Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'John Berry' _publ_contact_author_address ; Chemistry University of Wisconsin 1101 University Ave Madison WI 53706 UNITED STATES OF AMERICA ; _publ_contact_author_email BERRY@CHEM.WISC.EDU _publ_section_title ; Bond distances are not always what they appear to be: Discovery and un-discovery of the longest Cr(V)-N triple bond ; loop_ _publ_author_name 'John Berry' 'E. Bill' 'Yu-Fei Song.' 'Thomas Weyhermuller' ####################Compound 2#################### data_Cpd2 _database_code_depnum_ccdc_archive 'CCDC 667804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'L2CrCl, 2(H2O)' _chemical_melting_point ? _chemical_formula_moiety '[C13 H23 Cl Cr N3 O4], 2 (H2 O)' _chemical_formula_sum 'C13 H27 Cl Cr N3 O6' _chemical_formula_weight 408.83 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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.8717(3) _cell_length_b 31.2767(12) _cell_length_c 8.6425(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.478(4) _cell_angle_gamma 90.00 _cell_volume 1761.72(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 55292 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 31.00 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour violet _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.9002 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '1800 images at 0.8 deg stepwise rotation in omega and phi, 24 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54167 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 31.06 _reflns_number_total 5614 _reflns_number_gt 4813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.8645P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5614 _refine_ls_number_parameters 231 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.003 _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 0.39069(3) 0.611086(5) 1.05223(2) 0.00949(4) Uani 1 1 d . . . Cl1 Cl 0.24870(4) 0.543522(8) 1.00751(3) 0.01508(6) Uani 1 1 d . . . N1 N 0.69463(14) 0.58741(3) 1.15143(11) 0.01135(17) Uani 1 1 d . . . C2 C 0.80765(17) 0.62280(4) 1.26018(13) 0.0144(2) Uani 1 1 d . . . H2A H 0.9572 0.6176 1.2904 0.017 Uiso 1 1 calc R . . H2B H 0.7698 0.6231 1.3616 0.017 Uiso 1 1 calc R . . C3 C 0.75706(17) 0.66577(4) 1.17587(14) 0.0153(2) Uani 1 1 d . . . H3A H 0.8061 0.6889 1.2573 0.018 Uiso 1 1 calc R . . H3B H 0.8297 0.6685 1.0941 0.018 Uiso 1 1 calc R . . N4 N 0.52991(14) 0.67087(3) 1.09262(11) 0.01235(17) Uani 1 1 d . . . C5 C 0.49026(18) 0.69063(4) 0.92813(13) 0.0146(2) Uani 1 1 d . . . H5A H 0.5776 0.7162 0.9365 0.018 Uiso 1 1 calc R . . H5B H 0.3448 0.6995 0.8838 0.018 Uiso 1 1 calc R . . C6 C 0.53914(17) 0.65764(4) 0.81547(13) 0.0147(2) Uani 1 1 d . . . H6A H 0.4813 0.6673 0.7009 0.018 Uiso 1 1 calc R . . H6B H 0.6898 0.6553 0.8414 0.018 Uiso 1 1 calc R . . N7 N 0.45158(14) 0.61434(3) 0.83385(11) 0.01207(17) Uani 1 1 d . . . C8 C 0.60225(17) 0.57932(4) 0.84406(13) 0.0141(2) Uani 1 1 d . . . H8A H 0.6607 0.5821 0.7535 0.017 Uiso 1 1 calc R . . H8B H 0.5324 0.5513 0.8338 0.017 Uiso 1 1 calc R . . C9 C 0.77337(16) 0.58173(4) 1.00672(13) 0.0136(2) Uani 1 1 d . . . H9A H 0.8647 0.6060 1.0038 0.016 Uiso 1 1 calc R . . H9B H 0.8559 0.5552 1.0221 0.016 Uiso 1 1 calc R . . C10 C 0.72755(17) 0.54551(4) 1.24636(13) 0.0140(2) Uani 1 1 d . . . H10 H 0.6618 0.5224 1.1670 0.017 Uiso 1 1 calc R . . C11 C 0.6266(2) 0.54474(4) 1.38020(15) 0.0190(2) Uani 1 1 d . . . H11A H 0.6946 0.5655 1.4651 0.029 Uiso 1 1 calc R . . H11B H 0.6391 0.5161 1.4280 0.029 Uiso 1 1 calc R . . H11C H 0.4811 0.5522 1.3335 0.029 Uiso 1 1 calc R . . C12 C 0.95593(18) 0.53411(4) 1.31917(14) 0.0187(2) Uani 1 1 d . . . H12A H 1.0187 0.5519 1.4153 0.028 Uiso 1 1 calc R . . H12B H 1.0251 0.5392 1.2376 0.028 Uiso 1 1 calc R . . H12C H 0.9696 0.5039 1.3510 0.028 Uiso 1 1 calc R . . C13 C 0.42816(19) 0.69437(4) 1.19574(14) 0.0159(2) Uani 1 1 d . . . H13A H 0.3134 0.7116 1.1249 0.019 Uiso 1 1 calc R . . H13B H 0.5278 0.7142 1.2689 0.019 Uiso 1 1 calc R . . C14 C 0.34626(17) 0.66379(4) 1.29800(13) 0.0145(2) Uani 1 1 d . . . O15 O 0.28962(15) 0.67796(3) 1.40987(10) 0.02111(18) Uani 1 1 d . . . O16 O 0.33503(12) 0.62409(3) 1.25640(9) 0.01411(15) Uani 1 1 d . . . C17 C 0.25004(17) 0.60774(4) 0.70605(13) 0.0150(2) Uani 1 1 d . . . H17A H 0.2216 0.5768 0.6890 0.018 Uiso 1 1 calc R . . H17B H 0.2527 0.6203 0.6017 0.018 Uiso 1 1 calc R . . C18 C 0.08266(17) 0.62899(4) 0.76009(13) 0.0139(2) Uani 1 1 d . . . O19 O -0.08607(13) 0.63648(3) 0.65937(10) 0.01929(17) Uani 1 1 d . . . O20 O 0.13033(12) 0.63727(3) 0.91472(9) 0.01306(15) Uani 1 1 d . . . O30 O 0.05130(16) 0.74670(3) 1.44753(12) 0.02429(19) Uani 1 1 d D . . H30A H 0.126(2) 0.7267(5) 1.440(2) 0.036 Uiso 1 1 d D . . H30B H -0.015(3) 0.7385(6) 1.506(2) 0.036 Uiso 1 1 d D . . O40 O -0.17980(16) 0.77538(3) 1.14484(13) 0.0264(2) Uani 1 1 d D . . H40A H -0.170(3) 0.8017(4) 1.146(2) 0.040 Uiso 1 1 d D . . H40B H -0.114(3) 0.7670(6) 1.2372(16) 0.040 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.00995(8) 0.01009(8) 0.00910(7) -0.00064(6) 0.00399(6) -0.00102(6) Cl1 0.01401(12) 0.01197(11) 0.02063(12) -0.00309(9) 0.00744(9) -0.00258(9) N1 0.0124(4) 0.0121(4) 0.0099(4) 0.0002(3) 0.0040(3) -0.0006(3) C2 0.0139(5) 0.0141(5) 0.0129(5) -0.0003(4) 0.0012(4) -0.0018(4) C3 0.0139(5) 0.0141(5) 0.0159(5) -0.0001(4) 0.0018(4) -0.0033(4) N4 0.0135(4) 0.0113(4) 0.0123(4) -0.0003(3) 0.0042(3) -0.0013(3) C5 0.0160(5) 0.0133(5) 0.0146(5) 0.0036(4) 0.0050(4) -0.0012(4) C6 0.0151(5) 0.0170(5) 0.0133(5) 0.0037(4) 0.0063(4) -0.0011(4) N7 0.0109(4) 0.0151(4) 0.0105(4) -0.0003(3) 0.0039(3) -0.0002(3) C8 0.0138(5) 0.0175(5) 0.0123(4) -0.0003(4) 0.0062(4) 0.0021(4) C9 0.0124(5) 0.0176(5) 0.0124(4) 0.0015(4) 0.0060(4) 0.0014(4) C10 0.0162(5) 0.0123(5) 0.0139(5) 0.0022(4) 0.0054(4) 0.0006(4) C11 0.0242(6) 0.0181(5) 0.0174(5) 0.0055(4) 0.0103(4) 0.0020(4) C12 0.0183(5) 0.0205(6) 0.0165(5) 0.0043(4) 0.0043(4) 0.0033(4) C13 0.0209(5) 0.0116(5) 0.0159(5) -0.0027(4) 0.0069(4) 0.0007(4) C14 0.0154(5) 0.0165(5) 0.0105(4) -0.0003(4) 0.0026(4) 0.0026(4) O15 0.0290(5) 0.0218(4) 0.0148(4) -0.0025(3) 0.0102(3) 0.0052(4) O16 0.0175(4) 0.0140(4) 0.0125(3) -0.0005(3) 0.0070(3) 0.0003(3) C17 0.0129(5) 0.0203(5) 0.0106(4) -0.0022(4) 0.0023(4) -0.0002(4) C18 0.0134(5) 0.0138(5) 0.0145(5) -0.0003(4) 0.0043(4) -0.0017(4) O19 0.0133(4) 0.0256(4) 0.0162(4) -0.0016(3) 0.0008(3) 0.0019(3) O20 0.0121(4) 0.0145(4) 0.0128(3) -0.0002(3) 0.0042(3) 0.0001(3) O30 0.0287(5) 0.0177(4) 0.0282(5) -0.0020(4) 0.0116(4) 0.0002(4) O40 0.0286(5) 0.0212(5) 0.0288(5) -0.0025(4) 0.0083(4) -0.0015(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 O16 1.9629(8) . ? Cr1 O20 1.9840(8) . ? Cr1 N7 2.0610(9) . ? Cr1 N4 2.0789(9) . ? Cr1 N1 2.1238(9) . ? Cr1 Cl1 2.3082(3) . ? N1 C2 1.4996(14) . ? N1 C9 1.5223(14) . ? N1 C10 1.5245(14) . ? C2 C3 1.5157(16) . ? C3 N4 1.5059(14) . ? N4 C13 1.4895(14) . ? N4 C5 1.4937(14) . ? C5 C6 1.5273(16) . ? C6 N7 1.5105(14) . ? N7 C17 1.4869(14) . ? N7 C8 1.4906(14) . ? C8 C9 1.5221(15) . ? C10 C11 1.5260(16) . ? C10 C12 1.5362(16) . ? C13 C14 1.5256(16) . ? C14 O15 1.2333(14) . ? C14 O16 1.2882(14) . ? C17 C18 1.5242(16) . ? C18 O19 1.2318(14) . ? C18 O20 1.2972(13) . ? 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 O16 Cr1 O20 93.28(3) . . ? O16 Cr1 N7 165.20(4) . . ? O20 Cr1 N7 80.64(3) . . ? O16 Cr1 N4 82.71(4) . . ? O20 Cr1 N4 90.51(3) . . ? N7 Cr1 N4 83.86(4) . . ? O16 Cr1 N1 98.99(3) . . ? O20 Cr1 N1 166.05(3) . . ? N7 Cr1 N1 85.86(4) . . ? N4 Cr1 N1 84.52(4) . . ? O16 Cr1 Cl1 98.50(3) . . ? O20 Cr1 Cl1 91.41(3) . . ? N7 Cr1 Cl1 95.15(3) . . ? N4 Cr1 Cl1 177.67(3) . . ? N1 Cr1 Cl1 93.31(3) . . ? C2 N1 C9 110.65(8) . . ? C2 N1 C10 109.77(8) . . ? C9 N1 C10 108.13(8) . . ? C2 N1 Cr1 104.08(6) . . ? C9 N1 Cr1 105.61(6) . . ? C10 N1 Cr1 118.44(7) . . ? N1 C2 C3 111.03(9) . . ? N4 C3 C2 111.64(9) . . ? C13 N4 C5 112.75(9) . . ? C13 N4 C3 112.24(9) . . ? C5 N4 C3 110.33(9) . . ? C13 N4 Cr1 105.43(7) . . ? C5 N4 Cr1 106.07(6) . . ? C3 N4 Cr1 109.70(7) . . ? N4 C5 C6 108.46(9) . . ? N7 C6 C5 111.29(9) . . ? C17 N7 C8 114.07(9) . . ? C17 N7 C6 110.77(9) . . ? C8 N7 C6 111.88(9) . . ? C17 N7 Cr1 105.17(7) . . ? C8 N7 Cr1 104.37(6) . . ? C6 N7 Cr1 110.12(7) . . ? N7 C8 C9 109.69(9) . . ? C8 C9 N1 113.13(9) . . ? N1 C10 C11 113.31(9) . . ? N1 C10 C12 112.21(9) . . ? C11 C10 C12 109.68(9) . . ? N4 C13 C14 111.50(9) . . ? O15 C14 O16 124.00(11) . . ? O15 C14 C13 119.66(10) . . ? O16 C14 C13 116.30(9) . . ? C14 O16 Cr1 116.05(7) . . ? N7 C17 C18 109.12(9) . . ? O19 C18 O20 124.32(11) . . ? O19 C18 C17 119.94(10) . . ? O20 C18 C17 115.73(9) . . ? C18 O20 Cr1 114.83(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 31.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.445 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.055 #####################END Compound 2################# #####################Compound 4##################### data_Cpd4 _database_code_depnum_ccdc_archive 'CCDC 667805' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common L1CrN3 _chemical_formula_moiety (C17H23N3O4)CrN3 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H23 Cr N6 O4' _chemical_formula_weight 427.41 _chemical_melting_point ? _chemical_compound_source ? 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.4667(6) _cell_length_b 12.8766(9) _cell_length_c 18.7793(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1805.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40688 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 33.14 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method ? _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.9144 _exptl_absorpt_correction_T_max 0.9620 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa-CCD' _diffrn_measurement_method '738 images at 1.0 deg. stepwise rotation in omega and phi, 80 sec./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38954 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 33.00 _reflns_number_total 6802 _reflns_number_observed 5749 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+1.4694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 6796 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_obs 0.0475 _refine_ls_wR_factor_all 0.0847 _refine_ls_wR_factor_obs 0.0796 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.109 _refine_ls_restrained_S_all 1.082 _refine_ls_restrained_S_obs 1.109 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 0.59353(4) 0.24971(3) 0.17500(2) 0.00857(6) Uani 1 d . . N1 N 0.5402(2) 0.39888(13) 0.13333(9) 0.0099(3) Uani 1 d . . C2 C 0.4787(3) 0.4603(2) 0.19614(11) 0.0122(4) Uani 1 d . . H2A H 0.3552(3) 0.4393(2) 0.20895(11) 0.015 Uiso 1 calc R . H2B H 0.4770(3) 0.5351(2) 0.18380(11) 0.015 Uiso 1 calc R . C3 C 0.6021(3) 0.44287(14) 0.25938(11) 0.0123(4) Uani 1 d . . H3A H 0.7147(3) 0.48205(14) 0.25212(11) 0.015 Uiso 1 calc R . H3B H 0.5441(3) 0.46951(14) 0.30313(11) 0.015 Uiso 1 calc R . N4 N 0.6444(2) 0.32970(13) 0.26867(9) 0.0099(3) Uani 1 d . . C5 C 0.8398(3) 0.3147(2) 0.28289(11) 0.0115(4) Uani 1 d . . H5A H 0.8623(3) 0.2427(2) 0.29921(11) 0.014 Uiso 1 calc R . H5B H 0.8799(3) 0.3630(2) 0.32067(11) 0.014 Uiso 1 calc R . C6 C 0.9427(3) 0.3356(2) 0.21444(11) 0.0123(4) Uani 1 d . . H6A H 0.9479(3) 0.4114(2) 0.20592(11) 0.015 Uiso 1 calc R . H6B H 1.0669(3) 0.3099(2) 0.21960(11) 0.015 Uiso 1 calc R . N7 N 0.8556(2) 0.28317(13) 0.15143(9) 0.0106(3) Uani 1 d . . C8 C 0.8441(3) 0.3517(2) 0.08771(11) 0.0120(4) Uani 1 d . . H8A H 0.8027(3) 0.3110(2) 0.04612(11) 0.014 Uiso 1 calc R . H8B H 0.9639(3) 0.3804(2) 0.07658(11) 0.014 Uiso 1 calc R . C9 C 0.7128(3) 0.4404(2) 0.10263(11) 0.0124(4) Uani 1 d . . H9A H 0.7675(3) 0.4899(2) 0.13660(11) 0.015 Uiso 1 calc R . H9B H 0.6873(3) 0.4781(2) 0.05784(11) 0.015 Uiso 1 calc R . C10 C 0.3955(3) 0.3949(2) 0.07813(11) 0.0123(4) Uani 1 d . . H10A H 0.2932(3) 0.3556(2) 0.09808(11) 0.015 Uiso 1 calc R . H10B H 0.4412(3) 0.3552(2) 0.03680(11) 0.015 Uiso 1 calc R . C11 C 0.3261(3) 0.4985(2) 0.05133(11) 0.0116(4) Uani 1 d . . C12 C 0.1886(3) 0.5503(2) 0.08722(12) 0.0142(4) Uani 1 d . . H12 H 0.1432(3) 0.5223(2) 0.13040(12) 0.017 Uiso 1 calc R . C13 C 0.1174(3) 0.6422(2) 0.06057(12) 0.0155(4) Uani 1 d . . H13 H 0.0237(3) 0.6766(2) 0.08538(12) 0.019 Uiso 1 calc R . C14 C 0.1835(3) 0.6835(2) -0.00225(12) 0.0177(4) Uani 1 d . . H14 H 0.1357(3) 0.7465(2) -0.02037(12) 0.021 Uiso 1 calc R . C15 C 0.3195(3) 0.6328(2) -0.03880(12) 0.0157(4) Uani 1 d . . H15 H 0.3641(3) 0.6611(2) -0.08201(12) 0.019 Uiso 1 calc R . C16 C 0.3907(3) 0.5408(2) -0.01244(11) 0.0136(4) Uani 1 d . . H16 H 0.4836(3) 0.5065(2) -0.03776(11) 0.016 Uiso 1 calc R . C19 C 0.5272(3) 0.2796(2) 0.32277(12) 0.0129(4) Uani 1 d . . H19A H 0.4912(3) 0.3319(2) 0.35872(12) 0.016 Uiso 1 calc R . H19B H 0.5950(3) 0.2243(2) 0.34746(12) 0.016 Uiso 1 calc R . C20 C 0.3592(3) 0.23275(14) 0.28862(11) 0.0130(4) Uani 1 d . . O21 O 0.2366(2) 0.20172(12) 0.32617(9) 0.0187(3) Uani 1 d . . O22 O 0.3607(2) 0.22670(10) 0.21923(8) 0.0126(3) Uani 1 d . . C23 C 0.9385(3) 0.1798(2) 0.13792(12) 0.0147(4) Uani 1 d . . H23A H 1.0694(3) 0.1839(2) 0.14568(12) 0.018 Uiso 1 calc R . H23B H 0.9172(3) 0.1589(2) 0.08790(12) 0.018 Uiso 1 calc R . C24 C 0.8572(3) 0.0990(2) 0.18819(11) 0.0148(4) Uani 1 d . . O25 O 0.9346(2) 0.01795(12) 0.20060(9) 0.0238(4) Uani 1 d . . O26 O 0.7000(2) 0.12330(11) 0.21384(8) 0.0131(3) Uani 1 d . . N31 N 0.5437(2) 0.18069(14) 0.08130(10) 0.0145(3) Uani 1 d . . N32 N 0.4492(3) 0.1050(2) 0.07591(10) 0.0185(4) Uani 1 d . . N33 N 0.3582(4) 0.0332(2) 0.06753(12) 0.0347(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.00957(11) 0.00769(11) 0.00846(12) 0.00014(14) -0.00004(11) -0.00012(14) N1 0.0099(7) 0.0107(7) 0.0092(8) -0.0011(6) -0.0004(6) -0.0002(6) C2 0.0145(9) 0.0110(8) 0.0111(9) -0.0005(7) 0.0007(7) 0.0011(7) C3 0.0150(9) 0.0094(8) 0.0125(9) -0.0008(7) -0.0002(8) 0.0007(7) N4 0.0101(7) 0.0099(7) 0.0097(8) 0.0005(6) -0.0003(6) 0.0008(6) C5 0.0103(8) 0.0127(8) 0.0115(9) 0.0023(7) -0.0012(7) 0.0009(7) C6 0.0109(9) 0.0130(9) 0.0130(9) -0.0005(7) -0.0009(7) -0.0015(7) N7 0.0113(7) 0.0105(7) 0.0102(8) 0.0011(6) 0.0003(6) 0.0012(6) C8 0.0131(8) 0.0131(9) 0.0098(9) 0.0019(7) 0.0024(7) 0.0005(7) C9 0.0123(9) 0.0138(9) 0.0111(10) 0.0013(7) 0.0002(7) -0.0011(7) C10 0.0139(9) 0.0108(8) 0.0121(9) 0.0014(7) -0.0035(8) -0.0008(8) C11 0.0127(9) 0.0106(9) 0.0115(9) -0.0001(7) -0.0034(7) 0.0002(7) C12 0.0130(9) 0.0158(9) 0.0137(10) 0.0007(8) -0.0017(8) -0.0010(7) C13 0.0154(10) 0.0159(9) 0.0153(10) -0.0031(8) -0.0031(8) 0.0063(8) C14 0.0214(11) 0.0133(9) 0.0183(11) 0.0001(8) -0.0067(9) 0.0030(8) C15 0.0194(10) 0.0143(9) 0.0133(10) 0.0033(8) -0.0027(8) -0.0025(8) C16 0.0132(9) 0.0148(9) 0.0128(9) 0.0001(7) 0.0007(8) 0.0000(8) C19 0.0132(8) 0.0177(9) 0.0079(8) 0.0021(8) 0.0020(8) -0.0016(7) C20 0.0119(8) 0.0109(10) 0.0161(9) 0.0006(7) 0.0002(7) 0.0017(6) O21 0.0152(7) 0.0219(8) 0.0191(8) 0.0012(7) 0.0055(7) -0.0031(6) O22 0.0107(6) 0.0150(7) 0.0120(7) 0.0000(5) 0.0006(5) -0.0019(5) C23 0.0154(10) 0.0131(9) 0.0156(10) -0.0008(8) 0.0027(8) 0.0045(7) C24 0.0177(9) 0.0128(9) 0.0140(11) -0.0001(7) -0.0032(8) 0.0020(7) O25 0.0261(9) 0.0178(7) 0.0276(9) 0.0055(7) 0.0034(7) 0.0101(7) O26 0.0144(7) 0.0104(6) 0.0146(7) 0.0028(6) -0.0001(6) 0.0010(5) N31 0.0195(8) 0.0113(8) 0.0126(8) -0.0017(7) -0.0021(7) -0.0013(7) N32 0.0258(10) 0.0188(9) 0.0110(9) 0.0012(7) -0.0019(8) -0.0014(8) N33 0.057(2) 0.0295(12) 0.0178(11) 0.0028(9) -0.0100(10) -0.0230(11) _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 O22 1.9497(14) . ? Cr1 O26 1.9529(14) . ? Cr1 N31 2.006(2) . ? Cr1 N7 2.052(2) . ? Cr1 N4 2.073(2) . ? Cr1 N1 2.112(2) . ? N1 C2 1.493(3) . ? N1 C10 1.498(3) . ? N1 C9 1.509(3) . ? C2 C3 1.520(3) . ? C3 N4 1.501(2) . ? N4 C19 1.488(3) . ? N4 C5 1.496(2) . ? C5 C6 1.521(3) . ? C6 N7 1.509(3) . ? N7 C8 1.489(3) . ? N7 C23 1.490(3) . ? C8 C9 1.531(3) . ? C10 C11 1.517(3) . ? C11 C12 1.397(3) . ? C11 C16 1.401(3) . ? C12 C13 1.391(3) . ? C13 C14 1.385(3) . ? C14 C15 1.389(3) . ? C15 C16 1.389(3) . ? C19 C20 1.532(3) . ? C20 O21 1.223(2) . ? C20 O22 1.305(2) . ? C23 C24 1.530(3) . ? C24 O25 1.216(2) . ? C24 O26 1.306(2) . ? N31 N32 1.208(3) . ? N32 N33 1.158(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O22 Cr1 O26 94.44(6) . . ? O22 Cr1 N31 98.11(7) . . ? O26 Cr1 N31 91.94(7) . . ? O22 Cr1 N7 166.98(7) . . ? O26 Cr1 N7 82.37(6) . . ? N31 Cr1 N7 94.63(7) . . ? O22 Cr1 N4 82.95(6) . . ? O26 Cr1 N4 91.30(6) . . ? N31 Cr1 N4 176.50(7) . . ? N7 Cr1 N4 84.50(7) . . ? O22 Cr1 N1 97.35(6) . . ? O26 Cr1 N1 166.70(6) . . ? N31 Cr1 N1 92.46(7) . . ? N7 Cr1 N1 84.77(7) . . ? N4 Cr1 N1 84.09(6) . . ? C2 N1 C10 110.0(2) . . ? C2 N1 C9 112.2(2) . . ? C10 N1 C9 111.3(2) . . ? C2 N1 Cr1 104.32(12) . . ? C10 N1 Cr1 111.18(12) . . ? C9 N1 Cr1 107.62(12) . . ? N1 C2 C3 110.6(2) . . ? N4 C3 C2 111.2(2) . . ? C19 N4 C5 113.3(2) . . ? C19 N4 C3 112.1(2) . . ? C5 N4 C3 110.6(2) . . ? C19 N4 Cr1 104.86(12) . . ? C5 N4 Cr1 105.41(12) . . ? C3 N4 Cr1 110.19(12) . . ? N4 C5 C6 108.6(2) . . ? N7 C6 C5 111.5(2) . . ? C8 N7 C23 114.6(2) . . ? C8 N7 C6 113.0(2) . . ? C23 N7 C6 110.7(2) . . ? C8 N7 Cr1 104.06(12) . . ? C23 N7 Cr1 104.19(12) . . ? C6 N7 Cr1 109.61(12) . . ? N7 C8 C9 109.4(2) . . ? N1 C9 C8 110.6(2) . . ? N1 C10 C11 116.5(2) . . ? C12 C11 C16 118.7(2) . . ? C12 C11 C10 120.7(2) . . ? C16 C11 C10 120.5(2) . . ? C13 C12 C11 120.9(2) . . ? C14 C13 C12 119.8(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 120.3(2) . . ? C15 C16 C11 120.3(2) . . ? N4 C19 C20 111.5(2) . . ? O21 C20 O22 124.2(2) . . ? O21 C20 C19 120.0(2) . . ? O22 C20 C19 115.8(2) . . ? C20 O22 Cr1 115.06(12) . . ? N7 C23 C24 109.7(2) . . ? O25 C24 O26 124.2(2) . . ? O25 C24 C23 120.9(2) . . ? O26 C24 C23 114.9(2) . . ? C24 O26 Cr1 115.30(13) . . ? N32 N31 Cr1 122.6(2) . . ? N33 N32 N31 177.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.470 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.080 #####################END Compound 4################# #####################Compound 5##################### data_Cpd5 _database_code_depnum_ccdc_archive 'CCDC 667806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'L2CrN3, 0.5(H2O)' _chemical_melting_point ? _chemical_formula_moiety '[C13 H23 Cr N6 O4], 0.5 (H2 O)' _chemical_formula_sum 'C13 H24 Cr N6 O4.5' _chemical_formula_weight 388.38 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.2406(2) _cell_length_b 27.785(2) _cell_length_c 16.5271(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.459(5) _cell_angle_gamma 90.00 _cell_volume 3303.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 42831 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 30.00 _exptl_crystal_description 'transparent needle' _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8978 _exptl_absorpt_correction_T_max 0.9724 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42349 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9578 _reflns_number_gt 6987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+4.4178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9578 _refine_ls_number_parameters 452 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.89738(5) 0.016483(13) 0.24048(2) 0.01077(8) Uani 1 1 d . . . N1 N 0.6635(3) 0.01715(7) 0.30744(11) 0.0127(4) Uani 1 1 d . . . C2 C 0.4955(3) 0.02667(9) 0.24564(15) 0.0163(5) Uani 1 1 d . . . H2A H 0.4056 0.0470 0.2711 0.020 Uiso 1 1 calc R . . H2B H 0.4339 -0.0043 0.2299 0.020 Uiso 1 1 calc R . . C3 C 0.5489(3) 0.05180(9) 0.16961(15) 0.0172(5) Uani 1 1 d . . . H3A H 0.4407 0.0527 0.1273 0.021 Uiso 1 1 calc R . . H3B H 0.5875 0.0853 0.1829 0.021 Uiso 1 1 calc R . . N4 N 0.7055(3) 0.02494(7) 0.13849(12) 0.0143(4) Uani 1 1 d . . . C5 C 0.6422(3) -0.02367(9) 0.10435(14) 0.0158(5) Uani 1 1 d . . . H5A H 0.6291 -0.0224 0.0441 0.019 Uiso 1 1 calc R . . H5B H 0.5191 -0.0315 0.1216 0.019 Uiso 1 1 calc R . . C6 C 0.7811(3) -0.06260(9) 0.13406(14) 0.0148(5) Uani 1 1 d . . . H6A H 0.7239 -0.0947 0.1243 0.018 Uiso 1 1 calc R . . H6B H 0.8914 -0.0606 0.1038 0.018 Uiso 1 1 calc R . . N7 N 0.8380(3) -0.05577(7) 0.22277(11) 0.0122(4) Uani 1 1 d . . . C8 C 0.6821(3) -0.06941(8) 0.27156(14) 0.0130(4) Uani 1 1 d . . . H8A H 0.7066 -0.1018 0.2955 0.016 Uiso 1 1 calc R . . H8B H 0.5642 -0.0710 0.2350 0.016 Uiso 1 1 calc R . . C9 C 0.6618(3) -0.03363(8) 0.33905(14) 0.0140(4) Uani 1 1 d . . . H9A H 0.5436 -0.0396 0.3622 0.017 Uiso 1 1 calc R . . H9B H 0.7651 -0.0380 0.3830 0.017 Uiso 1 1 calc R . . C10 C 0.6642(3) 0.05342(9) 0.37666(15) 0.0173(5) Uani 1 1 d . . . H10 H 0.6661 0.0862 0.3518 0.021 Uiso 1 1 calc R . . C11 C 0.4886(4) 0.05056(11) 0.42097(17) 0.0253(6) Uani 1 1 d . . . H11A H 0.3851 0.0664 0.3880 0.038 Uiso 1 1 calc R . . H11B H 0.5118 0.0667 0.4739 0.038 Uiso 1 1 calc R . . H11C H 0.4572 0.0167 0.4292 0.038 Uiso 1 1 calc R . . C12 C 0.8376(4) 0.04938(10) 0.43830(16) 0.0240(6) Uani 1 1 d . . . H12A H 0.8305 0.0199 0.4704 0.036 Uiso 1 1 calc R . . H12B H 0.8449 0.0774 0.4746 0.036 Uiso 1 1 calc R . . H12C H 0.9485 0.0483 0.4094 0.036 Uiso 1 1 calc R . . C13 C 0.8075(3) 0.05213(9) 0.07999(15) 0.0179(5) Uani 1 1 d . . . H13A H 0.7957 0.0871 0.0897 0.022 Uiso 1 1 calc R . . H13B H 0.7524 0.0452 0.0236 0.022 Uiso 1 1 calc R . . C14 C 1.0133(3) 0.03793(8) 0.09003(14) 0.0145(4) Uani 1 1 d . . . O15 O 1.1119(2) 0.04913(7) 0.03763(10) 0.0199(4) Uani 1 1 d . . . O16 O 1.0713(2) 0.01542(6) 0.15744(10) 0.0156(3) Uani 1 1 d . . . C17 C 1.0148(3) -0.08127(9) 0.25123(15) 0.0152(5) Uani 1 1 d . . . H17A H 1.0908 -0.0846 0.2053 0.018 Uiso 1 1 calc R . . H17B H 0.9864 -0.1140 0.2702 0.018 Uiso 1 1 calc R . . C18 C 1.1251(3) -0.05347(9) 0.32074(14) 0.0151(5) Uani 1 1 d . . . O19 O 1.2487(2) -0.07385(7) 0.36443(11) 0.0190(4) Uani 1 1 d . . . O20 O 1.0827(2) -0.00822(6) 0.32518(10) 0.0150(3) Uani 1 1 d . . . N31 N 0.9377(3) 0.08788(8) 0.25791(14) 0.0190(4) Uani 1 1 d . . . N32 N 1.0825(3) 0.10843(7) 0.25484(13) 0.0161(4) Uani 1 1 d . . . N33 N 1.2176(3) 0.13041(8) 0.25250(15) 0.0259(5) Uani 1 1 d . . . Cr2 Cr 0.75563(5) 0.237146(14) 0.51801(2) 0.01336(9) Uani 1 1 d . . . N41 N 0.6360(3) 0.23490(8) 0.39417(12) 0.0165(4) Uani 1 1 d . . . C42 C 0.6104(3) 0.28708(9) 0.37244(16) 0.0194(5) Uani 1 1 d . . . H42A H 0.5293 0.2901 0.3203 0.023 Uiso 1 1 calc R . . H42B H 0.7324 0.3016 0.3652 0.023 Uiso 1 1 calc R . . C43 C 0.5236(3) 0.31390(9) 0.43893(16) 0.0193(5) Uani 1 1 d . . . H43A H 0.5337 0.3490 0.4297 0.023 Uiso 1 1 calc R . . H43B H 0.3899 0.3057 0.4356 0.023 Uiso 1 1 calc R . . N44 N 0.6150(3) 0.30191(7) 0.52260(13) 0.0162(4) Uani 1 1 d . . . C45 C 0.4733(3) 0.29444(9) 0.58093(16) 0.0195(5) Uani 1 1 d . . . H45A H 0.3825 0.3212 0.5763 0.023 Uiso 1 1 calc R . . H45B H 0.5349 0.2936 0.6375 0.023 Uiso 1 1 calc R . . C46 C 0.3741(3) 0.24680(9) 0.56026(16) 0.0185(5) Uani 1 1 d . . . H46A H 0.3045 0.2372 0.6059 0.022 Uiso 1 1 calc R . . H46B H 0.2835 0.2511 0.5113 0.022 Uiso 1 1 calc R . . N47 N 0.5089(3) 0.20758(7) 0.54468(12) 0.0154(4) Uani 1 1 d . . . C48 C 0.4445(3) 0.17909(10) 0.47040(15) 0.0196(5) Uani 1 1 d . . . H48A H 0.3163 0.1675 0.4737 0.023 Uiso 1 1 calc R . . H48B H 0.5260 0.1507 0.4670 0.023 Uiso 1 1 calc R . . C49 C 0.4489(3) 0.21006(10) 0.39509(15) 0.0188(5) Uani 1 1 d . . . H49A H 0.3497 0.2347 0.3935 0.023 Uiso 1 1 calc R . . H49B H 0.4240 0.1897 0.3459 0.023 Uiso 1 1 calc R . . C50 C 0.7447(3) 0.20799(10) 0.33433(15) 0.0199(5) Uani 1 1 d . . . H50 H 0.7501 0.1734 0.3513 0.024 Uiso 1 1 calc R . . C51 C 0.9449(4) 0.22574(11) 0.33694(18) 0.0265(6) Uani 1 1 d . . . H51A H 0.9455 0.2586 0.3155 0.040 Uiso 1 1 calc R . . H51B H 1.0140 0.2046 0.3037 0.040 Uiso 1 1 calc R . . H51C H 1.0037 0.2254 0.3933 0.040 Uiso 1 1 calc R . . C52 C 0.6519(4) 0.20967(12) 0.24647(17) 0.0309(7) Uani 1 1 d . . . H52A H 0.5226 0.1989 0.2448 0.046 Uiso 1 1 calc R . . H52B H 0.7188 0.1884 0.2124 0.046 Uiso 1 1 calc R . . H52C H 0.6548 0.2427 0.2259 0.046 Uiso 1 1 calc R . . C53 C 0.7597(3) 0.33777(9) 0.55227(16) 0.0194(5) Uani 1 1 d . . . H53A H 0.7759 0.3380 0.6126 0.023 Uiso 1 1 calc R . . H53B H 0.7196 0.3703 0.5332 0.023 Uiso 1 1 calc R . . C54 C 0.9445(3) 0.32523(9) 0.52075(15) 0.0181(5) Uani 1 1 d . . . O55 O 1.0629(3) 0.35632(7) 0.51617(12) 0.0252(4) Uani 1 1 d . . . O56 O 0.9635(2) 0.28025(6) 0.50231(11) 0.0176(4) Uani 1 1 d . . . C57 C 0.5612(4) 0.17818(9) 0.61933(16) 0.0199(5) Uani 1 1 d . . . H57A H 0.6073 0.1463 0.6040 0.024 Uiso 1 1 calc R . . H57B H 0.4510 0.1732 0.6488 0.024 Uiso 1 1 calc R . . C58 C 0.7125(3) 0.20444(9) 0.67421(16) 0.0192(5) Uani 1 1 d . . . O59 O 0.7375(3) 0.19561(7) 0.74726(11) 0.0261(4) Uani 1 1 d . . . O60 O 0.8099(2) 0.23485(6) 0.63703(11) 0.0189(4) Uani 1 1 d . . . N71 N 0.8779(3) 0.17421(8) 0.50461(14) 0.0225(5) Uani 1 1 d . . . N72 N 1.0033(3) 0.15763(8) 0.54944(14) 0.0196(4) Uani 1 1 d . . . N73 N 1.1243(3) 0.14014(10) 0.58915(17) 0.0353(6) Uani 1 1 d . . . O80 O 1.1467(3) 0.38030(8) 0.35557(13) 0.0335(5) Uani 1 1 d D . . H80A H 1.128(5) 0.3675(14) 0.4013(17) 0.050 Uiso 1 1 d D . . H80B H 1.121(5) 0.3547(11) 0.327(2) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01021(17) 0.00911(16) 0.01292(17) 0.00062(14) 0.00100(13) -0.00055(13) N1 0.0123(9) 0.0130(9) 0.0125(9) 0.0001(7) 0.0005(7) 0.0006(7) C2 0.0124(11) 0.0197(12) 0.0166(11) 0.0009(9) 0.0006(9) 0.0022(9) C3 0.0142(11) 0.0173(12) 0.0199(12) 0.0048(9) 0.0008(9) 0.0043(9) N4 0.0140(9) 0.0137(10) 0.0154(9) 0.0036(7) 0.0017(7) 0.0012(7) C5 0.0146(11) 0.0177(12) 0.0146(11) 0.0006(9) -0.0006(9) -0.0016(9) C6 0.0192(11) 0.0141(11) 0.0109(10) -0.0013(8) 0.0013(9) -0.0011(9) N7 0.0132(9) 0.0112(9) 0.0121(9) -0.0002(7) 0.0006(7) -0.0015(7) C8 0.0136(10) 0.0127(10) 0.0129(10) 0.0019(8) 0.0027(8) -0.0035(8) C9 0.0157(11) 0.0132(11) 0.0131(11) 0.0020(9) 0.0019(9) -0.0016(9) C10 0.0204(12) 0.0134(11) 0.0184(12) -0.0019(9) 0.0034(9) 0.0006(9) C11 0.0274(14) 0.0253(14) 0.0249(14) -0.0047(11) 0.0101(11) 0.0009(11) C12 0.0273(14) 0.0249(14) 0.0194(12) -0.0084(11) 0.0014(10) -0.0020(11) C13 0.0167(11) 0.0204(12) 0.0167(12) 0.0070(10) 0.0020(9) 0.0004(9) C14 0.0182(11) 0.0100(10) 0.0153(11) -0.0008(9) 0.0015(9) -0.0037(9) O15 0.0231(9) 0.0214(9) 0.0160(8) 0.0012(7) 0.0056(7) -0.0054(7) O16 0.0141(8) 0.0163(8) 0.0167(8) 0.0034(7) 0.0028(6) 0.0004(7) C17 0.0151(11) 0.0127(11) 0.0181(11) 0.0011(9) 0.0032(9) 0.0017(9) C18 0.0137(11) 0.0169(11) 0.0151(11) 0.0028(9) 0.0041(9) -0.0016(9) O19 0.0145(8) 0.0210(9) 0.0203(9) 0.0049(7) -0.0025(7) 0.0027(7) O20 0.0128(8) 0.0161(8) 0.0151(8) 0.0002(7) -0.0021(6) -0.0003(6) N31 0.0179(10) 0.0114(9) 0.0280(12) -0.0005(8) 0.0046(9) -0.0024(8) N32 0.0195(10) 0.0102(9) 0.0185(10) -0.0014(8) 0.0019(8) 0.0023(8) N33 0.0225(11) 0.0198(12) 0.0367(14) -0.0035(10) 0.0082(10) -0.0061(9) Cr2 0.01060(17) 0.01075(17) 0.01797(19) 0.00053(15) -0.00165(14) 0.00099(14) N41 0.0115(9) 0.0190(10) 0.0186(10) 0.0023(8) -0.0003(8) -0.0007(8) C42 0.0163(11) 0.0198(13) 0.0216(13) 0.0078(10) 0.0004(9) 0.0007(10) C43 0.0152(11) 0.0174(12) 0.0252(13) 0.0100(10) 0.0019(10) 0.0046(9) N44 0.0140(9) 0.0139(10) 0.0211(10) 0.0038(8) 0.0039(8) 0.0016(8) C45 0.0182(12) 0.0168(12) 0.0247(13) 0.0011(10) 0.0071(10) 0.0032(10) C46 0.0155(11) 0.0184(12) 0.0222(13) 0.0046(10) 0.0045(9) 0.0021(9) N47 0.0148(9) 0.0135(10) 0.0173(10) 0.0027(8) -0.0010(8) -0.0012(8) C48 0.0158(11) 0.0217(13) 0.0206(12) -0.0001(10) -0.0007(9) -0.0053(10) C49 0.0131(11) 0.0236(13) 0.0187(12) 0.0010(10) -0.0028(9) -0.0045(10) C50 0.0180(12) 0.0222(13) 0.0198(12) -0.0016(10) 0.0032(10) -0.0003(10) C51 0.0180(12) 0.0305(15) 0.0321(15) -0.0087(12) 0.0072(11) -0.0008(11) C52 0.0279(15) 0.0460(19) 0.0186(13) 0.0001(13) 0.0016(11) -0.0022(13) C53 0.0218(12) 0.0116(11) 0.0252(13) -0.0020(10) 0.0044(10) -0.0001(9) C54 0.0184(12) 0.0180(12) 0.0174(12) -0.0024(9) 0.0005(9) -0.0020(10) O55 0.0241(10) 0.0229(10) 0.0295(10) -0.0061(8) 0.0076(8) -0.0098(8) O56 0.0113(8) 0.0160(8) 0.0256(9) -0.0036(7) 0.0022(7) -0.0006(7) C57 0.0223(12) 0.0167(12) 0.0198(12) 0.0061(10) -0.0022(10) 0.0000(10) C58 0.0208(12) 0.0159(12) 0.0199(12) 0.0020(10) -0.0021(10) 0.0044(10) O59 0.0305(10) 0.0286(11) 0.0177(9) 0.0036(8) -0.0037(8) 0.0034(8) O60 0.0185(8) 0.0171(9) 0.0197(9) -0.0008(7) -0.0039(7) -0.0011(7) N71 0.0245(11) 0.0162(11) 0.0245(11) -0.0023(9) -0.0077(9) 0.0077(9) N72 0.0169(10) 0.0172(10) 0.0255(11) 0.0059(9) 0.0054(9) -0.0005(8) N73 0.0205(12) 0.0431(16) 0.0412(15) 0.0235(13) -0.0018(11) 0.0038(11) O80 0.0409(12) 0.0325(12) 0.0279(11) 0.0097(9) 0.0072(10) 0.0141(10) _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 O20 1.9514(16) . ? Cr1 O16 1.9642(16) . ? Cr1 N31 2.021(2) . ? Cr1 N7 2.067(2) . ? Cr1 N4 2.073(2) . ? Cr1 N1 2.1249(19) . ? N1 C9 1.505(3) . ? N1 C2 1.521(3) . ? N1 C10 1.524(3) . ? C2 C3 1.525(3) . ? C3 N4 1.496(3) . ? N4 C13 1.487(3) . ? N4 C5 1.515(3) . ? C5 C6 1.520(3) . ? C6 N7 1.490(3) . ? N7 C17 1.492(3) . ? N7 C8 1.508(3) . ? C8 C9 1.514(3) . ? C10 C12 1.529(4) . ? C10 C11 1.539(3) . ? C13 C14 1.533(3) . ? C14 O15 1.223(3) . ? C14 O16 1.305(3) . ? C17 C18 1.533(3) . ? C18 O19 1.224(3) . ? C18 O20 1.298(3) . ? N31 N32 1.200(3) . ? N32 N33 1.158(3) . ? Cr2 O60 1.9632(18) . ? Cr2 O56 1.9636(17) . ? Cr2 N71 1.984(2) . ? Cr2 N47 2.058(2) . ? Cr2 N44 2.073(2) . ? Cr2 N41 2.132(2) . ? N41 C42 1.500(3) . ? N41 C49 1.522(3) . ? N41 C50 1.527(3) . ? C42 C43 1.521(4) . ? C43 N44 1.502(3) . ? N44 C53 1.488(3) . ? N44 C45 1.499(3) . ? C45 C46 1.526(4) . ? C46 N47 1.504(3) . ? N47 C48 1.491(3) . ? N47 C57 1.492(3) . ? C48 C49 1.516(4) . ? C50 C51 1.528(3) . ? C50 C52 1.531(4) . ? C53 C54 1.529(3) . ? C54 O55 1.225(3) . ? C54 O56 1.297(3) . ? C57 C58 1.527(4) . ? C58 O59 1.225(3) . ? C58 O60 1.298(3) . ? N71 N72 1.197(3) . ? N72 N73 1.143(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O20 Cr1 O16 93.03(7) . . ? O20 Cr1 N31 99.57(8) . . ? O16 Cr1 N31 91.18(8) . . ? O20 Cr1 N7 82.84(7) . . ? O16 Cr1 N7 91.49(7) . . ? N31 Cr1 N7 176.30(8) . . ? O20 Cr1 N4 165.16(8) . . ? O16 Cr1 N4 81.79(7) . . ? N31 Cr1 N4 94.45(8) . . ? N7 Cr1 N4 83.41(8) . . ? O20 Cr1 N1 98.83(7) . . ? O16 Cr1 N1 167.19(7) . . ? N31 Cr1 N1 91.61(8) . . ? N7 Cr1 N1 85.23(8) . . ? N4 Cr1 N1 85.52(7) . . ? C9 N1 C2 111.05(18) . . ? C9 N1 C10 111.02(18) . . ? C2 N1 C10 108.91(18) . . ? C9 N1 Cr1 102.17(13) . . ? C2 N1 Cr1 106.01(13) . . ? C10 N1 Cr1 117.45(14) . . ? N1 C2 C3 112.05(19) . . ? N4 C3 C2 109.09(19) . . ? C13 N4 C3 114.90(19) . . ? C13 N4 C5 111.26(19) . . ? C3 N4 C5 111.30(18) . . ? C13 N4 Cr1 104.47(14) . . ? C3 N4 Cr1 103.97(14) . . ? C5 N4 Cr1 110.42(14) . . ? N4 C5 C6 110.63(18) . . ? N7 C6 C5 109.07(19) . . ? C6 N7 C17 112.46(18) . . ? C6 N7 C8 110.70(17) . . ? C17 N7 C8 112.30(18) . . ? C6 N7 Cr1 107.05(14) . . ? C17 N7 Cr1 105.01(14) . . ? C8 N7 Cr1 108.96(14) . . ? N7 C8 C9 111.69(18) . . ? N1 C9 C8 110.77(18) . . ? N1 C10 C12 112.6(2) . . ? N1 C10 C11 112.9(2) . . ? C12 C10 C11 109.8(2) . . ? N4 C13 C14 110.29(19) . . ? O15 C14 O16 124.7(2) . . ? O15 C14 C13 119.7(2) . . ? O16 C14 C13 115.5(2) . . ? C14 O16 Cr1 114.81(15) . . ? N7 C17 C18 110.69(19) . . ? O19 C18 O20 125.2(2) . . ? O19 C18 C17 119.6(2) . . ? O20 C18 C17 115.1(2) . . ? C18 O20 Cr1 116.63(15) . . ? N32 N31 Cr1 125.04(17) . . ? N33 N32 N31 176.6(3) . . ? O60 Cr2 O56 94.72(7) . . ? O60 Cr2 N71 92.39(8) . . ? O56 Cr2 N71 99.47(9) . . ? O60 Cr2 N47 81.56(8) . . ? O56 Cr2 N47 165.55(8) . . ? N71 Cr2 N47 94.64(9) . . ? O60 Cr2 N44 92.03(8) . . ? O56 Cr2 N44 82.08(8) . . ? N71 Cr2 N44 175.18(9) . . ? N47 Cr2 N44 84.10(8) . . ? O60 Cr2 N41 167.16(8) . . ? O56 Cr2 N41 97.22(8) . . ? N71 Cr2 N41 90.29(9) . . ? N47 Cr2 N41 85.71(8) . . ? N44 Cr2 N41 84.97(8) . . ? C42 N41 C49 110.78(18) . . ? C42 N41 C50 112.15(19) . . ? C49 N41 C50 107.97(19) . . ? C42 N41 Cr2 103.14(15) . . ? C49 N41 Cr2 105.64(14) . . ? C50 N41 Cr2 116.93(14) . . ? N41 C42 C43 110.5(2) . . ? N44 C43 C42 112.42(19) . . ? C53 N44 C45 112.8(2) . . ? C53 N44 C43 112.08(19) . . ? C45 N44 C43 111.10(19) . . ? C53 N44 Cr2 105.24(14) . . ? C45 N44 Cr2 106.12(15) . . ? C43 N44 Cr2 109.04(15) . . ? N44 C45 C46 108.4(2) . . ? N47 C46 C45 111.62(19) . . ? C48 N47 C57 114.6(2) . . ? C48 N47 C46 112.12(19) . . ? C57 N47 C46 111.34(19) . . ? C48 N47 Cr2 103.56(15) . . ? C57 N47 Cr2 104.47(14) . . ? C46 N47 Cr2 110.06(15) . . ? N47 C48 C49 109.9(2) . . ? C48 C49 N41 111.51(19) . . ? N41 C50 C51 112.4(2) . . ? N41 C50 C52 113.3(2) . . ? C51 C50 C52 109.3(2) . . ? N44 C53 C54 110.2(2) . . ? O55 C54 O56 124.8(2) . . ? O55 C54 C53 120.3(2) . . ? O56 C54 C53 114.8(2) . . ? C54 O56 Cr2 116.95(15) . . ? N47 C57 C58 109.1(2) . . ? O59 C58 O60 124.7(2) . . ? O59 C58 C57 120.4(2) . . ? O60 C58 C57 114.9(2) . . ? C58 O60 Cr2 115.92(15) . . ? N72 N71 Cr2 125.92(19) . . ? N73 N72 N71 176.5(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.476 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.084 #####################END Compound 5################# #####################Compound 6##################### data_Cpd6 _database_code_depnum_ccdc_archive 'CCDC 667807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L3CrN3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H25 Cr N6 O5' _chemical_formula_weight 457.44 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.2255(6) _cell_length_b 9.4894(4) _cell_length_c 30.5577(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3835.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38769 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5586 _reflns_number_gt 4275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+6.0778P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5586 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.55937(3) 0.35913(4) 0.159109(11) 0.00809(9) Uani 1 1 d . . . N1 N 0.41678(15) 0.2889(2) 0.13622(6) 0.0100(4) Uani 1 1 d . . . C2 C 0.37617(19) 0.1845(2) 0.16902(7) 0.0120(5) Uani 1 1 d . . . H2A H 0.3898 0.0875 0.1586 0.014 Uiso 1 1 calc R . . H2B H 0.3020 0.1962 0.1717 0.014 Uiso 1 1 calc R . . C3 C 0.42523(18) 0.2060(2) 0.21362(7) 0.0121(5) Uani 1 1 d . . . H3A H 0.4000 0.2943 0.2270 0.014 Uiso 1 1 calc R . . H3B H 0.4074 0.1268 0.2332 0.014 Uiso 1 1 calc R . . N4 N 0.53781(15) 0.2136(2) 0.20838(6) 0.0099(4) Uani 1 1 d . . . C5 C 0.58259(19) 0.0739(2) 0.19485(8) 0.0122(5) Uani 1 1 d . . . H5A H 0.5277 0.0100 0.1853 0.015 Uiso 1 1 calc R . . H5B H 0.6166 0.0302 0.2203 0.015 Uiso 1 1 calc R . . C6 C 0.65857(18) 0.0916(2) 0.15775(8) 0.0116(4) Uani 1 1 d . . . H6A H 0.7229 0.1295 0.1694 0.014 Uiso 1 1 calc R . . H6B H 0.6726 -0.0010 0.1441 0.014 Uiso 1 1 calc R . . N7 N 0.61602(15) 0.1907(2) 0.12428(6) 0.0099(4) Uani 1 1 d . . . C8 C 0.53253(19) 0.1226(2) 0.09833(8) 0.0131(5) Uani 1 1 d . . . H8A H 0.5108 0.0351 0.1133 0.016 Uiso 1 1 calc R . . H8B H 0.5583 0.0967 0.0690 0.016 Uiso 1 1 calc R . . C9 C 0.4419(2) 0.2209(2) 0.09326(7) 0.0121(5) Uani 1 1 d . . . H9A H 0.4575 0.2945 0.0713 0.015 Uiso 1 1 calc R . . H9B H 0.3828 0.1667 0.0827 0.015 Uiso 1 1 calc R . . C10 C 0.34383(19) 0.4108(2) 0.12989(8) 0.0118(4) Uani 1 1 d . . . H10A H 0.3181 0.4397 0.1590 0.014 Uiso 1 1 calc R . . H10B H 0.3819 0.4915 0.1176 0.014 Uiso 1 1 calc R . . C11 C 0.25454(19) 0.3817(2) 0.10058(7) 0.0113(4) Uani 1 1 d . . . C12 C 0.25656(19) 0.4297(2) 0.05696(8) 0.0131(5) Uani 1 1 d . . . H12 H 0.3145 0.4786 0.0465 0.016 Uiso 1 1 calc R . . C13 C 0.1759(2) 0.4072(3) 0.02900(8) 0.0151(5) Uani 1 1 d . . . H13 H 0.1782 0.4425 -0.0001 0.018 Uiso 1 1 calc R . . C14 C 0.09144(19) 0.3329(2) 0.04334(8) 0.0131(5) Uani 1 1 d . . . C15 C 0.08618(19) 0.2855(3) 0.08651(8) 0.0140(5) Uani 1 1 d . . . H15 H 0.0284 0.2359 0.0967 0.017 Uiso 1 1 calc R . . C16 C 0.16757(19) 0.3124(3) 0.11462(8) 0.0135(5) Uani 1 1 d . . . H16 H 0.1633 0.2824 0.1442 0.016 Uiso 1 1 calc R . . O17 O 0.01557(14) 0.3154(2) 0.01327(6) 0.0188(4) Uani 1 1 d . . . C18 C -0.0748(2) 0.2474(3) 0.02802(9) 0.0250(6) Uani 1 1 d . . . H18A H -0.0596 0.1496 0.0359 0.037 Uiso 1 1 calc R . . H18B H -0.1254 0.2490 0.0046 0.037 Uiso 1 1 calc R . . H18C H -0.1013 0.2972 0.0537 0.037 Uiso 1 1 calc R . . C19 C 0.59152(19) 0.2745(2) 0.24681(7) 0.0123(5) Uani 1 1 d . . . H19A H 0.6150 0.1973 0.2661 0.015 Uiso 1 1 calc R . . H19B H 0.5441 0.3339 0.2638 0.015 Uiso 1 1 calc R . . C20 C 0.68199(18) 0.3632(2) 0.23252(8) 0.0115(4) Uani 1 1 d . . . O21 O 0.74068(14) 0.40667(18) 0.26022(6) 0.0176(4) Uani 1 1 d . . . O22 O 0.68738(13) 0.38922(17) 0.19073(5) 0.0118(3) Uani 1 1 d . . . C23 C 0.69550(19) 0.2536(2) 0.09592(8) 0.0128(5) Uani 1 1 d . . . H23A H 0.7053 0.1940 0.0697 0.015 Uiso 1 1 calc R . . H23B H 0.7603 0.2572 0.1121 0.015 Uiso 1 1 calc R . . C24 C 0.6652(2) 0.4031(2) 0.08180(8) 0.0141(5) Uani 1 1 d . . . O25 O 0.70744(16) 0.4585(2) 0.05096(6) 0.0238(4) Uani 1 1 d . . . O26 O 0.59673(13) 0.46309(17) 0.10643(5) 0.0121(3) Uani 1 1 d . . . N31 N 0.50126(16) 0.5297(2) 0.18950(6) 0.0123(4) Uani 1 1 d . . . N32 N 0.54215(16) 0.6403(2) 0.18006(6) 0.0135(4) Uani 1 1 d . . . N33 N 0.57923(18) 0.7478(2) 0.17218(7) 0.0194(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.00891(17) 0.00693(15) 0.00845(15) 0.00014(13) 0.00062(14) -0.00059(14) N1 0.0098(10) 0.0103(9) 0.0099(9) 0.0004(7) -0.0004(7) 0.0007(7) C2 0.0118(12) 0.0114(10) 0.0127(11) 0.0023(8) 0.0005(9) -0.0029(9) C3 0.0124(13) 0.0115(10) 0.0124(10) 0.0013(8) 0.0005(9) -0.0014(9) N4 0.0100(10) 0.0092(9) 0.0104(9) 0.0006(7) -0.0006(7) -0.0005(7) C5 0.0116(12) 0.0107(10) 0.0143(10) 0.0023(8) 0.0016(9) 0.0004(9) C6 0.0099(11) 0.0108(10) 0.0141(10) 0.0026(9) 0.0000(10) 0.0036(8) N7 0.0094(10) 0.0089(9) 0.0115(9) -0.0016(7) -0.0002(8) -0.0001(7) C8 0.0120(12) 0.0114(11) 0.0158(11) -0.0034(9) 0.0017(9) 0.0017(9) C9 0.0141(12) 0.0122(11) 0.0100(10) -0.0022(8) 0.0001(9) 0.0012(9) C10 0.0106(12) 0.0106(10) 0.0142(11) -0.0007(9) 0.0000(9) 0.0013(9) C11 0.0109(11) 0.0097(10) 0.0134(10) 0.0007(8) 0.0009(9) 0.0027(8) C12 0.0109(12) 0.0138(11) 0.0145(11) 0.0010(9) 0.0031(9) -0.0005(9) C13 0.0160(13) 0.0181(12) 0.0113(11) 0.0018(9) 0.0007(10) 0.0011(10) C14 0.0110(12) 0.0139(11) 0.0144(11) -0.0002(8) -0.0011(9) 0.0014(9) C15 0.0103(12) 0.0166(12) 0.0151(11) 0.0032(9) 0.0027(9) -0.0003(9) C16 0.0114(12) 0.0159(11) 0.0133(11) 0.0033(9) 0.0015(9) 0.0031(9) O17 0.0129(9) 0.0288(10) 0.0148(9) 0.0026(7) -0.0031(7) -0.0068(8) C18 0.0148(15) 0.0396(17) 0.0205(13) 0.0045(12) -0.0010(11) -0.0111(12) C19 0.0130(12) 0.0133(11) 0.0106(10) 0.0025(8) -0.0003(9) -0.0015(9) C20 0.0100(11) 0.0096(10) 0.0148(10) -0.0005(9) -0.0011(9) 0.0006(9) O21 0.0147(10) 0.0199(9) 0.0181(9) -0.0009(7) -0.0034(8) -0.0025(7) O22 0.0101(9) 0.0122(8) 0.0130(8) 0.0006(6) -0.0001(7) -0.0025(6) C23 0.0115(12) 0.0129(11) 0.0140(11) -0.0009(9) 0.0048(9) -0.0005(9) C24 0.0157(13) 0.0115(10) 0.0152(11) -0.0001(9) 0.0007(10) -0.0022(9) O25 0.0310(12) 0.0182(9) 0.0222(10) 0.0066(8) 0.0152(9) 0.0016(8) O26 0.0141(9) 0.0102(8) 0.0120(8) 0.0007(6) 0.0023(7) 0.0008(6) N31 0.0127(11) 0.0095(9) 0.0147(9) -0.0029(7) 0.0028(8) 0.0001(8) N32 0.0137(11) 0.0141(9) 0.0126(9) -0.0019(8) -0.0002(8) 0.0022(8) N33 0.0258(14) 0.0127(10) 0.0196(10) -0.0022(8) 0.0035(9) -0.0026(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O26 1.9515(16) . ? Cr1 O22 1.9702(17) . ? Cr1 N31 2.0182(19) . ? Cr1 N7 2.0612(19) . ? Cr1 N4 2.0628(19) . ? Cr1 N1 2.119(2) . ? N1 C9 1.500(3) . ? N1 C2 1.508(3) . ? N1 C10 1.518(3) . ? C2 C3 1.523(3) . ? C3 N4 1.499(3) . ? N4 C19 1.489(3) . ? N4 C5 1.510(3) . ? C5 C6 1.524(3) . ? C6 N7 1.499(3) . ? N7 C23 1.488(3) . ? N7 C8 1.505(3) . ? C8 C9 1.527(3) . ? C10 C11 1.508(3) . ? C11 C16 1.393(3) . ? C11 C12 1.409(3) . ? C12 C13 1.383(3) . ? C13 C14 1.392(4) . ? C14 O17 1.371(3) . ? C14 C15 1.396(3) . ? C15 C16 1.400(3) . ? O17 C18 1.431(3) . ? C19 C20 1.527(3) . ? C20 O21 1.220(3) . ? C20 O22 1.302(3) . ? C23 C24 1.536(3) . ? C24 O25 1.215(3) . ? C24 O26 1.308(3) . ? N31 N32 1.216(3) . ? N32 N33 1.156(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O26 Cr1 O22 96.53(7) . . ? O26 Cr1 N31 94.04(7) . . ? O22 Cr1 N31 89.16(8) . . ? O26 Cr1 N7 82.77(7) . . ? O22 Cr1 N7 93.06(7) . . ? N31 Cr1 N7 176.30(8) . . ? O26 Cr1 N4 167.28(7) . . ? O22 Cr1 N4 81.82(7) . . ? N31 Cr1 N4 98.54(8) . . ? N7 Cr1 N4 84.72(8) . . ? O26 Cr1 N1 96.43(7) . . ? O22 Cr1 N1 166.48(7) . . ? N31 Cr1 N1 93.73(8) . . ? N7 Cr1 N1 84.79(8) . . ? N4 Cr1 N1 84.69(8) . . ? C9 N1 C2 112.19(17) . . ? C9 N1 C10 110.89(17) . . ? C2 N1 C10 111.02(18) . . ? C9 N1 Cr1 103.14(14) . . ? C2 N1 Cr1 107.71(14) . . ? C10 N1 Cr1 111.60(14) . . ? N1 C2 C3 110.79(19) . . ? N4 C3 C2 109.51(19) . . ? C19 N4 C3 114.10(18) . . ? C19 N4 C5 111.68(18) . . ? C3 N4 C5 112.12(18) . . ? C19 N4 Cr1 104.48(13) . . ? C3 N4 Cr1 104.32(13) . . ? C5 N4 Cr1 109.50(13) . . ? N4 C5 C6 111.46(18) . . ? N7 C6 C5 109.20(19) . . ? C23 N7 C6 112.59(19) . . ? C23 N7 C8 112.57(18) . . ? C6 N7 C8 111.44(18) . . ? C23 N7 Cr1 104.25(14) . . ? C6 N7 Cr1 105.71(14) . . ? C8 N7 Cr1 109.77(14) . . ? N7 C8 C9 111.56(18) . . ? N1 C9 C8 110.34(18) . . ? C11 C10 N1 115.71(18) . . ? C16 C11 C12 117.4(2) . . ? C16 C11 C10 123.4(2) . . ? C12 C11 C10 119.2(2) . . ? C13 C12 C11 121.3(2) . . ? C12 C13 C14 120.2(2) . . ? O17 C14 C13 116.0(2) . . ? O17 C14 C15 123.9(2) . . ? C13 C14 C15 120.0(2) . . ? C14 C15 C16 118.9(2) . . ? C11 C16 C15 122.1(2) . . ? C14 O17 C18 117.1(2) . . ? N4 C19 C20 111.23(18) . . ? O21 C20 O22 125.5(2) . . ? O21 C20 C19 119.1(2) . . ? O22 C20 C19 115.3(2) . . ? C20 O22 Cr1 113.98(15) . . ? N7 C23 C24 110.50(19) . . ? O25 C24 O26 125.2(2) . . ? O25 C24 C23 119.9(2) . . ? O26 C24 C23 114.9(2) . . ? C24 O26 Cr1 115.46(15) . . ? N32 N31 Cr1 114.46(16) . . ? N33 N32 N31 177.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.410 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.087 #####################END Compound 6################# #####################Compound 9##################### data_Cpd9 _database_code_depnum_ccdc_archive 'CCDC 667808' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'L3Cr(OH)0.3(N)0.7, 3(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H31.27 Cr N3.72 O8.27' _chemical_formula_weight 484.29 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.8409(10) _cell_length_b 6.7077(2) _cell_length_c 18.7774(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.07(3) _cell_angle_gamma 90.00 _cell_volume 4230.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour grey-violet _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9107 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38270 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 31.07 _reflns_number_total 6773 _reflns_number_gt 5182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+20.5016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6773 _refine_ls_number_parameters 290 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.16902(3) 0.74113(18) 0.04210(5) 0.00455(11) Uiso 0.73 1 d P A 1 N31 N 0.1995(2) 0.8069(11) -0.0112(4) 0.0101(6) Uiso 0.73 1 d P A 1 Cr1A Cr 0.16467(7) 0.7368(5) 0.04741(13) 0.00455(11) Uiso 0.27 1 d P A 2 O31A O 0.1991(5) 0.819(3) -0.0175(9) 0.0101(6) Uiso 0.27 1 d P A 2 H31A H 0.2090 0.9302 -0.0047 0.015 Uiso 0.27 1 calc PR A 2 N1 N 0.15229(6) 0.4710(3) -0.01179(11) 0.0068(4) Uani 1 1 d . . . C2 C 0.18121(8) 0.3136(4) 0.01952(13) 0.0085(5) Uani 1 1 d . A . H2A H 0.1891 0.2295 -0.0197 0.010 Uiso 1 1 calc R . . H2B H 0.1679 0.2268 0.0520 0.010 Uiso 1 1 calc R . . C3 C 0.21848(8) 0.4056(4) 0.06124(13) 0.0087(5) Uani 1 1 d . . . H3A H 0.2341 0.3014 0.0894 0.010 Uiso 1 1 calc R A . H3B H 0.2354 0.4656 0.0275 0.010 Uiso 1 1 calc R . . N4 N 0.20578(6) 0.5620(3) 0.11028(11) 0.0072(4) Uani 1 1 d . A . C5 C 0.18595(8) 0.4705(4) 0.17034(13) 0.0087(5) Uani 1 1 d . . . H5A H 0.2048 0.4716 0.2150 0.010 Uiso 1 1 calc R A . H5B H 0.1792 0.3299 0.1584 0.010 Uiso 1 1 calc R . . C6 C 0.14832(8) 0.5821(4) 0.18312(13) 0.0089(5) Uani 1 1 d . A . H6A H 0.1328 0.5016 0.2140 0.011 Uiso 1 1 calc R . . H6B H 0.1554 0.7098 0.2078 0.011 Uiso 1 1 calc R . . N7 N 0.12422(6) 0.6206(3) 0.11304(11) 0.0076(4) Uani 1 1 d . . . C8 C 0.10576(8) 0.4362(4) 0.08053(13) 0.0094(5) Uani 1 1 d . A . H8A H 0.0771 0.4351 0.0862 0.011 Uiso 1 1 calc R . . H8B H 0.1183 0.3187 0.1061 0.011 Uiso 1 1 calc R . . C9 C 0.11068(8) 0.4212(4) 0.00098(13) 0.0088(5) Uani 1 1 d . A . H9A H 0.1041 0.2842 -0.0162 0.011 Uiso 1 1 calc R . . H9B H 0.0919 0.5140 -0.0267 0.011 Uiso 1 1 calc R . . C10 C 0.15411(8) 0.4919(4) -0.09220(13) 0.0093(5) Uani 1 1 d . A . H10A H 0.1376 0.6075 -0.1103 0.011 Uiso 1 1 calc R . . H10B H 0.1819 0.5204 -0.1001 0.011 Uiso 1 1 calc R . . C11 C 0.13995(8) 0.3102(4) -0.13506(13) 0.0089(5) Uani 1 1 d . . . C12 C 0.09955(8) 0.2820(4) -0.15786(13) 0.0100(5) Uani 1 1 d . A . H12 H 0.0811 0.3826 -0.1484 0.012 Uiso 1 1 calc R . . C13 C 0.08547(8) 0.1097(4) -0.19421(14) 0.0113(5) Uani 1 1 d . . . H13 H 0.0578 0.0926 -0.2088 0.014 Uiso 1 1 calc R A . C14 C 0.11243(8) -0.0367(4) -0.20883(13) 0.0099(5) Uani 1 1 d . A . C15 C 0.15318(8) -0.0080(4) -0.18957(14) 0.0111(5) Uani 1 1 d . . . H15 H 0.1717 -0.1056 -0.2012 0.013 Uiso 1 1 calc R A . C16 C 0.16645(8) 0.1640(4) -0.15333(13) 0.0109(5) Uani 1 1 d . A . H16 H 0.1942 0.1832 -0.1406 0.013 Uiso 1 1 calc R . . O17 O 0.10147(6) -0.2112(3) -0.24319(11) 0.0160(4) Uani 1 1 d . . . C18 C 0.05984(9) -0.2555(5) -0.25635(16) 0.0196(6) Uani 1 1 d . A . H18A H 0.0560 -0.3839 -0.2812 0.029 Uiso 1 1 calc R . . H18B H 0.0462 -0.1506 -0.2863 0.029 Uiso 1 1 calc R . . H18C H 0.0488 -0.2624 -0.2106 0.029 Uiso 1 1 calc R . . C19 C 0.23809(8) 0.7006(4) 0.13915(14) 0.0091(5) Uani 1 1 d . . . H19A H 0.2578 0.7133 0.1045 0.011 Uiso 1 1 calc R A . H19B H 0.2520 0.6473 0.1847 0.011 Uiso 1 1 calc R . . C20 C 0.22029(8) 0.9054(4) 0.15232(14) 0.0103(5) Uani 1 1 d . A . O21 O 0.24023(7) 1.0295(3) 0.18842(11) 0.0190(5) Uani 1 1 d . . . O22 O 0.18442(6) 0.9352(3) 0.12039(9) 0.0085(4) Uani 1 1 d . . . C23 C 0.09555(8) 0.7848(4) 0.11478(13) 0.0102(5) Uani 1 1 d . A . H23A H 0.1051 0.8779 0.1541 0.012 Uiso 1 1 calc R . . H23B H 0.0695 0.7307 0.1244 0.012 Uiso 1 1 calc R . . C24 C 0.09049(8) 0.8966(4) 0.04359(13) 0.0088(5) Uani 1 1 d . . . O25 O 0.05990(6) 0.9977(3) 0.02734(10) 0.0137(4) Uani 1 1 d . A . O26 O 0.11916(6) 0.8866(3) 0.00508(9) 0.0094(4) Uani 1 1 d . A . O40 O 0.01570(9) 0.5628(4) -0.06277(19) 0.0395(7) Uani 1 1 d D . . H40A H -0.0008(11) 0.532(7) -0.045(3) 0.059 Uiso 1 1 d D . . H40B H 0.0125(14) 0.666(4) -0.073(3) 0.059 Uiso 1 1 d D . . O41 O -0.00648(7) 1.0201(4) 0.09774(11) 0.0169(4) Uani 1 1 d D . . H41A H 0.0108(7) 1.009(6) 0.0786(17) 0.025 Uiso 1 1 d D . . H41B H -0.0238(7) 0.997(6) 0.0722(16) 0.025 Uiso 1 1 d D . . O42 O 0.00608(8) 0.6723(4) 0.17978(12) 0.0226(5) Uiso 1 1 d D . . H42A H 0.0012(12) 0.604(4) 0.1502(15) 0.034 Uiso 1 1 d D . . H42B H 0.0037(12) 0.773(3) 0.1657(19) 0.034 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0085(10) 0.0064(9) 0.0051(9) 0.0025(7) -0.0005(8) -0.0006(8) C2 0.0112(12) 0.0059(11) 0.0084(11) 0.0002(9) 0.0013(9) 0.0002(9) C3 0.0085(12) 0.0078(11) 0.0095(11) -0.0011(9) 0.0005(9) 0.0022(9) N4 0.0065(10) 0.0065(9) 0.0085(9) 0.0001(8) 0.0004(8) -0.0006(8) C5 0.0112(12) 0.0086(11) 0.0062(11) 0.0029(9) 0.0009(9) -0.0014(9) C6 0.0106(12) 0.0103(12) 0.0057(10) 0.0024(9) 0.0008(9) -0.0021(10) N7 0.0078(10) 0.0090(10) 0.0058(9) 0.0000(8) 0.0005(8) -0.0013(8) C8 0.0108(12) 0.0082(11) 0.0093(11) 0.0013(9) 0.0012(9) -0.0049(9) C9 0.0088(12) 0.0089(11) 0.0084(11) 0.0000(9) 0.0000(9) -0.0029(9) C10 0.0130(13) 0.0102(12) 0.0046(10) 0.0009(9) 0.0005(9) -0.0021(10) C11 0.0119(12) 0.0098(11) 0.0047(10) 0.0006(9) 0.0002(9) -0.0009(9) C12 0.0128(12) 0.0078(12) 0.0093(11) -0.0038(9) 0.0009(9) 0.0040(9) C13 0.0086(12) 0.0153(13) 0.0097(11) -0.0015(10) -0.0002(9) 0.0009(10) C14 0.0125(13) 0.0088(12) 0.0083(11) -0.0017(9) 0.0012(9) 0.0005(10) C15 0.0117(13) 0.0110(12) 0.0107(11) -0.0008(10) 0.0016(10) 0.0040(10) C16 0.0104(13) 0.0140(12) 0.0079(11) -0.0025(10) -0.0006(9) -0.0001(10) O17 0.0158(10) 0.0109(10) 0.0209(10) -0.0083(8) 0.0002(8) -0.0005(8) C18 0.0181(14) 0.0180(14) 0.0220(14) -0.0080(13) -0.0002(11) -0.0049(13) C19 0.0092(12) 0.0081(12) 0.0094(11) -0.0011(9) -0.0014(9) -0.0013(9) C20 0.0139(13) 0.0076(11) 0.0091(11) 0.0015(9) -0.0004(10) -0.0025(10) O21 0.0211(11) 0.0128(10) 0.0199(10) -0.0043(8) -0.0101(8) -0.0025(8) O22 0.0093(9) 0.0067(8) 0.0089(8) -0.0010(7) -0.0015(7) -0.0003(7) C23 0.0095(12) 0.0119(13) 0.0095(11) 0.0009(9) 0.0025(9) 0.0025(10) C24 0.0092(12) 0.0063(11) 0.0104(11) -0.0001(9) -0.0009(9) -0.0037(9) O25 0.0090(9) 0.0144(10) 0.0177(10) 0.0027(8) 0.0011(8) 0.0038(8) O26 0.0084(9) 0.0101(9) 0.0096(8) 0.0019(7) 0.0009(7) 0.0011(7) O40 0.0387(17) 0.0175(13) 0.060(2) -0.0009(13) -0.0053(14) 0.0028(12) O41 0.0114(10) 0.0238(11) 0.0156(10) 0.0013(9) 0.0019(8) 0.0015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N31 1.585(8) . ? Cr1 O22 1.984(2) . ? Cr1 O26 1.999(2) . ? Cr1 N4 2.059(2) . ? Cr1 N1 2.118(2) . ? Cr1 N7 2.286(2) . ? Cr1A O31A 1.871(17) . ? Cr1A O26 1.927(3) . ? Cr1A O22 1.967(3) . ? Cr1A N4 2.074(3) . ? Cr1A N7 2.101(3) . ? Cr1A N1 2.116(4) . ? N1 C9 1.495(3) . ? N1 C2 1.509(3) . ? N1 C10 1.525(3) . ? C2 C3 1.531(4) . ? C3 N4 1.493(3) . ? N4 C19 1.486(3) . ? N4 C5 1.512(3) . ? C5 C6 1.521(4) . ? C6 N7 1.483(3) . ? N7 C23 1.471(3) . ? N7 C8 1.483(3) . ? C8 C9 1.527(4) . ? C10 C11 1.506(4) . ? C11 C12 1.394(4) . ? C11 C16 1.400(4) . ? C12 C13 1.396(4) . ? C13 C14 1.390(4) . ? C14 O17 1.366(3) . ? C14 C15 1.395(4) . ? C15 C16 1.386(4) . ? O17 C18 1.431(3) . ? C19 C20 1.532(4) . ? C20 O21 1.223(3) . ? C20 O22 1.302(3) . ? C23 C24 1.524(4) . ? C24 O25 1.244(3) . ? C24 O26 1.281(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Cr1 O22 98.9(3) . . ? N31 Cr1 O26 103.3(3) . . ? O22 Cr1 O26 94.06(9) . . ? N31 Cr1 N4 99.5(3) . . ? O22 Cr1 N4 80.72(9) . . ? O26 Cr1 N4 157.07(9) . . ? N31 Cr1 N1 95.3(3) . . ? O22 Cr1 N1 160.96(9) . . ? O26 Cr1 N1 94.99(9) . . ? N4 Cr1 N1 84.45(9) . . ? N31 Cr1 N7 174.8(3) . . ? O22 Cr1 N7 86.15(8) . . ? O26 Cr1 N7 77.48(8) . . ? N4 Cr1 N7 79.89(9) . . ? N1 Cr1 N7 79.53(9) . . ? O31A Cr1A O26 96.2(5) . . ? O31A Cr1A O22 93.9(6) . . ? O26 Cr1A O22 96.91(15) . . ? O31A Cr1A N4 96.3(5) . . ? O26 Cr1A N4 167.42(16) . . ? O22 Cr1A N4 80.75(12) . . ? O31A Cr1A N7 174.2(6) . . ? O26 Cr1A N7 83.69(12) . . ? O22 Cr1A N7 91.85(12) . . ? N4 Cr1A N7 84.03(13) . . ? O31A Cr1A N1 90.3(6) . . ? O26 Cr1A N1 97.25(13) . . ? O22 Cr1A N1 164.68(17) . . ? N4 Cr1A N1 84.15(14) . . ? N7 Cr1A N1 83.93(13) . . ? C9 N1 C2 111.1(2) . . ? C9 N1 C10 109.44(19) . . ? C2 N1 C10 110.3(2) . . ? C9 N1 Cr1A 103.50(16) . . ? C2 N1 Cr1A 107.94(16) . . ? C10 N1 Cr1A 114.40(17) . . ? C9 N1 Cr1 108.42(16) . . ? C2 N1 Cr1 106.86(15) . . ? C10 N1 Cr1 110.69(15) . . ? Cr1A N1 Cr1 5.14(8) . . ? N1 C2 C3 111.8(2) . . ? N4 C3 C2 108.5(2) . . ? C19 N4 C3 114.2(2) . . ? C19 N4 C5 110.86(19) . . ? C3 N4 C5 111.3(2) . . ? C19 N4 Cr1 102.86(15) . . ? C3 N4 Cr1 102.96(15) . . ? C5 N4 Cr1 114.27(16) . . ? C19 N4 Cr1A 105.41(17) . . ? C3 N4 Cr1A 105.66(16) . . ? C5 N4 Cr1A 109.02(17) . . ? Cr1 N4 Cr1A 5.25(8) . . ? N4 C5 C6 112.0(2) . . ? N7 C6 C5 109.0(2) . . ? C23 N7 C6 113.8(2) . . ? C23 N7 C8 112.8(2) . . ? C6 N7 C8 112.2(2) . . ? C23 N7 Cr1A 102.37(17) . . ? C6 N7 Cr1A 104.97(17) . . ? C8 N7 Cr1A 109.87(17) . . ? C23 N7 Cr1 103.57(15) . . ? C6 N7 Cr1 104.30(15) . . ? C8 N7 Cr1 109.35(15) . . ? Cr1A N7 Cr1 1.20(11) . . ? N7 C8 C9 111.5(2) . . ? N1 C9 C8 111.1(2) . . ? C11 C10 N1 113.9(2) . . ? C12 C11 C16 117.6(2) . . ? C12 C11 C10 120.6(2) . . ? C16 C11 C10 121.8(2) . . ? C11 C12 C13 121.7(2) . . ? C14 C13 C12 119.2(2) . . ? O17 C14 C13 123.5(2) . . ? O17 C14 C15 116.3(2) . . ? C13 C14 C15 120.2(2) . . ? C16 C15 C14 119.5(3) . . ? C15 C16 C11 121.6(3) . . ? C14 O17 C18 117.6(2) . . ? N4 C19 C20 109.5(2) . . ? O21 C20 O22 124.8(3) . . ? O21 C20 C19 119.9(2) . . ? O22 C20 C19 115.2(2) . . ? C20 O22 Cr1A 115.78(18) . . ? C20 O22 Cr1 112.69(17) . . ? Cr1A O22 Cr1 5.49(9) . . ? N7 C23 C24 110.6(2) . . ? O25 C24 O26 123.7(2) . . ? O25 C24 C23 118.9(2) . . ? O26 C24 C23 117.3(2) . . ? C24 O26 Cr1A 114.64(17) . . ? C24 O26 Cr1 119.66(16) . . ? Cr1A O26 Cr1 5.13(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.07 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.652 _refine_diff_density_min -0.832 _refine_diff_density_rms 0.107 #####################END Compound 9#################