#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:54:22 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288776 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247569.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_7247569 loop_ _publ_author_name 'Zhou, Mi' 'Wang, Yujiang' 'Yuan, Guoyuan' 'Ju, Zhanfeng' 'Yuan, Daqiang' _publ_section_title ; Synthesis and characterization of two metallo-hydrogen-bonded organic frameworks with diverse structures and properties ; _journal_issue 44 _journal_name_full CrystEngComm _journal_page_first 6132 _journal_page_last 6136 _journal_paper_doi 10.1039/D3CE00917C _journal_volume 25 _journal_year 2023 _chemical_absolute_configuration r,r _chemical_formula_sum 'C45 H69 Cu3 N6 O19 P' _chemical_formula_weight 1219.65 _chemical_name_systematic MHOF-PO4-1 _space_group_crystal_system cubic _space_group_IT_number 210 _space_group_name_Hall 'F 4d 2 3' _space_group_name_H-M_alt 'F 41 3 2' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2023-08-12 deposited with the CCDC. 2023-10-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 32 _cell_length_a 37.4254(2) _cell_length_b 37.4254(2) _cell_length_c 37.4254(2) _cell_measurement_reflns_used 6060 _cell_measurement_temperature 100.0(3) _cell_measurement_theta_max 71.9090 _cell_measurement_theta_min 3.8860 _cell_volume 52420.3(5) _computing_cell_refinement 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.0(3) _diffrn_detector_area_resol_mean 10.5594 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 15912 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.031 _diffrn_reflns_theta_min 3.917 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.904 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.236 _exptl_crystal_description block _exptl_crystal_F_000 20320 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O/MeOH' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.823 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.081 _refine_ls_abs_structure_details ; Flack x determined using 1206 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.025(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 4330 _refine_ls_number_restraints 157 _refine_ls_restrained_S_all 1.003 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0538 _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^)+(0.1193P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1547 _refine_ls_wR_factor_ref 0.1632 _reflns_Friedel_coverage 0.687 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.977 _reflns_number_gt 3485 _reflns_number_total 4330 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00917c2.cif _cod_data_source_block MHOF-PO4-1 _cod_depositor_comments 'Adding full bibliography for 7247568--7247569.cif.' _cod_original_cell_volume 52420.3(8) _cod_database_code 7247569 _shelx_shelxl_version_number 2017/1 _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 ; TITL C:\Users\ADMINI~1\Desktop\tmp\zm20170715a_a.res in F4(1)32 D:\xrd\HF-PO4-alpla\tmp\A_sq.res created by SHELXL-2017/1 at 10:33:28 on 06-Aug-2023 CELL 1.54184 37.4254 37.4254 37.4254 90.000 90.000 90.000 ZERR 32.0000 0.0002 0.0002 0.0002 0.000 0.000 0.000 LATT -4 SYMM 0.25-Y, 0.25+X, 0.25+Z SYMM -X, -Y, Z SYMM 0.25+Y, 0.25-X, 0.25+Z SYMM 0.25+X, 0.25-Z, 0.25+Y SYMM X, -Y, -Z SYMM 0.25+X, 0.25+Z, 0.25-Y SYMM 0.25+Z, 0.25+Y, 0.25-X SYMM -X, Y, -Z SYMM 0.25-Z, 0.25+Y, 0.25+X SYMM Z, X, Y SYMM Y, Z, X SYMM -Y, -Z, X SYMM Z, -X, -Y SYMM -Y, Z, -X SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, -Z, -X SYMM 0.25+Y, 0.25+X, 0.25-Z SYMM 0.25-Y, 0.25-X, 0.25-Z SYMM 0.25-X, 0.25+Z, 0.25+Y SYMM 0.25-X, 0.25-Z, 0.25-Y SYMM 0.25+Z, 0.25-Y, 0.25+X SYMM 0.25-Z, 0.25-Y, 0.25-X SFAC C H N O P CU UNIT 1440 2208 192 608 32 96 BOND $H ISOR 0.01 $O $C $N $P FLAT O1 O2 C3 H2 ABIN ABIN DFIX 0.85 0.002 O4 H41 DFIX 0.85 0.002 O4 H42 DFIX 0.85 0.002 O3 H31 DFIX 0.85 0.002 O3 H32 DANG 1.4 0.02 H41 H42 DANG 1.4 0.02 H31 H32 OMIT 0 2 2 ACTA FMAP 2 1 53 PLAN 50 0 0 TEMP -173.15 L.S. 50 0 40 WGHT 0.119300 FVAR 0.03346 CU21 6 0.401397 0.386930 0.327098 11.00000 0.03928 0.03939 = 0.04324 0.00532 0.00403 0.00341 P23 5 0.336289 0.336289 0.336289 10.33333 0.04014 0.04014 = 0.04014 0.00021 0.00021 0.00021 O22 4 0.366058 0.349885 0.312496 11.00000 0.04340 0.04384 = 0.04370 -0.00025 0.00336 0.00044 O20 4 0.420693 0.355469 0.363803 11.00000 0.03741 0.04416 = 0.04334 0.00936 0.00579 0.00629 O24 4 0.311841 0.311841 0.311841 10.33333 0.04801 0.04801 = 0.04801 -0.00311 -0.00311 -0.00311 O2 4 0.560307 0.271522 0.321337 11.00000 0.04265 0.05452 = 0.04584 0.00449 0.00570 0.00867 AFIX 87 0.9100 H2 2 0.582534 0.266555 0.312819 11.00000 -1.20000 AFIX 0 0.9100 O1 4 0.584433 0.325947 0.328263 11.00000 0.04727 0.05363 = 0.07185 0.00346 0.00757 0.00248 N18 3 0.391932 0.411973 0.280033 11.00000 0.04152 0.03666 = 0.04423 0.00333 0.00705 0.00418 AFIX 13 0.9100 H18 2 0.391068 0.394578 0.263066 11.00000 -1.20000 AFIX 0 0.9100 N11 3 0.444927 0.418560 0.328478 11.00000 0.04271 0.03976 = 0.05633 -0.00364 0.00223 0.00441 AFIX 13 0.9100 H11 2 0.437873 0.440738 0.335522 11.00000 -1.20000 AFIX 0 0.9100 C8 1 0.481355 0.367444 0.350318 11.00000 0.03924 0.04922 = 0.03892 0.00168 -0.00305 0.00018 C5 1 0.493515 0.294488 0.344746 11.00000 0.04475 0.04446 = 0.03034 0.00415 -0.00013 0.00512 AFIX 43 0.9100 H5 2 0.497683 0.270587 0.343147 11.00000 -1.20000 AFIX 0 0.9100 C6 1 0.459790 0.305960 0.352890 11.00000 0.04089 0.04214 = 0.03228 0.00116 0.00126 0.00072 C7 1 0.453195 0.343214 0.355971 11.00000 0.04009 0.04282 = 0.04077 0.00394 0.00228 0.00237 C4 1 0.521983 0.318250 0.338753 11.00000 0.03873 0.04630 = 0.03638 0.00632 -0.00395 0.00446 C3 1 0.558094 0.305989 0.329163 11.00000 0.04689 0.05029 = 0.04234 0.00224 0.00308 0.00484 C9 1 0.515234 0.355139 0.341576 11.00000 0.04117 0.05229 = 0.03661 0.00729 -0.00540 -0.00258 AFIX 43 0.9100 H9 2 0.533208 0.371035 0.337642 11.00000 -1.20000 AFIX 0 0.9100 C12 1 0.455855 0.420699 0.290730 11.00000 0.04411 0.03643 = 0.04738 0.00298 0.00304 0.00614 AFIX 13 0.9100 H12 2 0.460169 0.398095 0.282879 11.00000 -1.20000 AFIX 0 0.9100 C17 1 0.423087 0.434782 0.271074 11.00000 0.04067 0.03617 = 0.04976 0.00736 0.01149 0.00673 AFIX 13 0.9100 H17 2 0.418567 0.457360 0.278887 11.00000 -1.20000 AFIX 0 0.9100 C10 1 0.473150 0.406139 0.353510 11.00000 0.04984 0.04720 = 0.04943 0.00394 -0.00056 0.00188 AFIX 23 0.9100 H10A 2 0.493465 0.418838 0.349360 11.00000 -1.20000 H10B 2 0.466043 0.410802 0.376290 11.00000 -1.20000 AFIX 0 0.9100 C16 1 0.429475 0.436134 0.230611 11.00000 0.04803 0.05698 = 0.04967 0.00852 0.00353 0.00979 AFIX 23 0.9100 H16A 2 0.432627 0.413570 0.222118 11.00000 -1.20000 H16B 2 0.410004 0.445688 0.219620 11.00000 -1.20000 AFIX 0 0.9100 C19 1 0.356654 0.429803 0.279522 11.00000 0.04062 0.04373 = 0.04349 -0.00110 0.00136 0.00531 AFIX 23 0.9100 H19A 2 0.339476 0.413207 0.284074 11.00000 -1.20000 H19B 2 0.352682 0.438565 0.257191 11.00000 -1.20000 AFIX 0 0.9100 C13 1 0.487944 0.443056 0.282220 11.00000 0.04636 0.05485 = 0.07201 0.01545 0.00445 0.00054 AFIX 23 0.9100 H13A 2 0.507410 0.433822 0.293491 11.00000 -1.20000 H13B 2 0.484463 0.465636 0.290542 11.00000 -1.20000 AFIX 0 0.9100 C15 1 0.461862 0.458293 0.222190 11.00000 0.05949 0.06624 = 0.05854 0.02222 0.02084 0.01275 AFIX 23 0.9100 H15A 2 0.457733 0.481374 0.228624 11.00000 -1.20000 H15B 2 0.465963 0.457794 0.198229 11.00000 -1.20000 AFIX 0 0.9100 C14 1 0.494981 0.444398 0.241936 11.00000 0.04724 0.06144 = 0.07067 0.01624 0.01792 0.00902 AFIX 23 0.9100 H14A 2 0.500540 0.422140 0.233881 11.00000 -1.20000 H14B 2 0.513887 0.459012 0.237441 11.00000 -1.20000 AFIX 0 0.9100 O3 4 0.622742 0.242610 0.296993 11.00000 0.09434 0.07053 = 0.30726 -0.04704 0.01724 0.01261 O4 4 0.373572 0.362717 0.215083 11.00000 0.30370 0.24774 = 0.14064 -0.08171 0.02748 -0.16323 H41 2 0.356673 0.374129 0.205074 11.00000 -1.20000 H42 2 0.389411 0.356519 0.200025 11.00000 -1.20000 H32 2 0.614998 0.253389 0.278544 11.00000 -1.20000 H31 2 0.639152 0.228518 0.290054 11.00000 -1.20000 HKLF 4 REM C:\Users\ADMINI~1\Desktop\tmp\zm20170715a_a.res in F4(1)32 REM R1 = 0.0538 for 3485 Fo > 4sig(Fo) and 0.0651 for all 4330 data REM 236 parameters refined using 157 restraints END WGHT 0.1194 0.0000 REM Highest difference peak 0.823, deepest hole -0.276, 1-sigma level 0.081 Q1 1 0.4197 0.4231 0.3576 11.00000 0.05 0.82 Q2 1 0.4155 0.4277 0.3525 11.00000 0.05 0.74 Q3 1 0.6219 0.2422 0.3177 11.00000 0.05 0.49 Q4 1 0.6192 0.2608 0.2649 11.00000 0.05 0.47 Q5 1 0.6399 0.2430 0.2816 11.00000 0.05 0.46 Q6 1 0.6239 0.2686 0.2700 11.00000 0.05 0.45 Q7 1 0.3496 0.3894 0.2097 11.00000 0.05 0.44 Q8 1 0.3969 0.3397 0.2410 11.00000 0.05 0.44 Q9 1 0.6284 0.2387 0.3066 11.00000 0.05 0.40 Q10 1 0.3870 0.3320 0.2506 11.00000 0.05 0.40 Q11 1 0.6109 0.2500 0.2500 10.50000 0.05 0.37 Q12 1 0.3990 0.3396 0.1984 11.00000 0.05 0.35 Q13 1 0.4900 0.3681 0.3453 11.00000 0.05 0.30 Q14 1 0.4035 0.3441 0.1930 11.00000 0.05 0.28 Q15 1 0.3420 0.3830 0.2030 11.00000 0.05 0.27 Q16 1 0.6491 0.2299 0.2693 11.00000 0.05 0.26 Q17 1 0.3838 0.3583 0.2210 11.00000 0.05 0.26 Q18 1 0.3543 0.3653 0.3075 11.00000 0.05 0.23 Q19 1 0.6694 0.2500 0.2500 10.50000 0.05 0.22 Q20 1 0.3888 0.3377 0.2719 11.00000 0.05 0.21 Q21 1 0.3926 0.3392 0.2778 11.00000 0.05 0.21 Q22 1 0.3909 0.3279 0.3259 11.00000 0.05 0.21 Q23 1 0.4632 0.3174 0.3549 11.00000 0.05 0.21 Q24 1 0.4280 0.4653 0.2303 11.00000 0.05 0.21 Q25 1 0.5644 0.2719 0.3303 11.00000 0.05 0.21 Q26 1 0.3566 0.4227 0.2982 11.00000 0.05 0.20 Q27 1 0.3656 0.3382 0.2400 11.00000 0.05 0.20 Q28 1 0.3506 0.3723 0.2489 11.00000 0.05 0.20 Q29 1 0.3073 0.3073 0.3073 10.33333 0.05 0.19 Q30 1 0.5210 0.3455 0.3378 11.00000 0.05 0.19 Q31 1 0.3903 0.3676 0.2297 11.00000 0.05 0.19 Q32 1 0.3895 0.3310 0.2853 11.00000 0.05 0.19 Q33 1 0.3987 0.3978 0.2903 11.00000 0.05 0.19 Q34 1 0.5070 0.2347 0.3443 11.00000 0.05 0.18 Q35 1 0.5821 0.3357 0.3399 11.00000 0.05 0.17 Q36 1 0.5087 0.4280 0.2863 11.00000 0.05 0.17 Q37 1 0.5429 0.2487 0.3157 11.00000 0.05 0.17 Q38 1 0.3939 0.3998 0.2822 11.00000 0.05 0.17 Q39 1 0.4175 0.3739 0.3624 11.00000 0.05 0.17 Q40 1 0.3933 0.4125 0.3077 11.00000 0.05 0.17 Q41 1 0.4992 0.4228 0.3570 11.00000 0.05 0.17 Q42 1 0.4230 0.4397 0.2224 11.00000 0.05 0.16 Q43 1 0.4202 0.3475 0.3589 11.00000 0.05 0.16 Q44 1 0.3936 0.3921 0.2756 11.00000 0.05 0.16 Q45 1 0.4390 0.4862 0.2819 11.00000 0.05 0.16 Q46 1 0.4875 0.4109 0.3509 11.00000 0.05 0.16 Q47 1 0.5872 0.3504 0.3285 11.00000 0.05 0.16 Q48 1 0.5380 0.2440 0.3080 11.00000 0.05 0.15 Q49 1 0.3834 0.4400 0.2118 11.00000 0.05 0.15 Q50 1 0.5000 0.5000 0.2183 10.50000 0.05 0.15 ; _shelx_res_checksum 71064 _shelx_fab_file ; 2 2 2 -23.48 -652.28 1 1 3 47.06 56.24 1 3 3 -221.32 224.79 3 3 3 -264.81 -217.48 0 0 4 20.43 2.49 0 2 4 -63.51 1.58 2 2 4 -156.87 -14.74 0 4 4 163.48 -36.04 2 4 4 -9.53 -241.53 4 4 4 -629.09 31.63 1 1 5 130.04 -121.07 1 3 5 -126.94 -25.27 3 3 5 -70.63 90.91 1 5 5 -150.51 152.99 3 5 5 -151.42 -106.51 5 5 5 266.42 -279.29 0 2 6 64.49 -2.97 2 2 6 22.67 323.05 2 4 6 -26.45 -58.79 0 4 6 -137.53 0.86 4 4 6 -8.82 -250.48 0 6 6 66.10 0.93 2 6 6 -18.72 -273.15 4 6 6 84.83 -6.02 6 6 6 24.81 103.96 1 1 7 259.06 246.88 1 3 7 57.73 -218.14 3 3 7 -37.31 -37.70 3 5 7 106.60 -145.32 1 5 7 20.67 -80.82 5 5 7 -41.78 -35.61 1 7 7 -112.35 117.99 3 7 7 145.43 144.37 5 7 7 140.22 -141.35 7 7 7 6.03 7.43 0 0 8 276.67 7.55 0 2 8 -93.90 6.72 2 2 8 10.19 -0.55 2 4 8 72.43 59.47 0 4 8 -235.83 13.09 4 4 8 375.92 -30.48 4 6 8 109.99 5.52 2 6 8 161.20 -110.23 0 6 8 262.86 -5.07 6 6 8 70.10 9.84 0 8 8 185.98 4.47 2 8 8 7.82 58.88 4 8 8 81.19 12.82 6 8 8 2.70 -5.10 8 8 8 289.48 -27.41 1 1 9 -6.21 15.56 1 3 9 55.31 -32.00 3 3 9 72.71 -70.56 3 5 9 72.13 -229.84 1 5 9 159.47 47.46 5 5 9 88.75 -88.58 5 7 9 151.27 116.63 3 7 9 174.60 -32.54 1 7 9 97.90 -254.37 7 7 9 -32.99 14.55 1 9 9 -110.33 119.30 3 9 9 130.82 122.13 5 9 9 71.23 -76.86 7 9 9 -21.73 -41.96 9 9 9 -34.80 11.82 0 2 10 -129.33 7.26 2 2 10 -0.58 -97.99 2 4 10 -71.26 -130.00 0 4 10 216.59 8.39 4 4 10 13.79 -92.62 4 6 10 140.97 -20.12 2 6 10 315.36 99.80 0 6 10 -71.31 2.11 6 6 10 -7.22 -231.55 6 8 10 172.80 67.67 4 8 10 76.65 -28.35 2 8 10 36.68 0.16 0 8 10 192.53 -3.97 8 8 10 -5.29 -125.81 0 10 10 -72.95 7.12 2 10 10 -7.52 -191.77 4 10 10 72.49 14.80 6 10 10 19.24 64.35 8 10 10 -21.93 -23.65 10 10 10 -17.01 -171.30 1 1 11 13.55 14.08 1 3 11 -106.38 151.41 3 3 11 -56.14 -56.99 3 5 11 108.10 -136.08 1 5 11 53.83 -291.23 5 5 11 -43.22 -30.27 5 7 11 18.77 69.34 3 7 11 -39.32 -124.98 1 7 11 134.98 -16.66 7 7 11 20.23 18.92 7 9 11 103.74 -23.53 5 9 11 -64.52 -26.14 3 9 11 -32.98 68.29 1 9 11 -13.33 2.18 9 9 11 -45.58 -41.74 1 11 11 -12.45 23.55 3 11 11 -25.40 -29.34 5 11 11 57.10 -50.95 7 11 11 -78.15 -101.28 9 11 11 -130.66 168.33 11 11 11 -31.37 1.71 0 0 12 221.07 -12.97 0 2 12 50.49 2.14 2 2 12 39.21 -16.54 2 4 12 66.63 -62.75 0 4 12 66.43 -2.65 4 4 12 -152.35 -4.94 4 6 12 -38.70 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-3.00 6 26 38 0.52 -4.49 1 1 39 6.70 8.34 1 3 39 7.58 -1.42 3 3 39 -19.02 -11.74 3 5 39 -2.40 -4.47 1 5 39 -4.02 -5.71 5 5 39 -1.61 -1.08 5 7 39 -4.39 -9.08 3 7 39 -0.38 1.70 1 7 39 0.62 -7.66 7 7 39 -2.16 -3.60 7 9 39 -1.87 -5.44 5 9 39 -6.88 2.91 3 9 39 -6.38 -5.40 1 9 39 2.00 1.75 9 9 39 -9.34 -13.02 9 11 39 -1.04 -7.63 7 11 39 4.90 3.85 5 11 39 0.76 -2.43 3 11 39 -7.85 1.97 1 11 39 -1.29 -6.54 11 11 39 -14.88 -13.59 11 13 39 -9.00 3.70 9 13 39 -5.92 6.09 7 13 39 -1.34 -10.73 5 13 39 7.82 6.60 3 13 39 -7.21 -8.10 1 13 39 4.26 -2.57 13 13 39 10.96 4.19 13 15 39 8.25 -1.57 11 15 39 -1.77 12.79 9 15 39 -11.55 2.04 7 15 39 2.36 -6.35 5 15 39 2.04 -4.97 3 15 39 3.90 14.34 1 15 39 -16.45 1.68 15 15 39 3.90 -2.15 15 17 39 -1.21 3.69 13 17 39 -6.19 2.30 11 17 39 7.28 -5.68 9 17 39 -0.14 -7.08 7 17 39 4.27 13.18 5 17 39 -3.94 4.83 3 17 39 -14.94 0.64 1 17 39 5.91 5.57 17 17 39 -0.12 -0.61 15 19 39 4.82 4.37 13 19 39 3.43 -0.18 11 19 39 -7.61 -3.03 9 19 39 4.93 1.18 7 19 39 8.44 -6.08 5 19 39 -15.12 5.17 3 19 39 -5.04 0.22 1 19 39 7.19 -7.96 13 21 39 2.66 -0.24 11 21 39 1.81 1.91 9 21 39 -2.89 -5.59 7 21 39 0.18 -6.89 5 21 39 0.37 -5.46 3 21 39 -7.13 2.21 1 21 39 2.30 2.64 9 23 39 1.36 0.09 7 23 39 -3.14 -8.74 5 23 39 4.17 -2.24 3 23 39 0.86 -1.08 1 23 39 -2.79 2.49 0 0 40 14.05 -9.23 0 2 40 4.68 1.20 2 2 40 -14.76 -6.94 2 4 40 6.94 1.02 0 4 40 -20.35 -4.02 4 4 40 -9.68 -0.09 4 6 40 -3.84 4.51 2 6 40 -8.04 -13.08 0 6 40 16.95 -6.78 6 6 40 1.68 1.41 6 8 40 -1.82 13.89 4 8 40 -12.11 -4.82 2 8 40 5.54 -4.50 0 8 40 7.19 -4.79 8 8 40 4.62 -4.83 8 10 40 2.22 -3.48 6 10 40 1.77 0.69 4 10 40 4.42 8.00 2 10 40 -6.31 3.25 0 10 40 3.99 -0.18 10 10 40 -6.88 0.51 10 12 40 -8.18 -3.59 8 12 40 3.13 -6.64 6 12 40 9.93 0.94 4 12 40 5.19 7.88 2 12 40 1.22 7.69 0 12 40 -12.87 -1.39 12 12 40 3.83 -2.05 12 14 40 -4.19 1.22 10 14 40 7.80 0.48 8 14 40 -1.24 -1.02 6 14 40 0.66 -2.14 4 14 40 -5.22 -0.89 2 14 40 -1.25 0.07 0 14 40 3.56 0.33 14 14 40 0.72 -4.12 14 16 40 6.41 13.31 12 16 40 1.19 11.84 10 16 40 -4.91 -10.87 8 16 40 -0.49 0.62 6 16 40 2.52 -4.03 4 16 40 -10.32 5.67 2 16 40 -5.27 -3.61 0 16 40 6.93 -0.04 16 16 40 -10.13 -2.54 14 18 40 -0.82 4.85 12 18 40 -0.68 0.46 10 18 40 -7.82 7.77 8 18 40 5.59 -3.56 6 18 40 -0.82 6.20 4 18 40 -9.44 -5.72 2 18 40 -0.06 -4.78 0 18 40 4.90 -3.89 12 20 40 2.24 3.31 10 20 40 -0.40 11.42 8 20 40 -0.53 4.25 6 20 40 -5.37 -5.00 4 20 40 1.21 -1.47 2 20 40 -2.78 -3.69 0 20 40 4.40 -1.71 4 22 40 -4.92 0.29 0 22 40 0.69 -0.61 2 22 40 3.26 5.23 6 22 40 3.41 1.84 8 22 40 2.44 2.68 1 1 41 10.48 -8.72 1 3 41 3.97 -2.63 3 3 41 10.16 -7.91 3 5 41 0.56 -4.99 1 5 41 18.49 -2.30 5 5 41 2.30 -2.15 5 7 41 2.90 9.08 3 7 41 0.42 -2.45 1 7 41 15.79 -5.31 7 7 41 -3.35 -1.24 7 9 41 -2.27 -2.57 5 9 41 1.33 0.19 3 9 41 3.34 -2.68 1 9 41 1.03 2.63 9 9 41 -5.66 2.99 9 11 41 -4.71 2.89 7 11 41 3.21 -1.60 5 11 41 -0.04 -1.33 3 11 41 3.14 -1.06 1 11 41 0.12 -11.37 11 11 41 -4.80 6.05 11 13 41 -6.43 5.43 9 13 41 -4.49 -11.94 7 13 41 6.18 7.33 5 13 41 -1.94 -1.33 3 13 41 -6.17 -5.38 1 13 41 4.84 2.93 13 13 41 -12.48 11.61 13 15 41 7.40 7.56 11 15 41 -4.38 -0.37 9 15 41 -5.19 -1.72 7 15 41 -4.72 -7.21 5 15 41 -5.88 4.74 3 15 41 -5.21 1.46 1 15 41 5.22 -3.04 15 15 41 -6.24 7.98 13 17 41 2.84 -1.76 11 17 41 -4.62 -2.34 9 17 41 -7.75 3.71 7 17 41 -4.55 -12.01 5 17 41 0.60 -5.63 3 17 41 1.10 5.17 1 17 41 -3.40 7.19 9 19 41 4.14 -11.18 7 19 41 -0.66 0.81 5 19 41 -6.71 -3.52 3 19 41 -4.35 -4.55 1 19 41 3.11 -5.42 3 21 41 -5.66 -6.40 5 21 41 -5.64 0.34 0 2 42 -4.94 -2.94 2 2 42 1.77 -12.83 2 4 42 -15.93 -2.61 0 4 42 7.03 -0.96 4 4 42 0.21 -2.57 4 6 42 3.03 0.17 2 6 42 7.10 8.95 0 6 42 -4.17 -0.95 6 6 42 -2.11 0.69 6 8 42 -2.31 4.90 4 8 42 -4.22 7.84 2 8 42 6.52 -9.18 0 8 42 5.39 1.77 8 8 42 1.54 3.80 8 10 42 -0.04 -3.19 6 10 42 3.91 6.98 4 10 42 1.87 0.95 2 10 42 1.19 -4.53 0 10 42 6.49 -0.42 10 10 42 -2.37 -4.60 10 12 42 -1.22 -3.71 8 12 42 1.15 -5.23 6 12 42 6.17 -3.68 4 12 42 2.87 -0.49 2 12 42 5.92 4.80 0 12 42 5.71 2.76 12 12 42 -3.50 8.90 12 14 42 5.61 -1.53 10 14 42 -4.89 -3.90 8 14 42 2.21 -7.67 6 14 42 3.34 -6.13 4 14 42 6.99 4.32 2 14 42 -1.91 3.44 0 14 42 0.31 -2.38 14 14 42 -2.92 19.54 10 16 42 2.29 -1.67 8 16 42 1.43 -4.12 6 16 42 3.21 3.58 4 16 42 -1.44 -8.12 2 16 42 2.38 -4.81 0 16 42 -6.22 0.74 6 18 42 -3.09 -5.73 4 18 42 -0.68 0.53 2 18 42 1.40 -8.13 0 18 42 1.96 -1.14 8 18 42 2.26 -0.74 1 1 43 1.62 1.68 1 3 43 8.18 -2.85 3 3 43 -1.61 -5.57 3 5 43 7.57 -4.09 1 5 43 11.07 -1.52 5 5 43 -4.36 -1.14 5 7 43 -0.47 6.78 3 7 43 4.08 -4.41 1 7 43 5.08 -6.04 7 7 43 0.06 0.14 7 9 43 2.83 8.21 5 9 43 2.22 -2.73 3 9 43 -2.77 -3.93 1 9 43 -2.11 -5.32 9 9 43 -0.84 0.07 9 11 43 -4.62 -0.18 7 11 43 0.15 -6.48 5 11 43 4.72 0.92 3 11 43 2.03 -5.18 1 11 43 1.68 11.00 11 11 43 0.85 8.13 11 13 43 -3.53 -0.75 9 13 43 -1.19 -1.22 7 13 43 -4.01 -2.06 5 13 43 -0.40 -2.06 3 13 43 7.31 6.74 1 13 43 7.30 -8.05 7 15 43 3.48 2.86 5 15 43 -0.59 4.82 3 15 43 -1.37 -6.66 1 15 43 3.72 -4.28 9 15 43 1.43 -6.08 1 17 43 1.43 -3.54 0 0 44 -18.57 6.61 0 2 44 -2.28 3.12 2 2 44 -12.19 5.23 2 4 44 0.66 -6.03 0 4 44 3.20 5.19 4 4 44 -16.32 1.80 4 6 44 1.75 3.96 2 6 44 1.31 0.87 0 6 44 -5.15 -0.11 6 6 44 -4.33 3.54 6 8 44 0.65 -0.23 4 8 44 12.42 1.67 2 8 44 -7.12 4.68 0 8 44 0.46 3.50 8 8 44 -7.05 -1.31 8 10 44 3.22 -0.08 6 10 44 0.91 -1.24 4 10 44 -8.66 -3.14 2 10 44 10.75 -2.79 0 10 44 0.54 3.52 10 10 44 1.65 -5.49 8 12 44 -2.70 -9.04 6 12 44 2.32 0.57 4 12 44 5.44 -1.69 2 12 44 0.33 -4.77 0 12 44 8.08 -2.42 4 14 44 7.42 -1.70 2 14 44 2.99 -6.74 0 14 44 -14.93 3.87 1 1 45 -2.69 0.51 1 3 45 6.23 -0.70 3 3 45 -1.55 -3.52 3 5 45 1.21 -10.70 1 5 45 2.91 -3.76 5 5 45 -0.74 -1.77 5 7 45 -2.16 -5.91 3 7 45 1.79 -6.39 1 7 45 -6.60 -3.93 7 7 45 -0.70 8.64 7 9 45 5.07 -0.48 5 9 45 0.64 2.28 3 9 45 -6.45 -2.45 1 9 45 -3.03 2.61 3 11 45 0.70 6.30 1 11 45 -0.70 -8.38 1 1 1 405.76 -415.75 0 2 2 1128.40 -33.26 0 0 20 151.41 2.78 25 25 25 -16.09 9.04 26 26 26 3.45 9.62 23 27 27 -2.46 -7.80 25 27 27 -15.18 12.90 27 27 27 2.03 -0.18 24 26 28 3.88 4.93 26 26 28 -11.12 0.16 22 28 28 1.80 5.96 24 28 28 -9.83 2.99 25 25 29 -3.97 6.31 23 27 29 0.83 3.14 21 29 29 3.59 -6.63 24 26 30 -0.32 4.91 20 28 30 -3.91 11.06 22 28 30 2.76 2.09 18 30 30 1.47 -0.62 23 25 31 7.31 6.85 21 27 31 2.39 4.02 19 29 31 -0.49 0.43 15 31 31 -1.23 -3.19 24 24 32 1.95 0.82 22 26 32 -2.90 2.35 18 28 32 -4.97 1.63 16 30 32 3.73 -0.77 10 32 32 2.17 -7.00 23 23 33 0.92 -0.70 21 25 33 2.77 0.26 19 27 33 -4.39 -0.26 15 29 33 2.58 -3.78 11 31 33 -2.79 -0.95 1 33 33 -0.46 1.51 3 33 33 5.41 0.45 18 26 34 -4.20 -5.32 10 30 34 0.54 -3.97 0 32 34 -4.06 -0.02 2 32 34 -1.52 -3.71 15 27 35 -1.40 1.65 11 29 35 4.88 5.02 1 31 35 -0.28 -4.31 20 22 36 0.81 5.11 14 26 36 1.80 -8.03 10 28 36 1.40 -10.31 19 21 37 -6.99 -4.62 17 23 37 -6.65 -1.90 13 25 37 -1.00 0.69 9 27 37 -1.63 1.80 18 20 38 -2.52 1.32 16 22 38 -3.32 -1.31 12 24 38 -0.71 2.20 8 26 38 -1.26 -0.84 17 19 39 1.85 -6.64 15 21 39 -1.53 -1.00 11 23 39 -5.23 -3.04 1 25 39 -0.78 -3.96 3 25 39 -0.68 -3.76 5 25 39 0.87 -4.08 16 18 40 4.91 0.80 10 22 40 1.60 2.95 0 24 40 4.86 0.57 2 24 40 1.14 -5.22 11 19 41 -4.82 -3.19 1 21 41 7.18 -5.66 7 21 41 2.32 -4.34 12 16 42 -3.89 -1.25 10 18 42 -4.47 -1.69 0 20 42 3.90 -0.69 2 20 42 1.67 0.64 4 20 42 -10.45 -6.06 13 13 43 5.83 7.76 3 17 43 -0.38 0.06 5 17 43 -0.13 -0.55 7 17 43 -1.11 0.05 10 12 44 -2.21 -2.46 6 14 44 5.73 0.46 9 9 45 2.15 -0.39 5 11 45 0.52 0.31 0 2 46 -5.85 7.67 2 2 46 -3.03 8.22 0 4 46 -2.47 2.60 2 4 46 -1.88 1.25 4 4 46 -1.29 -0.60 0 6 46 3.52 5.19 2 6 46 -2.00 -7.62 4 6 46 -4.52 3.02 6 6 46 -1.11 7.23 0 8 46 -5.05 0.19 2 8 46 1.08 6.82 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 290617) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 924 256 ' ' 2 0.454 -0.008 0.006 4676 1017 ' ' 3 0.500 0.000 0.500 924 256 ' ' 4 0.250 0.250 0.250 924 255 ' ' 5 0.750 0.250 0.750 924 255 ' ' 6 0.125 0.125 0.125 73 22 ' ' 7 0.375 0.125 0.375 73 22 ' ' 8 0.625 0.125 0.625 73 22 ' ' 9 0.875 0.125 0.875 73 22 ' ' 10 0.500 0.500 0.000 924 256 ' ' 11 1.000 0.500 0.500 924 256 ' ' 12 0.375 0.375 0.125 73 22 ' ' 13 0.125 0.375 0.375 73 22 ' ' 14 0.875 0.375 0.625 73 22 ' ' 15 0.625 0.375 0.875 73 22 ' ' 16 0.750 0.750 0.250 924 255 ' ' 17 0.250 0.750 0.750 924 255 ' ' 18 0.625 0.625 0.125 73 22 ' ' 19 0.875 0.625 0.375 73 22 ' ' 20 0.125 0.625 0.625 73 22 ' ' 21 0.375 0.625 0.875 73 22 ' ' 22 0.875 0.875 0.125 73 22 ' ' 23 0.625 0.875 0.375 73 22 ' ' 24 0.375 0.875 0.625 73 22 ' ' 25 0.125 0.875 0.875 73 22 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 1 1 2.045 0 2 2 3.340 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL D:/xrd/HF-F 41 3 2a/tmpR = 0.12 CELL 37.4254 37.4254 37.4254 90.00 90.00 90.00 SPGR F4132 # Solvent Accessible Volume = 13211 # Electrons Found in S.A.V. = 3393 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.625 0.125 0.125 ! 12.91 eA-3 Q102 0.568 0.341 0.014 ! 4.43 eA-3 C103 0.500 0.500 0.000 ! 4.01 eA-3 C104 0.250 0.109 0.251 ! 3.71 eA-3 Q105 0.247 0.195 0.156 ! 3.61 eA-3 C106 0.039 0.039 0.039 ! 3.59 eA-3 C107 0.908 0.065 0.406 ! 1.94 eA-3 Q108 0.101 0.358 0.349 ! 1.83 eA-3 C109 0.022 0.385 0.451 ! 1.73 eA-3 Q110 0.483 0.415 0.477 ! 1.40 eA-3 C111 0.568 0.025 0.061 ! 1.30 eA-3 Q112 0.876 0.239 0.186 ! 1.17 eA-3 C113 0.581 0.081 0.081 ! 1.14 eA-3 Q114 0.604 0.176 0.333 ! 1.13 eA-3 C115 0.069 0.428 0.071 ! 1.10 eA-3 C116 0.483 0.479 0.478 ! 1.06 eA-3 Q117 0.824 0.200 0.212 ! 0.95 eA-3 Q118 0.445 0.031 0.064 ! 0.89 eA-3 Q119 0.750 0.252 0.155 ! 0.83 eA-3 Q120 0.120 0.211 0.145 ! 0.80 eA-3 Q121 0.101 0.111 0.098 ! 0.69 eA-3 Q122 0.580 0.086 0.162 ! 0.69 eA-3 Q123 0.988 0.368 0.016 ! 0.69 eA-3 Q124 0.127 0.413 0.386 ! 0.66 eA-3 Q125 0.888 0.032 0.047 ! 0.59 eA-3 Q126 0.048 0.445 0.392 ! 0.58 eA-3 C127 0.736 0.236 0.236 ! 0.56 eA-3 Q128 0.111 0.323 0.369 ! 0.56 eA-3 Q129 0.611 0.823 0.369 ! 0.56 eA-3 Q130 0.144 0.100 0.173 ! 0.55 eA-3 C131 0.510 0.456 0.496 ! 0.54 eA-3 C132 0.010 0.956 0.496 ! 0.54 eA-3 Q133 0.178 0.876 0.899 ! 0.54 eA-3 Q134 0.805 0.086 0.172 ! 0.53 eA-3 Q135 0.908 0.117 0.236 ! 0.52 eA-3 Q136 0.854 0.289 0.190 ! 0.52 eA-3 C137 0.236 0.236 0.715 ! 0.51 eA-3 ) ; _shelx_fab_checksum 24729 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/4, x+1/4, z+1/4' '-x, -y, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/4, -z+1/4, y+1/4' 'x, -y, -z' 'x+1/4, z+1/4, -y+1/4' 'z+1/4, y+1/4, -x+1/4' '-x, y, -z' '-z+1/4, y+1/4, x+1/4' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' 'y+1/4, x+1/4, -z+1/4' '-y+1/4, -x+1/4, -z+1/4' '-x+1/4, z+1/4, y+1/4' '-x+1/4, -z+1/4, -y+1/4' 'z+1/4, -y+1/4, x+1/4' '-z+1/4, -y+1/4, -x+1/4' 'x, y+1/2, z+1/2' '-y+1/4, x+3/4, z+3/4' '-x, -y+1/2, z+1/2' 'y+1/4, -x+3/4, z+3/4' 'x+1/4, -z+3/4, y+3/4' 'x, -y+1/2, -z+1/2' 'x+1/4, z+3/4, -y+3/4' 'z+1/4, y+3/4, -x+3/4' '-x, y+1/2, -z+1/2' '-z+1/4, y+3/4, x+3/4' 'z, x+1/2, y+1/2' 'y, z+1/2, x+1/2' '-y, -z+1/2, x+1/2' 'z, -x+1/2, -y+1/2' '-y, z+1/2, -x+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, -z+1/2, -x+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+3/4, -z+3/4' '-x+1/4, z+3/4, y+3/4' '-x+1/4, -z+3/4, -y+3/4' 'z+1/4, -y+3/4, x+3/4' '-z+1/4, -y+3/4, -x+3/4' 'x+1/2, y, z+1/2' '-y+3/4, x+1/4, z+3/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+1/4, z+3/4' 'x+3/4, -z+1/4, y+3/4' 'x+1/2, -y, -z+1/2' 'x+3/4, z+1/4, -y+3/4' 'z+3/4, y+1/4, -x+3/4' '-x+1/2, y, -z+1/2' '-z+3/4, y+1/4, x+3/4' 'z+1/2, x, y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, -z, x+1/2' 'z+1/2, -x, -y+1/2' '-y+1/2, z, -x+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, -z, -x+1/2' 'y+3/4, x+1/4, -z+3/4' '-y+3/4, -x+1/4, -z+3/4' '-x+3/4, z+1/4, y+3/4' '-x+3/4, -z+1/4, -y+3/4' 'z+3/4, -y+1/4, x+3/4' '-z+3/4, -y+1/4, -x+3/4' 'x+1/2, y+1/2, z' '-y+3/4, x+3/4, z+1/4' '-x+1/2, -y+1/2, z' 'y+3/4, -x+3/4, z+1/4' 'x+3/4, -z+3/4, y+1/4' 'x+1/2, -y+1/2, -z' 'x+3/4, z+3/4, -y+1/4' 'z+3/4, y+3/4, -x+1/4' '-x+1/2, y+1/2, -z' '-z+3/4, y+3/4, x+1/4' 'z+1/2, x+1/2, y' 'y+1/2, z+1/2, x' '-y+1/2, -z+1/2, x' 'z+1/2, -x+1/2, -y' '-y+1/2, z+1/2, -x' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, -z+1/2, -x' 'y+3/4, x+3/4, -z+1/4' '-y+3/4, -x+3/4, -z+1/4' '-x+3/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+1/4' 'z+3/4, -y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+1/4' 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 Cu21 Cu 0.40140(2) 0.38693(2) 0.32710(2) 0.0406(3) Uani 1 1 d . . . . . P23 P 0.33629(4) 0.33629(4) 0.33629(4) 0.0401(6) Uani 1 3 d S TU P . . O22 O 0.36606(11) 0.34989(11) 0.31250(11) 0.0436(9) Uani 1 1 d . U . . . O20 O 0.42069(10) 0.35547(11) 0.36380(11) 0.0416(9) Uani 1 1 d . U . . . O24 O 0.31184(11) 0.31184(11) 0.31184(11) 0.0480(17) Uani 1 3 d S TU P . . O2 O 0.56031(12) 0.27152(12) 0.32134(11) 0.0477(10) Uani 1 1 d . U . . . H2 H 0.582534 0.266555 0.312819 0.057 Uiso 1 1 calc R U . . . O1 O 0.58443(12) 0.32595(13) 0.32826(14) 0.0576(12) Uani 1 1 d . U . . . N18 N 0.39193(13) 0.41197(13) 0.28003(14) 0.0408(11) Uani 1 1 d . U . . . H18 H 0.391068 0.394578 0.263066 0.049 Uiso 1 1 calc R U . . . N11 N 0.44493(14) 0.41856(13) 0.32848(15) 0.0463(12) Uani 1 1 d . U . . . H11 H 0.437873 0.440738 0.335522 0.056 Uiso 1 1 calc R U . . . C8 C 0.48136(16) 0.36744(17) 0.35032(15) 0.0425(13) Uani 1 1 d . U . . . C5 C 0.49352(16) 0.29449(17) 0.34475(14) 0.0399(12) Uani 1 1 d . U . . . H5 H 0.497683 0.270587 0.343147 0.048 Uiso 1 1 calc R U . . . C6 C 0.45979(16) 0.30596(16) 0.35289(15) 0.0384(12) Uani 1 1 d . U . . . C7 C 0.45320(16) 0.34321(16) 0.35597(15) 0.0412(13) Uani 1 1 d . U . . . C4 C 0.52198(16) 0.31825(16) 0.33875(15) 0.0405(13) Uani 1 1 d . U . . . C3 C 0.55809(18) 0.30599(17) 0.32916(17) 0.0465(14) Uani 1 1 d . U . . . C9 C 0.51523(16) 0.35514(17) 0.34158(15) 0.0434(13) Uani 1 1 d . U . . . H9 H 0.533208 0.371035 0.337642 0.052 Uiso 1 1 calc R U . . . C12 C 0.45585(16) 0.42070(16) 0.29073(17) 0.0426(13) Uani 1 1 d . U . . . H12 H 0.460169 0.398095 0.282879 0.051 Uiso 1 1 calc R U . . . C17 C 0.42309(15) 0.43478(16) 0.27107(16) 0.0422(13) Uani 1 1 d . U . . . H17 H 0.418567 0.457360 0.278887 0.051 Uiso 1 1 calc R U . . . C10 C 0.47315(18) 0.40614(17) 0.35351(18) 0.0488(15) Uani 1 1 d . U . . . H10A H 0.493465 0.418838 0.349360 0.059 Uiso 1 1 calc R U . . . H10B H 0.466043 0.410802 0.376290 0.059 Uiso 1 1 calc R U . . . C16 C 0.42947(18) 0.43613(19) 0.23061(17) 0.0516(15) Uani 1 1 d . U . . . H16A H 0.432627 0.413570 0.222118 0.062 Uiso 1 1 calc R U . . . H16B H 0.410004 0.445688 0.219620 0.062 Uiso 1 1 calc R U . . . C19 C 0.35665(16) 0.42980(16) 0.27952(17) 0.0426(12) Uani 1 1 d . U . . . H19A H 0.339476 0.413207 0.284074 0.051 Uiso 1 1 calc R U . . . H19B H 0.352682 0.438565 0.257191 0.051 Uiso 1 1 calc R U . . . C13 C 0.48794(19) 0.4431(2) 0.2822(2) 0.0577(18) Uani 1 1 d . U . . . H13A H 0.507410 0.433822 0.293491 0.069 Uiso 1 1 calc R U . . . H13B H 0.484463 0.465636 0.290542 0.069 Uiso 1 1 calc R U . . . C15 C 0.4619(2) 0.4583(2) 0.2222(2) 0.0614(18) Uani 1 1 d . U . . . H15A H 0.457733 0.481374 0.228624 0.074 Uiso 1 1 calc R U . . . H15B H 0.465963 0.457794 0.198229 0.074 Uiso 1 1 calc R U . . . C14 C 0.4950(2) 0.4444(2) 0.2419(2) 0.0598(18) Uani 1 1 d . U . . . H14A H 0.500540 0.422140 0.233881 0.072 Uiso 1 1 calc R U . . . H14B H 0.513887 0.459012 0.237441 0.072 Uiso 1 1 calc R U . . . O3 O 0.6227(3) 0.2426(2) 0.2970(3) 0.157(4) Uani 1 1 d D U . . . O4 O 0.3736(5) 0.3627(5) 0.2151(3) 0.231(7) Uani 1 1 d D U . . . H41 H 0.357(2) 0.374(4) 0.205(3) 0.277 Uiso 1 1 d D U . . . H42 H 0.389(3) 0.357(5) 0.200(2) 0.277 Uiso 1 1 d D U . . . H32 H 0.615(4) 0.253(3) 0.2785(19) 0.277 Uiso 1 1 d D U . . . H31 H 0.639(2) 0.229(3) 0.290(3) 0.277 Uiso 1 1 d D U . . . 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 Cu21 0.0393(5) 0.0394(5) 0.0432(5) 0.0053(4) 0.0040(3) 0.0034(4) P23 0.0401(6) 0.0401(6) 0.0401(6) 0.0002(6) 0.0002(6) 0.0002(6) O22 0.043(2) 0.044(2) 0.044(2) -0.0003(17) 0.0034(17) 0.0004(18) O20 0.0374(19) 0.044(2) 0.043(2) 0.0094(17) 0.0058(16) 0.0063(16) O24 0.0480(17) 0.0480(17) 0.0480(17) -0.0031(19) -0.0031(19) -0.0031(19) O2 0.043(2) 0.055(3) 0.046(2) 0.004(2) 0.0057(19) 0.0087(19) O1 0.047(3) 0.054(3) 0.072(3) 0.003(2) 0.008(2) 0.002(2) N18 0.042(3) 0.037(2) 0.044(3) 0.003(2) 0.007(2) 0.004(2) N11 0.043(3) 0.040(3) 0.056(3) -0.004(2) 0.002(2) 0.004(2) C8 0.039(3) 0.049(3) 0.039(3) 0.002(3) -0.003(2) 0.000(2) C5 0.045(3) 0.044(3) 0.030(3) 0.004(2) 0.000(2) 0.005(2) C6 0.041(3) 0.042(3) 0.032(3) 0.001(2) 0.001(2) 0.001(2) C7 0.040(3) 0.043(3) 0.041(3) 0.004(2) 0.002(2) 0.002(2) C4 0.039(3) 0.046(3) 0.036(3) 0.006(2) -0.004(2) 0.004(2) C3 0.047(3) 0.050(3) 0.042(3) 0.002(3) 0.003(3) 0.005(3) C9 0.041(3) 0.052(3) 0.037(3) 0.007(3) -0.005(2) -0.003(3) C12 0.044(3) 0.036(3) 0.047(3) 0.003(2) 0.003(3) 0.006(2) C17 0.041(3) 0.036(3) 0.050(3) 0.007(2) 0.011(2) 0.007(2) C10 0.050(3) 0.047(3) 0.049(3) 0.004(3) -0.001(3) 0.002(3) C16 0.048(3) 0.057(4) 0.050(3) 0.009(3) 0.004(3) 0.010(3) C19 0.041(3) 0.044(3) 0.043(3) -0.001(2) 0.001(2) 0.005(2) C13 0.046(3) 0.055(4) 0.072(4) 0.015(3) 0.004(3) 0.001(3) C15 0.059(4) 0.066(4) 0.059(4) 0.022(3) 0.021(3) 0.013(3) C14 0.047(4) 0.061(4) 0.071(4) 0.016(3) 0.018(3) 0.009(3) O3 0.094(5) 0.071(5) 0.307(13) -0.047(7) 0.017(8) 0.013(4) O4 0.304(15) 0.248(14) 0.141(8) -0.082(9) 0.027(10) -0.163(12) 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' 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' P P 0.2955 0.4335 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O20 Cu21 O22 91.08(18) . . ? O20 Cu21 N11 92.1(2) . . ? O22 Cu21 N11 162.3(2) . . ? O20 Cu21 N18 163.19(18) . . ? O22 Cu21 N18 88.13(19) . . ? N11 Cu21 N18 83.8(2) . . ? O20 Cu21 O20 104.3(2) . 11 ? O22 Cu21 O20 96.26(17) . 11 ? N11 Cu21 O20 99.77(18) . 11 ? N18 Cu21 O20 92.44(17) . 11 ? O22 P23 O22 112.52(16) 11 12 ? O22 P23 O22 112.52(16) 11 . ? O22 P23 O22 112.52(16) 12 . ? O22 P23 O24 106.22(18) 11 . ? O22 P23 O24 106.22(18) 12 . ? O22 P23 O24 106.22(18) . . ? P23 O22 Cu21 124.1(3) . . ? C7 O20 Cu21 113.0(3) . . ? C7 O20 Cu21 120.4(3) . 12 ? Cu21 O20 Cu21 122.51(19) . 12 ? C3 O2 H2 109.5 . . ? C19 N18 C17 116.0(4) . . ? C19 N18 Cu21 112.1(4) . . ? C17 N18 Cu21 109.0(4) . . ? C19 N18 H18 106.4 . . ? C17 N18 H18 106.4 . . ? Cu21 N18 H18 106.4 . . ? C12 N11 C10 115.1(5) . . ? C12 N11 Cu21 103.4(4) . . ? C10 N11 Cu21 114.0(4) . . ? C12 N11 H11 108.0 . . ? C10 N11 H11 108.0 . . ? Cu21 N11 H11 108.0 . . ? C9 C8 C7 120.4(6) . . ? C9 C8 C10 122.1(6) . . ? C7 C8 C10 117.5(6) . . ? C6 C5 C4 122.4(6) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 119.1(6) . . ? C5 C6 C19 120.2(5) . 12 ? C7 C6 C19 120.6(5) . 12 ? O20 C7 C8 119.7(5) . . ? O20 C7 C6 120.9(5) . . ? C8 C7 C6 119.4(6) . . ? C5 C4 C9 118.2(6) . . ? C5 C4 C3 122.5(6) . . ? C9 C4 C3 119.3(6) . . ? O1 C3 O2 122.1(6) . . ? O1 C3 C4 123.4(6) . . ? O2 C3 C4 114.5(6) . . ? C8 C9 C4 120.5(6) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? N11 C12 C13 117.2(6) . . ? N11 C12 C17 105.0(5) . . ? C13 C12 C17 110.4(5) . . ? N11 C12 H12 108.0 . . ? C13 C12 H12 108.0 . . ? C17 C12 H12 108.0 . . ? N18 C17 C12 108.9(5) . . ? N18 C17 C16 111.4(5) . . ? C12 C17 C16 111.3(5) . . ? N18 C17 H17 108.4 . . ? C12 C17 H17 108.4 . . ? C16 C17 H17 108.4 . . ? C8 C10 N11 113.7(5) . . ? C8 C10 H10A 108.8 . . ? N11 C10 H10A 108.8 . . ? C8 C10 H10B 108.8 . . ? N11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C15 C16 C17 110.6(6) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N18 C19 C6 114.3(5) . 11 ? N18 C19 H19A 108.7 . . ? C6 C19 H19A 108.7 11 . ? N18 C19 H19B 108.7 . . ? C6 C19 H19B 108.7 11 . ? H19A C19 H19B 107.6 . . ? C12 C13 C14 111.4(6) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C16 C15 C14 111.3(6) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C13 C14 C15 110.3(6) . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? H32 O3 H31 107(3) . . ? H41 O4 H42 111(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu21 O20 1.948(4) . ? Cu21 O22 1.992(4) . ? Cu21 N11 2.014(5) . ? Cu21 N18 2.026(5) . ? Cu21 O20 2.169(4) 11 ? P23 O22 1.514(4) 11 ? P23 O22 1.514(4) 12 ? P23 O22 1.514(4) . ? P23 O24 1.585(8) . ? O20 C7 1.333(7) . ? O2 C3 1.325(8) . ? O2 H2 0.9100 . ? O1 C3 1.237(8) . ? N18 C19 1.479(7) . ? N18 C17 1.483(7) . ? N18 H18 0.9100 . ? N11 C12 1.473(8) . ? N11 C10 1.486(8) . ? N11 H11 0.9100 . ? C8 C9 1.388(9) . ? C8 C7 1.406(9) . ? C8 C10 1.485(9) . ? C5 C6 1.368(8) . ? C5 C4 1.406(9) . ? C5 H5 0.9100 . ? C6 C7 1.421(8) . ? C6 C19 1.503(8) 12 ? C4 C9 1.407(8) . ? C4 C3 1.472(9) . ? C9 H9 0.9100 . ? C12 C13 1.498(9) . ? C12 C17 1.524(8) . ? C12 H12 0.9100 . ? C17 C16 1.534(8) . ? C17 H17 0.9100 . ? C10 H10A 0.9100 . ? C10 H10B 0.9100 . ? C16 C15 1.502(9) . ? C16 H16A 0.9100 . ? C16 H16B 0.9100 . ? C19 H19A 0.9100 . ? C19 H19B 0.9100 . ? C13 C14 1.531(10) . ? C13 H13A 0.9100 . ? C13 H13B 0.9100 . ? C15 C14 1.534(10) . ? C15 H15A 0.9100 . ? C15 H15B 0.9100 . ? C14 H14A 0.9100 . ? C14 H14B 0.9100 . ? O3 H32 0.851(3) . ? O3 H31 0.850(3) . ? O4 H41 0.850(3) . ? O4 H42 0.850(3) . ?