# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Abraham Clearfield' 'Deyuan Kong' 'Yan Li' 'Joseph H. Ross' _publ_contact_author_name 'Dr Abraham Clearfield' _publ_contact_author_address ; Texas A & M University UNITED STATES OF AMERICA ; _publ_contact_author_email CLEARFIELD@MAIL.CHEM.TAMU.EDU _publ_section_title ; A novel copper arganophosphonate with a pore-like 3D network and Cu-Cu magnetic ordering ; data_solmc _database_code_CSD 205353 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cu3 N2 O12 P4' _chemical_formula_weight 594.66 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.4430(10) _cell_length_b 9.3681(10) _cell_length_c 16.0755(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1422.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 4.968 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.4078 _exptl_absorpt_correction_T_max 0.5644 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 7628 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1627 _reflns_number_gt 1310 _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. ; _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^)+(0.0940P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1627 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.74404(5) 0.06244(6) 0.36090(3) 0.0135(2) Uani 1 1 d . . . Cu2 Cu 1.0000 0.0000 0.5000 0.0118(2) Uani 1 2 d S . . P1 P 0.77715(13) 0.31430(13) 0.47673(7) 0.0124(3) Uani 1 1 d . . . P2 P 1.05332(12) 0.09743(13) 0.31051(7) 0.0131(3) Uani 1 1 d . . . O6 O 1.1191(3) 0.1640(3) 0.5255(2) 0.0141(7) Uani 1 1 d . . . O1 O 0.8124(3) 0.1568(3) 0.45961(19) 0.0143(7) Uani 1 1 d . . . O5 O 1.0656(3) -0.0063(3) 0.38321(19) 0.0126(7) Uani 1 1 d . . . O3 O 0.6429(3) -0.0827(3) 0.4205(2) 0.0152(7) Uani 1 1 d . . . O4 O 0.6274(3) 0.0380(4) 0.2647(2) 0.0180(7) Uani 1 1 d . . . O2 O 0.8994(3) 0.1357(3) 0.29341(19) 0.0162(7) Uani 1 1 d . . . C2 C 1.1398(5) 0.2624(5) 0.3403(3) 0.0149(9) Uani 1 1 d . . . H2A H 1.1224 0.3352 0.2969 0.018 Uiso 1 1 calc R . . H2B H 1.0974 0.2975 0.3928 0.018 Uiso 1 1 calc R . . C1 C 0.8460(5) 0.3522(5) 0.5802(3) 0.0134(9) Uani 1 1 d . . . H1A H 0.9506 0.3479 0.5779 0.016 Uiso 1 1 calc R . . H1B H 0.8194 0.4512 0.5952 0.016 Uiso 1 1 calc R . . N1 N 0.7962(4) 0.2546(5) 0.6479(2) 0.0145(8) Uani 1 1 d . . . H1C H 0.8339 0.2867 0.6972 0.017 Uiso 1 1 calc R . . H1D H 0.8339 0.1657 0.6380 0.017 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 0.0133(4) 0.0159(4) 0.0114(4) 0.0004(2) -0.0007(2) -0.0006(2) Cu2 0.0115(5) 0.0135(5) 0.0105(4) -0.0005(3) 0.0006(3) -0.0011(3) P1 0.0125(6) 0.0135(6) 0.0112(6) -0.0003(4) 0.0006(5) 0.0013(4) P2 0.0112(6) 0.0167(6) 0.0113(6) 0.0005(5) 0.0001(4) -0.0011(5) O6 0.0111(16) 0.0174(17) 0.0139(15) -0.0021(13) 0.0031(13) -0.0013(12) O1 0.0141(17) 0.0158(16) 0.0132(15) -0.0026(13) 0.0003(13) 0.0027(13) O5 0.0105(16) 0.0123(17) 0.0150(16) -0.0005(12) 0.0016(12) -0.0006(11) O3 0.0118(17) 0.0156(16) 0.0184(15) 0.0034(13) -0.0030(13) -0.0031(12) O4 0.0168(17) 0.0228(17) 0.0143(16) 0.0036(14) -0.0031(13) -0.0054(14) O2 0.0141(16) 0.0184(17) 0.0161(15) 0.0048(13) 0.0014(13) -0.0002(13) C2 0.013(2) 0.016(2) 0.015(2) -0.0004(18) -0.0018(17) -0.0009(18) C1 0.012(2) 0.015(2) 0.012(2) -0.0013(17) -0.0009(18) -0.0003(17) N1 0.015(2) 0.016(2) 0.0127(18) -0.0029(15) -0.0011(15) 0.0008(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 O4 1.913(3) . ? Cu1 O3 1.918(3) . ? Cu1 O1 1.928(3) . ? Cu1 O2 1.950(3) . ? Cu2 O6 1.947(3) 5_756 ? Cu2 O6 1.947(3) . ? Cu2 O5 1.978(3) 5_756 ? Cu2 O5 1.978(3) . ? Cu2 O1 2.391(3) . ? Cu2 O1 2.391(3) 5_756 ? P1 O6 1.507(3) 4_456 ? P1 O3 1.522(3) 8_765 ? P1 O1 1.538(3) . ? P1 C1 1.820(4) . ? P2 O4 1.503(3) 6_656 ? P2 O2 1.522(3) . ? P2 O5 1.524(3) . ? P2 C2 1.812(5) . ? O6 P1 1.507(3) 4_556 ? O3 P1 1.522(3) 8_755 ? O4 P2 1.503(3) 6_556 ? C2 N1 1.498(6) 4_556 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C1 N1 1.497(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N1 C2 1.498(6) 4_456 ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? 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 91.87(14) . . ? O4 Cu1 O1 156.00(14) . . ? O3 Cu1 O1 94.62(13) . . ? O4 Cu1 O2 91.44(14) . . ? O3 Cu1 O2 154.48(14) . . ? O1 Cu1 O2 92.55(13) . . ? O6 Cu2 O6 180.00(11) 5_756 . ? O6 Cu2 O5 92.41(13) 5_756 5_756 ? O6 Cu2 O5 87.59(13) . 5_756 ? O6 Cu2 O5 87.59(13) 5_756 . ? O6 Cu2 O5 92.41(13) . . ? O5 Cu2 O5 180.0 5_756 . ? O6 Cu2 O1 89.99(12) 5_756 . ? O6 Cu2 O1 90.01(12) . . ? O5 Cu2 O1 90.42(12) 5_756 . ? O5 Cu2 O1 89.58(12) . . ? O6 Cu2 O1 90.01(12) 5_756 5_756 ? O6 Cu2 O1 89.99(12) . 5_756 ? O5 Cu2 O1 89.58(12) 5_756 5_756 ? O5 Cu2 O1 90.42(12) . 5_756 ? O1 Cu2 O1 180.00(14) . 5_756 ? O6 P1 O3 113.07(18) 4_456 8_765 ? O6 P1 O1 109.88(19) 4_456 . ? O3 P1 O1 113.24(18) 8_765 . ? O6 P1 C1 110.4(2) 4_456 . ? O3 P1 C1 104.0(2) 8_765 . ? O1 P1 C1 105.9(2) . . ? O4 P2 O2 112.74(19) 6_656 . ? O4 P2 O5 110.15(19) 6_656 . ? O2 P2 O5 111.21(18) . . ? O4 P2 C2 108.6(2) 6_656 . ? O2 P2 C2 106.1(2) . . ? O5 P2 C2 107.8(2) . . ? P1 O6 Cu2 132.3(2) 4_556 . ? P1 O1 Cu1 120.98(19) . . ? P1 O1 Cu2 134.55(19) . . ? Cu1 O1 Cu2 100.96(13) . . ? P2 O5 Cu2 133.22(19) . . ? P1 O3 Cu1 119.92(19) 8_755 . ? P2 O4 Cu1 150.9(2) 6_556 . ? P2 O2 Cu1 122.34(19) . . ? N1 C2 P2 112.8(3) 4_556 . ? N1 C2 H2A 109.0 4_556 . ? P2 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 4_556 . ? P2 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N1 C1 P1 115.7(3) . . ? N1 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? N1 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C1 N1 C2 117.8(4) . 4_456 ? C1 N1 H1C 107.9 . . ? C2 N1 H1C 107.9 4_456 . ? C1 N1 H1D 107.9 . . ? C2 N1 H1D 107.9 4_456 . ? H1C N1 H1D 107.2 . . ? 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 O6 Cu2 O6 P1 -142(100) 5_756 . . 4_556 ? O5 Cu2 O6 P1 118.9(3) 5_756 . . 4_556 ? O5 Cu2 O6 P1 -61.1(3) . . . 4_556 ? O1 Cu2 O6 P1 -150.7(3) . . . 4_556 ? O1 Cu2 O6 P1 29.3(3) 5_756 . . 4_556 ? O6 P1 O1 Cu1 54.8(3) 4_456 . . . ? O3 P1 O1 Cu1 -72.7(3) 8_765 . . . ? C1 P1 O1 Cu1 174.1(2) . . . . ? O6 P1 O1 Cu2 -150.7(2) 4_456 . . . ? O3 P1 O1 Cu2 81.8(3) 8_765 . . . ? C1 P1 O1 Cu2 -31.5(3) . . . . ? O4 Cu1 O1 P1 -15.9(5) . . . . ? O3 Cu1 O1 P1 -121.1(2) . . . . ? O2 Cu1 O1 P1 83.4(2) . . . . ? O4 Cu1 O1 Cu2 -177.7(3) . . . . ? O3 Cu1 O1 Cu2 77.16(14) . . . . ? O2 Cu1 O1 Cu2 -78.33(14) . . . . ? O6 Cu2 O1 P1 160.0(3) 5_756 . . . ? O6 Cu2 O1 P1 -20.0(3) . . . . ? O5 Cu2 O1 P1 67.6(3) 5_756 . . . ? O5 Cu2 O1 P1 -112.4(3) . . . . ? O1 Cu2 O1 P1 170(100) 5_756 . . . ? O6 Cu2 O1 Cu1 -42.12(15) 5_756 . . . ? O6 Cu2 O1 Cu1 137.88(15) . . . . ? O5 Cu2 O1 Cu1 -134.54(14) 5_756 . . . ? O5 Cu2 O1 Cu1 45.46(14) . . . . ? O1 Cu2 O1 Cu1 -32(100) 5_756 . . . ? O4 P2 O5 Cu2 178.5(2) 6_656 . . . ? O2 P2 O5 Cu2 -55.7(3) . . . . ? C2 P2 O5 Cu2 60.2(3) . . . . ? O6 Cu2 O5 P2 116.6(3) 5_756 . . . ? O6 Cu2 O5 P2 -63.4(3) . . . . ? O5 Cu2 O5 P2 63.7(3) 5_756 . . . ? O1 Cu2 O5 P2 26.6(3) . . . . ? O1 Cu2 O5 P2 -153.4(3) 5_756 . . . ? O4 Cu1 O3 P1 141.0(2) . . . 8_755 ? O1 Cu1 O3 P1 -62.1(2) . . . 8_755 ? O2 Cu1 O3 P1 43.7(4) . . . 8_755 ? O3 Cu1 O4 P2 146.2(5) . . . 6_556 ? O1 Cu1 O4 P2 40.4(7) . . . 6_556 ? O2 Cu1 O4 P2 -59.1(5) . . . 6_556 ? O4 P2 O2 Cu1 126.2(2) 6_656 . . . ? O5 P2 O2 Cu1 1.9(3) . . . . ? C2 P2 O2 Cu1 -115.1(2) . . . . ? O4 Cu1 O2 P2 -140.8(2) . . . . ? O3 Cu1 O2 P2 -43.4(4) . . . . ? O1 Cu1 O2 P2 62.9(2) . . . . ? O4 P2 C2 N1 -53.5(3) 6_656 . . 4_556 ? O2 P2 C2 N1 -174.9(3) . . . 4_556 ? O5 P2 C2 N1 65.9(3) . . . 4_556 ? O6 P1 C1 N1 64.6(4) 4_456 . . . ? O3 P1 C1 N1 -173.8(3) 8_765 . . . ? O1 P1 C1 N1 -54.3(4) . . . . ? P1 C1 N1 C2 -54.9(5) . . . 4_456 ? 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 N1 H1D O5 0.92 1.80 2.713(5) 170.8 5_756 N1 H1C O2 0.92 1.82 2.735(5) 175.0 7_566 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 3.978 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.266