# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'R. Lescouezec' 'G. Marinescu' 'M. C. Munoz' 'D. Luneau' 'M. Andruh' 'F. Lloret' 'J. Faus' 'M. Julve' 'J. A. Mata' 'R. Llusar' 'J. Cano' _publ_contact_author_name 'M. Julve' #Comp1.cif data_Compound_1_PPh4[Cr(dpa)(ox)2] _database_code_CSD 161709 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety PPh4[Cr(dpa)(ox)2] _chemical_formula_sum 'C38 H29 Cr N3 O8 P' _chemical_formula_weight 738.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2002(11) _cell_length_b 13.4712(16) _cell_length_c 13.7964(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.574(3) _cell_angle_gamma 90.00 _cell_volume 1695.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 1.3 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type Bruker SADABS _exptl_absorpt_correction_T_min 1.463660 _exptl_absorpt_correction_T_max 1.955014 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 CCD area Detector _diffrn_measurement_method phi and omega scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13778 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 30.52 _reflns_number_total 9433 _reflns_number_gt 6924 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker SMART _computing_cell_refinement Bruker SMART _computing_data_reduction Bruker SHELXTL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Bruker SHELXTL _computing_publication_material Bruker SHELXTL _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^)+(0.0331P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.134(12) _refine_ls_number_reflns 9433 _refine_ls_number_parameters 497 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.811 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.004 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 Cr Cr 0.16698(3) 0.82340(2) 0.48711(2) 0.02429(7) Uani 1 1 d . . . N1 N 0.27529(18) 0.94713(13) 0.44348(11) 0.0267(4) Uani 1 1 d . . . C1 C 0.2646(2) 0.75740(17) 0.67208(16) 0.0330(5) Uani 1 1 d . . . O1 O 0.30394(13) 0.81858(13) 0.60814(9) 0.0303(3) Uani 1 1 d . . . P1 P 0.02177(6) 0.68974(4) 0.03450(4) 0.03267(13) Uani 1 1 d . . . N2 N 0.29898(18) 0.73825(13) 0.41082(12) 0.0268(4) Uani 1 1 d . . . O2 O 0.08637(15) 0.70348(11) 0.54101(10) 0.0326(3) Uani 1 1 d . . . C2 C 0.1420(2) 0.68284(18) 0.62959(15) 0.0351(5) Uani 1 1 d . . . N3 N 0.4867(2) 0.85769(14) 0.41587(14) 0.0359(4) Uani 1 1 d . . . H3 H 0.575(3) 0.870(2) 0.4117(18) 0.057(8) Uiso 1 1 d . . . C3 C -0.1079(2) 0.89391(16) 0.50108(16) 0.0340(5) Uani 1 1 d . . . O3 O 0.02163(16) 0.90074(12) 0.54842(10) 0.0327(4) Uani 1 1 d . . . O4 O 0.01351(13) 0.82589(14) 0.37438(8) 0.0316(3) Uani 1 1 d . . . C4 C -0.1115(2) 0.85633(15) 0.39458(15) 0.0313(5) Uani 1 1 d . . . C5 C 0.2076(3) 1.03741(17) 0.44325(16) 0.0343(5) Uani 1 1 d . . . H5 H 0.109(2) 1.0384(16) 0.4463(14) 0.027(6) Uiso 1 1 d . . . O5 O 0.3144(2) 0.75514(14) 0.75807(12) 0.0540(5) Uani 1 1 d . . . C6 C 0.2765(3) 1.12458(19) 0.43028(18) 0.0418(6) Uani 1 1 d . . . H6 H 0.227(3) 1.181(2) 0.4340(17) 0.047(7) Uiso 1 1 d . . . O6 O 0.1077(2) 0.61441(15) 0.67800(13) 0.0673(6) Uani 1 1 d . . . C7 C 0.4230(3) 1.12286(19) 0.41648(18) 0.0416(6) Uani 1 1 d . . . H7 H 0.470(3) 1.177(2) 0.4121(17) 0.044(7) Uiso 1 1 d . . . O7 O -0.22237(18) 0.91267(15) 0.53280(13) 0.0547(5) Uani 1 1 d . . . C8 C 0.4933(3) 1.03405(19) 0.41395(17) 0.0379(5) Uani 1 1 d . . . H8 H 0.584(3) 1.0323(17) 0.4042(16) 0.037(7) Uiso 1 1 d . . . O8 O -0.22648(16) 0.85714(12) 0.33872(11) 0.0473(4) Uani 1 1 d . . . C9 C 0.4154(2) 0.94607(16) 0.42551(14) 0.0295(4) Uani 1 1 d . . . C10 C 0.4309(2) 0.76528(17) 0.39000(15) 0.0308(5) Uani 1 1 d . . . C11 C 0.5174(3) 0.7008(2) 0.34216(19) 0.0464(6) Uani 1 1 d . . . H11 H 0.606(3) 0.7275(18) 0.3241(18) 0.049(7) Uiso 1 1 d . . . C12 C 0.4653(3) 0.6078(2) 0.3173(2) 0.0533(7) Uani 1 1 d . . . H12 H 0.534(3) 0.567(2) 0.290(2) 0.066(8) Uiso 1 1 d . . . C13 C 0.3292(3) 0.5802(2) 0.33785(17) 0.0428(6) Uani 1 1 d . . . H13 H 0.289(3) 0.5126(19) 0.3257(17) 0.049(7) Uiso 1 1 d . . . C14 C 0.2510(3) 0.64604(18) 0.38384(16) 0.0338(5) Uani 1 1 d . . . H14 H 0.174(2) 0.6294(16) 0.3949(15) 0.021(6) Uiso 1 1 d . . . C15 C -0.0975(3) 0.73006(17) -0.07206(16) 0.0365(5) Uani 1 1 d . . . C16 C -0.0387(3) 0.78476(18) -0.14282(17) 0.0467(6) Uani 1 1 d . . . H16 H 0.0609 0.7993 -0.1349 0.056 Uiso 1 1 calc R . . C17 C -0.1284(3) 0.8178(2) -0.22536(17) 0.0589(7) Uani 1 1 d . . . H17 H -0.0886 0.8535 -0.2732 0.071 Uiso 1 1 calc R . . C18 C -0.2747(4) 0.7978(2) -0.2362(2) 0.0611(8) Uani 1 1 d . . . H18 H -0.3344 0.8204 -0.2914 0.073 Uiso 1 1 calc R . . C19 C -0.3352(3) 0.7446(2) -0.1666(2) 0.0645(8) Uani 1 1 d . . . H19 H -0.4353 0.7316 -0.1751 0.077 Uiso 1 1 calc R . . C20 C -0.2474(3) 0.7100(2) -0.08293(19) 0.0501(6) Uani 1 1 d . . . H20 H -0.2882 0.6742 -0.0355 0.060 Uiso 1 1 calc R . . C21 C 0.1656(3) 0.61022(18) 0.00537(16) 0.0370(5) Uani 1 1 d . . . C22 C 0.2142(3) 0.6079(2) -0.08596(18) 0.0530(7) Uani 1 1 d . . . H22 H 0.1671 0.6461 -0.1368 0.064 Uiso 1 1 calc R . . C23 C 0.3314(4) 0.5496(3) -0.1013(2) 0.0806(11) Uani 1 1 d . . . H23 H 0.3639 0.5486 -0.1624 0.097 Uiso 1 1 calc R . . C24 C 0.4010(4) 0.4923(3) -0.0261(2) 0.0790(11) Uani 1 1 d . . . H24 H 0.4819 0.4541 -0.0361 0.095 Uiso 1 1 calc R . . C25 C 0.3509(4) 0.4917(2) 0.0633(2) 0.0695(9) Uani 1 1 d . . . H25 H 0.3965 0.4517 0.1133 0.083 Uiso 1 1 calc R . . C26 C 0.2349(3) 0.5493(2) 0.07924(18) 0.0561(7) Uani 1 1 d . . . H26 H 0.2014 0.5481 0.1400 0.067 Uiso 1 1 calc R . . C27 C -0.0783(2) 0.62151(17) 0.11599(15) 0.0337(5) Uani 1 1 d . . . C28 C -0.0736(3) 0.64926(19) 0.21266(16) 0.0404(5) Uani 1 1 d . . . H28 H -0.0268 0.7077 0.2348 0.048 Uiso 1 1 calc R . . C29 C -0.1385(3) 0.5900(2) 0.27628(17) 0.0494(7) Uani 1 1 d . . . H29 H -0.1339 0.6081 0.3417 0.059 Uiso 1 1 calc R . . C30 C -0.2096(3) 0.5048(2) 0.2439(2) 0.0494(7) Uani 1 1 d . . . H30 H -0.2531 0.4652 0.2872 0.059 Uiso 1 1 calc R . . C31 C -0.2171(3) 0.47731(19) 0.1461(2) 0.0493(6) Uani 1 1 d . . . H31 H -0.2670 0.4200 0.1238 0.059 Uiso 1 1 calc R . . C32 C -0.1505(3) 0.53497(19) 0.08260(19) 0.0444(6) Uani 1 1 d . . . H32 H -0.1538 0.5162 0.0175 0.053 Uiso 1 1 calc R . . C33 C 0.1030(3) 0.79797(16) 0.09626(15) 0.0378(5) Uani 1 1 d . . . C34 C 0.0110(3) 0.87076(19) 0.12582(17) 0.0499(6) Uani 1 1 d . . . H34 H -0.0901 0.8648 0.1105 0.060 Uiso 1 1 calc R . . C35 C 0.0707(4) 0.9528(2) 0.17852(18) 0.0595(8) Uani 1 1 d . . . H35 H 0.0101 1.0011 0.1998 0.071 Uiso 1 1 calc R . . C36 C 0.2206(4) 0.9611(2) 0.19852(18) 0.0653(9) Uani 1 1 d . . . H36 H 0.2606 1.0162 0.2329 0.078 Uiso 1 1 calc R . . C37 C 0.3124(4) 0.8907(3) 0.16932(19) 0.0627(8) Uani 1 1 d . . . H37 H 0.4135 0.8983 0.1830 0.075 Uiso 1 1 calc R . . C38 C 0.2533(3) 0.8076(2) 0.11896(17) 0.0503(7) Uani 1 1 d . . . H38 H 0.3150 0.7584 0.1005 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.01879(14) 0.03116(16) 0.02289(14) 0.00047(15) 0.00256(10) -0.00135(16) N1 0.0226(9) 0.0311(10) 0.0261(9) 0.0028(7) 0.0023(7) 0.0012(8) C1 0.0267(11) 0.0381(12) 0.0339(12) 0.0020(9) 0.0031(9) 0.0054(9) O1 0.0253(7) 0.0382(8) 0.0266(6) 0.0024(8) 0.0000(5) -0.0040(8) P1 0.0366(3) 0.0359(3) 0.0252(3) 0.0009(2) 0.0033(2) -0.0036(3) N2 0.0226(9) 0.0308(10) 0.0268(9) 0.0020(7) 0.0021(7) -0.0002(7) O2 0.0295(8) 0.0387(9) 0.0299(8) 0.0017(6) 0.0043(6) -0.0095(7) C2 0.0336(12) 0.0416(13) 0.0308(11) 0.0043(10) 0.0067(9) -0.0032(10) N3 0.0172(9) 0.0383(11) 0.0526(12) 0.0003(8) 0.0061(8) -0.0007(8) C3 0.0256(11) 0.0348(12) 0.0423(13) 0.0016(9) 0.0068(9) 0.0016(9) O3 0.0268(8) 0.0438(10) 0.0277(8) -0.0069(7) 0.0040(6) 0.0000(7) O4 0.0247(7) 0.0442(8) 0.0255(6) -0.0040(8) 0.0015(5) 0.0002(8) C4 0.0261(11) 0.0318(12) 0.0352(11) 0.0017(8) 0.0007(8) -0.0032(9) C5 0.0293(12) 0.0368(13) 0.0367(12) 0.0031(9) 0.0041(9) 0.0035(10) O5 0.0520(11) 0.0723(12) 0.0335(9) 0.0132(8) -0.0103(8) -0.0099(10) C6 0.0440(16) 0.0343(14) 0.0466(14) 0.0040(10) 0.0035(11) 0.0046(12) O6 0.0801(15) 0.0677(13) 0.0511(11) 0.0251(10) -0.0025(10) -0.0326(11) C7 0.0410(15) 0.0333(14) 0.0487(15) 0.0044(11) -0.0007(11) -0.0136(11) O7 0.0291(9) 0.0796(14) 0.0576(11) -0.0132(10) 0.0143(8) 0.0116(9) C8 0.0239(12) 0.0433(15) 0.0458(14) 0.0042(11) 0.0018(10) -0.0089(11) O8 0.0271(8) 0.0657(12) 0.0459(9) -0.0061(8) -0.0071(7) -0.0004(8) C9 0.0242(11) 0.0355(12) 0.0270(10) 0.0030(9) -0.0034(8) -0.0014(9) C10 0.0236(11) 0.0351(12) 0.0329(11) 0.0019(9) 0.0012(8) 0.0022(9) C11 0.0307(13) 0.0502(17) 0.0621(16) -0.0019(13) 0.0201(11) 0.0038(12) C12 0.0498(17) 0.0480(16) 0.0652(18) -0.0116(13) 0.0194(14) 0.0109(13) C13 0.0500(16) 0.0361(14) 0.0429(14) -0.0058(10) 0.0079(11) -0.0016(12) C14 0.0304(13) 0.0378(13) 0.0335(12) -0.0009(10) 0.0056(10) -0.0046(11) C15 0.0419(14) 0.0350(12) 0.0311(11) -0.0016(9) -0.0003(9) 0.0001(10) C16 0.0531(16) 0.0481(15) 0.0385(13) 0.0071(11) 0.0045(11) -0.0007(12) C17 0.089(2) 0.0496(15) 0.0364(12) 0.0088(14) 0.0025(12) 0.0095(19) C18 0.080(2) 0.0476(18) 0.0472(15) -0.0022(12) -0.0229(14) 0.0120(15) C19 0.0495(17) 0.0587(19) 0.077(2) -0.0082(16) -0.0214(14) -0.0015(15) C20 0.0456(15) 0.0489(16) 0.0539(15) 0.0011(12) -0.0005(11) -0.0037(12) C21 0.0375(14) 0.0427(13) 0.0311(12) 0.0034(10) 0.0063(10) -0.0017(11) C22 0.0601(19) 0.0648(18) 0.0371(14) 0.0161(12) 0.0177(12) 0.0144(15) C23 0.090(3) 0.108(3) 0.0514(18) 0.0231(18) 0.0378(17) 0.038(2) C24 0.079(2) 0.087(2) 0.079(2) 0.0189(19) 0.0392(19) 0.041(2) C25 0.077(2) 0.077(2) 0.0560(19) 0.0242(15) 0.0152(16) 0.0342(18) C26 0.0689(19) 0.0687(19) 0.0331(13) 0.0128(13) 0.0153(12) 0.0235(16) C27 0.0360(13) 0.0339(12) 0.0320(11) 0.0021(9) 0.0074(9) 0.0009(10) C28 0.0424(14) 0.0455(14) 0.0337(12) -0.0008(10) 0.0061(10) -0.0009(11) C29 0.0571(18) 0.0595(18) 0.0339(13) 0.0092(12) 0.0150(12) 0.0055(14) C30 0.0433(15) 0.0519(17) 0.0571(17) 0.0235(13) 0.0217(12) 0.0124(12) C31 0.0465(16) 0.0333(14) 0.0694(19) 0.0092(12) 0.0127(13) -0.0006(11) C32 0.0519(16) 0.0420(14) 0.0405(14) -0.0012(11) 0.0105(11) -0.0043(13) C33 0.0479(14) 0.0379(14) 0.0265(10) 0.0045(8) 0.0013(9) -0.0098(10) C34 0.0639(18) 0.0415(14) 0.0426(14) 0.0021(11) 0.0008(12) -0.0022(13) C35 0.098(3) 0.0411(15) 0.0364(14) -0.0021(12) -0.0013(14) 0.0012(16) C36 0.113(3) 0.0510(18) 0.0278(13) 0.0037(12) -0.0045(15) -0.0316(19) C37 0.066(2) 0.075(2) 0.0439(16) 0.0034(15) -0.0029(13) -0.0299(17) C38 0.0498(14) 0.0612(19) 0.0400(12) 0.0014(12) 0.0062(10) -0.0145(14) _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 Cr O1 1.9558(12) . ? Cr O4 1.9582(12) . ? Cr O2 1.9642(15) . ? Cr O3 1.9716(15) . ? Cr N2 2.0581(17) . ? Cr N1 2.0716(17) . ? N1 C9 1.344(3) . ? N1 C5 1.366(3) . ? C1 O5 1.214(3) . ? C1 O1 1.293(3) . ? C1 C2 1.566(3) . ? P1 C21 1.789(3) . ? P1 C27 1.797(2) . ? P1 C15 1.799(2) . ? P1 C33 1.801(2) . ? N2 C10 1.335(3) . ? N2 C14 1.354(3) . ? O2 C2 1.292(2) . ? C2 O6 1.205(3) . ? N3 C9 1.374(3) . ? N3 C10 1.375(3) . ? C3 O7 1.219(3) . ? C3 O3 1.284(2) . ? C3 C4 1.550(3) . ? O4 C4 1.285(2) . ? C4 O8 1.224(2) . ? C5 C6 1.357(3) . ? C6 C7 1.386(4) . ? C7 C8 1.363(4) . ? C8 C9 1.405(3) . ? C10 C11 1.401(3) . ? C11 C12 1.368(4) . ? C12 C13 1.372(4) . ? C13 C14 1.352(3) . ? C15 C16 1.388(3) . ? C15 C20 1.394(3) . ? C16 C17 1.388(3) . ? C17 C18 1.362(4) . ? C18 C19 1.373(4) . ? C19 C20 1.399(4) . ? C21 C22 1.392(3) . ? C21 C26 1.395(3) . ? C22 C23 1.373(4) . ? C23 C24 1.381(4) . ? C24 C25 1.373(4) . ? C25 C26 1.361(4) . ? C27 C28 1.380(3) . ? C27 C32 1.390(3) . ? C28 C29 1.380(3) . ? C29 C30 1.366(4) . ? C30 C31 1.392(4) . ? C31 C32 1.374(3) . ? C33 C38 1.383(3) . ? C33 C34 1.391(3) . ? C34 C35 1.395(4) . ? C35 C36 1.375(4) . ? C36 C37 1.365(4) . ? C37 C38 1.390(4) . ? 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 O1 Cr O4 174.02(6) . . ? O1 Cr O2 83.25(6) . . ? O4 Cr O2 92.64(6) . . ? O1 Cr O3 92.77(6) . . ? O4 Cr O3 82.70(6) . . ? O2 Cr O3 87.76(7) . . ? O1 Cr N2 93.49(6) . . ? O4 Cr N2 90.90(6) . . ? O2 Cr N2 90.74(7) . . ? O3 Cr N2 173.34(6) . . ? O1 Cr N1 89.68(6) . . ? O4 Cr N1 94.56(6) . . ? O2 Cr N1 172.67(6) . . ? O3 Cr N1 94.53(7) . . ? N2 Cr N1 87.76(7) . . ? C9 N1 C5 117.17(19) . . ? C9 N1 Cr 123.69(14) . . ? C5 N1 Cr 118.72(14) . . ? O5 C1 O1 125.4(2) . . ? O5 C1 C2 120.7(2) . . ? O1 C1 C2 113.95(17) . . ? C1 O1 Cr 113.39(13) . . ? C21 P1 C27 106.82(11) . . ? C21 P1 C15 112.76(10) . . ? C27 P1 C15 111.00(11) . . ? C21 P1 C33 108.53(11) . . ? C27 P1 C33 109.45(10) . . ? C15 P1 C33 108.22(10) . . ? C10 N2 C14 117.67(19) . . ? C10 N2 Cr 124.95(14) . . ? C14 N2 Cr 117.31(15) . . ? C2 O2 Cr 114.39(14) . . ? O6 C2 O2 126.1(2) . . ? O6 C2 C1 120.80(19) . . ? O2 C2 C1 113.10(18) . . ? C9 N3 C10 129.99(18) . . ? O7 C3 O3 126.2(2) . . ? O7 C3 C4 119.76(19) . . ? O3 C3 C4 114.07(18) . . ? C3 O3 Cr 112.34(13) . . ? C4 O4 Cr 113.90(12) . . ? O8 C4 O4 126.2(2) . . ? O8 C4 C3 120.16(19) . . ? O4 C4 C3 113.69(16) . . ? C6 C5 N1 123.4(2) . . ? C5 C6 C7 118.9(2) . . ? C8 C7 C6 119.4(2) . . ? C7 C8 C9 119.1(2) . . ? N1 C9 N3 120.57(19) . . ? N1 C9 C8 121.9(2) . . ? N3 C9 C8 117.56(19) . . ? N2 C10 N3 120.7(2) . . ? N2 C10 C11 121.4(2) . . ? N3 C10 C11 117.9(2) . . ? C12 C11 C10 118.9(2) . . ? C11 C12 C13 119.7(3) . . ? C14 C13 C12 118.4(3) . . ? C13 C14 N2 123.8(2) . . ? C16 C15 C20 119.9(2) . . ? C16 C15 P1 118.87(18) . . ? C20 C15 P1 121.17(18) . . ? C17 C16 C15 120.2(3) . . ? C18 C17 C16 119.9(3) . . ? C17 C18 C19 120.8(2) . . ? C18 C19 C20 120.5(3) . . ? C15 C20 C19 118.7(3) . . ? C22 C21 C26 118.6(2) . . ? C22 C21 P1 123.51(18) . . ? C26 C21 P1 117.91(19) . . ? C23 C22 C21 120.3(2) . . ? C22 C23 C24 120.0(3) . . ? C25 C24 C23 120.1(3) . . ? C26 C25 C24 120.3(3) . . ? C25 C26 C21 120.7(2) . . ? C28 C27 C32 120.0(2) . . ? C28 C27 P1 120.84(18) . . ? C32 C27 P1 118.92(17) . . ? C29 C28 C27 119.8(2) . . ? C30 C29 C28 120.5(2) . . ? C29 C30 C31 120.1(2) . . ? C32 C31 C30 119.9(2) . . ? C31 C32 C27 119.8(2) . . ? C38 C33 C34 119.8(2) . . ? C38 C33 P1 121.6(2) . . ? C34 C33 P1 118.60(19) . . ? C33 C34 C35 119.9(3) . . ? C36 C35 C34 119.0(3) . . ? C37 C36 C35 121.8(3) . . ? C36 C37 C38 119.4(3) . . ? C33 C38 C37 120.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cr N1 C9 63.96(16) . . . . ? O4 Cr N1 C9 -120.27(15) . . . . ? O2 Cr N1 C9 48.8(6) . . . . ? O3 Cr N1 C9 156.72(15) . . . . ? N2 Cr N1 C9 -29.54(15) . . . . ? O1 Cr N1 C5 -108.37(15) . . . . ? O4 Cr N1 C5 67.41(15) . . . . ? O2 Cr N1 C5 -123.5(5) . . . . ? O3 Cr N1 C5 -15.61(15) . . . . ? N2 Cr N1 C5 158.13(15) . . . . ? O5 C1 O1 Cr -164.9(2) . . . . ? C2 C1 O1 Cr 14.8(2) . . . . ? O4 Cr O1 C1 34.1(8) . . . . ? O2 Cr O1 C1 -12.69(15) . . . . ? O3 Cr O1 C1 74.72(15) . . . . ? N2 Cr O1 C1 -103.02(15) . . . . ? N1 Cr O1 C1 169.24(15) . . . . ? O1 Cr N2 C10 -65.13(16) . . . . ? O4 Cr N2 C10 118.94(16) . . . . ? O2 Cr N2 C10 -148.41(16) . . . . ? O3 Cr N2 C10 134.7(6) . . . . ? N1 Cr N2 C10 24.41(16) . . . . ? O1 Cr N2 C14 111.60(15) . . . . ? O4 Cr N2 C14 -64.33(15) . . . . ? O2 Cr N2 C14 28.32(15) . . . . ? O3 Cr N2 C14 -48.6(7) . . . . ? N1 Cr N2 C14 -158.87(15) . . . . ? O1 Cr O2 C2 7.43(15) . . . . ? O4 Cr O2 C2 -168.21(15) . . . . ? O3 Cr O2 C2 -85.63(15) . . . . ? N2 Cr O2 C2 100.86(15) . . . . ? N1 Cr O2 C2 22.7(6) . . . . ? Cr O2 C2 O6 178.4(2) . . . . ? Cr O2 C2 C1 -1.6(2) . . . . ? O5 C1 C2 O6 -9.2(4) . . . . ? O1 C1 C2 O6 171.0(2) . . . . ? O5 C1 C2 O2 170.8(2) . . . . ? O1 C1 C2 O2 -8.9(3) . . . . ? O7 C3 O3 Cr 161.0(2) . . . . ? C4 C3 O3 Cr -18.0(2) . . . . ? O1 Cr O3 C3 -159.17(15) . . . . ? O4 Cr O3 C3 16.90(15) . . . . ? O2 Cr O3 C3 -76.05(15) . . . . ? N2 Cr O3 C3 1.0(7) . . . . ? N1 Cr O3 C3 110.93(15) . . . . ? O1 Cr O4 C4 28.9(8) . . . . ? O2 Cr O4 C4 75.31(15) . . . . ? O3 Cr O4 C4 -12.09(15) . . . . ? N2 Cr O4 C4 166.10(16) . . . . ? N1 Cr O4 C4 -106.08(15) . . . . ? Cr O4 C4 O8 -173.89(18) . . . . ? Cr O4 C4 C3 5.8(2) . . . . ? O7 C3 C4 O8 9.1(3) . . . . ? O3 C3 C4 O8 -171.9(2) . . . . ? O7 C3 C4 O4 -170.6(2) . . . . ? O3 C3 C4 O4 8.4(3) . . . . ? C9 N1 C5 C6 -3.0(3) . . . . ? Cr N1 C5 C6 169.82(18) . . . . ? N1 C5 C6 C7 0.0(4) . . . . ? C5 C6 C7 C8 1.5(4) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C5 N1 C9 N3 -174.18(19) . . . . ? Cr N1 C9 N3 13.4(3) . . . . ? C5 N1 C9 C8 4.5(3) . . . . ? Cr N1 C9 C8 -167.92(15) . . . . ? C10 N3 C9 N1 23.9(3) . . . . ? C10 N3 C9 C8 -154.9(2) . . . . ? C7 C8 C9 N1 -3.1(3) . . . . ? C7 C8 C9 N3 175.6(2) . . . . ? C14 N2 C10 N3 -179.61(19) . . . . ? Cr N2 C10 N3 -2.9(3) . . . . ? C14 N2 C10 C11 -0.2(3) . . . . ? Cr N2 C10 C11 176.56(17) . . . . ? C9 N3 C10 N2 -29.9(3) . . . . ? C9 N3 C10 C11 150.7(2) . . . . ? N2 C10 C11 C12 -0.6(4) . . . . ? N3 C10 C11 C12 178.9(2) . . . . ? C10 C11 C12 C13 1.1(4) . . . . ? C11 C12 C13 C14 -0.9(4) . . . . ? C12 C13 C14 N2 0.1(4) . . . . ? C10 N2 C14 C13 0.4(3) . . . . ? Cr N2 C14 C13 -176.56(19) . . . . ? C21 P1 C15 C16 -60.7(2) . . . . ? C27 P1 C15 C16 179.49(18) . . . . ? C33 P1 C15 C16 59.4(2) . . . . ? C21 P1 C15 C20 121.3(2) . . . . ? C27 P1 C15 C20 1.5(2) . . . . ? C33 P1 C15 C20 -118.6(2) . . . . ? C20 C15 C16 C17 -1.3(4) . . . . ? P1 C15 C16 C17 -179.3(2) . . . . ? C15 C16 C17 C18 1.0(4) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? C17 C18 C19 C20 0.0(4) . . . . ? C16 C15 C20 C19 0.9(4) . . . . ? P1 C15 C20 C19 178.9(2) . . . . ? C18 C19 C20 C15 -0.3(4) . . . . ? C27 P1 C21 C22 144.2(2) . . . . ? C15 P1 C21 C22 22.0(3) . . . . ? C33 P1 C21 C22 -97.9(2) . . . . ? C27 P1 C21 C26 -37.5(2) . . . . ? C15 P1 C21 C26 -159.7(2) . . . . ? C33 P1 C21 C26 80.4(2) . . . . ? C26 C21 C22 C23 -2.4(4) . . . . ? P1 C21 C22 C23 175.9(3) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C25 1.6(6) . . . . ? C23 C24 C25 C26 -1.7(6) . . . . ? C24 C25 C26 C21 -0.4(5) . . . . ? C22 C21 C26 C25 2.4(4) . . . . ? P1 C21 C26 C25 -176.0(3) . . . . ? C21 P1 C27 C28 111.5(2) . . . . ? C15 P1 C27 C28 -125.2(2) . . . . ? C33 P1 C27 C28 -5.8(2) . . . . ? C21 P1 C27 C32 -63.0(2) . . . . ? C15 P1 C27 C32 60.3(2) . . . . ? C33 P1 C27 C32 179.73(19) . . . . ? C32 C27 C28 C29 1.1(4) . . . . ? P1 C27 C28 C29 -173.24(19) . . . . ? C27 C28 C29 C30 -1.1(4) . . . . ? C28 C29 C30 C31 0.0(4) . . . . ? C29 C30 C31 C32 1.2(4) . . . . ? C30 C31 C32 C27 -1.1(4) . . . . ? C28 C27 C32 C31 0.0(4) . . . . ? P1 C27 C32 C31 174.48(19) . . . . ? C21 P1 C33 C38 -3.4(2) . . . . ? C27 P1 C33 C38 112.79(19) . . . . ? C15 P1 C33 C38 -126.12(19) . . . . ? C21 P1 C33 C34 179.84(17) . . . . ? C27 P1 C33 C34 -63.92(19) . . . . ? C15 P1 C33 C34 57.2(2) . . . . ? C38 C33 C34 C35 -0.3(3) . . . . ? P1 C33 C34 C35 176.49(19) . . . . ? C33 C34 C35 C36 1.4(4) . . . . ? C34 C35 C36 C37 -0.9(4) . . . . ? C35 C36 C37 C38 -0.8(4) . . . . ? C34 C33 C38 C37 -1.4(3) . . . . ? P1 C33 C38 C37 -178.03(19) . . . . ? C36 C37 C38 C33 1.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.460 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.042 #COMP2.CIF data_Compound_2_AsPh4[Cr(dpa)(ox)2] _database_code_CSD 161710 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'AsPh4[Cr(dpa)(ox)2]' _chemical_formula_sum 'C38 H29 As Cr N3 O8' _chemical_formula_weight 782.56 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' 'As' 'As' 0.0499 2.0058 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2221(5) _cell_length_b 13.471(3) _cell_length_c 13.8725(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.418(7) _cell_angle_gamma 90.00 _cell_volume 1709.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 2651 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2452 _reflns_number_gt 2050 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0457P)^2^+1.0914P] 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 SHELXL _refine_ls_extinction_coef 0.0000(7) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2452 _refine_ls_number_parameters 462 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 1.501 _refine_ls_shift/su_mean 0.370 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As As 0.02040(9) -0.00037(5) 0.03199(4) 0.0376(2) Uani 1 1 d . . . C27 C 0.1781(10) -0.0815(6) 0.0022(6) 0.043(2) Uani 1 1 d . . . C15 C -0.1039(11) 0.0448(6) -0.0822(5) 0.039(2) Uani 1 1 d . . . C21 C 0.1044(11) 0.1167(6) 0.0992(5) 0.042(2) Uani 1 1 d . . . C33 C -0.0859(9) -0.0722(6) 0.1174(5) 0.035(2) Uani 1 1 d . . . C18 C -0.2833(16) 0.1100(7) -0.2424(6) 0.071(4) Uani 1 1 d . . . H18 H -0.3440 0.1333 -0.2964 0.057(5) Uiso 1 1 calc R . . C24 C 0.2200(15) 0.2783(8) 0.2017(6) 0.070(4) Uani 1 1 d . . . H24 H 0.2604 0.3331 0.2361 0.057(5) Uiso 1 1 calc R . . C26 C 0.2531(12) 0.1246(8) 0.1215(5) 0.051(2) Uani 1 1 d . . . H26 H 0.3147 0.0755 0.1027 0.057(5) Uiso 1 1 calc R . . C34 C -0.0791(9) -0.0433(6) 0.2137(5) 0.046(2) Uani 1 1 d . . . H34 H -0.0321 0.0152 0.2352 0.057(5) Uiso 1 1 calc R . . C38 C -0.1571(10) -0.1569(6) 0.0845(6) 0.049(2) Uani 1 1 d . . . H38 H -0.1619 -0.1750 0.0194 0.057(5) Uiso 1 1 calc R . . C35 C -0.1427(10) -0.1024(7) 0.2767(6) 0.056(3) Uani 1 1 d . . . H35 H -0.1386 -0.0844 0.3418 0.057(5) Uiso 1 1 calc R . . C23 C 0.0730(14) 0.2702(7) 0.1811(6) 0.061(3) Uani 1 1 d . . . H23 H 0.0126 0.3188 0.2019 0.057(5) Uiso 1 1 calc R . . C32 C 0.2395(11) -0.1439(7) 0.0752(6) 0.056(3) Uani 1 1 d . . . H32 H 0.2011 -0.1467 0.1340 0.057(5) Uiso 1 1 calc R . . C25 C 0.3094(14) 0.2070(9) 0.1723(6) 0.073(3) Uani 1 1 d . . . H25 H 0.4102 0.2139 0.1869 0.057(5) Uiso 1 1 calc R . . C22 C 0.0129(12) 0.1893(7) 0.1289(6) 0.058(3) Uani 1 1 d . . . H22 H -0.0880 0.1836 0.1138 0.057(5) Uiso 1 1 calc R . . C37 C -0.2217(10) -0.2155(6) 0.1486(6) 0.050(2) Uani 1 1 d . . . H37 H -0.2712 -0.2732 0.1271 0.057(5) Uiso 1 1 calc R . . C20 C -0.0460(11) 0.0945(7) -0.1526(6) 0.055(3) Uani 1 1 d . . . H20 H 0.0540 0.1066 -0.1468 0.057(5) Uiso 1 1 calc R . . C36 C -0.2123(10) -0.1879(7) 0.2440(7) 0.055(3) Uani 1 1 d . . . H36 H -0.2541 -0.2280 0.2875 0.057(5) Uiso 1 1 calc R . . C19 C -0.1380(14) 0.1274(8) -0.2341(6) 0.070(3) Uani 1 1 d . . . H19 H -0.0990 0.1615 -0.2830 0.057(5) Uiso 1 1 calc R . . C29 C 0.3432(12) -0.1396(10) -0.1021(7) 0.088(4) Uani 1 1 d . . . H29 H 0.3787 -0.1390 -0.1619 0.057(5) Uiso 1 1 calc R . . C30 C 0.4071(13) -0.1997(9) -0.0270(7) 0.086(4) Uani 1 1 d . . . H30 H 0.4860 -0.2398 -0.0368 0.057(5) Uiso 1 1 calc R . . C17 C -0.3410(12) 0.0586(8) -0.1722(8) 0.068(3) Uani 1 1 d . . . H17 H -0.4409 0.0459 -0.1789 0.057(5) Uiso 1 1 calc R . . C31 C 0.3556(12) -0.2009(9) 0.0612(7) 0.076(3) Uani 1 1 d . . . H31 H 0.4002 -0.2407 0.1112 0.057(5) Uiso 1 1 calc R . . C16 C -0.2514(13) 0.0247(7) -0.0902(6) 0.061(3) Uani 1 1 d . . . H16 H -0.2904 -0.0107 -0.0420 0.057(5) Uiso 1 1 calc R . . C28 C 0.2267(11) -0.0812(7) -0.0862(6) 0.060(3) Uani 1 1 d . . . H28 H 0.1810 -0.0414 -0.1359 0.057(5) Uiso 1 1 calc R . . Cr Cr 0.16507(13) 0.13171(8) 0.48530(7) 0.0287(3) Uani 1 1 d . . . O3 O 0.0207(6) 0.2101(4) 0.5468(3) 0.0366(15) Uani 1 1 d . . . O8 O -0.2271(6) 0.1654(4) 0.3383(4) 0.0536(17) Uani 1 1 d . . . O7 O -0.2247(8) 0.2241(5) 0.5311(4) 0.0573(19) Uani 1 1 d . . . C3 C -0.1100(12) 0.2038(6) 0.4983(6) 0.044(3) Uani 1 1 d . . . C4 C -0.1124(11) 0.1654(6) 0.3931(5) 0.035(2) Uani 1 1 d . . . O1 O 0.3006(5) 0.1273(4) 0.6048(3) 0.0331(11) Uani 1 1 d . . . O2 O 0.0846(5) 0.0128(4) 0.5381(3) 0.0355(12) Uani 1 1 d . . . O4 O 0.0124(6) 0.1358(4) 0.3725(3) 0.0355(13) Uani 1 1 d . . . N2 N 0.2965(8) 0.0477(5) 0.4084(4) 0.0304(16) Uani 1 1 d . . . N1 N 0.2751(9) 0.2570(5) 0.4431(4) 0.0312(17) Uani 1 1 d . . . C8 C 0.4917(10) 0.3421(6) 0.4169(6) 0.042(2) Uani 1 1 d . . . H8 H 0.5901 0.3395 0.4084 0.057(5) Uiso 1 1 calc R . . C14 C 0.2472(10) -0.0428(6) 0.3813(5) 0.040(2) Uani 1 1 d . . . H14 H 0.1543 -0.0612 0.3940 0.057(5) Uiso 1 1 calc R . . C6 C 0.2764(12) 0.4339(6) 0.4338(5) 0.042(2) Uani 1 1 d . . . H6 H 0.2260 0.4936 0.4347 0.057(5) Uiso 1 1 calc R . . O5 O 0.3102(7) 0.0637(5) 0.7540(4) 0.0594(17) Uani 1 1 d . . . C1 C 0.2599(9) 0.0652(6) 0.6684(5) 0.0343(19) Uani 1 1 d . . . C10 C 0.4277(10) 0.0745(6) 0.3885(5) 0.034(2) Uani 1 1 d . . . O6 O 0.1051(8) -0.0754(5) 0.6739(4) 0.072(2) Uani 1 1 d . . . C2 C 0.1398(8) -0.0073(7) 0.6267(5) 0.0395(19) Uani 1 1 d . . . C11 C 0.5142(10) 0.0109(8) 0.3405(6) 0.053(2) Uani 1 1 d . . . H11 H 0.6054 0.0310 0.3260 0.057(5) Uiso 1 1 calc R . . C9 C 0.4159(11) 0.2550(6) 0.4260(5) 0.034(2) Uani 1 1 d . . . N3 N 0.4855(8) 0.1665(4) 0.4149(5) 0.0386(17) Uani 1 1 d . . . H3 H 0.5793 0.1687 0.4262 0.057(5) Uiso 1 1 calc R . . C13 C 0.3268(11) -0.1091(6) 0.3360(5) 0.046(2) Uani 1 1 d . . . H13 H 0.2897 -0.1719 0.3195 0.057(5) Uiso 1 1 calc R . . C12 C 0.4614(12) -0.0823(7) 0.3151(7) 0.057(3) Uani 1 1 d . . . H12 H 0.5173 -0.1265 0.2839 0.057(5) Uiso 1 1 calc R . . C5 C 0.2101(10) 0.3471(6) 0.4453(6) 0.038(2) Uani 1 1 d . . . H5 H 0.1124 0.3486 0.4555 0.057(5) Uiso 1 1 calc R . . C7 C 0.4245(12) 0.4317(6) 0.4203(5) 0.044(2) Uani 1 1 d . . . H7 H 0.4757 0.4903 0.4138 0.057(5) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As 0.0400(6) 0.0423(4) 0.0300(3) 0.0015(4) 0.0024(3) -0.0036(5) C27 0.041(7) 0.044(5) 0.045(4) 0.002(4) 0.011(4) -0.004(4) C15 0.031(7) 0.042(4) 0.041(4) -0.004(3) -0.004(4) 0.000(4) C21 0.046(8) 0.045(5) 0.033(3) 0.000(3) 0.007(4) -0.017(4) C33 0.026(6) 0.043(4) 0.037(4) 0.010(3) 0.006(4) 0.003(4) C18 0.099(11) 0.052(6) 0.051(5) -0.006(4) -0.034(6) 0.017(6) C24 0.109(12) 0.060(7) 0.038(5) 0.006(5) 0.000(6) -0.032(7) C26 0.051(8) 0.065(6) 0.040(4) -0.004(5) 0.014(4) -0.014(5) C34 0.046(6) 0.057(5) 0.036(4) 0.001(3) 0.014(4) 0.004(4) C38 0.046(7) 0.050(5) 0.050(5) -0.003(4) 0.000(4) -0.003(5) C35 0.057(8) 0.073(7) 0.041(4) 0.006(4) 0.017(4) 0.007(5) C23 0.089(10) 0.049(5) 0.046(5) -0.005(4) 0.007(5) -0.001(6) C32 0.059(8) 0.072(6) 0.041(4) 0.016(4) 0.020(4) 0.025(5) C25 0.070(10) 0.105(9) 0.041(5) 0.007(6) 0.000(5) -0.040(7) C22 0.077(9) 0.053(6) 0.043(4) 0.000(4) -0.003(5) 0.000(5) C37 0.041(7) 0.044(5) 0.067(6) 0.008(4) 0.011(5) -0.002(4) C20 0.050(8) 0.068(6) 0.046(5) 0.017(4) 0.003(4) -0.001(5) C36 0.046(7) 0.054(6) 0.069(6) 0.030(5) 0.025(5) 0.014(5) C19 0.105(10) 0.066(6) 0.037(4) 0.020(5) 0.005(5) 0.019(7) C29 0.067(9) 0.138(11) 0.065(6) 0.026(7) 0.035(6) 0.060(8) C30 0.080(9) 0.108(10) 0.075(7) 0.008(6) 0.033(6) 0.044(8) C17 0.028(8) 0.073(6) 0.093(7) 0.006(6) -0.027(5) -0.002(5) C31 0.066(8) 0.102(8) 0.060(6) 0.021(5) 0.013(5) 0.042(7) C16 0.059(10) 0.063(7) 0.058(5) 0.012(4) -0.004(5) 0.004(5) C28 0.063(8) 0.079(6) 0.038(4) 0.021(4) 0.012(4) 0.019(5) Cr 0.0225(8) 0.0372(6) 0.0261(5) 0.0013(5) 0.0022(5) -0.0010(6) O3 0.025(5) 0.053(4) 0.030(3) -0.003(2) 0.000(3) 0.000(3) O8 0.023(5) 0.078(4) 0.056(3) -0.009(3) -0.009(3) 0.002(3) O7 0.029(5) 0.087(5) 0.059(4) -0.009(3) 0.018(3) 0.011(4) C3 0.051(9) 0.039(5) 0.044(5) 0.003(3) 0.010(5) 0.002(4) C4 0.021(7) 0.041(5) 0.043(4) 0.001(3) 0.005(4) -0.011(4) O1 0.022(3) 0.042(3) 0.035(2) 0.008(2) -0.001(2) -0.004(3) O2 0.032(3) 0.039(3) 0.035(2) 0.001(2) 0.007(2) -0.006(3) O4 0.022(4) 0.056(3) 0.028(2) -0.005(2) 0.001(2) 0.000(3) N2 0.023(5) 0.038(3) 0.031(3) -0.002(3) 0.008(3) -0.001(3) N1 0.019(6) 0.041(4) 0.033(3) 0.005(3) 0.003(3) 0.002(3) C8 0.023(7) 0.045(5) 0.055(5) 0.006(4) -0.001(4) -0.010(4) C14 0.034(6) 0.044(5) 0.040(4) -0.003(4) 0.001(4) -0.001(4) C6 0.041(8) 0.033(4) 0.053(5) -0.001(3) 0.009(4) 0.004(4) O5 0.048(4) 0.086(4) 0.039(3) 0.018(3) -0.011(3) -0.009(3) C1 0.019(6) 0.044(4) 0.039(4) 0.004(3) 0.003(3) 0.010(4) C10 0.025(7) 0.041(5) 0.034(4) 0.001(3) -0.001(4) 0.005(4) O6 0.074(6) 0.080(5) 0.058(4) 0.028(3) -0.006(3) -0.029(4) C2 0.030(6) 0.047(5) 0.043(4) 0.010(5) 0.009(3) -0.005(5) C11 0.024(6) 0.066(7) 0.073(5) -0.001(6) 0.015(4) 0.006(5) C9 0.021(7) 0.043(5) 0.036(4) 0.007(3) -0.003(4) -0.002(4) N3 0.020(5) 0.037(4) 0.058(4) 0.000(3) 0.004(3) -0.004(3) C13 0.047(7) 0.039(5) 0.054(5) -0.005(4) 0.009(4) -0.002(4) C12 0.038(8) 0.050(5) 0.085(7) -0.016(5) 0.017(6) 0.007(5) C5 0.027(6) 0.040(5) 0.046(4) 0.003(3) 0.002(4) -0.006(4) C7 0.048(8) 0.033(5) 0.048(5) 0.004(3) -0.002(4) -0.014(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 As C33 1.898(7) . ? As C27 1.907(9) . ? As C15 1.930(8) . ? As C21 1.942(7) . ? C27 C28 1.359(11) . ? C27 C32 1.379(11) . ? C15 C20 1.349(11) . ? C15 C16 1.377(13) . ? C21 C26 1.370(12) . ? C21 C22 1.388(12) . ? C33 C38 1.366(11) . ? C33 C34 1.385(10) . ? C18 C17 1.359(14) . ? C18 C19 1.350(15) . ? C24 C23 1.353(14) . ? C24 C25 1.362(15) . ? C26 C25 1.380(14) . ? C34 C35 1.369(11) . ? C38 C37 1.381(11) . ? C35 C36 1.368(12) . ? C23 C22 1.384(13) . ? C32 C31 1.352(12) . ? C37 C36 1.366(12) . ? C20 C19 1.395(12) . ? C29 C28 1.373(13) . ? C29 C30 1.389(14) . ? C30 C31 1.368(13) . ? C17 C16 1.393(13) . ? Cr O1 1.944(4) . ? Cr O2 1.948(5) . ? Cr O4 1.966(5) . ? Cr O3 1.977(5) . ? Cr N2 2.054(6) . ? Cr N1 2.092(7) . ? O3 C3 1.305(11) . ? O8 C4 1.221(9) . ? O7 C3 1.233(10) . ? C3 C4 1.546(11) . ? C4 O4 1.286(9) . ? O1 C1 1.305(8) . ? O2 C2 1.296(8) . ? N2 C10 1.326(10) . ? N2 C14 1.338(9) . ? N1 C9 1.350(10) . ? N1 C5 1.356(10) . ? C8 C7 1.361(12) . ? C8 C9 1.380(11) . ? C14 C13 1.361(11) . ? C6 C5 1.339(11) . ? C6 C7 1.403(12) . ? O5 C1 1.217(8) . ? C1 C2 1.533(11) . ? C10 N3 1.380(10) . ? C10 C11 1.397(11) . ? O6 C2 1.194(10) . ? C11 C12 1.376(14) . ? C9 N3 1.372(10) . ? C13 C12 1.359(12) . ? 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 C33 As C27 108.2(3) . . ? C33 As C15 111.9(4) . . ? C27 As C15 113.1(3) . . ? C33 As C21 108.7(3) . . ? C27 As C21 107.6(4) . . ? C15 As C21 107.2(3) . . ? C28 C27 C32 120.9(8) . . ? C28 C27 As 122.9(7) . . ? C32 C27 As 116.3(6) . . ? C20 C15 C16 121.2(8) . . ? C20 C15 As 120.1(7) . . ? C16 C15 As 118.7(6) . . ? C26 C21 C22 120.5(8) . . ? C26 C21 As 119.7(7) . . ? C22 C21 As 119.6(7) . . ? C38 C33 C34 121.2(8) . . ? C38 C33 As 118.8(6) . . ? C34 C33 As 119.8(6) . . ? C17 C18 C19 120.2(9) . . ? C23 C24 C25 120.6(10) . . ? C21 C26 C25 118.5(10) . . ? C35 C34 C33 118.9(8) . . ? C33 C38 C37 119.4(8) . . ? C36 C35 C34 119.9(8) . . ? C24 C23 C22 119.8(10) . . ? C31 C32 C27 119.9(7) . . ? C24 C25 C26 121.2(11) . . ? C23 C22 C21 119.4(10) . . ? C36 C37 C38 119.3(8) . . ? C15 C20 C19 119.2(10) . . ? C35 C36 C37 121.3(8) . . ? C18 C19 C20 120.5(9) . . ? C28 C29 C30 118.6(9) . . ? C31 C30 C29 121.0(10) . . ? C18 C17 C16 120.4(11) . . ? C32 C31 C30 119.6(9) . . ? C15 C16 C17 118.4(10) . . ? C27 C28 C29 119.9(8) . . ? O1 Cr O2 83.6(2) . . ? O1 Cr O4 174.4(2) . . ? O2 Cr O4 93.1(2) . . ? O1 Cr O3 92.5(2) . . ? O2 Cr O3 88.1(2) . . ? O4 Cr O3 82.9(2) . . ? O1 Cr N2 93.9(2) . . ? O2 Cr N2 91.2(2) . . ? O4 Cr N2 90.7(2) . . ? O3 Cr N2 173.5(2) . . ? O1 Cr N1 89.0(2) . . ? O2 Cr N1 172.3(2) . . ? O4 Cr N1 94.5(2) . . ? O3 Cr N1 93.9(3) . . ? N2 Cr N1 87.6(3) . . ? C3 O3 Cr 111.8(5) . . ? O7 C3 O3 125.1(8) . . ? O7 C3 C4 120.9(9) . . ? O3 C3 C4 114.0(8) . . ? O8 C4 O4 126.1(7) . . ? O8 C4 C3 119.6(9) . . ? O4 C4 C3 114.2(7) . . ? C1 O1 Cr 112.8(5) . . ? C2 O2 Cr 114.0(5) . . ? C4 O4 Cr 113.6(4) . . ? C10 N2 C14 118.4(7) . . ? C10 N2 Cr 125.0(5) . . ? C14 N2 Cr 116.5(6) . . ? C9 N1 C5 117.4(7) . . ? C9 N1 Cr 123.1(5) . . ? C5 N1 Cr 118.9(6) . . ? C7 C8 C9 120.8(8) . . ? N2 C14 C13 123.0(9) . . ? C5 C6 C7 117.7(8) . . ? O5 C1 O1 124.3(8) . . ? O5 C1 C2 121.5(7) . . ? O1 C1 C2 114.2(6) . . ? N2 C10 N3 121.3(7) . . ? N2 C10 C11 121.7(8) . . ? N3 C10 C11 116.9(8) . . ? O6 C2 O2 125.5(8) . . ? O6 C2 C1 120.9(7) . . ? O2 C2 C1 113.6(7) . . ? C12 C11 C10 118.5(8) . . ? N1 C9 N3 120.7(7) . . ? N1 C9 C8 120.7(8) . . ? N3 C9 C8 118.6(8) . . ? C9 N3 C10 129.8(7) . . ? C12 C13 C14 119.1(8) . . ? C13 C12 C11 119.4(8) . . ? C6 C5 N1 124.7(8) . . ? C8 C7 C6 118.6(8) . . ? _diffrn_measured_fraction_theta_max 0.782 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.782 _refine_diff_density_max 0.508 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.060 #COMP3.CIF data_Compound_3_Hdpa[Cr(dpa)(ox)2].4H2O _database_code_CSD 161711 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Hdpa[Cr(dpa)(ox)2] . 4H2O' _chemical_formula_sum 'C24 H27 Cr N6 O12' _chemical_formula_weight 643.52 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2942(16) _cell_length_b 11.380(3) _cell_length_c 14.292(3) _cell_angle_alpha 93.78(2) _cell_angle_beta 95.838(14) _cell_angle_gamma 111.39(2) _cell_volume 1391.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 4166 _diffrn_reflns_av_R_equivalents 0.3680 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3611 _reflns_number_gt 3108 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1105P)^2^+2.0131P] 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 SHELXL _refine_ls_extinction_coef 0.003(2) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3611 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.20884(5) 0.20680(5) 0.38264(3) 0.0284(2) Uani 1 1 d . . . N1 N 0.3438(3) 0.1632(3) 0.48646(18) 0.0297(6) Uani 1 1 d . . . N2 N 0.3973(3) 0.3747(3) 0.38341(19) 0.0312(6) Uani 1 1 d . . . N3 N 0.5789(3) 0.2790(3) 0.4305(2) 0.0351(7) Uani 1 1 d . . . O1 O 0.2820(2) 0.1327(2) 0.27789(16) 0.0345(6) Uani 1 1 d . . . O2 O 0.0512(2) 0.0329(2) 0.37109(16) 0.0380(6) Uani 1 1 d . . . O3 O 0.0647(3) 0.2528(2) 0.29400(15) 0.0373(6) Uani 1 1 d . . . O4 O 0.1097(2) 0.2717(2) 0.47742(15) 0.0362(6) Uani 1 1 d . . . O5 O 0.2027(3) -0.0330(3) 0.16855(19) 0.0552(7) Uani 1 1 d . . . O6 O -0.0276(3) -0.1547(3) 0.2818(2) 0.0587(8) Uani 1 1 d . . . O7 O -0.1624(3) 0.2796(3) 0.29502(19) 0.0588(8) Uani 1 1 d . . . O8 O -0.0943(3) 0.3279(3) 0.49070(18) 0.0483(7) Uani 1 1 d . . . C1 C 0.2693(4) 0.0905(3) 0.5522(2) 0.0382(8) Uani 1 1 d . . . H1 H 0.1625 0.0697 0.5506 0.056(3) Uiso 1 1 calc R . . C2 C 0.3446(4) 0.0472(4) 0.6198(3) 0.0433(9) Uani 1 1 d . . . H2 H 0.2906 -0.0019 0.6638 0.056(3) Uiso 1 1 calc R . . C3 C 0.5810(4) 0.1527(3) 0.5588(2) 0.0370(8) Uani 1 1 d . . . H3 H 0.6878 0.1739 0.5597 0.056(3) Uiso 1 1 calc R . . C4 C 0.5046(4) 0.0780(4) 0.6220(3) 0.0436(9) Uani 1 1 d . . . H4 H 0.5584 0.0476 0.6665 0.056(3) Uiso 1 1 calc R . . C5 C 0.4989(4) 0.1977(3) 0.4920(2) 0.0300(7) Uani 1 1 d . . . C6 C 0.5455(4) 0.3783(3) 0.3947(2) 0.0300(7) Uani 1 1 d . . . C7 C 0.6689(4) 0.4812(3) 0.3720(2) 0.0373(8) Uani 1 1 d . . . H7 H 0.7689 0.4799 0.3776 0.056(3) Uiso 1 1 calc R . . C8 C 0.6431(4) 0.5844(3) 0.3413(3) 0.0420(9) Uani 1 1 d . . . H8 H 0.7250 0.6536 0.3262 0.056(3) Uiso 1 1 calc R . . C9 C 0.4929(4) 0.5840(3) 0.3332(2) 0.0406(9) Uani 1 1 d . . . H9 H 0.4725 0.6534 0.3137 0.056(3) Uiso 1 1 calc R . . C10 C 0.3753(4) 0.4791(3) 0.3544(2) 0.0367(8) Uani 1 1 d . . . H10 H 0.2748 0.4793 0.3488 0.056(3) Uiso 1 1 calc R . . C11 C 0.1896(4) 0.0211(3) 0.2424(2) 0.0345(8) Uani 1 1 d . . . C12 C 0.0569(4) -0.0437(3) 0.3016(2) 0.0366(8) Uani 1 1 d . . . C13 C -0.0450(4) 0.2738(3) 0.3353(2) 0.0361(8) Uani 1 1 d . . . C14 C -0.0106(4) 0.2928(3) 0.4432(2) 0.0353(8) Uani 1 1 d . . . N4 N 0.7092(3) 0.3018(3) 0.1014(2) 0.0430(7) Uani 1 1 d . . . H4N H 0.760(6) 0.221(6) 0.097(4) 0.097(17) Uiso 1 1 d . . . N5 N 0.7371(4) 0.0787(3) 0.0960(2) 0.0476(8) Uani 1 1 d . . . N6 N 0.5114(4) 0.1125(3) 0.1221(2) 0.0419(8) Uani 1 1 d . . . H6N H 0.429(5) 0.082(4) 0.135(3) 0.046(13) Uiso 1 1 d . . . C15 C 0.7670(5) 0.4287(4) 0.0946(3) 0.0568(11) Uani 1 1 d . . . H15 H 0.8708 0.4691 0.0860 0.056(3) Uiso 1 1 calc R . . C16 C 0.6753(5) 0.4965(4) 0.1002(3) 0.0569(11) Uani 1 1 d . . . H16 H 0.7146 0.5832 0.0953 0.056(3) Uiso 1 1 calc R . . C17 C 0.5197(5) 0.4338(4) 0.1137(3) 0.0504(10) Uani 1 1 d . . . H17 H 0.4546 0.4791 0.1174 0.056(3) Uiso 1 1 calc R . . C18 C 0.4629(4) 0.3064(4) 0.1215(2) 0.0427(9) Uani 1 1 d . . . H18 H 0.3597 0.2649 0.1308 0.056(3) Uiso 1 1 calc R . . C19 C 0.5615(4) 0.2392(3) 0.1155(2) 0.0353(8) Uani 1 1 d . . . C20 C 0.5919(4) 0.0297(3) 0.1142(2) 0.0371(8) Uani 1 1 d . . . C21 C 0.5160(5) -0.0979(3) 0.1254(3) 0.0442(9) Uani 1 1 d . . . H21 H 0.4129 -0.1292 0.1371 0.056(3) Uiso 1 1 calc R . . C22 C 0.5986(5) -0.1768(4) 0.1186(3) 0.0546(11) Uani 1 1 d . . . H22 H 0.5529 -0.2623 0.1268 0.056(3) Uiso 1 1 calc R . . C23 C 0.7502(5) -0.1262(4) 0.0992(3) 0.0625(12) Uani 1 1 d . . . H23 H 0.8083 -0.1771 0.0935 0.056(3) Uiso 1 1 calc R . . C24 C 0.8134(5) -0.0001(4) 0.0886(3) 0.0590(11) Uani 1 1 d . . . H24 H 0.9157 0.0330 0.0754 0.056(3) Uiso 1 1 calc R . . O9 O 0.2165(4) 0.5934(3) 0.1576(2) 0.0782(10) Uani 1 1 d . . . O10 O 0.0508(4) -0.2792(3) 0.0673(2) 0.0745(9) Uani 1 1 d . . . O11 O 0.1035(4) 0.3309(4) 0.1123(2) 0.0785(10) Uani 1 1 d . . . O12 O 0.0615(4) -0.3695(4) 0.3087(2) 0.0838(10) 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 0.0167(3) 0.0389(4) 0.0305(3) 0.0034(2) 0.0060(2) 0.0109(2) N1 0.0199(14) 0.0372(15) 0.0334(15) 0.0048(12) 0.0082(11) 0.0109(12) N2 0.0217(14) 0.0359(16) 0.0371(15) 0.0016(12) 0.0048(11) 0.0122(12) N3 0.0217(14) 0.0410(17) 0.0476(17) 0.0116(14) 0.0119(12) 0.0145(13) O1 0.0214(12) 0.0409(14) 0.0402(13) 0.0029(11) 0.0129(10) 0.0086(11) O2 0.0240(12) 0.0466(14) 0.0377(13) 0.0048(11) 0.0115(10) 0.0045(10) O3 0.0286(13) 0.0558(15) 0.0308(12) 0.0032(11) 0.0038(10) 0.0201(11) O4 0.0238(12) 0.0572(15) 0.0322(12) 0.0023(11) 0.0046(10) 0.0207(11) O5 0.0498(16) 0.0542(17) 0.0525(17) -0.0145(14) 0.0211(13) 0.0086(13) O6 0.0522(17) 0.0406(17) 0.0682(19) 0.0019(14) 0.0127(14) -0.0008(14) O7 0.0416(16) 0.095(2) 0.0502(16) 0.0048(15) -0.0027(13) 0.0403(16) O8 0.0319(14) 0.0754(19) 0.0473(15) 0.0016(13) 0.0108(12) 0.0307(13) C1 0.0283(19) 0.045(2) 0.040(2) 0.0069(16) 0.0097(15) 0.0107(16) C2 0.042(2) 0.050(2) 0.039(2) 0.0122(17) 0.0087(16) 0.0166(18) C3 0.0259(18) 0.043(2) 0.045(2) 0.0033(16) 0.0022(15) 0.0169(15) C4 0.042(2) 0.049(2) 0.044(2) 0.0095(18) -0.0010(17) 0.0231(18) C5 0.0240(18) 0.0328(18) 0.0357(18) -0.0002(14) 0.0051(14) 0.0141(14) C6 0.0224(17) 0.0364(19) 0.0317(17) 0.0001(14) 0.0055(13) 0.0117(14) C7 0.0225(17) 0.042(2) 0.044(2) 0.0049(16) 0.0071(15) 0.0075(15) C8 0.037(2) 0.040(2) 0.043(2) 0.0060(17) 0.0099(16) 0.0048(16) C9 0.046(2) 0.036(2) 0.041(2) 0.0044(16) 0.0032(16) 0.0173(17) C10 0.0278(18) 0.041(2) 0.044(2) -0.0003(16) 0.0008(15) 0.0182(16) C11 0.0260(18) 0.038(2) 0.041(2) 0.0057(17) 0.0055(15) 0.0133(16) C12 0.0264(18) 0.041(2) 0.042(2) 0.0088(17) 0.0053(15) 0.0106(17) C13 0.0217(18) 0.046(2) 0.042(2) 0.0010(16) 0.0010(16) 0.0152(15) C14 0.0195(17) 0.045(2) 0.0420(19) 0.0049(16) 0.0081(15) 0.0114(15) N4 0.0379(18) 0.0432(19) 0.0504(19) 0.0103(14) 0.0074(14) 0.0169(15) N5 0.0389(19) 0.0482(19) 0.058(2) 0.0016(15) 0.0063(15) 0.0194(16) N6 0.0364(19) 0.044(2) 0.0470(19) 0.0066(14) 0.0142(15) 0.0141(16) C15 0.046(2) 0.050(3) 0.073(3) 0.016(2) 0.013(2) 0.013(2) C16 0.069(3) 0.034(2) 0.069(3) 0.0118(19) 0.013(2) 0.019(2) C17 0.062(3) 0.055(3) 0.046(2) 0.0090(18) 0.0104(19) 0.034(2) C18 0.045(2) 0.052(2) 0.040(2) 0.0082(17) 0.0113(16) 0.0261(19) C19 0.042(2) 0.038(2) 0.0264(17) 0.0042(14) 0.0048(14) 0.0150(17) C20 0.044(2) 0.043(2) 0.0280(17) 0.0026(15) 0.0042(15) 0.0212(18) C21 0.052(2) 0.040(2) 0.042(2) 0.0059(16) 0.0114(17) 0.0169(18) C22 0.070(3) 0.044(2) 0.054(2) 0.0080(19) 0.009(2) 0.026(2) C23 0.066(3) 0.060(3) 0.075(3) 0.002(2) -0.001(2) 0.042(2) C24 0.044(2) 0.059(3) 0.078(3) 0.003(2) 0.007(2) 0.026(2) O9 0.079(2) 0.085(2) 0.072(2) 0.0151(18) 0.0054(17) 0.0330(19) O10 0.079(2) 0.064(2) 0.068(2) -0.0060(16) -0.0119(17) 0.0202(17) O11 0.105(3) 0.087(2) 0.0465(17) 0.0100(16) 0.0067(17) 0.040(2) O12 0.092(3) 0.091(3) 0.065(2) -0.0049(18) 0.0093(18) 0.032(2) _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 O4 1.962(2) . ? Cr1 O2 1.971(2) . ? Cr1 O1 1.968(2) . ? Cr1 O3 1.982(2) . ? Cr1 N1 2.048(3) . ? Cr1 N2 2.067(3) . ? N1 C5 1.341(4) . ? N1 C1 1.365(4) . ? N2 C6 1.355(4) . ? N2 C10 1.360(4) . ? N3 C5 1.385(4) . ? N3 C6 1.390(4) . ? O1 C11 1.280(4) . ? O2 C12 1.296(4) . ? O3 C13 1.314(4) . ? O4 C14 1.283(4) . ? O5 C11 1.226(4) . ? O6 C12 1.215(4) . ? O7 C13 1.207(4) . ? O8 C14 1.234(4) . ? C1 C2 1.358(5) . ? C1 H1 0.9300 . ? C2 C4 1.395(5) . ? C2 H2 0.9300 . ? C3 C4 1.354(5) . ? C3 C5 1.399(5) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C6 C7 1.392(5) . ? C7 C8 1.371(5) . ? C7 H7 0.9300 . ? C8 C9 1.387(5) . ? C8 H8 0.9300 . ? C9 C10 1.369(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.553(5) . ? C13 C14 1.527(5) . ? N4 C19 1.340(5) . ? N4 C15 1.359(5) . ? N4 H4N 1.18(6) . ? N5 C20 1.320(5) . ? N5 C24 1.336(5) . ? N6 C19 1.357(5) . ? N6 C20 1.407(5) . ? N6 H6N 0.76(4) . ? C15 C16 1.346(6) . ? C15 H15 0.9300 . ? C16 C17 1.400(6) . ? C16 H16 0.9300 . ? C17 C18 1.367(6) . ? C17 H17 0.9300 . ? C18 C19 1.397(5) . ? C18 H18 0.9300 . ? C20 C21 1.392(5) . ? C21 C22 1.382(6) . ? C21 H21 0.9300 . ? C22 C23 1.379(6) . ? C22 H22 0.9300 . ? C23 C24 1.364(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cr1 O2 93.48(10) . . ? O4 Cr1 O1 172.74(9) . . ? O2 Cr1 O1 81.95(9) . . ? O4 Cr1 O3 82.26(9) . . ? O2 Cr1 O3 88.86(10) . . ? O1 Cr1 O3 91.97(9) . . ? O4 Cr1 N1 91.13(10) . . ? O2 Cr1 N1 90.43(10) . . ? O1 Cr1 N1 94.53(10) . . ? O3 Cr1 N1 173.30(9) . . ? O4 Cr1 N2 96.08(10) . . ? O2 Cr1 N2 170.02(10) . . ? O1 Cr1 N2 88.81(10) . . ? O3 Cr1 N2 95.25(10) . . ? N1 Cr1 N2 86.53(11) . . ? C5 N1 C1 118.3(3) . . ? C5 N1 Cr1 124.3(2) . . ? C1 N1 Cr1 117.4(2) . . ? C6 N2 C10 117.2(3) . . ? C6 N2 Cr1 121.3(2) . . ? C10 N2 Cr1 120.2(2) . . ? C5 N3 C6 127.4(3) . . ? C11 O1 Cr1 114.5(2) . . ? C12 O2 Cr1 115.4(2) . . ? C13 O3 Cr1 112.6(2) . . ? C14 O4 Cr1 114.3(2) . . ? C2 C1 N1 122.7(3) . . ? C2 C1 H1 118.6 . . ? N1 C1 H1 118.6 . . ? C1 C2 C4 118.6(3) . . ? C1 C2 H2 120.7 . . ? C4 C2 H2 120.7 . . ? C4 C3 C5 119.9(3) . . ? C4 C3 H3 120.1 . . ? C5 C3 H3 120.1 . . ? C3 C4 C2 119.4(3) . . ? C3 C4 H4 120.3 . . ? C2 C4 H4 120.3 . . ? N1 C5 N3 119.5(3) . . ? N1 C5 C3 120.9(3) . . ? N3 C5 C3 119.6(3) . . ? N2 C6 N3 120.6(3) . . ? N2 C6 C7 121.4(3) . . ? N3 C6 C7 117.9(3) . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 118.9(3) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 118.6(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C9 123.6(3) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? O5 C11 O1 124.1(3) . . ? O5 C11 C12 121.4(3) . . ? O1 C11 C12 114.4(3) . . ? O6 C12 O2 126.6(3) . . ? O6 C12 C11 120.9(3) . . ? O2 C12 C11 112.5(3) . . ? O7 C13 O3 125.4(3) . . ? O7 C13 C14 121.2(3) . . ? O3 C13 C14 113.4(3) . . ? O8 C14 O4 124.8(3) . . ? O8 C14 C13 120.2(3) . . ? O4 C14 C13 114.9(3) . . ? C19 N4 C15 122.3(3) . . ? C19 N4 H4N 103(3) . . ? C15 N4 H4N 135(3) . . ? C20 N5 C24 117.1(3) . . ? C19 N6 C20 129.6(3) . . ? C19 N6 H6N 115(3) . . ? C20 N6 H6N 115(3) . . ? N4 C15 C16 120.5(4) . . ? N4 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 118.7(4) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 119.3(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? N4 C19 N6 119.3(3) . . ? N4 C19 C18 118.7(3) . . ? N6 C19 C18 122.0(3) . . ? N5 C20 C21 123.6(3) . . ? N5 C20 N6 117.2(3) . . ? C21 C20 N6 119.2(3) . . ? C22 C21 C20 118.0(4) . . ? C22 C21 H21 121.0 . . ? C20 C21 H21 121.0 . . ? C21 C22 C23 118.7(4) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 118.8(4) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? N5 C24 C23 123.8(4) . . ? N5 C24 H24 118.1 . . ? C23 C24 H24 118.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.415 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.092 #Comp4.cif data_Compound_4_Rad[Cr(dpa)(ox)2].H2O _database_code_CSD 161712 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Rad[Cr(dpa)(ox)2] . H2O' _chemical_formula_sum 'C27 H30 Cr N6 O11' _chemical_formula_weight 666.57 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 21.999(8) _cell_length_b 16.248(4) _cell_length_c 17.111(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.18(3) _cell_angle_gamma 90.00 _cell_volume 5741(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18505 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 29.08 _reflns_number_total 6964 _reflns_number_gt 4344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1098P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6964 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1740 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.66674(2) 0.42689(3) 0.93000(3) 0.03024(15) Uani 1 1 d . . . O1 O 0.71543(10) 0.52940(12) 0.94865(13) 0.0396(5) Uani 1 1 d . . . O2 O 0.80983(13) 0.57867(15) 0.94891(19) 0.0643(7) Uani 1 1 d . . . O3 O 0.74914(10) 0.37864(12) 0.93332(13) 0.0385(5) Uani 1 1 d . . . O4 O 0.85045(11) 0.41600(14) 0.94883(16) 0.0551(6) Uani 1 1 d . . . O5 O 0.64126(10) 0.43900(11) 0.80793(12) 0.0363(5) Uani 1 1 d . . . O6 O 0.61803(12) 0.35971(13) 0.69537(13) 0.0494(6) Uani 1 1 d . . . O7 O 0.62130(10) 0.32125(12) 0.89735(12) 0.0362(5) Uani 1 1 d . . . O8 O 0.58662(13) 0.23594(14) 0.78905(15) 0.0575(7) Uani 1 1 d . . . N1 N 0.68988(11) 0.40643(14) 1.05506(14) 0.0317(5) Uani 1 1 d . . . N2 N 0.58603(11) 0.48824(14) 0.93602(14) 0.0312(5) Uani 1 1 d . . . N3 N 0.63832(12) 0.52774(15) 1.07569(16) 0.0342(6) Uani 1 1 d . . . H3N H 0.6317(13) 0.5529(17) 1.1079(19) 0.019(7) Uiso 1 1 d . . . C1 C 0.72633(15) 0.3394(2) 1.0892(2) 0.0416(7) Uani 1 1 d . . . H1 H 0.7342(15) 0.3008(19) 1.055(2) 0.042(9) Uiso 1 1 d . . . C2 C 0.75298(17) 0.3268(2) 1.1727(2) 0.0490(8) Uani 1 1 d . . . H2 H 0.7770(17) 0.281(2) 1.189(2) 0.051(10) Uiso 1 1 d . . . C3 C 0.74292(16) 0.3846(2) 1.2259(2) 0.0470(8) Uani 1 1 d . . . H3 H 0.7655(15) 0.3772(19) 1.294(2) 0.051(9) Uiso 1 1 d . . . C4 C 0.70439(15) 0.4515(2) 1.19349(19) 0.0398(7) Uani 1 1 d . . . H4 H 0.6898(16) 0.489(2) 1.224(2) 0.046(9) Uiso 1 1 d . . . C5 C 0.67796(13) 0.46051(17) 1.10715(17) 0.0312(6) Uani 1 1 d . . . C6 C 0.58881(13) 0.53657(17) 1.00141(17) 0.0296(6) Uani 1 1 d . . . C7 C 0.54079(15) 0.59571(18) 0.9946(2) 0.0364(7) Uani 1 1 d . . . H7 H 0.5438(14) 0.6254(19) 1.038(2) 0.037(8) Uiso 1 1 d . . . C8 C 0.48849(15) 0.6019(2) 0.9232(2) 0.0397(7) Uani 1 1 d . . . H8 H 0.4569(15) 0.6449(19) 0.9186(19) 0.040(8) Uiso 1 1 d . . . C9 C 0.48306(16) 0.5472(2) 0.8588(2) 0.0412(7) Uani 1 1 d . . . H9 H 0.4517(15) 0.5482(18) 0.810(2) 0.032(8) Uiso 1 1 d . . . C10 C 0.53176(15) 0.4926(2) 0.86713(19) 0.0384(7) Uani 1 1 d . . . H10 H 0.5308(16) 0.454(2) 0.826(2) 0.052(10) Uiso 1 1 d . . . C11 C 0.77442(16) 0.52195(19) 0.94784(18) 0.0395(7) Uani 1 1 d . . . C12 C 0.79455(15) 0.43226(19) 0.94324(18) 0.0392(7) Uani 1 1 d . . . C13 C 0.62340(14) 0.37063(17) 0.76771(18) 0.0331(6) Uani 1 1 d . . . C14 C 0.60842(14) 0.30161(17) 0.82008(18) 0.0343(6) Uani 1 1 d . . . O11 O 0.97892(13) 0.70813(15) 1.1295(2) 0.0703(8) Uani 1 1 d . . . O12 O 0.83363(16) 0.51968(16) 1.1639(3) 0.1030(13) Uani 1 1 d . . . N11 N 0.93072(12) 0.67583(15) 1.14281(16) 0.0397(6) Uani 1 1 d . . . N12 N 0.86225(14) 0.58643(16) 1.1610(2) 0.0518(7) Uani 1 1 d . . . N13 N 1.03536(12) 0.39998(15) 1.11403(16) 0.0395(6) Uani 1 1 d . . . C21 C 0.91829(14) 0.59455(19) 1.14546(19) 0.0376(7) Uani 1 1 d . . . C22 C 0.87602(15) 0.72887(19) 1.1463(2) 0.0403(7) Uani 1 1 d . . . C23 C 0.9030(2) 0.8031(3) 1.2009(3) 0.0604(10) Uani 1 1 d . . . H23C H 0.9289(18) 0.785(2) 1.256(2) 0.051(10) Uiso 1 1 d . . . H23A H 0.925(3) 0.842(3) 1.175(3) 0.118(19) Uiso 1 1 d . . . H23B H 0.866(2) 0.833(3) 1.196(3) 0.080(14) Uiso 1 1 d . . . C24 C 0.8402(2) 0.7579(2) 1.0575(2) 0.0507(9) Uani 1 1 d . . . H24B H 0.869(2) 0.783(2) 1.037(2) 0.072(13) Uiso 1 1 d . . . H24C H 0.825(2) 0.713(3) 1.021(3) 0.076(13) Uiso 1 1 d . . . H24A H 0.8089(16) 0.7923(19) 1.0600(19) 0.034(8) Uiso 1 1 d . . . C25 C 0.83736(15) 0.66677(19) 1.1804(2) 0.0420(7) Uani 1 1 d . . . C26 C 0.8545(2) 0.6695(4) 1.2740(3) 0.0674(12) Uani 1 1 d . . . H26C H 0.829(2) 0.617(3) 1.291(3) 0.082(13) Uiso 1 1 d . . . H26A H 0.835(2) 0.714(3) 1.289(3) 0.071(13) Uiso 1 1 d . . . H26B H 0.899(3) 0.672(3) 1.301(3) 0.111(18) Uiso 1 1 d . . . C27 C 0.76449(17) 0.6701(3) 1.1375(3) 0.0565(9) Uani 1 1 d . . . H27C H 0.7543(18) 0.649(2) 1.081(3) 0.065(12) Uiso 1 1 d . . . H27A H 0.752(2) 0.728(3) 1.141(3) 0.081(14) Uiso 1 1 d . . . H27B H 0.746(2) 0.629(3) 1.163(3) 0.078(13) Uiso 1 1 d . . . C28 C 0.95829(14) 0.52757(17) 1.13408(18) 0.0360(7) Uani 1 1 d . . . C29 C 1.01110(15) 0.5419(2) 1.1085(2) 0.0422(7) Uani 1 1 d . . . H29 H 1.0211(14) 0.599(2) 1.0961(19) 0.041(8) Uiso 1 1 d . . . C30 C 1.04849(16) 0.4781(2) 1.0994(2) 0.0430(8) Uani 1 1 d . . . H30 H 1.0799(18) 0.481(2) 1.079(2) 0.062(11) Uiso 1 1 d . . . C31 C 1.0741(2) 0.3312(3) 1.0997(3) 0.0546(9) Uani 1 1 d . . . H31B H 1.109(2) 0.354(2) 1.083(3) 0.077(13) Uiso 1 1 d . . . H31C H 1.045(2) 0.300(3) 1.051(3) 0.083(14) Uiso 1 1 d . . . H31A H 1.082(2) 0.295(3) 1.139(3) 0.080(14) Uiso 1 1 d . . . C32 C 0.98471(16) 0.3843(2) 1.1388(2) 0.0428(7) Uani 1 1 d . . . H32 H 0.9796(15) 0.332(2) 1.146(2) 0.048(10) Uiso 1 1 d . . . C33 C 0.94606(16) 0.44547(19) 1.1489(2) 0.0411(7) Uani 1 1 d . . . H33 H 0.9125(16) 0.4328(18) 1.163(2) 0.040(9) Uiso 1 1 d . . . O O 0.57908(16) 0.2352(2) 1.0180(2) 0.0680(8) Uani 1 1 d . . . H2O H 0.5956(19) 0.254(2) 0.987(3) 0.058(12) Uiso 1 1 d . . . H1O H 0.602(2) 0.193(3) 1.030(3) 0.063(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0372(3) 0.0281(3) 0.0278(3) -0.00198(17) 0.0143(2) -0.00187(18) O1 0.0482(13) 0.0297(11) 0.0442(13) -0.0052(8) 0.0201(11) -0.0030(9) O2 0.0676(17) 0.0499(16) 0.088(2) -0.0146(13) 0.0426(16) -0.0237(12) O3 0.0465(12) 0.0317(11) 0.0441(13) -0.0015(8) 0.0241(11) -0.0005(9) O4 0.0458(13) 0.0602(16) 0.0667(17) 0.0026(12) 0.0288(13) 0.0016(11) O5 0.0529(13) 0.0289(11) 0.0307(11) -0.0005(8) 0.0190(10) -0.0057(9) O6 0.0769(17) 0.0440(13) 0.0295(12) -0.0027(9) 0.0210(11) -0.0131(11) O7 0.0488(12) 0.0339(11) 0.0286(11) 0.0010(8) 0.0166(10) -0.0078(9) O8 0.0858(18) 0.0453(14) 0.0465(14) -0.0079(10) 0.0293(14) -0.0306(12) N1 0.0343(12) 0.0320(13) 0.0302(13) -0.0002(9) 0.0129(11) 0.0024(9) N2 0.0347(13) 0.0320(13) 0.0272(13) -0.0019(9) 0.0113(11) -0.0001(9) N3 0.0398(14) 0.0324(14) 0.0319(14) -0.0081(10) 0.0144(12) 0.0026(10) C1 0.0502(19) 0.0370(17) 0.0418(19) 0.0007(13) 0.0213(16) 0.0100(14) C2 0.049(2) 0.052(2) 0.047(2) 0.0109(16) 0.0173(17) 0.0173(16) C3 0.0441(19) 0.061(2) 0.0351(18) 0.0051(15) 0.0121(16) 0.0073(15) C4 0.0401(17) 0.0493(19) 0.0301(16) -0.0001(13) 0.0120(14) 0.0054(14) C5 0.0292(14) 0.0337(15) 0.0315(15) -0.0024(11) 0.0114(12) -0.0014(11) C6 0.0329(14) 0.0276(14) 0.0316(15) -0.0002(11) 0.0153(13) -0.0044(11) C7 0.0464(18) 0.0310(16) 0.0370(17) -0.0022(12) 0.0213(15) 0.0000(12) C8 0.0399(17) 0.0370(17) 0.0455(19) 0.0075(13) 0.0188(16) 0.0070(13) C9 0.0400(18) 0.0471(19) 0.0326(18) 0.0054(13) 0.0076(15) 0.0036(14) C10 0.0451(18) 0.0395(17) 0.0296(16) 0.0002(13) 0.0115(14) -0.0002(13) C11 0.0487(18) 0.0420(18) 0.0315(16) -0.0064(12) 0.0187(15) -0.0106(14) C12 0.0437(18) 0.0491(19) 0.0292(16) 0.0005(13) 0.0182(14) -0.0024(14) C13 0.0390(16) 0.0314(16) 0.0308(15) 0.0044(11) 0.0144(13) 0.0031(12) C14 0.0395(16) 0.0322(16) 0.0345(16) -0.0010(12) 0.0172(14) -0.0076(12) O11 0.0583(16) 0.0423(15) 0.122(3) 0.0025(14) 0.0464(17) -0.0103(12) O12 0.091(2) 0.0412(16) 0.219(4) 0.0112(19) 0.107(3) -0.0077(15) N11 0.0373(14) 0.0371(15) 0.0447(16) 0.0025(11) 0.0142(12) -0.0051(11) N12 0.0509(17) 0.0400(16) 0.075(2) 0.0075(13) 0.0346(16) -0.0028(12) N13 0.0408(14) 0.0390(14) 0.0382(15) 0.0040(11) 0.0130(12) -0.0018(11) C21 0.0336(15) 0.0425(18) 0.0351(17) 0.0007(12) 0.0099(13) -0.0067(12) C22 0.0382(17) 0.0376(17) 0.0400(18) -0.0049(13) 0.0069(14) -0.0035(13) C23 0.054(2) 0.050(2) 0.069(3) -0.019(2) 0.011(2) -0.0056(19) C24 0.053(2) 0.045(2) 0.049(2) 0.0116(17) 0.0114(19) -0.0014(18) C25 0.0356(16) 0.0458(18) 0.0440(19) 0.0028(14) 0.0130(15) 0.0021(13) C26 0.060(3) 0.097(4) 0.045(2) 0.011(2) 0.017(2) 0.017(3) C27 0.0392(19) 0.063(3) 0.063(3) 0.001(2) 0.0119(19) -0.0067(17) C28 0.0360(16) 0.0379(17) 0.0301(15) 0.0013(12) 0.0063(13) -0.0068(12) C29 0.0450(18) 0.0340(17) 0.050(2) 0.0021(14) 0.0188(16) -0.0101(14) C30 0.0398(18) 0.046(2) 0.047(2) 0.0009(14) 0.0196(16) -0.0069(14) C31 0.056(2) 0.048(2) 0.065(3) 0.009(2) 0.028(2) 0.0094(18) C32 0.053(2) 0.0341(18) 0.0451(19) 0.0075(14) 0.0220(16) -0.0047(14) C33 0.0469(19) 0.0391(18) 0.0428(19) 0.0019(13) 0.0224(16) -0.0079(14) O 0.081(2) 0.065(2) 0.073(2) 0.0129(15) 0.0463(18) 0.0060(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr O1 1.946(2) . ? Cr O3 1.958(2) . ? Cr O7 1.9677(19) . ? Cr O5 1.977(2) . ? Cr N1 2.049(2) . ? Cr N2 2.070(2) . ? O1 C11 1.308(4) . ? O2 C11 1.203(4) . ? O3 C12 1.292(4) . ? O4 C12 1.229(4) . ? O5 C13 1.294(3) . ? O6 C13 1.215(3) . ? O7 C14 1.293(3) . ? O8 C14 1.214(3) . ? N1 C5 1.340(3) . ? N1 C1 1.360(4) . ? N2 C6 1.351(3) . ? N2 C10 1.360(4) . ? N3 C6 1.366(4) . ? N3 C5 1.386(4) . ? C1 C2 1.359(5) . ? C2 C3 1.378(5) . ? C3 C4 1.373(5) . ? C4 C5 1.396(4) . ? C6 C7 1.403(4) . ? C7 C8 1.362(5) . ? C8 C9 1.387(5) . ? C9 C10 1.361(5) . ? C11 C12 1.533(4) . ? C13 C14 1.540(4) . ? O11 N11 1.272(3) . ? O12 N12 1.264(4) . ? N11 C21 1.353(4) . ? N11 C22 1.498(4) . ? N12 C21 1.355(4) . ? N12 C25 1.496(4) . ? N13 C30 1.344(4) . ? N13 C32 1.346(4) . ? N13 C31 1.476(4) . ? C21 C28 1.454(4) . ? C22 C23 1.516(5) . ? C22 C24 1.526(5) . ? C22 C25 1.557(4) . ? C25 C26 1.513(5) . ? C25 C27 1.517(5) . ? C28 C29 1.395(4) . ? C28 C33 1.401(4) . ? C29 C30 1.366(5) . ? C32 C33 1.358(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cr O3 83.47(9) . . ? O1 Cr O7 171.90(8) . . ? O3 Cr O7 91.93(9) . . ? O1 Cr O5 91.58(9) . . ? O3 Cr O5 89.59(9) . . ? O7 Cr O5 81.71(8) . . ? O1 Cr N1 92.48(9) . . ? O3 Cr N1 90.62(9) . . ? O7 Cr N1 94.23(9) . . ? O5 Cr N1 175.94(9) . . ? O1 Cr N2 90.73(9) . . ? O3 Cr N2 173.28(9) . . ? O7 Cr N2 94.23(9) . . ? O5 Cr N2 93.97(9) . . ? N1 Cr N2 86.24(9) . . ? C11 O1 Cr 114.26(18) . . ? C12 O3 Cr 113.58(19) . . ? C13 O5 Cr 113.56(17) . . ? C14 O7 Cr 114.60(16) . . ? C5 N1 C1 117.5(2) . . ? C5 N1 Cr 123.58(19) . . ? C1 N1 Cr 118.43(19) . . ? C6 N2 C10 117.6(2) . . ? C6 N2 Cr 121.79(18) . . ? C10 N2 Cr 119.57(19) . . ? C6 N3 C5 129.6(2) . . ? C2 C1 N1 123.3(3) . . ? C1 C2 C3 118.8(3) . . ? C4 C3 C2 119.4(3) . . ? C3 C4 C5 118.9(3) . . ? N1 C5 N3 120.0(2) . . ? N1 C5 C4 122.0(3) . . ? N3 C5 C4 118.0(3) . . ? N2 C6 N3 120.2(2) . . ? N2 C6 C7 120.8(3) . . ? N3 C6 C7 119.0(3) . . ? C8 C7 C6 120.2(3) . . ? C7 C8 C9 118.7(3) . . ? C10 C9 C8 119.0(3) . . ? N2 C10 C9 123.3(3) . . ? O2 C11 O1 124.6(3) . . ? O2 C11 C12 122.2(3) . . ? O1 C11 C12 113.2(2) . . ? O4 C12 O3 125.0(3) . . ? O4 C12 C11 120.0(3) . . ? O3 C12 C11 115.1(3) . . ? O6 C13 O5 124.9(3) . . ? O6 C13 C14 121.4(3) . . ? O5 C13 C14 113.7(2) . . ? O8 C14 O7 125.3(3) . . ? O8 C14 C13 121.1(3) . . ? O7 C14 C13 113.6(2) . . ? O11 N11 C21 126.8(3) . . ? O11 N11 C22 120.0(2) . . ? C21 N11 C22 112.7(2) . . ? O12 N12 C21 126.2(3) . . ? O12 N12 C25 121.0(3) . . ? C21 N12 C25 112.7(3) . . ? C30 N13 C32 119.5(3) . . ? C30 N13 C31 120.7(3) . . ? C32 N13 C31 119.8(3) . . ? N11 C21 N12 108.1(3) . . ? N11 C21 C28 126.0(3) . . ? N12 C21 C28 126.0(3) . . ? N11 C22 C23 109.5(3) . . ? N11 C22 C24 106.4(3) . . ? C23 C22 C24 109.0(3) . . ? N11 C22 C25 101.1(2) . . ? C23 C22 C25 115.7(3) . . ? C24 C22 C25 114.4(3) . . ? N12 C25 C26 106.4(3) . . ? N12 C25 C27 109.3(3) . . ? C26 C25 C27 110.4(3) . . ? N12 C25 C22 101.1(2) . . ? C26 C25 C22 114.1(3) . . ? C27 C25 C22 114.7(3) . . ? C29 C28 C33 116.7(3) . . ? C29 C28 C21 121.6(3) . . ? C33 C28 C21 121.7(3) . . ? C30 C29 C28 120.5(3) . . ? N13 C30 C29 121.3(3) . . ? N13 C32 C33 121.6(3) . . ? C32 C33 C28 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 29.08 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.951 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.097 #COMP5.CIF data_compound_5_Sr[Cr(dpa)(ox)2]2.8H2O _database_code_CSD 161713 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Sr[Cr(dpa)(ox)2]2 . 8H2O ' _chemical_formula_sum 'C28 H34 Cr2 N6 O24 Sr' _chemical_formula_weight 1030.23 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' 'Sr' 'Sr' -1.5307 3.2498 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4572(19) _cell_length_b 12.095(2) _cell_length_c 17.850(4) _cell_angle_alpha 99.95(3) _cell_angle_beta 99.57(3) _cell_angle_gamma 104.87(3) _cell_volume 1895.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 2.068 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 7114 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_sigmaI/netI 0.1632 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6674 _reflns_number_gt 4338 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0853P)^2^+1.8489P] 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 SHELXL _refine_ls_extinction_coef 551(34) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6674 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.498 _refine_ls_shift/su_mean 0.009 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.08286(14) 0.47840(11) 0.26773(11) 0.0940(6) Uani 1 1 d . . . Cr1 Cr -0.2851(2) 0.76689(16) 0.39497(10) 0.0543(5) Uani 1 1 d . . . Cr2 Cr 0.44521(19) 0.19148(16) 0.13288(10) 0.0536(5) Uani 1 1 d . . . O2 O -0.2623(9) 0.6949(8) 0.2906(5) 0.066(2) Uani 1 1 d . . . O10 O 0.2671(8) 0.1674(6) 0.1786(4) 0.0546(17) Uani 1 1 d . . . O6 O -0.4758(8) 0.7882(6) 0.3478(4) 0.0544(17) Uani 1 1 d . . . O13 O 0.5799(9) 0.2597(7) 0.2367(5) 0.063(2) Uani 1 1 d . . . O1 O -0.1020(9) 0.7231(8) 0.4300(5) 0.071(2) Uani 1 1 d . . . O14 O 0.6343(9) 0.2387(8) 0.0975(5) 0.067(2) Uani 1 1 d . . . O12 O 0.1272(9) 0.2685(8) 0.2300(5) 0.069(2) Uani 1 1 d . . . O16 O 0.8714(9) 0.3460(8) 0.1448(6) 0.075(2) Uani 1 1 d . . . O9 O 0.4148(9) 0.3468(7) 0.1331(5) 0.064(2) Uani 1 1 d . . . C19 C 0.2161(12) 0.0210(11) -0.0007(6) 0.059(3) Uani 1 1 d . . . O8 O -0.7133(9) 0.6851(7) 0.2957(5) 0.068(2) Uani 1 1 d . . . O7 O -0.6524(11) 0.5011(8) 0.3544(6) 0.076(2) Uani 1 1 d . . . N1 N -0.1650(10) 0.9323(8) 0.3897(5) 0.056(2) Uani 1 1 d . . . N2 N -0.2996(11) 0.8423(9) 0.5039(5) 0.058(2) Uani 1 1 d . . . N4 N 0.3176(11) 0.1273(9) 0.0221(5) 0.063(2) Uani 1 1 d . . . O15 O 0.8164(9) 0.3606(8) 0.2923(5) 0.073(2) Uani 1 1 d . . . O11 O 0.2725(11) 0.4567(8) 0.1755(5) 0.076(2) Uani 1 1 d . . . C14 C -0.5877(12) 0.6964(10) 0.3313(6) 0.052(2) Uani 1 1 d . . . C3 C 0.9458(17) 0.1413(12) 0.3463(8) 0.077(4) Uani 1 1 d . . . C28 C 0.7455(14) 0.2976(10) 0.1519(8) 0.063(3) Uani 1 1 d . . . C5 C -0.1991(13) 1.0280(10) 0.4189(7) 0.057(3) Uani 1 1 d . . . O5 O -0.4159(9) 0.6131(7) 0.3983(5) 0.0607(19) Uani 1 1 d . . . N6 N 0.2244(11) -0.0640(9) 0.0418(6) 0.066(3) Uani 1 1 d . . . O3 O 0.0428(10) 0.6222(9) 0.3834(7) 0.084(3) Uani 1 1 d . . . N5 N 0.4542(11) 0.0232(9) 0.1333(5) 0.059(2) Uani 1 1 d . . . O4 O -0.1308(13) 0.5892(9) 0.2379(6) 0.087(3) Uani 1 1 d . . . C6 C -0.3158(12) 0.9478(11) 0.5210(7) 0.057(3) Uani 1 1 d . . . N3 N -0.2884(11) 1.0259(9) 0.4741(6) 0.063(2) Uani 1 1 d . . . C25 C 0.3099(14) 0.3637(11) 0.1664(7) 0.060(3) Uani 1 1 d . . . C13 C -0.5520(14) 0.5937(11) 0.3631(7) 0.061(3) Uani 1 1 d . . . C11 C -0.0623(13) 0.6624(11) 0.3762(8) 0.062(3) Uani 1 1 d . . . C12 C -0.1582(14) 0.6453(11) 0.2936(7) 0.063(3) Uani 1 1 d . . . C10 C -0.3259(13) 0.7697(12) 0.5546(7) 0.066(3) Uani 1 1 d . . . C15 C 0.3110(15) 0.2044(12) -0.0251(7) 0.067(3) Uani 1 1 d . . . C24 C 0.5704(14) 0.0086(12) 0.1837(7) 0.064(3) Uani 1 1 d . . . C26 C 0.2241(12) 0.2582(10) 0.1954(6) 0.054(3) Uani 1 1 d . . . C22 C 0.4544(18) -0.1995(13) 0.1581(9) 0.078(4) Uani 1 1 d . . . C20 C 0.3421(14) -0.0721(11) 0.0943(6) 0.061(3) Uani 1 1 d . . . C21 C 0.3417(17) -0.1833(13) 0.1071(9) 0.079(4) Uani 1 1 d . . . C2 C 0.9950(15) 0.0445(12) 0.3204(7) 0.069(3) Uani 1 1 d . . . C4 C 0.8484(16) 0.1345(12) 0.3955(8) 0.072(3) Uani 1 1 d . . . C7 C -0.3593(14) 0.9895(12) 0.5910(7) 0.069(3) Uani 1 1 d . . . C8 C -0.3856(16) 0.9135(15) 0.6397(7) 0.077(4) Uani 1 1 d . . . C1 C -0.0632(13) 0.9413(12) 0.3428(8) 0.070(3) Uani 1 1 d . . . C27 C 0.7145(14) 0.3094(11) 0.2352(7) 0.063(3) Uani 1 1 d . . . C9 C -0.3686(16) 0.8038(13) 0.6221(7) 0.072(3) Uani 1 1 d . . . C23 C 0.5717(17) -0.0990(14) 0.1964(8) 0.077(4) Uani 1 1 d . . . C18 C 0.1039(16) -0.0118(13) -0.0682(8) 0.076(4) Uani 1 1 d . . . C16 C 0.2036(19) 0.1802(14) -0.0911(8) 0.082(4) Uani 1 1 d . . . C17 C 0.0954(17) 0.0698(14) -0.1123(8) 0.080(4) Uani 1 1 d . . . O17 O 0.3223(10) 0.7450(8) 0.4804(5) 0.070(2) Uani 1 1 d . . . O18 O 1.0032(13) 0.2766(9) 0.0270(6) 0.098(3) Uani 1 1 d . . . O19 O -0.2918(14) 0.4273(9) 0.4324(6) 0.093(3) Uani 1 1 d . . . O20 O 0.6215(15) 0.5428(11) 0.1021(7) 0.113(4) Uani 1 1 d . . . O21 O -0.8853(19) 0.8196(14) 0.2280(9) 0.134(5) Uani 1 1 d . . . O22 O 0.0897(18) 0.4116(13) 0.4195(9) 0.136(5) Uani 1 1 d . . . O23 O 0.215(2) 0.4911(15) 0.0093(12) 0.157(6) Uani 1 1 d . . . O24 O 0.061(2) 0.5730(16) 0.1252(11) 0.163(6) 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 Sr1 0.0457(7) 0.0542(7) 0.1609(15) -0.0195(8) 0.0217(8) 0.0079(5) Cr1 0.0483(10) 0.0562(10) 0.0560(10) 0.0080(8) 0.0083(8) 0.0165(8) Cr2 0.0452(9) 0.0564(10) 0.0530(10) 0.0057(8) 0.0109(7) 0.0087(8) O2 0.063(5) 0.072(5) 0.059(4) 0.003(4) 0.006(4) 0.024(4) O10 0.045(4) 0.052(4) 0.066(4) 0.011(3) 0.018(3) 0.011(3) O6 0.049(4) 0.052(4) 0.063(4) 0.014(3) 0.009(3) 0.017(3) O13 0.049(4) 0.069(5) 0.063(5) 0.009(4) 0.013(4) 0.006(4) O1 0.058(5) 0.083(6) 0.068(5) 0.011(4) 0.004(4) 0.028(4) O14 0.051(5) 0.078(6) 0.063(5) 0.008(4) 0.017(4) 0.008(4) O12 0.060(5) 0.065(5) 0.082(6) 0.011(4) 0.023(4) 0.019(4) O16 0.049(5) 0.080(6) 0.091(6) 0.012(5) 0.028(4) 0.011(4) O9 0.062(5) 0.058(5) 0.072(5) 0.011(4) 0.023(4) 0.013(4) C19 0.044(6) 0.074(8) 0.050(6) 0.001(5) 0.008(5) 0.012(5) O8 0.054(5) 0.066(5) 0.077(5) 0.010(4) 0.010(4) 0.015(4) O7 0.081(6) 0.051(5) 0.089(6) 0.009(4) 0.016(5) 0.013(5) N1 0.049(5) 0.055(5) 0.059(5) 0.007(4) 0.008(4) 0.010(4) N2 0.056(5) 0.064(6) 0.057(5) 0.018(4) 0.013(4) 0.021(5) N4 0.061(6) 0.061(6) 0.055(5) 0.001(4) 0.007(4) 0.010(5) O15 0.051(5) 0.078(6) 0.070(5) 0.006(4) -0.005(4) 0.007(4) O11 0.091(7) 0.058(5) 0.080(6) 0.014(4) 0.016(5) 0.024(5) C14 0.042(6) 0.055(6) 0.056(6) 0.012(5) 0.010(5) 0.008(5) C3 0.090(10) 0.071(8) 0.071(8) 0.022(7) 0.021(7) 0.018(7) C28 0.054(7) 0.055(7) 0.083(8) 0.015(6) 0.022(6) 0.016(5) C5 0.052(6) 0.055(6) 0.060(6) 0.005(5) 0.001(5) 0.020(5) O5 0.058(5) 0.059(5) 0.064(5) 0.014(4) 0.003(4) 0.021(4) N6 0.060(6) 0.059(6) 0.068(6) 0.008(5) 0.004(5) 0.010(5) O3 0.052(5) 0.080(6) 0.127(8) 0.018(6) 0.024(5) 0.032(5) N5 0.056(5) 0.063(6) 0.057(5) 0.014(4) 0.012(4) 0.015(5) O4 0.109(8) 0.085(7) 0.081(6) 0.006(5) 0.043(6) 0.048(6) C6 0.044(6) 0.064(7) 0.058(6) 0.012(5) 0.007(5) 0.013(5) N3 0.061(6) 0.074(6) 0.066(6) 0.023(5) 0.023(5) 0.030(5) C25 0.068(7) 0.060(7) 0.053(6) 0.014(5) 0.007(5) 0.020(6) C13 0.067(8) 0.061(7) 0.054(6) 0.013(5) 0.015(6) 0.019(6) C11 0.050(6) 0.058(7) 0.074(8) 0.012(6) 0.018(6) 0.008(5) C12 0.060(7) 0.055(7) 0.076(8) 0.010(6) 0.026(6) 0.013(6) C10 0.051(6) 0.078(8) 0.058(7) 0.017(6) 0.000(5) 0.006(6) C15 0.067(8) 0.080(8) 0.067(7) 0.027(6) 0.026(6) 0.031(7) C24 0.064(7) 0.085(9) 0.055(6) 0.027(6) 0.011(5) 0.034(7) C26 0.043(6) 0.056(6) 0.054(6) 0.000(5) 0.006(5) 0.006(5) C22 0.084(9) 0.076(9) 0.088(9) 0.024(7) 0.025(8) 0.037(8) C20 0.061(7) 0.071(8) 0.046(6) 0.006(5) 0.013(5) 0.019(6) C21 0.075(9) 0.074(9) 0.092(10) 0.026(7) 0.018(7) 0.024(7) C2 0.061(7) 0.077(9) 0.062(7) 0.010(6) 0.016(6) 0.009(6) C4 0.079(9) 0.067(8) 0.083(8) 0.030(7) 0.031(7) 0.029(7) C7 0.061(7) 0.082(9) 0.065(7) 0.012(6) 0.020(6) 0.018(6) C8 0.067(8) 0.110(12) 0.050(7) 0.010(7) 0.011(6) 0.027(8) C1 0.048(6) 0.079(9) 0.075(8) 0.005(7) 0.018(6) 0.011(6) C27 0.058(7) 0.057(7) 0.063(7) 0.001(5) 0.004(6) 0.013(6) C9 0.078(9) 0.086(9) 0.051(7) 0.022(6) 0.010(6) 0.021(7) C23 0.076(9) 0.093(10) 0.071(8) 0.023(7) 0.018(7) 0.035(8) C18 0.075(9) 0.087(10) 0.060(7) 0.007(7) 0.017(6) 0.019(7) C16 0.101(11) 0.082(10) 0.070(8) 0.019(7) 0.026(8) 0.036(9) C17 0.082(9) 0.094(10) 0.057(7) 0.000(7) 0.011(6) 0.028(8) O17 0.077(6) 0.066(5) 0.068(5) 0.014(4) 0.020(4) 0.024(4) O18 0.101(8) 0.075(6) 0.093(7) -0.011(5) 0.023(6) 0.005(6) O19 0.113(8) 0.079(7) 0.085(6) 0.021(5) 0.014(6) 0.029(6) O20 0.123(10) 0.105(9) 0.096(8) 0.037(7) 0.020(7) -0.001(7) O21 0.160(13) 0.143(12) 0.131(11) 0.041(9) 0.036(10) 0.089(11) O22 0.145(13) 0.109(10) 0.126(10) 0.009(8) -0.004(9) 0.020(9) O23 0.170(15) 0.129(12) 0.207(17) 0.071(12) 0.090(14) 0.055(11) O24 0.171(16) 0.151(14) 0.180(16) 0.061(12) 0.065(13) 0.036(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 Sr1 O3 2.606(10) . ? Sr1 O7 2.636(10) 1_655 ? Sr1 O8 2.643(9) 1_655 ? Sr1 O16 2.657(9) 1_455 ? Sr1 O11 2.659(10) . ? Sr1 O12 2.669(9) . ? Sr1 O15 2.704(9) 1_455 ? Sr1 O4 2.728(10) . ? Sr1 O22 2.954(16) . ? Sr1 O24 2.963(18) . ? Sr1 C14 3.394(11) 1_655 ? Sr1 C13 3.394(13) 1_655 ? Cr1 O6 1.958(7) . ? Cr1 O5 1.969(8) . ? Cr1 O1 1.973(8) . ? Cr1 O2 1.987(8) . ? Cr1 N2 2.042(9) . ? Cr1 N1 2.058(10) . ? Cr2 O10 1.968(7) . ? Cr2 O13 1.971(8) . ? Cr2 O9 1.971(9) . ? Cr2 O14 1.974(8) . ? Cr2 N4 2.041(9) . ? Cr2 N5 2.060(10) . ? O2 C12 1.276(15) . ? O10 C26 1.271(13) . ? O6 C14 1.273(13) . ? O13 C27 1.269(14) . ? O1 C11 1.273(15) . ? O14 C28 1.262(15) . ? O12 C26 1.208(13) . ? O16 C28 1.222(14) . ? O16 Sr1 2.657(9) 1_655 ? O9 C25 1.280(15) . ? C19 N4 1.340(15) . ? C19 N6 1.389(16) . ? C19 C18 1.389(17) . ? O8 C14 1.212(13) . ? O8 Sr1 2.643(9) 1_455 ? O7 C13 1.235(15) . ? O7 Sr1 2.636(10) 1_455 ? N1 C5 1.325(14) . ? N1 C1 1.373(15) . ? N2 C6 1.314(15) . ? N2 C10 1.374(15) . ? N4 C15 1.366(16) . ? O15 C27 1.225(14) . ? O15 Sr1 2.704(9) 1_655 ? O11 C25 1.255(14) . ? C14 C13 1.540(16) . ? C14 Sr1 3.394(11) 1_455 ? C3 C4 1.371(19) . ? C3 C2 1.40(2) . ? C28 C27 1.553(18) . ? C5 N3 1.399(15) . ? C5 C4 1.410(17) 1_465 ? O5 C13 1.277(14) . ? N6 C20 1.367(15) . ? O3 C11 1.211(15) . ? N5 C20 1.337(15) . ? N5 C24 1.369(14) . ? O4 C12 1.207(14) . ? C6 N3 1.371(15) . ? C6 C7 1.430(17) . ? C25 C26 1.547(17) . ? C13 Sr1 3.394(13) 1_455 ? C11 C12 1.548(18) . ? C10 C9 1.364(18) . ? C15 C16 1.355(19) . ? C24 C23 1.361(19) . ? C22 C21 1.36(2) . ? C22 C23 1.39(2) . ? C20 C21 1.402(19) . ? C2 C1 1.383(19) 1_645 ? C4 C5 1.410(17) 1_645 ? C7 C8 1.38(2) . ? C8 C9 1.37(2) . ? C1 C2 1.383(19) 1_465 ? C18 C17 1.37(2) . ? C16 C17 1.40(2) . ? 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 O3 Sr1 O7 87.4(3) . 1_655 ? O3 Sr1 O8 70.0(3) . 1_655 ? O7 Sr1 O8 63.1(3) 1_655 1_655 ? O3 Sr1 O16 125.7(3) . 1_455 ? O7 Sr1 O16 144.6(3) 1_655 1_455 ? O8 Sr1 O16 134.5(3) 1_655 1_455 ? O3 Sr1 O11 142.5(3) . . ? O7 Sr1 O11 71.0(3) 1_655 . ? O8 Sr1 O11 72.9(3) 1_655 . ? O16 Sr1 O11 85.1(3) 1_455 . ? O3 Sr1 O12 142.0(3) . . ? O7 Sr1 O12 75.2(3) 1_655 . ? O8 Sr1 O12 126.5(3) 1_655 . ? O16 Sr1 O12 70.6(3) 1_455 . ? O11 Sr1 O12 62.4(3) . . ? O3 Sr1 O15 76.6(3) . 1_455 ? O7 Sr1 O15 125.1(3) 1_655 1_455 ? O8 Sr1 O15 145.3(3) 1_655 1_455 ? O16 Sr1 O15 61.8(3) 1_455 1_455 ? O11 Sr1 O15 141.0(3) . 1_455 ? O12 Sr1 O15 86.1(3) . 1_455 ? O3 Sr1 O4 61.7(3) . . ? O7 Sr1 O4 144.1(3) 1_655 . ? O8 Sr1 O4 87.8(3) 1_655 . ? O16 Sr1 O4 71.0(3) 1_455 . ? O11 Sr1 O4 122.4(3) . . ? O12 Sr1 O4 140.5(3) . . ? O15 Sr1 O4 67.9(3) 1_455 . ? O3 Sr1 O22 61.4(4) . . ? O7 Sr1 O22 62.6(4) 1_655 . ? O8 Sr1 O22 106.0(3) 1_655 . ? O16 Sr1 O22 119.0(4) 1_455 . ? O11 Sr1 O22 126.3(4) . . ? O12 Sr1 O22 80.6(4) . . ? O15 Sr1 O22 63.7(4) 1_455 . ? O4 Sr1 O22 110.9(4) . . ? O3 Sr1 O24 110.6(4) . . ? O7 Sr1 O24 120.3(4) 1_655 . ? O8 Sr1 O24 70.7(4) 1_655 . ? O16 Sr1 O24 63.8(4) 1_455 . ? O11 Sr1 O24 60.5(4) . . ? O12 Sr1 O24 107.4(4) . . ? O15 Sr1 O24 114.5(4) 1_455 . ? O4 Sr1 O24 62.0(4) . . ? O22 Sr1 O24 171.9(5) . . ? O3 Sr1 C14 74.7(3) . 1_655 ? O7 Sr1 C14 44.9(3) 1_655 1_655 ? O8 Sr1 C14 18.3(3) 1_655 1_655 ? O16 Sr1 C14 146.1(3) 1_455 1_655 ? O11 Sr1 C14 68.3(3) . 1_655 ? O12 Sr1 C14 111.6(3) . 1_655 ? O15 Sr1 C14 149.8(3) 1_455 1_655 ? O4 Sr1 C14 105.2(3) . 1_655 ? O22 Sr1 C14 94.2(3) . 1_655 ? O24 Sr1 C14 84.3(4) . 1_655 ? O3 Sr1 C13 82.6(3) . 1_655 ? O7 Sr1 C13 18.8(3) 1_655 1_655 ? O8 Sr1 C13 44.5(3) 1_655 1_655 ? O16 Sr1 C13 151.3(3) 1_455 1_655 ? O11 Sr1 C13 67.0(3) . 1_655 ? O12 Sr1 C13 89.8(3) . 1_655 ? O15 Sr1 C13 139.7(3) 1_455 1_655 ? O4 Sr1 C13 129.3(3) . 1_655 ? O22 Sr1 C13 76.1(4) . 1_655 ? O24 Sr1 C13 105.0(4) . 1_655 ? C14 Sr1 C13 26.2(3) 1_655 1_655 ? O6 Cr1 O5 82.6(3) . . ? O6 Cr1 O1 171.2(4) . . ? O5 Cr1 O1 92.1(4) . . ? O6 Cr1 O2 90.5(3) . . ? O5 Cr1 O2 88.6(4) . . ? O1 Cr1 O2 82.3(4) . . ? O6 Cr1 N2 91.6(4) . . ? O5 Cr1 N2 92.4(4) . . ? O1 Cr1 N2 95.6(4) . . ? O2 Cr1 N2 177.7(4) . . ? O6 Cr1 N1 92.5(3) . . ? O5 Cr1 N1 175.0(4) . . ? O1 Cr1 N1 92.8(4) . . ? O2 Cr1 N1 92.7(4) . . ? N2 Cr1 N1 86.4(4) . . ? O10 Cr2 O13 91.4(3) . . ? O10 Cr2 O9 82.5(3) . . ? O13 Cr2 O9 88.2(4) . . ? O10 Cr2 O14 171.6(3) . . ? O13 Cr2 O14 82.6(3) . . ? O9 Cr2 O14 91.3(4) . . ? O10 Cr2 N4 92.3(4) . . ? O13 Cr2 N4 175.9(4) . . ? O9 Cr2 N4 90.7(4) . . ? O14 Cr2 N4 93.5(4) . . ? O10 Cr2 N5 92.0(4) . . ? O13 Cr2 N5 94.1(4) . . ? O9 Cr2 N5 174.1(4) . . ? O14 Cr2 N5 94.4(4) . . ? N4 Cr2 N5 87.5(4) . . ? C12 O2 Cr1 113.4(8) . . ? C26 O10 Cr2 114.9(7) . . ? C14 O6 Cr1 114.7(7) . . ? C27 O13 Cr2 114.2(7) . . ? C11 O1 Cr1 114.6(8) . . ? C28 O14 Cr2 113.6(7) . . ? C26 O12 Sr1 119.5(8) . . ? C28 O16 Sr1 121.0(9) . 1_655 ? C25 O9 Cr2 113.4(7) . . ? N4 C19 N6 120.1(10) . . ? N4 C19 C18 122.9(12) . . ? N6 C19 C18 116.9(11) . . ? C14 O8 Sr1 118.6(8) . 1_455 ? C13 O7 Sr1 117.9(8) . 1_455 ? C5 N1 C1 118.5(11) . . ? C5 N1 Cr1 122.5(8) . . ? C1 N1 Cr1 118.0(8) . . ? C6 N2 C10 119.0(10) . . ? C6 N2 Cr1 122.4(8) . . ? C10 N2 Cr1 117.0(8) . . ? C19 N4 C15 117.6(10) . . ? C19 N4 Cr2 122.8(8) . . ? C15 N4 Cr2 118.0(8) . . ? C27 O15 Sr1 117.9(8) . 1_655 ? C25 O11 Sr1 117.8(8) . . ? O8 C14 O6 126.7(11) . . ? O8 C14 C13 120.0(10) . . ? O6 C14 C13 113.3(10) . . ? O8 C14 Sr1 43.2(6) . 1_455 ? O6 C14 Sr1 169.8(8) . 1_455 ? C13 C14 Sr1 76.9(6) . 1_455 ? C4 C3 C2 120.4(13) . . ? O16 C28 O14 126.5(12) . . ? O16 C28 C27 118.3(11) . . ? O14 C28 C27 115.1(10) . . ? N1 C5 N3 120.4(11) . . ? N1 C5 C4 122.6(11) . 1_465 ? N3 C5 C4 117.0(10) . 1_465 ? C13 O5 Cr1 113.0(7) . . ? C20 N6 C19 130.0(10) . . ? C11 O3 Sr1 121.4(9) . . ? C20 N5 C24 118.3(11) . . ? C20 N5 Cr2 122.7(8) . . ? C24 N5 Cr2 118.4(8) . . ? C12 O4 Sr1 116.9(9) . . ? N2 C6 N3 122.3(10) . . ? N2 C6 C7 121.9(11) . . ? N3 C6 C7 115.8(11) . . ? C6 N3 C5 128.1(10) . . ? O11 C25 O9 125.1(11) . . ? O11 C25 C26 119.5(11) . . ? O9 C25 C26 115.4(10) . . ? O7 C13 O5 124.5(12) . . ? O7 C13 C14 120.0(11) . . ? O5 C13 C14 115.5(10) . . ? O7 C13 Sr1 43.3(6) . 1_455 ? O5 C13 Sr1 167.1(8) . 1_455 ? C14 C13 Sr1 76.9(6) . 1_455 ? O3 C11 O1 127.0(12) . . ? O3 C11 C12 118.9(11) . . ? O1 C11 C12 114.0(10) . . ? O3 C11 Sr1 40.9(7) . . ? O1 C11 Sr1 166.6(9) . . ? C12 C11 Sr1 78.7(7) . . ? O4 C12 O2 125.0(13) . . ? O4 C12 C11 119.9(12) . . ? O2 C12 C11 115.1(10) . . ? C9 C10 N2 122.0(13) . . ? C16 C15 N4 123.2(13) . . ? C23 C24 N5 121.7(12) . . ? O12 C26 O10 127.3(11) . . ? O12 C26 C25 119.4(11) . . ? O10 C26 C25 113.3(10) . . ? C21 C22 C23 116.1(13) . . ? N5 C20 N6 121.3(11) . . ? N5 C20 C21 120.5(11) . . ? N6 C20 C21 118.2(11) . . ? C22 C21 C20 122.1(14) . . ? C1 C2 C3 118.0(12) 1_645 . ? C3 C4 C5 117.9(12) . 1_645 ? C8 C7 C6 117.1(12) . . ? C9 C8 C7 121.1(12) . . ? N1 C1 C2 122.0(12) . 1_465 ? O15 C27 O13 125.7(12) . . ? O15 C27 C28 120.3(11) . . ? O13 C27 C28 114.0(10) . . ? C10 C9 C8 118.9(12) . . ? C24 C23 C22 121.2(13) . . ? C17 C18 C19 118.1(13) . . ? C15 C16 C17 118.1(14) . . ? C18 C17 C16 120.0(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.996 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.123