Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sylviane Sabo-Etienne' _publ_contact_author_address ; Laboratoire de Chimie de Coordination CNRS 205, route de Narbonne Toulouse Cedex 04 31077 FRANCE ; _publ_contact_author_email SABO@LCC-TOULOUSE.FR _publ_section_title ; Heterometallic Werner complexes as energetic materials ; loop_ _publ_author_name 'Sylviane Sabo-Etienne' 'Bruno Chaudret' 'Guy Jacob' 'Caroline Pradere' 'Samuel Suhard' 'Laure Vendier' #----------------------------------------------------------------------------# data_caro1009 _database_code_depnum_ccdc_archive 'CCDC 668884' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C36 H30 N P2), Mn N4 O12' _chemical_formula_sum 'C72 H60 Mn N6 O12 P4' _chemical_formula_weight 1380.08 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 16.5893(14) _cell_length_b 20.3078(14) _cell_length_c 20.8751(14) _cell_angle_alpha 90 _cell_angle_beta 109.607(7) _cell_angle_gamma 90 _cell_volume 6624.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180 _cell_measurement_reflns_used 5721 _cell_measurement_theta_min 2.7706 _cell_measurement_theta_max 32.2009 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.125 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2860 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8827 _exptl_absorpt_correction_T_max 0.959 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_number 22297 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 6042 _reflns_number_gt 4767 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2sigma(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^)+(0.1024P)^2^+8.5662P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 6042 _refine_ls_number_parameters 423 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.059 _refine_ls_wR_factor_ref 0.1765 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.034 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.56067(19) 0.23336(15) 0.92058(15) 0.0229(7) Uani 1 1 d . . . C2 C 0.6326(2) 0.27045(16) 0.95475(17) 0.0272(7) Uani 1 1 d . . . H2 H 0.6754 0.2524 0.9916 0.033 Uiso 1 1 calc R . . C3 C 0.6407(2) 0.33414(17) 0.93420(19) 0.0334(8) Uani 1 1 d . . . H3 H 0.6892 0.3587 0.9572 0.04 Uiso 1 1 calc R . . C4 C 0.5772(2) 0.36145(18) 0.8797(2) 0.0379(9) Uani 1 1 d . . . H4 H 0.583 0.4042 0.8658 0.045 Uiso 1 1 calc R . . C5 C 0.5059(3) 0.32534(19) 0.84603(19) 0.0411(9) Uani 1 1 d . . . H5 H 0.4631 0.3437 0.8093 0.049 Uiso 1 1 calc R . . C6 C 0.4968(2) 0.26141(17) 0.86641(18) 0.0333(8) Uani 1 1 d . . . H6 H 0.4478 0.2374 0.8436 0.04 Uiso 1 1 calc R . . C7 C 0.46254(19) 0.11114(15) 0.89167(15) 0.0224(7) Uani 1 1 d . . . C8 C 0.3962(2) 0.08732(17) 0.91167(17) 0.0283(7) Uani 1 1 d . . . H8 H 0.3983 0.0924 0.9565 0.034 Uiso 1 1 calc R . . C9 C 0.3269(2) 0.05598(17) 0.86525(18) 0.0331(8) Uani 1 1 d . . . H9 H 0.2826 0.04 0.8789 0.04 Uiso 1 1 calc R . . C10 C 0.3237(2) 0.04849(17) 0.79852(18) 0.0332(8) Uani 1 1 d . . . H10 H 0.277 0.0278 0.7671 0.04 Uiso 1 1 calc R . . C11 C 0.3896(2) 0.07169(17) 0.77864(17) 0.0325(8) Uani 1 1 d . . . H11 H 0.3875 0.0663 0.7339 0.039 Uiso 1 1 calc R . . C12 C 0.4588(2) 0.10287(16) 0.82473(16) 0.0275(7) Uani 1 1 d . . . H12 H 0.5031 0.1184 0.8109 0.033 Uiso 1 1 calc R . . C13 C 0.64583(19) 0.10736(15) 0.94955(16) 0.0229(7) Uani 1 1 d . . . C14 C 0.6734(2) 0.05293(16) 0.99204(17) 0.0283(7) Uani 1 1 d . . . H14 H 0.6457 0.0415 1.0225 0.034 Uiso 1 1 calc R . . C15 C 0.7424(2) 0.01571(17) 0.98881(19) 0.0356(8) Uani 1 1 d . . . H15 H 0.7612 -0.0205 1.0172 0.043 Uiso 1 1 calc R . . C16 C 0.7829(2) 0.03280(18) 0.94340(19) 0.0344(8) Uani 1 1 d . . . H16 H 0.8288 0.0077 0.9412 0.041 Uiso 1 1 calc R . . C17 C 0.7562(2) 0.08676(18) 0.90097(18) 0.0329(8) Uani 1 1 d . . . H17 H 0.784 0.0978 0.8705 0.04 Uiso 1 1 calc R . . C18 C 0.6876(2) 0.12427(17) 0.90417(17) 0.0274(7) Uani 1 1 d . . . H18 H 0.6696 0.1607 0.876 0.033 Uiso 1 1 calc R . . C19 C 0.6168(2) 0.23297(16) 1.13602(15) 0.0241(7) Uani 1 1 d . . . C20 C 0.6125(2) 0.28575(16) 1.17759(17) 0.0279(7) Uani 1 1 d . . . H20 H 0.5607 0.307 1.1711 0.033 Uiso 1 1 calc R . . C21 C 0.6859(2) 0.30620(18) 1.22853(19) 0.0351(8) Uani 1 1 d . . . H21 H 0.6834 0.3413 1.2564 0.042 Uiso 1 1 calc R . . C22 C 0.7622(2) 0.2748(2) 1.23806(19) 0.0407(9) Uani 1 1 d . . . H22 H 0.8112 0.2891 1.2724 0.049 Uiso 1 1 calc R . . C23 C 0.7675(2) 0.2228(2) 1.1978(2) 0.0440(10) Uani 1 1 d . . . H23 H 0.8197 0.2019 1.2049 0.053 Uiso 1 1 calc R . . C24 C 0.6944(2) 0.20149(19) 1.14614(19) 0.0343(8) Uani 1 1 d . . . H24 H 0.6976 0.1663 1.1186 0.041 Uiso 1 1 calc R . . C25 C 0.46538(19) 0.15567(16) 1.11987(15) 0.0232(7) Uani 1 1 d . . . C26 C 0.4635(2) 0.08729(17) 1.11946(18) 0.0323(8) Uani 1 1 d . . . H26 H 0.4921 0.0638 1.0954 0.039 Uiso 1 1 calc R . . C27 C 0.4189(3) 0.05443(18) 1.1550(2) 0.0410(9) Uani 1 1 d . . . H27 H 0.4168 0.0087 1.1541 0.049 Uiso 1 1 calc R . . C28 C 0.3775(2) 0.08919(18) 1.19182(18) 0.0361(8) Uani 1 1 d . . . H28 H 0.3479 0.0667 1.2158 0.043 Uiso 1 1 calc R . . C29 C 0.3799(2) 0.15703(18) 1.19304(18) 0.0314(8) Uani 1 1 d . . . H29 H 0.3523 0.1802 1.2181 0.038 Uiso 1 1 calc R . . C30 C 0.4234(2) 0.19076(16) 1.15706(17) 0.0274(7) Uani 1 1 d . . . H30 H 0.4248 0.2365 1.1576 0.033 Uiso 1 1 calc R . . C31 C 0.4537(2) 0.26416(16) 1.02783(16) 0.0246(7) Uani 1 1 d . . . C32 C 0.4830(2) 0.32735(17) 1.02118(18) 0.0307(8) Uani 1 1 d . . . H32 H 0.5386 0.3397 1.0463 0.037 Uiso 1 1 calc R . . C33 C 0.4286(3) 0.37133(19) 0.9768(2) 0.0428(9) Uani 1 1 d . . . H33 H 0.4477 0.4135 0.9723 0.051 Uiso 1 1 calc R . . C34 C 0.3456(3) 0.3531(2) 0.9391(2) 0.0457(10) Uani 1 1 d . . . H34 H 0.3096 0.383 0.9092 0.055 Uiso 1 1 calc R . . C35 C 0.3167(2) 0.2910(2) 0.9457(2) 0.0412(9) Uani 1 1 d . . . H35 H 0.2612 0.2789 0.9201 0.049 Uiso 1 1 calc R . . C36 C 0.3696(2) 0.24647(18) 0.99020(17) 0.0318(8) Uani 1 1 d . . . H36 H 0.3493 0.2048 0.9952 0.038 Uiso 1 1 calc R . . N1 N 0.3805(2) 0.60342(16) 0.64043(16) 0.0384(7) Uani 1 1 d . . . N3 N 0.54816(17) 0.14829(13) 1.02626(13) 0.0260(6) Uani 1 1 d . . . O1 O 0.38388(19) 0.54193(14) 0.64570(15) 0.0510(7) Uani 1 1 d . . . O2 O 0.43528(17) 0.63623(13) 0.68517(15) 0.0458(7) Uani 1 1 d . . . O3 O 0.3235(2) 0.63128(17) 0.59386(15) 0.0593(8) Uani 1 1 d . . . P1 P 0.55297(5) 0.15185(4) 0.95197(4) 0.0208(2) Uani 1 1 d . . . P2 P 0.52237(5) 0.19942(4) 1.07390(4) 0.0215(2) Uani 1 1 d . . . Mn1 Mn 0.5 0.54956(4) 0.75 0.0460(3) Uani 1 2 d SD . . N2A N 0.3959(5) 0.4985(3) 0.8111(4) 0.0573(7) Uani 0.63 1 d PD A 1 O4A O 0.3998(3) 0.5524(2) 0.8022(3) 0.0573(7) Uani 0.63 1 d PD A 1 O5A O 0.4295(3) 0.4626(2) 0.7725(3) 0.0573(7) Uani 0.63 1 d PD A 1 O6A O 0.3349(3) 0.4670(3) 0.8223(3) 0.0573(7) Uani 0.63 1 d PD A 1 N2B N 0.3905(7) 0.4782(5) 0.7831(6) 0.0573(7) Uani 0.37 1 d PD A 2 O4B O 0.4117(6) 0.5255(5) 0.8194(5) 0.0573(7) Uani 0.37 1 d PD A 2 O5B O 0.4527(5) 0.4522(4) 0.7651(6) 0.0573(7) Uani 0.37 1 d PD A 2 O6B O 0.3530(5) 0.4443(4) 0.8116(5) 0.0573(7) Uani 0.37 1 d PD A 2 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 0.0228(16) 0.0233(16) 0.0235(16) -0.0013(13) 0.0090(13) 0.0015(13) C2 0.0226(16) 0.0286(17) 0.0301(17) 0.0006(14) 0.0086(14) 0.0010(13) C3 0.0321(19) 0.0298(18) 0.039(2) -0.0035(16) 0.0121(16) -0.0059(15) C4 0.046(2) 0.0283(19) 0.043(2) 0.0043(16) 0.0192(18) -0.0021(16) C5 0.044(2) 0.035(2) 0.035(2) 0.0090(16) 0.0006(17) 0.0048(17) C6 0.0296(18) 0.0284(18) 0.0325(18) -0.0006(15) -0.0017(15) 0.0001(14) C7 0.0220(15) 0.0209(15) 0.0248(16) -0.0018(12) 0.0085(13) 0.0024(12) C8 0.0271(17) 0.0329(18) 0.0271(17) -0.0031(14) 0.0119(14) -0.0021(14) C9 0.0254(17) 0.0331(19) 0.042(2) -0.0007(16) 0.0123(16) -0.0025(14) C10 0.0267(18) 0.0296(18) 0.0360(19) -0.0065(15) 0.0008(15) -0.0019(14) C11 0.0367(19) 0.0349(19) 0.0236(17) -0.0072(14) 0.0070(15) -0.0011(15) C12 0.0262(17) 0.0290(17) 0.0283(17) -0.0020(14) 0.0107(14) -0.0036(13) C13 0.0206(15) 0.0239(16) 0.0239(15) -0.0026(13) 0.0071(13) -0.0008(12) C14 0.0301(17) 0.0266(17) 0.0297(17) 0.0042(14) 0.0122(14) 0.0019(14) C15 0.036(2) 0.0269(18) 0.043(2) 0.0077(16) 0.0128(17) 0.0094(15) C16 0.0252(17) 0.036(2) 0.043(2) -0.0023(16) 0.0118(16) 0.0090(15) C17 0.0280(18) 0.039(2) 0.0361(19) -0.0011(16) 0.0170(15) 0.0006(15) C18 0.0268(17) 0.0289(17) 0.0253(16) 0.0031(14) 0.0069(14) 0.0027(13) C19 0.0215(16) 0.0292(17) 0.0213(15) 0.0014(13) 0.0068(13) -0.0020(13) C20 0.0245(16) 0.0286(17) 0.0305(17) -0.0040(14) 0.0093(14) -0.0008(13) C21 0.035(2) 0.0324(19) 0.0351(19) -0.0078(15) 0.0076(16) -0.0094(15) C22 0.0245(18) 0.052(2) 0.036(2) -0.0028(18) -0.0019(16) -0.0079(16) C23 0.0205(18) 0.059(3) 0.047(2) -0.004(2) 0.0033(16) 0.0045(17) C24 0.0264(18) 0.040(2) 0.0346(19) -0.0057(16) 0.0079(15) 0.0056(15) C25 0.0205(15) 0.0269(16) 0.0195(15) -0.0005(12) 0.0029(13) 0.0004(13) C26 0.040(2) 0.0271(18) 0.0339(18) -0.0004(15) 0.0175(16) 0.0036(15) C27 0.056(2) 0.0278(19) 0.046(2) 0.0040(17) 0.026(2) -0.0006(17) C28 0.039(2) 0.037(2) 0.0358(19) 0.0055(16) 0.0182(17) -0.0034(16) C29 0.0288(18) 0.037(2) 0.0304(18) -0.0023(15) 0.0129(15) 0.0024(15) C30 0.0297(17) 0.0248(17) 0.0288(17) -0.0010(14) 0.0114(14) -0.0002(13) C31 0.0251(16) 0.0265(17) 0.0238(16) -0.0001(13) 0.0103(13) 0.0040(13) C32 0.0292(18) 0.0286(18) 0.0340(19) 0.0012(15) 0.0100(15) 0.0062(14) C33 0.049(2) 0.0295(19) 0.051(2) 0.0081(17) 0.018(2) 0.0101(17) C34 0.044(2) 0.048(2) 0.042(2) 0.0126(18) 0.0100(19) 0.0205(19) C35 0.0272(19) 0.054(2) 0.039(2) 0.0056(18) 0.0068(16) 0.0081(17) C36 0.0250(17) 0.0374(19) 0.0323(18) 0.0018(15) 0.0088(15) 0.0027(14) N1 0.0423(18) 0.0412(19) 0.0389(18) -0.0038(15) 0.0230(16) -0.0118(15) N3 0.0301(15) 0.0254(14) 0.0233(14) -0.0007(11) 0.0101(12) 0.0032(11) O1 0.0525(18) 0.0410(17) 0.0604(19) -0.0063(14) 0.0199(15) -0.0118(13) O2 0.0398(15) 0.0403(16) 0.0535(17) -0.0074(13) 0.0107(13) -0.0068(12) O3 0.0521(19) 0.075(2) 0.0431(17) 0.0177(16) 0.0060(15) -0.0119(16) P1 0.0196(4) 0.0227(4) 0.0198(4) -0.0010(3) 0.0061(3) 0.0005(3) P2 0.0197(4) 0.0236(4) 0.0203(4) -0.0013(3) 0.0056(3) 0.0014(3) Mn1 0.0298(5) 0.0263(4) 0.0752(7) 0 0.0087(4) 0 N2A 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) O4A 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) O5A 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) O6A 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) N2B 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) O4B 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) O5B 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) O6B 0.0408(13) 0.0521(18) 0.0915(18) 0.0248(14) 0.0388(12) 0.0285(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 1.386(5) . ? C1 C2 1.389(5) . ? C1 P1 1.800(3) . ? C2 C3 1.384(5) . ? C3 C4 1.382(5) . ? C4 C5 1.369(5) . ? C5 C6 1.390(5) . ? C7 C12 1.388(4) . ? C7 C8 1.389(4) . ? C7 P1 1.803(3) . ? C8 C9 1.385(5) . ? C9 C10 1.385(5) . ? C10 C11 1.377(5) . ? C11 C12 1.379(5) . ? C13 C18 1.391(4) . ? C13 C14 1.395(5) . ? C13 P1 1.801(3) . ? C14 C15 1.393(5) . ? C15 C16 1.377(5) . ? C16 C17 1.385(5) . ? C17 C18 1.389(5) . ? C19 C24 1.389(5) . ? C19 C20 1.396(5) . ? C19 P2 1.799(3) . ? C20 C21 1.384(5) . ? C21 C22 1.371(5) . ? C22 C23 1.371(6) . ? C23 C24 1.394(5) . ? C25 C26 1.389(5) . ? C25 C30 1.399(4) . ? C25 P2 1.793(3) . ? C26 C27 1.382(5) . ? C27 C28 1.385(5) . ? C28 C29 1.378(5) . ? C29 C30 1.385(5) . ? C31 C32 1.395(5) . ? C31 C36 1.400(5) . ? C31 P2 1.793(3) . ? C32 C33 1.382(5) . ? C33 C34 1.387(6) . ? C34 C35 1.372(6) . ? C35 C36 1.380(5) . ? N1 O3 1.242(4) . ? N1 O1 1.253(4) . ? N1 O2 1.254(4) . ? N3 P1 1.581(3) . ? N3 P2 1.592(3) . ? O1 Mn1 2.379(3) . ? O2 Mn1 2.260(3) . ? Mn1 O5B 2.188(8) 2_656 ? Mn1 O5B 2.188(8) . ? Mn1 O5A 2.252(5) 2_656 ? Mn1 O5A 2.252(5) . ? Mn1 O2 2.260(3) 2_656 ? Mn1 O4A 2.273(4) 2_656 ? Mn1 O4A 2.273(4) . ? Mn1 O1 2.379(3) 2_656 ? Mn1 O4B 2.430(6) 2_656 ? Mn1 O4B 2.430(6) . ? N2A O4A 1.117(6) . ? N2A O6A 1.283(6) . ? N2A O5A 1.339(7) . ? N2B O4B 1.201(5) . ? N2B O6B 1.209(8) . ? N2B O5B 1.322(8) . ? 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 119.1(3) . . ? C6 C1 P1 123.1(2) . . ? C2 C1 P1 117.7(2) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 120.3(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 120.5(3) . . ? C1 C6 C5 120.1(3) . . ? C12 C7 C8 119.2(3) . . ? C12 C7 P1 120.3(2) . . ? C8 C7 P1 120.5(2) . . ? C9 C8 C7 120.4(3) . . ? C10 C9 C8 119.8(3) . . ? C11 C10 C9 120.0(3) . . ? C10 C11 C12 120.4(3) . . ? C11 C12 C7 120.2(3) . . ? C18 C13 C14 119.8(3) . . ? C18 C13 P1 121.4(2) . . ? C14 C13 P1 118.7(2) . . ? C15 C14 C13 119.9(3) . . ? C16 C15 C14 119.7(3) . . ? C15 C16 C17 121.0(3) . . ? C16 C17 C18 119.6(3) . . ? C17 C18 C13 120.0(3) . . ? C24 C19 C20 119.8(3) . . ? C24 C19 P2 118.3(3) . . ? C20 C19 P2 121.7(2) . . ? C21 C20 C19 119.5(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C23 121.0(3) . . ? C22 C23 C24 119.7(3) . . ? C19 C24 C23 119.7(3) . . ? C26 C25 C30 119.9(3) . . ? C26 C25 P2 120.5(2) . . ? C30 C25 P2 119.6(2) . . ? C27 C26 C25 119.6(3) . . ? C26 C27 C28 120.5(3) . . ? C29 C28 C27 120.2(3) . . ? C28 C29 C30 120.1(3) . . ? C29 C30 C25 119.7(3) . . ? C32 C31 C36 119.7(3) . . ? C32 C31 P2 123.2(3) . . ? C36 C31 P2 116.6(3) . . ? C33 C32 C31 119.3(3) . . ? C32 C33 C34 120.6(4) . . ? C35 C34 C33 120.1(4) . . ? C34 C35 C36 120.4(4) . . ? C35 C36 C31 119.9(3) . . ? O3 N1 O1 121.5(3) . . ? O3 N1 O2 120.8(3) . . ? O1 N1 O2 117.7(3) . . ? P1 N3 P2 134.05(18) . . ? N1 O1 Mn1 90.8(2) . . ? N1 O2 Mn1 96.4(2) . . ? N3 P1 C1 115.60(14) . . ? N3 P1 C13 109.25(15) . . ? C1 P1 C13 106.57(14) . . ? N3 P1 C7 111.08(15) . . ? C1 P1 C7 108.15(14) . . ? C13 P1 C7 105.63(14) . . ? N3 P2 C25 108.15(15) . . ? N3 P2 C31 113.49(14) . . ? C25 P2 C31 107.24(15) . . ? N3 P2 C19 110.22(15) . . ? C25 P2 C19 106.86(14) . . ? C31 P2 C19 110.59(15) . . ? O5B Mn1 O5B 50.7(4) 2_656 . ? O5B Mn1 O5A 13.03(19) 2_656 2_656 ? O5B Mn1 O5A 63.8(3) . 2_656 ? O5B Mn1 O5A 63.8(3) 2_656 . ? O5B Mn1 O5A 13.03(19) . . ? O5A Mn1 O5A 76.8(2) 2_656 . ? O5B Mn1 O2 132.0(3) 2_656 2_656 ? O5B Mn1 O2 137.6(3) . 2_656 ? O5A Mn1 O2 124.03(15) 2_656 2_656 ? O5A Mn1 O2 131.38(17) . 2_656 ? O5B Mn1 O2 137.6(3) 2_656 . ? O5B Mn1 O2 132.0(3) . . ? O5A Mn1 O2 131.38(17) 2_656 . ? O5A Mn1 O2 124.03(15) . . ? O2 Mn1 O2 77.70(14) 2_656 . ? O5B Mn1 O4A 66.4(2) 2_656 2_656 ? O5B Mn1 O4A 116.5(3) . 2_656 ? O5A Mn1 O4A 53.55(17) 2_656 2_656 ? O5A Mn1 O4A 129.38(19) . 2_656 ? O2 Mn1 O4A 89.44(15) 2_656 2_656 ? O2 Mn1 O4A 88.27(16) . 2_656 ? O5B Mn1 O4A 116.5(3) 2_656 . ? O5B Mn1 O4A 66.4(2) . . ? O5A Mn1 O4A 129.38(19) 2_656 . ? O5A Mn1 O4A 53.55(17) . . ? O2 Mn1 O4A 88.27(16) 2_656 . ? O2 Mn1 O4A 89.44(15) . . ? O4A Mn1 O4A 177.1(3) 2_656 . ? O5B Mn1 O1 81.6(3) 2_656 2_656 ? O5B Mn1 O1 91.6(3) . 2_656 ? O5A Mn1 O1 79.75(17) 2_656 2_656 ? O5A Mn1 O1 94.35(17) . 2_656 ? O2 Mn1 O1 55.01(10) 2_656 2_656 ? O2 Mn1 O1 132.44(10) . 2_656 ? O4A Mn1 O1 86.71(17) 2_656 2_656 ? O4A Mn1 O1 93.48(17) . 2_656 ? O5B Mn1 O1 91.6(3) 2_656 . ? O5B Mn1 O1 81.6(3) . . ? O5A Mn1 O1 94.35(17) 2_656 . ? O5A Mn1 O1 79.75(17) . . ? O2 Mn1 O1 132.44(10) 2_656 . ? O2 Mn1 O1 55.01(10) . . ? O4A Mn1 O1 93.48(17) 2_656 . ? O4A Mn1 O1 86.71(17) . . ? O1 Mn1 O1 172.53(14) 2_656 . ? O5B Mn1 O4B 54.3(3) 2_656 2_656 ? O5B Mn1 O4B 102.8(3) . 2_656 ? O5A Mn1 O4B 42.2(2) 2_656 2_656 ? O5A Mn1 O4B 115.2(3) . 2_656 ? O2 Mn1 O4B 104.7(2) 2_656 2_656 ? O2 Mn1 O4B 93.4(2) . 2_656 ? O4A Mn1 O4B 15.3(2) 2_656 2_656 ? O4A Mn1 O4B 167.1(3) . 2_656 ? O1 Mn1 O4B 93.9(3) 2_656 2_656 ? O1 Mn1 O4B 84.6(3) . 2_656 ? O5B Mn1 O4B 102.8(4) 2_656 . ? O5B Mn1 O4B 54.3(3) . . ? O5A Mn1 O4B 115.2(3) 2_656 . ? O5A Mn1 O4B 42.2(3) . . ? O2 Mn1 O4B 93.4(2) 2_656 . ? O2 Mn1 O4B 104.7(2) . . ? O4A Mn1 O4B 167.1(3) 2_656 . ? O4A Mn1 O4B 15.3(2) . . ? O1 Mn1 O4B 84.6(3) 2_656 . ? O1 Mn1 O4B 93.9(3) . . ? O4B Mn1 O4B 156.8(5) 2_656 . ? O4A N2A O6A 127.8(5) . . ? O4A N2A O5A 111.9(6) . . ? O6A N2A O5A 110.6(6) . . ? N2A O4A Mn1 98.5(4) . . ? N2A O5A Mn1 92.9(4) . . ? O4B N2B O6B 103.7(10) . . ? O4B N2B O5B 114.0(9) . . ? O6B N2B O5B 119.5(9) . . ? N2B O4B Mn1 83.9(6) . . ? N2B O5B Mn1 91.8(5) . . ? # Attachment 'publicaro16071.cif' #----------------------------------------------------------------------------# data_caro1607 _database_code_depnum_ccdc_archive 'CCDC 668885' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C36 H30 N P2), Cu N4 O12' _chemical_formula_sum 'C72 H60 Cu N6 O12 P4' _chemical_formula_weight 1388.68 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 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' '-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 20.224(2) _cell_length_b 20.1491(19) _cell_length_c 16.3528(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6663.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180 _cell_measurement_reflns_used 4324 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 32.158 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2876 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7645 _exptl_absorpt_correction_T_max 0.9565 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_unetI/netI 0.05 _diffrn_reflns_number 48707 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6798 _reflns_number_gt 4095 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2sigma(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^)+(0.1134P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 6798 _refine_ls_number_parameters 424 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.2043 _refine_ls_wR_factor_gt 0.1751 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.586 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.12099(16) 0.41051(16) 0.9214(2) 0.0402(8) Uani 1 1 d . . . C2 C 0.18157(19) 0.40872(18) 0.8830(2) 0.0498(9) Uani 1 1 d . . . H2 H 0.2177 0.3885 0.9078 0.06 Uiso 1 1 calc R . . C3 C 0.1875(2) 0.4382(2) 0.8053(3) 0.0655(12) Uani 1 1 d . . . H3 H 0.2281 0.4372 0.7786 0.079 Uiso 1 1 calc R . . C4 C 0.1349(2) 0.4680(2) 0.7683(3) 0.0672(12) Uani 1 1 d . . . H4 H 0.1395 0.4865 0.7166 0.081 Uiso 1 1 calc R . . C5 C 0.0761(2) 0.4707(2) 0.8071(2) 0.0669(12) Uani 1 1 d . . . H5 H 0.0406 0.4921 0.7823 0.08 Uiso 1 1 calc R . . C6 C 0.0678(2) 0.44205(18) 0.8832(2) 0.0523(9) Uani 1 1 d . . . H6 H 0.0268 0.4438 0.9089 0.063 Uiso 1 1 calc R . . C7 C 0.02865(17) 0.34319(18) 1.0291(2) 0.0428(8) Uani 1 1 d . . . C8 C -0.01977(19) 0.3774(2) 1.0723(3) 0.0643(12) Uani 1 1 d . . . H8 H -0.0098 0.4165 1.0999 0.077 Uiso 1 1 calc R . . C9 C -0.0834(2) 0.3517(3) 1.0732(3) 0.0834(15) Uani 1 1 d . . . H9 H -0.1163 0.3739 1.1018 0.1 Uiso 1 1 calc R . . C10 C -0.0987(2) 0.2943(3) 1.0327(3) 0.0918(18) Uani 1 1 d . . . H10 H -0.1417 0.278 1.0335 0.11 Uiso 1 1 calc R . . C11 C -0.0506(3) 0.2611(3) 0.9911(3) 0.0805(15) Uani 1 1 d . . . H11 H -0.0607 0.2219 0.9639 0.097 Uiso 1 1 calc R . . C12 C 0.0129(2) 0.2854(2) 0.9893(2) 0.0599(11) Uani 1 1 d . . . H12 H 0.0455 0.2624 0.9609 0.072 Uiso 1 1 calc R . . C13 C 0.11970(16) 0.44125(17) 1.0947(2) 0.0425(8) Uani 1 1 d . . . C14 C 0.1186(2) 0.4266(2) 1.1771(2) 0.0660(12) Uani 1 1 d . . . H14 H 0.1152 0.3827 1.1939 0.079 Uiso 1 1 calc R . . C15 C 0.1225(2) 0.4763(2) 1.2347(3) 0.0726(13) Uani 1 1 d . . . H15 H 0.1216 0.4657 1.2901 0.087 Uiso 1 1 calc R . . C16 C 0.12779(19) 0.5414(2) 1.2105(3) 0.0657(12) Uani 1 1 d . . . H16 H 0.1305 0.5751 1.2494 0.079 Uiso 1 1 calc R . . C17 C 0.1289(2) 0.5564(2) 1.1291(3) 0.0732(13) Uani 1 1 d . . . H17 H 0.1324 0.6004 1.1124 0.088 Uiso 1 1 calc R . . C18 C 0.1250(2) 0.50674(19) 1.0718(3) 0.0576(11) Uani 1 1 d . . . H18 H 0.1259 0.5176 1.0165 0.069 Uiso 1 1 calc R . . C19 C 0.20551(17) 0.19081(17) 1.0041(2) 0.0410(8) Uani 1 1 d . . . C20 C 0.21479(18) 0.2076(2) 0.9230(2) 0.0502(9) Uani 1 1 d . . . H20 H 0.2084 0.2511 0.9059 0.06 Uiso 1 1 calc R . . C21 C 0.2336(2) 0.1595(2) 0.8672(3) 0.0652(12) Uani 1 1 d . . . H21 H 0.2416 0.1713 0.8132 0.078 Uiso 1 1 calc R . . C22 C 0.2406(2) 0.0948(2) 0.8910(3) 0.0678(12) Uani 1 1 d . . . H22 H 0.2515 0.0625 0.8526 0.081 Uiso 1 1 calc R . . C23 C 0.2316(2) 0.0775(2) 0.9705(3) 0.0668(12) Uani 1 1 d . . . H23 H 0.2374 0.0336 0.9866 0.08 Uiso 1 1 calc R . . C24 C 0.2139(2) 0.12461(18) 1.0271(3) 0.0568(10) Uani 1 1 d . . . H24 H 0.2075 0.1123 1.0814 0.068 Uiso 1 1 calc R . . C25 C 0.12263(17) 0.22054(17) 1.1436(2) 0.0430(8) Uani 1 1 d . . . C26 C 0.1164(2) 0.2445(2) 1.2220(2) 0.0606(11) Uani 1 1 d . . . H26 H 0.1476 0.2742 1.2422 0.073 Uiso 1 1 calc R . . C27 C 0.0644(3) 0.2249(3) 1.2709(3) 0.0865(16) Uani 1 1 d . . . H27 H 0.0601 0.242 1.3235 0.104 Uiso 1 1 calc R . . C28 C 0.0191(3) 0.1801(3) 1.2417(4) 0.0868(16) Uani 1 1 d . . . H28 H -0.0155 0.1663 1.275 0.104 Uiso 1 1 calc R . . C29 C 0.0245(2) 0.1561(3) 1.1654(4) 0.0814(14) Uani 1 1 d . . . H29 H -0.0066 0.126 1.146 0.098 Uiso 1 1 calc R . . C30 C 0.0763(2) 0.1760(2) 1.1153(2) 0.0603(11) Uani 1 1 d . . . H30 H 0.0797 0.1592 1.0625 0.072 Uiso 1 1 calc R . . C31 C 0.25780(17) 0.26795(18) 1.1380(2) 0.0472(9) Uani 1 1 d . . . C32 C 0.2796(2) 0.2211(2) 1.1940(3) 0.0666(12) Uani 1 1 d . . . H32 H 0.2556 0.1824 1.2026 0.08 Uiso 1 1 calc R . . C33 C 0.3380(3) 0.2327(3) 1.2372(3) 0.0831(15) Uani 1 1 d . . . H33 H 0.3532 0.2017 1.275 0.1 Uiso 1 1 calc R . . C34 C 0.3726(2) 0.2898(3) 1.2238(3) 0.0802(15) Uani 1 1 d . . . H34 H 0.4118 0.2969 1.2522 0.096 Uiso 1 1 calc R . . C35 C 0.3513(2) 0.3366(3) 1.1700(3) 0.0716(13) Uani 1 1 d . . . H35 H 0.3752 0.3756 1.1628 0.086 Uiso 1 1 calc R . . C36 C 0.29382(19) 0.3258(2) 1.1258(3) 0.0568(10) Uani 1 1 d . . . H36 H 0.2794 0.3572 1.0882 0.068 Uiso 1 1 calc R . . N1 N 0.16618(14) 0.31953(14) 1.03063(18) 0.0463(7) Uani 1 1 d . . . P1 P 0.11184(4) 0.37456(4) 1.02131(5) 0.0383(3) Uani 1 1 d . . . P2 P 0.18484(4) 0.25350(4) 1.07724(5) 0.0379(2) Uani 1 1 d . . . Cu1 Cu 0 0.5 0.5 0.0727(3) Uani 1 2 d SD . . N2A N 0.0078(14) 0.4094(12) 0.3794(14) 0.0981(9) Uani 0.27 1 d PDU A 1 O1A O 0.0486(7) 0.4182(8) 0.4517(10) 0.0981(9) Uani 0.27 1 d PD A 1 O2A O -0.0229(11) 0.4582(9) 0.3525(8) 0.0981(9) Uani 0.27 1 d PD A 1 O3A O 0.0083(7) 0.3728(7) 0.3211(10) 0.0981(9) Uani 0.27 1 d PD A 1 N2B N 0.0208(5) 0.4037(5) 0.3865(6) 0.0981(9) Uani 0.73 1 d PD A 2 O1B O 0.0253(3) 0.4121(3) 0.4634(4) 0.0981(9) Uani 0.73 1 d PD A 2 O2B O -0.0118(4) 0.4434(4) 0.3528(4) 0.0981(9) Uani 0.73 1 d PD A 2 O3B O 0.0435(3) 0.3541(3) 0.3577(3) 0.0981(9) Uani 0.73 1 d PD A 2 N3A N 0.1174(9) 0.5731(13) 0.4552(15) 0.094(4) Uani 0.43 1 d PD A 1 O4A O 0.0621(4) 0.5581(4) 0.4446(5) 0.0727(3) Uani 0.43 1 d PD A 1 O5A O 0.1509(6) 0.6024(9) 0.4052(7) 0.125(3) Uani 0.43 1 d PD A 1 O6A O 0.1373(7) 0.5536(8) 0.5227(11) 0.125(3) Uani 0.43 1 d PD A 1 N3B N 0.1201(7) 0.5494(8) 0.4748(11) 0.094(4) Uani 0.57 1 d PD A 2 O4B O 0.0690(3) 0.5370(3) 0.4231(4) 0.0727(3) Uani 0.57 1 d PD A 2 O5B O 0.1665(5) 0.5824(6) 0.4447(6) 0.125(3) Uani 0.57 1 d PD A 2 O6B O 0.1227(5) 0.5235(6) 0.5431(7) 0.125(3) Uani 0.57 1 d PD A 2 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 0.046(2) 0.0344(18) 0.0405(19) -0.0019(15) -0.0011(16) 0.0001(15) C2 0.050(2) 0.048(2) 0.051(2) 0.0023(18) 0.0070(18) -0.0044(17) C3 0.081(3) 0.055(3) 0.060(3) -0.001(2) 0.024(2) -0.013(2) C4 0.102(4) 0.052(3) 0.048(2) 0.004(2) 0.007(3) -0.009(2) C5 0.084(3) 0.066(3) 0.050(2) 0.012(2) -0.013(2) 0.012(2) C6 0.056(2) 0.052(2) 0.049(2) 0.0056(19) -0.0042(19) 0.0037(18) C7 0.0381(19) 0.050(2) 0.0402(19) 0.0092(17) 0.0019(16) 0.0017(16) C8 0.048(2) 0.068(3) 0.077(3) 0.011(2) 0.018(2) 0.008(2) C9 0.050(3) 0.106(4) 0.094(4) 0.018(3) 0.023(3) 0.008(3) C10 0.048(3) 0.135(5) 0.093(4) 0.030(4) -0.006(3) -0.024(3) C11 0.068(3) 0.103(4) 0.071(3) -0.011(3) -0.014(3) -0.029(3) C12 0.053(2) 0.078(3) 0.049(2) -0.012(2) -0.0016(19) -0.012(2) C13 0.040(2) 0.043(2) 0.044(2) -0.0026(16) 0.0000(16) 0.0048(15) C14 0.108(4) 0.042(2) 0.048(2) -0.0004(19) -0.001(2) 0.007(2) C15 0.095(4) 0.075(3) 0.048(2) -0.009(2) 0.000(2) 0.004(3) C16 0.063(3) 0.070(3) 0.064(3) -0.029(2) -0.005(2) -0.003(2) C17 0.098(4) 0.048(2) 0.073(3) -0.006(2) -0.008(3) -0.013(2) C18 0.078(3) 0.046(2) 0.049(2) -0.0021(18) 0.004(2) -0.0097(19) C19 0.0337(18) 0.042(2) 0.047(2) -0.0038(16) -0.0033(15) 0.0030(15) C20 0.055(2) 0.054(2) 0.042(2) -0.0006(18) -0.0044(17) 0.0095(18) C21 0.068(3) 0.078(3) 0.049(2) -0.009(2) 0.002(2) 0.014(2) C22 0.062(3) 0.074(3) 0.067(3) -0.032(3) -0.010(2) 0.016(2) C23 0.073(3) 0.042(2) 0.086(3) -0.017(2) -0.011(3) 0.011(2) C24 0.072(3) 0.044(2) 0.054(2) -0.0007(19) 0.001(2) 0.0043(19) C25 0.051(2) 0.0413(19) 0.0371(19) 0.0019(16) -0.0012(16) 0.0030(16) C26 0.078(3) 0.058(3) 0.046(2) 0.0011(19) 0.009(2) -0.005(2) C27 0.125(5) 0.074(3) 0.060(3) 0.008(3) 0.038(3) 0.021(3) C28 0.083(4) 0.083(4) 0.095(4) 0.027(3) 0.041(3) 0.007(3) C29 0.062(3) 0.088(4) 0.094(4) 0.013(3) 0.007(3) -0.017(3) C30 0.059(3) 0.068(3) 0.053(2) 0.000(2) 0.003(2) -0.017(2) C31 0.044(2) 0.047(2) 0.051(2) -0.0090(18) -0.0033(17) 0.0056(16) C32 0.074(3) 0.047(2) 0.078(3) -0.008(2) -0.029(2) 0.008(2) C33 0.085(3) 0.072(3) 0.093(4) -0.019(3) -0.039(3) 0.030(3) C34 0.054(3) 0.099(4) 0.088(4) -0.041(3) -0.023(3) 0.012(3) C35 0.054(3) 0.080(3) 0.081(3) -0.022(3) 0.002(2) -0.014(2) C36 0.052(2) 0.060(3) 0.058(2) -0.010(2) 0.003(2) -0.0035(19) N1 0.0412(17) 0.0425(17) 0.0553(18) 0.0104(15) 0.0068(14) 0.0085(13) P1 0.0380(5) 0.0368(5) 0.0400(5) 0.0022(4) 0.0029(4) 0.0043(4) P2 0.0402(5) 0.0351(5) 0.0385(5) -0.0003(4) -0.0007(4) 0.0015(4) Cu1 0.0686(6) 0.0662(6) 0.0833(6) 0.0025(4) -0.0243(4) 0.0043(4) N2A 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) O1A 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) O2A 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) O3A 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) N2B 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) O1B 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) O2B 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) O3B 0.1010(12) 0.0952(12) 0.0981(11) 0.0040(9) -0.0040(9) -0.0001(9) N3A 0.059(3) 0.085(14) 0.139(9) -0.036(7) -0.001(5) 0.005(6) O4A 0.0686(6) 0.0662(6) 0.0833(6) 0.0025(4) -0.0243(4) 0.0043(4) O5A 0.070(3) 0.186(7) 0.120(6) -0.027(6) -0.003(3) -0.018(3) O6A 0.070(3) 0.186(7) 0.120(6) -0.027(6) -0.003(3) -0.018(3) N3B 0.059(3) 0.085(14) 0.139(9) -0.036(7) -0.001(5) 0.005(6) O4B 0.0686(6) 0.0662(6) 0.0833(6) 0.0025(4) -0.0243(4) 0.0043(4) O5B 0.070(3) 0.186(7) 0.120(6) -0.027(6) -0.003(3) -0.018(3) O6B 0.070(3) 0.186(7) 0.120(6) -0.027(6) -0.003(3) -0.018(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 1.378(5) . ? C1 C6 1.397(5) . ? C1 P1 1.796(3) . ? C2 C3 1.407(5) . ? C3 C4 1.364(6) . ? C4 C5 1.349(6) . ? C5 C6 1.381(5) . ? C7 C12 1.371(6) . ? C7 C8 1.390(5) . ? C7 P1 1.802(4) . ? C8 C9 1.387(6) . ? C9 C10 1.368(7) . ? C10 C11 1.362(7) . ? C11 C12 1.375(6) . ? C13 C18 1.376(5) . ? C13 C14 1.380(5) . ? C13 P1 1.808(4) . ? C14 C15 1.377(6) . ? C15 C16 1.375(6) . ? C16 C17 1.366(6) . ? C17 C18 1.374(6) . ? C19 C20 1.382(5) . ? C19 C24 1.396(5) . ? C19 P2 1.790(3) . ? C20 C21 1.383(5) . ? C21 C22 1.369(6) . ? C22 C23 1.358(6) . ? C23 C24 1.374(5) . ? C25 C26 1.376(5) . ? C25 C30 1.378(5) . ? C25 P2 1.789(4) . ? C26 C27 1.379(6) . ? C27 C28 1.371(7) . ? C28 C29 1.343(8) . ? C29 C30 1.388(6) . ? C31 C32 1.386(5) . ? C31 C36 1.389(5) . ? C31 P2 1.803(4) . ? C32 C33 1.397(6) . ? C33 C34 1.364(7) . ? C34 C35 1.361(7) . ? C35 C36 1.385(6) . ? N1 P1 1.569(3) . ? N1 P2 1.579(3) . ? Cu1 O1B 1.939(6) 5_566 ? Cu1 O1B 1.939(6) . ? Cu1 O4A 1.941(8) 5_566 ? Cu1 O4A 1.941(8) . ? Cu1 O4B 2.021(6) 5_566 ? Cu1 O4B 2.021(6) . ? Cu1 O1A 2.075(14) . ? Cu1 O1A 2.075(14) 5_566 ? N2A O3A 1.205(17) . ? N2A O2A 1.244(17) . ? N2A O1A 1.453(17) . ? N2B O2B 1.175(8) . ? N2B O3B 1.195(8) . ? N2B O1B 1.272(9) . ? N3A O4A 1.171(15) . ? N3A O5A 1.215(15) . ? N3A O6A 1.240(17) . ? N3B O6B 1.234(13) . ? N3B O5B 1.252(13) . ? N3B O4B 1.358(13) . ? 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 119.5(3) . . ? C2 C1 P1 119.7(3) . . ? C6 C1 P1 120.8(3) . . ? C1 C2 C3 118.5(4) . . ? C4 C3 C2 121.3(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 120.9(4) . . ? C5 C6 C1 120.0(4) . . ? C12 C7 C8 119.9(4) . . ? C12 C7 P1 118.8(3) . . ? C8 C7 P1 121.3(3) . . ? C9 C8 C7 118.3(5) . . ? C10 C9 C8 121.4(5) . . ? C11 C10 C9 119.7(4) . . ? C10 C11 C12 120.2(5) . . ? C7 C12 C11 120.6(4) . . ? C18 C13 C14 118.2(3) . . ? C18 C13 P1 122.6(3) . . ? C14 C13 P1 119.2(3) . . ? C15 C14 C13 120.8(4) . . ? C16 C15 C14 120.1(4) . . ? C17 C16 C15 119.5(4) . . ? C16 C17 C18 120.2(4) . . ? C17 C18 C13 121.2(4) . . ? C20 C19 C24 118.5(3) . . ? C20 C19 P2 120.1(3) . . ? C24 C19 P2 121.5(3) . . ? C19 C20 C21 119.9(4) . . ? C22 C21 C20 120.6(4) . . ? C23 C22 C21 120.1(4) . . ? C22 C23 C24 120.2(4) . . ? C23 C24 C19 120.7(4) . . ? C26 C25 C30 118.6(4) . . ? C26 C25 P2 120.0(3) . . ? C30 C25 P2 121.1(3) . . ? C25 C26 C27 120.7(4) . . ? C28 C27 C26 119.7(5) . . ? C29 C28 C27 120.5(5) . . ? C28 C29 C30 120.4(5) . . ? C25 C30 C29 120.2(4) . . ? C32 C31 C36 119.9(4) . . ? C32 C31 P2 121.0(3) . . ? C36 C31 P2 119.1(3) . . ? C31 C32 C33 119.3(4) . . ? C34 C33 C32 119.5(5) . . ? C35 C34 C33 121.8(4) . . ? C34 C35 C36 119.6(4) . . ? C35 C36 C31 119.8(4) . . ? P1 N1 P2 144.1(2) . . ? N1 P1 C1 107.53(16) . . ? N1 P1 C7 113.54(17) . . ? C1 P1 C7 107.57(16) . . ? N1 P1 C13 113.53(16) . . ? C1 P1 C13 107.13(16) . . ? C7 P1 C13 107.21(16) . . ? N1 P2 C25 115.94(16) . . ? N1 P2 C19 109.13(16) . . ? C25 P2 C19 107.92(17) . . ? N1 P2 C31 109.00(17) . . ? C25 P2 C31 107.53(17) . . ? C19 P2 C31 106.95(16) . . ? O1B Cu1 O1B 180.0000(10) 5_566 . ? O1B Cu1 O4A 103.7(3) 5_566 5_566 ? O1B Cu1 O4A 76.3(3) . 5_566 ? O1B Cu1 O4A 76.3(3) 5_566 . ? O1B Cu1 O4A 103.7(3) . . ? O4A Cu1 O4A 180.0(3) 5_566 . ? O1B Cu1 O4B 87.9(2) 5_566 5_566 ? O1B Cu1 O4B 92.1(2) . 5_566 ? O4A Cu1 O4B 16.3(3) 5_566 5_566 ? O4A Cu1 O4B 163.7(3) . 5_566 ? O1B Cu1 O4B 92.1(2) 5_566 . ? O1B Cu1 O4B 87.9(2) . . ? O4A Cu1 O4B 163.7(3) 5_566 . ? O4A Cu1 O4B 16.3(3) . . ? O4B Cu1 O4B 180.0(3) 5_566 . ? O1B Cu1 O1A 165.5(5) 5_566 . ? O1B Cu1 O1A 14.5(5) . . ? O4A Cu1 O1A 90.3(5) 5_566 . ? O4A Cu1 O1A 89.7(5) . . ? O4B Cu1 O1A 105.7(5) 5_566 . ? O4B Cu1 O1A 74.3(5) . . ? O1B Cu1 O1A 14.5(5) 5_566 5_566 ? O1B Cu1 O1A 165.5(5) . 5_566 ? O4A Cu1 O1A 89.7(5) 5_566 5_566 ? O4A Cu1 O1A 90.3(5) . 5_566 ? O4B Cu1 O1A 74.3(5) 5_566 5_566 ? O4B Cu1 O1A 105.7(5) . 5_566 ? O1A Cu1 O1A 180.0(8) . 5_566 ? O3A N2A O2A 102.0(16) . . ? O3A N2A O1A 135.6(19) . . ? O2A N2A O1A 118.3(17) . . ? N2A O1A Cu1 97.9(12) . . ? O2B N2B O3B 126.8(8) . . ? O2B N2B O1B 114.4(8) . . ? O3B N2B O1B 118.3(8) . . ? N2B O1B Cu1 114.1(6) . . ? O4A N3A O5A 123.9(19) . . ? O4A N3A O6A 111.1(17) . . ? O5A N3A O6A 124.9(16) . . ? N3A O4A Cu1 134.8(11) . . ? O6B N3B O5B 123.3(11) . . ? O6B N3B O4B 121.2(12) . . ? O5B N3B O4B 115.0(13) . . ? N3B O4B Cu1 101.9(8) . . ?