########################################################################## # # # ### # # ### ### # ### # # ### # # ### # ### # # # # # # # # # # # # # ## ## # ## # # # # # # # # # # ### # # ### ### # ### # # # ### # ## # ### ### # # # # # # # # # # # # # # # # # # ## # # # ### ### # # ### ### # # ### # # # # # # # # # # # # # # # # # ### ### ### # # # # # ## ## # # # # # # # # # # # # # # # ### # ### ### # ### # # # # # # # # # ## # # # # # # # # # # # ### # # # # # ### # # # ########################################################################## # Compound: CoPEster ########################################################################## # # # This Supplementary Material is written in the Crystallographic # # Information File (CIF) format. For further details see: S.R. Hall, # # F.H. Allen and I.D. Brown, Acta Cryst. (1991) A47, 655-685. # # # ########################################################################## ########################################################################## _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [CoCl(dmgH)2(C5H4N-PO3Et2)] _chemical_melting_point ? _chemical_formula_moiety 'C17 H28 Cl Co N5 O7 P' _chemical_formula_sum 'C17 H28 Cl Co N5 O7 P' _chemical_formula_weight 539.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2787(6) _cell_length_b 12.8802(10) _cell_length_c 21.4315(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.937(7) _cell_angle_gamma 90.00 _cell_volume 2276.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.61 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8657 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details 'see below' _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7793 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4616 _reflns_number_gt 3178 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) (compiled Dec 8 2009,17:31:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4616 _refine_ls_number_parameters 301 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.76766(4) 0.95883(2) 0.157616(14) 0.00884(9) Uani 1 1 d . . . Cl1 Cl 0.62779(7) 0.96603(4) 0.06467(3) 0.01426(13) Uani 1 1 d . . . P1 P 1.22609(7) 0.93887(5) 0.41985(3) 0.01128(14) Uani 1 1 d . . . N1 N 0.8876(2) 0.95242(14) 0.24035(8) 0.0078(4) Uani 1 1 d . . . O3 O 0.65661(19) 0.75417(11) 0.17131(8) 0.0136(4) Uani 1 1 d . . . O2 O 0.9113(2) 0.76995(12) 0.11975(8) 0.0162(4) Uani 1 1 d D . . O1 O 0.8806(2) 1.16538(13) 0.13928(8) 0.0174(4) Uani 1 1 d D . . N2 N 0.6130(2) 1.04386(14) 0.19062(9) 0.0103(4) Uani 1 1 d . . . N3 N 0.6287(2) 0.85397(14) 0.18140(9) 0.0093(4) Uani 1 1 d . . . O4 O 0.6246(2) 1.14678(12) 0.19011(8) 0.0155(4) Uani 1 1 d . . . N5 N 0.9080(2) 1.06323(14) 0.13155(9) 0.0118(4) Uani 1 1 d . . . N4 N 0.9232(2) 0.87465(14) 0.12226(9) 0.0116(4) Uani 1 1 d . . . C2 C 1.0179(3) 1.03595(17) 0.33000(11) 0.0110(5) Uani 1 1 d . . . H2A H 1.0396 1.0981 0.3531 0.013 Uiso 1 1 calc R . . C11 C 1.0333(3) 1.03370(19) 0.10454(11) 0.0138(5) Uani 1 1 d . . . C6 C 0.4943(3) 0.99754(18) 0.21378(11) 0.0106(5) Uani 1 1 d . . . C3 C 1.0817(3) 0.94259(17) 0.35229(10) 0.0098(5) Uani 1 1 d . . . C10 C 1.0412(3) 0.92045(19) 0.09853(11) 0.0141(5) Uani 1 1 d . . . C7 C 0.5032(3) 0.88474(18) 0.20875(11) 0.0114(5) Uani 1 1 d . . . C5 C 0.9417(3) 0.86047(17) 0.26356(11) 0.0109(5) Uani 1 1 d . . . H5A H 0.9129 0.7987 0.2410 0.013 Uiso 1 1 calc R . . C4 C 1.0377(3) 0.85362(17) 0.31913(11) 0.0113(5) Uani 1 1 d . . . H4A H 1.0737 0.7877 0.3346 0.014 Uiso 1 1 calc R . . C1 C 0.9232(3) 1.03824(17) 0.27432(11) 0.0109(5) Uani 1 1 d . . . H1A H 0.8811 1.1030 0.2592 0.013 Uiso 1 1 calc R . . C13 C 1.1541(3) 1.1045(2) 0.08010(12) 0.0224(6) Uani 1 1 d . . . H13A H 1.1392 1.1057 0.0342 0.034 Uiso 1 1 calc R . . H13B H 1.2637 1.0799 0.0935 0.034 Uiso 1 1 calc R . . H13C H 1.1394 1.1746 0.0964 0.034 Uiso 1 1 calc R . . C9 C 0.3818(3) 0.81240(19) 0.23113(12) 0.0200(6) Uani 1 1 d . . . H9A H 0.3807 0.7481 0.2066 0.030 Uiso 1 1 calc R . . H9B H 0.2743 0.8447 0.2261 0.030 Uiso 1 1 calc R . . H9C H 0.4101 0.7965 0.2754 0.030 Uiso 1 1 calc R . . C8 C 0.3619(3) 1.05284(19) 0.24225(12) 0.0201(6) Uani 1 1 d . . . H8A H 0.3839 1.1276 0.2428 0.030 Uiso 1 1 calc R . . H8B H 0.3553 1.0281 0.2852 0.030 Uiso 1 1 calc R . . H8C H 0.2588 1.0394 0.2176 0.030 Uiso 1 1 calc R . . C12 C 1.1693(3) 0.8675(2) 0.06625(12) 0.0221(6) Uani 1 1 d . . . H12A H 1.1504 0.7924 0.0663 0.033 Uiso 1 1 calc R . . H12B H 1.2755 0.8827 0.0881 0.033 Uiso 1 1 calc R . . H12C H 1.1668 0.8924 0.0230 0.033 Uiso 1 1 calc R . . O5 O 1.2224(2) 1.03150(12) 0.45834(8) 0.0187(4) Uani 1 1 d . . . O6 O 1.38111(19) 0.91821(13) 0.38515(8) 0.0177(4) Uani 1 1 d . . . O7 O 1.20456(18) 0.83362(12) 0.45405(8) 0.0138(4) Uani 1 1 d . . . C16 C 1.0871(3) 0.8209(2) 0.50072(12) 0.0226(6) Uani 1 1 d . . . H16A H 1.0529 0.8900 0.5151 0.027 Uiso 1 1 calc R . . H16B H 1.1379 0.7828 0.5374 0.027 Uiso 1 1 calc R . . C14 C 1.5393(3) 0.9118(2) 0.42014(12) 0.0196(6) Uani 1 1 d . . . H14A H 1.5818 0.8401 0.4186 0.023 Uiso 1 1 calc R . . H14B H 1.5302 0.9305 0.4645 0.023 Uiso 1 1 calc R . . C17 C 0.9433(3) 0.7626(2) 0.47300(14) 0.0262(6) Uani 1 1 d . . . H17A H 0.8650 0.7544 0.5045 0.039 Uiso 1 1 calc R . . H17B H 0.9774 0.6940 0.4593 0.039 Uiso 1 1 calc R . . H17C H 0.8927 0.8010 0.4370 0.039 Uiso 1 1 calc R . . C18 C 1.6497(4) 0.9841(2) 0.39201(15) 0.0386(8) Uani 1 1 d U . . H18A H 1.7569 0.9808 0.4152 0.058 Uiso 1 1 calc R . . H18B H 1.6070 1.0549 0.3939 0.058 Uiso 1 1 calc R . . H18C H 1.6588 0.9647 0.3482 0.058 Uiso 1 1 calc R . . H1 H 0.788(3) 1.165(2) 0.1569(13) 0.035(9) Uiso 1 1 d D . . H2 H 0.817(3) 0.760(3) 0.1342(16) 0.066(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00782(17) 0.00941(16) 0.00918(16) 0.00041(13) 0.00009(11) 0.00006(14) Cl1 0.0134(3) 0.0182(3) 0.0104(3) 0.0013(2) -0.0026(2) -0.0005(3) P1 0.0081(3) 0.0150(3) 0.0102(3) -0.0009(2) -0.0018(2) -0.0005(3) N1 0.0040(9) 0.0088(9) 0.0111(10) 0.0006(8) 0.0026(7) 0.0001(8) O3 0.0143(9) 0.0071(8) 0.0194(9) -0.0014(7) 0.0011(7) -0.0018(7) O2 0.0163(10) 0.0087(8) 0.0239(10) -0.0034(7) 0.0039(8) 0.0014(8) O1 0.0178(10) 0.0108(9) 0.0238(10) 0.0018(7) 0.0031(8) -0.0030(8) N2 0.0123(10) 0.0079(10) 0.0099(9) 0.0002(8) -0.0030(8) 0.0035(9) N3 0.0092(10) 0.0087(10) 0.0092(10) -0.0005(8) -0.0027(8) 0.0006(8) O4 0.0190(10) 0.0061(8) 0.0213(10) 0.0005(7) 0.0013(7) 0.0029(7) N5 0.0149(11) 0.0096(10) 0.0102(10) 0.0011(8) -0.0023(8) -0.0003(8) N4 0.0118(11) 0.0102(10) 0.0123(11) 0.0000(8) -0.0019(8) 0.0000(9) C2 0.0086(11) 0.0111(11) 0.0137(12) -0.0031(10) 0.0039(9) -0.0023(10) C11 0.0108(12) 0.0197(13) 0.0111(12) 0.0009(10) 0.0020(9) -0.0024(11) C6 0.0073(12) 0.0142(12) 0.0104(12) 0.0015(9) 0.0002(9) 0.0034(10) C3 0.0034(11) 0.0147(12) 0.0113(11) 0.0002(9) 0.0012(8) 0.0000(10) C10 0.0105(12) 0.0206(13) 0.0113(12) -0.0017(10) 0.0016(9) 0.0001(11) C7 0.0087(12) 0.0154(12) 0.0098(12) 0.0011(10) -0.0009(9) -0.0009(10) C5 0.0088(12) 0.0098(11) 0.0146(12) 0.0007(10) 0.0031(9) -0.0028(10) C4 0.0092(12) 0.0095(11) 0.0151(13) 0.0021(9) 0.0014(9) 0.0008(10) C1 0.0083(11) 0.0092(11) 0.0154(12) 0.0002(10) 0.0020(9) 0.0003(10) C13 0.0197(15) 0.0283(15) 0.0196(14) 0.0048(11) 0.0046(11) -0.0105(12) C9 0.0154(14) 0.0224(14) 0.0231(14) 0.0029(11) 0.0066(11) -0.0037(11) C8 0.0159(13) 0.0229(14) 0.0227(14) 0.0026(11) 0.0072(10) 0.0086(12) C12 0.0143(14) 0.0299(15) 0.0230(15) -0.0025(12) 0.0074(11) 0.0018(12) O5 0.0209(10) 0.0157(9) 0.0182(9) -0.0034(7) -0.0061(7) 0.0000(8) O6 0.0059(9) 0.0320(10) 0.0148(9) -0.0030(8) -0.0011(7) -0.0001(8) O7 0.0115(9) 0.0162(9) 0.0138(9) 0.0021(7) 0.0015(7) 0.0009(7) C16 0.0239(15) 0.0300(15) 0.0148(14) 0.0045(11) 0.0071(11) -0.0062(12) C14 0.0068(13) 0.0290(14) 0.0217(14) -0.0037(11) -0.0055(10) -0.0001(11) C17 0.0231(15) 0.0254(15) 0.0312(17) 0.0040(13) 0.0087(12) -0.0052(13) C18 0.0257(13) 0.0540(15) 0.0353(14) 0.0078(12) -0.0011(11) -0.0122(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 Co1 N2 1.8697(19) . ? Co1 N3 1.8729(19) . ? Co1 N4 1.891(2) . ? Co1 N5 1.892(2) . ? Co1 N1 1.9578(18) . ? Co1 Cl1 2.2181(6) . ? P1 O5 1.4522(17) . ? P1 O7 1.5587(16) . ? P1 O6 1.5605(17) . ? P1 C3 1.797(2) . ? N1 C1 1.342(3) . ? N1 C5 1.346(3) . ? O3 N3 1.327(2) . ? O2 N4 1.353(2) . ? O2 H2 0.874(18) . ? O1 N5 1.348(2) . ? O1 H1 0.884(17) . ? N2 C6 1.285(3) . ? N2 O4 1.329(2) . ? N3 C7 1.298(3) . ? N5 C11 1.288(3) . ? N4 C10 1.283(3) . ? C2 C1 1.371(3) . ? C2 C3 1.382(3) . ? C2 H2A 0.9500 . ? C11 C10 1.466(3) . ? C11 C13 1.482(3) . ? C6 C7 1.459(3) . ? C6 C8 1.482(3) . ? C3 C4 1.381(3) . ? C10 C12 1.481(3) . ? C7 C9 1.480(3) . ? C5 C4 1.376(3) . ? C5 H5A 0.9500 . ? C4 H4A 0.9500 . ? C1 H1A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O6 C14 1.455(3) . ? O7 C16 1.463(3) . ? C16 C17 1.488(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C14 C18 1.469(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 N2 Co1 N3 82.11(8) . . ? N2 Co1 N4 178.54(8) . . ? N3 Co1 N4 98.68(8) . . ? N2 Co1 N5 98.82(8) . . ? N3 Co1 N5 178.55(8) . . ? N4 Co1 N5 80.37(8) . . ? N2 Co1 N1 89.57(7) . . ? N3 Co1 N1 89.92(8) . . ? N4 Co1 N1 91.66(8) . . ? N5 Co1 N1 91.21(8) . . ? N2 Co1 Cl1 89.64(6) . . ? N3 Co1 Cl1 89.38(6) . . ? N4 Co1 Cl1 89.14(6) . . ? N5 Co1 Cl1 89.51(6) . . ? N1 Co1 Cl1 179.00(6) . . ? O5 P1 O7 116.02(9) . . ? O5 P1 O6 117.98(10) . . ? O7 P1 O6 101.99(9) . . ? O5 P1 C3 113.00(10) . . ? O7 P1 C3 107.88(10) . . ? O6 P1 C3 97.93(10) . . ? C1 N1 C5 118.26(19) . . ? C1 N1 Co1 121.80(15) . . ? C5 N1 Co1 119.90(15) . . ? N4 O2 H2 101(2) . . ? N5 O1 H1 102(2) . . ? C6 N2 O4 121.65(19) . . ? C6 N2 Co1 116.45(15) . . ? O4 N2 Co1 121.90(15) . . ? C7 N3 O3 121.77(19) . . ? C7 N3 Co1 115.90(16) . . ? O3 N3 Co1 122.32(14) . . ? C11 N5 O1 119.6(2) . . ? C11 N5 Co1 117.47(16) . . ? O1 N5 Co1 122.92(15) . . ? C10 N4 O2 119.8(2) . . ? C10 N4 Co1 117.60(15) . . ? O2 N4 Co1 122.54(15) . . ? C1 C2 C3 119.5(2) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? N5 C11 C10 112.2(2) . . ? N5 C11 C13 124.9(2) . . ? C10 C11 C13 122.9(2) . . ? N2 C6 C7 112.9(2) . . ? N2 C6 C8 123.6(2) . . ? C7 C6 C8 123.6(2) . . ? C4 C3 C2 117.9(2) . . ? C4 C3 P1 121.35(17) . . ? C2 C3 P1 120.64(17) . . ? N4 C10 C11 112.4(2) . . ? N4 C10 C12 125.0(2) . . ? C11 C10 C12 122.6(2) . . ? N3 C7 C6 112.6(2) . . ? N3 C7 C9 123.1(2) . . ? C6 C7 C9 124.2(2) . . ? N1 C5 C4 121.7(2) . . ? N1 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C1 C2 122.5(2) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 O6 P1 120.33(16) . . ? C16 O7 P1 121.88(16) . . ? O7 C16 C17 109.8(2) . . ? O7 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? O7 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? O6 C14 C18 108.5(2) . . ? O6 C14 H14A 110.0 . . ? C18 C14 H14A 110.0 . . ? O6 C14 H14B 110.0 . . ? C18 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 O1 H1 O4 0.884(17) 1.598(18) 2.476(2) 172(3) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.509 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.074