13 6 129.47 4.76 -4 -13 -6 117.51 3.88 4 -13 5 114.33 4.38 -4 -13 -5 105.17 7.11 -4 -13 -5 99.15 3.75 -4 -13 -5 108.54 3.82 4 -13 5 105.76 8.25 4 -13 4 273.77 13.40 -4 -13 -4 271.02 6.85 -4 -13 -4 272.88 6.53 -4 -13 -4 273.30 11.47 4 -13 4 275.55 7.31 4 -13 3 6.13 2.44 -4 -13 -3 8.25 1.13 -4 -13 -3 5.90 1.62 -4 -13 -3 7.56 1.23 4 -13 3 8.63 1.41 4 -13 2 494.87 10.53 -4 -13 -2 471.16 10.15 -4 -13 -2 494.81 15.38 4 -13 2 472.10 17.80 -4 -13 -2 481.70 14.83 4 -13 1 120.86 8.50 4 -13 1 114.49 3.67 -4 -13 -1 124.69 4.36 -4 -13 -1 123.63 7.45 4 -13 1 130.93 4.50 4 -13 0 213.55 5.40 -4 -13 0 217.27 10.42 -4 -13 0 235.00 6.31 4 -13 0 217.07 11.39 4 -13 0 232.44 6.26 4 -13 -1 127.81 8.55 -4 -13 1 121.89 7.98 -4 -13 1 131.35 4.50 4 -13 -1 127.38 4.38 4 -13 -1 125.30 3.88 -4 -13 2 507.22 10.61 4 -13 -2 482.28 10.16 4 -13 -2 486.11 17.21 -4 -13 2 486.31 17.14 4 -13 -2 488.63 9.63 -4 -13 3 11.53 1.62 4 -13 -3 9.22 1.09 4 -13 -3 9.86 1.27 -4 -13 3 9.83 2.79 4 -13 -3 8.70 2.64 4 -13 -4 282.86 6.61 4 -13 -4 264.73 12.09 -4 -13 4 277.60 12.99 4 -13 -4 269.45 6.64 -4 -13 4 288.66 7.33 4 -13 -5 112.58 3.81 4 -13 -5 111.44 4.23 -4 -13 5 115.24 4.29 -4 13 -5 104.05 3.59 -4 -13 5 116.51 8.55 -4 -13 6 125.65 4.53 4 -13 -6 124.96 4.53 -4 13 -6 121.96 4.05 -4 -13 6 117.04 8.64 4 -13 -6 118.01 4.05 4 -13 -7 29.60 2.65 4 -13 -7 22.00 1.60 -4 -13 7 22.84 1.99 4 -13 -7 22.72 2.06 -4 -13 7 20.73 3.91 -4 13 -7 22.66 1.81 4 -13 -7 22.09 1.81 -4 -13 8 84.29 3.65 -4 -13 8 81.20 7.43 4 -13 -8 87.24 4.09 4 -13 -8 79.49 3.07 -4 13 -8 87.71 3.58 4 -13 -8 81.39 3.76 4 -13 -8 83.31 3.47 4 -13 -9 121.77 4.84 -4 -13 9 131.08 9.24 -4 -13 9 122.53 4.41 -4 13 -9 123.74 4.44 4 -13 -9 116.19 4.30 4 -13 -9 118.84 4.66 4 -13 -9 122.06 3.87 4 -13 -10 71.61 3.67 -4 13 -10 73.59 3.52 4 -13 -10 77.25 3.95 -4 -13 10 74.10 3.27 4 -13 -10 72.45 2.91 4 -13 -10 76.13 3.47 4 -13 -11 83.24 4.05 4 -13 -11 78.83 3.76 -4 13 -11 80.75 3.70 4 -13 -11 78.12 3.55 4 -13 -12 128.31 5.03 4 -13 -12 121.48 4.73 -4 13 -12 131.18 4.82 4 -13 -12 126.81 4.58 4 -13 -13 11.01 1.69 4 -13 -13 13.97 2.24 4 -13 -13 12.37 1.75 -4 13 -13 9.69 1.46 -4 13 -13 10.38 1.72 -4 13 -14 164.28 5.16 4 -13 -14 182.85 5.86 4 -13 -14 177.28 5.40 4 -13 -14 177.63 5.47 4 -13 -14 181.74 5.50 -4 13 -14 185.70 5.71 -4 13 -15 6.98 1.13 4 -13 -15 5.74 1.23 4 -13 -15 6.91 1.41 4 -13 -15 8.90 1.86 -4 13 -15 6.96 1.44 4 -13 -16 56.66 2.73 4 -13 -16 59.72 3.05 -4 13 -16 51.82 2.44 4 -13 -16 58.36 2.77 -4 13 -16 57.14 2.83 4 -13 -17 5.26 1.07 4 -13 -17 6.93 1.45 -4 13 -17 4.46 0.83 -4 13 -17 3.87 1.13 4 -13 -18 127.30 3.63 4 -13 -18 135.98 3.89 -4 13 -18 125.94 3.72 4 -13 -19 13.20 1.01 -4 13 -19 9.89 0.99 4 14 -18 6.17 0.91 -4 -14 -18 8.01 0.81 -4 -14 -17 13.41 1.23 4 14 -17 15.14 1.39 -4 -14 -17 12.26 1.01 -4 -14 -16 3.58 0.77 -4 -14 -16 6.08 1.12 4 14 -16 4.40 1.14 -4 -14 -15 29.66 1.81 -4 -14 -15 31.80 2.11 4 14 -15 32.18 2.19 -4 -14 -14 75.07 3.15 -4 -14 -14 81.28 3.50 4 14 -14 80.35 3.53 4 14 -13 118.77 4.48 -4 -14 -13 116.21 4.35 4 14 -12 139.45 4.01 -4 -14 -12 146.90 5.05 4 14 -12 148.33 5.09 4 14 -11 67.45 3.39 4 14 -11 61.95 2.68 4 -14 11 61.06 3.15 -4 -14 -11 60.98 3.24 4 -14 10 84.30 3.86 -4 -14 -10 90.04 3.88 -4 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