# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email hperry@mail.chem.tamu.edu _publ_contact_author_name 'Abraham Clearfield' loop_ _publ_author_name 'Houston Perry' 'Justin Law' 'Abraham Clearfield' data_test _database_code_depnum_ccdc_archive 'CCDC 849780' #TrackingRef '- Co2(L)(H2O)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 Co2 N2 O8 P2' _chemical_formula_weight 506.15 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)/c 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 15.1081(12) _cell_length_b 11.5458(7) _cell_length_c 10.5958(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.394(4) _cell_angle_gamma 90.00 _cell_volume 1732.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9162 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 29.34 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 2.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8471 _exptl_absorpt_correction_T_max 0.9191 _exptl_absorpt_process_details 'SADABS 2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEXII CCD Area Diffractometer' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56285 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5045 _reflns_number_gt 4663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically, and were constrained and refined using a riding model, except for the hydrogen atoms on the water molecules which were found in the difference map and allowed to refine. ; _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^)+(0.0543P)^2^+0.0209P] 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 5045 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 0.09481(3) 0.69038(3) 0.80212(4) 0.00955(9) Uani 1 1 d . . . Co2 Co -0.09751(3) 0.64578(3) 0.85075(4) 0.00985(9) Uani 1 1 d . . . P1 P -0.12745(5) 0.37350(6) 0.90890(8) 0.00821(14) Uani 1 1 d . . . P2 P -0.11808(5) 0.79103(7) 1.05249(8) 0.01296(15) Uani 1 1 d . . . O2W O 0.07535(15) 0.85885(19) 0.8773(2) 0.0146(4) Uani 1 1 d . . . H2WA H 0.071(3) 0.910(4) 0.825(4) 0.022 Uiso 1 1 d . . . H2WB H 0.029(3) 0.864(3) 0.924(4) 0.022 Uiso 1 1 d . . . N1 N 0.24245(17) 0.6837(2) 0.9465(3) 0.0101(5) Uani 1 1 d . . . O4 O -0.05109(14) 0.68599(19) 0.6959(2) 0.0134(4) Uani 1 1 d . . . C1 C 0.3068(2) 0.6358(3) 0.8807(3) 0.0128(6) Uani 1 1 d . . . H1A H 0.2993 0.6815 0.7985 0.015 Uiso 1 1 calc R . . H1B H 0.2876 0.5552 0.8524 0.015 Uiso 1 1 calc R . . O1 O 0.05003(14) 0.62601(17) 0.9519(2) 0.0102(4) Uani 1 1 d . . . O1W O 0.11037(16) 0.51024(19) 0.7596(3) 0.0166(4) Uani 1 1 d . . . H1WA H 0.095(3) 0.468(4) 0.807(5) 0.025 Uiso 1 1 d . . . H1WB H 0.111(3) 0.473(4) 0.695(5) 0.025 Uiso 1 1 d . . . C4 C 0.37912(19) 0.8109(2) 1.0827(3) 0.0132(5) Uani 1 1 d . . . H4A H 0.3892 0.7699 1.1687 0.016 Uiso 1 1 calc R . . H4B H 0.3958 0.8933 1.1039 0.016 Uiso 1 1 calc R . . C2 C 0.4113(2) 0.6362(2) 0.9701(3) 0.0134(6) Uani 1 1 d . . . H2A H 0.4204 0.5870 1.0501 0.016 Uiso 1 1 calc R . . H2B H 0.4495 0.6033 0.9195 0.016 Uiso 1 1 calc R . . O5 O -0.13415(17) 0.6610(2) 1.0221(3) 0.0222(5) Uani 1 1 d . . . O6 O -0.09137(18) 0.8429(2) 0.9398(3) 0.0249(5) Uani 1 1 d . . . C5 C 0.2745(2) 0.8026(2) 0.9947(3) 0.0128(6) Uani 1 1 d . . . H5A H 0.2360 0.8317 1.0469 0.015 Uiso 1 1 calc R . . H5B H 0.2627 0.8539 0.9156 0.015 Uiso 1 1 calc R . . C3 C 0.44509(19) 0.7590(3) 1.0153(3) 0.0125(5) Uani 1 1 d . . . H3 H 0.4377 0.8057 0.9328 0.015 Uiso 1 1 calc R . . O2 O -0.11975(13) 0.47429(16) 0.8206(2) 0.0107(4) Uani 1 1 d . . . O3 O -0.13656(14) 0.25811(17) 0.8387(2) 0.0122(4) Uani 1 1 d . . . C12 C -0.2258(2) 0.8589(3) 1.0580(3) 0.0147(6) Uani 1 1 d . . . H12A H -0.2196 0.9442 1.0560 0.018 Uiso 1 1 calc R . . H12B H -0.2800 0.8354 0.9779 0.018 Uiso 1 1 calc R . . C10 C 0.61745(19) 0.6891(3) 1.0723(4) 0.0152(6) Uani 1 1 d . . . H10A H 0.6153 0.7073 0.9800 0.018 Uiso 1 1 calc R . . H10B H 0.5977 0.6074 1.0734 0.018 Uiso 1 1 calc R . . C8 C 0.5858(2) 0.8917(3) 1.1173(3) 0.0155(6) Uani 1 1 d . . . H8A H 0.5813 0.9181 1.0264 0.019 Uiso 1 1 calc R . . H8B H 0.5457 0.9431 1.1494 0.019 Uiso 1 1 calc R . . C9 C 0.54886(19) 0.7678(2) 1.1084(3) 0.0123(5) Uani 1 1 d . . . H9 H 0.5514 0.7454 1.2007 0.015 Uiso 1 1 calc R . . C7 C 0.6878(2) 0.9019(3) 1.2120(3) 0.0150(6) Uani 1 1 d . . . H7A H 0.7087 0.9829 1.2097 0.018 Uiso 1 1 calc R . . H7B H 0.6899 0.8861 1.3048 0.018 Uiso 1 1 calc R . . N2 N -0.24364(17) 0.8242(2) 1.1827(3) 0.0120(5) Uani 1 1 d . . . C11 C 0.7188(2) 0.7036(2) 1.1708(3) 0.0129(6) Uani 1 1 d . . . H11A H 0.7214 0.6774 1.2610 0.016 Uiso 1 1 calc R . . H11B H 0.7607 0.6524 1.1419 0.016 Uiso 1 1 calc R . . C6 C 0.23654(19) 0.6062(2) 1.0550(3) 0.0105(5) Uani 1 1 d . . . H6A H 0.2913 0.6210 1.1380 0.013 Uiso 1 1 calc R . . H6B H 0.2402 0.5247 1.0283 0.013 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 Co1 0.00753(15) 0.01044(17) 0.00987(19) 0.00158(13) 0.00202(17) -0.00021(14) Co2 0.00833(15) 0.00982(16) 0.0113(2) 0.00063(13) 0.00333(17) -0.00050(13) P1 0.0073(3) 0.0075(3) 0.0094(3) 0.0002(2) 0.0025(3) -0.0001(2) P2 0.0088(3) 0.0181(3) 0.0117(4) -0.0023(3) 0.0033(3) 0.0008(2) O2W 0.0148(10) 0.0126(10) 0.0184(12) 0.0033(8) 0.0082(9) 0.0013(8) N1 0.0092(10) 0.0070(10) 0.0128(12) 0.0012(9) 0.0023(10) 0.0000(8) O4 0.0086(9) 0.0182(10) 0.0115(11) 0.0018(8) 0.0012(8) -0.0005(8) C1 0.0102(12) 0.0153(13) 0.0126(15) -0.0025(10) 0.0036(11) -0.0009(10) O1 0.0089(9) 0.0112(9) 0.0098(10) -0.0002(7) 0.0024(8) -0.0007(7) O1W 0.0190(11) 0.0139(10) 0.0169(11) -0.0020(8) 0.0062(10) -0.0005(8) C4 0.0100(11) 0.0129(13) 0.0159(15) -0.0013(11) 0.0037(12) -0.0006(9) C2 0.0096(12) 0.0127(13) 0.0178(16) -0.0012(11) 0.0045(12) 0.0004(9) O5 0.0190(10) 0.0230(11) 0.0278(14) -0.0129(10) 0.0120(11) -0.0051(9) O6 0.0174(11) 0.0396(14) 0.0182(13) 0.0117(10) 0.0067(11) 0.0081(10) C5 0.0088(11) 0.0113(12) 0.0175(15) 0.0003(11) 0.0036(11) -0.0003(10) C3 0.0082(11) 0.0115(12) 0.0165(14) -0.0010(11) 0.0027(11) -0.0004(10) O2 0.0113(9) 0.0093(8) 0.0105(10) 0.0007(7) 0.0025(8) 0.0006(7) O3 0.0129(8) 0.0095(9) 0.0157(11) -0.0013(8) 0.0069(9) -0.0011(7) C12 0.0125(13) 0.0188(15) 0.0127(15) 0.0012(11) 0.0043(12) 0.0003(11) C10 0.0103(12) 0.0129(13) 0.0210(17) -0.0027(11) 0.0039(12) -0.0003(10) C8 0.0105(12) 0.0140(13) 0.0218(17) -0.0019(12) 0.0056(12) 0.0017(10) C9 0.0102(12) 0.0109(13) 0.0155(14) 0.0008(11) 0.0039(11) -0.0014(10) C7 0.0108(12) 0.0146(13) 0.0184(15) -0.0046(11) 0.0037(11) -0.0017(10) N2 0.0097(10) 0.0107(11) 0.0149(13) -0.0003(9) 0.0032(10) -0.0004(9) C11 0.0094(12) 0.0120(13) 0.0154(15) 0.0005(11) 0.0018(11) 0.0015(10) C6 0.0092(11) 0.0106(12) 0.0119(14) 0.0012(10) 0.0039(11) -0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.973(2) 2_556 ? Co1 O1 2.068(2) . ? Co1 O4 2.098(2) . ? Co1 O1W 2.158(2) . ? Co1 O2W 2.160(2) . ? Co1 N1 2.223(2) . ? Co2 O2 2.0150(19) . ? Co2 O4 2.050(2) . ? Co2 O5 2.082(3) . ? Co2 O1 2.122(2) . ? Co2 N2 2.329(3) 4_575 ? P1 O3 1.508(2) . ? P1 O2 1.522(2) . ? P1 O1 1.530(2) 3_567 ? P1 C6 1.832(3) 3_567 ? P2 O6 1.511(3) . ? P2 O4 1.527(2) 4_576 ? P2 O5 1.537(2) . ? P2 C12 1.826(3) . ? O2W H2WA 0.80(4) . ? O2W H2WB 1.00(4) . ? N1 C6 1.485(4) . ? N1 C5 1.486(4) . ? N1 C1 1.487(4) . ? C1 C2 1.532(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O1W H1WA 0.79(5) . ? O1W H1WB 0.81(5) . ? C4 C5 1.534(4) . ? C4 C3 1.536(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C2 C3 1.526(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C3 C9 1.537(4) . ? C3 H3 1.0000 . ? C12 N2 1.492(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C10 C9 1.524(4) . ? C10 C11 1.532(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C8 C7 1.522(4) . ? C8 C9 1.527(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9 1.0000 . ? C7 N2 1.482(4) 1_655 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N2 C7 1.482(4) 1_455 ? N2 C11 1.492(4) 1_455 ? N2 Co2 2.329(3) 4_576 ? C11 N2 1.492(4) 1_655 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O1 177.71(8) 2_556 . ? O3 Co1 O4 99.02(8) 2_556 . ? O1 Co1 O4 80.77(8) . . ? O3 Co1 O1W 97.90(9) 2_556 . ? O1 Co1 O1W 84.39(9) . . ? O4 Co1 O1W 92.02(9) . . ? O3 Co1 O2W 92.43(9) 2_556 . ? O1 Co1 O2W 85.28(8) . . ? O4 Co1 O2W 88.11(9) . . ? O1W Co1 O2W 169.52(9) . . ? O3 Co1 N1 91.46(9) 2_556 . ? O1 Co1 N1 88.72(9) . . ? O4 Co1 N1 169.48(9) . . ? O1W Co1 N1 87.38(9) . . ? O2W Co1 N1 90.59(9) . . ? O2 Co2 O4 100.40(9) . . ? O2 Co2 O5 98.09(9) . . ? O4 Co2 O5 161.46(9) . . ? O2 Co2 O1 93.56(8) . . ? O4 Co2 O1 80.60(8) . . ? O5 Co2 O1 96.91(9) . . ? O2 Co2 N2 87.94(9) . 4_575 ? O4 Co2 N2 81.47(9) . 4_575 ? O5 Co2 N2 100.66(10) . 4_575 ? O1 Co2 N2 161.98(9) . 4_575 ? O2 Co2 P2 130.43(7) . . ? O4 Co2 P2 129.15(6) . . ? O5 Co2 P2 32.34(7) . . ? O1 Co2 P2 93.14(6) . . ? N2 Co2 P2 99.54(7) 4_575 . ? O3 P1 O2 112.69(12) . . ? O3 P1 O1 112.72(12) . 3_567 ? O2 P1 O1 113.13(11) . 3_567 ? O3 P1 C6 106.37(12) . 3_567 ? O2 P1 C6 107.27(12) . 3_567 ? O1 P1 C6 103.87(12) 3_567 3_567 ? O6 P2 O4 116.78(14) . 4_576 ? O6 P2 O5 106.70(16) . . ? O4 P2 O5 112.33(14) 4_576 . ? O6 P2 C12 109.99(14) . . ? O4 P2 C12 100.52(14) 4_576 . ? O5 P2 C12 110.41(14) . . ? O6 P2 Co2 60.39(11) . . ? O4 P2 Co2 130.40(9) 4_576 . ? O5 P2 Co2 46.43(10) . . ? C12 P2 Co2 127.96(11) . . ? Co1 O2W H2WA 114(3) . . ? Co1 O2W H2WB 117(2) . . ? H2WA O2W H2WB 113(4) . . ? C6 N1 C5 113.0(2) . . ? C6 N1 C1 111.4(2) . . ? C5 N1 C1 108.5(2) . . ? C6 N1 Co1 103.71(17) . . ? C5 N1 Co1 109.45(17) . . ? C1 N1 Co1 110.70(18) . . ? P2 O4 Co2 122.88(12) 4_575 . ? P2 O4 Co1 137.58(13) 4_575 . ? Co2 O4 Co1 99.47(9) . . ? N1 C1 C2 114.2(2) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? P1 O1 Co1 113.18(11) 3_567 . ? P1 O1 Co2 143.33(13) 3_567 . ? Co1 O1 Co2 98.08(9) . . ? Co1 O1W H1WA 112(3) . . ? Co1 O1W H1WB 136(3) . . ? H1WA O1W H1WB 108(4) . . ? C5 C4 C3 113.0(3) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C3 C2 C1 110.9(2) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? P2 O5 Co2 101.24(14) . . ? N1 C5 C4 114.2(2) . . ? N1 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? N1 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C2 C3 C4 108.0(2) . . ? C2 C3 C9 114.7(2) . . ? C4 C3 C9 111.0(3) . . ? C2 C3 H3 107.6 . . ? C4 C3 H3 107.6 . . ? C9 C3 H3 107.6 . . ? P1 O2 Co2 134.27(13) . . ? P1 O3 Co1 136.43(13) . 2_546 ? N2 C12 P2 110.6(2) . . ? N2 C12 H12A 109.5 . . ? P2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? P2 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C9 C10 C11 111.6(3) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C7 C8 C9 112.2(3) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 108.0(2) . . ? C10 C9 C3 115.5(3) . . ? C8 C9 C3 111.8(2) . . ? C10 C9 H9 107.1 . . ? C8 C9 H9 107.1 . . ? C3 C9 H9 107.1 . . ? N2 C7 C8 115.8(3) 1_655 . ? N2 C7 H7A 108.3 1_655 . ? C8 C7 H7A 108.3 . . ? N2 C7 H7B 108.3 1_655 . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 N2 C11 108.0(2) 1_455 1_455 ? C7 N2 C12 112.2(2) 1_455 . ? C11 N2 C12 110.9(2) 1_455 . ? C7 N2 Co2 107.12(18) 1_455 4_576 ? C11 N2 Co2 115.78(18) 1_455 4_576 ? C12 N2 Co2 102.78(17) . 4_576 ? N2 C11 C10 114.9(2) 1_655 . ? N2 C11 H11A 108.6 1_655 . ? C10 C11 H11A 108.6 . . ? N2 C11 H11B 108.6 1_655 . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? N1 C6 P1 112.67(19) . 3_567 ? N1 C6 H6A 109.1 . . ? P1 C6 H6A 109.1 3_567 . ? N1 C6 H6B 109.1 . . ? P1 C6 H6B 109.1 3_567 . ? H6A C6 H6B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.653 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.268 # Attachment '- Co2Cl2(H2L).cif' data_j1 _database_code_depnum_ccdc_archive 'CCDC 849781' #TrackingRef '- Co2Cl2(H2L).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 Cl Co N O3 P' _chemical_formula_weight 271.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 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 10.170(4) _cell_length_b 9.611(4) _cell_length_c 10.184(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.362(4) _cell_angle_gamma 90.00 _cell_volume 995.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5240 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 28.09 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.126 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; An abosrption correction was not applied because the refinement and completeness were better without it. ; _diffrn_ambient_temperature 110(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 APEXII CCD Area Diffractometer' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10732 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.97 _reflns_number_total 2152 _reflns_number_gt 1888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically, and were constrained and refined using a riding model. ; _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^)+(0.0353P)^2^+0.1701P] 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 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.88951(2) 0.10803(3) 0.36392(2) 0.01322(10) Uani 1 1 d . . . P2 P 1.01537(5) 0.29366(5) 0.13557(5) 0.01258(13) Uani 1 1 d . . . O1 O 0.90885(13) 0.20606(14) 0.19613(13) 0.0158(3) Uani 1 1 d . . . O2 O 1.00767(14) 0.20312(15) 0.48677(13) 0.0167(3) Uani 1 1 d . . . O3 O 0.97859(13) -0.06154(14) 0.30255(14) 0.0164(3) Uani 1 1 d . . . C6 C 1.17256(19) 0.2152(2) 0.1805(2) 0.0165(4) Uani 1 1 d . . . H6A H 1.2428 0.2611 0.1293 0.020 Uiso 1 1 calc R . . H6B H 1.1900 0.2342 0.2745 0.020 Uiso 1 1 calc R . . Cl1 Cl 0.68174(5) 0.07465(7) 0.42267(6) 0.03113(16) Uani 1 1 d . . . C4 C 1.42516(19) 0.0276(2) 0.1746(2) 0.0202(5) Uani 1 1 d . . . H4A H 1.4950 -0.0201 0.2256 0.024 Uiso 1 1 calc R . . H4B H 1.4408 0.1290 0.1808 0.024 Uiso 1 1 calc R . . C3 C 1.43327(19) -0.0173(2) 0.0305(2) 0.0177(4) Uani 1 1 d . . . H3 H 1.4210 -0.1205 0.0265 0.021 Uiso 1 1 calc R . . N1 N 1.18097(16) 0.06117(18) 0.15819(17) 0.0157(4) Uani 1 1 d . . . H1 H 1.1037 0.0234 0.1911 0.019 Uiso 1 1 calc R . . C2 C 1.31922(18) 0.0510(2) -0.0449(2) 0.0184(4) Uani 1 1 d . . . H2A H 1.3325 0.1530 -0.0463 0.022 Uiso 1 1 calc R . . H2B H 1.3194 0.0175 -0.1369 0.022 Uiso 1 1 calc R . . C5 C 1.29248(19) -0.0063(2) 0.2337(2) 0.0196(4) Uani 1 1 d . . . H5A H 1.2799 -0.1085 0.2339 0.024 Uiso 1 1 calc R . . H5B H 1.2908 0.0261 0.3259 0.024 Uiso 1 1 calc R . . C1 C 1.18714(19) 0.0190(2) 0.0160(2) 0.0173(4) Uani 1 1 d . . . H1A H 1.1174 0.0686 -0.0336 0.021 Uiso 1 1 calc R . . H1B H 1.1697 -0.0820 0.0087 0.021 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 Co1 0.01778(17) 0.01230(16) 0.00956(16) -0.00011(10) 0.00006(10) -0.00030(10) P2 0.0174(3) 0.0106(3) 0.0097(3) 0.00009(18) -0.00029(19) 0.00169(18) O1 0.0198(7) 0.0141(7) 0.0135(7) 0.0027(6) -0.0020(6) -0.0016(5) O2 0.0208(7) 0.0193(8) 0.0100(7) -0.0018(6) 0.0005(5) -0.0051(6) O3 0.0233(7) 0.0098(7) 0.0160(8) 0.0017(6) 0.0043(6) 0.0009(6) C6 0.0179(10) 0.0159(10) 0.0157(10) -0.0023(8) -0.0020(8) 0.0009(8) Cl1 0.0190(3) 0.0553(4) 0.0191(3) 0.0010(3) 0.0010(2) -0.0046(2) C4 0.0155(10) 0.0298(12) 0.0153(11) 0.0017(9) -0.0013(8) 0.0025(8) C3 0.0156(10) 0.0219(11) 0.0156(10) 0.0002(8) -0.0002(8) 0.0011(8) N1 0.0148(8) 0.0166(9) 0.0155(9) 0.0003(7) 0.0005(6) 0.0008(7) C2 0.0162(10) 0.0249(12) 0.0141(10) -0.0009(8) -0.0007(8) 0.0004(8) C5 0.0202(10) 0.0228(11) 0.0159(10) 0.0062(9) 0.0007(8) 0.0046(8) C1 0.0166(10) 0.0198(11) 0.0156(10) -0.0045(8) -0.0014(8) 0.0013(8) _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 1.9560(15) . ? Co1 O1 1.9624(15) . ? Co1 O3 1.9684(15) . ? Co1 Cl1 2.2230(9) . ? P2 O1 1.5071(15) . ? P2 O2 1.5173(15) 4_565 ? P2 O3 1.5289(15) 2_755 ? P2 C6 1.823(2) . ? C6 N1 1.501(3) . ? C4 C5 1.516(3) . ? C4 C3 1.532(3) . ? C3 C3 1.533(4) 3_855 ? C3 C2 1.535(3) . ? N1 C1 1.506(3) . ? N1 C5 1.512(3) . ? C2 C1 1.515(3) . ? 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 O1 105.55(6) . . ? O2 Co1 O3 107.93(6) . . ? O1 Co1 O3 94.14(6) . . ? O2 Co1 Cl1 118.46(5) . . ? O1 Co1 Cl1 113.85(4) . . ? O3 Co1 Cl1 113.96(5) . . ? O1 P2 O2 112.80(8) . 4_565 ? O1 P2 O3 111.53(8) . 2_755 ? O2 P2 O3 113.25(8) 4_565 2_755 ? O1 P2 C6 107.33(9) . . ? O2 P2 C6 107.37(9) 4_565 . ? O3 P2 C6 103.90(9) 2_755 . ? P2 O1 Co1 134.50(9) . . ? P2 O2 Co1 132.53(9) 4_566 . ? P2 O3 Co1 129.80(9) 2_745 . ? N1 C6 P2 114.89(13) . . ? C5 C4 C3 111.89(17) . . ? C4 C3 C3 112.3(2) . 3_855 ? C4 C3 C2 108.28(17) . . ? C3 C3 C2 111.9(2) 3_855 . ? C6 N1 C1 114.45(16) . . ? C6 N1 C5 112.94(16) . . ? C1 N1 C5 109.74(16) . . ? C1 C2 C3 112.18(17) . . ? N1 C5 C4 111.87(17) . . ? N1 C1 C2 112.45(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.485 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.080 # Attachment '- Mn2(L)(H2O)3.cif' data_jl2_108 _database_code_depnum_ccdc_archive 'CCDC 849782' #TrackingRef '- Mn2(L)(H2O)3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Mn2 N2 O9 P2' _chemical_formula_weight 516.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4350(16) _cell_length_b 11.641(3) _cell_length_c 12.750(3) _cell_angle_alpha 88.490(10) _cell_angle_beta 79.781(10) _cell_angle_gamma 79.276(9) _cell_volume 923.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1921 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.41 _exptl_crystal_description lath _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7963 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details 'SADABS 2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEXII CCD Area Diffractometer' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11397 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3595 _reflns_number_gt 2489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically, and were constrained and refined using a riding model, except for those on the water molecules which were placed according to peaks in the difference map and the O-H distances allowed to refine. ; _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^)+(0.0804P)^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 3595 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Mn1 Mn 0.12577(13) 0.09446(7) 0.42954(7) 0.0136(2) Uani 1 1 d . . . Mn2 Mn 0.34302(13) 0.23070(7) 0.59157(7) 0.0140(2) Uani 1 1 d . . . P2 P 0.6489(2) 0.05592(12) 0.37802(11) 0.0123(3) Uani 1 1 d . . . P1 P -0.1720(2) 0.31521(12) 0.57851(12) 0.0138(3) Uani 1 1 d . . . O4 O 0.4387(5) 0.1219(3) 0.4404(3) 0.0133(8) Uani 1 1 d . . . O1 O 0.0249(6) 0.2161(3) 0.5580(3) 0.0154(8) Uani 1 1 d . . . O5 O 0.1750(6) -0.0434(3) 0.5540(3) 0.0151(8) Uani 1 1 d . . . O2 O 0.6307(5) 0.2690(3) 0.6324(3) 0.0157(9) Uani 1 1 d . . . O3 O -0.2059(6) 0.3851(3) 0.4792(3) 0.0152(9) Uani 1 1 d . . . O6 O 0.3737(6) 0.0608(3) 0.6650(3) 0.0134(8) Uani 1 1 d . . . N1 N 0.0777(7) 0.3504(4) 0.7289(4) 0.0169(11) Uani 1 1 d . . . N2 N 0.5560(7) 0.1945(4) 0.2046(4) 0.0163(11) Uani 1 1 d . . . C1 C -0.0209(9) 0.2778(5) 0.8142(4) 0.0167(13) Uani 1 1 d . . . H1A H -0.0780 0.2168 0.7815 0.020 Uiso 1 1 calc R . . H1B H -0.1427 0.3276 0.8602 0.020 Uiso 1 1 calc R . . C8 C 0.4041(9) 0.2544(5) 1.0005(5) 0.0186(13) Uani 1 1 d . . . H8 H 0.5397 0.2277 0.9486 0.022 Uiso 1 1 calc R . . C11 C -0.0909(8) 0.4112(5) 0.6685(4) 0.0157(12) Uani 1 1 d . . . H11A H -0.0355 0.4753 0.6265 0.019 Uiso 1 1 calc R . . H11B H -0.2191 0.4468 0.7201 0.019 Uiso 1 1 calc R . . C4 C 0.3212(9) 0.3897(5) 0.8489(5) 0.0194(13) Uani 1 1 d . . . H4A H 0.3671 0.4539 0.8830 0.023 Uiso 1 1 calc R . . H4B H 0.4496 0.3445 0.8033 0.023 Uiso 1 1 calc R . . C7 C 0.3551(9) 0.1492(5) 1.0673(4) 0.0196(13) Uani 1 1 d . . . H7A H 0.3392 0.0864 1.0202 0.024 Uiso 1 1 calc R . . H7B H 0.2179 0.1718 1.1175 0.024 Uiso 1 1 calc R . . C2 C 0.1389(9) 0.2204(5) 0.8813(5) 0.0182(13) Uani 1 1 d . . . H2A H 0.2577 0.1684 0.8356 0.022 Uiso 1 1 calc R . . H2B H 0.0679 0.1716 0.9360 0.022 Uiso 1 1 calc R . . C12 C 0.7243(8) 0.1500(5) 0.2685(4) 0.0163(12) Uani 1 1 d . . . H12A H 0.7694 0.2177 0.2974 0.020 Uiso 1 1 calc R . . H12B H 0.8507 0.1065 0.2204 0.020 Uiso 1 1 calc R . . C3 C 0.2309(9) 0.3088(5) 0.9362(4) 0.0181(13) Uani 1 1 d . . . H3 H 0.1105 0.3572 0.9859 0.022 Uiso 1 1 calc R . . C6 C 0.5355(9) 0.1041(5) 0.1298(5) 0.0200(13) Uani 1 1 d . . . H6A H 0.5047 0.0335 0.1700 0.024 Uiso 1 1 calc R . . H6B H 0.6728 0.0820 0.0795 0.024 Uiso 1 1 calc R . . C9 C 0.4486(10) 0.3449(5) 1.0742(5) 0.0254(15) Uani 1 1 d . . . H9A H 0.4981 0.4095 1.0305 0.031 Uiso 1 1 calc R . . H9B H 0.3128 0.3782 1.1219 0.031 Uiso 1 1 calc R . . C5 C 0.1589(9) 0.4416(5) 0.7796(5) 0.0179(13) Uani 1 1 d . . . H5A H 0.0367 0.4930 0.8238 0.021 Uiso 1 1 calc R . . H5B H 0.2268 0.4901 0.7236 0.021 Uiso 1 1 calc R . . C10 C 0.6154(10) 0.2955(5) 0.1416(5) 0.0231(14) Uani 1 1 d . . . H10A H 0.7561 0.2709 0.0947 0.028 Uiso 1 1 calc R . . H10B H 0.6301 0.3572 0.1904 0.028 Uiso 1 1 calc R . . O3W O 0.1225(7) 0.2465(4) 0.3190(3) 0.0193(9) Uani 1 1 d . . . H3WA H 0.246(10) 0.243(5) 0.292(5) 0.029 Uiso 1 1 d . . . H3WB H 0.103(10) 0.302(6) 0.363(5) 0.029 Uiso 1 1 d . . . O1W O 0.3598(6) 0.3823(4) 0.4808(3) 0.0209(10) Uani 1 1 d D . . H1WA H 0.486(4) 0.391(6) 0.475(5) 0.031 Uiso 1 1 d D . . H1WB H 0.309(10) 0.448(5) 0.509(5) 0.031 Uiso 1 1 d . . . O2W O 0.2134(7) -0.0360(4) 0.3010(4) 0.0231(10) Uani 1 1 d . . . H2WA H 0.152(10) -0.096(6) 0.333(5) 0.035 Uiso 1 1 d . . . H2WB H 0.321(11) -0.066(6) 0.305(6) 0.035 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0125(4) 0.0133(5) 0.0178(5) 0.0013(4) -0.0058(3) -0.0067(4) Mn2 0.0135(5) 0.0115(5) 0.0194(5) 0.0011(4) -0.0065(4) -0.0054(4) P2 0.0126(7) 0.0121(8) 0.0147(8) 0.0022(6) -0.0061(6) -0.0056(6) P1 0.0132(7) 0.0116(8) 0.0189(8) 0.0007(6) -0.0055(6) -0.0052(6) O4 0.0106(19) 0.009(2) 0.021(2) 0.0005(16) -0.0069(16) -0.0016(15) O1 0.0122(19) 0.012(2) 0.023(2) -0.0011(16) -0.0068(16) -0.0017(16) O5 0.015(2) 0.018(2) 0.016(2) 0.0029(16) -0.0067(16) -0.0084(16) O2 0.0111(19) 0.016(2) 0.021(2) 0.0000(17) -0.0031(16) -0.0046(16) O3 0.017(2) 0.012(2) 0.019(2) 0.0038(16) -0.0052(16) -0.0077(16) O6 0.0141(19) 0.012(2) 0.016(2) -0.0012(16) -0.0057(16) -0.0046(16) N1 0.017(2) 0.018(3) 0.019(3) 0.004(2) -0.007(2) -0.008(2) N2 0.021(3) 0.015(3) 0.017(3) 0.004(2) -0.010(2) -0.009(2) C1 0.021(3) 0.018(3) 0.016(3) 0.004(2) -0.006(2) -0.012(2) C8 0.019(3) 0.016(3) 0.022(3) 0.002(3) -0.006(3) -0.004(2) C11 0.015(3) 0.008(3) 0.025(3) 0.003(2) -0.006(2) -0.005(2) C4 0.025(3) 0.018(3) 0.021(3) 0.004(3) -0.008(3) -0.014(3) C7 0.025(3) 0.020(3) 0.018(3) -0.004(3) -0.010(3) -0.006(3) C2 0.020(3) 0.017(3) 0.020(3) 0.004(2) -0.005(2) -0.007(2) C12 0.012(3) 0.021(3) 0.019(3) 0.001(2) -0.006(2) -0.007(2) C3 0.020(3) 0.017(3) 0.018(3) 0.000(3) -0.006(2) -0.003(3) C6 0.027(3) 0.014(3) 0.021(3) -0.002(3) -0.011(3) -0.005(3) C9 0.043(4) 0.013(3) 0.028(4) 0.007(3) -0.021(3) -0.011(3) C5 0.021(3) 0.016(3) 0.020(3) -0.004(2) -0.009(3) -0.007(2) C10 0.029(3) 0.017(3) 0.031(4) 0.010(3) -0.015(3) -0.015(3) O3W 0.020(2) 0.017(2) 0.022(2) 0.0006(18) -0.0043(19) -0.0070(19) O1W 0.017(2) 0.016(2) 0.032(3) 0.0005(19) -0.006(2) -0.0055(19) O2W 0.021(2) 0.017(2) 0.031(3) -0.0014(19) -0.007(2) -0.0013(19) _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 Mn1 O5 2.103(3) 2_556 ? Mn1 O1 2.124(4) . ? Mn1 O4 2.125(3) . ? Mn1 O2W 2.189(4) . ? Mn1 O3W 2.232(4) . ? Mn1 O5 2.247(4) . ? Mn2 O2 2.135(3) . ? Mn2 O6 2.156(4) . ? Mn2 O1 2.202(3) . ? Mn2 O1W 2.237(4) . ? Mn2 O4 2.262(4) . ? Mn2 N1 2.471(5) . ? P2 O6 1.519(4) 2_656 ? P2 O4 1.522(4) . ? P2 O5 1.529(4) 2_656 ? P2 C12 1.806(6) . ? P1 O3 1.513(4) . ? P1 O2 1.516(4) 1_455 ? P1 O1 1.536(4) . ? P1 C11 1.826(5) . ? N1 C5 1.476(7) . ? N1 C1 1.486(7) . ? N1 C11 1.501(7) . ? N2 C10 1.477(7) . ? N2 C12 1.479(6) . ? N2 C6 1.478(7) . ? C1 C2 1.504(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C8 C7 1.522(8) . ? C8 C9 1.529(8) . ? C8 C3 1.533(8) . ? C8 H8 1.0000 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C4 C5 1.518(7) . ? C4 C3 1.543(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C7 C6 1.529(7) 1_556 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C2 C3 1.520(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C3 H3 1.0000 . ? C6 C7 1.529(7) 1_554 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C9 C10 1.514(8) 1_556 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C10 C9 1.514(8) 1_554 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O3W H3WA 0.80(6) . ? O3W H3WB 0.84(6) . ? O1W H1WA 0.83(2) . ? O1W H1WB 0.84(6) . ? O2W H2WA 0.92(7) . ? O2W H2WB 0.72(7) . ? 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 O5 Mn1 O1 93.64(14) 2_556 . ? O5 Mn1 O4 167.91(14) 2_556 . ? O1 Mn1 O4 84.26(14) . . ? O5 Mn1 O2W 83.11(16) 2_556 . ? O1 Mn1 O2W 176.56(16) . . ? O4 Mn1 O2W 98.68(16) . . ? O5 Mn1 O3W 107.69(15) 2_556 . ? O1 Mn1 O3W 87.91(15) . . ? O4 Mn1 O3W 84.17(14) . . ? O2W Mn1 O3W 94.15(16) . . ? O5 Mn1 O5 82.11(14) 2_556 . ? O1 Mn1 O5 86.44(14) . . ? O4 Mn1 O5 85.87(13) . . ? O2W Mn1 O5 91.98(16) . . ? O3W Mn1 O5 168.99(14) . . ? O2 Mn2 O6 94.80(14) . . ? O2 Mn2 O1 171.91(14) . . ? O6 Mn2 O1 90.71(13) . . ? O2 Mn2 O1W 84.91(14) . . ? O6 Mn2 O1W 165.96(15) . . ? O1 Mn2 O1W 91.17(14) . . ? O2 Mn2 O4 107.23(13) . . ? O6 Mn2 O4 82.31(14) . . ? O1 Mn2 O4 79.35(13) . . ? O1W Mn2 O4 84.37(15) . . ? O2 Mn2 N1 99.07(14) . . ? O6 Mn2 N1 101.42(14) . . ? O1 Mn2 N1 73.98(14) . . ? O1W Mn2 N1 92.47(15) . . ? O4 Mn2 N1 153.08(14) . . ? O6 P2 O4 112.7(2) 2_656 . ? O6 P2 O5 112.4(2) 2_656 2_656 ? O4 P2 O5 109.9(2) . 2_656 ? O6 P2 C12 109.6(2) 2_656 . ? O4 P2 C12 105.5(2) . . ? O5 P2 C12 106.3(2) 2_656 . ? O3 P1 O2 113.4(2) . 1_455 ? O3 P1 O1 112.4(2) . . ? O2 P1 O1 110.8(2) 1_455 . ? O3 P1 C11 106.8(2) . . ? O2 P1 C11 110.8(2) 1_455 . ? O1 P1 C11 102.1(2) . . ? P2 O4 Mn1 126.0(2) . . ? P2 O4 Mn2 135.3(2) . . ? Mn1 O4 Mn2 96.74(14) . . ? P1 O1 Mn1 129.5(2) . . ? P1 O1 Mn2 123.6(2) . . ? Mn1 O1 Mn2 98.61(15) . . ? P2 O5 Mn1 134.9(2) 2_656 2_556 ? P2 O5 Mn1 124.5(2) 2_656 . ? Mn1 O5 Mn1 97.89(14) 2_556 . ? P1 O2 Mn2 138.3(2) 1_655 . ? P2 O6 Mn2 129.9(2) 2_656 . ? C5 N1 C1 108.3(4) . . ? C5 N1 C11 107.5(4) . . ? C1 N1 C11 109.5(4) . . ? C5 N1 Mn2 115.3(3) . . ? C1 N1 Mn2 112.2(3) . . ? C11 N1 Mn2 103.8(3) . . ? C10 N2 C12 109.0(4) . . ? C10 N2 C6 108.1(4) . . ? C12 N2 C6 111.1(4) . . ? N1 C1 C2 111.7(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C7 C8 C9 108.1(5) . . ? C7 C8 C3 115.0(5) . . ? C9 C8 C3 111.0(5) . . ? C7 C8 H8 107.5 . . ? C9 C8 H8 107.5 . . ? C3 C8 H8 107.5 . . ? N1 C11 P1 113.9(4) . . ? N1 C11 H11A 108.8 . . ? P1 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? P1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C5 C4 C3 112.7(5) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C8 C7 C6 110.5(5) . 1_556 ? C8 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 1_556 . ? C8 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 1_556 . ? H7A C7 H7B 108.1 . . ? C1 C2 C3 112.4(5) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N2 C12 P2 115.8(4) . . ? N2 C12 H12A 108.3 . . ? P2 C12 H12A 108.3 . . ? N2 C12 H12B 108.3 . . ? P2 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C2 C3 C8 114.3(5) . . ? C2 C3 C4 107.1(5) . . ? C8 C3 C4 110.6(5) . . ? C2 C3 H3 108.2 . . ? C8 C3 H3 108.2 . . ? C4 C3 H3 108.2 . . ? N2 C6 C7 110.7(4) . 1_554 ? N2 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 1_554 . ? N2 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 1_554 . ? H6A C6 H6B 108.1 . . ? C10 C9 C8 113.4(5) 1_556 . ? C10 C9 H9A 108.9 1_556 . ? C8 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 1_556 . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N1 C5 C4 112.0(4) . . ? N1 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? N1 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N2 C10 C9 111.5(4) . 1_554 ? N2 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 1_554 . ? N2 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 1_554 . ? H10A C10 H10B 108.0 . . ? Mn1 O3W H3WA 105(5) . . ? Mn1 O3W H3WB 100(4) . . ? H3WA O3W H3WB 102(6) . . ? Mn2 O1W H1WA 104(5) . . ? Mn2 O1W H1WB 115(5) . . ? H1WA O1W H1WB 94(6) . . ? Mn1 O2W H2WA 101(4) . . ? Mn1 O2W H2WB 106(6) . . ? H2WA O2W H2WB 93(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.779 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.287 # Attachment '- Sn6O2(H2L)(PO4)2 4H2O.cif' data_final _database_code_depnum_ccdc_archive 'CCDC 849783' #TrackingRef '- Sn6O2(H2L)(PO4)2 4H2O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 N O10 P2 Sn3' _chemical_formula_weight 680.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.78060(10) _cell_length_b 10.7596(2) _cell_length_c 11.5754(2) _cell_angle_alpha 88.3260(10) _cell_angle_beta 80.3550(10) _cell_angle_gamma 73.2260(10) _cell_volume 796.98(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.54 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 4.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4400 _exptl_absorpt_correction_T_max 0.5677 _exptl_absorpt_process_details 'SADABS 2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEXII CCD Area Diffractometer' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27434 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.50 _reflns_number_total 4000 _reflns_number_gt 3917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were found in the difference map and were constrained and refined using a riding model. ; _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^)+(0.0252P)^2^+2.4776P] 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 4000 _refine_ls_number_parameters 211 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.190 _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 Sn1 Sn 0.07896(3) 0.19621(2) 0.672186(19) 0.01064(6) Uani 1 1 d . . . Sn2 Sn 0.32992(3) 0.08128(2) 0.381552(18) 0.00865(6) Uani 1 1 d . . . Sn3 Sn 0.33063(3) 0.39191(2) 0.477430(19) 0.00963(6) Uani 1 1 d . . . P2 P 0.79500(12) 0.15922(8) 0.45918(7) 0.00821(15) Uani 1 1 d . . . P1 P 0.12729(14) 0.47963(8) 0.24076(8) 0.01328(16) Uani 1 1 d . . . O4 O -0.1778(4) 0.1961(2) 0.5813(2) 0.0130(5) Uani 1 1 d . . . O3 O 0.2590(4) 0.3682(2) 0.3048(2) 0.0155(5) Uani 1 1 d . . . O5 O 0.6348(4) 0.2682(2) 0.4085(2) 0.0130(5) Uani 1 1 d . . . O8 O 0.2522(3) 0.2208(2) 0.5134(2) 0.0103(4) Uani 1 1 d . . . O6 O 0.2799(4) -0.0355(2) 0.5305(2) 0.0118(4) Uani 1 1 d . . . O7 O 0.0005(3) 0.1307(2) 0.3699(2) 0.0105(4) Uani 1 1 d . . . O2 O -0.0286(4) 0.4042(2) 0.6736(2) 0.0157(5) Uani 1 1 d . . . O1 O 0.2374(4) 0.5114(3) 0.1254(2) 0.0210(5) Uani 1 1 d . . . N1 N -0.0534(4) 0.2894(3) 0.1733(2) 0.0125(5) Uani 1 1 d . . . H1 H -0.0307 0.2374 0.2381 0.015 Uiso 1 1 calc R . . C1 C -0.0969(5) 0.4284(3) 0.2122(3) 0.0158(7) Uani 1 1 d . . . H1A H -0.2022 0.4442 0.2846 0.019 Uiso 1 1 calc R . . H1B H -0.1606 0.4850 0.1512 0.019 Uiso 1 1 calc R . . C2 C 0.1329(5) 0.2432(3) 0.0798(3) 0.0163(7) Uani 1 1 d . . . H2A H 0.2576 0.2545 0.1070 0.020 Uiso 1 1 calc R . . H2B H 0.1110 0.2958 0.0089 0.020 Uiso 1 1 calc R . . C5 C -0.2124(5) 0.1302(3) 0.1042(3) 0.0148(6) Uani 1 1 d . . . H5A H -0.3377 0.1209 0.0762 0.018 Uiso 1 1 calc R . . H5B H -0.1974 0.0804 0.1771 0.018 Uiso 1 1 calc R . . C4 C -0.0189(5) 0.0731(3) 0.0111(3) 0.0136(6) Uani 1 1 d . . . H4 H -0.0426 0.1189 -0.0640 0.016 Uiso 1 1 calc R . . C3 C 0.1702(5) 0.1004(3) 0.0491(3) 0.0171(7) Uani 1 1 d . . . H3A H 0.2057 0.0475 0.1182 0.020 Uiso 1 1 calc R . . H3B H 0.2913 0.0732 -0.0151 0.020 Uiso 1 1 calc R . . C6 C -0.2430(5) 0.2725(3) 0.1309(3) 0.0152(6) Uani 1 1 d . . . H6A H -0.2663 0.3235 0.0593 0.018 Uiso 1 1 calc R . . H6B H -0.3679 0.3052 0.1918 0.018 Uiso 1 1 calc R . . O1W O 0.5364(5) 0.6360(3) 0.0731(3) 0.0336(7) Uani 1 1 d D . . H1WA H 0.429(7) 0.599(5) 0.093(5) 0.040 Uiso 1 1 d D . . H1WB H 0.621(8) 0.593(5) 0.008(3) 0.040 Uiso 1 1 d D . . O2W O 0.5809(5) 0.7225(4) 0.2830(3) 0.0427(9) Uani 1 1 d D . . H2WB H 0.450(6) 0.765(5) 0.323(5) 0.051 Uiso 1 1 d D . . H2WA H 0.556(10) 0.689(6) 0.214(4) 0.051 Uiso 1 1 d 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 Sn1 0.01175(11) 0.01074(11) 0.00888(11) 0.00069(8) -0.00002(8) -0.00335(8) Sn2 0.00752(10) 0.00818(10) 0.00937(10) -0.00169(7) 0.00028(7) -0.00164(7) Sn3 0.00932(10) 0.00668(10) 0.01298(11) -0.00095(8) -0.00104(8) -0.00283(8) P2 0.0064(3) 0.0073(3) 0.0108(4) -0.0002(3) -0.0006(3) -0.0022(3) P1 0.0131(4) 0.0130(4) 0.0130(4) -0.0011(3) -0.0007(3) -0.0034(3) O4 0.0099(10) 0.0165(11) 0.0125(11) -0.0037(9) 0.0000(9) -0.0041(9) O3 0.0157(11) 0.0143(11) 0.0150(11) -0.0021(9) -0.0037(9) -0.0009(9) O5 0.0092(10) 0.0107(11) 0.0174(12) 0.0032(9) -0.0013(9) -0.0011(8) O8 0.0114(10) 0.0082(10) 0.0117(11) -0.0016(8) -0.0006(8) -0.0037(8) O6 0.0136(11) 0.0087(10) 0.0147(11) 0.0013(8) -0.0031(9) -0.0053(9) O7 0.0070(10) 0.0132(11) 0.0100(10) -0.0006(8) 0.0008(8) -0.0021(8) O2 0.0174(12) 0.0120(11) 0.0165(12) -0.0034(9) -0.0019(9) -0.0024(9) O1 0.0246(13) 0.0211(13) 0.0169(12) 0.0010(10) 0.0017(10) -0.0089(11) N1 0.0132(13) 0.0105(13) 0.0127(13) -0.0021(10) -0.0007(11) -0.0024(10) C1 0.0151(15) 0.0116(15) 0.0210(17) -0.0033(13) -0.0032(13) -0.0037(12) C2 0.0144(15) 0.0151(16) 0.0188(17) -0.0075(13) 0.0037(13) -0.0060(13) C5 0.0126(15) 0.0158(16) 0.0161(16) -0.0013(12) -0.0012(12) -0.0046(12) C4 0.0154(15) 0.0150(16) 0.0105(15) -0.0016(12) -0.0007(12) -0.0052(13) C3 0.0127(15) 0.0159(16) 0.0217(17) -0.0068(13) -0.0001(13) -0.0036(13) C6 0.0130(15) 0.0155(16) 0.0163(16) -0.0028(13) -0.0024(12) -0.0026(12) O1W 0.0340(17) 0.0423(19) 0.0273(16) -0.0017(14) -0.0010(13) -0.0175(15) O2W 0.0264(16) 0.057(2) 0.042(2) -0.0198(17) -0.0071(15) -0.0052(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 Sn1 O8 2.063(2) . ? Sn1 O2 2.143(2) . ? Sn1 O4 2.180(2) . ? Sn2 O8 2.065(2) . ? Sn2 O6 2.143(2) . ? Sn2 O7 2.168(2) . ? Sn3 O8 2.072(2) . ? Sn3 O5 2.142(2) . ? Sn3 O3 2.173(2) . ? P2 O5 1.529(2) . ? P2 O4 1.533(2) 1_655 ? P2 O7 1.547(2) 1_655 ? P2 O6 1.551(2) 2_656 ? P1 O1 1.498(3) . ? P1 O3 1.529(3) . ? P1 O2 1.536(2) 2_566 ? P1 C1 1.840(4) . ? N1 C2 1.492(4) . ? N1 C1 1.505(4) . ? N1 C6 1.510(4) . ? N1 H1 0.9300 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.526(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 C6 1.518(5) . ? C5 C4 1.536(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C4 C3 1.529(5) . ? C4 C4 1.542(6) 2 ? C4 H4 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O1W H1WA 0.92(3) . ? O1W H1WB 0.91(3) . ? O2W H2WB 0.92(3) . ? O2W H2WA 0.95(3) . ? 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 O8 Sn1 O2 83.32(9) . . ? O8 Sn1 O4 89.02(9) . . ? O2 Sn1 O4 87.80(9) . . ? O8 Sn2 O6 80.24(9) . . ? O8 Sn2 O7 87.68(9) . . ? O6 Sn2 O7 89.89(9) . . ? O8 Sn3 O5 85.19(9) . . ? O8 Sn3 O3 84.35(9) . . ? O5 Sn3 O3 84.75(9) . . ? O5 P2 O4 111.56(14) . 1_655 ? O5 P2 O7 106.66(13) . 1_655 ? O4 P2 O7 112.51(13) 1_655 1_655 ? O5 P2 O6 109.16(13) . 2_656 ? O4 P2 O6 108.44(13) 1_655 2_656 ? O7 P2 O6 108.43(13) 1_655 2_656 ? O1 P1 O3 114.68(15) . . ? O1 P1 O2 114.59(15) . 2_566 ? O3 P1 O2 108.64(14) . 2_566 ? O1 P1 C1 107.58(16) . . ? O3 P1 C1 106.46(15) . . ? O2 P1 C1 104.03(15) 2_566 . ? P2 O4 Sn1 137.51(14) 1_455 . ? P1 O3 Sn3 122.86(14) . . ? P2 O5 Sn3 134.10(14) . . ? Sn1 O8 Sn2 120.56(11) . . ? Sn1 O8 Sn3 120.86(11) . . ? Sn2 O8 Sn3 118.39(11) . . ? P2 O6 Sn2 130.09(14) 2_656 . ? P2 O7 Sn2 135.32(13) 1_455 . ? P1 O2 Sn1 140.73(16) 2_566 . ? C2 N1 C1 114.2(3) . . ? C2 N1 C6 109.2(3) . . ? C1 N1 C6 109.3(3) . . ? C2 N1 H1 108.0 . . ? C1 N1 H1 108.0 . . ? C6 N1 H1 108.0 . . ? N1 C1 P1 116.9(2) . . ? N1 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? N1 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? N1 C2 C3 110.7(3) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C6 C5 C4 112.1(3) . . ? C6 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C3 C4 C5 108.9(3) . . ? C3 C4 C4 111.5(3) . 2 ? C5 C4 C4 112.0(3) . 2 ? C3 C4 H4 108.1 . . ? C5 C4 H4 108.1 . . ? C4 C4 H4 108.1 2 . ? C2 C3 C4 113.0(3) . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N1 C6 C5 110.3(3) . . ? N1 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? H1WA O1W H1WB 107(5) . . ? H2WB O2W H2WA 105(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.809 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.177 # Attachment '- Sn7O(L)3.cif' data_t2 _database_code_depnum_ccdc_archive 'CCDC 849784' #TrackingRef '- Sn7O(L)3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 N6 O19 P6 Sn7' _chemical_formula_weight 1903.60 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 9.8370(19) _cell_length_b 16.889(3) _cell_length_c 35.248(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.773(2) _cell_angle_gamma 90.00 _cell_volume 5853(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.87 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 3.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6650 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details 'SADABS 2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEXII CCD Area Diffractometer' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33630 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13542 _reflns_number_gt 12749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically, and were constrained and refined using a riding model. The flack parameter is necessarily zero (and meaningless) since the refinement included TWIN and BASF commands to account for the twinned (and/or cracked) crystal. No solvent molecules could be found in the void by inspection of the difference map. The second weighting parameter is quite large, but this is common in refinements on data which include very strong reflections on the same frame as very weak reflections. The presence of several strong scatterers (Sn atoms) within the structure exacerbates this problem. ; _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^)+(0.0147P)^2^+94.9558P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 6643 Friedel pairs' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 13542 _refine_ls_number_parameters 640 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Sn1 Sn 0.92313(5) 0.45990(4) 0.453680(16) 0.01226(12) Uani 1 1 d . . . Sn2 Sn 1.52914(5) 0.03575(3) 0.363407(16) 0.01247(12) Uani 1 1 d . . . Sn3 Sn 1.44082(5) 0.30079(3) 0.539796(17) 0.01185(12) Uani 1 1 d . . . Sn4 Sn 1.48084(6) 0.46105(3) 0.412750(17) 0.01252(12) Uani 1 1 d . . . Sn5 Sn 1.51312(6) 0.37128(3) 0.277550(17) 0.01186(12) Uani 1 1 d . . . Sn7 Sn 1.64361(5) 0.27188(3) 0.417299(17) 0.01180(12) Uani 1 1 d . . . P1 P 1.7358(2) -0.08250(13) 0.32401(6) 0.0116(4) Uani 1 1 d . . . P3 P 1.5501(2) 0.20305(13) 0.32581(6) 0.0115(4) Uani 1 1 d . . . O7 O 1.4740(6) 0.1246(3) 0.32329(17) 0.0143(13) Uani 1 1 d . . . O1 O 1.6496(6) -0.0078(4) 0.31938(17) 0.0185(14) Uani 1 1 d . . . O10 O 1.6238(6) 0.4478(4) 0.45839(16) 0.0153(9) Uani 1 1 d . . . O8 O 1.6131(6) 0.2119(4) 0.36545(16) 0.0156(13) Uani 1 1 d . . . O9 O 1.4580(6) 0.2701(3) 0.31373(17) 0.0157(13) Uani 1 1 d . . . O4 O 1.3689(6) -0.0339(4) 0.34103(17) 0.0156(13) Uani 1 1 d . . . C19 C 1.6977(9) 0.2013(6) 0.2954(2) 0.0170(18) Uani 1 1 d . . . H19A H 1.7625 0.2432 0.3036 0.020 Uiso 1 1 calc R . . H19B H 1.7445 0.1496 0.2982 0.020 Uiso 1 1 calc R . . O13 O 1.1057(6) 0.4423(3) 0.48691(16) 0.0112(12) Uani 1 1 d . . . O2 O 1.3816(6) 0.4339(4) 0.31386(17) 0.0150(13) Uani 1 1 d . . . O3 O 1.2219(6) 0.3856(3) 0.36394(17) 0.0125(8) Uani 1 1 d . . . Sn6 Sn 1.28353(5) 0.28296(3) 0.396297(17) 0.01198(12) Uani 1 1 d . . . P2 P 1.2134(2) -0.04102(14) 0.34149(6) 0.0138(4) Uani 1 1 d . . . O19 O 1.4695(7) 0.3381(3) 0.40775(19) 0.0125(8) Uani 1 1 d . . . P4 P 1.6636(2) 0.41639(13) 0.49781(6) 0.0107(4) Uani 1 1 d . . . P6 P 0.9788(2) 0.65386(13) 0.47828(6) 0.0100(4) Uani 1 1 d . . . P5 P 1.1916(2) 0.36762(13) 0.48298(6) 0.0123(4) Uani 1 1 d . . . O11 O 0.8202(6) 0.4193(3) 0.50204(16) 0.0140(13) Uani 1 1 d . . . O14 O 1.3301(6) 0.3805(4) 0.50122(17) 0.0159(13) Uani 1 1 d . . . O12 O 1.6086(6) 0.3338(4) 0.50550(16) 0.0153(9) Uani 1 1 d . . . O16 O 0.9092(6) 0.5736(4) 0.47699(18) 0.0182(13) Uani 1 1 d . . . O17 O 0.8910(6) 0.7145(3) 0.49895(17) 0.0146(13) Uani 1 1 d . . . O5 O 1.1697(6) -0.1151(4) 0.31986(18) 0.0186(14) Uani 1 1 d . . . O6 O 1.1633(6) -0.0405(4) 0.38163(17) 0.0195(14) Uani 1 1 d . . . N3 N 1.6573(7) 0.2138(4) 0.25521(19) 0.0108(14) Uani 1 1 d . . . O15 O 1.1915(6) 0.3430(4) 0.44136(17) 0.0185(14) Uani 1 1 d . . . O18 O 1.0144(6) 0.6807(4) 0.43855(17) 0.0160(13) Uani 1 1 d . . . N1 N 1.6999(8) -0.1431(4) 0.2526(2) 0.0156(16) Uani 1 1 d . . . C2 C 1.5948(10) -0.0910(5) 0.2347(3) 0.0203(14) Uani 1 1 d . . . H2A H 1.5914 -0.0405 0.2489 0.024 Uiso 1 1 calc R . . H2B H 1.5047 -0.1167 0.2362 0.024 Uiso 1 1 calc R . . N5 N 1.1458(7) 0.2930(4) 0.54956(19) 0.0134(15) Uani 1 1 d . . . C20 C 1.6162(8) 0.1401(5) 0.2364(2) 0.0124(17) Uani 1 1 d . . . H20A H 1.5440 0.1143 0.2509 0.015 Uiso 1 1 calc R . . H20B H 1.6950 0.1036 0.2359 0.015 Uiso 1 1 calc R . . C1 C 1.6683(9) -0.1574(6) 0.2927(2) 0.0167(18) Uani 1 1 d . . . H1A H 1.7059 -0.2094 0.3006 0.020 Uiso 1 1 calc R . . H1B H 1.5683 -0.1596 0.2950 0.020 Uiso 1 1 calc R . . C31 C 1.1122(9) 0.2873(5) 0.5085(2) 0.0155(18) Uani 1 1 d . . . H31A H 1.0123 0.2898 0.5043 0.019 Uiso 1 1 calc R . . H31B H 1.1443 0.2359 0.4987 0.019 Uiso 1 1 calc R . . C36 C 1.0642(10) 0.3518(6) 0.5685(3) 0.021(2) Uani 1 1 d . . . H36A H 0.9680 0.3346 0.5679 0.025 Uiso 1 1 calc R . . H36B H 1.0693 0.4027 0.5547 0.025 Uiso 1 1 calc R . . N2 N 1.1215(7) 0.0250(4) 0.27573(19) 0.0124(14) Uani 1 1 d . . . N4 N 1.5954(7) 0.4580(4) 0.57006(19) 0.0135(15) Uani 1 1 d . . . N6 N 1.1178(7) 0.6597(4) 0.5458(2) 0.0145(15) Uani 1 1 d . . . C22 C 1.6712(9) 0.1984(5) 0.1729(2) 0.0139(12) Uani 1 1 d . . . H22 H 1.7525 0.1631 0.1713 0.017 Uiso 1 1 calc R . . C23 C 1.7140(9) 0.2724(5) 0.1946(3) 0.0178(19) Uani 1 1 d . . . H23A H 1.7871 0.2995 0.1809 0.021 Uiso 1 1 calc R . . H23B H 1.6356 0.3091 0.1956 0.021 Uiso 1 1 calc R . . C24 C 1.7641(9) 0.2535(5) 0.2345(2) 0.0142(18) Uani 1 1 d . . . H24A H 1.8451 0.2188 0.2336 0.017 Uiso 1 1 calc R . . H24B H 1.7909 0.3030 0.2478 0.017 Uiso 1 1 calc R . . C5 C 1.7478(9) -0.2023(5) 0.1902(2) 0.0157(18) Uani 1 1 d . . . H5A H 1.7567 -0.2534 0.1767 0.019 Uiso 1 1 calc R . . H5B H 1.8369 -0.1751 0.1900 0.019 Uiso 1 1 calc R . . C35 C 1.1125(10) 0.3639(5) 0.6093(2) 0.0147(18) Uani 1 1 d . . . H35A H 1.0520 0.4024 0.6215 0.018 Uiso 1 1 calc R . . H35B H 1.2053 0.3866 0.6097 0.018 Uiso 1 1 calc R . . C26 C 1.4831(9) 0.4876(5) 0.5916(2) 0.0156(18) Uani 1 1 d . . . H26A H 1.3961 0.4739 0.5783 0.019 Uiso 1 1 calc R . . H26B H 1.4889 0.5460 0.5934 0.019 Uiso 1 1 calc R . . C9 C 1.1694(9) 0.6322(6) 0.6279(2) 0.0165(18) Uani 1 1 d . . . H9 H 1.2411 0.5902 0.6275 0.020 Uiso 1 1 calc R . . C3 C 1.6254(9) -0.0738(5) 0.1925(2) 0.0154(18) Uani 1 1 d . . . H3A H 1.5509 -0.0414 0.1811 0.018 Uiso 1 1 calc R . . H3B H 1.7106 -0.0429 0.1913 0.018 Uiso 1 1 calc R . . C34 C 1.1143(9) 0.2867(5) 0.6323(2) 0.0128(17) Uani 1 1 d . . . H34 H 1.0183 0.2681 0.6341 0.015 Uiso 1 1 calc R . . C13 C 1.1366(8) 0.0410(5) 0.3168(2) 0.0153(18) Uani 1 1 d . . . H13A H 1.0461 0.0517 0.3272 0.018 Uiso 1 1 calc R . . H13B H 1.1936 0.0888 0.3209 0.018 Uiso 1 1 calc R . . C10 C 1.0445(10) 0.6020(6) 0.6060(3) 0.020(2) Uani 1 1 d . . . H10A H 0.9705 0.6414 0.6078 0.024 Uiso 1 1 calc R . . H10B H 1.0133 0.5523 0.6179 0.024 Uiso 1 1 calc R . . C6 C 1.7087(10) -0.2176(5) 0.2310(3) 0.0203(14) Uani 1 1 d . . . H6A H 1.6198 -0.2450 0.2310 0.024 Uiso 1 1 calc R . . H6B H 1.7773 -0.2527 0.2434 0.024 Uiso 1 1 calc R . . C25 C 1.5872(8) 0.4857(5) 0.5307(2) 0.0100(16) Uani 1 1 d . . . H25A H 1.6339 0.5374 0.5290 0.012 Uiso 1 1 calc R . . H25B H 1.4905 0.4937 0.5230 0.012 Uiso 1 1 calc R . . C14 C 1.2531(9) 0.0349(5) 0.2573(2) 0.0145(12) Uani 1 1 d . . . H14A H 1.3230 0.0021 0.2705 0.017 Uiso 1 1 calc R . . H14B H 1.2820 0.0910 0.2591 0.017 Uiso 1 1 calc R . . C8 C 1.2221(9) 0.7061(6) 0.6058(3) 0.0180(19) Uani 1 1 d . . . H8A H 1.1550 0.7496 0.6076 0.022 Uiso 1 1 calc R . . H8B H 1.3086 0.7245 0.6179 0.022 Uiso 1 1 calc R . . C27 C 1.4858(8) 0.4524(5) 0.6312(2) 0.0144(17) Uani 1 1 d . . . H27A H 1.4785 0.3941 0.6295 0.017 Uiso 1 1 calc R . . H27B H 1.4072 0.4723 0.6453 0.017 Uiso 1 1 calc R . . C12 C 1.1374(9) 0.6461(5) 0.5060(3) 0.0153(18) Uani 1 1 d . . . H12A H 1.1766 0.5927 0.5026 0.018 Uiso 1 1 calc R . . H12B H 1.2032 0.6853 0.4966 0.018 Uiso 1 1 calc R . . C7 C 1.2442(9) 0.6881(5) 0.5651(2) 0.0157(18) Uani 1 1 d . . . H7A H 1.2764 0.7364 0.5522 0.019 Uiso 1 1 calc R . . H7B H 1.3157 0.6471 0.5633 0.019 Uiso 1 1 calc R . . C33 C 1.1911(9) 0.2257(5) 0.6100(2) 0.0157(18) Uani 1 1 d . . . H33A H 1.1839 0.1739 0.6229 0.019 Uiso 1 1 calc R . . H33B H 1.2885 0.2405 0.6103 0.019 Uiso 1 1 calc R . . C32 C 1.1417(9) 0.2161(5) 0.5689(3) 0.0165(19) Uani 1 1 d . . . H32A H 1.2004 0.1778 0.5559 0.020 Uiso 1 1 calc R . . H32B H 1.0475 0.1954 0.5680 0.020 Uiso 1 1 calc R . . C21 C 1.5644(9) 0.1553(5) 0.1963(2) 0.0150(18) Uani 1 1 d . . . H21A H 1.4807 0.1878 0.1969 0.018 Uiso 1 1 calc R . . H21B H 1.5408 0.1042 0.1840 0.018 Uiso 1 1 calc R . . C4 C 1.6397(9) -0.1509(5) 0.1694(2) 0.0139(12) Uani 1 1 d . . . H4 H 1.5510 -0.1797 0.1698 0.017 Uiso 1 1 calc R . . C28 C 1.7355(9) 0.4474(5) 0.6288(2) 0.0138(18) Uani 1 1 d . . . H28A H 1.7356 0.3888 0.6280 0.017 Uiso 1 1 calc R . . H28B H 1.8226 0.4647 0.6409 0.017 Uiso 1 1 calc R . . C30 C 1.7272(9) 0.4787(6) 0.5884(2) 0.0165(18) Uani 1 1 d . . . H30A H 1.7383 0.5369 0.5887 0.020 Uiso 1 1 calc R . . H30B H 1.8019 0.4558 0.5738 0.020 Uiso 1 1 calc R . . C29 C 1.6194(8) 0.4751(5) 0.6527(2) 0.0122(17) Uani 1 1 d . . . H29 H 1.6236 0.5342 0.6539 0.015 Uiso 1 1 calc R . . C16 C 1.1308(8) 0.0559(5) 0.1937(2) 0.0141(17) Uani 1 1 d . . . H16 H 1.1580 0.1129 0.1928 0.017 Uiso 1 1 calc R . . C17 C 0.9988(9) 0.0501(6) 0.2151(2) 0.0175(19) Uani 1 1 d . . . H17A H 0.9296 0.0849 0.2028 0.021 Uiso 1 1 calc R . . H17B H 0.9646 -0.0050 0.2136 0.021 Uiso 1 1 calc R . . C18 C 1.0171(9) 0.0738(5) 0.2567(2) 0.0145(12) Uani 1 1 d . . . H18A H 1.0437 0.1302 0.2584 0.017 Uiso 1 1 calc R . . H18B H 0.9298 0.0673 0.2696 0.017 Uiso 1 1 calc R . . C15 C 1.2415(9) 0.0108(6) 0.2159(2) 0.0170(19) Uani 1 1 d . . . H15A H 1.2216 -0.0466 0.2144 0.020 Uiso 1 1 calc R . . H15B H 1.3299 0.0200 0.2040 0.020 Uiso 1 1 calc R . . C11 C 1.0704(9) 0.5864(5) 0.5643(2) 0.0169(19) Uani 1 1 d . . . H11A H 1.1401 0.5444 0.5622 0.020 Uiso 1 1 calc R . . H11B H 0.9856 0.5676 0.5514 0.020 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 Sn1 0.0119(3) 0.0153(3) 0.0096(3) 0.0009(2) 0.0005(2) -0.0015(2) Sn2 0.0148(3) 0.0127(3) 0.0100(3) 0.0008(2) 0.0014(2) -0.0007(2) Sn3 0.0118(3) 0.0135(3) 0.0103(3) 0.0010(2) 0.0007(2) -0.0021(2) Sn4 0.0123(3) 0.0110(3) 0.0142(3) 0.0007(2) -0.0017(2) 0.0009(2) Sn5 0.0128(3) 0.0124(3) 0.0104(3) 0.0009(2) 0.0015(2) 0.0011(2) Sn7 0.0110(3) 0.0121(3) 0.0122(3) -0.0003(2) -0.0011(2) 0.0001(2) P1 0.0117(10) 0.0134(11) 0.0098(10) 0.0010(8) 0.0008(8) 0.0010(8) P3 0.0128(11) 0.0096(10) 0.0123(11) 0.0008(8) 0.0035(8) 0.0024(8) O7 0.019(3) 0.009(3) 0.015(3) -0.001(2) 0.003(2) 0.001(2) O1 0.016(3) 0.026(4) 0.013(3) 0.003(3) -0.001(2) 0.004(3) O10 0.020(2) 0.018(2) 0.008(2) 0.0023(17) 0.0001(17) 0.0008(18) O8 0.023(3) 0.017(3) 0.007(3) -0.002(2) -0.001(2) 0.003(3) O9 0.018(3) 0.012(3) 0.016(3) 0.000(2) -0.004(2) 0.000(2) O4 0.015(3) 0.015(3) 0.016(3) 0.002(2) 0.000(2) -0.001(2) C19 0.014(4) 0.022(5) 0.016(4) -0.001(4) 0.007(3) 0.002(4) O13 0.005(3) 0.012(3) 0.017(3) 0.001(2) 0.001(2) 0.000(2) O2 0.013(3) 0.014(3) 0.018(3) -0.004(2) 0.003(2) 0.005(2) O3 0.012(2) 0.0115(19) 0.014(2) -0.0002(17) 0.0044(15) 0.0014(16) Sn6 0.0127(3) 0.0109(3) 0.0123(3) -0.0003(2) -0.0003(2) -0.0007(2) P2 0.0121(11) 0.0176(11) 0.0117(10) 0.0048(9) -0.0004(8) -0.0013(9) O19 0.012(2) 0.0115(19) 0.014(2) -0.0002(17) 0.0044(15) 0.0014(16) P4 0.0125(10) 0.0123(11) 0.0072(10) 0.0006(8) -0.0001(8) -0.0017(8) P6 0.0100(10) 0.0088(10) 0.0113(10) 0.0009(8) -0.0005(8) -0.0007(8) P5 0.0104(11) 0.0140(11) 0.0126(11) 0.0016(9) 0.0019(8) 0.0001(8) O11 0.021(3) 0.012(3) 0.008(3) 0.004(2) -0.002(2) -0.005(2) O14 0.015(3) 0.013(3) 0.020(3) 0.009(2) 0.000(2) -0.001(2) O12 0.020(2) 0.018(2) 0.008(2) 0.0023(17) 0.0001(17) 0.0008(18) O16 0.018(3) 0.008(3) 0.028(4) 0.003(3) -0.001(3) -0.002(2) O17 0.016(3) 0.009(3) 0.019(3) -0.003(2) -0.002(2) 0.003(2) O5 0.013(3) 0.022(3) 0.021(3) 0.005(3) -0.003(3) -0.002(3) O6 0.015(3) 0.033(4) 0.010(3) 0.005(3) -0.003(2) -0.005(3) N3 0.009(3) 0.016(4) 0.007(3) 0.000(3) 0.003(3) -0.007(3) O15 0.013(3) 0.026(3) 0.016(3) -0.002(3) 0.000(2) 0.005(3) O18 0.021(3) 0.014(3) 0.013(3) 0.000(2) 0.000(2) -0.006(3) N1 0.020(4) 0.014(4) 0.014(4) 0.000(3) 0.001(3) 0.007(3) C2 0.023(3) 0.004(3) 0.034(4) 0.002(3) -0.001(3) 0.001(2) N5 0.015(4) 0.016(4) 0.009(3) 0.001(3) -0.006(3) -0.004(3) C20 0.008(4) 0.014(4) 0.015(4) -0.001(3) 0.005(3) -0.002(3) C1 0.008(4) 0.026(5) 0.015(4) -0.001(4) -0.004(3) -0.002(3) C31 0.017(4) 0.015(4) 0.014(4) 0.003(3) -0.001(3) -0.003(3) C36 0.026(5) 0.022(5) 0.014(5) 0.003(4) -0.003(4) -0.001(4) N2 0.012(3) 0.016(4) 0.009(3) 0.003(3) -0.001(3) -0.003(3) N4 0.016(4) 0.019(4) 0.005(3) 0.003(3) -0.001(3) -0.001(3) N6 0.016(4) 0.016(4) 0.012(4) 0.004(3) 0.002(3) 0.003(3) C22 0.016(3) 0.018(3) 0.008(3) 0.000(2) 0.001(2) -0.002(2) C23 0.016(4) 0.020(5) 0.018(5) 0.004(4) 0.005(4) -0.002(4) C24 0.015(4) 0.017(5) 0.012(4) 0.002(3) 0.006(3) -0.003(3) C5 0.015(4) 0.014(4) 0.018(5) -0.001(3) 0.000(3) 0.005(3) C35 0.027(5) 0.008(4) 0.010(4) 0.000(3) 0.006(3) -0.005(3) C26 0.018(5) 0.017(4) 0.012(4) 0.000(3) 0.005(3) 0.008(4) C9 0.014(4) 0.021(5) 0.015(4) 0.011(4) -0.002(3) 0.003(3) C3 0.016(4) 0.015(4) 0.015(4) 0.001(3) 0.002(3) 0.008(3) C34 0.015(4) 0.013(4) 0.011(4) -0.002(3) 0.008(3) 0.000(3) C13 0.007(4) 0.023(5) 0.017(4) -0.002(4) 0.003(3) -0.002(3) C10 0.027(5) 0.014(4) 0.020(5) -0.002(4) -0.001(4) -0.001(4) C6 0.023(3) 0.004(3) 0.034(4) 0.002(3) -0.001(3) 0.001(2) C25 0.008(4) 0.012(4) 0.010(4) -0.002(3) 0.001(3) 0.001(3) C14 0.013(3) 0.016(3) 0.014(3) 0.006(2) -0.003(2) 0.002(2) C8 0.009(4) 0.025(5) 0.020(5) 0.002(4) -0.005(3) -0.004(4) C27 0.012(4) 0.019(4) 0.012(4) -0.008(3) 0.004(3) -0.001(3) C12 0.012(4) 0.012(4) 0.022(5) 0.005(3) -0.004(3) 0.001(3) C7 0.011(4) 0.020(5) 0.016(4) 0.005(4) -0.002(3) -0.005(3) C33 0.013(4) 0.019(5) 0.015(4) 0.009(4) 0.003(3) -0.005(4) C32 0.017(5) 0.015(5) 0.018(5) 0.002(4) 0.010(4) 0.002(3) C21 0.015(4) 0.018(4) 0.012(4) 0.003(3) 0.000(3) -0.009(3) C4 0.016(3) 0.018(3) 0.008(3) 0.000(2) 0.001(2) -0.002(2) C28 0.016(4) 0.018(5) 0.007(4) -0.002(3) 0.005(3) 0.002(3) C30 0.016(4) 0.025(5) 0.009(4) 0.003(3) 0.002(3) 0.004(4) C29 0.012(4) 0.013(4) 0.012(4) -0.002(3) 0.001(3) 0.001(3) C16 0.009(4) 0.017(4) 0.016(4) 0.002(3) 0.001(3) 0.002(3) C17 0.020(5) 0.020(5) 0.013(4) -0.001(4) 0.008(4) 0.011(4) C18 0.013(3) 0.016(3) 0.014(3) 0.006(2) -0.003(2) 0.002(2) C15 0.008(4) 0.023(5) 0.021(5) 0.008(4) 0.000(3) 0.003(3) C11 0.022(5) 0.021(5) 0.009(4) 0.004(3) 0.006(3) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O16 2.095(6) . ? Sn1 O11 2.123(6) . ? Sn1 O13 2.134(6) . ? Sn2 O4 2.101(6) . ? Sn2 O1 2.114(6) . ? Sn2 O7 2.121(6) . ? Sn3 O17 2.096(6) 3_545 ? Sn3 O12 2.150(6) . ? Sn3 O14 2.181(6) . ? Sn4 O19 2.086(6) . ? Sn4 O10 2.115(6) . ? Sn4 O6 2.132(6) 3 ? Sn5 O5 2.123(6) 3 ? Sn5 O2 2.129(6) . ? Sn5 O9 2.210(6) . ? Sn7 O19 2.064(6) . ? Sn7 O8 2.103(6) . ? Sn7 O18 2.146(6) 3_545 ? P1 O2 1.514(6) 3_545 ? P1 O3 1.517(6) 3_545 ? P1 O1 1.526(7) . ? P1 C1 1.793(9) . ? P3 O9 1.503(6) . ? P3 O8 1.519(6) . ? P3 O7 1.523(6) . ? P3 C19 1.832(8) . ? O10 P4 1.527(6) . ? O4 P2 1.535(6) . ? C19 N3 1.475(11) . ? O13 P5 1.527(6) . ? Sn6 O19 2.082(7) . ? Sn6 O15 2.112(6) . ? P2 O6 1.513(6) . ? P2 O5 1.520(7) . ? P2 C13 1.790(9) . ? P4 O12 1.524(6) . ? P4 O11 1.544(7) 1_655 ? P4 C25 1.825(8) . ? P6 O16 1.518(6) . ? P6 O18 1.523(6) . ? P6 O17 1.538(6) . ? P6 C12 1.821(9) . ? P5 O14 1.504(6) . ? P5 O15 1.524(6) . ? P5 C31 1.817(9) . ? O5 Sn5 2.123(6) 3_445 ? O6 Sn4 2.132(6) 3_445 ? N3 C24 1.461(10) . ? N3 C20 1.463(11) . ? N1 C6 1.474(11) . ? N1 C1 1.477(11) . ? N1 C2 1.483(11) . ? C2 C3 1.553(13) . ? N5 C36 1.453(12) . ? N5 C32 1.468(11) . ? N5 C31 1.478(11) . ? C20 C21 1.509(12) . ? C36 C35 1.514(12) . ? N2 C18 1.463(10) . ? N2 C13 1.477(11) . ? N2 C14 1.476(11) . ? N4 C26 1.448(10) . ? N4 C25 1.465(10) . ? N4 C30 1.474(11) . ? N6 C12 1.437(11) . ? N6 C7 1.479(11) . ? N6 C11 1.482(11) . ? C22 C23 1.518(13) . ? C22 C21 1.539(11) . ? C22 C34 1.544(12) 4_554 ? C23 C24 1.511(12) . ? C5 C6 1.521(13) . ? C5 C4 1.540(12) . ? C35 C34 1.533(12) . ? C26 C27 1.516(12) . ? C9 C10 1.519(13) . ? C9 C4 1.533(12) 4_455 ? C9 C8 1.568(12) . ? C3 C4 1.546(12) . ? C34 C33 1.513(12) . ? C34 C22 1.544(12) 4_455 ? C10 C11 1.522(12) . ? C14 C15 1.515(12) . ? C8 C7 1.490(13) . ? C27 C29 1.545(11) . ? C33 C32 1.522(13) . ? C4 C9 1.533(12) 4_554 ? C28 C29 1.515(11) . ? C28 C30 1.516(11) . ? C29 C16 1.537(12) 4 ? C16 C15 1.526(11) . ? C16 C17 1.526(12) . ? C16 C29 1.537(12) 4_454 ? C17 C18 1.525(12) . ? 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 O16 Sn1 O11 86.7(2) . . ? O16 Sn1 O13 88.6(2) . . ? O11 Sn1 O13 85.9(2) . . ? O4 Sn2 O1 87.7(2) . . ? O4 Sn2 O7 88.4(2) . . ? O1 Sn2 O7 83.9(2) . . ? O17 Sn3 O12 87.8(2) 3_545 . ? O17 Sn3 O14 84.2(2) 3_545 . ? O12 Sn3 O14 82.4(2) . . ? O19 Sn4 O10 89.5(2) . . ? O19 Sn4 O6 89.3(3) . 3 ? O10 Sn4 O6 80.8(2) . 3 ? O5 Sn5 O2 88.0(2) 3 . ? O5 Sn5 O9 82.2(2) 3 . ? O2 Sn5 O9 82.7(2) . . ? O19 Sn7 O8 91.4(2) . . ? O19 Sn7 O18 87.0(2) . 3_545 ? O8 Sn7 O18 83.5(2) . 3_545 ? O2 P1 O3 113.4(3) 3_545 3_545 ? O2 P1 O1 110.6(4) 3_545 . ? O3 P1 O1 109.1(3) 3_545 . ? O2 P1 C1 108.6(4) 3_545 . ? O3 P1 C1 106.2(4) 3_545 . ? O1 P1 C1 108.8(4) . . ? O9 P3 O8 114.3(4) . . ? O9 P3 O7 110.4(4) . . ? O8 P3 O7 109.0(4) . . ? O9 P3 C19 109.2(4) . . ? O8 P3 C19 103.4(4) . . ? O7 P3 C19 110.4(4) . . ? P3 O7 Sn2 117.5(4) . . ? P1 O1 Sn2 122.1(4) . . ? P4 O10 Sn4 151.0(4) . . ? P3 O8 Sn7 152.9(4) . . ? P3 O9 Sn5 126.1(4) . . ? P2 O4 Sn2 140.9(4) . . ? N3 C19 P3 111.4(6) . . ? P5 O13 Sn1 121.6(3) . . ? P1 O2 Sn5 130.5(4) 3_455 . ? P1 O3 Sn6 138.2(3) 3_455 . ? O19 Sn6 O15 91.9(2) . . ? O19 Sn6 O3 88.5(2) . . ? O15 Sn6 O3 83.8(2) . . ? O6 P2 O5 112.3(4) . . ? O6 P2 O4 111.3(3) . . ? O5 P2 O4 109.0(4) . . ? O6 P2 C13 107.7(4) . . ? O5 P2 C13 106.5(4) . . ? O4 P2 C13 109.9(4) . . ? Sn7 O19 Sn6 120.6(3) . . ? Sn7 O19 Sn4 118.9(3) . . ? Sn6 O19 Sn4 120.4(3) . . ? O12 P4 O10 113.4(4) . . ? O12 P4 O11 111.8(3) . 1_655 ? O10 P4 O11 107.7(3) . 1_655 ? O12 P4 C25 108.6(4) . . ? O10 P4 C25 104.8(4) . . ? O11 P4 C25 110.4(4) 1_655 . ? O16 P6 O18 110.8(4) . . ? O16 P6 O17 110.4(4) . . ? O18 P6 O17 112.7(4) . . ? O16 P6 C12 109.3(4) . . ? O18 P6 C12 107.3(4) . . ? O17 P6 C12 106.1(4) . . ? O14 P5 O15 115.1(4) . . ? O14 P5 O13 109.7(3) . . ? O15 P5 O13 109.2(3) . . ? O14 P5 C31 107.1(4) . . ? O15 P5 C31 106.6(4) . . ? O13 P5 C31 108.9(4) . . ? P4 O11 Sn1 115.6(3) 1_455 . ? P5 O14 Sn3 127.3(3) . . ? P4 O12 Sn3 128.3(4) . . ? P6 O16 Sn1 142.7(4) . . ? P6 O17 Sn3 131.7(4) . 3_455 ? P2 O5 Sn5 129.0(4) . 3_445 ? P2 O6 Sn4 141.8(4) . 3_445 ? C24 N3 C20 110.9(6) . . ? C24 N3 C19 111.6(7) . . ? C20 N3 C19 112.1(7) . . ? P5 O15 Sn6 150.1(4) . . ? P6 O18 Sn7 133.6(4) . 3_455 ? C6 N1 C1 111.9(7) . . ? C6 N1 C2 109.8(7) . . ? C1 N1 C2 109.7(7) . . ? N1 C2 C3 111.3(7) . . ? C36 N5 C32 111.6(7) . . ? C36 N5 C31 112.6(7) . . ? C32 N5 C31 112.9(7) . . ? N3 C20 C21 111.1(7) . . ? N1 C1 P1 112.9(6) . . ? N5 C31 P5 110.5(6) . . ? N5 C36 C35 111.6(8) . . ? C18 N2 C13 113.2(7) . . ? C18 N2 C14 110.3(6) . . ? C13 N2 C14 110.4(6) . . ? C26 N4 C25 111.5(7) . . ? C26 N4 C30 111.3(7) . . ? C25 N4 C30 111.3(6) . . ? C12 N6 C7 111.4(7) . . ? C12 N6 C11 110.5(7) . . ? C7 N6 C11 109.8(7) . . ? C23 C22 C21 107.7(7) . . ? C23 C22 C34 114.8(7) . 4_554 ? C21 C22 C34 109.9(7) . 4_554 ? C24 C23 C22 111.8(7) . . ? N3 C24 C23 110.1(7) . . ? C6 C5 C4 110.8(7) . . ? C36 C35 C34 112.6(7) . . ? N4 C26 C27 110.8(7) . . ? C10 C9 C4 112.3(7) . 4_455 ? C10 C9 C8 106.8(7) . . ? C4 C9 C8 112.6(8) 4_455 . ? C4 C3 C2 111.8(7) . . ? C33 C34 C35 107.6(7) . . ? C33 C34 C22 114.9(7) . 4_455 ? C35 C34 C22 110.5(7) . 4_455 ? N2 C13 P2 111.2(6) . . ? C9 C10 C11 113.0(8) . . ? N1 C6 C5 111.4(7) . . ? N4 C25 P4 112.7(6) . . ? N2 C14 C15 110.6(7) . . ? C7 C8 C9 112.1(8) . . ? C26 C27 C29 110.2(7) . . ? N6 C12 P6 111.9(6) . . ? N6 C7 C8 111.4(7) . . ? C34 C33 C32 114.6(7) . . ? N5 C32 C33 109.6(7) . . ? C20 C21 C22 111.4(7) . . ? C9 C4 C5 114.9(7) 4_554 . ? C9 C4 C3 110.6(7) 4_554 . ? C5 C4 C3 107.3(7) . . ? C29 C28 C30 113.3(7) . . ? N4 C30 C28 110.5(7) . . ? C28 C29 C16 112.6(7) . 4 ? C28 C29 C27 107.1(7) . . ? C16 C29 C27 114.4(7) 4 . ? C15 C16 C17 108.5(7) . . ? C15 C16 C29 110.0(7) . 4_454 ? C17 C16 C29 113.9(7) . 4_454 ? C18 C17 C16 112.5(8) . . ? N2 C18 C17 110.7(7) . . ? C14 C15 C16 113.0(7) . . ? N6 C11 C10 110.2(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.004 _refine_diff_density_min -1.688 _refine_diff_density_rms 0.325 # Attachment '- Zn2(L)(H2O)2.cif' data_jl2_136 _database_code_depnum_ccdc_archive 'CCDC 849785' #TrackingRef '- Zn2(L)(H2O)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H13 N O4 P Zn' _chemical_formula_weight 259.51 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' Zn Zn 0.2839 1.4301 '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 8.9542(4) _cell_length_b 9.4374(4) _cell_length_c 21.4718(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1814.46(14) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3572 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.71 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8700 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details 'SADABS 2008/1 Bruker AXS Madison WI USA' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 APEXII CCD Area Diffractometer' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28587 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2074 _reflns_number_gt 1694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.34a' _computing_data_reduction 'Bruker SAINT v7.34a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed geometrically, and were constrained and refined using a riding model. Hydrogen atoms could neither be placed nor found for the solvent water molecule and were therefore omitted from the refinement. ; _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^)+(0.0637P)^2^+1.8907P] 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 2074 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _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 Zn1 Zn 0.09138(5) 0.88230(5) 0.29869(2) 0.01311(17) Uani 1 1 d . . . P1 P 0.13402(12) 0.57700(11) 0.28157(5) 0.0134(2) Uani 1 1 d . . . O1 O 0.1611(3) 0.7196(3) 0.25038(13) 0.0186(6) Uani 1 1 d . . . O3 O -0.0843(3) 0.9647(3) 0.26348(13) 0.0181(6) Uani 1 1 d . . . O2 O 0.2289(3) 1.0300(3) 0.31839(14) 0.0212(7) Uani 1 1 d . . . N1 N 0.0070(4) 0.7510(3) 0.36943(15) 0.0125(7) Uani 1 1 d . . . C4 C -0.1232(4) 0.9388(4) 0.42967(19) 0.0170(8) Uani 1 1 d . . . H4A H -0.2220 0.9660 0.4465 0.020 Uiso 1 1 calc R . . H4B H -0.0908 1.0144 0.4007 0.020 Uiso 1 1 calc R . . C2 C 0.1349(5) 0.8694(4) 0.45742(19) 0.0171(9) Uani 1 1 d . . . H2A H 0.1803 0.9400 0.4290 0.021 Uiso 1 1 calc R . . H2B H 0.2056 0.8530 0.4921 0.021 Uiso 1 1 calc R . . C6 C -0.0150(4) 0.6119(4) 0.3362(2) 0.0154(8) Uani 1 1 d . . . H6A H -0.1115 0.6137 0.3137 0.019 Uiso 1 1 calc R . . H6B H -0.0193 0.5344 0.3672 0.019 Uiso 1 1 calc R . . C3 C -0.0112(4) 0.9294(4) 0.48354(18) 0.0150(8) Uani 1 1 d . . . H3 H -0.0510 0.8602 0.5147 0.018 Uiso 1 1 calc R . . C5 C -0.1394(4) 0.8015(4) 0.39362(19) 0.0152(8) Uani 1 1 d . . . H5A H -0.1829 0.7281 0.4211 0.018 Uiso 1 1 calc R . . H5B H -0.2088 0.8163 0.3583 0.018 Uiso 1 1 calc R . . C1 C 0.1116(4) 0.7320(4) 0.4225(2) 0.0166(9) Uani 1 1 d . . . H1A H 0.2088 0.6973 0.4067 0.020 Uiso 1 1 calc R . . H1B H 0.0710 0.6597 0.4513 0.020 Uiso 1 1 calc R . . O1W O -0.0165(6) 0.7508(5) 0.1374(2) 0.0651(14) 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 Zn1 0.0139(3) 0.0117(3) 0.0137(3) 0.00029(17) -0.00007(18) -0.00086(16) P1 0.0130(5) 0.0125(5) 0.0146(5) -0.0034(4) -0.0008(4) 0.0008(4) O1 0.0231(15) 0.0157(14) 0.0171(15) -0.0005(12) 0.0085(13) 0.0002(12) O3 0.0181(15) 0.0188(14) 0.0173(16) 0.0081(12) -0.0018(12) -0.0006(12) O2 0.0186(15) 0.0244(16) 0.0206(15) -0.0082(13) 0.0061(13) -0.0073(13) N1 0.0153(16) 0.0117(16) 0.0105(16) -0.0012(12) 0.0006(13) 0.0009(13) C4 0.0140(19) 0.019(2) 0.017(2) -0.0047(17) 0.0006(16) 0.0033(16) C2 0.017(2) 0.019(2) 0.015(2) -0.0025(16) -0.0051(16) 0.0057(16) C6 0.016(2) 0.013(2) 0.018(2) -0.0041(16) 0.0019(16) -0.0032(15) C3 0.019(2) 0.0140(19) 0.012(2) -0.0018(16) -0.0021(16) 0.0034(16) C5 0.0123(18) 0.019(2) 0.014(2) -0.0033(16) 0.0022(16) -0.0004(15) C1 0.018(2) 0.018(2) 0.014(2) 0.0014(16) -0.0027(16) 0.0047(16) O1W 0.071(3) 0.064(3) 0.060(3) -0.004(2) -0.003(3) 0.003(3) _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 Zn1 O2 1.907(3) . ? Zn1 O3 1.911(3) . ? Zn1 O1 1.955(3) . ? Zn1 N1 2.101(3) . ? P1 O3 1.502(3) 3_545 ? P1 O1 1.522(3) . ? P1 O2 1.526(3) 8_655 ? P1 C6 1.807(4) . ? N1 C1 1.486(5) . ? N1 C5 1.488(5) . ? N1 C6 1.506(5) . ? C4 C5 1.516(6) . ? C4 C3 1.534(5) . ? C2 C1 1.513(5) . ? C2 C3 1.532(5) . ? C3 C3 1.521(8) 5_576 ? 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 Zn1 O3 108.77(13) . . ? O2 Zn1 O1 119.05(12) . . ? O3 Zn1 O1 111.88(13) . . ? O2 Zn1 N1 120.20(13) . . ? O3 Zn1 N1 103.29(12) . . ? O1 Zn1 N1 92.01(12) . . ? O2 Zn1 P1 131.49(10) . . ? O3 Zn1 P1 117.26(10) . . ? O1 Zn1 P1 28.30(8) . . ? N1 Zn1 P1 63.73(9) . . ? O3 P1 O1 112.78(17) 3_545 . ? O3 P1 O2 111.52(16) 3_545 8_655 ? O1 P1 O2 110.90(18) . 8_655 ? O3 P1 C6 109.15(17) 3_545 . ? O1 P1 C6 104.00(17) . . ? O2 P1 C6 108.10(19) 8_655 . ? O3 P1 Zn1 137.39(13) 3_545 . ? O2 P1 Zn1 109.01(12) 8_655 . ? C6 P1 Zn1 69.08(12) . . ? P1 O1 Zn1 114.20(16) . . ? P1 O3 Zn1 141.78(18) 3 . ? P1 O2 Zn1 128.08(18) 8_665 . ? C1 N1 C5 109.0(3) . . ? C1 N1 C6 109.9(3) . . ? C5 N1 C6 109.2(3) . . ? C1 N1 Zn1 113.5(2) . . ? C5 N1 Zn1 112.3(2) . . ? C6 N1 Zn1 102.6(2) . . ? C5 C4 C3 113.5(3) . . ? C1 C2 C3 112.4(3) . . ? N1 C6 P1 111.7(3) . . ? C3 C3 C2 112.4(4) 5_576 . ? C3 C3 C4 112.7(4) 5_576 . ? C2 C3 C4 107.7(3) . . ? N1 C5 C4 111.6(3) . . ? N1 C1 C2 111.3(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.796 _refine_diff_density_min -1.139 _refine_diff_density_rms 0.278 _publ_section_references ; Bruker (2008). SAINTP+ for NT. Data Reduction and Correction Program v. 7.34, Bruker AXS, Madison, Wisconsin, USA. Bruker (2008). APEX2 software package. Bruker Molecular Analysis Research Tool, v. 1.27. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2003). SADABS v.2.03, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. ;