# 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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN _publ_section_title ; Ferrimagnetism in Layer Compound Cu3(ImhedpH)2*2H2O [ImhedpH4 = (1-C3H3N2)CH2C(OH)(PO3H2)2] ; loop_ _publ_author_name 'Li-Min Zheng.' 'Deng-Ke Cao.' 'Xiao-Ji Xie.' # Attachment 'cu1-new.cif' data_60721d _database_code_depnum_ccdc_archive 'CCDC 683971' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Cu N4 O15 P4, 2(H2 O)' _chemical_formula_sum 'C10 H24 Cu N4 O17 P4' _chemical_formula_weight 659.75 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 11.9298(17) _cell_length_b 9.8104(15) _cell_length_c 18.801(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.790(3) _cell_angle_gamma 90.00 _cell_volume 2189.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 815 _cell_measurement_theta_min 2.6895 _cell_measurement_theta_max 21.867 _exptl_crystal_description blocky _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 1.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS,(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Apex CCD ' _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 5371 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2108 _reflns_number_gt 1426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. ; _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^)+(0.0663P)^2^] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2108 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3928(4) 0.7982(5) 0.5569(2) 0.0358(10) Uani 1 1 d . . . H1A H 0.4034 0.7327 0.5927 0.043 Uiso 1 1 calc R . . C2 C 0.3707(3) 0.8934(5) 0.4524(3) 0.0351(10) Uani 1 1 d . . . H2C H 0.3640 0.9054 0.4031 0.042 Uiso 1 1 calc R . . C3 C 0.3639(4) 0.9890(5) 0.5009(3) 0.0414(11) Uani 1 1 d . . . H3B H 0.3512 1.0812 0.4918 0.050 Uiso 1 1 calc R . . C4 C 0.3714(4) 0.9932(5) 0.6372(3) 0.0428(11) Uani 1 1 d . . . H4A H 0.3883 1.0897 0.6343 0.051 Uiso 1 1 calc R . . H4B H 0.4269 0.9524 0.6720 0.051 Uiso 1 1 calc R . . C5 C 0.2521(4) 0.9748(5) 0.6621(2) 0.0392(11) Uani 1 1 d . . . Cu1 Cu 0.0000 1.00654(8) 0.7500 0.0373(3) Uani 1 2 d S . . N1 N 0.3787(3) 0.9297(4) 0.5671(2) 0.0418(9) Uani 1 1 d . . . N2 N 0.3895(3) 0.7744(4) 0.48809(19) 0.0315(8) Uani 1 1 d . . . H2B H 0.390(4) 0.680(5) 0.468(2) 0.038 Uiso 1 1 d . . . O1 O 0.1552(3) 0.9942(3) 0.78913(19) 0.0457(8) Uani 1 1 d . . . O2 O 0.3168(3) 1.1510(3) 0.76425(17) 0.0403(8) Uani 1 1 d . . . O3 O 0.3527(3) 0.9077(3) 0.79200(18) 0.0390(8) Uani 1 1 d . . . H3A H 0.335(4) 0.860(5) 0.825(3) 0.047 Uiso 1 1 d . . . O4 O 0.0390(3) 1.0717(3) 0.65510(17) 0.0405(7) Uani 1 1 d . . . O5 O 0.1863(3) 1.2284(3) 0.60995(17) 0.0361(7) Uani 1 1 d . . . O6 O 0.1204(3) 1.0178(4) 0.54228(19) 0.0445(9) Uani 1 1 d . . . H6B H 0.125(5) 1.069(6) 0.511(3) 0.053 Uiso 1 1 d . . . O7 O 0.2136(3) 0.8397(3) 0.64536(18) 0.0392(8) Uani 1 1 d . . . H7A H 0.198(4) 0.796(5) 0.680(3) 0.047 Uiso 1 1 d . . . O1W O 0.0000 0.7904(5) 0.7500 0.0467(13) Uani 1 2 d S . . H1X H -0.028(12) 0.767(13) 0.788(6) 0.056 Uiso 0.50 1 d P . . H1Y H 0.059(11) 0.741(13) 0.748(8) 0.056 Uiso 0.50 1 d P . . O2W O 0.1173(3) 0.1562(4) 0.4261(2) 0.0448(8) Uani 1 1 d . . . H2X H 0.100(5) 0.112(6) 0.392(3) 0.054 Uiso 1 1 d . . . H2Y H 0.069(5) 0.219(6) 0.427(3) 0.054 Uiso 1 1 d . . . P1 P 0.26553(11) 1.01354(13) 0.75834(7) 0.0433(3) Uani 1 1 d . . . P2 P 0.14338(11) 1.08598(13) 0.61723(7) 0.0432(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(2) 0.033(2) 0.037(2) -0.0034(18) 0.005(2) 0.0060(19) C2 0.022(2) 0.042(3) 0.041(3) -0.005(2) 0.0030(19) -0.0063(17) C3 0.051(3) 0.029(2) 0.044(3) 0.015(2) 0.004(2) -0.002(2) C4 0.045(3) 0.044(3) 0.040(3) 0.001(2) 0.005(2) -0.001(2) C5 0.040(3) 0.043(3) 0.033(2) -0.0039(19) -0.003(2) -0.0030(19) Cu1 0.0406(5) 0.0285(4) 0.0426(5) 0.000 0.0031(4) 0.000 N1 0.044(2) 0.035(2) 0.046(2) 0.0030(18) 0.0060(18) 0.0010(18) N2 0.032(2) 0.033(2) 0.0309(19) -0.0127(14) 0.0087(15) 0.0019(14) O1 0.0397(18) 0.0519(19) 0.0460(19) -0.0012(15) 0.0066(15) 0.0011(15) O2 0.0371(18) 0.0407(18) 0.0432(18) -0.0069(14) 0.0052(14) -0.0056(14) O3 0.0407(19) 0.0321(17) 0.0441(19) 0.0084(14) 0.0043(15) 0.0002(13) O4 0.0363(17) 0.0461(19) 0.0390(18) 0.0106(14) 0.0039(13) 0.0047(14) O5 0.0283(16) 0.0374(17) 0.0428(18) 0.0008(13) 0.0041(14) 0.0010(13) O6 0.051(2) 0.044(2) 0.037(2) 0.0013(15) -0.0019(17) -0.0024(16) O7 0.0329(17) 0.0387(19) 0.0462(18) -0.0001(14) 0.0050(15) -0.0078(13) O1W 0.041(3) 0.038(3) 0.065(4) 0.000 0.022(3) 0.000 O2W 0.044(2) 0.046(2) 0.045(2) -0.0002(16) 0.0056(16) 0.0010(16) P1 0.0429(7) 0.0435(7) 0.0429(7) -0.0017(5) 0.0004(6) -0.0004(6) P2 0.0420(7) 0.0443(8) 0.0431(7) 0.0026(6) 0.0037(6) 0.0004(5) _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 N2 1.310(5) . ? C1 N1 1.318(6) . ? C1 H1A 0.9300 . ? C2 C3 1.316(6) . ? C2 N2 1.353(6) . ? C2 H2C 0.9300 . ? C3 N1 1.368(6) . ? C3 H3B 0.9300 . ? C4 N1 1.469(6) . ? C4 C5 1.553(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O7 1.427(5) . ? C5 P2 1.834(5) . ? C5 P1 1.840(5) . ? Cu1 O1 1.926(3) . ? Cu1 O1 1.926(3) 2_556 ? Cu1 O4 1.994(3) 2_556 ? Cu1 O4 1.994(3) . ? Cu1 O1W 2.121(5) . ? N2 H2B 1.01(5) . ? O1 P1 1.502(4) . ? O2 P1 1.481(3) . ? O3 P1 1.558(3) . ? O3 H3A 0.82(5) . ? O4 P2 1.502(3) . ? O5 P2 1.499(3) . ? O6 P2 1.559(4) . ? O6 H6B 0.78(6) . ? O7 H7A 0.82(5) . ? O1W H1X 0.85(12) . ? O1W H1Y 0.85(13) . ? O2W H2X 0.79(6) . ? O2W H2Y 0.85(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 109.0(4) . . ? N2 C1 H1A 125.5 . . ? N1 C1 H1A 125.5 . . ? C3 C2 N2 106.9(4) . . ? C3 C2 H2C 126.6 . . ? N2 C2 H2C 126.6 . . ? C2 C3 N1 108.4(4) . . ? C2 C3 H3B 125.8 . . ? N1 C3 H3B 125.8 . . ? N1 C4 C5 111.1(4) . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? O7 C5 C4 109.0(4) . . ? O7 C5 P2 104.7(3) . . ? C4 C5 P2 114.8(3) . . ? O7 C5 P1 113.8(3) . . ? C4 C5 P1 106.3(3) . . ? P2 C5 P1 108.5(2) . . ? O1 Cu1 O1 172.8(2) . 2_556 ? O1 Cu1 O4 88.90(14) . 2_556 ? O1 Cu1 O4 93.41(14) 2_556 2_556 ? O1 Cu1 O4 93.41(14) . . ? O1 Cu1 O4 88.90(14) 2_556 . ? O4 Cu1 O4 142.62(19) 2_556 . ? O1 Cu1 O1W 86.40(10) . . ? O1 Cu1 O1W 86.40(10) 2_556 . ? O4 Cu1 O1W 108.69(10) 2_556 . ? O4 Cu1 O1W 108.69(10) . . ? C1 N1 C3 106.9(4) . . ? C1 N1 C4 124.5(4) . . ? C3 N1 C4 128.4(4) . . ? C1 N2 C2 108.8(4) . . ? C1 N2 H2B 123(3) . . ? C2 N2 H2B 128(3) . . ? P1 O1 Cu1 133.7(2) . . ? P1 O3 H3A 118(4) . . ? P2 O4 Cu1 137.2(2) . . ? P2 O6 H6B 113(4) . . ? C5 O7 H7A 114(4) . . ? Cu1 O1W H1X 105(8) . . ? Cu1 O1W H1Y 124(9) . . ? H1X O1W H1Y 106(10) . . ? H2X O2W H2Y 107(6) . . ? O2 P1 O1 117.22(19) . . ? O2 P1 O3 108.83(19) . . ? O1 P1 O3 109.5(2) . . ? O2 P1 C5 104.9(2) . . ? O1 P1 C5 111.1(2) . . ? O3 P1 C5 104.5(2) . . ? O5 P2 O4 115.94(18) . . ? O5 P2 O6 110.37(19) . . ? O4 P2 O6 108.0(2) . . ? O5 P2 C5 111.4(2) . . ? O4 P2 C5 107.9(2) . . ? O6 P2 C5 102.3(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O6 1.01(5) 1.95(5) 2.923(5) 162(4) 7_566 N2 H2B O7 1.01(5) 2.36(5) 2.905(5) 113(3) 7_566 O3 H3A O5 0.82(5) 1.82(5) 2.624(4) 169(5) 4_546 O7 H7A O2 0.82(5) 1.78(5) 2.563(5) 158(5) 4_546 O1W H1Y O2 0.85(13) 1.76(13) 2.615(4) 173(13) 4_546 O6 H6B O2W 0.78(6) 1.80(6) 2.569(5) 166(6) 1_565 O1W H1X O2 0.85(12) 2.19(15) 2.615(4) 111(10) 3_445 O2W H2Y N2 0.85(6) 2.59(6) 3.276(5) 139(5) 3_445 O2W H2X O1 0.79(6) 2.34(6) 3.041(5) 148(6) 6_565 O2W H2X O4 0.79(6) 2.54(6) 3.199(5) 141(5) 5_566 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.406 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.084 # Attachment 'Cu-2.cif' data_Cu(ImhedpH3)2 _database_code_depnum_ccdc_archive 'CCDC 683972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H18 Cu N4 O14 P4' _chemical_formula_sum 'C10 H18 Cu N4 O14 P4' _chemical_formula_weight 605.70 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' 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.0186(19) _cell_length_b 8.509(3) _cell_length_c 10.039(3) _cell_angle_alpha 80.652(6) _cell_angle_beta 78.583(5) _cell_angle_gamma 81.676(6) _cell_volume 493.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 830 _cell_measurement_theta_min 2.9885 _cell_measurement_theta_max 25.997 _exptl_crystal_description blocky _exptl_crystal_colour 'navy blue' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 307 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details 'SADABS,(Bruker, 2000)' _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 'Bruker Smart Apex 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 2572 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1796 _reflns_number_gt 1550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. ; _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^)+(0.0668P)^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 1796 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.0000 1.0000 1.0000 0.0210(2) Uani 1 2 d S . . P1 P 0.40192(18) 1.05089(12) 0.75163(10) 0.0164(3) Uani 1 1 d . . . P2 P 0.34175(18) 0.71463(12) 0.90275(10) 0.0163(3) Uani 1 1 d . . . O1 O 0.1606(5) 1.0957(3) 0.8259(3) 0.0238(7) Uani 1 1 d . . . O2 O 0.4507(5) 1.1376(3) 0.6107(3) 0.0259(7) Uani 1 1 d . . . O3 O 0.5786(5) 1.0703(3) 0.8425(3) 0.0279(7) Uani 1 1 d . . . H3A H 0.5289 1.1445 0.8870 0.042 Uiso 1 1 calc R . . O4 O 0.1035(5) 0.7879(3) 0.9549(3) 0.0241(7) Uani 1 1 d . . . O5 O 0.5101(5) 0.7061(3) 0.9978(3) 0.0233(7) Uani 1 1 d . . . O6 O 0.3265(5) 0.5468(3) 0.8652(3) 0.0221(7) Uani 1 1 d . . . H6A H 0.3856 0.4771 0.9183 0.033 Uiso 1 1 calc R . . O7 O 0.3177(5) 0.8056(3) 0.6447(3) 0.0208(6) Uani 1 1 d . . . H7A H 0.3889 0.8230 0.5663 0.031 Uiso 1 1 calc R . . N1 N 0.7739(5) 0.6205(4) 0.6785(3) 0.0182(8) Uani 1 1 d . . . N2 N 0.9126(6) 0.3745(4) 0.7223(4) 0.0291(9) Uani 1 1 d . . . H2B H 0.9834 0.2888 0.7598 0.035 Uiso 1 1 calc R . . C1 C 0.8914(7) 0.5180(5) 0.7609(4) 0.0254(10) Uani 1 1 d . . . H1A H 0.9489 0.5430 0.8333 0.030 Uiso 1 1 calc R . . C2 C 0.8036(8) 0.3841(5) 0.6131(5) 0.0297(11) Uani 1 1 d . . . H2C H 0.7916 0.3000 0.5673 0.036 Uiso 1 1 calc R . . C3 C 0.7176(7) 0.5376(5) 0.5848(4) 0.0242(10) Uani 1 1 d . . . H3B H 0.6356 0.5802 0.5152 0.029 Uiso 1 1 calc R . . C4 C 0.7092(7) 0.7909(5) 0.6909(4) 0.0200(9) Uani 1 1 d . . . H4A H 0.7547 0.8536 0.6023 0.024 Uiso 1 1 calc R . . H4B H 0.7920 0.8205 0.7550 0.024 Uiso 1 1 calc R . . C5 C 0.4517(6) 0.8337(4) 0.7400(4) 0.0143(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0222(4) 0.0154(4) 0.0184(4) 0.0014(3) 0.0044(3) 0.0053(3) P1 0.0214(6) 0.0125(5) 0.0134(5) -0.0021(4) -0.0011(4) 0.0022(4) P2 0.0212(6) 0.0116(5) 0.0142(5) -0.0005(4) -0.0025(4) 0.0023(4) O1 0.0256(17) 0.0161(15) 0.0223(16) 0.0032(12) 0.0025(13) 0.0066(12) O2 0.0366(19) 0.0200(16) 0.0177(15) 0.0014(12) -0.0009(13) -0.0023(13) O3 0.0358(19) 0.0231(17) 0.0289(17) -0.0155(13) -0.0116(14) 0.0042(14) O4 0.0256(17) 0.0148(15) 0.0254(16) 0.0005(12) 0.0029(13) 0.0050(12) O5 0.0384(19) 0.0158(15) 0.0174(15) -0.0021(12) -0.0109(13) -0.0010(13) O6 0.0291(17) 0.0141(15) 0.0245(16) -0.0018(12) -0.0114(13) 0.0009(12) O7 0.0246(16) 0.0245(16) 0.0140(14) -0.0026(12) -0.0049(12) -0.0034(13) N1 0.0152(17) 0.0168(18) 0.0223(19) -0.0042(15) -0.0047(14) 0.0023(14) N2 0.028(2) 0.0151(19) 0.037(2) 0.0064(16) -0.0029(17) 0.0088(16) C1 0.021(2) 0.026(2) 0.026(2) -0.0038(19) -0.0048(19) 0.0038(19) C2 0.026(3) 0.024(2) 0.041(3) -0.014(2) -0.004(2) -0.003(2) C3 0.023(2) 0.023(2) 0.027(2) -0.0079(19) -0.0050(19) 0.0007(19) C4 0.021(2) 0.017(2) 0.023(2) -0.0078(17) -0.0024(17) 0.0009(17) C5 0.017(2) 0.0102(19) 0.015(2) -0.0026(15) -0.0039(16) 0.0026(16) _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 1.918(3) . ? Cu1 O4 1.918(3) 2_577 ? Cu1 O1 1.936(3) 2_577 ? Cu1 O1 1.936(3) . ? P1 O2 1.480(3) . ? P1 O1 1.521(3) . ? P1 O3 1.572(3) . ? P1 C5 1.848(4) . ? P2 O4 1.506(3) . ? P2 O5 1.511(3) . ? P2 O6 1.554(3) . ? P2 C5 1.834(4) . ? O3 H3A 0.8200 . ? O6 H6A 0.8200 . ? O7 C5 1.434(4) . ? O7 H7A 0.8200 . ? N1 C1 1.328(5) . ? N1 C3 1.382(5) . ? N1 C4 1.465(5) . ? N2 C1 1.321(5) . ? N2 C2 1.371(6) . ? N2 H2B 0.8600 . ? C1 H1A 0.9300 . ? C2 C3 1.340(6) . ? C2 H2C 0.9300 . ? C3 H3B 0.9300 . ? C4 C5 1.539(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? 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 O4 180.000(1) . 2_577 ? O4 Cu1 O1 88.38(11) . 2_577 ? O4 Cu1 O1 91.62(11) 2_577 2_577 ? O4 Cu1 O1 91.62(11) . . ? O4 Cu1 O1 88.38(11) 2_577 . ? O1 Cu1 O1 180.000(1) 2_577 . ? O2 P1 O1 113.19(17) . . ? O2 P1 O3 112.98(17) . . ? O1 P1 O3 109.73(16) . . ? O2 P1 C5 107.81(17) . . ? O1 P1 C5 110.29(16) . . ? O3 P1 C5 102.27(17) . . ? O4 P2 O5 115.14(17) . . ? O4 P2 O6 108.17(16) . . ? O5 P2 O6 111.68(16) . . ? O4 P2 C5 108.39(17) . . ? O5 P2 C5 107.81(17) . . ? O6 P2 C5 105.14(16) . . ? P1 O1 Cu1 129.63(17) . . ? P1 O3 H3A 109.5 . . ? P2 O4 Cu1 129.32(18) . . ? P2 O6 H6A 109.5 . . ? C5 O7 H7A 109.5 . . ? C1 N1 C3 108.4(4) . . ? C1 N1 C4 124.7(3) . . ? C3 N1 C4 126.8(3) . . ? C1 N2 C2 109.1(4) . . ? C1 N2 H2B 125.4 . . ? C2 N2 H2B 125.4 . . ? N2 C1 N1 108.3(4) . . ? N2 C1 H1A 125.8 . . ? N1 C1 H1A 125.8 . . ? C3 C2 N2 107.1(4) . . ? C3 C2 H2C 126.4 . . ? N2 C2 H2C 126.4 . . ? C2 C3 N1 107.0(4) . . ? C2 C3 H3B 126.5 . . ? N1 C3 H3B 126.5 . . ? N1 C4 C5 113.3(3) . . ? N1 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N1 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? O7 C5 C4 112.4(3) . . ? O7 C5 P2 105.1(2) . . ? C4 C5 P2 113.0(3) . . ? O7 C5 P1 106.9(2) . . ? C4 C5 P1 107.5(2) . . ? P2 C5 P1 111.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Cu1 171.45(19) . . . . ? O3 P1 O1 Cu1 -61.3(3) . . . . ? C5 P1 O1 Cu1 50.6(3) . . . . ? O4 Cu1 O1 P1 -44.8(2) . . . . ? O4 Cu1 O1 P1 135.2(2) 2_577 . . . ? O5 P2 O4 Cu1 61.5(3) . . . . ? O6 P2 O4 Cu1 -172.83(19) . . . . ? C5 P2 O4 Cu1 -59.3(3) . . . . ? O1 Cu1 O4 P2 -129.7(2) 2_577 . . . ? O1 Cu1 O4 P2 50.3(2) . . . . ? C2 N2 C1 N1 -0.7(5) . . . . ? C3 N1 C1 N2 0.4(5) . . . . ? C4 N1 C1 N2 178.1(3) . . . . ? C1 N2 C2 C3 0.7(5) . . . . ? N2 C2 C3 N1 -0.5(5) . . . . ? C1 N1 C3 C2 0.0(5) . . . . ? C4 N1 C3 C2 -177.6(4) . . . . ? C1 N1 C4 C5 -109.6(4) . . . . ? C3 N1 C4 C5 67.7(5) . . . . ? N1 C4 C5 O7 -63.3(4) . . . . ? N1 C4 C5 P2 55.5(4) . . . . ? N1 C4 C5 P1 179.3(3) . . . . ? O4 P2 C5 O7 -68.3(3) . . . . ? O5 P2 C5 O7 166.5(2) . . . . ? O6 P2 C5 O7 47.2(3) . . . . ? O4 P2 C5 C4 168.7(2) . . . . ? O5 P2 C5 C4 43.5(3) . . . . ? O6 P2 C5 C4 -75.8(3) . . . . ? O4 P2 C5 P1 47.3(2) . . . . ? O5 P2 C5 P1 -77.9(2) . . . . ? O6 P2 C5 P1 162.83(18) . . . . ? O2 P1 C5 O7 -53.8(3) . . . . ? O1 P1 C5 O7 70.2(3) . . . . ? O3 P1 C5 O7 -173.1(2) . . . . ? O2 P1 C5 C4 67.1(3) . . . . ? O1 P1 C5 C4 -168.9(2) . . . . ? O3 P1 C5 C4 -52.2(3) . . . . ? O2 P1 C5 P2 -168.33(19) . . . . ? O1 P1 C5 P2 -44.3(3) . . . . ? O3 P1 C5 P2 72.4(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O5 0.82 1.81 2.614(4) 164.8 2_677 O6 H6A O5 0.82 1.74 2.540(4) 163.7 2_667 O7 H7A O2 0.82 1.85 2.670(4) 180.0 2_676 N2 H2B O1 0.86 1.92 2.779(5) 174.3 1_645 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.585 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.113 # Attachment 'Cu-3.cif' data_Cu3(ImhedpH2)2(ImhedpH3)2.4H2O _database_code_depnum_ccdc_archive 'CCDC 683973' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H34 Cu3 N8 O28 P8, 4(H2 O)' _chemical_formula_sum 'C20 H42 Cu3 N8 O32 P8' _chemical_formula_weight 1345.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2187(19) _cell_length_b 11.367(2) _cell_length_c 18.353(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.156(4) _cell_angle_gamma 90.00 _cell_volume 2119.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2101 _cell_measurement_theta_min 2.836 _cell_measurement_theta_max 26.1325 _exptl_crystal_description 'Long rod' _exptl_crystal_colour Green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 1.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.826 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _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 'Bruker Smart Aepex 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 10647 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4114 _reflns_number_gt 3421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+4.7952P] 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 4114 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.5000 0.5000 0.0000 0.01699(18) Uani 1 2 d S . . Cu2 Cu 0.13170(5) 0.48965(4) 0.05357(3) 0.01534(15) Uani 1 1 d . . . P1 P 0.31150(10) 0.28821(9) 0.00102(6) 0.0136(2) Uani 1 1 d . . . P2 P 0.36398(10) 0.40425(10) 0.14514(6) 0.0140(2) Uani 1 1 d . . . P3 P 0.17513(10) 0.65087(10) -0.07007(6) 0.0142(2) Uani 1 1 d . . . P4 P 0.19783(10) 0.75067(10) 0.08384(6) 0.0160(2) Uani 1 1 d . . . O1 O 0.1771(3) 0.3435(3) 0.00172(15) 0.0167(6) Uani 1 1 d . . . O1W O 0.7029(3) 0.3237(4) 0.23880(18) 0.0442(11) Uani 1 1 d . . . H1WD H 0.6229 0.3455 0.2331 0.053 Uiso 1 1 d R . . H1WA H 0.7303 0.3234 0.2842 0.053 Uiso 1 1 d R . . O2 O 0.4115(3) 0.3592(3) -0.03511(15) 0.0170(6) Uani 1 1 d . . . O2W O 0.4544(3) 0.1129(3) 0.87026(18) 0.0352(9) Uani 1 1 d . . . H2WD H 0.4139 0.1066 0.8275 0.042 Uiso 1 1 d R . . H2WC H 0.5224 0.1555 0.8685 0.042 Uiso 1 1 d R . . O3 O 0.2943(3) 0.1662(3) -0.03653(16) 0.0218(7) Uani 1 1 d . . . H3A H 0.3500 0.1580 -0.0652 0.033 Uiso 1 1 calc R . . O4 O 0.2170(3) 0.4288(3) 0.14563(15) 0.0166(6) Uani 1 1 d . . . O5 O 0.4242(3) 0.4941(3) 0.09579(15) 0.0181(6) Uani 1 1 d . . . O6 O 0.4369(3) 0.3960(3) 0.21967(16) 0.0225(7) Uani 1 1 d . . . O7 O 0.5064(3) 0.2213(3) 0.10381(16) 0.0219(7) Uani 1 1 d . . . H7A H 0.5543 0.2731 0.0903 0.033 Uiso 1 1 calc R . . O8 O 0.0805(3) 0.5608(3) -0.04358(15) 0.0164(6) Uani 1 1 d . . . O9 O 0.1248(3) 0.6818(3) -0.15099(16) 0.0225(7) Uani 1 1 d . . . H9C H 0.1862 0.6782 -0.1762 0.034 Uiso 1 1 calc R . . O10 O 0.3176(3) 0.6175(3) -0.06096(16) 0.0211(7) Uani 1 1 d . . . O11 O 0.1205(3) 0.6429(3) 0.10120(15) 0.0199(6) Uani 1 1 d . . . O12 O 0.3508(3) 0.7230(3) 0.09324(17) 0.0228(7) Uani 1 1 d . . . H12A H 0.3620 0.6516 0.0933 0.034 Uiso 1 1 calc R . . O13 O 0.1813(3) 0.8591(3) 0.12655(16) 0.0227(7) Uani 1 1 d . . . O14 O 0.0166(3) 0.8165(3) -0.02187(17) 0.0205(7) Uani 1 1 d . . . H14A H -0.0288 0.7592 -0.0142 0.031 Uiso 1 1 calc R . . N1 N 0.2799(3) 0.1557(3) 0.20237(19) 0.0206(8) Uani 1 1 d . . . N2 N 0.3197(5) 0.1127(4) 0.3152(2) 0.0444(12) Uani 1 1 d . . . H2A H 0.3599 0.0883 0.3560 0.053 Uiso 1 1 calc R . . N3 N 0.1796(3) 0.9397(3) -0.10731(19) 0.0176(8) Uani 1 1 d . . . N4 N 0.1614(4) 0.9830(4) -0.2212(2) 0.0311(10) Uani 1 1 d . . . H4C H 0.1764 0.9869 -0.2664 0.037 Uiso 1 1 calc R . . C1 C 0.3687(5) 0.1108(5) 0.2516(3) 0.0329(12) Uani 1 1 d . . . H1A H 0.4512 0.0828 0.2432 0.039 Uiso 1 1 calc R . . C2 C 0.1968(6) 0.1586(5) 0.3068(3) 0.0404(14) Uani 1 1 d . . . H2B H 0.1411 0.1690 0.3431 0.049 Uiso 1 1 calc R . . C3 C 0.1714(5) 0.1861(5) 0.2359(3) 0.0311(11) Uani 1 1 d . . . H3B H 0.0943 0.2197 0.2136 0.037 Uiso 1 1 calc R . . C4 C 0.2877(4) 0.1632(4) 0.1234(2) 0.0203(9) Uani 1 1 d . . . H4A H 0.1991 0.1726 0.0993 0.024 Uiso 1 1 calc R . . H4B H 0.3210 0.0889 0.1072 0.024 Uiso 1 1 calc R . . C5 C 0.3732(4) 0.2621(4) 0.0969(2) 0.0159(9) Uani 1 1 d . . . C6 C 0.2347(5) 0.9270(4) -0.1691(3) 0.0265(10) Uani 1 1 d . . . H6B H 0.3116 0.8858 -0.1746 0.032 Uiso 1 1 calc R . . C7 C 0.0566(5) 1.0343(5) -0.1920(3) 0.0308(11) Uani 1 1 d . . . H7B H -0.0095 1.0795 -0.2170 0.037 Uiso 1 1 calc R . . C8 C 0.0682(4) 1.0068(4) -0.1210(3) 0.0254(10) Uani 1 1 d . . . H8A H 0.0114 1.0290 -0.0871 0.030 Uiso 1 1 calc R . . C9 C 0.2282(4) 0.8918(4) -0.0354(2) 0.0180(9) Uani 1 1 d . . . H9A H 0.2220 0.9522 0.0015 0.022 Uiso 1 1 calc R . . H9B H 0.3203 0.8714 -0.0354 0.022 Uiso 1 1 calc R . . C10 C 0.1526(4) 0.7831(4) -0.0143(2) 0.0167(9) 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 0.0185(4) 0.0192(4) 0.0141(4) -0.0026(3) 0.0056(3) -0.0065(3) Cu2 0.0140(3) 0.0180(3) 0.0138(3) 0.0012(2) 0.00008(19) 0.0002(2) P1 0.0130(5) 0.0149(5) 0.0131(5) -0.0003(4) 0.0018(4) -0.0019(4) P2 0.0130(5) 0.0169(5) 0.0121(5) -0.0002(4) 0.0016(4) -0.0004(4) P3 0.0120(5) 0.0172(5) 0.0134(5) 0.0008(4) 0.0011(4) -0.0008(4) P4 0.0144(5) 0.0184(6) 0.0149(5) -0.0010(4) 0.0003(4) 0.0023(4) O1 0.0137(14) 0.0189(15) 0.0177(15) -0.0016(12) 0.0029(11) 0.0014(12) O1W 0.0257(19) 0.089(3) 0.0178(18) 0.0005(19) 0.0036(14) 0.0181(19) O2 0.0168(14) 0.0200(16) 0.0147(14) -0.0020(12) 0.0037(11) -0.0051(12) O2W 0.034(2) 0.047(2) 0.0258(18) -0.0105(17) 0.0105(15) -0.0133(17) O3 0.0225(16) 0.0219(17) 0.0223(16) -0.0062(13) 0.0089(13) -0.0064(13) O4 0.0139(14) 0.0229(16) 0.0134(14) 0.0018(12) 0.0021(11) 0.0026(12) O5 0.0192(15) 0.0188(16) 0.0175(15) -0.0009(12) 0.0071(12) -0.0017(12) O6 0.0208(16) 0.0309(18) 0.0148(15) -0.0011(13) -0.0027(12) -0.0013(13) O7 0.0156(15) 0.0224(17) 0.0279(17) 0.0049(14) 0.0031(12) 0.0048(12) O8 0.0119(14) 0.0201(16) 0.0171(15) 0.0022(12) 0.0012(11) -0.0028(12) O9 0.0211(16) 0.0287(18) 0.0178(16) 0.0019(13) 0.0027(12) -0.0007(13) O10 0.0145(15) 0.0243(17) 0.0246(17) -0.0009(14) 0.0033(12) -0.0003(13) O11 0.0238(16) 0.0198(16) 0.0165(15) -0.0014(13) 0.0046(12) 0.0007(13) O12 0.0163(15) 0.0212(17) 0.0297(17) -0.0051(14) -0.0028(13) 0.0042(12) O13 0.0233(16) 0.0239(17) 0.0206(16) -0.0035(14) 0.0014(13) 0.0023(13) O14 0.0103(14) 0.0180(16) 0.0328(18) 0.0049(14) 0.0005(12) -0.0006(12) N1 0.0203(19) 0.024(2) 0.0172(19) 0.0053(16) -0.0015(15) -0.0037(16) N2 0.062(3) 0.051(3) 0.017(2) 0.011(2) -0.012(2) -0.010(3) N3 0.0167(18) 0.0158(18) 0.0209(19) 0.0029(15) 0.0049(14) -0.0025(14) N4 0.033(2) 0.042(3) 0.020(2) 0.0073(19) 0.0090(17) -0.0022(19) C1 0.031(3) 0.036(3) 0.029(3) 0.009(2) -0.008(2) 0.003(2) C2 0.047(3) 0.048(4) 0.028(3) -0.003(3) 0.015(2) -0.010(3) C3 0.029(3) 0.038(3) 0.028(3) 0.000(2) 0.010(2) -0.004(2) C4 0.023(2) 0.024(2) 0.013(2) 0.0038(18) 0.0009(17) -0.0053(18) C5 0.014(2) 0.016(2) 0.018(2) 0.0007(17) 0.0005(16) 0.0007(16) C6 0.026(2) 0.026(3) 0.029(3) 0.004(2) 0.009(2) 0.000(2) C7 0.021(2) 0.037(3) 0.035(3) 0.009(2) 0.003(2) 0.005(2) C8 0.024(2) 0.025(3) 0.028(3) 0.004(2) 0.0071(19) 0.0065(19) C9 0.019(2) 0.018(2) 0.017(2) -0.0002(18) 0.0004(17) -0.0008(17) C10 0.016(2) 0.017(2) 0.016(2) 0.0011(17) 0.0006(16) 0.0000(17) _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 O2 1.916(3) . ? Cu1 O2 1.916(3) 3_665 ? Cu1 O5 1.997(3) 3_665 ? Cu1 O5 1.997(3) . ? Cu1 O10 2.463(3) . ? Cu1 O10 2.463(3) 3_665 ? Cu2 O4 1.944(3) . ? Cu2 O11 1.958(3) . ? Cu2 O8 1.977(3) . ? Cu2 O1 1.994(3) . ? Cu2 O8 2.231(3) 3_565 ? P1 O2 1.510(3) . ? P1 O1 1.512(3) . ? P1 O3 1.551(3) . ? P1 C5 1.829(4) . ? P2 O6 1.489(3) . ? P2 O4 1.528(3) . ? P2 O5 1.537(3) . ? P2 C5 1.849(4) . ? P3 O10 1.496(3) . ? P3 O8 1.524(3) . ? P3 O9 1.559(3) . ? P3 C10 1.846(4) . ? P4 O13 1.480(3) . ? P4 O11 1.510(3) . ? P4 O12 1.585(3) . ? P4 C10 1.848(4) . ? O1W H1WD 0.8499 . ? O1W H1WA 0.8502 . ? O2W H2WD 0.8500 . ? O2W H2WC 0.8499 . ? O3 H3A 0.8200 . ? O7 C5 1.431(5) . ? O7 H7A 0.8200 . ? O8 Cu2 2.231(3) 3_565 ? O9 H9C 0.8200 . ? O12 H12A 0.8200 . ? O14 C10 1.434(5) . ? O14 H14A 0.8200 . ? N1 C1 1.313(6) . ? N1 C3 1.370(6) . ? N1 C4 1.462(5) . ? N2 C1 1.318(7) . ? N2 C2 1.354(7) . ? N2 H2A 0.8600 . ? N3 C6 1.327(6) . ? N3 C8 1.371(6) . ? N3 C9 1.465(5) . ? N4 C6 1.313(6) . ? N4 C7 1.377(6) . ? N4 H4C 0.8600 . ? C1 H1A 0.9300 . ? C2 C3 1.335(7) . ? C2 H2B 0.9300 . ? C3 H3B 0.9300 . ? C4 C5 1.534(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6B 0.9300 . ? C7 C8 1.333(7) . ? C7 H7B 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.528(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 O2 Cu1 O2 180.00(15) . 3_665 ? O2 Cu1 O5 86.88(11) . 3_665 ? O2 Cu1 O5 93.12(11) 3_665 3_665 ? O2 Cu1 O5 93.12(11) . . ? O2 Cu1 O5 86.88(11) 3_665 . ? O5 Cu1 O5 180.00(16) 3_665 . ? O2 Cu1 O10 89.62(11) . . ? O2 Cu1 O10 90.38(11) 3_665 . ? O5 Cu1 O10 85.88(11) 3_665 . ? O5 Cu1 O10 94.12(11) . . ? O2 Cu1 O10 90.38(11) . 3_665 ? O2 Cu1 O10 89.62(11) 3_665 3_665 ? O5 Cu1 O10 94.12(11) 3_665 3_665 ? O5 Cu1 O10 85.88(11) . 3_665 ? O10 Cu1 O10 180.00(13) . 3_665 ? O4 Cu2 O11 88.31(12) . . ? O4 Cu2 O8 168.67(11) . . ? O11 Cu2 O8 90.93(12) . . ? O4 Cu2 O1 90.73(12) . . ? O11 Cu2 O1 169.17(12) . . ? O8 Cu2 O1 87.89(12) . . ? O4 Cu2 O8 108.75(11) . 3_565 ? O11 Cu2 O8 99.37(11) . 3_565 ? O8 Cu2 O8 82.53(11) . 3_565 ? O1 Cu2 O8 91.16(11) . 3_565 ? O2 P1 O1 116.11(17) . . ? O2 P1 O3 109.42(16) . . ? O1 P1 O3 108.40(16) . . ? O2 P1 C5 109.25(17) . . ? O1 P1 C5 106.19(17) . . ? O3 P1 C5 107.08(18) . . ? O6 P2 O4 113.66(17) . . ? O6 P2 O5 113.02(17) . . ? O4 P2 O5 109.73(16) . . ? O6 P2 C5 109.79(19) . . ? O4 P2 C5 105.23(17) . . ? O5 P2 C5 104.74(17) . . ? O10 P3 O8 115.95(17) . . ? O10 P3 O9 112.41(17) . . ? O8 P3 O9 107.43(16) . . ? O10 P3 C10 108.76(18) . . ? O8 P3 C10 104.41(18) . . ? O9 P3 C10 107.28(18) . . ? O13 P4 O11 118.15(17) . . ? O13 P4 O12 105.96(17) . . ? O11 P4 O12 110.35(17) . . ? O13 P4 C10 108.64(18) . . ? O11 P4 C10 106.60(18) . . ? O12 P4 C10 106.62(18) . . ? P1 O1 Cu2 127.46(17) . . ? H1WD O1W H1WA 109.4 . . ? P1 O2 Cu1 128.02(17) . . ? H2WD O2W H2WC 109.5 . . ? P1 O3 H3A 109.5 . . ? P2 O4 Cu2 114.17(16) . . ? P2 O5 Cu1 139.35(18) . . ? C5 O7 H7A 109.5 . . ? P3 O8 Cu2 116.55(16) . . ? P3 O8 Cu2 142.30(17) . 3_565 ? Cu2 O8 Cu2 97.47(11) . 3_565 ? P3 O9 H9C 109.5 . . ? P3 O10 Cu1 150.26(18) . . ? P4 O11 Cu2 124.80(17) . . ? P4 O12 H12A 109.5 . . ? C10 O14 H14A 109.5 . . ? C1 N1 C3 108.8(4) . . ? C1 N1 C4 126.8(4) . . ? C3 N1 C4 124.3(4) . . ? C1 N2 C2 109.9(4) . . ? C1 N2 H2A 125.1 . . ? C2 N2 H2A 125.1 . . ? C6 N3 C8 108.9(4) . . ? C6 N3 C9 126.6(4) . . ? C8 N3 C9 124.5(4) . . ? C6 N4 C7 109.2(4) . . ? C6 N4 H4C 125.4 . . ? C7 N4 H4C 125.4 . . ? N1 C1 N2 107.7(5) . . ? N1 C1 H1A 126.2 . . ? N2 C1 H1A 126.2 . . ? C3 C2 N2 106.5(5) . . ? C3 C2 H2B 126.8 . . ? N2 C2 H2B 126.8 . . ? C2 C3 N1 107.2(5) . . ? C2 C3 H3B 126.4 . . ? N1 C3 H3B 126.4 . . ? N1 C4 C5 116.8(4) . . ? N1 C4 H4A 108.1 . . ? C5 C4 H4A 108.1 . . ? N1 C4 H4B 108.1 . . ? C5 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? O7 C5 C4 107.6(3) . . ? O7 C5 P1 111.4(3) . . ? C4 C5 P1 105.9(3) . . ? O7 C5 P2 109.7(3) . . ? C4 C5 P2 115.4(3) . . ? P1 C5 P2 106.8(2) . . ? N4 C6 N3 108.0(4) . . ? N4 C6 H6B 126.0 . . ? N3 C6 H6B 126.0 . . ? C8 C7 N4 106.8(4) . . ? C8 C7 H7B 126.6 . . ? N4 C7 H7B 126.6 . . ? C7 C8 N3 107.2(4) . . ? C7 C8 H8A 126.4 . . ? N3 C8 H8A 126.4 . . ? N3 C9 C10 113.4(3) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? O14 C10 C9 105.8(3) . . ? O14 C10 P3 109.8(3) . . ? C9 C10 P3 114.9(3) . . ? O14 C10 P4 106.6(3) . . ? C9 C10 P4 109.1(3) . . ? P3 C10 P4 110.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Cu2 -65.1(3) . . . . ? O3 P1 O1 Cu2 171.33(19) . . . . ? C5 P1 O1 Cu2 56.6(3) . . . . ? O4 Cu2 O1 P1 -53.6(2) . . . . ? O11 Cu2 O1 P1 31.3(8) . . . . ? O8 Cu2 O1 P1 115.2(2) . . . . ? O8 Cu2 O1 P1 -162.3(2) 3_565 . . . ? O1 P1 O2 Cu1 71.5(3) . . . . ? O3 P1 O2 Cu1 -165.4(2) . . . . ? C5 P1 O2 Cu1 -48.5(3) . . . . ? O5 Cu1 O2 P1 -174.3(2) 3_665 . . . ? O5 Cu1 O2 P1 5.7(2) . . . . ? O10 Cu1 O2 P1 -88.4(2) . . . . ? O10 Cu1 O2 P1 91.6(2) 3_665 . . . ? O6 P2 O4 Cu2 161.10(17) . . . . ? O5 P2 O4 Cu2 33.5(2) . . . . ? C5 P2 O4 Cu2 -78.7(2) . . . . ? O11 Cu2 O4 P2 -107.98(19) . . . . ? O8 Cu2 O4 P2 -21.7(7) . . . . ? O1 Cu2 O4 P2 61.23(18) . . . . ? O8 Cu2 O4 P2 152.70(16) 3_565 . . . ? O6 P2 O5 Cu1 121.3(3) . . . . ? O4 P2 O5 Cu1 -110.7(3) . . . . ? C5 P2 O5 Cu1 1.8(3) . . . . ? O2 Cu1 O5 P2 22.1(3) . . . . ? O2 Cu1 O5 P2 -157.9(3) 3_665 . . . ? O10 Cu1 O5 P2 111.9(3) . . . . ? O10 Cu1 O5 P2 -68.1(3) 3_665 . . . ? O10 P3 O8 Cu2 45.8(2) . . . . ? O9 P3 O8 Cu2 172.49(17) . . . . ? C10 P3 O8 Cu2 -73.8(2) . . . . ? O10 P3 O8 Cu2 -162.0(2) . . . 3_565 ? O9 P3 O8 Cu2 -35.4(3) . . . 3_565 ? C10 P3 O8 Cu2 78.3(3) . . . 3_565 ? O4 Cu2 O8 P3 -22.1(7) . . . . ? O11 Cu2 O8 P3 63.92(19) . . . . ? O1 Cu2 O8 P3 -105.31(19) . . . . ? O8 Cu2 O8 P3 163.2(2) 3_565 . . . ? O4 Cu2 O8 Cu2 174.6(6) . . . 3_565 ? O11 Cu2 O8 Cu2 -99.33(12) . . . 3_565 ? O1 Cu2 O8 Cu2 91.44(12) . . . 3_565 ? O8 Cu2 O8 Cu2 0.0 3_565 . . 3_565 ? O8 P3 O10 Cu1 -21.9(4) . . . . ? O9 P3 O10 Cu1 -146.1(3) . . . . ? C10 P3 O10 Cu1 95.3(4) . . . . ? O2 Cu1 O10 P3 61.2(4) . . . . ? O2 Cu1 O10 P3 -118.8(4) 3_665 . . . ? O5 Cu1 O10 P3 148.1(4) 3_665 . . . ? O5 Cu1 O10 P3 -31.9(4) . . . . ? O13 P4 O11 Cu2 -178.08(18) . . . . ? O12 P4 O11 Cu2 -56.0(2) . . . . ? C10 P4 O11 Cu2 59.4(2) . . . . ? O4 Cu2 O11 P4 110.9(2) . . . . ? O8 Cu2 O11 P4 -57.8(2) . . . . ? O1 Cu2 O11 P4 25.8(8) . . . . ? O8 Cu2 O11 P4 -140.4(2) 3_565 . . . ? C3 N1 C1 N2 -0.4(6) . . . . ? C4 N1 C1 N2 -175.2(4) . . . . ? C2 N2 C1 N1 0.5(6) . . . . ? C1 N2 C2 C3 -0.5(7) . . . . ? N2 C2 C3 N1 0.3(6) . . . . ? C1 N1 C3 C2 0.0(6) . . . . ? C4 N1 C3 C2 175.1(4) . . . . ? C1 N1 C4 C5 -78.6(6) . . . . ? C3 N1 C4 C5 107.3(5) . . . . ? N1 C4 C5 O7 83.8(4) . . . . ? N1 C4 C5 P1 -156.9(3) . . . . ? N1 C4 C5 P2 -39.0(5) . . . . ? O2 P1 C5 O7 -47.8(3) . . . . ? O1 P1 C5 O7 -173.8(3) . . . . ? O3 P1 C5 O7 70.6(3) . . . . ? O2 P1 C5 C4 -164.6(3) . . . . ? O1 P1 C5 C4 69.5(3) . . . . ? O3 P1 C5 C4 -46.2(3) . . . . ? O2 P1 C5 P2 71.9(2) . . . . ? O1 P1 C5 P2 -54.0(2) . . . . ? O3 P1 C5 P2 -169.66(18) . . . . ? O6 P2 C5 O7 -47.9(3) . . . . ? O4 P2 C5 O7 -170.6(3) . . . . ? O5 P2 C5 O7 73.7(3) . . . . ? O6 P2 C5 C4 73.8(3) . . . . ? O4 P2 C5 C4 -48.9(3) . . . . ? O5 P2 C5 C4 -164.5(3) . . . . ? O6 P2 C5 P1 -168.74(18) . . . . ? O4 P2 C5 P1 68.6(2) . . . . ? O5 P2 C5 P1 -47.1(2) . . . . ? C7 N4 C6 N3 0.6(6) . . . . ? C8 N3 C6 N4 -0.5(5) . . . . ? C9 N3 C6 N4 180.0(4) . . . . ? C6 N4 C7 C8 -0.6(6) . . . . ? N4 C7 C8 N3 0.3(6) . . . . ? C6 N3 C8 C7 0.1(5) . . . . ? C9 N3 C8 C7 179.7(4) . . . . ? C6 N3 C9 C10 -102.8(5) . . . . ? C8 N3 C9 C10 77.7(5) . . . . ? N3 C9 C10 O14 -53.5(4) . . . . ? N3 C9 C10 P3 67.8(4) . . . . ? N3 C9 C10 P4 -167.8(3) . . . . ? O10 P3 C10 O14 -179.7(3) . . . . ? O8 P3 C10 O14 -55.4(3) . . . . ? O9 P3 C10 O14 58.4(3) . . . . ? O10 P3 C10 C9 61.2(3) . . . . ? O8 P3 C10 C9 -174.5(3) . . . . ? O9 P3 C10 C9 -60.6(3) . . . . ? O10 P3 C10 P4 -62.6(2) . . . . ? O8 P3 C10 P4 61.8(2) . . . . ? O9 P3 C10 P4 175.58(18) . . . . ? O13 P4 C10 O14 -62.1(3) . . . . ? O11 P4 C10 O14 66.2(3) . . . . ? O12 P4 C10 O14 -175.9(2) . . . . ? O13 P4 C10 C9 51.7(3) . . . . ? O11 P4 C10 C9 -179.9(3) . . . . ? O12 P4 C10 C9 -62.1(3) . . . . ? O13 P4 C10 P3 178.81(19) . . . . ? O11 P4 C10 P3 -52.9(2) . . . . ? O12 P4 C10 P3 65.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WD O6 0.85 1.98 2.825(4) 179.9 . O12 H12A O5 0.82 1.90 2.706(4) 168.6 . O1W H1WA O13 0.85 1.83 2.654(5) 162.9 2_645 O2W H2WD O6 0.85 2.02 2.752(4) 144.1 4_566 O2W H2WC O12 0.85 1.97 2.757(5) 153.4 3_666 O3 H3A O2W 0.82 1.75 2.563(4) 168.6 1_554 O7 H7A O10 0.82 1.92 2.741(4) 173.7 3_665 N2 H2A O2 0.86 2.10 2.824(5) 141.8 4_566 O9 H9C O1W 0.82 1.70 2.512(4) 171.7 3_665 O14 H14A O1 0.82 1.95 2.741(4) 163.4 3_565 N4 H4C O4 0.86 1.96 2.757(5) 153.5 4_575 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.632 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.108 # Attachment 'Cu-4.cif' data_cu _database_code_depnum_ccdc_archive 'CCDC 683974' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H18 Cu3 N4 O16 P4' _chemical_formula_sum 'C10 H18 Cu3 N4 O16 P4' _chemical_formula_weight 764.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4745(19) _cell_length_b 8.140(2) _cell_length_c 9.527(3) _cell_angle_alpha 104.480(5) _cell_angle_beta 107.899(4) _cell_angle_gamma 101.887(5) _cell_volume 508.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 2.385 _cell_measurement_theta_max 27.013 _exptl_crystal_description blocky _exptl_crystal_colour sky-blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 381 _exptl_absorpt_coefficient_mu 3.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.871 _exptl_absorpt_process_details 'SADABS,(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Apex 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 4699 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1997 _reflns_number_gt 1638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. ; _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^)+(0.0500P)^2^+0.8800P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1997 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2942(7) 0.5663(6) 0.9481(6) 0.0327(11) Uani 1 1 d . . . H1A H 0.3993 0.6124 1.0446 0.039 Uiso 1 1 calc R . . C2 C 0.0213(7) 0.3962(7) 0.7550(6) 0.0346(11) Uani 1 1 d . . . H2B H -0.0953 0.3041 0.6923 0.042 Uiso 1 1 calc R . . C3 C 0.1073(7) 0.5331(7) 0.7193(6) 0.0326(11) Uani 1 1 d . . . H3A H 0.0569 0.5540 0.6255 0.039 Uiso 1 1 calc R . . C4 C 0.4049(7) 0.7996(6) 0.8460(6) 0.0318(11) Uani 1 1 d . . . H4A H 0.5136 0.8458 0.9471 0.038 Uiso 1 1 calc R . . H4B H 0.3331 0.8860 0.8419 0.038 Uiso 1 1 calc R . . C5 C 0.4908(7) 0.7841(6) 0.7174(5) 0.0326(11) Uani 1 1 d . . . Cu1 Cu 0.57715(9) 0.75668(8) 0.43190(7) 0.0367(2) Uani 1 1 d . . . Cu2 Cu 1.0000 1.0000 1.0000 0.0412(3) Uani 1 2 d S . . N1 N 0.2722(7) 0.6326(6) 0.8359(6) 0.0417(11) Uani 1 1 d . . . N2 N 0.1422(6) 0.4220(6) 0.9027(5) 0.0339(9) Uani 1 1 d . . . H2A H 0.123(9) 0.356(8) 0.958(7) 0.041 Uiso 1 1 d . . . O1 O 0.7005(5) 0.9809(5) 0.6038(4) 0.0406(9) Uani 1 1 d . . . O2 O 0.7907(5) 1.0884(4) 0.8976(4) 0.0351(8) Uani 1 1 d . . . O3 O 0.4823(5) 1.1194(4) 0.7203(4) 0.0297(7) Uani 1 1 d . . . O4 O 0.7049(5) 0.6366(4) 0.5788(4) 0.0365(8) Uani 1 1 d . . . O5 O 0.8414(5) 0.7525(4) 0.8776(4) 0.0355(8) Uani 1 1 d . . . O6 O 0.5641(5) 0.4710(5) 0.7309(4) 0.0343(8) Uani 1 1 d . . . O7 O 0.3383(5) 0.7106(5) 0.5646(4) 0.0386(9) Uani 1 1 d . . . H7A H 0.330(9) 0.606(9) 0.526(7) 0.046 Uiso 1 1 d . . . O1W O 1.1118(6) 1.0265(5) 0.7672(4) 0.0312(8) Uani 1 1 d . . . H1B H 1.150(9) 1.026(8) 0.692(7) 0.037 Uiso 1 1 d . . . H1C H 1.028(9) 0.927(8) 0.745(7) 0.037 Uiso 1 1 d . . . P1 P 0.6260(2) 1.01094(18) 0.73635(16) 0.0361(3) Uani 1 1 d . . . P2 P 0.6639(2) 0.65181(18) 0.72815(15) 0.0359(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(3) 0.022(2) 0.033(3) 0.0014(19) 0.007(2) 0.002(2) C2 0.028(2) 0.036(3) 0.034(3) 0.015(2) 0.011(2) -0.005(2) C3 0.031(2) 0.042(3) 0.029(3) 0.016(2) 0.015(2) 0.008(2) C4 0.033(3) 0.024(2) 0.032(3) 0.0044(19) 0.009(2) 0.007(2) C5 0.033(3) 0.027(2) 0.020(2) -0.0016(18) -0.0021(19) 0.004(2) Cu1 0.0336(4) 0.0334(4) 0.0284(3) 0.0030(3) 0.0031(3) 0.0027(3) Cu2 0.0336(5) 0.0342(5) 0.0351(5) 0.0026(4) -0.0021(4) 0.0028(4) N1 0.033(2) 0.036(2) 0.040(3) 0.009(2) 0.0063(19) -0.0065(19) N2 0.035(2) 0.035(2) 0.031(2) 0.0167(18) 0.0086(18) 0.0076(19) O1 0.0325(19) 0.0313(19) 0.036(2) -0.0009(15) 0.0030(16) -0.0042(16) O2 0.0293(18) 0.0280(18) 0.0289(18) 0.0035(13) -0.0025(14) -0.0014(14) O3 0.0296(17) 0.0259(16) 0.0237(16) 0.0043(13) 0.0028(14) 0.0047(14) O4 0.0333(18) 0.0300(18) 0.0326(19) 0.0061(14) 0.0023(15) 0.0031(15) O5 0.0318(18) 0.0257(17) 0.0369(19) 0.0085(14) 0.0028(15) 0.0027(14) O6 0.0307(18) 0.0326(18) 0.0194(16) -0.0049(13) -0.0008(14) 0.0011(15) O7 0.0347(19) 0.0284(19) 0.0284(18) -0.0026(15) -0.0064(15) 0.0036(16) O1W 0.045(2) 0.0231(17) 0.0342(19) 0.0136(14) 0.0201(17) 0.0150(15) P1 0.0277(7) 0.0349(7) 0.0317(7) 0.0040(5) 0.0031(5) 0.0025(5) P2 0.0311(7) 0.0349(7) 0.0239(6) 0.0007(5) 0.0007(5) 0.0003(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 C1 N1 1.296(7) . ? C1 N2 1.323(6) . ? C1 H1A 0.9300 . ? C2 C3 1.341(7) . ? C2 N2 1.354(7) . ? C2 H2B 0.9300 . ? C3 N1 1.306(7) . ? C3 H3A 0.9300 . ? C4 N1 1.470(6) . ? C4 C5 1.540(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O7 1.429(5) . ? C5 P2 1.841(5) . ? C5 P1 1.848(5) . ? Cu1 O6 1.925(3) 2_666 ? Cu1 O1 1.936(3) . ? Cu1 O3 1.958(3) 2_676 ? Cu1 O4 2.018(4) . ? Cu2 O2 1.948(4) 2_777 ? Cu2 O2 1.948(4) . ? Cu2 O5 1.953(3) 2_777 ? Cu2 O5 1.953(3) . ? N2 H2A 0.86(6) . ? O1 P1 1.516(4) . ? O2 P1 1.519(3) . ? O3 P1 1.522(4) . ? O3 Cu1 1.958(3) 2_676 ? O4 P2 1.526(4) . ? O5 P2 1.506(4) . ? O6 P2 1.518(4) . ? O6 Cu1 1.925(3) 2_666 ? O7 H7A 0.82(6) . ? O1W H1B 0.85(6) . ? O1W H1C 0.85(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 108.7(4) . . ? N1 C1 H1A 125.7 . . ? N2 C1 H1A 125.7 . . ? C3 C2 N2 104.5(4) . . ? C3 C2 H2B 127.7 . . ? N2 C2 H2B 127.7 . . ? N1 C3 C2 109.9(5) . . ? N1 C3 H3A 125.0 . . ? C2 C3 H3A 125.0 . . ? N1 C4 C5 115.3(4) . . ? N1 C4 H4A 108.5 . . ? C5 C4 H4A 108.5 . . ? N1 C4 H4B 108.5 . . ? C5 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? O7 C5 C4 111.5(4) . . ? O7 C5 P2 108.5(3) . . ? C4 C5 P2 114.1(4) . . ? O7 C5 P1 106.4(3) . . ? C4 C5 P1 108.3(3) . . ? P2 C5 P1 107.7(3) . . ? O6 Cu1 O1 174.63(16) 2_666 . ? O6 Cu1 O3 90.97(14) 2_666 2_676 ? O1 Cu1 O3 91.29(15) . 2_676 ? O6 Cu1 O4 90.55(15) 2_666 . ? O1 Cu1 O4 88.54(15) . . ? O3 Cu1 O4 164.96(15) 2_676 . ? O2 Cu2 O2 180.000(2) 2_777 . ? O2 Cu2 O5 91.94(14) 2_777 2_777 ? O2 Cu2 O5 88.06(14) . 2_777 ? O2 Cu2 O5 88.06(14) 2_777 . ? O2 Cu2 O5 91.94(14) . . ? O5 Cu2 O5 180.000(1) 2_777 . ? C1 N1 C3 108.4(4) . . ? C1 N1 C4 124.7(4) . . ? C3 N1 C4 126.7(5) . . ? C1 N2 C2 108.5(4) . . ? C1 N2 H2A 126(4) . . ? C2 N2 H2A 126(4) . . ? P1 O1 Cu1 118.7(2) . . ? P1 O2 Cu2 131.6(2) . . ? P1 O3 Cu1 126.0(2) . 2_676 ? P2 O4 Cu1 119.3(2) . . ? P2 O5 Cu2 137.9(2) . . ? P2 O6 Cu1 132.2(2) . 2_666 ? C5 O7 H7A 109(5) . . ? H1B O1W H1C 110(5) . . ? O1 P1 O2 113.3(2) . . ? O1 P1 O3 112.9(2) . . ? O2 P1 O3 111.2(2) . . ? O1 P1 C5 104.0(2) . . ? O2 P1 C5 106.6(2) . . ? O3 P1 C5 108.2(2) . . ? O5 P2 O6 110.4(2) . . ? O5 P2 O4 114.6(2) . . ? O6 P2 O4 111.84(19) . . ? O5 P2 C5 107.0(2) . . ? O6 P2 C5 108.9(2) . . ? O4 P2 C5 103.6(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O5 0.86(6) 1.96(6) 2.796(6) 163(6) 2_667 O7 H7A O4 0.82(6) 1.90(7) 2.717(5) 176(7) 2_666 O1W H1B O3 0.85(6) 2.35(6) 2.917(5) 125(5) 1_655 O1W H1C O5 0.85(6) 2.59(6) 3.284(5) 140(5) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.658 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.110