# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1955 data_ccd254b _publ_section_title ; First Single-Crystal X-ray Diffraction Study of a Lanthanide Tricarbonate Complex: [Co(NH~3~)~6~][Sm(CO~3~)3(H~2~O)]^.^4H~2~O ; _publ_requested_journal 'JCS Dalton Transactions' _publ_contact_author ; John G. Watkin CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _publ_contact_author_email 'jwatkin@lanl.gov' loop_ _publ_author_name _publ_author_address ; David L. Clark NMT-DO MS E500 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; ; Robert J. Donohoe B-2 MS J586 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; ; John C. Gordon CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; ; Pamela L. Gordon CST-18 MS G739 Los Alamos National Laboratory Los Alamos, NM 87545 ; ; D. Webster Keogh CST-18 MS G739 Los Alamos National Laboratory Los Alamos, NM 87545 ; ; Brian L. Scott CST-18 J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; ; C. Drew Tait CST-18 MS G739 Los Alamos National Laboratory Los Alamos, NM 87545 ; ; John G. Watkin CST-18 MS J514 Los Alamos National Laboratory Los Alamos, NM 87545 USA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cobalt(III)hexamine[aquo(samariumtricarbonato)]tetraaquosolvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H28 Co N6 O14 Sm' _chemical_formula_weight 581.59 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.895(2) _cell_length_b 6.7568(6) _cell_length_c 14.5776(14) _cell_angle_alpha 90.00 _cell_angle_beta 125.668(2) _cell_angle_gamma 90.00 _cell_volume 1752.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_crystal_preparation 'crystallized from water' _exptl_absorpt_coefficient_mu 4.346 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 1336 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.31 _reflns_number_total 1336 _reflns_number_gt 1234 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^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 1336 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Sm1 Sm 0.19147(2) 0.5000 0.41397(4) 0.0107(3) Uani 1 2 d S . . Co1 Co 0.5000 0.5000 1.0000 0.0154(5) Uani 1 4 d S . . Co2 Co 0.0000 0.0000 0.5000 0.0272(6) Uani 1 4 d S . . C1 C 0.0322(8) 0.553(2) 0.2604(12) 0.028(7) Uani 0.50 1 d P . . C2 C 0.3562(6) 0.5000 0.6018(8) 0.015(2) Uani 1 2 d S . . C3 C 0.2400(11) 0.559(3) 0.2685(14) 0.017(6) Uani 0.50 1 d P . . O1 O 0.0641(4) 0.5000 0.3652(6) 0.0296(19) Uani 1 2 d S . . O2 O 0.0744(5) 0.5000 0.2240(8) 0.095(5) Uani 1 2 d S . . O3 O -0.0368(6) 1.591(2) 0.1957(9) 0.061(5) Uani 0.50 1 d P . . O4 O 0.0765(4) 0.0000 0.3171(6) 0.0273(18) Uani 1 2 d S . . O5 O 0.1826(3) 0.1587(8) 0.4481(5) 0.0312(14) Uani 1 1 d . . . O6 O 0.2491(9) 0.394(3) 0.3194(13) 0.028(3) Uani 0.50 1 d P . . O6' O 0.2062(6) 0.3017(15) 0.2819(8) 0.015(2) Uani 0.50 1 d P . . O7 O 0.2646(7) 0.5797(15) 0.2079(9) 0.031(3) Uani 0.50 1 d P . . N1 N 0.4582(7) 0.5000 1.0868(9) 0.118(9) Uani 1 2 d S . . N2 N 0.5349(12) 0.758(3) 1.056(3) 0.20(2) Uani 0.50 1 d P . . N3 N 0.5995(8) 0.586(2) 1.1276(12) 0.047(5) Uani 0.50 1 d P . . N4 N -0.0704(3) -0.2091(12) 0.4781(5) 0.0346(18) Uani 1 1 d . . . N5 N -0.0507(5) 0.0000 0.3321(8) 0.040(3) Uani 1 2 d S . . O1W O 0.2069(4) 0.5000 0.6027(6) 0.0195(16) Uani 1 2 d S . . O2W O -0.0962(5) 0.5000 0.3065(7) 0.041(2) Uani 1 2 d S . . O3W O 0.2924(7) 0.384(2) 0.9458(10) 0.047(3) Uani 0.50 1 d P . . O4W O 0.6086(10) 1.0000 1.0252(16) 0.059(6) Uani 0.50 2 d SP . . O5W O 0.2829(7) 0.249(2) 0.1234(11) 0.046(3) Uani 0.50 1 d P . . O6W O 0.6185(16) 0.838(7) 0.954(4) 0.12(2) Uani 0.25 1 d P . . 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 Sm1 0.0143(4) 0.0060(4) 0.0122(3) 0.000 0.0079(3) 0.000 Co1 0.0199(10) 0.0131(12) 0.0082(9) 0.000 0.0053(9) 0.000 Co2 0.0158(11) 0.0531(16) 0.0150(11) 0.000 0.0102(9) 0.000 C1 0.020(7) 0.04(2) 0.021(8) -0.003(7) 0.009(6) 0.002(7) C2 0.033(7) 0.006(6) 0.025(6) 0.000 0.027(6) 0.000 C3 0.016(8) 0.02(2) 0.010(9) 0.004(7) 0.004(8) -0.001(6) O1 0.022(4) 0.055(6) 0.014(4) 0.000 0.012(4) 0.000 O2 0.023(5) 0.243(18) 0.025(5) 0.000 0.019(5) 0.000 O3 0.020(6) 0.125(15) 0.029(6) 0.018(7) 0.009(5) 0.031(7) O4 0.011(4) 0.035(5) 0.020(4) 0.000 0.000(4) 0.000 O5 0.021(3) 0.004(3) 0.050(4) 0.003(3) 0.011(3) -0.002(2) O6 0.039(9) 0.018(8) 0.039(10) 0.004(9) 0.029(9) 0.007(7) O6' 0.025(6) 0.007(6) 0.013(5) 0.003(4) 0.011(5) 0.003(5) O7 0.059(7) 0.017(6) 0.040(6) 0.005(5) 0.042(6) -0.005(5) N1 0.029(7) 0.30(3) 0.015(6) 0.000 0.010(6) 0.000 N2 0.046(11) 0.042(15) 0.35(5) -0.11(2) 0.03(2) 0.012(11) N3 0.030(7) 0.068(13) 0.035(8) -0.037(8) 0.015(7) -0.022(7) N4 0.017(3) 0.064(5) 0.025(3) -0.006(4) 0.013(3) -0.010(3) N5 0.031(6) 0.074(8) 0.019(5) 0.000 0.017(5) 0.000 O1W 0.024(4) 0.018(4) 0.019(4) 0.000 0.015(3) 0.000 O2W 0.036(5) 0.060(6) 0.040(5) 0.000 0.030(4) 0.000 O3W 0.060(8) 0.038(7) 0.039(7) -0.015(6) 0.027(7) -0.004(7) O4W 0.020(10) 0.11(2) 0.034(11) 0.000 0.008(9) 0.000 O5W 0.065(9) 0.028(7) 0.058(8) 0.007(6) 0.044(8) 0.008(7) O6W 0.024(15) 0.17(5) 0.12(3) 0.11(3) 0.011(19) -0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O5 2.391(5) 6_565 ? Sm1 O5 2.391(5) . ? Sm1 O2 2.442(9) . ? Sm1 O1 2.444(7) . ? Sm1 O6 2.457(14) 6_565 ? Sm1 O6 2.457(14) . ? Sm1 O5 2.516(5) 4_556 ? Sm1 O5 2.516(5) 7_556 ? Sm1 O6' 2.516(9) 6_565 ? Sm1 O6' 2.516(9) . ? Sm1 O1W 2.568(6) . ? Sm1 C1 2.863(14) . ? Co1 N2 1.89(2) . ? Co1 N2 1.89(2) 5_667 ? Co1 N2 1.888(19) 6_565 ? Co1 N2 1.888(19) 2_657 ? Co1 N1 1.946(12) . ? Co1 N1 1.946(12) 5_667 ? Co1 N3 1.955(13) . ? Co1 N3 1.955(13) 6_565 ? Co1 N3 1.955(13) 5_667 ? Co1 N3 1.955(13) 2_657 ? Co2 N4 1.976(7) 5_556 ? Co2 N4 1.976(7) . ? Co2 N4 1.976(7) 6 ? Co2 N4 1.976(7) 2_556 ? Co2 N5 2.014(9) . ? Co2 N5 2.014(9) 5_556 ? C1 C1 0.72(3) 6_565 ? C1 O3 1.255(18) 1_545 ? C1 O1 1.306(16) . ? C1 O2 1.357(17) . ? C1 O3 1.570(18) 6_575 ? C2 O4 1.239(13) 7_556 ? C2 O5 1.297(8) 7_556 ? C2 O5 1.297(8) 4_556 ? C3 O6 0.720(15) 6_565 ? C3 C3 0.79(4) 6_565 ? C3 O6' 1.28(2) 6_565 ? C3 O7 1.28(2) . ? C3 O6 1.287(19) . ? C3 O7 1.58(2) 6_565 ? O1 C1 1.306(16) 6_565 ? O2 C1 1.357(17) 6_565 ? O3 O3 1.23(3) 6_585 ? O3 C1 1.255(18) 1_565 ? O3 C1 1.570(19) 6_575 ? O4 C2 1.239(13) 7_556 ? O5 C2 1.297(8) 7_556 ? O5 Sm1 2.516(5) 7_556 ? O6 C3 0.720(15) 6_565 ? O6 O6' 0.986(16) . ? O6 O6 1.43(3) 6_565 ? O6' C3 1.28(2) 6_565 ? O7 O7 1.08(2) 6_565 ? O7 C3 1.58(2) 6_565 ? N2 N2 1.44(6) 2_657 ? N2 N3 1.65(3) . ? N3 N3 1.17(3) 6_565 ? O3W O3W 1.57(3) 6_565 ? O3W O5W 1.612(18) 7_556 ? O4W O6W 1.61(6) 6_575 ? O4W O6W 1.61(6) . ? O5W O3W 1.612(18) 7_556 ? 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 Sm1 O5 149.4(3) 6_565 . ? O5 Sm1 O2 94.42(14) 6_565 . ? O5 Sm1 O2 94.42(14) . . ? O5 Sm1 O1 80.98(13) 6_565 . ? O5 Sm1 O1 80.98(13) . . ? O2 Sm1 O1 53.5(3) . . ? O5 Sm1 O6 88.1(4) 6_565 6_565 ? O5 Sm1 O6 121.9(4) . 6_565 ? O2 Sm1 O6 84.6(4) . 6_565 ? O1 Sm1 O6 135.2(4) . 6_565 ? O5 Sm1 O6 121.9(4) 6_565 . ? O5 Sm1 O6 88.1(4) . . ? O2 Sm1 O6 84.6(4) . . ? O1 Sm1 O6 135.2(4) . . ? O6 Sm1 O6 33.9(8) 6_565 . ? O5 Sm1 O5 66.84(19) 6_565 4_556 ? O5 Sm1 O5 115.40(13) . 4_556 ? O2 Sm1 O5 147.45(19) . 4_556 ? O1 Sm1 O5 139.94(17) . 4_556 ? O6 Sm1 O5 69.0(4) 6_565 4_556 ? O6 Sm1 O5 83.7(4) . 4_556 ? O5 Sm1 O5 115.40(13) 6_565 7_556 ? O5 Sm1 O5 66.84(19) . 7_556 ? O2 Sm1 O5 147.45(19) . 7_556 ? O1 Sm1 O5 139.94(17) . 7_556 ? O6 Sm1 O5 83.7(4) 6_565 7_556 ? O6 Sm1 O5 69.0(4) . 7_556 ? O5 Sm1 O5 50.5(2) 4_556 7_556 ? O5 Sm1 O6' 73.0(3) 6_565 6_565 ? O5 Sm1 O6' 137.3(3) . 6_565 ? O2 Sm1 O6' 69.5(3) . 6_565 ? O1 Sm1 O6' 114.3(3) . 6_565 ? O6 Sm1 O6' 22.8(4) 6_565 6_565 ? O6 Sm1 O6' 52.3(5) . 6_565 ? O5 Sm1 O6' 79.3(3) 4_556 6_565 ? O5 Sm1 O6' 105.6(3) 7_556 6_565 ? O5 Sm1 O6' 137.3(3) 6_565 . ? O5 Sm1 O6' 73.0(3) . . ? O2 Sm1 O6' 69.5(3) . . ? O1 Sm1 O6' 114.3(3) . . ? O6 Sm1 O6' 52.3(5) 6_565 . ? O6 Sm1 O6' 22.8(4) . . ? O5 Sm1 O6' 105.6(3) 4_556 . ? O5 Sm1 O6' 79.3(3) 7_556 . ? O6' Sm1 O6' 64.4(5) 6_565 . ? O5 Sm1 O1W 75.72(15) 6_565 . ? O5 Sm1 O1W 75.72(15) . . ? O2 Sm1 O1W 127.6(3) . . ? O1 Sm1 O1W 74.1(2) . . ? O6 Sm1 O1W 144.2(4) 6_565 . ? O6 Sm1 O1W 144.2(4) . . ? O5 Sm1 O1W 75.2(2) 4_556 . ? O5 Sm1 O1W 75.2(2) 7_556 . ? O6' Sm1 O1W 145.5(2) 6_565 . ? O6' Sm1 O1W 145.5(2) . . ? O5 Sm1 C1 80.3(3) 6_565 . ? O5 Sm1 C1 94.3(3) . . ? O2 Sm1 C1 28.2(3) . . ? O1 Sm1 C1 27.0(3) . . ? O6 Sm1 C1 108.4(5) 6_565 . ? O6 Sm1 C1 112.9(5) . . ? O5 Sm1 C1 147.0(3) 4_556 . ? O5 Sm1 C1 161.1(3) 7_556 . ? O6' Sm1 C1 88.6(4) 6_565 . ? O6' Sm1 C1 96.3(4) . . ? O1W Sm1 C1 100.2(3) . . ? N2 Co1 N2 180.000(3) . 5_667 ? N2 Co1 N2 135(2) . 6_565 ? N2 Co1 N2 44.9(19) 5_667 6_565 ? N2 Co1 N2 44.9(19) . 2_657 ? N2 Co1 N2 135(2) 5_667 2_657 ? N2 Co1 N2 180.000(9) 6_565 2_657 ? N2 Co1 N1 86.9(13) . . ? N2 Co1 N1 93.1(13) 5_667 . ? N2 Co1 N1 86.9(13) 6_565 . ? N2 Co1 N1 93.1(13) 2_657 . ? N2 Co1 N1 93.1(13) . 5_667 ? N2 Co1 N1 86.9(13) 5_667 5_667 ? N2 Co1 N1 93.1(13) 6_565 5_667 ? N2 Co1 N1 86.9(13) 2_657 5_667 ? N1 Co1 N1 180.000(3) . 5_667 ? N2 Co1 N3 50.8(9) . . ? N2 Co1 N3 129.2(9) 5_667 . ? N2 Co1 N3 85.4(10) 6_565 . ? N2 Co1 N3 94.6(10) 2_657 . ? N1 Co1 N3 93.8(5) . . ? N1 Co1 N3 86.2(5) 5_667 . ? N2 Co1 N3 85.4(10) . 6_565 ? N2 Co1 N3 94.6(10) 5_667 6_565 ? N2 Co1 N3 50.8(9) 6_565 6_565 ? N2 Co1 N3 129.2(9) 2_657 6_565 ? N1 Co1 N3 93.8(5) . 6_565 ? N1 Co1 N3 86.2(5) 5_667 6_565 ? N3 Co1 N3 34.7(10) . 6_565 ? N2 Co1 N3 129.2(9) . 5_667 ? N2 Co1 N3 50.8(9) 5_667 5_667 ? N2 Co1 N3 94.6(10) 6_565 5_667 ? N2 Co1 N3 85.4(10) 2_657 5_667 ? N1 Co1 N3 86.2(5) . 5_667 ? N1 Co1 N3 93.8(5) 5_667 5_667 ? N3 Co1 N3 180.0(8) . 5_667 ? N3 Co1 N3 145.3(10) 6_565 5_667 ? N2 Co1 N3 94.6(10) . 2_657 ? N2 Co1 N3 85.4(10) 5_667 2_657 ? N2 Co1 N3 129.2(9) 6_565 2_657 ? N2 Co1 N3 50.8(9) 2_657 2_657 ? N1 Co1 N3 86.2(5) . 2_657 ? N1 Co1 N3 93.8(5) 5_667 2_657 ? N3 Co1 N3 145.3(10) . 2_657 ? N3 Co1 N3 180.000(7) 6_565 2_657 ? N3 Co1 N3 34.7(10) 5_667 2_657 ? N4 Co2 N4 180.0(3) 5_556 . ? N4 Co2 N4 88.7(4) 5_556 6 ? N4 Co2 N4 91.3(4) . 6 ? N4 Co2 N4 91.3(4) 5_556 2_556 ? N4 Co2 N4 88.7(4) . 2_556 ? N4 Co2 N4 180.0(4) 6 2_556 ? N4 Co2 N5 91.2(3) 5_556 . ? N4 Co2 N5 88.8(3) . . ? N4 Co2 N5 88.8(3) 6 . ? N4 Co2 N5 91.2(3) 2_556 . ? N4 Co2 N5 88.8(3) 5_556 5_556 ? N4 Co2 N5 91.2(3) . 5_556 ? N4 Co2 N5 91.2(3) 6 5_556 ? N4 Co2 N5 88.8(3) 2_556 5_556 ? N5 Co2 N5 180.000(1) . 5_556 ? C1 C1 O3 101.8(11) 6_565 1_545 ? C1 C1 O1 74.0(7) 6_565 . ? O3 C1 O1 121.6(13) 1_545 . ? C1 C1 O2 74.6(7) 6_565 . ? O3 C1 O2 123.7(13) 1_545 . ? O1 C1 O2 111.3(11) . . ? C1 C1 O3 51.5(8) 6_565 6_575 ? O3 C1 O3 50.3(14) 1_545 6_575 ? O1 C1 O3 101.6(11) . 6_575 ? O2 C1 O3 103.6(11) . 6_575 ? C1 C1 Sm1 82.8(3) 6_565 . ? O3 C1 Sm1 175.3(13) 1_545 . ? O1 C1 Sm1 58.3(6) . . ? O2 C1 Sm1 58.3(7) . . ? O3 C1 Sm1 134.2(10) 6_575 . ? O4 C2 O5 124.1(5) 7_556 7_556 ? O4 C2 O5 124.1(5) 7_556 4_556 ? O5 C2 O5 111.6(9) 7_556 4_556 ? O4 C2 Sm1 177.1(7) 7_556 . ? O5 C2 Sm1 56.0(4) 7_556 . ? O5 C2 Sm1 56.0(5) 4_556 . ? O6 C3 C3 116(2) 6_565 6_565 ? O6 C3 O6' 50(2) 6_565 6_565 ? C3 C3 O6' 137.4(9) 6_565 6_565 ? O6 C3 O7 133(3) 6_565 . ? C3 C3 O7 96.3(10) 6_565 . ? O6' C3 O7 122.4(15) 6_565 . ? O6 C3 O6 86(3) 6_565 . ? C3 C3 O6 30.1(8) 6_565 . ? O6' C3 O6 117.3(16) 6_565 . ? O7 C3 O6 120.3(16) . . ? O6 C3 O7 149(3) 6_565 6_565 ? C3 C3 O7 53.7(8) 6_565 6_565 ? O6' C3 O7 159.3(15) 6_565 6_565 ? O7 C3 O7 42.6(10) . 6_565 ? O6 C3 O7 79.7(10) . 6_565 ? O6 C3 Sm1 46(2) 6_565 . ? C3 C3 Sm1 82.1(4) 6_565 . ? O6' C3 Sm1 60.0(8) 6_565 . ? O7 C3 Sm1 177.0(13) . . ? O6 C3 Sm1 57.4(10) . . ? O7 C3 Sm1 135.8(10) 6_565 . ? C1 O1 C1 32.1(14) 6_565 . ? C1 O1 Sm1 94.7(7) 6_565 . ? C1 O1 Sm1 94.7(7) . . ? C1 O2 C1 30.8(14) . 6_565 ? C1 O2 Sm1 93.4(7) . . ? C1 O2 Sm1 93.4(7) 6_565 . ? O3 O3 C1 78.2(11) 6_585 1_565 ? O3 O3 C1 51.5(8) 6_585 6_575 ? C1 O3 C1 26.7(12) 1_565 6_575 ? C2 O5 Sm1 141.9(5) 7_556 . ? C2 O5 Sm1 98.7(5) 7_556 7_556 ? Sm1 O5 Sm1 113.16(19) . 7_556 ? C3 O6 O6' 96(3) 6_565 . ? C3 O6 C3 34(2) 6_565 . ? O6' O6 C3 116.7(19) . . ? C3 O6 O6 64(2) 6_565 6_565 ? O6' O6 O6 129.3(11) . 6_565 ? C3 O6 O6 30.1(8) . 6_565 ? C3 O6 Sm1 122(3) 6_565 . ? O6' O6 Sm1 82.0(10) . . ? C3 O6 Sm1 96.5(12) . . ? O6 O6 Sm1 73.0(4) 6_565 . ? O6 O6' C3 34.0(10) . 6_565 ? O6 O6' Sm1 75.2(11) . . ? C3 O6' Sm1 93.9(9) 6_565 . ? O7 O7 C3 83.7(10) 6_565 . ? O7 O7 C3 53.7(8) 6_565 6_565 ? C3 O7 C3 30.0(14) . 6_565 ? N2 N2 N3 132.0(18) 2_657 . ? N2 N2 Co1 67.6(10) 2_657 . ? N3 N2 Co1 66.7(8) . . ? N3 N3 N2 134.8(9) 6_565 . ? N3 N3 Co1 72.6(5) 6_565 . ? N2 N3 Co1 62.5(9) . . ? O3W O3W O5W 123.8(7) 6_565 7_556 ? O6W O4W O6W 86(2) 6_575 . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.304 _refine_diff_density_min -1.700 _refine_diff_density_rms 0.189