#Supplementary Material for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hui-Hua Song' 'Li-Min Zheng' 'Yong-Jiang Liu' 'Xin-Quan Xin' 'Allan J. Jacobson' 'Silvio Decurtins' _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_address ; State Key Lab of Coordination Chemistry, Nanjing University, Nanjing 210093, People's Republic of China ; _publ_contact_author_email 'lmzheng@netra.nju.edu.cn' _publ_section_title ; Syntheses, structures and magnetic properties of two copper(II) diphosphonates: [NH3(CH2)2NH3]2Cu2(hedp)2.H2O and [NH3CH(CH3)CH2NH3]2Cu2(hedp)2 (hedp = 1-hydroxyethylidenediphosphonate) ; data_(enH2)2Cu2(hedp)2.H2O _database_code_CSD 162088 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H30 Cu2 N4 O15 P4' _chemical_formula_weight 673.32 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2579(10) _cell_length_b 5.5010(4) _cell_length_c 16.8746(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.1880(10) _cell_angle_gamma 90.00 _cell_volume 1116.24(15) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'column' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_method ? _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 2.271 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens SMART CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 5008 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 23.30 _reflns_number_total 1781 _reflns_number_observed 1552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0321P)^2^+4.1513P] 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 SHELXL _refine_ls_extinction_coef 0.0073(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1599 _refine_ls_number_parameters 183 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.182 _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 0.95360(4) 0.26013(8) 0.47508(3) 0.0106(2) Uani 1 1 d . . . P1 P 0.85325(8) 0.54037(18) 0.59736(6) 0.0120(3) Uani 1 1 d . . . P2 P 0.80889(8) 0.70957(18) 0.42599(6) 0.0100(3) Uani 1 1 d . . . O1 O 0.8771(2) 0.2874(5) 0.56611(16) 0.0158(6) Uani 1 1 d . . . O3 O 0.8069(2) 0.5254(5) 0.67405(16) 0.0195(6) Uani 1 1 d . . . O4 O 0.8378(2) 0.4507(5) 0.40455(15) 0.0131(6) Uani 1 1 d . . . O6 O 0.7266(2) 0.8303(5) 0.35848(15) 0.0146(6) Uani 1 1 d . . . O7 O 0.7166(2) 0.9153(5) 0.54472(17) 0.0185(6) Uani 1 1 d D . . H4 H 0.777(2) 1.012(7) 0.556(3) 0.022 Uiso 1 1 d D . . O1W O 0.5370(5) 1.0086(10) 0.4089(3) 0.0235(13) Uani 0.50 1 d PD . . H1WA H 0.483(3) 0.983(9) 0.435(2) 0.028 Uiso 1 1 d D . . C1 C 0.7488(3) 0.6810(7) 0.5175(2) 0.0130(8) Uani 1 1 d . . . C2 C 0.6453(3) 0.5235(9) 0.5008(3) 0.0196(9) Uani 1 1 d . . . H1 H 0.584(4) 0.614(9) 0.463(3) 0.029 Uiso 1 1 d . . . H2 H 0.658(4) 0.388(10) 0.476(3) 0.029 Uiso 1 1 d . . . H3 H 0.621(4) 0.500(9) 0.546(3) 0.029 Uiso 1 1 d . . . N1 N 1.1217(3) -0.0811(7) 0.7253(2) 0.0185(8) Uani 1 1 d . . . H5 H 1.171(4) -0.033(9) 0.703(3) 0.022 Uiso 1 1 d . . . H6 H 1.156(4) -0.174(9) 0.768(3) 0.022 Uiso 1 1 d . . . H7 H 1.074(4) -0.176(9) 0.692(3) 0.022 Uiso 1 1 d . . . C3 C 1.0595(4) 0.1270(9) 0.7499(3) 0.0285(11) Uani 1 1 d D . . H8 H 1.107(5) 0.221(10) 0.787(3) 0.043 Uiso 1 1 d . . . H9 H 1.044(4) 0.257(10) 0.705(3) 0.043 Uiso 1 1 d . . . C4 C 0.9544(4) 0.0211(10) 0.7753(4) 0.0221(13) Uiso 0.75 1 d PD . . C4' C 0.9757(9) 0.100(4) 0.8041(8) 0.027(4) Uiso 0.25 1 d PD . . N2 N 0.8862(4) 0.2236(8) 0.7981(3) 0.0198(11) Uiso 0.75 1 d PD . . N2' N 0.8710(10) 0.060(2) 0.7458(8) 0.019(3) Uiso 0.25 1 d PD . . O2 O 0.9560(2) 0.7054(5) 0.60905(16) 0.0155(6) Uani 1 1 d . . . O5 O 0.9132(2) 0.8702(5) 0.44982(15) 0.0119(6) 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 0.0096(3) 0.0096(3) 0.0126(3) 0.00057(17) 0.0022(2) 0.00047(17) P1 0.0107(5) 0.0136(5) 0.0122(5) 0.0017(4) 0.0036(4) 0.0013(4) P2 0.0084(5) 0.0105(5) 0.0108(5) -0.0005(4) 0.0009(4) 0.0001(4) O1 0.0166(14) 0.0137(14) 0.0183(15) 0.0037(11) 0.0069(12) 0.0026(11) O2 0.0122(14) 0.0204(15) 0.0136(14) 0.0005(12) 0.0019(11) 0.0003(12) O3 0.0179(14) 0.0259(16) 0.0169(14) 0.0042(12) 0.0086(12) 0.0035(12) O4 0.0136(13) 0.0109(14) 0.0139(13) -0.0013(11) 0.0005(11) 0.0003(11) O5 0.0111(13) 0.0109(14) 0.0127(13) 0.0015(11) 0.0002(10) 0.0004(11) O6 0.0113(13) 0.0158(14) 0.0155(14) 0.0010(12) -0.0007(11) 0.0017(11) O7 0.0172(14) 0.0142(15) 0.0250(15) -0.0030(12) 0.0061(12) 0.0022(12) O1W 0.028(3) 0.013(3) 0.023(3) 0.003(2) -0.011(3) 0.014(3) C1 0.0124(19) 0.012(2) 0.015(2) -0.0006(17) 0.0033(16) 0.0020(16) C2 0.013(2) 0.024(2) 0.023(2) -0.001(2) 0.0062(19) -0.0037(19) N1 0.0145(18) 0.024(2) 0.0156(18) 0.0034(17) 0.0007(15) -0.0018(16) C3 0.028(3) 0.031(3) 0.030(3) 0.009(2) 0.014(2) 0.010(2) _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 1.955(3) . ? Cu1 O4 1.968(3) . ? Cu1 O2 1.972(3) 3_766 ? Cu1 O5 1.995(2) 3_766 ? Cu1 O5 2.224(3) 1_545 ? Cu1 Cu1 2.9316(9) 3_766 ? P1 O3 1.513(3) . ? P1 O2 1.534(3) . ? P1 O1 1.536(3) . ? P1 C1 1.840(4) . ? P2 O6 1.520(3) . ? P2 O4 1.528(3) . ? P2 O5 1.543(3) . ? P2 C1 1.842(4) . ? O7 C1 1.449(5) . ? C1 C2 1.516(6) . ? N1 C3 1.478(6) . ? C3 C4' 1.510(9) . ? C3 C4 1.549(6) . ? C4 C4' 0.667(16) . ? C4 N2' 1.069(13) . ? C4 N2 1.488(6) . ? C4' N2 1.278(16) . ? C4' N2' 1.475(10) . ? N2 N2' 1.248(14) . ? O2 Cu1 1.972(3) 3_766 ? O5 Cu1 1.995(2) 3_766 ? O5 Cu1 2.224(3) 1_565 ? 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 91.99(11) . . ? O1 Cu1 O2 168.70(12) . 3_766 ? O4 Cu1 O2 87.32(11) . 3_766 ? O1 Cu1 O5 89.24(11) . 3_766 ? O4 Cu1 O5 168.64(11) . 3_766 ? O2 Cu1 O5 89.27(10) 3_766 3_766 ? O1 Cu1 O5 95.84(10) . 1_545 ? O4 Cu1 O5 106.88(10) . 1_545 ? O2 Cu1 O5 95.15(10) 3_766 1_545 ? O5 Cu1 O5 84.21(10) 3_766 1_545 ? O1 Cu1 Cu1 85.65(8) . 3_766 ? O4 Cu1 Cu1 83.58(8) . 3_766 ? O2 Cu1 Cu1 83.06(8) 3_766 3_766 ? O5 Cu1 Cu1 85.25(8) 3_766 3_766 ? O5 Cu1 Cu1 169.34(7) 1_545 3_766 ? O3 P1 O2 110.94(16) . . ? O3 P1 O1 111.86(16) . . ? O2 P1 O1 111.98(16) . . ? O3 P1 C1 109.02(16) . . ? O2 P1 C1 106.44(17) . . ? O1 P1 C1 106.31(17) . . ? O6 P2 O4 112.38(15) . . ? O6 P2 O5 109.94(15) . . ? O4 P2 O5 112.13(14) . . ? O6 P2 C1 110.50(16) . . ? O4 P2 C1 105.54(16) . . ? O5 P2 C1 106.08(16) . . ? P1 O1 Cu1 119.43(15) . . ? P2 O4 Cu1 121.77(15) . . ? O7 C1 C2 107.4(3) . . ? O7 C1 P1 109.6(2) . . ? C2 C1 P1 109.5(3) . . ? O7 C1 P2 111.6(3) . . ? C2 C1 P2 110.4(3) . . ? P1 C1 P2 108.36(19) . . ? N1 C3 C4' 122.9(9) . . ? N1 C3 C4 106.8(4) . . ? C4' C3 C4 25.1(6) . . ? C4' C4 N2' 114.3(16) . . ? C4' C4 N2 58.9(14) . . ? N2' C4 N2 55.6(7) . . ? C4' C4 C3 74.2(10) . . ? N2' C4 C3 124.6(9) . . ? N2 C4 C3 109.2(4) . . ? C4 C4' N2 94.6(14) . . ? C4 C4' N2' 41.3(11) . . ? N2 C4' N2' 53.3(7) . . ? C4 C4' C3 80.7(11) . . ? N2 C4' C3 125.1(12) . . ? N2' C4' C3 102.5(10) . . ? N2' N2 C4' 71.4(7) . . ? N2' N2 C4 44.9(6) . . ? C4' N2 C4 26.5(7) . . ? C4 N2' N2 79.5(8) . . ? C4 N2' C4' 24.3(8) . . ? N2 N2' C4' 55.2(8) . . ? P1 O2 Cu1 121.75(16) . 3_766 ? P2 O5 Cu1 119.63(15) . 3_766 ? P2 O5 Cu1 138.16(15) . 1_565 ? Cu1 O5 Cu1 95.79(10) 3_766 1_565 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.769 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.097 #===END data_(1,2-pnH2)2Cu2(hedp)2 _database_code_CSD 162089 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H32 Cu2 N4 O14 P4' _chemical_formula_weight 683.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.410(5) _cell_length_b 5.4507(10) _cell_length_c 18.890(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.13(2) _cell_angle_gamma 90.00 _cell_volume 2205.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 4.69 _cell_measurement_theta_max 9.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 2.298 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4146 _exptl_absorpt_correction_T_max 0.4605 _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 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 3.72 _diffrn_reflns_number 4750 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1935 _reflns_number_gt 1713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0295P)^2^+5.3083P] 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 SHELXL _refine_ls_extinction_coef 0.00033(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1935 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.741875(15) 0.98948(6) 0.964554(18) 0.01210(14) Uani 1 1 d . . . P1 P 0.62560(3) 0.70433(13) 0.97447(4) 0.01200(19) Uani 1 1 d . . . P2 P 0.69316(3) 0.53865(13) 0.86829(4) 0.01068(18) Uani 1 1 d . . . O1 O 0.65729(9) 0.9524(4) 0.97377(11) 0.0169(4) Uani 1 1 d . . . O2 O 0.66771(9) 0.5303(4) 1.03217(11) 0.0157(4) Uani 1 1 d . . . O3 O 0.56270(9) 0.7358(4) 0.98817(11) 0.0204(5) Uani 1 1 d . . . O4 O 0.71949(9) 0.7995(3) 0.87291(10) 0.0145(4) Uani 1 1 d . . . O5 O 0.73252(9) 0.3784(4) 0.93270(10) 0.0134(4) Uani 1 1 d . . . O6 O 0.68736(9) 0.4174(4) 0.79435(10) 0.0158(4) Uani 1 1 d . . . O7 O 0.59011(9) 0.3163(4) 0.88518(12) 0.0243(5) Uani 1 1 d . . . H7A H 0.6158 0.2290 0.9143 0.036 Uiso 1 1 calc R . . C1 C 0.61603(13) 0.5584(5) 0.88424(15) 0.0139(6) Uani 1 1 d . . . C2 C 0.57071(14) 0.6981(7) 0.82254(16) 0.0270(8) Uani 1 1 d . . . H2A H 0.5309 0.7065 0.8319 0.040 Uiso 1 1 calc R . . H2B H 0.5661 0.6156 0.7763 0.040 Uiso 1 1 calc R . . H2C H 0.5862 0.8611 0.8201 0.040 Uiso 1 1 calc R . . C3 C 0.65985(14) 0.0937(6) 1.16672(17) 0.0215(7) Uani 1 1 d . . . H3A H 0.6713 0.0074 1.2137 0.026 Uiso 1 1 calc R . . H3B H 0.6711 -0.0098 1.1309 0.026 Uiso 1 1 calc R . . C4 C 0.58959(13) 0.1318(6) 1.14175(16) 0.0192(6) Uani 1 1 d . . . H4A H 0.5792 0.2666 1.1703 0.023 Uiso 1 1 calc R . . N2 N 0.56608(12) 0.1936(5) 1.06059(14) 0.0217(6) Uani 1 1 d . . . H5B H 0.5249 0.2150 1.0476 0.032 Uiso 1 1 calc R . . H5C H 0.5752 0.0715 1.0342 0.032 Uiso 1 1 calc R . . H5D H 0.5843 0.3309 1.0519 0.032 Uiso 1 1 calc R . . C5 C 0.55694(16) -0.0999(7) 1.15542(19) 0.0292(7) Uani 1 1 d . . . H6A H 0.5126 -0.0745 1.1395 0.044 Uiso 1 1 calc R . . H6B H 0.5703 -0.1382 1.2073 0.044 Uiso 1 1 calc R . . H6C H 0.5673 -0.2334 1.1280 0.044 Uiso 1 1 calc R . . N1 N 0.69632(11) 0.3251(5) 1.17534(13) 0.0185(5) Uani 1 1 d . . . H1C H 0.7369 0.2905 1.1900 0.028 Uiso 1 1 calc R . . H1A H 0.6870 0.4197 1.2090 0.028 Uiso 1 1 calc R . . H1B H 0.6869 0.4037 1.1322 0.028 Uiso 1 1 calc R . . 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 0.0134(2) 0.0104(2) 0.0122(2) -0.00025(13) 0.00350(14) -0.00007(13) P1 0.0104(3) 0.0133(4) 0.0126(3) -0.0007(3) 0.0037(3) 0.0004(3) P2 0.0111(4) 0.0110(3) 0.0096(3) -0.0004(3) 0.0026(3) 0.0002(3) O1 0.0162(10) 0.0144(10) 0.0207(10) -0.0008(9) 0.0065(8) -0.0005(8) O2 0.0156(10) 0.0170(10) 0.0140(10) 0.0018(8) 0.0036(8) 0.0019(8) O3 0.0138(10) 0.0279(12) 0.0209(10) -0.0039(10) 0.0069(8) 0.0002(9) O4 0.0187(10) 0.0113(10) 0.0135(9) 0.0006(8) 0.0050(8) -0.0014(8) O5 0.0152(10) 0.0114(10) 0.0127(9) 0.0012(8) 0.0025(7) 0.0020(8) O6 0.0178(10) 0.0174(10) 0.0118(9) -0.0012(9) 0.0037(8) 0.0006(9) O7 0.0191(11) 0.0183(11) 0.0348(13) -0.0030(10) 0.0068(9) -0.0065(9) C1 0.0120(13) 0.0157(14) 0.0133(13) -0.0011(12) 0.0026(11) -0.0016(11) C2 0.0210(16) 0.040(2) 0.0186(15) 0.0022(15) 0.0033(12) 0.0124(15) C3 0.0197(16) 0.0215(16) 0.0226(16) -0.0012(14) 0.0052(12) -0.0017(13) C4 0.0190(15) 0.0206(16) 0.0176(14) -0.0019(13) 0.0046(11) 0.0005(13) N2 0.0191(13) 0.0224(13) 0.0226(13) -0.0020(11) 0.0047(10) -0.0001(11) C5 0.0285(17) 0.0299(18) 0.0308(18) -0.0001(16) 0.0111(14) -0.0069(16) N1 0.0154(12) 0.0238(14) 0.0163(12) -0.0024(11) 0.0045(10) -0.0006(11) _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 1.9516(19) . ? Cu1 O1 1.964(2) . ? Cu1 O5 1.9897(19) 7_667 ? Cu1 O2 2.012(2) 7_667 ? Cu1 O5 2.197(2) 1_565 ? Cu1 Cu1 2.9076(8) 7_667 ? P1 O3 1.516(2) . ? P1 O1 1.529(2) . ? P1 O2 1.540(2) . ? P1 C1 1.835(3) . ? P2 O6 1.516(2) . ? P2 O4 1.532(2) . ? P2 O5 1.546(2) . ? P2 C1 1.843(3) . ? O2 Cu1 2.012(2) 7_667 ? O5 Cu1 1.9897(19) 7_667 ? O5 Cu1 2.197(2) 1_545 ? O7 C1 1.444(4) . ? C1 C2 1.507(4) . ? C3 N1 1.485(4) . ? C3 C4 1.519(4) . ? C4 N2 1.505(4) . ? C4 C5 1.520(5) . ? 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 O1 91.23(9) . . ? O4 Cu1 O5 169.18(8) . 7_667 ? O1 Cu1 O5 87.67(8) . 7_667 ? O4 Cu1 O2 89.56(8) . 7_667 ? O1 Cu1 O2 168.88(8) . 7_667 ? O5 Cu1 O2 89.48(8) 7_667 7_667 ? O4 Cu1 O5 106.87(8) . 1_565 ? O1 Cu1 O5 96.14(8) . 1_565 ? O5 Cu1 O5 83.95(8) 7_667 1_565 ? O2 Cu1 O5 94.25(8) 7_667 1_565 ? O4 Cu1 Cu1 84.07(6) . 7_667 ? O1 Cu1 Cu1 81.95(6) . 7_667 ? O5 Cu1 Cu1 85.11(6) 7_667 7_667 ? O2 Cu1 Cu1 87.10(6) 7_667 7_667 ? O5 Cu1 Cu1 168.97(5) 1_565 7_667 ? O3 P1 O1 111.03(12) . . ? O3 P1 O2 110.84(12) . . ? O1 P1 O2 111.18(12) . . ? O3 P1 C1 110.34(12) . . ? O1 P1 C1 107.61(13) . . ? O2 P1 C1 105.66(13) . . ? O6 P2 O4 112.60(11) . . ? O6 P2 O5 110.66(11) . . ? O4 P2 O5 111.02(11) . . ? O6 P2 C1 110.25(12) . . ? O4 P2 C1 107.48(12) . . ? O5 P2 C1 104.46(12) . . ? P1 O1 Cu1 123.68(12) . . ? P1 O2 Cu1 117.15(12) . 7_667 ? P2 O4 Cu1 122.48(11) . . ? P2 O5 Cu1 119.79(12) . 7_667 ? P2 O5 Cu1 138.36(12) . 1_545 ? Cu1 O5 Cu1 96.05(8) 7_667 1_545 ? O7 C1 C2 106.8(2) . . ? O7 C1 P1 108.78(19) . . ? C2 C1 P1 111.5(2) . . ? O7 C1 P2 110.39(19) . . ? C2 C1 P2 110.7(2) . . ? P1 C1 P2 108.58(14) . . ? N1 C3 C4 113.8(3) . . ? N2 C4 C3 111.5(2) . . ? N2 C4 C5 108.5(2) . . ? C3 C4 C5 109.9(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.586 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.141