# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'PARTHASARATHI Dastidar' _publ_contact_author_email PARTHOD123@REDIFFMAIL.COM _publ_section_title ; Metal-organic frameworks derived from bis-pyridyl-bis-amide ligands: Effect of positional isomerism of the ligands, hydrogen bonding backbone, counter anions on the supramolecular structures and selective uptake of sulfate anion ; loop_ _publ_author_name 'PARTHASARATHI Dastidar' 'N N Adarsh' 'D. Krishna Kumar' # Attachment 'L1_an0106m_FINAL.cif' data_an0106m _database_code_depnum_ccdc_archive 'CCDC 694503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 N4 O2' _chemical_formula_weight 318.33 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' _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 12.664(4) _cell_length_b 8.986(3) _cell_length_c 14.687(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.762(5) _cell_angle_gamma 90.00 _cell_volume 1517.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9685 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7746 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2942 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0571P)^2^+0.1747P] 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 2942 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 N1 N -0.21098(12) 0.93954(15) -0.21219(10) 0.0524(4) Uani 1 1 d . . . C2 C -0.22870(14) 0.8914(2) -0.13449(14) 0.0567(5) Uani 1 1 d . . . H2 H -0.3037 0.8990 -0.1385 0.068 Uiso 1 1 calc R . . C3 C -0.14514(13) 0.8310(2) -0.04838(12) 0.0527(4) Uani 1 1 d . . . H3 H -0.1637 0.7997 0.0035 0.063 Uiso 1 1 calc R . . C4 C -0.03298(12) 0.81791(16) -0.04080(11) 0.0405(3) Uani 1 1 d . . . C5 C -0.01122(13) 0.87079(17) -0.11984(11) 0.0445(4) Uani 1 1 d . . . H5 H 0.0634 0.8668 -0.1172 0.053 Uiso 1 1 calc R . . C6 C -0.10161(14) 0.92933(18) -0.20247(12) 0.0509(4) Uani 1 1 d . . . H6 H -0.0854 0.9640 -0.2549 0.061 Uiso 1 1 calc R . . N7 N 0.05841(11) 0.75810(15) 0.04345(9) 0.0441(3) Uani 1 1 d . . . C8 C 0.04555(14) 0.65731(19) 0.10781(12) 0.0498(4) Uani 1 1 d . . . O9 O -0.04847(11) 0.60716(18) 0.09553(10) 0.0817(5) Uani 1 1 d . . . C10 C 0.15231(13) 0.61129(17) 0.19619(11) 0.0436(4) Uani 1 1 d . . . C11 C 0.15112(14) 0.47404(18) 0.23935(12) 0.0506(4) Uani 1 1 d . . . H11 H 0.0864 0.4126 0.2109 0.061 Uiso 1 1 calc R . . C12 C 0.24531(15) 0.42875(19) 0.32388(12) 0.0538(4) Uani 1 1 d . . . H12 H 0.2441 0.3367 0.3524 0.065 Uiso 1 1 calc R . . C13 C 0.34131(14) 0.51919(18) 0.36631(12) 0.0495(4) Uani 1 1 d . . . H13 H 0.4050 0.4878 0.4233 0.059 Uiso 1 1 calc R . . C14 C 0.34364(13) 0.65743(17) 0.32442(11) 0.0417(4) Uani 1 1 d . . . C15 C 0.24856(13) 0.70238(17) 0.23910(11) 0.0421(4) Uani 1 1 d . . . H15 H 0.2495 0.7944 0.2105 0.051 Uiso 1 1 calc R . . C16 C 0.45163(13) 0.74817(18) 0.37296(11) 0.0443(4) Uani 1 1 d . . . O17 O 0.54398(10) 0.68818(14) 0.42412(9) 0.0616(4) Uani 1 1 d . . . N18 N 0.44073(11) 0.89848(15) 0.35647(9) 0.0450(3) Uani 1 1 d . . . C19 C 0.52982(12) 1.00467(18) 0.39328(11) 0.0418(4) Uani 1 1 d . . . C20 C 0.64438(14) 0.9730(2) 0.45527(13) 0.0552(4) Uani 1 1 d . . . H20 H 0.6675 0.8762 0.4768 0.066 Uiso 1 1 calc R . . C21 C 0.72358(14) 1.0877(2) 0.48452(13) 0.0603(5) Uani 1 1 d . . . H21 H 0.8000 1.0638 0.5267 0.072 Uiso 1 1 calc R . . N22 N 0.70072(11) 1.22895(17) 0.45796(10) 0.0537(4) Uani 1 1 d . . . C23 C 0.58932(14) 1.2579(2) 0.40022(13) 0.0539(4) Uani 1 1 d . . . H23 H 0.5687 1.3562 0.3813 0.065 Uiso 1 1 calc R . . C24 C 0.50310(13) 1.15297(18) 0.36678(12) 0.0490(4) Uani 1 1 d . . . H24 H 0.4269 1.1808 0.3265 0.059 Uiso 1 1 calc R . . H7 H 0.1289(15) 0.767(2) 0.0473(12) 0.054(5) Uiso 1 1 d . . . H18 H 0.3694(15) 0.9349(19) 0.3212(12) 0.050(5) 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 N1 0.0431(8) 0.0454(8) 0.0554(8) 0.0040(7) 0.0075(6) -0.0001(6) C2 0.0358(9) 0.0589(11) 0.0685(11) 0.0017(9) 0.0150(8) 0.0017(7) C3 0.0415(9) 0.0629(11) 0.0523(9) 0.0031(8) 0.0183(8) -0.0011(8) C4 0.0350(8) 0.0379(8) 0.0416(8) -0.0046(6) 0.0091(6) -0.0035(6) C5 0.0367(8) 0.0449(9) 0.0487(8) -0.0006(7) 0.0148(7) -0.0006(6) C6 0.0508(10) 0.0470(9) 0.0487(9) 0.0038(7) 0.0146(7) -0.0008(7) N7 0.0340(7) 0.0487(8) 0.0439(7) 0.0044(6) 0.0106(6) -0.0017(6) C8 0.0443(9) 0.0512(10) 0.0464(9) -0.0001(7) 0.0116(7) -0.0114(7) O9 0.0498(8) 0.1032(12) 0.0721(9) 0.0288(8) 0.0057(6) -0.0272(7) C10 0.0444(9) 0.0416(8) 0.0409(8) 0.0001(7) 0.0142(7) -0.0023(6) C11 0.0546(10) 0.0407(9) 0.0541(9) -0.0034(7) 0.0203(8) -0.0072(7) C12 0.0669(11) 0.0363(8) 0.0570(10) 0.0088(7) 0.0248(9) 0.0028(7) C13 0.0527(10) 0.0436(9) 0.0441(8) 0.0058(7) 0.0122(7) 0.0072(7) C14 0.0432(8) 0.0397(8) 0.0386(7) 0.0005(6) 0.0134(7) 0.0041(6) C15 0.0449(8) 0.0365(8) 0.0405(8) 0.0035(6) 0.0135(7) -0.0005(6) C16 0.0417(8) 0.0484(9) 0.0372(7) 0.0045(7) 0.0111(7) 0.0046(7) O17 0.0427(7) 0.0559(7) 0.0685(8) 0.0155(6) 0.0060(6) 0.0085(5) N18 0.0344(7) 0.0436(8) 0.0463(7) 0.0014(6) 0.0063(6) 0.0033(6) C19 0.0340(8) 0.0489(9) 0.0387(8) -0.0024(7) 0.0115(6) -0.0001(6) C20 0.0382(9) 0.0533(10) 0.0623(10) 0.0094(8) 0.0093(8) 0.0038(7) C21 0.0331(9) 0.0698(13) 0.0639(11) 0.0072(9) 0.0063(8) 0.0008(8) N22 0.0396(8) 0.0569(9) 0.0579(8) -0.0041(7) 0.0138(6) -0.0028(6) C23 0.0443(9) 0.0498(10) 0.0621(10) -0.0045(8) 0.0168(8) 0.0006(7) C24 0.0346(8) 0.0485(9) 0.0535(9) -0.0009(7) 0.0083(7) 0.0044(7) _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 N1 C2 1.325(2) . ? N1 C6 1.335(2) . ? C2 C3 1.376(2) . ? C2 H2 0.9300 . ? C3 C4 1.383(2) . ? C3 H3 0.9300 . ? C4 C5 1.385(2) . ? C4 N7 1.3999(19) . ? C5 C6 1.377(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.367(2) . ? N7 H7 0.875(18) . ? C8 O9 1.2138(19) . ? C8 C10 1.488(2) . ? C10 C15 1.382(2) . ? C10 C11 1.390(2) . ? C11 C12 1.374(2) . ? C11 H11 0.9300 . ? C12 C13 1.376(2) . ? C12 H12 0.9300 . ? C13 C14 1.392(2) . ? C13 H13 0.9300 . ? C14 C15 1.386(2) . ? C14 C16 1.492(2) . ? C15 H15 0.9300 . ? C16 O17 1.2193(17) . ? C16 N18 1.369(2) . ? N18 C19 1.402(2) . ? N18 H18 0.894(17) . ? C19 C20 1.381(2) . ? C19 C24 1.390(2) . ? C20 C21 1.375(2) . ? C20 H20 0.9300 . ? C21 N22 1.324(2) . ? C21 H21 0.9300 . ? N22 C23 1.332(2) . ? C23 C24 1.369(2) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? 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 C2 N1 C6 115.35(14) . . ? N1 C2 C3 125.33(16) . . ? N1 C2 H2 117.3 . . ? C3 C2 H2 117.3 . . ? C2 C3 C4 118.44(16) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 117.51(14) . . ? C3 C4 N7 123.02(14) . . ? C5 C4 N7 119.45(14) . . ? C6 C5 C4 119.09(15) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N1 C6 C5 124.25(16) . . ? N1 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? C8 N7 C4 124.87(14) . . ? C8 N7 H7 115.4(11) . . ? C4 N7 H7 117.8(11) . . ? O9 C8 N7 122.45(15) . . ? O9 C8 C10 120.20(15) . . ? N7 C8 C10 117.35(14) . . ? C15 C10 C11 119.58(14) . . ? C15 C10 C8 122.61(14) . . ? C11 C10 C8 117.72(14) . . ? C12 C11 C10 120.25(15) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.15(15) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 120.35(14) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 119.25(14) . . ? C15 C14 C16 123.25(14) . . ? C13 C14 C16 117.47(13) . . ? C10 C15 C14 120.42(14) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O17 C16 N18 123.01(15) . . ? O17 C16 C14 120.23(15) . . ? N18 C16 C14 116.76(13) . . ? C16 N18 C19 126.74(13) . . ? C16 N18 H18 117.8(11) . . ? C19 N18 H18 115.4(11) . . ? C20 C19 C24 116.57(15) . . ? C20 C19 N18 124.58(15) . . ? C24 C19 N18 118.85(13) . . ? C21 C20 C19 118.62(16) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N22 C21 C20 125.83(16) . . ? N22 C21 H21 117.1 . . ? C20 C21 H21 117.1 . . ? C21 N22 C23 114.65(15) . . ? N22 C23 C24 124.55(17) . . ? N22 C23 H23 117.7 . . ? C24 C23 H23 117.7 . . ? C23 C24 C19 119.72(14) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 N22 0.875(18) 2.217(18) 3.070(2) 165.0(16) 2_645 N18 H18 N1 0.894(17) 2.274(18) 3.1480(19) 165.6(14) 3_575 C2 H2 O17 0.93 2.58 3.408(2) 148.4 4_475 C6 H6 O9 0.93 2.51 3.322(2) 145.6 4_575 C13 H13 O17 0.93 2.59 3.363(2) 140.4 3_666 C15 H15 N1 0.93 2.44 3.252(2) 145.7 3_575 C21 H21 O9 0.93 2.33 3.180(2) 151.5 4_676 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.192 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.035 # Attachment 'MOF 1_an0204fm_FINAL.cif' data_an0204fm _database_code_depnum_ccdc_archive 'CCDC 694504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Cl2 Co N8 O4' _chemical_formula_weight 766.49 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRIGONAL _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' '-x, -x+y, -z+2/3' 'x-y, -y, -z+1/3' _cell_length_a 14.4804(7) _cell_length_b 14.4804(7) _cell_length_c 18.9354(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3438.5(4) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour PINK _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1179 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8157 _exptl_absorpt_correction_T_max 0.9739 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17509 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.1625 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4956 _reflns_number_gt 2501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4.1' _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^)+(0.0621P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 4956 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.25588(7) 0.0000 0.1667 0.0411(3) Uani 1 2 d S . . Cl2 Cl 0.22341(12) -0.06194(11) 0.04059(6) 0.0480(3) Uani 1 1 d . . . N1 N 0.4220(4) 0.1176(4) 0.1458(2) 0.0525(12) Uani 1 1 d . . . C2 C 0.4527(4) 0.1825(4) 0.0881(3) 0.0485(13) Uani 1 1 d . . . H2 H 0.4005 0.1769 0.0570 0.058 Uiso 1 1 calc R . . C3 C 0.5539(4) 0.2534(4) 0.0744(3) 0.0444(13) Uani 1 1 d . . . H3 H 0.5708 0.2965 0.0346 0.053 Uiso 1 1 calc R . . C4 C 0.6342(4) 0.2636(4) 0.1186(3) 0.0441(13) Uani 1 1 d . . . C5 C 0.6051(4) 0.2009(5) 0.1784(3) 0.0482(14) Uani 1 1 d . . . H5 H 0.6565 0.2067 0.2103 0.058 Uiso 1 1 calc R . . C6 C 0.5001(5) 0.1304(5) 0.1902(3) 0.0555(15) Uani 1 1 d . . . H6 H 0.4814 0.0891 0.2309 0.067 Uiso 1 1 calc R . . N7 N 0.7452(3) 0.3318(4) 0.1075(2) 0.0494(12) Uani 1 1 d . . . H7 H 0.7874 0.3239 0.1356 0.059 Uiso 1 1 calc R . . C8 C 0.7919(4) 0.4086(4) 0.0569(3) 0.0453(13) Uani 1 1 d . . . O9 O 0.7427(3) 0.4283(4) 0.0149(2) 0.0702(13) Uani 1 1 d . . . C10 C 0.9108(4) 0.4690(4) 0.0570(3) 0.0416(12) Uani 1 1 d . . . C11 C 0.9624(5) 0.5719(4) 0.0344(3) 0.0534(15) Uani 1 1 d . . . H11 H 0.9240 0.6026 0.0168 0.064 Uiso 1 1 calc R . . C12 C 1.0732(5) 0.6309(4) 0.0377(3) 0.0591(16) Uani 1 1 d . . . H12 H 1.1075 0.7015 0.0226 0.071 Uiso 1 1 calc R . . C13 C 1.1325(5) 0.5905(5) 0.0617(3) 0.0567(16) Uani 1 1 d . . . H13 H 1.2063 0.6327 0.0648 0.068 Uiso 1 1 calc R . . C14 C 1.0809(4) 0.4825(4) 0.0820(3) 0.0430(13) Uani 1 1 d . . . C15 C 0.9711(5) 0.4250(4) 0.0804(3) 0.0471(13) Uani 1 1 d . . . H15 H 0.9364 0.3544 0.0954 0.057 Uiso 1 1 calc R . . C16 C 1.1474(5) 0.4390(5) 0.1062(3) 0.0545(14) Uani 1 1 d . . . O17 O 1.2334(4) 0.4889(4) 0.1366(3) 0.0920(16) Uani 1 1 d . . . N18 N 1.1048(3) 0.3302(3) 0.0896(2) 0.0462(12) Uani 1 1 d . . . H18 H 1.0475 0.3017 0.0647 0.055 Uiso 1 1 calc R . . C19 C 1.1433(4) 0.2634(4) 0.1085(3) 0.0449(13) Uani 1 1 d . . . C20 C 1.2316(5) 0.2915(5) 0.1507(3) 0.0594(16) Uani 1 1 d . . . H20 H 1.2720 0.3602 0.1686 0.071 Uiso 1 1 calc R . . C21 C 1.2578(5) 0.2133(5) 0.1654(3) 0.0555(15) Uani 1 1 d . . . H21 H 1.3169 0.2328 0.1940 0.067 Uiso 1 1 calc R . . N22 N 1.2063(3) 0.1136(3) 0.1423(2) 0.0437(11) Uani 1 1 d . . . C23 C 1.1238(4) 0.0886(5) 0.1007(3) 0.0532(15) Uani 1 1 d . . . H23 H 1.0865 0.0197 0.0828 0.064 Uiso 1 1 calc R . . C24 C 1.0889(5) 0.1605(5) 0.0821(3) 0.0560(15) Uani 1 1 d . . . H24 H 1.0303 0.1391 0.0526 0.067 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 0.0366(4) 0.0424(6) 0.0464(5) 0.0100(5) 0.0050(2) 0.0212(3) Cl2 0.0532(8) 0.0470(7) 0.0460(7) 0.0091(6) 0.0049(7) 0.0267(7) N1 0.048(3) 0.056(3) 0.051(2) 0.012(2) 0.007(2) 0.025(3) C2 0.037(3) 0.052(3) 0.048(3) 0.008(3) 0.003(3) 0.016(3) C3 0.039(3) 0.049(3) 0.037(3) 0.008(2) 0.009(2) 0.016(3) C4 0.050(3) 0.047(3) 0.040(3) -0.001(2) 0.005(3) 0.029(3) C5 0.035(3) 0.065(4) 0.050(3) 0.009(3) 0.006(2) 0.028(3) C6 0.048(3) 0.071(4) 0.048(3) 0.007(3) 0.005(3) 0.030(3) N7 0.038(3) 0.056(3) 0.049(3) 0.002(2) 0.003(2) 0.019(2) C8 0.044(3) 0.036(3) 0.057(3) 0.010(3) 0.007(3) 0.022(3) O9 0.049(3) 0.073(3) 0.083(3) 0.028(3) 0.001(2) 0.026(2) C10 0.045(3) 0.033(3) 0.046(3) 0.000(2) 0.008(2) 0.018(3) C11 0.052(4) 0.040(3) 0.077(4) 0.001(3) 0.017(3) 0.029(3) C12 0.062(4) 0.033(3) 0.082(4) 0.007(3) 0.019(4) 0.024(3) C13 0.045(3) 0.034(3) 0.084(4) 0.000(3) 0.013(3) 0.014(3) C14 0.039(3) 0.029(3) 0.054(3) -0.008(2) 0.000(2) 0.012(2) C15 0.059(4) 0.035(3) 0.048(3) 0.003(2) 0.015(3) 0.023(3) C16 0.048(3) 0.042(3) 0.065(4) -0.012(3) -0.004(3) 0.016(3) O17 0.071(3) 0.053(3) 0.147(4) -0.032(3) -0.052(3) 0.028(3) N18 0.035(2) 0.040(3) 0.059(3) -0.009(2) -0.013(2) 0.016(2) C19 0.046(3) 0.040(3) 0.056(3) 0.001(3) -0.010(3) 0.027(3) C20 0.061(4) 0.040(3) 0.074(4) -0.016(3) -0.023(3) 0.023(3) C21 0.051(4) 0.065(4) 0.048(3) 0.001(3) -0.021(3) 0.027(3) N22 0.037(2) 0.039(3) 0.053(3) 0.000(2) -0.004(2) 0.018(2) C23 0.046(4) 0.048(4) 0.062(3) -0.011(3) -0.011(3) 0.022(3) C24 0.064(4) 0.047(3) 0.061(3) -0.008(3) -0.019(3) 0.031(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 Co1 N22 2.148(4) 1_455 ? Co1 N22 2.148(4) 6_455 ? Co1 N1 2.178(5) . ? Co1 N1 2.178(5) 6 ? Co1 Cl2 2.5106(13) . ? Co1 Cl2 2.5106(13) 6 ? N1 C6 1.344(7) . ? N1 C2 1.363(7) . ? C2 C3 1.329(7) . ? C2 H2 0.9300 . ? C3 C4 1.379(7) . ? C3 H3 0.9300 . ? C4 C5 1.378(7) . ? C4 N7 1.419(7) . ? C5 C6 1.360(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.364(6) . ? N7 H7 0.8600 . ? C8 O9 1.194(6) . ? C8 C10 1.491(7) . ? C10 C11 1.360(7) . ? C10 C15 1.385(8) . ? C11 C12 1.392(8) . ? C11 H11 0.9300 . ? C12 C13 1.338(8) . ? C12 H12 0.9300 . ? C13 C14 1.408(8) . ? C13 H13 0.9300 . ? C14 C15 1.377(7) . ? C14 C16 1.463(8) . ? C15 H15 0.9300 . ? C16 O17 1.227(7) . ? C16 N18 1.411(7) . ? N18 C19 1.383(7) . ? N18 H18 0.8600 . ? C19 C24 1.385(8) . ? C19 C20 1.385(8) . ? C20 C21 1.390(8) . ? C20 H20 0.9300 . ? C21 N22 1.325(7) . ? C21 H21 0.9300 . ? N22 C23 1.322(7) . ? N22 Co1 2.148(4) 1_655 ? C23 C24 1.409(7) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? 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 N22 Co1 N22 88.4(2) 1_455 6_455 ? N22 Co1 N1 91.38(16) 1_455 . ? N22 Co1 N1 177.90(18) 6_455 . ? N22 Co1 N1 177.91(18) 1_455 6 ? N22 Co1 N1 91.38(16) 6_455 6 ? N1 Co1 N1 88.9(3) . 6 ? N22 Co1 Cl2 89.71(12) 1_455 . ? N22 Co1 Cl2 89.59(12) 6_455 . ? N1 Co1 Cl2 92.49(12) . . ? N1 Co1 Cl2 88.22(12) 6 . ? N22 Co1 Cl2 89.58(12) 1_455 6 ? N22 Co1 Cl2 89.70(12) 6_455 6 ? N1 Co1 Cl2 88.22(12) . 6 ? N1 Co1 Cl2 92.49(12) 6 6 ? Cl2 Co1 Cl2 179.01(8) . 6 ? C6 N1 C2 116.3(5) . . ? C6 N1 Co1 121.3(3) . . ? C2 N1 Co1 122.4(4) . . ? C3 C2 N1 122.8(5) . . ? C3 C2 H2 118.6 . . ? N1 C2 H2 118.6 . . ? C2 C3 C4 120.7(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 117.6(5) . . ? C5 C4 N7 116.6(5) . . ? C3 C4 N7 125.8(5) . . ? C6 C5 C4 119.2(5) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 123.3(5) . . ? N1 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? C8 N7 C4 126.8(5) . . ? C8 N7 H7 116.6 . . ? C4 N7 H7 116.6 . . ? O9 C8 N7 123.4(5) . . ? O9 C8 C10 120.9(5) . . ? N7 C8 C10 115.7(5) . . ? C11 C10 C15 118.5(5) . . ? C11 C10 C8 118.8(5) . . ? C15 C10 C8 122.7(5) . . ? C10 C11 C12 119.5(6) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 122.8(5) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C14 118.6(6) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 118.5(5) . . ? C15 C14 C16 123.8(5) . . ? C13 C14 C16 117.7(5) . . ? C14 C15 C10 122.1(5) . . ? C14 C15 H15 118.9 . . ? C10 C15 H15 118.9 . . ? O17 C16 N18 120.7(6) . . ? O17 C16 C14 125.9(5) . . ? N18 C16 C14 113.4(5) . . ? C19 N18 C16 128.3(4) . . ? C19 N18 H18 115.8 . . ? C16 N18 H18 115.8 . . ? N18 C19 C24 116.6(5) . . ? N18 C19 C20 125.4(5) . . ? C24 C19 C20 118.0(5) . . ? C19 C20 C21 117.6(5) . . ? C19 C20 H20 121.2 . . ? C21 C20 H20 121.2 . . ? N22 C21 C20 126.0(5) . . ? N22 C21 H21 117.0 . . ? C20 C21 H21 117.0 . . ? C23 N22 C21 115.7(5) . . ? C23 N22 Co1 121.4(4) . 1_655 ? C21 N22 Co1 122.8(4) . 1_655 ? N22 C23 C24 123.8(5) . . ? N22 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C19 C24 C23 118.9(5) . . ? C19 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N18 H18 Cl2 0.86 2.44 3.251(4) 156.5 4_655 _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.289 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.068 # Attachment 'MOF 2_AN0312UM_FINAL.cif' data_an0312um _database_code_depnum_ccdc_archive 'CCDC 694505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Cd N10 O10' _chemical_formula_weight 873.08 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' Cd Cd -0.8075 1.2024 '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' H H 0.0000 0.0000 '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 9.131(4) _cell_length_b 11.139(4) _cell_length_c 20.248(7) _cell_angle_alpha 89.912(7) _cell_angle_beta 85.131(9) _cell_angle_gamma 70.814(7) _cell_volume 1937.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8733 _exptl_absorpt_correction_T_max 0.9813 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10426 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.1608 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7415 _reflns_number_gt 3932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART' _computing_cell_refinement 'BRUKER AXS SMART' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'MERCURY 1.4.1' _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^)+(0.0870P)^2^+0.5000P] 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 7415 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1438 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _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 Cd1 Cd 0.57148(8) 0.47509(5) 0.22131(3) 0.0420(2) Uani 1 1 d . . . N1 N 0.4627(9) 0.6018(6) 0.1304(3) 0.0468(18) Uani 1 1 d . . . C2 C 0.5096(11) 0.6977(8) 0.1104(4) 0.050(2) Uani 1 1 d . . . H2 H 0.5910 0.7107 0.1307 0.060 Uiso 1 1 calc R . . C3 C 0.4456(11) 0.7788(8) 0.0617(4) 0.052(2) Uani 1 1 d . . . H3 H 0.4838 0.8444 0.0499 0.062 Uiso 1 1 calc R . . C4 C 0.3257(9) 0.7633(7) 0.0303(3) 0.0351(19) Uani 1 1 d . . . C5 C 0.2815(11) 0.6607(8) 0.0479(4) 0.052(2) Uani 1 1 d . . . H5 H 0.2071 0.6415 0.0253 0.062 Uiso 1 1 calc R . . C6 C 0.3470(12) 0.5864(8) 0.0987(4) 0.061(3) Uani 1 1 d . . . H6 H 0.3088 0.5215 0.1119 0.073 Uiso 1 1 calc R . . N7 N 0.2511(8) 0.8415(6) -0.0194(3) 0.0416(18) Uani 1 1 d . . . H7 H 0.2123 0.8064 -0.0480 0.050 Uiso 1 1 calc R . . C8 C 0.2330(9) 0.9653(7) -0.0275(3) 0.0344(19) Uani 1 1 d . . . O9 O 0.2934(7) 1.0222(5) 0.0079(3) 0.0490(15) Uani 1 1 d . . . C10 C 0.1358(10) 1.0339(7) -0.0805(3) 0.039(2) Uani 1 1 d . . . C11 C 0.1455(12) 1.1498(8) -0.0991(4) 0.058(3) Uani 1 1 d . . . H11 H 0.2111 1.1835 -0.0785 0.070 Uiso 1 1 calc R . . C12 C 0.0587(12) 1.2172(8) -0.1483(4) 0.062(3) Uani 1 1 d . . . H12 H 0.0693 1.2942 -0.1615 0.075 Uiso 1 1 calc R . . C13 C -0.0435(11) 1.1704(7) -0.1778(4) 0.051(2) Uani 1 1 d . . . H13 H -0.1012 1.2155 -0.2109 0.061 Uiso 1 1 calc R . . C14 C -0.0592(9) 1.0557(7) -0.1576(3) 0.0334(18) Uani 1 1 d . . . C15 C 0.0340(9) 0.9869(7) -0.1100(3) 0.0311(18) Uani 1 1 d . . . H15 H 0.0275 0.9081 -0.0980 0.037 Uiso 1 1 calc R . . C16 C -0.1692(9) 1.0086(7) -0.1909(4) 0.0330(18) Uani 1 1 d . . . O17 O -0.2069(7) 1.0365(5) -0.2455(3) 0.0501(16) Uani 1 1 d . . . N18 N -0.2248(9) 0.9292(6) -0.1523(3) 0.050(2) Uani 1 1 d . . . H18 H -0.2038 0.9251 -0.1115 0.060 Uiso 1 1 calc R . . C19 C -0.3114(10) 0.8540(7) -0.1707(4) 0.038(2) Uani 1 1 d . . . C20 C -0.3234(10) 0.8241(7) -0.2366(4) 0.044(2) Uani 1 1 d . . . H20 H -0.2792 0.8592 -0.2713 0.053 Uiso 1 1 calc R . . C21 C -0.4017(11) 0.7421(8) -0.2489(4) 0.051(2) Uani 1 1 d . . . H21 H -0.4104 0.7231 -0.2928 0.062 Uiso 1 1 calc R . . N22 N -0.4666(8) 0.6875(6) -0.2011(3) 0.0442(18) Uani 1 1 d . . . C23 C -0.4610(10) 0.7213(7) -0.1363(4) 0.039(2) Uani 1 1 d . . . H23 H -0.5124 0.6895 -0.1026 0.047 Uiso 1 1 calc R . . C24 C -0.3825(12) 0.7996(8) -0.1202(4) 0.056(3) Uani 1 1 d . . . H24 H -0.3756 0.8174 -0.0760 0.067 Uiso 1 1 calc R . . N25 N 0.7441(9) 0.3341(6) 0.2891(3) 0.054(2) Uani 1 1 d . . . C26 C 0.7924(10) 0.2097(8) 0.2759(4) 0.047(2) Uani 1 1 d . . . H26 H 0.7546 0.1820 0.2397 0.057 Uiso 1 1 calc R . . C27 C 0.8934(10) 0.1184(7) 0.3112(4) 0.042(2) Uani 1 1 d . . . H27 H 0.9198 0.0326 0.2999 0.051 Uiso 1 1 calc R . . C28 C 0.9548(10) 0.1579(7) 0.3642(4) 0.044(2) Uani 1 1 d . . . C29 C 0.9083(14) 0.2894(8) 0.3785(5) 0.079(4) Uani 1 1 d . . . H29 H 0.9507 0.3210 0.4119 0.095 Uiso 1 1 calc R . . C30 C 0.7989(15) 0.3700(9) 0.3420(5) 0.088(4) Uani 1 1 d . . . H30 H 0.7603 0.4555 0.3550 0.105 Uiso 1 1 calc R . . N31 N 1.0661(9) 0.0751(6) 0.4013(3) 0.054(2) Uani 1 1 d . . . H31 H 1.1279 0.1064 0.4193 0.065 Uiso 1 1 calc R . . C32 C 1.0866(11) -0.0494(7) 0.4116(4) 0.044(2) Uani 1 1 d . . . O33 O 1.0098(7) -0.1056(5) 0.3870(3) 0.0514(16) Uani 1 1 d . . . C34 C 1.2100(10) -0.1167(7) 0.4552(4) 0.042(2) Uani 1 1 d . . . C35 C 1.2645(12) -0.2474(8) 0.4533(4) 0.058(3) Uani 1 1 d . . . H35 H 1.2254 -0.2908 0.4239 0.070 Uiso 1 1 calc R . . C36 C 1.3751(13) -0.3161(8) 0.4934(5) 0.070(3) Uani 1 1 d . . . H36 H 1.4123 -0.4044 0.4900 0.084 Uiso 1 1 calc R . . C37 C 1.4299(12) -0.2535(8) 0.5384(4) 0.064(3) Uani 1 1 d . . . H37 H 1.5058 -0.2996 0.5651 0.076 Uiso 1 1 calc R . . C38 C 1.3731(10) -0.1215(7) 0.5445(4) 0.043(2) Uani 1 1 d . . . C39 C 1.2632(10) -0.0537(7) 0.5024(4) 0.045(2) Uani 1 1 d . . . H39 H 1.2249 0.0346 0.5059 0.053 Uiso 1 1 calc R . . C40 C 1.4292(11) -0.0542(7) 0.5953(4) 0.043(2) Uani 1 1 d . . . O41 O 1.5673(7) -0.0972(5) 0.6086(3) 0.0529(16) Uani 1 1 d . . . N42 N 1.3278(8) 0.0545(6) 0.6207(3) 0.0406(17) Uani 1 1 d . . . H42 H 1.2337 0.0702 0.6107 0.049 Uiso 1 1 calc R . . C43 C 1.3511(10) 0.1468(7) 0.6609(4) 0.0353(19) Uani 1 1 d . . . C44 C 1.4957(10) 0.1466(7) 0.6769(4) 0.040(2) Uani 1 1 d . . . H44 H 1.5849 0.0789 0.6635 0.048 Uiso 1 1 calc R . . C45 C 1.5055(11) 0.2477(7) 0.7127(4) 0.052(3) Uani 1 1 d . . . H45 H 1.6034 0.2457 0.7233 0.063 Uiso 1 1 calc R . . N46 N 1.3852(9) 0.3472(6) 0.7331(3) 0.0452(19) Uani 1 1 d . . . C47 C 1.2405(10) 0.3457(7) 0.7214(4) 0.041(2) Uani 1 1 d . . . H47 H 1.1526 0.4109 0.7388 0.050 Uiso 1 1 calc R . . C48 C 1.2235(11) 0.2480(8) 0.6838(4) 0.049(2) Uani 1 1 d . . . H48 H 1.1248 0.2508 0.6740 0.058 Uiso 1 1 calc R . . O49 O 0.9709(10) 0.3276(8) 0.0772(4) 0.096(3) Uani 1 1 d . . . N50 N 0.8661(11) 0.3828(7) 0.1192(4) 0.057(2) Uani 1 1 d . . . O51 O 0.8614(11) 0.4791(7) 0.1507(4) 0.106(3) Uani 1 1 d . . . O52 O 0.7593(9) 0.3390(6) 0.1289(3) 0.0677(19) Uani 1 1 d . . . O53A O 0.3892(15) 0.4912(11) 0.3440(6) 0.076(4) Uiso 0.70 1 d P . . O53B O 0.431(3) 0.5001(19) 0.3192(11) 0.046(6) Uiso 0.30 1 d P . . N54 N 0.2723(12) 0.5386(8) 0.3153(4) 0.061(2) Uiso 1 1 d . . . O55A O 0.232(9) 0.505(6) 0.366(3) 0.085(19) Uiso 0.14 1 d P . . O55B O 0.147(2) 0.543(2) 0.3583(10) 0.055(5) Uiso 0.47 1 d P . . O55C O 0.146(5) 0.581(4) 0.342(3) 0.053(13) Uiso 0.20 1 d P . . O55D O 0.148(7) 0.545(7) 0.327(3) 0.08(2) Uiso 0.17 1 d P . . O56A O 0.198(3) 0.583(2) 0.2650(12) 0.090(8) Uiso 0.35 1 d P . . O56B O 0.2892(14) 0.5749(10) 0.2583(5) 0.059(3) Uiso 0.65 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 Cd1 0.0659(5) 0.0265(3) 0.0406(3) 0.0051(2) -0.0266(3) -0.0193(3) N1 0.063(5) 0.039(4) 0.044(4) 0.008(3) -0.017(4) -0.020(4) C2 0.058(6) 0.058(6) 0.040(5) 0.006(4) -0.015(4) -0.025(5) C3 0.066(7) 0.057(6) 0.046(5) 0.015(4) -0.026(5) -0.033(5) C4 0.037(5) 0.035(4) 0.029(4) -0.002(3) -0.002(4) -0.006(4) C5 0.067(7) 0.045(5) 0.052(5) 0.005(4) -0.027(5) -0.025(5) C6 0.083(8) 0.049(6) 0.070(6) 0.023(5) -0.043(6) -0.038(5) N7 0.056(5) 0.042(4) 0.032(3) 0.002(3) -0.025(3) -0.019(4) C8 0.037(5) 0.037(5) 0.029(4) -0.002(3) 0.000(4) -0.015(4) O9 0.066(4) 0.049(3) 0.045(3) 0.006(3) -0.024(3) -0.032(3) C10 0.053(6) 0.042(5) 0.030(4) 0.002(3) -0.014(4) -0.027(4) C11 0.086(8) 0.053(6) 0.062(6) 0.019(5) -0.037(5) -0.050(6) C12 0.096(8) 0.047(6) 0.067(6) 0.030(5) -0.032(6) -0.049(6) C13 0.073(7) 0.037(5) 0.053(5) 0.015(4) -0.035(5) -0.024(5) C14 0.043(5) 0.027(4) 0.033(4) -0.002(3) 0.000(4) -0.015(4) C15 0.041(5) 0.024(4) 0.030(4) -0.001(3) -0.003(4) -0.014(4) C16 0.025(5) 0.042(5) 0.032(4) 0.004(4) -0.001(4) -0.012(4) O17 0.062(4) 0.052(4) 0.044(3) 0.015(3) -0.030(3) -0.023(3) N18 0.073(6) 0.055(5) 0.038(4) -0.002(3) -0.021(4) -0.040(4) C19 0.046(5) 0.034(4) 0.040(4) -0.001(4) -0.017(4) -0.016(4) C20 0.063(6) 0.041(5) 0.033(4) 0.002(4) -0.013(4) -0.022(5) C21 0.089(8) 0.048(5) 0.035(5) 0.009(4) -0.021(5) -0.044(5) N22 0.058(5) 0.033(4) 0.046(4) -0.003(3) -0.021(4) -0.018(4) C23 0.043(6) 0.040(5) 0.041(4) -0.003(4) -0.006(4) -0.021(4) C24 0.096(8) 0.049(5) 0.042(5) 0.008(4) -0.031(5) -0.042(6) N25 0.077(6) 0.031(4) 0.053(4) 0.006(3) -0.035(4) -0.008(4) C26 0.056(6) 0.045(5) 0.045(5) 0.005(4) -0.016(4) -0.019(5) C27 0.064(6) 0.029(4) 0.034(4) 0.002(3) -0.011(4) -0.014(4) C28 0.058(6) 0.039(5) 0.042(5) 0.003(4) -0.018(4) -0.020(4) C29 0.150(11) 0.044(6) 0.064(6) 0.014(5) -0.070(7) -0.046(7) C30 0.161(12) 0.035(5) 0.075(7) 0.011(5) -0.074(8) -0.028(6) N31 0.074(6) 0.041(4) 0.062(5) 0.017(4) -0.047(4) -0.028(4) C32 0.073(7) 0.035(5) 0.031(4) -0.001(4) -0.016(4) -0.023(5) O33 0.065(4) 0.038(3) 0.059(4) 0.000(3) -0.031(3) -0.021(3) C34 0.064(6) 0.027(4) 0.042(4) 0.000(4) -0.018(4) -0.019(4) C35 0.074(7) 0.036(5) 0.065(6) -0.008(4) -0.022(5) -0.015(5) C36 0.094(9) 0.026(5) 0.082(7) -0.011(5) -0.036(6) -0.002(5) C37 0.076(8) 0.047(6) 0.064(6) -0.001(5) -0.034(6) -0.007(5) C38 0.060(6) 0.024(4) 0.044(5) 0.001(4) -0.023(4) -0.009(4) C39 0.074(7) 0.024(4) 0.042(5) 0.006(3) -0.021(4) -0.020(4) C40 0.057(6) 0.025(4) 0.049(5) 0.008(4) -0.030(5) -0.009(4) O41 0.059(4) 0.040(3) 0.058(4) -0.005(3) -0.024(3) -0.009(3) N42 0.048(5) 0.029(4) 0.047(4) -0.010(3) -0.016(3) -0.013(3) C43 0.037(5) 0.034(4) 0.035(4) 0.000(3) -0.007(4) -0.011(4) C44 0.035(5) 0.037(5) 0.047(5) -0.002(4) -0.003(4) -0.009(4) C45 0.068(7) 0.033(5) 0.056(5) 0.001(4) -0.037(5) -0.010(5) N46 0.065(6) 0.031(4) 0.042(4) 0.002(3) -0.021(4) -0.014(4) C47 0.032(5) 0.041(5) 0.047(5) -0.005(4) -0.004(4) -0.008(4) C48 0.056(6) 0.050(5) 0.050(5) -0.004(4) -0.022(5) -0.027(5) O49 0.075(6) 0.112(7) 0.083(5) -0.005(5) 0.017(5) -0.015(5) N50 0.073(7) 0.046(5) 0.052(5) -0.008(4) -0.011(5) -0.021(5) O51 0.170(9) 0.068(5) 0.106(6) -0.021(4) -0.041(6) -0.066(6) O52 0.076(5) 0.068(5) 0.074(4) 0.010(4) -0.021(4) -0.040(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 Cd1 O53B 2.23(2) . ? Cd1 N46 2.347(6) 2_766 ? Cd1 N25 2.360(6) . ? Cd1 N22 2.361(6) 2_565 ? Cd1 N1 2.397(6) . ? Cd1 O56B 2.497(12) . ? Cd1 O52 2.548(7) . ? N1 C2 1.326(10) . ? N1 C6 1.340(10) . ? C2 C3 1.372(11) . ? C2 H2 0.9300 . ? C3 C4 1.369(11) . ? C3 H3 0.9300 . ? C4 C5 1.368(11) . ? C4 N7 1.400(9) . ? C5 C6 1.371(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7 C8 1.346(9) . ? N7 H7 0.8600 . ? C8 O9 1.232(8) . ? C8 C10 1.496(10) . ? C10 C11 1.373(10) . ? C10 C15 1.382(10) . ? C11 C12 1.386(11) . ? C11 H11 0.9300 . ? C12 C13 1.383(11) . ? C12 H12 0.9300 . ? C13 C14 1.390(10) . ? C13 H13 0.9300 . ? C14 C15 1.395(10) . ? C14 C16 1.484(10) . ? C15 H15 0.9300 . ? C16 O17 1.197(8) . ? C16 N18 1.370(9) . ? N18 C19 1.397(9) . ? N18 H18 0.8600 . ? C19 C20 1.399(9) . ? C19 C24 1.405(11) . ? C20 C21 1.367(11) . ? C20 H20 0.9300 . ? C21 N22 1.339(10) . ? C21 H21 0.9300 . ? N22 C23 1.376(9) . ? N22 Cd1 2.361(6) 2_565 ? C23 C24 1.354(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? N25 C26 1.329(10) . ? N25 C30 1.335(10) . ? C26 C27 1.375(10) . ? C26 H26 0.9300 . ? C27 C28 1.387(10) . ? C27 H27 0.9300 . ? C28 N31 1.399(9) . ? C28 C29 1.408(11) . ? C29 C30 1.372(12) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? N31 C32 1.355(9) . ? N31 H31 0.8600 . ? C32 O33 1.217(9) . ? C32 C34 1.491(11) . ? C34 C35 1.375(10) . ? C34 C39 1.394(10) . ? C35 C36 1.376(12) . ? C35 H35 0.9300 . ? C36 C37 1.370(11) . ? C36 H36 0.9300 . ? C37 C38 1.391(11) . ? C37 H37 0.9300 . ? C38 C39 1.396(10) . ? C38 C40 1.492(10) . ? C39 H39 0.9300 . ? C40 O41 1.246(9) . ? C40 N42 1.331(9) . ? N42 C43 1.395(9) . ? N42 H42 0.8600 . ? C43 C48 1.374(11) . ? C43 C44 1.385(11) . ? C44 C45 1.372(10) . ? C44 H44 0.9300 . ? C45 N46 1.315(10) . ? C45 H45 0.9300 . ? N46 C47 1.368(10) . ? N46 Cd1 2.347(6) 2_766 ? C47 C48 1.386(10) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? O49 N50 1.222(10) . ? N50 O52 1.228(10) . ? N50 O51 1.235(9) . ? O53A O53B 0.63(2) . ? O53A N54 1.221(14) . ? O53A O55A 1.43(7) . ? O53B N54 1.38(2) . ? N54 O55D 1.12(6) . ? N54 O55A 1.16(6) . ? N54 O55C 1.18(5) . ? N54 O56B 1.235(12) . ? N54 O56A 1.28(2) . ? N54 O55B 1.37(2) . ? O55A O55B 0.78(6) . ? O55A O55C 1.09(8) . ? O55A O55D 1.14(9) . ? O55B O55C 0.53(5) . ? O55B O55D 0.64(7) . ? O55C O56A 1.59(7) . ? O55D O56A 1.41(7) . ? O56A O56B 0.80(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 O53B Cd1 N46 78.4(6) . 2_766 ? O53B Cd1 N25 77.1(6) . . ? N46 Cd1 N25 92.3(2) 2_766 . ? O53B Cd1 N22 84.9(6) . 2_565 ? N46 Cd1 N22 162.7(2) 2_766 2_565 ? N25 Cd1 N22 88.3(2) . 2_565 ? O53B Cd1 N1 119.4(6) . . ? N46 Cd1 N1 89.0(2) 2_766 . ? N25 Cd1 N1 163.3(3) . . ? N22 Cd1 N1 95.3(2) 2_565 . ? O53B Cd1 O56B 45.8(6) . . ? N46 Cd1 O56B 88.4(3) 2_766 . ? N25 Cd1 O56B 121.4(3) . . ? N22 Cd1 O56B 76.7(3) 2_565 . ? N1 Cd1 O56B 75.2(3) . . ? O53B Cd1 O52 152.5(6) . . ? N46 Cd1 O52 120.9(2) 2_766 . ? N25 Cd1 O52 82.4(2) . . ? N22 Cd1 O52 76.3(2) 2_565 . ? N1 Cd1 O52 82.7(2) . . ? O56B Cd1 O52 143.0(3) . . ? C2 N1 C6 115.3(7) . . ? C2 N1 Cd1 121.1(5) . . ? C6 N1 Cd1 123.5(6) . . ? N1 C2 C3 124.1(8) . . ? N1 C2 H2 118.0 . . ? C3 C2 H2 118.0 . . ? C4 C3 C2 120.1(8) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 116.5(7) . . ? C5 C4 N7 118.8(7) . . ? C3 C4 N7 124.7(8) . . ? C4 C5 C6 120.0(8) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? N1 C6 C5 123.8(9) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? C8 N7 C4 127.4(6) . . ? C8 N7 H7 116.3 . . ? C4 N7 H7 116.3 . . ? O9 C8 N7 121.4(7) . . ? O9 C8 C10 120.2(7) . . ? N7 C8 C10 118.4(6) . . ? C11 C10 C15 119.0(7) . . ? C11 C10 C8 118.4(7) . . ? C15 C10 C8 122.7(7) . . ? C10 C11 C12 120.8(8) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 120.3(8) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 119.5(7) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 119.2(7) . . ? C13 C14 C16 117.7(7) . . ? C15 C14 C16 123.0(7) . . ? C10 C15 C14 121.1(7) . . ? C10 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? O17 C16 N18 122.9(7) . . ? O17 C16 C14 124.3(8) . . ? N18 C16 C14 112.8(6) . . ? C16 N18 C19 128.2(6) . . ? C16 N18 H18 115.9 . . ? C19 N18 H18 115.9 . . ? N18 C19 C20 123.4(8) . . ? N18 C19 C24 118.2(7) . . ? C20 C19 C24 118.4(7) . . ? C21 C20 C19 118.4(8) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? N22 C21 C20 123.6(7) . . ? N22 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? C21 N22 C23 118.0(7) . . ? C21 N22 Cd1 123.8(5) . 2_565 ? C23 N22 Cd1 118.1(5) . 2_565 ? C24 C23 N22 121.7(8) . . ? C24 C23 H23 119.1 . . ? N22 C23 H23 119.1 . . ? C23 C24 C19 119.8(7) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C26 N25 C30 115.5(7) . . ? C26 N25 Cd1 120.1(5) . . ? C30 N25 Cd1 124.4(6) . . ? N25 C26 C27 125.5(7) . . ? N25 C26 H26 117.2 . . ? C27 C26 H26 117.2 . . ? C26 C27 C28 118.2(7) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? C27 C28 N31 123.6(7) . . ? C27 C28 C29 117.5(7) . . ? N31 C28 C29 118.8(7) . . ? C30 C29 C28 118.5(8) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? N25 C30 C29 124.5(8) . . ? N25 C30 H30 117.8 . . ? C29 C30 H30 117.8 . . ? C32 N31 C28 126.8(7) . . ? C32 N31 H31 116.6 . . ? C28 N31 H31 116.6 . . ? O33 C32 N31 122.8(7) . . ? O33 C32 C34 120.5(7) . . ? N31 C32 C34 116.7(7) . . ? C35 C34 C39 117.9(7) . . ? C35 C34 C32 118.8(7) . . ? C39 C34 C32 123.0(7) . . ? C34 C35 C36 122.1(8) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C37 C36 C35 119.6(8) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.5(8) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 118.9(7) . . ? C37 C38 C40 120.2(7) . . ? C39 C38 C40 120.9(6) . . ? C34 C39 C38 120.9(7) . . ? C34 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? O41 C40 N42 124.0(7) . . ? O41 C40 C38 119.5(7) . . ? N42 C40 C38 116.4(7) . . ? C40 N42 C43 129.7(7) . . ? C40 N42 H42 115.1 . . ? C43 N42 H42 115.1 . . ? C48 C43 C44 117.6(7) . . ? C48 C43 N42 118.1(7) . . ? C44 C43 N42 124.2(7) . . ? C45 C44 C43 119.0(8) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? N46 C45 C44 124.2(8) . . ? N46 C45 H45 117.9 . . ? C44 C45 H45 117.9 . . ? C45 N46 C47 117.7(7) . . ? C45 N46 Cd1 119.1(6) . 2_766 ? C47 N46 Cd1 123.0(5) . 2_766 ? N46 C47 C48 120.6(8) . . ? N46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C43 C48 C47 120.7(8) . . ? C43 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? O49 N50 O52 116.5(8) . . ? O49 N50 O51 124.0(10) . . ? O52 N50 O51 119.5(10) . . ? N50 O52 Cd1 106.8(6) . . ? O53B O53A N54 90(3) . . ? O53B O53A O55A 142(4) . . ? N54 O53A O55A 52(2) . . ? O53A O53B N54 62(2) . . ? O53A O53B Cd1 162(3) . . ? N54 O53B Cd1 114.4(13) . . ? O55D N54 O55A 60(5) . . ? O55A N54 O55C 56(4) . . ? O55D N54 O53A 133(4) . . ? O55A N54 O53A 73(4) . . ? O55C N54 O53A 124(3) . . ? O55D N54 O56B 109(4) . . ? O55A N54 O56B 168(4) . . ? O55C N54 O56B 115(3) . . ? O53A N54 O56B 117.6(13) . . ? O55D N54 O56A 72(4) . . ? O55A N54 O56A 131(4) . . ? O55C N54 O56A 81(3) . . ? O53A N54 O56A 154.4(18) . . ? O53A N54 O55B 107.6(13) . . ? O56B N54 O55B 134.7(15) . . ? O56A N54 O55B 97.8(18) . . ? O55D N54 O53B 159(4) . . ? O55A N54 O53B 101(4) . . ? O55C N54 O53B 149(3) . . ? O56B N54 O53B 90.4(13) . . ? O56A N54 O53B 127.4(19) . . ? O55B N54 O53B 134.7(16) . . ? O55B O55A N54 87(6) . . ? O55C O55A N54 63(4) . . ? O55D O55A N54 58(5) . . ? O55B O55A O53A 141(8) . . ? O55C O55A O53A 114(6) . . ? O55D O55A O53A 113(6) . . ? N54 O55A O53A 55(3) . . ? O55C O55B O55D 49(7) . . ? O55C O55B O55A 111(8) . . ? O55D O55B O55A 106(8) . . ? O55C O55B N54 58(6) . . ? O55D O55B N54 54(6) . . ? O55A O55B N54 58(5) . . ? O55B O55C N54 99(7) . . ? O55A O55C N54 62(5) . . ? O55B O55C O56A 133(8) . . ? O55A O55C O56A 111(5) . . ? N54 O55C O56A 52(3) . . ? O55B O55D N54 98(7) . . ? N54 O55D O55A 62(5) . . ? O55B O55D O56A 152(10) . . ? N54 O55D O56A 59(4) . . ? O55A O55D O56A 121(7) . . ? O56B O56A N54 69(2) . . ? O56B O56A O55D 117(4) . . ? N54 O56A O55D 49(3) . . ? O56B O56A O55C 112(3) . . ? N54 O56A O55C 46.8(18) . . ? O56A O56B N54 74(2) . . ? O56A O56B Cd1 159(2) . . ? N54 O56B Cd1 105.8(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O52 0.86 2.24 3.024(9) 150.7 2_665 N18 H18 O9 0.86 2.19 2.949(9) 146.4 2_575 N42 H42 O33 0.86 2.12 2.962(9) 165.1 2_756 C24 H24 O9 0.93 2.59 3.340(9) 137.9 2_575 C45 H45 O17 0.93 2.52 3.075(10) 118.4 1_746 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.436 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.128 # Attachment 'MOF3_an425a4m_FINAL_R.cif' data_an425a4m _database_code_depnum_ccdc_archive 'CCDC 694506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Co N4 O13 S' _chemical_formula_weight 599.43 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' S S 0.1246 0.1234 '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 9.9398(8) _cell_length_b 16.8130(13) _cell_length_c 14.9567(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.1460(10) _cell_angle_gamma 90.00 _cell_volume 2489.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description RHOMBOHEDRAL _exptl_crystal_colour PINK _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7618 _exptl_absorpt_correction_T_max 0.9354 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20673 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0370 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5677 _reflns_number_gt 5029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0619P)^2^+2.1427P] 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 5677 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.004 _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 0.48842(3) 0.00825(2) 0.24283(2) 0.01242(12) Uani 1 1 d . . . N1 N 0.6975(2) -0.01201(13) 0.28449(15) 0.0152(5) Uani 1 1 d . . . C2 C 0.7493(3) -0.08467(16) 0.27516(19) 0.0177(6) Uani 1 1 d . . . H2 H 0.6952 -0.1240 0.2468 0.021 Uiso 1 1 calc R . . C3 C 0.8804(3) -0.10315(16) 0.30619(19) 0.0184(6) Uani 1 1 d . . . H3 H 0.9137 -0.1542 0.2986 0.022 Uiso 1 1 calc R . . C4 C 0.9619(3) -0.04557(17) 0.3486(2) 0.0193(6) Uani 1 1 d . . . H4 H 1.0500 -0.0574 0.3707 0.023 Uiso 1 1 calc R . . C5 C 0.9097(3) 0.03038(16) 0.35773(18) 0.0134(5) Uani 1 1 d . . . C6 C 0.7767(3) 0.04424(16) 0.32468(18) 0.0146(5) Uani 1 1 d . . . H6 H 0.7411 0.0949 0.3308 0.018 Uiso 1 1 calc R . . N7 N 0.9815(2) 0.09588(14) 0.39765(15) 0.0152(5) Uani 1 1 d . . . H7 H 0.9359 0.1385 0.4045 0.018 Uiso 1 1 calc R . . C8 C 1.1147(3) 0.09840(16) 0.42616(18) 0.0147(5) Uani 1 1 d . . . O9 O 1.18938(19) 0.03954(11) 0.42581(14) 0.0180(4) Uani 1 1 d . . . C10 C 1.1714(3) 0.17621(16) 0.45954(18) 0.0141(5) Uani 1 1 d . . . C11 C 1.2892(3) 0.17334(17) 0.51786(18) 0.0163(6) Uani 1 1 d . . . H11 H 1.319(3) 0.1214(19) 0.540(2) 0.020 Uiso 1 1 d . . . C12 C 1.3507(3) 0.24332(17) 0.5484(2) 0.0184(6) Uani 1 1 d . . . H12 H 1.4276 0.2414 0.5886 0.022 Uiso 1 1 calc R . . C13 C 1.2983(3) 0.31581(17) 0.51963(18) 0.0164(6) Uani 1 1 d . . . H13 H 1.3417 0.3626 0.5389 0.020 Uiso 1 1 calc R . . C14 C 1.1800(3) 0.31905(16) 0.46137(18) 0.0142(5) Uani 1 1 d . . . C15 C 1.1170(3) 0.24930(15) 0.43117(19) 0.0151(6) Uani 1 1 d . . . H15 H 1.0388 0.2513 0.3922 0.018 Uiso 1 1 calc R . . C16 C 1.1308(3) 0.39995(16) 0.43189(18) 0.0148(5) Uani 1 1 d . . . O17 O 1.20973(19) 0.45626(12) 0.43282(14) 0.0196(4) Uani 1 1 d . . . N18 N 0.9975(2) 0.40684(14) 0.40495(16) 0.0156(5) Uani 1 1 d . . . H18 H 0.9485 0.3654 0.4112 0.019 Uiso 1 1 calc R . . C19 C 0.9306(3) 0.47476(16) 0.36773(18) 0.0136(5) Uani 1 1 d . . . C20 C 0.9914(3) 0.54867(17) 0.35943(19) 0.0165(6) Uani 1 1 d . . . H20 H 1.084(3) 0.5571(19) 0.382(2) 0.020 Uiso 1 1 d . . . C21 C 0.9142(3) 0.60955(16) 0.31888(19) 0.0170(6) Uani 1 1 d . . . H21 H 0.9520 0.6595 0.3117 0.020 Uiso 1 1 calc R . . C22 C 0.7807(3) 0.59565(16) 0.28913(19) 0.0173(6) Uani 1 1 d . . . H22 H 0.7302 0.6371 0.2620 0.021 Uiso 1 1 calc R . . N23 N 0.7212(2) 0.52514(13) 0.29770(15) 0.0143(5) Uani 1 1 d . . . C24 C 0.7955(3) 0.46601(16) 0.33614(18) 0.0136(5) Uani 1 1 d . . . H24 H 0.7548 0.4167 0.3420 0.016 Uiso 1 1 calc R . . O25 O 0.5222(2) -0.04035(13) 0.11707(14) 0.0192(4) Uani 1 1 d . . . H25A H 0.4804 -0.0823 0.1098 0.029 Uiso 1 1 calc R . . O26 O 0.4490(2) -0.10381(11) 0.29394(14) 0.0167(4) Uani 1 1 d . . . H26A H 0.4548 -0.1374 0.2548 0.025 Uiso 1 1 calc R . . O27 O 0.5304(2) 0.12053(11) 0.19753(14) 0.0167(4) Uani 1 1 d . . . H27A H 0.5359 0.1517 0.2399 0.025 Uiso 1 1 calc R . . O28 O 0.4562(2) 0.05647(12) 0.37012(14) 0.0188(4) Uani 1 1 d . . . H28A H 0.5030 0.0963 0.3793 0.028 Uiso 1 1 calc R . . S29 S 0.35059(7) 0.75401(4) 0.11723(5) 0.01250(16) Uani 1 1 d . . . O30 O 0.39083(19) 0.68217(11) 0.06965(13) 0.0172(4) Uani 1 1 d . . . O31 O 0.4293(2) 0.75699(10) 0.20620(14) 0.0180(4) Uani 1 1 d . . . O32 O 0.3784(2) 0.82596(11) 0.06630(13) 0.0175(4) Uani 1 1 d . . . O33 O 0.2044(2) 0.74969(11) 0.12867(15) 0.0201(5) Uani 1 1 d . . . O34 O 0.1307(2) 0.76979(14) 0.30468(16) 0.0253(5) Uani 1 1 d . . . O35 O 0.7355(2) 0.14464(14) 0.10207(17) 0.0236(5) Uani 1 1 d . . . O36 O 0.7270(2) 0.11913(14) 0.57956(15) 0.0218(5) Uani 1 1 d . . . H36A H 0.756(5) 0.072(3) 0.564(3) 0.064(15) Uiso 1 1 d . . . H36B H 0.695(4) 0.141(3) 0.535(3) 0.047(13) Uiso 1 1 d . . . H35A H 0.711(4) 0.147(3) 0.052(3) 0.039(13) Uiso 1 1 d . . . H35B H 0.784(4) 0.192(3) 0.126(3) 0.050(12) Uiso 1 1 d . . . H34A H 0.182(5) 0.810(3) 0.350(3) 0.076(16) Uiso 1 1 d . . . H34B H 0.172(5) 0.761(3) 0.249(4) 0.069(16) Uiso 1 1 d . . . H27B H 0.594(4) 0.125(2) 0.165(2) 0.023(9) Uiso 1 1 d . . . H28B H 0.387(4) 0.055(2) 0.387(3) 0.032(11) Uiso 1 1 d . . . H26B H 0.405(4) -0.107(2) 0.335(3) 0.044(13) Uiso 1 1 d . . . H25B H 0.592(4) -0.045(2) 0.103(3) 0.034(12) 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 Co1 0.01025(19) 0.00953(19) 0.0172(2) -0.00100(14) -0.00022(14) -0.00153(13) N1 0.0148(11) 0.0126(11) 0.0182(12) -0.0014(9) 0.0013(9) -0.0016(9) C2 0.0197(14) 0.0138(13) 0.0195(14) -0.0001(11) 0.0019(11) -0.0014(11) C3 0.0192(14) 0.0117(13) 0.0245(15) -0.0015(11) 0.0034(12) 0.0030(11) C4 0.0123(13) 0.0140(14) 0.0311(16) -0.0011(12) 0.0000(12) 0.0024(10) C5 0.0112(12) 0.0136(13) 0.0156(13) -0.0009(10) 0.0023(10) -0.0018(10) C6 0.0139(13) 0.0116(13) 0.0181(14) -0.0006(10) 0.0001(10) 0.0009(10) N7 0.0113(11) 0.0137(11) 0.0202(12) -0.0042(9) -0.0004(9) 0.0009(9) C8 0.0123(13) 0.0171(13) 0.0147(13) 0.0023(10) 0.0010(10) 0.0015(10) O9 0.0110(9) 0.0156(10) 0.0267(11) -0.0001(8) -0.0020(8) 0.0026(7) C10 0.0103(12) 0.0187(14) 0.0134(13) -0.0005(10) 0.0019(10) -0.0003(10) C11 0.0134(13) 0.0215(14) 0.0135(13) 0.0025(11) -0.0021(10) 0.0029(11) C12 0.0118(13) 0.0266(16) 0.0159(14) -0.0017(11) -0.0033(11) 0.0011(11) C13 0.0118(13) 0.0221(14) 0.0153(13) -0.0034(11) 0.0012(10) -0.0030(11) C14 0.0119(13) 0.0162(13) 0.0144(13) 0.0008(10) 0.0013(10) 0.0007(10) C15 0.0080(12) 0.0222(15) 0.0149(14) -0.0003(10) 0.0000(10) -0.0005(10) C16 0.0153(13) 0.0153(13) 0.0140(13) -0.0029(10) 0.0018(10) 0.0009(10) O17 0.0125(9) 0.0172(10) 0.0285(11) -0.0014(8) -0.0014(8) -0.0008(8) N18 0.0103(11) 0.0143(11) 0.0219(12) 0.0032(9) 0.0000(9) 0.0000(9) C19 0.0129(13) 0.0133(13) 0.0145(13) -0.0005(10) 0.0016(10) 0.0028(10) C20 0.0119(13) 0.0164(14) 0.0212(14) -0.0013(11) 0.0020(11) -0.0009(10) C21 0.0193(14) 0.0102(13) 0.0218(14) 0.0000(11) 0.0033(11) -0.0029(10) C22 0.0186(14) 0.0144(13) 0.0189(14) -0.0005(11) 0.0017(11) 0.0023(11) N23 0.0128(11) 0.0115(11) 0.0188(12) 0.0011(9) 0.0016(9) 0.0013(9) C24 0.0125(13) 0.0102(12) 0.0180(13) 0.0004(10) 0.0006(10) -0.0008(10) O25 0.0141(11) 0.0209(11) 0.0228(11) -0.0066(8) 0.0035(9) -0.0052(8) O26 0.0200(11) 0.0105(9) 0.0200(11) -0.0020(8) 0.0042(9) -0.0032(8) O27 0.0184(10) 0.0124(10) 0.0198(10) -0.0005(8) 0.0032(9) -0.0031(8) O28 0.0149(11) 0.0181(11) 0.0237(11) -0.0054(8) 0.0045(9) -0.0052(8) S29 0.0122(3) 0.0098(3) 0.0154(3) -0.0003(2) 0.0001(2) 0.0000(2) O30 0.0205(10) 0.0105(9) 0.0200(10) -0.0018(8) -0.0015(8) 0.0028(8) O31 0.0247(11) 0.0129(10) 0.0155(10) 0.0001(7) -0.0039(8) 0.0007(8) O32 0.0222(10) 0.0119(9) 0.0181(10) 0.0028(8) 0.0005(8) -0.0038(8) O33 0.0139(10) 0.0208(11) 0.0256(12) -0.0009(8) 0.0024(8) 0.0000(8) O34 0.0197(11) 0.0288(12) 0.0281(12) -0.0039(10) 0.0049(9) 0.0017(9) O35 0.0224(11) 0.0241(12) 0.0240(13) 0.0070(9) 0.0005(10) 0.0008(9) O36 0.0235(11) 0.0201(11) 0.0218(12) 0.0049(9) 0.0024(9) 0.0054(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 O27 2.0610(19) . ? Co1 O26 2.084(2) . ? Co1 O25 2.105(2) . ? Co1 O28 2.120(2) . ? Co1 N23 2.136(2) 2_645 ? Co1 N1 2.143(2) . ? N1 C6 1.338(3) . ? N1 C2 1.338(4) . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C4 C5 1.389(4) . ? C4 H4 0.9300 . ? C5 C6 1.389(4) . ? C5 N7 1.415(3) . ? C6 H6 0.9300 . ? N7 C8 1.354(3) . ? N7 H7 0.8600 . ? C8 O9 1.238(3) . ? C8 C10 1.493(4) . ? C10 C15 1.394(4) . ? C10 C11 1.396(4) . ? C11 C12 1.385(4) . ? C11 H11 0.97(3) . ? C12 C13 1.379(4) . ? C12 H12 0.9300 . ? C13 C14 1.401(4) . ? C13 H13 0.9300 . ? C14 C15 1.386(4) . ? C14 C16 1.498(4) . ? C15 H15 0.9300 . ? C16 O17 1.229(3) . ? C16 N18 1.355(3) . ? N18 C19 1.411(3) . ? N18 H18 0.8600 . ? C19 C24 1.391(4) . ? C19 C20 1.392(4) . ? C20 C21 1.386(4) . ? C20 H20 0.96(3) . ? C21 C22 1.381(4) . ? C21 H21 0.9300 . ? C22 N23 1.336(4) . ? C22 H22 0.9300 . ? N23 C24 1.337(3) . ? N23 Co1 2.136(2) 2_655 ? C24 H24 0.9300 . ? O25 H25A 0.8200 . ? O25 H25B 0.74(4) . ? O26 H26A 0.8200 . ? O26 H26B 0.79(4) . ? O27 H27A 0.8200 . ? O27 H27B 0.83(4) . ? O28 H28A 0.8200 . ? O28 H28B 0.75(4) . ? S29 O32 1.4689(19) . ? S29 O30 1.4752(19) . ? S29 O33 1.480(2) 1 ? S29 O33 1.480(2) . ? S29 O31 1.483(2) . ? O34 H34A 1.05(5) . ? O34 H34B 0.98(6) . ? O35 H35A 0.76(4) . ? O35 H35B 0.98(5) . ? O36 H36A 0.88(5) . ? O36 H36B 0.81(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O27 Co1 O26 177.63(8) . . ? O27 Co1 O25 90.50(8) . . ? O26 Co1 O25 91.56(8) . . ? O27 Co1 O28 89.78(8) . . ? O26 Co1 O28 88.15(8) . . ? O25 Co1 O28 179.39(9) . . ? O27 Co1 N23 90.34(8) . 2_645 ? O26 Co1 N23 90.77(8) . 2_645 ? O25 Co1 N23 91.59(9) . 2_645 ? O28 Co1 N23 88.96(9) . 2_645 ? O27 Co1 N1 91.24(8) . . ? O26 Co1 N1 87.66(8) . . ? O25 Co1 N1 88.28(9) . . ? O28 Co1 N1 91.16(9) . . ? N23 Co1 N1 178.42(8) 2_645 . ? C6 N1 C2 118.4(2) . . ? C6 N1 Co1 122.31(18) . . ? C2 N1 Co1 119.16(18) . . ? N1 C2 C3 122.1(3) . . ? N1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 118.1(2) . . ? C6 C5 N7 116.6(2) . . ? C4 C5 N7 125.3(2) . . ? N1 C6 C5 123.0(2) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? C8 N7 C5 126.8(2) . . ? C8 N7 H7 116.6 . . ? C5 N7 H7 116.6 . . ? O9 C8 N7 122.9(3) . . ? O9 C8 C10 119.6(2) . . ? N7 C8 C10 117.5(2) . . ? C15 C10 C11 120.1(3) . . ? C15 C10 C8 123.1(2) . . ? C11 C10 C8 116.7(2) . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 122.6(18) . . ? C10 C11 H11 117.3(19) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.1(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 C16 123.1(2) . . ? C13 C14 C16 116.9(2) . . ? C14 C15 C10 119.7(3) . . ? C14 C15 H15 120.2 . . ? C10 C15 H15 120.2 . . ? O17 C16 N18 122.9(3) . . ? O17 C16 C14 120.3(2) . . ? N18 C16 C14 116.7(2) . . ? C16 N18 C19 126.9(2) . . ? C16 N18 H18 116.5 . . ? C19 N18 H18 116.5 . . ? C24 C19 C20 118.5(2) . . ? C24 C19 N18 117.1(2) . . ? C20 C19 N18 124.4(2) . . ? C21 C20 C19 118.0(3) . . ? C21 C20 H20 121.2(19) . . ? C19 C20 H20 120.7(19) . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? N23 C22 C21 122.7(3) . . ? N23 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C22 N23 C24 118.0(2) . . ? C22 N23 Co1 121.30(18) . 2_655 ? C24 N23 Co1 120.66(18) . 2_655 ? N23 C24 C19 123.1(2) . . ? N23 C24 H24 118.4 . . ? C19 C24 H24 118.4 . . ? Co1 O25 H25A 109.5 . . ? Co1 O25 H25B 121(3) . . ? H25A O25 H25B 110.3 . . ? Co1 O26 H26A 109.5 . . ? Co1 O26 H26B 119(3) . . ? H26A O26 H26B 126.5 . . ? Co1 O27 H27A 109.5 . . ? Co1 O27 H27B 118(2) . . ? H27A O27 H27B 112.7 . . ? Co1 O28 H28A 109.5 . . ? Co1 O28 H28B 120(3) . . ? H28A O28 H28B 119.2 . . ? O32 S29 O30 110.63(12) . . ? O32 S29 O33 109.44(12) . 1 ? O30 S29 O33 109.09(11) . 1 ? O32 S29 O33 109.44(12) . . ? O30 S29 O33 109.09(11) . . ? O32 S29 O31 109.20(11) . . ? O30 S29 O31 108.45(11) . . ? O33 S29 O31 110.02(13) 1 . ? O33 S29 O31 110.02(13) . . ? H34A O34 H34B 115(4) . . ? H35A O35 H35B 115(4) . . ? H36A O36 H36B 107(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7 H7 O33 0.86 2.36 3.182(3) 160.8 2_645 N18 H18 O33 0.86 2.51 3.329(3) 160.0 2_645 O25 H25A O32 0.82 1.93 2.734(3) 167.9 1_545 O25 H25B O17 0.74(4) 2.09(4) 2.832(3) 173(4) 2_745 O26 H26A O31 0.82 1.93 2.682(3) 152.8 1_545 O26 H26B O36 0.79(4) 1.92(4) 2.702(3) 170(4) 3_656 O27 H27A O31 0.82 1.96 2.719(3) 153.0 2_645 O27 H27B O35 0.83(4) 1.80(4) 2.623(3) 174(4) 1 O28 H28A O30 0.82 1.91 2.710(3) 166.1 2_645 O28 H28B O9 0.75(4) 2.12(4) 2.864(3) 173(4) 1_455 O34 H34A O36 1.05(5) 1.79(5) 2.837(3) 177(4) 3_666 O34 H34B O33 0.98(6) 1.86(6) 2.816(3) 165(5) 1 O35 H35A O32 0.76(4) 1.97(4) 2.712(3) 166(4) 3_665 O35 H35B O34 0.98(5) 1.84(5) 2.795(3) 167(4) 2_645 O36 H36A O9 0.88(5) 1.96(5) 2.797(3) 159(4) 3_756 O36 H36B O30 0.81(5) 1.84(5) 2.647(3) 175(4) 2_645 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.992 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.098