#------------------------------------------------------------------------------ #$Date: 2021-09-24 01:23:15 +0300 (Fri, 24 Sep 2021) $ #$Revision: 269266 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564722.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_1564722 loop_ _publ_author_name 'Aldridge, Simon' 'McManus, Caitil\'in' 'Hicks, Jamie' 'Goicoechea, Jose M.' 'Cui, Xianlu' 'Zhao, Lili' 'Frenking, Gernot' _publ_section_title ; Coinage metal aluminyl complexes: probing regiochemistry and mechanism in the insertion and reduction of carbon dioxide ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04676D _journal_year 2021 _chemical_formula_moiety 'C72 H60 Cu4 I2 P4, 0.5(C4 H10 O)' _chemical_formula_sum 'C74 H65 Cu4 I2 O0.5 P4' _chemical_formula_weight 1594.10 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-05-24 deposited with the CCDC. 2021-09-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.636(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.5914(3) _cell_length_b 19.1763(3) _cell_length_c 27.3025(5) _cell_measurement_reflns_used 6766 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 76.4360 _cell_measurement_theta_min 4.0510 _cell_volume 6943.6(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.5035 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.981 _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 0.0231 _diffrn_reflns_av_unetI/netI 0.0330 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 14244 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.424 _diffrn_reflns_theta_min 4.053 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 9.542 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.51420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.525 _exptl_crystal_description block _exptl_crystal_F_000 3180 _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _refine_diff_density_max 1.267 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 418 _refine_ls_number_reflns 7154 _refine_ls_number_restraints 31 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+3.5104P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.0894 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6398 _reflns_number_total 7154 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04676d2.cif _cod_data_source_block S1 _cod_original_sg_symbol_H-M 'C 2/c' _cod_original_formula_sum 'C74 H65 Cu4 I2 O0.50 P4' _cod_database_code 1564722 _shelx_shelxl_version_number 2018/3 _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_estimated_absorpt_t_min 0.516 _shelx_estimated_absorpt_t_max 0.763 _shelx_res_file ; TITL C:\280CMJ~1\280cmjh18_a.res in C2/c C:\280CMJ~1\280cmjh18_a.res created by SHELXL-2018/3 at 21:57:26 on 11-Dec-2018 CELL 1.54184 13.5914 19.1763 27.3025 90.000 102.636 90.000 ZERR 4.0000 0.0003 0.0003 0.0005 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H P CU I O UNIT 296 260 16 16 8 2 MERG 2 FMAP 2 GRID PLAN 20 TEMP -123 SIZE 0.08 0.03 0.03 DFIX 1.53 0.008 C37 C38 C39 C40 DFIX 1.40 0.008 C38 O1 O1 C39 DANG 2.48 0.008 C37 O1 O1 C40 DANG 2.40 0.008 C38 C39 SIMU 0.005 C37 C38 O1 C39 C40 OMIT 0 2 2 OMIT -2 2 2 OMIT 1 1 4 OMIT -1 1 2 L.S. 20 ACTA WGHT 0.050800 3.510400 FVAR 0.13163 I1 5 0.500000 0.380518 0.250000 10.50000 0.04247 0.02067 = 0.03350 0.00000 0.00940 0.00000 I2 5 0.500000 0.732144 0.250000 10.50000 0.04709 0.02062 = 0.06007 0.00000 0.01387 0.00000 CU1 4 0.499704 0.507534 0.292764 11.00000 0.03383 0.02605 = 0.02004 0.00094 0.00591 -0.00105 CU2 4 0.587944 0.606344 0.260379 11.00000 0.02784 0.02509 = 0.03113 -0.00065 0.00558 -0.00243 P1 3 0.498697 0.503641 0.373259 11.00000 0.03586 0.03113 = 0.01994 0.00049 0.00610 -0.00159 P2 3 0.752742 0.618474 0.272978 11.00000 0.02781 0.02204 = 0.03538 0.00004 0.00381 -0.00243 C1 1 0.380182 0.473766 0.386567 11.00000 0.03283 0.03683 = 0.02845 0.01037 0.00545 0.00460 C2 1 0.342532 0.497792 0.426967 11.00000 0.04267 0.06145 = 0.02868 0.00884 0.01098 0.00711 AFIX 43 H2 2 0.378547 0.532363 0.448639 11.00000 -1.20000 AFIX 0 C3 1 0.252676 0.471619 0.435859 11.00000 0.04273 0.07981 = 0.03721 0.01727 0.01440 0.01302 AFIX 43 H3 2 0.227731 0.488205 0.463608 11.00000 -1.20000 AFIX 0 C4 1 0.199674 0.421644 0.404498 11.00000 0.03270 0.07268 = 0.06460 0.02764 0.01160 0.00317 AFIX 43 H4 2 0.138770 0.403414 0.410964 11.00000 -1.20000 AFIX 0 C5 1 0.234800 0.398043 0.363778 11.00000 0.03821 0.05033 = 0.06625 0.00958 0.00543 -0.00459 AFIX 43 H5 2 0.197515 0.364072 0.342015 11.00000 -1.20000 AFIX 0 C6 1 0.325143 0.423928 0.354380 11.00000 0.03584 0.03970 = 0.04438 0.00430 0.00543 -0.00052 AFIX 43 H6 2 0.349044 0.407709 0.326223 11.00000 -1.20000 AFIX 0 C7 1 0.593425 0.446038 0.410642 11.00000 0.03838 0.03408 = 0.02632 -0.00371 0.00393 0.00032 C8 1 0.687478 0.442421 0.398703 11.00000 0.04167 0.06088 = 0.03938 -0.00036 0.01021 0.00503 AFIX 43 H8 2 0.700698 0.468939 0.371462 11.00000 -1.20000 AFIX 0 C9 1 0.762419 0.400071 0.426522 11.00000 0.04218 0.07093 = 0.06041 -0.01037 0.00719 0.01316 AFIX 43 H9 2 0.826956 0.398360 0.418500 11.00000 -1.20000 AFIX 0 C10 1 0.743549 0.360454 0.465775 11.00000 0.05590 0.05052 = 0.05312 -0.00423 -0.00933 0.01571 AFIX 43 H10 2 0.795013 0.331510 0.484513 11.00000 -1.20000 AFIX 0 C11 1 0.649904 0.362870 0.477821 11.00000 0.05717 0.04379 = 0.03976 0.00425 -0.00056 0.00441 AFIX 43 H11 2 0.636880 0.335527 0.504720 11.00000 -1.20000 AFIX 0 C12 1 0.574924 0.405479 0.450401 11.00000 0.04280 0.03541 = 0.03222 0.00294 0.00439 0.00046 AFIX 43 H12 2 0.510608 0.407127 0.458672 11.00000 -1.20000 AFIX 0 C13 1 0.522770 0.587457 0.405687 11.00000 0.04007 0.03440 = 0.02507 -0.00311 0.01080 -0.00299 C14 1 0.470121 0.645439 0.383189 11.00000 0.04913 0.03960 = 0.03651 -0.00405 0.00363 0.00264 AFIX 43 H14 2 0.421786 0.640251 0.352506 11.00000 -1.20000 AFIX 0 C15 1 0.487553 0.710801 0.405155 11.00000 0.06351 0.03792 = 0.05066 -0.00361 0.01008 0.00464 AFIX 43 H15 2 0.450768 0.750085 0.389742 11.00000 -1.20000 AFIX 0 C16 1 0.559266 0.718683 0.449950 11.00000 0.06246 0.04000 = 0.04688 -0.01284 0.01626 -0.00676 AFIX 43 H16 2 0.570898 0.763332 0.465193 11.00000 -1.20000 AFIX 0 C17 1 0.613211 0.661875 0.472107 11.00000 0.05908 0.04869 = 0.03040 -0.01126 0.00856 -0.00913 AFIX 43 H17 2 0.663079 0.667464 0.502206 11.00000 -1.20000 AFIX 0 C18 1 0.594478 0.596235 0.450285 11.00000 0.04980 0.04135 = 0.02602 -0.00292 0.00690 -0.00452 AFIX 43 H18 2 0.630976 0.557001 0.465967 11.00000 -1.20000 AFIX 0 C19 1 0.827933 0.539397 0.286148 11.00000 0.03592 0.02470 = 0.03705 0.00120 0.00542 -0.00121 C20 1 0.932176 0.540504 0.303072 11.00000 0.03722 0.02766 = 0.11466 0.00932 -0.00917 0.00121 AFIX 43 H20 2 0.966603 0.583863 0.308722 11.00000 -1.20000 AFIX 0 C21 1 0.986281 0.478542 0.311770 11.00000 0.04442 0.03432 = 0.12715 0.00843 -0.01600 0.00764 AFIX 43 H21 2 1.057620 0.479937 0.322525 11.00000 -1.20000 AFIX 0 C22 1 0.937212 0.414711 0.304911 11.00000 0.06091 0.02800 = 0.06117 0.00848 0.01154 0.01119 AFIX 43 H22 2 0.974048 0.372404 0.311682 11.00000 -1.20000 AFIX 0 C23 1 0.834822 0.413895 0.288220 11.00000 0.05914 0.02258 = 0.07509 -0.00332 0.02175 -0.00496 AFIX 43 H23 2 0.800623 0.370435 0.282763 11.00000 -1.20000 AFIX 0 C24 1 0.779623 0.475474 0.279053 11.00000 0.04171 0.02752 = 0.05889 -0.00523 0.01355 -0.00614 AFIX 43 H24 2 0.708391 0.473612 0.267863 11.00000 -1.20000 AFIX 0 C25 1 0.810256 0.678147 0.323009 11.00000 0.03160 0.02409 = 0.03698 0.00020 0.00559 -0.00169 C26 1 0.898512 0.715794 0.322996 11.00000 0.03225 0.02703 = 0.04053 -0.00084 0.00883 -0.00444 AFIX 43 H26 2 0.929838 0.712288 0.295213 11.00000 -1.20000 AFIX 0 C27 1 0.940320 0.758052 0.363209 11.00000 0.03675 0.03432 = 0.04511 -0.00356 0.00563 -0.00864 AFIX 43 H27 2 0.999319 0.784389 0.362763 11.00000 -1.20000 AFIX 0 C28 1 0.895588 0.761776 0.404245 11.00000 0.05130 0.04903 = 0.04168 -0.01259 0.00647 -0.01206 AFIX 43 H28 2 0.925425 0.789537 0.432404 11.00000 -1.20000 AFIX 0 C29 1 0.808266 0.725480 0.404364 11.00000 0.05954 0.05388 = 0.04132 -0.00820 0.02019 -0.01483 AFIX 43 H29 2 0.777605 0.728781 0.432386 11.00000 -1.20000 AFIX 0 C30 1 0.765025 0.684211 0.363797 11.00000 0.03786 0.04286 = 0.04272 -0.00177 0.01207 -0.01001 AFIX 43 H30 2 0.704130 0.659905 0.363822 11.00000 -1.20000 AFIX 0 C31 1 0.783509 0.652912 0.215972 11.00000 0.02958 0.02850 = 0.03503 0.00129 0.00225 -0.00406 C32 1 0.804840 0.608196 0.179416 11.00000 0.03735 0.03166 = 0.04315 -0.00228 0.00680 -0.00374 AFIX 43 H32 2 0.811239 0.559518 0.185781 11.00000 -1.20000 AFIX 0 C33 1 0.816776 0.634615 0.133679 11.00000 0.04507 0.04979 = 0.04182 -0.00760 0.01283 -0.00869 AFIX 43 H33 2 0.830667 0.603761 0.108818 11.00000 -1.20000 AFIX 0 C34 1 0.808685 0.704816 0.124109 11.00000 0.05173 0.05286 = 0.03653 0.00384 0.00809 -0.01368 AFIX 43 H34 2 0.816752 0.722517 0.092726 11.00000 -1.20000 AFIX 0 C35 1 0.788740 0.749696 0.160332 11.00000 0.06858 0.03476 = 0.04895 0.00844 0.00882 -0.00564 AFIX 43 H35 2 0.783815 0.798404 0.153915 11.00000 -1.20000 AFIX 0 C36 1 0.775892 0.724058 0.205934 11.00000 0.05705 0.02994 = 0.04043 0.00080 0.00939 -0.00119 AFIX 43 H36 2 0.761779 0.755273 0.230532 11.00000 -1.20000 PART -1 AFIX 0 C37 1 -0.004740 0.406039 0.557850 10.25000 0.03025 0.10120 = 0.08720 0.02941 -0.00915 -0.01429 AFIX 137 H37A 2 -0.072376 0.426430 0.548520 10.25000 -1.50000 H37B 2 0.017383 0.405129 0.594501 10.25000 -1.50000 H37C 2 -0.006280 0.358378 0.544750 10.25000 -1.50000 AFIX 0 O1 6 0.029110 0.475834 0.487750 10.25000 0.07329 0.10746 = 0.10631 0.05283 0.01733 -0.01626 C40 1 -0.029080 0.577619 0.433907 10.25000 0.04467 0.11662 = 0.10853 0.06336 0.02227 -0.01290 AFIX 137 H40A 2 0.036518 0.596821 0.431502 10.25000 -1.50000 H40B 2 -0.077760 0.615679 0.432431 10.25000 -1.50000 H40C 2 -0.052779 0.545419 0.405941 10.25000 -1.50000 AFIX 0 C38 1 0.067509 0.449307 0.536013 10.25000 0.06895 0.10624 = 0.10460 0.04737 0.01062 -0.01734 AFIX 23 H38A 2 0.090392 0.488951 0.558900 10.25000 -1.20000 H38B 2 0.127444 0.420470 0.534990 10.25000 -1.20000 AFIX 0 C39 1 -0.018702 0.539262 0.482645 10.25000 0.05880 0.10994 = 0.10993 0.04579 0.01409 -0.02015 AFIX 23 H39A 2 0.017774 0.570052 0.509709 10.25000 -1.20000 H39B 2 -0.087268 0.532210 0.488632 10.25000 -1.20000 AFIX 0 HKLF 4 REM C:\280CMJ~1\280cmjh18_a.res in C2/c REM wR2 = 0.0894, GooF = S = 1.047, Restrained GooF = 1.052 for all data REM R1 = 0.0317 for 6398 Fo > 4sig(Fo) and 0.0367 for all 7154 data REM 418 parameters refined using 31 restraints END WGHT 0.0498 3.6883 REM Highest difference peak 1.267, deepest hole -0.385, 1-sigma level 0.088 Q1 1 -0.0733 0.5035 0.4944 11.00000 0.05 1.27 Q2 1 -0.0004 0.5357 0.4640 11.00000 0.05 1.11 Q3 1 0.0000 0.5000 0.5000 10.50000 0.05 0.90 Q4 1 -0.0365 0.5445 0.4232 11.00000 0.05 0.87 Q5 1 -0.0237 0.4869 0.4944 11.00000 0.05 0.87 Q6 1 0.0051 0.4201 0.5461 11.00000 0.05 0.78 Q7 1 0.0163 0.4044 0.5440 11.00000 0.05 0.76 Q8 1 0.5617 0.3798 0.2562 11.00000 0.05 0.53 Q9 1 0.5628 0.7303 0.2561 11.00000 0.05 0.45 Q10 1 0.5000 0.5227 0.2500 10.50000 0.05 0.39 Q11 1 0.9441 0.4512 0.3020 11.00000 0.05 0.38 Q12 1 0.5109 0.6039 0.2119 11.00000 0.05 0.37 Q13 1 0.6693 0.6051 0.2683 11.00000 0.05 0.32 Q14 1 0.5000 0.5820 0.2500 10.50000 0.05 0.32 Q15 1 0.4017 0.6939 0.2578 11.00000 0.05 0.30 Q16 1 0.4352 0.5119 0.2841 11.00000 0.05 0.29 Q17 1 0.4103 0.5102 0.2429 11.00000 0.05 0.29 Q18 1 0.5150 0.6521 0.2308 11.00000 0.05 0.29 Q19 1 0.8906 0.4179 0.2810 11.00000 0.05 0.29 Q20 1 0.7744 0.6400 0.2375 11.00000 0.05 0.29 ; _shelx_res_checksum 45845 _shelx_hkl_file ; 0 0 -3 0.88 1.11 0 0 -4 2726.37 33.31 0 0 -5 2.98 2.11 0 0 -6 8030.21 70.37 0 0 -7 1.07 2.08 0 0 -8 2487.24 45.46 0 0 -9 5.70 3.51 0 0 9 0.21 1.34 0 0 -10 520.00 23.84 0 0 10 538.65 14.18 0 0 -11 -0.23 2.59 0 0 11 1.31 1.87 0 0 12 29.34 4.55 0 0 12 30.56 4.12 0 0 -12 30.04 6.45 0 0 13 0.04 2.27 0 0 13 -0.66 2.11 0 0 14 569.18 18.44 0 0 14 605.62 20.54 0 0 15 1.31 2.78 0 0 15 0.63 1.79 0 0 16 586.27 20.58 0 0 16 567.64 21.85 0 0 17 -1.12 2.63 0 0 17 -2.58 2.88 0 0 18 927.61 30.24 0 0 19 -0.71 3.10 0 0 20 459.04 22.83 0 0 21 -3.38 2.93 0 0 22 263.96 18.38 0 0 23 6.44 3.61 0 0 25 2.51 1.84 0 0 26 659.92 14.80 0 0 27 1.49 1.72 0 0 28 41.81 3.73 0 0 29 -1.09 1.55 0 0 30 18.14 2.45 0 0 31 -0.18 1.26 0 0 32 37.79 2.90 0 0 33 0.38 1.08 0 2 0 1979.29 25.90 0 2 1 1173.03 19.85 0 -2 -1 1211.73 19.91 0 -2 -2 7.50 2.03 0 -2 -3 527.21 15.07 0 -2 3 522.65 17.83 0 -2 4 19.30 3.85 0 -2 5 26.03 4.74 0 -2 6 4.25 3.19 0 -2 7 37.04 6.76 0 2 -8 967.57 22.59 0 -2 8 937.98 17.49 0 -2 9 22.37 3.42 0 2 9 20.55 2.87 0 -2 9 12.78 2.70 0 2 -9 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3 7 7.35 1.89 -11 -3 -7 12.09 3.82 11 -3 7 14.14 2.53 -11 3 -7 15.98 2.98 -11 3 -7 11.44 3.50 11 3 8 177.74 7.54 11 -3 8 176.01 7.64 -11 3 -8 185.43 8.19 -11 3 -8 165.48 8.97 11 3 9 11.26 2.42 11 -3 9 12.16 2.45 -11 3 -9 11.86 2.48 11 3 10 297.26 9.66 11 -3 10 307.06 9.84 11 3 11 25.24 3.03 11 -3 11 22.67 2.94 11 3 12 451.54 11.47 11 -3 12 412.64 10.89 11 3 13 3.34 1.71 11 -3 13 3.90 1.70 11 3 14 126.56 5.95 11 -3 14 141.56 6.05 11 3 15 5.19 1.71 11 -3 15 3.55 1.61 11 3 16 30.29 2.83 11 -3 16 30.79 2.76 11 3 17 9.93 1.75 11 3 17 11.25 1.79 11 -3 17 7.85 1.59 11 3 18 20.24 2.00 11 -3 18 20.10 1.92 11 3 18 21.92 2.00 11 3 19 13.88 1.46 11 3 19 15.09 1.57 11 -3 19 14.87 1.51 11 -3 20 26.54 1.61 11 3 20 28.49 1.79 -11 5 29 10.13 1.38 -11 5 28 10.85 1.61 -11 5 27 21.74 2.32 -11 5 26 2.98 1.44 -11 5 25 59.19 3.98 -11 -5 24 62.06 4.46 -11 5 24 63.47 4.31 -11 5 24 65.00 4.19 -11 5 23 97.45 6.16 -11 -5 23 101.66 5.85 -11 5 23 100.39 5.40 -11 -5 23 99.37 5.21 -11 5 23 89.48 5.22 -11 5 22 8.23 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34.08 4.81 -11 9 -2 770.75 15.98 -11 9 -2 742.82 18.48 -11 9 -3 22.51 3.27 -11 9 -3 22.11 4.03 -11 9 -4 449.88 11.79 -11 9 -4 458.96 14.23 -11 9 -5 2.82 1.67 -11 9 -5 -1.67 2.37 -11 9 -6 428.05 10.93 -11 9 -6 438.23 13.52 -11 9 -7 7.00 2.10 -11 9 -7 5.34 2.48 -11 9 -8 349.74 11.64 -11 9 -9 3.48 2.20 11 -9 9 4.32 1.94 -11 9 -10 227.01 8.77 11 -9 10 226.93 8.00 -11 9 -11 8.75 2.47 11 -9 11 4.50 1.63 11 -9 12 30.16 2.87 11 9 13 2.96 1.25 11 -9 13 3.31 1.59 11 -9 14 77.39 3.71 11 9 14 88.11 4.10 11 9 15 3.80 1.25 11 -9 15 2.44 1.05 11 9 16 179.52 4.87 11 9 17 2.98 0.81 -11 11 24 2.35 0.91 -11 11 24 2.44 0.90 -11 11 23 12.97 1.51 -11 11 23 12.23 1.68 -11 11 22 20.26 2.17 -11 11 21 24.99 3.04 -11 11 21 25.33 2.61 -11 11 20 40.13 3.73 -11 11 20 49.38 3.56 -11 11 19 43.90 4.01 -11 11 19 39.03 3.33 -11 11 18 18.68 3.03 -11 11 18 22.00 2.94 -11 11 17 46.59 4.40 -11 11 17 58.28 4.36 -11 11 16 6.81 2.20 -11 11 16 12.43 2.46 -11 11 15 85.07 6.01 -11 11 15 94.33 5.65 -11 11 14 120.08 7.03 -11 11 14 120.88 6.48 -11 11 13 90.43 6.32 -11 11 13 107.16 6.16 -11 11 12 334.69 11.81 -11 11 12 356.97 10.94 -11 11 11 132.69 6.83 -11 11 10 34.96 3.93 -11 11 10 29.86 3.53 -11 11 9 138.01 7.49 -11 11 9 137.52 6.94 -11 11 8 14.77 3.16 -11 11 8 11.69 2.48 -11 11 7 85.32 6.14 -11 11 7 84.72 5.42 -11 11 6 38.83 3.89 -11 11 6 37.06 4.22 -11 11 6 41.12 3.88 -11 11 5 49.71 4.39 -11 11 5 58.28 5.31 -11 11 4 66.55 4.89 -11 11 4 69.89 5.85 -11 11 3 27.56 3.37 -11 11 3 31.50 4.36 -11 11 2 8.82 2.08 -11 11 2 5.63 2.67 -11 11 1 6.13 2.02 -11 11 1 5.88 2.32 -11 11 0 38.49 3.55 -11 11 0 40.06 4.64 -11 11 -1 9.39 2.22 -11 11 -1 6.02 2.57 -11 11 -2 18.47 2.68 -11 11 -2 13.04 3.02 -11 11 -3 4.18 2.06 -11 11 -4 51.06 4.85 11 -11 4 47.55 4.24 -11 11 -5 9.67 2.61 11 -11 5 10.48 2.36 -11 11 -6 75.36 5.52 11 -11 6 83.25 5.17 -11 11 -7 20.22 3.10 11 -11 7 23.92 2.97 -11 11 -8 11.35 2.54 11 -11 8 15.65 2.60 -11 11 -9 3.06 1.68 11 -11 9 5.00 1.86 -11 11 -10 44.34 3.68 11 -11 10 47.54 3.72 11 11 11 14.40 1.86 -11 11 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1.53 1.89 11 -13 2 2.52 1.57 -11 13 -3 34.57 3.82 11 -13 3 35.91 3.31 -11 13 -4 52.42 4.50 11 -13 4 62.16 4.23 -11 13 -5 40.77 3.84 11 -13 5 48.76 3.79 -11 13 -6 59.42 4.47 11 -13 6 68.68 4.28 -11 13 -7 20.40 2.91 11 -13 7 23.22 2.81 -11 13 -8 38.12 3.37 11 -13 8 42.94 3.37 -11 13 -9 5.68 1.65 11 -13 9 5.65 1.64 -11 13 -10 96.87 4.11 11 -13 10 109.36 4.58 11 -13 11 1.88 1.22 11 -13 12 164.09 4.73 11 -13 13 1.78 0.91 -11 15 19 53.11 2.51 -11 15 19 54.25 2.66 -11 15 18 11.36 1.49 -11 15 18 13.59 1.65 -11 15 17 21.31 2.12 -11 15 16 16.69 2.02 -11 15 15 47.66 3.21 -11 15 14 68.05 3.66 -11 15 14 71.03 3.92 -11 15 13 31.71 2.63 -11 15 13 30.90 2.83 -11 15 12 104.70 4.54 -11 15 12 109.44 4.92 -11 15 11 3.85 1.57 -11 15 11 3.50 1.75 -11 15 11 4.07 1.66 -11 15 10 179.28 5.99 -11 15 10 183.32 6.78 -11 15 10 184.14 6.45 -11 15 9 10.24 1.79 -11 15 9 9.06 2.25 -11 15 9 10.94 2.10 -11 15 8 44.13 3.15 -11 15 8 39.62 3.53 -11 15 8 39.89 3.17 -11 15 7 41.20 3.83 -11 15 7 35.85 2.91 -11 15 6 64.68 4.62 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21 8.84 1.63 -13 9 20 150.38 5.15 -13 9 20 158.37 5.53 -13 9 19 1.37 1.32 -13 9 19 1.01 1.24 -13 9 18 300.64 8.33 -13 9 17 6.64 1.99 -13 9 16 330.07 9.24 -13 9 15 -0.77 1.56 -13 9 15 2.55 1.74 -13 9 14 179.38 7.07 -13 9 14 181.11 7.11 -13 9 13 1.26 2.02 -13 9 13 -1.14 1.53 -13 9 12 95.17 5.40 -13 9 12 86.75 5.10 -13 9 11 6.71 2.02 -13 9 11 7.76 2.02 -13 9 10 183.70 7.50 -13 9 10 173.59 7.11 -13 9 9 2.01 2.05 -13 9 9 2.40 1.70 -13 9 8 278.67 9.25 -13 9 8 280.31 9.44 -13 9 8 280.23 8.85 -13 9 7 36.77 3.79 -13 9 7 35.63 3.80 -13 9 6 325.25 9.93 -13 9 6 333.09 10.83 -13 9 5 0.24 1.81 -13 9 5 1.71 2.05 -13 9 4 268.04 8.88 -13 9 4 259.90 9.85 -13 9 3 7.61 2.18 -13 9 3 10.17 2.81 -13 9 2 303.50 9.25 -13 9 2 309.78 10.85 -13 9 1 6.84 2.42 -13 9 1 4.68 2.73 -13 9 0 519.35 11.63 -13 9 0 535.80 13.99 -13 9 -1 8.23 2.36 -13 9 -1 6.90 2.71 -13 9 -2 199.14 6.91 -13 9 -2 215.67 8.76 -13 9 -3 1.67 1.26 -13 9 -3 1.98 1.87 -13 9 -4 31.25 2.79 -13 9 -4 35.19 3.82 -13 9 -5 6.36 1.66 -13 9 -5 5.95 2.28 13 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9.18 1.27 -15 9 13 11.72 1.57 -15 9 13 10.45 1.34 -15 9 12 2.29 1.15 -15 9 12 2.04 0.97 -15 9 11 8.45 1.50 -15 9 11 7.60 1.24 -15 9 10 26.21 2.31 -15 9 9 26.21 2.25 -15 9 8 28.29 2.39 -15 9 7 14.00 1.89 -15 9 6 34.23 2.58 -15 9 5 3.32 1.28 -15 9 4 42.58 2.70 15 -9 -4 37.03 2.31 -15 9 3 1.38 1.15 15 -9 -3 1.30 1.05 -15 9 2 89.60 3.65 15 -9 -2 85.01 3.42 -15 9 1 3.56 1.21 15 -9 -1 1.87 1.11 -15 9 0 160.08 4.43 15 -9 0 163.25 4.63 15 -9 1 15.77 1.68 15 -9 2 69.74 2.95 15 -9 3 11.25 1.30 -15 11 12 97.41 3.01 -15 11 11 60.48 2.49 -15 11 10 35.37 2.00 -15 11 9 68.16 2.76 -15 11 8 3.40 1.00 -15 11 7 67.94 2.75 -15 11 6 10.53 1.29 -15 11 5 31.47 1.88 -15 11 4 41.93 2.02 -16 0 18 47.27 2.41 -16 0 17 1.88 0.98 -16 0 16 105.15 3.86 -16 0 15 0.20 0.99 -16 0 14 42.45 2.64 -16 0 13 1.55 1.01 -16 0 12 1.47 1.10 -16 0 11 -1.24 0.92 16 0 -4 24.46 2.04 16 0 -3 0.90 1.00 16 0 -2 181.20 5.07 16 0 -1 2.13 1.21 16 0 0 232.98 5.49 16 0 1 2.60 1.00 16 0 2 33.11 2.05 16 0 3 2.73 0.89 16 0 4 7.73 1.03 16 0 5 0.06 0.56 -16 2 18 25.89 1.79 -16 2 17 5.49 1.09 -16 2 16 0.89 0.87 -16 2 15 22.02 1.94 -16 2 14 20.57 1.96 -16 2 13 15.39 1.76 -16 2 12 104.82 4.03 -16 2 11 11.71 1.55 -16 2 10 82.27 3.32 -16 2 9 14.30 1.67 -16 2 8 6.29 1.32 -16 2 7 33.36 2.41 -16 2 6 19.63 1.96 16 2 -5 16.83 1.66 -16 2 5 17.63 1.93 16 2 -4 34.73 2.24 16 -2 -4 40.57 2.66 -16 2 4 33.31 2.43 16 2 -3 1.24 0.82 16 -2 -3 0.95 0.88 16 2 -2 -0.63 0.79 16 -2 -2 1.23 0.98 16 2 -1 24.03 1.87 16 -2 -1 26.28 2.07 16 2 0 8.68 1.26 16 -2 0 5.39 1.17 16 2 1 9.27 1.21 16 -2 1 8.23 1.27 16 2 2 0.61 0.73 16 -2 2 -0.75 0.72 16 2 3 20.50 1.49 16 -2 3 22.74 1.67 16 2 4 4.79 0.80 16 -2 4 5.86 0.93 -16 4 17 5.98 1.08 -16 4 16 1.86 0.85 -16 4 15 9.04 1.26 -16 4 14 12.91 1.50 -16 4 13 20.95 1.64 -16 4 13 22.10 1.90 -16 4 12 62.57 2.81 -16 4 12 60.83 2.89 -16 4 11 24.22 2.02 -16 4 10 12.49 1.65 16 4 -9 9.48 1.17 -16 4 9 11.74 1.55 16 4 -8 -1.45 0.77 -16 4 8 -1.82 1.25 16 4 -7 6.23 1.02 -16 4 7 12.43 1.68 16 4 -6 2.09 0.76 -16 4 6 6.43 1.37 16 4 -5 5.49 1.01 -16 4 5 4.38 1.38 16 4 -4 0.93 0.65 16 -4 -4 0.91 0.82 -16 4 4 1.67 1.10 16 4 -3 0.92 0.76 16 -4 -3 -0.31 0.80 16 4 -2 4.35 0.98 16 -4 -2 2.06 0.90 -16 4 2 1.90 1.09 16 4 -1 9.49 1.07 16 -4 -1 15.35 1.57 16 4 0 33.04 1.79 16 -4 0 37.93 2.22 16 4 1 1.02 0.57 16 -4 1 1.32 0.74 16 -4 2 9.25 1.09 16 -4 3 0.67 0.61 -16 6 13 25.84 1.75 -16 6 12 48.44 2.42 -16 6 11 30.72 2.07 -16 6 10 26.06 2.03 -16 6 9 23.64 2.02 -16 6 8 11.55 1.61 -16 6 7 38.35 2.49 16 -6 -6 16.17 1.52 -16 6 6 19.81 1.96 16 -6 -5 66.94 2.77 -16 6 5 68.67 3.16 16 -6 -4 6.71 1.12 -16 6 4 10.17 1.59 16 -6 -3 41.32 2.12 -16 6 3 39.48 2.39 16 -6 -2 2.68 0.74 -16 6 2 3.81 1.35 16 -6 -1 48.49 2.12 16 -6 0 12.89 1.38 16 -6 1 55.55 2.51 -16 8 11 7.03 1.23 -16 8 10 9.60 1.25 -16 8 9 2.98 0.94 -16 8 8 54.78 2.49 -16 8 7 1.43 1.07 -16 8 6 56.79 2.49 -16 8 5 0.72 0.86 -16 8 4 29.81 1.81 17 -1 -10 2.40 0.71 17 -1 -9 -0.58 0.60 17 -1 -8 3.93 0.76 17 1 -7 0.65 0.53 17 -1 -7 1.17 0.61 17 -1 -6 0.86 0.62 17 -1 -5 -0.31 0.56 17 -1 -4 0.75 0.57 17 -3 -8 5.43 0.89 17 -3 -7 57.48 2.23 0 0 0 0.00 0.00 TITL 280cmjh18 in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 13.591361 19.176283 27.302458 90.0000 102.6364 90.0000 ZERR 8.00 0.000270 0.000317 0.000503 0.0000 0.0019 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O Al P Cu UNIT 320.00 320.00 16.00 8.00 8.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 73349 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 I1 I 0.500000 0.38052(2) 0.250000 0.03205(7) Uani 1 2 d S T P . . I2 I 0.500000 0.73214(2) 0.250000 0.04226(8) Uani 1 2 d S T P . . Cu1 Cu 0.49970(3) 0.50753(2) 0.29276(2) 0.02664(9) Uani 1 1 d . . . . . Cu2 Cu 0.58794(3) 0.60634(2) 0.26038(2) 0.02815(10) Uani 1 1 d . . . . . P1 P 0.49870(5) 0.50364(4) 0.37326(2) 0.02898(14) Uani 1 1 d . . . . . P2 P 0.75274(5) 0.61847(4) 0.27298(3) 0.02888(14) Uani 1 1 d . . . . . C1 C 0.3802(2) 0.47377(17) 0.38657(10) 0.0329(6) Uani 1 1 d . . . . . C2 C 0.3425(3) 0.4978(2) 0.42697(12) 0.0438(8) Uani 1 1 d . . . . . H2 H 0.378547 0.532363 0.448639 0.053 Uiso 1 1 calc R U . . . C3 C 0.2527(3) 0.4716(3) 0.43586(13) 0.0524(10) Uani 1 1 d . . . . . H3 H 0.227731 0.488205 0.463608 0.063 Uiso 1 1 calc R U . . . C4 C 0.1997(3) 0.4216(3) 0.40450(16) 0.0565(10) Uani 1 1 d . . . . . H4 H 0.138770 0.403414 0.410964 0.068 Uiso 1 1 calc R U . . . C5 C 0.2348(3) 0.3980(2) 0.36378(16) 0.0525(9) Uani 1 1 d . . . . . H5 H 0.197515 0.364072 0.342015 0.063 Uiso 1 1 calc R U . . . C6 C 0.3251(2) 0.42393(19) 0.35438(13) 0.0405(7) Uani 1 1 d . . . . . H6 H 0.349044 0.407709 0.326223 0.049 Uiso 1 1 calc R U . . . C7 C 0.5934(2) 0.44604(16) 0.41064(11) 0.0334(6) Uani 1 1 d . . . . . C8 C 0.6875(3) 0.4424(2) 0.39870(13) 0.0471(8) Uani 1 1 d . . . . . H8 H 0.700698 0.468939 0.371462 0.057 Uiso 1 1 calc R U . . . C9 C 0.7624(3) 0.4001(3) 0.42652(16) 0.0585(10) Uani 1 1 d . . . . . H9 H 0.826956 0.398360 0.418500 0.070 Uiso 1 1 calc R U . . . C10 C 0.7435(3) 0.3605(2) 0.46577(15) 0.0564(10) Uani 1 1 d . . . . . H10 H 0.795013 0.331510 0.484513 0.068 Uiso 1 1 calc R U . . . C11 C 0.6499(3) 0.3629(2) 0.47782(13) 0.0486(8) Uani 1 1 d . . . . . H11 H 0.636880 0.335527 0.504720 0.058 Uiso 1 1 calc R U . . . C12 C 0.5749(3) 0.40548(18) 0.45040(11) 0.0374(6) Uani 1 1 d . . . . . H12 H 0.510608 0.407127 0.458672 0.045 Uiso 1 1 calc R U . . . C13 C 0.5228(2) 0.58746(17) 0.40569(10) 0.0326(6) Uani 1 1 d . . . . . C14 C 0.4701(3) 0.64544(19) 0.38319(12) 0.0426(7) Uani 1 1 d . . . . . H14 H 0.421786 0.640251 0.352506 0.051 Uiso 1 1 calc R U . . . C15 C 0.4876(3) 0.7108(2) 0.40516(15) 0.0511(8) Uani 1 1 d . . . . . H15 H 0.450768 0.750085 0.389742 0.061 Uiso 1 1 calc R U . . . C16 C 0.5593(3) 0.7187(2) 0.44995(14) 0.0491(8) Uani 1 1 d . . . . . H16 H 0.570898 0.763332 0.465193 0.059 Uiso 1 1 calc R U . . . C17 C 0.6132(3) 0.6619(2) 0.47211(12) 0.0462(8) Uani 1 1 d . . . . . H17 H 0.663079 0.667464 0.502206 0.055 Uiso 1 1 calc R U . . . C18 C 0.5945(3) 0.59623(19) 0.45028(11) 0.0393(7) Uani 1 1 d . . . . . H18 H 0.630976 0.557001 0.465967 0.047 Uiso 1 1 calc R U . . . C19 C 0.8279(2) 0.53940(16) 0.28615(11) 0.0329(6) Uani 1 1 d . . . . . C20 C 0.9322(3) 0.5405(2) 0.3031(2) 0.0638(13) Uani 1 1 d . . . . . H20 H 0.966603 0.583863 0.308722 0.077 Uiso 1 1 calc R U . . . C21 C 0.9863(3) 0.4785(2) 0.3118(2) 0.0740(16) Uani 1 1 d . . . . . H21 H 1.057620 0.479937 0.322525 0.089 Uiso 1 1 calc R U . . . C22 C 0.9372(3) 0.41471(19) 0.30491(15) 0.0503(9) Uani 1 1 d . . . . . H22 H 0.974048 0.372404 0.311682 0.060 Uiso 1 1 calc R U . . . C23 C 0.8348(3) 0.41389(19) 0.28822(16) 0.0512(9) Uani 1 1 d . . . . . H23 H 0.800623 0.370435 0.282763 0.061 Uiso 1 1 calc R U . . . C24 C 0.7796(3) 0.47547(18) 0.27905(14) 0.0423(7) Uani 1 1 d . . . . . H24 H 0.708391 0.473612 0.267863 0.051 Uiso 1 1 calc R U . . . C25 C 0.8103(2) 0.67815(15) 0.32301(11) 0.0312(5) Uani 1 1 d . . . . . C26 C 0.8985(2) 0.71579(16) 0.32300(11) 0.0331(6) Uani 1 1 d . . . . . H26 H 0.929838 0.712288 0.295213 0.040 Uiso 1 1 calc R U . . . C27 C 0.9403(2) 0.75805(18) 0.36321(13) 0.0392(7) Uani 1 1 d . . . . . H27 H 0.999319 0.784389 0.362763 0.047 Uiso 1 1 calc R U . . . C28 C 0.8956(3) 0.7618(2) 0.40424(13) 0.0479(8) Uani 1 1 d . . . . . H28 H 0.925425 0.789537 0.432404 0.057 Uiso 1 1 calc R U . . . C29 C 0.8083(3) 0.7255(2) 0.40436(14) 0.0502(9) Uani 1 1 d . . . . . H29 H 0.777605 0.728781 0.432386 0.060 Uiso 1 1 calc R U . . . C30 C 0.7650(2) 0.68421(19) 0.36380(12) 0.0406(7) Uani 1 1 d . . . . . H30 H 0.704130 0.659905 0.363822 0.049 Uiso 1 1 calc R U . . . C31 C 0.7835(2) 0.65291(16) 0.21597(11) 0.0318(6) Uani 1 1 d . . . . . C32 C 0.8048(2) 0.60820(18) 0.17942(12) 0.0377(6) Uani 1 1 d . . . . . H32 H 0.811239 0.559518 0.185781 0.045 Uiso 1 1 calc R U . . . C33 C 0.8168(3) 0.6346(2) 0.13368(13) 0.0450(8) Uani 1 1 d . . . . . H33 H 0.830667 0.603761 0.108818 0.054 Uiso 1 1 calc R U . . . C34 C 0.8087(3) 0.7048(2) 0.12411(13) 0.0473(8) Uani 1 1 d . . . . . H34 H 0.816752 0.722517 0.092726 0.057 Uiso 1 1 calc R U . . . C35 C 0.7887(3) 0.7497(2) 0.16033(14) 0.0514(9) Uani 1 1 d . . . . . H35 H 0.783815 0.798404 0.153915 0.062 Uiso 1 1 calc R U . . . C36 C 0.7759(3) 0.72406(18) 0.20593(13) 0.0427(7) Uani 1 1 d . . . . . H36 H 0.761779 0.755273 0.230532 0.051 Uiso 1 1 calc R U . . . C37 C -0.0047(13) 0.4060(14) 0.5578(7) 0.076(5) Uani 0.25 1 d D U P A -1 H37A H -0.072376 0.426430 0.548520 0.114 Uiso 0.25 1 calc R U P A -1 H37B H 0.017383 0.405129 0.594501 0.114 Uiso 0.25 1 calc R U P A -1 H37C H -0.006280 0.358378 0.544750 0.114 Uiso 0.25 1 calc R U P A -1 O1 O 0.0291(11) 0.4758(8) 0.4878(5) 0.096(4) Uani 0.25 1 d D U P A -1 C40 C -0.0291(15) 0.5776(12) 0.4339(9) 0.089(5) Uani 0.25 1 d D U P A -1 H40A H 0.036518 0.596821 0.431502 0.134 Uiso 0.25 1 calc R U P A -1 H40B H -0.077760 0.615679 0.432431 0.134 Uiso 0.25 1 calc R U P A -1 H40C H -0.052779 0.545419 0.405941 0.134 Uiso 0.25 1 calc R U P A -1 C38 C 0.0675(11) 0.4493(12) 0.5360(7) 0.095(4) Uani 0.25 1 d D U P A -1 H38A H 0.090392 0.488951 0.558900 0.113 Uiso 0.25 1 calc R U P A -1 H38B H 0.127444 0.420470 0.534990 0.113 Uiso 0.25 1 calc R U P A -1 C39 C -0.0187(15) 0.5393(10) 0.4826(7) 0.094(4) Uani 0.25 1 d D U P A -1 H39A H 0.017774 0.570052 0.509709 0.112 Uiso 0.25 1 calc R U P A -1 H39B H -0.087268 0.532210 0.488632 0.112 Uiso 0.25 1 calc R U P A -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 I1 0.04247(14) 0.02067(12) 0.03350(13) 0.000 0.00940(9) 0.000 I2 0.04709(16) 0.02062(13) 0.06007(18) 0.000 0.01387(13) 0.000 Cu1 0.0338(2) 0.0260(2) 0.02004(18) 0.00094(14) 0.00591(14) -0.00105(15) Cu2 0.0278(2) 0.0251(2) 0.0311(2) -0.00065(15) 0.00558(15) -0.00243(15) P1 0.0359(3) 0.0311(3) 0.0199(3) 0.0005(2) 0.0061(2) -0.0016(3) P2 0.0278(3) 0.0220(3) 0.0354(3) 0.0000(3) 0.0038(2) -0.0024(2) C1 0.0328(13) 0.0368(15) 0.0285(13) 0.0104(11) 0.0055(10) 0.0046(12) C2 0.0427(17) 0.061(2) 0.0287(14) 0.0088(14) 0.0110(12) 0.0071(16) C3 0.0427(18) 0.080(3) 0.0372(16) 0.0173(18) 0.0144(13) 0.0130(18) C4 0.0327(16) 0.073(3) 0.065(2) 0.028(2) 0.0116(15) 0.0032(17) C5 0.0382(17) 0.050(2) 0.066(2) 0.0096(18) 0.0054(16) -0.0046(16) C6 0.0358(15) 0.0397(17) 0.0444(16) 0.0043(14) 0.0054(12) -0.0005(13) C7 0.0384(15) 0.0341(15) 0.0263(12) -0.0037(11) 0.0039(10) 0.0003(12) C8 0.0417(17) 0.061(2) 0.0394(16) -0.0004(15) 0.0102(13) 0.0050(16) C9 0.0422(18) 0.071(3) 0.060(2) -0.010(2) 0.0072(16) 0.0132(19) C10 0.056(2) 0.051(2) 0.053(2) -0.0042(17) -0.0093(16) 0.0157(18) C11 0.057(2) 0.0438(19) 0.0398(17) 0.0042(15) -0.0006(14) 0.0044(17) C12 0.0428(16) 0.0354(16) 0.0322(14) 0.0029(12) 0.0044(11) 0.0005(13) C13 0.0401(14) 0.0344(15) 0.0251(12) -0.0031(11) 0.0108(11) -0.0030(12) C14 0.0491(18) 0.0396(18) 0.0365(15) -0.0041(13) 0.0036(13) 0.0026(14) C15 0.064(2) 0.0379(19) 0.0507(19) -0.0036(15) 0.0101(16) 0.0046(17) C16 0.062(2) 0.0400(18) 0.0469(18) -0.0128(15) 0.0163(16) -0.0068(17) C17 0.059(2) 0.049(2) 0.0304(14) -0.0113(14) 0.0086(13) -0.0091(17) C18 0.0498(17) 0.0414(18) 0.0260(13) -0.0029(12) 0.0069(12) -0.0045(14) C19 0.0359(14) 0.0247(14) 0.0370(14) 0.0012(11) 0.0054(11) -0.0012(11) C20 0.0372(18) 0.0277(17) 0.115(4) 0.009(2) -0.009(2) 0.0012(14) C21 0.044(2) 0.034(2) 0.127(4) 0.008(2) -0.016(2) 0.0076(17) C22 0.061(2) 0.0280(16) 0.061(2) 0.0085(15) 0.0115(17) 0.0112(16) C23 0.059(2) 0.0226(15) 0.075(3) -0.0033(16) 0.0218(18) -0.0050(15) C24 0.0417(16) 0.0275(16) 0.059(2) -0.0052(14) 0.0136(14) -0.0061(13) C25 0.0316(13) 0.0241(13) 0.0370(14) 0.0002(11) 0.0056(10) -0.0017(11) C26 0.0323(13) 0.0270(14) 0.0405(15) -0.0008(12) 0.0088(11) -0.0044(11) C27 0.0367(15) 0.0343(16) 0.0451(16) -0.0036(13) 0.0056(12) -0.0086(12) C28 0.0513(19) 0.049(2) 0.0417(17) -0.0126(15) 0.0065(14) -0.0121(16) C29 0.060(2) 0.054(2) 0.0413(17) -0.0082(16) 0.0202(15) -0.0148(18) C30 0.0379(15) 0.0429(18) 0.0427(16) -0.0018(14) 0.0121(12) -0.0100(13) C31 0.0296(12) 0.0285(14) 0.0350(14) 0.0013(11) 0.0022(10) -0.0041(11) C32 0.0373(15) 0.0317(15) 0.0431(16) -0.0023(13) 0.0068(12) -0.0037(12) C33 0.0451(17) 0.050(2) 0.0418(17) -0.0076(15) 0.0128(13) -0.0087(15) C34 0.0517(19) 0.053(2) 0.0365(15) 0.0038(15) 0.0081(13) -0.0137(17) C35 0.069(2) 0.0348(17) 0.0489(19) 0.0084(15) 0.0088(16) -0.0056(17) C36 0.057(2) 0.0299(16) 0.0404(16) 0.0008(13) 0.0094(14) -0.0012(14) C37 0.030(8) 0.101(11) 0.087(10) 0.029(9) -0.009(7) -0.014(8) O1 0.073(7) 0.107(9) 0.106(9) 0.053(7) 0.017(6) -0.016(6) C40 0.045(9) 0.117(12) 0.109(11) 0.063(10) 0.022(8) -0.013(9) C38 0.069(7) 0.106(9) 0.105(9) 0.047(7) 0.011(6) -0.017(7) C39 0.059(7) 0.110(9) 0.110(9) 0.046(8) 0.014(7) -0.020(7) 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' 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' I I -0.3257 6.8362 '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 _geom_angle_publ_flag Cu1 I1 Cu1 51.258(16) . 2_655 ? Cu2 I2 Cu2 51.613(17) . 2_655 ? P1 Cu1 Cu1 178.05(2) . 2_655 ? P1 Cu1 Cu2 119.07(3) . . ? Cu1 Cu1 Cu2 62.658(15) 2_655 . ? P1 Cu1 Cu2 119.63(3) . 2_655 ? Cu1 Cu1 Cu2 61.934(15) 2_655 2_655 ? Cu2 Cu1 Cu2 55.31(2) . 2_655 ? P1 Cu1 I1 113.69(3) . . ? Cu1 Cu1 I1 64.372(8) 2_655 . ? Cu2 Cu1 I1 118.906(17) . . ? Cu2 Cu1 I1 118.296(17) 2_655 . ? P2 Cu2 Cu2 172.22(3) . 2_655 ? P2 Cu2 Cu1 125.01(3) . . ? Cu2 Cu2 Cu1 62.707(15) 2_655 . ? P2 Cu2 Cu1 120.36(3) . 2_655 ? Cu2 Cu2 Cu1 61.982(15) 2_655 2_655 ? Cu1 Cu2 Cu1 55.410(18) . 2_655 ? P2 Cu2 I2 109.65(2) . . ? Cu2 Cu2 I2 64.194(9) 2_655 . ? Cu1 Cu2 I2 118.777(18) . . ? Cu1 Cu2 I2 118.163(18) 2_655 . ? C1 P1 C7 104.14(14) . . ? C1 P1 C13 104.62(14) . . ? C7 P1 C13 103.36(14) . . ? C1 P1 Cu1 114.14(10) . . ? C7 P1 Cu1 114.84(10) . . ? C13 P1 Cu1 114.44(10) . . ? C19 P2 C31 104.30(14) . . ? C19 P2 C25 104.18(14) . . ? C31 P2 C25 105.78(13) . . ? C19 P2 Cu2 116.79(10) . . ? C31 P2 Cu2 108.69(9) . . ? C25 P2 Cu2 115.99(10) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 P1 123.3(3) . . ? C6 C1 P1 117.7(2) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 120.2(4) . . ? C4 C5 C6 120.3(4) . . ? C1 C6 C5 119.8(3) . . ? C8 C7 C12 119.0(3) . . ? C8 C7 P1 118.1(3) . . ? C12 C7 P1 122.9(2) . . ? C7 C8 C9 120.2(4) . . ? C10 C9 C8 120.4(4) . . ? C9 C10 C11 120.1(4) . . ? C10 C11 C12 119.7(4) . . ? C11 C12 C7 120.6(3) . . ? C14 C13 C18 118.9(3) . . ? C14 C13 P1 117.9(2) . . ? C18 C13 P1 123.1(3) . . ? C15 C14 C13 120.6(3) . . ? C14 C15 C16 119.8(4) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C13 120.7(3) . . ? C24 C19 C20 118.5(3) . . ? C24 C19 P2 118.8(2) . . ? C20 C19 P2 122.7(3) . . ? C21 C20 C19 120.4(4) . . ? C22 C21 C20 120.7(4) . . ? C23 C22 C21 118.7(3) . . ? C22 C23 C24 121.3(3) . . ? C19 C24 C23 120.4(3) . . ? C30 C25 C26 119.1(3) . . ? C30 C25 P2 117.4(2) . . ? C26 C25 P2 123.4(2) . . ? C27 C26 C25 120.4(3) . . ? C26 C27 C28 119.6(3) . . ? C29 C28 C27 120.4(3) . . ? C28 C29 C30 120.2(3) . . ? C29 C30 C25 120.3(3) . . ? C36 C31 C32 118.7(3) . . ? C36 C31 P2 120.2(3) . . ? C32 C31 P2 120.8(2) . . ? C33 C32 C31 120.2(3) . . ? C34 C33 C32 120.6(3) . . ? C33 C34 C35 119.7(3) . . ? C34 C35 C36 120.4(4) . . ? C35 C36 C31 120.5(3) . . ? C39 O1 C38 119.2(10) . . ? O1 C38 C37 115.6(8) . . ? O1 C39 C40 118.4(10) . . ? 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 I1 Cu1 2.7015(5) . ? I1 Cu1 2.7015(5) 2_655 ? I2 Cu2 2.6796(5) . ? I2 Cu2 2.6796(5) 2_655 ? Cu1 P1 2.2020(7) . ? Cu1 Cu1 2.3370(7) 2_655 ? Cu1 Cu2 2.5049(6) . ? Cu1 Cu2 2.5215(6) 2_655 ? Cu2 P2 2.2028(8) . ? Cu2 Cu2 2.3330(8) 2_655 ? P1 C1 1.820(3) . ? P1 C7 1.829(3) . ? P1 C13 1.830(3) . ? P2 C19 1.820(3) . ? P2 C31 1.822(3) . ? P2 C25 1.822(3) . ? C1 C2 1.392(4) . ? C1 C6 1.399(5) . ? C2 C3 1.390(5) . ? C3 C4 1.379(7) . ? C4 C5 1.379(6) . ? C5 C6 1.399(5) . ? C7 C8 1.388(5) . ? C7 C12 1.402(4) . ? C8 C9 1.391(5) . ? C9 C10 1.383(7) . ? C10 C11 1.383(6) . ? C11 C12 1.390(5) . ? C13 C14 1.390(5) . ? C13 C18 1.393(4) . ? C14 C15 1.387(5) . ? C15 C16 1.395(5) . ? C16 C17 1.377(6) . ? C17 C18 1.392(5) . ? C19 C24 1.384(4) . ? C19 C20 1.391(5) . ? C20 C21 1.390(5) . ? C21 C22 1.387(6) . ? C22 C23 1.366(6) . ? C23 C24 1.392(5) . ? C25 C30 1.390(4) . ? C25 C26 1.400(4) . ? C26 C27 1.383(4) . ? C27 C28 1.389(5) . ? C28 C29 1.376(5) . ? C29 C30 1.383(5) . ? C31 C36 1.391(4) . ? C31 C32 1.394(4) . ? C32 C33 1.390(5) . ? C33 C34 1.371(6) . ? C34 C35 1.382(6) . ? C35 C36 1.385(5) . ? C37 C38 1.505(8) . ? O1 C39 1.372(8) . ? O1 C38 1.402(8) . ? C40 C39 1.500(8) . ?