# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_platon _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H36 Cu6 O70 P W12' _chemical_formula_weight 4351.18 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 18.7659(11) _cell_length_b 18.7659(11) _cell_length_c 11.3114(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3449.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1284 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 21.05 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1961 _exptl_absorpt_coefficient_mu 10.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1415 _exptl_absorpt_correction_T_max 0.2616 _exptl_absorpt_process_details sadabs _exptl_special_details ; ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.004 0.477 -0.009 1695.8 180.6 2 0.000 0.000 0.500 7.3 -0.3 _platon_squeeze_details ; Very little remaining electron density was left, because of the highly disordered nature of solvent molecules.SQUEEZE shows about 180 electron counts in voids in each unit cell, which accounts for about 4.5 DMF molecules. ; _diffrn_ambient_temperature 296(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 28318 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5213 _reflns_number_gt 2978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. DFIX and ISOR instructions were used.Hydrogens in water attached to Cu were generated by WINGX. Coordinates do not form a properly connected set, due to the encapsulation of POMs in the extended framework. ; _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^)+(0.2000P)^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_extinction_coef ? _refine_ls_number_reflns 5213 _refine_ls_number_parameters 213 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1406 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.3418 _refine_ls_wR_factor_gt 0.3207 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.186 _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 Cu1 Cu 0.47719(9) -0.04566(8) 0.40412(13) 0.0209(4) Uani 1 1 d . . . W1 W 0.93698(6) 0.06303(6) 0.25757(13) 0.0890(5) Uani 1 1 d . . . W2 W 0.99999(6) 0.18941(5) 0.00000(9) 0.0668(4) Uani 1 1 d . . . P1 P 1.0000 0.0000 0.0000 0.0296(18) Uani 1 6 d SD . . C1 C 0.7402(10) 0.1322(10) 0.2448(14) 0.046(4) Uani 1 1 d . . . H1 H 0.7041 0.0839 0.2054 0.055 Uiso 1 1 calc R . . C2 C 0.7196(8) 0.1499(8) 0.3565(14) 0.032(3) Uani 1 1 d . . . C3 C 0.7769(8) 0.2226(8) 0.4114(13) 0.031(3) Uani 1 1 d . . . H3 H 0.7661 0.2331 0.4877 0.037 Uiso 1 1 calc R . . C4 C 0.8502(8) 0.2807(7) 0.3569(13) 0.028(3) Uani 1 1 d . . . C5 C 0.8684(8) 0.2595(10) 0.2466(15) 0.046(4) Uani 1 1 d . . . H5 H 0.9176 0.2948 0.2086 0.055 Uiso 1 1 calc R . . C6 C 0.8132(11) 0.1863(12) 0.1954(18) 0.061(5) Uani 1 1 d . . . H6 H 0.8266 0.1730 0.1227 0.073 Uiso 1 1 calc R . . C8 C 0.6403(8) 0.0927(8) 0.4118(13) 0.032(3) Uani 1 1 d . . . C9 C 0.4528(8) 0.0937(8) 0.4103(13) 0.032(3) Uani 1 1 d . . . O1 O 0.5898(6) 0.0334(5) 0.3494(9) 0.034(2) Uani 1 1 d . . . O2 O 0.4430(6) 0.0332(5) 0.3497(9) 0.035(2) Uani 1 1 d . . . O3 O 0.3722(6) -0.1127(5) 0.4861(10) 0.039(2) Uani 1 1 d . . . O4 O 0.5159(6) -0.1117(5) 0.4856(10) 0.037(2) Uani 1 1 d . . . O5 O 0.4435(9) -0.1125(8) 0.2392(12) 0.066(4) Uani 1 1 d . . . H1O5 H 0.4221 -0.1566 0.1959 0.099 Uiso 1 1 d R . . H2O5 H 0.4707 -0.0726 0.1998 0.099 Uiso 1 1 d R . . O6 O 0.8424(12) 0.0183(11) 0.1595(16) 0.101(6) Uani 1 1 d . . . O7 O 0.9082(12) 0.0919(12) 0.3759(18) 0.112(7) Uani 1 1 d . . . O8 O 0.9816(10) 0.1593(11) 0.1578(18) 0.102(6) Uani 1 1 d . . . O9 O 0.8889(13) 0.1139(13) -0.0277(18) 0.110(6) Uani 1 1 d . . . O10 O 1.0003(15) 0.2809(12) -0.001(2) 0.131(9) Uani 1 1 d . . . O11 O 0.9147(17) -0.0434(17) 0.290(3) 0.164(11) Uani 1 1 d . . . O13 O 0.9505(15) -0.0982(11) 0.027(3) 0.075(8) Uani 0.50 1 d PDU . . O15 O 1.0000 0.0000 -0.1469(17) 0.063(11) Uani 0.50 3 d SPDU . . 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 Cu1 0.0224(7) 0.0057(6) 0.0285(8) -0.0046(5) -0.0022(6) 0.0025(5) W1 0.0642(7) 0.0650(7) 0.1343(12) -0.0163(6) 0.0159(6) 0.0297(5) W2 0.0630(6) 0.0496(5) 0.0924(8) 0.0049(4) 0.0101(4) 0.0315(4) P1 0.021(2) 0.021(2) 0.047(6) 0.000 0.000 0.0103(11) C1 0.037(8) 0.034(8) 0.046(10) -0.010(7) 0.014(7) 0.003(7) C2 0.020(6) 0.022(6) 0.046(9) 0.004(6) 0.009(6) 0.005(5) C3 0.025(6) 0.025(6) 0.046(9) -0.003(6) 0.001(6) 0.014(5) C4 0.027(6) 0.018(6) 0.035(8) -0.003(5) -0.003(5) 0.007(5) C5 0.017(6) 0.038(8) 0.059(11) -0.022(7) 0.006(6) -0.004(6) C6 0.040(9) 0.052(10) 0.068(13) -0.018(9) 0.020(9) 0.007(8) C8 0.030(7) 0.018(6) 0.040(9) 0.005(6) 0.005(6) 0.006(5) C9 0.028(7) 0.024(6) 0.042(9) 0.006(6) 0.007(6) 0.012(5) O1 0.033(5) 0.017(4) 0.041(6) -0.010(4) 0.006(4) 0.003(4) O2 0.046(6) 0.014(4) 0.044(6) -0.008(4) -0.014(5) 0.015(4) O3 0.023(5) 0.020(4) 0.046(6) 0.000(4) -0.003(4) -0.010(4) O4 0.052(6) 0.020(4) 0.047(6) -0.002(4) -0.003(5) 0.024(5) O5 0.069(9) 0.056(8) 0.063(9) -0.041(7) -0.021(7) 0.025(7) O6 0.098(13) 0.077(11) 0.094(13) 0.017(10) 0.045(11) 0.020(10) O7 0.089(13) 0.107(14) 0.117(16) -0.019(12) 0.032(11) 0.032(12) O8 0.058(9) 0.090(12) 0.125(16) -0.041(11) 0.001(9) 0.012(9) O9 0.106(15) 0.101(14) 0.097(14) -0.013(11) 0.015(11) 0.032(12) O10 0.15(2) 0.083(13) 0.20(2) -0.038(14) -0.069(17) 0.089(15) O11 0.119(19) 0.14(2) 0.24(3) 0.00(2) -0.03(2) 0.073(17) O13 0.062(13) 0.107(17) 0.077(16) -0.018(13) -0.001(11) 0.058(12) O15 0.061(12) 0.061(12) 0.068(19) 0.000 0.000 0.030(6) _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 Cu1 O4 1.953(9) . ? Cu1 O3 1.961(10) . ? Cu1 O1 1.978(9) . ? Cu1 O2 1.983(9) . ? Cu1 O5 2.159(11) . ? Cu1 Cu1 2.628(3) 4_656 ? W1 O7 1.634(18) . ? W1 O11 1.83(3) 3_765 ? W1 O11 1.86(3) . ? W1 O6 1.90(2) . ? W1 O8 1.93(2) . ? W1 O15 2.401(10) 4_755 ? W2 O10 1.713(16) . ? W2 O8 1.85(2) . ? W2 O9 1.87(2) . ? W2 O6 1.88(2) 5_665 ? W2 O9 1.92(2) 5_665 ? W2 O13 2.33(2) 3_765 ? W2 O13 2.34(2) 4_755 ? P1 O13 1.626(18) 2_645 ? P1 O13 1.626(18) 5_665 ? P1 O13 1.626(18) . ? P1 O13 1.626(18) 6_545 ? P1 O13 1.626(18) 4_755 ? P1 O13 1.626(18) 3_765 ? P1 O15 1.662(19) 4_755 ? P1 O15 1.662(19) . ? C1 C6 1.35(2) . ? C1 C2 1.41(2) . ? C2 C3 1.392(19) . ? C2 C8 1.470(18) . ? C3 C4 1.400(19) . ? C4 C5 1.40(2) . ? C4 C9 1.445(18) 2_655 ? C5 C6 1.37(2) . ? C8 O1 1.258(17) . ? C8 O3 1.271(18) 4_656 ? C9 O2 1.259(17) . ? C9 O4 1.284(18) 4_656 ? C9 C4 1.445(18) 3_665 ? O3 C8 1.271(18) 4_656 ? O4 C9 1.284(18) 4_656 ? O6 W2 1.88(2) 6_545 ? O9 W2 1.92(2) 6_545 ? O11 W1 1.83(3) 2_645 ? O13 O13 1.71(3) 6_545 ? O13 O13 1.71(3) 5_665 ? O13 W2 2.33(2) 2_645 ? O13 W2 2.34(2) 4_755 ? O15 W1 2.401(10) 4_755 ? O15 W1 2.401(10) 6_545 ? O15 W1 2.401(10) 5_665 ? 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 O4 Cu1 O3 86.7(5) . . ? O4 Cu1 O1 91.6(4) . . ? O3 Cu1 O1 169.3(4) . . ? O4 Cu1 O2 169.2(4) . . ? O3 Cu1 O2 91.7(4) . . ? O1 Cu1 O2 88.0(4) . . ? O4 Cu1 O5 97.7(5) . . ? O3 Cu1 O5 97.3(5) . . ? O1 Cu1 O5 93.3(5) . . ? O2 Cu1 O5 93.1(5) . . ? O4 Cu1 Cu1 85.5(3) . 4_656 ? O3 Cu1 Cu1 85.6(3) . 4_656 ? O1 Cu1 Cu1 83.8(3) . 4_656 ? O2 Cu1 Cu1 83.7(3) . 4_656 ? O5 Cu1 Cu1 175.8(4) . 4_656 ? O7 W1 O11 104.9(13) . 3_765 ? O7 W1 O11 105.1(13) . . ? O11 W1 O11 81.1(17) 3_765 . ? O7 W1 O6 103.6(9) . . ? O11 W1 O6 151.4(12) 3_765 . ? O11 W1 O6 88.9(10) . . ? O7 W1 O8 103.3(9) . . ? O11 W1 O8 89.4(10) 3_765 . ? O11 W1 O8 151.5(11) . . ? O6 W1 O8 86.8(7) . . ? O7 W1 O15 156.4(9) . 4_755 ? O11 W1 O15 58.6(11) 3_765 4_755 ? O11 W1 O15 58.3(11) . 4_755 ? O6 W1 O15 93.4(6) . 4_755 ? O8 W1 O15 93.8(6) . 4_755 ? O10 W2 O8 102.6(10) . . ? O10 W2 O9 101.6(10) . . ? O8 W2 O9 87.9(8) . . ? O10 W2 O6 102.8(10) . 5_665 ? O8 W2 O6 154.7(9) . 5_665 ? O9 W2 O6 87.0(8) . 5_665 ? O10 W2 O9 101.9(10) . 5_665 ? O8 W2 O9 87.4(8) . 5_665 ? O9 W2 O9 156.4(14) . 5_665 ? O6 W2 O9 87.5(8) 5_665 5_665 ? O10 W2 O13 158.9(10) . 3_765 ? O8 W2 O13 67.7(9) . 3_765 ? O9 W2 O13 60.5(9) . 3_765 ? O6 W2 O13 88.3(10) 5_665 3_765 ? O9 W2 O13 96.4(9) 5_665 3_765 ? O10 W2 O13 158.1(10) . 4_755 ? O8 W2 O13 89.2(10) . 4_755 ? O9 W2 O13 97.1(9) . 4_755 ? O6 W2 O13 66.9(9) 5_665 4_755 ? O9 W2 O13 59.7(9) 5_665 4_755 ? O13 W2 O13 43.0(8) 3_765 4_755 ? O13 P1 O13 180.0(18) 2_645 5_665 ? O13 P1 O13 116.5(7) 2_645 . ? O13 P1 O13 63.5(7) 5_665 . ? O13 P1 O13 63.5(7) 2_645 6_545 ? O13 P1 O13 116.5(7) 5_665 6_545 ? O13 P1 O13 63.5(7) . 6_545 ? O13 P1 O13 63.5(7) 2_645 4_755 ? O13 P1 O13 116.5(7) 5_665 4_755 ? O13 P1 O13 180(2) . 4_755 ? O13 P1 O13 116.5(7) 6_545 4_755 ? O13 P1 O13 116.5(7) 2_645 3_765 ? O13 P1 O13 63.5(7) 5_665 3_765 ? O13 P1 O13 116.5(7) . 3_765 ? O13 P1 O13 180.0(8) 6_545 3_765 ? O13 P1 O13 63.5(7) 4_755 3_765 ? O13 P1 O15 79.1(11) 2_645 4_755 ? O13 P1 O15 100.9(11) 5_665 4_755 ? O13 P1 O15 79.1(11) . 4_755 ? O13 P1 O15 100.9(11) 6_545 4_755 ? O13 P1 O15 100.9(11) 4_755 4_755 ? O13 P1 O15 79.1(11) 3_765 4_755 ? O13 P1 O15 100.9(11) 2_645 . ? O13 P1 O15 79.1(11) 5_665 . ? O13 P1 O15 100.9(11) . . ? O13 P1 O15 79.1(11) 6_545 . ? O13 P1 O15 79.1(11) 4_755 . ? O13 P1 O15 100.9(11) 3_765 . ? O15 P1 O15 180.000(1) 4_755 . ? C6 C1 C2 119.2(15) . . ? C3 C2 C1 117.5(12) . . ? C3 C2 C8 122.0(13) . . ? C1 C2 C8 120.5(13) . . ? C2 C3 C4 122.9(13) . . ? C3 C4 C5 117.0(12) . . ? C3 C4 C9 122.7(13) . 2_655 ? C5 C4 C9 120.2(13) . 2_655 ? C6 C5 C4 119.4(14) . . ? C1 C6 C5 123.6(17) . . ? O1 C8 O3 127.0(12) . 4_656 ? O1 C8 C2 116.6(13) . . ? O3 C8 C2 116.1(12) 4_656 . ? O2 C9 O4 125.3(13) . 4_656 ? O2 C9 C4 117.7(13) . 3_665 ? O4 C9 C4 116.9(12) 4_656 3_665 ? C8 O1 Cu1 122.6(9) . . ? C9 O2 Cu1 123.3(9) . . ? C8 O3 Cu1 121.0(8) 4_656 . ? C9 O4 Cu1 122.2(8) 4_656 . ? W2 O6 W1 141.7(9) 6_545 . ? W2 O8 W1 141.0(9) . . ? W2 O9 W2 139.3(14) . 6_545 ? W1 O11 W1 148(2) 2_645 . ? P1 O13 O13 58.2(3) . 6_545 ? P1 O13 O13 58.2(3) . 5_665 ? O13 O13 O13 108(2) 6_545 5_665 ? P1 O13 W2 127.1(14) . 2_645 ? O13 O13 W2 150(3) 6_545 2_645 ? O13 O13 W2 68.9(13) 5_665 2_645 ? P1 O13 W2 126.4(13) . 4_755 ? O13 O13 W2 68.1(13) 6_545 4_755 ? O13 O13 W2 150(3) 5_665 4_755 ? W2 O13 W2 99.2(7) 2_645 4_755 ? P1 O15 W1 121.4(4) . 4_755 ? P1 O15 W1 121.4(4) . 6_545 ? W1 O15 W1 95.3(5) 4_755 6_545 ? P1 O15 W1 121.4(4) . 5_665 ? W1 O15 W1 95.3(5) 4_755 5_665 ? W1 O15 W1 95.3(5) 6_545 5_665 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 6.603 _refine_diff_density_min -3.999 _refine_diff_density_rms 0.466 _database_code_depnum_ccdc_archive 'CCDC 943144' ####################################################################### # # 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_ql_hz45_2_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H21 Cu N O5' _chemical_formula_weight 466.96 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' 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 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 29.26(4) _cell_length_b 9.821(14) _cell_length_c 18.95(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.821(17) _cell_angle_gamma 90.00 _cell_volume 4981(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 671 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 21.23 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Large voids remain structure, but SQUEEZE lower down the Goodness-of-fit significantly. The structure without SQUEEZE was reported here. ; _diffrn_ambient_temperature 296(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 11170 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.1261 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 24.81 _reflns_number_total 4211 _reflns_number_gt 2171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. One carbon atom in DMF molecule coordinated to Cu is disordered into two positions. VERY LARGE Solvent Accessible VOID(S) in Structure: This is due to the porous nature of the MOF structure, and solvents could not be located precisely in the voids ; _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^)+(0.2000P)^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_extinction_coef ? _refine_ls_number_reflns 4211 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.2320 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 0.707 _refine_ls_restrained_S_all 0.707 _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 Cu1 Cu 0.23757(2) 0.65806(7) 0.04035(4) 0.0434(3) Uani 1 1 d . . . O1 O 0.18607(15) 0.7907(5) 0.0358(3) 0.0579(12) Uani 1 1 d . . . O2 O 0.29323(16) 0.5533(5) 0.0332(3) 0.0609(13) Uani 1 1 d . . . O3 O 0.28728(16) 0.7563(5) 0.1297(3) 0.0633(13) Uani 1 1 d . . . O4 O 0.19201(17) 0.5845(5) -0.0601(3) 0.0613(12) Uani 1 1 d . . . O5 O 0.2230(3) 0.5035(9) 0.1092(5) 0.099(2) Uani 1 1 d . . . C1 C 0.1388(2) 0.9958(6) -0.0004(4) 0.0499(16) Uani 1 1 d . . . C2 C 0.1276(2) 1.1169(7) -0.0414(4) 0.0601(19) Uani 1 1 d . . . H2 H 0.1469 1.1444 -0.0676 0.072 Uiso 1 1 calc R . . C3 C 0.0885(2) 1.1972(7) -0.0441(4) 0.0611(19) Uani 1 1 d . . . H3 H 0.0816 1.2771 -0.0729 0.073 Uiso 1 1 calc R . . C4 C 0.0589(2) 1.1612(6) -0.0045(4) 0.0511(16) Uani 1 1 d . . . C5 C 0.0706(2) 1.0411(7) 0.0396(4) 0.0571(17) Uani 1 1 d . . . H5 H 0.0519 1.0164 0.0673 0.068 Uiso 1 1 calc R . . C6 C 0.1100(2) 0.9588(7) 0.0419(4) 0.0553(17) Uani 1 1 d . . . H6 H 0.1175 0.8793 0.0711 0.066 Uiso 1 1 calc R . . C7 C 0.0147(2) 1.2451(6) -0.0094(4) 0.0504(16) Uani 1 1 d . . . C8 C -0.0161(2) 1.3094(7) -0.0796(4) 0.0549(18) Uani 1 1 d . . . H8 H -0.0082 1.3006 -0.1224 0.066 Uiso 1 1 calc R . . C9 C -0.0578(2) 1.3856(6) -0.0860(4) 0.0501(16) Uani 1 1 d . . . C10 C -0.0687(2) 1.3995(7) -0.0194(4) 0.0609(19) Uani 1 1 d . . . H10 H -0.0963 1.4502 -0.0226 0.073 Uiso 1 1 calc R . . C11 C -0.0388(3) 1.3385(7) 0.0505(4) 0.0627(19) Uani 1 1 d . . . C12 C 0.0031(2) 1.2615(7) 0.0557(4) 0.0578(18) Uani 1 1 d . . . H12 H 0.0233 1.2211 0.1024 0.069 Uiso 1 1 calc R . . C13 C -0.0503(3) 1.3581(9) 0.1211(5) 0.094(3) Uani 1 1 d . . . H13A H -0.0708 1.4377 0.1143 0.141 Uiso 1 1 calc R . . H13B H -0.0197 1.3693 0.1659 0.141 Uiso 1 1 calc R . . H13C H -0.0679 1.2798 0.1277 0.141 Uiso 1 1 calc R . . C14 C -0.0904(2) 1.4505(7) -0.1597(4) 0.0513(16) Uani 1 1 d . . . C15 C -0.0971(3) 1.3951(7) -0.2300(4) 0.064(2) Uani 1 1 d . . . H15 H -0.0802 1.3152 -0.2305 0.077 Uiso 1 1 calc R . . C16 C -0.1161(2) 1.5718(7) -0.1613(4) 0.0584(18) Uani 1 1 d . . . H16 H -0.1124 1.6126 -0.1150 0.070 Uiso 1 1 calc R . . C17 C -0.1465(2) 1.6317(6) -0.2294(4) 0.0581(18) Uani 1 1 d . . . H17 H -0.1626 1.7127 -0.2281 0.070 Uiso 1 1 calc R . . C18 C -0.1541(2) 1.5745(6) -0.3009(4) 0.0533(17) Uani 1 1 d . . . C19 C -0.1282(2) 1.4532(7) -0.3009(4) 0.0624(18) Uani 1 1 d . . . H19 H -0.1317 1.4124 -0.3471 0.075 Uiso 1 1 calc R . . C20 C 0.1805(2) 0.9035(7) 0.0009(4) 0.0519(17) Uani 1 1 d . . . C21 C -0.1890(2) 1.6380(7) -0.3770(5) 0.0548(18) Uani 1 1 d . . . C22 C 0.2506(7) 0.459(3) 0.1641(12) 0.079(8) Uani 0.54(4) 1 d P A 1 H22 H 0.2723 0.5179 0.2006 0.095 Uiso 0.54(4) 1 calc PR A 1 C221 C 0.2287(10) 0.400(3) 0.121(2) 0.079(10) Uani 0.46(4) 1 d P A 2 H221 H 0.2105 0.3480 0.0777 0.095 Uiso 0.46(4) 1 calc PR A 2 C23 C 0.2887(6) 0.3032(17) 0.2638(8) 0.177(6) Uani 1 1 d . A . H23A H 0.2912 0.3884 0.2899 0.265 Uiso 1 1 calc R . . H23B H 0.3212 0.2764 0.2678 0.265 Uiso 1 1 calc R . . H23C H 0.2758 0.2350 0.2870 0.265 Uiso 1 1 calc R . . C24 C 0.2348(6) 0.1946(19) 0.1454(11) 0.215(8) Uani 1 1 d . A . H24A H 0.2023 0.1815 0.1457 0.323 Uiso 1 1 calc R . . H24B H 0.2563 0.1210 0.1724 0.323 Uiso 1 1 calc R . . H24C H 0.2318 0.1969 0.0931 0.323 Uiso 1 1 calc R . . N1 N 0.2550(3) 0.3185(8) 0.1820(5) 0.090(2) 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 Cu1 0.0374(5) 0.0373(5) 0.0541(5) 0.0023(4) 0.0171(4) 0.0033(3) O1 0.053(3) 0.049(3) 0.075(3) 0.009(2) 0.029(3) 0.016(2) O2 0.056(3) 0.058(3) 0.077(3) 0.010(2) 0.036(3) 0.014(2) O3 0.054(3) 0.065(3) 0.060(3) -0.007(2) 0.012(2) -0.013(2) O4 0.061(3) 0.061(3) 0.057(3) -0.002(2) 0.019(3) -0.006(2) O5 0.094(5) 0.087(6) 0.121(7) 0.048(4) 0.050(5) 0.011(4) C1 0.038(3) 0.050(4) 0.061(4) -0.004(3) 0.020(3) 0.007(3) C2 0.057(4) 0.053(4) 0.077(5) 0.018(4) 0.034(4) 0.015(3) C3 0.057(4) 0.053(4) 0.082(5) 0.022(4) 0.037(4) 0.021(3) C4 0.044(4) 0.043(4) 0.063(4) 0.007(3) 0.018(3) 0.011(3) C5 0.046(4) 0.055(4) 0.073(5) 0.004(4) 0.027(4) 0.007(3) C6 0.044(4) 0.045(4) 0.073(5) 0.009(3) 0.019(4) 0.008(3) C7 0.043(4) 0.044(4) 0.064(5) 0.005(3) 0.022(3) 0.007(3) C8 0.046(4) 0.061(4) 0.061(5) 0.003(3) 0.026(4) 0.007(3) C9 0.043(4) 0.049(4) 0.059(4) 0.007(3) 0.021(3) 0.006(3) C10 0.046(4) 0.056(4) 0.080(5) 0.006(4) 0.025(4) 0.016(3) C11 0.061(4) 0.067(5) 0.068(5) 0.004(4) 0.034(4) 0.019(4) C12 0.053(4) 0.057(4) 0.060(5) 0.010(3) 0.019(4) 0.013(3) C13 0.096(6) 0.125(8) 0.074(6) 0.009(5) 0.048(5) 0.038(6) C14 0.039(3) 0.056(4) 0.056(4) 0.008(3) 0.016(3) 0.007(3) C15 0.056(4) 0.062(4) 0.075(6) 0.014(4) 0.026(4) 0.024(3) C16 0.046(4) 0.064(4) 0.054(4) 0.000(4) 0.008(3) 0.015(3) C17 0.049(4) 0.050(4) 0.069(5) 0.000(4) 0.017(4) 0.012(3) C18 0.039(3) 0.050(4) 0.069(5) 0.012(4) 0.019(3) -0.002(3) C19 0.058(4) 0.063(4) 0.071(5) 0.005(4) 0.031(4) 0.004(4) C20 0.038(4) 0.050(4) 0.057(4) -0.011(4) 0.007(3) 0.002(3) C21 0.029(3) 0.053(4) 0.076(5) 0.018(4) 0.016(3) -0.002(3) C22 0.062(11) 0.108(18) 0.053(12) -0.039(13) 0.008(9) -0.023(11) C221 0.085(17) 0.059(15) 0.10(2) 0.022(15) 0.042(17) 0.019(12) C23 0.182(14) 0.258(18) 0.100(10) -0.021(11) 0.066(10) -0.016(13) C24 0.171(15) 0.215(17) 0.22(2) -0.089(16) 0.044(14) -0.015(14) N1 0.099(6) 0.071(5) 0.113(7) 0.028(5) 0.058(5) 0.023(4) _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 Cu1 O1 1.967(5) . ? Cu1 O4 1.968(5) . ? Cu1 O2 1.976(5) . ? Cu1 O3 1.981(5) . ? Cu1 O5 2.154(7) . ? Cu1 Cu1 2.651(3) 7_565 ? O1 C20 1.266(8) . ? O2 C20 1.263(8) 7_565 ? O3 C21 1.284(8) 8_576 ? O4 C21 1.271(8) 2_544 ? O5 C221 1.04(2) . ? O5 C22 1.12(2) . ? C1 C2 1.386(9) . ? C1 C6 1.425(8) . ? C1 C20 1.511(8) . ? C2 C3 1.372(9) . ? C2 H2 0.9300 . ? C3 C4 1.402(9) . ? C3 H3 0.9300 . ? C4 C5 1.405(9) . ? C4 C7 1.506(8) . ? C5 C6 1.395(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.414(9) . ? C7 C8 1.419(9) . ? C8 C9 1.396(8) . ? C8 H8 0.9300 . ? C9 C10 1.427(9) . ? C9 C14 1.480(9) . ? C10 C11 1.393(10) . ? C10 H10 0.9300 . ? C11 C12 1.409(9) . ? C11 C13 1.520(10) . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.377(9) . ? C14 C16 1.402(9) . ? C15 C19 1.404(9) . ? C15 H15 0.9300 . ? C16 C17 1.369(9) . ? C16 H16 0.9300 . ? C17 C18 1.399(9) . ? C17 H17 0.9300 . ? C18 C19 1.411(9) . ? C18 C21 1.524(9) . ? C19 H19 0.9300 . ? C20 O2 1.263(8) 7_565 ? C21 O4 1.271(8) 2_564 ? C21 O3 1.284(8) 8_475 ? C22 N1 1.41(3) . ? C22 H22 0.9300 . ? C221 N1 1.36(3) . ? C221 H221 0.9300 . ? C23 N1 1.470(15) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N1 1.407(16) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 Cu1 O4 89.6(2) . . ? O1 Cu1 O2 168.38(19) . . ? O4 Cu1 O2 89.9(2) . . ? O1 Cu1 O3 90.0(2) . . ? O4 Cu1 O3 169.17(19) . . ? O2 Cu1 O3 88.3(2) . . ? O1 Cu1 O5 99.0(2) . . ? O4 Cu1 O5 96.0(3) . . ? O2 Cu1 O5 92.6(2) . . ? O3 Cu1 O5 94.8(3) . . ? O1 Cu1 Cu1 84.70(17) . 7_565 ? O4 Cu1 Cu1 85.90(18) . 7_565 ? O2 Cu1 Cu1 83.68(16) . 7_565 ? O3 Cu1 Cu1 83.28(18) . 7_565 ? O5 Cu1 Cu1 175.79(18) . 7_565 ? C20 O1 Cu1 122.5(4) . . ? C20 O2 Cu1 123.3(4) 7_565 . ? C21 O3 Cu1 123.3(5) 8_576 . ? C21 O4 Cu1 121.2(4) 2_544 . ? C221 O5 C22 54.6(16) . . ? C221 O5 Cu1 140.1(14) . . ? C22 O5 Cu1 126.5(13) . . ? C2 C1 C6 118.3(6) . . ? C2 C1 C20 122.1(6) . . ? C6 C1 C20 119.6(6) . . ? C3 C2 C1 121.3(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 121.4(6) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C3 C4 C5 118.4(6) . . ? C3 C4 C7 122.1(6) . . ? C5 C4 C7 119.5(6) . . ? C6 C5 C4 120.3(6) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.3(6) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 119.0(6) . . ? C12 C7 C4 120.7(6) . . ? C8 C7 C4 120.3(6) . . ? C9 C8 C7 121.4(6) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 118.3(6) . . ? C8 C9 C14 121.3(6) . . ? C10 C9 C14 120.3(6) . . ? C11 C10 C9 121.4(6) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 119.6(6) . . ? C10 C11 C13 120.3(6) . . ? C12 C11 C13 120.2(7) . . ? C11 C12 C7 120.4(6) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 116.7(6) . . ? C15 C14 C9 121.9(6) . . ? C16 C14 C9 121.5(6) . . ? C14 C15 C19 123.2(6) . . ? C14 C15 H15 118.4 . . ? C19 C15 H15 118.4 . . ? C17 C16 C14 121.6(6) . . ? C17 C16 H16 119.2 . . ? C14 C16 H16 119.2 . . ? C16 C17 C18 121.9(6) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 117.6(6) . . ? C17 C18 C21 122.4(6) . . ? C19 C18 C21 120.0(7) . . ? C15 C19 C18 118.9(7) . . ? C15 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? O2 C20 O1 125.8(6) 7_565 . ? O2 C20 C1 116.4(6) 7_565 . ? O1 C20 C1 117.8(6) . . ? O4 C21 O3 126.2(6) 2_564 8_475 ? O4 C21 C18 119.0(6) 2_564 . ? O3 C21 C18 114.8(7) 8_475 . ? O5 C22 N1 125(2) . . ? O5 C22 H22 117.6 . . ? N1 C22 H22 117.6 . . ? O5 C221 N1 138(4) . . ? O5 C221 H221 110.9 . . ? N1 C221 H221 110.9 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C221 N1 C24 96.2(19) . . ? C221 N1 C22 42.0(12) . . ? C24 N1 C22 138.2(15) . . ? C221 N1 C23 149.8(19) . . ? C24 N1 C23 113.7(12) . . ? C22 N1 C23 108.1(13) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 24.81 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.033 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 943145' ####################################################################### # # 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_hz33 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C118 H142 Cu4 N10 O88 P W12' _chemical_formula_weight 5599.75 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 18.0410(38) _cell_length_b 27.8300(58) _cell_length_c 24.1272(51) _cell_angle_alpha 90.00 _cell_angle_beta 106.695(3) _cell_angle_gamma 90.00 _cell_volume 11603(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1954 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.32 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5286 _exptl_absorpt_coefficient_mu 6.353 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_reflns_number 50340 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 21540 _reflns_number_gt 12795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Several atoms, such as C19 and C37, were not refined anisotropically, since making them anisotropically leads to non positive definite. SQUEEZE shows that there are 2543 electrons left in voids, but refinement using hkl files provided by SQUEEZE doesn't lead to stable refinement. DFIX was used for the ethyl groups attached to the nitrogen. ISOR and DELU were also used to refine. 5 DMF molecules could be located, and other peaks were refined as oxygens in the voids. Coordinates do not form a properly connected set, due to the encapsulation of POMs in the extended framework. Very large Solvent Accessible VOID(S) in Structure: This is due to the porous nature of the MOF structure, and solvents could not be located precisely in the voids. Like other MOF structures, due to the disordered nature of the structure and quality of the collected data, these structures show several level A alerts. ; _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^)+(0.1612P)^2^+31.0665P] 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_extinction_coef ? _refine_ls_number_reflns 21540 _refine_ls_number_parameters 937 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.2716 _refine_ls_wR_factor_gt 0.2236 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _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 Cu1 Cu -0.21799(9) 0.16495(5) 0.20737(7) 0.0273(4) Uani 1 1 d . . . Cu2 Cu 0.32228(9) 0.67086(5) 0.28272(7) 0.0220(3) Uani 1 1 d . . . W1 W 0.2500 0.04513(3) 0.7500 0.0315(2) Uani 1 2 d S . . W2 W 0.36439(3) 0.10844(2) 0.87296(2) 0.03058(17) Uani 1 1 d . . . W3 W 0.41770(3) 0.10936(2) 0.74180(3) 0.03583(18) Uani 1 1 d . . . W4 W 0.36372(3) 0.23726(2) 0.87218(3) 0.04142(19) Uani 1 1 d . . . W5 W 0.30350(4) 0.17259(2) 0.61923(3) 0.0438(2) Uani 1 1 d . . . W6 W 0.2500 0.30033(3) 0.7500 0.0517(3) Uani 1 2 d S . . W7 W 0.41474(4) 0.23630(2) 0.74181(3) 0.0505(2) Uani 1 1 d . . . P1 P 0.2500 0.17291(13) 0.7500 0.0116(8) Uani 1 2 d S . . C1 C 0.2743(7) 0.7366(4) 0.1855(5) 0.025(3) Uani 1 1 d . . . C2 C 0.2920(7) 0.7783(4) 0.1525(5) 0.026(3) Uani 1 1 d . . . C3 C 0.3669(7) 0.7975(4) 0.1648(6) 0.030(3) Uani 1 1 d . . . H3A H 0.4074 0.7833 0.1928 0.036 Uiso 1 1 calc R . . C4 C 0.3804(9) 0.8375(5) 0.1351(6) 0.034(3) Uani 1 1 d . . . H4A H 0.4303 0.8497 0.1429 0.041 Uiso 1 1 calc R . . C5 C 0.3202(7) 0.8598(4) 0.0938(5) 0.025(3) Uani 1 1 d . . . C6 C 0.2482(8) 0.8406(5) 0.0810(6) 0.030(3) Uani 1 1 d . . . H6A H 0.2085 0.8546 0.0522 0.036 Uiso 1 1 calc R . . C7 C 0.2325(8) 0.8010(5) 0.1095(5) 0.033(3) Uani 1 1 d . . . H7A H 0.1823 0.7890 0.1004 0.040 Uiso 1 1 calc R . . C8 C 0.3356(8) 0.9040(5) 0.0643(6) 0.032(3) Uani 1 1 d . . . C9 C 0.3973(8) 0.9354(5) 0.0921(6) 0.035(3) Uani 1 1 d . . . H9A H 0.4306 0.9269 0.1279 0.042 Uiso 1 1 calc R . . C10 C 0.4086(8) 0.9785(4) 0.0667(5) 0.032(3) Uani 1 1 d . . . C11 C 0.3612(7) 0.9892(4) 0.0108(5) 0.030(3) Uani 1 1 d . . . H11A H 0.3693 1.0175 -0.0071 0.036 Uiso 1 1 calc R . . C12 C 0.3033(8) 0.9586(5) -0.0177(5) 0.032(3) Uani 1 1 d . . . C13 C 0.2894(8) 0.9156(5) 0.0081(6) 0.033(3) Uani 1 1 d . . . H13A H 0.2501 0.8950 -0.0116 0.039 Uiso 1 1 calc R . . C14 C 0.4702(7) 1.0105(5) 0.0972(5) 0.030(3) Uani 1 1 d . . . C15 C 0.5143(7) 1.0384(5) 0.0703(5) 0.029(3) Uani 1 1 d . . . H15A H 0.5036 1.0371 0.0303 0.035 Uiso 1 1 calc R . . C16 C 0.5736(8) 1.0680(5) 0.1014(6) 0.037(3) Uani 1 1 d . . . H16A H 0.6013 1.0861 0.0819 0.044 Uiso 1 1 calc R . . C17 C 0.4883(9) 1.0121(5) 0.1599(6) 0.048(4) Uani 1 1 d . . . H17A H 0.4610 0.9936 0.1796 0.058 Uiso 1 1 calc R . . C18 C 0.2501(8) 0.9683(5) -0.0799(6) 0.041(4) Uani 1 1 d . . . H18A H 0.2694 0.9964 -0.0951 0.049 Uiso 1 1 calc R . . H18B H 0.2541 0.9413 -0.1042 0.049 Uiso 1 1 calc R . . C19 C 0.166(2) 1.0492(10) -0.0581(15) 0.175(15) Uiso 1 1 d D . . H19A H 0.1543 1.0720 -0.0322 0.262 Uiso 1 1 calc R . . H19B H 0.1338 1.0550 -0.0967 0.262 Uiso 1 1 calc R . . H19C H 0.2195 1.0525 -0.0573 0.262 Uiso 1 1 calc R . . C20 C 0.1529(17) 1.0016(8) -0.0407(10) 0.123(10) Uani 1 1 d DU . . H20A H 0.1871 0.9937 -0.0028 0.147 Uiso 1 1 calc R . . H20B H 0.0996 0.9969 -0.0410 0.147 Uiso 1 1 calc R . . C21 C 0.0418(15) 0.9738(14) -0.1577(9) 0.172(17) Uani 1 1 d . . . H21A H 0.0209 0.9763 -0.1989 0.257 Uiso 1 1 calc R . . H21B H 0.0203 0.9987 -0.1394 0.257 Uiso 1 1 calc R . . H21C H 0.0288 0.9430 -0.1451 0.257 Uiso 1 1 calc R . . C22 C 0.1235(10) 0.9789(9) -0.1423(6) 0.096(8) Uani 1 1 d D . . H22A H 0.1422 0.9547 -0.1640 0.115 Uiso 1 1 calc R . . H22B H 0.1339 1.0098 -0.1569 0.115 Uiso 1 1 calc R . . C23 C 0.2185(8) 0.6056(4) 0.3112(6) 0.033(3) Uani 1 1 d . . . C24 C 0.1982(8) 0.5643(4) 0.3450(6) 0.034(3) Uani 1 1 d . . . C25 C 0.2534(10) 0.5434(5) 0.3898(7) 0.050(4) Uani 1 1 d . . . H25A H 0.3030 0.5563 0.4014 0.060 Uiso 1 1 calc R . . C26 C 0.2369(10) 0.5037(5) 0.4177(7) 0.054(5) Uani 1 1 d . . . H26A H 0.2757 0.4897 0.4473 0.065 Uiso 1 1 calc R . . C27 C 0.1225(9) 0.5465(5) 0.3308(7) 0.045(4) Uani 1 1 d . . . H27A H 0.0831 0.5616 0.3026 0.054 Uiso 1 1 calc R . . C28 C 0.1070(9) 0.5063(5) 0.3591(7) 0.049(4) Uani 1 1 d . . . H28A H 0.0573 0.4934 0.3486 0.059 Uiso 1 1 calc R . . C29 C 0.1646(10) 0.4848(5) 0.4028(6) 0.047(4) Uani 1 1 d . . . C30 C 0.1473(10) 0.4389(5) 0.4311(6) 0.047(4) Uani 1 1 d . . . C31 C 0.1865(10) 0.4285(6) 0.4879(7) 0.058(5) Uani 1 1 d . . . H31A H 0.2220 0.4504 0.5095 0.069 Uiso 1 1 calc R . . C32 C 0.1737(10) 0.3853(5) 0.5136(6) 0.050(4) Uani 1 1 d . . . C33 C 0.1146(9) 0.3558(5) 0.4833(7) 0.050(4) Uani 1 1 d . . . H33A H 0.1013 0.3292 0.5016 0.060 Uiso 1 1 calc R . . C34 C 0.0756(9) 0.3647(5) 0.4277(7) 0.047(4) Uani 1 1 d . . . C35 C 0.0917(9) 0.4059(5) 0.3993(6) 0.047(4) Uani 1 1 d . . . H35A H 0.0662 0.4113 0.3605 0.057 Uiso 1 1 calc R . . C36 C 0.2236(13) 0.3729(7) 0.5729(8) 0.091(7) Uani 1 1 d U . . H36A H 0.1977 0.3491 0.5902 0.109 Uiso 1 1 calc R . . H36B H 0.2322 0.4014 0.5971 0.109 Uiso 1 1 calc R . . C37 C 0.3505(18) 0.3379(10) 0.6237(10) 0.141(12) Uiso 1 1 d D . . H37A H 0.3986 0.3244 0.6203 0.169 Uiso 1 1 calc R . . H37B H 0.3248 0.3145 0.6416 0.169 Uiso 1 1 calc R . . C38 C 0.363(2) 0.3826(11) 0.6556(15) 0.186(16) Uiso 1 1 d D . . H38A H 0.3959 0.3769 0.6941 0.280 Uiso 1 1 calc R . . H38B H 0.3147 0.3955 0.6572 0.280 Uiso 1 1 calc R . . H38C H 0.3882 0.4051 0.6365 0.280 Uiso 1 1 calc R . . C39 C 0.296(2) 0.3107(14) 0.536(2) 0.188(19) Uani 1 1 d DU . . H39A H 0.2602 0.3176 0.4986 0.225 Uiso 1 1 calc R . . H39B H 0.2715 0.2864 0.5540 0.225 Uiso 1 1 calc R . . C40 C 0.3640(15) 0.2893(14) 0.5266(19) 0.25(3) Uani 1 1 d D . . H40A H 0.3515 0.2581 0.5098 0.370 Uiso 1 1 calc R . . H40B H 0.4036 0.2865 0.5628 0.370 Uiso 1 1 calc R . . H40C H 0.3824 0.3093 0.5009 0.370 Uiso 1 1 calc R . . C41 C 0.0141(9) 0.3315(5) 0.3939(7) 0.040(4) Uani 1 1 d . . . C42 C -0.0381(12) 0.3113(6) 0.4167(8) 0.062(5) Uani 1 1 d . . . H42A H -0.0357 0.3191 0.4546 0.074 Uiso 1 1 calc R . . C43 C -0.0947(9) 0.2800(6) 0.3880(6) 0.049(4) Uani 1 1 d . . . H43A H -0.1314 0.2686 0.4050 0.058 Uiso 1 1 calc R . . C44 C -0.0957(8) 0.2655(5) 0.3321(6) 0.037(3) Uani 1 1 d . . . C45 C -0.0433(9) 0.2843(5) 0.3070(7) 0.048(4) Uani 1 1 d . . . H45A H -0.0439 0.2750 0.2699 0.057 Uiso 1 1 calc R . . C46 C 0.0106(10) 0.3172(6) 0.3370(9) 0.061(5) Uani 1 1 d . . . H46A H 0.0454 0.3303 0.3193 0.073 Uiso 1 1 calc R . . C47 C -0.1544(9) 0.2292(5) 0.2998(7) 0.042(4) Uani 1 1 d . . . C49 C -0.4083(8) 0.0707(4) 0.1604(6) 0.032(3) Uani 1 1 d . . . C50 C -0.4498(10) 0.0434(5) 0.1904(5) 0.044(4) Uani 1 1 d . . . H50A H -0.4371 0.0456 0.2305 0.053 Uiso 1 1 calc R . . N1 N 0.3026(12) 0.3527(11) 0.5698(10) 0.170(14) Uani 1 1 d DU . . N2 N 0.1710(7) 0.9758(6) -0.0844(5) 0.060(4) Uani 1 1 d D . . O1 O -0.3465(5) 0.1135(3) 0.2458(4) 0.035(2) Uani 1 1 d . . . O2 O -0.1632(7) 0.1626(5) 0.1398(5) 0.068(4) Uani 1 1 d . . . H2A H -0.1795 0.1734 0.1055 0.103 Uiso 1 1 d R . . H2B H -0.1242 0.1448 0.1416 0.103 Uiso 1 1 d R . . O3 O -0.2983(5) 0.1190(3) 0.1695(4) 0.032(2) Uani 1 1 d . . . O4 O -0.1461(5) 0.2122(3) 0.2534(4) 0.036(2) Uani 1 1 d . . . O5 O -0.2068(6) 0.2168(3) 0.3228(4) 0.040(2) Uani 1 1 d . . . O6 O 0.4417(6) 0.6733(4) 0.3319(5) 0.052(3) Uani 1 1 d . . . H1O6 H 0.4641 0.6873 0.3636 0.078 Uiso 1 1 d R . . H2O6 H 0.4679 0.6789 0.3084 0.078 Uiso 1 1 d R . . O7 O 0.1624(6) 0.6213(3) 0.2691(4) 0.040(2) Uani 1 1 d . . . O8 O 0.2854(5) 0.6209(3) 0.3262(4) 0.034(2) Uani 1 1 d . . . O9 O 0.3300(5) 0.7211(3) 0.2272(4) 0.035(2) Uani 1 1 d . . . O10 O 0.2082(5) 0.7203(3) 0.1714(4) 0.029(2) Uani 1 1 d . . . O11 O 0.2761(7) 0.2191(4) 0.8985(7) 0.085(5) Uani 1 1 d . . . O12 O 0.4164(6) 0.2672(4) 0.9317(5) 0.063(3) Uani 1 1 d . . . O13 O 0.2758(6) 0.1250(4) 0.8969(7) 0.077(4) Uani 1 1 d . . . O14 O 0.4188(6) 0.0791(4) 0.9326(4) 0.050(3) Uani 1 1 d . . . O15 O 0.3978(7) 0.1719(3) 0.8898(8) 0.077(5) Uani 1 1 d . . . O16 O 0.4278(7) 0.1060(5) 0.8231(4) 0.064(4) Uani 1 1 d . . . O17 O 0.3010(6) 0.0599(5) 0.8282(4) 0.064(4) Uani 1 1 d . . . O18 O 0.2500 -0.0157(4) 0.7500 0.058(5) Uani 1 2 d S . . O19 O 0.4962(6) 0.0784(4) 0.7380(4) 0.047(3) Uani 1 1 d . . . O20 O 0.3442(6) 0.0586(5) 0.7325(5) 0.070(4) Uani 1 1 d . . . O21 O 0.3715(8) 0.1246(4) 0.6626(5) 0.076(4) Uani 1 1 d . . . O22 O 0.3286(8) 0.1739(4) 0.5569(5) 0.065(4) Uani 1 1 d . . . O23 O 0.3709(8) 0.2197(4) 0.6624(6) 0.082(4) Uani 1 1 d . . . O24 O 0.4938(6) 0.2662(5) 0.7375(5) 0.069(4) Uani 1 1 d . . . O25 O 0.3427(7) 0.2869(5) 0.7329(5) 0.074(4) Uani 1 1 d . . . O26 O 0.2500 0.3616(7) 0.7500 0.085(6) Uani 1 2 d S . . O27 O 0.3021(7) 0.2872(5) 0.8281(6) 0.082(4) Uani 1 1 d . . . O28 O 0.2005(9) 0.2166(5) 0.7309(7) 0.099(5) Uani 1 1 d . . . O29 O 0.2791(11) 0.1722(5) 0.8141(9) 0.109(6) Uani 1 1 d U . . O30 O 0.3002(9) 0.1283(5) 0.7697(7) 0.091(5) Uani 1 1 d . . . O31 O 0.3156(10) 0.1734(5) 0.7240(7) 0.090(5) Uani 1 1 d . . . O32 O 0.4602(9) 0.1733(3) 0.7532(5) 0.074(5) Uani 1 1 d . . . O33 O 0.4270(7) 0.2387(5) 0.8224(5) 0.067(4) Uani 1 1 d . . . N3 N 0.1215(8) 0.7929(5) 0.5063(5) 0.053(4) Uani 1 1 d . . . N5 N 0.0121(16) 0.8367(9) 0.9598(11) 0.126(8) Uiso 1 1 d . . . N6 N 0.1627(18) 0.1767(9) 0.4342(12) 0.138(10) Uiso 1 1 d D . . O51 O 0.2525(7) 0.7869(4) 0.5481(5) 0.059(3) Uani 1 1 d . . . O53 O 0.1020(15) 0.8995(9) 0.9680(10) 0.167(9) Uiso 1 1 d . . . C48 C -0.3454(8) 0.1030(5) 0.1965(6) 0.030(3) Uiso 1 1 d . . . C51 C 0.0472(12) 0.8175(9) 0.5008(13) 0.123(12) Uani 1 1 d . . . H51A H 0.0555 0.8440 0.5273 0.184 Uiso 1 1 calc R . . H51B H 0.0114 0.7953 0.5095 0.184 Uiso 1 1 calc R . . H51C H 0.0265 0.8292 0.4620 0.184 Uiso 1 1 calc R . . C52 C 0.1170(12) 0.7521(7) 0.4683(8) 0.076(6) Uani 1 1 d . . . H52A H 0.1675 0.7383 0.4748 0.114 Uiso 1 1 calc R . . H52B H 0.0979 0.7624 0.4288 0.114 Uiso 1 1 calc R . . H52C H 0.0826 0.7285 0.4762 0.114 Uiso 1 1 calc R . . C53 C 0.1881(10) 0.8078(6) 0.5442(7) 0.051(4) Uani 1 1 d . . . H53A H 0.1872 0.8339 0.5680 0.061 Uiso 1 1 calc R . . C57 C 0.0582(18) 0.7974(11) 0.9676(12) 0.131(10) Uiso 1 1 d . . . H57A H 0.1109 0.8072 0.9733 0.197 Uiso 1 1 calc R . . H57B H 0.0422 0.7772 0.9340 0.197 Uiso 1 1 calc R . . H57C H 0.0542 0.7799 1.0009 0.197 Uiso 1 1 calc R . . C58 C -0.081(2) 0.8342(12) 0.9479(18) 0.176(16) Uiso 1 1 d . . . H58A H -0.1021 0.8662 0.9438 0.264 Uiso 1 1 calc R . . H58B H -0.0930 0.8186 0.9798 0.264 Uiso 1 1 calc R . . H58C H -0.1038 0.8164 0.9130 0.264 Uiso 1 1 calc R . . C59 C 0.033(3) 0.8801(16) 0.9517(17) 0.185(16) Uiso 1 1 d . . . H59A H -0.0063 0.9003 0.9313 0.221 Uiso 1 1 calc R . . C60 C 0.132(2) 0.1379(12) 0.4556(14) 0.150(12) Uiso 1 1 d . . . H60A H 0.1553 0.1088 0.4470 0.225 Uiso 1 1 calc R . . H60B H 0.0772 0.1367 0.4378 0.225 Uiso 1 1 calc R . . H60C H 0.1424 0.1411 0.4967 0.225 Uiso 1 1 calc R . . C62 C 0.231(3) 0.1790(14) 0.418(2) 0.203(19) Uiso 1 1 d D . . H62A H 0.2595 0.1511 0.4194 0.244 Uiso 1 1 calc R . . C61 C 0.128(2) 0.2204(14) 0.4453(17) 0.187(16) Uiso 1 1 d . . . H61A H 0.1501 0.2472 0.4308 0.281 Uiso 1 1 calc R . . H61B H 0.1360 0.2241 0.4862 0.281 Uiso 1 1 calc R . . H61C H 0.0730 0.2194 0.4263 0.281 Uiso 1 1 calc R . . O34 O 0.3831(12) 0.4209(7) 0.5257(9) 0.142(7) Uiso 1 1 d . . . O35 O 0.082(3) 0.8287(14) 0.172(2) 0.32(2) Uiso 1 1 d . . . O36 O 0.014(2) 0.8401(11) 0.8288(15) 0.230(14) Uiso 1 1 d . . . O37 O 0.847(2) 0.3102(14) 0.1443(17) 0.285(18) Uiso 1 1 d . . . O38 O 0.243(3) 0.0162(17) 0.149(2) 0.37(2) Uiso 1 1 d . . . O54 O 0.254(4) 0.216(2) 0.402(4) 0.65(6) Uiso 1 1 d D . . O39 O 0.037(2) 0.8733(12) 0.1096(15) 0.245(14) Uiso 1 1 d . . . O40 O 0.4669(16) 0.7688(10) 0.3813(12) 0.200(11) Uiso 1 1 d . . . O41 O 0.930(3) 0.858(2) 0.740(2) 0.39(3) Uiso 1 1 d . . . O42 O 0.3638(19) 0.6461(12) 0.4955(14) 0.232(13) 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 Cu1 0.0263(9) 0.0230(8) 0.0310(9) 0.0016(6) 0.0055(7) 0.0005(6) Cu2 0.0212(8) 0.0159(7) 0.0279(8) 0.0004(6) 0.0056(6) -0.0004(6) W1 0.0366(5) 0.0205(4) 0.0373(5) 0.000 0.0106(4) 0.000 W2 0.0273(3) 0.0344(3) 0.0271(3) 0.0066(2) 0.0031(2) -0.0010(2) W3 0.0303(3) 0.0408(4) 0.0350(3) -0.0007(2) 0.0072(3) 0.0110(3) W4 0.0310(4) 0.0412(4) 0.0472(4) -0.0183(3) 0.0036(3) -0.0031(3) W5 0.0472(4) 0.0536(4) 0.0345(4) 0.0107(3) 0.0181(3) -0.0014(3) W6 0.0449(6) 0.0288(5) 0.0769(7) 0.000 0.0104(5) 0.000 W7 0.0336(4) 0.0494(4) 0.0655(5) 0.0171(3) 0.0094(3) -0.0074(3) P1 0.0108(19) 0.0089(18) 0.015(2) 0.000 0.0030(16) 0.000 C1 0.028(7) 0.022(6) 0.026(7) -0.003(5) 0.011(6) 0.002(5) C2 0.028(7) 0.012(6) 0.033(7) -0.001(5) 0.001(6) -0.006(5) C3 0.018(6) 0.024(7) 0.038(8) 0.013(6) -0.006(6) 0.001(5) C4 0.036(8) 0.028(7) 0.042(8) -0.007(6) 0.016(7) -0.007(6) C5 0.026(7) 0.030(7) 0.016(6) 0.005(5) 0.000(5) -0.002(5) C6 0.033(8) 0.029(7) 0.025(7) 0.005(5) 0.004(6) -0.001(6) C7 0.031(8) 0.034(8) 0.029(7) -0.002(6) -0.001(6) -0.013(6) C8 0.035(8) 0.028(7) 0.031(7) -0.002(6) 0.008(6) -0.012(6) C9 0.044(9) 0.034(7) 0.026(7) 0.010(6) 0.006(6) -0.005(6) C10 0.041(8) 0.028(7) 0.027(7) 0.009(6) 0.011(6) 0.007(6) C11 0.034(8) 0.026(7) 0.027(7) -0.001(5) 0.005(6) -0.008(6) C12 0.040(8) 0.031(7) 0.025(7) 0.012(6) 0.009(6) 0.003(6) C13 0.035(8) 0.029(7) 0.030(7) 0.004(6) 0.003(6) -0.006(6) C14 0.026(7) 0.032(7) 0.027(7) 0.010(6) 0.001(6) 0.002(6) C15 0.035(8) 0.038(7) 0.016(6) 0.003(5) 0.008(6) -0.011(6) C16 0.043(9) 0.039(8) 0.024(7) 0.004(6) 0.004(6) -0.004(7) C17 0.053(10) 0.045(9) 0.036(8) 0.025(7) -0.003(7) -0.018(8) C18 0.042(9) 0.047(9) 0.027(8) 0.004(6) 0.001(7) -0.007(7) C20 0.121(10) 0.122(10) 0.122(10) 0.003(5) 0.030(5) -0.001(5) C21 0.10(2) 0.35(5) 0.046(14) 0.08(2) -0.007(14) -0.05(3) C22 0.047(12) 0.16(2) 0.069(14) 0.071(15) 0.000(10) 0.010(13) C23 0.040(9) 0.019(7) 0.045(9) 0.002(6) 0.020(7) -0.004(6) C24 0.042(8) 0.016(6) 0.042(8) 0.000(6) 0.010(7) -0.012(6) C25 0.057(10) 0.028(8) 0.058(10) 0.007(7) 0.005(8) -0.020(7) C26 0.068(12) 0.030(8) 0.058(11) 0.019(7) 0.006(9) -0.014(8) C27 0.048(9) 0.035(8) 0.057(10) 0.016(7) 0.022(8) -0.002(7) C28 0.047(9) 0.047(9) 0.048(9) 0.019(7) 0.005(8) -0.029(8) C29 0.057(10) 0.046(9) 0.037(8) 0.014(7) 0.011(8) -0.023(8) C30 0.062(11) 0.032(8) 0.042(9) 0.002(7) 0.008(8) -0.020(7) C31 0.056(11) 0.069(11) 0.041(9) 0.009(8) 0.002(8) -0.022(9) C32 0.063(11) 0.045(9) 0.037(9) 0.026(7) 0.006(8) -0.010(8) C33 0.062(11) 0.029(8) 0.045(9) 0.009(7) -0.007(8) -0.019(7) C34 0.056(10) 0.035(8) 0.044(9) 0.007(7) 0.006(8) -0.018(7) C35 0.060(10) 0.037(8) 0.038(8) 0.011(7) 0.003(8) -0.025(8) C36 0.107(15) 0.068(13) 0.064(13) 0.035(10) -0.027(12) -0.047(11) C39 0.187(19) 0.186(19) 0.189(19) -0.002(5) 0.053(7) 0.001(5) C40 0.047(17) 0.24(5) 0.41(7) 0.17(5) -0.01(3) 0.02(2) C41 0.043(9) 0.030(8) 0.053(10) 0.001(7) 0.019(8) -0.020(6) C42 0.090(15) 0.044(9) 0.051(11) -0.010(8) 0.021(10) -0.030(10) C43 0.049(10) 0.058(10) 0.040(9) 0.000(7) 0.013(8) -0.031(8) C44 0.038(8) 0.026(7) 0.041(8) 0.003(6) 0.002(7) -0.011(6) C45 0.049(10) 0.047(9) 0.045(9) -0.007(7) 0.009(8) -0.025(8) C46 0.043(10) 0.069(12) 0.074(13) 0.007(9) 0.023(9) -0.024(9) C47 0.036(9) 0.031(8) 0.047(9) 0.010(7) -0.006(7) -0.014(7) C49 0.035(8) 0.009(6) 0.047(9) 0.000(5) 0.002(7) -0.001(5) C50 0.082(12) 0.038(8) 0.012(6) -0.002(6) 0.011(7) -0.026(8) N1 0.051(12) 0.29(4) 0.13(2) 0.13(2) -0.038(12) -0.039(14) N2 0.034(8) 0.097(12) 0.042(8) 0.003(8) -0.002(6) 0.029(8) O1 0.038(6) 0.027(5) 0.032(5) 0.000(4) -0.002(4) -0.007(4) O2 0.043(7) 0.128(11) 0.038(7) 0.010(7) 0.016(6) 0.025(7) O3 0.034(5) 0.028(5) 0.032(5) -0.001(4) 0.005(4) -0.004(4) O4 0.029(5) 0.037(5) 0.042(6) -0.006(4) 0.011(4) -0.013(4) O5 0.047(6) 0.031(5) 0.037(6) -0.004(4) 0.005(5) -0.016(5) O6 0.023(5) 0.073(8) 0.053(7) 0.009(5) 0.000(5) 0.002(5) O7 0.041(6) 0.025(5) 0.058(7) 0.015(5) 0.020(5) -0.004(4) O8 0.034(5) 0.023(5) 0.043(6) 0.013(4) 0.006(4) -0.006(4) O9 0.028(5) 0.032(5) 0.043(6) 0.010(4) 0.008(4) -0.005(4) O10 0.027(5) 0.021(4) 0.035(5) 0.008(4) 0.001(4) -0.001(4) O11 0.048(7) 0.049(7) 0.174(15) -0.028(8) 0.060(9) -0.006(6) O12 0.046(7) 0.062(7) 0.064(8) -0.029(6) -0.008(6) 0.012(6) O13 0.037(7) 0.048(7) 0.155(14) -0.021(8) 0.041(8) -0.004(6) O14 0.042(6) 0.064(7) 0.032(6) 0.027(5) -0.009(5) -0.001(5) O15 0.055(8) 0.027(6) 0.166(15) -0.002(7) 0.058(9) -0.007(5) O16 0.061(7) 0.105(10) 0.037(6) -0.031(6) 0.032(6) -0.055(7) O17 0.054(7) 0.111(10) 0.036(6) -0.035(6) 0.030(5) -0.053(7) O18 0.102(14) 0.013(6) 0.057(10) 0.000 0.020(9) 0.000 O19 0.032(6) 0.055(7) 0.056(7) -0.012(5) 0.014(5) 0.006(5) O20 0.049(7) 0.119(11) 0.050(7) -0.041(7) 0.028(6) -0.047(7) O21 0.108(11) 0.036(6) 0.051(7) 0.004(5) -0.031(7) -0.007(7) O22 0.071(9) 0.085(9) 0.049(7) 0.024(6) 0.032(7) 0.005(7) O23 0.091(10) 0.047(7) 0.072(9) 0.017(6) -0.035(7) 0.005(7) O24 0.033(6) 0.093(9) 0.081(9) 0.030(7) 0.017(6) 0.004(6) O25 0.050(7) 0.107(10) 0.065(8) 0.035(7) 0.014(6) 0.044(7) O26 0.065(13) 0.066(12) 0.122(18) 0.000 0.022(12) 0.000 O27 0.048(8) 0.119(12) 0.076(9) 0.003(8) 0.012(7) 0.047(8) O28 0.106(12) 0.077(10) 0.114(13) -0.016(9) 0.031(10) -0.006(9) O29 0.108(7) 0.108(7) 0.113(7) -0.001(5) 0.036(5) -0.002(5) O30 0.101(11) 0.070(9) 0.105(12) -0.022(8) 0.036(9) -0.030(8) O31 0.095(12) 0.078(10) 0.092(12) -0.010(8) 0.016(10) -0.004(8) O32 0.111(11) 0.026(6) 0.046(7) 0.012(5) -0.037(7) -0.002(6) O33 0.054(7) 0.087(9) 0.060(8) 0.024(7) 0.018(6) 0.044(7) N3 0.062(9) 0.053(8) 0.040(8) -0.001(6) 0.007(7) -0.008(7) O51 0.064(8) 0.074(8) 0.043(7) -0.006(6) 0.019(6) -0.005(7) C51 0.040(12) 0.13(2) 0.16(3) -0.095(19) -0.030(14) 0.022(12) C52 0.088(15) 0.070(13) 0.082(14) -0.016(11) 0.043(12) -0.024(11) C53 0.044(10) 0.056(10) 0.052(10) 0.007(8) 0.014(8) -0.009(9) _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 Cu1 O3 1.952(9) . ? Cu1 O4 1.954(9) . ? Cu1 O5 1.971(9) 2_455 ? Cu1 O1 1.981(8) 2_455 ? Cu1 O2 2.137(11) . ? Cu1 Cu1 2.633(3) 2_455 ? Cu2 O7 1.934(9) 2 ? Cu2 O10 1.942(8) 2 ? Cu2 O9 1.968(9) . ? Cu2 O8 1.968(8) . ? Cu2 O6 2.142(10) . ? Cu2 Cu2 2.633(3) 2 ? W1 O18 1.693(12) . ? W1 O17 1.893(10) . ? W1 O17 1.893(10) 2_556 ? W1 O20 1.904(10) . ? W1 O20 1.904(10) 2_556 ? W1 O30 2.483(13) . ? W1 O30 2.483(13) 2_556 ? W2 O14 1.700(9) . ? W2 O15 1.873(10) . ? W2 O16 1.885(10) . ? W2 O17 1.895(10) . ? W2 O13 1.905(11) . ? W2 O30 2.491(16) . ? W2 O29 2.505(18) . ? W3 O19 1.683(9) . ? W3 O21 1.901(11) . ? W3 O20 1.906(11) . ? W3 O16 1.919(10) . ? W3 O32 1.927(10) . ? W3 O30 2.458(16) . ? W3 O31 2.511(16) . ? W4 O12 1.696(10) . ? W4 O33 1.880(12) . ? W4 O27 1.903(12) . ? W4 O15 1.928(10) . ? W4 O11 1.933(12) . ? W4 O28 2.492(17) 2_556 ? W4 O29 2.519(18) . ? W5 O22 1.692(11) . ? W5 O23 1.887(12) . ? W5 O11 1.889(12) 2_556 ? W5 O13 1.906(11) 2_556 ? W5 O21 1.910(11) . ? W5 O31 2.475(17) . ? W5 O29 2.488(19) 2_556 ? W6 O26 1.707(19) . ? W6 O25 1.872(11) . ? W6 O25 1.872(11) 2_556 ? W6 O27 1.885(13) . ? W6 O27 1.885(13) 2_556 ? W6 O28 2.492(15) . ? W6 O28 2.492(14) 2_556 ? W7 O24 1.680(11) . ? W7 O25 1.887(11) . ? W7 O33 1.896(12) . ? W7 O23 1.908(13) . ? W7 O32 1.921(10) . ? W7 O28 2.419(17) 2_556 ? W7 O31 2.452(15) . ? P1 O29 1.49(2) 2_556 ? P1 O29 1.49(2) . ? P1 O31 1.490(18) . ? P1 O31 1.490(18) 2_556 ? P1 O28 1.500(16) 2_556 ? P1 O28 1.500(16) . ? P1 O30 1.529(16) 2_556 ? P1 O30 1.529(16) . ? C1 O10 1.230(14) . ? C1 O9 1.277(14) . ? C1 C2 1.493(16) . ? C2 C3 1.402(17) . ? C2 C7 1.410(17) . ? C3 C4 1.383(17) . ? C3 H3A 0.9300 . ? C4 C5 1.392(18) . ? C4 H4A 0.9300 . ? C5 C6 1.356(18) . ? C5 C8 1.487(17) . ? C6 C7 1.371(18) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.410(18) . ? C8 C9 1.422(18) . ? C9 C10 1.389(17) . ? C9 H9A 0.9300 . ? C10 C11 1.406(17) . ? C10 C14 1.449(18) . ? C11 C12 1.369(18) . ? C11 H11A 0.9300 . ? C12 C13 1.405(17) . ? C12 C18 1.557(18) . ? C13 H13A 0.9300 . ? C14 C15 1.398(17) . ? C14 C17 1.455(19) . ? C15 C16 1.386(18) . ? C15 H15A 0.9300 . ? C16 C49 1.369(18) 1_665 ? C16 H16A 0.9300 . ? C17 C50 1.442(19) 1_665 ? C17 H17A 0.9300 . ? C18 N2 1.414(19) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.430(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N2 1.390(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.42(3) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N2 1.416(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O8 1.233(15) . ? C23 O7 1.288(16) . ? C23 C24 1.514(17) . ? C24 C25 1.37(2) . ? C24 C27 1.400(19) . ? C25 C26 1.370(19) . ? C25 H25A 0.9300 . ? C26 C29 1.36(2) . ? C26 H26A 0.9300 . ? C27 C28 1.382(18) . ? C27 H27A 0.9300 . ? C28 C29 1.39(2) . ? C28 H28A 0.9300 . ? C29 C30 1.522(18) . ? C30 C31 1.38(2) . ? C30 C35 1.413(19) . ? C31 C32 1.40(2) . ? C31 H31A 0.9300 . ? C32 C33 1.38(2) . ? C32 C36 1.50(2) . ? C33 C34 1.35(2) . ? C33 H33A 0.9300 . ? C34 C35 1.409(18) . ? C34 C41 1.49(2) . ? C35 H35A 0.9300 . ? C36 N1 1.55(3) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 N1 1.400(10) . ? C37 C38 1.446(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N1 1.408(10) . ? C39 C40 1.444(10) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.34(2) . ? C41 C46 1.41(2) . ? C42 C43 1.37(2) . ? C42 H42A 0.9300 . ? C43 C44 1.40(2) . ? C43 H43A 0.9300 . ? C44 C45 1.36(2) . ? C44 C47 1.510(18) . ? C45 C46 1.38(2) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 O4 1.262(18) . ? C47 O5 1.275(18) . ? C49 C16 1.369(18) 1_445 ? C49 C50 1.405(18) . ? C49 C48 1.513(17) . ? C50 C17 1.442(19) 1_445 ? C50 H50A 0.9300 . ? O1 C48 1.232(15) . ? O1 Cu1 1.981(8) 2_455 ? O2 H2A 0.8500 . ? O2 H2B 0.8501 . ? O3 C48 1.288(15) . ? O5 Cu1 1.971(9) 2_455 ? O6 H1O6 0.8501 . ? O6 H2O6 0.8504 . ? O7 Cu2 1.934(9) 2 ? O10 Cu2 1.942(8) 2 ? O11 W5 1.889(12) 2_556 ? O13 W5 1.906(11) 2_556 ? O28 O31 1.70(2) 2_556 ? O28 O29 1.75(2) 2_556 ? O28 O28 1.76(3) 2_556 ? O28 W7 2.419(16) 2_556 ? O28 W4 2.492(17) 2_556 ? O29 O31 1.69(2) 2_556 ? O29 O30 1.74(2) . ? O29 O28 1.75(2) 2_556 ? O29 W5 2.488(19) 2_556 ? O30 O31 1.74(2) . ? O30 O30 1.79(3) 2_556 ? O31 O29 1.69(2) 2_556 ? O31 O28 1.70(2) 2_556 ? N3 C53 1.35(2) . ? N3 C52 1.45(2) . ? N3 C51 1.48(2) . ? N5 C59 1.30(4) . ? N5 C57 1.35(3) . ? N5 C58 1.63(4) . ? N6 C60 1.38(3) . ? N6 C62 1.39(5) . ? N6 C61 1.43(4) . ? O51 C53 1.279(19) . ? O53 C59 1.31(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9300 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C62 O54 1.208(10) . ? C62 H62A 0.9300 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? 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 O3 Cu1 O4 171.7(4) . . ? O3 Cu1 O5 88.1(4) . 2_455 ? O4 Cu1 O5 89.5(4) . 2_455 ? O3 Cu1 O1 91.7(4) . 2_455 ? O4 Cu1 O1 88.7(4) . 2_455 ? O5 Cu1 O1 165.7(4) 2_455 2_455 ? O3 Cu1 O2 93.8(4) . . ? O4 Cu1 O2 94.4(4) . . ? O5 Cu1 O2 99.3(4) 2_455 . ? O1 Cu1 O2 95.0(4) 2_455 . ? O3 Cu1 Cu1 86.1(3) . 2_455 ? O4 Cu1 Cu1 85.7(3) . 2_455 ? O5 Cu1 Cu1 83.0(3) 2_455 2_455 ? O1 Cu1 Cu1 82.7(3) 2_455 2_455 ? O2 Cu1 Cu1 177.7(3) . 2_455 ? O7 Cu2 O10 172.0(4) 2 2 ? O7 Cu2 O9 90.9(4) 2 . ? O10 Cu2 O9 88.4(4) 2 . ? O7 Cu2 O8 88.5(4) 2 . ? O10 Cu2 O8 90.2(4) 2 . ? O9 Cu2 O8 164.7(4) . . ? O7 Cu2 O6 94.2(4) 2 . ? O10 Cu2 O6 93.8(4) 2 . ? O9 Cu2 O6 95.6(4) . . ? O8 Cu2 O6 99.6(4) . . ? O7 Cu2 Cu2 85.0(3) 2 2 ? O10 Cu2 Cu2 87.0(3) 2 2 ? O9 Cu2 Cu2 81.0(3) . 2 ? O8 Cu2 Cu2 83.8(3) . 2 ? O6 Cu2 Cu2 176.5(3) . 2 ? O18 W1 O17 102.5(4) . . ? O18 W1 O17 102.5(4) . 2_556 ? O17 W1 O17 154.9(8) . 2_556 ? O18 W1 O20 101.4(4) . . ? O17 W1 O20 88.3(4) . . ? O17 W1 O20 86.8(5) 2_556 . ? O18 W1 O20 101.4(4) . 2_556 ? O17 W1 O20 86.8(5) . 2_556 ? O17 W1 O20 88.3(4) 2_556 2_556 ? O20 W1 O20 157.3(8) . 2_556 ? O18 W1 O30 158.9(4) . . ? O17 W1 O30 63.9(5) . . ? O17 W1 O30 92.0(6) 2_556 . ? O20 W1 O30 63.8(5) . . ? O20 W1 O30 94.2(6) 2_556 . ? O18 W1 O30 158.9(4) . 2_556 ? O17 W1 O30 92.0(6) . 2_556 ? O17 W1 O30 63.9(5) 2_556 2_556 ? O20 W1 O30 94.2(6) . 2_556 ? O20 W1 O30 63.8(5) 2_556 2_556 ? O30 W1 O30 42.2(7) . 2_556 ? O14 W2 O15 101.4(6) . . ? O14 W2 O16 102.4(6) . . ? O15 W2 O16 87.5(5) . . ? O14 W2 O17 104.3(6) . . ? O15 W2 O17 154.2(6) . . ? O16 W2 O17 89.3(4) . . ? O14 W2 O13 101.0(6) . . ? O15 W2 O13 87.2(5) . . ? O16 W2 O13 156.6(6) . . ? O17 W2 O13 85.6(5) . . ? O14 W2 O30 160.6(5) . . ? O15 W2 O30 92.0(6) . . ? O16 W2 O30 64.0(5) . . ? O17 W2 O30 63.7(5) . . ? O13 W2 O30 93.4(6) . . ? O14 W2 O29 158.7(6) . . ? O15 W2 O29 64.0(6) . . ? O16 W2 O29 92.9(6) . . ? O17 W2 O29 90.6(6) . . ? O13 W2 O29 64.4(6) . . ? O30 W2 O29 40.7(5) . . ? O19 W3 O21 101.1(6) . . ? O19 W3 O20 100.5(5) . . ? O21 W3 O20 87.6(5) . . ? O19 W3 O16 101.3(5) . . ? O21 W3 O16 157.5(6) . . ? O20 W3 O16 86.8(5) . . ? O19 W3 O32 100.0(6) . . ? O21 W3 O32 88.8(5) . . ? O20 W3 O32 159.5(6) . . ? O16 W3 O32 88.9(5) . . ? O19 W3 O30 158.5(5) . . ? O21 W3 O30 93.7(6) . . ? O20 W3 O30 64.3(5) . . ? O16 W3 O30 64.4(5) . . ? O32 W3 O30 95.8(6) . . ? O19 W3 O31 160.4(5) . . ? O21 W3 O31 65.2(6) . . ? O20 W3 O31 93.1(5) . . ? O16 W3 O31 93.4(6) . . ? O32 W3 O31 67.1(6) . . ? O30 W3 O31 41.1(5) . . ? O12 W4 O33 103.6(6) . . ? O12 W4 O27 102.1(6) . . ? O33 W4 O27 89.6(5) . . ? O12 W4 O15 102.2(6) . . ? O33 W4 O15 87.0(5) . . ? O27 W4 O15 155.5(7) . . ? O12 W4 O11 99.3(6) . . ? O33 W4 O11 156.9(6) . . ? O27 W4 O11 88.5(6) . . ? O15 W4 O11 85.4(5) . . ? O12 W4 O28 161.1(6) . 2_556 ? O33 W4 O28 64.0(5) . 2_556 ? O27 W4 O28 65.2(5) . 2_556 ? O15 W4 O28 91.7(6) . 2_556 ? O11 W4 O28 94.5(6) . 2_556 ? O12 W4 O29 158.0(6) . . ? O33 W4 O29 92.4(6) . . ? O27 W4 O29 92.9(6) . . ? O15 W4 O29 63.1(6) . . ? O11 W4 O29 64.7(6) . . ? O28 W4 O29 40.9(5) 2_556 . ? O22 W5 O23 100.5(7) . . ? O22 W5 O11 99.4(6) . 2_556 ? O23 W5 O11 88.7(6) . 2_556 ? O22 W5 O13 102.2(6) . 2_556 ? O23 W5 O13 157.4(7) . 2_556 ? O11 W5 O13 87.2(5) 2_556 2_556 ? O22 W5 O21 102.0(6) . . ? O23 W5 O21 88.4(5) . . ? O11 W5 O21 158.5(6) 2_556 . ? O13 W5 O21 87.3(5) 2_556 . ? O22 W5 O31 160.2(6) . . ? O23 W5 O31 64.9(6) . . ? O11 W5 O31 93.6(6) 2_556 . ? O13 W5 O31 93.2(6) 2_556 . ? O21 W5 O31 65.9(5) . . ? O22 W5 O29 159.8(7) . 2_556 ? O23 W5 O29 93.3(7) . 2_556 ? O11 W5 O29 65.9(6) 2_556 2_556 ? O13 W5 O29 64.8(6) 2_556 2_556 ? O21 W5 O29 93.0(6) . 2_556 ? O31 W5 O29 39.9(6) . 2_556 ? O26 W6 O25 101.5(4) . . ? O26 W6 O25 101.5(4) . 2_556 ? O25 W6 O25 156.9(9) . 2_556 ? O26 W6 O27 101.2(5) . . ? O25 W6 O27 87.8(5) . . ? O25 W6 O27 87.8(6) 2_556 . ? O26 W6 O27 101.2(5) . 2_556 ? O25 W6 O27 87.8(6) . 2_556 ? O25 W6 O27 87.8(5) 2_556 2_556 ? O27 W6 O27 157.6(9) . 2_556 ? O26 W6 O28 159.3(4) . . ? O25 W6 O28 93.9(6) . . ? O25 W6 O28 63.8(6) 2_556 . ? O27 W6 O28 93.0(6) . . ? O27 W6 O28 65.4(6) 2_556 . ? O26 W6 O28 159.3(4) . 2_556 ? O25 W6 O28 63.8(6) . 2_556 ? O25 W6 O28 93.9(6) 2_556 2_556 ? O27 W6 O28 65.4(6) . 2_556 ? O27 W6 O28 93.0(6) 2_556 2_556 ? O28 W6 O28 41.3(7) . 2_556 ? O24 W7 O25 101.1(6) . . ? O24 W7 O33 101.3(6) . . ? O25 W7 O33 88.0(5) . . ? O24 W7 O23 99.9(6) . . ? O25 W7 O23 89.6(5) . . ? O33 W7 O23 158.8(6) . . ? O24 W7 O32 97.2(6) . . ? O25 W7 O32 161.6(6) . . ? O33 W7 O32 88.0(5) . . ? O23 W7 O32 87.7(5) . . ? O24 W7 O28 160.3(6) . 2_556 ? O25 W7 O28 65.3(5) . 2_556 ? O33 W7 O28 65.4(6) . 2_556 ? O23 W7 O28 94.5(6) . 2_556 ? O32 W7 O28 96.8(6) . 2_556 ? O24 W7 O31 158.8(6) . . ? O25 W7 O31 93.9(6) . . ? O33 W7 O31 94.0(6) . . ? O23 W7 O31 65.2(6) . . ? O32 W7 O31 68.5(6) . . ? O28 W7 O31 40.9(5) 2_556 . ? O29 P1 O29 178.4(12) 2_556 . ? O29 P1 O31 69.4(9) 2_556 . ? O29 P1 O31 110.7(9) . . ? O29 P1 O31 110.7(9) 2_556 2_556 ? O29 P1 O31 69.4(9) . 2_556 ? O31 P1 O31 178.9(11) . 2_556 ? O29 P1 O28 109.5(9) 2_556 2_556 ? O29 P1 O28 71.9(9) . 2_556 ? O31 P1 O28 69.4(8) . 2_556 ? O31 P1 O28 109.7(9) 2_556 2_556 ? O29 P1 O28 71.9(9) 2_556 . ? O29 P1 O28 109.5(9) . . ? O31 P1 O28 109.7(9) . . ? O31 P1 O28 69.4(8) 2_556 . ? O28 P1 O28 71.8(12) 2_556 . ? O29 P1 O30 70.4(8) 2_556 2_556 ? O29 P1 O30 108.3(9) . 2_556 ? O31 P1 O30 110.4(8) . 2_556 ? O31 P1 O30 70.5(8) 2_556 2_556 ? O28 P1 O30 179.8(9) 2_556 2_556 ? O28 P1 O30 108.3(8) . 2_556 ? O29 P1 O30 108.3(9) 2_556 . ? O29 P1 O30 70.4(8) . . ? O31 P1 O30 70.5(8) . . ? O31 P1 O30 110.4(8) 2_556 . ? O28 P1 O30 108.3(8) 2_556 . ? O28 P1 O30 179.8(9) . . ? O30 P1 O30 71.6(10) 2_556 . ? O10 C1 O9 125.0(11) . . ? O10 C1 C2 118.6(11) . . ? O9 C1 C2 116.3(11) . . ? C3 C2 C7 118.0(11) . . ? C3 C2 C1 121.6(11) . . ? C7 C2 C1 120.4(11) . . ? C4 C3 C2 119.9(11) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.9(12) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 119.1(11) . . ? C6 C5 C8 121.1(11) . . ? C4 C5 C8 119.8(11) . . ? C5 C6 C7 121.8(12) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C6 C7 C2 120.3(12) . . ? C6 C7 H7A 119.8 . . ? C2 C7 H7A 119.8 . . ? C13 C8 C9 118.7(11) . . ? C13 C8 C5 120.6(11) . . ? C9 C8 C5 120.7(11) . . ? C10 C9 C8 121.1(12) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C11 118.8(12) . . ? C9 C10 C14 119.6(12) . . ? C11 C10 C14 121.6(11) . . ? C12 C11 C10 121.0(12) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 121.0(12) . . ? C11 C12 C18 123.1(11) . . ? C13 C12 C18 115.9(12) . . ? C12 C13 C8 119.3(12) . . ? C12 C13 H13A 120.4 . . ? C8 C13 H13A 120.4 . . ? C15 C14 C10 124.2(12) . . ? C15 C14 C17 118.5(12) . . ? C10 C14 C17 117.2(11) . . ? C16 C15 C14 122.2(12) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C49 C16 C15 120.9(13) 1_665 . ? C49 C16 H16A 119.6 1_665 . ? C15 C16 H16A 119.6 . . ? C50 C17 C14 117.3(12) 1_665 . ? C50 C17 H17A 121.3 1_665 . ? C14 C17 H17A 121.3 . . ? N2 C18 C12 115.4(12) . . ? N2 C18 H18A 108.4 . . ? C12 C18 H18A 108.4 . . ? N2 C18 H18B 108.4 . . ? C12 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C19 99(2) . . ? N2 C20 H20A 111.9 . . ? C19 C20 H20A 111.9 . . ? N2 C20 H20B 111.9 . . ? C19 C20 H20B 111.9 . . ? H20A C20 H20B 109.6 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 C21 122.8(17) . . ? N2 C22 H22A 106.6 . . ? C21 C22 H22A 106.6 . . ? N2 C22 H22B 106.6 . . ? C21 C22 H22B 106.6 . . ? H22A C22 H22B 106.6 . . ? O8 C23 O7 126.5(11) . . ? O8 C23 C24 118.3(12) . . ? O7 C23 C24 115.2(12) . . ? C25 C24 C27 118.7(12) . . ? C25 C24 C23 120.9(13) . . ? C27 C24 C23 120.5(13) . . ? C26 C25 C24 121.2(15) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C29 C26 C25 120.8(15) . . ? C29 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C28 C27 C24 119.2(14) . . ? C28 C27 H27A 120.4 . . ? C24 C27 H27A 120.4 . . ? C27 C28 C29 120.8(14) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C26 C29 C28 119.2(13) . . ? C26 C29 C30 120.8(14) . . ? C28 C29 C30 119.9(13) . . ? C31 C30 C35 119.0(13) . . ? C31 C30 C29 120.7(14) . . ? C35 C30 C29 120.3(13) . . ? C30 C31 C32 121.2(15) . . ? C30 C31 H31A 119.4 . . ? C32 C31 H31A 119.4 . . ? C33 C32 C31 118.4(14) . . ? C33 C32 C36 122.2(13) . . ? C31 C32 C36 119.4(15) . . ? C34 C33 C32 121.6(13) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 120.8(14) . . ? C33 C34 C41 121.6(13) . . ? C35 C34 C41 117.6(13) . . ? C34 C35 C30 118.5(13) . . ? C34 C35 H35A 120.7 . . ? C30 C35 H35A 120.7 . . ? C32 C36 N1 110.3(18) . . ? C32 C36 H36A 109.6 . . ? N1 C36 H36A 109.6 . . ? C32 C36 H36B 109.6 . . ? N1 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? N1 C37 C38 102(3) . . ? N1 C37 H37A 111.4 . . ? C38 C37 H37A 111.4 . . ? N1 C37 H37B 111.4 . . ? C38 C37 H37B 111.4 . . ? H37A C37 H37B 109.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 C40 120(4) . . ? N1 C39 H39A 107.4 . . ? C40 C39 H39A 107.4 . . ? N1 C39 H39B 107.4 . . ? C40 C39 H39B 107.4 . . ? H39A C39 H39B 106.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 116.0(14) . . ? C42 C41 C34 122.3(15) . . ? C46 C41 C34 121.6(13) . . ? C41 C42 C43 124.7(16) . . ? C41 C42 H42A 117.7 . . ? C43 C42 H42A 117.7 . . ? C42 C43 C44 118.1(14) . . ? C42 C43 H43A 121.0 . . ? C44 C43 H43A 121.0 . . ? C45 C44 C43 119.8(13) . . ? C45 C44 C47 120.0(14) . . ? C43 C44 C47 120.2(13) . . ? C44 C45 C46 119.7(15) . . ? C44 C45 H45A 120.2 . . ? C46 C45 H45A 120.2 . . ? C45 C46 C41 121.7(15) . . ? C45 C46 H46A 119.2 . . ? C41 C46 H46A 119.2 . . ? O4 C47 O5 125.3(12) . . ? O4 C47 C44 117.7(13) . . ? O5 C47 C44 117.0(14) . . ? C16 C49 C50 120.1(12) 1_445 . ? C16 C49 C48 123.3(12) 1_445 . ? C50 C49 C48 116.6(12) . . ? C49 C50 C17 120.9(12) . 1_445 ? C49 C50 H50A 119.5 . . ? C17 C50 H50A 119.5 1_445 . ? C37 N1 C39 103(3) . . ? C37 N1 C36 113(2) . . ? C39 N1 C36 114(2) . . ? C20 N2 C18 118.0(17) . . ? C20 N2 C22 120.6(19) . . ? C18 N2 C22 113.3(14) . . ? C48 O1 Cu1 123.5(9) . 2_455 ? Cu1 O2 H2A 128.6 . . ? Cu1 O2 H2B 122.6 . . ? H2A O2 H2B 107.7 . . ? C48 O3 Cu1 119.9(8) . . ? C47 O4 Cu1 121.8(9) . . ? C47 O5 Cu1 123.7(9) . 2_455 ? Cu2 O6 H1O6 131.1 . . ? Cu2 O6 H2O6 107.5 . . ? H1O6 O6 H2O6 107.7 . . ? C23 O7 Cu2 121.8(8) . 2 ? C23 O8 Cu2 122.7(8) . . ? C1 O9 Cu2 125.8(8) . . ? C1 O10 Cu2 121.0(8) . 2 ? W5 O11 W4 138.2(8) 2_556 . ? W2 O13 W5 138.8(8) . 2_556 ? W2 O15 W4 141.3(9) . . ? W2 O16 W3 138.9(7) . . ? W1 O17 W2 139.8(7) . . ? W1 O20 W3 139.0(7) . . ? W3 O21 W5 137.3(8) . . ? W5 O23 W7 137.6(8) . . ? W6 O25 W7 139.0(7) . . ? W6 O27 W4 138.1(8) . . ? P1 O28 O31 55.1(8) . 2_556 ? P1 O28 O29 53.7(8) . 2_556 ? O31 O28 O29 90.2(10) 2_556 2_556 ? P1 O28 O28 54.1(6) . 2_556 ? O31 O28 O28 89.9(11) 2_556 2_556 ? O29 O28 O28 87.9(12) 2_556 2_556 ? P1 O28 W7 125.6(9) . 2_556 ? O31 O28 W7 70.6(8) 2_556 2_556 ? O29 O28 W7 132.7(10) 2_556 2_556 ? O28 O28 W7 132.8(14) 2_556 2_556 ? P1 O28 W4 124.0(9) . 2_556 ? O31 O28 W4 133.3(10) 2_556 2_556 ? O29 O28 W4 70.4(8) 2_556 2_556 ? O28 O28 W4 129.4(14) 2_556 2_556 ? W7 O28 W4 91.7(5) 2_556 2_556 ? P1 O28 W6 123.5(8) . . ? O31 O28 W6 131.3(10) 2_556 . ? O29 O28 W6 130.3(11) 2_556 . ? O28 O28 W6 69.3(4) 2_556 . ? W7 O28 W6 91.6(5) 2_556 . ? W4 O28 W6 90.4(5) 2_556 . ? P1 O29 O31 55.5(9) . 2_556 ? P1 O29 O30 56.0(8) . . ? O31 O29 O30 92.6(12) 2_556 . ? P1 O29 O28 54.4(8) . 2_556 ? O31 O29 O28 90.4(12) 2_556 2_556 ? O30 O29 O28 89.4(12) . 2_556 ? P1 O29 W5 125.1(11) . 2_556 ? O31 O29 W5 69.7(9) 2_556 2_556 ? O30 O29 W5 132.9(10) . 2_556 ? O28 O29 W5 132.0(10) 2_556 2_556 ? P1 O29 W2 125.2(9) . . ? O31 O29 W2 133.0(10) 2_556 . ? O30 O29 W2 69.2(8) . . ? O28 O29 W2 130.3(11) 2_556 . ? W5 O29 W2 91.2(6) 2_556 . ? P1 O29 W4 123.1(9) . . ? O31 O29 W4 130.0(10) 2_556 . ? O30 O29 W4 130.0(11) . . ? O28 O29 W4 68.7(8) 2_556 . ? W5 O29 W4 91.0(6) 2_556 . ? W2 O29 W4 91.1(6) . . ? P1 O30 O29 53.6(8) . . ? P1 O30 O31 53.7(7) . . ? O29 O30 O31 89.3(10) . . ? P1 O30 O30 54.2(5) . 2_556 ? O29 O30 O30 87.7(11) . 2_556 ? O31 O30 O30 89.1(11) . 2_556 ? P1 O30 W3 124.8(8) . . ? O29 O30 W3 132.8(10) . . ? O31 O30 W3 71.1(8) . . ? O30 O30 W3 132.6(12) 2_556 . ? P1 O30 W1 123.1(8) . . ? O29 O30 W1 129.8(10) . . ? O31 O30 W1 131.7(9) . . ? O30 O30 W1 68.9(4) 2_556 . ? W3 O30 W1 92.5(5) . . ? P1 O30 W2 123.7(8) . . ? O29 O30 W2 70.1(8) . . ? O31 O30 W2 132.9(9) . . ? O30 O30 W2 129.8(12) 2_556 . ? W3 O30 W2 92.1(5) . . ? W1 O30 W2 91.3(5) . . ? P1 O31 O29 55.2(9) . 2_556 ? P1 O31 O28 55.6(8) . 2_556 ? O29 O31 O28 91.8(12) 2_556 2_556 ? P1 O31 O30 55.8(8) . . ? O29 O31 O30 90.6(11) 2_556 . ? O28 O31 O30 90.9(11) 2_556 . ? P1 O31 W7 124.1(8) . . ? O29 O31 W7 133.0(9) 2_556 . ? O28 O31 W7 68.5(7) 2_556 . ? O30 O31 W7 130.0(10) . . ? P1 O31 W5 125.7(9) . . ? O29 O31 W5 70.5(9) 2_556 . ? O28 O31 W5 132.8(9) 2_556 . ? O30 O31 W5 131.0(9) . . ? W7 O31 W5 91.8(6) . . ? P1 O31 W3 123.6(8) . . ? O29 O31 W3 130.9(9) 2_556 . ? O28 O31 W3 130.0(10) 2_556 . ? O30 O31 W3 67.8(7) . . ? W7 O31 W3 90.8(6) . . ? W5 O31 W3 90.8(5) . . ? W7 O32 W3 133.4(8) . . ? W4 O33 W7 137.9(7) . . ? C53 N3 C52 123.2(16) . . ? C53 N3 C51 121.8(15) . . ? C52 N3 C51 115.0(15) . . ? C59 N5 C57 125(4) . . ? C59 N5 C58 110(3) . . ? C57 N5 C58 124(3) . . ? C60 N6 C62 128(3) . . ? C60 N6 C61 110(3) . . ? C62 N6 C61 119(3) . . ? O1 C48 O3 127.1(12) . . ? O1 C48 C49 118.6(12) . . ? O3 C48 C49 114.1(11) . . ? N3 C51 H51A 109.5 . . ? N3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N3 C52 H52A 109.5 . . ? N3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O51 C53 N3 121.6(17) . . ? O51 C53 H53A 119.2 . . ? N3 C53 H53A 119.2 . . ? N5 C57 H57A 109.5 . . ? N5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N5 C58 H58A 109.5 . . ? N5 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N5 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N5 C59 O53 129(4) . . ? N5 C59 H59A 115.3 . . ? O53 C59 H59A 115.3 . . ? N6 C60 H60A 109.5 . . ? N6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O54 C62 N6 122(5) . . ? O54 C62 H62A 118.8 . . ? N6 C62 H62A 118.8 . . ? N6 C61 H61A 109.5 . . ? N6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.920 _refine_diff_density_min -3.272 _refine_diff_density_rms 0.536 _database_code_depnum_ccdc_archive 'CCDC 943146'