#------------------------------------------------------------------------------ #$Date: 2017-09-15 05:38:12 +0300 (Fri, 15 Sep 2017) $ #$Revision: 200914 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044228.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_7044228 loop_ _publ_author_name 'Bhat, Gulzar A.' 'Maqbool, Raihana' 'Dar, Aijaz' 'Hussain, Mahboob Ul' 'Murugavel, Ramaswamy' _publ_section_title ; Selective formation of discrete versus polymeric copper organophosphates: DNA cleavage and cytotoxic activity ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT02763J _journal_year 2017 _chemical_formula_sum 'C94 H122 Br4 Cu3 N8 O24 P4' _chemical_formula_weight 2382.13 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-07-27 deposited with the CCDC. 2017-09-14 downloaded from the CCDC. ; _cell_angle_alpha 95.074(8) _cell_angle_beta 99.545(6) _cell_angle_gamma 111.150(18) _cell_formula_units_Z 1 _cell_length_a 10.270(5) _cell_length_b 13.932(7) _cell_length_c 19.316(7) _cell_measurement_reflns_used 6009 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 52.46 _cell_measurement_theta_min 6.706 _cell_volume 2509(2) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_collection 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5419 _diffrn_reflns_av_R_equivalents 0.1254 _diffrn_reflns_av_unetI/netI 0.0807 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 32762 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 59.993 _diffrn_reflns_theta_max 59.993 _diffrn_reflns_theta_min 6.706 _exptl_absorpt_coefficient_mu 3.840 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.577 _exptl_crystal_description needle _exptl_crystal_F_000 1221 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.691 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 635 _refine_ls_number_reflns 7359 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0484 _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^)+(0.0756P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1215 _refine_ls_wR_factor_ref 0.1439 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5843 _reflns_number_total 7359 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt02763j2.cif _cod_data_source_block 4 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7044228 _shelx_shelxl_version_number 2014/7 _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 0.700 _shelx_estimated_absorpt_t_max 0.831 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL gb-241-p_a.res in P-1 CELL 1.54190 10.2700 13.9320 19.3160 95.074 99.545 111.150 ZERR 1.00 0.0050 0.0070 0.0070 0.008 0.006 0.018 LATT 1 SFAC C H BR CU N O P UNIT 94 122 4 3 8 24 4 MERG 2 OMIT -4.00 120.00 OMIT 5 -10 3 OMIT 4 -11 6 OMIT 3 -10 8 OMIT -1 -9 9 OMIT -6 13 0 OMIT 5 -12 11 OMIT 5 -11 8 OMIT -1 -2 2 OMIT 6 -13 1 BIND O9 Cu2 MORE -1 HTAB O2 O5 HTAB O11 O3 HTAB O10 O3 EQIV $1 x-1, y, z HTAB O9 O12_$1 EQIV $2 -x+1, -y+2, -z+1 HTAB O9 O6_$2 HTAB O12 O6 EQIV $3 -x+1, -y+1, -z+1 HTAB C7 O11_$3 HTAB C12 O3_$1 HTAB C1 O6 HTAB C9 O10_$1 HTAB C17 O11_$3 EQIV $4 -x+1, -y+2, -z+2 HTAB C14 Br2_$4 HTAB C4 O11_$3 HTAB C20 O10_$1 HTAB O2 O5 HTAB O11 O3 HTAB O10 O3 HTAB O9 O12_$1 HTAB O9 O6_$2 HTAB O12 O6 HTAB C7 O11_$3 HTAB C12 O3_$1 HTAB C1 O6 HTAB C9 O10_$1 HTAB C17 O11_$3 HTAB C14 Br2_$4 HTAB C4 O11_$3 HTAB C20 O10_$1 FMAP 2 PLAN 20 SIZE 0.050 0.090 0.100 ACTA BOND $H CONF LIST 6 L.S. 30 TEMP -123.00 WGHT 0.075600 FVAR 0.27649 C1 1 0.582132 0.707959 0.513612 11.00000 0.02996 0.02618 = 0.03046 0.00068 0.00593 0.00697 AFIX 43 H1 2 0.660880 0.770103 0.535922 11.00000 -1.20000 AFIX 0 C2 1 0.580799 0.661587 0.447524 11.00000 0.04068 0.02878 = 0.03515 0.00656 0.01548 0.00535 AFIX 43 H2A 2 0.657373 0.692085 0.424609 11.00000 -1.20000 AFIX 0 C3 1 0.468552 0.571020 0.414601 11.00000 0.04423 0.02930 = 0.02852 0.00691 0.01428 0.01329 AFIX 43 H3 2 0.466780 0.538027 0.369062 11.00000 -1.20000 AFIX 0 C4 1 0.357758 0.528763 0.449335 11.00000 0.02607 0.02769 = 0.02719 -0.00185 0.00205 0.00397 AFIX 43 H4 2 0.278608 0.466399 0.427861 11.00000 -1.20000 AFIX 0 C5 1 0.364541 0.578507 0.515049 11.00000 0.02888 0.02014 = 0.02177 0.00468 0.00091 0.00796 C6 1 0.252295 0.542490 0.556044 11.00000 0.02730 0.02543 = 0.02149 0.00124 0.00113 0.01305 C7 1 0.130551 0.452628 0.537209 11.00000 0.02649 0.02629 = 0.02007 -0.00070 -0.00100 0.00760 AFIX 43 H7 2 0.113704 0.406565 0.494456 11.00000 -1.20000 AFIX 0 C8 1 0.032941 0.429907 0.580998 11.00000 0.02998 0.02650 = 0.01877 0.00895 -0.00077 0.01469 C9 1 0.060171 0.499943 0.643488 11.00000 0.02551 0.02677 = 0.02516 0.00353 0.00321 0.00615 AFIX 43 H9 2 -0.006450 0.487178 0.673671 11.00000 -1.20000 AFIX 0 C10 1 0.185409 0.587823 0.660494 11.00000 0.02793 0.02334 = 0.02006 0.00582 0.00370 0.00864 C11 1 0.238406 0.666198 0.726131 11.00000 0.02854 0.01767 = 0.02465 0.00672 0.00262 0.00528 C12 1 0.162178 0.668559 0.778533 11.00000 0.02388 0.03263 = 0.02862 0.00750 0.00677 0.00741 AFIX 43 H12 2 0.066283 0.620695 0.772510 11.00000 -1.20000 AFIX 0 C13 1 0.226656 0.740786 0.839258 11.00000 0.03131 0.02647 = 0.02514 0.00451 0.00807 0.00508 AFIX 43 H13 2 0.175128 0.744770 0.875239 11.00000 -1.20000 AFIX 0 C14 1 0.365810 0.806953 0.847446 11.00000 0.04400 0.02472 = 0.02573 0.00383 0.00418 0.00783 AFIX 43 H14 2 0.413570 0.855508 0.890006 11.00000 -1.20000 AFIX 0 C15 1 0.436230 0.802206 0.792790 11.00000 0.02474 0.02972 = 0.02634 -0.00199 0.00088 0.00248 AFIX 43 H15 2 0.532906 0.848419 0.798455 11.00000 -1.20000 AFIX 0 C16 1 -0.098722 0.332151 0.561826 11.00000 0.02425 0.02157 = 0.03002 0.00845 0.00230 0.01071 C17 1 -0.138989 0.271101 0.494863 11.00000 0.02794 0.02638 = 0.02589 0.00928 0.00396 0.00885 AFIX 43 H17 2 -0.084847 0.293287 0.459762 11.00000 -1.20000 AFIX 0 C18 1 -0.255942 0.179473 0.479384 11.00000 0.03192 0.03480 = 0.02280 0.00266 0.00052 0.00614 AFIX 43 H18 2 -0.281721 0.139933 0.433083 11.00000 -1.20000 AFIX 0 C19 1 -0.301579 0.202505 0.589556 11.00000 0.03570 0.02491 = 0.02958 0.00484 0.00956 0.00511 AFIX 43 H19 2 -0.359995 0.179560 0.622880 11.00000 -1.20000 AFIX 0 C20 1 -0.185340 0.296178 0.609154 11.00000 0.03857 0.02976 = 0.02176 0.00537 0.00461 0.01151 AFIX 43 H20 2 -0.165079 0.335713 0.655055 11.00000 -1.20000 AFIX 0 C21 1 0.622429 0.568751 0.868372 11.00000 0.03025 0.02865 = 0.02233 0.00891 0.00736 0.01082 C22 1 0.736476 0.580052 0.924607 11.00000 0.03668 0.03132 = 0.02203 0.01038 0.00371 0.01157 C23 1 0.719624 0.499594 0.963583 11.00000 0.03598 0.04586 = 0.02676 0.00717 0.00722 0.01454 AFIX 43 H23 2 0.794441 0.504613 1.001726 11.00000 -1.20000 AFIX 0 C24 1 0.594630 0.411864 0.947437 11.00000 0.03906 0.03603 = 0.02976 0.01481 0.00781 0.01252 C25 1 0.482362 0.403000 0.893977 11.00000 0.03037 0.03296 = 0.03498 0.00443 0.00596 0.00720 AFIX 43 H25 2 0.396664 0.342501 0.884503 11.00000 -1.20000 AFIX 0 C26 1 0.494380 0.483173 0.853502 11.00000 0.03337 0.02428 = 0.02407 0.00723 0.00536 0.01060 C27 1 0.869425 0.678918 0.942666 11.00000 0.03377 0.04291 = 0.02676 0.00424 0.00057 0.00596 AFIX 13 H27 2 0.897802 0.696822 0.896917 11.00000 -1.20000 AFIX 0 C28 1 0.837787 0.769753 0.976538 11.00000 0.04885 0.04005 = 0.04992 -0.00229 -0.00071 0.00772 AFIX 137 H28A 2 0.758978 0.777814 0.944606 11.00000 -1.50000 H28B 2 0.923145 0.834166 0.984586 11.00000 -1.50000 H28C 2 0.811038 0.755276 1.022048 11.00000 -1.50000 AFIX 0 C29 1 0.997195 0.668242 0.990389 11.00000 0.04232 0.06823 = 0.04334 0.01635 -0.00494 0.01172 AFIX 137 H29A 2 0.976134 0.656653 1.037321 11.00000 -1.50000 H29B 2 1.082133 0.732253 0.995516 11.00000 -1.50000 H29C 2 1.014867 0.609006 0.968788 11.00000 -1.50000 AFIX 0 C30 1 0.366987 0.474239 0.796401 11.00000 0.03336 0.02541 = 0.03123 0.01222 0.00256 0.01040 AFIX 13 H30 2 0.391707 0.541560 0.777338 11.00000 -1.20000 AFIX 0 C31 1 0.338444 0.387842 0.734924 11.00000 0.04310 0.04326 = 0.02724 0.00396 -0.00053 0.01306 AFIX 137 H31A 2 0.427369 0.397144 0.718992 11.00000 -1.50000 H31B 2 0.267184 0.390831 0.695483 11.00000 -1.50000 H31C 2 0.302420 0.319987 0.750758 11.00000 -1.50000 AFIX 0 C32 1 0.235451 0.457813 0.827207 11.00000 0.03655 0.03600 = 0.03841 0.01727 0.00690 0.01682 AFIX 137 H32A 2 0.208610 0.392031 0.846158 11.00000 -1.50000 H32B 2 0.156464 0.455184 0.789825 11.00000 -1.50000 H32C 2 0.256261 0.515607 0.865551 11.00000 -1.50000 AFIX 0 C33 1 0.732883 1.047270 0.769019 11.00000 0.02668 0.01858 = 0.02620 0.00010 0.00235 -0.00152 C34 1 0.618382 1.065942 0.789384 11.00000 0.02450 0.01525 = 0.03445 0.00276 0.00312 0.00030 C35 1 0.612626 1.067283 0.860770 11.00000 0.02776 0.02376 = 0.03376 -0.00227 0.00582 0.00385 AFIX 43 H35 2 0.538689 1.081651 0.877606 11.00000 -1.20000 AFIX 0 C36 1 0.713952 1.047813 0.907236 11.00000 0.03366 0.03273 = 0.02267 -0.00511 0.00069 0.00484 C37 1 0.827710 1.032766 0.886683 11.00000 0.02740 0.02678 = 0.02749 -0.00166 -0.00188 0.00207 AFIX 43 H37 2 0.896949 1.021422 0.920494 11.00000 -1.20000 AFIX 0 C38 1 0.841655 1.034126 0.816222 11.00000 0.03088 0.01960 = 0.02652 0.00243 0.00144 0.00628 C39 1 0.505334 1.083668 0.736733 11.00000 0.03370 0.03024 = 0.03467 0.01162 0.01095 0.01336 AFIX 13 H39 2 0.529654 1.077292 0.688954 11.00000 -1.20000 AFIX 0 C40 1 0.508027 1.192349 0.753295 11.00000 0.11561 0.06125 = 0.07750 -0.00103 -0.01699 0.05942 AFIX 137 H40A 2 0.488191 1.202578 0.800711 11.00000 -1.50000 H40B 2 0.435180 1.201564 0.717828 11.00000 -1.50000 H40C 2 0.602458 1.243490 0.752101 11.00000 -1.50000 AFIX 0 C41 1 0.358447 1.002708 0.730936 11.00000 0.03815 0.08448 = 0.06164 0.04661 0.00662 0.02084 AFIX 137 H41A 2 0.358104 0.933426 0.716322 11.00000 -1.50000 H41B 2 0.289888 1.016375 0.695504 11.00000 -1.50000 H41C 2 0.331474 1.005479 0.777196 11.00000 -1.50000 AFIX 0 C42 1 0.971546 1.029245 0.792231 11.00000 0.02393 0.02627 = 0.02803 0.00023 0.00194 -0.00140 AFIX 13 H42 2 0.938699 0.982716 0.745060 11.00000 -1.20000 AFIX 0 C43 1 1.066747 1.136963 0.782165 11.00000 0.03090 0.04415 = 0.04934 0.00649 0.00773 0.01201 AFIX 137 H43A 2 1.013356 1.162602 0.746583 11.00000 -1.50000 H43B 2 1.150541 1.133215 0.765945 11.00000 -1.50000 H43C 2 1.097839 1.184652 0.827463 11.00000 -1.50000 AFIX 0 C44 1 1.057809 0.984862 0.843605 11.00000 0.03287 0.04347 = 0.03399 0.00151 0.00031 0.01461 AFIX 137 H44A 2 1.097932 1.032324 0.889121 11.00000 -1.50000 H44B 2 1.135513 0.977525 0.823114 11.00000 -1.50000 H44C 2 0.994962 0.916448 0.851323 11.00000 -1.50000 AFIX 0 C45 1 1.063937 1.136198 0.584806 11.00000 0.05445 0.04874 = 0.11571 0.03638 0.02760 0.01497 AFIX 137 H45A 2 1.073016 1.139494 0.535276 11.00000 -1.50000 H45B 2 1.141223 1.195884 0.615961 11.00000 -1.50000 H45C 2 0.971584 1.138102 0.590083 11.00000 -1.50000 AFIX 0 C46 1 0.867778 0.404497 0.827770 11.00000 0.06678 0.06087 = 0.04087 0.01258 0.01397 0.02560 AFIX 137 H46A 2 0.895639 0.344249 0.824467 11.00000 -1.50000 H46B 2 0.777503 0.385554 0.843917 11.00000 -1.50000 H46C 2 0.942268 0.462296 0.861777 11.00000 -1.50000 AFIX 0 C47 1 0.981986 0.791188 0.652313 11.00000 0.08386 0.05097 = 0.06541 0.00634 0.03399 0.02324 AFIX 137 H47A 2 1.034752 0.820233 0.616221 11.00000 -1.50000 H47B 2 1.045792 0.815994 0.699433 11.00000 -1.50000 H47C 2 0.901673 0.813648 0.651242 11.00000 -1.50000 AFIX 0 BR1 3 0.574741 0.299508 0.999388 11.00000 0.05535 0.05409 = 0.05531 0.03442 0.00750 0.01952 BR2 3 0.699992 1.041944 1.003985 11.00000 0.04676 0.05944 = 0.02551 0.00310 0.00805 0.01722 CU1 4 0.464383 0.719118 0.648254 11.00000 0.02731 0.02256 = 0.02104 0.00203 0.00346 0.00533 CU2 4 0.500000 1.000000 0.500000 10.50000 0.02980 0.02341 = 0.02453 0.00549 -0.00397 0.00193 N1 5 0.475839 0.668206 0.547477 11.00000 0.02938 0.02203 = 0.02290 0.00244 0.00429 0.00724 N2 5 0.278465 0.606131 0.617548 11.00000 0.02062 0.02397 = 0.02336 0.00285 0.00161 0.00345 N3 5 0.373165 0.735395 0.732982 11.00000 0.03109 0.01834 = 0.02299 0.00701 0.00556 0.00751 N4 5 -0.335730 0.143037 0.526642 11.00000 0.02892 0.02894 = 0.02354 0.00928 -0.00107 0.00817 O1 6 0.569284 0.626620 0.696435 11.00000 0.03425 0.02396 = 0.02630 0.00313 0.00101 0.00841 O2 6 0.773938 0.782596 0.769040 11.00000 0.03150 0.02886 = 0.03028 0.00663 -0.00431 0.00139 AFIX 147 H2 2 0.730920 0.807408 0.739312 11.00000 -1.50000 AFIX 0 O3 6 0.798994 0.609918 0.755607 11.00000 0.03168 0.03628 = 0.03705 0.01211 0.00910 0.01345 O4 6 0.638144 0.650798 0.830631 11.00000 0.03098 0.02439 = 0.02554 0.00254 0.00291 0.00674 O5 6 0.624612 0.852852 0.674989 11.00000 0.03163 0.02036 = 0.02467 0.00661 -0.00131 0.00565 O6 6 0.785973 0.946063 0.596457 11.00000 0.02663 0.02860 = 0.02778 0.00053 0.00356 0.00312 O7 6 0.746345 1.047553 0.697953 11.00000 0.02559 0.02248 = 0.02450 0.00289 0.00106 0.00356 O8 6 0.546002 0.958829 0.591750 11.00000 0.02319 0.02929 = 0.02433 0.00403 -0.00020 0.00231 O9 6 0.323280 1.064900 0.544487 11.00000 0.05892 0.04255 = 0.04454 0.01500 -0.00033 0.01918 AFIX 7 H9A 2 0.274686 1.021750 0.570874 11.00000 -1.50000 H9B 2 0.261374 1.069132 0.507895 11.00000 -1.50000 AFIX 0 O10 6 0.850375 0.435331 0.760245 11.00000 0.06423 0.04340 = 0.03920 0.00931 0.01970 0.02930 AFIX 147 H10 2 0.830397 0.488728 0.763478 11.00000 -1.50000 AFIX 0 O11 6 0.929535 0.680800 0.637910 11.00000 0.04237 0.03924 = 0.03714 0.00099 0.01142 0.01090 AFIX 147 H11 2 0.887478 0.655958 0.669862 11.00000 -1.50000 AFIX 0 O12 6 1.072565 1.042675 0.603687 11.00000 0.04282 0.06251 = 0.07643 0.02325 0.01202 0.01808 AFIX 147 H12A 2 0.994158 1.004841 0.612151 11.00000 -1.50000 AFIX 0 P1 7 0.694498 0.661410 0.757729 11.00000 0.02752 0.02390 = 0.02514 0.00612 0.00326 0.00575 P2 7 0.673673 0.946496 0.636076 11.00000 0.02325 0.02108 = 0.02138 0.00313 0.00094 0.00325 HKLF 4 REM gb-241-p_a.res in P-1 REM R1 = 0.0484 for 5843 Fo > 4sig(Fo) and 0.0611 for all 7359 data REM 635 parameters refined using 0 restraints END WGHT 0.0756 0.0000 REM Highest difference peak 0.691, deepest hole -0.521, 1-sigma level 0.107 Q1 1 0.4646 1.0994 0.8897 11.00000 0.05 0.69 Q2 1 0.6420 0.3010 0.9840 11.00000 0.05 0.64 Q3 1 0.9886 0.8747 0.5990 11.00000 0.05 0.53 Q4 1 0.6085 0.3572 1.0205 11.00000 0.05 0.52 Q5 1 0.6657 0.4538 0.9683 11.00000 0.05 0.49 Q6 1 0.5521 0.7996 0.6602 11.00000 0.05 0.48 Q7 1 0.1905 1.0745 0.5542 11.00000 0.05 0.47 Q8 1 0.4828 0.9180 0.9773 11.00000 0.05 0.44 Q9 1 0.7426 0.9403 0.6162 11.00000 0.05 0.43 Q10 1 -0.4233 0.0815 0.5112 11.00000 0.05 0.43 Q11 1 0.8590 0.9887 0.5981 11.00000 0.05 0.42 Q12 1 0.6662 0.8369 0.6419 11.00000 0.05 0.41 Q13 1 -0.3613 0.1773 0.5166 11.00000 0.05 0.41 Q14 1 0.6879 1.0570 0.5913 11.00000 0.05 0.41 Q15 1 0.3822 0.7318 0.7030 11.00000 0.05 0.40 Q16 1 0.3546 1.0987 0.8014 11.00000 0.05 0.38 Q17 1 0.6601 0.6832 0.6430 11.00000 0.05 0.38 Q18 1 0.5048 0.9969 0.9704 11.00000 0.05 0.38 Q19 1 0.8850 1.0147 0.9902 11.00000 0.05 0.38 Q20 1 0.5056 0.8384 0.9751 11.00000 0.05 0.37 ; _shelx_res_checksum 31566 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 C1 C 0.5821(5) 0.7080(4) 0.5136(2) 0.0303(11) Uani 1 1 d . . . H1 H 0.6609 0.7701 0.5359 0.036 Uiso 1 1 calc R U . C2 C 0.5808(6) 0.6616(4) 0.4475(2) 0.0361(11) Uani 1 1 d . . . H2A H 0.6574 0.6921 0.4246 0.043 Uiso 1 1 calc R U . C3 C 0.4686(5) 0.5710(4) 0.4146(2) 0.0333(11) Uani 1 1 d . . . H3 H 0.4668 0.5380 0.3691 0.040 Uiso 1 1 calc R U . C4 C 0.3578(5) 0.5288(3) 0.4493(2) 0.0297(11) Uani 1 1 d . . . H4 H 0.2786 0.4664 0.4279 0.036 Uiso 1 1 calc R U . C5 C 0.3645(5) 0.5785(3) 0.5150(2) 0.0245(10) Uani 1 1 d . . . C6 C 0.2523(5) 0.5425(3) 0.5560(2) 0.0246(10) Uani 1 1 d . . . C7 C 0.1306(5) 0.4526(3) 0.5372(2) 0.0260(10) Uani 1 1 d . . . H7 H 0.1137 0.4066 0.4945 0.031 Uiso 1 1 calc R U . C8 C 0.0329(5) 0.4299(3) 0.5810(2) 0.0244(10) Uani 1 1 d . . . C9 C 0.0602(5) 0.4999(3) 0.6435(2) 0.0272(10) Uani 1 1 d . . . H9 H -0.0065 0.4872 0.6737 0.033 Uiso 1 1 calc R U . C10 C 0.1854(5) 0.5878(3) 0.6605(2) 0.0241(10) Uani 1 1 d . . . C11 C 0.2384(5) 0.6662(3) 0.7261(2) 0.0248(10) Uani 1 1 d . . . C12 C 0.1622(5) 0.6686(4) 0.7785(2) 0.0290(10) Uani 1 1 d . . . H12 H 0.0663 0.6207 0.7725 0.035 Uiso 1 1 calc R U . C13 C 0.2267(5) 0.7408(3) 0.8393(2) 0.0291(10) Uani 1 1 d . . . H13 H 0.1751 0.7448 0.8752 0.035 Uiso 1 1 calc R U . C14 C 0.3658(5) 0.8070(4) 0.8474(2) 0.0334(11) Uani 1 1 d . . . H14 H 0.4136 0.8555 0.8900 0.040 Uiso 1 1 calc R U . C15 C 0.4362(5) 0.8022(3) 0.7928(2) 0.0302(10) Uani 1 1 d . . . H15 H 0.5329 0.8484 0.7985 0.036 Uiso 1 1 calc R U . C16 C -0.0987(5) 0.3322(3) 0.5618(2) 0.0249(10) Uani 1 1 d . . . C17 C -0.1390(5) 0.2711(3) 0.4949(2) 0.0271(10) Uani 1 1 d . . . H17 H -0.0848 0.2933 0.4598 0.032 Uiso 1 1 calc R U . C18 C -0.2559(5) 0.1795(4) 0.4794(2) 0.0325(11) Uani 1 1 d . . . H18 H -0.2817 0.1399 0.4331 0.039 Uiso 1 1 calc R U . C19 C -0.3016(5) 0.2025(3) 0.5896(2) 0.0316(11) Uani 1 1 d . . . H19 H -0.3600 0.1796 0.6229 0.038 Uiso 1 1 calc R U . C20 C -0.1853(5) 0.2962(3) 0.6092(2) 0.0306(11) Uani 1 1 d . . . H20 H -0.1651 0.3357 0.6551 0.037 Uiso 1 1 calc R U . C21 C 0.6224(5) 0.5688(3) 0.8684(2) 0.0267(10) Uani 1 1 d . . . C22 C 0.7365(5) 0.5801(3) 0.9246(2) 0.0303(11) Uani 1 1 d . . . C23 C 0.7196(5) 0.4996(4) 0.9636(2) 0.0364(12) Uani 1 1 d . . . H23 H 0.7944 0.5046 1.0017 0.044 Uiso 1 1 calc R U . C24 C 0.5946(5) 0.4119(4) 0.9474(2) 0.0348(12) Uani 1 1 d . . . C25 C 0.4824(5) 0.4030(4) 0.8940(2) 0.0344(11) Uani 1 1 d . . . H25 H 0.3967 0.3425 0.8845 0.041 Uiso 1 1 calc R U . C26 C 0.4944(5) 0.4832(3) 0.8535(2) 0.0272(10) Uani 1 1 d . . . C27 C 0.8694(5) 0.6789(4) 0.9427(2) 0.0378(12) Uani 1 1 d . . . H27 H 0.8978 0.6968 0.8969 0.045 Uiso 1 1 calc R U . C28 C 0.8378(6) 0.7698(4) 0.9765(3) 0.0510(14) Uani 1 1 d . . . H28A H 0.7590 0.7778 0.9446 0.076 Uiso 1 1 calc R U . H28B H 0.9231 0.8342 0.9846 0.076 Uiso 1 1 calc R U . H28C H 0.8110 0.7553 1.0220 0.076 Uiso 1 1 calc R U . C29 C 0.9972(6) 0.6682(5) 0.9904(3) 0.0553(15) Uani 1 1 d . . . H29A H 0.9761 0.6567 1.0373 0.083 Uiso 1 1 calc R U . H29B H 1.0821 0.7323 0.9955 0.083 Uiso 1 1 calc R U . H29C H 1.0149 0.6090 0.9688 0.083 Uiso 1 1 calc R U . C30 C 0.3670(5) 0.4742(3) 0.7964(2) 0.0303(11) Uani 1 1 d . . . H30 H 0.3917 0.5416 0.7773 0.036 Uiso 1 1 calc R U . C31 C 0.3384(6) 0.3878(4) 0.7349(2) 0.0400(12) Uani 1 1 d . . . H31A H 0.4274 0.3971 0.7190 0.060 Uiso 1 1 calc R U . H31B H 0.2672 0.3908 0.6955 0.060 Uiso 1 1 calc R U . H31C H 0.3024 0.3200 0.7508 0.060 Uiso 1 1 calc R U . C32 C 0.2355(5) 0.4578(4) 0.8272(2) 0.0355(11) Uani 1 1 d . . . H32A H 0.2086 0.3920 0.8462 0.053 Uiso 1 1 calc R U . H32B H 0.1565 0.4552 0.7898 0.053 Uiso 1 1 calc R U . H32C H 0.2563 0.5156 0.8656 0.053 Uiso 1 1 calc R U . C33 C 0.7329(5) 1.0473(3) 0.7690(2) 0.0274(10) Uani 1 1 d . . . C34 C 0.6184(5) 1.0659(3) 0.7894(2) 0.0273(10) Uani 1 1 d . . . C35 C 0.6126(5) 1.0673(3) 0.8608(2) 0.0307(11) Uani 1 1 d . . . H35 H 0.5387 1.0817 0.8776 0.037 Uiso 1 1 calc R U . C36 C 0.7140(5) 1.0478(4) 0.9072(2) 0.0332(11) Uani 1 1 d . . . C37 C 0.8277(5) 1.0328(3) 0.8867(2) 0.0310(11) Uani 1 1 d . . . H37 H 0.8969 1.0214 0.9205 0.037 Uiso 1 1 calc R U . C38 C 0.8417(5) 1.0341(3) 0.8162(2) 0.0273(10) Uani 1 1 d . . . C39 C 0.5053(5) 1.0837(3) 0.7367(2) 0.0317(11) Uani 1 1 d . . . H39 H 0.5297 1.0773 0.6890 0.038 Uiso 1 1 calc R U . C40 C 0.5080(9) 1.1923(5) 0.7533(4) 0.083(2) Uani 1 1 d . . . H40A H 0.4882 1.2026 0.8007 0.124 Uiso 1 1 calc R U . H40B H 0.4352 1.2016 0.7178 0.124 Uiso 1 1 calc R U . H40C H 0.6025 1.2435 0.7521 0.124 Uiso 1 1 calc R U . C41 C 0.3584(6) 1.0027(5) 0.7309(3) 0.0604(17) Uani 1 1 d . . . H41A H 0.3581 0.9334 0.7163 0.091 Uiso 1 1 calc R U . H41B H 0.2899 1.0164 0.6955 0.091 Uiso 1 1 calc R U . H41C H 0.3315 1.0055 0.7772 0.091 Uiso 1 1 calc R U . C42 C 0.9715(5) 1.0292(3) 0.7922(2) 0.0299(10) Uani 1 1 d . . . H42 H 0.9387 0.9827 0.7451 0.036 Uiso 1 1 calc R U . C43 C 1.0667(5) 1.1370(4) 0.7822(3) 0.0423(13) Uani 1 1 d . . . H43A H 1.0134 1.1626 0.7466 0.063 Uiso 1 1 calc R U . H43B H 1.1505 1.1332 0.7659 0.063 Uiso 1 1 calc R U . H43C H 1.0978 1.1847 0.8275 0.063 Uiso 1 1 calc R U . C44 C 1.0578(5) 0.9849(4) 0.8436(2) 0.0379(12) Uani 1 1 d . . . H44A H 1.0979 1.0323 0.8891 0.057 Uiso 1 1 calc R U . H44B H 1.1355 0.9775 0.8231 0.057 Uiso 1 1 calc R U . H44C H 0.9950 0.9164 0.8513 0.057 Uiso 1 1 calc R U . C45 C 1.0639(7) 1.1362(5) 0.5848(4) 0.072(2) Uani 1 1 d . . . H45A H 1.0730 1.1395 0.5353 0.107 Uiso 1 1 calc R U . H45B H 1.1412 1.1959 0.6160 0.107 Uiso 1 1 calc R U . H45C H 0.9716 1.1381 0.5901 0.107 Uiso 1 1 calc R U . C46 C 0.8678(7) 0.4045(5) 0.8278(3) 0.0552(15) Uani 1 1 d . . . H46A H 0.8956 0.3442 0.8245 0.083 Uiso 1 1 calc R U . H46B H 0.7775 0.3856 0.8439 0.083 Uiso 1 1 calc R U . H46C H 0.9423 0.4623 0.8618 0.083 Uiso 1 1 calc R U . C47 C 0.9820(8) 0.7912(4) 0.6523(3) 0.0654(18) Uani 1 1 d . . . H47A H 1.0348 0.8202 0.6162 0.098 Uiso 1 1 calc R U . H47B H 1.0458 0.8160 0.6994 0.098 Uiso 1 1 calc R U . H47C H 0.9017 0.8136 0.6512 0.098 Uiso 1 1 calc R U . Br1 Br 0.57474(7) 0.29951(5) 0.99939(3) 0.0542(2) Uani 1 1 d . . . Br2 Br 0.69999(6) 1.04194(4) 1.00398(2) 0.04499(19) Uani 1 1 d . . . Cu1 Cu 0.46438(7) 0.71912(5) 0.64825(3) 0.02514(19) Uani 1 1 d . . . Cu2 Cu 0.5000 1.0000 0.5000 0.0294(2) Uani 1 2 d S . P N1 N 0.4758(4) 0.6682(3) 0.54748(17) 0.0257(8) Uani 1 1 d . . . N2 N 0.2785(4) 0.6061(3) 0.61755(17) 0.0246(8) Uani 1 1 d . . . N3 N 0.3732(4) 0.7354(3) 0.73298(17) 0.0245(8) Uani 1 1 d . . . N4 N -0.3357(4) 0.1430(3) 0.52664(18) 0.0285(9) Uani 1 1 d . . . O1 O 0.5693(3) 0.6266(2) 0.69643(15) 0.0297(7) Uani 1 1 d . . . O2 O 0.7739(3) 0.7826(2) 0.76904(16) 0.0344(8) Uani 1 1 d . . . H2 H 0.7309 0.8074 0.7393 0.052 Uiso 1 1 calc R U . O3 O 0.7990(3) 0.6099(2) 0.75561(16) 0.0342(7) Uani 1 1 d . . . O4 O 0.6381(3) 0.6508(2) 0.83063(14) 0.0286(7) Uani 1 1 d . . . O5 O 0.6246(3) 0.8529(2) 0.67499(14) 0.0275(7) Uani 1 1 d . . . O6 O 0.7860(3) 0.9461(2) 0.59646(15) 0.0303(7) Uani 1 1 d . . . O7 O 0.7463(3) 1.0476(2) 0.69795(14) 0.0264(7) Uani 1 1 d . . . O8 O 0.5460(3) 0.9588(2) 0.59175(14) 0.0285(7) Uani 1 1 d . . . O9 O 0.3233(4) 1.0649(3) 0.54449(18) 0.0496(9) Uani 1 1 d . . . H9A H 0.2747 1.0217 0.5709 0.074 Uiso 1 1 d R U . H9B H 0.2614 1.0691 0.5079 0.074 Uiso 1 1 d R U . O10 O 0.8504(4) 0.4353(3) 0.76024(17) 0.0452(9) Uani 1 1 d . . . H10 H 0.8304 0.4887 0.7635 0.068 Uiso 1 1 calc R U . O11 O 0.9295(4) 0.6808(3) 0.63791(17) 0.0409(8) Uani 1 1 d . . . H11 H 0.8875 0.6560 0.6699 0.061 Uiso 1 1 calc R U . O12 O 1.0726(4) 1.0427(3) 0.6037(2) 0.0605(11) Uani 1 1 d . . . H12A H 0.9942 1.0048 0.6122 0.091 Uiso 1 1 calc R U . P1 P 0.69450(13) 0.66141(9) 0.75773(6) 0.0268(3) Uani 1 1 d . . . P2 P 0.67367(12) 0.94650(8) 0.63608(5) 0.0239(3) Uani 1 1 d . . . 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 C1 0.030(3) 0.026(3) 0.030(2) 0.0007(19) 0.006(2) 0.007(2) C2 0.041(3) 0.029(3) 0.035(3) 0.007(2) 0.015(2) 0.005(3) C3 0.044(3) 0.029(3) 0.029(2) 0.007(2) 0.014(2) 0.013(3) C4 0.026(3) 0.028(3) 0.027(2) -0.0019(19) 0.002(2) 0.004(2) C5 0.029(3) 0.020(2) 0.022(2) 0.0047(18) 0.0009(19) 0.008(2) C6 0.027(3) 0.025(3) 0.021(2) 0.0012(18) 0.0011(19) 0.013(2) C7 0.026(3) 0.026(3) 0.020(2) -0.0007(18) -0.0010(19) 0.008(2) C8 0.030(3) 0.026(3) 0.019(2) 0.0090(17) -0.0008(19) 0.015(2) C9 0.026(3) 0.027(3) 0.025(2) 0.0035(18) 0.003(2) 0.006(2) C10 0.028(3) 0.023(2) 0.020(2) 0.0058(18) 0.0037(19) 0.009(2) C11 0.029(3) 0.018(2) 0.025(2) 0.0067(17) 0.0026(19) 0.005(2) C12 0.024(3) 0.033(3) 0.029(2) 0.007(2) 0.007(2) 0.007(2) C13 0.031(3) 0.026(3) 0.025(2) 0.0045(19) 0.008(2) 0.005(2) C14 0.044(3) 0.025(3) 0.026(2) 0.0038(19) 0.004(2) 0.008(3) C15 0.025(3) 0.030(3) 0.026(2) -0.0020(19) 0.001(2) 0.002(2) C16 0.024(3) 0.022(2) 0.030(2) 0.0085(18) 0.002(2) 0.011(2) C17 0.028(3) 0.026(3) 0.026(2) 0.0093(19) 0.004(2) 0.009(2) C18 0.032(3) 0.035(3) 0.023(2) 0.003(2) 0.001(2) 0.006(3) C19 0.036(3) 0.025(3) 0.030(2) 0.005(2) 0.010(2) 0.005(2) C20 0.039(3) 0.030(3) 0.022(2) 0.0054(19) 0.005(2) 0.012(2) C21 0.030(3) 0.029(3) 0.022(2) 0.0089(19) 0.007(2) 0.011(2) C22 0.037(3) 0.031(3) 0.022(2) 0.0104(19) 0.004(2) 0.012(2) C23 0.036(3) 0.046(3) 0.027(2) 0.007(2) 0.007(2) 0.015(3) C24 0.039(3) 0.036(3) 0.030(2) 0.015(2) 0.008(2) 0.013(3) C25 0.030(3) 0.033(3) 0.035(3) 0.004(2) 0.006(2) 0.007(2) C26 0.033(3) 0.024(3) 0.024(2) 0.0072(18) 0.005(2) 0.011(2) C27 0.034(3) 0.043(3) 0.027(2) 0.004(2) 0.001(2) 0.006(3) C28 0.049(4) 0.040(3) 0.050(3) -0.002(3) -0.001(3) 0.008(3) C29 0.042(4) 0.068(4) 0.043(3) 0.016(3) -0.005(3) 0.012(3) C30 0.033(3) 0.025(3) 0.031(2) 0.0122(19) 0.003(2) 0.010(2) C31 0.043(3) 0.043(3) 0.027(2) 0.004(2) -0.001(2) 0.013(3) C32 0.037(3) 0.036(3) 0.038(3) 0.017(2) 0.007(2) 0.017(3) C33 0.027(3) 0.019(2) 0.026(2) 0.0001(18) 0.002(2) -0.002(2) C34 0.024(3) 0.015(2) 0.034(2) 0.0028(18) 0.003(2) 0.000(2) C35 0.028(3) 0.024(2) 0.034(2) -0.0023(19) 0.006(2) 0.004(2) C36 0.034(3) 0.033(3) 0.023(2) -0.0051(19) 0.001(2) 0.005(2) C37 0.027(3) 0.027(3) 0.027(2) -0.0017(19) -0.002(2) 0.002(2) C38 0.031(3) 0.020(2) 0.027(2) 0.0024(18) 0.001(2) 0.006(2) C39 0.034(3) 0.030(3) 0.035(2) 0.012(2) 0.011(2) 0.013(2) C40 0.116(6) 0.061(4) 0.077(5) -0.001(4) -0.017(4) 0.059(5) C41 0.038(4) 0.084(5) 0.062(4) 0.047(3) 0.007(3) 0.021(3) C42 0.024(3) 0.026(3) 0.028(2) 0.0002(19) 0.002(2) -0.001(2) C43 0.031(3) 0.044(3) 0.049(3) 0.006(2) 0.008(2) 0.012(3) C44 0.033(3) 0.043(3) 0.034(3) 0.002(2) 0.000(2) 0.015(3) C45 0.054(4) 0.049(4) 0.116(6) 0.036(4) 0.028(4) 0.015(4) C46 0.067(4) 0.061(4) 0.041(3) 0.013(3) 0.014(3) 0.026(3) C47 0.084(5) 0.051(4) 0.065(4) 0.006(3) 0.034(4) 0.023(4) Br1 0.0554(4) 0.0541(4) 0.0553(4) 0.0344(3) 0.0075(3) 0.0195(3) Br2 0.0468(4) 0.0594(4) 0.0255(3) 0.0031(2) 0.0081(2) 0.0172(3) Cu1 0.0273(4) 0.0226(4) 0.0210(3) 0.0020(3) 0.0035(3) 0.0053(3) Cu2 0.0298(6) 0.0234(5) 0.0245(5) 0.0055(4) -0.0040(4) 0.0019(5) N1 0.029(2) 0.022(2) 0.0229(18) 0.0024(15) 0.0043(17) 0.0072(19) N2 0.021(2) 0.024(2) 0.0234(18) 0.0028(15) 0.0016(16) 0.0034(17) N3 0.031(2) 0.0183(19) 0.0230(18) 0.0070(15) 0.0056(16) 0.0075(19) N4 0.029(2) 0.029(2) 0.0235(19) 0.0093(16) -0.0011(17) 0.0082(19) O1 0.0342(19) 0.0240(17) 0.0263(15) 0.0031(12) 0.0010(14) 0.0084(15) O2 0.032(2) 0.0289(18) 0.0303(17) 0.0066(13) -0.0043(14) 0.0014(16) O3 0.0317(19) 0.0363(19) 0.0370(17) 0.0121(14) 0.0091(15) 0.0135(16) O4 0.0310(19) 0.0244(17) 0.0255(15) 0.0025(12) 0.0029(13) 0.0067(15) O5 0.0316(19) 0.0204(16) 0.0247(15) 0.0066(12) -0.0013(13) 0.0057(15) O6 0.0266(18) 0.0286(17) 0.0278(15) 0.0005(13) 0.0036(13) 0.0031(15) O7 0.0256(18) 0.0225(16) 0.0245(15) 0.0029(12) 0.0011(13) 0.0036(14) O8 0.0232(18) 0.0293(17) 0.0243(15) 0.0040(12) -0.0002(13) 0.0023(15) O9 0.059(3) 0.043(2) 0.045(2) 0.0150(17) -0.0003(18) 0.019(2) O10 0.064(3) 0.043(2) 0.0392(19) 0.0093(16) 0.0197(18) 0.029(2) O11 0.042(2) 0.039(2) 0.0371(18) 0.0010(15) 0.0114(16) 0.0109(18) O12 0.043(3) 0.063(3) 0.076(3) 0.023(2) 0.012(2) 0.018(2) P1 0.0275(7) 0.0239(6) 0.0251(6) 0.0061(5) 0.0033(5) 0.0057(6) P2 0.0233(7) 0.0211(6) 0.0214(5) 0.0031(4) 0.0009(5) 0.0033(5) 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' Br Br -0.6763 1.2805 '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' P P 0.2955 0.4335 '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 N1 C1 C2 122.0(4) . . N1 C1 H1 119.0 . . C2 C1 H1 119.0 . . C1 C2 C3 120.0(5) . . C1 C2 H2A 120.0 . . C3 C2 H2A 120.0 . . C2 C3 C4 118.6(4) . . C2 C3 H3 120.7 . . C4 C3 H3 120.7 . . C5 C4 C3 118.9(4) . . C5 C4 H4 120.5 . . C3 C4 H4 120.5 . . N1 C5 C4 122.3(4) . . N1 C5 C6 113.9(3) . . C4 C5 C6 123.7(4) . . N2 C6 C7 120.3(4) . . N2 C6 C5 113.4(4) . . C7 C6 C5 126.3(4) . . C6 C7 C8 119.6(4) . . C6 C7 H7 120.2 . . C8 C7 H7 120.2 . . C7 C8 C9 118.9(4) . . C7 C8 C16 120.3(4) . . C9 C8 C16 120.8(4) . . C10 C9 C8 119.0(4) . . C10 C9 H9 120.5 . . C8 C9 H9 120.5 . . N2 C10 C9 120.4(4) . . N2 C10 C11 112.4(4) . . C9 C10 C11 127.1(4) . . N3 C11 C12 121.1(4) . . N3 C11 C10 114.1(4) . . C12 C11 C10 124.7(4) . . C13 C12 C11 119.2(5) . . C13 C12 H12 120.4 . . C11 C12 H12 120.4 . . C14 C13 C12 119.3(4) . . C14 C13 H13 120.4 . . C12 C13 H13 120.4 . . C13 C14 C15 119.0(4) . . C13 C14 H14 120.5 . . C15 C14 H14 120.5 . . N3 C15 C14 122.1(4) . . N3 C15 H15 119.0 . . C14 C15 H15 119.0 . . C20 C16 C17 116.3(4) . . C20 C16 C8 122.5(4) . . C17 C16 C8 121.2(4) . . C18 C17 C16 120.4(4) . . C18 C17 H17 119.8 . . C16 C17 H17 119.8 . . N4 C18 C17 122.9(4) . . N4 C18 H18 118.6 . . C17 C18 H18 118.6 . . N4 C19 C20 123.4(4) . . N4 C19 H19 118.3 . . C20 C19 H19 118.3 . . C16 C20 C19 119.8(4) . . C16 C20 H20 120.1 . . C19 C20 H20 120.1 . . C26 C21 O4 119.8(4) . . C26 C21 C22 122.5(4) . . O4 C21 C22 117.5(4) . . C23 C22 C21 117.7(4) . . C23 C22 C27 121.7(4) . . C21 C22 C27 120.6(4) . . C22 C23 C24 120.4(4) . . C22 C23 H23 119.8 . . C24 C23 H23 119.8 . . C25 C24 C23 121.5(4) . . C25 C24 Br1 118.4(4) . . C23 C24 Br1 120.1(3) . . C24 C25 C26 120.0(5) . . C24 C25 H25 120.0 . . C26 C25 H25 120.0 . . C21 C26 C25 117.8(4) . . C21 C26 C30 122.8(4) . . C25 C26 C30 119.4(4) . . C22 C27 C28 110.6(4) . . C22 C27 C29 113.8(4) . . C28 C27 C29 110.2(4) . . C22 C27 H27 107.3 . . C28 C27 H27 107.3 . . C29 C27 H27 107.3 . . C27 C28 H28A 109.5 . . C27 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C27 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . C27 C29 H29A 109.5 . . C27 C29 H29B 109.5 . . H29A C29 H29B 109.5 . . C27 C29 H29C 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . C32 C30 C31 111.4(4) . . C32 C30 C26 111.2(4) . . C31 C30 C26 110.7(4) . . C32 C30 H30 107.8 . . C31 C30 H30 107.8 . . C26 C30 H30 107.8 . . C30 C31 H31A 109.5 . . C30 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . C30 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . C30 C32 H32A 109.5 . . C30 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C30 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C38 C33 C34 124.0(4) . . C38 C33 O7 116.7(4) . . C34 C33 O7 119.2(4) . . C35 C34 C33 116.6(4) . . C35 C34 C39 121.1(4) . . C33 C34 C39 122.3(4) . . C36 C35 C34 120.1(4) . . C36 C35 H35 119.9 . . C34 C35 H35 119.9 . . C37 C36 C35 122.3(4) . . C37 C36 Br2 117.5(3) . . C35 C36 Br2 120.1(4) . . C36 C37 C38 120.0(4) . . C36 C37 H37 120.0 . . C38 C37 H37 120.0 . . C37 C38 C33 116.7(4) . . C37 C38 C42 122.3(4) . . C33 C38 C42 120.8(4) . . C41 C39 C40 111.3(5) . . C41 C39 C34 112.5(4) . . C40 C39 C34 111.6(4) . . C41 C39 H39 107.0 . . C40 C39 H39 107.0 . . C34 C39 H39 107.0 . . C39 C40 H40A 109.5 . . C39 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C39 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C39 C41 H41A 109.5 . . C39 C41 H41B 109.5 . . H41A C41 H41B 109.5 . . C39 C41 H41C 109.5 . . H41A C41 H41C 109.5 . . H41B C41 H41C 109.5 . . C38 C42 C43 109.8(4) . . C38 C42 C44 113.2(4) . . C43 C42 C44 109.8(4) . . C38 C42 H42 107.9 . . C43 C42 H42 107.9 . . C44 C42 H42 107.9 . . C42 C43 H43A 109.5 . . C42 C43 H43B 109.5 . . H43A C43 H43B 109.5 . . C42 C43 H43C 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C42 C44 H44A 109.5 . . C42 C44 H44B 109.5 . . H44A C44 H44B 109.5 . . C42 C44 H44C 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . O12 C45 H45A 109.5 . . O12 C45 H45B 109.5 . . H45A C45 H45B 109.5 . . O12 C45 H45C 109.5 . . H45A C45 H45C 109.5 . . H45B C45 H45C 109.5 . . O10 C46 H46A 109.5 . . O10 C46 H46B 109.5 . . H46A C46 H46B 109.5 . . O10 C46 H46C 109.5 . . H46A C46 H46C 109.5 . . H46B C46 H46C 109.5 . . O11 C47 H47A 109.5 . . O11 C47 H47B 109.5 . . H47A C47 H47B 109.5 . . O11 C47 H47C 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . N2 Cu1 O5 166.41(13) . . N2 Cu1 N1 79.69(15) . . O5 Cu1 N1 103.30(14) . . N2 Cu1 N3 79.12(15) . . O5 Cu1 N3 96.12(14) . . N1 Cu1 N3 158.14(15) . . N2 Cu1 O1 95.45(14) . . O5 Cu1 O1 97.57(12) . . N1 Cu1 O1 93.59(12) . . N3 Cu1 O1 93.69(12) . . O8 Cu2 O8 180.0 . 2_676 O8 Cu2 N4 93.55(13) . 1_665 O8 Cu2 N4 86.45(13) 2_676 1_665 O8 Cu2 N4 86.45(13) . 2_566 O8 Cu2 N4 93.55(13) 2_676 2_566 N4 Cu2 N4 180.0 1_665 2_566 O8 Cu2 O9 90.17(12) . . O8 Cu2 O9 89.83(12) 2_676 . N4 Cu2 O9 93.78(14) 1_665 . N4 Cu2 O9 86.22(14) 2_566 . C1 N1 C5 118.2(4) . . C1 N1 Cu1 127.9(3) . . C5 N1 Cu1 113.7(3) . . C10 N2 C6 121.7(4) . . C10 N2 Cu1 119.7(3) . . C6 N2 Cu1 118.3(3) . . C15 N3 C11 119.2(4) . . C15 N3 Cu1 126.2(3) . . C11 N3 Cu1 114.5(3) . . C19 N4 C18 117.2(4) . . C19 N4 Cu2 123.3(3) . 1_445 C18 N4 Cu2 119.5(3) . 1_445 P1 O1 Cu1 127.78(17) . . P1 O2 H2 109.5 . . C21 O4 P1 125.8(3) . . P2 O5 Cu1 131.79(17) . . C33 O7 P2 124.7(3) . . P2 O8 Cu2 136.87(19) . . Cu2 O9 H9A 110.8 . . Cu2 O9 H9B 110.1 . . H9A O9 H9B 108.4 . . C46 O10 H10 109.5 . . C47 O11 H11 109.5 . . C45 O12 H12A 109.5 . . O3 P1 O1 116.71(18) . . O3 P1 O2 110.03(19) . . O1 P1 O2 110.20(17) . . O3 P1 O4 110.24(16) . . O1 P1 O4 109.18(18) . . O2 P1 O4 99.04(17) . . O6 P2 O8 114.19(17) . . O6 P2 O5 113.33(17) . . O8 P2 O5 110.45(18) . . O6 P2 O7 106.53(17) . . O8 P2 O7 106.25(16) . . O5 P2 O7 105.36(16) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N1 1.338(6) . C1 C2 1.374(6) . C1 H1 0.9500 . C2 C3 1.375(7) . C2 H2A 0.9500 . C3 C4 1.390(6) . C3 H3 0.9500 . C4 C5 1.370(6) . C4 H4 0.9500 . C5 N1 1.362(6) . C5 C6 1.471(6) . C6 N2 1.344(5) . C6 C7 1.379(6) . C7 C8 1.386(6) . C7 H7 0.9500 . C8 C9 1.404(6) . C8 C16 1.495(6) . C9 C10 1.383(6) . C9 H9 0.9500 . C10 N2 1.338(5) . C10 C11 1.481(6) . C11 N3 1.348(6) . C11 C12 1.383(6) . C12 C13 1.371(6) . C12 H12 0.9500 . C13 C14 1.366(7) . C13 H13 0.9500 . C14 C15 1.385(6) . C14 H14 0.9500 . C15 N3 1.322(5) . C15 H15 0.9500 . C16 C20 1.381(6) . C16 C17 1.393(6) . C17 C18 1.367(6) . C17 H17 0.9500 . C18 N4 1.339(6) . C18 H18 0.9500 . C19 N4 1.326(6) . C19 C20 1.382(7) . C19 H19 0.9500 . C20 H20 0.9500 . C21 C26 1.384(6) . C21 O4 1.385(5) . C21 C22 1.411(6) . C22 C23 1.380(6) . C22 C27 1.511(7) . C23 C24 1.381(7) . C23 H23 0.9500 . C24 C25 1.375(7) . C24 Br1 1.901(4) . C25 C26 1.400(6) . C25 H25 0.9500 . C26 C30 1.524(6) . C27 C28 1.535(7) . C27 C29 1.535(7) . C27 H27 1.0000 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C30 C32 1.516(6) . C30 C31 1.524(6) . C30 H30 1.0000 . C31 H31A 0.9800 . C31 H31B 0.9800 . C31 H31C 0.9800 . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C33 C38 1.397(6) . C33 C34 1.400(6) . C33 O7 1.402(5) . C34 C35 1.389(6) . C34 C39 1.518(6) . C35 C36 1.378(6) . C35 H35 0.9500 . C36 C37 1.372(7) . C36 Br2 1.904(4) . C37 C38 1.393(6) . C37 H37 0.9500 . C38 C42 1.505(6) . C39 C41 1.501(7) . C39 C40 1.509(7) . C39 H39 1.0000 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C41 H41A 0.9800 . C41 H41B 0.9800 . C41 H41C 0.9800 . C42 C43 1.517(7) . C42 C44 1.538(6) . C42 H42 1.0000 . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . C45 O12 1.413(6) . C45 H45A 0.9800 . C45 H45B 0.9800 . C45 H45C 0.9800 . C46 O10 1.412(6) . C46 H46A 0.9800 . C46 H46B 0.9800 . C46 H46C 0.9800 . C47 O11 1.418(6) . C47 H47A 0.9800 . C47 H47B 0.9800 . C47 H47C 0.9800 . Cu1 N2 1.941(4) . Cu1 O5 1.945(3) . Cu1 N1 2.049(3) . Cu1 N3 2.050(3) . Cu1 O1 2.138(3) . Cu2 O8 1.947(3) . Cu2 O8 1.947(3) 2_676 Cu2 N4 2.046(4) 1_665 Cu2 N4 2.046(4) 2_566 Cu2 O9 2.533(4) . N4 Cu2 2.046(4) 1_445 O1 P1 1.495(3) . O2 P1 1.564(3) . O2 H2 0.8400 . O3 P1 1.494(3) . O4 P1 1.608(3) . O5 P2 1.532(3) . O6 P2 1.488(3) . O7 P2 1.617(3) . O8 P2 1.516(3) . O9 H9A 0.8901 . O9 H9B 0.8903 . O10 H10 0.8400 . O11 H11 0.8400 . O12 H12A 0.8400 . 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 O2 H2 O5 0.84 1.82 2.662(4) 175.5 . O11 H11 O3 0.84 2.06 2.897(5) 173.7 . O10 H10 O3 0.84 1.84 2.674(4) 169.5 . O9 H9A O12 0.89 2.37 2.915(6) 119.3 1_455 O9 H9B O6 0.89 1.97 2.736(4) 143.7 2_676 O12 H12A O6 0.84 1.95 2.732(5) 154.0 . C7 H7 O11 0.95 2.63 3.556(5) 166.1 2_666 C12 H12 O3 0.95 2.66 3.459(6) 142.4 1_455 C1 H1 O6 0.95 2.40 3.299(6) 158.3 . C9 H9 O10 0.95 2.40 3.333(6) 168.7 1_455 C17 H17 O11 0.95 2.63 3.570(6) 168.7 2_666 C14 H14 Br2 0.95 3.01 3.705(5) 131.0 2_677 C4 H4 O11 0.95 2.42 3.367(6) 173.1 2_666 C20 H20 O10 0.95 2.31 3.247(5) 170.8 1_455 O2 H2 O5 0.84 1.82 2.662(4) 175.5 . O11 H11 O3 0.84 2.06 2.897(5) 173.7 . O10 H10 O3 0.84 1.84 2.674(4) 169.5 . O9 H9A O12 0.89 2.37 2.915(6) 119.3 1_455 O9 H9B O6 0.89 1.97 2.736(4) 143.7 2_676 O12 H12A O6 0.84 1.95 2.732(5) 154.0 . C7 H7 O11 0.95 2.63 3.556(5) 166.1 2_666 C12 H12 O3 0.95 2.66 3.459(6) 142.4 1_455 C1 H1 O6 0.95 2.40 3.299(6) 158.3 . C9 H9 O10 0.95 2.40 3.333(6) 168.7 1_455 C17 H17 O11 0.95 2.63 3.570(6) 168.7 2_666 C14 H14 Br2 0.95 3.01 3.705(5) 131.0 2_677 C4 H4 O11 0.95 2.42 3.367(6) 173.1 2_666 C20 H20 O10 0.95 2.31 3.247(5) 170.8 1_455 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_4 N1 C1 C2 C3 -0.7(7) . C1 C2 C3 C4 0.4(7) . C2 C3 C4 C5 -0.2(6) . C3 C4 C5 N1 0.3(6) . C3 C4 C5 C6 178.5(4) . N1 C5 C6 N2 1.4(5) . C4 C5 C6 N2 -177.0(4) . N1 C5 C6 C7 -177.7(4) . C4 C5 C6 C7 3.9(6) . N2 C6 C7 C8 2.0(6) . C5 C6 C7 C8 -178.9(4) . C6 C7 C8 C9 0.6(6) . C6 C7 C8 C16 -179.2(3) . C7 C8 C9 C10 -1.9(6) . C16 C8 C9 C10 177.9(3) . C8 C9 C10 N2 0.6(6) . C8 C9 C10 C11 -175.0(4) . N2 C10 C11 N3 -5.0(5) . C9 C10 C11 N3 170.9(4) . N2 C10 C11 C12 177.5(4) . C9 C10 C11 C12 -6.6(6) . N3 C11 C12 C13 -1.9(6) . C10 C11 C12 C13 175.5(4) . C11 C12 C13 C14 -1.7(6) . C12 C13 C14 C15 2.7(6) . C13 C14 C15 N3 -0.2(7) . C7 C8 C16 C20 167.8(4) . C9 C8 C16 C20 -12.1(6) . C7 C8 C16 C17 -11.0(5) . C9 C8 C16 C17 169.2(4) . C20 C16 C17 C18 -1.9(6) . C8 C16 C17 C18 176.9(4) . C16 C17 C18 N4 -0.9(6) . C17 C16 C20 C19 2.1(6) . C8 C16 C20 C19 -176.7(4) . N4 C19 C20 C16 0.4(7) . C26 C21 C22 C23 2.9(6) . O4 C21 C22 C23 178.3(4) . C26 C21 C22 C27 -174.8(4) . O4 C21 C22 C27 0.5(6) . C21 C22 C23 C24 -0.2(7) . C27 C22 C23 C24 177.5(4) . C22 C23 C24 C25 -1.9(7) . C22 C23 C24 Br1 178.0(3) . C23 C24 C25 C26 1.3(7) . Br1 C24 C25 C26 -178.5(3) . O4 C21 C26 C25 -178.7(4) . C22 C21 C26 C25 -3.5(6) . O4 C21 C26 C30 0.1(6) . C22 C21 C26 C30 175.4(4) . C24 C25 C26 C21 1.3(6) . C24 C25 C26 C30 -177.6(4) . C23 C22 C27 C28 -106.9(5) . C21 C22 C27 C28 70.8(5) . C23 C22 C27 C29 17.9(6) . C21 C22 C27 C29 -164.4(4) . C21 C26 C30 C32 -123.2(4) . C25 C26 C30 C32 55.7(5) . C21 C26 C30 C31 112.4(5) . C25 C26 C30 C31 -68.8(5) . C38 C33 C34 C35 -2.4(7) . O7 C33 C34 C35 -178.4(4) . C38 C33 C34 C39 177.7(4) . O7 C33 C34 C39 1.7(6) . C33 C34 C35 C36 -1.9(7) . C39 C34 C35 C36 178.0(4) . C34 C35 C36 C37 4.0(7) . C34 C35 C36 Br2 -176.5(3) . C35 C36 C37 C38 -1.7(7) . Br2 C36 C37 C38 178.7(3) . C36 C37 C38 C33 -2.4(7) . C36 C37 C38 C42 173.5(4) . C34 C33 C38 C37 4.5(7) . O7 C33 C38 C37 -179.4(4) . C34 C33 C38 C42 -171.4(4) . O7 C33 C38 C42 4.7(6) . C35 C34 C39 C41 -61.2(6) . C33 C34 C39 C41 118.7(5) . C35 C34 C39 C40 64.8(6) . C33 C34 C39 C40 -115.4(6) . C37 C38 C42 C43 -102.8(5) . C33 C38 C42 C43 72.9(5) . C37 C38 C42 C44 20.3(6) . C33 C38 C42 C44 -164.0(4) . C2 C1 N1 C5 0.7(6) . C2 C1 N1 Cu1 175.2(3) . C4 C5 N1 C1 -0.5(6) . C6 C5 N1 C1 -178.9(3) . C4 C5 N1 Cu1 -175.8(3) . C6 C5 N1 Cu1 5.8(4) . C9 C10 N2 C6 2.0(6) . C11 C10 N2 C6 178.3(3) . C9 C10 N2 Cu1 -171.8(3) . C11 C10 N2 Cu1 4.5(4) . C7 C6 N2 C10 -3.4(6) . C5 C6 N2 C10 177.5(3) . C7 C6 N2 Cu1 170.5(3) . C5 C6 N2 Cu1 -8.7(4) . C14 C15 N3 C11 -3.3(6) . C14 C15 N3 Cu1 -179.6(3) . C12 C11 N3 C15 4.3(6) . C10 C11 N3 C15 -173.3(3) . C12 C11 N3 Cu1 -179.0(3) . C10 C11 N3 Cu1 3.4(4) . C20 C19 N4 C18 -3.2(6) . C20 C19 N4 Cu2 175.9(3) 1_445 C17 C18 N4 C19 3.4(6) . C17 C18 N4 Cu2 -175.7(3) 1_445 C26 C21 O4 P1 -89.7(4) . C22 C21 O4 P1 94.8(4) . C38 C33 O7 P2 94.9(4) . C34 C33 O7 P2 -88.8(4) . Cu1 O1 P1 O3 -144.5(2) . Cu1 O1 P1 O2 -18.1(3) . Cu1 O1 P1 O4 89.7(2) . C21 O4 P1 O3 -31.2(4) . C21 O4 P1 O1 98.2(3) . C21 O4 P1 O2 -146.6(3) . Cu2 O8 P2 O6 -14.2(3) . Cu2 O8 P2 O5 -143.3(2) . Cu2 O8 P2 O7 102.9(3) . Cu1 O5 P2 O6 -95.6(3) . Cu1 O5 P2 O8 34.0(3) . Cu1 O5 P2 O7 148.3(2) . C33 O7 P2 O6 -134.4(3) . C33 O7 P2 O8 103.5(3) . C33 O7 P2 O5 -13.7(4) .