#------------------------------------------------------------------------------ #$Date: 2017-04-28 08:08:23 +0300 (Fri, 28 Apr 2017) $ #$Revision: 195844 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/81/7228146.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_7228146 loop_ _publ_author_name 'Shi, Lu-Lu' 'Zheng, Tian-Rui' 'Li, Min' 'Qian, Lin-Lu' 'Li, Bao-Long' 'Li, Hai-Yan' _publ_section_title ; A series of five-coordinated copper coordination polymers for efficient degradation of organic dyes under visible light irradiation ; _journal_issue 38 _journal_name_full 'RSC Adv.' _journal_page_first 23432 _journal_paper_doi 10.1039/C7RA03268D _journal_volume 7 _journal_year 2017 _chemical_formula_moiety 'C36 H32 Cu2 N4 O8,H2O' _chemical_formula_sum 'C36 H34 Cu2 N4 O9' _chemical_formula_weight 793.75 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2017-03-16 _audit_creation_method ; Olex2 1.2-alpha (compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261) ; _audit_update_record ; 2017-03-16 deposited with the CCDC. 2017-04-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.520(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.2620(3) _cell_length_b 21.1852(5) _cell_length_c 15.7859(4) _cell_measurement_reflns_used 3184 _cell_measurement_temperature 223.00(10) _cell_measurement_theta_max 73.1890 _cell_measurement_theta_min 4.8150 _cell_volume 3402.38(16) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 223.00(10) _diffrn_detector_area_resol_mean 10.4471 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -28.00 36.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -40.2343 37.0000 -180.0000 64 #__ type_ start__ end____ width___ exp.time_ 2 omega -42.00 15.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -40.2343 37.0000 -30.0000 57 #__ type_ start__ end____ width___ exp.time_ 3 omega 11.00 108.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.2343 57.0000 -90.0000 97 #__ type_ start__ end____ width___ exp.time_ 4 omega -4.00 37.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.2343 -99.0000 120.0000 41 #__ type_ start__ end____ width___ exp.time_ 5 omega 86.00 165.00 1.0000 13.3300 omega____ theta____ kappa____ phi______ frames - 105.9522 45.0000 -30.0000 79 #__ type_ start__ end____ width___ exp.time_ 6 omega 29.00 57.00 1.0000 13.3300 omega____ theta____ kappa____ phi______ frames - 105.9522 -30.0000 -30.0000 28 #__ type_ start__ end____ width___ exp.time_ 7 omega 104.00 164.00 1.0000 13.3300 omega____ theta____ kappa____ phi______ frames - 105.9522 111.0000 -180.0000 60 #__ type_ start__ end____ width___ exp.time_ 8 omega 29.00 138.00 1.0000 13.3300 omega____ theta____ kappa____ phi______ frames - 105.9522 -77.0000 -180.0000 109 #__ type_ start__ end____ width___ exp.time_ 9 omega 31.00 87.00 1.0000 13.3300 omega____ theta____ kappa____ phi______ frames - 105.9522 -30.0000 150.0000 56 #__ type_ start__ end____ width___ exp.time_ 10 omega 75.00 149.00 1.0000 13.3300 omega____ theta____ kappa____ phi______ frames - 105.9522 30.0000 -60.0000 74 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0023319000 _diffrn_orient_matrix_UB_12 0.0266814000 _diffrn_orient_matrix_UB_13 0.0909157000 _diffrn_orient_matrix_UB_21 0.0620035000 _diffrn_orient_matrix_UB_22 0.0615535000 _diffrn_orient_matrix_UB_23 -0.0280071000 _diffrn_orient_matrix_UB_31 -0.1380605000 _diffrn_orient_matrix_UB_32 0.0281854000 _diffrn_orient_matrix_UB_33 -0.0252303000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 6089 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 66.601 _diffrn_reflns_theta_max 66.601 _diffrn_reflns_theta_min 4.174 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.072 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.56962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.550 _exptl_crystal_description block _exptl_crystal_F_000 1632 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.763 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 2999 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0460 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+2.9813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1238 _refine_ls_wR_factor_ref 0.1299 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2610 _reflns_number_total 2999 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL g160312c_a.res in C2/c g160312c.res created by SHELXL-2016/6 at 16:37:12 on 16-Mar-2017 REM Old TITL g160312c in C2/c #15 REM SHELXT solution in C2/c REM R1 0.136, Rweak 0.062, Alpha 0.060, Orientation as input REM Formula found by SHELXT: C20 O4 Cu CELL 1.54184 10.262001 21.185248 15.785851 90 97.5203 90 ZERR 4 0.00026 0.000492 0.000418 0 0.0025 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cu N O UNIT 144 136 8 16 36 EQIV $1 0.5-X,1.5-Y,1-Z DFIX 0.93 H5' C5' DFIX 0.93 H4' C4' L.S. 35 PLAN 20 HTAB C4 N1'_$1 HTAB C4 N1_$1 HTAB C8' O1 BOND BOND $H MORE -1 CONF HTAB fmap 2 acta SHEL 999 0.84 REM REM REM WGHT 0.084800 2.981300 FVAR 0.24507 CU1 3 0.420379 0.547525 0.517175 11.00000 0.02017 0.02517 = 0.02811 -0.00024 0.00443 -0.00032 O1 5 0.538213 0.545953 0.627074 11.00000 0.04289 0.06092 = 0.02844 -0.00788 -0.00578 0.00716 O2 5 0.666697 0.465653 0.602120 11.00000 0.02958 0.06873 = 0.03890 -0.00397 -0.01051 0.00725 O3 5 0.551880 0.600116 0.470992 11.00000 0.03044 0.02971 = 0.05568 0.00384 0.01543 -0.00267 O4 5 0.687401 0.521802 0.446673 11.00000 0.04187 0.03005 = 0.06440 0.00059 0.02893 -0.00437 C1 1 0.067574 0.761464 0.678692 11.00000 0.04296 0.03709 = 0.03515 0.00245 0.01099 0.00760 C2 1 0.033897 0.818115 0.714803 11.00000 0.04472 0.02976 = 0.03796 0.00392 0.01284 0.00196 AFIX 43 H2 2 0.057017 0.856207 0.691563 11.00000 -1.20000 AFIX 0 C3 1 0.033605 0.705057 0.714775 11.00000 0.05643 0.02769 = 0.04013 -0.00043 0.01170 0.00764 AFIX 43 H3 2 0.056220 0.666933 0.691391 11.00000 -1.20000 AFIX 0 C4 1 0.134415 0.764954 0.598960 11.00000 0.08425 0.04823 = 0.05209 0.01628 0.03586 0.02436 PART 1 AFIX 43 H4A 2 0.148976 0.803370 0.573278 10.60000 -1.20000 AFIX 43 PART 0 PART 2 H4B 2 0.120642 0.796575 0.557898 10.40000 -1.20000 AFIX 0 PART 0 C9 1 0.633727 0.510406 0.646886 11.00000 0.02203 0.06876 = 0.02621 -0.00195 0.00462 -0.00771 C10 1 0.713376 0.522657 0.733388 11.00000 0.02739 0.16806 = 0.03337 -0.02124 0.00011 0.00780 AFIX 23 H10A 2 0.688184 0.563720 0.753046 11.00000 -1.20000 H10B 2 0.687668 0.491584 0.773180 11.00000 -1.20000 AFIX 0 C11 1 0.861605 0.521324 0.738986 11.00000 0.02491 0.05510 = 0.02788 -0.00529 -0.00247 0.00235 C12 1 0.932699 0.521621 0.820112 11.00000 0.02924 0.05051 = 0.02716 0.00047 0.00300 0.00314 AFIX 43 H12 2 0.888432 0.521175 0.867888 11.00000 -1.20000 AFIX 0 C13 1 1.069160 0.522577 0.830703 11.00000 0.03156 0.07125 = 0.02497 0.00613 -0.00613 -0.00049 AFIX 43 H13 2 1.114920 0.524089 0.885556 11.00000 -1.20000 AFIX 0 C14 1 0.655740 0.578578 0.448927 11.00000 0.02906 0.02942 = 0.02653 -0.00223 0.00350 -0.00812 C15 1 0.755129 0.625523 0.422399 11.00000 0.03757 0.03210 = 0.05541 -0.00387 0.01826 -0.00831 AFIX 23 H15A 2 0.842610 0.608153 0.437167 11.00000 -1.20000 H15B 2 0.740027 0.630241 0.360773 11.00000 -1.20000 AFIX 0 C16 1 0.751011 0.689992 0.462543 11.00000 0.02513 0.03170 = 0.04794 -0.00147 0.00849 -0.01069 C17 1 0.749696 0.696834 0.549908 11.00000 0.04075 0.03345 = 0.04440 0.00291 0.00720 -0.01046 AFIX 43 H17 2 0.749566 0.661072 0.584063 11.00000 -1.20000 AFIX 0 C18 1 0.751426 0.744041 0.413025 11.00000 0.03864 0.03963 = 0.03950 -0.00065 0.00906 -0.01093 AFIX 43 H18 2 0.752470 0.740506 0.354396 11.00000 -1.20000 AFIX 0 PART 1 H4' 2 0.129970 0.586181 0.445418 10.60000 0.01751 H5' 2 0.009432 0.691990 0.482321 10.60000 0.02168 AFIX 56 C7' 1 0.289910 0.672437 0.586884 10.60000 0.04320 0.02852 = 0.03158 0.00448 0.01512 0.00760 N1' 4 0.278038 0.616239 0.537447 10.60000 0.02338 0.02191 = 0.03181 -0.00340 0.01189 0.00962 C4' 1 0.153950 0.617274 0.485729 10.60000 0.03986 0.02858 = 0.04474 -0.00998 0.01077 0.00968 C5' 1 0.089132 0.674110 0.503202 10.60000 0.02147 0.03991 = 0.05532 0.00098 0.01152 0.00887 N2' 4 0.173160 0.708203 0.565719 10.60000 0.03634 0.02941 = 0.04083 0.00114 0.01978 0.01424 AFIX 0 C8' 1 0.394895 0.688808 0.645503 10.60000 0.03892 0.04280 = 0.05126 -0.00246 -0.00242 0.01348 AFIX 137 H8'A 2 0.366085 0.694271 0.700496 10.60000 -1.50000 H8'B 2 0.432185 0.727579 0.628342 10.60000 -1.50000 H8'C 2 0.459993 0.656048 0.648752 10.60000 -1.50000 AFIX 56 PART 0 PART 2 C7 1 0.216241 0.656516 0.551476 10.40000 0.06587 0.06890 = 0.02919 0.02012 0.01959 -0.01443 N1 4 0.340766 0.627302 0.572737 10.40000 0.04614 0.02874 = 0.03643 -0.01083 0.01114 -0.00372 C6 1 0.419653 0.667620 0.630233 10.40000 0.03987 0.04367 = 0.08108 0.00491 0.01963 0.02449 AFIX 43 H6 2 0.505815 0.659924 0.654313 10.40000 -1.20000 AFIX 55 C5 1 0.343883 0.721753 0.644505 10.40000 0.05421 0.05485 = 0.04980 -0.00783 0.02178 0.00647 AFIX 43 H5 2 0.371709 0.755735 0.679574 10.40000 -1.20000 AFIX 55 N2 4 0.218168 0.714891 0.595831 10.40000 0.03970 0.05771 = 0.05183 0.01604 0.02040 0.01846 AFIX 0 C8 1 0.117037 0.634310 0.498893 10.40000 0.06514 0.03649 = 0.03257 -0.01602 0.00177 0.00844 AFIX 137 H8A 2 0.120742 0.589033 0.498558 10.40000 -1.50000 H8B 2 0.121934 0.649974 0.442332 10.40000 -1.50000 H8C 2 0.035933 0.647694 0.517361 10.40000 -1.50000 AFIX 0 O6 5 0.500000 0.858141 0.750000 10.25000 0.49819 0.30411 = 0.58999 0.00000 0.12922 0.00000 PART 0 PART 1 O5 5 0.355886 0.870166 0.718403 10.25000 0.20362 0.11585 = 0.10516 -0.01447 0.05691 -0.03344 HKLF 4 REM g160312c_a.res in C2/c REM R1 = 0.0460 for 2610 Fo > 4sig(Fo) and 0.0524 for all 2999 data REM 286 parameters refined using 2 restraints END WGHT 0.0848 2.9818 REM Instructions for potential hydrogen bonds HTAB C4 N1'_$1 HTAB C4 N1_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C4' O2_$2 HTAB C8' O1 REM Highest difference peak 0.763, deepest hole -0.566, 1-sigma level 0.083 Q1 1 0.2599 0.6583 0.5665 11.00000 0.05 0.76 Q2 1 0.6137 0.4514 0.5500 11.00000 0.05 0.52 Q3 1 0.4593 0.5489 0.5781 11.00000 0.05 0.40 Q4 1 0.0822 0.7815 0.5558 11.00000 0.05 0.38 Q5 1 0.2021 0.6971 0.5563 11.00000 0.05 0.37 Q6 1 0.6883 0.5291 0.7725 11.00000 0.05 0.36 Q7 1 0.2420 0.7899 0.6194 11.00000 0.05 0.36 Q8 1 0.7541 0.7202 0.4384 11.00000 0.05 0.29 Q9 1 0.7492 0.6583 0.4429 11.00000 0.05 0.29 Q10 1 0.0365 0.6994 0.7617 11.00000 0.05 0.28 Q11 1 0.8986 0.5382 0.7766 11.00000 0.05 0.28 Q12 1 0.4281 0.5125 0.5551 11.00000 0.05 0.28 Q13 1 0.3388 0.5825 0.5495 11.00000 0.05 0.27 Q14 1 0.7203 0.5500 0.7075 11.00000 0.05 0.26 Q15 1 1.1113 0.5411 0.7997 11.00000 0.05 0.26 Q16 1 0.6629 0.5098 0.6924 11.00000 0.05 0.26 Q17 1 0.7537 0.6973 0.5127 11.00000 0.05 0.25 Q18 1 0.0658 0.7803 0.7086 11.00000 0.05 0.24 Q19 1 0.6553 0.5352 0.4104 11.00000 0.05 0.24 Q20 1 0.1081 0.7647 0.6418 11.00000 0.05 0.23 REM The information below was added by Olex2. REM REM R1 = 0.0460 for 2610 Fo > 4sig(Fo) and 0.0524 for all 6601 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.76, deepest hole -0.57 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0524 REM R1_gt = 0.0460 REM wR_ref = 0.1299 REM GOOF = 1.044 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 6601 REM Reflections_gt = 2610 REM Parameters = n/a REM Hole = -0.57 REM Peak = 0.76 REM Flack = n/a ; _cod_data_source_file c7ra03268d2.cif _cod_data_source_block 4 _cod_original_cell_volume 3402.37(15) _cod_database_code 7228146 _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. ; _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances H5'-C5' 0.93 with sigma of 0.02 H4'-C4' 0.93 with sigma of 0.02 3. Others Fixed Sof: H4A(0.6) H4B(0.4) H4'(0.6) H5'(0.6) C7'(0.6) N1'(0.6) C4'(0.6) C5'(0.6) N2'(0.6) C8'(0.6) H8'A(0.6) H8'B(0.6) H8'C(0.6) C7(0.4) N1(0.4) C6(0.4) H6(0.4) C5(0.4) H5(0.4) N2(0.4) C8(0.4) H8A(0.4) H8B(0.4) H8C(0.4) O6(0.25) O5(0.25) 4.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C15(H15A,H15B) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4A), C4(H4B), C12(H12), C13(H13), C17(H17), C18(H18), C6(H6), C5(H5) 4.c Fitted pentagon refined as free rotating group: C7'(N1',C4',C5',N2'), C7(N1,C6,C5,N2) 4.d Idealised Me refined as rotating group: C8'(H8'A,H8'B,H8'C), C8(H8A,H8B,H8C) ; _shelx_shelxl_version_number 2016/6 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.42038(4) 0.54753(2) 0.51717(2) 0.02437(18) Uani 1 1 d . . . . . O1 O 0.5382(3) 0.54595(12) 0.62707(15) 0.0450(6) Uani 1 1 d . . . . . O2 O 0.6667(2) 0.46565(14) 0.60212(16) 0.0471(6) Uani 1 1 d . . . . . O3 O 0.5519(2) 0.60012(10) 0.47099(16) 0.0377(5) Uani 1 1 d . . . . . O4 O 0.6874(2) 0.52180(10) 0.44667(18) 0.0435(6) Uani 1 1 d . . . . . C1 C 0.0676(3) 0.76146(16) 0.6787(2) 0.0379(7) Uani 1 1 d . . . . . C2 C 0.0339(3) 0.81811(14) 0.7148(2) 0.0368(7) Uani 1 1 d . . . . . H2 H 0.057017 0.856207 0.691563 0.044 Uiso 1 1 calc R . . . . C3 C 0.0336(4) 0.70506(15) 0.7148(2) 0.0409(7) Uani 1 1 d . . . . . H3 H 0.056220 0.666933 0.691391 0.049 Uiso 1 1 calc R . . . . C4 C 0.1344(5) 0.7650(2) 0.5990(3) 0.0591(11) Uani 1 1 d . . . . . H4A H 0.148976 0.803370 0.573278 0.071 Uiso 0.6 1 calc R . . A 1 H4B H 0.120642 0.796575 0.557898 0.071 Uiso 0.4 1 calc R . . B 2 C9 C 0.6337(3) 0.51041(18) 0.64689(19) 0.0389(8) Uani 1 1 d . . . . . C10 C 0.7134(4) 0.5227(3) 0.7334(3) 0.0766(17) Uani 1 1 d . . . . . H10A H 0.688184 0.563720 0.753046 0.092 Uiso 1 1 calc R . . . . H10B H 0.687668 0.491584 0.773180 0.092 Uiso 1 1 calc R . . . . C11 C 0.8616(3) 0.52132(17) 0.7390(2) 0.0365(7) Uani 1 1 d . . . . . C12 C 0.9327(3) 0.52162(16) 0.8201(2) 0.0357(7) Uani 1 1 d . . . . . H12 H 0.888432 0.521175 0.867888 0.043 Uiso 1 1 calc R . . . . C13 C 1.0692(3) 0.52258(19) 0.8307(2) 0.0435(8) Uani 1 1 d . . . . . H13 H 1.114920 0.524089 0.885556 0.052 Uiso 1 1 calc R . . . . C14 C 0.6557(3) 0.57858(13) 0.44893(17) 0.0283(6) Uani 1 1 d . . . . . C15 C 0.7551(3) 0.62552(15) 0.4224(2) 0.0406(7) Uani 1 1 d . . . . . H15A H 0.842610 0.608153 0.437167 0.049 Uiso 1 1 calc R . . . . H15B H 0.740027 0.630241 0.360773 0.049 Uiso 1 1 calc R . . . . C16 C 0.7510(3) 0.68999(14) 0.4625(2) 0.0346(6) Uani 1 1 d . . . . . C17 C 0.7497(3) 0.69683(15) 0.5499(2) 0.0394(7) Uani 1 1 d . . . . . H17 H 0.749566 0.661072 0.584063 0.047 Uiso 1 1 calc R . . . . C18 C 0.7514(3) 0.74404(16) 0.4130(2) 0.0389(7) Uani 1 1 d . . . . . H18 H 0.752470 0.740506 0.354396 0.047 Uiso 1 1 calc R . . . . H4' H 0.130(5) 0.5862(18) 0.445(3) 0.018(11) Uiso 0.6 1 d D . . C 1 H5' H 0.009(3) 0.692(2) 0.482(3) 0.022(12) Uiso 0.6 1 d D . . D 1 C7' C 0.2899(3) 0.67244(16) 0.5869(2) 0.0335(11) Uani 0.6 1 d . . . E 1 N1' N 0.2780(3) 0.61624(14) 0.5374(2) 0.0250(8) Uani 0.6 1 d G . . E 1 C4' C 0.1540(4) 0.6173(2) 0.4857(3) 0.0373(17) Uani 0.6 1 d DG . . E 1 C5' C 0.0891(3) 0.6741(2) 0.5032(3) 0.0383(12) Uani 0.6 1 d DG . . E 1 N2' N 0.1732(4) 0.70820(15) 0.5657(3) 0.0342(14) Uani 0.6 1 d G . . E 1 C8' C 0.3949(8) 0.6888(4) 0.6455(5) 0.0451(18) Uani 0.6 1 d . . . E 1 H8'A H 0.366085 0.694271 0.700496 0.068 Uiso 0.6 1 calc GR . . E 1 H8'B H 0.432185 0.727579 0.628342 0.068 Uiso 0.6 1 calc GR . . E 1 H8'C H 0.459993 0.656048 0.648752 0.068 Uiso 0.6 1 calc GR . . E 1 C7 C 0.2162(6) 0.6565(3) 0.5515(4) 0.053(3) Uani 0.4 1 d . . . E 2 N1 N 0.3408(7) 0.6273(2) 0.5727(4) 0.0366(15) Uani 0.4 1 d G . . E 2 C6 C 0.4197(5) 0.6676(4) 0.6302(5) 0.054(4) Uani 0.4 1 d G . . E 2 H6 H 0.505815 0.659924 0.654313 0.065 Uiso 0.4 1 calc R . . E 2 C5 C 0.3439(8) 0.7218(3) 0.6445(5) 0.052(2) Uani 0.4 1 d G . . E 2 H5 H 0.371709 0.755735 0.679574 0.062 Uiso 0.4 1 calc R . . E 2 N2 N 0.2182(7) 0.7149(3) 0.5958(5) 0.048(3) Uani 0.4 1 d G . . E 2 C8 C 0.1170(13) 0.6343(6) 0.4989(7) 0.045(3) Uani 0.4 1 d . . . E 2 H8A H 0.120742 0.589033 0.498558 0.068 Uiso 0.4 1 calc GR . . E 2 H8B H 0.121934 0.649974 0.442332 0.068 Uiso 0.4 1 calc GR . . E 2 H8C H 0.035933 0.647694 0.517361 0.068 Uiso 0.4 1 calc GR . . E 2 O6 O 0.500000 0.858(3) 0.750000 0.46(4) Uani 0.5 2 d S T P F 2 O5 O 0.356(3) 0.8702(12) 0.7184(16) 0.138(10) Uani 0.25 1 d . . . G 1 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 Cu1 0.0202(2) 0.0252(3) 0.0281(3) -0.00024(14) 0.00443(16) -0.00032(14) O1 0.0429(13) 0.0609(15) 0.0284(11) -0.0079(10) -0.0058(10) 0.0072(11) O2 0.0296(11) 0.0687(16) 0.0389(13) -0.0040(12) -0.0105(10) 0.0073(11) O3 0.0304(10) 0.0297(10) 0.0557(13) 0.0038(9) 0.0154(9) -0.0027(9) O4 0.0419(12) 0.0300(11) 0.0644(15) 0.0006(10) 0.0289(11) -0.0044(10) C1 0.0430(17) 0.0371(16) 0.0351(16) 0.0024(12) 0.0110(13) 0.0076(13) C2 0.0447(17) 0.0298(14) 0.0380(15) 0.0039(12) 0.0128(13) 0.0020(13) C3 0.056(2) 0.0277(14) 0.0401(16) -0.0004(13) 0.0117(15) 0.0076(14) C4 0.084(3) 0.048(2) 0.052(2) 0.0163(17) 0.036(2) 0.024(2) C9 0.0220(14) 0.069(2) 0.0262(14) -0.0020(14) 0.0046(11) -0.0077(14) C10 0.0274(18) 0.168(6) 0.0334(19) -0.021(3) 0.0001(14) 0.008(2) C11 0.0249(14) 0.0551(19) 0.0279(15) -0.0053(13) -0.0025(11) 0.0024(13) C12 0.0292(15) 0.0505(18) 0.0272(14) 0.0005(12) 0.0030(11) 0.0031(13) C13 0.0316(16) 0.071(2) 0.0250(14) 0.0061(15) -0.0061(12) -0.0005(15) C14 0.0291(14) 0.0294(14) 0.0265(13) -0.0022(11) 0.0035(11) -0.0081(12) C15 0.0376(16) 0.0321(15) 0.0554(19) -0.0039(14) 0.0183(14) -0.0083(13) C16 0.0251(14) 0.0317(14) 0.0479(17) -0.0015(13) 0.0085(12) -0.0107(11) C17 0.0408(17) 0.0334(15) 0.0444(18) 0.0029(13) 0.0072(14) -0.0105(13) C18 0.0386(16) 0.0396(16) 0.0395(16) -0.0007(13) 0.0091(13) -0.0109(14) C7' 0.043(3) 0.029(3) 0.032(3) 0.004(2) 0.015(2) 0.008(2) N1' 0.023(2) 0.022(2) 0.032(2) -0.0034(16) 0.0119(18) 0.0096(18) C4' 0.040(3) 0.029(4) 0.045(4) -0.010(3) 0.011(3) 0.010(3) C5' 0.021(2) 0.040(3) 0.055(3) 0.001(3) 0.012(2) 0.009(2) N2' 0.036(3) 0.029(2) 0.041(3) 0.001(2) 0.020(3) 0.014(2) C8' 0.039(4) 0.043(5) 0.051(4) -0.002(3) -0.002(3) 0.013(3) C7 0.066(6) 0.069(7) 0.029(4) 0.020(4) 0.020(5) -0.014(6) N1 0.046(4) 0.029(4) 0.036(4) -0.011(3) 0.011(3) -0.004(3) C6 0.040(6) 0.044(7) 0.081(9) 0.005(6) 0.020(5) 0.024(5) C5 0.054(6) 0.055(6) 0.050(5) -0.008(5) 0.022(5) 0.006(5) N2 0.040(5) 0.058(6) 0.052(6) 0.016(4) 0.020(5) 0.018(4) C8 0.065(8) 0.036(7) 0.033(5) -0.016(4) 0.002(5) 0.008(6) O6 0.50(10) 0.30(7) 0.59(11) 0.000 0.13(9) 0.000 O5 0.20(3) 0.116(16) 0.105(15) -0.014(13) 0.057(18) -0.033(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Cu1 Cu1 81.19(7) . 5_666 O1 Cu1 O2 166.11(11) . 5_666 O1 Cu1 N1' 103.50(13) . . O1 Cu1 N1 82.8(2) . . O2 Cu1 Cu1 85.06(8) 5_666 5_666 O2 Cu1 N1' 90.36(13) 5_666 . O2 Cu1 N1 110.7(2) 5_666 . O3 Cu1 Cu1 83.39(7) . 5_666 O3 Cu1 O1 87.95(11) . . O3 Cu1 O2 88.49(11) . 5_666 O3 Cu1 O4 166.29(9) . 5_666 O3 Cu1 N1' 100.80(12) . . O3 Cu1 N1 91.27(19) . . O4 Cu1 Cu1 83.06(7) 5_666 5_666 O4 Cu1 O1 92.02(12) 5_666 . O4 Cu1 O2 88.28(12) 5_666 5_666 O4 Cu1 N1' 92.54(12) 5_666 . O4 Cu1 N1 102.34(19) 5_666 . N1' Cu1 Cu1 173.73(11) . 5_666 C9 O1 Cu1 127.0(2) . . C9 O2 Cu1 121.1(2) . 5_666 C14 O3 Cu1 123.30(19) . . C14 O4 Cu1 123.57(19) . 5_666 C2 C1 C4 117.6(3) . . C3 C1 C2 119.0(3) . . C3 C1 C4 123.3(3) . . C1 C2 H2 119.8 . . C2 C2 C1 120.40(18) 2_556 . C2 C2 H2 119.8 2_556 . C1 C3 H3 119.7 . . C3 C3 C1 120.56(19) 2_556 . C3 C3 H3 119.7 2_556 . C1 C4 H4A 121.5 . . C1 C4 H4B 124.8 . . N2' C4 C1 117.1(3) . . N2' C4 H4A 121.5 . . N2 C4 C1 110.3(4) . . N2 C4 H4B 124.8 . . O1 C9 O2 125.3(3) . . O1 C9 C10 115.9(3) . . O2 C9 C10 118.8(3) . . C9 C10 H10A 107.8 . . C9 C10 H10B 107.8 . . H10A C10 H10B 107.2 . . C11 C10 C9 117.9(3) . . C11 C10 H10A 107.8 . . C11 C10 H10B 107.8 . . C12 C11 C10 117.2(3) . . C13 C11 C10 124.7(3) 2_756 . C13 C11 C12 118.0(3) 2_756 . C11 C12 H12 119.6 . . C11 C12 C13 120.7(3) . . C13 C12 H12 119.6 . . C11 C13 C12 121.2(3) 2_756 . C11 C13 H13 119.4 2_756 . C12 C13 H13 119.4 . . O3 C14 C15 117.7(3) . . O4 C14 O3 126.5(3) . . O4 C14 C15 115.8(3) . . C14 C15 H15A 108.6 . . C14 C15 H15B 108.6 . . H15A C15 H15B 107.5 . . C16 C15 C14 114.8(3) . . C16 C15 H15A 108.6 . . C16 C15 H15B 108.6 . . C17 C16 C15 121.1(3) . . C18 C16 C15 120.6(3) . . C18 C16 C17 118.3(3) . . C16 C17 H17 119.5 . . C18 C17 C16 121.1(3) 7_666 . C18 C17 H17 119.5 7_666 . C16 C18 H18 119.7 . . C17 C18 C16 120.6(3) 7_666 . C17 C18 H18 119.7 7_666 . N1' C7' N2' 108.0 . . C8' C7' N1' 125.9(4) . . C8' C7' N2' 126.1(4) . . C7' N1' Cu1 130.4(2) . . C4' N1' Cu1 120.6(2) . . C4' N1' C7' 108.0 . . N1' C4' H4' 121(3) . . N1' C4' C5' 108.0 . . C5' C4' H4' 130(3) . . C4' C5' H5' 134(3) . . N2' C5' H5' 118(3) . . N2' C5' C4' 108.0 . . C4 N2' C7' 130.3(4) . . C4 N2' C5' 121.6(4) . . C7' N2' C5' 108.0 . . C7' C8' H8'A 109.5 . . C7' C8' H8'B 109.5 . . C7' C8' H8'C 109.5 . . H8'A C8' H8'B 109.5 . . H8'A C8' H8'C 109.5 . . H8'B C8' H8'C 109.5 . . N2 C7 N1 108.0 . . C8 C7 N1 126.3(8) . . C8 C7 N2 125.7(8) . . C7 N1 Cu1 129.4(4) . . C6 N1 Cu1 121.8(4) . . C6 N1 C7 108.0 . . N1 C6 H6 126.0 . . N1 C6 C5 108.0 . . C5 C6 H6 126.0 . . C6 C5 H5 126.0 . . N2 C5 C6 108.0 . . N2 C5 H5 126.0 . . C4 N2 C7 136.4(6) . . C4 N2 C5 115.5(6) . . C5 N2 C7 108.0 . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . C7 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 Cu1 2.6928(7) 5_666 Cu1 O1 1.981(2) . Cu1 O2 1.996(2) 5_666 Cu1 O3 1.962(2) . Cu1 O4 1.968(2) 5_666 Cu1 N1' 2.116(2) . Cu1 N1 2.117(5) . O1 C9 1.243(4) . O2 C9 1.255(5) . O3 C14 1.250(4) . O4 C14 1.248(4) . C1 C2 1.392(4) . C1 C3 1.388(5) . C1 C4 1.512(5) . C2 C2 1.386(6) 2_556 C2 H2 0.9300 . C3 C3 1.383(7) 2_556 C3 H3 0.9300 . C4 H4A 0.9300 . C4 H4B 0.9300 . C4 N2' 1.391(5) . C4 N2 1.370(6) . C9 C10 1.519(5) . C10 H10A 0.9700 . C10 H10B 0.9700 . C10 C11 1.512(5) . C11 C12 1.388(4) . C11 C13 1.386(5) 2_756 C12 H12 0.9300 . C12 C13 1.389(5) . C13 H13 0.9300 . C14 C15 1.522(4) . C15 H15A 0.9700 . C15 H15B 0.9700 . C15 C16 1.509(4) . C16 C17 1.389(5) . C16 C18 1.387(5) . C17 H17 0.9300 . C17 C18 1.383(5) 7_666 C18 H18 0.9300 . C7' N1' 1.4200 . C7' N2' 1.4200 . C7' C8' 1.370(8) . N1' C4' 1.4200 . C4' H4' 0.93(2) . C4' C5' 1.4200 . C5' H5' 0.92(2) . C5' N2' 1.4200 . C8' H8'A 0.9600 . C8' H8'B 0.9600 . C8' H8'C 0.9600 . C7 N1 1.4200 . C7 N2 1.4200 . C7 C8 1.314(13) . N1 C6 1.4200 . C6 H6 0.9300 . C6 C5 1.4200 . C5 H5 0.9300 . C5 N2 1.4200 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A N1' 0.93 2.62 3.505(9) 159.4 7_566 C4 H4B N1 0.93 2.69 3.578(14) 160.5 7_566 C8' H8'C O1 0.96 2.50 3.394(10) 154.0 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Cu1 O1 C9 O2 -5.5(5) . . Cu1 O1 C9 C10 175.7(3) . . Cu1 O2 C9 O1 8.0(5) 5_666 . Cu1 O2 C9 C10 -173.2(3) 5_666 . Cu1 O3 C14 O4 5.5(5) . . Cu1 O3 C14 C15 -174.1(2) . . Cu1 O4 C14 O3 -2.5(5) 5_666 . Cu1 O4 C14 C15 177.1(2) 5_666 . Cu1 N1' C4' C5' -169.7(3) . . Cu1 N1 C6 C5 170.3(5) . . O1 C9 C10 C11 -136.4(5) . . O2 C9 C10 C11 44.7(7) . . O3 C14 C15 C16 27.3(4) . . O4 C14 C15 C16 -152.4(3) . . C1 C4 N2' C7' -85.3(5) . . C1 C4 N2' C5' 91.1(5) . . C1 C4 N2 C7 102.3(7) . . C1 C4 N2 C5 -82.1(6) . . C2 C1 C3 C3 0.5(7) . 2_556 C2 C1 C4 N2' 177.1(4) . . C2 C1 C4 N2 149.0(5) . . C3 C1 C2 C2 -0.7(6) . 2_556 C3 C1 C4 N2' -5.8(6) . . C3 C1 C4 N2 -33.9(7) . . C4 C1 C2 C2 176.5(4) . 2_556 C4 C1 C3 C3 -176.6(5) . 2_556 C9 C10 C11 C12 -169.1(4) . . C9 C10 C11 C13 13.8(8) . 2_756 C10 C11 C12 C13 -177.8(4) . . C11 C12 C13 C11 -2.0(5) . 2_756 C13 C11 C12 C13 -0.6(5) 2_756 . C14 C15 C16 C17 48.5(4) . . C14 C15 C16 C18 -133.0(3) . . C15 C16 C17 C18 178.7(3) . 7_666 C15 C16 C18 C17 -178.7(3) . 7_666 C17 C16 C18 C17 -0.1(5) . 7_666 C18 C16 C17 C18 0.1(5) . 7_666 C7' N1' C4' C5' 0.0 . . N1' C7' N2' C4 176.8(5) . . N1' C7' N2' C5' 0.0 . . N1' C4' C5' N2' 0.0 . . C4' C5' N2' C4 -177.1(4) . . C4' C5' N2' C7' 0.0 . . N2' C7' N1' Cu1 168.4(3) . . N2' C7' N1' C4' 0.0 . . C8' C7' N1' Cu1 -12.4(7) . . C8' C7' N1' C4' 179.2(6) . . C8' C7' N2' C4 -2.4(6) . . C8' C7' N2' C5' -179.2(6) . . C7 N1 C6 C5 0.0 . . N1 C7 N2 C4 175.8(9) . . N1 C7 N2 C5 0.0 . . N1 C6 C5 N2 0.0 . . C6 C5 N2 C4 -176.8(7) . . C6 C5 N2 C7 0.0 . . N2 C7 N1 Cu1 -169.3(5) . . N2 C7 N1 C6 0.0 . . C8 C7 N1 Cu1 9.6(11) . . C8 C7 N1 C6 178.9(10) . . C8 C7 N2 C4 -3.1(11) . . C8 C7 N2 C5 -178.9(10) . .