#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 18/08/2019' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Eigner, V\'aclav' ; eigner@fzu.cz ; ; Institute of Physics AS CR, v.v.i. Na Slovance 2 182 21 Prague 8 Czech Republic ; 'Du\3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_gt 0.0794 _refine_ls_R_factor_all 0.0305 _refine_ls_wR_factor_ref 0.0821 _refine_ls_goodness_of_fit_ref 1.47 _refine_ls_goodness_of_fit_gt 1.50 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4764 _refine_ls_number_parameters 386 _refine_ls_number_restraints 15 _refine_ls_number_constraints 139 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0016I^2^)' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_shift/su_max 0.0452 _refine_ls_shift/su_mean 0.0015 _refine_diff_density_max 0.48 _refine_diff_density_min -0.40 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Cu -1.9646 0.5888 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param H1o2a . O2a . 0.82 0.001 H1o2b . O2b . 0.82 0.001 H1n2a . N2a . 0.86 0.001 H1n2b . N2b . 0.86 0.001 loop_ _restr_angle_atom_site_label_1 _restr_angle_site_symmetry_1 _restr_angle_atom_site_label_2 _restr_angle_site_symmetry_2 _restr_angle_atom_site_label_3 _restr_angle_site_symmetry_3 _restr_angle_target _restr_angle_target_weight_param O4c . N2c . O5c . 120 1 O4c . N2c . O6c . 120 1 O5c . N2c . O6c . 120 1 O7c . N3c . O8c . 120 1 O7c . N3c . O9c . 120 1 O8c . N3c . O9c . 120 1 loop_ _restr_torsion_atom_site_label_1 _restr_torsion_site_symmetry_1 _restr_torsion_atom_site_label_2 _restr_torsion_site_symmetry_2 _restr_torsion_atom_site_label_3 _restr_torsion_site_symmetry_3 _restr_torsion_atom_site_label_4 _restr_torsion_site_symmetry_4 _restr_torsion_angle_target _restr_torsion_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param N2c . O4c . 1 0.001 N2c . O5c . 1 0.001 N2c . O6c . 1 0.001 N3c . O7c . 1 0.001 N3c . O8c . 1 0.001 N3c . O9c . 1 0.001 loop_ _restr_equal_angle_atom_site_label_1 _restr_equal_angle_site_symmetry_1 _restr_equal_angle_atom_site_label_2 _restr_equal_angle_site_symmetry_2 _restr_equal_angle_atom_site_label_3 _restr_equal_angle_site_symmetry_3 _restr_equal_angle_class_class_id _restr_equal_angle_class_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_equal_torsion_atom_site_label_1 _restr_equal_torsion_site_symmetry_1 _restr_equal_torsion_atom_site_label_2 _restr_equal_torsion_site_symmetry_2 _restr_equal_torsion_atom_site_label_3 _restr_equal_torsion_site_symmetry_3 _restr_equal_torsion_atom_site_label_4 _restr_equal_torsion_site_symmetry_4 _restr_equal_torsion_class_class_id _restr_equal_torsion_class_target_weight_param ? ? ? ? ? ? ? ? ? ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1a Cu 0.06239(3) 0.36157(2) 0.264544(10) Uani 0.01915(9) 4 1 d . . . Cu1b Cu -0.16014(3) 0.76410(2) 0.077468(10) Uani 0.01879(9) 4 1 d . . . O1a O 0.22510(13) 0.44386(12) 0.30421(5) Uani 0.0201(4) 4 1 d . . . O2a O -0.08917(13) 0.40920(11) 0.30789(5) Uani 0.0192(4) 4 1 d . . . O1b O -0.00162(14) 0.87495(12) 0.09555(5) Uani 0.0224(4) 4 1 d . . . O2b O -0.32177(13) 0.86152(11) 0.10385(5) Uani 0.0194(4) 4 1 d . . . O1c O -0.02630(16) 0.56196(12) 0.21450(6) Uani 0.0292(4) 4 1 d . . . O2c O -0.11762(14) 0.70296(12) 0.16329(5) Uani 0.0242(4) 4 1 d . . . O3c O -0.02382(19) 0.54932(14) 0.13189(6) Uani 0.0382(5) 4 1 d . . . O4c O 0.7039(3) 0.3734(3) 0.05926(9) Uani 0.0351(7) 4 0.883(10) d . 1 1 O5c O 0.5610(4) 0.2653(2) 0.09780(11) Uani 0.0467(8) 4 0.883(10) d . 1 1 O6c O 0.5635(5) 0.4532(2) 0.10776(12) Uani 0.0512(10) 4 0.883(10) d . 1 1 N1a N 0.16521(16) 0.33629(14) 0.20654(6) Uani 0.0197(4) 4 1 d . . . N2a N -0.10636(17) 0.27134(14) 0.22413(7) Uani 0.0227(5) 4 1 d . . . N1b N -0.07237(16) 0.70014(14) 0.02099(6) Uani 0.0204(4) 4 1 d . . . N2b N -0.33188(17) 0.65508(14) 0.05393(6) Uani 0.0217(4) 4 1 d . . . N1c N -0.05499(16) 0.60253(14) 0.16979(6) Uani 0.0218(4) 4 1 d . . . N2c N 0.6100(5) 0.36347(18) 0.08871(18) Uani 0.0262(8) 4 0.883(10) d . 1 1 N3c N 0.596(4) 0.366(2) 0.0959(14) Uani 0.0262(8) 4 0.117(10) d . 1 2 C1a C 0.33713(18) 0.49372(15) 0.28512(7) Uani 0.0171(5) 4 1 d . . . C2a C 0.36233(18) 0.47848(16) 0.23347(7) Uani 0.0185(5) 4 1 d . . . C3a C 0.4809(2) 0.54005(17) 0.21695(8) Uani 0.0229(5) 4 1 d . . . C4a C 0.5761(2) 0.61233(17) 0.24962(8) Uani 0.0238(6) 4 1 d . . . C5a C 0.55365(19) 0.62358(16) 0.30081(8) Uani 0.0216(5) 4 1 d . . . C6a C 0.43713(18) 0.56592(16) 0.31818(7) Uani 0.0195(5) 4 1 d . . . C7a C 0.27575(19) 0.39867(16) 0.19682(7) Uani 0.0198(5) 4 1 d . . . C8a C 0.0819(2) 0.25592(17) 0.16856(8) Uani 0.0247(6) 4 1 d . . . C9a C -0.0852(2) 0.27211(18) 0.16973(8) Uani 0.0268(6) 4 1 d . . . C10a C -0.2456(2) 0.32576(19) 0.23547(9) Uani 0.0298(6) 4 1 d . . . C11a C -0.2271(2) 0.34348(17) 0.29296(8) Uani 0.0256(6) 4 1 d . . . C1b C 0.09443(18) 0.90974(16) 0.06548(7) Uani 0.0187(5) 4 1 d . . . C2b C 0.11326(19) 0.85273(16) 0.01898(7) Uani 0.0198(5) 4 1 d . . . C3b C 0.2155(2) 0.89829(19) -0.01050(8) Uani 0.0257(6) 4 1 d . . . C4b C 0.3008(2) 0.99665(19) 0.00477(8) Uani 0.0279(6) 4 1 d . . . C5b C 0.2868(2) 1.05042(18) 0.05134(8) Uani 0.0261(6) 4 1 d . . . C6b C 0.1858(2) 1.00849(17) 0.08089(8) Uani 0.0235(5) 4 1 d . . . C7b C 0.03128(19) 0.74781(17) 0.00001(7) Uani 0.0217(5) 4 1 d . . . C8b C -0.1543(2) 0.59518(17) -0.00059(8) Uani 0.0260(6) 4 1 d . . . C9b C -0.3200(2) 0.61709(17) 0.00090(8) Uani 0.0251(6) 4 1 d . . . C10b C -0.4751(2) 0.71552(18) 0.05794(9) Uani 0.0278(6) 4 1 d . . . C11b C -0.4508(2) 0.78825(18) 0.10663(8) Uani 0.0257(6) 4 1 d . . . H1c3a H 0.496094 0.531465 0.181826 Uiso 0.0275 4 1 d . . . H1c4a H 0.65601 0.654042 0.237522 Uiso 0.0285 4 1 d . . . H1c5a H 0.620452 0.672237 0.324229 Uiso 0.026 4 1 d . . . H1c6a H 0.424088 0.575272 0.35348 Uiso 0.0234 4 1 d . . . H1c7a H 0.302958 0.392138 0.163137 Uiso 0.0237 4 1 d . . . H1c8a H 0.110623 0.176759 0.177836 Uiso 0.0297 4 1 d . . . H2c8a H 0.101964 0.274928 0.134769 Uiso 0.0297 4 1 d . . . H1c9a H -0.118175 0.345923 0.15429 Uiso 0.0322 4 1 d . . . H2c9a H -0.141041 0.208678 0.151609 Uiso 0.0322 4 1 d . . . H1c10a H -0.329619 0.274562 0.224382 Uiso 0.0358 4 1 d . . . H2c10a H -0.26039 0.400209 0.21837 Uiso 0.0358 4 1 d . . . H1c11a H -0.310719 0.388018 0.300935 Uiso 0.0307 4 1 d . . . H2c11a H -0.217856 0.26876 0.309962 Uiso 0.0307 4 1 d . . . H1c3b H 0.22672 0.860097 -0.042193 Uiso 0.0308 4 1 d . . . H1c4b H 0.368713 1.027555 -0.016391 Uiso 0.0334 4 1 d . . . H1c5b H 0.348165 1.117242 0.062941 Uiso 0.0314 4 1 d . . . H1c6b H 0.177172 1.047268 0.112697 Uiso 0.0282 4 1 d . . . H1c7b H 0.05637 0.711488 -0.030392 Uiso 0.026 4 1 d . . . H1c8b H -0.120206 0.528623 0.020553 Uiso 0.0312 4 1 d . . . H2c8b H -0.140504 0.584829 -0.035762 Uiso 0.0312 4 1 d . . . H1c9b H -0.356862 0.678085 -0.023116 Uiso 0.0302 4 1 d . . . H2c9b H -0.375741 0.545808 -0.007009 Uiso 0.0302 4 1 d . . . H1c10b H -0.552497 0.65846 0.059729 Uiso 0.0333 4 1 d . . . H2c10b H -0.503176 0.765691 0.028537 Uiso 0.0333 4 1 d . . . H1c11b H -0.537857 0.836524 0.107405 Uiso 0.0309 4 1 d . . . H2c11b H -0.428866 0.737658 0.136153 Uiso 0.0309 4 1 d . . . H1n2a H -0.101(3) 0.2013(8) 0.2364(9) Uiso 0.0273 4 1 d . . . H1n2b H -0.318(3) 0.5940(13) 0.0733(8) Uiso 0.026 4 1 d . . . H1o2a H -0.062(2) 0.399(2) 0.33902(19) Uiso 0.0231 4 1 d . . . H1o2b H -0.292(2) 0.892(2) 0.1321(4) Uiso 0.0232 4 1 d . . . O7c O 0.504(3) 0.2947(19) 0.1086(9) Uani 0.0467(8) 4 0.117(10) d . 1 2 O8c O 0.620(3) 0.4597(16) 0.1198(9) Uani 0.0512(10) 4 0.117(10) d . 1 2 O9c O 0.673(3) 0.3399(19) 0.0624(8) Uani 0.0351(7) 4 0.117(10) d . 1 2 loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1a Cu 0.01369(14) 0.02377(16) 0.01976(15) -0.00305(9) 0.00217(10) -0.00723(10) Cu1b Cu 0.01748(15) 0.01994(15) 0.01932(15) -0.00449(9) 0.00417(11) -0.00311(10) O1a O 0.0168(5) 0.0258(7) 0.0178(6) -0.0058(5) 0.0030(5) -0.0024(5) O2a O 0.0157(5) 0.0229(6) 0.0190(6) -0.0004(5) 0.0024(5) 0.0008(5) O1b O 0.0213(6) 0.0262(7) 0.0209(6) -0.0077(5) 0.0067(5) -0.0048(5) O2b O 0.0179(6) 0.0211(6) 0.0190(6) -0.0005(5) 0.0026(5) 0.0003(5) O1c O 0.0400(7) 0.0213(7) 0.0240(7) 0.0056(5) -0.0004(6) 0.0078(6) O2c O 0.0258(6) 0.0183(6) 0.0268(7) 0.0043(5) -0.0004(5) 0.0054(5) O3c O 0.0521(9) 0.0326(8) 0.0293(8) 0.0104(7) 0.0052(7) -0.0022(7) O4c O 0.0382(12) 0.0341(14) 0.0349(9) 0.0003(9) 0.0116(8) 0.0053(9) O5c O 0.0386(16) 0.0344(12) 0.0609(14) -0.0137(10) -0.0095(12) 0.0263(11) O6c O 0.086(2) 0.0414(11) 0.0316(14) 0.0120(13) 0.0263(14) -0.0010(10) N1a N 0.0177(7) 0.0211(7) 0.0193(7) 0.0030(6) 0.0002(6) -0.0059(6) N2a N 0.0187(7) 0.0206(8) 0.0278(8) -0.0004(6) 0.0007(6) -0.0043(7) N1b N 0.0201(7) 0.0196(8) 0.0206(7) -0.0011(6) 0.0007(6) -0.0028(6) N2b N 0.0207(7) 0.0193(7) 0.0239(8) -0.0025(6) 0.0010(6) 0.0015(6) N1c N 0.0199(7) 0.0201(8) 0.0241(8) -0.0008(6) -0.0002(6) 0.0021(7) N2c N 0.0298(13) 0.0256(9) 0.0204(17) -0.0050(8) -0.0035(9) 0.0054(8) N3c N 0.0298(13) 0.0256(9) 0.0204(17) -0.0050(8) -0.0035(9) 0.0054(8) C1a C 0.0145(7) 0.0166(8) 0.0200(8) 0.0019(6) 0.0023(6) -0.0002(7) C2a C 0.0160(7) 0.0186(8) 0.0202(8) 0.0037(6) 0.0016(6) -0.0005(7) C3a C 0.0223(8) 0.0242(9) 0.0238(9) 0.0045(7) 0.0085(7) 0.0018(8) C4a C 0.0181(8) 0.0228(9) 0.0317(10) -0.0016(7) 0.0079(8) 0.0024(8) C5a C 0.0161(8) 0.0188(9) 0.0289(10) -0.0010(6) 0.0005(7) -0.0009(8) C6a C 0.0188(8) 0.0194(9) 0.0197(9) 0.0006(6) 0.0015(7) -0.0012(7) C7a C 0.0200(8) 0.0218(9) 0.0173(8) 0.0050(7) 0.0026(7) -0.0019(7) C8a C 0.0247(9) 0.0259(10) 0.0221(9) -0.0004(7) 0.0000(8) -0.0096(8) C9a C 0.0239(9) 0.0297(10) 0.0240(10) -0.0023(7) -0.0039(8) -0.0066(8) C10a C 0.0164(8) 0.0296(10) 0.0420(12) -0.0014(7) 0.0011(8) -0.0066(9) C11a C 0.0163(8) 0.0236(9) 0.0375(11) -0.0028(7) 0.0064(8) 0.0003(8) C1b C 0.0170(8) 0.0192(8) 0.0198(9) -0.0013(6) 0.0027(7) 0.0021(7) C2b C 0.0168(8) 0.0241(9) 0.0180(8) 0.0015(7) 0.0012(7) 0.0020(7) C3b C 0.0212(8) 0.0358(11) 0.0196(9) 0.0004(8) 0.0025(7) 0.0048(8) C4b C 0.0198(8) 0.0356(11) 0.0283(10) -0.0015(8) 0.0046(7) 0.0134(9) C5b C 0.0209(8) 0.0243(10) 0.0315(10) -0.0038(7) -0.0006(8) 0.0075(8) C6b C 0.0234(8) 0.0201(9) 0.0266(9) -0.0032(7) 0.0029(7) -0.0003(8) C7b C 0.0208(8) 0.0271(10) 0.0171(8) 0.0015(7) 0.0028(7) -0.0025(7) C8b C 0.0292(10) 0.0215(9) 0.0269(10) -0.0043(7) 0.0037(8) -0.0045(8) C9b C 0.0268(9) 0.0228(9) 0.0241(9) -0.0057(7) -0.0009(8) -0.0020(8) C10b C 0.0175(8) 0.0265(10) 0.0377(11) -0.0032(7) 0.0001(8) -0.0020(9) C11b C 0.0165(8) 0.0274(10) 0.0337(10) -0.0015(7) 0.0054(8) 0.0028(9) O7c O 0.0386(16) 0.0344(12) 0.0609(14) -0.0137(10) -0.0095(12) 0.0263(11) O8c O 0.086(2) 0.0414(11) 0.0316(14) 0.0120(13) 0.0263(14) -0.0010(10) O9c O 0.0382(12) 0.0341(14) 0.0349(9) 0.0003(9) 0.0116(8) 0.0053(9) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1a O1a . . 1.8942(12) ? Cu1a O2a . . 1.9941(14) ? Cu1a N1a . . 1.9335(16) ? Cu1a N2a . . 1.9849(15) ? Cu1a O1c . . 2.6909(14) ? Cu1a O2c . 2_545 2.6073(14) ? Cu1b O1b . . 1.9046(13) ? Cu1b O2b . . 2.0426(13) ? Cu1b N1b . . 1.9377(17) ? Cu1b N2b . . 1.9974(15) ? Cu1b O2c . . 2.3279(14) ? O1a C1a . . 1.327(2) ? O2a C11a . . 1.445(2) ? O2a H1o2a . . 0.820(7) ? O1b C1b . . 1.326(2) ? O2b C11b . . 1.442(2) ? O2b H1o2b . . 0.820(14) ? O1c N1c . . 1.248(2) ? O2c N1c . . 1.276(2) ? O3c N1c . . 1.238(2) ? O4c N2c . . 1.243(6) ? O5c N2c . . 1.242(4) ? O6c N2c . . 1.244(5) ? N1a C7a . . 1.283(2) ? N1a C8a . . 1.464(2) ? N2a C9a . . 1.473(3) ? N2a C10a . . 1.473(3) ? N2a H1n2a . . 0.860(13) ? N1b C7b . . 1.282(3) ? N1b C8b . . 1.469(2) ? N2b C9b . . 1.480(3) ? N2b C10b . . 1.480(2) ? N2b H1n2b . . 0.860(17) ? N3c O7c . . 1.24(4) ? N3c O8c . . 1.24(3) ? N3c O9c . . 1.24(5) ? C1a C2a . . 1.423(3) ? C1a C6a . . 1.406(2) ? C2a C3a . . 1.406(3) ? C2a C7a . . 1.452(2) ? C3a C4a . . 1.378(3) ? C3a H1c3a . . 0.96 ? C4a C5a . . 1.399(3) ? C4a H1c4a . . 0.96 ? C5a C6a . . 1.379(3) ? C5a H1c5a . . 0.96 ? C6a H1c6a . . 0.96 ? C7a H1c7a . . 0.96 ? C8a C9a . . 1.519(3) ? C8a H1c8a . . 0.96 ? C8a H2c8a . . 0.96 ? C9a H1c9a . . 0.96 ? C9a H2c9a . . 0.96 ? C10a C11a . . 1.504(3) ? C10a H1c10a . . 0.96 ? C10a H2c10a . . 0.96 ? C11a H1c11a . . 0.96 ? C11a H2c11a . . 0.96 ? C1b C2b . . 1.419(3) ? C1b C6b . . 1.413(3) ? C2b C3b . . 1.399(3) ? C2b C7b . . 1.450(3) ? C3b C4b . . 1.380(3) ? C3b H1c3b . . 0.96 ? C4b C5b . . 1.393(3) ? C4b H1c4b . . 0.96 ? C5b C6b . . 1.378(3) ? C5b H1c5b . . 0.96 ? C6b H1c6b . . 0.96 ? C7b H1c7b . . 0.96 ? C8b C9b . . 1.517(3) ? C8b H1c8b . . 0.96 ? C8b H2c8b . . 0.96 ? C9b H1c9b . . 0.96 ? C9b H2c9b . . 0.96 ? C10b C11b . . 1.509(3) ? C10b H1c10b . . 0.96 ? C10b H2c10b . . 0.96 ? C11b H1c11b . . 0.96 ? C11b H2c11b . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1a Cu1a O2a . . . 95.13(5) ? O1a Cu1a O1c . . . 89.05(5) ? O1a Cu1a O2c . . 2_545 84.91(5) ? O1a Cu1a N1a . . . 94.55(6) ? O1a Cu1a N2a . . . 178.40(6) ? O2a Cu1a O1c . . . 82.68(5) ? O2a Cu1a O2c . . 2_545 80.70(5) ? O2a Cu1a N1a . . . 162.82(6) ? O2a Cu1a N2a . . . 84.99(6) ? O1c Cu1a O2c . . 2_545 161.72(5) ? O1c Cu1a N1a . . . 83.33(6) ? O1c Cu1a N2a . . . 92.55(5) ? O2c Cu1a N1a 2_545 . . 114.31(6) ? O2c Cu1a N2a 2_545 . . 93.53(6) ? N1a Cu1a N2a . . . 85.74(7) ? O1b Cu1b O2b . . . 95.67(5) ? O1b Cu1b O2c . . . 88.03(5) ? O1b Cu1b N1b . . . 93.23(6) ? O1b Cu1b N2b . . . 175.78(6) ? O2b Cu1b O2c . . . 81.01(5) ? O2b Cu1b N1b . . . 150.58(6) ? O2b Cu1b N2b . . . 83.54(6) ? O2c Cu1b N1b . . . 127.37(6) ? O2c Cu1b N2b . . . 95.93(6) ? N1b Cu1b N2b . . . 85.55(7) ? Cu1a O1a C1a . . . 124.72(11) ? Cu1a O2a C11a . . . 109.97(11) ? Cu1a O2a H1o2a . . . 114.6(16) ? C11a O2a H1o2a . . . 107.1(16) ? Cu1b O1b C1b . . . 125.86(11) ? Cu1b O2b C11b . . . 109.03(11) ? Cu1b O2b H1o2b . . . 113.0(15) ? C11b O2b H1o2b . . . 110.0(15) ? Cu1a N1a C7a . . . 124.35(13) ? Cu1a N1a C8a . . . 111.88(12) ? C7a N1a C8a . . . 122.41(16) ? Cu1a N2a C9a . . . 107.59(12) ? Cu1a N2a C10a . . . 105.75(12) ? Cu1a N2a H1n2a . . . 107.0(14) ? C9a N2a C10a . . . 116.64(15) ? C9a N2a H1n2a . . . 111.0(16) ? C10a N2a H1n2a . . . 108.3(17) ? Cu1b N1b C7b . . . 126.13(13) ? Cu1b N1b C8b . . . 111.11(12) ? C7b N1b C8b . . . 122.27(17) ? Cu1b N2b C9b . . . 107.32(12) ? Cu1b N2b C10b . . . 108.86(12) ? Cu1b N2b H1n2b . . . 107.2(13) ? C9b N2b C10b . . . 114.01(14) ? C9b N2b H1n2b . . . 107.0(13) ? C10b N2b H1n2b . . . 112.1(16) ? O1c N1c O2c . . . 118.38(16) ? O1c N1c O3c . . . 122.37(16) ? O2c N1c O3c . . . 119.25(16) ? O4c N2c O5c . . . 120.1(3) ? O4c N2c O6c . . . 119.0(3) ? O5c N2c O6c . . . 120.8(5) ? O7c N3c O8c . . . 119(4) ? O7c N3c O9c . . . 121(3) ? O8c N3c O9c . . . 120(3) ? O1a C1a C2a . . . 124.18(15) ? O1a C1a C6a . . . 117.70(16) ? C2a C1a C6a . . . 118.12(16) ? C1a C2a C3a . . . 119.03(15) ? C1a C2a C7a . . . 123.65(16) ? C3a C2a C7a . . . 117.27(17) ? C2a C3a C4a . . . 122.01(19) ? C2a C3a H1c3a . . . 118.99 ? C4a C3a H1c3a . . . 118.99 ? C3a C4a C5a . . . 118.52(18) ? C3a C4a H1c4a . . . 120.74 ? C5a C4a H1c4a . . . 120.74 ? C4a C5a C6a . . . 121.08(16) ? C4a C5a H1c5a . . . 119.46 ? C6a C5a H1c5a . . . 119.46 ? C1a C6a C5a . . . 121.17(18) ? C1a C6a H1c6a . . . 119.41 ? C5a C6a H1c6a . . . 119.41 ? N1a C7a C2a . . . 124.22(17) ? N1a C7a H1c7a . . . 117.89 ? C2a C7a H1c7a . . . 117.89 ? N1a C8a C9a . . . 107.61(16) ? N1a C8a H1c8a . . . 109.47 ? N1a C8a H2c8a . . . 109.47 ? C9a C8a H1c8a . . . 109.47 ? C9a C8a H2c8a . . . 109.47 ? H1c8a C8a H2c8a . . . 111.27 ? N2a C9a C8a . . . 108.09(15) ? N2a C9a H1c9a . . . 109.47 ? N2a C9a H2c9a . . . 109.47 ? C8a C9a H1c9a . . . 109.47 ? C8a C9a H2c9a . . . 109.47 ? H1c9a C9a H2c9a . . . 110.82 ? N2a C10a C11a . . . 107.88(15) ? N2a C10a H1c10a . . . 109.47 ? N2a C10a H2c10a . . . 109.47 ? C11a C10a H1c10a . . . 109.47 ? C11a C10a H2c10a . . . 109.47 ? H1c10a C10a H2c10a . . . 111.01 ? O2a C11a C10a . . . 106.58(16) ? O2a C11a H1c11a . . . 109.47 ? O2a C11a H2c11a . . . 109.47 ? C10a C11a H1c11a . . . 109.47 ? C10a C11a H2c11a . . . 109.47 ? H1c11a C11a H2c11a . . . 112.21 ? O1b C1b C2b . . . 124.07(16) ? O1b C1b C6b . . . 118.29(17) ? C2b C1b C6b . . . 117.63(17) ? C1b C2b C3b . . . 119.44(17) ? C1b C2b C7b . . . 123.13(17) ? C3b C2b C7b . . . 117.43(17) ? C2b C3b C4b . . . 121.78(19) ? C2b C3b H1c3b . . . 119.11 ? C4b C3b H1c3b . . . 119.11 ? C3b C4b C5b . . . 119.01(19) ? C3b C4b H1c4b . . . 120.5 ? C5b C4b H1c4b . . . 120.5 ? C4b C5b C6b . . . 120.54(18) ? C4b C5b H1c5b . . . 119.73 ? C6b C5b H1c5b . . . 119.73 ? C1b C6b C5b . . . 121.53(19) ? C1b C6b H1c6b . . . 119.23 ? C5b C6b H1c6b . . . 119.23 ? N1b C7b C2b . . . 124.57(18) ? N1b C7b H1c7b . . . 117.72 ? C2b C7b H1c7b . . . 117.72 ? N1b C8b C9b . . . 106.57(16) ? N1b C8b H1c8b . . . 109.47 ? N1b C8b H2c8b . . . 109.47 ? C9b C8b H1c8b . . . 109.47 ? C9b C8b H2c8b . . . 109.47 ? H1c8b C8b H2c8b . . . 112.22 ? N2b C9b C8b . . . 107.55(15) ? N2b C9b H1c9b . . . 109.47 ? N2b C9b H2c9b . . . 109.47 ? C8b C9b H1c9b . . . 109.47 ? C8b C9b H2c9b . . . 109.47 ? H1c9b C9b H2c9b . . . 111.33 ? N2b C10b C11b . . . 108.35(14) ? N2b C10b H1c10b . . . 109.47 ? N2b C10b H2c10b . . . 109.47 ? C11b C10b H1c10b . . . 109.47 ? C11b C10b H2c10b . . . 109.47 ? H1c10b C10b H2c10b . . . 110.57 ? O2b C11b C10b . . . 106.13(16) ? O2b C11b H1c11b . . . 109.47 ? O2b C11b H2c11b . . . 109.47 ? C10b C11b H1c11b . . . 109.47 ? C10b C11b H2c11b . . . 109.47 ? H1c11b C11b H2c11b . . . 112.62 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C3a H1c3a O6c . . . 0.96 2.31 3.237(4) 161 ? C3a H1c3a O8c . . . 0.96 2.27 3.16(3) 153 ? C9b H1c9b O7c . . 3_565 0.96 2.43 3.23(2) 140.75 ? N2a H1n2a O1c . . 2_545 0.860(13) 2.236(17) 3.013(2) 150.3(19) ? N2b H1n2b O6c . . 1_455 0.860(17) 2.21(2) 2.941(4) 143(2) ? N2b H1n2b O8c . . 1_455 0.860(17) 2.10(3) 2.90(2) 156(2) ? O2a H1o2a O1b . . 2_545 0.820(7) 1.739(7) 2.5579(18) 178(2) ? O2b H1o2b O1a . . 2_555 0.820(14) 1.781(13) 2.5986(17) 175(2) ? _iucr_refine_instructions_details ; # # .m40 # 74 0 0 1 0 3.457499 0.000000 0.000000 0.000000 0.000000 0.000000 100000 0.000000 0.000000 0.000000 000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 000000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 000000 Cu1a 3 2 1.000000 0.062385 0.361570 0.264544 0.013686 0.023768 0.019765-0.003046 0.002174-0.007231 0111111111 Cu1b 3 2 1.000000-0.160141 0.764101 0.077468 0.017481 0.019935 0.019316-0.004492 0.004171-0.003108 0111111111 O1a 5 2 1.000000 0.225103 0.443861 0.304211 0.016832 0.025793 0.017772-0.005771 0.002968-0.002435 0111111111 O2a 5 2 1.000000-0.089165 0.409200 0.307890 0.015676 0.022855 0.018987-0.000435 0.002366 0.000835 0111111111 O1b 5 2 1.000000-0.001622 0.874952 0.095553 0.021259 0.026216 0.020902-0.007680 0.006674-0.004769 0111111111 O2b 5 2 1.000000-0.321774 0.861519 0.103855 0.017859 0.021053 0.019007-0.000538 0.002577 0.000283 0111111111 O1c 5 2 1.000000-0.026299 0.561958 0.214500 0.040005 0.021341 0.024045 0.005641-0.000410 0.007816 0111111111 O2c 5 2 1.000000-0.117623 0.702959 0.163287 0.025795 0.018291 0.026813 0.004301-0.000381 0.005403 0111111111 O3c 5 2 1.000000-0.023818 0.549322 0.131889 0.052051 0.032642 0.029311 0.010353 0.005159-0.002187 0111111111 O4c 5 2 0.883069 0.703855 0.373394 0.059259 0.038155 0.034088 0.034892 0.000318 0.011597 0.005310 0111111111 O5c 5 2 0.883069 0.561042 0.265315 0.097804 0.038557 0.034411 0.060902-0.013652-0.009541 0.026276 0111111111 O6c 5 2 0.883069 0.563474 0.453230 0.107757 0.086392 0.041437 0.031616 0.012042 0.026324-0.001038 0111111111 N1a 4 2 1.000000 0.165207 0.336286 0.206538 0.017729 0.021058 0.019320 0.002956 0.000230-0.005893 0111111111 N2a 4 2 1.000000-0.106357 0.271345 0.224131 0.018676 0.020552 0.027849-0.000435 0.000722-0.004345 0111111111 N1b 4 2 1.000000-0.072366 0.700136 0.020993 0.020111 0.019644 0.020552-0.001141 0.000662-0.002797 0111111111 N2b 4 2 1.000000-0.331877 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0.000000 0.000000 H2c11b 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H1n2a 0.000000 0.002673 0.000848 0.000919 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H1n2b 0.000000 0.002523 0.001288 0.000786 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H1o2a 0.000000 0.002447 0.002189 0.000188 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H1o2b 0.000000 0.002412 0.001969 0.000439 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 O7c 0.009551 0.002525 0.001922 0.000851 0.001618 0.001152 0.001419 0.001039 0.001209 0.001076 O8c 0.009551 0.003269 0.001603 0.000934 0.002242 0.001082 0.001417 0.001284 0.001411 0.000967 O9c 0.009551 0.002583 0.001897 0.000825 0.001177 0.001411 0.000899 0.000914 0.000790 0.000940 -------------------------- Saved points ---------------------------- 0 -------------------------- Fourier maxima -------------------------- 1 1 1 max1 1 1 1.000000 0.953660 0.150683 0.897564 000 0 0 0 0.22 0.19 max2 1 1 1.000000 0.083125 0.218045 0.417175 000 0 0 0 0.48 0.17 max3 1 1 1.000000 0.042557 0.138720 0.909495 000 0 0 0 0.20 0.17 max4 1 1 1.000000 0.268844 0.162712 0.912653 000 0 0 0 0.22 0.16 max5 1 1 1.000000 0.945024 0.092356 0.796566 000 0 0 0 0.19 0.16 max6 1 1 1.000000 0.767623 0.036905 0.006596 000 0 0 0 0.24 0.15 max7 1 1 1.000000 0.530797 0.184049 0.608760 000 0 0 0 0.22 0.15 max8 1 1 1.000000 0.306185 0.044352 0.716307 000 0 0 0 0.25 0.14 max9 1 1 1.000000 0.709340 0.057013 0.631662 000 0 0 0 0.28 0.14 max10 1 1 1.000000 0.263193 0.031424 0.795564 000 0 0 0 0.20 0.14 -------------------------- Fourier minima -------------------------- 1 1 1 min1 1 1 1.000000 0.210222 0.200806 0.924765 000 0 0 0 0.39 0.26 min2 1 1 1.000000 0.133667 0.233561 0.903963 000 0 0 0 0.27 0.19 min3 1 1 1.000000 0.091658 0.183192 0.779952 000 0 0 0 0.40 0.15 min4 1 1 1.000000 0.787769 0.099185 0.960813 000 0 0 0 0.18 0.13 min5 1 1 1.000000 0.038776 0.099074 0.779202 000 0 0 0 0.23 0.12 min6 1 1 1.000000 0.171273 0.219584 0.428496 000 0 0 0 0.21 0.11 min7 1 1 1.000000 0.876376 0.043749 0.973096 000 0 0 0 0.14 0.11 min8 1 1 1.000000 0.753110 0.183003 0.706027 000 0 0 0 0.20 0.10 min9 1 1 1.000000 0.740296 0.053089 0.950211 000 0 0 0 0.15 0.10 min10 1 1 1.000000 0.068494 0.110242 0.508415 000 0 0 0 0.15 0.10 ------------------------------------------------------------------------ # # .m50 # Version Jana2006 title cell 8.9894 11.4187 26.2615 90 99.8189 90 esdcell 0.0002 0.0003 0.0007 0 0.0019 0 spgroup P21/c 14 22 lattice P symmetry x y z symmetry -x y+1/2 -z+1/2 symmetry -x -y -z symmetry x -y+1/2 z+1/2 unitsnumb 4 chemform C22 H30 Cu2 N6 O10 atlist C22 H30 Cu2 N6 O10 formtab -62 atom C atradius 0.77 color 128073041 atom H atradius 0.46 color 255204204 atom Cu atradius 1.28 color 34071220 atom N atradius 0.74 color 176185230 atom O atradius 0.74 color 254003000 roundmethod 1 end ******************************************************************************* contour end contour dist angles 1 dhamin 120 expdmax 10 end dist fourier maptype 6 end fourier refine fsquare 1 unstab 0.02 restric N2c 12 N3c restric O4c 12 O9c restric O5c 12 O7c restric O6c 12 O8c equation : ai[O4c]=ai[N2c] equation : ai[O5c]=ai[N2c] equation : ai[O6c]=ai[N2c] equation : ai[N3c]=1-ai[N2c] equation : ai[O7c]=ai[N3c] equation : ai[O8c]=ai[N3c] equation : ai[O9c]=ai[N3c] distfix 0.82 0.001 H1o2a O2a; H1o2b O2b; distfix 0.86 0.001 H1n2a N2a; H1n2b N2b; distfix = 0.001 N2c O4c; N2c O5c; N2c O6c; N3c O7c; N3c O8c; N3c O9c; anglefix 120 1 O4c N2c O5c; O4c N2c O6c; O5c N2c O6c; anglefix 120 1 O7c N3c O8c; O7c N3c O9c; O8c N3c O9c; keep hydro triang C3a 2 1 C2a C4a 0.96 H1c3a keep ADP riding C3a 1.2 H1c3a keep hydro triang C4a 2 1 C5a C3a 0.96 H1c4a keep ADP riding C4a 1.2 H1c4a keep hydro triang C5a 2 1 C6a C4a 0.96 H1c5a keep ADP riding C5a 1.2 H1c5a keep hydro triang C6a 2 1 C5a C1a 0.96 H1c6a keep ADP riding C6a 1.2 H1c6a keep hydro triang C7a 2 1 N1a C2a 0.96 H1c7a keep ADP riding C7a 1.2 H1c7a keep hydro tetrahed C8a 2 2 N1a C9a 0.96 H1c8a H2c8a keep ADP riding C8a 1.2 H1c8a H2c8a keep hydro tetrahed C9a 2 2 N2a C8a 0.96 H1c9a H2c9a keep ADP riding C9a 1.2 H1c9a H2c9a keep hydro tetrahed C10a 2 2 N2a C11a 0.96 H1c10a H2c10a keep ADP riding C10a 1.2 H1c10a H2c10a keep hydro tetrahed C11a 2 2 O2a C10a 0.96 H1c11a H2c11a keep ADP riding C11a 1.2 H1c11a H2c11a keep hydro triang C3b 2 1 C2b C4b 0.96 H1c3b keep ADP riding C3b 1.2 H1c3b keep hydro triang C4b 2 1 C3b C5b 0.96 H1c4b keep ADP riding C4b 1.2 H1c4b keep hydro triang C5b 2 1 C6b C4b 0.96 H1c5b keep ADP riding C5b 1.2 H1c5b keep hydro triang C6b 2 1 C5b C1b 0.96 H1c6b keep ADP riding C6b 1.2 H1c6b keep hydro triang C7b 2 1 N1b C2b 0.96 H1c7b keep ADP riding C7b 1.2 H1c7b keep hydro tetrahed C8b 2 2 N1b C9b 0.96 H1c8b H2c8b keep ADP riding C8b 1.2 H1c8b H2c8b keep hydro tetrahed C9b 2 2 N2b C8b 0.96 H1c9b H2c9b keep ADP riding C9b 1.2 H1c9b H2c9b keep hydro tetrahed C10b 2 2 N2b C11b 0.96 H1c10b H2c10b keep ADP riding C10b 1.2 H1c10b H2c10b keep hydro tetrahed C11b 2 2 O2b C10b 0.96 H1c11b H2c11b keep ADP riding C11b 1.2 H1c11b H2c11b keep ADP riding N2a 1.2 H1n2a keep ADP riding N2b 1.2 H1n2b keep ADP riding O2a 1.2 H1o2a keep ADP riding O2b 1.2 H1o2b end refine ; loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 1 0 0 40993.90 41836.10 176.54 o 2 0 0 9494.28 9907.48 123.04 o 3 0 0 2.46 7.43 4.82 < 4 0 0 2609.13 2469.60 56.77 o 5 0 0 4181.32 4172.83 138.92 o 6 0 0 19.42 44.86 5.08 o 7 0 0 74.16 78.89 5.91 o 8 0 0 5938.91 6069.72 77.50 o 9 0 0 320.23 302.44 14.22 o 10 0 0 1160.24 1112.72 43.16 o 1 1 0 21055.30 21459.60 83.12 o 2 1 0 11269.70 11284.80 69.73 o 3 1 0 7020.70 7182.85 68.74 o 4 1 0 633.32 640.97 33.44 o 5 1 0 2079.97 2117.53 57.23 o 6 1 0 23.19 19.51 3.81 o 7 1 0 9719.93 9517.90 45.74 o 8 1 0 2088.23 2205.91 30.05 o 9 1 0 25.76 28.83 5.38 o 10 1 0 1593.35 1539.38 33.65 o 0 2 0 11259.70 10338.50 107.84 o 1 2 0 15427.30 15909.70 75.58 o 2 2 0 1562.48 1860.45 36.24 o 3 2 0 19779.10 19776.40 136.77 o 4 2 0 8283.93 8382.25 174.93 o 5 2 0 1004.22 1048.75 40.48 o 6 2 0 79.05 60.51 5.80 o 7 2 0 432.28 411.89 13.06 o 8 2 0 78.20 81.64 6.37 o 9 2 0 522.78 567.22 16.52 o 10 2 0 787.57 716.73 18.67 o 1 3 0 12.09 26.12 5.14 o 2 3 0 4115.47 4178.92 60.62 o 3 3 0 158.56 244.95 17.17 o 4 3 0 15199.10 14713.40 235.65 o 5 3 0 7507.85 7184.20 49.88 o 6 3 0 3553.30 3729.77 28.45 o 7 3 0 238.12 254.20 9.56 o 8 3 0 27.12 28.68 5.62 o 9 3 0 1.44 4.21 4.17 < 10 3 0 681.77 742.44 22.25 o 0 4 0 4121.86 3754.27 96.94 o 1 4 0 1234.20 1364.96 31.03 o 2 4 0 248.76 167.54 14.06 o 3 4 0 21171.90 20917.70 164.14 o 4 4 0 2327.62 2389.42 56.09 o 5 4 0 802.45 736.50 14.97 o 6 4 0 5414.12 5447.65 37.57 o 7 4 0 1756.13 1713.74 29.76 o 8 4 0 1013.56 998.80 22.29 o 9 4 0 50.57 53.16 6.10 o 10 4 0 12.33 8.82 6.32 < 1 5 0 2338.75 2265.31 45.49 o 2 5 0 2538.24 2745.15 62.47 o 3 5 0 11299.80 10805.40 134.45 o 4 5 0 7246.52 7003.09 46.03 o 5 5 0 5632.92 5240.17 36.91 o 6 5 0 41.78 60.68 6.63 o 7 5 0 469.66 479.63 16.76 o 8 5 0 1263.65 1256.57 24.96 o 9 5 0 1335.10 1352.99 27.64 o 0 6 0 5536.46 5778.10 154.71 o 1 6 0 3486.44 3662.56 87.76 o 2 6 0 1580.34 1857.02 90.14 o 3 6 0 5431.36 5299.42 39.95 o 4 6 0 55.25 46.54 4.33 o 5 6 0 180.87 162.38 7.09 o 6 6 0 5.63 5.74 4.28 < 7 6 0 2458.67 2469.44 36.26 o 8 6 0 7.16 2.39 5.03 < 9 6 0 71.89 67.74 6.10 o 1 7 0 308.48 238.98 12.41 o 2 7 0 155.61 131.57 8.20 o 3 7 0 0.50 10.40 4.12 < 4 7 0 1904.21 1940.42 21.67 o 5 7 0 81.27 71.47 5.46 o 6 7 0 495.23 508.39 13.90 o 7 7 0 657.55 721.06 19.52 o 8 7 0 1041.85 980.80 23.70 o 9 7 0 163.77 168.70 14.41 o 0 8 0 13365.70 13498.30 117.83 o 1 8 0 1400.74 1419.02 26.89 o 2 8 0 4.78 0.56 3.82 < 3 8 0 360.27 356.81 14.32 o 4 8 0 1663.24 1668.96 23.41 o 5 8 0 100.13 111.47 7.19 o 6 8 0 496.00 537.91 15.16 o 7 8 0 5.83 1.15 5.82 < 8 8 0 1663.85 1702.18 28.16 o 1 9 0 1900.14 1989.33 40.30 o 2 9 0 1844.28 1776.69 38.07 o 3 9 0 779.82 751.76 19.84 o 4 9 0 853.30 871.60 17.26 o 5 9 0 74.45 65.27 7.52 o 6 9 0 467.87 445.56 15.19 o 7 9 0 842.12 918.43 28.27 o 0 10 0 3690.66 3674.16 58.10 o 1 10 0 766.39 790.21 22.95 o 2 10 0 226.81 189.91 11.79 o 3 10 0 2.91 2.23 5.30 < 4 10 0 7.69 4.68 6.50 < 5 10 0 228.22 216.60 10.60 o 6 10 0 102.00 96.41 7.25 o 7 10 0 0.04 12.35 5.71 < 1 11 0 0.87 1.52 5.27 < 2 11 0 681.25 738.85 22.17 o 3 11 0 522.93 525.76 22.87 o 4 11 0 0.29 7.52 5.29 < 5 11 0 812.82 763.62 17.04 o 6 11 0 23.96 32.59 5.81 o 0 12 0 130.30 129.07 11.12 o 1 12 0 266.56 303.30 11.87 o 2 12 0 1500.99 1496.94 35.10 o 3 12 0 474.74 477.09 15.68 o 4 12 0 580.64 539.59 15.80 o 5 12 0 56.01 53.44 6.71 o 1 13 0 5.05 2.18 4.61 < 2 13 0 163.40 167.09 11.17 o 3 13 0 152.70 163.09 10.39 o -10 1 1 1037.10 963.20 26.68 o -9 1 1 118.68 99.13 9.27 o -8 1 1 14.89 9.92 3.94 < -7 1 1 663.40 724.84 14.07 o -6 1 1 825.59 849.69 13.15 o -5 1 1 45.91 76.07 10.18 o -4 1 1 12.18 19.48 7.24 < -3 1 1 7.37 25.19 5.30 o -2 1 1 1218.34 1133.43 21.20 o -1 1 1 487.29 472.38 11.39 o 0 1 1 408.70 348.63 10.45 o 1 1 1 2714.65 2989.77 26.90 o 2 1 1 5957.87 6376.78 55.52 o 3 1 1 2644.09 2748.22 44.53 o 4 1 1 1250.43 1221.73 40.55 o 5 1 1 33.57 62.14 10.66 o 6 1 1 140.29 181.07 5.94 o 7 1 1 326.38 382.75 9.59 o 8 1 1 364.27 375.53 12.67 o 9 1 1 360.74 343.39 13.17 o 10 1 1 7.49 7.75 5.82 < -10 2 1 390.84 397.85 14.20 o -9 2 1 1007.95 1033.23 22.18 o -8 2 1 2.65 12.87 4.92 < -7 2 1 2059.36 1966.30 27.61 o -6 2 1 2463.11 2448.85 25.96 o -5 2 1 1169.47 1143.88 42.97 o -4 2 1 600.35 495.89 43.11 o -3 2 1 15.34 32.95 5.78 o -2 2 1 25484.80 26268.30 132.81 o -1 2 1 8044.61 7898.45 54.20 o 0 2 1 33669.80 33628.20 99.40 o 1 2 1 24954.40 25626.60 96.15 o 2 2 1 1284.93 1395.51 32.43 o 3 2 1 3147.73 3503.23 59.85 o 4 2 1 606.91 688.77 50.66 o 5 2 1 1662.93 1677.37 22.90 o 6 2 1 1521.16 1421.16 19.89 o 7 2 1 4154.00 4182.65 36.06 o 8 2 1 2165.26 2309.38 27.77 o 9 2 1 829.44 846.27 17.39 o 10 2 1 0.72 5.30 4.78 < -10 3 1 522.50 496.56 18.96 o -9 3 1 959.71 869.59 20.31 o -8 3 1 648.44 696.29 17.96 o -7 3 1 1393.26 1377.25 23.97 o -6 3 1 738.03 707.94 15.89 o -5 3 1 49.46 62.99 4.58 o -4 3 1 1489.37 1443.68 74.75 o -3 3 1 4520.61 4039.79 65.43 o -2 3 1 1520.22 1415.72 35.27 o -1 3 1 6457.13 6635.19 73.08 o 0 3 1 2407.71 2528.71 34.07 o 1 3 1 34.91 35.64 5.55 o 2 3 1 21897.60 22662.90 117.32 o 3 3 1 31.65 27.67 7.50 o 4 3 1 3726.00 3791.14 119.08 o 5 3 1 3564.89 3371.82 28.18 o 6 3 1 1358.42 1309.07 18.09 o 7 3 1 3003.91 2951.80 28.32 o 8 3 1 2782.45 2912.15 31.13 o 9 3 1 106.75 129.04 8.18 o 10 3 1 1444.86 1422.76 24.41 o -10 4 1 343.05 354.32 20.49 o -9 4 1 374.84 360.51 13.24 o -8 4 1 60.91 60.48 7.25 o -7 4 1 454.24 439.67 13.99 o -6 4 1 196.12 188.96 8.53 o -5 4 1 101.19 102.73 6.98 o -4 4 1 438.08 437.76 24.49 o -3 4 1 319.84 327.97 32.88 o -2 4 1 7889.85 7746.78 130.61 o -1 4 1 2954.11 2488.01 51.15 o 0 4 1 10116.90 9757.33 88.24 o 1 4 1 704.17 819.24 21.36 o 2 4 1 1300.71 1628.48 31.27 o 3 4 1 339.39 389.20 18.96 o 4 4 1 2217.37 2473.80 56.98 o 5 4 1 696.35 761.02 12.36 o 6 4 1 5.01 15.79 3.66 o 7 4 1 64.00 71.58 6.52 o 8 4 1 1489.89 1440.63 24.02 o 9 4 1 313.97 331.70 14.33 o 10 4 1 247.40 252.04 17.63 o -9 5 1 769.76 782.71 16.26 o -8 5 1 342.15 351.96 13.86 o -7 5 1 276.29 272.81 11.62 o -6 5 1 1746.30 1765.29 25.90 o -5 5 1 1825.48 1803.75 24.07 o -4 5 1 102.10 133.79 6.98 o -3 5 1 1151.55 1103.28 59.43 o -2 5 1 1864.44 1982.66 69.83 o -1 5 1 413.89 419.75 24.18 o 0 5 1 14.97 56.19 12.88 o 1 5 1 600.64 763.91 26.13 o 2 5 1 9511.59 10856.30 89.99 o 3 5 1 163.37 227.62 16.40 o 4 5 1 1013.13 857.15 13.74 o 5 5 1 106.37 105.04 5.63 o 6 5 1 1759.65 1787.83 24.65 o 7 5 1 2428.00 2565.66 36.69 o 8 5 1 188.83 172.82 9.94 o 9 5 1 726.94 713.71 19.57 o -9 6 1 813.68 827.85 17.86 o -8 6 1 275.55 303.50 12.57 o -7 6 1 991.44 1092.71 21.78 o -6 6 1 6.49 7.32 4.42 < -5 6 1 134.97 131.84 6.37 o -4 6 1 5427.25 5391.92 39.02 o -3 6 1 5707.81 5734.66 47.26 o -2 6 1 729.50 844.19 61.83 o -1 6 1 2258.95 2580.39 74.29 o 0 6 1 4158.07 4220.31 94.16 o 1 6 1 14908.50 15274.60 178.45 o 2 6 1 6891.15 6670.75 119.56 o 3 6 1 1687.05 1498.35 21.39 o 4 6 1 318.09 332.11 8.42 o 5 6 1 2698.59 2712.39 26.59 o 6 6 1 331.72 368.13 11.91 o 7 6 1 60.52 59.97 7.59 o 8 6 1 16.16 19.52 5.81 o 9 6 1 734.40 687.39 15.29 o -9 7 1 558.65 621.56 25.85 o -8 7 1 271.16 294.68 13.87 o -7 7 1 385.41 395.21 14.71 o -6 7 1 1137.26 1206.24 20.75 o -5 7 1 2228.68 2224.01 24.58 o -4 7 1 6650.95 6565.12 41.97 o -3 7 1 3794.88 3728.99 36.43 o -2 7 1 101.05 108.19 7.16 o -1 7 1 32.95 38.40 8.32 o 0 7 1 247.09 415.51 15.79 o 1 7 1 1793.06 1995.87 33.88 o 2 7 1 10331.90 10344.00 66.66 o 3 7 1 10585.60 10762.40 61.83 o 4 7 1 15092.60 14994.50 56.63 o 5 7 1 97.48 111.98 7.28 o 6 7 1 191.54 158.05 8.28 o 7 7 1 7.42 7.44 6.00 < 8 7 1 58.15 52.37 6.78 o 9 7 1 14.01 17.32 7.11 < -8 8 1 696.16 678.66 18.63 o -7 8 1 1578.18 1675.07 32.26 o -6 8 1 198.36 204.94 10.10 o -5 8 1 1749.15 1843.39 22.80 o -4 8 1 850.72 867.93 16.77 o -3 8 1 928.29 903.52 20.37 o -2 8 1 42.48 36.30 6.10 o -1 8 1 116.53 130.70 9.08 o 0 8 1 362.31 374.18 14.96 o 1 8 1 30.50 20.50 5.32 o 2 8 1 307.97 258.62 12.10 o 3 8 1 424.38 426.54 15.61 o 4 8 1 631.58 724.57 15.69 o 5 8 1 65.83 79.44 6.87 o 6 8 1 386.72 427.53 13.62 o 7 8 1 103.69 111.71 9.85 o 8 8 1 16.24 28.91 5.80 o -8 9 1 485.89 541.38 24.34 o -7 9 1 0.78 -0.08 5.96 < -6 9 1 409.61 424.63 14.80 o -5 9 1 2032.56 2193.90 33.58 o -4 9 1 534.28 555.29 13.99 o -3 9 1 116.97 126.57 9.21 o -2 9 1 6.76 8.42 5.91 < -1 9 1 199.27 198.70 13.68 o 0 9 1 726.50 689.53 20.19 o 1 9 1 483.11 436.45 16.55 o 2 9 1 298.94 297.45 11.96 o 3 9 1 2047.88 2172.93 33.23 o 4 9 1 21.21 23.83 5.85 o 5 9 1 244.40 267.16 14.71 o 6 9 1 2332.00 2400.53 39.89 o 7 9 1 446.63 499.01 20.92 o -7 10 1 121.52 131.51 10.32 o -6 10 1 0.98 2.48 4.22 < -5 10 1 357.65 338.05 15.20 o -4 10 1 1461.67 1508.87 27.35 o -3 10 1 1932.66 1861.62 30.62 o -2 10 1 1711.62 1690.09 32.98 o -1 10 1 5487.39 5488.33 59.20 o 0 10 1 2715.36 2721.15 35.58 o 1 10 1 47.34 44.56 6.79 o 2 10 1 17.64 35.33 6.37 o 3 10 1 66.63 59.60 6.92 o 4 10 1 9.15 9.75 5.90 < 5 10 1 137.41 145.70 9.02 o 6 10 1 144.38 119.20 9.08 o 7 10 1 456.11 487.56 17.79 o -6 11 1 2.13 -3.95 5.25 < -5 11 1 113.74 96.54 6.98 o -4 11 1 692.43 625.66 19.21 o -3 11 1 1528.52 1586.07 31.86 o -2 11 1 3797.15 3905.94 42.98 o -1 11 1 11.61 9.14 5.17 < 0 11 1 150.59 146.82 13.15 o 1 11 1 1820.31 1791.39 41.91 o 2 11 1 679.59 701.33 21.67 o 3 11 1 4.21 3.16 6.83 < 4 11 1 37.05 31.74 4.95 o 5 11 1 565.39 622.28 18.73 o 6 11 1 1793.84 1789.12 49.42 o -5 12 1 238.69 229.34 12.05 o -4 12 1 428.21 430.88 14.30 o -3 12 1 206.44 195.30 10.47 o -2 12 1 902.11 883.52 22.14 o -1 12 1 4552.38 4758.81 51.86 o 0 12 1 1805.31 1789.42 31.35 o 1 12 1 10.57 12.61 5.70 < 2 12 1 130.04 155.27 12.72 o 3 12 1 711.57 706.21 23.97 o 4 12 1 60.29 60.24 6.52 o 5 12 1 15.71 20.65 7.28 < -3 13 1 1041.05 1003.30 23.72 o -2 13 1 256.35 242.56 12.98 o -1 13 1 21.18 16.63 5.68 < 0 13 1 982.20 965.48 24.90 o 1 13 1 753.41 718.12 21.42 o 2 13 1 60.59 56.76 7.41 o 3 13 1 22.05 21.50 5.16 o -10 0 2 251.98 224.02 21.49 o -9 0 2 207.89 187.34 11.75 o -8 0 2 154.24 144.70 8.96 o -7 0 2 794.99 826.98 20.04 o -6 0 2 17296.60 16415.60 90.24 o -5 0 2 438.45 277.36 36.63 o -4 0 2 76.02 101.80 20.27 o -3 0 2 19001.80 18378.30 119.58 o -2 0 2 11598.50 11871.70 134.39 o -1 0 2 60580.60 60010.40 219.15 o 0 0 2 6732.20 7059.90 67.23 o 2 0 2 19824.20 20982.70 131.26 o 3 0 2 5896.43 6139.62 84.75 o 4 0 2 2745.16 2550.91 63.35 o 5 0 2 37.60 44.29 10.18 o 6 0 2 11769.40 11178.10 57.86 o 7 0 2 18725.80 18790.80 92.04 o 8 0 2 1867.27 1936.01 43.31 o 9 0 2 386.94 389.57 20.14 o 10 0 2 1720.70 1561.76 32.08 o -10 1 2 452.70 436.15 15.69 o -9 1 2 42.16 32.42 5.51 o -8 1 2 134.87 168.41 8.26 o -7 1 2 129.09 116.70 8.11 o -6 1 2 419.69 387.96 10.02 o -5 1 2 7909.69 7827.87 109.88 o -4 1 2 4902.73 4367.33 86.16 o -3 1 2 12488.20 11805.30 118.82 o -2 1 2 1.10 6.46 4.71 < -1 1 2 19739.00 20704.20 73.96 o 0 1 2 15645.10 16062.10 112.29 o 1 1 2 5504.11 6536.97 42.59 o 2 1 2 61.02 64.35 5.75 o 3 1 2 1257.66 1335.57 26.87 o 4 1 2 2348.68 2293.91 47.91 o 5 1 2 8534.53 8237.44 83.04 o 6 1 2 13243.30 12502.00 54.85 o 7 1 2 155.77 150.99 6.76 o 8 1 2 22.39 27.91 6.03 o 9 1 2 470.72 497.14 15.45 o 10 1 2 350.02 335.87 15.68 o -10 2 2 0.28 -4.98 6.31 < -9 2 2 114.02 132.15 9.19 o -8 2 2 237.40 257.30 11.44 o -7 2 2 382.07 441.02 15.23 o -6 2 2 10849.00 10911.10 54.36 o -5 2 2 9176.92 8813.77 117.96 o -4 2 2 4077.26 3809.79 81.49 o -3 2 2 1961.71 1938.93 49.12 o -2 2 2 95.20 34.17 6.45 o -1 2 2 23750.70 23625.30 123.42 o 0 2 2 6350.67 6697.54 64.42 o 1 2 2 3712.99 3659.91 37.16 o 2 2 2 21751.40 22639.40 105.35 o 3 2 2 910.52 1176.44 27.07 o 4 2 2 1298.88 1191.60 41.58 o 5 2 2 341.10 332.73 9.64 o 6 2 2 9.49 8.52 3.32 < 7 2 2 711.43 718.14 14.34 o 8 2 2 313.78 298.22 10.48 o 9 2 2 16.22 34.97 4.75 o 10 2 2 2651.71 2686.40 41.86 o -10 3 2 1653.85 1701.38 34.96 o -9 3 2 1092.58 1202.44 24.33 o -8 3 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2 29 10.22 15.94 4.50 o -2 2 29 42.28 39.23 5.41 o -1 2 29 392.75 417.56 13.95 o 0 2 29 1821.91 1713.95 25.97 o 1 2 29 473.59 450.57 16.39 o 2 2 29 163.35 142.38 12.72 o -5 3 29 384.71 338.39 18.67 o -4 3 29 700.54 699.29 19.81 o -3 3 29 732.57 728.65 17.37 o -2 3 29 98.39 106.10 7.39 o -1 3 29 236.30 218.88 10.11 o 0 3 29 418.12 388.91 15.33 o 1 3 29 252.52 266.92 12.45 o -4 4 29 121.61 137.51 8.59 o -3 4 29 209.25 194.54 10.62 o -2 4 29 35.57 22.59 5.13 o -1 4 29 32.98 26.74 8.42 o 0 4 29 617.97 557.71 25.36 o -3 5 29 107.63 92.05 10.40 o -2 5 29 156.52 139.47 12.65 o -1 5 29 77.46 105.12 11.36 o -4 0 30 285.52 307.62 19.21 o -3 0 30 178.16 171.25 15.66 o -2 0 30 7.54 8.04 7.30 < -1 0 30 362.52 375.41 22.37 o 0 0 30 1250.10 1216.11 25.92 o 1 0 30 2181.15 2159.50 46.91 o -4 1 30 58.88 52.89 6.42 o -3 1 30 31.16 27.00 4.32 o -2 1 30 62.48 60.43 5.78 o -1 1 30 97.05 99.59 7.04 o 0 1 30 330.92 366.81 11.51 o 1 1 30 12.75 0.95 4.41 < -4 2 30 852.59 833.35 30.03 o -3 2 30 358.17 341.23 11.61 o -2 2 30 7.88 13.64 4.12 o -1 2 30 197.34 167.28 8.49 o 0 2 30 49.99 46.38 8.38 o -3 3 30 1859.10 1869.50 25.07 o -2 3 30 479.23 455.89 12.88 o -1 3 30 214.41 207.66 15.59 o 0 3 30 331.76 330.67 18.69 o -2 4 30 1.63 8.24 5.28 < -3 1 31 30.79 38.55 5.45 o -2 1 31 5.32 7.19 4.05 < -1 1 31 268.56 307.46 18.43 o -2 2 31 0.07 -2.11 4.48 <