# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ivan Lukes' _publ_contact_author_name 'Ivan Lukes' _publ_contact_author_address ; Hlavova 2030 Prague 2 Cz 128 40 ; _publ_contact_author_email lukes@natur.cuni.cz # Attachment '- lukes.cif' data_9n2o _database_code_depnum_ccdc_archive 'CCDC 819615' #TrackingRef '- lukes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 N2 O, 2(Br)' _chemical_formula_sum 'C6 H16 Br2 N2 O' _chemical_formula_weight 292.03 _chemical_compound_source 'synthesized by the authors' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 12.3828(2) _cell_length_b 8.3185(2) _cell_length_c 9.8806(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1017.76(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 7267 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 7.920 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.334 _exptl_absorpt_correction_T_max 0.468 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13656 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2335 _reflns_number_gt 2222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0197P)^2^+0.5802P] 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 SHELXL _refine_ls_extinction_coef 0.0075(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(11) _refine_ls_number_reflns 2335 _refine_ls_number_parameters 101 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0463 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 O1 O 0.09156(16) 0.8754(3) 0.24386(19) 0.0195(4) Uani 1 1 d . . . C2 C 0.1343(3) 0.7219(4) 0.2088(3) 0.0210(7) Uani 1 1 d . . . H21 H 0.2127 0.7335 0.1920 0.025 Uiso 1 1 calc R . . H22 H 0.1004 0.6864 0.1231 0.025 Uiso 1 1 calc R . . C3 C 0.1176(3) 0.5921(3) 0.3143(3) 0.0221(6) Uani 1 1 d . . . H31 H 0.1383 0.4867 0.2756 0.026 Uiso 1 1 calc R . . H32 H 0.1652 0.6134 0.3928 0.026 Uiso 1 1 calc R . . N4 N 0.0023(2) 0.5853(3) 0.3610(2) 0.0203(5) Uani 1 1 d . . . H41 H -0.0397 0.6315 0.2947 0.024 Uiso 1 1 calc R . . H42 H -0.0172 0.4788 0.3661 0.024 Uiso 1 1 calc R . . C5 C -0.0271(3) 0.6627(3) 0.4930(3) 0.0197(6) Uani 1 1 d . . . H51 H 0.0323 0.6439 0.5581 0.024 Uiso 1 1 calc R . . H52 H -0.0923 0.6088 0.5290 0.024 Uiso 1 1 calc R . . C6 C -0.0489(2) 0.8423(4) 0.4861(3) 0.0201(6) Uani 1 1 d . . . H61 H -0.0649 0.8712 0.3910 0.024 Uiso 1 1 calc R . . H62 H -0.1144 0.8659 0.5402 0.024 Uiso 1 1 calc R . . N7 N 0.0416(2) 0.9482(3) 0.5360(2) 0.0210(5) Uani 1 1 d . . . H71 H 0.0212 1.0532 0.5216 0.025 Uiso 1 1 calc R . . H72 H 0.0466 0.9342 0.6281 0.025 Uiso 1 1 calc R . . C8 C 0.1522(2) 0.9280(4) 0.4786(3) 0.0209(6) Uani 1 1 d . . . H81 H 0.1750 0.8148 0.4899 0.025 Uiso 1 1 calc R . . H82 H 0.2032 0.9963 0.5301 0.025 Uiso 1 1 calc R . . C9 C 0.1584(2) 0.9723(3) 0.3300(3) 0.0196(6) Uani 1 1 d . . . H91 H 0.1369 1.0863 0.3195 0.023 Uiso 1 1 calc R . . H92 H 0.2343 0.9624 0.2997 0.023 Uiso 1 1 calc R . . Br1 Br 0.41896(2) 0.77742(3) 0.33640(3) 0.01886(8) Uani 1 1 d . . . Br2 Br 0.32859(2) 0.32392(3) 0.12317(3) 0.02617(9) 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 O1 0.0212(11) 0.0166(10) 0.0206(10) 0.0013(8) -0.0019(8) 0.0018(9) C2 0.0250(17) 0.0233(16) 0.0147(14) -0.0021(12) 0.0012(12) 0.0010(12) C3 0.0292(16) 0.0155(14) 0.0215(16) -0.0040(11) -0.0006(12) 0.0027(12) N4 0.0278(14) 0.0130(12) 0.0200(13) 0.0017(9) -0.0010(10) -0.0038(10) C5 0.0237(16) 0.0162(14) 0.0193(14) 0.0012(11) 0.0040(12) -0.0025(12) C6 0.0204(15) 0.0165(15) 0.0234(15) 0.0005(11) 0.0017(12) 0.0023(12) N7 0.0283(14) 0.0152(12) 0.0196(12) -0.0013(10) 0.0024(10) -0.0002(11) C8 0.0220(15) 0.0175(15) 0.0232(15) -0.0021(12) -0.0034(12) -0.0004(12) C9 0.0180(13) 0.0155(13) 0.0252(14) 0.0021(14) 0.0027(13) -0.0006(10) Br1 0.02274(14) 0.01316(13) 0.02068(13) -0.00024(13) -0.00175(13) 0.00113(11) Br2 0.02579(16) 0.02408(15) 0.02864(16) -0.00367(14) -0.00464(13) 0.00061(13) _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 O1 C2 1.425(4) . ? O1 C9 1.435(3) . ? C2 C3 1.515(4) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C3 N4 1.502(4) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? N4 C5 1.499(4) . ? N4 H41 0.9200 . ? N4 H42 0.9200 . ? C5 C6 1.520(4) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N7 1.508(4) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N7 C8 1.492(4) . ? N7 H71 0.9200 . ? N7 H72 0.9200 . ? C8 C9 1.516(4) . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 H91 0.9900 . ? C9 H92 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 C2 O1 C9 115.7(2) . . ? O1 C2 C3 114.9(2) . . ? O1 C2 H21 108.5 . . ? C3 C2 H21 108.5 . . ? O1 C2 H22 108.5 . . ? C3 C2 H22 108.5 . . ? H21 C2 H22 107.5 . . ? N4 C3 C2 111.6(2) . . ? N4 C3 H31 109.3 . . ? C2 C3 H31 109.3 . . ? N4 C3 H32 109.3 . . ? C2 C3 H32 109.3 . . ? H31 C3 H32 108.0 . . ? C5 N4 C3 118.8(2) . . ? C5 N4 H41 107.6 . . ? C3 N4 H41 107.6 . . ? C5 N4 H42 107.6 . . ? C3 N4 H42 107.6 . . ? H41 N4 H42 107.0 . . ? N4 C5 C6 115.3(2) . . ? N4 C5 H51 108.5 . . ? C6 C5 H51 108.5 . . ? N4 C5 H52 108.5 . . ? C6 C5 H52 108.5 . . ? H51 C5 H52 107.5 . . ? N7 C6 C5 115.3(2) . . ? N7 C6 H61 108.4 . . ? C5 C6 H61 108.4 . . ? N7 C6 H62 108.4 . . ? C5 C6 H62 108.4 . . ? H61 C6 H62 107.5 . . ? C8 N7 C6 119.5(2) . . ? C8 N7 H71 107.4 . . ? C6 N7 H71 107.4 . . ? C8 N7 H72 107.4 . . ? C6 N7 H72 107.4 . . ? H71 N7 H72 107.0 . . ? N7 C8 C9 112.8(2) . . ? N7 C8 H81 109.0 . . ? C9 C8 H81 109.0 . . ? N7 C8 H82 109.0 . . ? C9 C8 H82 109.0 . . ? H81 C8 H82 107.8 . . ? O1 C9 C8 114.1(2) . . ? O1 C9 H91 108.7 . . ? C8 C9 H91 108.7 . . ? O1 C9 H92 108.7 . . ? C8 C9 H92 108.7 . . ? H91 C9 H92 107.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.310 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.073 _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; #==END data_n2opph _database_code_depnum_ccdc_archive 'CCDC 819616' #TrackingRef '- lukes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H27 N2 O5 P2, H4 N, 2(H2 O)' _chemical_formula_sum 'C20 H35 N3 O7 P2' _chemical_formula_weight 491.45 _chemical_compound_source 'synthesized by the authors' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.28540(10) _cell_length_b 19.6410(2) _cell_length_c 25.1887(2) _cell_angle_alpha 87.6708(4) _cell_angle_beta 84.8707(5) _cell_angle_gamma 82.4380(5) _cell_volume 5021.91(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 19623 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29411 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.04 _reflns_number_total 19457 _reflns_number_gt 16097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0348P)^2^+13.3556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19457 _refine_ls_number_parameters 1153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 O1A O 0.3387(2) 0.76474(13) 0.07159(11) 0.0358(6) Uani 1 1 d . . . C2A C 0.4367(4) 0.7272(2) 0.10216(18) 0.0398(9) Uani 1 1 d . . . H2A H 0.3964 0.7179 0.1385 0.048 Uiso 1 1 calc R . . H2B H 0.5074 0.7560 0.1055 0.048 Uiso 1 1 calc R . . C3A C 0.4970(4) 0.6597(2) 0.07807(17) 0.0351(9) Uani 1 1 d . . . H3A H 0.5185 0.6677 0.0394 0.042 Uiso 1 1 calc R . . H3B H 0.5807 0.6443 0.0941 0.042 Uiso 1 1 calc R . . N4A N 0.4138(3) 0.60412(15) 0.08514(12) 0.0271(6) Uani 1 1 d . . . C5A C 0.3543(3) 0.59014(18) 0.03655(14) 0.0287(7) Uani 1 1 d . . . H5A H 0.3028 0.5512 0.0444 0.034 Uiso 1 1 calc R . . H5B H 0.4260 0.5752 0.0090 0.034 Uiso 1 1 calc R . . C6A C 0.2656(3) 0.64898(18) 0.01333(14) 0.0278(7) Uani 1 1 d . . . H6A H 0.2445 0.6360 -0.0222 0.033 Uiso 1 1 calc R . . H6B H 0.3145 0.6892 0.0080 0.033 Uiso 1 1 calc R . . N7A N 0.1381(3) 0.67009(14) 0.04665(11) 0.0232(6) Uani 1 1 d . . . H7A H 0.0915 0.7048 0.0271 0.028 Uiso 1 1 calc R . . C8A C 0.1520(3) 0.69977(18) 0.09964(14) 0.0274(7) Uani 1 1 d . . . H8A H 0.2107 0.6666 0.1201 0.033 Uiso 1 1 calc R . . H8B H 0.0647 0.7065 0.1200 0.033 Uiso 1 1 calc R . . C9A C 0.2075(4) 0.76792(19) 0.09420(16) 0.0354(8) Uani 1 1 d . . . H9A H 0.1509 0.7999 0.0720 0.042 Uiso 1 1 calc R . . H9B H 0.2023 0.7876 0.1300 0.042 Uiso 1 1 calc R . . C10A C 0.4815(3) 0.53965(19) 0.10669(15) 0.0319(8) Uani 1 1 d . . . H10A H 0.5581 0.5502 0.1246 0.038 Uiso 1 1 calc R . . H10B H 0.5155 0.5094 0.0767 0.038 Uiso 1 1 calc R . . P1A P 0.37804(9) 0.49318(5) 0.15389(4) 0.0274(2) Uani 1 1 d . . . O11A O 0.2528(2) 0.47989(14) 0.13217(10) 0.0345(6) Uani 1 1 d . . . O12A O 0.4699(3) 0.43235(13) 0.17241(11) 0.0373(6) Uani 1 1 d . . . C11A C 0.3330(4) 0.55354(18) 0.20719(14) 0.0301(8) Uani 1 1 d . . . C12A C 0.4286(4) 0.5722(2) 0.23788(17) 0.0413(9) Uani 1 1 d . . . H12A H 0.5173 0.5516 0.2321 0.050 Uiso 1 1 calc R . . C13A C 0.3944(5) 0.6207(2) 0.27671(19) 0.0533(12) Uani 1 1 d . . . H13A H 0.4598 0.6336 0.2972 0.064 Uiso 1 1 calc R . . C14A C 0.2654(6) 0.6505(2) 0.28574(19) 0.0553(12) Uani 1 1 d . . . H14A H 0.2425 0.6840 0.3123 0.066 Uiso 1 1 calc R . . C15A C 0.1699(5) 0.6317(2) 0.25642(19) 0.0506(11) Uani 1 1 d . . . H15A H 0.0811 0.6520 0.2628 0.061 Uiso 1 1 calc R . . C16A C 0.2037(4) 0.5829(2) 0.21752(15) 0.0359(9) Uani 1 1 d . . . H16A H 0.1374 0.5695 0.1977 0.043 Uiso 1 1 calc R . . C20A C 0.0545(3) 0.61334(17) 0.05369(14) 0.0260(7) Uani 1 1 d . . . H20A H 0.0826 0.5832 0.0841 0.031 Uiso 1 1 calc R . . H20B H 0.0686 0.5855 0.0213 0.031 Uiso 1 1 calc R . . P2A P -0.12244(8) 0.64457(5) 0.06578(3) 0.02393(18) Uani 1 1 d . . . O21A O -0.1425(2) 0.71725(12) 0.04463(10) 0.0292(5) Uani 1 1 d . . . O22A O -0.1922(2) 0.59160(13) 0.04276(10) 0.0309(5) Uani 1 1 d . . . C21A C -0.1619(3) 0.64293(18) 0.13732(14) 0.0262(7) Uani 1 1 d . . . C22A C -0.1410(4) 0.58097(19) 0.16686(15) 0.0322(8) Uani 1 1 d . . . H22A H -0.1030 0.5404 0.1492 0.039 Uiso 1 1 calc R . . C23A C -0.1747(4) 0.5779(2) 0.22097(16) 0.0403(9) Uani 1 1 d . . . H23A H -0.1597 0.5356 0.2404 0.048 Uiso 1 1 calc R . . C24A C -0.2310(4) 0.6375(2) 0.24716(16) 0.0449(10) Uani 1 1 d . . . H24A H -0.2538 0.6359 0.2845 0.054 Uiso 1 1 calc R . . C25A C -0.2535(4) 0.6986(2) 0.21838(17) 0.0449(10) Uani 1 1 d . . . H25A H -0.2937 0.7389 0.2360 0.054 Uiso 1 1 calc R . . C26A C -0.2178(4) 0.70177(19) 0.16391(15) 0.0333(8) Uani 1 1 d . . . H26A H -0.2317 0.7444 0.1447 0.040 Uiso 1 1 calc R . . O1C O 0.5648(2) 0.83567(15) 1.00990(10) 0.0362(6) Uani 1 1 d . . . C2C C 0.4671(4) 0.8661(2) 0.97568(15) 0.0397(10) Uani 1 1 d . . . H2C H 0.4962 0.9083 0.9583 0.048 Uiso 1 1 calc R . . H2D H 0.3836 0.8796 0.9976 0.048 Uiso 1 1 calc R . . C3C C 0.4425(3) 0.8183(2) 0.93317(15) 0.0348(9) Uani 1 1 d . . . H3C H 0.4333 0.7725 0.9499 0.042 Uiso 1 1 calc R . . H3D H 0.3582 0.8358 0.9183 0.042 Uiso 1 1 calc R . . N4C N 0.5474(3) 0.81068(15) 0.88931(11) 0.0253(6) Uani 1 1 d . . . C5C C 0.6309(3) 0.74452(17) 0.88912(14) 0.0275(7) Uani 1 1 d . . . H5C H 0.6941 0.7433 0.8570 0.033 Uiso 1 1 calc R . . H5D H 0.5749 0.7077 0.8862 0.033 Uiso 1 1 calc R . . C6C C 0.7074(3) 0.72887(18) 0.93787(15) 0.0282(7) Uani 1 1 d . . . H6C H 0.7471 0.6802 0.9371 0.034 Uiso 1 1 calc R . . H6D H 0.6446 0.7342 0.9700 0.034 Uiso 1 1 calc R . . N7C N 0.8158(3) 0.77291(14) 0.94348(11) 0.0242(6) Uani 1 1 d . . . H7C H 0.8563 0.7566 0.9739 0.029 Uiso 1 1 calc R . . C8C C 0.7682(3) 0.84785(17) 0.95161(14) 0.0256(7) Uani 1 1 d . . . H8C H 0.7152 0.8656 0.9219 0.031 Uiso 1 1 calc R . . H8D H 0.8455 0.8733 0.9501 0.031 Uiso 1 1 calc R . . C9C C 0.6863(4) 0.8624(2) 1.00387(15) 0.0347(8) Uani 1 1 d . . . H9C H 0.7390 0.8434 1.0333 0.042 Uiso 1 1 calc R . . H9D H 0.6688 0.9128 1.0078 0.042 Uiso 1 1 calc R . . C10C C 0.5019(3) 0.82889(18) 0.83610(13) 0.0256(7) Uani 1 1 d . . . H10C H 0.4130 0.8555 0.8400 0.031 Uiso 1 1 calc R . . H10D H 0.4958 0.7864 0.8171 0.031 Uiso 1 1 calc R . . P1C P 0.61454(8) 0.87956(4) 0.79733(3) 0.02248(18) Uani 1 1 d . . . O11C O 0.7517(2) 0.84048(12) 0.79592(10) 0.0272(5) Uani 1 1 d . . . O12C O 0.5624(2) 0.89949(13) 0.74409(9) 0.0297(5) Uani 1 1 d . . . C11C C 0.6109(3) 0.95626(17) 0.83551(13) 0.0266(7) Uani 1 1 d . . . C12C C 0.4919(4) 0.9947(2) 0.85186(15) 0.0351(8) Uani 1 1 d . . . H12C H 0.4116 0.9800 0.8439 0.042 Uiso 1 1 calc R . . C13C C 0.4895(5) 1.0545(2) 0.87986(17) 0.0449(10) Uani 1 1 d . . . H13C H 0.4077 1.0805 0.8909 0.054 Uiso 1 1 calc R . . C14C C 0.6058(5) 1.0762(2) 0.89162(16) 0.0470(11) Uani 1 1 d . . . H14C H 0.6040 1.1168 0.9111 0.056 Uiso 1 1 calc R . . C15C C 0.7239(5) 1.0390(2) 0.87515(18) 0.0466(11) Uani 1 1 d . . . H15C H 0.8039 1.0542 0.8829 0.056 Uiso 1 1 calc R . . C16C C 0.7270(4) 0.9788(2) 0.84709(16) 0.0361(9) Uani 1 1 d . . . H16C H 0.8091 0.9532 0.8359 0.043 Uiso 1 1 calc R . . C20C C 0.9195(3) 0.76433(17) 0.89774(13) 0.0244(7) Uani 1 1 d . . . H20C H 0.8896 0.7943 0.8675 0.029 Uiso 1 1 calc R . . H20D H 0.9296 0.7162 0.8862 0.029 Uiso 1 1 calc R . . P2C P 1.08139(8) 0.78511(4) 0.91341(3) 0.02257(18) Uani 1 1 d . . . O21C O 1.0895(2) 0.76827(13) 0.97161(10) 0.0296(5) Uani 1 1 d . . . O22C O 1.1792(2) 0.74947(12) 0.87245(10) 0.0291(5) Uani 1 1 d . . . C21C C 1.0866(3) 0.87702(17) 0.90390(13) 0.0241(7) Uani 1 1 d . . . C22C C 1.0840(4) 0.90851(19) 0.85367(15) 0.0316(8) Uani 1 1 d . . . H22C H 1.0737 0.8824 0.8238 0.038 Uiso 1 1 calc R . . C23C C 1.0963(4) 0.9776(2) 0.84675(17) 0.0419(10) Uani 1 1 d . . . H23C H 1.0932 0.9987 0.8122 0.050 Uiso 1 1 calc R . . C24C C 1.1131(4) 1.0162(2) 0.89009(19) 0.0448(10) Uani 1 1 d . . . H24C H 1.1226 1.0636 0.8852 0.054 Uiso 1 1 calc R . . C25C C 1.1159(4) 0.9855(2) 0.94020(18) 0.0432(10) Uani 1 1 d . . . H25C H 1.1271 1.0118 0.9699 0.052 Uiso 1 1 calc R . . C26C C 1.1024(3) 0.91628(19) 0.94725(15) 0.0319(8) Uani 1 1 d . . . H26C H 1.1038 0.8954 0.9819 0.038 Uiso 1 1 calc R . . O1E O 0.9933(3) 0.73584(14) 0.42370(11) 0.0386(6) Uani 1 1 d . . . C2E C 1.0885(4) 0.7744(2) 0.39584(17) 0.0379(9) Uani 1 1 d . . . H2E H 1.0626 0.7858 0.3593 0.045 Uiso 1 1 calc R . . H2F H 1.1749 0.7454 0.3928 0.045 Uiso 1 1 calc R . . C3E C 1.1028(4) 0.8405(2) 0.42284(16) 0.0350(8) Uani 1 1 d . . . H3E H 1.1078 0.8303 0.4615 0.042 Uiso 1 1 calc R . . H3F H 1.1874 0.8560 0.4088 0.042 Uiso 1 1 calc R . . N4E N 0.9973(3) 0.89745(15) 0.41615(12) 0.0277(6) Uani 1 1 d . . . C5E C 0.9080(3) 0.91015(18) 0.46397(14) 0.0286(7) Uani 1 1 d . . . H5E H 0.8406 0.9492 0.4562 0.034 Uiso 1 1 calc R . . H5F H 0.9586 0.9243 0.4924 0.034 Uiso 1 1 calc R . . C6E C 0.8385(3) 0.85011(19) 0.48516(14) 0.0294(8) Uani 1 1 d . . . H6E H 0.9055 0.8096 0.4892 0.035 Uiso 1 1 calc R . . H6F H 0.7957 0.8611 0.5211 0.035 Uiso 1 1 calc R . . N7E N 0.7362(3) 0.83089(14) 0.45124(11) 0.0253(6) Uani 1 1 d . . . H7E H 0.7000 0.7948 0.4695 0.030 Uiso 1 1 calc R . . C8E C 0.7883(3) 0.80473(18) 0.39733(14) 0.0271(7) Uani 1 1 d . . . H8E H 0.8400 0.8388 0.3785 0.033 Uiso 1 1 calc R . . H8F H 0.7131 0.8003 0.3763 0.033 Uiso 1 1 calc R . . C9E C 0.8741(4) 0.7360(2) 0.39973(17) 0.0373(9) Uani 1 1 d . . . H9E H 0.8226 0.7026 0.4196 0.045 Uiso 1 1 calc R . . H9F H 0.8953 0.7196 0.3629 0.045 Uiso 1 1 calc R . . C10E C 1.0455(4) 0.96204(19) 0.39621(15) 0.0312(8) Uani 1 1 d . . . H10E H 1.1372 0.9515 0.3803 0.037 Uiso 1 1 calc R . . H10F H 1.0467 0.9922 0.4267 0.037 Uiso 1 1 calc R . . P1E P 0.94629(9) 1.00824(5) 0.34678(4) 0.0281(2) Uani 1 1 d . . . O11E O 0.8045(3) 1.02501(14) 0.36691(11) 0.0372(6) Uani 1 1 d . . . O12E O 1.0209(3) 1.06644(14) 0.32669(11) 0.0387(6) Uani 1 1 d . . . C11E C 0.9530(4) 0.94550(19) 0.29543(15) 0.0314(8) Uani 1 1 d . . . C12E C 1.0721(4) 0.9176(2) 0.27013(17) 0.0459(10) Uani 1 1 d . . . H12E H 1.1513 0.9337 0.2779 0.055 Uiso 1 1 calc R . . C13E C 1.0763(5) 0.8661(3) 0.2333(2) 0.0599(13) Uani 1 1 d . . . H13E H 1.1585 0.8464 0.2168 0.072 Uiso 1 1 calc R . . C14E C 0.9620(5) 0.8438(3) 0.2207(2) 0.0574(13) Uani 1 1 d . . . H14E H 0.9653 0.8085 0.1958 0.069 Uiso 1 1 calc R . . C15E C 0.8428(5) 0.8725(2) 0.24434(18) 0.0489(11) Uani 1 1 d . . . H15E H 0.7636 0.8579 0.2350 0.059 Uiso 1 1 calc R . . C16E C 0.8382(4) 0.9225(2) 0.28152(15) 0.0350(8) Uani 1 1 d . . . H16E H 0.7555 0.9416 0.2980 0.042 Uiso 1 1 calc R . . C20E C 0.6258(3) 0.88735(18) 0.44668(14) 0.0285(7) Uani 1 1 d . . . H20E H 0.6499 0.9194 0.4172 0.034 Uiso 1 1 calc R . . H20F H 0.6123 0.9133 0.4801 0.034 Uiso 1 1 calc R . . P2E P 0.47063(9) 0.85568(5) 0.43424(3) 0.02552(19) Uani 1 1 d . . . O21E O 0.4792(2) 0.78266(13) 0.45490(9) 0.0302(5) Uani 1 1 d . . . O22E O 0.3642(2) 0.90822(13) 0.45758(10) 0.0331(6) Uani 1 1 d . . . C21E C 0.4627(3) 0.85771(18) 0.36275(14) 0.0262(7) Uani 1 1 d . . . C22E C 0.4650(4) 0.91994(19) 0.33397(15) 0.0339(8) Uani 1 1 d . . . H22E H 0.4721 0.9605 0.3522 0.041 Uiso 1 1 calc R . . C23E C 0.4572(4) 0.9235(2) 0.27956(16) 0.0396(9) Uani 1 1 d . . . H23E H 0.4594 0.9661 0.2605 0.048 Uiso 1 1 calc R . . C24E C 0.4461(4) 0.8641(2) 0.25283(16) 0.0430(10) Uani 1 1 d . . . H24E H 0.4407 0.8662 0.2153 0.052 Uiso 1 1 calc R . . C25E C 0.4429(4) 0.8024(2) 0.28054(16) 0.0411(9) Uani 1 1 d . . . H25E H 0.4340 0.7622 0.2622 0.049 Uiso 1 1 calc R . . C26E C 0.4526(4) 0.7990(2) 0.33553(15) 0.0337(8) Uani 1 1 d . . . H26E H 0.4523 0.7561 0.3544 0.040 Uiso 1 1 calc R . . O1G O 0.2246(2) 0.67178(13) 0.48664(10) 0.0312(6) Uani 1 1 d . . . C2G C 0.1242(4) 0.6425(2) 0.51927(14) 0.0313(8) Uani 1 1 d . . . H2G H 0.1629 0.5984 0.5352 0.038 Uiso 1 1 calc R . . H2H H 0.0557 0.6325 0.4965 0.038 Uiso 1 1 calc R . . C3G C 0.0601(3) 0.68874(18) 0.56355(14) 0.0280(7) Uani 1 1 d . . . H3G H 0.0386 0.7358 0.5485 0.034 Uiso 1 1 calc R . . H3H H -0.0236 0.6723 0.5776 0.034 Uiso 1 1 calc R . . N4G N 0.1424(3) 0.69142(14) 0.60774(11) 0.0233(6) Uani 1 1 d . . . C5G C 0.1963(3) 0.75647(16) 0.61071(14) 0.0244(7) Uani 1 1 d . . . H5G H 0.2456 0.7547 0.6428 0.029 Uiso 1 1 calc R . . H5H H 0.1223 0.7941 0.6151 0.029 Uiso 1 1 calc R . . C6G C 0.2869(3) 0.77345(17) 0.56238(14) 0.0257(7) Uani 1 1 d . . . H6G H 0.2401 0.7704 0.5300 0.031 Uiso 1 1 calc R . . H6H H 0.3036 0.8217 0.5646 0.031 Uiso 1 1 calc R . . N7G N 0.4182(3) 0.72850(14) 0.55541(11) 0.0228(6) Uani 1 1 d . . . H7G H 0.4640 0.7456 0.5253 0.027 Uiso 1 1 calc R . . C8G C 0.4091(3) 0.65413(17) 0.54548(14) 0.0263(7) Uani 1 1 d . . . H8G H 0.3514 0.6359 0.5748 0.032 Uiso 1 1 calc R . . H8H H 0.4978 0.6277 0.5464 0.032 Uiso 1 1 calc R . . C9G C 0.3562(3) 0.64240(19) 0.49287(15) 0.0314(8) Uani 1 1 d . . . H9G H 0.4141 0.6610 0.4638 0.038 Uiso 1 1 calc R . . H9H H 0.3624 0.5922 0.4882 0.038 Uiso 1 1 calc R . . C10G C 0.0816(3) 0.67029(17) 0.66029(13) 0.0248(7) Uani 1 1 d . . . H10G H 0.0069 0.6449 0.6550 0.030 Uiso 1 1 calc R . . H10H H 0.0467 0.7117 0.6808 0.030 Uiso 1 1 calc R . . P1G P 0.20011(8) 0.61617(4) 0.69795(3) 0.02333(18) Uani 1 1 d . . . O11G O 0.3190(2) 0.65303(12) 0.70073(10) 0.0280(5) Uani 1 1 d . . . O12G O 0.1328(2) 0.59506(13) 0.75054(10) 0.0308(5) Uani 1 1 d . . . C11G C 0.2487(3) 0.54095(17) 0.65734(13) 0.0239(7) Uani 1 1 d . . . C12G C 0.1537(4) 0.50525(18) 0.63900(15) 0.0314(8) Uani 1 1 d . . . H12G H 0.0629 0.5201 0.6479 0.038 Uiso 1 1 calc R . . C13G C 0.1912(4) 0.4481(2) 0.60773(17) 0.0400(9) Uani 1 1 d . . . H13G H 0.1259 0.4245 0.5949 0.048 Uiso 1 1 calc R . . C14G C 0.3230(4) 0.4255(2) 0.59528(17) 0.0409(9) Uani 1 1 d . . . H14G H 0.3483 0.3862 0.5741 0.049 Uiso 1 1 calc R . . C15G C 0.4180(4) 0.4601(2) 0.61370(17) 0.0401(9) Uani 1 1 d . . . H15G H 0.5086 0.4446 0.6053 0.048 Uiso 1 1 calc R . . C16G C 0.3801(4) 0.51773(19) 0.64466(15) 0.0316(8) Uani 1 1 d . . . H16G H 0.4456 0.5414 0.6572 0.038 Uiso 1 1 calc R . . C20G C 0.4993(3) 0.73414(17) 0.60140(13) 0.0243(7) Uani 1 1 d . . . H20G H 0.4719 0.7025 0.6307 0.029 Uiso 1 1 calc R . . H20H H 0.4805 0.7815 0.6147 0.029 Uiso 1 1 calc R . . P2G P 0.67770(8) 0.71409(4) 0.58468(3) 0.02212(18) Uani 1 1 d . . . O21G O 0.7022(2) 0.73226(13) 0.52666(10) 0.0305(5) Uani 1 1 d . . . O22G O 0.7403(2) 0.74844(12) 0.62596(10) 0.0282(5) Uani 1 1 d . . . C21G C 0.7237(3) 0.62206(17) 0.59277(13) 0.0228(7) Uani 1 1 d . . . C22G C 0.7107(4) 0.58843(18) 0.64215(14) 0.0291(7) Uani 1 1 d . . . H22G H 0.6727 0.6133 0.6725 0.035 Uiso 1 1 calc R . . C23G C 0.7533(4) 0.51837(19) 0.64731(17) 0.0380(9) Uani 1 1 d . . . H23G H 0.7432 0.4954 0.6811 0.046 Uiso 1 1 calc R . . C24G C 0.8102(4) 0.48208(19) 0.60327(19) 0.0402(10) Uani 1 1 d . . . H24G H 0.8395 0.4343 0.6068 0.048 Uiso 1 1 calc R . . C25G C 0.8241(4) 0.5154(2) 0.55436(18) 0.0414(10) Uani 1 1 d . . . H25G H 0.8634 0.4905 0.5242 0.050 Uiso 1 1 calc R . . C26G C 0.7811(4) 0.58486(19) 0.54898(15) 0.0317(8) Uani 1 1 d . . . H26G H 0.7908 0.6074 0.5150 0.038 Uiso 1 1 calc R . . N1I N 0.2600(3) 0.61138(15) 0.84321(12) 0.0290(6) Uani 1 1 d . . . H1I H 0.3495 0.6024 0.8369 0.035 Uiso 1 1 d R . . H1J H 0.2311 0.5795 0.8686 0.035 Uiso 1 1 d R . . H1K H 0.2423 0.6517 0.8546 0.035 Uiso 1 1 d R . . H1L H 0.2276 0.6012 0.8121 0.035 Uiso 1 1 d R . . N2I N 0.2342(3) 0.77505(15) 0.76098(12) 0.0285(6) Uani 1 1 d . . . H2I H 0.2298 0.7750 0.7994 0.034 Uiso 1 1 d R . . H2J H 0.1496 0.7828 0.7528 0.034 Uiso 1 1 d R . . H2K H 0.2576 0.7341 0.7449 0.034 Uiso 1 1 d R . . H2L H 0.2838 0.8042 0.7450 0.034 Uiso 1 1 d R . . N3I N 0.7435(3) 0.88628(15) 0.65370(12) 0.0284(6) Uani 1 1 d . . . H3I H 0.6893 0.8915 0.6868 0.034 Uiso 1 1 d R . . H3J H 0.7489 0.8412 0.6448 0.034 Uiso 1 1 d R . . H3K H 0.7027 0.9143 0.6245 0.034 Uiso 1 1 d R . . H3L H 0.8167 0.9017 0.6597 0.034 Uiso 1 1 d R . . N4I N 0.7537(3) 0.71922(15) 0.73714(12) 0.0287(6) Uani 1 1 d . . . H4I H 0.7559 0.7624 0.7548 0.034 Uiso 1 1 d R . . H4J H 0.6677 0.7069 0.7431 0.034 Uiso 1 1 d R . . H4K H 0.7704 0.7215 0.7014 0.034 Uiso 1 1 d R . . H4L H 0.8122 0.6912 0.7521 0.034 Uiso 1 1 d R . . O1W O 0.8488(3) 0.45561(14) 0.06958(10) 0.0381(6) Uani 1 1 d . . . H1W H 0.9431 0.4493 0.0667 0.046 Uiso 1 1 d R . . H1X H 0.8387 0.5031 0.0603 0.046 Uiso 1 1 d R . . O2W O 0.6055(3) 0.06888(16) 0.43851(12) 0.0461(7) Uani 1 1 d . . . H2W H 0.6381 0.0744 0.4722 0.055 Uiso 1 1 d R . . H2X H 0.6903 0.0542 0.4179 0.055 Uiso 1 1 d R . . O3W O 0.5166(3) 0.67290(13) 0.75884(11) 0.0370(6) Uani 1 1 d . . . H3W H 0.5283 0.6344 0.7786 0.044 Uiso 1 1 d R . . H3X H 0.4532 0.6618 0.7362 0.044 Uiso 1 1 d R . . O4W O 0.1114(3) 0.42893(15) 0.06222(11) 0.0449(7) Uani 1 1 d . . . H4W H 0.1594 0.4231 0.0288 0.054 Uiso 1 1 d R . . H4X H 0.1704 0.4429 0.0835 0.054 Uiso 1 1 d R . . O5W O 0.3590(3) 0.04407(14) 0.43264(11) 0.0400(6) Uani 1 1 d . . . H5W H 0.3530 -0.0022 0.4414 0.048 Uiso 1 1 d R . . H5X H 0.4515 0.0524 0.4332 0.048 Uiso 1 1 d R . . O6W O 0.9850(2) 0.82444(13) 0.73836(11) 0.0368(6) Uani 1 1 d . . . H6W H 0.9838 0.8617 0.7182 0.044 Uiso 1 1 d R . . H6X H 0.9059 0.8347 0.7591 0.044 Uiso 1 1 d R . . O7W O 0.6529(3) 0.12704(18) 0.30293(15) 0.0630(10) Uani 1 1 d . . . H7W H 0.7115 0.1000 0.3200 0.076 Uiso 1 1 d R . . H7X H 0.5915 0.1078 0.2847 0.076 Uiso 1 1 d R . . O8W O 0.1145(3) 0.38076(19) 0.19925(16) 0.0723(12) Uani 1 1 d . . . H8W H 0.1553 0.4085 0.1788 0.087 Uiso 1 1 d R . . H8X H 0.0279 0.3912 0.2139 0.087 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0303(13) 0.0333(14) 0.0451(16) 0.0054(12) -0.0062(12) -0.0088(11) C2A 0.035(2) 0.037(2) 0.052(3) 0.0017(18) -0.0120(18) -0.0148(17) C3A 0.0242(18) 0.038(2) 0.044(2) 0.0097(17) -0.0029(16) -0.0096(15) N4A 0.0234(14) 0.0271(15) 0.0301(16) 0.0073(12) -0.0015(12) -0.0031(11) C5A 0.0270(18) 0.0309(18) 0.0267(18) 0.0006(14) 0.0028(14) -0.0016(14) C6A 0.0273(18) 0.0307(18) 0.0239(17) 0.0022(14) 0.0039(14) -0.0030(14) N7A 0.0212(14) 0.0244(14) 0.0238(14) 0.0050(11) -0.0024(11) -0.0027(11) C8A 0.0248(17) 0.0329(19) 0.0243(17) -0.0043(14) 0.0019(13) -0.0050(14) C9A 0.034(2) 0.032(2) 0.041(2) -0.0077(17) -0.0039(16) -0.0054(16) C10A 0.0226(17) 0.0332(19) 0.037(2) 0.0086(16) 0.0007(15) 0.0019(14) P1A 0.0263(4) 0.0276(5) 0.0275(5) 0.0057(4) -0.0008(4) -0.0034(4) O11A 0.0334(14) 0.0398(15) 0.0312(14) 0.0004(11) -0.0033(11) -0.0083(11) O12A 0.0359(14) 0.0312(14) 0.0423(16) 0.0116(12) -0.0009(12) -0.0002(11) C11A 0.0339(19) 0.0273(18) 0.0284(19) 0.0090(14) -0.0027(15) -0.0044(15) C12A 0.041(2) 0.040(2) 0.045(2) -0.0013(18) -0.0047(18) -0.0128(18) C13A 0.070(3) 0.047(3) 0.048(3) -0.004(2) -0.010(2) -0.023(2) C14A 0.084(4) 0.038(2) 0.044(3) -0.012(2) 0.007(2) -0.013(2) C15A 0.059(3) 0.042(2) 0.046(3) -0.002(2) 0.007(2) 0.004(2) C16A 0.039(2) 0.038(2) 0.030(2) 0.0041(16) -0.0017(16) -0.0024(16) C20A 0.0295(18) 0.0225(16) 0.0256(18) 0.0012(13) -0.0017(14) -0.0032(13) P2A 0.0237(4) 0.0265(4) 0.0215(4) 0.0021(3) -0.0013(3) -0.0045(3) O21A 0.0311(13) 0.0287(13) 0.0267(13) 0.0061(10) -0.0025(10) -0.0015(10) O22A 0.0322(13) 0.0350(14) 0.0273(13) -0.0015(10) -0.0038(10) -0.0096(11) C21A 0.0231(16) 0.0302(18) 0.0262(18) 0.0011(14) -0.0011(13) -0.0085(14) C22A 0.038(2) 0.0302(19) 0.0278(19) 0.0013(15) 0.0002(15) -0.0065(15) C23A 0.053(2) 0.038(2) 0.030(2) 0.0122(17) -0.0006(18) -0.0135(18) C24A 0.056(3) 0.054(3) 0.025(2) 0.0001(18) 0.0097(18) -0.016(2) C25A 0.055(3) 0.039(2) 0.040(2) -0.0096(18) 0.0116(19) -0.0086(19) C26A 0.035(2) 0.0306(19) 0.033(2) 0.0000(15) 0.0043(16) -0.0046(15) O1C 0.0252(13) 0.0565(17) 0.0246(13) 0.0057(12) 0.0016(10) -0.0020(12) C2C 0.0283(19) 0.062(3) 0.0245(19) 0.0020(18) 0.0014(15) 0.0073(18) C3C 0.0234(18) 0.054(2) 0.0264(19) 0.0048(17) 0.0027(14) -0.0070(16) N4C 0.0213(14) 0.0317(16) 0.0230(15) 0.0005(12) 0.0001(11) -0.0049(11) C5C 0.0293(18) 0.0241(17) 0.0307(19) 0.0013(14) -0.0041(14) -0.0088(14) C6C 0.0278(18) 0.0236(17) 0.0340(19) 0.0074(14) -0.0029(15) -0.0080(14) N7C 0.0243(14) 0.0271(15) 0.0212(14) 0.0043(11) -0.0031(11) -0.0042(11) C8C 0.0232(16) 0.0261(17) 0.0271(18) -0.0008(14) -0.0010(13) -0.0032(13) C9C 0.0313(19) 0.039(2) 0.033(2) -0.0072(16) 0.0026(16) -0.0017(16) C10C 0.0230(16) 0.0296(18) 0.0247(17) 0.0008(14) -0.0036(13) -0.0050(13) P1C 0.0237(4) 0.0236(4) 0.0199(4) 0.0008(3) -0.0006(3) -0.0035(3) O11C 0.0242(12) 0.0272(12) 0.0290(13) 0.0016(10) 0.0016(10) -0.0017(9) O12C 0.0365(14) 0.0326(13) 0.0204(12) 0.0011(10) -0.0044(10) -0.0048(11) C11C 0.0356(19) 0.0243(17) 0.0200(17) 0.0039(13) -0.0008(14) -0.0065(14) C12C 0.038(2) 0.033(2) 0.033(2) -0.0018(16) 0.0039(16) -0.0055(16) C13C 0.061(3) 0.034(2) 0.036(2) -0.0050(17) 0.010(2) 0.0001(19) C14C 0.086(3) 0.026(2) 0.030(2) -0.0051(16) -0.004(2) -0.010(2) C15C 0.064(3) 0.034(2) 0.047(3) 0.0004(19) -0.018(2) -0.017(2) C16C 0.042(2) 0.031(2) 0.037(2) 0.0002(16) -0.0074(17) -0.0085(16) C20C 0.0259(17) 0.0252(17) 0.0208(16) -0.0014(13) 0.0011(13) -0.0007(13) P2C 0.0216(4) 0.0227(4) 0.0223(4) 0.0031(3) -0.0002(3) -0.0012(3) O21C 0.0302(13) 0.0330(13) 0.0255(13) 0.0085(10) -0.0041(10) -0.0054(10) O22C 0.0277(12) 0.0253(12) 0.0319(13) -0.0011(10) 0.0052(10) 0.0007(10) C21C 0.0183(15) 0.0265(17) 0.0264(17) 0.0001(13) 0.0027(13) -0.0017(13) C22C 0.0350(19) 0.0309(19) 0.0279(19) 0.0032(15) -0.0004(15) -0.0032(15) C23C 0.049(2) 0.035(2) 0.040(2) 0.0122(18) 0.0036(18) -0.0066(18) C24C 0.048(2) 0.027(2) 0.060(3) 0.0023(19) 0.003(2) -0.0112(17) C25C 0.043(2) 0.037(2) 0.051(3) -0.0123(19) -0.0012(19) -0.0108(18) C26C 0.0302(19) 0.034(2) 0.032(2) -0.0026(15) -0.0008(15) -0.0061(15) O1E 0.0323(14) 0.0342(14) 0.0478(17) 0.0061(12) 0.0010(12) -0.0041(11) C2E 0.031(2) 0.037(2) 0.043(2) 0.0033(17) 0.0048(17) -0.0006(16) C3E 0.0299(19) 0.039(2) 0.037(2) 0.0122(17) -0.0070(16) -0.0069(16) N4E 0.0248(15) 0.0307(16) 0.0284(16) 0.0039(12) -0.0008(12) -0.0097(12) C5E 0.0318(18) 0.0309(19) 0.0247(18) -0.0013(14) -0.0036(14) -0.0090(15) C6E 0.0283(18) 0.0349(19) 0.0262(18) 0.0044(15) -0.0048(14) -0.0088(15) N7E 0.0269(15) 0.0260(15) 0.0239(15) 0.0050(11) -0.0013(11) -0.0086(12) C8E 0.0269(17) 0.0301(18) 0.0250(18) -0.0044(14) -0.0003(14) -0.0062(14) C9E 0.036(2) 0.032(2) 0.045(2) -0.0079(17) -0.0008(17) -0.0053(16) C10E 0.0301(19) 0.034(2) 0.0320(19) 0.0048(15) -0.0038(15) -0.0147(15) P1E 0.0282(5) 0.0307(5) 0.0263(5) 0.0048(4) -0.0017(4) -0.0092(4) O11E 0.0322(14) 0.0453(16) 0.0331(15) -0.0005(12) 0.0013(11) -0.0044(12) O12E 0.0422(15) 0.0351(15) 0.0413(16) 0.0112(12) -0.0061(12) -0.0168(12) C11E 0.0318(19) 0.035(2) 0.0276(19) 0.0079(15) -0.0007(15) -0.0089(15) C12E 0.038(2) 0.061(3) 0.040(2) -0.010(2) 0.0015(18) -0.011(2) C13E 0.053(3) 0.071(3) 0.055(3) -0.025(3) 0.005(2) -0.004(2) C14E 0.073(3) 0.054(3) 0.049(3) -0.014(2) -0.003(2) -0.016(2) C15E 0.057(3) 0.052(3) 0.042(2) -0.002(2) -0.008(2) -0.023(2) C16E 0.036(2) 0.040(2) 0.031(2) 0.0016(16) -0.0005(16) -0.0142(17) C20E 0.0304(18) 0.0267(18) 0.0278(18) 0.0007(14) 0.0006(14) -0.0039(14) P2E 0.0262(4) 0.0289(5) 0.0216(4) 0.0030(3) -0.0004(3) -0.0064(3) O21E 0.0354(14) 0.0319(13) 0.0243(13) 0.0081(10) -0.0052(10) -0.0090(11) O22E 0.0304(13) 0.0371(14) 0.0304(14) -0.0025(11) 0.0032(10) -0.0021(11) C21E 0.0212(16) 0.0317(18) 0.0250(17) 0.0047(14) 0.0003(13) -0.0036(13) C22E 0.042(2) 0.0300(19) 0.0283(19) 0.0046(15) -0.0011(16) -0.0035(16) C23E 0.048(2) 0.038(2) 0.029(2) 0.0133(17) -0.0023(17) 0.0007(18) C24E 0.049(2) 0.055(3) 0.025(2) 0.0053(18) -0.0057(17) -0.009(2) C25E 0.049(2) 0.045(2) 0.031(2) -0.0022(18) -0.0057(18) -0.0135(19) C26E 0.038(2) 0.035(2) 0.0299(19) 0.0041(15) -0.0028(16) -0.0113(16) O1G 0.0283(13) 0.0401(15) 0.0262(13) 0.0011(11) -0.0030(10) -0.0081(11) C2G 0.0295(18) 0.039(2) 0.0277(19) -0.0022(15) -0.0036(15) -0.0110(15) C3G 0.0230(17) 0.0315(18) 0.0293(19) 0.0004(15) -0.0024(14) -0.0033(14) N4G 0.0204(13) 0.0258(14) 0.0240(14) -0.0042(11) 0.0000(11) -0.0043(11) C5G 0.0241(16) 0.0187(16) 0.0297(18) -0.0019(13) 0.0015(14) -0.0018(13) C6G 0.0264(17) 0.0218(16) 0.0279(18) 0.0046(13) -0.0025(14) -0.0011(13) N7G 0.0205(13) 0.0256(14) 0.0221(14) 0.0032(11) -0.0001(11) -0.0053(11) C8G 0.0243(17) 0.0235(17) 0.0305(18) -0.0003(14) 0.0007(14) -0.0026(13) C9G 0.0287(18) 0.0337(19) 0.032(2) -0.0056(15) 0.0008(15) -0.0062(15) C10G 0.0207(16) 0.0273(17) 0.0264(18) 0.0009(14) 0.0027(13) -0.0066(13) P1G 0.0253(4) 0.0240(4) 0.0208(4) 0.0010(3) -0.0001(3) -0.0055(3) O11G 0.0283(12) 0.0270(12) 0.0300(13) -0.0007(10) -0.0040(10) -0.0075(10) O12G 0.0345(14) 0.0335(14) 0.0235(13) 0.0028(10) 0.0052(10) -0.0075(11) C11G 0.0280(17) 0.0247(17) 0.0186(16) 0.0030(13) 0.0000(13) -0.0043(13) C12G 0.0303(19) 0.0277(18) 0.037(2) -0.0034(15) 0.0000(15) -0.0063(14) C13G 0.042(2) 0.033(2) 0.047(2) -0.0096(18) -0.0085(18) -0.0079(17) C14G 0.047(2) 0.033(2) 0.041(2) -0.0122(17) 0.0015(18) 0.0000(17) C15G 0.034(2) 0.041(2) 0.042(2) -0.0063(18) 0.0044(17) 0.0033(17) C16G 0.0310(19) 0.0303(19) 0.033(2) -0.0026(15) -0.0009(15) -0.0051(15) C20G 0.0275(17) 0.0247(17) 0.0212(16) 0.0011(13) -0.0020(13) -0.0062(13) P2G 0.0233(4) 0.0213(4) 0.0223(4) 0.0033(3) -0.0015(3) -0.0060(3) O21G 0.0306(13) 0.0337(14) 0.0261(13) 0.0115(10) 0.0008(10) -0.0063(10) O22G 0.0298(13) 0.0224(12) 0.0339(14) -0.0021(10) -0.0051(10) -0.0071(10) C21G 0.0228(16) 0.0229(16) 0.0243(17) 0.0005(13) -0.0042(13) -0.0080(13) C22G 0.0348(19) 0.0256(17) 0.0273(18) 0.0027(14) -0.0004(15) -0.0082(14) C23G 0.042(2) 0.0289(19) 0.043(2) 0.0143(17) -0.0048(18) -0.0070(16) C24G 0.034(2) 0.0212(18) 0.065(3) -0.0016(18) -0.0044(19) -0.0024(15) C25G 0.044(2) 0.034(2) 0.047(2) -0.0147(18) -0.0006(19) -0.0032(17) C26G 0.035(2) 0.035(2) 0.0261(18) -0.0031(15) -0.0010(15) -0.0087(16) N1I 0.0331(16) 0.0252(15) 0.0275(16) 0.0001(12) 0.0024(12) -0.0024(12) N2I 0.0306(16) 0.0266(15) 0.0277(16) -0.0015(12) -0.0014(12) -0.0018(12) N3I 0.0350(16) 0.0241(15) 0.0267(15) 0.0003(12) -0.0026(12) -0.0061(12) N4I 0.0300(15) 0.0271(15) 0.0296(16) -0.0005(12) -0.0012(12) -0.0066(12) O1W 0.0492(16) 0.0328(14) 0.0328(14) 0.0001(11) 0.0039(12) -0.0123(12) O2W 0.0464(17) 0.0556(19) 0.0360(16) -0.0087(14) 0.0025(13) -0.0076(14) O3W 0.0367(14) 0.0350(14) 0.0422(16) 0.0116(12) -0.0127(12) -0.0131(11) O4W 0.0469(17) 0.0541(18) 0.0355(16) -0.0119(13) -0.0015(13) -0.0112(14) O5W 0.0499(17) 0.0330(14) 0.0356(15) 0.0009(12) -0.0060(12) 0.0010(12) O6W 0.0311(14) 0.0336(14) 0.0422(16) 0.0098(12) 0.0061(11) -0.0005(11) O7W 0.0521(19) 0.062(2) 0.083(3) 0.0338(19) -0.0317(18) -0.0291(16) O8W 0.0392(18) 0.071(2) 0.096(3) 0.045(2) 0.0164(18) 0.0063(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 O1A C9A 1.411(4) . ? O1A C2A 1.432(5) . ? C2A C3A 1.514(6) . ? C2A H2A 0.9900 . ? C2A H2B 0.9900 . ? C3A N4A 1.469(4) . ? C3A H3A 0.9900 . ? C3A H3B 0.9900 . ? N4A C5A 1.467(5) . ? N4A C10A 1.471(4) . ? C5A C6A 1.507(5) . ? C5A H5A 0.9900 . ? C5A H5B 0.9900 . ? C6A N7A 1.512(4) . ? C6A H6A 0.9900 . ? C6A H6B 0.9900 . ? N7A C20A 1.490(4) . ? N7A C8A 1.504(4) . ? N7A H7A 0.9300 . ? C8A C9A 1.519(5) . ? C8A H8A 0.9900 . ? C8A H8B 0.9900 . ? C9A H9A 0.9900 . ? C9A H9B 0.9900 . ? C10A P1A 1.822(4) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? P1A O11A 1.501(3) . ? P1A O12A 1.508(3) . ? P1A C11A 1.816(4) . ? C11A C16A 1.385(5) . ? C11A C12A 1.397(5) . ? C12A C13A 1.383(6) . ? C12A H12A 0.9500 . ? C13A C14A 1.381(7) . ? C13A H13A 0.9500 . ? C14A C15A 1.376(7) . ? C14A H14A 0.9500 . ? C15A C16A 1.388(6) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C20A P2A 1.845(3) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? P2A O21A 1.498(2) . ? P2A O22A 1.501(3) . ? P2A C21A 1.811(4) . ? C21A C26A 1.391(5) . ? C21A C22A 1.402(5) . ? C22A C23A 1.377(5) . ? C22A H22A 0.9500 . ? C23A C24A 1.398(6) . ? C23A H23A 0.9500 . ? C24A C25A 1.381(6) . ? C24A H24A 0.9500 . ? C25A C26A 1.389(6) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? O1C C9C 1.411(5) . ? O1C C2C 1.437(4) . ? C2C C3C 1.512(6) . ? C2C H2C 0.9900 . ? C2C H2D 0.9900 . ? C3C N4C 1.471(4) . ? C3C H3C 0.9900 . ? C3C H3D 0.9900 . ? N4C C5C 1.460(4) . ? N4C C10C 1.474(4) . ? C5C C6C 1.517(5) . ? C5C H5C 0.9900 . ? C5C H5D 0.9900 . ? C6C N7C 1.517(4) . ? C6C H6C 0.9900 . ? C6C H6D 0.9900 . ? N7C C20C 1.497(4) . ? N7C C8C 1.505(4) . ? N7C H7C 0.9300 . ? C8C C9C 1.515(5) . ? C8C H8C 0.9900 . ? C8C H8D 0.9900 . ? C9C H9C 0.9900 . ? C9C H9D 0.9900 . ? C10C P1C 1.819(3) . ? C10C H10C 0.9900 . ? C10C H10D 0.9900 . ? P1C O12C 1.507(2) . ? P1C O11C 1.513(2) . ? P1C C11C 1.814(4) . ? C11C C16C 1.385(5) . ? C11C C12C 1.389(5) . ? C12C C13C 1.391(6) . ? C12C H12C 0.9500 . ? C13C C14C 1.381(7) . ? C13C H13C 0.9500 . ? C14C C15C 1.373(7) . ? C14C H14C 0.9500 . ? C15C C16C 1.396(6) . ? C15C H15C 0.9500 . ? C16C H16C 0.9500 . ? C20C P2C 1.845(3) . ? C20C H20C 0.9900 . ? C20C H20D 0.9900 . ? P2C O21C 1.497(2) . ? P2C O22C 1.501(2) . ? P2C C21C 1.818(3) . ? C21C C22C 1.386(5) . ? C21C C26C 1.395(5) . ? C22C C23C 1.381(5) . ? C22C H22C 0.9500 . ? C23C C24C 1.391(6) . ? C23C H23C 0.9500 . ? C24C C25C 1.378(6) . ? C24C H24C 0.9500 . ? C25C C26C 1.388(5) . ? C25C H25C 0.9500 . ? C26C H26C 0.9500 . ? O1E C9E 1.413(5) . ? O1E C2E 1.433(5) . ? C2E C3E 1.520(6) . ? C2E H2E 0.9900 . ? C2E H2F 0.9900 . ? C3E N4E 1.468(5) . ? C3E H3E 0.9900 . ? C3E H3F 0.9900 . ? N4E C5E 1.457(4) . ? N4E C10E 1.476(4) . ? C5E C6E 1.513(5) . ? C5E H5E 0.9900 . ? C5E H5F 0.9900 . ? C6E N7E 1.507(4) . ? C6E H6E 0.9900 . ? C6E H6F 0.9900 . ? N7E C20E 1.488(4) . ? N7E C8E 1.500(4) . ? N7E H7E 0.9300 . ? C8E C9E 1.515(5) . ? C8E H8E 0.9900 . ? C8E H8F 0.9900 . ? C9E H9E 0.9900 . ? C9E H9F 0.9900 . ? C10E P1E 1.819(4) . ? C10E H10E 0.9900 . ? C10E H10F 0.9900 . ? P1E O11E 1.499(3) . ? P1E O12E 1.505(3) . ? P1E C11E 1.813(4) . ? C11E C12E 1.385(6) . ? C11E C16E 1.396(5) . ? C12E C13E 1.394(6) . ? C12E H12E 0.9500 . ? C13E C14E 1.375(7) . ? C13E H13E 0.9500 . ? C14E C15E 1.375(7) . ? C14E H14E 0.9500 . ? C15E C16E 1.377(6) . ? C15E H15E 0.9500 . ? C16E H16E 0.9500 . ? C20E P2E 1.844(4) . ? C20E H20E 0.9900 . ? C20E H20F 0.9900 . ? P2E O22E 1.499(3) . ? P2E O21E 1.500(3) . ? P2E C21E 1.808(4) . ? C21E C26E 1.386(5) . ? C21E C22E 1.397(5) . ? C22E C23E 1.378(5) . ? C22E H22E 0.9500 . ? C23E C24E 1.393(6) . ? C23E H23E 0.9500 . ? C24E C25E 1.376(6) . ? C24E H24E 0.9500 . ? C25E C26E 1.396(5) . ? C25E H25E 0.9500 . ? C26E H26E 0.9500 . ? O1G C9G 1.419(4) . ? O1G C2G 1.428(4) . ? C2G C3G 1.515(5) . ? C2G H2G 0.9900 . ? C2G H2H 0.9900 . ? C3G N4G 1.464(4) . ? C3G H3G 0.9900 . ? C3G H3H 0.9900 . ? N4G C5G 1.465(4) . ? N4G C10G 1.480(4) . ? C5G C6G 1.519(5) . ? C5G H5G 0.9900 . ? C5G H5H 0.9900 . ? C6G N7G 1.514(4) . ? C6G H6G 0.9900 . ? C6G H6H 0.9900 . ? N7G C20G 1.502(4) . ? N7G C8G 1.508(4) . ? N7G H7G 0.9300 . ? C8G C9G 1.514(5) . ? C8G H8G 0.9900 . ? C8G H8H 0.9900 . ? C9G H9G 0.9900 . ? C9G H9H 0.9900 . ? C10G P1G 1.816(3) . ? C10G H10G 0.9900 . ? C10G H10H 0.9900 . ? P1G O12G 1.508(2) . ? P1G O11G 1.509(2) . ? P1G C11G 1.821(3) . ? C11G C16G 1.382(5) . ? C11G C12G 1.396(5) . ? C12G C13G 1.390(5) . ? C12G H12G 0.9500 . ? C13G C14G 1.383(6) . ? C13G H13G 0.9500 . ? C14G C15G 1.383(6) . ? C14G H14G 0.9500 . ? C15G C16G 1.394(5) . ? C15G H15G 0.9500 . ? C16G H16G 0.9500 . ? C20G P2G 1.840(3) . ? C20G H20G 0.9900 . ? C20G H20H 0.9900 . ? P2G O22G 1.497(2) . ? P2G O21G 1.497(2) . ? P2G C21G 1.815(3) . ? C21G C22G 1.389(5) . ? C21G C26G 1.391(5) . ? C22G C23G 1.392(5) . ? C22G H22G 0.9500 . ? C23G C24G 1.385(6) . ? C23G H23G 0.9500 . ? C24G C25G 1.376(6) . ? C24G H24G 0.9500 . ? C25G C26G 1.383(5) . ? C25G H25G 0.9500 . ? C26G H26G 0.9500 . ? N1I H1I 0.9153 . ? N1I H1J 0.9330 . ? N1I H1K 0.8448 . ? N1I H1L 0.9170 . ? N2I H2I 0.9642 . ? N2I H2J 0.9046 . ? N2I H2K 0.9094 . ? N2I H2L 0.8787 . ? N3I H3I 0.9614 . ? N3I H3J 0.9166 . ? N3I H3K 0.9910 . ? N3I H3L 0.8755 . ? N4I H4I 0.9773 . ? N4I H4J 0.9452 . ? N4I H4K 0.9011 . ? N4I H4L 0.8613 . ? O1W H1W 0.9574 . ? O1W H1X 0.9469 . ? O2W H2W 0.9541 . ? O2W H2X 0.9896 . ? O3W H3W 0.8889 . ? O3W H3X 0.9543 . ? O4W H4W 0.9396 . ? O4W H4X 0.9194 . ? O5W H5W 0.9349 . ? O5W H5X 0.9872 . ? O6W H6W 0.8742 . ? O6W H6X 0.9295 . ? O7W H7W 0.8788 . ? O7W H7X 0.9394 . ? O8W H8W 0.8580 . ? O8W H8X 0.9337 . ? 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 C9A O1A C2A 116.0(3) . . ? O1A C2A C3A 113.5(3) . . ? O1A C2A H2A 108.9 . . ? C3A C2A H2A 108.9 . . ? O1A C2A H2B 108.9 . . ? C3A C2A H2B 108.9 . . ? H2A C2A H2B 107.7 . . ? N4A C3A C2A 115.0(3) . . ? N4A C3A H3A 108.5 . . ? C2A C3A H3A 108.5 . . ? N4A C3A H3B 108.5 . . ? C2A C3A H3B 108.5 . . ? H3A C3A H3B 107.5 . . ? C5A N4A C3A 113.5(3) . . ? C5A N4A C10A 109.4(3) . . ? C3A N4A C10A 113.5(3) . . ? N4A C5A C6A 116.2(3) . . ? N4A C5A H5A 108.2 . . ? C6A C5A H5A 108.2 . . ? N4A C5A H5B 108.2 . . ? C6A C5A H5B 108.2 . . ? H5A C5A H5B 107.4 . . ? C5A C6A N7A 115.1(3) . . ? C5A C6A H6A 108.5 . . ? N7A C6A H6A 108.5 . . ? C5A C6A H6B 108.5 . . ? N7A C6A H6B 108.5 . . ? H6A C6A H6B 107.5 . . ? C20A N7A C8A 110.4(3) . . ? C20A N7A C6A 111.9(3) . . ? C8A N7A C6A 115.5(3) . . ? C20A N7A H7A 106.2 . . ? C8A N7A H7A 106.2 . . ? C6A N7A H7A 106.2 . . ? N7A C8A C9A 112.8(3) . . ? N7A C8A H8A 109.0 . . ? C9A C8A H8A 109.0 . . ? N7A C8A H8B 109.0 . . ? C9A C8A H8B 109.0 . . ? H8A C8A H8B 107.8 . . ? O1A C9A C8A 115.4(3) . . ? O1A C9A H9A 108.4 . . ? C8A C9A H9A 108.4 . . ? O1A C9A H9B 108.4 . . ? C8A C9A H9B 108.4 . . ? H9A C9A H9B 107.5 . . ? N4A C10A P1A 114.1(2) . . ? N4A C10A H10A 108.7 . . ? P1A C10A H10A 108.7 . . ? N4A C10A H10B 108.7 . . ? P1A C10A H10B 108.7 . . ? H10A C10A H10B 107.6 . . ? O11A P1A O12A 118.16(16) . . ? O11A P1A C11A 107.19(16) . . ? O12A P1A C11A 110.44(16) . . ? O11A P1A C10A 113.10(16) . . ? O12A P1A C10A 104.21(15) . . ? C11A P1A C10A 102.70(17) . . ? C16A C11A C12A 118.8(4) . . ? C16A C11A P1A 120.6(3) . . ? C12A C11A P1A 120.6(3) . . ? C13A C12A C11A 120.2(4) . . ? C13A C12A H12A 119.9 . . ? C11A C12A H12A 119.9 . . ? C14A C13A C12A 120.2(4) . . ? C14A C13A H13A 119.9 . . ? C12A C13A H13A 119.9 . . ? C15A C14A C13A 120.2(4) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C14A C15A C16A 119.8(4) . . ? C14A C15A H15A 120.1 . . ? C16A C15A H15A 120.1 . . ? C11A C16A C15A 120.8(4) . . ? C11A C16A H16A 119.6 . . ? C15A C16A H16A 119.6 . . ? N7A C20A P2A 112.9(2) . . ? N7A C20A H20A 109.0 . . ? P2A C20A H20A 109.0 . . ? N7A C20A H20B 109.0 . . ? P2A C20A H20B 109.0 . . ? H20A C20A H20B 107.8 . . ? O21A P2A O22A 119.29(15) . . ? O21A P2A C21A 109.51(15) . . ? O22A P2A C21A 107.81(15) . . ? O21A P2A C20A 107.17(15) . . ? O22A P2A C20A 105.30(15) . . ? C21A P2A C20A 107.09(16) . . ? C26A C21A C22A 118.5(3) . . ? C26A C21A P2A 121.3(3) . . ? C22A C21A P2A 120.1(3) . . ? C23A C22A C21A 121.2(4) . . ? C23A C22A H22A 119.4 . . ? C21A C22A H22A 119.4 . . ? C22A C23A C24A 119.7(4) . . ? C22A C23A H23A 120.2 . . ? C24A C23A H23A 120.2 . . ? C25A C24A C23A 119.7(4) . . ? C25A C24A H24A 120.2 . . ? C23A C24A H24A 120.2 . . ? C24A C25A C26A 120.6(4) . . ? C24A C25A H25A 119.7 . . ? C26A C25A H25A 119.7 . . ? C25A C26A C21A 120.4(4) . . ? C25A C26A H26A 119.8 . . ? C21A C26A H26A 119.8 . . ? C9C O1C C2C 115.9(3) . . ? O1C C2C C3C 112.8(3) . . ? O1C C2C H2C 109.0 . . ? C3C C2C H2C 109.0 . . ? O1C C2C H2D 109.0 . . ? C3C C2C H2D 109.0 . . ? H2C C2C H2D 107.8 . . ? N4C C3C C2C 113.6(3) . . ? N4C C3C H3C 108.8 . . ? C2C C3C H3C 108.8 . . ? N4C C3C H3D 108.8 . . ? C2C C3C H3D 108.8 . . ? H3C C3C H3D 107.7 . . ? C5C N4C C3C 114.7(3) . . ? C5C N4C C10C 111.0(3) . . ? C3C N4C C10C 114.2(3) . . ? N4C C5C C6C 114.8(3) . . ? N4C C5C H5C 108.6 . . ? C6C C5C H5C 108.6 . . ? N4C C5C H5D 108.6 . . ? C6C C5C H5D 108.6 . . ? H5C C5C H5D 107.5 . . ? C5C C6C N7C 115.9(3) . . ? C5C C6C H6C 108.3 . . ? N7C C6C H6C 108.3 . . ? C5C C6C H6D 108.3 . . ? N7C C6C H6D 108.3 . . ? H6C C6C H6D 107.4 . . ? C20C N7C C8C 110.5(2) . . ? C20C N7C C6C 111.5(3) . . ? C8C N7C C6C 114.5(3) . . ? C20C N7C H7C 106.6 . . ? C8C N7C H7C 106.6 . . ? C6C N7C H7C 106.6 . . ? N7C C8C C9C 114.0(3) . . ? N7C C8C H8C 108.7 . . ? C9C C8C H8C 108.7 . . ? N7C C8C H8D 108.7 . . ? C9C C8C H8D 108.7 . . ? H8C C8C H8D 107.6 . . ? O1C C9C C8C 115.8(3) . . ? O1C C9C H9C 108.3 . . ? C8C C9C H9C 108.3 . . ? O1C C9C H9D 108.3 . . ? C8C C9C H9D 108.3 . . ? H9C C9C H9D 107.4 . . ? N4C C10C P1C 110.7(2) . . ? N4C C10C H10C 109.5 . . ? P1C C10C H10C 109.5 . . ? N4C C10C H10D 109.5 . . ? P1C C10C H10D 109.5 . . ? H10C C10C H10D 108.1 . . ? O12C P1C O11C 116.24(14) . . ? O12C P1C C11C 109.15(15) . . ? O11C P1C C11C 108.49(16) . . ? O12C P1C C10C 109.30(15) . . ? O11C P1C C10C 108.56(15) . . ? C11C P1C C10C 104.45(16) . . ? C16C C11C C12C 119.0(3) . . ? C16C C11C P1C 120.5(3) . . ? C12C C11C P1C 120.5(3) . . ? C11C C12C C13C 120.4(4) . . ? C11C C12C H12C 119.8 . . ? C13C C12C H12C 119.8 . . ? C14C C13C C12C 120.2(4) . . ? C14C C13C H13C 119.9 . . ? C12C C13C H13C 119.9 . . ? C15C C14C C13C 119.8(4) . . ? C15C C14C H14C 120.1 . . ? C13C C14C H14C 120.1 . . ? C14C C15C C16C 120.3(4) . . ? C14C C15C H15C 119.8 . . ? C16C C15C H15C 119.8 . . ? C11C C16C C15C 120.3(4) . . ? C11C C16C H16C 119.8 . . ? C15C C16C H16C 119.8 . . ? N7C C20C P2C 113.8(2) . . ? N7C C20C H20C 108.8 . . ? P2C C20C H20C 108.8 . . ? N7C C20C H20D 108.8 . . ? P2C C20C H20D 108.8 . . ? H20C C20C H20D 107.7 . . ? O21C P2C O22C 120.84(14) . . ? O21C P2C C21C 107.33(15) . . ? O22C P2C C21C 107.57(14) . . ? O21C P2C C20C 105.86(15) . . ? O22C P2C C20C 105.40(15) . . ? C21C P2C C20C 109.52(15) . . ? C22C C21C C26C 118.8(3) . . ? C22C C21C P2C 121.4(3) . . ? C26C C21C P2C 119.7(3) . . ? C23C C22C C21C 120.6(4) . . ? C23C C22C H22C 119.7 . . ? C21C C22C H22C 119.7 . . ? C22C C23C C24C 120.3(4) . . ? C22C C23C H23C 119.8 . . ? C24C C23C H23C 119.8 . . ? C25C C24C C23C 119.7(4) . . ? C25C C24C H24C 120.2 . . ? C23C C24C H24C 120.2 . . ? C24C C25C C26C 120.0(4) . . ? C24C C25C H25C 120.0 . . ? C26C C25C H25C 120.0 . . ? C25C C26C C21C 120.6(4) . . ? C25C C26C H26C 119.7 . . ? C21C C26C H26C 119.7 . . ? C9E O1E C2E 116.1(3) . . ? O1E C2E C3E 113.5(3) . . ? O1E C2E H2E 108.9 . . ? C3E C2E H2E 108.9 . . ? O1E C2E H2F 108.9 . . ? C3E C2E H2F 108.9 . . ? H2E C2E H2F 107.7 . . ? N4E C3E C2E 115.7(3) . . ? N4E C3E H3E 108.4 . . ? C2E C3E H3E 108.4 . . ? N4E C3E H3F 108.4 . . ? C2E C3E H3F 108.4 . . ? H3E C3E H3F 107.4 . . ? C5E N4E C3E 113.5(3) . . ? C5E N4E C10E 109.8(3) . . ? C3E N4E C10E 113.6(3) . . ? N4E C5E C6E 115.6(3) . . ? N4E C5E H5E 108.4 . . ? C6E C5E H5E 108.4 . . ? N4E C5E H5F 108.4 . . ? C6E C5E H5F 108.4 . . ? H5E C5E H5F 107.5 . . ? N7E C6E C5E 115.4(3) . . ? N7E C6E H6E 108.4 . . ? C5E C6E H6E 108.4 . . ? N7E C6E H6F 108.4 . . ? C5E C6E H6F 108.4 . . ? H6E C6E H6F 107.5 . . ? C20E N7E C8E 110.8(3) . . ? C20E N7E C6E 112.0(3) . . ? C8E N7E C6E 115.2(3) . . ? C20E N7E H7E 106.1 . . ? C8E N7E H7E 106.1 . . ? C6E N7E H7E 106.1 . . ? N7E C8E C9E 113.3(3) . . ? N7E C8E H8E 108.9 . . ? C9E C8E H8E 108.9 . . ? N7E C8E H8F 108.9 . . ? C9E C8E H8F 108.9 . . ? H8E C8E H8F 107.7 . . ? O1E C9E C8E 115.6(3) . . ? O1E C9E H9E 108.4 . . ? C8E C9E H9E 108.4 . . ? O1E C9E H9F 108.4 . . ? C8E C9E H9F 108.4 . . ? H9E C9E H9F 107.4 . . ? N4E C10E P1E 113.4(2) . . ? N4E C10E H10E 108.9 . . ? P1E C10E H10E 108.9 . . ? N4E C10E H10F 108.9 . . ? P1E C10E H10F 108.9 . . ? H10E C10E H10F 107.7 . . ? O11E P1E O12E 118.23(16) . . ? O11E P1E C11E 106.98(16) . . ? O12E P1E C11E 110.19(16) . . ? O11E P1E C10E 112.79(16) . . ? O12E P1E C10E 104.96(16) . . ? C11E P1E C10E 102.63(18) . . ? C12E C11E C16E 118.2(4) . . ? C12E C11E P1E 121.0(3) . . ? C16E C11E P1E 120.7(3) . . ? C11E C12E C13E 120.3(4) . . ? C11E C12E H12E 119.8 . . ? C13E C12E H12E 119.8 . . ? C14E C13E C12E 120.3(5) . . ? C14E C13E H13E 119.9 . . ? C12E C13E H13E 119.9 . . ? C15E C14E C13E 120.0(5) . . ? C15E C14E H14E 120.0 . . ? C13E C14E H14E 120.0 . . ? C14E C15E C16E 120.0(4) . . ? C14E C15E H15E 120.0 . . ? C16E C15E H15E 120.0 . . ? C15E C16E C11E 121.2(4) . . ? C15E C16E H16E 119.4 . . ? C11E C16E H16E 119.4 . . ? N7E C20E P2E 112.6(2) . . ? N7E C20E H20E 109.1 . . ? P2E C20E H20E 109.1 . . ? N7E C20E H20F 109.1 . . ? P2E C20E H20F 109.1 . . ? H20E C20E H20F 107.8 . . ? O22E P2E O21E 119.60(15) . . ? O22E P2E C21E 108.23(15) . . ? O21E P2E C21E 109.32(16) . . ? O22E P2E C20E 104.96(16) . . ? O21E P2E C20E 107.06(15) . . ? C21E P2E C20E 106.95(16) . . ? C26E C21E C22E 118.7(3) . . ? C26E C21E P2E 121.6(3) . . ? C22E C21E P2E 119.6(3) . . ? C23E C22E C21E 121.2(4) . . ? C23E C22E H22E 119.4 . . ? C21E C22E H22E 119.4 . . ? C22E C23E C24E 119.4(4) . . ? C22E C23E H23E 120.3 . . ? C24E C23E H23E 120.3 . . ? C25E C24E C23E 120.2(4) . . ? C25E C24E H24E 119.9 . . ? C23E C24E H24E 119.9 . . ? C24E C25E C26E 120.1(4) . . ? C24E C25E H25E 120.0 . . ? C26E C25E H25E 120.0 . . ? C21E C26E C25E 120.4(4) . . ? C21E C26E H26E 119.8 . . ? C25E C26E H26E 119.8 . . ? C9G O1G C2G 116.3(3) . . ? O1G C2G C3G 113.3(3) . . ? O1G C2G H2G 108.9 . . ? C3G C2G H2G 108.9 . . ? O1G C2G H2H 108.9 . . ? C3G C2G H2H 108.9 . . ? H2G C2G H2H 107.7 . . ? N4G C3G C2G 113.6(3) . . ? N4G C3G H3G 108.8 . . ? C2G C3G H3G 108.8 . . ? N4G C3G H3H 108.8 . . ? C2G C3G H3H 108.8 . . ? H3G C3G H3H 107.7 . . ? C3G N4G C5G 114.4(3) . . ? C3G N4G C10G 114.4(3) . . ? C5G N4G C10G 111.2(3) . . ? N4G C5G C6G 114.3(3) . . ? N4G C5G H5G 108.7 . . ? C6G C5G H5G 108.7 . . ? N4G C5G H5H 108.7 . . ? C6G C5G H5H 108.7 . . ? H5G C5G H5H 107.6 . . ? N7G C6G C5G 116.0(3) . . ? N7G C6G H6G 108.3 . . ? C5G C6G H6G 108.3 . . ? N7G C6G H6H 108.3 . . ? C5G C6G H6H 108.3 . . ? H6G C6G H6H 107.4 . . ? C20G N7G C8G 110.4(2) . . ? C20G N7G C6G 111.5(3) . . ? C8G N7G C6G 114.5(3) . . ? C20G N7G H7G 106.7 . . ? C8G N7G H7G 106.7 . . ? C6G N7G H7G 106.7 . . ? N7G C8G C9G 114.1(3) . . ? N7G C8G H8G 108.7 . . ? C9G C8G H8G 108.7 . . ? N7G C8G H8H 108.7 . . ? C9G C8G H8H 108.7 . . ? H8G C8G H8H 107.6 . . ? O1G C9G C8G 116.2(3) . . ? O1G C9G H9G 108.2 . . ? C8G C9G H9G 108.2 . . ? O1G C9G H9H 108.2 . . ? C8G C9G H9H 108.2 . . ? H9G C9G H9H 107.4 . . ? N4G C10G P1G 111.2(2) . . ? N4G C10G H10G 109.4 . . ? P1G C10G H10G 109.4 . . ? N4G C10G H10H 109.4 . . ? P1G C10G H10H 109.4 . . ? H10G C10G H10H 108.0 . . ? O12G P1G O11G 116.31(15) . . ? O12G P1G C10G 109.10(15) . . ? O11G P1G C10G 108.47(15) . . ? O12G P1G C11G 109.60(15) . . ? O11G P1G C11G 108.33(15) . . ? C10G P1G C11G 104.36(16) . . ? C16G C11G C12G 118.8(3) . . ? C16G C11G P1G 120.7(3) . . ? C12G C11G P1G 120.5(3) . . ? C13G C12G C11G 120.3(3) . . ? C13G C12G H12G 119.8 . . ? C11G C12G H12G 119.8 . . ? C14G C13G C12G 120.2(4) . . ? C14G C13G H13G 119.9 . . ? C12G C13G H13G 119.9 . . ? C13G C14G C15G 119.9(4) . . ? C13G C14G H14G 120.0 . . ? C15G C14G H14G 120.0 . . ? C14G C15G C16G 119.7(4) . . ? C14G C15G H15G 120.1 . . ? C16G C15G H15G 120.1 . . ? C11G C16G C15G 121.0(4) . . ? C11G C16G H16G 119.5 . . ? C15G C16G H16G 119.5 . . ? N7G C20G P2G 113.9(2) . . ? N7G C20G H20G 108.8 . . ? P2G C20G H20G 108.8 . . ? N7G C20G H20H 108.8 . . ? P2G C20G H20H 108.8 . . ? H20G C20G H20H 107.7 . . ? O22G P2G O21G 120.86(14) . . ? O22G P2G C21G 107.78(14) . . ? O21G P2G C21G 107.30(15) . . ? O22G P2G C20G 105.29(15) . . ? O21G P2G C20G 106.40(15) . . ? C21G P2G C20G 108.79(15) . . ? C22G C21G C26G 119.0(3) . . ? C22G C21G P2G 121.8(3) . . ? C26G C21G P2G 119.1(3) . . ? C21G C22G C23G 120.2(3) . . ? C21G C22G H22G 119.9 . . ? C23G C22G H22G 119.9 . . ? C24G C23G C22G 120.1(4) . . ? C24G C23G H23G 120.0 . . ? C22G C23G H23G 120.0 . . ? C25G C24G C23G 119.9(4) . . ? C25G C24G H24G 120.1 . . ? C23G C24G H24G 120.1 . . ? C24G C25G C26G 120.2(4) . . ? C24G C25G H25G 119.9 . . ? C26G C25G H25G 119.9 . . ? C25G C26G C21G 120.6(4) . . ? C25G C26G H26G 119.7 . . ? C21G C26G H26G 119.7 . . ? H1I N1I H1J 109.0 . . ? H1I N1I H1K 107.6 . . ? H1J N1I H1K 110.7 . . ? H1I N1I H1L 104.9 . . ? H1J N1I H1L 105.2 . . ? H1K N1I H1L 119.0 . . ? H2I N2I H2J 105.3 . . ? H2I N2I H2K 117.6 . . ? H2J N2I H2K 98.4 . . ? H2I N2I H2L 114.4 . . ? H2J N2I H2L 113.3 . . ? H2K N2I H2L 106.9 . . ? H3I N3I H3J 107.1 . . ? H3I N3I H3K 111.4 . . ? H3J N3I H3K 107.0 . . ? H3I N3I H3L 104.9 . . ? H3J N3I H3L 117.4 . . ? H3K N3I H3L 109.1 . . ? H4I N4I H4J 108.4 . . ? H4I N4I H4K 114.5 . . ? H4J N4I H4K 105.2 . . ? H4I N4I H4L 103.2 . . ? H4J N4I H4L 113.6 . . ? H4K N4I H4L 112.0 . . ? H1W O1W H1X 96.4 . . ? H2W O2W H2X 98.6 . . ? H3W O3W H3X 100.8 . . ? H4W O4W H4X 103.9 . . ? H5W O5W H5X 108.9 . . ? H6W O6W H6X 99.8 . . ? H7W O7W H7X 119.7 . . ? H8W O8W H8X 123.8 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.794 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.071 _publ_section_references ; A. Altomare, G. Cascarano, C. Giacovazzo, A. Guagliardi, M.C. Burla, G. Polidori & M. Camalli (1994). J. Appl. Cryst. 27, 435. R.W. Hooft (1998). COLLECT. Nonius BV, Delft, The Netherlands. Z. Otwinowski & W. Minor (1997). Methods Enzymol. 276, 307. G.M. Sheldrick (1997). SHELXL97. University of Gottingen, Germany. A.L. Spek (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; #==END data_mnphp _database_code_depnum_ccdc_archive 'CCDC 819617' #TrackingRef '- lukes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H52 Mn2 N4 O10 P4, 2(H2 O)' _chemical_formula_sum 'C40 H56 Mn2 N4 O12 P4' _chemical_formula_weight 1018.65 _chemical_compound_source 'synthesized by the authors' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8641(10) _cell_length_b 9.9409(14) _cell_length_c 15.085(2) _cell_angle_alpha 80.556(5) _cell_angle_beta 87.468(5) _cell_angle_gamma 76.778(4) _cell_volume 1132.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5122 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5122 _reflns_number_gt 4558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0000P)^2^+2.0665P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5122 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.212 _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 Mn1 Mn 0.44895(5) 0.69422(4) 0.85748(3) 0.01250(9) Uani 1 1 d . . . O1 O 0.5093(3) 0.90455(19) 0.88219(13) 0.0199(4) Uani 1 1 d . . . C2 C 0.5490(4) 0.9966(3) 0.8036(2) 0.0235(6) Uani 1 1 d . . . H21 H 0.6749 0.9969 0.8027 0.028 Uiso 1 1 calc R . . H22 H 0.4816 1.0933 0.8056 0.028 Uiso 1 1 calc R . . C3 C 0.5029(4) 0.9476(3) 0.71945(19) 0.0202(6) Uani 1 1 d . . . H31 H 0.3744 0.9703 0.7127 0.024 Uiso 1 1 calc R . . H32 H 0.5530 0.9978 0.6662 0.024 Uiso 1 1 calc R . . N4 N 0.5709(3) 0.7943(2) 0.72357(15) 0.0162(5) Uani 1 1 d . . . C5 C 0.7653(3) 0.7554(3) 0.7226(2) 0.0206(6) Uani 1 1 d . . . H51 H 0.8117 0.8354 0.7342 0.025 Uiso 1 1 calc R . . H52 H 0.8073 0.7336 0.6626 0.025 Uiso 1 1 calc R . . C6 C 0.8322(3) 0.6291(3) 0.79377(19) 0.0196(6) Uani 1 1 d . . . H61 H 0.8068 0.5449 0.7750 0.024 Uiso 1 1 calc R . . H62 H 0.9606 0.6142 0.7985 0.024 Uiso 1 1 calc R . . N7 N 0.7515(3) 0.6464(2) 0.88313(16) 0.0176(5) Uani 1 1 d . . . C8 C 0.8034(4) 0.7624(3) 0.9192(2) 0.0254(6) Uani 1 1 d . . . H81 H 0.8672 0.8134 0.8720 0.030 Uiso 1 1 calc R . . H82 H 0.8828 0.7229 0.9707 0.030 Uiso 1 1 calc R . . C9 C 0.6434(4) 0.8641(3) 0.9493(2) 0.0255(6) Uani 1 1 d . . . H91 H 0.5963 0.8194 1.0056 0.031 Uiso 1 1 calc R . . H92 H 0.6784 0.9485 0.9619 0.031 Uiso 1 1 calc R . . C10 C 0.4983(4) 0.7436(3) 0.65011(18) 0.0197(6) Uani 1 1 d . . . H101 H 0.5662 0.6482 0.6447 0.024 Uiso 1 1 calc R . . H102 H 0.5102 0.8054 0.5927 0.024 Uiso 1 1 calc R . . P1 P 0.26642(9) 0.73946(7) 0.66947(4) 0.01486(14) Uani 1 1 d . . . O11 O 0.2403(2) 0.72436(19) 0.77071(12) 0.0159(4) Uani 1 1 d . . . O12 O 0.1518(3) 0.8615(2) 0.61309(13) 0.0221(4) Uani 1 1 d . . . C11 C 0.2487(4) 0.5796(3) 0.6324(2) 0.0213(6) Uani 1 1 d . . . C12 C 0.2677(4) 0.4543(3) 0.6908(2) 0.0323(7) Uani 1 1 d . . . H121 H 0.2875 0.4513 0.7528 0.039 Uiso 1 1 calc R . . C13 C 0.2578(5) 0.3324(4) 0.6587(3) 0.0443(10) Uani 1 1 d . . . H131 H 0.2689 0.2468 0.6991 0.053 Uiso 1 1 calc R . . C14 C 0.2317(5) 0.3362(4) 0.5677(3) 0.0497(11) Uani 1 1 d . . . H141 H 0.2277 0.2529 0.5455 0.060 Uiso 1 1 calc R . . C15 C 0.2118(6) 0.4600(5) 0.5104(3) 0.0515(11) Uani 1 1 d . . . H151 H 0.1929 0.4626 0.4483 0.062 Uiso 1 1 calc R . . C16 C 0.2189(5) 0.5819(4) 0.5417(2) 0.0390(8) Uani 1 1 d . . . H161 H 0.2035 0.6676 0.5012 0.047 Uiso 1 1 calc R . . C20 C 0.7957(4) 0.5131(3) 0.94553(19) 0.0190(6) Uani 1 1 d . . . H201 H 0.7732 0.5323 1.0078 0.023 Uiso 1 1 calc R . . H202 H 0.9221 0.4718 0.9399 0.023 Uiso 1 1 calc R . . P2 P 0.67201(9) 0.38530(7) 0.92549(4) 0.01337(14) Uani 1 1 d . . . O21 O 0.5066(2) 0.46891(19) 0.87869(13) 0.0169(4) Uani 1 1 d . . . O22 O 0.6593(3) 0.29508(19) 1.01505(12) 0.0200(4) Uani 1 1 d . . . C21 C 0.7939(3) 0.2699(3) 0.85311(18) 0.0145(5) Uani 1 1 d . . . C22 C 0.9290(4) 0.1580(3) 0.8886(2) 0.0221(6) Uani 1 1 d . . . H221 H 0.9569 0.1444 0.9505 0.027 Uiso 1 1 calc R . . C23 C 1.0223(4) 0.0669(3) 0.8337(2) 0.0293(7) Uani 1 1 d . . . H231 H 1.1151 -0.0077 0.8579 0.035 Uiso 1 1 calc R . . C24 C 0.9799(4) 0.0850(3) 0.7441(2) 0.0334(8) Uani 1 1 d . . . H241 H 1.0433 0.0223 0.7067 0.040 Uiso 1 1 calc R . . C25 C 0.8456(5) 0.1939(3) 0.7083(2) 0.0299(7) Uani 1 1 d . . . H251 H 0.8168 0.2052 0.6467 0.036 Uiso 1 1 calc R . . C26 C 0.7522(4) 0.2871(3) 0.76241(19) 0.0220(6) Uani 1 1 d . . . H261 H 0.6606 0.3621 0.7375 0.026 Uiso 1 1 calc R . . O1W O 0.2015(3) 0.0429(3) 0.45543(16) 0.0429(6) Uani 1 1 d . . . H11W H 0.1008 0.0722 0.4379 0.064 Uiso 1 1 d R . . H12W H 0.1942 -0.0118 0.5015 0.064 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01244(19) 0.01181(18) 0.01229(19) -0.00088(14) -0.00118(14) -0.00127(14) O1 0.0218(10) 0.0147(9) 0.0231(10) -0.0010(8) -0.0046(8) -0.0042(8) C2 0.0227(14) 0.0118(12) 0.0354(17) -0.0004(11) 0.0009(12) -0.0052(11) C3 0.0179(13) 0.0141(13) 0.0256(15) 0.0022(11) 0.0042(11) -0.0021(10) N4 0.0134(11) 0.0130(10) 0.0203(12) 0.0005(9) 0.0013(9) -0.0015(8) C5 0.0135(13) 0.0183(13) 0.0288(15) -0.0016(11) 0.0044(11) -0.0038(10) C6 0.0125(12) 0.0168(13) 0.0290(15) -0.0032(11) 0.0016(11) -0.0028(10) N7 0.0164(11) 0.0123(10) 0.0248(12) -0.0030(9) -0.0047(9) -0.0037(9) C8 0.0239(15) 0.0148(13) 0.0401(18) -0.0072(12) -0.0117(13) -0.0058(11) C9 0.0306(16) 0.0153(13) 0.0321(17) -0.0062(12) -0.0125(13) -0.0042(12) C10 0.0187(14) 0.0213(14) 0.0181(14) -0.0026(11) 0.0043(11) -0.0035(11) P1 0.0151(3) 0.0158(3) 0.0118(3) -0.0009(2) -0.0011(2) -0.0004(3) O11 0.0135(9) 0.0232(10) 0.0099(9) -0.0014(7) 0.0005(7) -0.0031(7) O12 0.0241(10) 0.0219(10) 0.0162(10) 0.0001(8) -0.0029(8) 0.0016(8) C11 0.0164(13) 0.0227(14) 0.0258(15) -0.0091(12) 0.0008(11) -0.0029(11) C12 0.0291(17) 0.0250(16) 0.043(2) -0.0041(14) -0.0120(15) -0.0047(13) C13 0.037(2) 0.0224(17) 0.074(3) -0.0089(17) -0.0156(19) -0.0026(15) C14 0.035(2) 0.042(2) 0.082(3) -0.041(2) -0.004(2) -0.0045(17) C15 0.060(3) 0.062(3) 0.044(2) -0.035(2) 0.008(2) -0.019(2) C16 0.055(2) 0.042(2) 0.0242(17) -0.0127(15) 0.0016(16) -0.0146(17) C20 0.0189(13) 0.0148(12) 0.0231(14) -0.0041(11) -0.0082(11) -0.0010(10) P2 0.0153(3) 0.0109(3) 0.0132(3) -0.0026(2) -0.0009(2) -0.0009(2) O21 0.0152(9) 0.0142(9) 0.0216(10) -0.0036(7) -0.0030(7) -0.0030(7) O22 0.0299(11) 0.0156(9) 0.0124(9) -0.0019(7) 0.0020(8) -0.0016(8) C21 0.0154(12) 0.0115(11) 0.0179(13) -0.0042(10) 0.0024(10) -0.0047(10) C22 0.0185(14) 0.0186(14) 0.0293(16) -0.0061(11) -0.0010(12) -0.0025(11) C23 0.0176(14) 0.0212(15) 0.049(2) -0.0124(14) 0.0061(13) -0.0009(12) C24 0.0334(18) 0.0298(17) 0.044(2) -0.0224(15) 0.0197(15) -0.0140(14) C25 0.0430(19) 0.0314(17) 0.0210(15) -0.0103(13) 0.0102(14) -0.0173(15) C26 0.0283(15) 0.0199(14) 0.0191(14) -0.0024(11) 0.0023(12) -0.0089(12) O1W 0.0289(13) 0.0554(16) 0.0359(14) 0.0212(12) -0.0044(10) -0.0117(12) _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 O22 2.0772(19) 2_667 ? Mn1 O11 2.0816(18) . ? Mn1 O21 2.1535(18) . ? Mn1 O1 2.3371(19) . ? Mn1 N7 2.353(2) . ? Mn1 N4 2.366(2) . ? O1 C9 1.436(3) . ? O1 C2 1.443(3) . ? C2 C3 1.519(4) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C3 N4 1.487(3) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? N4 C10 1.476(4) . ? N4 C5 1.489(3) . ? C5 C6 1.521(4) . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 N7 1.484(4) . ? C6 H61 0.9900 . ? C6 H62 0.9900 . ? N7 C20 1.473(3) . ? N7 C8 1.495(3) . ? C8 C9 1.526(4) . ? C8 H81 0.9900 . ? C8 H82 0.9900 . ? C9 H91 0.9900 . ? C9 H92 0.9900 . ? C10 P1 1.842(3) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? P1 O12 1.495(2) . ? P1 O11 1.5194(18) . ? P1 C11 1.804(3) . ? C11 C12 1.384(4) . ? C11 C16 1.394(4) . ? C12 C13 1.396(5) . ? C12 H121 0.9500 . ? C13 C14 1.390(6) . ? C13 H131 0.9500 . ? C14 C15 1.365(6) . ? C14 H141 0.9500 . ? C15 C16 1.384(5) . ? C15 H151 0.9500 . ? C16 H161 0.9500 . ? C20 P2 1.836(3) . ? C20 H201 0.9900 . ? C20 H202 0.9900 . ? P2 O22 1.5070(19) . ? P2 O21 1.5083(19) . ? P2 C21 1.801(3) . ? O22 Mn1 2.0772(19) 2_667 ? C21 C26 1.395(4) . ? C21 C22 1.402(4) . ? C22 C23 1.391(4) . ? C22 H221 0.9500 . ? C23 C24 1.380(5) . ? C23 H231 0.9500 . ? C24 C25 1.383(5) . ? C24 H241 0.9500 . ? C25 C26 1.396(4) . ? C25 H251 0.9500 . ? C26 H261 0.9500 . ? O1W H11W 0.8178 . ? O1W H12W 0.8177 . ? 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 O22 Mn1 O11 106.17(8) 2_667 . ? O22 Mn1 O21 93.03(7) 2_667 . ? O11 Mn1 O21 96.59(7) . . ? O22 Mn1 O1 80.14(7) 2_667 . ? O11 Mn1 O1 112.72(7) . . ? O21 Mn1 O1 150.67(7) . . ? O22 Mn1 N7 103.46(8) 2_667 . ? O11 Mn1 N7 150.32(8) . . ? O21 Mn1 N7 80.07(7) . . ? O1 Mn1 N7 73.99(7) . . ? O22 Mn1 N4 151.77(8) 2_667 . ? O11 Mn1 N4 80.19(7) . . ? O21 Mn1 N4 113.86(7) . . ? O1 Mn1 N4 72.19(7) . . ? N7 Mn1 N4 74.50(8) . . ? C9 O1 C2 114.5(2) . . ? C9 O1 Mn1 104.80(15) . . ? C2 O1 Mn1 116.39(16) . . ? O1 C2 C3 109.8(2) . . ? O1 C2 H21 109.7 . . ? C3 C2 H21 109.7 . . ? O1 C2 H22 109.7 . . ? C3 C2 H22 109.7 . . ? H21 C2 H22 108.2 . . ? N4 C3 C2 111.2(2) . . ? N4 C3 H31 109.4 . . ? C2 C3 H31 109.4 . . ? N4 C3 H32 109.4 . . ? C2 C3 H32 109.4 . . ? H31 C3 H32 108.0 . . ? C10 N4 C3 110.7(2) . . ? C10 N4 C5 111.1(2) . . ? C3 N4 C5 112.0(2) . . ? C10 N4 Mn1 105.59(15) . . ? C3 N4 Mn1 104.35(15) . . ? C5 N4 Mn1 112.75(16) . . ? N4 C5 C6 110.6(2) . . ? N4 C5 H51 109.5 . . ? C6 C5 H51 109.5 . . ? N4 C5 H52 109.5 . . ? C6 C5 H52 109.5 . . ? H51 C5 H52 108.1 . . ? N7 C6 C5 112.2(2) . . ? N7 C6 H61 109.2 . . ? C5 C6 H61 109.2 . . ? N7 C6 H62 109.2 . . ? C5 C6 H62 109.2 . . ? H61 C6 H62 107.9 . . ? C20 N7 C6 110.2(2) . . ? C20 N7 C8 111.9(2) . . ? C6 N7 C8 111.1(2) . . ? C20 N7 Mn1 106.96(16) . . ? C6 N7 Mn1 104.47(16) . . ? C8 N7 Mn1 111.88(16) . . ? N7 C8 C9 110.9(2) . . ? N7 C8 H81 109.5 . . ? C9 C8 H81 109.5 . . ? N7 C8 H82 109.5 . . ? C9 C8 H82 109.5 . . ? H81 C8 H82 108.0 . . ? O1 C9 C8 111.7(2) . . ? O1 C9 H91 109.3 . . ? C8 C9 H91 109.3 . . ? O1 C9 H92 109.3 . . ? C8 C9 H92 109.3 . . ? H91 C9 H92 107.9 . . ? N4 C10 P1 112.00(18) . . ? N4 C10 H101 109.2 . . ? P1 C10 H101 109.2 . . ? N4 C10 H102 109.2 . . ? P1 C10 H102 109.2 . . ? H101 C10 H102 107.9 . . ? O12 P1 O11 117.52(11) . . ? O12 P1 C11 109.47(13) . . ? O11 P1 C11 109.07(13) . . ? O12 P1 C10 110.58(12) . . ? O11 P1 C10 105.51(12) . . ? C11 P1 C10 103.76(13) . . ? P1 O11 Mn1 121.57(10) . . ? C12 C11 C16 119.0(3) . . ? C12 C11 P1 122.1(2) . . ? C16 C11 P1 118.9(2) . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H121 119.9 . . ? C13 C12 H121 119.9 . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H131 120.0 . . ? C12 C13 H131 120.0 . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H141 120.1 . . ? C13 C14 H141 120.1 . . ? C14 C15 C16 120.8(4) . . ? C14 C15 H151 119.6 . . ? C16 C15 H151 119.6 . . ? C15 C16 C11 120.3(4) . . ? C15 C16 H161 119.8 . . ? C11 C16 H161 119.8 . . ? N7 C20 P2 113.48(18) . . ? N7 C20 H201 108.9 . . ? P2 C20 H201 108.9 . . ? N7 C20 H202 108.9 . . ? P2 C20 H202 108.9 . . ? H201 C20 H202 107.7 . . ? O22 P2 O21 119.18(11) . . ? O22 P2 C21 105.91(11) . . ? O21 P2 C21 109.12(12) . . ? O22 P2 C20 106.00(12) . . ? O21 P2 C20 106.14(11) . . ? C21 P2 C20 110.36(13) . . ? P2 O21 Mn1 120.62(10) . . ? P2 O22 Mn1 141.24(12) . 2_667 ? C26 C21 C22 119.2(2) . . ? C26 C21 P2 120.9(2) . . ? C22 C21 P2 119.9(2) . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H221 119.8 . . ? C21 C22 H221 119.8 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H231 120.1 . . ? C22 C23 H231 120.1 . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H241 119.8 . . ? C25 C24 H241 119.8 . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H251 119.8 . . ? C26 C25 H251 119.8 . . ? C21 C26 C25 119.8(3) . . ? C21 C26 H261 120.1 . . ? C25 C26 H261 120.1 . . ? H11W O1W H12W 104.6 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.456 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.074 _publ_section_references ; A. Altomare, G. Cascarano, C. Giacovazzo, A. Guagliardi, M.C. Burla, G. Polidori & M. Camalli (1994). J. Appl. Cryst. 27, 435. R.W. Hooft (1998). COLLECT. Nonius BV, Delft, The Netherlands. Z. Otwinowski & W. Minor (1997). Methods Enzymol. 276, 307. G.M. Sheldrick (1997). SHELXL97. University of Gottingen, Germany. A.L. Spek (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ;