Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Li-Min Zheng' 'Song Gao' 'Zai-Chao Zhang' _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_address ; School of Chemistry Nanjing University Nanjing 210093 ; _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Cobalt diphosphonate with a new ladder-like chain structure exhibiting field-induced magnetic transition ; data_60908am _database_code_depnum_ccdc_archive 'CCDC 652148' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H11 Co N O8 P2' _chemical_formula_sum 'C7 H11 Co N O8 P2' _chemical_formula_weight 358.04 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' Co Co 0.3494 0.9721 '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 ' _symmetry_space_group_name_Hall '-P 2yn' 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 6.5514(15) _cell_length_b 12.477(3) _cell_length_c 13.595(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.029(4) _cell_angle_gamma 90.00 _cell_volume 1100.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 724 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.37 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.683 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5768 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2152 _reflns_number_gt 1895 _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^)+(0.0313P)^2^+0.3588P] 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 2152 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Co1 Co 1.16923(6) -0.06120(3) 0.56528(3) 0.01472(14) Uani 1 1 d . . . P2 P 0.95093(12) 0.13085(6) 0.66339(5) 0.01371(19) Uani 1 1 d . . . P1 P 0.70428(12) -0.06982(6) 0.62703(5) 0.01348(19) Uani 1 1 d . . . N1 N 1.0286(5) 0.2079(2) 1.00986(19) 0.0274(7) Uani 1 1 d . . . H1C H 1.1367 0.2456 1.0288 0.033 Uiso 1 1 calc R . . C1 C 0.7670(5) 0.0431(2) 0.7161(2) 0.0146(6) Uani 1 1 d . . . C2 C 0.8598(5) -0.0019(2) 0.8186(2) 0.0220(7) Uani 1 1 d . . . H2A H 0.7809 -0.0643 0.8332 0.026 Uiso 1 1 calc R . . H2B H 0.9999 -0.0253 0.8152 0.026 Uiso 1 1 calc R . . C3 C 0.8625(5) 0.0774(2) 0.9022(2) 0.0190(7) Uani 1 1 d . . . C4 C 1.0330(5) 0.1379(3) 0.9355(2) 0.0237(7) Uani 1 1 d . . . H4 H 1.1522 0.1304 0.9061 0.028 Uiso 1 1 calc R . . C5 C 0.8645(6) 0.2212(3) 1.0555(2) 0.0316(8) Uani 1 1 d . . . H5 H 0.8673 0.2707 1.1069 0.038 Uiso 1 1 calc R . . C6 C 0.6912(6) 0.1620(3) 1.0268(2) 0.0318(8) Uani 1 1 d . . . H6 H 0.5755 0.1697 1.0589 0.038 Uiso 1 1 calc R . . C7 C 0.6911(5) 0.0911(3) 0.9498(2) 0.0248(7) Uani 1 1 d . . . H7 H 0.5729 0.0513 0.9291 0.030 Uiso 1 1 calc R . . O1 O 0.8404(3) -0.06184(15) 0.54578(14) 0.0143(4) Uani 1 1 d . . . O2 O 0.4789(3) -0.06445(16) 0.59556(15) 0.0200(5) Uani 1 1 d . . . O3 O 0.7690(3) -0.17569(16) 0.68379(14) 0.0184(5) Uani 1 1 d . . . H3D H 0.6718 -0.1986 0.7096 0.028 Uiso 1 1 calc R . . O4 O 0.8451(3) 0.16203(15) 0.55931(14) 0.0164(5) Uani 1 1 d . . . O5 O 1.1451(3) 0.06573(15) 0.66352(14) 0.0170(5) Uani 1 1 d . . . O6 O 0.9871(3) 0.23077(16) 0.72809(14) 0.0183(5) Uani 1 1 d . . . O7 O 0.5869(3) 0.10426(17) 0.72582(15) 0.0213(5) Uani 1 1 d . . . H7D H 0.4843 0.0715 0.7004 0.032 Uiso 1 1 calc R . . O1W O 1.1677(3) -0.19391(18) 0.65977(16) 0.0298(6) Uani 1 1 d . . . H1WA H 1.0444 -0.2040 0.6803 0.045 Uiso 1 1 d R . . H1WB H 1.2787 -0.2211 0.6981 0.045 Uiso 1 1 d 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 Co1 0.0122(2) 0.0173(2) 0.0147(2) -0.00070(16) 0.00179(16) 0.00100(16) P2 0.0137(4) 0.0146(4) 0.0131(4) -0.0011(3) 0.0028(3) -0.0010(3) P1 0.0122(4) 0.0138(4) 0.0147(4) -0.0005(3) 0.0026(3) -0.0005(3) N1 0.0319(18) 0.0218(15) 0.0253(15) 0.0043(12) -0.0068(13) -0.0089(13) C1 0.0147(16) 0.0162(15) 0.0132(14) -0.0004(11) 0.0031(12) 0.0000(12) C2 0.0263(19) 0.0210(17) 0.0189(16) 0.0008(13) 0.0038(14) -0.0014(14) C3 0.0262(18) 0.0179(16) 0.0124(14) 0.0031(12) 0.0005(13) -0.0013(13) C4 0.0263(19) 0.0275(18) 0.0161(15) 0.0038(13) -0.0007(14) -0.0024(15) C5 0.045(2) 0.0236(18) 0.0246(18) -0.0043(15) 0.0007(17) 0.0035(17) C6 0.034(2) 0.035(2) 0.0278(18) -0.0045(16) 0.0093(16) 0.0045(17) C7 0.0229(19) 0.0288(18) 0.0218(16) -0.0010(14) 0.0005(14) -0.0056(15) O1 0.0135(11) 0.0148(10) 0.0147(10) -0.0004(8) 0.0023(8) -0.0001(8) O2 0.0136(12) 0.0261(12) 0.0201(11) -0.0017(9) 0.0019(9) -0.0010(9) O3 0.0162(12) 0.0159(11) 0.0243(11) 0.0042(9) 0.0072(9) 0.0000(9) O4 0.0194(12) 0.0159(11) 0.0135(10) -0.0001(8) 0.0009(9) 0.0019(9) O5 0.0127(11) 0.0220(12) 0.0162(10) -0.0033(8) 0.0012(9) 0.0014(9) O6 0.0173(12) 0.0189(11) 0.0186(11) -0.0068(9) 0.0027(9) -0.0039(9) O7 0.0150(12) 0.0206(11) 0.0289(12) -0.0072(9) 0.0048(9) 0.0008(9) O1W 0.0142(12) 0.0383(14) 0.0368(13) 0.0191(11) 0.0033(10) 0.0035(10) _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 Co1 O2 2.013(2) 1_655 ? Co1 O5 2.092(2) . ? Co1 O1W 2.097(2) . ? Co1 O4 2.1015(19) 3_756 ? Co1 O1 2.134(2) . ? Co1 O1 2.1481(19) 3_756 ? P2 O5 1.509(2) . ? P2 O6 1.525(2) . ? P2 O4 1.536(2) . ? P2 C1 1.845(3) . ? P1 O2 1.480(2) . ? P1 O1 1.517(2) . ? P1 O3 1.558(2) . ? P1 C1 1.865(3) . ? N1 C5 1.325(5) . ? N1 C4 1.339(4) . ? N1 H1C 0.8600 . ? C1 O7 1.427(3) . ? C1 C2 1.546(4) . ? C2 C3 1.506(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.371(4) . ? C3 C7 1.383(5) . ? C4 H4 0.9300 . ? C5 C6 1.365(5) . ? C5 H5 0.9300 . ? C6 C7 1.371(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O1 Co1 2.1481(19) 3_756 ? O2 Co1 2.013(2) 1_455 ? O3 H3D 0.8200 . ? O4 Co1 2.1015(19) 3_756 ? O7 H7D 0.8200 . ? O1W H1WA 0.9002 . ? O1W H1WB 0.9000 . ? 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 Co1 O5 92.78(8) 1_655 . ? O2 Co1 O1W 87.12(8) 1_655 . ? O5 Co1 O1W 101.51(9) . . ? O2 Co1 O4 94.76(8) 1_655 3_756 ? O5 Co1 O4 165.69(8) . 3_756 ? O1W Co1 O4 91.01(8) . 3_756 ? O2 Co1 O1 175.19(8) 1_655 . ? O5 Co1 O1 85.24(8) . . ? O1W Co1 O1 88.97(8) . . ? O4 Co1 O1 88.11(8) 3_756 . ? O2 Co1 O1 95.03(8) 1_655 3_756 ? O5 Co1 O1 84.85(8) . 3_756 ? O1W Co1 O1 173.20(8) . 3_756 ? O4 Co1 O1 82.39(7) 3_756 3_756 ? O1 Co1 O1 89.17(7) . 3_756 ? O5 P2 O6 112.11(12) . . ? O5 P2 O4 114.16(11) . . ? O6 P2 O4 109.76(11) . . ? O5 P2 C1 106.01(13) . . ? O6 P2 C1 108.59(12) . . ? O4 P2 C1 105.81(13) . . ? O2 P1 O1 116.78(12) . . ? O2 P1 O3 111.89(12) . . ? O1 P1 O3 105.63(11) . . ? O2 P1 C1 105.89(13) . . ? O1 P1 C1 108.93(12) . . ? O3 P1 C1 107.38(12) . . ? C5 N1 C4 122.7(3) . . ? C5 N1 H1C 118.6 . . ? C4 N1 H1C 118.6 . . ? O7 C1 C2 109.7(2) . . ? O7 C1 P2 108.16(19) . . ? C2 C1 P2 111.7(2) . . ? O7 C1 P1 110.7(2) . . ? C2 C1 P1 109.5(2) . . ? P2 C1 P1 107.05(14) . . ? C3 C2 C1 113.8(2) . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C7 117.1(3) . . ? C4 C3 C2 122.3(3) . . ? C7 C3 C2 120.7(3) . . ? N1 C4 C3 120.3(3) . . ? N1 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C6 119.7(3) . . ? N1 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 118.6(3) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C6 C7 C3 121.6(3) . . ? C6 C7 H7 119.2 . . ? C3 C7 H7 119.2 . . ? P1 O1 Co1 126.57(12) . . ? P1 O1 Co1 126.62(12) . 3_756 ? Co1 O1 Co1 90.83(7) . 3_756 ? P1 O2 Co1 174.83(14) . 1_455 ? P1 O3 H3D 109.5 . . ? P2 O4 Co1 123.67(11) . 3_756 ? P2 O5 Co1 123.08(12) . . ? C1 O7 H7D 109.5 . . ? Co1 O1W H1WA 112.5 . . ? Co1 O1W H1WB 125.5 . . ? H1WA O1W H1WB 117.1 . . ? 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 O5 P2 C1 O7 174.88(17) . . . . ? O6 P2 C1 O7 54.2(2) . . . . ? O4 P2 C1 O7 -63.5(2) . . . . ? O5 P2 C1 C2 54.1(2) . . . . ? O6 P2 C1 C2 -66.5(2) . . . . ? O4 P2 C1 C2 175.70(19) . . . . ? O5 P2 C1 P1 -65.75(16) . . . . ? O6 P2 C1 P1 173.61(13) . . . . ? O4 P2 C1 P1 55.84(16) . . . . ? O2 P1 C1 O7 -2.3(2) . . . . ? O1 P1 C1 O7 124.06(19) . . . . ? O3 P1 C1 O7 -121.99(19) . . . . ? O2 P1 C1 C2 118.8(2) . . . . ? O1 P1 C1 C2 -114.9(2) . . . . ? O3 P1 C1 C2 -0.9(2) . . . . ? O2 P1 C1 P2 -119.99(15) . . . . ? O1 P1 C1 P2 6.37(18) . . . . ? O3 P1 C1 P2 120.31(14) . . . . ? O7 C1 C2 C3 -42.5(3) . . . . ? P2 C1 C2 C3 77.4(3) . . . . ? P1 C1 C2 C3 -164.2(2) . . . . ? C1 C2 C3 C4 -96.0(3) . . . . ? C1 C2 C3 C7 84.7(4) . . . . ? C5 N1 C4 C3 0.9(5) . . . . ? C7 C3 C4 N1 -0.9(4) . . . . ? C2 C3 C4 N1 179.7(3) . . . . ? C4 N1 C5 C6 0.1(5) . . . . ? N1 C5 C6 C7 -1.0(5) . . . . ? C5 C6 C7 C3 1.0(5) . . . . ? C4 C3 C7 C6 0.0(5) . . . . ? C2 C3 C7 C6 179.3(3) . . . . ? O2 P1 O1 Co1 177.71(12) . . . . ? O3 P1 O1 Co1 -57.19(15) . . . . ? C1 P1 O1 Co1 57.89(16) . . . . ? O2 P1 O1 Co1 52.68(18) . . . 3_756 ? O3 P1 O1 Co1 177.78(12) . . . 3_756 ? C1 P1 O1 Co1 -67.14(17) . . . 3_756 ? O5 Co1 O1 P1 -54.00(14) . . . . ? O1W Co1 O1 P1 47.64(14) . . . . ? O4 Co1 O1 P1 138.68(14) 3_756 . . . ? O1 Co1 O1 P1 -138.91(17) 3_756 . . . ? O5 Co1 O1 Co1 84.90(8) . . . 3_756 ? O1W Co1 O1 Co1 -173.46(8) . . . 3_756 ? O4 Co1 O1 Co1 -82.41(7) 3_756 . . 3_756 ? O1 Co1 O1 Co1 0.0 3_756 . . 3_756 ? O5 P2 O4 Co1 37.10(18) . . . 3_756 ? O6 P2 O4 Co1 163.94(12) . . . 3_756 ? C1 P2 O4 Co1 -79.08(16) . . . 3_756 ? O6 P2 O5 Co1 -169.05(12) . . . . ? O4 P2 O5 Co1 -43.45(17) . . . . ? C1 P2 O5 Co1 72.62(16) . . . . ? O2 Co1 O5 P2 165.32(14) 1_655 . . . ? O1W Co1 O5 P2 -107.06(14) . . . . ? O4 Co1 O5 P2 43.5(4) 3_756 . . . ? O1 Co1 O5 P2 -19.08(14) . . . . ? O1 Co1 O5 P2 70.51(14) 3_756 . . . ? 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 O7 H7D O2 0.82 2.21 2.778(3) 126.3 . O1W H1WA O3 0.90 1.85 2.687(3) 154.7 . N1 H1C O4 0.86 1.79 2.645(3) 172.7 4_666 O3 H3D O6 0.82 1.68 2.485(3) 166.2 2_646 O7 H7D O5 0.82 2.21 2.939(3) 148.2 1_455 O1W H1WB O6 0.90 1.81 2.713(3) 176.1 2_746 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.453 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.083