# SUBMISSION DETAILS _publ_contact_author_name 'Dr. James K. McCusker' _publ_contact_author_address ; Department of Chemistry Michigan State University East Lansing, MI 48824 USA ; _publ_contact_author_email 'jkm@cem.msu.edu' _publ_contact_author_fax '(517) 353-1793' _publ_contact_author_phone '(517) 355-9715 ext.106' _publ_contact_letter ; Fellowed please find the CIF file of the crystal structure about our manuscript. Dr. James K. McCusker Associate Professor Department of Chemistry Michigan State University East Lansing, MI 48824 Jkm@cem.msu.edu ; _publ_requested_journal 'Inorganic Chemistry' _publ_requested_category '' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Title : Spin Exchange Effects on the Physicochemical Properties of Tetraoxalene-bridged Bimetallic Complexes ; loop_ _publ_author_name _publ_author_address 'Dong Guo' ; Department of Chemistry Michigan State University East Lansing, MI 48824 ; 'James K. McCusker' ; Department of Chemistry Michigan State University East Lansing, MI 48824 ; #============================================================================== data_complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H84 B2 Cl2 Ga2 N8 O6' _chemical_formula_weight 1341.39 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6041(17) _cell_length_b 9.6219(12) _cell_length_c 25.158(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.093(2) _cell_angle_gamma 90.00 _cell_volume 3274.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 821 _cell_measurement_theta_min 2.671 _cell_measurement_theta_max 21.908 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 31855 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5756 _reflns_number_gt 3541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0433P)^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 5756 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.89116(3) 0.32955(4) 0.553317(15) 0.02479(13) Uani 1 1 d . . . Cl1 Cl 1.05433(8) 0.16092(11) 0.39950(4) 0.0461(3) Uani 1 1 d . . . O1 O 0.95993(17) 0.2819(2) 0.49246(9) 0.0265(6) Uani 1 1 d . . . O2 O 0.90773(18) 0.1400(2) 0.57672(9) 0.0273(6) Uani 1 1 d . . . N1 N 0.8676(2) 0.5289(3) 0.52446(11) 0.0280(7) Uani 1 1 d . . . H1A H 0.9201 0.5828 0.5352 0.034 Uiso 1 1 calc R . . H1B H 0.8597 0.5279 0.4885 0.034 Uiso 1 1 calc R . . N2 N 1.0086(2) 0.3812(3) 0.61005(11) 0.0275(8) Uani 1 1 d . . . H2A H 1.0439 0.3045 0.6197 0.033 Uiso 1 1 calc R . . H2B H 1.0486 0.4423 0.5959 0.033 Uiso 1 1 calc R . . N3 N 0.7464(2) 0.2642(3) 0.51669(12) 0.0367(9) Uani 1 1 d . . . H3A H 0.7302 0.3130 0.4865 0.044 Uiso 1 1 calc R . . H3B H 0.7482 0.1736 0.5080 0.044 Uiso 1 1 calc R . . N4 N 0.8045(2) 0.3936(3) 0.61303(11) 0.0253(7) Uani 1 1 d . . . C1 C 0.7782(3) 0.5855(4) 0.54498(15) 0.0360(10) Uani 1 1 d . . . H1C H 0.7200 0.5523 0.5230 0.043 Uiso 1 1 calc R . . H1D H 0.7790 0.6861 0.5428 0.043 Uiso 1 1 calc R . . C2 C 0.7724(3) 0.5417(4) 0.60291(14) 0.0304(9) Uani 1 1 d . . . H2C H 0.8141 0.6025 0.6264 0.037 Uiso 1 1 calc R . . H2D H 0.7049 0.5525 0.6115 0.037 Uiso 1 1 calc R . . C3 C 0.9700(3) 0.4431(4) 0.65762(14) 0.0296(9) Uani 1 1 d . . . H3C H 0.9642 0.5431 0.6533 0.036 Uiso 1 1 calc R . . H3D H 1.0151 0.4242 0.6893 0.036 Uiso 1 1 calc R . . C4 C 0.8700(3) 0.3811(4) 0.66374(14) 0.0285(9) Uani 1 1 d . . . H4A H 0.8776 0.2838 0.6735 0.034 Uiso 1 1 calc R . . H4B H 0.8405 0.4288 0.6921 0.034 Uiso 1 1 calc R . . C5 C 0.6708(3) 0.2871(4) 0.55446(16) 0.0448(12) Uani 1 1 d . . . H5A H 0.6238 0.2109 0.5517 0.054 Uiso 1 1 calc R . . H5B H 0.6350 0.3724 0.5453 0.054 Uiso 1 1 calc R . . C6 C 0.7199(3) 0.2962(4) 0.61031(15) 0.0377(11) Uani 1 1 d . . . H6A H 0.6726 0.3279 0.6339 0.045 Uiso 1 1 calc R . . H6B H 0.7430 0.2048 0.6222 0.045 Uiso 1 1 calc R . . C7 C 1.0266(3) 0.0725(4) 0.45624(13) 0.0226(8) Uani 1 1 d . . . C8 C 0.9810(3) 0.1421(3) 0.49543(14) 0.0228(9) Uani 1 1 d . . . C9 C 0.9532(2) 0.0703(4) 0.53979(14) 0.0221(8) Uani 1 1 d . . . B1 B 0.9687(3) 0.5583(4) 0.16157(16) 0.0251(10) Uani 1 1 d . . . C10 C 0.8349(3) 0.6251(4) 0.22862(14) 0.0350(10) Uani 1 1 d . . . H10A H 0.7973 0.5494 0.2156 0.042 Uiso 1 1 calc R . . C11 C 0.8010(3) 0.7045(5) 0.26879(16) 0.0468(12) Uani 1 1 d . . . H11A H 0.7420 0.6812 0.2822 0.056 Uiso 1 1 calc R . . C12 C 0.8544(4) 0.8181(5) 0.28890(16) 0.0528(13) Uani 1 1 d . . . H12A H 0.8314 0.8722 0.3156 0.063 Uiso 1 1 calc R . . C13 C 0.9420(4) 0.8507(4) 0.26899(16) 0.0469(12) Uani 1 1 d . . . H13A H 0.9789 0.9266 0.2825 0.056 Uiso 1 1 calc R . . C14 C 0.9751(3) 0.7704(4) 0.22890(15) 0.0355(10) Uani 1 1 d . . . H14A H 1.0344 0.7948 0.2160 0.043 Uiso 1 1 calc R . . C15 C 0.9237(3) 0.6538(4) 0.20659(13) 0.0262(9) Uani 1 1 d . . . C16 C 1.0499(3) 0.7926(5) 0.01934(17) 0.0448(12) Uani 1 1 d . . . H16A H 1.0645 0.8388 -0.0113 0.054 Uiso 1 1 calc R . . C17 C 1.0765(3) 0.6566(5) 0.02736(16) 0.0438(11) Uani 1 1 d . . . H17A H 1.1101 0.6097 0.0025 0.053 Uiso 1 1 calc R . . C18 C 1.0530(3) 0.5901(4) 0.07274(15) 0.0385(11) Uani 1 1 d . . . H18A H 1.0714 0.4975 0.0773 0.046 Uiso 1 1 calc R . . C19 C 1.0032(3) 0.6516(4) 0.11253(14) 0.0260(9) Uani 1 1 d . . . C20 C 0.9788(3) 0.7912(4) 0.10249(15) 0.0339(10) Uani 1 1 d . . . H20A H 0.9461 0.8398 0.1273 0.041 Uiso 1 1 calc R . . C21 C 1.0018(3) 0.8598(4) 0.05669(17) 0.0430(11) Uani 1 1 d . . . H21A H 0.9842 0.9526 0.0515 0.052 Uiso 1 1 calc R . . C22 C 0.7240(3) 0.4355(4) 0.07641(15) 0.0380(11) Uani 1 1 d . . . H22A H 0.6689 0.4801 0.0591 0.046 Uiso 1 1 calc R . . C23 C 0.7319(3) 0.2932(5) 0.07428(16) 0.0414(11) Uani 1 1 d . . . H23A H 0.6817 0.2403 0.0563 0.050 Uiso 1 1 calc R . . C24 C 0.8147(3) 0.2308(4) 0.09906(15) 0.0393(11) Uani 1 1 d . . . H24A H 0.8211 0.1347 0.0974 0.047 Uiso 1 1 calc R . . C25 C 0.8899(3) 0.3094(4) 0.12696(14) 0.0322(10) Uani 1 1 d . . . H25A H 0.9458 0.2641 0.1429 0.039 Uiso 1 1 calc R . . C26 C 0.8836(3) 0.4539(4) 0.13165(14) 0.0259(9) Uani 1 1 d . . . C27 C 0.7985(3) 0.5119(4) 0.10455(14) 0.0323(10) Uani 1 1 d . . . H27A H 0.7915 0.6080 0.1054 0.039 Uiso 1 1 calc R . . C28 C 1.0454(3) 0.3660(4) 0.22953(14) 0.0317(10) Uani 1 1 d . . . H28A H 0.9807 0.3419 0.2342 0.038 Uiso 1 1 calc R . . C29 C 1.1220(3) 0.2944(4) 0.25876(15) 0.0386(11) Uani 1 1 d . . . H29A H 1.1083 0.2227 0.2816 0.046 Uiso 1 1 calc R . . C30 C 1.2189(3) 0.3311(4) 0.25338(15) 0.0416(11) Uani 1 1 d . . . H30A H 1.2707 0.2840 0.2727 0.050 Uiso 1 1 calc R . . C31 C 1.2383(3) 0.4367(4) 0.21968(16) 0.0374(10) Uani 1 1 d . . . H31A H 1.3033 0.4627 0.2166 0.045 Uiso 1 1 calc R . . C32 C 1.1613(3) 0.5050(4) 0.19016(14) 0.0303(9) Uani 1 1 d . . . H32A H 1.1766 0.5754 0.1671 0.036 Uiso 1 1 calc R . . C33 C 1.0613(3) 0.4731(4) 0.19329(14) 0.0261(9) Uani 1 1 d . . . O100 O 0.84061(19) 0.4105(3) 0.41348(10) 0.0409(7) Uani 1 1 d . . . H100 H 0.8802 0.3440 0.4326 0.061 Uiso 1 1 d R . . C100 C 0.8069(3) 0.3701(4) 0.35835(18) 0.0595(14) Uani 1 1 d . . . H10D H 0.7412 0.3329 0.3568 0.071 Uiso 1 1 calc R . . H10B H 0.8506 0.3009 0.3466 0.071 Uiso 1 1 calc R . . H10C H 0.8068 0.4501 0.3355 0.071 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 Ga1 0.0330(2) 0.0177(2) 0.0240(2) 0.0010(2) 0.00434(17) 0.0021(2) Cl1 0.0685(8) 0.0323(6) 0.0392(6) 0.0051(5) 0.0138(5) 0.0006(6) O1 0.0421(16) 0.0138(13) 0.0241(14) 0.0016(10) 0.0056(12) 0.0042(11) O2 0.0426(16) 0.0159(14) 0.0240(14) 0.0017(10) 0.0062(12) 0.0057(11) N1 0.0348(19) 0.0237(18) 0.0264(18) 0.0038(14) 0.0070(15) 0.0046(15) N2 0.0307(19) 0.0258(18) 0.0266(18) 0.0032(14) 0.0055(15) 0.0054(14) N3 0.046(2) 0.0268(19) 0.035(2) 0.0013(15) -0.0067(18) 0.0001(16) N4 0.0303(19) 0.0224(18) 0.0236(18) 0.0031(14) 0.0046(15) 0.0006(14) C1 0.039(3) 0.026(2) 0.044(3) 0.0075(19) 0.007(2) 0.0099(19) C2 0.033(2) 0.027(2) 0.032(2) -0.0018(18) 0.0042(18) 0.0079(18) C3 0.037(2) 0.028(2) 0.023(2) -0.0013(17) 0.0009(18) 0.0027(19) C4 0.036(2) 0.028(2) 0.022(2) 0.0052(17) 0.0033(18) 0.0066(18) C5 0.034(3) 0.046(3) 0.053(3) 0.009(2) -0.004(2) -0.011(2) C6 0.033(3) 0.041(3) 0.039(3) 0.009(2) 0.003(2) -0.005(2) C7 0.028(2) 0.019(2) 0.021(2) 0.0041(16) 0.0024(17) 0.0003(16) C8 0.025(2) 0.017(2) 0.025(2) 0.0011(16) -0.0028(17) -0.0015(16) C9 0.022(2) 0.020(2) 0.024(2) -0.0011(17) -0.0012(17) 0.0007(16) B1 0.031(3) 0.024(2) 0.021(2) 0.0007(19) 0.003(2) -0.002(2) C10 0.039(3) 0.041(3) 0.025(2) 0.0033(18) 0.003(2) 0.006(2) C11 0.041(3) 0.067(4) 0.033(3) 0.009(2) 0.011(2) 0.022(2) C12 0.073(4) 0.056(3) 0.029(3) -0.009(2) 0.001(2) 0.037(3) C13 0.067(3) 0.033(3) 0.038(3) -0.009(2) -0.009(2) 0.015(2) C14 0.039(3) 0.030(2) 0.037(3) -0.005(2) -0.001(2) 0.006(2) C15 0.029(2) 0.026(2) 0.023(2) 0.0062(18) -0.0009(17) 0.0068(18) C16 0.036(3) 0.063(4) 0.035(3) 0.021(2) 0.003(2) -0.013(2) C17 0.045(3) 0.058(3) 0.030(2) -0.001(2) 0.011(2) -0.004(2) C18 0.048(3) 0.033(3) 0.036(3) -0.001(2) 0.011(2) -0.001(2) C19 0.024(2) 0.023(2) 0.030(2) -0.0027(18) -0.0015(17) -0.0059(17) C20 0.028(2) 0.034(3) 0.040(3) 0.0010(19) 0.0037(19) 0.0002(18) C21 0.042(3) 0.032(3) 0.054(3) 0.020(2) 0.005(2) -0.003(2) C22 0.034(3) 0.052(3) 0.028(2) -0.002(2) 0.004(2) -0.004(2) C23 0.039(3) 0.055(3) 0.031(2) -0.012(2) 0.007(2) -0.022(2) C24 0.059(3) 0.030(2) 0.033(3) -0.009(2) 0.020(2) -0.017(2) C25 0.037(2) 0.034(3) 0.027(2) -0.0032(19) 0.0090(18) -0.004(2) C26 0.031(2) 0.027(2) 0.020(2) 0.0002(17) 0.0060(18) -0.0043(18) C27 0.035(2) 0.033(2) 0.030(2) -0.0017(19) 0.007(2) -0.004(2) C28 0.036(2) 0.028(2) 0.031(2) -0.0063(18) 0.0037(19) 0.0033(19) C29 0.057(3) 0.027(3) 0.031(2) 0.0000(18) 0.001(2) 0.011(2) C30 0.046(3) 0.041(3) 0.035(2) -0.011(2) -0.011(2) 0.024(2) C31 0.033(3) 0.035(3) 0.043(3) -0.010(2) 0.002(2) 0.004(2) C32 0.038(3) 0.024(2) 0.029(2) -0.0071(18) 0.0035(19) 0.0004(19) C33 0.032(2) 0.019(2) 0.027(2) -0.0074(17) 0.0016(18) 0.0013(18) O100 0.0537(19) 0.0334(17) 0.0330(17) 0.0040(13) -0.0077(14) 0.0020(14) C100 0.061(3) 0.051(3) 0.064(3) 0.005(3) -0.001(3) -0.015(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 Ga1 O2 1.922(2) . ? Ga1 O1 1.932(2) . ? Ga1 N1 2.064(3) . ? Ga1 N2 2.086(3) . ? Ga1 N4 2.099(3) . ? Ga1 N3 2.176(3) . ? Cl1 C7 1.737(3) . ? O1 C8 1.375(4) . ? O2 C9 1.348(4) . ? N1 C1 1.476(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.482(4) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C5 1.489(5) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C6 1.481(4) . ? N4 C4 1.482(4) . ? N4 C2 1.504(4) . ? C1 C2 1.527(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.508(5) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.493(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.392(5) . ? C7 C9 1.402(5) 3_756 ? C8 C9 1.399(5) . ? C9 C7 1.402(5) 3_756 ? B1 C15 1.628(5) . ? B1 C19 1.635(5) . ? B1 C33 1.638(5) . ? B1 C26 1.652(5) . ? C10 C11 1.384(5) . ? C10 C15 1.409(5) . ? C10 H10A 0.9300 . ? C11 C12 1.379(6) . ? C11 H11A 0.9300 . ? C12 C13 1.378(6) . ? C12 H12A 0.9300 . ? C13 C14 1.383(5) . ? C13 H13A 0.9300 . ? C14 C15 1.407(5) . ? C14 H14A 0.9300 . ? C16 C21 1.364(5) . ? C16 C17 1.366(5) . ? C16 H16A 0.9300 . ? C17 C18 1.376(5) . ? C17 H17A 0.9300 . ? C18 C19 1.397(5) . ? C18 H18A 0.9300 . ? C19 C20 1.400(5) . ? C20 C21 1.392(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.375(5) . ? C22 C27 1.385(5) . ? C22 H22A 0.9300 . ? C23 C24 1.367(5) . ? C23 H23A 0.9300 . ? C24 C25 1.400(5) . ? C24 H24A 0.9300 . ? C25 C26 1.399(5) . ? C25 H25A 0.9300 . ? C26 C27 1.396(5) . ? C27 H27A 0.9300 . ? C28 C29 1.392(5) . ? C28 C33 1.408(5) . ? C28 H28A 0.9300 . ? C29 C30 1.385(5) . ? C29 H29A 0.9300 . ? C30 C31 1.367(5) . ? C30 H30A 0.9300 . ? C31 C32 1.383(5) . ? C31 H31A 0.9300 . ? C32 C33 1.405(5) . ? C32 H32A 0.9300 . ? O100 C100 1.466(5) . ? O100 H100 0.9362 . ? C100 H10D 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? 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 O2 Ga1 O1 88.10(9) . . ? O2 Ga1 N1 176.61(11) . . ? O1 Ga1 N1 90.67(10) . . ? O2 Ga1 N2 87.72(11) . . ? O1 Ga1 N2 101.46(10) . . ? N1 Ga1 N2 95.62(11) . . ? O2 Ga1 N4 96.67(10) . . ? O1 Ga1 N4 173.25(10) . . ? N1 Ga1 N4 84.30(11) . . ? N2 Ga1 N4 83.56(11) . . ? O2 Ga1 N3 85.81(11) . . ? O1 Ga1 N3 95.07(11) . . ? N1 Ga1 N3 91.15(12) . . ? N2 Ga1 N3 162.03(11) . . ? N4 Ga1 N3 80.57(12) . . ? C8 O1 Ga1 107.7(2) . . ? C9 O2 Ga1 108.0(2) . . ? C1 N1 Ga1 108.8(2) . . ? C1 N1 H1A 109.9 . . ? Ga1 N1 H1A 109.9 . . ? C1 N1 H1B 109.9 . . ? Ga1 N1 H1B 109.9 . . ? H1A N1 H1B 108.3 . . ? C3 N2 Ga1 109.7(2) . . ? C3 N2 H2A 109.7 . . ? Ga1 N2 H2A 109.7 . . ? C3 N2 H2B 109.7 . . ? Ga1 N2 H2B 109.7 . . ? H2A N2 H2B 108.2 . . ? C5 N3 Ga1 110.0(2) . . ? C5 N3 H3A 109.7 . . ? Ga1 N3 H3A 109.7 . . ? C5 N3 H3B 109.7 . . ? Ga1 N3 H3B 109.7 . . ? H3A N3 H3B 108.2 . . ? C6 N4 C4 112.5(3) . . ? C6 N4 C2 112.5(3) . . ? C4 N4 C2 111.1(3) . . ? C6 N4 Ga1 105.9(2) . . ? C4 N4 Ga1 105.0(2) . . ? C2 N4 Ga1 109.4(2) . . ? N1 C1 C2 111.1(3) . . ? N1 C1 H1C 109.4 . . ? C2 C1 H1C 109.4 . . ? N1 C1 H1D 109.4 . . ? C2 C1 H1D 109.4 . . ? H1C C1 H1D 108.0 . . ? N4 C2 C1 112.3(3) . . ? N4 C2 H2C 109.1 . . ? C1 C2 H2C 109.1 . . ? N4 C2 H2D 109.1 . . ? C1 C2 H2D 109.1 . . ? H2C C2 H2D 107.9 . . ? N2 C3 C4 108.9(3) . . ? N2 C3 H3C 109.9 . . ? C4 C3 H3C 109.9 . . ? N2 C3 H3D 109.9 . . ? C4 C3 H3D 109.9 . . ? H3C C3 H3D 108.3 . . ? N4 C4 C3 110.3(3) . . ? N4 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N4 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 109.8(3) . . ? N3 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? N3 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N4 C6 C5 110.4(3) . . ? N4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C9 121.3(3) . 3_756 ? C8 C7 Cl1 119.9(3) . . ? C9 C7 Cl1 118.7(3) 3_756 . ? O1 C8 C7 122.6(3) . . ? O1 C8 C9 117.0(3) . . ? C7 C8 C9 120.4(3) . . ? O2 C9 C8 119.1(3) . . ? O2 C9 C7 122.6(3) . 3_756 ? C8 C9 C7 118.3(3) . 3_756 ? C15 B1 C19 112.0(3) . . ? C15 B1 C33 105.7(3) . . ? C19 B1 C33 112.0(3) . . ? C15 B1 C26 111.3(3) . . ? C19 B1 C26 103.5(3) . . ? C33 B1 C26 112.6(3) . . ? C11 C10 C15 123.0(4) . . ? C11 C10 H10A 118.5 . . ? C15 C10 H10A 118.5 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C13 C12 C11 119.3(4) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 120.0(4) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C15 123.3(4) . . ? C13 C14 H14A 118.3 . . ? C15 C14 H14A 118.3 . . ? C14 C15 C10 114.2(3) . . ? C14 C15 B1 121.3(3) . . ? C10 C15 B1 124.4(3) . . ? C21 C16 C17 119.4(4) . . ? C21 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C17 C18 C19 124.8(4) . . ? C17 C18 H18A 117.6 . . ? C19 C18 H18A 117.6 . . ? C18 C19 C20 113.6(3) . . ? C18 C19 B1 120.5(3) . . ? C20 C19 B1 125.6(3) . . ? C21 C20 C19 122.3(4) . . ? C21 C20 H20A 118.8 . . ? C19 C20 H20A 118.8 . . ? C16 C21 C20 120.8(4) . . ? C16 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C23 C22 C27 119.5(4) . . ? C23 C22 H22A 120.3 . . ? C27 C22 H22A 120.3 . . ? C24 C23 C22 119.0(4) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C23 C24 C25 120.9(4) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C26 C25 C24 122.1(4) . . ? C26 C25 H25A 118.9 . . ? C24 C25 H25A 118.9 . . ? C27 C26 C25 114.3(3) . . ? C27 C26 B1 119.0(3) . . ? C25 C26 B1 126.6(3) . . ? C22 C27 C26 124.2(4) . . ? C22 C27 H27A 117.9 . . ? C26 C27 H27A 117.9 . . ? C29 C28 C33 123.1(4) . . ? C29 C28 H28A 118.5 . . ? C33 C28 H28A 118.5 . . ? C30 C29 C28 119.3(4) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.1(4) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C33 123.2(4) . . ? C31 C32 H32A 118.4 . . ? C33 C32 H32A 118.4 . . ? C32 C33 C28 114.4(3) . . ? C32 C33 B1 124.3(3) . . ? C28 C33 B1 121.2(3) . . ? C100 O100 H100 114.3 . . ? O100 C100 H10D 109.5 . . ? O100 C100 H10B 109.5 . . ? H10D C100 H10B 109.5 . . ? O100 C100 H10C 109.5 . . ? H10D C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.497 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.067 ################################################## ###### END OF CIF FOR COMPLEX 1 ####### ################################################## data_complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H84 B2 Cl2 Cr Ga N8 O6' _chemical_formula_weight 1323.67 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.646(6) _cell_length_b 9.668(4) _cell_length_c 25.117(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.149(7) _cell_angle_gamma 90.00 _cell_volume 3294(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 888 _cell_measurement_theta_min 2.665 _cell_measurement_theta_max 25.440 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1390 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details PSI-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 31578 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5801 _reflns_number_gt 3852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0359P)^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 SHELXL _refine_ls_extinction_coef 0.0041(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5801 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.60981(3) 1.82979(4) -0.552793(14) 0.02374(13) Uani 0.50 1 d P . . Cr1 Cr 0.60981(3) 1.82979(4) -0.552793(14) 0.02374(13) Uani 0.50 1 d P . . Cl1 Cl 0.44461(6) 1.66005(7) -0.39922(3) 0.03282(19) Uani 1 1 d . . . O1 O 0.53962(13) 1.78020(18) -0.49235(7) 0.0255(5) Uani 1 1 d . . . O2 O 0.59152(14) 1.64146(17) -0.57640(7) 0.0260(5) Uani 1 1 d . . . N1 N 0.63302(16) 2.0302(2) -0.52498(9) 0.0268(6) Uani 1 1 d . . . H1C H 0.6441 2.0285 -0.4890 0.032 Uiso 1 1 d R . . H1D H 0.5859 2.0951 -0.5316 0.032 Uiso 1 1 d R . . N2 N 0.49214(16) 1.8805(2) -0.60895(9) 0.0274(6) Uani 1 1 d . . . H2C H 0.4643 1.8005 -0.6210 0.033 Uiso 1 1 d R . . H2D H 0.4462 1.9432 -0.6023 0.033 Uiso 1 1 d R . . N3 N 0.75138(18) 1.7642(2) -0.51561(9) 0.0368(7) Uani 1 1 d . . . H3C H 0.7449 1.6721 -0.5121 0.044 Uiso 1 1 d R . . H3D H 0.7722 1.8123 -0.4859 0.044 Uiso 1 1 d R . . N4 N 0.69552(16) 1.8926(2) -0.61239(9) 0.0242(5) Uani 1 1 d . . . C3 C 0.5301(2) 1.9420(3) -0.65719(11) 0.0297(7) Uani 1 1 d . . . H1A H 0.5362 2.0414 -0.6530 0.036 Uiso 1 1 calc R . . H1B H 0.4845 1.9232 -0.6887 0.036 Uiso 1 1 calc R . . C4 C 0.6297(2) 1.8792(3) -0.66376(11) 0.0281(7) Uani 1 1 d . . . H2A H 0.6219 1.7823 -0.6734 0.034 Uiso 1 1 calc R . . H2B H 0.6590 1.9264 -0.6922 0.034 Uiso 1 1 calc R . . C1 C 0.7240(2) 2.0854(3) -0.54494(11) 0.0296(7) Uani 1 1 d . . . H3A H 0.7816 2.0509 -0.5229 0.036 Uiso 1 1 calc R . . H3B H 0.7244 2.1855 -0.5428 0.036 Uiso 1 1 calc R . . C2 C 0.7277(2) 2.0399(3) -0.60309(11) 0.0304(7) Uani 1 1 d . . . H4A H 0.6853 2.0998 -0.6264 0.036 Uiso 1 1 calc R . . H4B H 0.7944 2.0503 -0.6124 0.036 Uiso 1 1 calc R . . C5 C 0.8283(2) 1.7858(4) -0.55372(13) 0.0490(9) Uani 1 1 d . . . H5A H 0.8643 1.8706 -0.5447 0.059 Uiso 1 1 calc R . . H5B H 0.8748 1.7096 -0.5507 0.059 Uiso 1 1 calc R . . C6 C 0.7796(2) 1.7943(3) -0.60965(12) 0.0388(8) Uani 1 1 d . . . H6A H 0.8269 1.8251 -0.6333 0.047 Uiso 1 1 calc R . . H6B H 0.7561 1.7034 -0.6214 0.047 Uiso 1 1 calc R . . C7 C 0.47320(19) 1.5709(3) -0.45614(10) 0.0201(6) Uani 1 1 d . . . C8 C 0.51924(19) 1.6414(3) -0.49501(10) 0.0223(6) Uani 1 1 d . . . C9 C 0.54674(19) 1.5698(3) -0.53976(10) 0.0222(6) Uani 1 1 d . . . B1 B 0.5317(2) 1.0586(3) -0.16134(12) 0.0250(8) Uani 1 1 d . . . C10 C 0.6988(3) 1.2064(4) -0.26873(12) 0.0473(9) Uani 1 1 d . . . H10A H 0.7579 1.1837 -0.2819 0.057 Uiso 1 1 calc R . . C11 C 0.6651(2) 1.1266(3) -0.22860(11) 0.0338(8) Uani 1 1 d . . . H11A H 0.7025 1.0510 -0.2156 0.041 Uiso 1 1 calc R . . C12 C 0.5768(2) 1.1551(3) -0.20680(10) 0.0263(7) Uani 1 1 d . . . C13 C 0.5247(2) 1.2701(3) -0.22907(12) 0.0350(8) Uani 1 1 d . . . H13A H 0.4651 1.2930 -0.2165 0.042 Uiso 1 1 calc R . . C14 C 0.5580(3) 1.3514(3) -0.26898(13) 0.0488(9) Uani 1 1 d . . . H14A H 0.5214 1.4275 -0.2822 0.059 Uiso 1 1 calc R . . C15 C 0.6456(3) 1.3189(4) -0.28915(13) 0.0540(10) Uani 1 1 d . . . H15A H 0.6681 1.3724 -0.3161 0.065 Uiso 1 1 calc R . . C16 C 0.4507(2) 1.2930(4) -0.01872(13) 0.0443(9) Uani 1 1 d . . . H16A H 0.4356 1.3392 0.0118 0.053 Uiso 1 1 calc R . . C17 C 0.4252(2) 1.1570(4) -0.02663(12) 0.0433(8) Uani 1 1 d . . . H17A H 0.3924 1.1102 -0.0015 0.052 Uiso 1 1 calc R . . C18 C 0.4484(2) 1.0891(3) -0.07231(11) 0.0362(8) Uani 1 1 d . . . H18A H 0.4305 0.9967 -0.0769 0.043 Uiso 1 1 calc R . . C19 C 0.4977(2) 1.1531(3) -0.11201(11) 0.0266(7) Uani 1 1 d . . . C20 C 0.5220(2) 1.2909(3) -0.10241(12) 0.0359(8) Uani 1 1 d . . . H20A H 0.5547 1.3387 -0.1274 0.043 Uiso 1 1 calc R . . C21 C 0.4989(2) 1.3605(3) -0.05651(14) 0.0460(9) Uani 1 1 d . . . H21A H 0.5163 1.4529 -0.0515 0.055 Uiso 1 1 calc R . . C22 C 0.2621(2) 0.9388(3) -0.21948(12) 0.0372(8) Uani 1 1 d . . . H22A H 0.1973 0.9649 -0.2164 0.045 Uiso 1 1 calc R . . C23 C 0.2806(2) 0.8324(3) -0.25359(13) 0.0429(8) Uani 1 1 d . . . H23A H 0.2290 0.7857 -0.2730 0.051 Uiso 1 1 calc R . . C24 C 0.3773(2) 0.7965(3) -0.25849(12) 0.0375(8) Uani 1 1 d . . . H24A H 0.3911 0.7248 -0.2812 0.045 Uiso 1 1 calc R . . C25 C 0.4544(2) 0.8678(3) -0.22927(11) 0.0318(7) Uani 1 1 d . . . H25A H 0.5189 0.8437 -0.2340 0.038 Uiso 1 1 calc R . . C26 C 0.4389(2) 0.9742(3) -0.19312(11) 0.0269(7) Uani 1 1 d . . . C27 C 0.3389(2) 1.0073(3) -0.18969(11) 0.0305(7) Uani 1 1 d . . . H27A H 0.3240 1.0777 -0.1666 0.037 Uiso 1 1 calc R . . C28 C 0.7675(2) 0.7953(3) -0.07405(12) 0.0403(9) Uani 1 1 d . . . H28A H 0.8173 0.7428 -0.0557 0.048 Uiso 1 1 calc R . . C29 C 0.6854(2) 0.7321(3) -0.09896(12) 0.0395(8) Uani 1 1 d . . . H29A H 0.6792 0.6364 -0.0974 0.047 Uiso 1 1 calc R . . C30 C 0.6103(2) 0.8112(3) -0.12682(11) 0.0311(7) Uani 1 1 d . . . H30A H 0.5544 0.7666 -0.1429 0.037 Uiso 1 1 calc R . . C31 C 0.6168(2) 0.9549(3) -0.13111(10) 0.0256(7) Uani 1 1 d . . . C32 C 0.7020(2) 1.0133(3) -0.10423(11) 0.0320(7) Uani 1 1 d . . . H32A H 0.7090 1.1090 -0.1052 0.038 Uiso 1 1 calc R . . C33 C 0.7764(2) 0.9372(3) -0.07625(11) 0.0354(8) Uani 1 1 d . . . H33A H 0.8316 0.9811 -0.0591 0.043 Uiso 1 1 calc R . . O100 O 0.65822(15) 1.9113(2) -0.41281(8) 0.0405(6) Uani 1 1 d . . . H100 H 0.6337 1.8354 -0.4250 0.061 Uiso 1 1 d R . . C100 C 0.6930(2) 1.8718(3) -0.35851(12) 0.0483(9) Uani 1 1 d . . . H10D H 0.7589 1.8362 -0.3574 0.058 Uiso 1 1 calc R . . H10B H 0.6505 1.8018 -0.3465 0.058 Uiso 1 1 calc R . . H10C H 0.6927 1.9511 -0.3355 0.058 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 Ga1 0.0294(2) 0.0189(2) 0.0232(2) -0.00093(17) 0.00401(16) -0.00115(18) Cr1 0.0294(2) 0.0189(2) 0.0232(2) -0.00093(17) 0.00401(16) -0.00115(18) Cl1 0.0509(5) 0.0228(4) 0.0266(4) -0.0061(3) 0.0129(3) -0.0010(4) O1 0.0366(12) 0.0167(10) 0.0240(11) -0.0035(8) 0.0065(9) -0.0036(9) O2 0.0386(12) 0.0186(10) 0.0220(10) -0.0016(8) 0.0088(9) -0.0050(9) N1 0.0323(14) 0.0227(13) 0.0266(13) -0.0032(10) 0.0079(11) -0.0001(11) N2 0.0286(14) 0.0250(13) 0.0291(14) -0.0021(10) 0.0051(11) -0.0006(11) N3 0.0432(17) 0.0319(15) 0.0332(15) -0.0043(12) -0.0061(13) 0.0012(13) N4 0.0246(13) 0.0237(13) 0.0248(13) -0.0040(10) 0.0050(11) 0.0013(11) C3 0.0326(18) 0.0293(17) 0.0261(17) 0.0030(13) -0.0013(14) -0.0027(14) C4 0.0349(18) 0.0301(17) 0.0202(16) -0.0051(12) 0.0069(14) -0.0049(14) C1 0.0316(18) 0.0233(16) 0.0346(18) -0.0047(13) 0.0064(14) -0.0060(14) C2 0.0302(18) 0.0301(17) 0.0317(17) -0.0010(14) 0.0068(14) -0.0082(14) C5 0.036(2) 0.053(2) 0.057(2) -0.0123(18) -0.0019(18) 0.0162(17) C6 0.0350(19) 0.042(2) 0.040(2) -0.0072(15) 0.0091(16) 0.0082(15) C7 0.0223(16) 0.0214(15) 0.0163(14) -0.0033(11) 0.0009(12) 0.0026(12) C8 0.0247(16) 0.0167(15) 0.0244(15) -0.0042(12) -0.0021(12) -0.0004(12) C9 0.0220(16) 0.0198(15) 0.0244(16) -0.0006(12) 0.0009(13) 0.0022(12) B1 0.0274(19) 0.0246(18) 0.0236(18) -0.0005(14) 0.0058(15) 0.0012(15) C10 0.047(2) 0.067(3) 0.0293(19) -0.0047(18) 0.0116(17) -0.0220(19) C11 0.0351(19) 0.0410(19) 0.0251(17) -0.0034(14) 0.0027(15) -0.0030(15) C12 0.0303(17) 0.0270(17) 0.0206(15) -0.0065(13) -0.0016(13) -0.0083(14) C13 0.0380(19) 0.0298(18) 0.0369(19) 0.0055(15) 0.0020(15) -0.0047(15) C14 0.066(3) 0.037(2) 0.040(2) 0.0131(16) -0.0088(19) -0.0135(19) C15 0.073(3) 0.059(3) 0.0295(19) 0.0092(19) 0.0051(19) -0.039(2) C16 0.0317(19) 0.060(3) 0.041(2) -0.0151(18) 0.0043(16) 0.0116(17) C17 0.040(2) 0.060(2) 0.0312(19) -0.0012(17) 0.0097(15) 0.0089(18) C18 0.045(2) 0.0337(19) 0.0309(18) 0.0017(14) 0.0089(16) 0.0026(15) C19 0.0255(16) 0.0284(17) 0.0249(16) 0.0050(13) -0.0021(13) 0.0039(14) C20 0.0315(18) 0.0345(19) 0.043(2) -0.0045(15) 0.0085(15) 0.0008(14) C21 0.041(2) 0.037(2) 0.060(2) -0.0188(17) 0.0031(18) 0.0029(16) C22 0.0307(19) 0.039(2) 0.042(2) 0.0133(16) 0.0035(16) -0.0057(15) C23 0.048(2) 0.041(2) 0.0377(19) 0.0109(17) -0.0060(16) -0.0223(18) C24 0.053(2) 0.0299(19) 0.0295(18) -0.0005(14) 0.0026(16) -0.0058(16) C25 0.0357(19) 0.0317(18) 0.0278(17) 0.0032(14) 0.0027(14) -0.0017(14) C26 0.0296(18) 0.0272(17) 0.0240(16) 0.0078(13) 0.0037(13) -0.0021(14) C27 0.0320(19) 0.0273(17) 0.0322(17) 0.0065(14) 0.0040(14) -0.0013(14) C28 0.040(2) 0.054(2) 0.0280(18) 0.0134(16) 0.0108(16) 0.0214(17) C29 0.054(2) 0.0325(18) 0.0346(19) 0.0073(15) 0.0170(18) 0.0120(17) C30 0.0375(18) 0.0307(19) 0.0260(16) 0.0026(14) 0.0069(14) 0.0038(15) C31 0.0316(18) 0.0267(17) 0.0195(15) 0.0007(12) 0.0077(13) 0.0038(14) C32 0.0340(19) 0.0325(18) 0.0302(17) 0.0004(14) 0.0060(15) 0.0046(15) C33 0.0288(18) 0.047(2) 0.0305(18) 0.0037(15) 0.0039(14) 0.0032(16) O100 0.0549(15) 0.0339(13) 0.0313(12) -0.0043(10) -0.0017(11) -0.0044(11) C100 0.053(2) 0.053(2) 0.038(2) -0.0026(16) -0.0020(17) 0.0140(18) _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 Ga1 O2 1.9228(18) . ? Ga1 O1 1.9400(19) . ? Ga1 N1 2.073(2) . ? Ga1 N2 2.079(2) . ? Ga1 N4 2.086(2) . ? Ga1 N3 2.149(2) . ? Cl1 C7 1.749(3) . ? O1 C8 1.370(3) . ? O2 C9 1.349(3) . ? N1 C1 1.487(3) . ? N1 H1C 0.9003 . ? N1 H1D 0.9001 . ? N2 C3 1.491(3) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 C5 1.509(4) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 C6 1.486(3) . ? N4 C4 1.496(3) . ? N4 C2 1.501(3) . ? C3 C4 1.514(4) . ? C3 H1A 0.9700 . ? C3 H1B 0.9700 . ? C4 H2A 0.9700 . ? C4 H2B 0.9700 . ? C1 C2 1.531(4) . ? C1 H3A 0.9700 . ? C1 H3B 0.9700 . ? C2 H4A 0.9700 . ? C2 H4B 0.9700 . ? C5 C6 1.491(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.389(4) 3_684 ? C7 C8 1.394(4) . ? C8 C9 1.405(4) . ? C9 C7 1.389(4) 3_684 ? B1 C26 1.641(4) . ? B1 C12 1.644(4) . ? B1 C19 1.646(4) . ? B1 C31 1.655(4) . ? C10 C15 1.377(5) . ? C10 C11 1.387(4) . ? C10 H10A 0.9300 . ? C11 C12 1.402(4) . ? C11 H11A 0.9300 . ? C12 C13 1.403(4) . ? C13 C14 1.388(4) . ? C13 H13A 0.9300 . ? C14 C15 1.383(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.369(4) . ? C16 C21 1.376(4) . ? C16 H16A 0.9300 . ? C17 C18 1.388(4) . ? C17 H17A 0.9300 . ? C18 C19 1.404(4) . ? C18 H18A 0.9300 . ? C19 C20 1.387(4) . ? C20 C21 1.399(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.379(4) . ? C22 C27 1.389(4) . ? C22 H22A 0.9300 . ? C23 C24 1.382(4) . ? C23 H23A 0.9300 . ? C24 C25 1.399(4) . ? C24 H24A 0.9300 . ? C25 C26 1.403(4) . ? C25 H25A 0.9300 . ? C26 C27 1.413(4) . ? C27 H27A 0.9300 . ? C28 C29 1.369(4) . ? C28 C33 1.378(4) . ? C28 H28A 0.9300 . ? C29 C30 1.404(4) . ? C29 H29A 0.9300 . ? C30 C31 1.397(4) . ? C30 H30A 0.9300 . ? C31 C32 1.399(4) . ? C32 C33 1.383(4) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? O100 C100 1.447(3) . ? O100 H100 0.8500 . ? C100 H10D 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? 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 O2 Ga1 O1 87.05(7) . . ? O2 Ga1 N1 177.89(9) . . ? O1 Ga1 N1 92.16(8) . . ? O2 Ga1 N2 87.06(8) . . ? O1 Ga1 N2 100.31(9) . . ? N1 Ga1 N2 95.00(9) . . ? O2 Ga1 N4 96.81(8) . . ? O1 Ga1 N4 174.35(8) . . ? N1 Ga1 N4 83.83(9) . . ? N2 Ga1 N4 84.04(9) . . ? O2 Ga1 N3 86.31(9) . . ? O1 Ga1 N3 94.77(9) . . ? N1 Ga1 N3 91.81(9) . . ? N2 Ga1 N3 163.18(9) . . ? N4 Ga1 N3 81.42(9) . . ? C8 O1 Ga1 108.57(15) . . ? C9 O2 Ga1 109.21(15) . . ? C1 N1 Ga1 108.93(16) . . ? C1 N1 H1C 106.8 . . ? Ga1 N1 H1C 108.9 . . ? C1 N1 H1D 107.0 . . ? Ga1 N1 H1D 120.5 . . ? H1C N1 H1D 103.8 . . ? C3 N2 Ga1 109.58(16) . . ? C3 N2 H2C 103.9 . . ? Ga1 N2 H2C 107.0 . . ? C3 N2 H2D 101.0 . . ? Ga1 N2 H2D 122.4 . . ? H2C N2 H2D 111.3 . . ? C5 N3 Ga1 109.72(17) . . ? C5 N3 H3C 106.3 . . ? Ga1 N3 H3C 103.9 . . ? C5 N3 H3D 106.0 . . ? Ga1 N3 H3D 113.4 . . ? H3C N3 H3D 117.2 . . ? C6 N4 C4 111.9(2) . . ? C6 N4 C2 112.9(2) . . ? C4 N4 C2 110.8(2) . . ? C6 N4 Ga1 105.67(17) . . ? C4 N4 Ga1 105.23(16) . . ? C2 N4 Ga1 109.97(16) . . ? N2 C3 C4 108.8(2) . . ? N2 C3 H1A 109.9 . . ? C4 C3 H1A 109.9 . . ? N2 C3 H1B 109.9 . . ? C4 C3 H1B 109.9 . . ? H1A C3 H1B 108.3 . . ? N4 C4 C3 109.5(2) . . ? N4 C4 H2A 109.8 . . ? C3 C4 H2A 109.8 . . ? N4 C4 H2B 109.8 . . ? C3 C4 H2B 109.8 . . ? H2A C4 H2B 108.2 . . ? N1 C1 C2 109.4(2) . . ? N1 C1 H3A 109.8 . . ? C2 C1 H3A 109.8 . . ? N1 C1 H3B 109.8 . . ? C2 C1 H3B 109.8 . . ? H3A C1 H3B 108.2 . . ? N4 C2 C1 112.5(2) . . ? N4 C2 H4A 109.1 . . ? C1 C2 H4A 109.1 . . ? N4 C2 H4B 109.1 . . ? C1 C2 H4B 109.1 . . ? H4A C2 H4B 107.8 . . ? C6 C5 N3 109.6(3) . . ? C6 C5 H5A 109.8 . . ? N3 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? N3 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? N4 C6 C5 110.0(2) . . ? N4 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N4 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C9 C7 C8 121.8(2) 3_684 . ? C9 C7 Cl1 119.0(2) 3_684 . ? C8 C7 Cl1 119.2(2) . . ? O1 C8 C7 123.3(2) . . ? O1 C8 C9 116.8(2) . . ? C7 C8 C9 119.9(2) . . ? O2 C9 C7 123.5(2) . 3_684 ? O2 C9 C8 118.2(2) . . ? C7 C9 C8 118.4(2) 3_684 . ? C26 B1 C12 105.8(2) . . ? C26 B1 C19 112.1(2) . . ? C12 B1 C19 111.4(2) . . ? C26 B1 C31 112.9(2) . . ? C12 B1 C31 111.5(2) . . ? C19 B1 C31 103.4(2) . . ? C15 C10 C11 120.5(3) . . ? C15 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 122.7(3) . . ? C10 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C13 C12 C11 114.8(3) . . ? C13 C12 B1 121.0(3) . . ? C11 C12 B1 124.1(3) . . ? C14 C13 C12 123.1(3) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C10 C15 C14 119.0(3) . . ? C10 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C17 C16 C21 119.2(3) . . ? C17 C16 H16A 120.4 . . ? C21 C16 H16A 120.4 . . ? C16 C17 C18 119.8(3) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C19 123.2(3) . . ? C17 C18 H18A 118.4 . . ? C19 C18 H18A 118.4 . . ? C20 C19 C18 115.0(3) . . ? C20 C19 B1 125.6(2) . . ? C18 C19 B1 119.0(3) . . ? C19 C20 C21 122.3(3) . . ? C19 C20 H20A 118.9 . . ? C21 C20 H20A 118.9 . . ? C16 C21 C20 120.4(3) . . ? C16 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C23 C22 C27 120.8(3) . . ? C23 C22 H22A 119.6 . . ? C27 C22 H22A 119.6 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 122.9(3) . . ? C24 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C25 C26 C27 114.8(3) . . ? C25 C26 B1 121.1(2) . . ? C27 C26 B1 123.9(3) . . ? C22 C27 C26 122.5(3) . . ? C22 C27 H27A 118.8 . . ? C26 C27 H27A 118.8 . . ? C29 C28 C33 119.8(3) . . ? C29 C28 H28A 120.1 . . ? C33 C28 H28A 120.1 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C31 C30 C29 122.1(3) . . ? C31 C30 H30A 119.0 . . ? C29 C30 H30A 119.0 . . ? C30 C31 C32 114.9(3) . . ? C30 C31 B1 126.1(3) . . ? C32 C31 B1 118.8(3) . . ? C33 C32 C31 123.8(3) . . ? C33 C32 H32A 118.1 . . ? C31 C32 H32A 118.1 . . ? C28 C33 C32 119.2(3) . . ? C28 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C100 O100 H100 100.8 . . ? O100 C100 H10D 109.5 . . ? O100 C100 H10B 109.5 . . ? H10D C100 H10B 109.5 . . ? O100 C100 H10C 109.5 . . ? H10D C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.424 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.065 ################################################## ###### END OF CIF FOR COMPLEX 3 ####### ################################################## data_complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H84 B2 Cl2 Cr2 N8 O6' _chemical_formula_weight 1305.95 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6357(13) _cell_length_b 9.6821(9) _cell_length_c 24.999(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.219(3) _cell_angle_gamma 90.00 _cell_volume 3280.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 912 _cell_measurement_theta_min 2.663 _cell_measurement_theta_max 21.186 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark-brown' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.470 _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 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 18115 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.1531 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5626 _reflns_number_gt 3157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0246P)^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 5626 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1598 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.38858(5) 0.66906(7) 0.05199(3) 0.0258(2) Uani 1 1 d . . . Cl1 Cl 0.55620(9) 0.84213(11) -0.10152(4) 0.0366(3) Uani 1 1 d . . . O1 O 0.4601(2) 0.7204(2) -0.00820(10) 0.0267(8) Uani 1 1 d . . . O2 O 0.4077(2) 0.8563(3) 0.07594(10) 0.0270(8) Uani 1 1 d . . . N3 N 0.5069(2) 0.6193(3) 0.10850(12) 0.0269(10) Uani 1 1 d . . . H1A H 0.5468 0.5588 0.0942 0.032 Uiso 1 1 calc R . . H1B H 0.5420 0.6959 0.1180 0.032 Uiso 1 1 calc R . . N1 N 0.3657(3) 0.4672(3) 0.02487(13) 0.0291(10) Uani 1 1 d . . . H2A H 0.3588 0.4654 -0.0113 0.035 Uiso 1 1 calc R . . H2B H 0.4177 0.4142 0.0368 0.035 Uiso 1 1 calc R . . N2 N 0.2498(3) 0.7336(3) 0.01540(14) 0.0363(11) Uani 1 1 d . . . H3A H 0.2526 0.8232 0.0062 0.044 Uiso 1 1 calc R . . H3B H 0.2335 0.6843 -0.0148 0.044 Uiso 1 1 calc R . . N4 N 0.3042(3) 0.6062(3) 0.11223(14) 0.0252(9) Uani 1 1 d . . . C5 C 0.4693(3) 0.5577(4) 0.15664(16) 0.0278(12) Uani 1 1 d . . . H1C H 0.5154 0.5753 0.1883 0.033 Uiso 1 1 calc R . . H1D H 0.4626 0.4585 0.1521 0.033 Uiso 1 1 calc R . . C6 C 0.3704(3) 0.6210(4) 0.16378(16) 0.0288(12) Uani 1 1 d . . . H2C H 0.3414 0.5746 0.1927 0.035 Uiso 1 1 calc R . . H2D H 0.3785 0.7179 0.1731 0.035 Uiso 1 1 calc R . . C1 C 0.2750(3) 0.4137(4) 0.04546(17) 0.0310(12) Uani 1 1 d . . . H3C H 0.2742 0.3136 0.0435 0.037 Uiso 1 1 calc R . . H3D H 0.2173 0.4482 0.0233 0.037 Uiso 1 1 calc R . . C2 C 0.2714(3) 0.4591(4) 0.10336(16) 0.0310(12) Uani 1 1 d . . . H4A H 0.2046 0.4494 0.1127 0.037 Uiso 1 1 calc R . . H4B H 0.3137 0.3993 0.1270 0.037 Uiso 1 1 calc R . . C3 C 0.1729(4) 0.7139(5) 0.0532(2) 0.0549(16) Uani 1 1 d . . . H5A H 0.1273 0.7911 0.0500 0.066 Uiso 1 1 calc R . . H5B H 0.1358 0.6302 0.0439 0.066 Uiso 1 1 calc R . . C4 C 0.2200(4) 0.7040(5) 0.10946(19) 0.0417(14) Uani 1 1 d . . . H6A H 0.1721 0.6722 0.1327 0.050 Uiso 1 1 calc R . . H6B H 0.2432 0.7944 0.1219 0.050 Uiso 1 1 calc R . . C7 C 0.5272(3) 0.9302(4) -0.04415(16) 0.0229(11) Uani 1 1 d . . . C8 C 0.4810(3) 0.8582(4) -0.00525(16) 0.0212(11) Uani 1 1 d . . . C9 C 0.4533(3) 0.9288(4) 0.03978(16) 0.0213(11) Uani 1 1 d . . . B1 B 0.0316(4) 0.9410(5) -0.1614(2) 0.0273(14) Uani 1 1 d . . . C10 C 0.1860(4) 1.2677(5) -0.09920(18) 0.0418(15) Uani 1 1 d . . . H10A H 0.1803 1.3633 -0.0981 0.050 Uiso 1 1 calc R . . C11 C 0.2692(4) 1.2029(5) -0.07365(19) 0.0440(15) Uani 1 1 d . . . H11A H 0.3193 1.2546 -0.0550 0.053 Uiso 1 1 calc R . . C12 C 0.2765(4) 1.0615(5) -0.07629(18) 0.0401(13) Uani 1 1 d . . . H12A H 0.3315 1.0169 -0.0591 0.048 Uiso 1 1 calc R . . C13 C 0.2024(4) 0.9856(5) -0.10429(18) 0.0343(13) Uani 1 1 d . . . H13A H 0.2096 0.8902 -0.1055 0.041 Uiso 1 1 calc R . . C14 C 0.1164(3) 1.0442(5) -0.13120(17) 0.0278(12) Uani 1 1 d . . . C15 C 0.1104(4) 1.1882(5) -0.12674(17) 0.0352(13) Uani 1 1 d . . . H15A H 0.0543 1.2329 -0.1426 0.042 Uiso 1 1 calc R . . C16 C -0.0485(4) 0.7081(6) -0.0184(2) 0.0492(15) Uani 1 1 d . . . H16A H -0.0628 0.6621 0.0125 0.059 Uiso 1 1 calc R . . C17 C -0.0748(4) 0.8437(6) -0.02616(19) 0.0462(14) Uani 1 1 d . . . H17A H -0.1081 0.8900 -0.0010 0.055 Uiso 1 1 calc R . . C18 C -0.0511(3) 0.9108(5) -0.07180(18) 0.0391(14) Uani 1 1 d . . . H18A H -0.0688 1.0031 -0.0763 0.047 Uiso 1 1 calc R . . C19 C -0.0019(3) 0.8475(5) -0.11172(17) 0.0293(11) Uani 1 1 d . . . C20 C 0.0217(3) 0.7094(5) -0.10191(18) 0.0364(13) Uani 1 1 d . . . H20A H 0.0542 0.6618 -0.1271 0.044 Uiso 1 1 calc R . . C21 C -0.0004(4) 0.6395(5) -0.0567(2) 0.0462(14) Uani 1 1 d . . . H21A H 0.0167 0.5470 -0.0520 0.055 Uiso 1 1 calc R . . C22 C 0.1987(4) 0.7936(6) -0.26903(19) 0.0492(16) Uani 1 1 d . . . H22A H 0.2575 0.8169 -0.2824 0.059 Uiso 1 1 calc R . . C23 C 0.1459(5) 0.6808(6) -0.2892(2) 0.0580(18) Uani 1 1 d . . . H23A H 0.1691 0.6268 -0.3160 0.070 Uiso 1 1 calc R . . C24 C 0.0574(4) 0.6483(5) -0.26929(18) 0.0486(15) Uani 1 1 d . . . H24A H 0.0209 0.5723 -0.2827 0.058 Uiso 1 1 calc R . . C25 C 0.0237(4) 0.7300(4) -0.22924(18) 0.0364(13) Uani 1 1 d . . . H25A H -0.0362 0.7077 -0.2168 0.044 Uiso 1 1 calc R . . C26 C 0.0765(3) 0.8451(5) -0.20675(16) 0.0293(12) Uani 1 1 d . . . C27 C 0.1646(4) 0.8726(5) -0.22873(17) 0.0377(13) Uani 1 1 d . . . H27A H 0.2022 0.9479 -0.2156 0.045 Uiso 1 1 calc R . . C28 C -0.2386(4) 1.0614(5) -0.2189(2) 0.0389(13) Uani 1 1 d . . . H28A H -0.3033 1.0357 -0.2154 0.047 Uiso 1 1 calc R . . C29 C -0.2198(4) 1.1672(5) -0.25327(19) 0.0451(14) Uani 1 1 d . . . H29A H -0.2716 1.2139 -0.2727 0.054 Uiso 1 1 calc R . . C30 C -0.1233(4) 1.2032(4) -0.25858(18) 0.0427(14) Uani 1 1 d . . . H30A H -0.1097 1.2745 -0.2816 0.051 Uiso 1 1 calc R . . C31 C -0.0458(4) 1.1321(4) -0.22909(17) 0.0342(13) Uani 1 1 d . . . H31A H 0.0187 1.1564 -0.2337 0.041 Uiso 1 1 calc R . . C32 C -0.0615(4) 1.0255(4) -0.19286(17) 0.0277(12) Uani 1 1 d . . . C33 C -0.1608(4) 0.9929(4) -0.18944(18) 0.0323(13) Uani 1 1 d . . . H33A H -0.1754 0.9222 -0.1664 0.039 Uiso 1 1 calc R . . O100 O 0.3409(2) 0.5890(3) -0.08749(12) 0.0433(9) Uani 1 1 d . . . H100 H 0.3749 0.6429 -0.0660 0.065 Uiso 1 1 d R . . C100 C 0.3078(4) 0.6292(5) -0.14111(18) 0.0547(16) Uani 1 1 d . . . H10D H 0.3091 0.5508 -0.1645 0.066 Uiso 1 1 calc R . . H10B H 0.3503 0.7001 -0.1524 0.066 Uiso 1 1 calc R . . H10C H 0.2416 0.6640 -0.1426 0.066 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 Cr1 0.0340(5) 0.0205(4) 0.0225(4) -0.0006(4) 0.0013(4) -0.0012(4) Cl1 0.0590(9) 0.0242(6) 0.0283(7) -0.0049(6) 0.0123(6) 0.0002(6) O1 0.042(2) 0.0116(16) 0.0269(18) -0.0007(13) 0.0060(16) -0.0045(14) O2 0.042(2) 0.0184(16) 0.0214(17) -0.0010(14) 0.0048(16) -0.0062(15) N3 0.028(2) 0.027(2) 0.025(2) -0.0039(17) 0.002(2) -0.0038(17) N1 0.036(3) 0.029(2) 0.023(2) -0.0030(17) 0.006(2) -0.0008(19) N2 0.043(3) 0.037(2) 0.027(2) -0.0050(18) -0.009(2) -0.002(2) N4 0.030(3) 0.020(2) 0.026(2) -0.0048(17) 0.005(2) 0.0007(18) C5 0.034(3) 0.034(3) 0.015(3) 0.002(2) -0.001(2) -0.008(2) C6 0.039(3) 0.028(3) 0.020(3) -0.004(2) 0.007(3) -0.008(2) C1 0.039(3) 0.020(3) 0.033(3) -0.004(2) 0.003(3) -0.006(2) C2 0.036(3) 0.025(3) 0.032(3) -0.001(2) 0.003(3) -0.005(2) C3 0.041(4) 0.066(4) 0.056(4) -0.008(3) -0.003(3) 0.020(3) C4 0.041(4) 0.045(3) 0.039(3) -0.005(3) 0.005(3) 0.010(3) C7 0.024(3) 0.024(3) 0.020(3) -0.001(2) -0.001(2) 0.004(2) C8 0.027(3) 0.017(3) 0.018(3) 0.000(2) -0.003(2) -0.002(2) C9 0.024(3) 0.022(2) 0.018(3) -0.001(2) -0.002(2) 0.001(2) B1 0.035(4) 0.028(3) 0.019(3) -0.001(3) 0.002(3) -0.002(3) C10 0.061(4) 0.037(3) 0.030(3) -0.011(3) 0.019(3) -0.015(3) C11 0.040(4) 0.062(4) 0.031(3) -0.015(3) 0.008(3) -0.018(3) C12 0.038(4) 0.047(3) 0.034(3) -0.004(3) -0.002(3) -0.002(3) C13 0.040(4) 0.031(3) 0.032(3) 0.000(2) 0.003(3) -0.004(3) C14 0.036(3) 0.032(3) 0.016(3) 0.001(2) 0.004(2) -0.001(2) C15 0.040(3) 0.039(3) 0.027(3) -0.003(2) 0.006(3) -0.003(3) C16 0.040(4) 0.068(4) 0.039(3) 0.020(3) 0.002(3) -0.010(3) C17 0.046(4) 0.060(4) 0.033(3) -0.002(3) 0.008(3) -0.008(3) C18 0.052(4) 0.031(3) 0.034(3) 0.000(2) 0.008(3) -0.003(3) C19 0.028(3) 0.031(3) 0.027(3) -0.005(2) -0.002(2) -0.007(2) C20 0.037(3) 0.038(3) 0.035(3) 0.003(3) 0.007(3) -0.004(2) C21 0.053(4) 0.035(3) 0.050(4) 0.017(3) 0.003(3) -0.003(3) C22 0.057(4) 0.065(4) 0.027(3) 0.003(3) 0.013(3) 0.026(3) C23 0.084(5) 0.062(4) 0.028(3) -0.005(3) 0.008(3) 0.046(4) C24 0.074(5) 0.035(3) 0.034(3) -0.014(3) -0.011(3) 0.019(3) C25 0.043(4) 0.029(3) 0.036(3) -0.002(2) 0.000(3) 0.003(3) C26 0.034(3) 0.032(3) 0.021(3) 0.010(2) -0.003(2) 0.009(3) C27 0.040(4) 0.044(3) 0.029(3) 0.005(2) 0.001(3) 0.005(3) C28 0.036(4) 0.036(3) 0.043(4) -0.018(3) 0.001(3) 0.002(3) C29 0.046(4) 0.050(4) 0.036(3) -0.014(3) -0.006(3) 0.022(3) C30 0.068(5) 0.032(3) 0.028(3) -0.002(2) 0.004(3) 0.009(3) C31 0.038(3) 0.033(3) 0.031(3) -0.004(2) 0.000(3) 0.006(3) C32 0.036(4) 0.021(3) 0.024(3) -0.009(2) -0.002(3) 0.003(2) C33 0.042(4) 0.026(3) 0.029(3) -0.009(2) 0.004(3) 0.003(3) O100 0.058(3) 0.042(2) 0.027(2) -0.0042(16) -0.0099(19) 0.0012(17) C100 0.060(4) 0.061(4) 0.040(4) -0.010(3) -0.008(3) 0.013(3) _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 O2 1.918(3) . ? Cr1 O1 1.944(3) . ? Cr1 N1 2.081(3) . ? Cr1 N3 2.082(3) . ? Cr1 N4 2.083(3) . ? Cr1 N2 2.105(4) . ? Cl1 C7 1.750(4) . ? O1 C8 1.364(4) . ? O2 C9 1.348(4) . ? N3 C5 1.483(4) . ? N3 H1A 0.9000 . ? N3 H1B 0.9000 . ? N1 C1 1.484(4) . ? N1 H2A 0.9000 . ? N1 H2B 0.9000 . ? N2 C3 1.499(5) . ? N2 H3A 0.9000 . ? N2 H3B 0.9000 . ? N4 C4 1.485(5) . ? N4 C6 1.498(5) . ? N4 C2 1.502(5) . ? C5 C6 1.510(5) . ? C5 H1C 0.9700 . ? C5 H1D 0.9700 . ? C6 H2C 0.9700 . ? C6 H2D 0.9700 . ? C1 C2 1.518(5) . ? C1 H3C 0.9700 . ? C1 H3D 0.9700 . ? C2 H4A 0.9700 . ? C2 H4B 0.9700 . ? C3 C4 1.484(6) . ? C3 H5A 0.9700 . ? C3 H5B 0.9700 . ? C4 H6A 0.9700 . ? C4 H6B 0.9700 . ? C7 C9 1.393(5) 3_675 ? C7 C8 1.401(5) . ? C8 C9 1.403(5) . ? C9 C7 1.393(5) 3_675 ? B1 C26 1.636(6) . ? B1 C32 1.638(7) . ? B1 C19 1.641(6) . ? B1 C14 1.647(7) . ? C10 C11 1.390(6) . ? C10 C15 1.404(6) . ? C10 H10A 0.9300 . ? C11 C12 1.375(6) . ? C11 H11A 0.9300 . ? C12 C13 1.377(6) . ? C12 H12A 0.9300 . ? C13 C14 1.406(6) . ? C13 H13A 0.9300 . ? C14 C15 1.403(5) . ? C15 H15A 0.9300 . ? C16 C17 1.370(6) . ? C16 C21 1.387(6) . ? C16 H16A 0.9300 . ? C17 C18 1.381(6) . ? C17 H17A 0.9300 . ? C18 C19 1.402(5) . ? C18 H18A 0.9300 . ? C19 C20 1.392(5) . ? C20 C21 1.378(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.373(7) . ? C22 C27 1.385(6) . ? C22 H22A 0.9300 . ? C23 C24 1.391(6) . ? C23 H23A 0.9300 . ? C24 C25 1.392(6) . ? C24 H24A 0.9300 . ? C25 C26 1.410(6) . ? C25 H25A 0.9300 . ? C26 C27 1.399(5) . ? C27 H27A 0.9300 . ? C28 C29 1.379(6) . ? C28 C33 1.392(6) . ? C28 H28A 0.9300 . ? C29 C30 1.382(6) . ? C29 H29A 0.9300 . ? C30 C31 1.402(6) . ? C30 H30A 0.9300 . ? C31 C32 1.404(5) . ? C31 H31A 0.9300 . ? C32 C33 1.401(6) . ? C33 H33A 0.9300 . ? O100 C100 1.422(5) . ? O100 H100 0.8500 . ? C100 H10D 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? 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 O2 Cr1 O1 86.39(11) . . ? O2 Cr1 N1 178.88(14) . . ? O1 Cr1 N1 93.34(11) . . ? O2 Cr1 N3 86.43(12) . . ? O1 Cr1 N3 99.65(12) . . ? N1 Cr1 N3 94.69(13) . . ? O2 Cr1 N4 96.77(12) . . ? O1 Cr1 N4 175.58(13) . . ? N1 Cr1 N4 83.44(12) . . ? N3 Cr1 N4 83.68(14) . . ? O2 Cr1 N2 86.61(12) . . ? O1 Cr1 N2 95.19(13) . . ? N1 Cr1 N2 92.34(14) . . ? N3 Cr1 N2 163.17(13) . . ? N4 Cr1 N2 81.95(14) . . ? C8 O1 Cr1 109.1(2) . . ? C9 O2 Cr1 109.9(2) . . ? C5 N3 Cr1 109.5(2) . . ? C5 N3 H1A 109.8 . . ? Cr1 N3 H1A 109.8 . . ? C5 N3 H1B 109.8 . . ? Cr1 N3 H1B 109.8 . . ? H1A N3 H1B 108.2 . . ? C1 N1 Cr1 108.5(2) . . ? C1 N1 H2A 110.0 . . ? Cr1 N1 H2A 110.0 . . ? C1 N1 H2B 110.0 . . ? Cr1 N1 H2B 110.0 . . ? H2A N1 H2B 108.4 . . ? C3 N2 Cr1 110.2(3) . . ? C3 N2 H3A 109.6 . . ? Cr1 N2 H3A 109.6 . . ? C3 N2 H3B 109.6 . . ? Cr1 N2 H3B 109.6 . . ? H3A N2 H3B 108.1 . . ? C4 N4 C6 111.7(3) . . ? C4 N4 C2 112.5(4) . . ? C6 N4 C2 111.1(3) . . ? C4 N4 Cr1 105.4(3) . . ? C6 N4 Cr1 105.4(2) . . ? C2 N4 Cr1 110.5(2) . . ? N3 C5 C6 108.9(3) . . ? N3 C5 H1C 109.9 . . ? C6 C5 H1C 109.9 . . ? N3 C5 H1D 109.9 . . ? C6 C5 H1D 109.9 . . ? H1C C5 H1D 108.3 . . ? N4 C6 C5 108.8(3) . . ? N4 C6 H2C 109.9 . . ? C5 C6 H2C 109.9 . . ? N4 C6 H2D 109.9 . . ? C5 C6 H2D 109.9 . . ? H2C C6 H2D 108.3 . . ? N1 C1 C2 110.1(4) . . ? N1 C1 H3C 109.6 . . ? C2 C1 H3C 109.6 . . ? N1 C1 H3D 109.6 . . ? C2 C1 H3D 109.6 . . ? H3C C1 H3D 108.2 . . ? N4 C2 C1 112.1(3) . . ? N4 C2 H4A 109.2 . . ? C1 C2 H4A 109.2 . . ? N4 C2 H4B 109.2 . . ? C1 C2 H4B 109.2 . . ? H4A C2 H4B 107.9 . . ? C4 C3 N2 110.2(4) . . ? C4 C3 H5A 109.6 . . ? N2 C3 H5A 109.6 . . ? C4 C3 H5B 109.6 . . ? N2 C3 H5B 109.6 . . ? H5A C3 H5B 108.1 . . ? C3 C4 N4 109.8(4) . . ? C3 C4 H6A 109.7 . . ? N4 C4 H6A 109.7 . . ? C3 C4 H6B 109.7 . . ? N4 C4 H6B 109.7 . . ? H6A C4 H6B 108.2 . . ? C9 C7 C8 122.0(4) 3_675 . ? C9 C7 Cl1 118.9(3) 3_675 . ? C8 C7 Cl1 119.0(3) . . ? O1 C8 C7 123.8(4) . . ? O1 C8 C9 116.5(3) . . ? C7 C8 C9 119.7(4) . . ? O2 C9 C7 123.7(4) . 3_675 ? O2 C9 C8 117.9(4) . . ? C7 C9 C8 118.3(4) 3_675 . ? C26 B1 C32 106.2(4) . . ? C26 B1 C19 111.5(4) . . ? C32 B1 C19 111.9(4) . . ? C26 B1 C14 111.4(4) . . ? C32 B1 C14 112.7(4) . . ? C19 B1 C14 103.1(4) . . ? C11 C10 C15 119.8(5) . . ? C11 C10 H10A 120.1 . . ? C15 C10 H10A 120.1 . . ? C12 C11 C10 119.1(5) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 120.2(5) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C14 123.8(5) . . ? C12 C13 H13A 118.1 . . ? C14 C13 H13A 118.1 . . ? C15 C14 C13 114.5(4) . . ? C15 C14 B1 126.5(4) . . ? C13 C14 B1 118.8(4) . . ? C14 C15 C10 122.6(5) . . ? C14 C15 H15A 118.7 . . ? C10 C15 H15A 118.7 . . ? C17 C16 C21 119.8(4) . . ? C17 C16 H16A 120.1 . . ? C21 C16 H16A 120.1 . . ? C16 C17 C18 119.2(5) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C17 C18 C19 123.7(5) . . ? C17 C18 H18A 118.1 . . ? C19 C18 H18A 118.1 . . ? C20 C19 C18 114.5(4) . . ? C20 C19 B1 125.8(4) . . ? C18 C19 B1 119.4(4) . . ? C21 C20 C19 123.3(4) . . ? C21 C20 H20A 118.4 . . ? C19 C20 H20A 118.4 . . ? C20 C21 C16 119.6(5) . . ? C20 C21 H21A 120.2 . . ? C16 C21 H21A 120.2 . . ? C23 C22 C27 120.2(5) . . ? C23 C22 H22A 119.9 . . ? C27 C22 H22A 119.9 . . ? C22 C23 C24 119.3(5) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C23 C24 C25 119.7(5) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 122.8(5) . . ? C24 C25 H25A 118.6 . . ? C26 C25 H25A 118.6 . . ? C27 C26 C25 114.6(4) . . ? C27 C26 B1 124.5(4) . . ? C25 C26 B1 120.8(4) . . ? C22 C27 C26 123.4(5) . . ? C22 C27 H27A 118.3 . . ? C26 C27 H27A 118.3 . . ? C29 C28 C33 120.1(5) . . ? C29 C28 H28A 120.0 . . ? C33 C28 H28A 120.0 . . ? C28 C29 C30 119.4(5) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C29 C30 C31 119.8(5) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C30 C31 C32 122.8(5) . . ? C30 C31 H31A 118.6 . . ? C32 C31 H31A 118.6 . . ? C33 C32 C31 114.9(4) . . ? C33 C32 B1 124.2(4) . . ? C31 C32 B1 120.8(4) . . ? C28 C33 C32 123.1(4) . . ? C28 C33 H33A 118.4 . . ? C32 C33 H33A 118.4 . . ? C100 O100 H100 121.6 . . ? O100 C100 H10D 109.5 . . ? O100 C100 H10B 109.5 . . ? H10D C100 H10B 109.5 . . ? O100 C100 H10C 109.5 . . ? H10D C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.344 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.059 ################################################## ###### END OF CIF FOR COMPLEX 5 ####### ##################################################