# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 898350' #TrackingRef 'web_deposit_cif_file_0_DebajyotiGhoshal_1350570455.898350.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H56 Cu2 N4 O16 P4' _chemical_formula_weight 1436.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_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' _cell_length_a 15.6162(3) _cell_length_b 15.6658(3) _cell_length_c 25.5674(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.9760(10) _cell_angle_gamma 90.00 _cell_volume 6251.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.6 _exptl_crystal_description Parallelopiped _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8210 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50778 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.58 _reflns_number_total 13781 _reflns_number_gt 12206 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Restraints are DELU C8 C1, C14 C46 and floating origin restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+7.6949P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.037(8) _refine_ls_number_reflns 13781 _refine_ls_number_parameters 848 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C6 C 0.5473(3) 0.4261(3) -0.01135(19) 0.0290(10) Uani 1 1 d . . . H6 H 0.5608 0.4818 -0.0205 0.035 Uiso 1 1 calc R . . C7 C 0.61175(18) 0.36816(19) -0.01070(13) 0.0319(7) Uani 1 1 d . . . H7 H 0.6677 0.3841 -0.0174 0.038 Uiso 1 1 calc R . . C8 C 0.5911(2) 0.2849(2) 0.00027(14) 0.0282(7) Uani 1 1 d U . . C9 C 0.50846(19) 0.26426(19) 0.01105(13) 0.0329(7) Uani 1 1 d . . . H9 H 0.4940 0.2081 0.0185 0.040 Uiso 1 1 calc R . . C10 C 0.4476(3) 0.3261(3) 0.01086(19) 0.0294(10) Uani 1 1 d . . . H10 H 0.3916 0.3115 0.0183 0.035 Uiso 1 1 calc R . . C11 C 0.3937(2) 0.2529(2) -0.11012(15) 0.0303(9) Uani 1 1 d . . . C12 C 0.4222(2) 0.1716(2) -0.12234(14) 0.0389(7) Uani 1 1 d . . . H12 H 0.3904 0.1238 -0.1136 0.047 Uiso 1 1 calc R . . C13 C 0.34666(18) 0.09906(19) 0.03846(12) 0.0308(6) Uani 1 1 d . . . H13 H 0.3917 0.1017 0.0632 0.037 Uiso 1 1 calc R . . C14 C 0.3426(2) 0.0350(2) 0.00215(13) 0.0269(7) Uani 1 1 d U . . C15 C 0.5181(2) 0.3126(3) -0.14610(15) 0.0464(9) Uani 1 1 d . . . H15 H 0.5503 0.3603 -0.1545 0.056 Uiso 1 1 calc R . . C16 C 0.4403(3) 0.3227(3) -0.12025(17) 0.0347(11) Uani 1 1 d . . . H16 H 0.4217 0.3766 -0.1104 0.042 Uiso 1 1 calc R . . C17 C 0.2174(2) 0.4240(2) -0.16956(12) 0.0333(7) Uani 1 1 d . . . C18 C 0.1460(2) 0.4233(3) -0.20253(15) 0.0528(10) Uani 1 1 d . . . H18 H 0.1119 0.3748 -0.2049 0.063 Uiso 1 1 calc R . . C19 C 0.1250(4) 0.4942(4) -0.2320(2) 0.0653(16) Uani 1 1 d . . . H19 H 0.0783 0.4936 -0.2556 0.078 Uiso 1 1 calc R . . C20 C 0.1726(5) 0.5628(5) -0.2259(3) 0.077(2) Uani 1 1 d . . . H20 H 0.1563 0.6114 -0.2446 0.093 Uiso 1 1 calc R . . C21 C 0.2455(3) 0.5679(3) -0.19357(16) 0.0563(10) Uani 1 1 d . . . H21 H 0.2783 0.6175 -0.1916 0.068 Uiso 1 1 calc R . . C22 C 0.2676(3) 0.4960(2) -0.16428(15) 0.0434(8) Uani 1 1 d . . . H22 H 0.3154 0.4965 -0.1415 0.052 Uiso 1 1 calc R . . C23 C 0.3735(2) 0.7745(2) -0.10853(15) 0.0294(8) Uani 1 1 d . . . C24 C 0.4429(3) 0.8226(3) -0.11795(17) 0.0346(11) Uani 1 1 d . . . H24 H 0.4975 0.8028 -0.1088 0.042 Uiso 1 1 calc R . . C25 C 0.4321(3) 0.9022(2) -0.14152(14) 0.0437(8) Uani 1 1 d . . . H25 H 0.4798 0.9352 -0.1488 0.052 Uiso 1 1 calc R . . C26 C 0.3520(3) 0.9322(2) -0.15390(14) 0.0459(9) Uani 1 1 d . . . H26 H 0.3450 0.9858 -0.1691 0.055 Uiso 1 1 calc R . . C27 C 0.2818(3) 0.8834(3) -0.14402(15) 0.0456(9) Uani 1 1 d . . . H27 H 0.2272 0.9035 -0.1529 0.055 Uiso 1 1 calc R . . C28 C 0.2918(2) 0.8040(2) -0.12079(13) 0.0377(7) Uani 1 1 d . . . H28 H 0.2442 0.7709 -0.1135 0.045 Uiso 1 1 calc R . . C29 C 0.5376(2) 0.5990(2) -0.17118(12) 0.0340(7) Uani 1 1 d . . . C30 C 0.5288(3) 0.5312(3) -0.20544(14) 0.0515(9) Uani 1 1 d . . . H30 H 0.4768 0.5026 -0.2093 0.062 Uiso 1 1 calc R . . C31 C 0.5988(4) 0.5061(4) -0.2343(2) 0.0670(16) Uani 1 1 d . . . H31 H 0.5931 0.4615 -0.2582 0.080 Uiso 1 1 calc R . . C32 C 0.6724(4) 0.5452(4) -0.2276(2) 0.0649(17) Uani 1 1 d . . . H32 H 0.7191 0.5257 -0.2458 0.078 Uiso 1 1 calc R . . C33 C 0.6836(3) 0.6167(3) -0.19360(17) 0.0615(12) Uani 1 1 d . . . H33 H 0.7358 0.6450 -0.1904 0.074 Uiso 1 1 calc R . . C34 C 0.6136(2) 0.6424(3) -0.16532(14) 0.0433(8) Uani 1 1 d . . . H34 H 0.6182 0.6887 -0.1426 0.052 Uiso 1 1 calc R . . C35 C 0.1325(2) -0.0241(2) 0.10914(14) 0.0295(8) Uani 1 1 d . . . C36 C 0.2139(2) -0.0526(2) 0.12241(14) 0.0377(7) Uani 1 1 d . . . H36 H 0.2612 -0.0192 0.1148 0.045 Uiso 1 1 calc R . . C37 C 0.2256(3) -0.1309(3) 0.14712(16) 0.0470(10) Uani 1 1 d . . . H37 H 0.2806 -0.1505 0.1555 0.056 Uiso 1 1 calc R . . C38 C 0.1557(3) -0.1794(2) 0.15909(15) 0.0511(10) Uani 1 1 d . . . H38 H 0.1632 -0.2312 0.1763 0.061 Uiso 1 1 calc R . . C39 C 0.0745(3) -0.1512(2) 0.14561(15) 0.0487(9) Uani 1 1 d . . . H39 H 0.0279 -0.1856 0.1531 0.058 Uiso 1 1 calc R . . C40 C 0.0599(3) -0.0741(3) 0.1214(2) 0.0417(13) Uani 1 1 d . . . H40 H 0.0045 -0.0553 0.1134 0.050 Uiso 1 1 calc R . . C41 C -0.0368(2) 0.1460(2) 0.17181(12) 0.0318(6) Uani 1 1 d . . . C42 C -0.1089(2) 0.0943(2) 0.16827(14) 0.0434(8) Uani 1 1 d . . . H42 H -0.1104 0.0466 0.1465 0.052 Uiso 1 1 calc R . . C43 C -0.1783(3) 0.1152(3) 0.19775(16) 0.0558(10) Uani 1 1 d . . . H43 H -0.2272 0.0815 0.1951 0.067 Uiso 1 1 calc R . . C44 C -0.1771(3) 0.1829(3) 0.2301(2) 0.0486(12) Uani 1 1 d . . . H44 H -0.2235 0.1944 0.2509 0.058 Uiso 1 1 calc R . . C45 C -0.1049(4) 0.2356(3) 0.2320(2) 0.0587(14) Uani 1 1 d . . . H45 H -0.1047 0.2845 0.2526 0.070 Uiso 1 1 calc R . . C51 C 0.2863(2) 0.3283(2) 0.17110(12) 0.0347(7) Uani 1 1 d . . . C52 C 0.2380(3) 0.2556(3) 0.16662(15) 0.0489(10) Uani 1 1 d . . . H52 H 0.1886 0.2542 0.1452 0.059 Uiso 1 1 calc R . . C53 C 0.2644(4) 0.1838(3) 0.19481(19) 0.0780(16) Uani 1 1 d . . . H53 H 0.2332 0.1336 0.1902 0.094 Uiso 1 1 calc R . . C54 C 0.3330(6) 0.1828(4) 0.2285(3) 0.082(2) Uani 1 1 d . . . H54 H 0.3476 0.1349 0.2483 0.099 Uiso 1 1 calc R . . C55 C 0.1090(2) 0.4986(2) 0.11024(15) 0.0309(8) Uani 1 1 d . . . C56 C 0.0601(3) 0.4264(3) 0.1231(2) 0.0406(13) Uani 1 1 d . . . H56 H 0.0794 0.3718 0.1155 0.049 Uiso 1 1 calc R . . C57 C -0.0154(2) 0.4379(3) 0.14676(14) 0.0453(8) Uani 1 1 d . . . H57 H -0.0488 0.3905 0.1541 0.054 Uiso 1 1 calc R . . C58 C -0.0440(2) 0.5180(3) 0.16027(15) 0.0497(10) Uani 1 1 d . . . H58 H -0.0955 0.5243 0.1770 0.060 Uiso 1 1 calc R . . C59 C 0.0044(3) 0.5880(3) 0.14869(16) 0.0475(10) Uani 1 1 d . . . H59 H -0.0147 0.6423 0.1574 0.057 Uiso 1 1 calc R . . C60 C 0.0818(2) 0.5788(2) 0.12413(14) 0.0404(8) Uani 1 1 d . . . H60 H 0.1150 0.6265 0.1171 0.049 Uiso 1 1 calc R . . C61 C 0.2827(3) 0.1596(3) 0.03769(18) 0.0286(10) Uani 1 1 d . . . H61 H 0.2842 0.2020 0.0632 0.034 Uiso 1 1 calc R . . C62 C 0.4981(3) 0.1628(3) -0.14752(16) 0.0475(10) Uani 1 1 d . . . H62 H 0.5168 0.1087 -0.1569 0.057 Uiso 1 1 calc R . . C63 C 0.5461(2) 0.2325(3) -0.15889(16) 0.0525(11) Uani 1 1 d . . . H63 H 0.5979 0.2259 -0.1753 0.063 Uiso 1 1 calc R . . C64 C 0.27686(19) 0.0333(2) -0.03448(12) 0.0310(6) Uani 1 1 d . . . H64 H 0.2731 -0.0098 -0.0595 0.037 Uiso 1 1 calc R . . C65 C 0.2161(3) 0.0974(3) -0.03347(19) 0.0314(10) Uani 1 1 d . . . H65 H 0.1716 0.0966 -0.0586 0.038 Uiso 1 1 calc R . . O1 O 0.28785(14) 0.40973(14) -0.05651(9) 0.0296(5) Uani 1 1 d . . . O2 O 0.17022(13) 0.29704(14) -0.06432(9) 0.0271(5) Uani 1 1 d . . . O3 O 0.31728(13) 0.25565(13) -0.08349(9) 0.0334(5) Uani 1 1 d . . . O4 O 0.24032(17) 0.34773(15) -0.14492(9) 0.0351(6) Uani 1 1 d . . . O5 O 0.42045(14) 0.54761(14) -0.06547(9) 0.0275(5) Uani 1 1 d . . . O6 O 0.37710(13) 0.69588(14) -0.08314(9) 0.0339(5) Uani 1 1 d . . . O7 O 0.46475(15) 0.62515(16) -0.14588(9) 0.0356(6) Uani 1 1 d . . . O8 O 0.53386(14) 0.66441(15) -0.05699(9) 0.0305(5) Uani 1 1 d . . . O9 O 0.08282(14) 0.20169(14) 0.06671(9) 0.0278(5) Uani 1 1 d . . . O10 O 0.12630(13) 0.05333(14) 0.08352(9) 0.0331(5) Uani 1 1 d . . . O11 O 0.33264(14) 0.45272(14) 0.06584(9) 0.0282(5) Uani 1 1 d . . . O12 O 0.21434(15) 0.34007(14) 0.05834(9) 0.0310(5) Uani 1 1 d . . . O13 O 0.26114(17) 0.40328(16) 0.14639(9) 0.0362(6) Uani 1 1 d . . . O14 O 0.18542(14) 0.49493(14) 0.08462(9) 0.0350(5) Uani 1 1 d . . . O15 O -0.03030(13) 0.08475(15) 0.05797(9) 0.0306(5) Uani 1 1 d . . . O16 O 0.03776(15) 0.12366(16) 0.14628(9) 0.0331(5) Uani 1 1 d . . . P1 P 0.25086(4) 0.41624(5) 0.08441(3) 0.02336(14) Uani 1 1 d . . . P2 P 0.25183(4) 0.33412(5) -0.08290(3) 0.02332(14) Uani 1 1 d . . . P3 P 0.45596(4) 0.63050(5) -0.08343(3) 0.02393(15) Uani 1 1 d . . . P4 P 0.04734(4) 0.11848(5) 0.08441(3) 0.02316(15) Uani 1 1 d . . . Cu1 Cu 0.37642(2) 0.50024(3) 0.000223(14) 0.02407(7) Uani 1 1 d . . . Cu2 Cu 0.12762(2) 0.24933(3) 0.001446(14) 0.02369(7) Uani 1 1 d . . . N2 N 0.46638(15) 0.40999(16) -0.00001(10) 0.0241(5) Uani 1 1 d . . . N4 N 0.21824(16) 0.15976(16) 0.00151(10) 0.0252(5) Uani 1 1 d . . . C66 C -0.0337(3) 0.2160(3) 0.20361(15) 0.0489(9) Uani 1 1 d . . . H66 H 0.0152 0.2498 0.2061 0.059 Uiso 1 1 calc R . . C67 C 0.3584(3) 0.3324(3) 0.20381(15) 0.0545(10) Uani 1 1 d . . . H67 H 0.3904 0.3823 0.2069 0.065 Uiso 1 1 calc R . . C68 C 0.3815(5) 0.2597(5) 0.2319(2) 0.088(2) Uani 1 1 d . . . H68 H 0.4304 0.2612 0.2536 0.105 Uiso 1 1 calc R . . C2 C 0.65842(19) 0.15283(19) -0.03696(12) 0.0314(6) Uani 1 1 d . . . H2 H 0.6152 0.1508 -0.0629 0.038 Uiso 1 1 calc R . . C1 C 0.6586(2) 0.2176(2) 0.00034(13) 0.0251(6) Uani 1 1 d U . . C3 C 0.7221(3) 0.0915(3) -0.03562(19) 0.0303(10) Uani 1 1 d . . . H3 H 0.7204 0.0490 -0.0610 0.036 Uiso 1 1 calc R . . N1 N 0.78538(15) 0.09064(15) 0.00024(10) 0.0238(5) Uani 1 1 d . . . C4 C 0.7867(3) 0.1515(3) 0.03709(18) 0.0282(9) Uani 1 1 d . . . H4 H 0.8297 0.1503 0.0632 0.034 Uiso 1 1 calc R . . C5 C 0.72597(19) 0.21621(19) 0.03765(12) 0.0317(6) Uani 1 1 d . . . H5 H 0.7302 0.2588 0.0630 0.038 Uiso 1 1 calc R . . C46 C 0.4098(2) -0.0326(2) 0.00198(13) 0.0260(7) Uani 1 1 d U . . C47 C 0.49522(19) -0.01459(19) -0.00895(13) 0.0310(6) Uani 1 1 d . . . H47 H 0.5120 0.0412 -0.0157 0.037 Uiso 1 1 calc R . . C49 C 0.4554(3) -0.1812(2) 0.01234(18) 0.0255(9) Uani 1 1 d . . . H49 H 0.4419 -0.2376 0.0196 0.031 Uiso 1 1 calc R . . C48 C 0.5552(3) -0.0811(2) -0.00971(17) 0.0254(9) Uani 1 1 d . . . H48 H 0.6111 -0.0684 -0.0186 0.030 Uiso 1 1 calc R . . C50 C 0.39129(18) -0.11839(19) 0.01272(13) 0.0317(7) Uani 1 1 d . . . H50 H 0.3356 -0.1339 0.0202 0.038 Uiso 1 1 calc R . . N3 N 0.53645(15) -0.15992(15) 0.00143(10) 0.0224(5) 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 C6 0.0219(19) 0.0236(19) 0.042(2) 0.0038(16) 0.0020(16) 0.0020(15) C7 0.0190(13) 0.0249(15) 0.0518(18) 0.0050(14) 0.0039(12) 0.0019(12) C8 0.0217(16) 0.0186(15) 0.0444(18) -0.0009(13) 0.0003(13) 0.0152(13) C9 0.0245(14) 0.0199(14) 0.055(2) 0.0047(13) 0.0060(13) 0.0054(12) C10 0.0167(18) 0.0236(19) 0.048(3) -0.0006(16) 0.0014(16) -0.0013(14) C11 0.0210(16) 0.036(2) 0.0345(17) -0.0064(15) 0.0069(13) 0.0071(14) C12 0.0390(18) 0.0302(17) 0.0478(19) -0.0033(15) 0.0051(15) 0.0069(14) C13 0.0233(14) 0.0281(15) 0.0405(17) -0.0031(13) -0.0062(12) 0.0048(12) C14 0.0175(15) 0.0176(15) 0.0459(18) 0.0038(13) 0.0066(13) 0.0119(12) C15 0.0293(17) 0.060(2) 0.051(2) 0.0077(18) 0.0108(15) -0.0026(16) C16 0.030(2) 0.042(3) 0.033(2) 0.0045(18) 0.0082(18) 0.0138(19) C17 0.0334(17) 0.0419(19) 0.0248(15) 0.0018(13) 0.0067(12) 0.0036(14) C18 0.0377(19) 0.076(3) 0.044(2) -0.0023(19) -0.0024(15) 0.0012(19) C19 0.062(3) 0.094(4) 0.039(3) -0.001(3) -0.008(2) 0.035(3) C20 0.099(5) 0.088(5) 0.045(3) 0.023(3) 0.017(3) 0.051(4) C21 0.074(3) 0.042(2) 0.054(2) 0.0170(18) 0.014(2) 0.003(2) C22 0.047(2) 0.040(2) 0.0431(19) 0.0055(15) 0.0034(16) -0.0022(17) C23 0.036(2) 0.0198(17) 0.0322(17) 0.0050(13) -0.0056(14) 0.0085(14) C24 0.037(3) 0.039(3) 0.028(2) 0.0085(17) 0.0016(18) 0.0135(19) C25 0.058(2) 0.0291(17) 0.0435(19) 0.0029(14) 0.0008(16) -0.0058(16) C26 0.072(3) 0.0258(17) 0.0395(19) 0.0037(14) -0.0018(17) 0.0102(17) C27 0.051(2) 0.041(2) 0.045(2) 0.0034(17) -0.0049(18) 0.0233(19) C28 0.0336(17) 0.0353(18) 0.0442(19) 0.0055(14) -0.0003(14) 0.0078(14) C29 0.0375(17) 0.0375(18) 0.0274(15) 0.0070(13) 0.0046(13) 0.0044(14) C30 0.068(3) 0.044(2) 0.042(2) -0.0029(16) 0.0000(17) 0.0000(19) C31 0.090(4) 0.072(3) 0.038(2) -0.010(2) -0.002(2) 0.026(3) C32 0.082(4) 0.068(3) 0.046(3) 0.015(2) 0.025(3) 0.035(3) C33 0.042(2) 0.090(3) 0.053(2) 0.018(2) 0.0129(17) 0.005(2) C34 0.045(2) 0.047(2) 0.0386(18) 0.0025(15) 0.0048(15) -0.0031(16) C35 0.034(2) 0.0261(18) 0.0290(16) -0.0004(13) 0.0060(14) 0.0064(15) C36 0.0327(16) 0.0336(18) 0.0467(19) 0.0040(15) -0.0021(14) 0.0065(14) C37 0.051(2) 0.037(2) 0.052(2) 0.0031(18) -0.0103(19) 0.0161(18) C38 0.073(3) 0.0332(19) 0.047(2) 0.0090(16) -0.0046(19) 0.0133(19) C39 0.059(2) 0.0306(18) 0.057(2) 0.0082(16) 0.0089(18) -0.0016(16) C40 0.038(3) 0.028(2) 0.059(3) 0.001(2) 0.000(2) -0.0105(19) C41 0.0342(16) 0.0357(17) 0.0255(14) 0.0026(12) 0.0009(12) 0.0029(13) C42 0.0373(18) 0.044(2) 0.050(2) -0.0052(16) 0.0142(15) -0.0070(15) C43 0.043(2) 0.067(3) 0.058(2) 0.004(2) 0.0182(17) -0.0060(18) C44 0.046(2) 0.063(3) 0.038(2) 0.007(2) 0.0175(18) 0.003(2) C45 0.071(3) 0.054(3) 0.052(3) -0.021(2) 0.014(2) 0.012(2) C51 0.0394(18) 0.0409(19) 0.0242(15) 0.0021(13) 0.0070(13) 0.0065(15) C52 0.059(3) 0.043(2) 0.044(2) 0.0114(17) 0.0026(18) -0.0025(19) C53 0.127(5) 0.047(3) 0.062(3) 0.020(2) 0.029(3) 0.010(3) C54 0.133(6) 0.070(4) 0.045(3) 0.022(3) 0.011(3) 0.054(4) C55 0.0267(18) 0.031(2) 0.0349(18) 0.0049(14) 0.0006(13) 0.0064(14) C56 0.030(3) 0.032(2) 0.059(3) -0.005(2) 0.001(2) -0.0120(19) C57 0.0293(17) 0.057(2) 0.050(2) -0.0011(17) 0.0053(14) -0.0051(16) C58 0.0268(17) 0.073(3) 0.050(2) -0.0021(19) 0.0060(15) 0.0122(18) C59 0.035(2) 0.050(3) 0.057(2) -0.012(2) 0.0053(18) 0.0193(18) C60 0.0358(17) 0.0351(18) 0.051(2) -0.0036(16) 0.0053(15) 0.0053(15) C61 0.029(2) 0.0232(19) 0.034(2) -0.0040(16) 0.0026(17) 0.0060(17) C62 0.045(2) 0.044(2) 0.054(2) -0.0048(19) 0.0100(19) 0.0188(19) C63 0.0301(18) 0.077(3) 0.051(2) -0.005(2) 0.0132(16) 0.0163(19) C64 0.0282(15) 0.0265(15) 0.0385(16) -0.0065(13) 0.0015(12) 0.0067(12) C65 0.023(2) 0.028(2) 0.043(3) -0.0012(18) -0.0001(18) 0.0055(17) O1 0.0297(11) 0.0224(11) 0.0365(12) 0.0012(9) -0.0011(9) -0.0023(9) O2 0.0225(11) 0.0256(12) 0.0335(12) 0.0050(9) 0.0043(9) 0.0006(9) O3 0.0287(11) 0.0234(10) 0.0489(13) 0.0034(10) 0.0142(10) 0.0074(9) O4 0.0489(16) 0.0288(13) 0.0279(11) -0.0009(10) 0.0035(11) -0.0016(11) O5 0.0246(11) 0.0232(11) 0.0348(12) 0.0032(9) 0.0036(9) 0.0005(9) O6 0.0265(11) 0.0264(11) 0.0489(13) 0.0113(10) 0.0045(9) 0.0082(9) O7 0.0283(13) 0.0492(16) 0.0291(12) 0.0033(11) -0.0013(9) 0.0000(11) O8 0.0234(11) 0.0296(12) 0.0385(13) -0.0013(10) 0.0007(9) -0.0027(9) O9 0.0254(11) 0.0219(11) 0.0363(12) 0.0017(9) 0.0047(9) 0.0010(9) O10 0.0277(11) 0.0280(12) 0.0441(12) 0.0117(9) 0.0077(9) 0.0070(9) O11 0.0237(11) 0.0252(12) 0.0357(12) 0.0028(9) 0.0031(9) 0.0016(9) O12 0.0317(12) 0.0238(11) 0.0373(12) -0.0010(9) -0.0035(9) -0.0033(9) O13 0.0468(16) 0.0319(13) 0.0300(12) -0.0003(10) 0.0026(11) -0.0027(11) O14 0.0310(11) 0.0264(11) 0.0487(13) 0.0033(10) 0.0151(10) 0.0059(9) O15 0.0231(11) 0.0329(12) 0.0356(12) -0.0017(10) -0.0014(9) -0.0030(10) O16 0.0301(13) 0.0406(15) 0.0286(12) 0.0030(10) 0.0030(10) 0.0008(10) P1 0.0222(3) 0.0191(3) 0.0290(4) 0.0001(3) 0.0035(3) 0.0013(3) P2 0.0226(3) 0.0192(3) 0.0284(3) 0.0006(3) 0.0034(3) 0.0016(3) P3 0.0194(3) 0.0224(4) 0.0299(4) 0.0031(3) 0.0001(3) 0.0017(3) P4 0.0191(3) 0.0222(4) 0.0283(4) 0.0032(3) 0.0015(3) 0.0018(3) Cu1 0.01895(16) 0.01861(17) 0.03489(17) 0.00386(13) 0.00441(13) 0.00816(13) Cu2 0.01871(16) 0.01892(17) 0.03374(17) 0.00428(13) 0.00507(13) 0.00835(13) N2 0.0214(13) 0.0223(14) 0.0285(13) -0.0001(10) 0.0005(10) 0.0012(11) N4 0.0236(13) 0.0229(14) 0.0294(13) 0.0059(11) 0.0057(10) 0.0028(11) C66 0.049(2) 0.049(2) 0.049(2) -0.0092(17) -0.0001(16) 0.0007(17) C67 0.051(2) 0.070(3) 0.043(2) -0.0062(18) -0.0040(17) 0.011(2) C68 0.079(4) 0.135(6) 0.048(3) 0.010(3) -0.014(3) 0.052(4) C2 0.0232(14) 0.0280(15) 0.0426(17) -0.0001(13) -0.0045(12) 0.0083(12) C1 0.0214(15) 0.0174(15) 0.0367(17) 0.0038(13) 0.0044(13) 0.0004(12) C3 0.027(2) 0.022(2) 0.042(3) -0.0045(18) -0.0001(18) 0.0068(17) N1 0.0188(12) 0.0173(12) 0.0358(14) 0.0031(11) 0.0055(10) 0.0079(10) C4 0.024(2) 0.028(2) 0.032(2) 0.0016(17) -0.0033(16) 0.0067(17) C5 0.0296(15) 0.0228(15) 0.0424(17) -0.0052(13) -0.0008(12) 0.0066(12) C46 0.0240(16) 0.0225(16) 0.0315(16) -0.0021(13) 0.0019(13) 0.0009(13) C47 0.0252(14) 0.0180(14) 0.0498(19) 0.0029(12) 0.0022(13) 0.0027(12) C49 0.0214(18) 0.0109(15) 0.044(2) 0.0020(14) 0.0000(16) 0.0034(13) C48 0.0186(18) 0.0182(17) 0.040(2) 0.0018(15) 0.0049(15) 0.0063(14) C50 0.0184(13) 0.0242(15) 0.0528(19) 0.0023(13) 0.0046(12) 0.0055(12) N3 0.0180(12) 0.0175(13) 0.0317(14) -0.0023(10) -0.0007(10) 0.0080(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C6 N2 1.330(5) . ? C6 C7 1.355(5) . ? C6 H6 0.9300 . ? C7 C8 1.375(4) . ? C7 H7 0.9300 . ? C8 C9 1.368(4) . ? C8 C1 1.490(4) . ? C9 C10 1.358(5) . ? C9 H9 0.9300 . ? C10 N2 1.376(5) . ? C10 H10 0.9300 . ? C11 C16 1.343(6) . ? C11 O3 1.395(4) . ? C11 C12 1.389(5) . ? C12 C62 1.375(5) . ? C12 H12 0.9300 . ? C13 C14 1.368(5) . ? C13 C61 1.377(5) . ? C13 H13 0.9300 . ? C14 C64 1.365(4) . ? C14 C46 1.491(4) . ? C15 C63 1.372(6) . ? C15 C16 1.411(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.374(5) . ? C17 C22 1.378(5) . ? C17 O4 1.392(4) . ? C18 C19 1.375(7) . ? C18 H18 0.9300 . ? C19 C20 1.313(9) . ? C19 H19 0.9300 . ? C20 C21 1.385(9) . ? C20 H20 0.9300 . ? C21 C22 1.389(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.349(6) . ? C23 O6 1.393(4) . ? C23 C28 1.382(5) . ? C24 C25 1.393(5) . ? C24 H24 0.9300 . ? C25 C26 1.364(6) . ? C25 H25 0.9300 . ? C26 C27 1.366(6) . ? C26 H26 0.9300 . ? C27 C28 1.385(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C34 1.371(5) . ? C29 C30 1.381(5) . ? C29 O7 1.389(4) . ? C30 C31 1.395(7) . ? C30 H30 0.9300 . ? C31 C32 1.308(9) . ? C31 H31 0.9300 . ? C32 C33 1.424(8) . ? C32 H32 0.9300 . ? C33 C34 1.391(5) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.379(5) . ? C35 O10 1.380(4) . ? C35 C40 1.423(6) . ? C36 C37 1.390(5) . ? C36 H36 0.9300 . ? C37 C38 1.373(6) . ? C37 H37 0.9300 . ? C38 C39 1.375(6) . ? C38 H38 0.9300 . ? C39 C40 1.372(6) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C66 1.365(5) . ? C41 C42 1.387(5) . ? C41 O16 1.399(4) . ? C42 C43 1.380(5) . ? C42 H42 0.9300 . ? C43 C44 1.345(7) . ? C43 H43 0.9300 . ? C44 C45 1.396(8) . ? C44 H44 0.9300 . ? C45 C66 1.383(6) . ? C45 H45 0.9300 . ? C51 C52 1.369(5) . ? C51 C67 1.380(5) . ? C51 O13 1.384(4) . ? C52 C53 1.392(6) . ? C52 H52 0.9300 . ? C53 C54 1.351(10) . ? C53 H53 0.9300 . ? C54 C68 1.423(10) . ? C54 H54 0.9300 . ? C55 C60 1.376(5) . ? C55 O14 1.382(4) . ? C55 C56 1.409(6) . ? C56 C57 1.356(6) . ? C56 H56 0.9300 . ? C57 C58 1.380(6) . ? C57 H57 0.9300 . ? C58 C59 1.371(6) . ? C58 H58 0.9300 . ? C59 C60 1.388(5) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 N4 1.343(5) . ? C61 H61 0.9300 . ? C62 C63 1.363(6) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 C65 1.382(5) . ? C64 H64 0.9300 . ? C65 N4 1.324(5) . ? C65 H65 0.9300 . ? O1 P2 1.466(2) . ? O1 Cu1 2.427(2) . ? O2 P2 1.493(2) . ? O2 Cu2 1.976(2) . ? O3 P2 1.599(2) . ? O4 P2 1.604(2) . ? O5 P3 1.491(2) . ? O5 Cu1 1.981(2) . ? O6 P3 1.602(2) . ? O7 P3 1.609(2) . ? O8 P3 1.470(2) . ? O9 P4 1.493(2) . ? O9 Cu2 1.978(2) . ? O10 P4 1.601(2) . ? O11 P1 1.492(2) . ? O11 Cu1 1.979(2) . ? O12 P1 1.472(2) . ? O12 Cu2 2.416(2) . ? O13 P1 1.600(2) . ? O14 P1 1.601(2) . ? O15 P4 1.466(2) . ? O15 Cu1 2.430(2) 3_445 ? O16 P4 1.596(2) . ? Cu1 N1 2.007(2) 3_455 ? Cu1 N2 1.993(3) . ? Cu1 O15 2.430(2) 3 ? Cu2 N4 1.993(3) . ? Cu2 N3 2.012(2) 3_455 ? C66 H66 0.9300 . ? C67 C68 1.387(8) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C2 C3 1.382(5) . ? C2 C1 1.393(5) . ? C2 H2 0.9300 . ? C1 C5 1.395(4) . ? C3 N1 1.325(5) . ? C3 H3 0.9300 . ? N1 C4 1.340(5) . ? N1 Cu1 2.007(2) 3_545 ? C4 C5 1.389(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C46 C47 1.401(4) . ? C46 C50 1.403(4) . ? C47 C48 1.402(5) . ? C47 H47 0.9300 . ? C49 N3 1.347(5) . ? C49 C50 1.404(5) . ? C49 H49 0.9300 . ? C48 N3 1.303(5) . ? C48 H48 0.9300 . ? C50 H50 0.9300 . ? N3 Cu2 2.012(2) 3_545 ? 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 N2 C6 C7 125.5(4) . . ? N2 C6 H6 117.2 . . ? C7 C6 H6 117.2 . . ? C6 C7 C8 117.3(3) . . ? C6 C7 H7 121.3 . . ? C8 C7 H7 121.3 . . ? C9 C8 C7 119.6(3) . . ? C9 C8 C1 120.3(3) . . ? C7 C8 C1 120.0(3) . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 121.8(4) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C16 C11 O3 123.2(3) . . ? C16 C11 C12 121.5(3) . . ? O3 C11 C12 115.1(3) . . ? C62 C12 C11 119.0(3) . . ? C62 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C61 118.6(3) . . ? C14 C13 H13 120.7 . . ? C61 C13 H13 120.7 . . ? C13 C14 C64 119.7(3) . . ? C13 C14 C46 120.5(3) . . ? C64 C14 C46 119.8(3) . . ? C63 C15 C16 120.1(4) . . ? C63 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 118.7(4) . . ? C11 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C22 120.9(4) . . ? C18 C17 O4 117.5(3) . . ? C22 C17 O4 121.5(3) . . ? C17 C18 C19 120.2(5) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 118.2(6) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C21 124.6(6) . . ? C19 C20 H20 117.7 . . ? C21 C20 H20 117.7 . . ? C20 C21 C22 117.3(5) . . ? C20 C21 H21 121.4 . . ? C22 C21 H21 121.4 . . ? C17 C22 C21 118.7(4) . . ? C17 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 O6 123.9(3) . . ? C24 C23 C28 121.0(3) . . ? O6 C23 C28 115.0(3) . . ? C23 C24 C25 119.4(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.3(4) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.2(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 119.1(4) . . ? C23 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C34 C29 C30 121.2(3) . . ? C34 C29 O7 121.5(3) . . ? C30 C29 O7 117.2(3) . . ? C29 C30 C31 119.3(4) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 119.9(5) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 122.5(5) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C34 C33 C32 117.6(4) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 121.2 . . ? C29 C34 C33 119.5(4) . . ? C29 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 O10 116.7(3) . . ? C36 C35 C40 120.2(4) . . ? O10 C35 C40 123.1(4) . . ? C35 C36 C37 120.2(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 119.8(4) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 122.2(4) . . ? C38 C39 H39 118.9 . . ? C40 C39 H39 118.9 . . ? C39 C40 C35 117.6(5) . . ? C39 C40 H40 121.2 . . ? C35 C40 H40 121.2 . . ? C66 C41 C42 121.3(3) . . ? C66 C41 O16 117.8(3) . . ? C42 C41 O16 120.7(3) . . ? C43 C42 C41 118.4(4) . . ? C43 C42 H42 120.8 . . ? C41 C42 H42 120.8 . . ? C44 C43 C42 122.0(4) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C43 C44 C45 118.7(4) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C44 C45 C66 120.9(4) . . ? C44 C45 H45 119.5 . . ? C66 C45 H45 119.5 . . ? C52 C51 C67 121.6(4) . . ? C52 C51 O13 121.4(3) . . ? C67 C51 O13 116.8(3) . . ? C51 C52 C53 118.5(4) . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? C54 C53 C52 123.6(5) . . ? C54 C53 H53 118.2 . . ? C52 C53 H53 118.2 . . ? C53 C54 C68 116.0(5) . . ? C53 C54 H54 122.0 . . ? C68 C54 H54 122.0 . . ? C60 C55 O14 116.1(3) . . ? C60 C55 C56 119.8(4) . . ? O14 C55 C56 124.1(3) . . ? C57 C56 C55 119.0(4) . . ? C57 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C56 C57 C58 121.7(4) . . ? C56 C57 H57 119.1 . . ? C58 C57 H57 119.1 . . ? C59 C58 C57 119.2(3) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 120.6(4) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C55 C60 C59 119.5(4) . . ? C55 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? N4 C61 C13 122.5(4) . . ? N4 C61 H61 118.8 . . ? C13 C61 H61 118.8 . . ? C63 C62 C12 120.6(4) . . ? C63 C62 H62 119.7 . . ? C12 C62 H62 119.7 . . ? C62 C63 C15 120.0(3) . . ? C62 C63 H63 120.0 . . ? C15 C63 H63 120.0 . . ? C14 C64 C65 118.3(3) . . ? C14 C64 H64 120.9 . . ? C65 C64 H64 120.9 . . ? N4 C65 C64 123.2(4) . . ? N4 C65 H65 118.4 . . ? C64 C65 H65 118.4 . . ? P2 O1 Cu1 161.63(15) . . ? P2 O2 Cu2 137.23(14) . . ? C11 O3 P2 125.9(2) . . ? C17 O4 P2 125.5(2) . . ? P3 O5 Cu1 136.98(15) . . ? C23 O6 P3 125.6(2) . . ? C29 O7 P3 125.2(2) . . ? P4 O9 Cu2 136.99(14) . . ? C35 O10 P4 126.5(2) . . ? P1 O11 Cu1 137.62(14) . . ? P1 O12 Cu2 161.81(15) . . ? C51 O13 P1 125.2(2) . . ? C55 O14 P1 126.5(2) . . ? P4 O15 Cu1 160.95(15) . 3_445 ? C41 O16 P4 125.7(2) . . ? O12 P1 O11 119.27(14) . . ? O12 P1 O14 112.85(13) . . ? O11 P1 O14 105.05(12) . . ? O12 P1 O13 111.69(13) . . ? O11 P1 O13 107.82(13) . . ? O14 P1 O13 97.85(13) . . ? O1 P2 O2 119.08(14) . . ? O1 P2 O3 112.97(13) . . ? O2 P2 O3 104.88(12) . . ? O1 P2 O4 112.07(13) . . ? O2 P2 O4 107.37(13) . . ? O3 P2 O4 98.21(13) . . ? O8 P3 O5 118.93(14) . . ? O8 P3 O6 113.01(13) . . ? O5 P3 O6 105.15(12) . . ? O8 P3 O7 112.17(13) . . ? O5 P3 O7 107.79(13) . . ? O6 P3 O7 97.45(13) . . ? O15 P4 O9 118.98(14) . . ? O15 P4 O16 111.78(13) . . ? O9 P4 O16 107.73(13) . . ? O15 P4 O10 112.87(13) . . ? O9 P4 O10 104.96(12) . . ? O16 P4 O10 98.34(13) . . ? O5 Cu1 O11 179.88(13) . . ? O5 Cu1 N1 90.14(10) . 3_455 ? O11 Cu1 N1 89.99(10) . 3_455 ? O5 Cu1 N2 89.88(10) . . ? O11 Cu1 N2 89.99(10) . . ? N1 Cu1 N2 179.67(13) 3_455 . ? O5 Cu1 O1 85.38(8) . . ? O11 Cu1 O1 94.62(8) . . ? N1 Cu1 O1 91.33(9) 3_455 . ? N2 Cu1 O1 88.34(9) . . ? O5 Cu1 O15 95.32(8) . 3 ? O11 Cu1 O15 84.68(8) . 3 ? N1 Cu1 O15 91.44(9) 3_455 3 ? N2 Cu1 O15 88.88(9) . 3 ? O1 Cu1 O15 177.14(10) . 3 ? O2 Cu2 O9 178.95(11) . . ? O2 Cu2 N4 90.41(10) . . ? O9 Cu2 N4 90.31(10) . . ? O2 Cu2 N3 89.51(10) . 3_455 ? O9 Cu2 N3 89.77(10) . 3_455 ? N4 Cu2 N3 179.79(13) . 3_455 ? O2 Cu2 O12 95.25(8) . . ? O9 Cu2 O12 85.49(9) . . ? N4 Cu2 O12 91.75(9) . . ? N3 Cu2 O12 88.07(9) 3_455 . ? C6 N2 C10 115.8(3) . . ? C6 N2 Cu1 122.8(2) . . ? C10 N2 Cu1 121.4(2) . . ? C65 N4 C61 117.7(4) . . ? C65 N4 Cu2 121.2(3) . . ? C61 N4 Cu2 121.1(3) . . ? C41 C66 C45 118.5(4) . . ? C41 C66 H66 120.7 . . ? C45 C66 H66 120.7 . . ? C68 C67 C51 117.9(5) . . ? C68 C67 H67 121.1 . . ? C51 C67 H67 121.1 . . ? C67 C68 C54 122.3(6) . . ? C67 C68 H68 118.8 . . ? C54 C68 H68 118.8 . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C5 C1 C2 116.1(3) . . ? C5 C1 C8 121.9(3) . . ? C2 C1 C8 122.0(3) . . ? C2 C3 N1 122.9(4) . . ? C2 C3 H3 118.5 . . ? N1 C3 H3 118.5 . . ? C4 N1 C3 118.2(4) . . ? C4 N1 Cu1 120.6(3) . 3_545 ? C3 N1 Cu1 121.2(3) . 3_545 ? N1 C4 C5 122.2(4) . . ? N1 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C4 C5 C1 120.2(3) . . ? C4 C5 H5 119.9 . . ? C1 C5 H5 119.9 . . ? C47 C46 C50 115.9(3) . . ? C47 C46 C14 122.2(3) . . ? C50 C46 C14 122.0(3) . . ? C46 C47 C48 119.6(3) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? N3 C49 C50 120.3(3) . . ? N3 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? N3 C48 C47 123.1(4) . . ? N3 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C49 C50 C46 121.1(3) . . ? C49 C50 H50 119.4 . . ? C46 C50 H50 119.4 . . ? C48 N3 C49 120.0(3) . . ? C48 N3 Cu2 120.3(2) . 3_545 ? C49 N3 Cu2 119.7(2) . 3_545 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.476 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.054 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 898351' #TrackingRef 'web_deposit_cif_file_1_DebajyotiGhoshal_1350570455.898351.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H138 Cu3 N14 O25 P4' _chemical_formula_weight 2611.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' _cell_length_a 54.913(3) _cell_length_b 9.8670(4) _cell_length_c 22.0227(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.587(4) _cell_angle_gamma 90.00 _cell_volume 11827.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.7 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5452 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8501 _exptl_absorpt_correction_T_max 0.9359 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93138 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -71 _diffrn_reflns_limit_h_max 70 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.67 _reflns_number_total 13717 _reflns_number_gt 10279 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Restraints are DFIX C35 C34, DFIX C34 c33. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+95.8339P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13717 _refine_ls_number_parameters 814 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.30759(7) 0.3794(4) 0.00397(17) 0.0185(7) Uani 1 1 d . . . H1 H 0.3016 0.3126 0.0279 0.022 Uiso 1 1 calc R . . C1S C 0.21458(17) 1.4691(10) 0.2184(4) 0.086(2) Uani 1 1 d . . . H1SA H 0.2000 1.4607 0.2380 0.129 Uiso 1 1 calc R . . H1SB H 0.2112 1.5258 0.1829 0.129 Uiso 1 1 calc R . . H1SC H 0.2275 1.5090 0.2464 0.129 Uiso 1 1 calc R . . C2 C 0.29766(7) 0.3906(4) -0.05692(17) 0.0178(7) Uani 1 1 d . . . H2 H 0.2856 0.3303 -0.0736 0.021 Uiso 1 1 calc R . . C2S C 0.2220(3) 1.3398(12) 0.2006(6) 0.144(5) Uani 1 1 d . . . H2SA H 0.2069 1.3048 0.1780 0.173 Uiso 1 1 calc R . . H2SB H 0.2238 1.2908 0.2392 0.173 Uiso 1 1 calc R . . C3 C 0.30582(7) 0.4922(4) -0.09328(16) 0.0169(7) Uani 1 1 d . . . C4 C 0.32496(7) 0.5727(4) -0.06665(17) 0.0189(7) Uani 1 1 d . . . H4 H 0.3313 0.6398 -0.0897 0.023 Uiso 1 1 calc R . . C5 C 0.33478(7) 0.5544(4) -0.00617(17) 0.0194(8) Uani 1 1 d . . . H5 H 0.3480 0.6073 0.0102 0.023 Uiso 1 1 calc R . . C6 C 0.29327(7) 0.5167(4) -0.15726(16) 0.0203(8) Uani 1 1 d . . . H6A H 0.2912 0.4310 -0.1789 0.024 Uiso 1 1 calc R . . H6B H 0.3035 0.5745 -0.1789 0.024 Uiso 1 1 calc R . . C7 C 0.26801(7) 0.5838(4) -0.15697(17) 0.0202(8) Uani 1 1 d . . . H7A H 0.2603 0.5956 -0.1989 0.024 Uiso 1 1 calc R . . H7B H 0.2576 0.5247 -0.1363 0.024 Uiso 1 1 calc R . . C8 C 0.27004(7) 0.7210(4) -0.1250(2) 0.0253(9) Uani 1 1 d . . . H8A H 0.2779 0.7086 -0.0833 0.030 Uiso 1 1 calc R . . H8B H 0.2805 0.7794 -0.1458 0.030 Uiso 1 1 calc R . . C9 C 0.24582(7) 0.7902(4) -0.12347(18) 0.0216(8) Uani 1 1 d . . . C10 C 0.23074(7) 0.7581(4) -0.07960(18) 0.0215(8) Uani 1 1 d . . . H10 H 0.2355 0.6911 -0.0508 0.026 Uiso 1 1 calc R . . C11 C 0.20877(8) 0.8244(4) -0.07848(17) 0.0210(8) Uani 1 1 d . . . H11 H 0.1990 0.8008 -0.0487 0.025 Uiso 1 1 calc R . . C12 C 0.21523(8) 0.9527(4) -0.16220(18) 0.0232(8) Uani 1 1 d . . . H12 H 0.2100 1.0191 -0.1909 0.028 Uiso 1 1 calc R . . C13 C 0.23725(8) 0.8897(4) -0.16568(18) 0.0244(8) Uani 1 1 d . . . H13 H 0.2465 0.9136 -0.1965 0.029 Uiso 1 1 calc R . . C14 C 0.33598(8) 0.6955(4) 0.21860(18) 0.0231(8) Uani 1 1 d . . . H14 H 0.3297 0.7508 0.1860 0.028 Uiso 1 1 calc R . . C15 C 0.33984(8) 0.7500(4) 0.27677(18) 0.0242(8) Uani 1 1 d . . . H15 H 0.3359 0.8402 0.2829 0.029 Uiso 1 1 calc R . . C16 C 0.34954(7) 0.6712(4) 0.32584(18) 0.0228(8) Uani 1 1 d . . . C17 C 0.35531(7) 0.5371(4) 0.31375(18) 0.0223(8) Uani 1 1 d . . . H17 H 0.3621 0.4809 0.3454 0.027 Uiso 1 1 calc R . . C18 C 0.35078(7) 0.4876(4) 0.25371(17) 0.0197(8) Uani 1 1 d . . . H18 H 0.3548 0.3981 0.2461 0.024 Uiso 1 1 calc R . . C19 C 0.35484(8) 0.7314(5) 0.38901(18) 0.0253(9) Uani 1 1 d . . . H19A H 0.3533 0.6619 0.4194 0.030 Uiso 1 1 calc R . . H19B H 0.3430 0.8021 0.3939 0.030 Uiso 1 1 calc R . . C20 C 0.38074(7) 0.7905(4) 0.39881(18) 0.0221(8) Uani 1 1 d . . . H20A H 0.3820 0.8618 0.3691 0.027 Uiso 1 1 calc R . . H20B H 0.3925 0.7203 0.3922 0.027 Uiso 1 1 calc R . . C21 C 0.38709(7) 0.8484(5) 0.46355(18) 0.0243(8) Uani 1 1 d . . . H21A H 0.3772 0.9285 0.4679 0.029 Uiso 1 1 calc R . . H21B H 0.3832 0.7819 0.4933 0.029 Uiso 1 1 calc R . . C22 C 0.41391(7) 0.8846(5) 0.47613(18) 0.0244(9) Uani 1 1 d . . . C23 C 0.42186(7) 1.0169(4) 0.48524(18) 0.0233(8) Uani 1 1 d . . . H23 H 0.4105 1.0867 0.4857 0.028 Uiso 1 1 calc R . . C24 C 0.44680(7) 1.0452(5) 0.49366(18) 0.0253(9) Uani 1 1 d . . . H24 H 0.4519 1.1347 0.4996 0.030 Uiso 1 1 calc R . . C25 C 0.45606(8) 0.8192(5) 0.4846(2) 0.0365(11) Uani 1 1 d . . . H25 H 0.4676 0.7505 0.4841 0.044 Uiso 1 1 calc R . . C26 C 0.43150(8) 0.7857(5) 0.4762(3) 0.0388(12) Uani 1 1 d . . . H26 H 0.4268 0.6955 0.4706 0.047 Uiso 1 1 calc R . . C27 C 0.38663(8) 0.5014(4) 0.14191(18) 0.0266(9) Uani 1 1 d . . . H27 H 0.3836 0.5917 0.1504 0.032 Uiso 1 1 calc R . . C28 C 0.41070(8) 0.4576(5) 0.14730(18) 0.0263(9) Uani 1 1 d . . . H28 H 0.4234 0.5177 0.1596 0.032 Uiso 1 1 calc R . . C29 C 0.41584(7) 0.3236(5) 0.13434(18) 0.0259(9) Uani 1 1 d . B . C30 C 0.39566(8) 0.2401(4) 0.11698(18) 0.0245(8) Uani 1 1 d . . . H30 H 0.3982 0.1494 0.1083 0.029 Uiso 1 1 calc R . . C31 C 0.37214(7) 0.2897(4) 0.11253(16) 0.0198(8) Uani 1 1 d . . . H31 H 0.3591 0.2313 0.1005 0.024 Uiso 1 1 calc R . . C32 C 0.44159(9) 0.2693(6) 0.1385(3) 0.0449(14) Uani 1 1 d . . . H32A H 0.4428 0.2180 0.1014 0.054 Uiso 1 1 calc R A 1 H32B H 0.4526 0.3461 0.1383 0.054 Uiso 1 1 calc R A 1 C33 C 0.45100(13) 0.1823(8) 0.1914(3) 0.0312(18) Uani 0.659(12) 1 d PD B 1 H33A H 0.4656 0.1340 0.1829 0.037 Uiso 0.659(12) 1 calc PR B 1 H33B H 0.4386 0.1162 0.1988 0.037 Uiso 0.659(12) 1 calc PR B 1 C33A C 0.4476(2) 0.2464(15) 0.2184(7) 0.020(3) Uani 0.341(12) 1 d P B 2 H33C H 0.4458 0.3307 0.2400 0.024 Uiso 0.341(12) 1 calc PR B 2 H33D H 0.4367 0.1789 0.2323 0.024 Uiso 0.341(12) 1 calc PR B 2 C35 C 0.47267(19) 0.1928(9) 0.3013(3) 0.112(4) Uani 1 1 d D . . C34 C 0.4572(2) 0.2728(9) 0.2474(3) 0.049(3) Uani 0.659(12) 1 d PD B 1 H34A H 0.4421 0.3054 0.2608 0.059 Uiso 0.659(12) 1 calc PR B 1 H34B H 0.4665 0.3507 0.2365 0.059 Uiso 0.659(12) 1 calc PR B 1 C34A C 0.4745(2) 0.1975(19) 0.2283(5) 0.038(4) Uani 0.341(12) 1 d P B 2 H34C H 0.4862 0.2636 0.2168 0.046 Uiso 0.341(12) 1 calc PR B 2 H34D H 0.4770 0.1096 0.2104 0.046 Uiso 0.341(12) 1 calc PR B 2 C36 C 0.47188(15) 0.0528(9) 0.3122(3) 0.081(3) Uani 1 1 d . B . H36 H 0.4650 -0.0046 0.2811 0.097 Uiso 1 1 calc R . . C37 C 0.48129(10) -0.0009(6) 0.3687(2) 0.0439(13) Uani 1 1 d . . . H37 H 0.4803 -0.0938 0.3750 0.053 Uiso 1 1 calc R B . C38 C 0.49383(10) 0.2102(6) 0.4029(2) 0.0411(12) Uani 1 1 d . . . H38 H 0.5013 0.2656 0.4342 0.049 Uiso 1 1 calc R B . C39 C 0.48542(16) 0.2684(8) 0.3474(3) 0.086(3) Uani 1 1 d . B . H39 H 0.4884 0.3598 0.3409 0.104 Uiso 1 1 calc R . . C40 C 0.29052(8) 0.0735(4) 0.07642(18) 0.0236(8) Uani 1 1 d . . . C41 C 0.27049(8) 0.0969(4) 0.0321(2) 0.0264(9) Uani 1 1 d . . . H41 H 0.2559 0.1313 0.0431 0.032 Uiso 1 1 calc R . . C42 C 0.27249(8) 0.0684(4) -0.0286(2) 0.0292(9) Uani 1 1 d . . . H42 H 0.2592 0.0832 -0.0586 0.035 Uiso 1 1 calc R . . C43 C 0.29414(9) 0.0183(5) -0.04447(19) 0.0311(10) Uani 1 1 d . . . H43 H 0.2955 0.0001 -0.0853 0.037 Uiso 1 1 calc R . . C44 C 0.31397(9) -0.0052(4) 0.0002(2) 0.0298(9) Uani 1 1 d . . . H44 H 0.3286 -0.0393 -0.0108 0.036 Uiso 1 1 calc R . . C45 C 0.31208(8) 0.0221(4) 0.06135(19) 0.0244(8) Uani 1 1 d . . . H45 H 0.3253 0.0057 0.0915 0.029 Uiso 1 1 calc R . . C46 C 0.34399(9) 0.1011(4) 0.25409(19) 0.0303(10) Uani 1 1 d . . . C47 C 0.36681(10) 0.0842(5) 0.2354(2) 0.0353(11) Uani 1 1 d . . . H47 H 0.3683 0.0585 0.1954 0.042 Uiso 1 1 calc R . . C48 C 0.38749(11) 0.1062(5) 0.2774(2) 0.0402(12) Uani 1 1 d . . . H48 H 0.4030 0.0953 0.2653 0.048 Uiso 1 1 calc R . . C49 C 0.38548(10) 0.1442(5) 0.3370(2) 0.0385(12) Uani 1 1 d . . . H49 H 0.3995 0.1605 0.3647 0.046 Uiso 1 1 calc R . . C50 C 0.36264(10) 0.1575(5) 0.3548(2) 0.0383(12) Uani 1 1 d . . . H50 H 0.3612 0.1801 0.3952 0.046 Uiso 1 1 calc R . . C51 C 0.34154(10) 0.1377(4) 0.31374(19) 0.0333(10) Uani 1 1 d . . . H51 H 0.3261 0.1488 0.3259 0.040 Uiso 1 1 calc R . . C52 C 0.45030(8) 1.2157(5) 0.66394(19) 0.0344(11) Uani 1 1 d . . . C53 C 0.46043(10) 1.2665(7) 0.7202(2) 0.0547(17) Uani 1 1 d . . . H53 H 0.4768 1.2939 0.7270 0.066 Uiso 1 1 calc R . . C54 C 0.44547(12) 1.2755(7) 0.7664(2) 0.0608(19) Uani 1 1 d . . . H54 H 0.4521 1.3087 0.8046 0.073 Uiso 1 1 calc R . . C55 C 0.42143(11) 1.2370(6) 0.7573(2) 0.0472(14) Uani 1 1 d . . . H55 H 0.4117 1.2452 0.7886 0.057 Uiso 1 1 calc R . . C56 C 0.41170(10) 1.1859(5) 0.7011(2) 0.0391(12) Uani 1 1 d . . . H56 H 0.3954 1.1583 0.6946 0.047 Uiso 1 1 calc R . . C57 C 0.42622(9) 1.1753(5) 0.6541(2) 0.0320(10) Uani 1 1 d . . . H57 H 0.4196 1.1408 0.6162 0.038 Uiso 1 1 calc R . . C58 C 0.45127(9) 1.4293(5) 0.5136(2) 0.0360(11) Uani 1 1 d . . . C59 C 0.46086(10) 1.4717(6) 0.4620(3) 0.0502(15) Uani 1 1 d . . . H59 H 0.4773 1.4969 0.4646 0.060 Uiso 1 1 calc R . . C60 C 0.44590(11) 1.4766(7) 0.4064(3) 0.0608(18) Uani 1 1 d . . . H60 H 0.4524 1.5037 0.3714 0.073 Uiso 1 1 calc R . . C61 C 0.42130(11) 1.4414(6) 0.4024(3) 0.0498(14) Uani 1 1 d . . . H61 H 0.4112 1.4458 0.3651 0.060 Uiso 1 1 calc R . . C62 C 0.41193(9) 1.3996(5) 0.4550(2) 0.0384(11) Uani 1 1 d . . . H62 H 0.3955 1.3754 0.4527 0.046 Uiso 1 1 calc R . . C63 C 0.42687(9) 1.3938(5) 0.5103(2) 0.0347(10) Uani 1 1 d . . . H63 H 0.4205 1.3660 0.5454 0.042 Uiso 1 1 calc R . . N1 N 0.32558(6) 0.4614(3) 0.02983(14) 0.0179(6) Uani 1 1 d . . . N2 N 0.20082(6) 0.9229(3) -0.11921(14) 0.0193(7) Uani 1 1 d . . . N3 N 0.34096(6) 0.5648(3) 0.20733(14) 0.0201(7) Uani 1 1 d . . . N4 N 0.46398(6) 0.9477(4) 0.49355(16) 0.0260(8) Uani 1 1 d . . . N5 N 0.36731(6) 0.4197(3) 0.12490(13) 0.0184(6) Uani 1 1 d . . . N6 N 0.49182(6) 0.0777(4) 0.41422(16) 0.0291(8) Uani 1 1 d . . . N7 N 0.36618(6) 0.8392(4) 0.06812(15) 0.0221(7) Uani 1 1 d . . . O1 O 0.31897(5) 0.2878(3) 0.15018(12) 0.0207(6) Uani 1 1 d . . . O1S O 0.24079(8) 1.2759(5) 0.16885(19) 0.0540(10) Uani 1 1 d . . . H1S H 0.2538 1.2729 0.1918 0.081 Uiso 1 1 calc R . . O2 O 0.28693(6) 0.1006(3) 0.13691(13) 0.0293(7) Uani 1 1 d . . . O3 O 0.29016(7) 0.2397(3) 0.23019(13) 0.0361(8) Uani 1 1 d . . . O2W O 0.5000 0.4860(9) 0.2500 0.120(4) Uani 1 2 d S . . H2WB H 0.4979 0.5451 0.2218 0.179 Uiso 1 1 d R . . O4 O 0.32344(7) 0.0709(3) 0.21171(14) 0.0377(8) Uani 1 1 d . . . O5 O 0.49174(5) 1.2332(3) 0.54006(13) 0.0306(7) Uani 1 1 d . . . O6 O 0.46410(6) 1.1975(4) 0.61604(14) 0.0361(8) Uani 1 1 d . . . O7 O 0.46612(6) 1.4303(4) 0.57024(18) 0.0470(10) Uani 1 1 d . . . O8 O 0.50131(6) 1.3537(5) 0.64412(17) 0.0529(11) Uani 1 1 d . . . O9 O 0.37283(6) 0.7955(3) 0.01992(14) 0.0357(8) Uani 1 1 d . . . O10 O 0.37173(6) 0.9568(3) 0.08608(15) 0.0327(7) Uani 1 1 d . . . O11 O 0.35329(6) 0.7656(3) 0.09827(13) 0.0283(7) Uani 1 1 d . . . P1 P 0.30507(2) 0.19045(11) 0.18364(5) 0.0242(2) Uani 1 1 d . . . P2 P 0.48351(2) 1.30321(15) 0.59309(6) 0.0359(3) Uani 1 1 d . . . Cu1 Cu 0.332599(9) 0.48647(5) 0.12185(2) 0.01860(12) Uani 1 1 d . . . Cu2 Cu 0.5000 1.0000 0.5000 0.02755(18) Uani 1 2 d S . . 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 0.0215(19) 0.0143(18) 0.0198(17) -0.0007(14) 0.0032(14) -0.0012(14) C1S 0.092(6) 0.086(6) 0.081(6) -0.009(5) 0.014(5) -0.006(5) C2 0.0162(17) 0.0143(18) 0.0225(18) -0.0035(14) 0.0014(14) -0.0013(14) C2S 0.198(14) 0.083(8) 0.135(10) 0.016(8) -0.038(10) -0.016(9) C3 0.0200(18) 0.0145(18) 0.0166(16) -0.0015(13) 0.0039(13) 0.0049(14) C4 0.0230(19) 0.0128(18) 0.0215(18) 0.0011(14) 0.0053(14) 0.0002(15) C5 0.0207(19) 0.0171(19) 0.0202(18) -0.0024(14) 0.0022(14) -0.0040(15) C6 0.0231(19) 0.023(2) 0.0151(16) -0.0017(15) 0.0033(14) -0.0006(16) C7 0.0234(19) 0.0179(19) 0.0186(17) 0.0015(15) 0.0001(14) -0.0002(15) C8 0.022(2) 0.017(2) 0.036(2) -0.0027(17) -0.0019(16) -0.0002(16) C9 0.024(2) 0.0146(19) 0.0251(19) -0.0035(15) -0.0014(15) -0.0039(15) C10 0.028(2) 0.0128(18) 0.0219(18) 0.0004(14) -0.0044(15) -0.0009(15) C11 0.031(2) 0.0129(18) 0.0185(17) 0.0007(14) 0.0013(15) -0.0038(15) C12 0.028(2) 0.018(2) 0.0228(19) 0.0027(15) 0.0017(16) 0.0002(16) C13 0.030(2) 0.020(2) 0.0237(19) 0.0036(16) 0.0046(16) -0.0005(16) C14 0.031(2) 0.0144(19) 0.0245(19) 0.0011(15) 0.0048(16) -0.0006(16) C15 0.032(2) 0.0142(19) 0.028(2) -0.0038(15) 0.0103(17) -0.0051(16) C16 0.023(2) 0.024(2) 0.0228(19) -0.0045(16) 0.0065(15) -0.0103(16) C17 0.025(2) 0.023(2) 0.0189(18) 0.0010(15) 0.0026(15) -0.0026(16) C18 0.0230(19) 0.0145(19) 0.0225(18) -0.0007(14) 0.0064(14) 0.0001(15) C19 0.028(2) 0.027(2) 0.0224(19) -0.0090(16) 0.0085(16) -0.0082(17) C20 0.0227(19) 0.022(2) 0.0227(19) -0.0030(15) 0.0065(15) -0.0029(16) C21 0.020(2) 0.030(2) 0.0223(19) -0.0065(16) 0.0015(15) -0.0028(16) C22 0.020(2) 0.031(2) 0.0219(19) -0.0024(16) 0.0024(15) -0.0004(17) C23 0.0183(19) 0.028(2) 0.0220(18) -0.0058(16) -0.0012(14) 0.0011(16) C24 0.022(2) 0.028(2) 0.0242(19) -0.0084(17) -0.0014(15) -0.0025(17) C25 0.026(2) 0.027(2) 0.058(3) 0.008(2) 0.009(2) 0.0047(19) C26 0.023(2) 0.025(2) 0.068(3) 0.005(2) 0.005(2) 0.0004(18) C27 0.033(2) 0.022(2) 0.0235(19) 0.0001(16) -0.0003(16) -0.0074(18) C28 0.025(2) 0.028(2) 0.0233(19) 0.0039(17) -0.0043(16) -0.0103(17) C29 0.024(2) 0.031(2) 0.0210(19) 0.0132(17) -0.0031(15) -0.0028(17) C30 0.027(2) 0.021(2) 0.0235(19) 0.0059(16) -0.0009(16) -0.0002(16) C31 0.026(2) 0.020(2) 0.0132(16) -0.0019(14) -0.0009(14) -0.0015(15) C32 0.027(2) 0.048(3) 0.057(3) 0.028(3) -0.008(2) 0.000(2) C33 0.030(4) 0.030(4) 0.032(4) 0.002(3) -0.001(3) 0.011(3) C33A 0.010(6) 0.033(8) 0.017(7) 0.009(6) 0.004(5) 0.006(5) C35 0.181(10) 0.107(7) 0.033(3) 0.036(4) -0.041(5) -0.075(7) C34 0.081(7) 0.044(5) 0.020(4) 0.002(4) -0.003(4) 0.031(5) C34A 0.012(6) 0.086(13) 0.018(6) 0.016(7) 0.006(4) 0.014(6) C36 0.114(6) 0.102(6) 0.023(3) 0.000(3) -0.008(3) -0.056(5) C37 0.047(3) 0.057(4) 0.028(2) -0.001(2) 0.004(2) -0.014(3) C38 0.058(3) 0.041(3) 0.023(2) 0.005(2) -0.004(2) 0.006(2) C39 0.139(7) 0.074(5) 0.034(3) 0.028(3) -0.031(4) -0.026(5) C40 0.035(2) 0.0122(18) 0.0227(19) -0.0005(15) 0.0002(16) -0.0084(16) C41 0.027(2) 0.015(2) 0.037(2) 0.0031(17) 0.0005(17) -0.0057(16) C42 0.037(2) 0.018(2) 0.029(2) 0.0044(17) -0.0083(18) -0.0080(18) C43 0.049(3) 0.023(2) 0.0203(19) -0.0051(16) -0.0008(18) -0.006(2) C44 0.039(2) 0.022(2) 0.029(2) -0.0074(17) 0.0046(18) 0.0013(18) C45 0.032(2) 0.0138(19) 0.0252(19) 0.0001(15) -0.0052(16) -0.0011(16) C46 0.056(3) 0.0108(19) 0.0211(19) 0.0029(15) -0.0054(19) 0.0005(19) C47 0.065(3) 0.019(2) 0.022(2) 0.0029(17) 0.004(2) -0.001(2) C48 0.059(3) 0.031(3) 0.031(2) 0.002(2) 0.006(2) 0.001(2) C49 0.059(3) 0.023(2) 0.031(2) -0.0013(19) -0.006(2) 0.009(2) C50 0.069(4) 0.023(2) 0.020(2) -0.0043(17) -0.006(2) 0.014(2) C51 0.057(3) 0.018(2) 0.024(2) 0.0009(17) 0.0024(19) 0.011(2) C52 0.034(2) 0.049(3) 0.020(2) -0.0056(19) 0.0030(17) 0.017(2) C53 0.038(3) 0.093(5) 0.030(2) -0.023(3) -0.005(2) 0.020(3) C54 0.075(4) 0.084(5) 0.022(2) -0.012(3) 0.001(2) 0.036(4) C55 0.062(4) 0.055(4) 0.029(2) 0.011(2) 0.020(2) 0.030(3) C56 0.053(3) 0.033(3) 0.034(2) 0.013(2) 0.016(2) 0.014(2) C57 0.039(3) 0.033(3) 0.025(2) 0.0000(18) 0.0064(18) 0.008(2) C58 0.034(2) 0.018(2) 0.055(3) -0.009(2) 0.004(2) 0.0020(19) C59 0.033(3) 0.033(3) 0.086(4) 0.021(3) 0.012(3) 0.006(2) C60 0.051(4) 0.061(4) 0.073(4) 0.039(3) 0.017(3) 0.016(3) C61 0.054(3) 0.038(3) 0.055(3) 0.016(3) 0.000(3) 0.010(3) C62 0.036(3) 0.020(2) 0.057(3) -0.004(2) -0.002(2) -0.0025(19) C63 0.035(3) 0.025(2) 0.045(3) -0.007(2) 0.008(2) -0.0042(19) N1 0.0205(16) 0.0159(16) 0.0172(14) -0.0001(12) 0.0021(12) 0.0003(12) N2 0.0299(18) 0.0110(15) 0.0169(15) 0.0005(12) 0.0024(13) -0.0003(13) N3 0.0284(17) 0.0137(16) 0.0178(15) -0.0023(12) 0.0019(13) -0.0008(13) N4 0.0190(17) 0.032(2) 0.0269(17) 0.0041(15) 0.0006(13) -0.0003(14) N5 0.0239(16) 0.0188(16) 0.0123(14) -0.0004(12) 0.0018(12) -0.0010(13) N6 0.0238(18) 0.041(2) 0.0224(17) 0.0024(16) 0.0028(14) 0.0033(16) N7 0.0238(17) 0.0211(18) 0.0202(16) -0.0019(13) -0.0017(13) -0.0019(14) O1 0.0256(14) 0.0145(13) 0.0215(13) -0.0007(11) 0.0008(11) -0.0026(11) O1S 0.047(2) 0.062(3) 0.049(2) -0.004(2) -0.0042(18) -0.014(2) O2 0.0433(18) 0.0235(16) 0.0215(14) -0.0054(12) 0.0061(12) -0.0139(13) O3 0.058(2) 0.0334(18) 0.0189(14) -0.0039(13) 0.0119(14) -0.0114(16) O2W 0.192(11) 0.065(6) 0.093(7) 0.000 -0.013(7) 0.000 O4 0.067(2) 0.0122(15) 0.0288(16) 0.0019(12) -0.0112(15) -0.0021(15) O5 0.0223(15) 0.0405(19) 0.0287(15) -0.0106(14) 0.0027(12) 0.0000(13) O6 0.0269(16) 0.055(2) 0.0265(15) -0.0200(15) 0.0056(12) -0.0001(15) O7 0.0352(19) 0.043(2) 0.060(2) -0.0289(18) -0.0055(16) 0.0050(16) O8 0.0289(18) 0.080(3) 0.048(2) -0.035(2) -0.0034(15) -0.0051(18) O9 0.0447(19) 0.0359(19) 0.0307(16) -0.0141(14) 0.0204(14) -0.0183(15) O10 0.0409(18) 0.0196(16) 0.0366(17) -0.0091(13) 0.0017(14) -0.0072(13) O11 0.0382(17) 0.0231(16) 0.0247(14) 0.0039(12) 0.0083(12) -0.0046(13) P1 0.0408(6) 0.0139(5) 0.0174(5) 0.0005(4) 0.0015(4) -0.0061(4) P2 0.0226(6) 0.0487(8) 0.0351(6) -0.0228(6) -0.0004(5) 0.0006(5) Cu1 0.0251(3) 0.0151(2) 0.0150(2) -0.00198(17) 0.00051(17) 0.00167(19) Cu2 0.0155(3) 0.0427(5) 0.0233(3) 0.0105(3) -0.0014(3) -0.0005(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 N1 1.344(5) . ? C1 C2 1.384(5) . ? C1S C2S 1.411(15) . ? C2 C3 1.394(5) . ? C2S O1S 1.464(15) . ? C3 C4 1.384(5) . ? C3 C6 1.504(5) . ? C4 C5 1.381(5) . ? C5 N1 1.353(5) . ? C6 C7 1.538(5) . ? C7 C8 1.522(5) . ? C8 C9 1.500(6) . ? C9 C10 1.389(6) . ? C9 C13 1.390(6) . ? C10 C11 1.376(6) . ? C11 N2 1.355(5) . ? C12 N2 1.344(5) . ? C12 C13 1.371(6) . ? C14 N3 1.348(5) . ? C14 C15 1.380(6) . ? C15 C16 1.380(6) . ? C16 C17 1.395(6) . ? C16 C19 1.505(5) . ? C17 C18 1.401(5) . ? C18 N3 1.330(5) . ? C19 C20 1.526(5) . ? C20 C21 1.532(5) . ? C21 C22 1.505(5) . ? C22 C26 1.373(6) . ? C22 C23 1.382(6) . ? C23 C24 1.386(6) . ? C24 N4 1.347(6) . ? C25 N4 1.346(6) . ? C25 C26 1.377(6) . ? C27 N5 1.346(5) . ? C27 C28 1.381(6) . ? C28 C29 1.390(6) . ? C29 C30 1.393(6) . ? C29 C32 1.504(6) . ? C30 C31 1.372(6) . ? C31 N5 1.345(5) . ? C32 C33 1.483(8) . ? C32 C33A 1.762(15) . ? C33 C34 1.524(8) . ? C33A C34A 1.544(16) . ? C35 C39 1.375(10) . ? C35 C36 1.404(12) . ? C35 C34 1.578(8) . ? C35 C34A 1.625(14) . ? C36 C37 1.388(8) . ? C37 N6 1.338(6) . ? C38 N6 1.338(7) . ? C38 C39 1.376(7) . ? C40 C45 1.369(6) . ? C40 C41 1.390(6) . ? C40 O2 1.398(5) . ? C41 C42 1.385(6) . ? C42 C43 1.375(7) . ? C43 C44 1.387(6) . ? C44 C45 1.391(6) . ? C46 C47 1.380(7) . ? C46 C51 1.386(6) . ? C46 O4 1.398(5) . ? C47 C48 1.384(7) . ? C48 C49 1.384(7) . ? C49 C50 1.369(8) . ? C50 C51 1.386(7) . ? C52 C57 1.371(7) . ? C52 C53 1.384(6) . ? C52 O6 1.389(5) . ? C53 C54 1.392(8) . ? C54 C55 1.363(9) . ? C55 C56 1.377(8) . ? C56 C57 1.391(6) . ? C58 C63 1.378(7) . ? C58 C59 1.380(8) . ? C58 O7 1.397(6) . ? C59 C60 1.381(9) . ? C60 C61 1.386(8) . ? C61 C62 1.389(8) . ? C62 C63 1.378(7) . ? N1 Cu1 2.027(3) . ? N2 Cu1 2.035(3) 7_565 ? N3 Cu1 2.031(3) . ? N4 Cu2 2.031(3) . ? N5 Cu1 2.010(3) . ? N6 Cu2 2.033(4) 1_545 ? N7 O9 1.244(4) . ? N7 O10 1.251(4) . ? N7 O11 1.262(4) . ? O1 P1 1.482(3) . ? O1 Cu1 2.217(3) . ? O2 P1 1.602(3) . ? O3 P1 1.476(3) . ? O4 P1 1.620(3) . ? O5 P2 1.478(3) . ? O6 P2 1.619(4) . ? O7 P2 1.616(4) . ? O8 P2 1.476(3) . ? Cu1 N2 2.035(3) 7_565 ? Cu2 N4 2.031(3) 5_676 ? Cu2 N6 2.033(4) 1_565 ? Cu2 N6 2.033(4) 5_666 ? 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 N1 C1 C2 122.4(4) . . ? C1 C2 C3 119.9(3) . . ? C1S C2S O1S 140.3(11) . . ? C4 C3 C2 116.9(3) . . ? C4 C3 C6 122.2(3) . . ? C2 C3 C6 120.7(3) . . ? C5 C4 C3 120.7(4) . . ? N1 C5 C4 121.7(3) . . ? C3 C6 C7 111.6(3) . . ? C8 C7 C6 112.0(3) . . ? C9 C8 C7 113.9(3) . . ? C10 C9 C13 116.5(4) . . ? C10 C9 C8 121.6(4) . . ? C13 C9 C8 122.0(4) . . ? C11 C10 C9 120.5(4) . . ? N2 C11 C10 122.4(4) . . ? N2 C12 C13 123.1(4) . . ? C12 C13 C9 120.4(4) . . ? N3 C14 C15 122.3(4) . . ? C16 C15 C14 120.2(4) . . ? C15 C16 C17 117.3(4) . . ? C15 C16 C19 120.6(4) . . ? C17 C16 C19 122.0(4) . . ? C16 C17 C18 119.7(4) . . ? N3 C18 C17 121.9(4) . . ? C16 C19 C20 110.1(3) . . ? C19 C20 C21 111.6(3) . . ? C22 C21 C20 110.9(3) . . ? C26 C22 C23 117.5(4) . . ? C26 C22 C21 120.1(4) . . ? C23 C22 C21 122.3(4) . . ? C22 C23 C24 119.8(4) . . ? N4 C24 C23 122.4(4) . . ? N4 C25 C26 122.5(4) . . ? C22 C26 C25 120.4(5) . . ? N5 C27 C28 123.2(4) . . ? C27 C28 C29 119.9(4) . . ? C28 C29 C30 116.3(4) . . ? C28 C29 C32 122.8(4) . . ? C30 C29 C32 120.9(4) . . ? C31 C30 C29 121.1(4) . . ? N5 C31 C30 122.3(4) . . ? C33 C32 C29 118.8(5) . . ? C33 C32 C33A 30.9(5) . . ? C29 C32 C33A 99.1(5) . . ? C32 C33 C34 108.3(6) . . ? C34A C33A C32 103.3(9) . . ? C39 C35 C36 115.6(6) . . ? C39 C35 C34 117.1(8) . . ? C36 C35 C34 126.5(7) . . ? C39 C35 C34A 128.5(9) . . ? C36 C35 C34A 101.8(9) . . ? C34 C35 C34A 48.7(6) . . ? C33 C34 C35 110.9(6) . . ? C33A C34A C35 87.9(9) . . ? C37 C36 C35 120.9(6) . . ? N6 C37 C36 121.5(6) . . ? N6 C38 C39 123.2(5) . . ? C35 C39 C38 120.6(7) . . ? C45 C40 C41 121.4(4) . . ? C45 C40 O2 122.5(4) . . ? C41 C40 O2 116.0(4) . . ? C42 C41 C40 119.2(4) . . ? C43 C42 C41 120.0(4) . . ? C42 C43 C44 120.3(4) . . ? C43 C44 C45 120.2(4) . . ? C40 C45 C44 119.0(4) . . ? C47 C46 C51 121.3(4) . . ? C47 C46 O4 117.4(4) . . ? C51 C46 O4 121.1(5) . . ? C46 C47 C48 118.6(4) . . ? C47 C48 C49 121.1(5) . . ? C50 C49 C48 119.2(5) . . ? C49 C50 C51 121.2(4) . . ? C46 C51 C50 118.5(5) . . ? C57 C52 C53 120.8(4) . . ? C57 C52 O6 117.0(4) . . ? C53 C52 O6 122.2(5) . . ? C52 C53 C54 118.1(6) . . ? C55 C54 C53 121.8(5) . . ? C54 C55 C56 119.3(5) . . ? C55 C56 C57 120.2(5) . . ? C52 C57 C56 119.8(4) . . ? C63 C58 C59 120.5(5) . . ? C63 C58 O7 119.9(5) . . ? C59 C58 O7 119.5(5) . . ? C58 C59 C60 119.6(5) . . ? C59 C60 C61 120.5(6) . . ? C60 C61 C62 119.1(5) . . ? C63 C62 C61 120.4(5) . . ? C58 C63 C62 119.8(5) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Cu1 121.9(3) . . ? C5 N1 Cu1 117.8(3) . . ? C12 N2 C11 117.1(3) . . ? C12 N2 Cu1 119.8(3) . 7_565 ? C11 N2 Cu1 123.0(3) . 7_565 ? C18 N3 C14 118.6(3) . . ? C18 N3 Cu1 120.8(3) . . ? C14 N3 Cu1 120.6(3) . . ? C25 N4 C24 117.4(4) . . ? C25 N4 Cu2 122.8(3) . . ? C24 N4 Cu2 119.6(3) . . ? C31 N5 C27 117.3(4) . . ? C31 N5 Cu1 121.2(3) . . ? C27 N5 Cu1 121.5(3) . . ? C38 N6 C37 117.7(4) . . ? C38 N6 Cu2 121.8(3) . 1_545 ? C37 N6 Cu2 119.9(4) . 1_545 ? O9 N7 O10 120.3(3) . . ? O9 N7 O11 119.9(3) . . ? O10 N7 O11 119.8(3) . . ? P1 O1 Cu1 158.13(18) . . ? C40 O2 P1 124.3(3) . . ? C46 O4 P1 120.4(3) . . ? C52 O6 P2 126.9(3) . . ? C58 O7 P2 121.6(3) . . ? O3 P1 O1 120.10(18) . . ? O3 P1 O2 105.85(18) . . ? O1 P1 O2 110.90(16) . . ? O3 P1 O4 110.42(19) . . ? O1 P1 O4 109.02(18) . . ? O2 P1 O4 98.34(17) . . ? O8 P2 O5 121.2(2) . . ? O8 P2 O7 106.2(2) . . ? O5 P2 O7 110.3(2) . . ? O8 P2 O6 112.2(2) . . ? O5 P2 O6 103.17(18) . . ? O7 P2 O6 102.2(2) . . ? N5 Cu1 N1 92.74(12) . . ? N5 Cu1 N3 89.80(13) . . ? N1 Cu1 N3 164.35(13) . . ? N5 Cu1 N2 173.08(13) . 7_565 ? N1 Cu1 N2 88.47(13) . 7_565 ? N3 Cu1 N2 87.24(13) . 7_565 ? N5 Cu1 O1 93.13(12) . . ? N1 Cu1 O1 98.43(11) . . ? N3 Cu1 O1 96.84(12) . . ? N2 Cu1 O1 93.44(12) 7_565 . ? N4 Cu2 N4 180.00(5) 5_676 . ? N4 Cu2 N6 93.61(14) 5_676 1_565 ? N4 Cu2 N6 86.39(14) . 1_565 ? N4 Cu2 N6 86.39(14) 5_676 5_666 ? N4 Cu2 N6 93.60(14) . 5_666 ? N6 Cu2 N6 180.000(2) 1_565 5_666 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.257 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.116 data_complex3 _database_code_depnum_ccdc_archive 'CCDC 898352' #TrackingRef 'web_deposit_cif_file_2_DebajyotiGhoshal_1350570455.898352.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H34 Cl0 Mn N2 O8 P2' _chemical_formula_weight 751.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 5.52360(10) _cell_length_b 23.2071(5) _cell_length_c 27.1572(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3481.19(12) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8795 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60169 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7981 _reflns_number_gt 7017 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Restraints are DELU o6 P2, C24 N2, C21 C22, C39 C40. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.5889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.009(13) _refine_ls_number_reflns 7981 _refine_ls_number_parameters 533 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0085(5) 0.34221(10) 0.89080(9) 0.0460(5) Uani 1 1 d . . . C2 C -0.1948(5) 0.33092(10) 0.86312(10) 0.0538(6) Uani 1 1 d . . . H2 H -0.2271 0.3520 0.8347 0.065 Uiso 1 1 calc R . . C3 C -0.3503(6) 0.28759(11) 0.87833(11) 0.0648(8) Uani 1 1 d . . . H3 H -0.4886 0.2797 0.8600 0.078 Uiso 1 1 calc R . . C4 C -0.3035(7) 0.25616(13) 0.92000(12) 0.0711(9) Uani 1 1 d . . . H4 H -0.4085 0.2269 0.9297 0.085 Uiso 1 1 calc R . . C5 C -0.1019(7) 0.26802(14) 0.94714(12) 0.0745(10) Uani 1 1 d . . . H5 H -0.0710 0.2471 0.9757 0.089 Uiso 1 1 calc R . . C6 C 0.0572(6) 0.31093(13) 0.93271(10) 0.0623(7) Uani 1 1 d . . . H6 H 0.1956 0.3185 0.9511 0.075 Uiso 1 1 calc R . . C7 C 0.2274(4) 0.41177(10) 0.74236(9) 0.0438(5) Uani 1 1 d . . . C8 C 0.0562(6) 0.39943(13) 0.70714(12) 0.0650(8) Uani 1 1 d . . . H8 H -0.0805 0.3779 0.7150 0.078 Uiso 1 1 calc R . . C9 C 0.0919(7) 0.41987(15) 0.65949(13) 0.0791(10) Uani 1 1 d . . . H9 H -0.0217 0.4115 0.6352 0.095 Uiso 1 1 calc R . . C10 C 0.2897(7) 0.45180(14) 0.64782(11) 0.0727(9) Uani 1 1 d . . . H10 H 0.3105 0.4653 0.6159 0.087 Uiso 1 1 calc R . . C11 C 0.4590(6) 0.46406(14) 0.68334(10) 0.0674(8) Uani 1 1 d . . . H11 H 0.5936 0.4863 0.6755 0.081 Uiso 1 1 calc R . . C12 C 0.4304(5) 0.44343(12) 0.73084(10) 0.0538(6) Uani 1 1 d . . . H12 H 0.5471 0.4509 0.7547 0.065 Uiso 1 1 calc R . . C13 C -0.0735(4) 0.55585(10) 0.75567(9) 0.0453(6) Uani 1 1 d . . . H13 H 0.0408 0.5301 0.7679 0.054 Uiso 1 1 calc R . . C14 C -0.0249(5) 0.58322(11) 0.71195(9) 0.0484(6) Uani 1 1 d . . . H14 H 0.1178 0.5752 0.6951 0.058 Uiso 1 1 calc R . . C15 C -0.1857(6) 0.62237(9) 0.69294(8) 0.0464(5) Uani 1 1 d . A . C16 C -0.3967(5) 0.63089(11) 0.71952(9) 0.0549(7) Uani 1 1 d . . . H16 H -0.5137 0.6565 0.7082 0.066 Uiso 1 1 calc R . . C17 C -0.4323(5) 0.60146(11) 0.76266(9) 0.0483(6) Uani 1 1 d . . . H17 H -0.5754 0.6081 0.7798 0.058 Uiso 1 1 calc R . . C18 C -0.1330(8) 0.65628(12) 0.64614(10) 0.0716(9) Uani 1 1 d . . . H18A H -0.2330 0.6867 0.6430 0.086 Uiso 1 1 d R A . H18B H 0.0558 0.6617 0.6476 0.086 Uiso 1 1 d R . . C19 C -0.2255(14) 0.6278(3) 0.5989(2) 0.0528(17) Uani 0.50 1 d P A 1 H19A H -0.2198 0.6549 0.5718 0.063 Uiso 0.50 1 calc PR A 1 H19B H -0.3918 0.6153 0.6032 0.063 Uiso 0.50 1 calc PR A 1 C20 C -0.0594(15) 0.5748(4) 0.58770(19) 0.0551(15) Uani 0.50 1 d P A 1 H20A H 0.1097 0.5861 0.5885 0.066 Uiso 0.50 1 calc PR A 1 H20B H -0.0849 0.5447 0.6119 0.066 Uiso 0.50 1 calc PR A 1 C19A C -0.066(3) 0.6178(5) 0.6006(3) 0.099(3) Uani 0.50 1 d P A 2 H19C H -0.0317 0.6430 0.5730 0.119 Uiso 0.50 1 calc PR A 2 H19D H 0.0815 0.5970 0.6082 0.119 Uiso 0.50 1 calc PR A 2 C20A C -0.234(3) 0.5798(6) 0.5867(3) 0.117(4) Uani 0.50 1 d P A 2 H20C H -0.3887 0.5986 0.5814 0.140 Uiso 0.50 1 calc PR A 2 H20D H -0.2540 0.5499 0.6113 0.140 Uiso 0.50 1 calc PR A 2 C21 C -0.1297(11) 0.55296(16) 0.53542(12) 0.0989(15) Uani 1 1 d U . . C22 C -0.1654(14) 0.4992(2) 0.52802(16) 0.0591(14) Uani 0.50 1 d PU A 1 H22 H -0.1908 0.4743 0.5543 0.071 Uiso 0.50 1 calc PR A 1 C23 C -0.1657(12) 0.4792(2) 0.48057(15) 0.0496(12) Uani 0.50 1 d P A 1 H23 H -0.1787 0.4395 0.4767 0.060 Uiso 0.50 1 calc PR A 1 C24 C -0.1036(10) 0.5689(2) 0.45034(16) 0.0487(12) Uani 0.50 1 d PU A 1 H24 H -0.0754 0.5939 0.4242 0.058 Uiso 0.50 1 calc PR A 1 C25 C -0.0986(16) 0.5911(2) 0.49674(19) 0.075(2) Uani 0.50 1 d P A 1 H25 H -0.0751 0.6302 0.5022 0.089 Uiso 0.50 1 calc PR A 1 C22A C -0.363(3) 0.5429(6) 0.5081(4) 0.152(5) Uani 0.50 1 d P A 2 H22A H -0.5079 0.5530 0.5231 0.183 Uiso 0.50 1 calc PR A 2 C23A C -0.3675(16) 0.5191(3) 0.4612(2) 0.085(2) Uani 0.50 1 d P A 2 H23A H -0.5123 0.5098 0.4456 0.102 Uiso 0.50 1 calc PR A 2 C24A C 0.0469(16) 0.5140(3) 0.4592(2) 0.085(2) Uani 0.50 1 d P A 2 H24A H 0.1868 0.5014 0.4435 0.102 Uiso 0.50 1 calc PR A 2 C25A C 0.057(2) 0.5378(5) 0.5060(3) 0.130(4) Uani 0.50 1 d P A 2 H25A H 0.2112 0.5440 0.5187 0.156 Uiso 0.50 1 calc PR A 2 C30 C 0.0331(5) 0.64462(13) 0.97907(10) 0.0587(8) Uani 1 1 d . . . C31 C -0.1738(5) 0.67198(13) 0.96483(10) 0.0638(8) Uani 1 1 d . . . H31 H -0.2077 0.6775 0.9316 0.077 Uiso 1 1 calc R . . C32 C -0.3325(6) 0.69142(12) 1.00061(10) 0.0586(7) Uani 1 1 d . . . H32 H -0.4742 0.7102 0.9913 0.070 Uiso 1 1 calc R B . C33 C -0.2831(6) 0.68331(14) 1.04931(11) 0.0660(8) Uani 1 1 d . . . H33 H -0.3886 0.6973 1.0732 0.079 Uiso 1 1 calc R . . C34 C -0.0759(6) 0.65435(15) 1.06294(12) 0.0711(9) Uani 1 1 d . . . H34 H -0.0435 0.6479 1.0961 0.085 Uiso 1 1 calc R B . C35 C 0.0831(6) 0.63494(13) 1.02771(11) 0.0648(8) Uani 1 1 d . . . H35 H 0.2231 0.6154 1.0368 0.078 Uiso 1 1 calc R . . C36 C 0.2054(6) 0.70322(11) 0.83398(14) 0.0700(10) Uani 1 1 d . . . C37 C 0.0906(7) 0.71430(14) 0.79026(18) 0.0864(12) Uani 1 1 d . B . H37 H -0.0549 0.6962 0.7826 0.104 Uiso 1 1 calc R . . C38 C 0.1931(11) 0.75204(18) 0.75839(14) 0.0948(13) Uani 1 1 d . . . H38 H 0.1157 0.7597 0.7287 0.114 Uiso 1 1 calc R B . C39 C 0.3961(9) 0.77789(16) 0.76810(16) 0.0889(12) Uani 1 1 d U B . H39 H 0.4626 0.8031 0.7452 0.107 Uiso 1 1 calc R . . C40 C 0.5097(7) 0.76860(14) 0.81048(17) 0.0851(11) Uani 1 1 d U . . H40 H 0.6531 0.7881 0.8172 0.102 Uiso 1 1 calc R B . C41 C 0.4179(7) 0.73037(15) 0.84479(12) 0.0773(10) Uani 1 1 d . B . H41 H 0.4984 0.7234 0.8743 0.093 Uiso 1 1 calc R . . N1 N -0.2762(3) 0.56416(8) 0.78158(7) 0.0381(4) Uani 1 1 d . B . N1A N -0.1493(5) 0.51004(10) 0.43927(7) 0.0542(5) Uani 1 1 d U . . O6 O 0.0604(5) 0.65959(13) 0.85547(11) 0.0337(6) Uani 0.50 1 d PU B 1 O6A O 0.1834(11) 0.67909(16) 0.88723(17) 0.0821(15) Uani 0.50 1 d P B 2 O1 O -0.0800(3) 0.45665(7) 0.83444(6) 0.0396(3) Uani 1 1 d . B . O3 O 0.1971(4) 0.38902(6) 0.78949(6) 0.0489(4) Uani 1 1 d . . . O4 O 0.1788(4) 0.38352(7) 0.87894(6) 0.0531(4) Uani 1 1 d . . . O2 O 0.3767(3) 0.46812(7) 0.84207(6) 0.0458(4) Uani 1 1 d . . . O5 O -0.0250(9) 0.5837(2) 0.87553(19) 0.0528(12) Uani 0.50 1 d P B 1 O5A O -0.0207(8) 0.56456(18) 0.89359(14) 0.0310(8) Uani 0.50 1 d P B 2 O8 O 0.4217(3) 0.59198(7) 0.87358(7) 0.0473(4) Uani 1 1 d . . . O7 O 0.2208(7) 0.63884(16) 0.94031(14) 0.0339(8) Uani 0.50 1 d P B 1 O7A O 0.1934(9) 0.6108(2) 0.95244(15) 0.0530(11) Uani 0.50 1 d P B 2 P1 P 0.16330(10) 0.43101(2) 0.836262(19) 0.03307(12) Uani 1 1 d . . . P2 P 0.18057(11) 0.60982(2) 0.890989(19) 0.03340(12) Uani 1 1 d U . . Mn1 Mn -0.32412(6) 0.524439(13) 0.859755(11) 0.03300(8) 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 0.0472(14) 0.0387(12) 0.0522(13) 0.0046(10) 0.0083(11) 0.0005(10) C2 0.0591(16) 0.0470(13) 0.0553(14) 0.0024(11) 0.0009(14) -0.0126(13) C3 0.0655(19) 0.0536(15) 0.0753(18) -0.0068(14) 0.0092(16) -0.0136(15) C4 0.082(2) 0.0549(16) 0.0770(19) 0.0080(14) 0.028(2) -0.0178(17) C5 0.088(3) 0.0657(19) 0.0701(19) 0.0245(16) 0.0144(18) -0.0036(18) C6 0.0617(18) 0.0649(17) 0.0604(17) 0.0166(14) 0.0009(14) 0.0020(14) C7 0.0384(13) 0.0403(11) 0.0527(14) -0.0148(10) 0.0059(10) 0.0044(9) C8 0.0462(16) 0.0663(18) 0.083(2) -0.0152(15) -0.0045(15) -0.0022(14) C9 0.079(2) 0.091(2) 0.068(2) -0.0154(18) -0.0222(18) 0.014(2) C10 0.082(2) 0.080(2) 0.0559(17) -0.0053(15) 0.0052(17) 0.0161(19) C11 0.069(2) 0.0761(19) 0.0569(17) -0.0083(14) 0.0185(15) -0.0047(16) C12 0.0466(15) 0.0647(17) 0.0501(14) -0.0131(12) 0.0082(11) -0.0078(13) C13 0.0350(12) 0.0488(14) 0.0521(13) 0.0056(11) 0.0076(10) 0.0101(10) C14 0.0433(14) 0.0566(15) 0.0454(13) 0.0001(11) 0.0124(11) 0.0008(11) C15 0.0619(15) 0.0388(11) 0.0385(11) -0.0059(9) -0.0036(12) -0.0005(12) C16 0.0614(18) 0.0551(15) 0.0483(14) -0.0050(12) -0.0114(12) 0.0208(13) C17 0.0373(13) 0.0651(16) 0.0425(12) -0.0085(11) 0.0010(10) 0.0140(11) C18 0.114(3) 0.0566(15) 0.0445(14) 0.0063(12) 0.0049(17) 0.0012(18) C19 0.058(4) 0.053(4) 0.047(3) 0.002(2) -0.007(3) 0.013(3) C20 0.061(4) 0.071(4) 0.033(3) -0.009(3) 0.001(3) 0.026(3) C19A 0.156(11) 0.104(8) 0.037(4) 0.010(4) 0.018(5) -0.014(8) C20A 0.132(10) 0.151(11) 0.069(5) -0.008(6) 0.029(6) -0.050(8) C21 0.175(5) 0.080(2) 0.0419(16) -0.0020(15) 0.002(2) 0.002(3) C22 0.101(5) 0.049(3) 0.028(2) 0.0075(19) 0.001(3) -0.012(3) C23 0.076(3) 0.040(2) 0.032(2) 0.0026(18) -0.005(2) -0.010(3) C24 0.072(4) 0.044(2) 0.029(2) 0.0070(19) 0.007(2) 0.000(2) C25 0.149(7) 0.034(3) 0.040(3) -0.004(2) 0.008(3) -0.009(3) C22A 0.171(12) 0.175(10) 0.110(7) -0.080(7) 0.067(8) -0.012(10) C23A 0.096(6) 0.097(5) 0.062(4) -0.019(4) 0.028(4) 0.000(4) C24A 0.093(6) 0.107(6) 0.054(3) -0.017(4) -0.014(4) 0.024(5) C25A 0.150(10) 0.172(10) 0.067(5) -0.051(6) -0.040(6) 0.035(8) C30 0.0328(13) 0.089(2) 0.0541(14) -0.0422(14) -0.0040(11) 0.0057(13) C31 0.0387(13) 0.099(2) 0.0540(14) -0.0285(14) -0.0024(13) 0.0125(16) C32 0.0381(13) 0.0693(16) 0.0684(16) -0.0223(13) 0.0068(14) 0.0063(14) C33 0.0598(19) 0.0759(19) 0.0623(17) -0.0183(14) 0.0240(15) -0.0010(15) C34 0.075(2) 0.085(2) 0.0534(16) -0.0077(15) 0.0128(15) 0.0017(18) C35 0.0524(17) 0.0763(19) 0.0656(18) -0.0197(15) -0.0044(14) 0.0096(14) C36 0.066(2) 0.0387(13) 0.106(2) 0.0211(15) 0.051(2) 0.0172(14) C37 0.054(2) 0.0570(19) 0.148(4) -0.036(2) -0.008(2) 0.0028(15) C38 0.121(4) 0.093(3) 0.071(2) -0.006(2) -0.015(3) 0.025(3) C39 0.111(4) 0.065(2) 0.091(3) 0.021(2) 0.032(2) 0.014(2) C40 0.056(2) 0.0604(19) 0.139(3) -0.015(2) 0.016(2) -0.0183(16) C41 0.076(2) 0.089(2) 0.0670(19) -0.0002(18) -0.0064(17) 0.028(2) N1 0.0313(10) 0.0419(10) 0.0413(9) -0.0033(8) 0.0018(7) -0.0002(8) N1A 0.0605(14) 0.0650(13) 0.0373(10) 0.0043(9) 0.0041(11) 0.0075(12) O6 0.0189(13) 0.0451(16) 0.0371(15) 0.0112(13) -0.0035(12) -0.0003(12) O6A 0.113(4) 0.049(2) 0.085(3) 0.005(2) 0.055(3) 0.005(3) O1 0.0303(8) 0.0428(8) 0.0455(8) -0.0028(7) 0.0011(7) 0.0031(6) O3 0.0525(10) 0.0364(8) 0.0577(10) -0.0096(7) 0.0140(9) -0.0018(8) O4 0.0419(9) 0.0547(9) 0.0629(10) 0.0191(8) -0.0094(9) -0.0049(9) O2 0.0315(9) 0.0509(9) 0.0548(9) -0.0021(7) 0.0002(7) -0.0096(7) O5 0.035(2) 0.060(3) 0.064(4) -0.017(2) -0.007(2) -0.005(2) O5A 0.0286(16) 0.037(2) 0.0278(19) 0.0024(14) -0.0019(15) -0.0069(15) O8 0.0309(8) 0.0502(9) 0.0609(11) -0.0118(8) 0.0134(7) 0.0010(7) O7 0.0260(16) 0.041(2) 0.0343(19) -0.0048(15) 0.0004(13) -0.0067(15) O7A 0.036(2) 0.088(3) 0.035(2) -0.014(2) -0.0044(18) 0.019(3) P1 0.0249(2) 0.0342(3) 0.0401(3) -0.0006(2) 0.0008(2) -0.0008(2) P2 0.0265(2) 0.0367(3) 0.0370(3) -0.0015(2) 0.0068(2) 0.0002(2) Mn1 0.02185(14) 0.04487(17) 0.03230(15) -0.00655(13) 0.00059(13) -0.00086(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.376(4) . ? C1 C6 1.377(4) . ? C1 O4 1.381(3) . ? C2 C3 1.386(4) . ? C3 C4 1.371(4) . ? C4 C5 1.363(5) . ? C5 C6 1.385(4) . ? C7 C8 1.375(4) . ? C7 C12 1.377(3) . ? C7 O3 1.395(3) . ? C8 C9 1.392(5) . ? C9 C10 1.358(5) . ? C10 C11 1.374(5) . ? C11 C12 1.385(4) . ? C13 N1 1.337(3) . ? C13 C14 1.373(3) . ? C14 C15 1.372(4) . ? C15 C16 1.385(4) . ? C15 C18 1.523(3) . ? C16 C17 1.370(4) . ? C17 N1 1.325(3) . ? C18 C19 1.532(7) . ? C18 C19A 1.568(10) . ? C19 C20 1.564(8) . ? C20 C21 1.557(7) . ? C19A C20A 1.336(14) . ? C20A C21 1.631(11) . ? C21 C22 1.278(6) . ? C21 C25A 1.351(12) . ? C21 C25 1.384(6) . ? C21 C22A 1.503(15) . ? C22 C23 1.370(6) . ? C23 N1A 1.334(5) . ? C24 C25 1.361(7) . ? C24 N1A 1.422(5) . ? C22A C23A 1.389(11) . ? C23A N1A 1.361(8) . ? C24A N1A 1.215(8) . ? C24A C25A 1.386(10) . ? C30 C31 1.363(4) . ? C30 C35 1.368(4) . ? C30 O7A 1.387(5) . ? C30 O7 1.484(5) . ? C31 C32 1.384(4) . ? C32 C33 1.363(4) . ? C33 C34 1.378(5) . ? C34 C35 1.375(4) . ? C36 C41 1.364(5) . ? C36 C37 1.370(5) . ? C36 O6 1.417(4) . ? C36 O6A 1.556(5) . ? C37 C38 1.355(6) . ? C38 C39 1.299(6) . ? C39 C40 1.328(6) . ? C40 C41 1.383(5) . ? N1 Mn1 2.3296(19) . ? N1A Mn1 2.308(2) 2_464 ? O6 P2 1.645(3) . ? O6A P2 1.611(4) . ? O1 P1 1.4705(16) . ? O1 Mn1 2.1832(15) . ? O3 P1 1.6118(16) . ? O4 P1 1.6016(16) . ? O2 P1 1.4682(16) . ? O2 Mn1 2.1611(15) 1_655 ? O5 P2 1.354(5) . ? O5 Mn1 2.192(5) . ? O5A P2 1.531(4) . ? O5A Mn1 2.126(4) . ? O8 P2 1.4729(16) . ? O8 Mn1 2.1374(16) 1_655 ? O7 P2 1.515(4) . ? O7A P2 1.670(4) . ? Mn1 O8 2.1374(16) 1_455 ? Mn1 O2 2.1611(16) 1_455 ? Mn1 N1A 2.308(2) 2_465 ? 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 C2 C1 C6 120.7(2) . . ? C2 C1 O4 124.1(2) . . ? C6 C1 O4 115.2(2) . . ? C1 C2 C3 118.8(3) . . ? C4 C3 C2 121.0(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 120.7(3) . . ? C1 C6 C5 119.3(3) . . ? C8 C7 C12 120.9(3) . . ? C8 C7 O3 118.5(2) . . ? C12 C7 O3 120.6(2) . . ? C7 C8 C9 118.6(3) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 120.3(3) . . ? C7 C12 C11 119.3(3) . . ? N1 C13 C14 123.5(2) . . ? C15 C14 C13 120.4(2) . . ? C14 C15 C16 116.3(2) . . ? C14 C15 C18 122.2(3) . . ? C16 C15 C18 121.5(3) . . ? C17 C16 C15 119.7(2) . . ? N1 C17 C16 124.3(2) . . ? C15 C18 C19 114.3(3) . . ? C15 C18 C19A 114.1(4) . . ? C19 C18 C19A 34.2(4) . . ? C18 C19 C20 107.9(5) . . ? C21 C20 C19 106.7(5) . . ? C20A C19A C18 115.9(12) . . ? C19A C20A C21 104.4(9) . . ? C22 C21 C25A 76.7(6) . . ? C22 C21 C25 121.6(4) . . ? C25A C21 C25 67.9(6) . . ? C22 C21 C22A 68.8(6) . . ? C25A C21 C22A 108.7(5) . . ? C25 C21 C22A 80.3(6) . . ? C22 C21 C20 120.0(4) . . ? C25A C21 C20 115.7(6) . . ? C25 C21 C20 117.0(5) . . ? C22A C21 C20 135.6(6) . . ? C22 C21 C20A 116.9(6) . . ? C25A C21 C20A 150.9(8) . . ? C25 C21 C20A 116.6(6) . . ? C22A C21 C20A 100.3(7) . . ? C20 C21 C20A 35.4(4) . . ? C21 C22 C23 118.6(4) . . ? N1A C23 C22 127.5(4) . . ? C25 C24 N1A 124.2(4) . . ? C24 C25 C21 117.3(4) . . ? C23A C22A C21 122.1(9) . . ? N1A C23A C22A 116.4(9) . . ? N1A C24A C25A 118.4(8) . . ? C21 C25A C24A 127.9(9) . . ? C31 C30 C35 121.3(2) . . ? C31 C30 O7A 130.6(3) . . ? C35 C30 O7A 106.4(3) . . ? C31 C30 O7 115.2(3) . . ? C35 C30 O7 122.0(3) . . ? O7A C30 O7 29.8(2) . . ? C30 C31 C32 118.9(3) . . ? C33 C32 C31 120.6(3) . . ? C32 C33 C34 119.6(3) . . ? C35 C34 C33 120.2(3) . . ? C30 C35 C34 119.3(3) . . ? C41 C36 C37 119.9(3) . . ? C41 C36 O6 136.7(4) . . ? C37 C36 O6 103.3(4) . . ? C41 C36 O6A 91.9(4) . . ? C37 C36 O6A 146.8(4) . . ? O6 C36 O6A 46.8(2) . . ? C38 C37 C36 118.8(4) . . ? C39 C38 C37 122.0(4) . . ? C38 C39 C40 120.6(4) . . ? C39 C40 C41 121.0(4) . . ? C36 C41 C40 117.8(3) . . ? C17 N1 C13 115.8(2) . . ? C17 N1 Mn1 122.54(15) . . ? C13 N1 Mn1 121.18(15) . . ? C24A N1A C23 74.1(5) . . ? C24A N1A C23A 125.7(5) . . ? C23 N1A C23A 69.8(4) . . ? C24A N1A C24 71.0(5) . . ? C23 N1A C24 110.5(3) . . ? C23A N1A C24 85.2(4) . . ? C24A N1A Mn1 120.1(4) . 2_464 ? C23 N1A Mn1 126.6(2) . 2_464 ? C23A N1A Mn1 114.0(4) . 2_464 ? C24 N1A Mn1 122.8(2) . 2_464 ? C36 O6 P2 121.0(2) . . ? C36 O6A P2 114.8(3) . . ? P1 O1 Mn1 147.72(10) . . ? C7 O3 P1 120.54(13) . . ? C1 O4 P1 127.57(17) . . ? P1 O2 Mn1 173.00(11) . 1_655 ? P2 O5 Mn1 166.8(4) . . ? P2 O5A Mn1 148.5(2) . . ? P2 O8 Mn1 148.94(11) . 1_655 ? C30 O7 P2 124.4(3) . . ? C30 O7A P2 120.1(3) . . ? O2 P1 O1 119.98(9) . . ? O2 P1 O4 106.44(10) . . ? O1 P1 O4 110.59(10) . . ? O2 P1 O3 110.27(10) . . ? O1 P1 O3 108.90(10) . . ? O4 P1 O3 98.52(9) . . ? O5 P2 O8 122.2(2) . . ? O5 P2 O7 126.6(3) . . ? O8 P2 O7 106.03(18) . . ? O5 P2 O5A 25.6(2) . . ? O8 P2 O5A 118.60(19) . . ? O7 P2 O5A 111.7(2) . . ? O5 P2 O6A 115.8(3) . . ? O8 P2 O6A 104.6(2) . . ? O7 P2 O6A 67.1(2) . . ? O5A P2 O6A 134.0(3) . . ? O5 P2 O6 78.1(2) . . ? O8 P2 O6 111.97(13) . . ? O7 P2 O6 105.39(19) . . ? O5A P2 O6 102.46(18) . . ? O6A P2 O6 42.8(2) . . ? O5 P2 O7A 110.6(3) . . ? O8 P2 O7A 106.63(18) . . ? O7 P2 O7A 26.48(16) . . ? O5A P2 O7A 89.7(2) . . ? O6A P2 O7A 92.8(3) . . ? O6 P2 O7A 126.4(2) . . ? O5A Mn1 O8 96.93(13) . 1_455 ? O5A Mn1 O2 164.53(10) . 1_455 ? O8 Mn1 O2 88.86(7) 1_455 1_455 ? O5A Mn1 O1 87.99(14) . . ? O8 Mn1 O1 171.67(7) 1_455 . ? O2 Mn1 O1 88.09(6) 1_455 . ? O5A Mn1 O5 17.55(12) . . ? O8 Mn1 O5 90.04(15) 1_455 . ? O2 Mn1 O5 177.90(15) 1_455 . ? O1 Mn1 O5 92.75(15) . . ? O5A Mn1 N1A 78.32(11) . 2_465 ? O8 Mn1 N1A 92.75(8) 1_455 2_465 ? O2 Mn1 N1A 87.11(8) 1_455 2_465 ? O1 Mn1 N1A 94.83(7) . 2_465 ? O5 Mn1 N1A 94.74(15) . 2_465 ? O5A Mn1 N1 97.53(10) . . ? O8 Mn1 N1 86.82(7) 1_455 . ? O2 Mn1 N1 97.11(6) 1_455 . ? O1 Mn1 N1 85.87(6) . . ? O5 Mn1 N1 81.04(14) . . ? N1A Mn1 N1 175.75(8) 2_465 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.252 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.058 data_complex4 _database_code_depnum_ccdc_archive 'CCDC 898353' #TrackingRef 'web_deposit_cif_file_3_DebajyotiGhoshal_1346073361.complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Mn N2 O8 P2' _chemical_formula_weight 737.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5538(2) _cell_length_b 13.6180(3) _cell_length_c 13.8223(3) _cell_angle_alpha 60.9880(10) _cell_angle_beta 87.7220(10) _cell_angle_gamma 79.3440(10) _cell_volume 1704.44(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29056 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8271 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29056 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.55 _reflns_number_total 7827 _reflns_number_gt 6871 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.8744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7827 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6201(2) 1.22136(19) 0.32789(18) 0.0474(5) Uani 1 1 d . . . H1 H 0.5452 1.2001 0.3634 0.057 Uiso 1 1 calc R . . C2 C 0.6086(2) 1.3225(2) 0.2301(2) 0.0553(6) Uani 1 1 d . . . H2 H 0.5276 1.3684 0.2020 0.066 Uiso 1 1 calc R . . C3 C 0.7170(2) 1.35628(19) 0.17358(19) 0.0518(6) Uani 1 1 d . . . C4 C 0.8341(2) 1.28304(19) 0.22106(19) 0.0513(6) Uani 1 1 d . . . H4 H 0.9100 1.3010 0.1858 0.062 Uiso 1 1 calc R . . C5 C 0.8380(2) 1.18349(17) 0.32053(17) 0.0402(4) Uani 1 1 d . . . H5 H 0.9177 1.1363 0.3512 0.048 Uiso 1 1 calc R . . C6 C 0.7053(3) 0.4679(3) 1.0657(3) 0.0818(11) Uani 1 1 d . . . H6A H 0.6492 0.4651 1.0135 0.098 Uiso 1 1 calc R . . H6B H 0.6633 0.5293 1.0793 0.098 Uiso 1 1 calc R . . C7 C 0.8267(3) 0.4967(2) 1.0132(2) 0.0660(8) Uani 1 1 d . . . H7A H 0.8689 0.4364 0.9981 0.079 Uiso 1 1 calc R . . H7B H 0.8835 0.5001 1.0646 0.079 Uiso 1 1 calc R . . C8 C 0.8075(2) 0.60944(19) 0.90639(18) 0.0496(5) Uani 1 1 d . . . C9 C 0.7786(3) 0.61644(19) 0.8069(2) 0.0551(6) Uani 1 1 d . . . H9 H 0.7698 0.5510 0.8044 0.066 Uiso 1 1 calc R . . C10 C 0.7627(2) 0.72078(18) 0.71050(19) 0.0477(5) Uani 1 1 d . . . H10 H 0.7425 0.7235 0.6443 0.057 Uiso 1 1 calc R . . C11 C 0.8027(2) 0.81080(19) 0.80384(18) 0.0486(5) Uani 1 1 d . . . H11 H 0.8117 0.8774 0.8040 0.058 Uiso 1 1 calc R . . C12 C 0.8189(3) 0.7095(2) 0.90396(19) 0.0582(6) Uani 1 1 d . . . H12 H 0.8374 0.7094 0.9693 0.070 Uiso 1 1 calc R . . C13 C 0.96431(19) 1.33568(16) 0.46096(17) 0.0361(4) Uani 1 1 d . . . C14 C 0.8898(2) 1.42507(19) 0.3717(2) 0.0507(5) Uani 1 1 d . . . H14 H 0.8090 1.4185 0.3536 0.061 Uiso 1 1 calc R . . C15 C 0.9366(3) 1.5256(2) 0.3088(2) 0.0608(6) Uani 1 1 d . . . H15 H 0.8873 1.5863 0.2479 0.073 Uiso 1 1 calc R . . C16 C 1.0555(3) 1.5355(2) 0.3365(2) 0.0607(7) Uani 1 1 d . . . H16 H 1.0861 1.6031 0.2949 0.073 Uiso 1 1 calc R . . C17 C 1.1288(3) 1.4453(2) 0.4256(2) 0.0591(6) Uani 1 1 d . . . H17 H 1.2095 1.4519 0.4438 0.071 Uiso 1 1 calc R . . C18 C 1.0837(2) 1.34436(19) 0.4889(2) 0.0478(5) Uani 1 1 d . . . H18 H 1.1336 1.2834 0.5493 0.057 Uiso 1 1 calc R . . C19 C 1.0069(2) 1.11787(18) 0.76824(17) 0.0411(4) Uani 1 1 d . . . C20 C 1.0938(3) 1.1293(2) 0.8323(2) 0.0599(6) Uani 1 1 d . . . H20 H 1.1814 1.1215 0.8198 0.072 Uiso 1 1 calc R . . C21 C 1.0484(4) 1.1528(3) 0.9158(3) 0.0811(10) Uani 1 1 d . . . H21 H 1.1063 1.1604 0.9597 0.097 Uiso 1 1 calc R . . C22 C 0.9199(4) 1.1649(3) 0.9348(3) 0.0838(10) Uani 1 1 d . . . H22 H 0.8907 1.1802 0.9914 0.101 Uiso 1 1 calc R . . C23 C 0.8346(3) 1.1545(3) 0.8698(3) 0.0743(8) Uani 1 1 d . . . H23 H 0.7469 1.1642 0.8817 0.089 Uiso 1 1 calc R . . C24 C 0.8770(3) 1.1295(2) 0.7864(2) 0.0563(6) Uani 1 1 d . . . H24 H 0.8188 1.1208 0.7436 0.068 Uiso 1 1 calc R . . C25 C 0.5316(2) 0.71391(18) 0.4053(2) 0.0438(5) Uani 1 1 d . . . C26 C 0.4061(2) 0.7001(2) 0.4250(2) 0.0540(6) Uani 1 1 d . . . H26 H 0.3555 0.7334 0.4619 0.065 Uiso 1 1 calc R . . C27 C 0.3563(3) 0.6357(2) 0.3891(3) 0.0633(7) Uani 1 1 d . . . H27 H 0.2713 0.6255 0.4021 0.076 Uiso 1 1 calc R . . C28 C 0.4306(3) 0.5868(2) 0.3345(3) 0.0622(7) Uani 1 1 d . . . H28 H 0.3963 0.5431 0.3112 0.075 Uiso 1 1 calc R . . C29 C 0.5556(3) 0.6022(2) 0.3144(2) 0.0581(6) Uani 1 1 d . . . H29 H 0.6058 0.5693 0.2770 0.070 Uiso 1 1 calc R . . C30 C 0.6075(2) 0.6666(2) 0.3496(2) 0.0522(6) Uani 1 1 d . . . H30 H 0.6921 0.6777 0.3357 0.063 Uiso 1 1 calc R . . C31 C 0.5467(3) 1.0303(3) 0.1880(2) 0.0578(6) Uani 1 1 d . . . C32 C 0.4480(3) 1.0002(3) 0.1520(2) 0.0721(8) Uani 1 1 d . . . H32 H 0.4187 0.9335 0.2001 0.086 Uiso 1 1 calc R . . C33 C 0.3926(4) 1.0664(4) 0.0473(3) 0.1007(13) Uani 1 1 d . . . H33 H 0.3281 1.0441 0.0228 0.121 Uiso 1 1 calc R . . C34 C 0.4335(6) 1.1653(4) -0.0205(4) 0.1183(18) Uani 1 1 d . . . H34 H 0.3948 1.2107 -0.0916 0.142 Uiso 1 1 calc R . . C35 C 0.5278(6) 1.2011(4) 0.0107(4) 0.1168(18) Uani 1 1 d . . . H35 H 0.5517 1.2707 -0.0371 0.140 Uiso 1 1 calc R . . C36 C 0.5907(5) 1.1281(4) 0.1205(3) 0.1016(14) Uani 1 1 d . . . H36 H 0.6588 1.1475 0.1439 0.122 Uiso 1 1 calc R . . N1 N 0.73268(15) 1.15184(13) 0.37466(13) 0.0348(3) Uani 1 1 d . . . N2 N 0.77507(15) 0.81723(13) 0.70812(13) 0.0342(3) Uani 1 1 d . . . P1 P 0.98491(4) 1.11026(4) 0.58053(4) 0.02745(11) Uani 1 1 d . . . P2 P 0.54831(4) 0.90454(4) 0.40681(4) 0.03061(11) Uani 1 1 d . . . Mn1 Mn 0.75161(2) 0.98491(2) 0.54290(2) 0.02366(8) Uani 1 1 d . . . O1 O 0.88232(12) 1.04086(11) 0.61439(11) 0.0334(3) Uani 1 1 d . . . O2 O 1.08644(12) 1.09495(12) 0.51031(12) 0.0357(3) Uani 1 1 d . . . O3 O 0.90863(12) 1.24028(11) 0.52264(12) 0.0376(3) Uani 1 1 d . . . O4 O 1.06005(13) 1.09345(13) 0.68756(12) 0.0397(3) Uani 1 1 d . . . O5 O 0.62463(13) 0.91956(13) 0.48356(13) 0.0411(3) Uani 1 1 d . . . O6 O 0.40618(12) 0.94053(11) 0.39463(11) 0.0324(3) Uani 1 1 d . . . O7 O 0.58748(15) 0.76911(15) 0.44998(17) 0.0592(5) Uani 1 1 d . . . O8 O 0.60899(17) 0.9551(2) 0.29020(15) 0.0858(8) 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 0.0381(10) 0.0429(12) 0.0366(11) -0.0006(9) 0.0083(8) -0.0082(9) C2 0.0368(11) 0.0469(13) 0.0436(12) 0.0054(10) 0.0030(9) -0.0008(9) C3 0.0438(11) 0.0369(11) 0.0392(11) 0.0086(9) 0.0043(9) -0.0071(9) C4 0.0373(11) 0.0412(12) 0.0421(12) 0.0061(9) 0.0079(9) -0.0104(9) C5 0.0370(10) 0.0315(10) 0.0347(10) -0.0023(8) 0.0014(8) -0.0073(8) C6 0.0529(15) 0.0566(17) 0.0599(17) 0.0275(13) 0.0095(12) -0.0034(12) C7 0.0644(16) 0.0448(14) 0.0445(13) 0.0121(11) 0.0049(11) -0.0095(12) C8 0.0482(12) 0.0357(11) 0.0360(11) 0.0045(9) 0.0075(9) -0.0081(9) C9 0.0762(17) 0.0254(10) 0.0486(13) -0.0050(10) 0.0074(12) -0.0145(10) C10 0.0673(14) 0.0300(10) 0.0369(11) -0.0083(9) 0.0036(10) -0.0125(10) C11 0.0714(15) 0.0338(11) 0.0326(10) -0.0089(9) 0.0040(10) -0.0137(10) C12 0.0842(18) 0.0471(13) 0.0282(11) -0.0051(10) 0.0028(11) -0.0170(12) C13 0.0359(9) 0.0267(9) 0.0476(11) -0.0188(9) 0.0079(8) -0.0088(7) C14 0.0451(12) 0.0360(11) 0.0613(15) -0.0167(11) -0.0034(10) -0.0049(9) C15 0.0704(17) 0.0331(12) 0.0618(16) -0.0110(11) -0.0001(13) -0.0056(11) C16 0.0754(17) 0.0346(12) 0.0711(17) -0.0210(12) 0.0172(14) -0.0247(12) C17 0.0554(14) 0.0481(14) 0.0760(18) -0.0261(13) 0.0067(13) -0.0274(11) C18 0.0434(11) 0.0372(11) 0.0595(14) -0.0181(10) -0.0001(10) -0.0155(9) C19 0.0507(12) 0.0380(11) 0.0366(10) -0.0181(9) 0.0009(9) -0.0129(9) C20 0.0671(16) 0.0609(16) 0.0570(15) -0.0318(13) -0.0132(12) -0.0115(13) C21 0.114(3) 0.079(2) 0.0642(19) -0.0465(18) -0.0202(18) -0.0110(19) C22 0.132(3) 0.076(2) 0.0526(17) -0.0414(17) 0.0082(18) -0.012(2) C23 0.084(2) 0.086(2) 0.0648(18) -0.0456(17) 0.0264(16) -0.0208(17) C24 0.0556(14) 0.0708(17) 0.0542(14) -0.0376(13) 0.0138(11) -0.0193(12) C25 0.0390(10) 0.0329(10) 0.0613(14) -0.0250(10) -0.0094(9) -0.0018(8) C26 0.0478(12) 0.0505(14) 0.0750(17) -0.0382(13) 0.0085(11) -0.0136(10) C27 0.0535(14) 0.0566(15) 0.095(2) -0.0435(16) 0.0117(14) -0.0262(12) C28 0.0684(16) 0.0511(15) 0.0809(19) -0.0395(14) -0.0030(14) -0.0194(12) C29 0.0681(16) 0.0513(14) 0.0618(16) -0.0352(13) 0.0009(12) -0.0037(12) C30 0.0412(11) 0.0494(13) 0.0690(16) -0.0320(12) 0.0005(10) -0.0054(10) C31 0.0582(14) 0.0743(17) 0.0367(12) -0.0244(12) 0.0167(10) -0.0134(13) C32 0.0650(17) 0.094(2) 0.0479(15) -0.0297(16) -0.0019(12) -0.0071(16) C33 0.101(3) 0.123(3) 0.058(2) -0.036(2) -0.0117(19) 0.006(2) C34 0.146(5) 0.090(3) 0.063(2) -0.008(2) 0.015(3) 0.020(3) C35 0.170(5) 0.073(3) 0.085(3) -0.025(2) 0.066(3) -0.022(3) C36 0.141(4) 0.096(3) 0.089(3) -0.054(2) 0.065(3) -0.056(3) N1 0.0374(8) 0.0286(8) 0.0266(8) -0.0032(6) 0.0023(6) -0.0092(6) N2 0.0366(8) 0.0252(7) 0.0294(8) -0.0045(6) 0.0051(6) -0.0062(6) P1 0.0222(2) 0.0271(2) 0.0341(2) -0.01473(19) 0.00294(16) -0.00788(16) P2 0.0226(2) 0.0374(3) 0.0336(2) -0.0177(2) 0.00321(17) -0.00874(17) Mn1 0.02172(13) 0.02038(13) 0.02272(14) -0.00464(10) 0.00184(9) -0.00731(9) O1 0.0296(6) 0.0352(7) 0.0379(7) -0.0169(6) 0.0051(5) -0.0151(5) O2 0.0303(6) 0.0344(7) 0.0428(8) -0.0190(6) 0.0082(5) -0.0074(5) O3 0.0259(6) 0.0288(7) 0.0538(8) -0.0165(6) 0.0060(6) -0.0069(5) O4 0.0305(7) 0.0512(9) 0.0433(8) -0.0266(7) -0.0013(6) -0.0096(6) O5 0.0332(7) 0.0469(8) 0.0494(8) -0.0262(7) -0.0019(6) -0.0128(6) O6 0.0253(6) 0.0368(7) 0.0365(7) -0.0189(6) 0.0023(5) -0.0065(5) O7 0.0416(8) 0.0504(10) 0.0956(14) -0.0460(10) -0.0225(9) 0.0050(7) O8 0.0368(9) 0.153(2) 0.0388(9) -0.0232(12) 0.0130(7) -0.0239(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 N1 1.333(3) . ? C1 C2 1.373(3) . ? C2 C3 1.380(3) . ? C3 C4 1.388(3) . ? C3 C6 1.515(3) 1_564 ? C4 C5 1.380(3) . ? C5 N1 1.334(2) . ? C6 C7 1.469(4) . ? C6 C3 1.515(3) 1_546 ? C7 C8 1.513(3) . ? C8 C9 1.374(4) . ? C8 C12 1.374(4) . ? C9 C10 1.384(3) . ? C10 N2 1.328(3) . ? C11 N2 1.324(3) . ? C11 C12 1.388(3) . ? C13 C18 1.374(3) . ? C13 C14 1.374(3) . ? C13 O3 1.389(2) . ? C14 C15 1.391(3) . ? C15 C16 1.374(4) . ? C16 C17 1.372(4) . ? C17 C18 1.387(3) . ? C19 C24 1.378(3) . ? C19 C20 1.379(3) . ? C19 O4 1.382(2) . ? C20 C21 1.386(4) . ? C21 C22 1.366(5) . ? C22 C23 1.369(5) . ? C23 C24 1.388(4) . ? C25 C26 1.371(3) . ? C25 C30 1.374(3) . ? C25 O7 1.392(2) . ? C26 C27 1.380(3) . ? C27 C28 1.369(4) . ? C28 C29 1.371(4) . ? C29 C30 1.385(3) . ? C31 C36 1.359(4) . ? C31 O8 1.377(3) . ? C31 C32 1.378(4) . ? C32 C33 1.363(4) . ? C33 C34 1.355(7) . ? C34 C35 1.353(7) . ? C35 C36 1.451(7) . ? N1 Mn1 2.3144(15) . ? N2 Mn1 2.2953(15) . ? P1 O2 1.4713(13) . ? P1 O1 1.4811(12) . ? P1 O4 1.6024(14) . ? P1 O3 1.6041(14) . ? P2 O5 1.4682(14) . ? P2 O6 1.4787(13) . ? P2 O8 1.5769(17) . ? P2 O7 1.6120(17) . ? Mn1 O5 2.1206(13) . ? Mn1 O2 2.1526(13) 2_776 ? Mn1 O6 2.1588(12) 2_676 ? Mn1 O1 2.1650(13) . ? O2 Mn1 2.1526(13) 2_776 ? O6 Mn1 2.1588(12) 2_676 ? 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 N1 C1 C2 123.59(19) . . ? C1 C2 C3 120.1(2) . . ? C2 C3 C4 116.40(19) . . ? C2 C3 C6 120.5(2) . 1_564 ? C4 C3 C6 123.1(2) . 1_564 ? C5 C4 C3 120.06(19) . . ? N1 C5 C4 123.04(19) . . ? C7 C6 C3 116.1(2) . 1_546 ? C6 C7 C8 113.1(2) . . ? C9 C8 C12 116.8(2) . . ? C9 C8 C7 121.5(2) . . ? C12 C8 C7 121.7(2) . . ? C8 C9 C10 120.0(2) . . ? N2 C10 C9 123.1(2) . . ? N2 C11 C12 123.2(2) . . ? C8 C12 C11 119.9(2) . . ? C18 C13 C14 121.0(2) . . ? C18 C13 O3 123.07(19) . . ? C14 C13 O3 115.82(18) . . ? C13 C14 C15 119.2(2) . . ? C16 C15 C14 120.3(2) . . ? C17 C16 C15 119.8(2) . . ? C16 C17 C18 120.6(2) . . ? C13 C18 C17 119.1(2) . . ? C24 C19 C20 120.8(2) . . ? C24 C19 O4 123.85(19) . . ? C20 C19 O4 115.3(2) . . ? C19 C20 C21 118.9(3) . . ? C22 C21 C20 121.1(3) . . ? C21 C22 C23 119.4(3) . . ? C22 C23 C24 121.0(3) . . ? C19 C24 C23 118.7(3) . . ? C26 C25 C30 121.5(2) . . ? C26 C25 O7 119.6(2) . . ? C30 C25 O7 118.7(2) . . ? C25 C26 C27 118.7(2) . . ? C28 C27 C26 120.7(2) . . ? C27 C28 C29 120.0(2) . . ? C28 C29 C30 120.3(2) . . ? C25 C30 C29 118.8(2) . . ? C36 C31 O8 119.6(3) . . ? C36 C31 C32 120.9(3) . . ? O8 C31 C32 119.2(3) . . ? C33 C32 C31 121.2(4) . . ? C34 C33 C32 118.7(5) . . ? C35 C34 C33 123.0(4) . . ? C34 C35 C36 118.2(4) . . ? C31 C36 C35 117.8(4) . . ? C1 N1 C5 116.77(17) . . ? C1 N1 Mn1 123.27(13) . . ? C5 N1 Mn1 119.96(13) . . ? C11 N2 C10 117.02(18) . . ? C11 N2 Mn1 122.75(14) . . ? C10 N2 Mn1 120.22(14) . . ? O2 P1 O1 120.43(8) . . ? O2 P1 O4 105.34(8) . . ? O1 P1 O4 110.26(8) . . ? O2 P1 O3 110.56(8) . . ? O1 P1 O3 104.68(7) . . ? O4 P1 O3 104.58(8) . . ? O5 P2 O6 120.55(8) . . ? O5 P2 O8 109.07(11) . . ? O6 P2 O8 110.91(9) . . ? O5 P2 O7 102.78(9) . . ? O6 P2 O7 110.16(8) . . ? O8 P2 O7 101.42(13) . . ? O5 Mn1 O2 89.97(5) . 2_776 ? O5 Mn1 O6 91.58(5) . 2_676 ? O2 Mn1 O6 176.88(5) 2_776 2_676 ? O5 Mn1 O1 176.03(5) . . ? O2 Mn1 O1 90.00(5) 2_776 . ? O6 Mn1 O1 88.26(5) 2_676 . ? O5 Mn1 N2 88.29(6) . . ? O2 Mn1 N2 87.52(5) 2_776 . ? O6 Mn1 N2 89.81(5) 2_676 . ? O1 Mn1 N2 87.75(6) . . ? O5 Mn1 N1 91.74(6) . . ? O2 Mn1 N1 90.93(6) 2_776 . ? O6 Mn1 N1 91.73(5) 2_676 . ? O1 Mn1 N1 92.23(5) . . ? N2 Mn1 N1 178.46(6) . . ? P1 O1 Mn1 139.59(8) . . ? P1 O2 Mn1 160.19(9) . 2_776 ? C13 O3 P1 125.10(12) . . ? C19 O4 P1 126.55(13) . . ? P2 O5 Mn1 160.61(10) . . ? P2 O6 Mn1 141.54(8) . 2_676 ? C25 O7 P2 123.20(14) . . ? C31 O8 P2 127.83(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.879 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.072 data_complex5 _database_code_depnum_ccdc_archive 'CCDC 898354' #TrackingRef 'web_deposit_cif_file_3_DebajyotiGhoshal_1350570455.898354.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H50 Co N4 O9 P2' _chemical_formula_weight 971.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' _cell_length_a 13.6529(6) _cell_length_b 18.4192(6) _cell_length_c 19.7519(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.075(2) _cell_angle_gamma 90.00 _cell_volume 4694.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8271 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38230 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0112 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.58 _reflns_number_total 5404 _reflns_number_gt 4977 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+2.9147P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5404 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.33992(11) 0.09459(7) 0.48659(7) 0.0381(3) Uani 1 1 d . . . C2 C -0.43589(12) 0.07079(9) 0.44380(9) 0.0493(3) Uani 1 1 d . . . H2 H -0.4656 0.0299 0.4566 0.059 Uiso 1 1 calc R . . C3 C -0.48754(14) 0.10797(11) 0.38187(10) 0.0608(4) Uani 1 1 d . . . H3 H -0.5525 0.0922 0.3531 0.073 Uiso 1 1 calc R . . C4 C -0.44357(16) 0.16814(11) 0.36241(10) 0.0644(5) Uani 1 1 d . . . H4 H -0.4785 0.1931 0.3205 0.077 Uiso 1 1 calc R . . C5 C -0.34755(16) 0.19128(9) 0.40524(10) 0.0590(4) Uani 1 1 d . . . H5 H -0.3174 0.2317 0.3918 0.071 Uiso 1 1 calc R . . C6 C -0.29510(13) 0.15521(8) 0.46817(9) 0.0471(3) Uani 1 1 d . . . H6 H -0.2308 0.1716 0.4975 0.057 Uiso 1 1 calc R . . C7 C -0.21328(11) -0.07633(8) 0.63934(9) 0.0443(3) Uani 1 1 d . . . C8 C -0.21416(15) -0.11228(10) 0.70035(11) 0.0629(5) Uani 1 1 d . . . H8 H -0.1915 -0.0893 0.7447 0.075 Uiso 1 1 calc R . . C9 C -0.2494(2) -0.18326(13) 0.69423(16) 0.0905(8) Uani 1 1 d . . . H9 H -0.2511 -0.2081 0.7348 0.109 Uiso 1 1 calc R . . C10 C -0.2818(2) -0.21720(12) 0.62904(18) 0.0955(9) Uani 1 1 d . . . H10 H -0.3044 -0.2651 0.6255 0.115 Uiso 1 1 calc R . . C11 C -0.28094(16) -0.18050(11) 0.56909(14) 0.0772(6) Uani 1 1 d . . . H11 H -0.3037 -0.2036 0.5248 0.093 Uiso 1 1 calc R . . C12 C -0.24641(13) -0.10922(9) 0.57359(10) 0.0556(4) Uani 1 1 d . . . H12 H -0.2458 -0.0843 0.5328 0.067 Uiso 1 1 calc R . . C14 C -0.01939(11) 0.16756(7) 0.49659(7) 0.0391(3) Uani 1 1 d . . . H14 H -0.0244 0.1600 0.5419 0.047 Uiso 1 1 calc R . . C15 C -0.02062(11) 0.23805(7) 0.47296(8) 0.0403(3) Uani 1 1 d . . . H15 H -0.0262 0.2765 0.5020 0.048 Uiso 1 1 calc R . . C16 C -0.01352(10) 0.25140(7) 0.40576(7) 0.0378(3) Uani 1 1 d . . . C17 C -0.00712(13) 0.19127(8) 0.36536(8) 0.0454(3) Uani 1 1 d . . . H17 H -0.0032 0.1974 0.3196 0.054 Uiso 1 1 calc R . . C18 C -0.00658(12) 0.12259(8) 0.39270(7) 0.0406(3) Uani 1 1 d . . . H18 H -0.0026 0.0832 0.3642 0.049 Uiso 1 1 calc R . . C19 C -0.01514(12) 0.32796(8) 0.37825(8) 0.0458(3) Uani 1 1 d . . . H19A H 0.0444 0.3352 0.3625 0.055 Uiso 1 1 calc R . . H19B H -0.0097 0.3618 0.4169 0.055 Uiso 1 1 calc R . . C20 C -0.11375(12) 0.34392(8) 0.31623(8) 0.0456(3) Uani 1 1 d . . . H20A H -0.1152 0.3137 0.2757 0.055 Uiso 1 1 calc R . . H20B H -0.1733 0.3313 0.3303 0.055 Uiso 1 1 calc R . . C21 C -0.12212(11) 0.42274(7) 0.29351(7) 0.0396(3) Uani 1 1 d . . . H21A H -0.1309 0.4522 0.3318 0.048 Uiso 1 1 calc R . . H21B H -0.0577 0.4373 0.2867 0.048 Uiso 1 1 calc R . . C22 C -0.21033(10) 0.43809(7) 0.22565(7) 0.0344(3) Uani 1 1 d . . . C23 C -0.30804(11) 0.40972(8) 0.21358(7) 0.0402(3) Uani 1 1 d . . . H23 H -0.3205 0.3792 0.2474 0.048 Uiso 1 1 calc R . . C24 C -0.38741(11) 0.42653(8) 0.15154(7) 0.0386(3) Uani 1 1 d . . . H24 H -0.4525 0.4068 0.1452 0.046 Uiso 1 1 calc R . . C26 C -0.28154(13) 0.49689(10) 0.11255(9) 0.0549(4) Uani 1 1 d . . . H26 H -0.2710 0.5274 0.0780 0.066 Uiso 1 1 calc R . . C27 C -0.19847(12) 0.48312(10) 0.17312(9) 0.0543(4) Uani 1 1 d . . . H27 H -0.1344 0.5042 0.1786 0.065 Uiso 1 1 calc R . . N1 N -0.01147(8) 0.10940(6) 0.45820(6) 0.0327(2) Uani 1 1 d . . . N2 N -0.37632(9) 0.46927(6) 0.10013(6) 0.0347(2) Uani 1 1 d . . . O1 O -0.29402(8) 0.05487(6) 0.54836(6) 0.0436(2) Uani 1 1 d . . . O2 O -0.11510(7) 0.02418(5) 0.54570(5) 0.0366(2) Uani 1 1 d . . . O1W O 0.0000 0.19515(11) 0.7500 0.0822(7) Uani 1 2 d S . . O3 O -0.13701(9) 0.12139(5) 0.63077(5) 0.0462(2) Uani 1 1 d . . . O4 O -0.17553(9) -0.00597(5) 0.65093(5) 0.0438(2) Uani 1 1 d . . . P1 P -0.17188(3) 0.052815(18) 0.592411(17) 0.03219(9) Uani 1 1 d . . . Co1 Co 0.0000 0.0000 0.5000 0.02746(7) Uani 1 2 d S . . H1W H -0.043(2) 0.1650(15) 0.7106(14) 0.112(9) Uiso 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 0.0380(7) 0.0368(7) 0.0400(7) 0.0004(5) 0.0133(5) 0.0069(5) C2 0.0427(8) 0.0472(8) 0.0552(9) -0.0005(7) 0.0120(7) -0.0013(6) C3 0.0528(10) 0.0639(11) 0.0525(9) -0.0040(8) -0.0009(8) 0.0045(8) C4 0.0754(12) 0.0619(11) 0.0455(9) 0.0081(8) 0.0054(8) 0.0162(9) C5 0.0766(12) 0.0430(8) 0.0577(10) 0.0108(7) 0.0225(9) 0.0025(8) C6 0.0470(8) 0.0387(7) 0.0528(8) 0.0016(6) 0.0125(7) -0.0001(6) C7 0.0367(7) 0.0392(7) 0.0551(8) 0.0121(6) 0.0123(6) 0.0040(6) C8 0.0593(10) 0.0587(10) 0.0679(11) 0.0285(9) 0.0173(9) 0.0089(8) C9 0.0830(16) 0.0665(14) 0.117(2) 0.0522(14) 0.0252(15) 0.0041(12) C10 0.0759(15) 0.0433(11) 0.151(3) 0.0269(14) 0.0156(16) -0.0084(10) C11 0.0579(11) 0.0490(10) 0.1091(17) -0.0075(11) 0.0059(11) -0.0091(8) C12 0.0491(9) 0.0450(8) 0.0665(10) 0.0004(7) 0.0107(8) -0.0051(7) C14 0.0490(8) 0.0346(7) 0.0335(6) -0.0001(5) 0.0132(6) -0.0011(6) C15 0.0473(8) 0.0314(6) 0.0394(7) -0.0024(5) 0.0103(6) 0.0013(5) C16 0.0328(6) 0.0343(6) 0.0388(7) 0.0077(5) 0.0014(5) 0.0024(5) C17 0.0568(9) 0.0452(8) 0.0337(7) 0.0094(6) 0.0142(6) 0.0093(6) C18 0.0513(8) 0.0367(7) 0.0325(6) 0.0009(5) 0.0117(6) 0.0081(6) C19 0.0440(8) 0.0368(7) 0.0460(8) 0.0121(6) 0.0002(6) 0.0010(6) C20 0.0451(8) 0.0364(7) 0.0435(7) 0.0095(6) -0.0015(6) 0.0009(6) C21 0.0368(7) 0.0381(7) 0.0370(7) 0.0104(5) 0.0026(5) -0.0004(5) C22 0.0358(6) 0.0321(6) 0.0325(6) 0.0063(5) 0.0071(5) 0.0026(5) C23 0.0394(7) 0.0449(7) 0.0341(6) 0.0126(6) 0.0089(5) -0.0018(6) C24 0.0340(6) 0.0434(7) 0.0361(6) 0.0078(5) 0.0082(5) -0.0020(5) C26 0.0432(8) 0.0709(11) 0.0433(8) 0.0287(7) 0.0042(7) -0.0100(7) C27 0.0373(8) 0.0687(10) 0.0492(9) 0.0261(8) 0.0036(7) -0.0105(7) N1 0.0357(5) 0.0290(5) 0.0312(5) 0.0015(4) 0.0079(4) 0.0014(4) N2 0.0360(6) 0.0356(6) 0.0291(5) 0.0067(4) 0.0057(4) 0.0013(4) O1 0.0351(5) 0.0465(6) 0.0483(6) 0.0110(4) 0.0123(4) 0.0022(4) O2 0.0374(5) 0.0400(5) 0.0330(4) -0.0036(4) 0.0124(4) 0.0012(4) O1W 0.1109(18) 0.0511(11) 0.0602(12) 0.000 -0.0054(12) 0.000 O3 0.0581(6) 0.0373(5) 0.0432(5) -0.0088(4) 0.0164(5) -0.0025(4) O4 0.0567(6) 0.0408(5) 0.0343(5) 0.0036(4) 0.0153(5) -0.0024(4) P1 0.03492(17) 0.03194(17) 0.02959(16) -0.00112(12) 0.01037(13) 0.00011(12) Co1 0.03173(13) 0.02485(12) 0.02357(12) -0.00257(8) 0.00600(9) -0.00058(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C6 1.378(2) . ? C1 C2 1.378(2) . ? C1 O1 1.3845(17) . ? C2 C3 1.378(2) . ? C3 C4 1.374(3) . ? C4 C5 1.375(3) . ? C5 C6 1.385(2) . ? C7 C12 1.369(2) . ? C7 C8 1.379(2) . ? C7 O4 1.3858(18) . ? C8 C9 1.385(3) . ? C9 C10 1.368(4) . ? C10 C11 1.367(4) . ? C11 C12 1.388(2) . ? C14 N1 1.3372(17) . ? C14 C15 1.3779(19) . ? C15 C16 1.384(2) . ? C16 C17 1.385(2) . ? C16 C19 1.5088(18) . ? C17 C18 1.374(2) . ? C18 N1 1.3395(17) . ? C19 C20 1.5238(19) . ? C20 C21 1.5127(18) . ? C21 C22 1.5073(17) . ? C22 C27 1.3785(19) . ? C22 C23 1.3790(19) . ? C23 C24 1.3798(18) . ? C24 N2 1.3320(16) . ? C26 N2 1.3365(19) . ? C26 C27 1.377(2) . ? N1 Co1 2.1637(10) . ? N2 Co1 2.2138(10) 4_455 ? O1 P1 1.6097(10) . ? O2 P1 1.4825(9) . ? O2 Co1 2.1000(9) . ? O3 P1 1.4699(10) . ? O4 P1 1.5964(10) . ? Co1 O2 2.1000(9) 5_556 ? Co1 N1 2.1637(10) 5_556 ? Co1 N2 2.2138(10) 8_556 ? Co1 N2 2.2138(10) 4_445 ? 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 C6 C1 C2 120.73(14) . . ? C6 C1 O1 123.28(13) . . ? C2 C1 O1 115.98(13) . . ? C3 C2 C1 119.63(16) . . ? C4 C3 C2 120.38(17) . . ? C3 C4 C5 119.59(16) . . ? C4 C5 C6 120.86(17) . . ? C1 C6 C5 118.80(15) . . ? C12 C7 C8 121.48(16) . . ? C12 C7 O4 124.07(14) . . ? C8 C7 O4 114.45(16) . . ? C7 C8 C9 118.6(2) . . ? C10 C9 C8 120.7(2) . . ? C11 C10 C9 119.8(2) . . ? C10 C11 C12 120.7(2) . . ? C7 C12 C11 118.65(19) . . ? N1 C14 C15 123.86(12) . . ? C14 C15 C16 119.69(13) . . ? C15 C16 C17 116.62(12) . . ? C15 C16 C19 120.93(13) . . ? C17 C16 C19 122.43(13) . . ? C18 C17 C16 120.20(13) . . ? N1 C18 C17 123.43(13) . . ? C16 C19 C20 112.02(12) . . ? C21 C20 C19 112.64(12) . . ? C22 C21 C20 113.88(12) . . ? C27 C22 C23 116.29(12) . . ? C27 C22 C21 121.73(12) . . ? C23 C22 C21 121.96(12) . . ? C22 C23 C24 120.20(12) . . ? N2 C24 C23 123.90(13) . . ? N2 C26 C27 124.23(14) . . ? C26 C27 C22 119.92(14) . . ? C14 N1 C18 116.17(11) . . ? C14 N1 Co1 122.62(9) . . ? C18 N1 Co1 121.15(9) . . ? C24 N2 C26 115.45(11) . . ? C24 N2 Co1 126.06(9) . 4_455 ? C26 N2 Co1 118.47(9) . 4_455 ? C1 O1 P1 125.40(9) . . ? P1 O2 Co1 163.72(6) . . ? C7 O4 P1 127.78(10) . . ? O3 P1 O2 118.65(6) . . ? O3 P1 O4 106.92(6) . . ? O2 P1 O4 110.84(6) . . ? O3 P1 O1 111.24(6) . . ? O2 P1 O1 109.39(6) . . ? O4 P1 O1 97.77(6) . . ? O2 Co1 O2 180.00(4) . 5_556 ? O2 Co1 N1 90.26(4) . 5_556 ? O2 Co1 N1 89.74(4) 5_556 5_556 ? O2 Co1 N1 89.74(4) . . ? O2 Co1 N1 90.26(4) 5_556 . ? N1 Co1 N1 180.00(5) 5_556 . ? O2 Co1 N2 91.21(4) . 8_556 ? O2 Co1 N2 88.79(4) 5_556 8_556 ? N1 Co1 N2 87.61(4) 5_556 8_556 ? N1 Co1 N2 92.39(4) . 8_556 ? O2 Co1 N2 88.79(4) . 4_445 ? O2 Co1 N2 91.21(4) 5_556 4_445 ? N1 Co1 N2 92.39(4) 5_556 4_445 ? N1 Co1 N2 87.61(4) . 4_445 ? N2 Co1 N2 180.0 8_556 4_445 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.274 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.042 data_complex6 _database_code_depnum_ccdc_archive 'CCDC 898355' #TrackingRef 'web_deposit_cif_file_5_DebajyotiGhoshal_1346073361.complex6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H50 N4 Ni O9 P2' _chemical_formula_weight 971.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' _cell_length_a 13.7300(4) _cell_length_b 18.3498(4) _cell_length_c 19.7497(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.5670(10) _cell_angle_gamma 90.00 _cell_volume 4688.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39944 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8281 _exptl_absorpt_correction_T_max 0.8892 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39944 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.30 _reflns_number_total 5780 _reflns_number_gt 4681 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+2.5421P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5780 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.88970(12) -0.07243(9) 0.34976(8) 0.0361(3) Uani 1 1 d . . . H1 H 0.9550 -0.0912 0.3558 0.043 Uiso 1 1 calc R . . C2 C 0.81026(12) -0.08926(9) 0.28741(8) 0.0383(4) Uani 1 1 d . . . H2 H 0.8229 -0.1190 0.2531 0.046 Uiso 1 1 calc R . . C3 C 0.71207(12) -0.06230(8) 0.27556(8) 0.0328(3) Uani 1 1 d . . . C4 C 0.70029(14) -0.01844(12) 0.32891(10) 0.0520(5) Uani 1 1 d . . . H4 H 0.6360 0.0017 0.3237 0.062 Uiso 1 1 calc R . . C5 C 0.78341(14) -0.00431(11) 0.38993(10) 0.0520(5) Uani 1 1 d . . . H5 H 0.7727 0.0255 0.4249 0.062 Uiso 1 1 calc R . . C6 C 0.62407(12) -0.07776(9) 0.20723(9) 0.0385(4) Uani 1 1 d . . . H6A H 0.6328 -0.0482 0.1690 0.046 Uiso 1 1 calc R . . H6B H 0.5599 -0.0631 0.2137 0.046 Uiso 1 1 calc R . . C7 C 0.61542(13) -0.15701(9) 0.18425(10) 0.0445(4) Uani 1 1 d . . . H7A H 0.6169 -0.1874 0.2248 0.053 Uiso 1 1 calc R . . H7B H 0.6748 -0.1697 0.1705 0.053 Uiso 1 1 calc R . . C8 C 0.51723(13) -0.17311(9) 0.12174(10) 0.0442(4) Uani 1 1 d . . . H8A H 0.4579 -0.1658 0.1372 0.053 Uiso 1 1 calc R . . H8B H 0.5118 -0.1391 0.0831 0.053 Uiso 1 1 calc R . . C9 C 0.51521(11) -0.24983(9) 0.09398(9) 0.0360(3) Uani 1 1 d . . . C10 C 0.50719(14) -0.31039(10) 0.13381(9) 0.0438(4) Uani 1 1 d . . . H10 H 0.5029 -0.3043 0.1795 0.053 Uiso 1 1 calc R . . C11 C 0.50552(13) -0.37936(9) 0.10624(9) 0.0390(4) Uani 1 1 d . . . H11 H 0.4999 -0.4188 0.1343 0.047 Uiso 1 1 calc R . . C12 C 0.52104(13) -0.33436(9) 0.00317(8) 0.0371(3) Uani 1 1 d . . . H12 H 0.5267 -0.3419 -0.0419 0.045 Uiso 1 1 calc R . . C13 C 0.52294(13) -0.26354(9) 0.02710(9) 0.0388(3) Uani 1 1 d . . . H13 H 0.5294 -0.2250 -0.0017 0.047 Uiso 1 1 calc R . . C14 C 0.66013(12) 0.09356(9) 0.48624(9) 0.0369(3) Uani 1 1 d . . . C15 C 0.56405(14) 0.06946(10) 0.44353(10) 0.0478(4) Uani 1 1 d . . . H15 H 0.5350 0.0283 0.4565 0.057 Uiso 1 1 calc R . . C16 C 0.51132(16) 0.10683(12) 0.38136(11) 0.0605(5) Uani 1 1 d . . . H16 H 0.4463 0.0910 0.3526 0.073 Uiso 1 1 calc R . . C17 C 0.55457(18) 0.16720(12) 0.36188(11) 0.0630(6) Uani 1 1 d . . . H17 H 0.5191 0.1921 0.3198 0.076 Uiso 1 1 calc R . . C18 C 0.65035(17) 0.19078(11) 0.40463(11) 0.0572(5) Uani 1 1 d . . . H18 H 0.6796 0.2316 0.3911 0.069 Uiso 1 1 calc R . . C19 C 0.70397(14) 0.15454(10) 0.46769(10) 0.0452(4) Uani 1 1 d . . . H19 H 0.7683 0.1711 0.4969 0.054 Uiso 1 1 calc R . . C20 C 0.78742(13) -0.07718(10) 0.64010(10) 0.0436(4) Uani 1 1 d . . . C21 C 0.78526(16) -0.11251(12) 0.70130(13) 0.0623(6) Uani 1 1 d . . . H21 H 0.8080 -0.0892 0.7456 0.075 Uiso 1 1 calc R . . C22 C 0.7487(2) -0.18322(15) 0.69545(19) 0.0906(9) Uani 1 1 d . . . H22 H 0.7465 -0.2075 0.7362 0.109 Uiso 1 1 calc R . . C23 C 0.7158(2) -0.21788(14) 0.6302(2) 0.0960(10) Uani 1 1 d . . . H23 H 0.6922 -0.2657 0.6268 0.115 Uiso 1 1 calc R . . C24 C 0.71784(18) -0.18180(13) 0.57007(17) 0.0764(7) Uani 1 1 d . . . H24 H 0.6947 -0.2053 0.5258 0.092 Uiso 1 1 calc R . . C25 C 0.75382(15) -0.11068(11) 0.57412(12) 0.0556(5) Uani 1 1 d . . . H25 H 0.7551 -0.0863 0.5331 0.067 Uiso 1 1 calc R . . N1 N 0.87815(10) -0.03068(7) 0.40201(7) 0.0329(3) Uani 1 1 d . . . N2 N 0.51157(9) -0.39260(7) 0.04094(7) 0.0315(3) Uani 1 1 d . . . O1W O 1.0000 0.19526(14) 0.7500 0.0807(8) Uani 1 2 d S . . O5 O 0.88576(8) 0.02338(6) 0.54598(6) 0.0353(2) Uani 1 1 d . . . O6 O 0.70714(9) 0.05356(7) 0.54810(6) 0.0423(3) Uani 1 1 d . . . O7 O 0.86323(10) 0.12117(6) 0.63073(6) 0.0448(3) Uani 1 1 d . . . O8 O 0.82649(10) -0.00681(6) 0.65142(6) 0.0427(3) Uani 1 1 d . . . P2 P 0.82926(3) 0.05203(2) 0.59243(2) 0.03146(10) Uani 1 1 d . . . Ni1 Ni 1.0000 0.0000 0.5000 0.02686(8) Uani 1 2 d S . . H1W H 0.963(2) 0.1687(15) 0.7162(14) 0.096(10) Uiso 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 0.0322(7) 0.0418(9) 0.0324(8) -0.0087(7) 0.0085(6) 0.0016(6) C2 0.0373(8) 0.0451(9) 0.0312(8) -0.0124(7) 0.0098(6) 0.0008(7) C3 0.0347(7) 0.0318(8) 0.0286(7) -0.0056(6) 0.0062(6) -0.0021(6) C4 0.0352(8) 0.0693(13) 0.0443(10) -0.0238(9) 0.0038(7) 0.0118(8) C5 0.0418(9) 0.0684(13) 0.0392(9) -0.0273(9) 0.0050(7) 0.0099(8) C6 0.0361(8) 0.0376(8) 0.0349(8) -0.0099(7) 0.0027(6) 0.0005(6) C7 0.0437(9) 0.0358(9) 0.0425(9) -0.0095(7) -0.0007(7) -0.0021(7) C8 0.0436(9) 0.0362(9) 0.0426(9) -0.0112(7) 0.0007(7) 0.0002(7) C9 0.0318(7) 0.0332(8) 0.0357(8) -0.0074(6) 0.0015(6) -0.0024(6) C10 0.0561(10) 0.0443(9) 0.0308(8) -0.0085(7) 0.0144(7) -0.0081(8) C11 0.0480(9) 0.0369(8) 0.0314(8) -0.0009(7) 0.0124(7) -0.0084(7) C12 0.0464(9) 0.0339(8) 0.0314(8) 0.0005(6) 0.0135(7) 0.0000(7) C13 0.0459(9) 0.0313(8) 0.0366(8) 0.0016(7) 0.0105(7) -0.0009(7) C14 0.0359(8) 0.0377(8) 0.0377(8) 0.0004(7) 0.0130(7) 0.0071(6) C15 0.0426(9) 0.0460(10) 0.0526(11) -0.0001(8) 0.0131(8) -0.0016(8) C16 0.0531(11) 0.0639(13) 0.0517(12) -0.0023(10) 0.0007(9) 0.0051(10) C17 0.0726(14) 0.0626(13) 0.0442(11) 0.0076(10) 0.0070(10) 0.0144(11) C18 0.0745(14) 0.0418(10) 0.0563(12) 0.0108(9) 0.0230(11) 0.0031(10) C19 0.0440(9) 0.0381(9) 0.0512(10) 0.0019(8) 0.0131(8) 0.0000(7) C20 0.0360(8) 0.0390(9) 0.0538(11) 0.0117(8) 0.0125(8) 0.0029(7) C21 0.0586(12) 0.0592(13) 0.0667(14) 0.0288(11) 0.0180(10) 0.0088(10) C22 0.0800(18) 0.0693(17) 0.116(2) 0.0545(18) 0.0246(17) 0.0036(14) C23 0.0740(17) 0.0448(13) 0.153(3) 0.0281(17) 0.0157(18) -0.0095(12) C24 0.0571(13) 0.0504(13) 0.106(2) -0.0089(13) 0.0067(13) -0.0089(10) C25 0.0504(10) 0.0457(11) 0.0654(13) 0.0000(9) 0.0124(9) -0.0056(9) N1 0.0337(6) 0.0344(7) 0.0273(6) -0.0059(5) 0.0057(5) -0.0013(5) N2 0.0334(6) 0.0291(6) 0.0297(6) -0.0011(5) 0.0078(5) -0.0018(5) O1W 0.109(2) 0.0514(13) 0.0561(15) 0.000 -0.0066(14) 0.000 O5 0.0359(5) 0.0392(6) 0.0315(6) -0.0034(5) 0.0122(4) 0.0013(5) O6 0.0343(6) 0.0464(7) 0.0454(7) 0.0108(5) 0.0125(5) 0.0018(5) O7 0.0560(7) 0.0376(6) 0.0411(7) -0.0087(5) 0.0169(6) -0.0023(5) O8 0.0539(7) 0.0420(7) 0.0322(6) 0.0045(5) 0.0144(5) -0.0032(5) P2 0.03416(19) 0.0327(2) 0.02736(19) -0.00105(15) 0.01011(15) -0.00056(15) Ni1 0.03050(14) 0.02528(14) 0.02260(13) -0.00259(10) 0.00597(10) -0.00039(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 N1 1.3366(19) . ? C1 C2 1.379(2) . ? C2 C3 1.381(2) . ? C3 C4 1.378(2) . ? C3 C6 1.507(2) . ? C4 C5 1.379(2) . ? C5 N1 1.332(2) . ? C6 C7 1.516(2) . ? C7 C8 1.521(2) . ? C8 C9 1.508(2) . ? C9 C13 1.383(2) . ? C9 C10 1.387(2) . ? C10 C11 1.375(2) . ? C11 N2 1.342(2) . ? C12 N2 1.334(2) . ? C12 C13 1.380(2) . ? C14 C19 1.377(2) . ? C14 C15 1.379(2) . ? C14 O6 1.3855(19) . ? C15 C16 1.381(3) . ? C16 C17 1.371(3) . ? C17 C18 1.373(3) . ? C18 C19 1.386(3) . ? C20 C25 1.373(3) . ? C20 C21 1.381(3) . ? C20 O8 1.388(2) . ? C21 C22 1.382(3) . ? C22 C23 1.371(4) . ? C23 C24 1.368(4) . ? C24 C25 1.388(3) . ? N1 Ni1 2.1662(12) . ? N2 Ni1 2.1158(12) 4_645 ? O5 P2 1.4820(11) . ? O5 Ni1 2.1030(10) . ? O6 P2 1.6111(12) . ? O7 P2 1.4707(12) . ? O8 P2 1.5982(12) . ? Ni1 O5 2.1030(10) 5_756 ? Ni1 N2 2.1158(12) 4_655 ? Ni1 N2 2.1158(12) 8_546 ? Ni1 N1 2.1662(12) 5_756 ? 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 N1 C1 C2 123.71(14) . . ? C1 C2 C3 120.43(14) . . ? C4 C3 C2 115.97(14) . . ? C4 C3 C6 122.06(14) . . ? C2 C3 C6 121.94(14) . . ? C3 C4 C5 120.22(16) . . ? N1 C5 C4 124.13(16) . . ? C3 C6 C7 114.06(14) . . ? C6 C7 C8 112.86(14) . . ? C9 C8 C7 112.33(14) . . ? C13 C9 C10 116.24(15) . . ? C13 C9 C8 121.27(16) . . ? C10 C9 C8 122.49(15) . . ? C11 C10 C9 120.45(15) . . ? N2 C11 C10 123.30(15) . . ? N2 C12 C13 123.84(15) . . ? C12 C13 C9 119.97(15) . . ? C19 C14 C15 120.77(16) . . ? C19 C14 O6 123.30(15) . . ? C15 C14 O6 115.92(15) . . ? C14 C15 C16 119.60(18) . . ? C17 C16 C15 120.2(2) . . ? C16 C17 C18 119.83(19) . . ? C17 C18 C19 120.82(19) . . ? C14 C19 C18 118.75(18) . . ? C25 C20 C21 121.44(19) . . ? C25 C20 O8 123.95(17) . . ? C21 C20 O8 114.61(18) . . ? C20 C21 C22 118.8(3) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 119.7(2) . . ? C23 C24 C25 121.0(3) . . ? C20 C25 C24 118.4(2) . . ? C5 N1 C1 115.53(13) . . ? C5 N1 Ni1 118.76(10) . . ? C1 N1 Ni1 125.66(10) . . ? C12 N2 C11 116.18(13) . . ? C12 N2 Ni1 122.77(10) . 4_645 ? C11 N2 Ni1 121.00(10) . 4_645 ? P2 O5 Ni1 163.81(7) . . ? C14 O6 P2 125.52(10) . . ? C20 O8 P2 127.84(12) . . ? O7 P2 O5 118.87(7) . . ? O7 P2 O8 106.78(7) . . ? O5 P2 O8 110.91(7) . . ? O7 P2 O6 110.95(7) . . ? O5 P2 O6 109.58(6) . . ? O8 P2 O6 97.67(6) . . ? O5 Ni1 O5 180.00(4) . 5_756 ? O5 Ni1 N2 90.21(5) . 4_655 ? O5 Ni1 N2 89.79(5) 5_756 4_655 ? O5 Ni1 N2 89.79(5) . 8_546 ? O5 Ni1 N2 90.21(5) 5_756 8_546 ? N2 Ni1 N2 180.000(1) 4_655 8_546 ? O5 Ni1 N1 88.53(4) . . ? O5 Ni1 N1 91.47(4) 5_756 . ? N2 Ni1 N1 87.93(5) 4_655 . ? N2 Ni1 N1 92.07(5) 8_546 . ? O5 Ni1 N1 91.47(4) . 5_756 ? O5 Ni1 N1 88.53(4) 5_756 5_756 ? N2 Ni1 N1 92.07(5) 4_655 5_756 ? N2 Ni1 N1 87.93(5) 8_546 5_756 ? N1 Ni1 N1 180.00(5) . 5_756 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.333 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.046 data_complex7 _database_code_depnum_ccdc_archive 'CCDC 898356' #TrackingRef 'web_deposit_cif_file_4_DebajyotiGhoshal_1350570455.898356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Ca N2 O8 P2' _chemical_formula_weight 694.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.606(5) _cell_length_b 5.763(5) _cell_length_c 12.118(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 111.975(5) _cell_angle_gamma 90.000(5) _cell_volume 1593.5(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 31.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8268 _exptl_absorpt_correction_T_max 0.8859 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15277 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 31.05 _reflns_number_total 4858 _reflns_number_gt 4195 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.floating origin restraint is present. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.2979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.99(4) _refine_ls_number_reflns 4858 _refine_ls_number_parameters 213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.66704(8) 0.6235(4) 0.98134(18) 0.0351(5) Uani 1 1 d . . . C2 C 0.69636(10) 0.7982(5) 0.9482(2) 0.0478(6) Uani 1 1 d . . . H2 H 0.7112 0.9249 0.9979 0.057 Uiso 1 1 calc R . . C3 C 0.70330(12) 0.7825(6) 0.8405(2) 0.0609(7) Uani 1 1 d . . . H3 H 0.7236 0.8981 0.8185 0.073 Uiso 1 1 calc R . . C4 C 0.68067(13) 0.5992(6) 0.7657(2) 0.0648(9) Uani 1 1 d . . . H4 H 0.6848 0.5915 0.6926 0.078 Uiso 1 1 calc R . . C5 C 0.65130(12) 0.4240(6) 0.8000(2) 0.0640(8) Uani 1 1 d . . . H5 H 0.6362 0.2982 0.7498 0.077 Uiso 1 1 calc R . . C6 C 0.64444(10) 0.4355(5) 0.9081(2) 0.0503(6) Uani 1 1 d . . . H6 H 0.6249 0.3182 0.9310 0.060 Uiso 1 1 calc R . . C7 C 0.64356(8) 0.8782(4) 1.31252(16) 0.0319(4) Uani 1 1 d . . . C8 C 0.66930(10) 1.0626(4) 1.27688(19) 0.0393(5) Uani 1 1 d . . . H8 H 0.6695 1.0685 1.2003 0.047 Uiso 1 1 calc R . . C9 C 0.69478(10) 1.2383(4) 1.3582(2) 0.0470(6) Uani 1 1 d . . . H9 H 0.7124 1.3628 1.3356 0.056 Uiso 1 1 calc R . . C10 C 0.69451(11) 1.2317(5) 1.4717(2) 0.0547(7) Uani 1 1 d . . . H10 H 0.7119 1.3505 1.5253 0.066 Uiso 1 1 calc R . . C11 C 0.66834(11) 1.0478(5) 1.5052(2) 0.0539(7) Uani 1 1 d . . . H11 H 0.6679 1.0431 1.5816 0.065 Uiso 1 1 calc R . . C12 C 0.64260(10) 0.8694(4) 1.42574(18) 0.0428(5) Uani 1 1 d . . . H12 H 0.6249 0.7454 1.4485 0.051 Uiso 1 1 calc R . . C13 C 0.52412(11) -0.0489(4) 0.75420(18) 0.0422(5) Uani 1 1 d . . . H13 H 0.5412 -0.1693 0.8069 0.051 Uiso 1 1 calc R . . C14 C 0.52434(10) -0.0616(4) 0.64028(18) 0.0410(5) Uani 1 1 d . . . H14 H 0.5407 -0.1892 0.6172 0.049 Uiso 1 1 calc R . . C15 C 0.50003(8) 0.1174(3) 0.56125(14) 0.0311(5) Uani 1 1 d . . . C16 C 0.47600(11) 0.3005(4) 0.60069(18) 0.0427(5) Uani 1 1 d . . . H16 H 0.4596 0.4253 0.5506 0.051 Uiso 1 1 calc R . . C17 C 0.47645(11) 0.2976(4) 0.71485(19) 0.0438(5) Uani 1 1 d . . . H17 H 0.4590 0.4203 0.7390 0.053 Uiso 1 1 calc R . . N1 N 0.50064(7) 0.1279(3) 0.79210(13) 0.0352(4) Uani 1 1 d . . . O1 O 0.66305(5) 0.6383(3) 1.09278(11) 0.0356(3) Uani 1 1 d . . . O2 O 0.56718(7) 0.4447(3) 1.06900(14) 0.0384(4) Uani 1 1 d . . . O3 O 0.61814(6) 0.6901(3) 1.24053(11) 0.0357(3) Uani 1 1 d . . . O4 O 0.57185(7) 0.8799(3) 1.03749(12) 0.0337(3) Uani 1 1 d . . . P1 P 0.599415(16) 0.66590(9) 1.10014(3) 0.02559(10) Uani 1 1 d . . . Ca1 Ca 0.5000 0.15604(9) 1.0000 0.02104(10) Uani 1 2 d S . . 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 0.0278(8) 0.0368(13) 0.0419(10) -0.0016(9) 0.0144(8) 0.0039(8) C2 0.0467(13) 0.0438(14) 0.0545(15) -0.0029(11) 0.0209(11) -0.0060(10) C3 0.0642(17) 0.0630(18) 0.0654(17) 0.0081(14) 0.0356(14) -0.0037(14) C4 0.0656(16) 0.085(3) 0.0515(15) -0.0031(15) 0.0312(13) 0.0042(16) C5 0.0625(16) 0.074(2) 0.0599(17) -0.0278(15) 0.0286(14) -0.0085(15) C6 0.0486(13) 0.0483(14) 0.0614(15) -0.0146(12) 0.0292(12) -0.0075(12) C7 0.0310(10) 0.0303(10) 0.0289(9) -0.0025(8) 0.0049(7) 0.0014(8) C8 0.0427(11) 0.0348(11) 0.0363(11) -0.0006(9) 0.0101(9) -0.0048(9) C9 0.0443(12) 0.0364(12) 0.0508(14) -0.0044(10) 0.0071(10) -0.0045(10) C10 0.0517(14) 0.0472(15) 0.0501(14) -0.0189(11) 0.0019(11) 0.0028(11) C11 0.0599(16) 0.0635(17) 0.0336(12) -0.0133(12) 0.0121(11) 0.0063(13) C12 0.0466(12) 0.0476(14) 0.0347(11) 0.0012(10) 0.0159(9) 0.0008(10) C13 0.0651(14) 0.0383(12) 0.0252(10) 0.0056(9) 0.0189(9) 0.0099(11) C14 0.0604(13) 0.0372(12) 0.0286(10) -0.0002(9) 0.0204(9) 0.0124(11) C15 0.0368(9) 0.0368(13) 0.0222(8) -0.0011(7) 0.0139(7) -0.0013(8) C16 0.0626(14) 0.0427(12) 0.0286(10) 0.0096(9) 0.0237(9) 0.0166(11) C17 0.0619(14) 0.0427(12) 0.0354(11) 0.0034(9) 0.0281(10) 0.0148(11) N1 0.0469(9) 0.0382(11) 0.0237(7) 0.0009(7) 0.0169(6) 0.0009(8) O1 0.0272(6) 0.0394(9) 0.0389(7) -0.0046(7) 0.0108(5) 0.0022(7) O2 0.0422(8) 0.0303(8) 0.0414(8) -0.0048(6) 0.0141(7) -0.0109(6) O3 0.0483(7) 0.0286(8) 0.0278(6) -0.0002(6) 0.0114(5) -0.0078(7) O4 0.0370(8) 0.0306(7) 0.0320(7) 0.0027(6) 0.0112(6) 0.0090(6) P1 0.0266(2) 0.0219(2) 0.0274(2) -0.0008(2) 0.00915(16) -0.0008(2) Ca1 0.0291(2) 0.0176(2) 0.01799(19) 0.000 0.01058(15) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C6 1.379(3) . ? C1 C2 1.383(3) . ? C1 O1 1.393(2) . ? C2 C3 1.382(3) . ? C3 C4 1.368(4) . ? C4 C5 1.392(4) . ? C5 C6 1.383(3) . ? C7 C12 1.382(3) . ? C7 O3 1.385(2) . ? C7 C8 1.386(3) . ? C8 C9 1.388(3) . ? C9 C10 1.379(4) . ? C10 C11 1.377(4) . ? C11 C12 1.389(3) . ? C13 N1 1.334(3) . ? C13 C14 1.384(3) . ? C14 C15 1.382(3) . ? C15 C16 1.380(3) . ? C15 C15 1.484(3) 2_656 ? C16 C17 1.379(3) . ? C17 N1 1.330(3) . ? N1 Ca1 2.5306(18) . ? O1 P1 1.6092(13) . ? O2 P1 1.4739(18) . ? O2 Ca1 2.2726(18) . ? O3 P1 1.5935(14) . ? O4 P1 1.4738(18) . ? O4 Ca1 2.2943(18) 1_565 ? Ca1 O2 2.2726(19) 2_657 ? Ca1 O4 2.2943(18) 2_647 ? Ca1 O4 2.2943(18) 1_545 ? Ca1 N1 2.5306(18) 2_657 ? 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 C6 C1 C2 120.9(2) . . ? C6 C1 O1 121.0(2) . . ? C2 C1 O1 118.08(19) . . ? C3 C2 C1 119.3(2) . . ? C4 C3 C2 120.9(3) . . ? C3 C4 C5 119.4(3) . . ? C6 C5 C4 120.6(3) . . ? C1 C6 C5 119.0(2) . . ? C12 C7 O3 115.14(19) . . ? C12 C7 C8 121.1(2) . . ? O3 C7 C8 123.70(19) . . ? C7 C8 C9 118.4(2) . . ? C10 C9 C8 121.2(2) . . ? C11 C10 C9 119.5(2) . . ? C10 C11 C12 120.5(2) . . ? C7 C12 C11 119.2(2) . . ? N1 C13 C14 123.2(2) . . ? C15 C14 C13 119.29(19) . . ? C16 C15 C14 117.47(17) . . ? C16 C15 C15 120.42(14) . 2_656 ? C14 C15 C15 122.10(14) . 2_656 ? C17 C16 C15 119.63(19) . . ? N1 C17 C16 123.2(2) . . ? C17 N1 C13 117.15(17) . . ? C17 N1 Ca1 119.05(14) . . ? C13 N1 Ca1 123.80(13) . . ? C1 O1 P1 118.88(11) . . ? P1 O2 Ca1 167.16(11) . . ? C7 O3 P1 128.53(13) . . ? P1 O4 Ca1 148.69(9) . 1_565 ? O4 P1 O2 119.47(9) . . ? O4 P1 O3 111.72(9) . . ? O2 P1 O3 105.20(8) . . ? O4 P1 O1 108.89(9) . . ? O2 P1 O1 110.00(10) . . ? O3 P1 O1 99.74(7) . . ? O2 Ca1 O2 85.88(10) . 2_657 ? O2 Ca1 O4 168.85(5) . 2_647 ? O2 Ca1 O4 91.97(7) 2_657 2_647 ? O2 Ca1 O4 91.97(7) . 1_545 ? O2 Ca1 O4 168.85(5) 2_657 1_545 ? O4 Ca1 O4 92.17(10) 2_647 1_545 ? O2 Ca1 N1 97.96(6) . . ? O2 Ca1 N1 87.44(6) 2_657 . ? O4 Ca1 N1 92.86(6) 2_647 . ? O4 Ca1 N1 82.02(5) 1_545 . ? O2 Ca1 N1 87.44(6) . 2_657 ? O2 Ca1 N1 97.96(6) 2_657 2_657 ? O4 Ca1 N1 82.02(5) 2_647 2_657 ? O4 Ca1 N1 92.86(6) 1_545 2_657 ? N1 Ca1 N1 172.65(9) . 2_657 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.299 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.046 data_complex8 _database_code_depnum_ccdc_archive 'CCDC 898357' #TrackingRef 'web_deposit_cif_file_5_DebajyotiGhoshal_1350570455.898357.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 N2 O8 P2 Pb' _chemical_formula_weight 861.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.233(5) _cell_length_b 12.492(5) _cell_length_c 13.480(5) _cell_angle_alpha 76.321(5) _cell_angle_beta 87.150(5) _cell_angle_gamma 87.484(5) _cell_volume 1671.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 5.197 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8271 _exptl_absorpt_correction_T_max 0.8864 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26277 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7587 _reflns_number_gt 5772 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1244P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7587 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1803 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2520(13) -0.3063(10) 1.0876(9) 0.057(3) Uani 1 1 d . . . H1 H 0.2443 -0.2825 1.1480 0.068 Uiso 1 1 calc R . . C2 C 0.2500(13) -0.4181(9) 1.0928(8) 0.053(3) Uani 1 1 d . . . H2 H 0.2405 -0.4683 1.1556 0.064 Uiso 1 1 calc R . . C3 C 0.2623(11) -0.4541(8) 1.0037(8) 0.046(3) Uani 1 1 d . . . C4 C 0.2753(14) -0.3767(9) 0.9122(9) 0.059(3) Uani 1 1 d . . . H4 H 0.2839 -0.3977 0.8504 0.071 Uiso 1 1 calc R . . C5 C 0.2753(13) -0.2677(9) 0.9155(9) 0.053(3) Uani 1 1 d . . . H5 H 0.2837 -0.2154 0.8539 0.064 Uiso 1 1 calc R . . C6 C 0.2593(12) -0.5752(9) 1.0059(9) 0.048(3) Uani 1 1 d . . . C7 C 0.1643(14) -0.6400(10) 1.0577(10) 0.060(3) Uani 1 1 d . . . H7 H 0.0973 -0.6100 1.0930 0.072 Uiso 1 1 calc R . . C8 C 0.1665(16) -0.7497(11) 1.0582(12) 0.071(4) Uani 1 1 d . . . H8 H 0.1001 -0.7921 1.0953 0.085 Uiso 1 1 calc R . . C9 C 0.3502(14) -0.7349(10) 0.9594(11) 0.063(3) Uani 1 1 d . . . H9 H 0.4175 -0.7672 0.9264 0.075 Uiso 1 1 calc R . . C10 C 0.3549(13) -0.6238(10) 0.9526(10) 0.058(3) Uani 1 1 d . . . H10 H 0.4205 -0.5822 0.9133 0.070 Uiso 1 1 calc R . . C11 C 0.0505(11) -0.0588(11) 0.6750(9) 0.051(3) Uani 1 1 d . . . C12 C -0.0128(16) -0.1322(19) 0.6365(17) 0.130(9) Uani 1 1 d . . . H12 H -0.1033 -0.1264 0.6316 0.156 Uiso 1 1 calc R . . C13 C 0.055(2) -0.212(2) 0.606(2) 0.172(14) Uani 1 1 d . . . H13 H 0.0100 -0.2675 0.5885 0.207 Uiso 1 1 calc R . . C14 C 0.1904(18) -0.2146(19) 0.5997(15) 0.118(8) Uani 1 1 d . . . H14 H 0.2371 -0.2675 0.5727 0.141 Uiso 1 1 calc R . . C15 C 0.2524(13) -0.1384(13) 0.6340(10) 0.067(4) Uani 1 1 d . . . H15 H 0.3435 -0.1398 0.6315 0.081 Uiso 1 1 calc R . . C16 C 0.1853(12) -0.0593(12) 0.6720(10) 0.059(3) Uani 1 1 d . . . H16 H 0.2294 -0.0070 0.6954 0.071 Uiso 1 1 calc R . . C17 C 0.1030(10) 0.2395(9) 0.7356(9) 0.043(3) Uani 1 1 d . . . C18 C 0.1230(12) 0.2578(12) 0.6331(10) 0.060(3) Uani 1 1 d . . . H18 H 0.1381 0.1988 0.6025 0.072 Uiso 1 1 calc R . . C19 C 0.1207(13) 0.3657(13) 0.5735(11) 0.065(4) Uani 1 1 d . . . H19 H 0.1340 0.3793 0.5029 0.078 Uiso 1 1 calc R . . C20 C 0.0994(15) 0.4485(15) 0.6188(14) 0.079(5) Uani 1 1 d . . . H20 H 0.0979 0.5201 0.5784 0.095 Uiso 1 1 calc R . . C21 C 0.0790(14) 0.4332(13) 0.7244(15) 0.086(5) Uani 1 1 d . . . H21 H 0.0656 0.4926 0.7547 0.103 Uiso 1 1 calc R . . C22 C 0.0798(12) 0.3236(11) 0.7829(11) 0.063(3) Uani 1 1 d . . . H22 H 0.0645 0.3089 0.8533 0.076 Uiso 1 1 calc R . . C23 C 0.5401(11) 0.2265(9) 0.6866(8) 0.042(2) Uani 1 1 d . . . C24 C 0.4645(12) 0.3209(10) 0.6740(9) 0.054(3) Uani 1 1 d . . . H24 H 0.3746 0.3175 0.6872 0.065 Uiso 1 1 calc R . . C25 C 0.5224(14) 0.4215(12) 0.6417(12) 0.072(4) Uani 1 1 d . . . H25 H 0.4717 0.4863 0.6334 0.086 Uiso 1 1 calc R . . C26 C 0.6550(16) 0.4256(12) 0.6216(12) 0.074(4) Uani 1 1 d . . . H26 H 0.6938 0.4935 0.5992 0.088 Uiso 1 1 calc R . . C27 C 0.7315(14) 0.3296(12) 0.6346(10) 0.066(4) Uani 1 1 d . . . H27 H 0.8216 0.3329 0.6223 0.080 Uiso 1 1 calc R . . C28 C 0.6730(11) 0.2281(10) 0.6661(8) 0.047(3) Uani 1 1 d . . . H28 H 0.7227 0.1628 0.6730 0.056 Uiso 1 1 calc R . . C29 C 0.6140(10) -0.1054(9) 0.7103(8) 0.041(2) Uani 1 1 d . . . C30 C 0.6259(12) -0.0699(12) 0.6061(9) 0.057(3) Uani 1 1 d . . . H30 H 0.6417 0.0035 0.5756 0.068 Uiso 1 1 calc R . . C31 C 0.6140(12) -0.1461(14) 0.5470(10) 0.065(4) Uani 1 1 d . . . H31 H 0.6216 -0.1222 0.4763 0.078 Uiso 1 1 calc R . . C32 C 0.5922(14) -0.2508(13) 0.5877(12) 0.067(4) Uani 1 1 d . . . H32 H 0.5857 -0.2998 0.5460 0.080 Uiso 1 1 calc R . . C33 C 0.5792(14) -0.2870(11) 0.6922(11) 0.071(4) Uani 1 1 d . . . H33 H 0.5629 -0.3606 0.7217 0.085 Uiso 1 1 calc R . . C34 C 0.5904(13) -0.2139(10) 0.7525(10) 0.058(3) Uani 1 1 d . . . H34 H 0.5819 -0.2384 0.8232 0.070 Uiso 1 1 calc R . . N1 N 0.2642(9) -0.2325(7) 1.0006(6) 0.040(2) Uani 1 1 d . . . N2 N 0.2573(13) -0.8002(10) 1.0092(8) 0.067(3) Uani 1 1 d . . . O1 O 0.0503(7) -0.0468(6) 0.8940(6) 0.0461(18) Uani 1 1 d . . . O2 O -0.0247(7) 0.0204(7) 0.7131(6) 0.0490(19) Uani 1 1 d . . . O3 O -0.1237(6) 0.1086(6) 0.8456(5) 0.0452(17) Uani 1 1 d . . . O4 O 0.1169(7) 0.1339(6) 0.7945(6) 0.0474(18) Uani 1 1 d . . . O5 O 0.3992(7) -0.0395(6) 0.8431(6) 0.0467(18) Uani 1 1 d . . . O6 O 0.5676(7) 0.0845(6) 0.8907(5) 0.0448(18) Uani 1 1 d . . . O7 O 0.4733(7) 0.1270(6) 0.7169(6) 0.0457(18) Uani 1 1 d . . . O8 O 0.6336(6) -0.0352(6) 0.7720(5) 0.0444(17) Uani 1 1 d . . . P1 P -0.0015(3) 0.0482(2) 0.8187(2) 0.0357(6) Uani 1 1 d . . . P2 P 0.5143(2) 0.0336(2) 0.8137(2) 0.0339(6) Uani 1 1 d . . . Pb1 Pb 0.24935(3) -0.02876(3) 0.99608(3) 0.03203(15) 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 0.097(10) 0.037(6) 0.038(6) -0.013(5) 0.002(6) 0.000(6) C2 0.096(9) 0.026(5) 0.036(6) -0.005(5) 0.006(6) -0.005(6) C3 0.063(8) 0.024(5) 0.053(7) -0.018(5) 0.001(6) -0.001(5) C4 0.109(11) 0.026(6) 0.045(7) -0.013(5) 0.014(7) -0.004(6) C5 0.101(10) 0.027(6) 0.032(6) -0.008(5) 0.003(6) -0.012(6) C6 0.080(9) 0.024(5) 0.043(6) -0.014(5) 0.002(6) 0.000(5) C7 0.081(9) 0.036(6) 0.063(8) -0.013(6) 0.014(7) -0.011(6) C8 0.099(11) 0.031(7) 0.087(10) -0.022(7) -0.002(8) -0.014(7) C9 0.080(9) 0.037(7) 0.078(9) -0.032(7) -0.004(7) 0.010(6) C10 0.073(8) 0.039(6) 0.068(8) -0.026(6) 0.008(6) -0.001(6) C11 0.041(6) 0.069(8) 0.048(6) -0.025(6) -0.008(5) 0.014(6) C12 0.068(10) 0.18(2) 0.20(2) -0.149(19) -0.043(12) 0.023(12) C13 0.100(16) 0.20(3) 0.29(4) -0.20(3) -0.077(19) 0.049(17) C14 0.104(14) 0.16(2) 0.126(16) -0.107(15) -0.024(12) 0.057(13) C15 0.061(8) 0.092(11) 0.054(7) -0.031(8) 0.011(6) 0.014(7) C16 0.055(7) 0.071(9) 0.055(7) -0.022(7) 0.008(6) 0.003(6) C17 0.039(6) 0.036(6) 0.051(6) -0.002(5) -0.004(5) -0.006(4) C18 0.060(8) 0.058(8) 0.061(8) -0.010(7) 0.000(6) -0.001(6) C19 0.063(8) 0.065(9) 0.059(8) 0.006(7) -0.007(6) -0.014(7) C20 0.070(10) 0.066(10) 0.092(12) 0.000(10) -0.009(9) -0.004(8) C21 0.073(10) 0.051(9) 0.138(16) -0.032(10) -0.018(10) 0.002(7) C22 0.065(8) 0.057(8) 0.069(9) -0.017(7) -0.006(7) -0.001(7) C23 0.048(6) 0.038(6) 0.042(6) -0.010(5) -0.005(5) -0.005(5) C24 0.051(7) 0.044(7) 0.068(8) -0.013(6) -0.001(6) -0.001(5) C25 0.069(9) 0.044(8) 0.096(11) -0.004(8) 0.006(8) 0.005(7) C26 0.098(12) 0.044(8) 0.075(10) -0.004(7) 0.004(8) -0.024(8) C27 0.072(9) 0.066(9) 0.056(8) -0.003(7) 0.016(6) -0.020(7) C28 0.049(7) 0.039(6) 0.049(6) -0.003(5) 0.005(5) -0.002(5) C29 0.035(5) 0.047(6) 0.048(6) -0.027(5) 0.001(5) 0.005(5) C30 0.054(7) 0.062(8) 0.054(7) -0.015(6) 0.007(6) 0.009(6) C31 0.057(8) 0.098(12) 0.047(7) -0.036(8) 0.007(6) 0.012(7) C32 0.081(10) 0.058(9) 0.070(9) -0.032(8) -0.008(7) 0.006(7) C33 0.101(11) 0.042(7) 0.076(10) -0.027(7) -0.016(8) 0.015(7) C34 0.079(9) 0.046(7) 0.049(7) -0.013(6) -0.005(6) 0.006(6) N1 0.050(5) 0.033(5) 0.038(5) -0.009(4) -0.003(4) -0.008(4) N2 0.102(9) 0.048(7) 0.054(7) -0.014(6) -0.017(6) 0.001(6) O1 0.051(4) 0.036(4) 0.049(4) -0.005(3) -0.003(3) -0.001(3) O2 0.040(4) 0.064(5) 0.051(4) -0.030(4) -0.009(3) 0.013(4) O3 0.040(4) 0.046(4) 0.050(4) -0.014(4) 0.007(3) 0.001(3) O4 0.039(4) 0.042(4) 0.055(5) 0.002(4) -0.004(3) -0.001(3) O5 0.050(4) 0.037(4) 0.053(4) -0.010(4) 0.005(3) -0.010(3) O6 0.057(4) 0.042(4) 0.042(4) -0.023(4) -0.007(3) 0.005(3) O7 0.046(4) 0.036(4) 0.056(5) -0.009(4) -0.015(3) -0.007(3) O8 0.038(4) 0.052(5) 0.050(4) -0.027(4) -0.004(3) 0.006(3) P1 0.0353(14) 0.0367(14) 0.0361(14) -0.0103(11) -0.0009(11) -0.0019(11) P2 0.0357(13) 0.0339(14) 0.0333(13) -0.0097(11) 0.0004(10) -0.0041(10) Pb1 0.0378(2) 0.0229(2) 0.0369(2) -0.01020(15) -0.00031(15) -0.00193(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 N1 1.314(14) . ? C1 C2 1.382(16) . ? C2 C3 1.376(15) . ? C3 C4 1.380(15) . ? C3 C6 1.507(14) . ? C4 C5 1.372(16) . ? C5 N1 1.321(14) . ? C6 C7 1.350(17) . ? C6 C10 1.389(16) . ? C7 C8 1.368(17) . ? C8 N2 1.336(18) . ? C9 N2 1.328(17) . ? C9 C10 1.372(17) . ? C11 C12 1.36(2) . ? C11 C16 1.379(16) . ? C11 O2 1.403(13) . ? C12 C13 1.32(3) . ? C13 C14 1.39(3) . ? C14 C15 1.35(2) . ? C15 C16 1.363(18) . ? C17 C22 1.359(18) . ? C17 C18 1.352(17) . ? C17 O4 1.374(12) . ? C18 C19 1.397(19) . ? C19 C20 1.33(2) . ? C20 C21 1.40(2) . ? C21 C22 1.41(2) . ? C23 C24 1.362(15) . ? C23 C28 1.375(15) . ? C23 O7 1.408(13) . ? C24 C25 1.379(18) . ? C25 C26 1.37(2) . ? C26 C27 1.38(2) . ? C27 C28 1.390(18) . ? C29 C30 1.370(16) . ? C29 C34 1.367(17) . ? C29 O8 1.371(12) . ? C30 C31 1.39(2) . ? C31 C32 1.32(2) . ? C32 C33 1.38(2) . ? C33 C34 1.371(18) . ? N1 Pb1 2.529(9) . ? O1 P1 1.466(7) . ? O1 Pb1 2.561(7) . ? O2 P1 1.574(8) . ? O3 P1 1.505(7) . ? O3 Pb1 2.457(7) 2_557 ? O4 P1 1.621(8) . ? O5 P2 1.501(7) . ? O5 Pb1 2.534(7) . ? O6 P2 1.476(7) . ? O6 Pb1 2.448(7) 2_657 ? O7 P2 1.592(8) . ? O8 P2 1.616(7) . ? Pb1 O6 2.448(7) 2_657 ? Pb1 O3 2.457(7) 2_557 ? 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 N1 C1 C2 122.6(11) . . ? C3 C2 C1 119.1(10) . . ? C2 C3 C4 118.5(10) . . ? C2 C3 C6 120.8(10) . . ? C4 C3 C6 120.7(10) . . ? C5 C4 C3 117.8(11) . . ? N1 C5 C4 124.1(11) . . ? C7 C6 C10 117.5(11) . . ? C7 C6 C3 122.1(12) . . ? C10 C6 C3 120.4(11) . . ? C6 C7 C8 120.0(13) . . ? N2 C8 C7 124.6(14) . . ? N2 C9 C10 125.4(13) . . ? C9 C10 C6 118.2(13) . . ? C12 C11 C16 120.4(13) . . ? C12 C11 O2 118.3(11) . . ? C16 C11 O2 121.2(11) . . ? C13 C12 C11 119.7(16) . . ? C12 C13 C14 122(2) . . ? C15 C14 C13 117.8(16) . . ? C14 C15 C16 121.7(14) . . ? C15 C16 C11 118.2(13) . . ? C22 C17 C18 121.8(12) . . ? C22 C17 O4 118.8(11) . . ? C18 C17 O4 119.2(11) . . ? C17 C18 C19 119.6(14) . . ? C20 C19 C18 119.1(14) . . ? C19 C20 C21 123.0(16) . . ? C20 C21 C22 116.9(15) . . ? C17 C22 C21 119.5(13) . . ? C24 C23 C28 121.9(11) . . ? C24 C23 O7 116.2(9) . . ? C28 C23 O7 121.9(10) . . ? C23 C24 C25 119.5(11) . . ? C26 C25 C24 119.8(13) . . ? C25 C26 C27 120.6(13) . . ? C26 C27 C28 119.7(13) . . ? C23 C28 C27 118.5(12) . . ? C30 C29 C34 119.1(11) . . ? C30 C29 O8 120.7(11) . . ? C34 C29 O8 120.0(10) . . ? C29 C30 C31 118.5(13) . . ? C32 C31 C30 122.4(13) . . ? C31 C32 C33 119.5(14) . . ? C34 C33 C32 119.5(14) . . ? C29 C34 C33 120.9(12) . . ? C1 N1 C5 117.9(10) . . ? C1 N1 Pb1 120.7(7) . . ? C5 N1 Pb1 121.2(7) . . ? C9 N2 C8 114.3(12) . . ? P1 O1 Pb1 120.7(4) . . ? C11 O2 P1 123.4(7) . . ? P1 O3 Pb1 118.8(4) . 2_557 ? C17 O4 P1 123.0(6) . . ? P2 O5 Pb1 121.2(4) . . ? P2 O6 Pb1 131.5(4) . 2_657 ? C23 O7 P2 121.7(6) . . ? C29 O8 P2 122.1(6) . . ? O1 P1 O3 119.4(4) . . ? O1 P1 O2 112.6(5) . . ? O3 P1 O2 106.4(4) . . ? O1 P1 O4 104.6(4) . . ? O3 P1 O4 108.4(4) . . ? O2 P1 O4 104.5(4) . . ? O6 P2 O5 119.2(4) . . ? O6 P2 O7 109.7(4) . . ? O5 P2 O7 106.3(4) . . ? O6 P2 O8 107.0(4) . . ? O5 P2 O8 108.8(4) . . ? O7 P2 O8 104.9(4) . . ? O6 Pb1 O3 81.5(2) 2_657 2_557 ? O6 Pb1 N1 80.5(3) 2_657 . ? O3 Pb1 N1 77.7(3) 2_557 . ? O6 Pb1 O5 90.2(2) 2_657 . ? O3 Pb1 O5 153.8(3) 2_557 . ? N1 Pb1 O5 76.4(3) . . ? O6 Pb1 O1 159.0(3) 2_657 . ? O3 Pb1 O1 89.2(2) 2_557 . ? N1 Pb1 O1 79.2(3) . . ? O5 Pb1 O1 90.0(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 8.141 _refine_diff_density_min -2.457 _refine_diff_density_rms 0.312 data_complex9 _database_code_depnum_ccdc_archive 'CCDC 898358' #TrackingRef 'web_deposit_cif_file_8_DebajyotiGhoshal_1346073361.complex9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H50 N4 O9 P2 Zn' _chemical_formula_weight 978.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' _cell_length_a 13.7022(3) _cell_length_b 18.4230(3) _cell_length_c 19.8629(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.3670(10) _cell_angle_gamma 90.00 _cell_volume 4730.37(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39325 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8276 _exptl_absorpt_correction_T_max 0.8878 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39325 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.61 _reflns_number_total 5462 _reflns_number_gt 4646 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+2.2574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5462 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.0000 0.0000 0.5000 0.02873(8) Uani 1 2 d S . . O1 O 1.11661(8) -0.02406(6) 0.45398(6) 0.0359(2) Uani 1 1 d . . . N1 N 1.01155(9) -0.10929(6) 0.54137(6) 0.0320(3) Uani 1 1 d . . . C3 C 1.01341(11) -0.25131(8) 0.59350(8) 0.0356(3) Uani 1 1 d . . . C7 C 1.11317(13) -0.34383(9) 0.68321(9) 0.0441(4) Uani 1 1 d . . . H7A H 1.1728 -0.3312 0.6697 0.053 Uiso 1 1 calc R . . H7B H 1.1142 -0.3135 0.7234 0.053 Uiso 1 1 calc R . . C2 C 1.02128(12) -0.23781(8) 0.52695(9) 0.0386(3) Uani 1 1 d . . . H2 H 1.0273 -0.2762 0.4982 0.046 Uiso 1 1 calc R . . C6 C 1.01518(13) -0.32786(9) 0.62090(9) 0.0440(4) Uani 1 1 d . . . H6A H 1.0102 -0.3617 0.5825 0.053 Uiso 1 1 calc R . . H6B H 0.9555 -0.3352 0.6360 0.053 Uiso 1 1 calc R . . C1 C 1.02024(12) -0.16738(8) 0.50338(8) 0.0369(3) Uani 1 1 d . . . H1 H 1.0259 -0.1598 0.4585 0.044 Uiso 1 1 calc R . . C8 C 1.12171(12) -0.42252(8) 0.70619(8) 0.0377(3) Uani 1 1 d . . . H8A H 1.0574 -0.4370 0.7128 0.045 Uiso 1 1 calc R . . H8B H 1.1304 -0.4521 0.6682 0.045 Uiso 1 1 calc R . . C4 C 1.00608(14) -0.19110(9) 0.63341(9) 0.0436(4) Uani 1 1 d . . . H4 H 1.0017 -0.1972 0.6788 0.052 Uiso 1 1 calc R . . C5 C 1.00531(13) -0.12243(9) 0.60616(8) 0.0390(3) Uani 1 1 d . . . H5 H 1.0002 -0.0831 0.6341 0.047 Uiso 1 1 calc R . . P1 P 1.17264(3) -0.05304(2) 0.407369(19) 0.03051(10) Uani 1 1 d . . . O3 O 1.17585(10) 0.00572(6) 0.34873(6) 0.0417(3) Uani 1 1 d . . . O2 O 1.13745(10) -0.12159(6) 0.36908(6) 0.0443(3) Uani 1 1 d . . . O4 O 1.29491(8) -0.05523(6) 0.45114(6) 0.0408(3) Uani 1 1 d . . . C15 C 1.29580(13) -0.15490(9) 0.53174(10) 0.0441(4) Uani 1 1 d . . . H15 H 1.2316 -0.1713 0.5025 0.053 Uiso 1 1 calc R . . C10 C 1.30767(12) -0.41005(9) 0.78579(8) 0.0374(3) Uani 1 1 d . . . H10 H 1.3201 -0.3800 0.7519 0.045 Uiso 1 1 calc R . . C14 C 1.34050(12) -0.09448(8) 0.51320(8) 0.0352(3) Uani 1 1 d . . . C9 C 1.20974(11) -0.43775(8) 0.77394(8) 0.0325(3) Uani 1 1 d . . . C13 C 1.19778(13) -0.48158(11) 0.82695(10) 0.0515(5) Uani 1 1 d . . . H13 H 1.1336 -0.5019 0.8218 0.062 Uiso 1 1 calc R . . C11 C 1.38710(12) -0.42676(9) 0.84768(8) 0.0360(3) Uani 1 1 d . . . H11 H 1.4524 -0.4079 0.8537 0.043 Uiso 1 1 calc R . . C12 C 1.28073(14) -0.49533(10) 0.88753(10) 0.0521(5) Uani 1 1 d . . . H12 H 1.2701 -0.5251 0.9222 0.062 Uiso 1 1 calc R . . C20 C 1.21348(12) 0.07607(9) 0.36018(10) 0.0428(4) Uani 1 1 d . . . C19 C 1.43602(13) -0.07050(10) 0.55613(10) 0.0462(4) Uani 1 1 d . . . H19 H 1.4656 -0.0296 0.5433 0.055 Uiso 1 1 calc R . . C16 C 1.34809(17) -0.19075(10) 0.59465(11) 0.0557(5) Uani 1 1 d . . . H16 H 1.3181 -0.2311 0.6080 0.067 Uiso 1 1 calc R . . C17 C 1.44376(17) -0.16744(11) 0.63765(11) 0.0609(5) Uani 1 1 d . . . H17 H 1.4785 -0.1921 0.6796 0.073 Uiso 1 1 calc R . . C21 C 1.21436(16) 0.11204(11) 0.29931(12) 0.0615(5) Uani 1 1 d . . . H21 H 1.1917 0.0890 0.2552 0.074 Uiso 1 1 calc R . . C18 C 1.48766(16) -0.10735(11) 0.61816(11) 0.0584(5) Uani 1 1 d . . . H18 H 1.5525 -0.0915 0.6470 0.070 Uiso 1 1 calc R . . C25 C 1.24696(14) 0.10927(10) 0.42571(12) 0.0542(5) Uani 1 1 d . . . H25 H 1.2466 0.0846 0.4665 0.065 Uiso 1 1 calc R . . C22 C 1.2495(2) 0.18305(14) 0.30510(18) 0.0899(9) Uani 1 1 d . . . H22 H 1.2507 0.2078 0.2646 0.108 Uiso 1 1 calc R . . N2 N 1.37531(10) -0.46854(7) 0.89942(6) 0.0343(3) Uani 1 1 d . . . C24 C 1.28140(17) 0.18069(12) 0.42978(16) 0.0751(7) Uani 1 1 d . . . H24 H 1.3041 0.2040 0.4738 0.090 Uiso 1 1 calc R . . C23 C 1.2823(2) 0.21711(13) 0.3699(2) 0.0958(10) Uani 1 1 d . . . H23 H 1.3053 0.2649 0.3733 0.115 Uiso 1 1 calc R . . O1W O 1.0000 -0.19536(13) 0.2500 0.0780(8) Uani 1 2 d S . . H1W H 1.035(2) -0.1686(13) 0.2830(13) 0.084(8) Uiso 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 Zn1 0.03284(13) 0.02588(12) 0.02504(12) -0.00218(8) 0.00634(9) -0.00075(8) O1 0.0368(5) 0.0392(6) 0.0325(5) -0.0037(4) 0.0128(4) 0.0017(4) N1 0.0334(6) 0.0299(6) 0.0308(6) 0.0012(5) 0.0079(5) 0.0015(5) C3 0.0305(7) 0.0334(8) 0.0357(8) 0.0079(6) 0.0011(6) 0.0025(6) C7 0.0432(9) 0.0353(8) 0.0422(9) 0.0093(7) -0.0015(7) 0.0009(7) C2 0.0445(9) 0.0310(7) 0.0378(8) -0.0019(6) 0.0100(7) 0.0013(6) C6 0.0429(9) 0.0360(8) 0.0431(9) 0.0121(7) 0.0007(7) 0.0003(6) C1 0.0450(9) 0.0343(8) 0.0314(8) -0.0002(6) 0.0127(7) -0.0006(6) C8 0.0353(8) 0.0373(8) 0.0340(8) 0.0097(6) 0.0026(6) -0.0007(6) C4 0.0557(10) 0.0439(9) 0.0311(8) 0.0091(7) 0.0143(7) 0.0094(7) C5 0.0471(9) 0.0373(8) 0.0316(8) 0.0004(6) 0.0116(7) 0.0087(6) P1 0.03341(19) 0.03084(19) 0.02688(18) -0.00089(14) 0.00947(15) -0.00014(14) O3 0.0538(7) 0.0396(6) 0.0313(6) 0.0042(4) 0.0135(5) -0.0031(5) O2 0.0561(7) 0.0361(6) 0.0401(6) -0.0082(5) 0.0152(5) -0.0029(5) O4 0.0332(6) 0.0444(6) 0.0440(6) 0.0106(5) 0.0119(5) 0.0015(4) C15 0.0432(9) 0.0373(8) 0.0499(10) 0.0021(7) 0.0128(8) -0.0007(7) C10 0.0366(8) 0.0426(9) 0.0320(8) 0.0117(6) 0.0099(6) -0.0009(6) C14 0.0353(8) 0.0346(8) 0.0365(8) 0.0000(6) 0.0131(6) 0.0064(6) C9 0.0337(7) 0.0308(7) 0.0298(7) 0.0065(6) 0.0063(6) 0.0027(6) C13 0.0341(8) 0.0673(12) 0.0465(10) 0.0252(9) 0.0046(7) -0.0095(8) C11 0.0323(7) 0.0409(8) 0.0331(8) 0.0070(6) 0.0086(6) -0.0025(6) C12 0.0423(9) 0.0673(12) 0.0410(10) 0.0274(8) 0.0062(8) -0.0092(8) C20 0.0341(8) 0.0377(8) 0.0533(10) 0.0115(7) 0.0102(7) 0.0035(6) C19 0.0414(9) 0.0439(9) 0.0506(10) 0.0000(8) 0.0117(8) -0.0013(7) C16 0.0714(13) 0.0410(10) 0.0549(11) 0.0112(8) 0.0213(10) 0.0020(9) C17 0.0727(14) 0.0583(12) 0.0423(10) 0.0082(9) 0.0066(10) 0.0146(10) C21 0.0584(12) 0.0568(12) 0.0662(13) 0.0284(10) 0.0167(10) 0.0090(9) C18 0.0506(11) 0.0616(12) 0.0492(11) -0.0032(9) -0.0017(9) 0.0049(9) C25 0.0471(10) 0.0443(10) 0.0651(12) 0.0004(9) 0.0105(9) -0.0053(8) C22 0.0809(17) 0.0668(16) 0.116(2) 0.0530(16) 0.0250(17) 0.0032(13) N2 0.0340(6) 0.0367(7) 0.0292(6) 0.0068(5) 0.0065(5) 0.0007(5) C24 0.0565(12) 0.0482(12) 0.1053(19) -0.0079(12) 0.0062(13) -0.0089(9) C23 0.0733(16) 0.0442(13) 0.153(3) 0.0283(16) 0.0157(18) -0.0086(11) O1W 0.1063(19) 0.0476(12) 0.0546(13) 0.000 -0.0076(13) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 Zn1 O1 2.1339(10) . ? Zn1 O1 2.1339(10) 5_756 ? Zn1 N1 2.1607(12) . ? Zn1 N1 2.1607(12) 5_756 ? Zn1 N2 2.2322(12) 8_445 ? Zn1 N2 2.2322(12) 4_756 ? O1 P1 1.4843(11) . ? N1 C1 1.3373(19) . ? N1 C5 1.3398(19) . ? C3 C2 1.384(2) . ? C3 C4 1.386(2) . ? C3 C6 1.509(2) . ? C7 C8 1.513(2) . ? C7 C6 1.523(2) . ? C2 C1 1.378(2) . ? C8 C9 1.506(2) . ? C4 C5 1.375(2) . ? P1 O2 1.4707(11) . ? P1 O3 1.6013(11) . ? P1 O4 1.6119(11) . ? O3 C20 1.386(2) . ? O4 C14 1.3863(18) . ? C15 C14 1.378(2) . ? C15 C16 1.385(2) . ? C10 C11 1.380(2) . ? C10 C9 1.381(2) . ? C14 C19 1.377(2) . ? C9 C13 1.379(2) . ? C13 C12 1.377(2) . ? C11 N2 1.3359(19) . ? C12 N2 1.333(2) . ? C20 C25 1.372(3) . ? C20 C21 1.382(3) . ? C19 C18 1.379(3) . ? C16 C17 1.375(3) . ? C17 C18 1.375(3) . ? C21 C22 1.385(3) . ? C25 C24 1.391(3) . ? C22 C23 1.366(4) . ? N2 Zn1 2.2322(12) 4_746 ? C24 C23 1.370(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 O1 Zn1 O1 180.0 . 5_756 ? O1 Zn1 N1 89.92(4) . . ? O1 Zn1 N1 90.08(4) 5_756 . ? O1 Zn1 N1 90.08(4) . 5_756 ? O1 Zn1 N1 89.92(4) 5_756 5_756 ? N1 Zn1 N1 180.000(1) . 5_756 ? O1 Zn1 N2 91.28(4) . 8_445 ? O1 Zn1 N2 88.72(4) 5_756 8_445 ? N1 Zn1 N2 92.07(5) . 8_445 ? N1 Zn1 N2 87.93(5) 5_756 8_445 ? O1 Zn1 N2 88.72(4) . 4_756 ? O1 Zn1 N2 91.28(4) 5_756 4_756 ? N1 Zn1 N2 87.93(5) . 4_756 ? N1 Zn1 N2 92.07(5) 5_756 4_756 ? N2 Zn1 N2 180.0 8_445 4_756 ? P1 O1 Zn1 163.25(7) . . ? C1 N1 C5 116.32(13) . . ? C1 N1 Zn1 122.69(10) . . ? C5 N1 Zn1 120.91(10) . . ? C2 C3 C4 116.48(14) . . ? C2 C3 C6 121.03(15) . . ? C4 C3 C6 122.48(15) . . ? C8 C7 C6 112.93(13) . . ? C1 C2 C3 119.90(15) . . ? C3 C6 C7 112.22(13) . . ? N1 C1 C2 123.69(14) . . ? C9 C8 C7 114.03(13) . . ? C5 C4 C3 120.25(15) . . ? N1 C5 C4 123.35(15) . . ? O2 P1 O1 118.87(7) . . ? O2 P1 O3 106.72(6) . . ? O1 P1 O3 110.81(6) . . ? O2 P1 O4 111.18(7) . . ? O1 P1 O4 109.43(6) . . ? O3 P1 O4 97.76(6) . . ? C20 O3 P1 127.70(11) . . ? C14 O4 P1 125.03(10) . . ? C14 C15 C16 118.92(17) . . ? C11 C10 C9 120.27(14) . . ? C19 C14 C15 120.61(15) . . ? C19 C14 O4 116.04(14) . . ? C15 C14 O4 123.34(14) . . ? C13 C9 C10 116.17(14) . . ? C13 C9 C8 121.91(14) . . ? C10 C9 C8 121.90(13) . . ? C12 C13 C9 120.14(16) . . ? N2 C11 C10 123.59(14) . . ? N2 C12 C13 123.99(15) . . ? C25 C20 C21 121.26(18) . . ? C25 C20 O3 124.18(16) . . ? C21 C20 O3 114.56(17) . . ? C14 C19 C18 119.74(17) . . ? C17 C16 C15 120.88(18) . . ? C16 C17 C18 119.50(18) . . ? C20 C21 C22 118.9(2) . . ? C17 C18 C19 120.34(18) . . ? C20 C25 C24 118.5(2) . . ? C23 C22 C21 120.6(2) . . ? C12 N2 C11 115.82(13) . . ? C12 N2 Zn1 118.24(10) . 4_746 ? C11 N2 Zn1 125.89(10) . 4_746 ? C23 C24 C25 120.9(2) . . ? C22 C23 C24 119.9(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.221 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.054 data_complex10 _database_code_depnum_ccdc_archive 'CCDC 898359' #TrackingRef 'web_deposit_cif_file_9_DebajyotiGhoshal_1346073361.complex10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 Cd N4 O8 P2' _chemical_formula_weight 1007.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.010(3) _cell_length_b 11.104(3) _cell_length_c 11.500(3) _cell_angle_alpha 63.251(12) _cell_angle_beta 65.029(12) _cell_angle_gamma 83.120(13) _cell_volume 1133.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16819 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.7 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 518 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8277 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details ; 'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL SPACE EXPLORATION, Bruker Analytical X-ray Systems, 1997 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16819 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.67 _reflns_number_total 5198 _reflns_number_gt 4896 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART APEX II (Bruker,2010)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SAINT (Bruker,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3v2 for windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.2467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5198 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6438(3) 0.4458(3) 0.7207(3) 0.0416(5) Uani 1 1 d . . . H1 H 0.5647 0.4777 0.7661 0.050 Uiso 1 1 calc R . . C2 C 0.7352(3) 0.4062(3) 0.7818(3) 0.0443(6) Uani 1 1 d . . . H2 H 0.7180 0.4141 0.8644 0.053 Uiso 1 1 calc R . . C3 C 0.8518(2) 0.3551(2) 0.7200(3) 0.0391(5) Uani 1 1 d . . . C4 C 0.8733(3) 0.3509(3) 0.5946(3) 0.0469(6) Uani 1 1 d . . . H4 H 0.9514 0.3187 0.5481 0.056 Uiso 1 1 calc R . . C5 C 0.7785(3) 0.3948(3) 0.5383(3) 0.0439(6) Uani 1 1 d . . . H5 H 0.7961 0.3923 0.4529 0.053 Uiso 1 1 calc R . . C6 C 0.9476(3) 0.3041(3) 0.7919(3) 0.0494(6) Uani 1 1 d . . . H6A H 0.9774 0.3775 0.8002 0.059 Uiso 1 1 calc R . . H6B H 1.0261 0.2759 0.7326 0.059 Uiso 1 1 calc R . . C7 C 0.8816(3) 0.1831(3) 0.9435(3) 0.0442(6) Uani 1 1 d . . . H7A H 0.9378 0.1669 0.9944 0.053 Uiso 1 1 calc R . . H7B H 0.7945 0.2047 0.9978 0.053 Uiso 1 1 calc R . . C8 C 0.8652(3) 0.0588(3) 0.9299(3) 0.0468(6) Uani 1 1 d . . . H8A H 0.9540 0.0361 0.8807 0.056 Uiso 1 1 calc R . . H8B H 0.8178 0.0808 0.8693 0.056 Uiso 1 1 calc R . . C9 C 0.7911(2) -0.0671(3) 1.0682(3) 0.0397(5) Uani 1 1 d . . . C10 C 0.7334(3) -0.0769(3) 1.2052(3) 0.0448(6) Uani 1 1 d . . . H10 H 0.7409 -0.0028 1.2198 0.054 Uiso 1 1 calc R . . C11 C 0.6641(3) -0.1978(3) 1.3211(3) 0.0437(6) Uani 1 1 d . . . H11 H 0.6269 -0.2019 1.4121 0.052 Uiso 1 1 calc R . . C12 C 0.7069(3) -0.2981(3) 1.1761(3) 0.0423(5) Uani 1 1 d . . . H12 H 0.6988 -0.3735 1.1637 0.051 Uiso 1 1 calc R . . C13 C 0.7788(3) -0.1829(3) 1.0568(3) 0.0470(6) Uani 1 1 d . . . H13 H 0.8194 -0.1831 0.9678 0.056 Uiso 1 1 calc R . . C14 C 0.8613(2) 0.2321(3) 0.2674(3) 0.0404(5) Uani 1 1 d . . . C15 C 0.9338(3) 0.3569(4) 0.1850(4) 0.0599(8) Uani 1 1 d . . . H15 H 0.8969 0.4327 0.1373 0.072 Uiso 1 1 calc R . . C16 C 1.0639(3) 0.3676(6) 0.1742(6) 0.0861(15) Uani 1 1 d . . . H16 H 1.1136 0.4514 0.1184 0.103 Uiso 1 1 calc R . . C17 C 1.1186(4) 0.2585(6) 0.2431(5) 0.0889(16) Uani 1 1 d . . . H17 H 1.2040 0.2675 0.2377 0.107 Uiso 1 1 calc R . . C18 C 1.0455(4) 0.1323(6) 0.3226(4) 0.0937(17) Uani 1 1 d . . . H18 H 1.0835 0.0560 0.3677 0.112 Uiso 1 1 calc R . . C19 C 0.9176(3) 0.1202(4) 0.3345(3) 0.0648(9) Uani 1 1 d . . . H19 H 0.8690 0.0359 0.3882 0.078 Uiso 1 1 calc R . . C40 C 0.4665(2) 0.1605(2) 0.2813(2) 0.0336(5) Uani 1 1 d . . . C41 C 0.4145(3) 0.0281(3) 0.3741(3) 0.0477(6) Uani 1 1 d . . . H41 H 0.4016 -0.0086 0.4693 0.057 Uiso 1 1 calc R . . C42 C 0.3821(3) -0.0492(4) 0.3231(5) 0.0641(9) Uani 1 1 d . . . H42 H 0.3453 -0.1381 0.3850 0.077 Uiso 1 1 calc R . . C43 C 0.4036(3) 0.0036(5) 0.1831(5) 0.0703(11) Uani 1 1 d . . . H43 H 0.3839 -0.0499 0.1490 0.084 Uiso 1 1 calc R . . C44 C 0.4853(3) 0.2174(3) 0.1406(3) 0.0494(6) Uani 1 1 d . . . H44 H 0.5179 0.3076 0.0798 0.059 Uiso 1 1 calc R . . C45 C 0.4545(4) 0.1368(5) 0.0918(4) 0.0691(10) Uani 1 1 d . . . H45 H 0.4683 0.1727 -0.0036 0.083 Uiso 1 1 calc R . . N1 N 0.6625(2) 0.4408(2) 0.6002(2) 0.0372(4) Uani 1 1 d . . . N2 N 0.6479(2) -0.3086(2) 1.3088(2) 0.0349(4) Uani 1 1 d . . . O1 O 0.61034(18) 0.37892(19) 0.37544(19) 0.0426(4) Uani 1 1 d . . . O2 O 0.73155(17) 0.21099(18) 0.2850(2) 0.0399(4) Uani 1 1 d . . . O3 O 0.49335(16) 0.23380(17) 0.33993(17) 0.0363(4) Uani 1 1 d . . . O4 O 0.6652(2) 0.42423(19) 0.11972(19) 0.0472(4) Uani 1 1 d . . . P1 P 0.62893(6) 0.32840(6) 0.27027(6) 0.03065(13) Uani 1 1 d . . . Cd1 Cd 0.5000 0.5000 0.5000 0.02876(9) Uani 1 2 d S . . 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 0.0405(13) 0.0441(13) 0.0399(12) -0.0176(11) -0.0191(10) 0.0090(10) C2 0.0464(14) 0.0466(14) 0.0398(12) -0.0145(11) -0.0229(11) 0.0042(11) C3 0.0355(12) 0.0277(11) 0.0436(12) -0.0030(9) -0.0195(10) -0.0037(9) C4 0.0354(12) 0.0398(13) 0.0566(15) -0.0192(12) -0.0142(11) 0.0047(10) C5 0.0408(13) 0.0473(14) 0.0451(13) -0.0231(12) -0.0161(11) 0.0022(11) C6 0.0393(13) 0.0358(13) 0.0597(16) -0.0038(12) -0.0261(12) -0.0027(10) C7 0.0458(14) 0.0386(13) 0.0489(14) -0.0150(11) -0.0256(11) 0.0057(10) C8 0.0527(15) 0.0390(13) 0.0414(13) -0.0109(11) -0.0187(12) -0.0037(11) C9 0.0342(12) 0.0347(12) 0.0416(12) -0.0068(10) -0.0180(10) -0.0018(9) C10 0.0435(14) 0.0328(12) 0.0554(15) -0.0214(11) -0.0148(11) -0.0020(10) C11 0.0439(13) 0.0419(13) 0.0396(12) -0.0217(11) -0.0063(10) -0.0046(10) C12 0.0509(14) 0.0372(13) 0.0361(11) -0.0147(10) -0.0153(10) -0.0041(10) C13 0.0548(16) 0.0457(15) 0.0329(12) -0.0124(11) -0.0139(11) -0.0085(12) C14 0.0326(11) 0.0527(15) 0.0409(12) -0.0289(12) -0.0123(9) 0.0097(10) C15 0.0371(14) 0.0625(19) 0.084(2) -0.0451(18) -0.0148(14) 0.0010(13) C16 0.0370(16) 0.126(4) 0.121(4) -0.092(3) -0.012(2) -0.004(2) C17 0.0373(17) 0.170(5) 0.090(3) -0.087(4) -0.0260(19) 0.025(2) C18 0.053(2) 0.161(5) 0.056(2) -0.044(3) -0.0275(17) 0.047(3) C19 0.0442(16) 0.082(2) 0.0439(15) -0.0171(15) -0.0130(12) 0.0196(15) C40 0.0227(9) 0.0435(12) 0.0393(11) -0.0236(10) -0.0114(8) 0.0026(8) C41 0.0445(14) 0.0454(15) 0.0559(15) -0.0213(13) -0.0227(12) -0.0027(11) C42 0.0517(17) 0.0537(18) 0.100(3) -0.0445(19) -0.0305(17) 0.0002(14) C43 0.0486(17) 0.101(3) 0.104(3) -0.078(3) -0.0335(18) 0.0090(17) C44 0.0422(14) 0.0659(18) 0.0406(13) -0.0228(13) -0.0161(11) -0.0045(12) C45 0.0539(18) 0.117(3) 0.0579(18) -0.056(2) -0.0229(15) 0.0020(19) N1 0.0395(10) 0.0327(10) 0.0378(10) -0.0117(8) -0.0187(8) 0.0022(8) N2 0.0368(10) 0.0295(9) 0.0332(9) -0.0109(8) -0.0124(8) -0.0009(7) O1 0.0445(10) 0.0424(10) 0.0498(10) -0.0308(9) -0.0161(8) 0.0032(8) O2 0.0360(9) 0.0353(9) 0.0519(10) -0.0236(8) -0.0175(8) 0.0065(7) O3 0.0326(8) 0.0417(9) 0.0318(8) -0.0192(7) -0.0055(6) -0.0056(7) O4 0.0484(10) 0.0436(10) 0.0366(9) -0.0075(8) -0.0142(8) -0.0091(8) P1 0.0313(3) 0.0276(3) 0.0318(3) -0.0144(2) -0.0102(2) 0.0006(2) Cd1 0.03147(14) 0.02571(13) 0.02729(13) -0.01046(9) -0.01107(9) -0.00125(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 N1 1.339(3) . ? C1 C2 1.383(4) . ? C2 C3 1.376(4) . ? C3 C4 1.380(4) . ? C3 C6 1.513(4) . ? C4 C5 1.382(4) . ? C5 N1 1.342(3) . ? C6 C7 1.559(4) . ? C7 C8 1.498(4) . ? C8 C9 1.525(3) . ? C9 C13 1.377(4) . ? C9 C10 1.383(4) . ? C10 C11 1.391(4) . ? C11 N2 1.340(3) . ? C12 N2 1.336(3) . ? C12 C13 1.376(4) . ? C14 C19 1.370(4) . ? C14 C15 1.379(4) . ? C14 O2 1.389(3) . ? C15 C16 1.399(5) . ? C16 C17 1.350(7) . ? C17 C18 1.394(8) . ? C18 C19 1.374(5) . ? C40 C44 1.374(4) . ? C40 C41 1.379(4) . ? C40 O3 1.387(3) . ? C41 C42 1.383(4) . ? C42 C43 1.361(6) . ? C43 C45 1.381(6) . ? C44 C45 1.385(4) . ? N1 Cd1 2.395(2) . ? N2 Cd1 2.367(2) 1_546 ? O1 P1 1.4811(16) . ? O1 Cd1 2.2821(16) . ? O2 P1 1.6170(18) . ? O3 P1 1.6068(17) . ? O4 P1 1.4659(19) . ? Cd1 O1 2.2821(16) 2_666 ? Cd1 N2 2.367(2) 2_657 ? Cd1 N2 2.367(2) 1_564 ? Cd1 N1 2.395(2) 2_666 ? 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 N1 C1 C2 123.8(2) . . ? C3 C2 C1 119.8(2) . . ? C2 C3 C4 117.0(2) . . ? C2 C3 C6 119.7(2) . . ? C4 C3 C6 123.4(2) . . ? C3 C4 C5 120.0(2) . . ? N1 C5 C4 123.5(2) . . ? C3 C6 C7 112.3(2) . . ? C8 C7 C6 109.8(2) . . ? C7 C8 C9 117.0(2) . . ? C13 C9 C10 116.2(2) . . ? C13 C9 C8 117.3(2) . . ? C10 C9 C8 126.5(2) . . ? C9 C10 C11 119.9(2) . . ? N2 C11 C10 123.7(2) . . ? N2 C12 C13 124.1(2) . . ? C12 C13 C9 120.5(2) . . ? C19 C14 C15 120.2(3) . . ? C19 C14 O2 116.5(3) . . ? C15 C14 O2 123.3(3) . . ? C14 C15 C16 118.9(4) . . ? C17 C16 C15 121.2(4) . . ? C16 C17 C18 119.2(4) . . ? C19 C18 C17 120.3(4) . . ? C14 C19 C18 120.2(4) . . ? C44 C40 C41 121.7(2) . . ? C44 C40 O3 122.2(2) . . ? C41 C40 O3 116.0(2) . . ? C40 C41 C42 118.8(3) . . ? C43 C42 C41 120.6(3) . . ? C42 C43 C45 119.9(3) . . ? C40 C44 C45 118.2(3) . . ? C43 C45 C44 120.7(3) . . ? C1 N1 C5 115.9(2) . . ? C1 N1 Cd1 123.83(17) . . ? C5 N1 Cd1 120.26(17) . . ? C12 N2 C11 115.5(2) . . ? C12 N2 Cd1 120.83(16) . 1_546 ? C11 N2 Cd1 123.04(16) . 1_546 ? P1 O1 Cd1 151.49(12) . . ? C14 O2 P1 123.06(16) . . ? C40 O3 P1 125.35(14) . . ? O4 P1 O1 119.90(12) . . ? O4 P1 O3 112.80(10) . . ? O1 P1 O3 104.36(9) . . ? O4 P1 O2 110.97(11) . . ? O1 P1 O2 108.36(11) . . ? O3 P1 O2 98.08(10) . . ? O1 Cd1 O1 180.0 . 2_666 ? O1 Cd1 N2 91.76(7) . 2_657 ? O1 Cd1 N2 88.24(7) 2_666 2_657 ? O1 Cd1 N2 88.24(7) . 1_564 ? O1 Cd1 N2 91.76(7) 2_666 1_564 ? N2 Cd1 N2 180.00(9) 2_657 1_564 ? O1 Cd1 N1 87.28(7) . . ? O1 Cd1 N1 92.72(7) 2_666 . ? N2 Cd1 N1 91.98(7) 2_657 . ? N2 Cd1 N1 88.02(7) 1_564 . ? O1 Cd1 N1 92.72(7) . 2_666 ? O1 Cd1 N1 87.28(7) 2_666 2_666 ? N2 Cd1 N1 88.02(7) 2_657 2_666 ? N2 Cd1 N1 91.98(7) 1_564 2_666 ? N1 Cd1 N1 180.0 . 2_666 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.843 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.094