# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 N2 Ni O10, 2(C13 H11 N2), 4(H2 O)' _chemical_formula_sum 'C40 H36 N6 Ni O14' _chemical_formula_weight 883.46 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' Ni Ni 0.3393 1.1124 '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 11.8637(16) _cell_length_b 13.8353(18) _cell_length_c 14.0619(18) _cell_angle_alpha 111.7810(10) _cell_angle_beta 113.2290(10) _cell_angle_gamma 92.745(2) _cell_volume 1917.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.44 _exptl_crystal_description Block _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7765 _exptl_absorpt_correction_T_max 0.9404 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 30 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16906 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.53 _reflns_number_total 8752 _reflns_number_gt 7550 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2008)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2008)' _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. H-atoms attached to carbon were placed in calculated positions (C---H = 0.95 \%A) while those attached to nitrogen and oxygen were placed in locations derived from a difference map and their coordinates adjusted to give N---H distances of 0.88 \%A (aliphatic) and 0.91 \%A (aromatic) and O---H distances of 0.84 \%A. All were included as riding contributions with isotropic displacement parameters 1.2 times those of the attached atoms. ; _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^)+(0.0480P)^2^+1.2546P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8752 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ni1 Ni 0.81130(2) -0.009153(19) 0.69193(2) 0.01565(8) Uani 1 1 d . . . O1 O 0.69990(13) -0.07005(11) 0.75469(11) 0.0190(3) Uani 1 1 d . . . O2 O 0.71871(13) -0.13228(12) 0.88558(12) 0.0219(3) Uani 1 1 d . . . O3 O 0.97448(14) 0.01797(12) 0.66947(13) 0.0237(3) Uani 1 1 d . . . O4 O 1.16573(16) -0.01820(13) 0.71079(16) 0.0314(4) Uani 1 1 d . . . O5 O 1.19218(15) -0.15782(14) 1.01024(13) 0.0305(4) Uani 1 1 d . . . H5O H 1.1721 -0.1585 1.0610 0.037 Uiso 1 1 d R . . O6 O 0.72812(14) -0.13576(11) 0.52508(12) 0.0207(3) Uani 1 1 d . . . O7 O 0.61552(14) -0.16834(11) 0.34103(12) 0.0210(3) Uani 1 1 d . . . O8 O 0.84349(13) 0.14919(11) 0.81784(11) 0.0193(3) Uani 1 1 d . . . O9 O 0.78399(15) 0.30391(12) 0.83358(12) 0.0272(3) Uani 1 1 d . . . O10 O 0.50372(13) 0.20784(10) 0.41003(12) 0.0189(3) Uani 1 1 d . . . H10O H 0.4413 0.1636 0.3511 0.023 Uiso 1 1 d R . . N1 N 0.92945(15) -0.06702(12) 0.78889(13) 0.0151(3) Uani 1 1 d . . . N2 N 0.70753(15) 0.05892(12) 0.59931(13) 0.0137(3) Uani 1 1 d . . . C1 C 0.76077(18) -0.10260(15) 0.83069(16) 0.0161(4) Uani 1 1 d . . . C2 C 0.89641(17) -0.10368(14) 0.85174(15) 0.0142(3) Uani 1 1 d . . . C3 C 0.97990(18) -0.13650(14) 0.92824(15) 0.0157(4) Uani 1 1 d . . . H3 H 0.9546 -0.1633 0.9717 0.019 Uiso 1 1 calc R . . C4 C 1.10350(19) -0.12886(15) 0.93957(16) 0.0185(4) Uani 1 1 d . . . C5 C 1.13657(18) -0.09007(15) 0.87287(16) 0.0178(4) Uani 1 1 d . . . H5 H 1.2195 -0.0845 0.8790 0.021 Uiso 1 1 calc R . . C6 C 1.04673(18) -0.06035(14) 0.79859(16) 0.0163(4) Uani 1 1 d . . . C7 C 1.0664(2) -0.01666(16) 0.72059(19) 0.0215(4) Uani 1 1 d . . . C8 C 0.66232(18) -0.11014(15) 0.44600(16) 0.0165(4) Uani 1 1 d . . . C9 C 0.64287(17) 0.00301(14) 0.48583(15) 0.0133(3) Uani 1 1 d . . . C10 C 0.57179(17) 0.04902(14) 0.41736(15) 0.0137(3) Uani 1 1 d . . . H10 H 0.5250 0.0085 0.3371 0.016 Uiso 1 1 calc R . . C11 C 0.57039(17) 0.15710(14) 0.46922(16) 0.0133(3) Uani 1 1 d . . . C12 C 0.64279(17) 0.21502(14) 0.58745(16) 0.0139(3) Uani 1 1 d . . . H12 H 0.6463 0.2890 0.6241 0.017 Uiso 1 1 calc R . . C13 C 0.70847(17) 0.16202(14) 0.64890(15) 0.0131(3) Uani 1 1 d . . . C14 C 0.78486(18) 0.21148(16) 0.77742(16) 0.0178(4) Uani 1 1 d . . . N3 N 0.65012(16) 0.63650(13) 0.20613(14) 0.0187(3) Uani 1 1 d . . . H3N H 0.6458 0.7014 0.2523 0.022 Uiso 1 1 d R . . N4 N 0.65988(19) 0.34672(15) -0.01850(16) 0.0297(4) Uani 1 1 d . . . H4A H 0.6055 0.2886 -0.0394 0.036 Uiso 1 1 d R . . H4B H 0.7025 0.3363 -0.0590 0.036 Uiso 1 1 d R . . C15 C 0.57508(19) 0.54583(15) 0.18426(16) 0.0186(4) Uani 1 1 d . . . C16 C 0.4931(2) 0.55424(16) 0.23576(18) 0.0233(4) Uani 1 1 d . . . H16 H 0.4912 0.6224 0.2854 0.028 Uiso 1 1 calc R . . C17 C 0.4163(2) 0.46389(18) 0.21401(19) 0.0281(5) Uani 1 1 d . . . H17 H 0.3602 0.4698 0.2479 0.034 Uiso 1 1 calc R . . C18 C 0.4194(2) 0.36222(18) 0.14191(19) 0.0304(5) Uani 1 1 d . . . H18 H 0.3667 0.3000 0.1286 0.037 Uiso 1 1 calc R . . C19 C 0.4980(2) 0.35284(17) 0.09123(18) 0.0272(5) Uani 1 1 d . . . H19 H 0.4996 0.2839 0.0429 0.033 Uiso 1 1 calc R . . C20 C 0.57738(19) 0.44460(16) 0.10971(16) 0.0210(4) Uani 1 1 d . . . C21 C 0.6582(2) 0.43915(17) 0.05464(17) 0.0225(4) Uani 1 1 d . . . C22 C 0.73646(19) 0.53695(17) 0.08067(17) 0.0214(4) Uani 1 1 d . . . C23 C 0.8208(2) 0.54002(19) 0.03280(18) 0.0283(5) Uani 1 1 d . . . H23 H 0.8269 0.4753 -0.0190 0.034 Uiso 1 1 calc R . . C24 C 0.8932(2) 0.6343(2) 0.05989(19) 0.0321(5) Uani 1 1 d . . . H24 H 0.9499 0.6347 0.0275 0.038 Uiso 1 1 calc R . . C25 C 0.8847(2) 0.73143(19) 0.13571(19) 0.0291(5) Uani 1 1 d . . . H25 H 0.9350 0.7969 0.1534 0.035 Uiso 1 1 calc R . . C26 C 0.80439(19) 0.73221(17) 0.18419(18) 0.0243(4) Uani 1 1 d . . . H26 H 0.7993 0.7979 0.2355 0.029 Uiso 1 1 calc R . . C27 C 0.72942(18) 0.63503(16) 0.15750(16) 0.0193(4) Uani 1 1 d . . . N5 N 0.81432(16) 0.41147(13) 0.36041(15) 0.0210(3) Uani 1 1 d . . . H5N H 0.7894 0.3402 0.3384 0.025 Uiso 1 1 d R . . N6 N 0.90047(16) 0.73904(13) 0.47697(15) 0.0202(3) Uani 1 1 d . . . H6A H 0.8454 0.7715 0.4958 0.024 Uiso 1 1 d R . . H6B H 0.9594 0.7788 0.4755 0.024 Uiso 1 1 d R . . C28 C 0.76764(18) 0.47174(15) 0.43124(16) 0.0181(4) Uani 1 1 d . . . C29 C 0.68857(19) 0.42012(16) 0.45945(18) 0.0209(4) Uani 1 1 d . . . H29 H 0.6668 0.3443 0.4281 0.025 Uiso 1 1 calc R . . C30 C 0.6435(2) 0.48005(17) 0.53213(18) 0.0225(4) Uani 1 1 d . . . H30 H 0.5907 0.4454 0.5517 0.027 Uiso 1 1 calc R . . C31 C 0.6741(2) 0.59264(16) 0.57869(18) 0.0226(4) Uani 1 1 d . . . H31 H 0.6427 0.6332 0.6298 0.027 Uiso 1 1 calc R . . C32 C 0.74877(19) 0.64325(16) 0.55040(17) 0.0202(4) Uani 1 1 d . . . H32 H 0.7683 0.7191 0.5815 0.024 Uiso 1 1 calc R . . C33 C 0.79775(18) 0.58423(15) 0.47509(17) 0.0179(4) Uani 1 1 d . . . C34 C 0.87784(18) 0.63470(15) 0.44427(16) 0.0169(4) Uani 1 1 d . . . C35 C 0.93166(18) 0.56770(16) 0.37524(16) 0.0180(4) Uani 1 1 d . . . C36 C 1.01606(19) 0.60976(17) 0.34417(17) 0.0208(4) Uani 1 1 d . . . H36 H 1.0426 0.6850 0.3726 0.025 Uiso 1 1 calc R . . C37 C 1.0599(2) 0.54293(18) 0.27349(18) 0.0253(4) Uani 1 1 d . . . H37 H 1.1161 0.5719 0.2528 0.030 Uiso 1 1 calc R . . C38 C 1.0214(2) 0.43142(18) 0.23169(19) 0.0284(5) Uani 1 1 d . . . H38 H 1.0515 0.3855 0.1824 0.034 Uiso 1 1 calc R . . C39 C 0.9416(2) 0.38848(17) 0.26086(19) 0.0269(5) Uani 1 1 d . . . H39 H 0.9169 0.3131 0.2325 0.032 Uiso 1 1 calc R . . C40 C 0.89542(18) 0.45592(16) 0.33322(16) 0.0193(4) Uani 1 1 d . . . O11 O 0.92509(15) 0.12209(12) 0.53011(14) 0.0281(3) Uani 1 1 d . . . H11A H 0.8899 0.0765 0.4612 0.034 Uiso 1 1 d R . . H11B H 0.9463 0.0891 0.5717 0.034 Uiso 1 1 d R . . O12 O 0.49078(15) 0.04790(13) 0.10554(14) 0.0312(4) Uani 1 1 d . . . H12A H 0.4309 0.0771 0.1080 0.037 Uiso 1 1 d R . . H12B H 0.4759 -0.0105 0.1087 0.037 Uiso 1 1 d R . . O13 O 0.71736(14) 0.19350(11) 0.28593(14) 0.0272(3) Uani 1 1 d . . . H13A H 0.6809 0.1802 0.2152 0.033 Uiso 1 1 d R . . H13B H 0.7567 0.1451 0.2907 0.033 Uiso 1 1 d R . . O14 O 0.4968(4) 0.8465(3) 0.1347(3) 0.0260(6) Uani 0.510(4) 1 d P A 1 H14A H 0.5500 0.8571 0.2004 0.031 Uiso 0.510(4) 1 d PR A 1 H14B H 0.5020 0.9049 0.1294 0.031 Uiso 0.510(4) 1 d PR A 1 O14A O 0.5575(4) 0.8763(3) 0.1514(3) 0.0260(6) Uani 0.490(4) 1 d P A 2 H14C H 0.5579 0.8616 0.2043 0.031 Uiso 0.490(4) 1 d PR A 2 H14D H 0.6305 0.9107 0.1744 0.031 Uiso 0.490(4) 1 d PR A 2 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 Ni1 0.02098(14) 0.01928(14) 0.01606(13) 0.01189(10) 0.01220(10) 0.01178(10) O1 0.0175(7) 0.0262(7) 0.0167(7) 0.0120(6) 0.0080(6) 0.0069(5) O2 0.0211(7) 0.0270(8) 0.0217(7) 0.0133(6) 0.0110(6) 0.0014(6) O3 0.0350(8) 0.0267(8) 0.0329(8) 0.0233(7) 0.0261(7) 0.0199(6) O4 0.0371(9) 0.0331(9) 0.0558(11) 0.0308(8) 0.0378(9) 0.0220(7) O5 0.0344(9) 0.0554(11) 0.0189(7) 0.0241(7) 0.0178(7) 0.0318(8) O6 0.0337(8) 0.0186(7) 0.0211(7) 0.0125(6) 0.0179(6) 0.0162(6) O7 0.0327(8) 0.0154(7) 0.0173(7) 0.0053(5) 0.0146(6) 0.0088(6) O8 0.0228(7) 0.0261(7) 0.0142(6) 0.0107(6) 0.0103(6) 0.0134(6) O9 0.0345(8) 0.0255(8) 0.0157(7) 0.0025(6) 0.0101(6) 0.0181(7) O10 0.0214(7) 0.0140(6) 0.0171(7) 0.0081(5) 0.0031(6) 0.0060(5) N1 0.0185(8) 0.0149(8) 0.0165(7) 0.0094(6) 0.0091(6) 0.0062(6) N2 0.0183(8) 0.0145(7) 0.0130(7) 0.0070(6) 0.0099(6) 0.0078(6) C1 0.0177(9) 0.0149(9) 0.0134(8) 0.0040(7) 0.0067(7) 0.0015(7) C2 0.0190(9) 0.0102(8) 0.0128(8) 0.0038(7) 0.0075(7) 0.0025(7) C3 0.0248(10) 0.0123(8) 0.0119(8) 0.0054(7) 0.0095(7) 0.0061(7) C4 0.0244(10) 0.0191(9) 0.0114(8) 0.0051(7) 0.0080(8) 0.0119(8) C5 0.0177(9) 0.0185(9) 0.0159(9) 0.0045(7) 0.0084(7) 0.0081(7) C6 0.0216(9) 0.0127(8) 0.0183(9) 0.0059(7) 0.0127(8) 0.0063(7) C7 0.0298(11) 0.0177(9) 0.0302(11) 0.0145(8) 0.0210(9) 0.0121(8) C8 0.0230(9) 0.0154(9) 0.0187(9) 0.0089(7) 0.0145(8) 0.0078(7) C9 0.0171(9) 0.0137(8) 0.0143(8) 0.0067(7) 0.0109(7) 0.0052(7) C10 0.0157(8) 0.0134(8) 0.0132(8) 0.0054(7) 0.0078(7) 0.0029(7) C11 0.0141(8) 0.0134(8) 0.0163(9) 0.0092(7) 0.0077(7) 0.0037(6) C12 0.0152(8) 0.0125(8) 0.0162(9) 0.0061(7) 0.0089(7) 0.0043(6) C13 0.0153(8) 0.0131(8) 0.0139(8) 0.0050(7) 0.0098(7) 0.0051(7) C14 0.0186(9) 0.0239(10) 0.0130(9) 0.0074(8) 0.0089(7) 0.0094(7) N3 0.0226(8) 0.0159(8) 0.0159(8) 0.0029(6) 0.0102(7) 0.0081(6) N4 0.0352(10) 0.0262(10) 0.0212(9) 0.0022(7) 0.0126(8) 0.0166(8) C15 0.0240(10) 0.0162(9) 0.0130(8) 0.0054(7) 0.0061(8) 0.0086(7) C16 0.0326(11) 0.0178(10) 0.0200(10) 0.0050(8) 0.0148(9) 0.0079(8) C17 0.0365(12) 0.0263(11) 0.0239(11) 0.0093(9) 0.0170(10) 0.0065(9) C18 0.0427(13) 0.0192(10) 0.0256(11) 0.0082(9) 0.0133(10) 0.0025(9) C19 0.0369(12) 0.0167(10) 0.0199(10) 0.0038(8) 0.0083(9) 0.0087(9) C20 0.0253(10) 0.0179(10) 0.0140(9) 0.0035(7) 0.0058(8) 0.0104(8) C21 0.0247(10) 0.0230(10) 0.0130(9) 0.0039(8) 0.0042(8) 0.0142(8) C22 0.0203(10) 0.0248(10) 0.0146(9) 0.0043(8) 0.0067(8) 0.0117(8) C23 0.0230(10) 0.0382(13) 0.0169(10) 0.0035(9) 0.0093(9) 0.0147(9) C24 0.0208(11) 0.0482(15) 0.0227(11) 0.0067(10) 0.0130(9) 0.0101(10) C25 0.0209(10) 0.0362(13) 0.0227(11) 0.0053(9) 0.0099(9) 0.0026(9) C26 0.0218(10) 0.0264(11) 0.0195(10) 0.0037(8) 0.0098(8) 0.0064(8) C27 0.0174(9) 0.0242(10) 0.0131(8) 0.0045(8) 0.0065(7) 0.0095(8) N5 0.0240(9) 0.0154(8) 0.0219(8) 0.0053(7) 0.0108(7) 0.0064(7) N6 0.0246(9) 0.0176(8) 0.0266(9) 0.0111(7) 0.0169(7) 0.0097(7) C28 0.0185(9) 0.0184(9) 0.0166(9) 0.0077(7) 0.0064(8) 0.0072(7) C29 0.0234(10) 0.0148(9) 0.0234(10) 0.0086(8) 0.0085(8) 0.0062(7) C30 0.0246(10) 0.0227(10) 0.0266(10) 0.0150(9) 0.0128(9) 0.0080(8) C31 0.0288(11) 0.0212(10) 0.0273(10) 0.0128(8) 0.0183(9) 0.0129(8) C32 0.0266(10) 0.0160(9) 0.0232(10) 0.0096(8) 0.0140(9) 0.0097(8) C33 0.0191(9) 0.0178(9) 0.0183(9) 0.0091(8) 0.0081(8) 0.0082(7) C34 0.0183(9) 0.0193(9) 0.0140(8) 0.0085(7) 0.0063(7) 0.0087(7) C35 0.0171(9) 0.0218(10) 0.0144(9) 0.0074(7) 0.0061(7) 0.0094(7) C36 0.0188(9) 0.0221(10) 0.0193(9) 0.0070(8) 0.0076(8) 0.0078(8) C37 0.0217(10) 0.0307(11) 0.0228(10) 0.0080(9) 0.0120(9) 0.0087(9) C38 0.0283(11) 0.0305(12) 0.0235(11) 0.0035(9) 0.0156(9) 0.0132(9) C39 0.0304(11) 0.0205(10) 0.0241(11) 0.0024(8) 0.0129(9) 0.0085(9) C40 0.0185(9) 0.0211(10) 0.0160(9) 0.0054(8) 0.0072(8) 0.0085(7) O11 0.0414(9) 0.0298(8) 0.0360(9) 0.0246(7) 0.0279(8) 0.0172(7) O12 0.0328(9) 0.0267(8) 0.0372(9) 0.0111(7) 0.0208(8) 0.0060(7) O13 0.0280(8) 0.0177(7) 0.0352(9) 0.0069(6) 0.0173(7) 0.0081(6) O14 0.0317(18) 0.0195(15) 0.0184(11) 0.0060(11) 0.0054(15) 0.0030(12) O14A 0.0317(18) 0.0195(15) 0.0184(11) 0.0060(11) 0.0054(15) 0.0030(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 Ni1 N2 1.9636(15) . ? Ni1 N1 1.9685(16) . ? Ni1 O3 2.1188(15) . ? Ni1 O6 2.1226(14) . ? Ni1 O8 2.1419(14) . ? Ni1 O1 2.1449(14) . ? O1 C1 1.283(2) . ? O2 C1 1.238(2) . ? O3 C7 1.274(2) . ? O4 C7 1.239(2) . ? O5 C4 1.329(2) . ? O5 H5O 0.8399 . ? O6 C8 1.267(2) . ? O7 C8 1.251(2) . ? O8 C14 1.288(2) . ? O9 C14 1.232(2) . ? O10 C11 1.334(2) . ? O10 H10O 0.8400 . ? N1 C2 1.334(2) . ? N1 C6 1.339(2) . ? N2 C13 1.332(2) . ? N2 C9 1.340(2) . ? C1 C2 1.519(3) . ? C2 C3 1.382(3) . ? C3 C4 1.405(3) . ? C3 H3 0.9500 . ? C4 C5 1.402(3) . ? C5 C6 1.371(3) . ? C5 H5 0.9500 . ? C6 C7 1.518(3) . ? C8 C9 1.518(2) . ? C9 C10 1.382(2) . ? C10 C11 1.404(2) . ? C10 H10 0.9500 . ? C11 C12 1.401(3) . ? C12 C13 1.373(2) . ? C12 H12 0.9500 . ? C13 C14 1.512(3) . ? N3 C15 1.361(3) . ? N3 C27 1.361(3) . ? N3 H3N 0.9100 . ? N4 C21 1.317(3) . ? N4 H4A 0.8800 . ? N4 H4B 0.8799 . ? C15 C16 1.409(3) . ? C15 C20 1.414(3) . ? C16 C17 1.369(3) . ? C16 H16 0.9500 . ? C17 C18 1.409(3) . ? C17 H17 0.9500 . ? C18 C19 1.364(3) . ? C18 H18 0.9500 . ? C19 C20 1.419(3) . ? C19 H19 0.9500 . ? C20 C21 1.441(3) . ? C21 C22 1.439(3) . ? C22 C23 1.416(3) . ? C22 C27 1.418(3) . ? C23 C24 1.361(4) . ? C23 H23 0.9500 . ? C24 C25 1.409(3) . ? C24 H24 0.9500 . ? C25 C26 1.371(3) . ? C25 H25 0.9500 . ? C26 C27 1.410(3) . ? C26 H26 0.9500 . ? N5 C28 1.363(2) . ? N5 C40 1.363(3) . ? N5 H5N 0.9100 . ? N6 C34 1.319(3) . ? N6 H6A 0.8799 . ? N6 H6B 0.8800 . ? C28 C29 1.409(3) . ? C28 C33 1.411(3) . ? C29 C30 1.365(3) . ? C29 H29 0.9500 . ? C30 C31 1.410(3) . ? C30 H30 0.9500 . ? C31 C32 1.363(3) . ? C31 H31 0.9500 . ? C32 C33 1.419(3) . ? C32 H32 0.9500 . ? C33 C34 1.437(3) . ? C34 C35 1.445(3) . ? C35 C40 1.408(3) . ? C35 C36 1.418(3) . ? C36 C37 1.373(3) . ? C36 H36 0.9500 . ? C37 C38 1.408(3) . ? C37 H37 0.9500 . ? C38 C39 1.360(3) . ? C38 H38 0.9500 . ? C39 C40 1.410(3) . ? C39 H39 0.9500 . ? O11 H11A 0.8448 . ? O11 H11B 0.8408 . ? O12 H12A 0.8406 . ? O12 H12B 0.8397 . ? O13 H13A 0.8524 . ? O13 H13B 0.8414 . ? O14 H14A 0.8401 . ? O14 H14B 0.8400 . ? O14A H14C 0.8398 . ? O14A H14D 0.8400 . ? 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 Ni1 N1 174.48(7) . . ? N2 Ni1 O3 97.61(6) . . ? N1 Ni1 O3 77.80(6) . . ? N2 Ni1 O6 77.68(6) . . ? N1 Ni1 O6 105.02(6) . . ? O3 Ni1 O6 88.17(6) . . ? N2 Ni1 O8 77.71(6) . . ? N1 Ni1 O8 99.61(6) . . ? O3 Ni1 O8 96.35(6) . . ? O6 Ni1 O8 155.36(5) . . ? N2 Ni1 O1 107.58(6) . . ? N1 Ni1 O1 77.10(6) . . ? O3 Ni1 O1 154.79(5) . . ? O6 Ni1 O1 96.06(6) . . ? O8 Ni1 O1 90.10(5) . . ? C1 O1 Ni1 114.84(12) . . ? C7 O3 Ni1 115.46(12) . . ? C4 O5 H5O 109.1 . . ? C8 O6 Ni1 115.08(12) . . ? C14 O8 Ni1 114.42(12) . . ? C11 O10 H10O 109.4 . . ? C2 N1 C6 120.45(16) . . ? C2 N1 Ni1 120.24(13) . . ? C6 N1 Ni1 119.05(13) . . ? C13 N2 C9 120.62(15) . . ? C13 N2 Ni1 119.67(12) . . ? C9 N2 Ni1 119.57(12) . . ? O2 C1 O1 126.08(18) . . ? O2 C1 C2 119.26(17) . . ? O1 C1 C2 114.66(16) . . ? N1 C2 C3 122.15(17) . . ? N1 C2 C1 112.56(16) . . ? C3 C2 C1 125.28(17) . . ? C2 C3 C4 117.71(17) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? O5 C4 C5 117.35(18) . . ? O5 C4 C3 123.30(18) . . ? C5 C4 C3 119.35(17) . . ? C6 C5 C4 118.62(18) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 121.72(17) . . ? N1 C6 C7 112.77(16) . . ? C5 C6 C7 125.51(18) . . ? O4 C7 O3 126.13(19) . . ? O4 C7 C6 119.43(18) . . ? O3 C7 C6 114.44(17) . . ? O7 C8 O6 126.05(17) . . ? O7 C8 C9 118.76(16) . . ? O6 C8 C9 115.18(16) . . ? N2 C9 C10 121.29(16) . . ? N2 C9 C8 112.16(15) . . ? C10 C9 C8 126.51(16) . . ? C9 C10 C11 118.41(16) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? O10 C11 C12 118.24(16) . . ? O10 C11 C10 122.54(16) . . ? C12 C11 C10 119.22(16) . . ? C13 C12 C11 118.24(16) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N2 C13 C12 122.14(17) . . ? N2 C13 C14 113.19(16) . . ? C12 C13 C14 124.64(16) . . ? O9 C14 O8 126.12(18) . . ? O9 C14 C13 119.06(17) . . ? O8 C14 C13 114.81(16) . . ? C15 N3 C27 122.41(17) . . ? C15 N3 H3N 120.0 . . ? C27 N3 H3N 117.6 . . ? C21 N4 H4A 119.7 . . ? C21 N4 H4B 126.8 . . ? H4A N4 H4B 112.8 . . ? N3 C15 C16 119.01(17) . . ? N3 C15 C20 120.79(19) . . ? C16 C15 C20 120.20(19) . . ? C17 C16 C15 119.78(19) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.7(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 120.1(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.92(19) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C15 C20 C19 118.19(19) . . ? C15 C20 C21 118.81(19) . . ? C19 C20 C21 122.99(18) . . ? N4 C21 C22 120.8(2) . . ? N4 C21 C20 120.7(2) . . ? C22 C21 C20 118.53(17) . . ? C23 C22 C27 118.1(2) . . ? C23 C22 C21 122.92(19) . . ? C27 C22 C21 119.00(18) . . ? C24 C23 C22 121.0(2) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 120.6(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 119.6(2) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N3 C27 C26 119.26(18) . . ? N3 C27 C22 120.43(19) . . ? C26 C27 C22 120.31(19) . . ? C28 N5 C40 122.33(17) . . ? C28 N5 H5N 112.4 . . ? C40 N5 H5N 125.2 . . ? C34 N6 H6A 115.8 . . ? C34 N6 H6B 127.6 . . ? H6A N6 H6B 116.3 . . ? N5 C28 C29 119.09(18) . . ? N5 C28 C33 120.28(18) . . ? C29 C28 C33 120.63(18) . . ? C30 C29 C28 119.41(18) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 121.01(19) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 120.01(19) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.95(18) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C28 C33 C32 117.97(18) . . ? C28 C33 C34 119.45(18) . . ? C32 C33 C34 122.57(18) . . ? N6 C34 C33 120.98(17) . . ? N6 C34 C35 120.95(18) . . ? C33 C34 C35 118.06(17) . . ? C40 C35 C36 118.41(18) . . ? C40 C35 C34 118.95(18) . . ? C36 C35 C34 122.60(18) . . ? C37 C36 C35 120.7(2) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.8(2) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 121.0(2) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 120.0(2) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? N5 C40 C35 120.70(17) . . ? N5 C40 C39 119.17(19) . . ? C35 C40 C39 120.12(19) . . ? H11A O11 H11B 108.1 . . ? H12A O12 H12B 106.9 . . ? H13A O13 H13B 106.4 . . ? H14A O14 H14B 107.6 . . ? H14C O14A H14D 106.9 . . ? 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 O5 H5O O8 0.84 1.74 2.576(2) 171 2_757 O10 H10O O1 0.84 1.76 2.589(2) 170 2_656 N3 H3N O7 0.91 1.92 2.824(2) 173 1_565 N4 H4B O9 0.88 2.03 2.904(3) 174 1_554 N4 H4A O14 0.88 1.84 2.675(4) 157 2_665 N5 H5N O13 0.91 1.90 2.809(2) 173 . N6 H6A O6 0.88 2.00 2.863(2) 168 1_565 N6 H6B O11 0.88 1.94 2.812(2) 173 2_766 O11 H11A O4 0.84 2.04 2.839(2) 157 2_756 O11 H11B O3 0.84 1.91 2.744(2) 172 . O12 H12A O2 0.84 1.99 2.823(2) 174 2_656 O12 H12B O14 0.84 2.15 2.964(4) 163 1_545 O13 H13A O12 0.85 2.36 2.834(2) 115.3 . O13 H13B O4 0.84 2.02 2.857(2) 174 2_756 O14 H14A O7 0.84 1.99 2.773(4) 155 1_565 O14 H14B O12 0.84 2.13 2.964(4) 173 1_565 _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.636 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.071 _iucr_refine_instructions_details ; TITL JTM362_0m in P-1 CELL 0.71073 11.8637 13.8353 14.0619 111.781 113.229 92.745 ZERR 2.00 0.0016 0.0018 0.0018 0.001 0.001 0.002 LATT 1 SFAC C H N O Ni UNIT 80 72 12 28 2 L.S. 4 ACTA 52 BOND $H FMAP 2 PLAN 5 SIZE 0.106 0.177 0.210 MPLA N5 C28 > C40 MPLA N3 C15 > C27 MPLA Ni1 O6 C8 C9 N2 C13 C14 O8 MPLA Ni1 O1 C1 C2 N1 C6 C7 O3 EADP O14 O14a HTAB O5 O8_$1 HTAB O10 O1_$2 HTAB N3 O7_$3 HTAB N4 O9_$8 HTAB N4 O14_$4 HTAB N5 O13 HTAB N6 O6_$3 HTAB N6 O11_$5 HTAB O11 O4_$6 HTAB O11 O3 HTAB O12 O2_$2 HTAB O12 O14_$7 HTAB O13 O12 HTAB O13 O4_$6 HTAB O14 O7_$3 HTAB O14 O12_$3 EQIV $8 x, y, z-1 EQIV $7 x, y-1, z EQIV $6 -x+2, -y, -z+1 EQIV $5 -x+2, -y+1, -z+1 EQIV $4 -x+1, -y+1, -z EQIV $3 x, y+1, z EQIV $2 -x+1, -y, -z+1 EQIV $1 -x+2, -y, -z+2 TEMP -173 WGHT 0.048000 1.254600 FVAR 0.12966 0.51024 NI1 5 0.811299 -0.009153 0.691933 11.00000 0.02098 0.01928 = 0.01606 0.01189 0.01220 0.01178 O1 4 0.699901 -0.070054 0.754689 11.00000 0.01750 0.02618 = 0.01670 0.01196 0.00802 0.00687 O2 4 0.718713 -0.132285 0.885581 11.00000 0.02114 0.02697 = 0.02169 0.01328 0.01101 0.00143 O3 4 0.974485 0.017968 0.669471 11.00000 0.03502 0.02674 = 0.03286 0.02326 0.02612 0.01986 O4 4 1.165734 -0.018198 0.710788 11.00000 0.03711 0.03307 = 0.05579 0.03082 0.03780 0.02197 O5 4 1.192178 -0.157824 1.010242 11.00000 0.03445 0.05543 = 0.01886 0.02410 0.01785 0.03176 AFIX 3 H5O 2 1.172138 -0.158534 1.061022 11.00000 -1.20000 AFIX 0 O6 4 0.728120 -0.135763 0.525078 11.00000 0.03368 0.01860 = 0.02113 0.01250 0.01792 0.01617 O7 4 0.615523 -0.168336 0.341029 11.00000 0.03274 0.01535 = 0.01734 0.00535 0.01461 0.00884 O8 4 0.843487 0.149191 0.817838 11.00000 0.02276 0.02611 = 0.01425 0.01075 0.01035 0.01338 O9 4 0.783987 0.303914 0.833578 11.00000 0.03449 0.02554 = 0.01570 0.00254 0.01013 0.01809 O10 4 0.503725 0.207843 0.410028 11.00000 0.02145 0.01401 = 0.01705 0.00808 0.00307 0.00600 AFIX 3 H10O 2 0.441295 0.163633 0.351108 11.00000 -1.20000 AFIX 0 N1 3 0.929446 -0.067023 0.788895 11.00000 0.01846 0.01485 = 0.01646 0.00938 0.00913 0.00615 N2 3 0.707533 0.058921 0.599307 11.00000 0.01829 0.01448 = 0.01304 0.00705 0.00989 0.00781 C1 1 0.760766 -0.102599 0.830686 11.00000 0.01766 0.01492 = 0.01336 0.00398 0.00671 0.00150 C2 1 0.896410 -0.103680 0.851736 11.00000 0.01901 0.01017 = 0.01276 0.00384 0.00750 0.00253 C3 1 0.979899 -0.136500 0.928237 11.00000 0.02475 0.01227 = 0.01189 0.00536 0.00946 0.00613 AFIX 43 H3 2 0.954617 -0.163303 0.971673 11.00000 -1.20000 AFIX 0 C4 1 1.103502 -0.128862 0.939568 11.00000 0.02436 0.01914 = 0.01136 0.00508 0.00796 0.01188 C5 1 1.136565 -0.090070 0.872872 11.00000 0.01766 0.01848 = 0.01592 0.00447 0.00841 0.00806 AFIX 43 H5 2 1.219518 -0.084497 0.879029 11.00000 -1.20000 AFIX 0 C6 1 1.046729 -0.060349 0.798592 11.00000 0.02156 0.01268 = 0.01827 0.00588 0.01271 0.00626 C7 1 1.066416 -0.016658 0.720585 11.00000 0.02976 0.01770 = 0.03023 0.01452 0.02104 0.01206 C8 1 0.662315 -0.110138 0.446001 11.00000 0.02301 0.01538 = 0.01868 0.00887 0.01453 0.00776 C9 1 0.642870 0.003007 0.485828 11.00000 0.01708 0.01371 = 0.01431 0.00667 0.01090 0.00524 C10 1 0.571789 0.049022 0.417358 11.00000 0.01575 0.01340 = 0.01318 0.00543 0.00781 0.00292 AFIX 43 H10 2 0.524984 0.008488 0.337109 11.00000 -1.20000 AFIX 0 C11 1 0.570393 0.157097 0.469216 11.00000 0.01414 0.01341 = 0.01632 0.00920 0.00768 0.00372 C12 1 0.642793 0.215016 0.587452 11.00000 0.01522 0.01253 = 0.01623 0.00609 0.00894 0.00434 AFIX 43 H12 2 0.646346 0.289000 0.624138 11.00000 -1.20000 AFIX 0 C13 1 0.708471 0.162015 0.648895 11.00000 0.01530 0.01310 = 0.01392 0.00504 0.00981 0.00507 C14 1 0.784856 0.211476 0.777422 11.00000 0.01855 0.02387 = 0.01300 0.00737 0.00891 0.00943 N3 3 0.650117 0.636503 0.206133 11.00000 0.02264 0.01594 = 0.01591 0.00291 0.01015 0.00809 AFIX 3 H3N 2 0.645797 0.701393 0.252293 11.00000 -1.20000 AFIX 0 N4 3 0.659879 0.346719 -0.018496 11.00000 0.03518 0.02619 = 0.02122 0.00218 0.01258 0.01663 AFIX 3 H4A 2 0.605530 0.288589 -0.039396 11.00000 -1.20000 H4B 2 0.702538 0.336329 -0.058976 11.00000 -1.20000 AFIX 0 C15 1 0.575077 0.545834 0.184259 11.00000 0.02398 0.01621 = 0.01296 0.00538 0.00613 0.00863 C16 1 0.493142 0.554242 0.235760 11.00000 0.03262 0.01778 = 0.01996 0.00498 0.01482 0.00785 AFIX 43 H16 2 0.491250 0.622378 0.285405 11.00000 -1.20000 AFIX 0 C17 1 0.416285 0.463891 0.214007 11.00000 0.03654 0.02635 = 0.02388 0.00934 0.01703 0.00646 AFIX 43 H17 2 0.360225 0.469833 0.247904 11.00000 -1.20000 AFIX 0 C18 1 0.419423 0.362218 0.141915 11.00000 0.04268 0.01924 = 0.02557 0.00822 0.01330 0.00254 AFIX 43 H18 2 0.366703 0.300040 0.128566 11.00000 -1.20000 AFIX 0 C19 1 0.497984 0.352843 0.091234 11.00000 0.03690 0.01665 = 0.01986 0.00378 0.00826 0.00874 AFIX 43 H19 2 0.499576 0.283925 0.042887 11.00000 -1.20000 AFIX 0 C20 1 0.577377 0.444598 0.109711 11.00000 0.02529 0.01794 = 0.01396 0.00347 0.00576 0.01044 C21 1 0.658235 0.439148 0.054635 11.00000 0.02465 0.02299 = 0.01295 0.00393 0.00420 0.01418 C22 1 0.736464 0.536946 0.080674 11.00000 0.02030 0.02485 = 0.01464 0.00426 0.00674 0.01168 C23 1 0.820786 0.540020 0.032800 11.00000 0.02298 0.03824 = 0.01693 0.00354 0.00934 0.01473 AFIX 43 H23 2 0.826897 0.475257 -0.019026 11.00000 -1.20000 AFIX 0 C24 1 0.893217 0.634334 0.059894 11.00000 0.02080 0.04824 = 0.02273 0.00668 0.01300 0.01012 AFIX 43 H24 2 0.949882 0.634740 0.027503 11.00000 -1.20000 AFIX 0 C25 1 0.884696 0.731425 0.135713 11.00000 0.02085 0.03620 = 0.02274 0.00533 0.00987 0.00264 AFIX 43 H25 2 0.935017 0.796881 0.153380 11.00000 -1.20000 AFIX 0 C26 1 0.804393 0.732213 0.184194 11.00000 0.02178 0.02639 = 0.01951 0.00368 0.00981 0.00640 AFIX 43 H26 2 0.799311 0.797881 0.235482 11.00000 -1.20000 AFIX 0 C27 1 0.729417 0.635032 0.157504 11.00000 0.01742 0.02422 = 0.01310 0.00445 0.00652 0.00954 N5 3 0.814322 0.411467 0.360412 11.00000 0.02399 0.01536 = 0.02191 0.00527 0.01080 0.00643 AFIX 3 H5N 2 0.789432 0.340227 0.338422 11.00000 -1.20000 AFIX 0 N6 3 0.900467 0.739041 0.476971 11.00000 0.02463 0.01760 = 0.02659 0.01113 0.01693 0.00972 AFIX 3 H6A 2 0.845437 0.771481 0.495821 11.00000 -1.20000 H6B 2 0.959447 0.778751 0.475541 11.00000 -1.20000 AFIX 0 C28 1 0.767640 0.471736 0.431244 11.00000 0.01852 0.01835 = 0.01658 0.00772 0.00638 0.00718 C29 1 0.688573 0.420124 0.459446 11.00000 0.02338 0.01475 = 0.02341 0.00865 0.00850 0.00620 AFIX 43 H29 2 0.666846 0.344304 0.428140 11.00000 -1.20000 AFIX 0 C30 1 0.643503 0.480045 0.532131 11.00000 0.02458 0.02267 = 0.02662 0.01496 0.01280 0.00800 AFIX 43 H30 2 0.590711 0.445371 0.551661 11.00000 -1.20000 AFIX 0 C31 1 0.674096 0.592644 0.578691 11.00000 0.02878 0.02122 = 0.02731 0.01283 0.01827 0.01288 AFIX 43 H31 2 0.642666 0.633240 0.629779 11.00000 -1.20000 AFIX 0 C32 1 0.748770 0.643249 0.550398 11.00000 0.02660 0.01595 = 0.02318 0.00963 0.01404 0.00970 AFIX 43 H32 2 0.768308 0.719105 0.581532 11.00000 -1.20000 AFIX 0 C33 1 0.797747 0.584231 0.475091 11.00000 0.01911 0.01779 = 0.01835 0.00906 0.00811 0.00820 C34 1 0.877843 0.634699 0.444271 11.00000 0.01825 0.01933 = 0.01402 0.00848 0.00629 0.00873 C35 1 0.931662 0.567700 0.375236 11.00000 0.01712 0.02182 = 0.01438 0.00743 0.00609 0.00938 C36 1 1.016062 0.609761 0.344167 11.00000 0.01882 0.02210 = 0.01932 0.00704 0.00758 0.00779 AFIX 43 H36 2 1.042565 0.684976 0.372550 11.00000 -1.20000 AFIX 0 C37 1 1.059887 0.542927 0.273495 11.00000 0.02167 0.03073 = 0.02281 0.00796 0.01203 0.00872 AFIX 43 H37 2 1.116090 0.571855 0.252845 11.00000 -1.20000 AFIX 0 C38 1 1.021352 0.431423 0.231691 11.00000 0.02832 0.03046 = 0.02355 0.00347 0.01557 0.01316 AFIX 43 H38 2 1.051504 0.385507 0.182401 11.00000 -1.20000 AFIX 0 C39 1 0.941561 0.388480 0.260859 11.00000 0.03039 0.02051 = 0.02411 0.00237 0.01293 0.00851 AFIX 43 H39 2 0.916925 0.313093 0.232501 11.00000 -1.20000 AFIX 0 C40 1 0.895424 0.455925 0.333218 11.00000 0.01850 0.02105 = 0.01598 0.00544 0.00717 0.00852 O11 4 0.925095 0.122094 0.530111 11.00000 0.04144 0.02977 = 0.03605 0.02463 0.02788 0.01722 AFIX 3 H11A 2 0.889855 0.076494 0.461171 11.00000 -1.20000 H11B 2 0.946295 0.089084 0.571691 11.00000 -1.20000 AFIX 0 O12 4 0.490777 0.047897 0.105541 11.00000 0.03281 0.02673 = 0.03719 0.01112 0.02079 0.00605 AFIX 3 H12A 2 0.430870 0.077137 0.108021 11.00000 -1.20000 H12B 2 0.475917 -0.010497 0.108716 11.00000 -1.20000 AFIX 0 O13 4 0.717358 0.193498 0.285934 11.00000 0.02803 0.01768 = 0.03522 0.00688 0.01729 0.00810 AFIX 3 H13A 2 0.680918 0.180208 0.215244 11.00000 -1.20000 H13B 2 0.756658 0.145137 0.290654 11.00000 -1.20000 AFIX 0 PART 1 O14 4 0.496763 0.846455 0.134662 21.00000 0.03173 0.01955 = 0.01842 0.00601 0.00542 0.00300 AFIX 3 H14A 2 0.550042 0.857055 0.200432 21.00000 -1.20000 H14B 2 0.502012 0.904865 0.129402 21.00000 -1.20000 AFIX 0 PART 2 O14A 4 0.557517 0.876298 0.151375 -21.00000 0.03173 0.01955 = 0.01842 0.00601 0.00542 0.00300 AFIX 3 H14C 2 0.557887 0.861589 0.204305 -21.00000 -1.20000 H14D 2 0.630487 0.910679 0.174415 -21.00000 -1.20000 PART 0 HKLF 4 REM JTM362_0m in P-1 REM R1 = 0.0416 for 7550 Fo > 4sig(Fo) and 0.0487 for all 8752 data REM 554 parameters refined using 0 restraints END WGHT 0.0481 1.2510 REM Highest difference peak 0.636, deepest hole -0.754, 1-sigma level 0.071 Q1 1 0.6763 0.8919 0.0771 11.00000 0.05 0.64 Q2 1 0.6376 0.1562 0.2352 11.00000 0.05 0.61 Q3 1 0.8745 -0.0300 0.6816 11.00000 0.05 0.59 Q4 1 0.7853 0.0018 0.6266 11.00000 0.05 0.58 Q5 1 0.7549 0.0160 0.7123 11.00000 0.05 0.58 ; _database_code_depnum_ccdc_archive 'CCDC 940542' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Co N2 O10, 2(C13 H11 N2), 3(H2 O)' _chemical_formula_sum 'C40 H34 Co N6 O13' _chemical_formula_weight 865.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.574(3) _cell_length_b 23.672(6) _cell_length_c 14.903(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.379(3) _cell_angle_gamma 90.00 _cell_volume 3613.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9891 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.34 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7873 _exptl_absorpt_correction_T_max 0.9781 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63175 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.41 _reflns_number_total 9000 _reflns_number_gt 7263 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2008)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2008)' _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. H-atoms attached to carbon were placed in calculated positions (C---H = 0.95 \%A) while those attached to nitrogen and oxygen were placed in locations derived from a difference map and their coordinates adjusted to give N---H and O---H distances of 0.91 and 0.84 \%A, respectively. All were included as riding contributions with isotropic displacement parameters 1.2 times those of the attached atoms. ; _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^)+(0.0406P)^2^+2.1516P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9000 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _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 0.67498(2) 0.499817(9) 0.766908(14) 0.01054(6) Uani 1 1 d . . . O1 O 0.77630(11) 0.44909(5) 0.68648(8) 0.0140(2) Uani 1 1 d . . . O2 O 0.53357(11) 0.56743(5) 0.77991(8) 0.0138(2) Uani 1 1 d . . . O3 O 0.81351(11) 0.44045(5) 0.54514(8) 0.0170(2) Uani 1 1 d . . . O4 O 0.37920(11) 0.61953(5) 0.68559(8) 0.0152(2) Uani 1 1 d . . . O5 O 0.53791(11) 0.61681(5) 0.39054(8) 0.0152(2) Uani 1 1 d . . . H5O H 0.5362 0.5984 0.3420 0.018 Uiso 1 1 d R . . O6 O 0.85381(11) 0.53826(5) 0.84214(8) 0.0144(2) Uani 1 1 d . . . O7 O 0.51647(11) 0.44108(5) 0.75733(8) 0.0143(2) Uani 1 1 d . . . O8 O 0.95226(11) 0.56795(5) 0.98576(8) 0.0150(2) Uani 1 1 d . . . O9 O 0.39229(11) 0.40276(5) 0.84327(8) 0.0184(3) Uani 1 1 d . . . O10 O 0.68072(11) 0.45769(5) 1.16999(8) 0.0178(3) Uani 1 1 d . . . H10O H 0.6092 0.4447 1.1758 0.021 Uiso 1 1 d R . . N1 N 0.62746(12) 0.53547(5) 0.64037(9) 0.0105(3) Uani 1 1 d . . . N2 N 0.68728(12) 0.47757(5) 0.89925(9) 0.0105(3) Uani 1 1 d . . . C1 C 0.76467(15) 0.46443(7) 0.60306(11) 0.0121(3) Uani 1 1 d . . . C2 C 0.67949(14) 0.51618(7) 0.57295(11) 0.0112(3) Uani 1 1 d . . . C3 C 0.65183(15) 0.54090(7) 0.48603(11) 0.0120(3) Uani 1 1 d . . . H3 H 0.6887 0.5265 0.4387 0.014 Uiso 1 1 calc R . . C4 C 0.56784(15) 0.58777(6) 0.46967(10) 0.0114(3) Uani 1 1 d . . . C5 C 0.50983(14) 0.60568(6) 0.53950(11) 0.0117(3) Uani 1 1 d . . . H5 H 0.4492 0.6360 0.5291 0.014 Uiso 1 1 calc R . . C6 C 0.54256(14) 0.57829(6) 0.62356(11) 0.0104(3) Uani 1 1 d . . . C7 C 0.47926(14) 0.59044(6) 0.70201(11) 0.0110(3) Uani 1 1 d . . . C8 C 0.87224(14) 0.53840(6) 0.93018(11) 0.0119(3) Uani 1 1 d . . . C9 C 0.78012(14) 0.50085(6) 0.96699(11) 0.0110(3) Uani 1 1 d . . . C10 C 0.78156(15) 0.49373(6) 1.05900(11) 0.0122(3) Uani 1 1 d . . . H10 H 0.8496 0.5094 1.1065 0.015 Uiso 1 1 calc R . . C11 C 0.68017(15) 0.46280(7) 1.08087(11) 0.0127(3) Uani 1 1 d . . . C12 C 0.58179(15) 0.43987(6) 1.00904(11) 0.0120(3) Uani 1 1 d . . . H12 H 0.5114 0.4192 1.0220 0.014 Uiso 1 1 calc R . . C13 C 0.59008(14) 0.44822(6) 0.91944(11) 0.0111(3) Uani 1 1 d . . . C14 C 0.48929(15) 0.42836(7) 0.83382(11) 0.0124(3) Uani 1 1 d . . . N3 N -0.00585(13) 0.79803(6) 0.19148(9) 0.0133(3) Uani 1 1 d . . . H3N H -0.0197 0.8358 0.1948 0.016 Uiso 1 1 d R . . N4 N 0.03705(14) 0.62466(6) 0.19260(11) 0.0211(3) Uani 1 1 d . . . H4A H -0.0247 0.6029 0.1547 0.025 Uiso 1 1 d R . . H4B H 0.1080 0.6073 0.2295 0.025 Uiso 1 1 d R . . C15 C 0.10763(15) 0.77484(7) 0.24113(11) 0.0125(3) Uani 1 1 d . . . C16 C 0.20778(16) 0.81088(7) 0.29005(11) 0.0153(3) Uani 1 1 d . . . H16 H 0.1947 0.8506 0.2892 0.018 Uiso 1 1 calc R . . C17 C 0.32346(16) 0.78823(7) 0.33851(11) 0.0173(3) Uani 1 1 d . . . H17 H 0.3910 0.8125 0.3711 0.021 Uiso 1 1 calc R . . C18 C 0.34391(16) 0.72935(7) 0.34084(11) 0.0170(3) Uani 1 1 d . . . H18 H 0.4249 0.7143 0.3748 0.020 Uiso 1 1 calc R . . C19 C 0.24767(15) 0.69386(7) 0.29448(11) 0.0151(3) Uani 1 1 d . . . H19 H 0.2623 0.6542 0.2966 0.018 Uiso 1 1 calc R . . C20 C 0.12617(15) 0.71562(7) 0.24319(11) 0.0125(3) Uani 1 1 d . . . C21 C 0.02330(15) 0.68018(7) 0.19198(11) 0.0130(3) Uani 1 1 d . . . C22 C -0.09485(15) 0.70651(7) 0.13924(11) 0.0124(3) Uani 1 1 d . . . C23 C -0.20326(16) 0.67546(7) 0.08854(11) 0.0159(3) Uani 1 1 d . . . H23 H -0.1989 0.6354 0.0872 0.019 Uiso 1 1 calc R . . C24 C -0.31471(16) 0.70234(8) 0.04123(12) 0.0180(3) Uani 1 1 d . . . H24 H -0.3872 0.6809 0.0080 0.022 Uiso 1 1 calc R . . C25 C -0.32201(16) 0.76154(8) 0.04177(12) 0.0192(4) Uani 1 1 d . . . H25 H -0.3990 0.7798 0.0077 0.023 Uiso 1 1 calc R . . C26 C -0.22012(15) 0.79324(7) 0.09058(12) 0.0162(3) Uani 1 1 d . . . H26 H -0.2263 0.8333 0.0907 0.019 Uiso 1 1 calc R . . C27 C -0.10548(15) 0.76614(7) 0.14086(11) 0.0128(3) Uani 1 1 d . . . N5 N 0.98118(12) 0.82027(6) 0.42914(9) 0.0124(3) Uani 1 1 d . . . H5N H 0.9798 0.8584 0.4368 0.015 Uiso 1 1 d R . . N6 N 1.00067(13) 0.64632(6) 0.41400(10) 0.0151(3) Uani 1 1 d . . . H6A H 1.0766 0.6279 0.4393 0.018 Uiso 1 1 d R . . H6B H 0.9335 0.6268 0.3769 0.018 Uiso 1 1 d R . . C28 C 1.09076(15) 0.79338(7) 0.47862(11) 0.0119(3) Uani 1 1 d . . . C29 C 1.19584(15) 0.82620(7) 0.52931(11) 0.0141(3) Uani 1 1 d . . . H29 H 1.1904 0.8663 0.5279 0.017 Uiso 1 1 calc R . . C30 C 1.30585(16) 0.79998(7) 0.58061(11) 0.0155(3) Uani 1 1 d . . . H30 H 1.3771 0.8221 0.6140 0.019 Uiso 1 1 calc R . . C31 C 1.31422(16) 0.74058(7) 0.58429(11) 0.0152(3) Uani 1 1 d . . . H31 H 1.3896 0.7228 0.6217 0.018 Uiso 1 1 calc R . . C32 C 1.21363(15) 0.70839(7) 0.53390(11) 0.0136(3) Uani 1 1 d . . . H32 H 1.2205 0.6684 0.5363 0.016 Uiso 1 1 calc R . . C33 C 1.09976(14) 0.73381(6) 0.47845(11) 0.0114(3) Uani 1 1 d . . . C34 C 0.99294(14) 0.70160(7) 0.42250(11) 0.0115(3) Uani 1 1 d . . . C35 C 0.87664(14) 0.73174(7) 0.37559(11) 0.0114(3) Uani 1 1 d . . . C36 C 0.76366(15) 0.70330(7) 0.32490(11) 0.0150(3) Uani 1 1 d . . . H36 H 0.7639 0.6633 0.3208 0.018 Uiso 1 1 calc R . . C37 C 0.65415(15) 0.73276(7) 0.28176(12) 0.0163(3) Uani 1 1 d . . . H37 H 0.5788 0.7132 0.2481 0.020 Uiso 1 1 calc R . . C38 C 0.65346(16) 0.79214(7) 0.28739(12) 0.0168(3) Uani 1 1 d . . . H38 H 0.5769 0.8123 0.2576 0.020 Uiso 1 1 calc R . . C39 C 0.76099(15) 0.82126(7) 0.33491(11) 0.0148(3) Uani 1 1 d . . . H39 H 0.7595 0.8614 0.3374 0.018 Uiso 1 1 calc R . . C40 C 0.87431(15) 0.79131(7) 0.38027(11) 0.0119(3) Uani 1 1 d . . . O11 O 0.05083(12) 0.41229(5) 0.30058(9) 0.0212(3) Uani 1 1 d . . . H11A H 0.0704 0.4310 0.2581 0.025 Uiso 1 1 d R . . H11B H -0.0008 0.4329 0.3205 0.025 Uiso 1 1 d R . . O12 O 0.84498(11) 0.45548(5) 0.36743(8) 0.0193(3) Uani 1 1 d . . . H12A H 0.8384 0.4526 0.4223 0.023 Uiso 1 1 d R . . H12B H 0.7865 0.4352 0.3342 0.023 Uiso 1 1 d R . . O13 O 0.16509(12) 0.43291(5) 0.70818(9) 0.0255(3) Uani 1 1 d . . . H13A H 0.2360 0.4301 0.7486 0.031 Uiso 1 1 d R . . H13B H 0.1669 0.4674 0.6955 0.031 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 Co1 0.01195(11) 0.01144(11) 0.00822(11) 0.00183(8) 0.00252(7) 0.00047(7) O1 0.0172(5) 0.0133(5) 0.0120(6) 0.0037(4) 0.0045(4) 0.0041(4) O2 0.0163(5) 0.0145(6) 0.0113(5) 0.0019(4) 0.0049(4) 0.0019(4) O3 0.0199(6) 0.0175(6) 0.0150(6) 0.0018(5) 0.0068(5) 0.0076(5) O4 0.0164(5) 0.0142(6) 0.0167(6) 0.0015(5) 0.0072(4) 0.0047(4) O5 0.0234(6) 0.0134(6) 0.0082(5) 0.0013(4) 0.0029(4) 0.0036(4) O6 0.0143(5) 0.0169(6) 0.0126(6) 0.0030(4) 0.0043(4) -0.0019(4) O7 0.0172(6) 0.0160(6) 0.0092(5) -0.0004(4) 0.0020(4) -0.0031(4) O8 0.0136(5) 0.0129(5) 0.0170(6) 0.0000(5) 0.0010(4) -0.0032(4) O9 0.0160(6) 0.0219(6) 0.0156(6) 0.0030(5) 0.0008(4) -0.0076(5) O10 0.0185(6) 0.0270(7) 0.0085(6) 0.0010(5) 0.0043(4) -0.0063(5) N1 0.0112(6) 0.0097(6) 0.0105(6) -0.0002(5) 0.0024(5) 0.0001(5) N2 0.0102(6) 0.0106(6) 0.0103(6) 0.0013(5) 0.0020(5) -0.0001(5) C1 0.0117(7) 0.0113(7) 0.0129(8) 0.0002(6) 0.0025(6) -0.0006(5) C2 0.0096(7) 0.0111(7) 0.0125(7) 0.0002(6) 0.0021(5) -0.0001(5) C3 0.0132(7) 0.0131(7) 0.0103(7) -0.0012(6) 0.0041(6) 0.0004(6) C4 0.0141(7) 0.0109(7) 0.0083(7) -0.0005(6) 0.0008(5) -0.0015(5) C5 0.0117(7) 0.0094(7) 0.0132(8) 0.0003(6) 0.0015(5) 0.0008(5) C6 0.0101(7) 0.0104(7) 0.0106(7) -0.0007(6) 0.0026(5) -0.0012(5) C7 0.0125(7) 0.0086(7) 0.0122(7) -0.0010(6) 0.0039(6) -0.0023(5) C8 0.0106(7) 0.0099(7) 0.0151(8) 0.0024(6) 0.0027(6) 0.0018(5) C9 0.0105(7) 0.0090(7) 0.0135(7) 0.0010(6) 0.0026(5) 0.0003(5) C10 0.0122(7) 0.0119(7) 0.0112(7) -0.0004(6) 0.0006(5) -0.0006(5) C11 0.0149(7) 0.0123(7) 0.0110(7) 0.0013(6) 0.0033(6) 0.0022(6) C12 0.0135(7) 0.0112(7) 0.0122(8) 0.0022(6) 0.0047(6) 0.0003(5) C13 0.0113(7) 0.0083(7) 0.0133(8) 0.0008(6) 0.0025(6) 0.0012(5) C14 0.0129(7) 0.0116(7) 0.0120(8) 0.0002(6) 0.0014(6) 0.0011(6) N3 0.0140(6) 0.0104(6) 0.0155(7) 0.0000(5) 0.0036(5) 0.0005(5) N4 0.0175(7) 0.0120(7) 0.0295(8) 0.0023(6) -0.0025(6) -0.0004(5) C15 0.0134(7) 0.0157(8) 0.0094(7) 0.0008(6) 0.0046(6) 0.0007(6) C16 0.0181(8) 0.0147(8) 0.0142(8) -0.0010(6) 0.0058(6) -0.0032(6) C17 0.0165(8) 0.0222(9) 0.0128(8) -0.0017(7) 0.0029(6) -0.0052(6) C18 0.0139(7) 0.0239(9) 0.0123(8) 0.0022(7) 0.0014(6) 0.0008(6) C19 0.0153(7) 0.0161(8) 0.0140(8) 0.0031(6) 0.0035(6) 0.0019(6) C20 0.0133(7) 0.0143(8) 0.0107(7) 0.0008(6) 0.0044(6) 0.0000(6) C21 0.0142(7) 0.0134(8) 0.0116(7) 0.0020(6) 0.0037(6) -0.0011(6) C22 0.0131(7) 0.0122(7) 0.0122(7) 0.0014(6) 0.0035(6) 0.0003(6) C23 0.0168(8) 0.0159(8) 0.0151(8) -0.0006(6) 0.0039(6) -0.0017(6) C24 0.0137(7) 0.0241(9) 0.0150(8) -0.0021(7) 0.0013(6) -0.0031(6) C25 0.0143(8) 0.0256(9) 0.0163(8) 0.0017(7) 0.0011(6) 0.0044(6) C26 0.0160(8) 0.0159(8) 0.0165(8) 0.0023(6) 0.0035(6) 0.0038(6) C27 0.0133(7) 0.0150(8) 0.0107(7) 0.0008(6) 0.0039(6) 0.0000(6) N5 0.0131(6) 0.0081(6) 0.0151(7) 0.0005(5) 0.0019(5) 0.0006(5) N6 0.0126(6) 0.0106(6) 0.0196(7) 0.0004(5) -0.0004(5) 0.0010(5) C28 0.0127(7) 0.0137(8) 0.0100(7) 0.0017(6) 0.0041(6) 0.0018(6) C29 0.0166(8) 0.0116(7) 0.0142(8) -0.0001(6) 0.0042(6) -0.0010(6) C30 0.0155(7) 0.0173(8) 0.0129(8) -0.0009(6) 0.0018(6) -0.0025(6) C31 0.0141(7) 0.0171(8) 0.0133(8) 0.0007(6) 0.0014(6) 0.0023(6) C32 0.0148(7) 0.0125(7) 0.0137(8) 0.0007(6) 0.0040(6) 0.0016(6) C33 0.0117(7) 0.0108(7) 0.0124(7) -0.0002(6) 0.0041(6) 0.0003(5) C34 0.0115(7) 0.0120(7) 0.0110(7) 0.0013(6) 0.0031(6) 0.0005(5) C35 0.0119(7) 0.0116(7) 0.0112(7) 0.0006(6) 0.0037(5) 0.0006(5) C36 0.0151(7) 0.0117(7) 0.0176(8) -0.0007(6) 0.0032(6) 0.0000(6) C37 0.0131(7) 0.0165(8) 0.0178(8) -0.0004(6) 0.0009(6) -0.0014(6) C38 0.0146(7) 0.0170(8) 0.0170(8) 0.0024(6) 0.0005(6) 0.0045(6) C39 0.0164(8) 0.0117(7) 0.0158(8) 0.0009(6) 0.0032(6) 0.0035(6) C40 0.0125(7) 0.0124(7) 0.0113(7) 0.0004(6) 0.0039(6) 0.0010(6) O11 0.0259(6) 0.0152(6) 0.0272(7) 0.0045(5) 0.0153(5) 0.0013(5) O12 0.0194(6) 0.0243(7) 0.0142(6) -0.0015(5) 0.0043(5) -0.0015(5) O13 0.0207(6) 0.0160(6) 0.0322(8) -0.0010(5) -0.0076(5) -0.0026(5) _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 N1 2.0125(14) . ? Co1 N2 2.0141(14) . ? Co1 O6 2.1467(12) . ? Co1 O7 2.1552(12) . ? Co1 O1 2.1597(12) . ? Co1 O2 2.2315(12) . ? O1 C1 1.271(2) . ? O2 C7 1.2819(19) . ? O3 C1 1.2471(19) . ? O4 C7 1.2350(19) . ? O5 C4 1.3334(19) . ? O5 H5O 0.8400 . ? O6 C8 1.278(2) . ? O7 C14 1.279(2) . ? O8 C8 1.2422(19) . ? O9 C14 1.2292(19) . ? O10 C11 1.332(2) . ? O10 H10O 0.8401 . ? N1 C6 1.3359(19) . ? N1 C2 1.340(2) . ? N2 C13 1.335(2) . ? N2 C9 1.340(2) . ? C1 C2 1.521(2) . ? C2 C3 1.385(2) . ? C3 C4 1.404(2) . ? C3 H3 0.9500 . ? C4 C5 1.399(2) . ? C5 C6 1.376(2) . ? C5 H5 0.9500 . ? C6 C7 1.512(2) . ? C8 C9 1.518(2) . ? C9 C10 1.378(2) . ? C10 C11 1.402(2) . ? C10 H10 0.9500 . ? C11 C12 1.403(2) . ? C12 C13 1.374(2) . ? C12 H12 0.9500 . ? C13 C14 1.520(2) . ? N3 C15 1.359(2) . ? N3 C27 1.362(2) . ? N3 H3N 0.9100 . ? N4 C21 1.322(2) . ? N4 H4A 0.9099 . ? N4 H4B 0.9100 . ? C15 C16 1.413(2) . ? C15 C20 1.415(2) . ? C16 C17 1.366(2) . ? C16 H16 0.9500 . ? C17 C18 1.409(2) . ? C17 H17 0.9500 . ? C18 C19 1.367(2) . ? C18 H18 0.9500 . ? C19 C20 1.419(2) . ? C19 H19 0.9500 . ? C20 C21 1.434(2) . ? C21 C22 1.442(2) . ? C22 C23 1.412(2) . ? C22 C27 1.417(2) . ? C23 C24 1.370(2) . ? C23 H23 0.9500 . ? C24 C25 1.404(3) . ? C24 H24 0.9500 . ? C25 C26 1.365(2) . ? C25 H25 0.9500 . ? C26 C27 1.411(2) . ? C26 H26 0.9500 . ? N5 C28 1.3665(19) . ? N5 C40 1.367(2) . ? N5 H5N 0.9100 . ? N6 C34 1.319(2) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C28 C29 1.411(2) . ? C28 C33 1.413(2) . ? C29 C30 1.372(2) . ? C29 H29 0.9500 . ? C30 C31 1.409(2) . ? C30 H30 0.9500 . ? C31 C32 1.371(2) . ? C31 H31 0.9500 . ? C32 C33 1.414(2) . ? C32 H32 0.9500 . ? C33 C34 1.444(2) . ? C34 C35 1.443(2) . ? C35 C40 1.412(2) . ? C35 C36 1.415(2) . ? C36 C37 1.368(2) . ? C36 H36 0.9500 . ? C37 C38 1.408(2) . ? C37 H37 0.9500 . ? C38 C39 1.367(2) . ? C38 H38 0.9500 . ? C39 C40 1.412(2) . ? C39 H39 0.9500 . ? O11 H11A 0.8400 . ? O11 H11B 0.8400 . ? O12 H12A 0.8399 . ? O12 H12B 0.8400 . ? O13 H13A 0.8399 . ? O13 H13B 0.8400 . ? 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 N1 Co1 N2 165.37(5) . . ? N1 Co1 O6 107.11(5) . . ? N2 Co1 O6 76.41(5) . . ? N1 Co1 O7 101.50(5) . . ? N2 Co1 O7 75.89(5) . . ? O6 Co1 O7 151.39(4) . . ? N1 Co1 O1 75.88(5) . . ? N2 Co1 O1 118.54(5) . . ? O6 Co1 O1 91.80(5) . . ? O7 Co1 O1 95.13(5) . . ? N1 Co1 O2 76.34(5) . . ? N2 Co1 O2 89.09(5) . . ? O6 Co1 O2 99.96(5) . . ? O7 Co1 O2 86.65(5) . . ? O1 Co1 O2 151.95(4) . . ? C1 O1 Co1 116.29(10) . . ? C7 O2 Co1 112.66(10) . . ? C4 O5 H5O 116.3 . . ? C8 O6 Co1 115.30(10) . . ? C14 O7 Co1 115.86(10) . . ? C11 O10 H10O 110.8 . . ? C6 N1 C2 120.00(13) . . ? C6 N1 Co1 119.59(10) . . ? C2 N1 Co1 120.41(10) . . ? C13 N2 C9 120.35(14) . . ? C13 N2 Co1 119.37(10) . . ? C9 N2 Co1 119.17(11) . . ? O3 C1 O1 126.21(14) . . ? O3 C1 C2 118.63(14) . . ? O1 C1 C2 115.15(13) . . ? N1 C2 C3 121.78(14) . . ? N1 C2 C1 112.13(13) . . ? C3 C2 C1 126.05(14) . . ? C2 C3 C4 118.29(14) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? O5 C4 C5 116.75(14) . . ? O5 C4 C3 124.19(14) . . ? C5 C4 C3 119.06(14) . . ? C6 C5 C4 118.48(14) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? N1 C6 C5 122.24(14) . . ? N1 C6 C7 113.91(13) . . ? C5 C6 C7 123.69(14) . . ? O4 C7 O2 125.83(14) . . ? O4 C7 C6 118.36(14) . . ? O2 C7 C6 115.77(13) . . ? O8 C8 O6 126.23(15) . . ? O8 C8 C9 118.73(14) . . ? O6 C8 C9 114.94(13) . . ? N2 C9 C10 121.64(14) . . ? N2 C9 C8 112.61(14) . . ? C10 C9 C8 125.57(14) . . ? C9 C10 C11 118.37(14) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? O10 C11 C10 117.70(14) . . ? O10 C11 C12 122.97(14) . . ? C10 C11 C12 119.31(15) . . ? C13 C12 C11 118.13(14) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N2 C13 C12 122.15(14) . . ? N2 C13 C14 112.98(14) . . ? C12 C13 C14 124.80(14) . . ? O9 C14 O7 126.65(15) . . ? O9 C14 C13 119.17(14) . . ? O7 C14 C13 114.17(14) . . ? C15 N3 C27 122.32(14) . . ? C15 N3 H3N 120.0 . . ? C27 N3 H3N 117.6 . . ? C21 N4 H4A 119.8 . . ? C21 N4 H4B 121.7 . . ? H4A N4 H4B 118.5 . . ? N3 C15 C16 118.95(15) . . ? N3 C15 C20 120.72(14) . . ? C16 C15 C20 120.33(14) . . ? C17 C16 C15 119.58(15) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.86(15) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 120.32(15) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.65(16) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 118.27(14) . . ? C15 C20 C21 119.04(14) . . ? C19 C20 C21 122.68(15) . . ? N4 C21 C20 120.68(14) . . ? N4 C21 C22 120.82(14) . . ? C20 C21 C22 118.50(14) . . ? C23 C22 C27 118.05(14) . . ? C23 C22 C21 123.02(15) . . ? C27 C22 C21 118.88(14) . . ? C24 C23 C22 120.90(16) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.14(15) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.96(16) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 119.57(16) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N3 C27 C26 119.12(15) . . ? N3 C27 C22 120.54(14) . . ? C26 C27 C22 120.34(15) . . ? C28 N5 C40 122.14(14) . . ? C28 N5 H5N 115.6 . . ? C40 N5 H5N 121.8 . . ? C34 N6 H6A 120.4 . . ? C34 N6 H6B 120.2 . . ? H6A N6 H6B 119.0 . . ? N5 C28 C29 118.80(14) . . ? N5 C28 C33 120.81(14) . . ? C29 C28 C33 120.39(14) . . ? C30 C29 C28 119.69(15) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.63(15) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 120.05(15) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 121.03(15) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C28 C33 C32 118.13(14) . . ? C28 C33 C34 118.99(14) . . ? C32 C33 C34 122.88(14) . . ? N6 C34 C35 120.63(14) . . ? N6 C34 C33 121.41(14) . . ? C35 C34 C33 117.97(14) . . ? C40 C35 C36 118.58(14) . . ? C40 C35 C34 119.53(14) . . ? C36 C35 C34 121.89(14) . . ? C37 C36 C35 120.82(15) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 119.81(15) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 121.21(15) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 119.50(15) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? N5 C40 C39 119.63(14) . . ? N5 C40 C35 120.31(14) . . ? C39 C40 C35 120.06(14) . . ? H11A O11 H11B 105.2 . . ? H12A O12 H12B 107.6 . . ? H13A O13 H13B 100.0 . . ? 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 O5 H5O O7 0.84 1.72 2.5366(17) 163 3_666 O10 H10O O2 0.84 1.81 2.6241(17) 161 3_667 N3 H3N O11 0.91 1.84 2.7537(19) 179 2 N4 H4B O1 0.91 2.02 2.9024(18) 162 3_666 N5 H5N O8 0.91 1.94 2.8172(18) 161 4_575 N6 H6A O3 0.91 1.97 2.8030(18) 151 3_766 N6 H6B O13 0.91 2.01 2.8844(19) 161 3_666 O11 H11A O6 0.84 2.00 2.8242(17) 167 3_666 O11 H11B O12 0.84 2.00 2.8024(18) 160 1_455 O12 H12A O3 0.84 1.94 2.7728(18) 175 . O12 H12B O4 0.84 2.14 2.9098(17) 152 3_666 O13 H13A O9 0.84 2.00 2.8165(18) 166 . O13 H13B O12 0.84 2.04 2.8638(19) 166 3_666 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.448 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.067 _iucr_refine_instructions_details ; TITL JTM364_0m in P2(1)/c CELL 0.71073 10.5745 23.6722 14.9026 90.000 104.379 90.000 ZERR 4.00 0.0026 0.0060 0.0038 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Co UNIT 160 136 24 52 4 L.S. 6 ACTA BOND $H FMAP 2 PLAN 5 EQIV $1 -x+1, -y+1, -z+1 EQIV $2 -x+1, -y+1, -z+2 EQIV $3 -x, y+0.5, -z+0.5 EQIV $4 x, -y+1.5, z-0.5 EQIV $5 -x+2, -y+1, -z+1 EQIV $6 x-1, y, z HTAB O5 O7_$1 HTAB O10 O2_$2 HTAB N3 O11_$3 HTAB N4 O1_$1 HTAB N5 O8_$4 HTAB N6 O3_$5 HTAB N6 O13_$1 HTAB O11 O6_$1 HTAB O11 O12_$6 HTAB O12 O3 HTAB O12 O4_$1 HTAB O13 O9 HTAB O13 O12_$1 MPLA Co1 O1 O2 N1 C1 C2 C6 C7 MPLA Co1 O6 O7 N2 C8 C9 C13 C14 MPLA N3 C15 > C27 MPLA N5 C28 > C40 SIZE 0.04 0.14 0.28 TEMP -173 WGHT 0.040600 2.151600 FVAR 0.05864 CO1 5 0.674982 0.499817 0.766908 11.00000 0.01195 0.01144 = 0.00822 0.00183 0.00252 0.00047 O1 4 0.776302 0.449090 0.686485 11.00000 0.01717 0.01329 = 0.01195 0.00365 0.00448 0.00411 O2 4 0.533570 0.567432 0.779912 11.00000 0.01628 0.01450 = 0.01129 0.00186 0.00488 0.00192 O3 4 0.813514 0.440455 0.545140 11.00000 0.01986 0.01752 = 0.01497 0.00177 0.00682 0.00756 O4 4 0.379196 0.619531 0.685594 11.00000 0.01636 0.01417 = 0.01667 0.00152 0.00721 0.00469 O5 4 0.537911 0.616806 0.390538 11.00000 0.02344 0.01339 = 0.00817 0.00127 0.00294 0.00359 AFIX 3 H5O 2 0.536181 0.598406 0.342048 11.00000 -1.20000 AFIX 0 O6 4 0.853814 0.538262 0.842143 11.00000 0.01430 0.01694 = 0.01260 0.00301 0.00434 -0.00188 O7 4 0.516471 0.441076 0.757328 11.00000 0.01718 0.01598 = 0.00916 -0.00042 0.00202 -0.00311 O8 4 0.952255 0.567945 0.985758 11.00000 0.01358 0.01286 = 0.01703 0.00001 0.00096 -0.00324 O9 4 0.392294 0.402757 0.843274 11.00000 0.01604 0.02188 = 0.01558 0.00297 0.00081 -0.00757 O10 4 0.680717 0.457685 1.169993 11.00000 0.01850 0.02702 = 0.00851 0.00098 0.00434 -0.00634 AFIX 3 H10O 2 0.609217 0.444735 1.175815 11.00000 -1.20000 AFIX 0 N1 3 0.627464 0.535474 0.640370 11.00000 0.01122 0.00975 = 0.01049 -0.00016 0.00241 0.00014 N2 3 0.687281 0.477573 0.899248 11.00000 0.01022 0.01064 = 0.01033 0.00131 0.00198 -0.00008 C1 1 0.764670 0.464427 0.603060 11.00000 0.01169 0.01128 = 0.01293 0.00020 0.00254 -0.00060 C2 1 0.679494 0.516178 0.572952 11.00000 0.00961 0.01107 = 0.01249 0.00019 0.00214 -0.00011 C3 1 0.651831 0.540899 0.486032 11.00000 0.01320 0.01313 = 0.01029 -0.00119 0.00411 0.00042 AFIX 43 H3 2 0.688729 0.526519 0.438694 11.00000 -1.20000 AFIX 0 C4 1 0.567843 0.587766 0.469669 11.00000 0.01409 0.01092 = 0.00830 -0.00051 0.00084 -0.00155 C5 1 0.509827 0.605676 0.539502 11.00000 0.01172 0.00945 = 0.01319 0.00032 0.00149 0.00085 AFIX 43 H5 2 0.449212 0.636049 0.529144 11.00000 -1.20000 AFIX 0 C6 1 0.542558 0.578292 0.623560 11.00000 0.01011 0.01036 = 0.01061 -0.00074 0.00258 -0.00116 C7 1 0.479259 0.590438 0.702008 11.00000 0.01252 0.00864 = 0.01215 -0.00104 0.00390 -0.00230 C8 1 0.872238 0.538400 0.930182 11.00000 0.01057 0.00985 = 0.01512 0.00240 0.00268 0.00183 C9 1 0.780125 0.500849 0.966991 11.00000 0.01047 0.00900 = 0.01348 0.00102 0.00262 0.00029 C10 1 0.781560 0.493731 1.059003 11.00000 0.01220 0.01194 = 0.01117 -0.00040 0.00058 -0.00055 AFIX 43 H10 2 0.849581 0.509401 1.106461 11.00000 -1.20000 AFIX 0 C11 1 0.680167 0.462796 1.080866 11.00000 0.01487 0.01233 = 0.01101 0.00130 0.00332 0.00216 C12 1 0.581792 0.439870 1.009042 11.00000 0.01347 0.01125 = 0.01219 0.00218 0.00473 0.00031 AFIX 43 H12 2 0.511441 0.419160 1.022007 11.00000 -1.20000 AFIX 0 C13 1 0.590084 0.448219 0.919436 11.00000 0.01129 0.00827 = 0.01331 0.00081 0.00252 0.00117 C14 1 0.489286 0.428360 0.833816 11.00000 0.01287 0.01156 = 0.01203 0.00024 0.00141 0.00110 N3 3 -0.005855 0.798033 0.191477 11.00000 0.01402 0.01043 = 0.01552 0.00004 0.00365 0.00051 AFIX 3 H3N 2 -0.019675 0.835833 0.194817 11.00000 -1.20000 AFIX 0 N4 3 0.037053 0.624661 0.192604 11.00000 0.01753 0.01196 = 0.02953 0.00226 -0.00250 -0.00042 AFIX 3 H4A 2 -0.024707 0.602911 0.154664 11.00000 -1.20000 H4B 2 0.107953 0.607331 0.229514 11.00000 -1.20000 AFIX 0 C15 1 0.107634 0.774839 0.241130 11.00000 0.01344 0.01573 = 0.00937 0.00084 0.00457 0.00065 C16 1 0.207778 0.810878 0.290050 11.00000 0.01805 0.01466 = 0.01424 -0.00102 0.00582 -0.00322 AFIX 43 H16 2 0.194745 0.850600 0.289244 11.00000 -1.20000 AFIX 0 C17 1 0.323457 0.788225 0.338509 11.00000 0.01653 0.02216 = 0.01280 -0.00167 0.00293 -0.00518 AFIX 43 H17 2 0.390981 0.812471 0.371058 11.00000 -1.20000 AFIX 0 C18 1 0.343912 0.729355 0.340836 11.00000 0.01388 0.02394 = 0.01234 0.00216 0.00143 0.00084 AFIX 43 H18 2 0.424950 0.714262 0.374772 11.00000 -1.20000 AFIX 0 C19 1 0.247671 0.693858 0.294480 11.00000 0.01526 0.01608 = 0.01399 0.00309 0.00346 0.00185 AFIX 43 H19 2 0.262313 0.654231 0.296642 11.00000 -1.20000 AFIX 0 C20 1 0.126171 0.715624 0.243189 11.00000 0.01328 0.01425 = 0.01070 0.00084 0.00440 -0.00003 C21 1 0.023301 0.680178 0.191982 11.00000 0.01423 0.01343 = 0.01160 0.00199 0.00366 -0.00113 C22 1 -0.094851 0.706507 0.139240 11.00000 0.01308 0.01216 = 0.01216 0.00135 0.00354 0.00033 C23 1 -0.203257 0.675460 0.088539 11.00000 0.01678 0.01591 = 0.01505 -0.00059 0.00389 -0.00168 AFIX 43 H23 2 -0.198854 0.635396 0.087214 11.00000 -1.20000 AFIX 0 C24 1 -0.314709 0.702341 0.041231 11.00000 0.01369 0.02413 = 0.01500 -0.00212 0.00132 -0.00306 AFIX 43 H24 2 -0.387175 0.680861 0.008001 11.00000 -1.20000 AFIX 0 C25 1 -0.322015 0.761544 0.041770 11.00000 0.01430 0.02559 = 0.01634 0.00170 0.00114 0.00437 AFIX 43 H25 2 -0.398987 0.779822 0.007671 11.00000 -1.20000 AFIX 0 C26 1 -0.220118 0.793240 0.090582 11.00000 0.01598 0.01587 = 0.01651 0.00227 0.00354 0.00385 AFIX 43 H26 2 -0.226349 0.833273 0.090699 11.00000 -1.20000 AFIX 0 C27 1 -0.105479 0.766145 0.140861 11.00000 0.01330 0.01503 = 0.01069 0.00075 0.00393 -0.00001 N5 3 0.981177 0.820265 0.429142 11.00000 0.01311 0.00811 = 0.01514 0.00052 0.00187 0.00059 AFIX 3 H5N 2 0.979757 0.858375 0.436812 11.00000 -1.20000 AFIX 0 N6 3 1.000674 0.646320 0.413995 11.00000 0.01265 0.01059 = 0.01960 0.00040 -0.00043 0.00105 AFIX 3 H6A 2 1.076645 0.627860 0.439295 11.00000 -1.20000 H6B 2 0.933455 0.626849 0.376905 11.00000 -1.20000 AFIX 0 C28 1 1.090764 0.793376 0.478625 11.00000 0.01270 0.01366 = 0.00998 0.00166 0.00406 0.00175 C29 1 1.195838 0.826198 0.529307 11.00000 0.01660 0.01159 = 0.01419 -0.00005 0.00416 -0.00098 AFIX 43 H29 2 1.190393 0.866260 0.527894 11.00000 -1.20000 AFIX 0 C30 1 1.305849 0.799983 0.580610 11.00000 0.01549 0.01733 = 0.01290 -0.00091 0.00183 -0.00249 AFIX 43 H30 2 1.377089 0.822084 0.613985 11.00000 -1.20000 AFIX 0 C31 1 1.314219 0.740582 0.584290 11.00000 0.01413 0.01712 = 0.01330 0.00075 0.00140 0.00226 AFIX 43 H31 2 1.389622 0.722832 0.621715 11.00000 -1.20000 AFIX 0 C32 1 1.213627 0.708387 0.533901 11.00000 0.01482 0.01252 = 0.01371 0.00068 0.00404 0.00158 AFIX 43 H32 2 1.220505 0.668372 0.536260 11.00000 -1.20000 AFIX 0 C33 1 1.099761 0.733814 0.478454 11.00000 0.01169 0.01076 = 0.01235 -0.00016 0.00415 0.00030 C34 1 0.992942 0.701600 0.422505 11.00000 0.01152 0.01202 = 0.01103 0.00130 0.00315 0.00048 C35 1 0.876640 0.731738 0.375589 11.00000 0.01190 0.01164 = 0.01122 0.00056 0.00371 0.00063 C36 1 0.763658 0.703305 0.324900 11.00000 0.01513 0.01172 = 0.01762 -0.00066 0.00320 0.00004 AFIX 43 H36 2 0.763878 0.663258 0.320787 11.00000 -1.20000 AFIX 0 C37 1 0.654154 0.732760 0.281759 11.00000 0.01307 0.01645 = 0.01782 -0.00045 0.00091 -0.00145 AFIX 43 H37 2 0.578775 0.713218 0.248088 11.00000 -1.20000 AFIX 0 C38 1 0.653458 0.792138 0.287393 11.00000 0.01462 0.01700 = 0.01704 0.00237 0.00046 0.00448 AFIX 43 H38 2 0.576878 0.812330 0.257639 11.00000 -1.20000 AFIX 0 C39 1 0.760994 0.821264 0.334907 11.00000 0.01645 0.01169 = 0.01580 0.00092 0.00322 0.00352 AFIX 43 H39 2 0.759466 0.861353 0.337371 11.00000 -1.20000 AFIX 0 C40 1 0.874306 0.791311 0.380272 11.00000 0.01246 0.01239 = 0.01134 0.00043 0.00385 0.00095 O11 4 0.050834 0.412285 0.300583 11.00000 0.02585 0.01518 = 0.02723 0.00445 0.01531 0.00129 AFIX 3 H11A 2 0.070364 0.431025 0.258083 11.00000 -1.20000 H11B 2 -0.000836 0.432905 0.320513 11.00000 -1.20000 AFIX 0 O12 4 0.844981 0.455484 0.367432 11.00000 0.01943 0.02431 = 0.01415 -0.00152 0.00429 -0.00148 AFIX 3 H12A 2 0.838401 0.452644 0.422272 11.00000 -1.20000 H12B 2 0.786541 0.435214 0.334182 11.00000 -1.20000 AFIX 0 O13 4 0.165086 0.432908 0.708178 11.00000 0.02066 0.01603 = 0.03216 -0.00098 -0.00763 -0.00259 AFIX 3 H13A 2 0.236006 0.430078 0.748608 11.00000 -1.20000 H13B 2 0.166876 0.467428 0.695488 11.00000 -1.20000 HKLF 4 REM JTM364_0m in P2(1)/c REM R1 = 0.0350 for 7263 Fo > 4sig(Fo) and 0.0485 for all 9000 data REM 541 parameters refined using 0 restraints END WGHT 0.0406 2.1545 REM Highest difference peak 0.448, deepest hole -0.339, 1-sigma level 0.067 Q1 1 1.0460 0.7178 0.4592 11.00000 0.05 0.45 Q2 1 1.0962 0.7630 0.4780 11.00000 0.05 0.44 Q3 1 -0.1007 0.7342 0.1412 11.00000 0.05 0.43 Q4 1 -0.0341 0.6922 0.1608 11.00000 0.05 0.43 Q5 1 0.8666 0.7614 0.3793 11.00000 0.05 0.43 ; _database_code_depnum_ccdc_archive 'CCDC 940543' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Cr N2 O10, C13 H11 N2, 4(H2 O)' _chemical_formula_sum 'C27 H21 Cr N4 O14' _chemical_formula_weight 677.48 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' Cr Cr 0.3209 0.6236 '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 7.8867(12) _cell_length_b 11.0204(17) _cell_length_c 16.859(3) _cell_angle_alpha 84.453(2) _cell_angle_beta 89.358(2) _cell_angle_gamma 75.087(2) _cell_volume 1409.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.93 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7942 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 14 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25141 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 29.12 _reflns_number_total 7136 _reflns_number_gt 6062 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2008)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2008)' _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. H-atoms attached to carbon were placed in calculated positions (C---H = 0.95 \%A) while those attached to nitrogen and oxygen were placed in locations derived from a difference map. Not all of the latter could be located with confidence due to disorder. All were included as riding contributions with isotropic displacement parameters 1.2 times those of the attached atoms. The cation portion of the asymmetric unit consists of two half-cations disordered about centers of symmetry. ; _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^)+(0.0866P)^2^+1.5229P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7136 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1532 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Cr1 Cr 0.42125(4) 0.74365(3) 0.25252(2) 0.02224(12) Uani 1 1 d . . . O1 O 0.3377(2) 0.58536(17) 0.27016(10) 0.0312(4) Uani 1 1 d . . . O2 O 0.4948(2) 0.89350(16) 0.28325(10) 0.0291(4) Uani 1 1 d . . . O3 O 0.2320(3) 0.46196(18) 0.36123(12) 0.0397(4) Uani 1 1 d . . . O4 O 0.5121(3) 1.00837(18) 0.38417(12) 0.0372(4) Uani 1 1 d . . . O5 O 0.3079(3) 0.71144(19) 0.60825(10) 0.0367(4) Uani 1 1 d . . . H5O H 0.2465 0.6605 0.6203 0.044 Uiso 1 1 d R . . O6 O 0.6712(2) 0.64682(16) 0.23990(10) 0.0296(4) Uani 1 1 d . . . O7 O 0.1832(2) 0.84999(18) 0.21763(10) 0.0318(4) Uani 1 1 d . . . O8 O 0.8910(3) 0.6055(2) 0.15299(13) 0.0497(6) Uani 1 1 d . . . O9 O 0.0152(3) 0.9452(3) 0.11150(12) 0.0567(7) Uani 1 1 d . . . O10 O 0.5433(3) 0.8691(3) -0.09509(12) 0.0603(7) Uani 1 1 d . . . H10O H 0.4591 0.9156 -0.1227 0.072 Uiso 1 1 d R . . N1 N 0.3924(2) 0.72763(17) 0.36919(11) 0.0223(4) Uani 1 1 d . . . N2 N 0.4510(3) 0.77322(19) 0.13682(11) 0.0270(4) Uani 1 1 d . . . C1 C 0.2958(3) 0.5512(2) 0.34164(15) 0.0298(5) Uani 1 1 d . . . C2 C 0.3310(3) 0.6334(2) 0.40320(14) 0.0247(4) Uani 1 1 d . . . C3 C 0.3014(3) 0.6220(2) 0.48407(14) 0.0281(5) Uani 1 1 d . . . H3 H 0.2586 0.5543 0.5082 0.034 Uiso 1 1 calc R . . C4 C 0.3364(3) 0.7134(2) 0.52994(14) 0.0280(5) Uani 1 1 d . . . C5 C 0.4006(3) 0.8123(2) 0.49287(14) 0.0271(5) Uani 1 1 d . . . H5 H 0.4259 0.8744 0.5228 0.033 Uiso 1 1 calc R . . C6 C 0.4254(3) 0.8160(2) 0.41177(13) 0.0233(4) Uani 1 1 d . . . C7 C 0.4828(3) 0.9157(2) 0.35818(14) 0.0273(5) Uani 1 1 d . . . C8 C 0.7397(3) 0.6549(3) 0.16946(15) 0.0337(5) Uani 1 1 d . . . C9 C 0.6105(3) 0.7332(3) 0.10667(15) 0.0329(5) Uani 1 1 d . . . C10 C 0.6438(4) 0.7647(3) 0.02849(16) 0.0470(8) Uani 1 1 d . . . H10 H 0.7580 0.7361 0.0076 0.056 Uiso 1 1 calc R . . C11 C 0.5058(4) 0.8401(3) -0.02008(16) 0.0443(7) Uani 1 1 d . . . C12 C 0.3376(3) 0.8819(3) 0.01268(15) 0.0388(6) Uani 1 1 d . . . H12 H 0.2416 0.9326 -0.0189 0.047 Uiso 1 1 calc R . . C13 C 0.3181(3) 0.8466(2) 0.09205(14) 0.0305(5) Uani 1 1 d . . . C14 C 0.1557(3) 0.8854(3) 0.14194(15) 0.0349(6) Uani 1 1 d . . . N3 N 0.0922(6) 0.0562(4) 0.3387(2) 0.0320(9) Uani 0.50 1 d P . . H3A H 0.0868 -0.0012 0.3042 0.038 Uiso 0.50 1 d PR . . H3B H 0.1525 0.1124 0.3307 0.038 Uiso 0.50 1 d PR . . N4 N 0.0370(3) 0.0369(2) 0.42209(16) 0.0367(5) Uani 0.50 1 d P . . H4N H 0.0442 0.0604 0.3692 0.044 Uiso 0.50 1 d PR . . C15 C -0.1190(4) -0.2452(3) 0.39421(19) 0.0439(7) Uani 1 1 d . . . H15 H -0.1375 -0.2931 0.3527 0.053 Uiso 1 1 calc R . . C16 C -0.0588(3) -0.1408(3) 0.37648(17) 0.0411(7) Uani 1 1 d . . . H16 H -0.0360 -0.1160 0.3227 0.049 Uiso 1 1 calc R . . C17 C -0.0300(3) -0.0688(3) 0.43766(16) 0.0343(6) Uani 1 1 d . . . C18 C 0.0370(3) 0.0369(2) 0.42209(16) 0.0367(5) Uani 0.50 1 d P . . C19 C 0.0672(3) 0.1058(2) 0.48248(16) 0.0307(5) Uani 1 1 d . . . C20 C 0.1307(3) 0.2139(2) 0.46618(16) 0.0319(5) Uani 1 1 d . . . H20 H 0.1574 0.2390 0.4130 0.038 Uiso 1 1 calc R . . N5 N 0.7433(6) 0.5276(6) 0.8764(3) 0.0524(15) Uani 0.50 1 d P . . H5A H 0.8603 0.4899 0.8752 0.063 Uiso 0.50 1 d PR . . N6 N 0.6125(5) 0.5092(3) 0.9373(2) 0.0588(8) Uani 0.50 1 d P . . H6N H 0.6898 0.5211 0.8987 0.071 Uiso 0.50 1 d PR . . C21 C 0.1541(3) 0.2827(3) 0.52652(19) 0.0397(6) Uani 1 1 d . . . H21 H 0.1943 0.3566 0.5148 0.048 Uiso 1 1 calc R . . C22 C 0.1943(5) 0.7054(4) 0.8479(3) 0.0694(12) Uani 1 1 d . . . H22 H 0.1500 0.7536 0.7993 0.083 Uiso 1 1 calc R . . C23 C 0.3689(4) 0.6434(3) 0.8557(3) 0.0599(10) Uani 1 1 d . . . H23 H 0.4454 0.6491 0.8123 0.072 Uiso 1 1 calc R . . C24 C 0.4358(4) 0.5713(3) 0.9276(2) 0.0550(9) Uani 1 1 d . . . C25 C 0.6125(5) 0.5092(3) 0.9373(2) 0.0588(8) Uani 0.50 1 d P . . C26 C 0.6798(5) 0.4379(3) 1.0082(2) 0.0572(9) Uani 1 1 d . . . C27 C 0.8591(5) 0.3735(3) 1.0181(3) 0.0693(12) Uani 1 1 d . . . H27 H 0.9381 0.3796 0.9758 0.083 Uiso 1 1 calc R . . C28 C 0.9194(5) 0.3029(4) 1.0875(3) 0.0752(14) Uani 1 1 d . . . H28 H 1.0397 0.2584 1.0926 0.090 Uiso 1 1 calc R . . O11 O 0.1397(3) 0.5412(2) 0.65334(12) 0.0434(5) Uani 1 1 d . . . H11A H 0.1811 0.4841 0.6899 0.052 Uiso 1 1 d R . . H11B H 0.0318 0.5463 0.6498 0.052 Uiso 1 1 d R . . O12 O 0.2914(3) -0.0074(4) 0.81413(17) 0.0938(13) Uani 1 1 d . . . H12B H 0.3254 0.0159 0.7679 0.113 Uiso 1 1 d R . . O13 O -0.3339(6) -0.2389(4) 0.7205(2) 0.0834(13) Uani 0.798(5) 1 d P A 1 H13A H -0.3031 -0.3052 0.6962 0.100 Uiso 0.731(4) 1 d PR A 1 H13B H -0.4149 -0.1720 0.7061 0.100 Uiso 0.731(4) 1 d PR A 1 O13A O -0.622(2) -0.1478(14) 0.7112(8) 0.0834(13) Uani 0.202(5) 1 d P A 2 O14 O -0.1148(6) -0.1109(4) 0.7269(2) 0.0433(9) Uani 0.50 1 d P . . O15 O 0.1912(12) 0.4391(12) 1.1837(6) 0.067(4) Uani 0.28 1 d P . 1 O15A O 0.1892(12) 0.3969(11) 1.1535(8) 0.046(2) Uani 0.22 1 d P . 2 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 Cr1 0.02137(18) 0.02357(19) 0.01979(18) -0.00218(13) -0.00118(12) -0.00210(13) O1 0.0347(9) 0.0316(9) 0.0292(9) -0.0057(7) -0.0035(7) -0.0107(7) O2 0.0364(9) 0.0267(8) 0.0248(8) -0.0025(6) 0.0029(7) -0.0095(7) O3 0.0466(11) 0.0344(10) 0.0428(11) -0.0031(8) -0.0009(9) -0.0193(8) O4 0.0462(11) 0.0331(9) 0.0376(10) -0.0115(8) 0.0032(8) -0.0169(8) O5 0.0376(10) 0.0458(11) 0.0241(8) -0.0008(8) 0.0021(7) -0.0072(8) O6 0.0249(8) 0.0323(9) 0.0272(8) -0.0028(7) -0.0031(6) 0.0009(7) O7 0.0250(8) 0.0410(10) 0.0222(8) 0.0011(7) 0.0014(6) 0.0028(7) O8 0.0282(10) 0.0664(15) 0.0421(11) -0.0054(10) 0.0032(8) 0.0099(9) O9 0.0314(10) 0.0856(18) 0.0311(10) 0.0128(11) 0.0012(8) 0.0179(10) O10 0.0382(11) 0.107(2) 0.0225(9) 0.0074(11) 0.0058(8) -0.0002(12) N1 0.0183(8) 0.0240(9) 0.0229(9) -0.0017(7) -0.0017(6) -0.0024(7) N2 0.0242(9) 0.0313(10) 0.0216(9) -0.0039(7) 0.0001(7) 0.0003(8) C1 0.0285(11) 0.0280(11) 0.0327(12) -0.0019(9) -0.0045(9) -0.0069(9) C2 0.0198(9) 0.0248(10) 0.0276(11) 0.0003(8) -0.0023(8) -0.0035(8) C3 0.0241(10) 0.0277(11) 0.0292(11) 0.0036(9) -0.0019(8) -0.0028(9) C4 0.0224(10) 0.0341(12) 0.0226(10) 0.0000(9) -0.0020(8) 0.0006(9) C5 0.0216(10) 0.0329(12) 0.0257(11) -0.0064(9) -0.0021(8) -0.0035(9) C6 0.0191(9) 0.0245(10) 0.0252(10) -0.0045(8) -0.0006(8) -0.0028(8) C7 0.0267(11) 0.0261(11) 0.0287(11) -0.0048(9) 0.0006(9) -0.0053(9) C8 0.0269(11) 0.0398(13) 0.0297(12) -0.0061(10) 0.0002(9) 0.0011(10) C9 0.0258(11) 0.0419(14) 0.0263(11) -0.0081(10) 0.0015(9) 0.0014(10) C10 0.0295(13) 0.074(2) 0.0272(13) -0.0062(13) 0.0063(10) 0.0050(13) C11 0.0349(14) 0.069(2) 0.0222(12) -0.0016(12) 0.0046(10) -0.0015(13) C12 0.0300(12) 0.0537(17) 0.0238(11) 0.0021(11) 0.0010(9) 0.0032(11) C13 0.0267(11) 0.0372(13) 0.0223(10) -0.0013(9) -0.0004(8) 0.0010(9) C14 0.0276(12) 0.0445(14) 0.0239(11) 0.0012(10) 0.0021(9) 0.0046(10) N3 0.035(2) 0.031(2) 0.0271(19) 0.0008(16) 0.0055(16) -0.0038(17) N4 0.0234(10) 0.0384(13) 0.0436(13) 0.0160(10) -0.0109(9) -0.0064(9) C15 0.0297(13) 0.0495(17) 0.0470(16) -0.0116(13) -0.0055(11) 0.0027(12) C16 0.0228(11) 0.0580(18) 0.0326(13) 0.0032(12) -0.0008(10) 0.0046(11) C17 0.0161(10) 0.0418(14) 0.0384(13) 0.0112(11) -0.0039(9) -0.0010(9) C18 0.0234(10) 0.0384(13) 0.0436(13) 0.0160(10) -0.0109(9) -0.0064(9) C19 0.0167(10) 0.0327(12) 0.0382(13) 0.0070(10) -0.0049(9) -0.0021(9) C20 0.0227(10) 0.0311(12) 0.0397(13) 0.0009(10) 0.0012(9) -0.0045(9) N5 0.023(2) 0.095(5) 0.044(3) -0.029(3) 0.008(2) -0.016(3) N6 0.064(2) 0.0382(15) 0.068(2) -0.0100(14) 0.0079(16) -0.0004(14) C21 0.0269(12) 0.0334(13) 0.0571(17) -0.0056(12) -0.0003(11) -0.0042(10) C22 0.0389(17) 0.056(2) 0.100(3) 0.026(2) 0.0152(18) -0.0017(15) C23 0.0379(16) 0.0478(18) 0.085(3) 0.0108(18) 0.0166(16) -0.0021(14) C24 0.0466(17) 0.0341(15) 0.077(2) -0.0024(15) 0.0124(16) 0.0018(13) C25 0.064(2) 0.0382(15) 0.068(2) -0.0100(14) 0.0079(16) -0.0004(14) C26 0.060(2) 0.0297(14) 0.075(2) -0.0017(15) 0.0165(18) -0.0008(13) C27 0.057(2) 0.0425(18) 0.101(3) 0.0056(19) 0.035(2) -0.0047(16) C28 0.0407(18) 0.056(2) 0.115(4) 0.019(2) 0.027(2) 0.0011(16) O11 0.0354(10) 0.0467(11) 0.0406(11) 0.0165(9) -0.0011(8) -0.0044(8) O12 0.0396(13) 0.157(3) 0.0645(17) 0.072(2) 0.0021(12) -0.0184(16) O13 0.108(3) 0.070(2) 0.0482(18) -0.0061(16) 0.0209(19) 0.020(2) O13A 0.108(3) 0.070(2) 0.0482(18) -0.0061(16) 0.0209(19) 0.020(2) O14 0.051(2) 0.042(2) 0.0298(19) -0.0065(16) -0.0047(17) 0.0034(18) O15 0.036(4) 0.111(9) 0.041(5) -0.055(6) -0.011(4) 0.020(5) O15A 0.020(4) 0.057(7) 0.052(7) 0.008(5) 0.007(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N2 1.968(2) . ? Cr1 N1 1.9737(19) . ? Cr1 O2 1.9991(17) . ? Cr1 O7 2.0006(17) . ? Cr1 O6 2.0053(17) . ? Cr1 O1 2.0132(18) . ? O1 C1 1.292(3) . ? O2 C7 1.308(3) . ? O3 C1 1.232(3) . ? O4 C7 1.224(3) . ? O5 C4 1.336(3) . ? O5 H5O 0.8400 . ? O6 C8 1.304(3) . ? O7 C14 1.301(3) . ? O8 C8 1.218(3) . ? O9 C14 1.224(3) . ? O10 C11 1.324(3) . ? O10 H10O 0.8399 . ? N1 C2 1.334(3) . ? N1 C6 1.342(3) . ? N2 C9 1.334(3) . ? N2 C13 1.336(3) . ? C1 C2 1.514(3) . ? C2 C3 1.380(3) . ? C3 C4 1.410(3) . ? C3 H3 0.9500 . ? C4 C5 1.407(4) . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 C7 1.511(3) . ? C8 C9 1.516(4) . ? C9 C10 1.370(4) . ? C10 C11 1.403(4) . ? C10 H10 0.9500 . ? C11 C12 1.412(4) . ? C12 C13 1.375(3) . ? C12 H12 0.9500 . ? C13 C14 1.515(3) . ? N3 O14 1.241(6) 2_556 ? N3 N4 1.479(5) . ? N3 H3A 0.9100 . ? N3 H3B 0.8721 . ? N3 H4N 0.6331 . ? N4 C19 1.385(4) . ? N4 C17 1.399(4) . ? N4 H4N 0.9100 . ? C15 C16 1.360(5) . ? C15 C21 1.406(4) 2_556 ? C15 H15 0.9500 . ? C16 C17 1.415(4) . ? C16 H16 0.9500 . ? C17 C19 1.418(4) 2_556 ? C19 C20 1.409(4) . ? C19 C17 1.418(4) 2_556 ? C20 C21 1.368(4) . ? C20 H20 0.9500 . ? N5 O15A 1.170(12) 2_667 ? N5 O15 1.200(13) 2_667 ? N5 N6 1.484(6) . ? N5 H5A 0.9100 . ? N5 H6N 0.5757 . ? N6 C24 1.389(5) . ? N6 C26 1.395(5) . ? N6 H6N 0.9100 . ? C21 C15 1.406(4) 2_556 ? C21 H21 0.9500 . ? C22 C23 1.372(5) . ? C22 C28 1.414(5) 2_667 ? C22 H22 0.9500 . ? C23 C24 1.411(5) . ? C23 H23 0.9500 . ? C24 C26 1.421(5) 2_667 ? C26 C27 1.413(5) . ? C26 C24 1.421(5) 2_667 ? C27 C28 1.359(6) . ? C27 H27 0.9500 . ? C28 C22 1.414(5) 2_667 ? C28 H28 0.9500 . ? O11 H11A 0.8404 . ? O11 H11B 0.8404 . ? O12 H12B 0.8580 . ? O13 H13A 0.8516 . ? O13 H13B 0.8587 . ? O14 N3 1.241(6) 2_556 ? O15 N5 1.200(13) 2_667 ? O15A N5 1.170(12) 2_667 ? 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 Cr1 N1 175.53(8) . . ? N2 Cr1 O2 97.22(8) . . ? N1 Cr1 O2 78.46(7) . . ? N2 Cr1 O7 78.23(7) . . ? N1 Cr1 O7 100.62(7) . . ? O2 Cr1 O7 91.88(8) . . ? N2 Cr1 O6 78.59(7) . . ? N1 Cr1 O6 102.55(7) . . ? O2 Cr1 O6 91.83(7) . . ? O7 Cr1 O6 156.80(7) . . ? N2 Cr1 O1 106.27(8) . . ? N1 Cr1 O1 78.05(7) . . ? O2 Cr1 O1 156.51(7) . . ? O7 Cr1 O1 92.94(8) . . ? O6 Cr1 O1 92.72(7) . . ? C1 O1 Cr1 117.96(15) . . ? C7 O2 Cr1 117.87(15) . . ? C4 O5 H5O 107.9 . . ? C8 O6 Cr1 117.63(15) . . ? C14 O7 Cr1 118.02(15) . . ? C11 O10 H10O 115.1 . . ? C2 N1 C6 121.5(2) . . ? C2 N1 Cr1 119.21(15) . . ? C6 N1 Cr1 119.12(15) . . ? C9 N2 C13 121.2(2) . . ? C9 N2 Cr1 118.68(16) . . ? C13 N2 Cr1 119.53(16) . . ? O3 C1 O1 125.8(2) . . ? O3 C1 C2 120.6(2) . . ? O1 C1 C2 113.6(2) . . ? N1 C2 C3 121.1(2) . . ? N1 C2 C1 111.0(2) . . ? C3 C2 C1 127.8(2) . . ? C2 C3 C4 118.2(2) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? O5 C4 C5 117.9(2) . . ? O5 C4 C3 122.3(2) . . ? C5 C4 C3 119.8(2) . . ? C6 C5 C4 117.8(2) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? N1 C6 C5 121.6(2) . . ? N1 C6 C7 110.74(19) . . ? C5 C6 C7 127.7(2) . . ? O4 C7 O2 124.6(2) . . ? O4 C7 C6 121.7(2) . . ? O2 C7 C6 113.66(19) . . ? O8 C8 O6 125.4(2) . . ? O8 C8 C9 121.4(2) . . ? O6 C8 C9 113.2(2) . . ? N2 C9 C10 121.3(2) . . ? N2 C9 C8 111.3(2) . . ? C10 C9 C8 127.4(2) . . ? C9 C10 C11 118.6(2) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? O10 C11 C10 116.8(2) . . ? O10 C11 C12 123.7(3) . . ? C10 C11 C12 119.5(2) . . ? C13 C12 C11 117.5(2) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? N2 C13 C12 121.9(2) . . ? N2 C13 C14 110.4(2) . . ? C12 C13 C14 127.6(2) . . ? O9 C14 O7 125.3(2) . . ? O9 C14 C13 121.2(2) . . ? O7 C14 C13 113.5(2) . . ? N4 N3 H3A 119.5 . . ? N4 N3 H3B 114.3 . . ? H3A N3 H3B 124.3 . . ? H3A N3 H4N 119.3 . . ? H3B N3 H4N 116.1 . . ? C19 N4 C17 121.7(2) . . ? C19 N4 N3 124.1(3) . . ? C17 N4 N3 113.8(3) . . ? C19 N4 H4N 124.5 . . ? C17 N4 H4N 113.4 . . ? C16 C15 C21 120.5(3) . 2_556 ? C16 C15 H15 119.8 . . ? C21 C15 H15 119.8 2_556 . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? N4 C17 C16 122.1(3) . . ? N4 C17 C19 118.8(3) . 2_556 ? C16 C17 C19 119.2(3) . 2_556 ? N4 C19 C20 121.4(2) . . ? N4 C19 C17 119.5(2) . 2_556 ? C20 C19 C17 119.0(3) . 2_556 ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C24 N6 C26 122.0(3) . . ? C24 N6 N5 121.6(4) . . ? C26 N6 N5 116.1(4) . . ? C24 N6 H6N 119.8 . . ? C26 N6 H6N 117.9 . . ? C20 C21 C15 120.6(3) . 2_556 ? C20 C21 H21 119.7 . . ? C15 C21 H21 119.7 2_556 . ? C23 C22 C28 119.8(4) . 2_667 ? C23 C22 H22 120.1 . . ? C28 C22 H22 120.1 2_667 . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? N6 C24 C23 121.6(3) . . ? N6 C24 C26 119.0(4) . 2_667 ? C23 C24 C26 119.4(3) . 2_667 ? N6 C26 C27 122.2(4) . . ? N6 C26 C24 119.0(3) . 2_667 ? C27 C26 C24 118.8(4) . 2_667 ? C28 C27 C26 120.6(4) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C22 121.0(4) . 2_667 ? C27 C28 H28 119.5 . . ? C22 C28 H28 119.5 2_667 . ? H11A O11 H11B 107.0 . . ? H13A O13 H13B 126.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5O O11 0.84 1.78 2.615(3) 173 . O10 H10O O12 0.84 1.70 2.533(3) 172 1_564 N3 H3A O7 0.91 2.28 3.142(5) 158 1_545 N3 H3B O13 0.87 2.35 3.198(6) 166 2_556 N5 H5A O8 0.91 2.05 2.941(5) 167 2_766 O11 H11A O6 0.84 1.92 2.740(3) 166 2_666 O11 H11B O3 0.84 2.12 2.954(3) 174 2_566 O12 H12B O2 0.86 2.07 2.782(3) 140 2_666 O13 H13B O4 0.86 2.22 2.982(4) 148 2_566 _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.333 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.090 _iucr_refine_instructions_details ; TITL JTM363_0m in P-1 CELL 0.71073 7.8867 11.0204 16.8595 84.453 89.358 75.087 ZERR 2.00 0.0012 0.0017 0.0026 0.002 0.002 0.002 LATT 1 SFAC C H N O Cr UNIT 54 42 8 28 2 L.S. 6 ACTA 55.5 BOND $H FMAP 2 PLAN 5 SIZE 0.13 0.15 0.21 EADP O13 O13A EADP N6 C25 EXYZ N6 C25 EADP N4 C18 EXYZ N4 C18 EQIV $1 x, y+1, z-1 EQIV $2 x, y-1, z EQIV $3 -x, -y, -z+1 EQIV $4 -x+2, -y+1, -z+1 EQIV $5 -x+1, -y+1, -z+1 EQIV $6 -x, -y+1, -z+1 HTAB O5 O11 HTAB O10 O12_$1 HTAB N3 O7_$2 HTAB N3 O13_$3 HTAB N5 O8_$4 HTAB O11 O6_$5 HTAB O11 O3_$6 HTAB O12 O2_$5 HTAB O13 O4_$6 MPLA Cr1 O1 O2 N1 C1 C2 C6 C7 MPLA Cr1 O6 O7 N2 C8 C9 C13 C14 TEMP -173 WGHT 0.086600 1.522900 FVAR 0.15172 0.79837 CR1 5 0.421248 0.743652 0.252523 11.00000 0.02137 0.02357 = 0.01979 -0.00218 -0.00118 -0.00210 O1 4 0.337668 0.585361 0.270157 11.00000 0.03474 0.03157 = 0.02922 -0.00567 -0.00354 -0.01070 O2 4 0.494780 0.893496 0.283249 11.00000 0.03642 0.02670 = 0.02483 -0.00252 0.00288 -0.00953 O3 4 0.232027 0.461957 0.361234 11.00000 0.04665 0.03438 = 0.04279 -0.00311 -0.00091 -0.01935 O4 4 0.512065 1.008368 0.384174 11.00000 0.04623 0.03314 = 0.03762 -0.01148 0.00318 -0.01689 O5 4 0.307862 0.711435 0.608254 11.00000 0.03758 0.04584 = 0.02406 -0.00077 0.00206 -0.00721 AFIX 3 H5O 2 0.246502 0.660517 0.620263 11.00000 -1.20000 AFIX 0 O6 4 0.671184 0.646823 0.239903 11.00000 0.02487 0.03229 = 0.02716 -0.00280 -0.00309 0.00085 O7 4 0.183234 0.849986 0.217628 11.00000 0.02501 0.04099 = 0.02224 0.00113 0.00137 0.00276 O8 4 0.890958 0.605523 0.152987 11.00000 0.02824 0.06641 = 0.04207 -0.00543 0.00321 0.00992 O9 4 0.015170 0.945196 0.111504 11.00000 0.03138 0.08559 = 0.03113 0.01281 0.00115 0.01791 O10 4 0.543349 0.869143 -0.095087 11.00000 0.03817 0.10699 = 0.02252 0.00738 0.00577 -0.00019 AFIX 3 H10O 2 0.459149 0.915603 -0.122687 11.00000 -1.20000 AFIX 0 N1 3 0.392442 0.727625 0.369195 11.00000 0.01830 0.02398 = 0.02292 -0.00175 -0.00170 -0.00241 N2 3 0.450954 0.773225 0.136821 11.00000 0.02423 0.03125 = 0.02157 -0.00392 0.00011 0.00026 C1 1 0.295815 0.551230 0.341636 11.00000 0.02848 0.02796 = 0.03274 -0.00188 -0.00452 -0.00692 C2 1 0.331010 0.633441 0.403199 11.00000 0.01979 0.02477 = 0.02765 0.00029 -0.00230 -0.00350 C3 1 0.301390 0.621959 0.484066 11.00000 0.02414 0.02768 = 0.02915 0.00362 -0.00194 -0.00278 AFIX 43 H3 2 0.258586 0.554328 0.508172 11.00000 -1.20000 AFIX 0 C4 1 0.336426 0.713408 0.529936 11.00000 0.02238 0.03408 = 0.02258 -0.00005 -0.00199 0.00060 C5 1 0.400568 0.812274 0.492873 11.00000 0.02157 0.03294 = 0.02573 -0.00638 -0.00210 -0.00353 AFIX 43 H5 2 0.425938 0.874395 0.522783 11.00000 -1.20000 AFIX 0 C6 1 0.425362 0.816008 0.411774 11.00000 0.01913 0.02446 = 0.02522 -0.00450 -0.00060 -0.00277 C7 1 0.482832 0.915711 0.358175 11.00000 0.02666 0.02608 = 0.02869 -0.00479 0.00060 -0.00528 C8 1 0.739711 0.654921 0.169455 11.00000 0.02691 0.03978 = 0.02969 -0.00610 0.00016 0.00111 C9 1 0.610488 0.733162 0.106670 11.00000 0.02585 0.04193 = 0.02632 -0.00807 0.00150 0.00143 C10 1 0.643805 0.764687 0.028486 11.00000 0.02947 0.07439 = 0.02721 -0.00620 0.00626 0.00500 AFIX 43 H10 2 0.757986 0.736093 0.007600 11.00000 -1.20000 AFIX 0 C11 1 0.505764 0.840079 -0.020077 11.00000 0.03487 0.06851 = 0.02222 -0.00160 0.00461 -0.00147 C12 1 0.337605 0.881929 0.012683 11.00000 0.03002 0.05369 = 0.02378 0.00206 0.00095 0.00319 AFIX 43 H12 2 0.241619 0.932601 -0.018907 11.00000 -1.20000 AFIX 0 C13 1 0.318061 0.846554 0.092045 11.00000 0.02671 0.03719 = 0.02226 -0.00135 -0.00042 0.00102 C14 1 0.155686 0.885365 0.141943 11.00000 0.02764 0.04445 = 0.02388 0.00124 0.00212 0.00464 N3 3 0.092247 0.056228 0.338705 10.50000 0.03469 0.03074 = 0.02706 0.00075 0.00554 -0.00381 AFIX 3 H3A 2 0.086757 -0.001233 0.304155 10.50000 -1.20000 H3B 2 0.152477 0.112377 0.330655 10.50000 -1.20000 AFIX 0 N4 3 0.037012 0.036866 0.422094 10.50000 0.02342 0.03838 = 0.04356 0.01598 -0.01090 -0.00644 AFIX 3 H4N 2 0.044192 0.060356 0.369174 10.50000 -1.20000 AFIX 0 C15 1 -0.118992 -0.245209 0.394207 11.00000 0.02974 0.04948 = 0.04697 -0.01163 -0.00554 0.00271 AFIX 43 H15 2 -0.137476 -0.293135 0.352731 11.00000 -1.20000 AFIX 0 C16 1 -0.058795 -0.140782 0.376481 11.00000 0.02282 0.05802 = 0.03260 0.00315 -0.00082 0.00459 AFIX 43 H16 2 -0.035995 -0.116048 0.322702 11.00000 -1.20000 AFIX 0 C17 1 -0.029954 -0.068814 0.437660 11.00000 0.01605 0.04184 = 0.03840 0.01123 -0.00394 -0.00098 C18 1 0.037012 0.036866 0.422094 10.50000 0.02342 0.03838 = 0.04356 0.01598 -0.01090 -0.00644 C19 1 0.067214 0.105771 0.482478 11.00000 0.01672 0.03271 = 0.03824 0.00695 -0.00487 -0.00213 C20 1 0.130686 0.213864 0.466176 11.00000 0.02273 0.03110 = 0.03972 0.00086 0.00124 -0.00452 AFIX 43 H20 2 0.157376 0.239027 0.413007 11.00000 -1.20000 AFIX 0 N5 3 0.743303 0.527620 0.876390 10.50000 0.02286 0.09537 = 0.04368 -0.02929 0.00779 -0.01594 AFIX 3 H5A 2 0.860272 0.489902 0.875150 10.50000 -1.20000 AFIX 0 N6 3 0.612453 0.509170 0.937263 10.50000 0.06413 0.03818 = 0.06778 -0.00997 0.00790 -0.00045 AFIX 3 H6N 2 0.689763 0.521130 0.898682 10.50000 -1.20000 AFIX 0 C21 1 0.154052 0.282724 0.526520 11.00000 0.02691 0.03335 = 0.05707 -0.00560 -0.00026 -0.00424 AFIX 43 H21 2 0.194326 0.356551 0.514780 11.00000 -1.20000 AFIX 0 C22 1 0.194334 0.705364 0.847932 11.00000 0.03894 0.05629 = 0.09998 0.02616 0.01524 -0.00173 AFIX 43 H22 2 0.149992 0.753621 0.799349 11.00000 -1.20000 AFIX 0 C23 1 0.368938 0.643420 0.855684 11.00000 0.03787 0.04781 = 0.08533 0.01085 0.01656 -0.00215 AFIX 43 H23 2 0.445396 0.649111 0.812331 11.00000 -1.20000 AFIX 0 C24 1 0.435782 0.571317 0.927582 11.00000 0.04661 0.03411 = 0.07658 -0.00243 0.01239 0.00179 C25 1 0.612453 0.509170 0.937263 10.50000 0.06413 0.03818 = 0.06778 -0.00997 0.00790 -0.00045 C26 1 0.679836 0.437925 1.008201 11.00000 0.06003 0.02967 = 0.07499 -0.00171 0.01649 -0.00085 C27 1 0.859062 0.373484 1.018070 11.00000 0.05660 0.04249 = 0.10098 0.00561 0.03490 -0.00468 AFIX 43 H27 2 0.938084 0.379561 0.975825 11.00000 -1.20000 AFIX 0 C28 1 0.919404 0.302891 1.087456 11.00000 0.04073 0.05632 = 0.11483 0.01892 0.02705 0.00113 AFIX 43 H28 2 1.039730 0.258436 1.092646 11.00000 -1.20000 AFIX 0 O11 4 0.139694 0.541189 0.653341 11.00000 0.03545 0.04674 = 0.04059 0.01649 -0.00111 -0.00441 AFIX 3 H11A 2 0.181074 0.484069 0.689890 11.00000 -1.20000 H11B 2 0.031824 0.546309 0.649810 11.00000 -1.20000 AFIX 0 O12 4 0.291427 -0.007350 0.814125 11.00000 0.03958 0.15671 = 0.06449 0.07169 0.00208 -0.01836 AFIX 3 H12B 2 0.325428 0.015950 0.767945 11.00000 -1.20000 AFIX 0 PART 1 O13 4 -0.333947 -0.238903 0.720500 21.00000 0.10761 0.07009 = 0.04824 -0.00608 0.02090 0.02042 AFIX 3 H13A 2 -0.303101 -0.305219 0.696203 20.91500 -1.20000 H13B 2 -0.414897 -0.171963 0.706080 20.91500 -1.20000 AFIX 0 PART 2 O13A 4 -0.622383 -0.147820 0.711187 -21.00000 0.10761 0.07009 = 0.04824 -0.00608 0.02090 0.02042 PART 0 O14 4 -0.114757 -0.110941 0.726907 10.50000 0.05066 0.04169 = 0.02979 -0.00649 -0.00471 0.00336 PART 1 O15 4 0.191172 0.439094 1.183651 10.28000 0.03564 0.11111 = 0.04137 -0.05462 -0.01083 0.02028 PART 2 O15A 4 0.189236 0.396898 1.153466 10.22000 0.01996 0.05735 = 0.05153 0.00837 0.00668 -0.00033 HKLF 4 REM JTM363_0m in P-1 REM R1 = 0.0573 for 6062 Fo > 4sig(Fo) and 0.0666 for all 7136 data REM 446 parameters refined using 0 restraints END WGHT 0.0866 1.5229 REM Highest difference peak 1.333, deepest hole -1.182, 1-sigma level 0.090 Q1 1 -0.2394 -0.2106 0.7499 11.00000 0.05 1.33 Q2 1 0.2838 0.0611 0.8371 11.00000 0.05 1.30 Q3 1 -0.1898 -0.1625 0.7298 11.00000 0.05 0.72 Q4 1 -0.2751 -0.2975 0.7603 11.00000 0.05 0.69 Q5 1 0.1820 0.0295 0.8308 11.00000 0.05 0.65 ; _database_code_depnum_ccdc_archive 'CCDC 940544' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Cd N2 O10, 2(C13, H11 N2), 4(H2 O)' _chemical_formula_sum 'C40 H36 Cd N6 O14' _chemical_formula_weight 937.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 12.0580(12) _cell_length_b 13.9067(14) _cell_length_c 14.0032(15) _cell_angle_alpha 111.967(1) _cell_angle_beta 115.126(1) _cell_angle_gamma 94.003(2) _cell_volume 1897.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9845 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 29.10 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7218 _exptl_absorpt_correction_T_max 0.8716 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 7 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33817 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 29.14 _reflns_number_total 9618 _reflns_number_gt 9056 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2012)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2008)' _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. H-atoms attached to carbon were placed in calculated positions (C---H = 0.95 \%A) while those attached to nitrogen and oxygen were placed in locations derived from a difference map and their coordinates adjusted to give N---H and O---H = 0.91 and o.84 \%A, respectively. All were included as riding contributions with isotropic displacement parameters 1.2 times those of the attached atoms. ; _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^)+(0.0428P)^2^+1.7530P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9618 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.810385(12) 0.985613(10) 0.685389(11) 0.01486(5) Uani 1 1 d . . . O1 O 0.72118(13) 0.91567(11) 0.77200(12) 0.0185(3) Uani 1 1 d . . . O2 O 0.75988(14) 0.84547(12) 0.89907(14) 0.0223(3) Uani 1 1 d . . . O3 O 0.99470(13) 1.00728(11) 0.66772(12) 0.0178(3) Uani 1 1 d . . . O4 O 1.18260(14) 0.97039(12) 0.71286(13) 0.0200(3) Uani 1 1 d . . . O5 O 1.22795(14) 0.84466(12) 1.02338(12) 0.0213(3) Uani 1 1 d . . . H5O H 1.2082 0.8352 1.0706 0.026 Uiso 1 1 d R . . O6 O 0.82469(13) 1.15839(11) 0.81671(11) 0.0172(3) Uani 1 1 d . . . O7 O 0.76020(15) 1.30712(11) 0.82489(12) 0.0203(3) Uani 1 1 d . . . O8 O 0.70764(14) 0.86150(10) 0.48606(13) 0.0194(3) Uani 1 1 d . . . O9 O 0.60291(15) 0.84823(11) 0.30381(13) 0.0226(3) Uani 1 1 d . . . O10 O 0.49608(13) 1.21522(11) 0.39409(12) 0.0188(3) Uani 1 1 d . . . H10O H 0.4319 1.1711 0.3307 0.023 Uiso 1 1 d R . . N1 N 0.95151(15) 0.92530(12) 0.79466(13) 0.0132(3) Uani 1 1 d . . . N2 N 0.69584(14) 1.06238(12) 0.58246(13) 0.0124(3) Uani 1 1 d . . . C1 C 0.79145(18) 0.88198(14) 0.84369(16) 0.0157(3) Uani 1 1 d . . . C2 C 0.92534(17) 0.88864(13) 0.86064(15) 0.0131(3) Uani 1 1 d . . . C3 C 1.01356(18) 0.85907(14) 0.93875(16) 0.0151(3) Uani 1 1 d . . . H3 H 0.9923 0.8323 0.9838 0.018 Uiso 1 1 calc R . . C4 C 1.13579(18) 0.86979(14) 0.94971(16) 0.0153(3) Uani 1 1 d . . . C5 C 1.16204(18) 0.90704(15) 0.87919(16) 0.0155(3) Uani 1 1 d . . . H5 H 1.2434 0.9139 0.8839 0.019 Uiso 1 1 calc R . . C6 C 1.06729(17) 0.93345(14) 0.80295(15) 0.0133(3) Uani 1 1 d . . . C7 C 1.08440(18) 0.97378(14) 0.72160(16) 0.0152(3) Uani 1 1 d . . . C8 C 0.76651(17) 1.21618(14) 0.77070(16) 0.0142(3) Uani 1 1 d . . . C9 C 0.69542(17) 1.16482(14) 0.63677(15) 0.0126(3) Uani 1 1 d . . . C10 C 0.63097(17) 1.21848(14) 0.57546(16) 0.0141(3) Uani 1 1 d . . . H10 H 0.6341 1.2917 0.6158 0.017 Uiso 1 1 calc R . . C11 C 0.56057(17) 1.16278(14) 0.45224(16) 0.0143(3) Uani 1 1 d . . . C12 C 0.56131(17) 1.05562(14) 0.39550(16) 0.0147(3) Uani 1 1 d . . . H12 H 0.5146 1.0160 0.3120 0.018 Uiso 1 1 calc R . . C13 C 0.63206(17) 1.00925(14) 0.46452(16) 0.0129(3) Uani 1 1 d . . . C14 C 0.64805(17) 0.89641(14) 0.41285(17) 0.0159(3) Uani 1 1 d . . . N3 N 0.64597(15) 0.65071(12) 0.19353(14) 0.0149(3) Uani 1 1 d . . . H3N H 0.6428 0.7174 0.2360 0.018 Uiso 1 1 d R . . N4 N 0.66381(16) 0.35185(13) -0.00694(14) 0.0175(3) Uani 1 1 d . . . H4A H 0.6172 0.2888 -0.0214 0.021 Uiso 1 1 d R . . H4B H 0.7077 0.3452 -0.0474 0.021 Uiso 1 1 d R . . C15 C 0.57807(17) 0.56080(14) 0.18196(15) 0.0142(3) Uani 1 1 d . . . C16 C 0.49841(19) 0.57277(16) 0.23383(17) 0.0185(4) Uani 1 1 d . . . H16 H 0.4934 0.6424 0.2764 0.022 Uiso 1 1 calc R . . C17 C 0.4285(2) 0.48293(17) 0.22202(18) 0.0214(4) Uani 1 1 d . . . H17 H 0.3739 0.4907 0.2557 0.026 Uiso 1 1 calc R . . C18 C 0.4361(2) 0.37901(16) 0.16064(18) 0.0217(4) Uani 1 1 d . . . H18 H 0.3884 0.3178 0.1548 0.026 Uiso 1 1 calc R . . C19 C 0.51245(19) 0.36649(15) 0.10952(17) 0.0185(4) Uani 1 1 d . . . H19 H 0.5170 0.2963 0.0681 0.022 Uiso 1 1 calc R . . C20 C 0.58499(17) 0.45726(14) 0.11777(15) 0.0139(3) Uani 1 1 d . . . C21 C 0.66172(17) 0.44774(14) 0.06072(15) 0.0137(3) Uani 1 1 d . . . C22 C 0.73581(17) 0.54492(14) 0.07889(15) 0.0137(3) Uani 1 1 d . . . C23 C 0.82063(18) 0.54475(15) 0.03305(16) 0.0174(4) Uani 1 1 d . . . H23 H 0.8292 0.4782 -0.0126 0.021 Uiso 1 1 calc R . . C24 C 0.89039(19) 0.63962(16) 0.05387(17) 0.0207(4) Uani 1 1 d . . . H24 H 0.9471 0.6384 0.0230 0.025 Uiso 1 1 calc R . . C25 C 0.8782(2) 0.73914(16) 0.12108(18) 0.0215(4) Uani 1 1 d . . . H25 H 0.9267 0.8044 0.1348 0.026 Uiso 1 1 calc R . . C26 C 0.79732(19) 0.74276(15) 0.16680(17) 0.0187(4) Uani 1 1 d . . . H26 H 0.7896 0.8101 0.2117 0.022 Uiso 1 1 calc R . . C27 C 0.72553(17) 0.64579(14) 0.14683(15) 0.0144(3) Uani 1 1 d . . . N5 N 0.81808(15) 0.41808(12) 0.36197(14) 0.0148(3) Uani 1 1 d . . . H5N H 0.7928 0.3450 0.3309 0.018 Uiso 1 1 d R . . N6 N 0.89551(16) 0.74563(13) 0.46417(15) 0.0176(3) Uani 1 1 d . . . H6A H 0.8421 0.7805 0.4846 0.021 Uiso 1 1 d R . . H6B H 0.9484 0.7822 0.4508 0.021 Uiso 1 1 d R . . C28 C 0.89948(17) 0.46268(14) 0.33639(15) 0.0137(3) Uani 1 1 d . . . C29 C 0.94882(19) 0.39481(15) 0.26968(17) 0.0183(4) Uani 1 1 d . . . H29 H 0.9261 0.3193 0.2444 0.022 Uiso 1 1 calc R . . C30 C 1.02905(19) 0.43802(16) 0.24165(17) 0.0196(4) Uani 1 1 d . . . H30 H 1.0616 0.3921 0.1967 0.023 Uiso 1 1 calc R . . C31 C 1.06397(19) 0.54989(16) 0.27872(18) 0.0193(4) Uani 1 1 d . . . H31 H 1.1196 0.5789 0.2585 0.023 Uiso 1 1 calc R . . C32 C 1.01780(18) 0.61712(15) 0.34408(16) 0.0167(3) Uani 1 1 d . . . H32 H 1.0426 0.6925 0.3694 0.020 Uiso 1 1 calc R . . C33 C 0.93364(17) 0.57533(14) 0.37420(15) 0.0136(3) Uani 1 1 d . . . C34 C 0.87678(17) 0.64169(14) 0.43656(16) 0.0140(3) Uani 1 1 d . . . C35 C 0.79787(17) 0.59189(14) 0.46826(16) 0.0140(3) Uani 1 1 d . . . C36 C 0.74898(19) 0.65186(15) 0.54099(17) 0.0176(4) Uani 1 1 d . . . H36 H 0.7672 0.7279 0.5693 0.021 Uiso 1 1 calc R . . C37 C 0.6763(2) 0.60212(16) 0.57081(18) 0.0200(4) Uani 1 1 d . . . H37 H 0.6459 0.6435 0.6208 0.024 Uiso 1 1 calc R . . C38 C 0.64655(19) 0.48862(16) 0.52701(18) 0.0187(4) Uani 1 1 d . . . H38 H 0.5945 0.4542 0.5467 0.022 Uiso 1 1 calc R . . C39 C 0.69157(18) 0.42784(15) 0.45678(17) 0.0167(3) Uani 1 1 d . . . H39 H 0.6703 0.3517 0.4273 0.020 Uiso 1 1 calc R . . C40 C 0.76989(17) 0.47915(14) 0.42849(15) 0.0138(3) Uani 1 1 d . . . O11 O 0.92243(14) 0.11661(11) 0.53436(12) 0.0192(3) Uani 1 1 d . . . H11A H 0.8796 0.0767 0.4614 0.023 Uiso 1 1 d R . . H11B H 0.9488 0.0796 0.5706 0.023 Uiso 1 1 d R . . O12 O 0.48973(16) 0.12081(14) 0.91444(14) 0.0332(4) Uani 1 1 d . . . H12A H 0.5263 0.0715 0.9142 0.040 Uiso 1 1 d R . . H12B H 0.4260 0.1039 0.8487 0.040 Uiso 1 1 d R . . O13 O 0.29448(14) 0.79939(11) 0.71764(14) 0.0225(3) Uani 1 1 d . . . H13A H 0.3705 0.8260 0.7719 0.027 Uiso 1 1 d R . . H13B H 0.2595 0.8481 0.7092 0.027 Uiso 1 1 d R . . O14 O 0.54628(15) 0.91004(14) 0.90662(15) 0.0287(3) Uani 1 1 d . . . H14A H 0.6082 0.8887 0.9022 0.034 Uiso 1 1 d R . . H14B H 0.5494 0.9018 0.9642 0.034 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 Cd1 0.01854(8) 0.01455(7) 0.01465(7) 0.00882(5) 0.00819(6) 0.00815(5) O1 0.0164(6) 0.0207(6) 0.0218(7) 0.0120(6) 0.0096(5) 0.0066(5) O2 0.0248(7) 0.0248(7) 0.0280(7) 0.0161(6) 0.0180(6) 0.0071(6) O3 0.0221(7) 0.0201(6) 0.0190(6) 0.0140(5) 0.0116(6) 0.0087(5) O4 0.0228(7) 0.0243(7) 0.0233(7) 0.0150(6) 0.0155(6) 0.0095(6) O5 0.0269(7) 0.0324(8) 0.0176(6) 0.0177(6) 0.0144(6) 0.0184(6) O6 0.0232(7) 0.0168(6) 0.0123(6) 0.0069(5) 0.0088(5) 0.0063(5) O7 0.0305(8) 0.0145(6) 0.0156(6) 0.0032(5) 0.0137(6) 0.0070(6) O8 0.0232(7) 0.0114(6) 0.0237(7) 0.0061(5) 0.0125(6) 0.0082(5) O9 0.0269(7) 0.0166(6) 0.0175(7) 0.0011(5) 0.0105(6) 0.0076(6) O10 0.0197(7) 0.0151(6) 0.0178(6) 0.0085(5) 0.0051(5) 0.0051(5) N1 0.0174(7) 0.0120(6) 0.0126(7) 0.0063(6) 0.0083(6) 0.0053(6) N2 0.0158(7) 0.0104(6) 0.0137(7) 0.0050(6) 0.0097(6) 0.0042(5) C1 0.0182(8) 0.0118(7) 0.0160(8) 0.0045(6) 0.0091(7) 0.0028(7) C2 0.0180(8) 0.0096(7) 0.0123(7) 0.0039(6) 0.0086(7) 0.0032(6) C3 0.0217(9) 0.0127(8) 0.0136(8) 0.0062(6) 0.0105(7) 0.0052(7) C4 0.0210(9) 0.0147(8) 0.0119(7) 0.0060(6) 0.0088(7) 0.0089(7) C5 0.0187(8) 0.0156(8) 0.0128(8) 0.0058(7) 0.0083(7) 0.0065(7) C6 0.0186(8) 0.0111(7) 0.0112(7) 0.0047(6) 0.0083(7) 0.0042(6) C7 0.0207(9) 0.0123(7) 0.0144(8) 0.0063(6) 0.0098(7) 0.0039(7) C8 0.0172(8) 0.0129(8) 0.0136(8) 0.0046(6) 0.0099(7) 0.0023(6) C9 0.0149(8) 0.0113(7) 0.0136(8) 0.0043(6) 0.0098(7) 0.0033(6) C10 0.0173(8) 0.0106(7) 0.0154(8) 0.0047(6) 0.0097(7) 0.0042(6) C11 0.0133(8) 0.0141(8) 0.0167(8) 0.0075(7) 0.0079(7) 0.0036(6) C12 0.0151(8) 0.0145(8) 0.0131(8) 0.0043(6) 0.0073(7) 0.0035(7) C13 0.0141(8) 0.0105(7) 0.0147(8) 0.0037(6) 0.0092(7) 0.0028(6) C14 0.0147(8) 0.0116(7) 0.0201(9) 0.0036(7) 0.0102(7) 0.0044(6) N3 0.0167(7) 0.0113(7) 0.0140(7) 0.0018(6) 0.0086(6) 0.0035(6) N4 0.0229(8) 0.0135(7) 0.0180(7) 0.0052(6) 0.0128(7) 0.0072(6) C15 0.0142(8) 0.0149(8) 0.0107(7) 0.0045(6) 0.0050(6) 0.0037(6) C16 0.0207(9) 0.0194(9) 0.0154(8) 0.0051(7) 0.0110(7) 0.0062(7) C17 0.0231(9) 0.0261(10) 0.0183(9) 0.0091(8) 0.0138(8) 0.0056(8) C18 0.0250(10) 0.0202(9) 0.0211(9) 0.0104(8) 0.0118(8) 0.0024(8) C19 0.0226(9) 0.0151(8) 0.0174(8) 0.0070(7) 0.0098(7) 0.0045(7) C20 0.0145(8) 0.0146(8) 0.0110(7) 0.0053(6) 0.0050(6) 0.0053(6) C21 0.0145(8) 0.0141(8) 0.0099(7) 0.0048(6) 0.0040(6) 0.0058(6) C22 0.0135(8) 0.0141(8) 0.0107(7) 0.0038(6) 0.0050(6) 0.0041(6) C23 0.0176(8) 0.0181(8) 0.0143(8) 0.0040(7) 0.0088(7) 0.0056(7) C24 0.0212(9) 0.0219(9) 0.0178(9) 0.0046(7) 0.0127(8) 0.0033(8) C25 0.0217(9) 0.0174(9) 0.0205(9) 0.0041(7) 0.0109(8) -0.0008(7) C26 0.0212(9) 0.0133(8) 0.0170(8) 0.0025(7) 0.0097(7) 0.0016(7) C27 0.0142(8) 0.0146(8) 0.0120(7) 0.0041(6) 0.0060(7) 0.0035(7) N5 0.0185(7) 0.0103(6) 0.0151(7) 0.0047(6) 0.0086(6) 0.0041(6) N6 0.0205(8) 0.0130(7) 0.0239(8) 0.0089(6) 0.0135(7) 0.0071(6) C28 0.0142(8) 0.0136(8) 0.0114(7) 0.0051(6) 0.0049(6) 0.0049(6) C29 0.0223(9) 0.0135(8) 0.0173(8) 0.0044(7) 0.0101(7) 0.0063(7) C30 0.0216(9) 0.0194(9) 0.0186(9) 0.0061(7) 0.0121(8) 0.0084(7) C31 0.0181(9) 0.0205(9) 0.0208(9) 0.0092(7) 0.0105(7) 0.0056(7) C32 0.0163(8) 0.0148(8) 0.0176(8) 0.0074(7) 0.0070(7) 0.0040(7) C33 0.0150(8) 0.0126(8) 0.0123(7) 0.0059(6) 0.0054(6) 0.0051(6) C34 0.0138(8) 0.0132(8) 0.0132(8) 0.0060(6) 0.0049(6) 0.0048(6) C35 0.0149(8) 0.0127(8) 0.0146(8) 0.0070(6) 0.0063(7) 0.0056(6) C36 0.0220(9) 0.0133(8) 0.0195(9) 0.0072(7) 0.0113(7) 0.0084(7) C37 0.0242(9) 0.0187(9) 0.0235(9) 0.0099(8) 0.0158(8) 0.0113(8) C38 0.0200(9) 0.0198(9) 0.0217(9) 0.0121(8) 0.0121(8) 0.0075(7) C39 0.0189(9) 0.0143(8) 0.0182(8) 0.0085(7) 0.0088(7) 0.0051(7) C40 0.0156(8) 0.0131(8) 0.0128(8) 0.0061(6) 0.0063(7) 0.0061(6) O11 0.0276(7) 0.0177(6) 0.0187(6) 0.0118(5) 0.0133(6) 0.0076(6) O12 0.0327(9) 0.0385(9) 0.0200(7) 0.0066(7) 0.0095(7) 0.0224(8) O13 0.0234(7) 0.0149(6) 0.0296(8) 0.0082(6) 0.0145(6) 0.0067(6) O14 0.0247(8) 0.0343(8) 0.0311(8) 0.0139(7) 0.0170(7) 0.0113(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.1889(16) . ? Cd1 N1 2.2111(16) . ? Cd1 O1 2.3278(14) . ? Cd1 O8 2.3378(14) . ? Cd1 O3 2.3496(14) . ? Cd1 O6 2.3562(13) . ? O1 C1 1.277(2) . ? O2 C1 1.234(2) . ? O3 C7 1.264(2) . ? O4 C7 1.243(2) . ? O5 C4 1.331(2) . ? O5 H5O 0.8400 . ? O6 C8 1.279(2) . ? O7 C8 1.235(2) . ? O8 C14 1.264(2) . ? O9 C14 1.247(2) . ? O10 C11 1.336(2) . ? O10 H10O 0.8400 . ? N1 C2 1.338(2) . ? N1 C6 1.344(2) . ? N2 C13 1.339(2) . ? N2 C9 1.342(2) . ? C1 C2 1.519(3) . ? C2 C3 1.381(3) . ? C3 C4 1.406(3) . ? C3 H3 0.9500 . ? C4 C5 1.403(3) . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 C7 1.522(2) . ? C8 C9 1.520(2) . ? C9 C10 1.375(3) . ? C10 C11 1.401(2) . ? C10 H10 0.9500 . ? C11 C12 1.405(2) . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.528(2) . ? N3 C15 1.361(2) . ? N3 C27 1.364(2) . ? N3 H3N 0.9099 . ? N4 C21 1.325(2) . ? N4 H4A 0.9098 . ? N4 H4B 0.9117 . ? C15 C20 1.414(2) . ? C15 C16 1.415(3) . ? C16 C17 1.371(3) . ? C16 H16 0.9500 . ? C17 C18 1.412(3) . ? C17 H17 0.9500 . ? C18 C19 1.370(3) . ? C18 H18 0.9500 . ? C19 C20 1.422(3) . ? C19 H19 0.9500 . ? C20 C21 1.441(3) . ? C21 C22 1.439(3) . ? C22 C27 1.419(2) . ? C22 C23 1.419(3) . ? C23 C24 1.372(3) . ? C23 H23 0.9500 . ? C24 C25 1.412(3) . ? C24 H24 0.9500 . ? C25 C26 1.370(3) . ? C25 H25 0.9500 . ? C26 C27 1.413(3) . ? C26 H26 0.9500 . ? N5 C28 1.362(2) . ? N5 C40 1.365(2) . ? N5 H5N 0.9103 . ? N6 C34 1.324(2) . ? N6 H6A 0.9100 . ? N6 H6B 0.9105 . ? C28 C33 1.417(2) . ? C28 C29 1.417(2) . ? C29 C30 1.367(3) . ? C29 H29 0.9500 . ? C30 C31 1.409(3) . ? C30 H30 0.9500 . ? C31 C32 1.374(3) . ? C31 H31 0.9500 . ? C32 C33 1.418(3) . ? C32 H32 0.9500 . ? C33 C34 1.442(2) . ? C34 C35 1.442(3) . ? C35 C40 1.413(2) . ? C35 C36 1.422(3) . ? C36 C37 1.365(3) . ? C36 H36 0.9500 . ? C37 C38 1.416(3) . ? C37 H37 0.9500 . ? C38 C39 1.368(3) . ? C38 H38 0.9500 . ? C39 C40 1.412(3) . ? C39 H39 0.9500 . ? O11 H11A 0.8402 . ? O11 H11B 0.8398 . ? O12 H12A 0.8402 . ? O12 H12B 0.8403 . ? O13 H13A 0.8400 . ? O13 H13B 0.8419 . ? O14 H14A 0.8402 . ? O14 H14B 0.8411 . ? 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 Cd1 N1 171.24(6) . . ? N2 Cd1 O1 116.46(5) . . ? N1 Cd1 O1 71.26(5) . . ? N2 Cd1 O8 71.71(5) . . ? N1 Cd1 O8 111.15(5) . . ? O1 Cd1 O8 105.53(5) . . ? N2 Cd1 O3 101.80(5) . . ? N1 Cd1 O3 70.55(5) . . ? O1 Cd1 O3 141.74(5) . . ? O8 Cd1 O3 86.14(5) . . ? N2 Cd1 O6 71.45(5) . . ? N1 Cd1 O6 105.85(5) . . ? O1 Cd1 O6 87.60(5) . . ? O8 Cd1 O6 142.96(5) . . ? O3 Cd1 O6 104.93(5) . . ? C1 O1 Cd1 117.76(12) . . ? C7 O3 Cd1 118.13(12) . . ? C4 O5 H5O 110.8 . . ? C8 O6 Cd1 116.71(11) . . ? C14 O8 Cd1 116.60(11) . . ? C11 O10 H10O 109.7 . . ? C2 N1 C6 119.60(16) . . ? C2 N1 Cd1 119.69(12) . . ? C6 N1 Cd1 120.48(12) . . ? C13 N2 C9 119.80(16) . . ? C13 N2 Cd1 119.90(12) . . ? C9 N2 Cd1 120.18(12) . . ? O2 C1 O1 125.79(18) . . ? O2 C1 C2 118.44(17) . . ? O1 C1 C2 115.77(16) . . ? N1 C2 C3 122.52(17) . . ? N1 C2 C1 115.21(16) . . ? C3 C2 C1 122.27(16) . . ? C2 C3 C4 118.09(17) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? O5 C4 C5 118.18(17) . . ? O5 C4 C3 122.77(17) . . ? C5 C4 C3 119.05(17) . . ? C6 C5 C4 118.54(17) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 122.18(17) . . ? N1 C6 C7 114.63(16) . . ? C5 C6 C7 123.19(17) . . ? O4 C7 O3 125.90(17) . . ? O4 C7 C6 118.43(17) . . ? O3 C7 C6 115.67(16) . . ? O7 C8 O6 126.02(17) . . ? O7 C8 C9 118.09(17) . . ? O6 C8 C9 115.85(15) . . ? N2 C9 C10 122.29(16) . . ? N2 C9 C8 115.53(16) . . ? C10 C9 C8 122.14(16) . . ? C9 C10 C11 118.50(16) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? O10 C11 C10 117.80(16) . . ? O10 C11 C12 123.07(16) . . ? C10 C11 C12 119.12(17) . . ? C13 C12 C11 118.23(16) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? N2 C13 C12 122.01(16) . . ? N2 C13 C14 114.89(16) . . ? C12 C13 C14 123.05(16) . . ? O9 C14 O8 126.32(17) . . ? O9 C14 C13 117.54(17) . . ? O8 C14 C13 116.14(16) . . ? C15 N3 C27 122.05(16) . . ? C15 N3 H3N 120.9 . . ? C27 N3 H3N 117.0 . . ? C21 N4 H4A 123.2 . . ? C21 N4 H4B 121.2 . . ? H4A N4 H4B 115.3 . . ? N3 C15 C20 120.88(17) . . ? N3 C15 C16 118.62(16) . . ? C20 C15 C16 120.49(17) . . ? C17 C16 C15 119.34(18) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.12(18) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 119.99(18) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.80(18) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C15 C20 C19 118.23(17) . . ? C15 C20 C21 118.94(17) . . ? C19 C20 C21 122.81(17) . . ? N4 C21 C22 120.83(17) . . ? N4 C21 C20 120.81(17) . . ? C22 C21 C20 118.35(16) . . ? C27 C22 C23 118.15(17) . . ? C27 C22 C21 118.98(16) . . ? C23 C22 C21 122.87(16) . . ? C24 C23 C22 120.75(17) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.23(18) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.81(18) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.62(18) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N3 C27 C26 118.94(16) . . ? N3 C27 C22 120.62(17) . . ? C26 C27 C22 120.44(17) . . ? C28 N5 C40 122.13(16) . . ? C28 N5 H5N 118.4 . . ? C40 N5 H5N 119.4 . . ? C34 N6 H6A 118.6 . . ? C34 N6 H6B 124.1 . . ? H6A N6 H6B 116.2 . . ? N5 C28 C33 120.86(16) . . ? N5 C28 C29 119.21(16) . . ? C33 C28 C29 119.93(17) . . ? C30 C29 C28 119.98(17) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.73(18) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 120.18(18) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 120.79(17) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C28 C33 C32 118.38(16) . . ? C28 C33 C34 118.69(16) . . ? C32 C33 C34 122.85(16) . . ? N6 C34 C33 121.41(17) . . ? N6 C34 C35 120.33(17) . . ? C33 C34 C35 118.26(16) . . ? C40 C35 C36 117.99(17) . . ? C40 C35 C34 119.21(16) . . ? C36 C35 C34 122.78(16) . . ? C37 C36 C35 121.14(17) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 119.78(18) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 120.98(18) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 119.49(17) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? N5 C40 C39 118.95(16) . . ? N5 C40 C35 120.50(17) . . ? C39 C40 C35 120.55(17) . . ? H11A O11 H11B 110.3 . . ? H12A O12 H12B 112.4 . . ? H13A O13 H13B 111.0 . . ? H14A O14 H14B 102.2 . . ? 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 O5 H5O O6 0.84 1.76 2.587(2) 169 2_777 O10 H10O O1 0.84 1.75 2.565(2) 162 2_676 N3 H3N O9 0.91 1.91 2.812(2) 169 . N4 H4A O12 0.91 2.32 3.224(3) 172 1_554 N4 H4B O7 0.91 2.04 2.935(2) 165 1_544 N5 H5N O13 0.91 1.92 2.802(2) 163 2_666 N6 H6A O8 0.91 2.04 2.924(2) 163 . N6 H6B O11 0.91 1.91 2.799(2) 165 2_766 O11 H11A O4 0.84 2.03 2.825(2) 157 2_766 O11 H11B O3 0.84 1.90 2.7360(19) 170 1_545 O12 H12A O14 0.84 2.24 3.028(2) 156 1_545 O12 H12B O9 0.84 2.36 2.988(2) 132 2_666 O13 H13A O14 0.84 2.01 2.840(2) 172 . O13 H13B O4 0.84 1.99 2.823(2) 172 1_455 O14 H14A O2 0.84 1.98 2.817(2) 177 . O14 H14B O12 0.84 2.07 2.890(3) 166 2_667 _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.841 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.115 _iucr_refine_instructions_details ; TITL JTM377_0m in P-1 CELL 0.71073 12.0580 13.9067 14.0032 111.967 115.126 94.003 ZERR 2.00 0.0012 0.0014 0.0015 0.001 0.001 0.002 LATT 1 SFAC C H N O Cd UNIT 80 72 12 28 2 L.S. 6 ACTA 55.5 BOND $H FMAP 2 PLAN 5 EQIV $1 -x+2, -y+2, -z+2 EQIV $2 -x+1, -y+2, -z+1 EQIV $3 x, y, z-1 EQIV $4 x, y-1, z-1 EQIV $5 -x+1, -y+1, -z+1 EQIV $6 -x+2, -y+1, -z+1 EQIV $7 x, y-1, z EQIV $8 x-1, y, z EQIV $9 -x+1, -y+1, -z+2 HTAB O5 O6_$1 HTAB O10 O1_$2 HTAB N3 O9 HTAB N4 O12_$3 HTAB N4 O7_$4 HTAB N5 O13_$5 HTAB N6 O8 HTAB N6 O11_$6 HTAB O11 O4_$6 HTAB O11 O3_$7 HTAB O12 O14_$7 HTAB O12 O9_$5 HTAB O13 O14 HTAB O13 O4_$8 HTAB O14 O2 HTAB O14 O12_$9 MPLA Cd1 O1 O3 N1 MPLA Cd1 O6 O8 N2 SIZE 0.215 0.227 0.311 TEMP -173 WGHT 0.042800 1.753000 FVAR 0.13818 CD1 5 0.810385 0.985613 0.685389 11.00000 0.01854 0.01455 = 0.01465 0.00882 0.00819 0.00815 O1 4 0.721185 0.915668 0.772003 11.00000 0.01635 0.02073 = 0.02177 0.01205 0.00963 0.00661 O2 4 0.759879 0.845466 0.899066 11.00000 0.02477 0.02475 = 0.02799 0.01606 0.01797 0.00708 O3 4 0.994702 1.007282 0.667723 11.00000 0.02210 0.02014 = 0.01900 0.01396 0.01158 0.00871 O4 4 1.182605 0.970386 0.712857 11.00000 0.02279 0.02432 = 0.02326 0.01502 0.01550 0.00954 O5 4 1.227951 0.844660 1.023377 11.00000 0.02688 0.03240 = 0.01759 0.01766 0.01440 0.01839 AFIX 3 H5O 2 1.208201 0.835212 1.070596 11.00000 -1.20000 AFIX 0 O6 4 0.824687 1.158393 0.816707 11.00000 0.02320 0.01683 = 0.01229 0.00690 0.00881 0.00625 O7 4 0.760196 1.307123 0.824892 11.00000 0.03045 0.01449 = 0.01558 0.00320 0.01371 0.00700 O8 4 0.707641 0.861500 0.486061 11.00000 0.02315 0.01140 = 0.02366 0.00609 0.01246 0.00824 O9 4 0.602912 0.848232 0.303811 11.00000 0.02688 0.01662 = 0.01750 0.00106 0.01054 0.00758 O10 4 0.496082 1.215221 0.394095 11.00000 0.01973 0.01510 = 0.01782 0.00851 0.00508 0.00514 AFIX 3 H10O 2 0.431909 1.171131 0.330732 11.00000 -1.20000 AFIX 0 N1 3 0.951515 0.925298 0.794661 11.00000 0.01736 0.01203 = 0.01255 0.00631 0.00826 0.00529 N2 3 0.695841 1.062385 0.582462 11.00000 0.01581 0.01041 = 0.01368 0.00500 0.00965 0.00424 C1 1 0.791448 0.881977 0.843689 11.00000 0.01818 0.01176 = 0.01600 0.00450 0.00907 0.00278 C2 1 0.925342 0.888635 0.860644 11.00000 0.01796 0.00955 = 0.01225 0.00386 0.00859 0.00323 C3 1 1.013562 0.859071 0.938752 11.00000 0.02170 0.01271 = 0.01358 0.00616 0.01046 0.00525 AFIX 43 H3 2 0.992310 0.832261 0.983800 11.00000 -1.20000 AFIX 0 C4 1 1.135786 0.869785 0.949712 11.00000 0.02104 0.01472 = 0.01195 0.00603 0.00882 0.00886 C5 1 1.162038 0.907038 0.879192 11.00000 0.01872 0.01556 = 0.01278 0.00576 0.00834 0.00645 AFIX 43 H5 2 1.243388 0.913883 0.883943 11.00000 -1.20000 AFIX 0 C6 1 1.067288 0.933453 0.802950 11.00000 0.01861 0.01111 = 0.01124 0.00469 0.00826 0.00424 C7 1 1.084403 0.973776 0.721601 11.00000 0.02071 0.01227 = 0.01439 0.00627 0.00978 0.00386 C8 1 0.766513 1.216180 0.770696 11.00000 0.01721 0.01287 = 0.01361 0.00458 0.00990 0.00227 C9 1 0.695420 1.164815 0.636766 11.00000 0.01494 0.01133 = 0.01363 0.00426 0.00982 0.00332 C10 1 0.630975 1.218483 0.575461 11.00000 0.01731 0.01059 = 0.01535 0.00474 0.00969 0.00421 AFIX 43 H10 2 0.634136 1.291671 0.615769 11.00000 -1.20000 AFIX 0 C11 1 0.560570 1.162782 0.452240 11.00000 0.01333 0.01408 = 0.01669 0.00750 0.00790 0.00358 C12 1 0.561306 1.055620 0.395497 11.00000 0.01508 0.01445 = 0.01305 0.00433 0.00727 0.00350 AFIX 43 H12 2 0.514551 1.016006 0.312043 11.00000 -1.20000 AFIX 0 C13 1 0.632060 1.009250 0.464525 11.00000 0.01407 0.01049 = 0.01471 0.00370 0.00916 0.00282 C14 1 0.648048 0.896409 0.412849 11.00000 0.01467 0.01162 = 0.02012 0.00364 0.01020 0.00441 N3 3 0.645971 0.650709 0.193528 11.00000 0.01672 0.01132 = 0.01398 0.00182 0.00856 0.00352 AFIX 3 H3N 2 0.642785 0.717425 0.236037 11.00000 -1.20000 AFIX 0 N4 3 0.663811 0.351845 -0.006941 11.00000 0.02292 0.01347 = 0.01800 0.00520 0.01276 0.00715 AFIX 3 H4A 2 0.617195 0.288768 -0.021433 11.00000 -1.20000 H4B 2 0.707669 0.345209 -0.047398 11.00000 -1.20000 AFIX 0 C15 1 0.578072 0.560801 0.181963 11.00000 0.01423 0.01488 = 0.01074 0.00449 0.00498 0.00369 C16 1 0.498410 0.572766 0.233827 11.00000 0.02066 0.01938 = 0.01539 0.00513 0.01095 0.00623 AFIX 43 H16 2 0.493442 0.642361 0.276406 11.00000 -1.20000 AFIX 0 C17 1 0.428470 0.482928 0.222021 11.00000 0.02311 0.02610 = 0.01831 0.00907 0.01380 0.00558 AFIX 43 H17 2 0.373915 0.490740 0.255722 11.00000 -1.20000 AFIX 0 C18 1 0.436139 0.379012 0.160637 11.00000 0.02500 0.02019 = 0.02114 0.01040 0.01179 0.00236 AFIX 43 H18 2 0.388400 0.317765 0.154762 11.00000 -1.20000 AFIX 0 C19 1 0.512454 0.366488 0.109523 11.00000 0.02262 0.01511 = 0.01738 0.00703 0.00980 0.00446 AFIX 43 H19 2 0.516965 0.296321 0.068076 11.00000 -1.20000 AFIX 0 C20 1 0.584991 0.457263 0.117770 11.00000 0.01451 0.01463 = 0.01104 0.00529 0.00505 0.00533 C21 1 0.661722 0.447742 0.060721 11.00000 0.01447 0.01410 = 0.00994 0.00483 0.00405 0.00582 C22 1 0.735808 0.544921 0.078888 11.00000 0.01355 0.01414 = 0.01069 0.00383 0.00502 0.00410 C23 1 0.820628 0.544749 0.033052 11.00000 0.01761 0.01814 = 0.01432 0.00399 0.00883 0.00558 AFIX 43 H23 2 0.829184 0.478184 -0.012564 11.00000 -1.20000 AFIX 0 C24 1 0.890394 0.639616 0.053873 11.00000 0.02122 0.02190 = 0.01780 0.00459 0.01271 0.00333 AFIX 43 H24 2 0.947109 0.638354 0.022972 11.00000 -1.20000 AFIX 0 C25 1 0.878195 0.739138 0.121081 11.00000 0.02174 0.01743 = 0.02045 0.00408 0.01088 -0.00075 AFIX 43 H25 2 0.926674 0.804379 0.134751 11.00000 -1.20000 AFIX 0 C26 1 0.797319 0.742757 0.166803 11.00000 0.02119 0.01326 = 0.01702 0.00254 0.00966 0.00163 AFIX 43 H26 2 0.789555 0.810092 0.211681 11.00000 -1.20000 AFIX 0 C27 1 0.725532 0.645788 0.146833 11.00000 0.01418 0.01465 = 0.01201 0.00410 0.00602 0.00350 N5 3 0.818078 0.418078 0.361971 11.00000 0.01847 0.01033 = 0.01515 0.00466 0.00858 0.00408 AFIX 3 H5N 2 0.792828 0.344988 0.330893 11.00000 -1.20000 AFIX 0 N6 3 0.895505 0.745627 0.464165 11.00000 0.02046 0.01297 = 0.02392 0.00894 0.01353 0.00707 AFIX 3 H6A 2 0.842102 0.780490 0.484614 11.00000 -1.20000 H6B 2 0.948417 0.782211 0.450760 11.00000 -1.20000 AFIX 0 C28 1 0.899477 0.462684 0.336390 11.00000 0.01423 0.01356 = 0.01144 0.00514 0.00491 0.00492 C29 1 0.948819 0.394810 0.269675 11.00000 0.02226 0.01350 = 0.01734 0.00438 0.01013 0.00625 AFIX 43 H29 2 0.926148 0.319303 0.244439 11.00000 -1.20000 AFIX 0 C30 1 1.029047 0.438023 0.241646 11.00000 0.02164 0.01936 = 0.01862 0.00615 0.01214 0.00837 AFIX 43 H30 2 1.061618 0.392127 0.196676 11.00000 -1.20000 AFIX 0 C31 1 1.063969 0.549891 0.278718 11.00000 0.01809 0.02049 = 0.02075 0.00919 0.01054 0.00563 AFIX 43 H31 2 1.119594 0.578891 0.258456 11.00000 -1.20000 AFIX 0 C32 1 1.017795 0.617120 0.344077 11.00000 0.01629 0.01482 = 0.01756 0.00743 0.00702 0.00400 AFIX 43 H32 2 1.042550 0.692516 0.369395 11.00000 -1.20000 AFIX 0 C33 1 0.933637 0.575331 0.374201 11.00000 0.01504 0.01259 = 0.01228 0.00586 0.00541 0.00508 C34 1 0.876776 0.641685 0.436564 11.00000 0.01378 0.01321 = 0.01320 0.00598 0.00488 0.00476 C35 1 0.797875 0.591893 0.468261 11.00000 0.01486 0.01271 = 0.01462 0.00696 0.00635 0.00557 C36 1 0.748983 0.651860 0.540986 11.00000 0.02205 0.01325 = 0.01954 0.00723 0.01133 0.00837 AFIX 43 H36 2 0.767215 0.727854 0.569286 11.00000 -1.20000 AFIX 0 C37 1 0.676342 0.602124 0.570811 11.00000 0.02423 0.01873 = 0.02346 0.00985 0.01581 0.01125 AFIX 43 H37 2 0.645859 0.643491 0.620783 11.00000 -1.20000 AFIX 0 C38 1 0.646545 0.488616 0.527014 11.00000 0.02004 0.01985 = 0.02173 0.01212 0.01207 0.00748 AFIX 43 H38 2 0.594526 0.454174 0.546700 11.00000 -1.20000 AFIX 0 C39 1 0.691570 0.427841 0.456779 11.00000 0.01891 0.01429 = 0.01815 0.00850 0.00882 0.00513 AFIX 43 H39 2 0.670293 0.351700 0.427277 11.00000 -1.20000 AFIX 0 C40 1 0.769887 0.479148 0.428486 11.00000 0.01560 0.01314 = 0.01277 0.00613 0.00632 0.00608 O11 4 0.922427 0.116605 0.534360 11.00000 0.02758 0.01769 = 0.01871 0.01180 0.01331 0.00762 AFIX 3 H11A 2 0.879632 0.076696 0.461420 11.00000 -1.20000 H11B 2 0.948772 0.079556 0.570592 11.00000 -1.20000 AFIX 0 O12 4 0.489732 0.120807 0.914444 11.00000 0.03265 0.03852 = 0.01997 0.00663 0.00953 0.02235 AFIX 3 H12A 2 0.526262 0.071498 0.914184 11.00000 -1.20000 H12B 2 0.425957 0.103868 0.848671 11.00000 -1.20000 AFIX 0 O13 4 0.294478 0.799394 0.717641 11.00000 0.02340 0.01493 = 0.02961 0.00817 0.01452 0.00672 AFIX 3 H13A 2 0.370516 0.825958 0.771909 11.00000 -1.20000 H13B 2 0.259466 0.848114 0.709192 11.00000 -1.20000 AFIX 0 O14 4 0.546282 0.910040 0.906623 11.00000 0.02467 0.03426 = 0.03105 0.01387 0.01699 0.01131 AFIX 3 H14A 2 0.608205 0.888681 0.902215 11.00000 -1.20000 H14B 2 0.549360 0.901830 0.964153 11.00000 -1.20000 HKLF 4 REM JTM377_0m in P-1 REM R1 = 0.0318 for 9056 Fo > 4sig(Fo) and 0.0337 for all 9618 data REM 550 parameters refined using 0 restraints END WGHT 0.0428 1.7530 REM Highest difference peak 0.841, deepest hole -0.618, 1-sigma level 0.115 Q1 1 0.8765 1.0346 0.7339 11.00000 0.05 0.84 Q2 1 0.7423 0.9365 0.6364 11.00000 0.05 0.81 Q3 1 0.4402 0.0814 0.9061 11.00000 0.05 0.63 Q4 1 1.0782 0.9563 0.7693 11.00000 0.05 0.58 Q5 1 0.7252 1.1870 0.7028 11.00000 0.05 0.58 ; _database_code_depnum_ccdc_archive 'CCDC 940545'