# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a10077a _database_code_depnum_ccdc_archive 'CCDC 903290' #TrackingRef '16361_web_deposit_cif_file_0_Yi-ChouTsai_1356074359.compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "C42 H54 Cr N6 O2', 1.3(C5 H12)" _chemical_formula_sum 'C48.50 H69.60 Cr N6 O2' _chemical_formula_weight 820.70 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 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.6712(12) _cell_length_b 11.3892(11) _cell_length_c 16.3973(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.700(5) _cell_angle_gamma 90.00 _cell_volume 2288.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 885 _exptl_absorpt_coefficient_mu 0.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8965 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 14996 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3962 _reflns_number_gt 2228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1534P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3962 _refine_ls_number_parameters 229 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2553 _refine_ls_wR_factor_gt 0.2343 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.2638(3) 0.7372(4) 0.1059(3) 0.0595(12) Uani 1 1 d . A . C2 C 0.2366(4) 0.8485(4) 0.0697(3) 0.0743(13) Uani 1 1 d . . . C3 C 0.3170(14) 0.9582(16) 0.0830(10) 0.088(5) Uiso 0.45 1 d P A 1 H3A H 0.2759 1.0330 0.0746 0.105 Uiso 0.45 1 calc PR A 1 H3B H 0.3674 0.9577 0.1400 0.105 Uiso 0.45 1 calc PR A 1 C4 C 0.3796(9) 0.9408(10) 0.0146(7) 0.118(3) Uiso 0.62 1 d P A 1 H4A H 0.4338 1.0034 0.0190 0.177 Uiso 0.62 1 calc PR A 1 H4B H 0.3283 0.9435 -0.0412 0.177 Uiso 0.62 1 calc PR A 1 H4C H 0.4166 0.8645 0.0226 0.177 Uiso 0.62 1 calc PR A 1 C3' C 0.3249(12) 0.9297(13) 0.0668(9) 0.090(5) Uiso 0.55 1 d P A 2 H3'1 H 0.3899 0.8828 0.0646 0.109 Uiso 0.55 1 calc PR A 2 H3'2 H 0.3436 0.9746 0.1203 0.109 Uiso 0.55 1 calc PR A 2 C4' C 0.3035(15) 1.0161(15) -0.0051(10) 0.114(5) Uiso 0.38 1 d P A 2 H4'1 H 0.3637 1.0726 0.0038 0.170 Uiso 0.38 1 calc PR A 2 H4'2 H 0.2352 1.0580 -0.0076 0.170 Uiso 0.38 1 calc PR A 2 H4'3 H 0.2976 0.9740 -0.0582 0.170 Uiso 0.38 1 calc PR A 2 C5 C 0.1319(5) 0.8724(5) 0.0308(4) 0.0962(17) Uani 1 1 d . A . H5 H 0.1133 0.9479 0.0067 0.115 Uiso 1 1 calc R . . C6 C 0.0516(5) 0.7903(7) 0.0251(4) 0.112(2) Uani 1 1 d . . . H6 H -0.0214 0.8089 -0.0035 0.135 Uiso 1 1 calc R A . C7 C 0.0760(4) 0.6802(6) 0.0607(3) 0.0932(17) Uani 1 1 d . A . H7 H 0.0195 0.6242 0.0575 0.112 Uiso 1 1 calc R . . C8 C 0.1828(4) 0.6519(5) 0.1011(3) 0.0739(13) Uani 1 1 d . . . C9 C 0.2100(4) 0.5300(5) 0.1374(3) 0.0917(17) Uani 1 1 d . A . H9A H 0.2405 0.4839 0.0975 0.110 Uiso 1 1 calc R . . H9B H 0.2678 0.5371 0.1906 0.110 Uiso 1 1 calc R . . C10 C 0.1172(6) 0.4626(7) 0.1550(6) 0.176(4) Uani 1 1 d . . . H10A H 0.1433 0.3860 0.1791 0.265 Uiso 1 1 calc R A . H10B H 0.0607 0.4512 0.1024 0.265 Uiso 1 1 calc R . . H10C H 0.0867 0.5064 0.1952 0.265 Uiso 1 1 calc R . . C11 C 0.4323(3) 0.6323(3) 0.1190(2) 0.0552(10) Uani 1 1 d . A . H11 H 0.4044 0.5873 0.0694 0.066 Uiso 1 1 calc R . . C12 C 0.6072(4) 0.5408(4) 0.1456(2) 0.0641(12) Uani 1 1 d . A . C13 C 0.5804(4) 0.4229(5) 0.1333(3) 0.0764(14) Uani 1 1 d D . . C14 C 0.4708(11) 0.378(2) 0.1295(17) 0.126(11) Uiso 0.50 1 d PD B 3 H14A H 0.4197 0.4073 0.0773 0.151 Uiso 0.50 1 calc PR B 3 H14B H 0.4465 0.4095 0.1780 0.151 Uiso 0.50 1 calc PR B 3 C15 C 0.4646(13) 0.2451(12) 0.1307(10) 0.137(5) Uiso 0.53 1 d P B 3 H15A H 0.3928 0.2210 0.1368 0.206 Uiso 0.53 1 calc PR B 3 H15B H 0.5214 0.2147 0.1783 0.206 Uiso 0.53 1 calc PR B 3 H15C H 0.4758 0.2136 0.0779 0.206 Uiso 0.53 1 calc PR B 3 C14' C 0.4796(9) 0.3693(14) 0.1447(12) 0.068(5) Uiso 0.50 1 d PD B 4 H14C H 0.4427 0.4285 0.1721 0.082 Uiso 0.50 1 calc PR B 4 H14D H 0.5009 0.3036 0.1851 0.082 Uiso 0.50 1 calc PR B 4 C15' C 0.3953(12) 0.3222(14) 0.0682(9) 0.127(5) Uiso 0.47 1 d P B 4 H15D H 0.3312 0.2943 0.0856 0.191 Uiso 0.47 1 calc PR B 4 H15E H 0.4270 0.2571 0.0433 0.191 Uiso 0.47 1 calc PR B 4 H15F H 0.3735 0.3850 0.0264 0.191 Uiso 0.47 1 calc PR B 4 C16 C 0.6594(6) 0.3480(6) 0.1137(3) 0.1025(19) Uani 1 1 d . B . H16 H 0.6430 0.2669 0.1052 0.123 Uiso 1 1 calc R . . C17 C 0.7560(7) 0.3870(8) 0.1068(3) 0.111(2) Uani 1 1 d . . . H17 H 0.8069 0.3346 0.0926 0.134 Uiso 1 1 calc R B . C18 C 0.7808(5) 0.5028(8) 0.1204(4) 0.115(2) Uani 1 1 d . B . H18 H 0.8500 0.5294 0.1154 0.138 Uiso 1 1 calc R . . C19 C 0.7101(4) 0.5846(6) 0.1412(3) 0.0882(16) Uani 1 1 d . . . C20 C 0.7367(6) 0.7139(7) 0.1539(6) 0.133(3) Uani 1 1 d . B . H20A H 0.6723 0.7586 0.1223 0.159 Uiso 1 1 calc R . . H20B H 0.7461 0.7317 0.2145 0.159 Uiso 1 1 calc R . . C21 C 0.8282(10) 0.7577(11) 0.1306(12) 0.307(10) Uani 1 1 d . . . H21A H 0.8374 0.8412 0.1453 0.461 Uiso 1 1 calc R B . H21B H 0.8179 0.7483 0.0697 0.461 Uiso 1 1 calc R . . H21C H 0.8933 0.7143 0.1606 0.461 Uiso 1 1 calc R . . N1 N 0.5598(3) 0.8649(3) 0.2075(2) 0.0637(10) Uani 1 1 d . . . N2 N 0.3745(3) 0.7115(3) 0.1478(2) 0.0564(9) Uani 1 1 d . . . N3 N 0.5322(3) 0.6225(3) 0.1660(2) 0.0554(9) Uani 1 1 d . . . O1 O 0.5976(3) 0.9507(3) 0.1878(2) 0.0983(12) Uani 1 1 d . . . Cr Cr 0.5000 0.75220(7) 0.2500 0.0515(4) Uani 1 2 d S . . 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 C1 0.050(3) 0.079(3) 0.047(2) -0.002(2) 0.0068(19) 0.009(2) C2 0.063(3) 0.091(4) 0.061(3) 0.010(2) 0.001(2) 0.011(3) C5 0.082(4) 0.100(4) 0.097(4) 0.015(3) 0.004(3) 0.018(3) C6 0.069(4) 0.165(6) 0.092(4) 0.011(4) -0.002(3) 0.029(4) C7 0.056(3) 0.128(5) 0.088(4) 0.000(4) 0.005(3) 0.000(3) C8 0.059(3) 0.097(4) 0.059(3) 0.004(2) 0.004(2) 0.001(3) C9 0.067(3) 0.108(4) 0.089(4) 0.012(3) -0.002(3) -0.018(3) C10 0.120(6) 0.178(8) 0.195(8) 0.059(6) -0.028(5) -0.084(5) C11 0.058(3) 0.058(3) 0.047(2) 0.0021(19) 0.009(2) 0.004(2) C12 0.068(3) 0.081(3) 0.042(2) -0.002(2) 0.012(2) 0.015(2) C13 0.089(4) 0.086(4) 0.048(3) -0.011(2) 0.005(2) 0.027(3) C16 0.106(5) 0.108(5) 0.081(4) -0.026(3) 0.002(4) 0.041(4) C17 0.119(6) 0.152(7) 0.060(3) -0.005(4) 0.016(4) 0.072(5) C18 0.087(4) 0.168(7) 0.102(5) 0.022(5) 0.044(4) 0.047(5) C19 0.070(4) 0.116(5) 0.087(4) 0.008(3) 0.036(3) 0.020(3) C20 0.092(5) 0.130(6) 0.202(8) -0.014(5) 0.084(5) -0.012(4) C21 0.219(13) 0.234(14) 0.55(3) -0.033(13) 0.241(19) -0.052(9) N1 0.060(2) 0.072(3) 0.060(2) -0.0011(18) 0.0153(18) -0.0057(19) N2 0.048(2) 0.070(2) 0.049(2) -0.0003(16) 0.0083(16) 0.0034(17) N3 0.050(2) 0.066(2) 0.051(2) -0.0021(16) 0.0148(17) 0.0063(17) O1 0.107(3) 0.078(3) 0.115(3) 0.016(2) 0.036(2) -0.025(2) Cr 0.0486(6) 0.0576(7) 0.0475(6) 0.000 0.0107(4) 0.000 _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 C1 C8 1.402(6) . ? C1 C2 1.405(6) . ? C1 N2 1.427(5) . ? C2 C5 1.347(7) . ? C2 C3' 1.462(14) . ? C2 C3 1.592(17) . ? C3 C4 1.541(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3' C4' 1.51(2) . ? C3' H3'1 0.9900 . ? C3' H3'2 0.9900 . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C4' H4'3 0.9800 . ? C5 C6 1.367(8) . ? C5 H5 0.9500 . ? C6 C7 1.384(8) . ? C6 H6 0.9500 . ? C7 C8 1.386(7) . ? C7 H7 0.9500 . ? C8 C9 1.516(7) . ? C9 C10 1.493(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.309(5) . ? C11 N2 1.323(5) . ? C11 Cr 2.506(4) . ? C11 H11 0.9500 . ? C12 C13 1.387(7) . ? C12 C19 1.414(7) . ? C12 N3 1.430(5) . ? C13 C16 1.411(7) . ? C13 C14 1.467(8) . ? C13 C14' 1.471(7) . ? C14 C15 1.52(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14' C15' 1.52(2) . ? C14' H14C 0.9900 . ? C14' H14D 0.9900 . ? C15' H15D 0.9800 . ? C15' H15E 0.9800 . ? C15' H15F 0.9800 . ? C16 C17 1.334(8) . ? C16 H16 0.9500 . ? C17 C18 1.361(9) . ? C17 H17 0.9500 . ? C18 C19 1.394(8) . ? C18 H18 0.9500 . ? C19 C20 1.513(8) . ? C20 C21 1.402(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N1 O1 1.169(4) . ? N1 Cr 1.725(4) . ? N2 Cr 2.049(3) . ? N3 Cr 2.128(3) . ? Cr N1 1.725(4) 2_655 ? Cr N2 2.049(3) 2_655 ? Cr N3 2.128(3) 2_655 ? Cr C11 2.506(4) 2_655 ? 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 C8 C1 C2 120.3(4) . . ? C8 C1 N2 120.1(4) . . ? C2 C1 N2 119.7(4) . . ? C5 C2 C1 119.3(5) . . ? C5 C2 C3' 121.8(7) . . ? C1 C2 C3' 118.4(7) . . ? C5 C2 C3 115.2(8) . . ? C1 C2 C3 124.8(8) . . ? C3' C2 C3 16.1(9) . . ? C4 C3 C2 103.3(11) . . ? C4 C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? C4 C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C3' C4' 116.8(12) . . ? C2 C3' H3'1 108.1 . . ? C4' C3' H3'1 108.1 . . ? C2 C3' H3'2 108.1 . . ? C4' C3' H3'2 108.1 . . ? H3'1 C3' H3'2 107.3 . . ? C3' C4' H4'1 109.5 . . ? C3' C4' H4'2 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? C3' C4' H4'3 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? C2 C5 C6 121.4(6) . . ? C2 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 119.9(5) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C1 118.6(5) . . ? C7 C8 C9 119.9(5) . . ? C1 C8 C9 121.5(4) . . ? C10 C9 C8 115.8(5) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 N2 112.8(4) . . ? N3 C11 Cr 58.1(2) . . ? N2 C11 Cr 54.7(2) . . ? N3 C11 H11 123.6 . . ? N2 C11 H11 123.6 . . ? Cr C11 H11 178.2 . . ? C13 C12 C19 121.9(5) . . ? C13 C12 N3 120.8(4) . . ? C19 C12 N3 117.3(4) . . ? C12 C13 C16 117.1(5) . . ? C12 C13 C14 122.5(10) . . ? C16 C13 C14 119.9(11) . . ? C12 C13 C14' 124.9(7) . . ? C16 C13 C14' 117.8(8) . . ? C14 C13 C14' 10.4(16) . . ? C13 C14 C15 113.5(16) . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C14' C15' 119.4(12) . . ? C13 C14' H14C 107.5 . . ? C15' C14' H14C 107.5 . . ? C13 C14' H14D 107.5 . . ? C15' C14' H14D 107.5 . . ? H14C C14' H14D 107.0 . . ? C14' C15' H15D 109.5 . . ? C14' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C14' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C17 C16 C13 122.5(6) . . ? C17 C16 H16 118.8 . . ? C13 C16 H16 118.8 . . ? C16 C17 C18 119.1(6) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C19 123.4(7) . . ? C17 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? C18 C19 C12 115.8(6) . . ? C18 C19 C20 123.3(6) . . ? C12 C19 C20 120.8(5) . . ? C21 C20 C19 118.7(7) . . ? C21 C20 H20A 107.6 . . ? C19 C20 H20A 107.6 . . ? C21 C20 H20B 107.6 . . ? C19 C20 H20B 107.6 . . ? H20A C20 H20B 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 N1 Cr 170.5(3) . . ? C11 N2 C1 122.2(3) . . ? C11 N2 Cr 93.5(2) . . ? C1 N2 Cr 144.2(3) . . ? C11 N3 C12 121.2(3) . . ? C11 N3 Cr 90.4(2) . . ? C12 N3 Cr 148.4(3) . . ? N1 Cr N1 83.8(2) . 2_655 ? N1 Cr N2 99.65(15) . . ? N1 Cr N2 99.75(15) 2_655 . ? N1 Cr N2 99.75(15) . 2_655 ? N1 Cr N2 99.65(15) 2_655 2_655 ? N2 Cr N2 153.8(2) . 2_655 ? N1 Cr N3 94.55(15) . . ? N1 Cr N3 162.51(15) 2_655 . ? N2 Cr N3 63.27(13) . . ? N2 Cr N3 97.80(13) 2_655 . ? N1 Cr N3 162.51(15) . 2_655 ? N1 Cr N3 94.55(15) 2_655 2_655 ? N2 Cr N3 97.80(13) . 2_655 ? N2 Cr N3 63.27(13) 2_655 2_655 ? N3 Cr N3 92.10(18) . 2_655 ? N1 Cr C11 98.58(14) . . ? N1 Cr C11 131.44(15) 2_655 . ? N2 Cr C11 31.79(12) . . ? N2 Cr C11 127.12(14) 2_655 . ? N3 Cr C11 31.49(11) . . ? N3 Cr C11 95.54(13) 2_655 . ? N1 Cr C11 131.44(15) . 2_655 ? N1 Cr C11 98.58(14) 2_655 2_655 ? N2 Cr C11 127.12(14) . 2_655 ? N2 Cr C11 31.79(12) 2_655 2_655 ? N3 Cr C11 95.54(13) . 2_655 ? N3 Cr C11 31.49(11) 2_655 2_655 ? C11 Cr C11 113.97(18) . 2_655 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.463 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.090 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.085 0.250 217.8 54.1 2 0.000 -0.085 0.750 217.9 55.5 _platon_squeeze_details ; The unit cell volume comprises a large region of disordered solvent which could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 109.6 electrons per unit cell, which were assigned to be 2.6 n-pentane molecules per unit cell. ; data_10661 _database_code_depnum_ccdc_archive 'CCDC 903291' #TrackingRef '16362_web_deposit_cif_file_1_Yi-ChouTsai_1356074359.compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "C42 H54 Cr2 N10 O8', 0.7(C7 H8)" _chemical_formula_sum 'C46.9 H59.60 Cr2 N10 O8' _chemical_formula_weight 996.55 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 19.5267(5) _cell_length_b 17.9584(5) _cell_length_c 14.7203(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.6360(10) _cell_angle_gamma 90.00 _cell_volume 5116.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 26312 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour green(dark) _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2094 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8232 _exptl_absorpt_correction_T_max 0.9639 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22628 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.07 _reflns_number_total 4532 _reflns_number_gt 3156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1424P)^2^+13.8497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4532 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2620 _refine_ls_wR_factor_gt 0.2428 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0727(3) 0.1843(3) 0.0327(4) 0.0427(12) Uani 1 1 d . . . C2 C 0.0162(3) 0.2169(4) -0.0217(4) 0.0523(14) Uani 1 1 d . . . C3 C 0.0235(4) 0.2921(5) -0.0659(6) 0.084(2) Uani 1 1 d . . . H3A H 0.0321 0.3297 -0.0164 0.100 Uiso 1 1 calc R . . H3B H 0.0651 0.2906 -0.0976 0.100 Uiso 1 1 calc R . . C4 C -0.0327(7) 0.3175(6) -0.1296(11) 0.170(7) Uani 1 1 d . . . H4A H -0.0225 0.3674 -0.1509 0.255 Uiso 1 1 calc R . . H4B H -0.0747 0.3191 -0.0999 0.255 Uiso 1 1 calc R . . H4C H -0.0396 0.2833 -0.1820 0.255 Uiso 1 1 calc R . . C5 C -0.0465(3) 0.1785(4) -0.0315(5) 0.071(2) Uani 1 1 d . . . H5 H -0.0850 0.1983 -0.0700 0.085 Uiso 1 1 calc R . . C6 C -0.0535(4) 0.1121(5) 0.0135(5) 0.076(2) Uani 1 1 d . . . H6 H -0.0968 0.0872 0.0062 0.092 Uiso 1 1 calc R . . C7 C 0.0010(3) 0.0822(4) 0.0683(5) 0.0621(17) Uani 1 1 d . . . H7 H -0.0050 0.0367 0.0992 0.074 Uiso 1 1 calc R . . C8 C 0.0657(3) 0.1169(3) 0.0802(4) 0.0481(13) Uani 1 1 d . . . C9 C 0.1247(3) 0.0844(4) 0.1426(5) 0.0712(19) Uani 1 1 d . . . H9A H 0.1515 0.0527 0.1051 0.085 Uiso 1 1 calc R . . H9B H 0.1553 0.1260 0.1664 0.085 Uiso 1 1 calc R . . C10 C 0.1100(5) 0.0408(7) 0.2201(7) 0.138(5) Uani 1 1 d . . . H10A H 0.1534 0.0237 0.2549 0.208 Uiso 1 1 calc R . . H10B H 0.0817 -0.0023 0.1984 0.208 Uiso 1 1 calc R . . H10C H 0.0848 0.0715 0.2597 0.208 Uiso 1 1 calc R . . C11 C 0.1529(3) 0.2687(3) 0.1048(4) 0.0413(12) Uani 1 1 d . . . H11 H 0.1174 0.2767 0.1421 0.050 Uiso 1 1 calc R . . C12 C 0.2119(3) 0.3577(4) 0.2039(4) 0.0552(16) Uani 1 1 d . . . C13 C 0.2384(4) 0.3320(5) 0.2894(4) 0.075(2) Uani 1 1 d . . . C14 C 0.2595(4) 0.2489(7) 0.3068(5) 0.103(3) Uani 1 1 d . . . H14A H 0.2565 0.2231 0.2469 0.123 Uiso 1 1 calc R . . H14B H 0.3083 0.2471 0.3353 0.123 Uiso 1 1 calc R . . C15 C 0.2180(10) 0.2083(8) 0.3645(11) 0.194(5) Uani 1 1 d . . . H15A H 0.2350 0.1570 0.3721 0.291 Uiso 1 1 calc R . . H15B H 0.1698 0.2078 0.3360 0.291 Uiso 1 1 calc R . . H15C H 0.2213 0.2324 0.4246 0.291 Uiso 1 1 calc R . . C16 C 0.2423(5) 0.3840(8) 0.3635(6) 0.109(4) Uani 1 1 d . . . H16 H 0.2584 0.3678 0.4240 0.131 Uiso 1 1 calc R . . C17 C 0.2236(6) 0.4554(8) 0.3489(9) 0.124(5) Uani 1 1 d . . . H17 H 0.2291 0.4897 0.3985 0.148 Uiso 1 1 calc R . . C18 C 0.1969(5) 0.4790(5) 0.2639(8) 0.098(3) Uani 1 1 d . . . H18 H 0.1823 0.5294 0.2557 0.118 Uiso 1 1 calc R . . C19 C 0.1901(4) 0.4317(4) 0.1884(5) 0.072(2) Uani 1 1 d . B . C20 C 0.1582(4) 0.4559(4) 0.0978(7) 0.089(2) Uani 1 1 d . . . H20A H 0.1840 0.4330 0.0514 0.107 Uiso 1 1 calc R A 1 H20B H 0.1105 0.4360 0.0874 0.107 Uiso 1 1 calc R A 1 C21 C 0.1552(9) 0.5322(8) 0.0825(10) 0.194(5) Uani 1 1 d . B 1 H21A H 0.1332 0.5420 0.0198 0.291 Uiso 1 1 calc R B 1 H21B H 0.2022 0.5528 0.0906 0.291 Uiso 1 1 calc R B 1 H21C H 0.1283 0.5557 0.1262 0.291 Uiso 1 1 calc R B 1 O4 O 0.1563(4) 0.3431(4) -0.1704(5) 0.1268(4) Uani 1 1 d . . . Cr1 Cr 0.20426(4) 0.19178(5) -0.05598(5) 0.0384(3) Uani 1 1 d . . . N1 N 0.1424(3) 0.1894(3) -0.1522(3) 0.0543(12) Uani 1 1 d . . . N2 N 0.1913(2) 0.0959(3) -0.0531(3) 0.0485(12) Uani 1 1 d . . . N3 N 0.2001(2) 0.3549(3) -0.1027(4) 0.0543(12) Uani 1 1 d . . . N4 N 0.1395(2) 0.2201(2) 0.0388(3) 0.0393(10) Uani 1 1 d . . . N5 N 0.2101(2) 0.3081(2) 0.1258(3) 0.0439(11) Uani 1 1 d . . . O1 O 0.1013(3) 0.1764(3) -0.2160(4) 0.0886(16) Uani 1 1 d . . . O2 O 0.1760(3) 0.0332(3) -0.0606(3) 0.0753(13) Uani 1 1 d . . . O3 O 0.22264(19) 0.3019(2) -0.0532(2) 0.0462(9) 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 C1 0.033(3) 0.055(3) 0.041(3) -0.006(3) 0.009(2) -0.008(2) C2 0.037(3) 0.063(4) 0.058(4) 0.005(3) 0.006(3) -0.002(3) C3 0.054(4) 0.092(6) 0.102(6) 0.017(5) 0.004(4) 0.013(4) C4 0.128(10) 0.118(9) 0.246(17) 0.084(10) -0.039(11) 0.007(7) C5 0.042(3) 0.084(5) 0.086(5) -0.003(4) 0.001(3) -0.011(3) C6 0.052(4) 0.091(6) 0.087(5) -0.012(4) 0.014(4) -0.028(4) C7 0.057(4) 0.055(4) 0.078(5) -0.004(3) 0.025(3) -0.013(3) C8 0.048(3) 0.054(3) 0.045(3) -0.002(3) 0.015(2) -0.007(3) C9 0.055(4) 0.085(5) 0.075(5) 0.027(4) 0.016(3) -0.003(3) C10 0.104(7) 0.215(13) 0.100(7) 0.083(8) 0.030(6) 0.017(8) C11 0.036(3) 0.051(3) 0.039(3) 0.003(2) 0.011(2) -0.001(2) C12 0.045(3) 0.077(5) 0.046(3) -0.022(3) 0.018(3) -0.021(3) C13 0.074(4) 0.114(6) 0.041(4) -0.013(4) 0.021(3) -0.036(4) C14 0.078(5) 0.179(11) 0.051(4) 0.025(5) 0.011(4) -0.008(6) C15 0.292(15) 0.128(8) 0.182(10) 0.028(7) 0.109(11) 0.003(8) C16 0.095(6) 0.188(11) 0.050(5) -0.045(6) 0.025(4) -0.066(7) C17 0.131(9) 0.145(10) 0.107(9) -0.079(8) 0.062(7) -0.075(8) C18 0.097(6) 0.090(6) 0.119(8) -0.053(6) 0.053(6) -0.036(5) C19 0.074(4) 0.064(4) 0.084(5) -0.031(4) 0.039(4) -0.020(4) C20 0.092(6) 0.059(5) 0.120(7) -0.020(5) 0.029(5) 0.011(4) C21 0.292(15) 0.128(8) 0.182(10) 0.028(7) 0.109(11) 0.003(8) O4 0.131 0.120 0.124 0.007(4) -0.004(5) 0.000(5) Cr1 0.0361(5) 0.0456(5) 0.0343(5) -0.0026(4) 0.0080(3) -0.0059(4) N1 0.047(3) 0.067(3) 0.049(3) -0.004(2) 0.004(2) -0.008(2) N2 0.050(3) 0.050(3) 0.047(3) -0.009(2) 0.013(2) -0.008(2) N3 0.047(3) 0.062(3) 0.051(3) 0.002(3) -0.002(2) -0.003(2) N4 0.035(2) 0.046(2) 0.038(2) -0.004(2) 0.0096(18) -0.0085(19) N5 0.042(2) 0.053(3) 0.038(2) -0.007(2) 0.0128(19) -0.008(2) O1 0.081(3) 0.113(4) 0.065(3) -0.003(3) -0.017(3) -0.007(3) O2 0.094(3) 0.055(3) 0.079(3) -0.012(2) 0.018(3) -0.023(3) O3 0.044(2) 0.053(2) 0.043(2) 0.0038(18) 0.0116(17) -0.0003(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 C1 C2 1.403(8) . ? C1 C8 1.414(8) . ? C1 N4 1.446(6) . ? C2 C5 1.395(8) . ? C2 C3 1.514(10) . ? C3 C4 1.420(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.379(10) . ? C5 H5 0.9500 . ? C6 C7 1.357(10) . ? C6 H6 0.9500 . ? C7 C8 1.399(8) . ? C7 H7 0.9500 . ? C8 C9 1.494(8) . ? C9 C10 1.444(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N4 1.307(7) . ? C11 N5 1.323(6) . ? C11 H11 0.9500 . ? C12 C13 1.376(10) . ? C12 C19 1.404(10) . ? C12 N5 1.451(7) . ? C13 C16 1.431(12) . ? C13 C14 1.561(13) . ? C14 C15 1.446(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.342(16) . ? C16 H16 0.9500 . ? C17 C18 1.359(16) . ? C17 H17 0.9500 . ? C18 C19 1.392(10) . ? C18 H18 0.9500 . ? C19 C20 1.461(11) . ? C20 C21 1.389(14) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O4 N3 1.242(8) . ? Cr1 N1 1.736(5) . ? Cr1 N2 1.742(5) . ? Cr1 O3 2.006(4) 7 ? Cr1 O3 2.010(4) . ? Cr1 N4 2.067(4) . ? Cr1 N5 2.077(4) 7 ? N1 O1 1.174(6) . ? N2 O2 1.166(6) . ? N3 O3 1.242(6) . ? N5 Cr1 2.077(4) 7 ? O3 Cr1 2.006(4) 7 ? 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 C2 C1 C8 121.3(5) . . ? C2 C1 N4 119.0(5) . . ? C8 C1 N4 119.7(5) . . ? C5 C2 C1 117.7(6) . . ? C5 C2 C3 121.9(6) . . ? C1 C2 C3 120.4(5) . . ? C4 C3 C2 117.4(7) . . ? C4 C3 H3A 107.9 . . ? C2 C3 H3A 107.9 . . ? C4 C3 H3B 107.9 . . ? C2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C2 121.3(6) . . ? C6 C5 H5 119.3 . . ? C2 C5 H5 119.3 . . ? C7 C6 C5 120.5(6) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 121.4(6) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C1 117.7(5) . . ? C7 C8 C9 120.9(6) . . ? C1 C8 C9 121.4(5) . . ? C10 C9 C8 118.6(6) . . ? C10 C9 H9A 107.7 . . ? C8 C9 H9A 107.7 . . ? C10 C9 H9B 107.7 . . ? C8 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N5 127.7(5) . . ? N4 C11 H11 116.2 . . ? N5 C11 H11 116.2 . . ? C13 C12 C19 122.4(6) . . ? C13 C12 N5 119.0(6) . . ? C19 C12 N5 118.5(6) . . ? C12 C13 C16 117.0(9) . . ? C12 C13 C14 122.0(6) . . ? C16 C13 C14 120.9(8) . . ? C15 C14 C13 115.0(9) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C13 121.0(10) . . ? C17 C16 H16 119.5 . . ? C13 C16 H16 119.5 . . ? C16 C17 C18 120.6(9) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 121.9(10) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C12 117.0(8) . . ? C18 C19 C20 122.1(8) . . ? C12 C19 C20 120.8(6) . . ? C21 C20 C19 116.4(10) . . ? C21 C20 H20A 108.2 . . ? C19 C20 H20A 108.2 . . ? C21 C20 H20B 108.2 . . ? C19 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 Cr1 N2 84.8(2) . . ? N1 Cr1 O3 177.7(2) . 7 ? N2 Cr1 O3 97.23(19) . 7 ? N1 Cr1 O3 98.3(2) . . ? N2 Cr1 O3 176.97(19) . . ? O3 Cr1 O3 79.75(17) 7 . ? N1 Cr1 N4 97.7(2) . . ? N2 Cr1 N4 97.04(19) . . ? O3 Cr1 N4 83.10(15) 7 . ? O3 Cr1 N4 82.42(16) . . ? N1 Cr1 N5 96.6(2) . 7 ? N2 Cr1 N5 98.16(19) . 7 ? O3 Cr1 N5 82.07(16) 7 7 ? O3 Cr1 N5 81.71(16) . 7 ? N4 Cr1 N5 159.94(17) . 7 ? O1 N1 Cr1 169.9(5) . . ? O2 N2 Cr1 171.1(5) . . ? O4 N3 O3 119.5(6) . . ? C11 N4 C1 115.6(4) . . ? C11 N4 Cr1 125.8(3) . . ? C1 N4 Cr1 118.5(3) . . ? C11 N5 C12 116.5(4) . . ? C11 N5 Cr1 126.5(4) . 7 ? C12 N5 Cr1 117.0(3) . 7 ? N3 O3 Cr1 125.9(3) . 7 ? N3 O3 Cr1 133.8(3) . . ? Cr1 O3 Cr1 100.25(17) 7 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.983 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.182 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 -0.003 415.5 67.7 2 0.000 0.500 -0.003 415.5 67.7 _platon_squeeze_details ; The unit cell volume comprises a large region of disordered solvent which could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 135.4 electrons per unit cell, which were assigned to be 2.8 toluene molecules per unit cell. ; data_ic14319 _database_code_depnum_ccdc_archive 'CCDC 903292' #TrackingRef '16363_web_deposit_cif_file_2_Yi-ChouTsai_1356074359.compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "C50 H70 Cr2 N8 O5', (C4 H8 O)" _chemical_formula_sum 'C54 H78 Cr2 N8 O6' _chemical_formula_weight 1039.24 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 24.1046(14) _cell_length_b 10.2903(6) _cell_length_c 22.6641(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.516(1) _cell_angle_gamma 90.00 _cell_volume 5361.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5800 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8370 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15876 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4727 _reflns_number_gt 4307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0646P)^2^+32.5856P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4727 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.015 _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 0.19679(2) 0.71269(6) 0.47051(3) 0.0230(2) Uani 1 1 d . . . N1 N 0.27420(14) 0.6332(3) 0.49130(14) 0.0257(7) Uani 1 1 d . . . O1 O 0.2907(3) 0.5277(5) 0.4810(3) 0.0448(14) Uiso 0.65 1 d P A 1 O1' O 0.2656(5) 0.5303(10) 0.4712(5) 0.044(3) Uiso 0.35 1 d P B 2 N2 N 0.11605(17) 0.7267(5) 0.43823(18) 0.0637(13) Uani 0.50 1 d P C 1 O2 O 0.0700(3) 0.7159(7) 0.4160(3) 0.0498(16) Uiso 0.50 1 d P C 1 N3 N 0.1086(5) 0.6010(11) 0.4144(5) 0.068(3) Uiso 0.50 1 d P C 2 O3 O 0.11605(17) 0.7267(5) 0.43823(18) 0.0637(13) Uani 0.50 1 d P C 2 O4 O 0.1544(3) 0.5632(8) 0.4257(3) 0.0587(19) Uiso 0.50 1 d P C 2 N4 N 0.19330(12) 0.6487(3) 0.55379(13) 0.0212(6) Uani 1 1 d . C . N5 N 0.28801(13) 0.7191(3) 0.60682(13) 0.0213(6) Uani 1 1 d . . . C1 C 0.23774(15) 0.6648(3) 0.60450(15) 0.0198(7) Uani 1 1 d . . . H1 H 0.2331 0.6349 0.6424 0.024 Uiso 1 1 calc R C . C2 C 0.14105(16) 0.5923(4) 0.56242(16) 0.0269(8) Uani 1 1 d . . . C3 C 0.13164(19) 0.4587(5) 0.55499(18) 0.0364(10) Uani 1 1 d . C . C4 C 0.0794(2) 0.4099(6) 0.5612(2) 0.0528(14) Uani 1 1 d . . . H4 H 0.0718 0.3193 0.5564 0.063 Uiso 1 1 calc R C . C5 C 0.0391(2) 0.4893(7) 0.5741(2) 0.0592(17) Uani 1 1 d . C . H5 H 0.0040 0.4536 0.5781 0.071 Uiso 1 1 calc R . . C6 C 0.0491(2) 0.6203(7) 0.5811(2) 0.0539(14) Uani 1 1 d . . . H6 H 0.0206 0.6745 0.5899 0.065 Uiso 1 1 calc R C . C7 C 0.09989(18) 0.6754(5) 0.57577(19) 0.0372(10) Uani 1 1 d . C . C8 C 0.1747(2) 0.3670(5) 0.5411(2) 0.0508(13) Uani 1 1 d . . . H8 H 0.2095 0.4107 0.5350 0.061 Uiso 0.50 1 calc PR C 1 H8' H 0.2081 0.4255 0.5423 0.061 Uiso 0.50 1 d PR C 2 C9 C 0.1887(8) 0.2637(19) 0.5892(9) 0.064(5) Uiso 0.50 1 d P C 1 H9A H 0.2114 0.3011 0.6290 0.077 Uiso 0.50 1 calc PR C 1 H9B H 0.2115 0.1953 0.5773 0.077 Uiso 0.50 1 calc PR C 1 H9C H 0.1526 0.2266 0.5932 0.077 Uiso 0.50 1 calc PR C 1 C10 C 0.1390(6) 0.2801(13) 0.4839(6) 0.063(3) Uiso 0.50 1 d P C 1 H10A H 0.1201 0.3366 0.4488 0.075 Uiso 0.50 1 calc PR C 1 H10B H 0.1094 0.2299 0.4956 0.075 Uiso 0.50 1 calc PR C 1 H10C H 0.1656 0.2206 0.4722 0.075 Uiso 0.50 1 calc PR C 1 C9' C 0.2031(8) 0.2659(18) 0.5959(8) 0.059(5) Uiso 0.50 1 d P C 2 H9'A H 0.2259 0.3135 0.6327 0.071 Uiso 0.50 1 calc PR C 2 H9'B H 0.2285 0.2057 0.5827 0.071 Uiso 0.50 1 calc PR C 2 H9'C H 0.1722 0.2169 0.6058 0.071 Uiso 0.50 1 calc PR C 2 C10' C 0.1612(7) 0.3090(15) 0.4792(7) 0.081(4) Uiso 0.50 1 d P C 2 H10D H 0.1895 0.3394 0.4590 0.097 Uiso 0.50 1 calc PR C 2 H10E H 0.1220 0.3347 0.4545 0.097 Uiso 0.50 1 calc PR C 2 H10F H 0.1633 0.2141 0.4829 0.097 Uiso 0.50 1 calc PR C 2 C11 C 0.1092(2) 0.8218(5) 0.5855(2) 0.0498(13) Uani 1 1 d . . . H11 H 0.1510 0.8385 0.5891 0.060 Uiso 0.50 1 calc PR C 1 H11' H 0.1460 0.8499 0.5775 0.060 Uiso 0.50 1 d PR C 2 C12 C 0.0747(7) 0.9110(17) 0.5370(8) 0.076(5) Uiso 0.50 1 d P C 1 H12A H 0.0781 0.8844 0.4967 0.092 Uiso 0.50 1 calc PR C 1 H12B H 0.0894 0.9998 0.5462 0.092 Uiso 0.50 1 calc PR C 1 H12C H 0.0338 0.9077 0.5359 0.092 Uiso 0.50 1 calc PR C 1 C13 C 0.0996(8) 0.8755(19) 0.6428(9) 0.085(6) Uiso 0.50 1 d P C 1 H13A H 0.0759 0.9543 0.6326 0.102 Uiso 0.50 1 calc PR C 1 H13B H 0.1373 0.8966 0.6729 0.102 Uiso 0.50 1 calc PR C 1 H13C H 0.0795 0.8108 0.6607 0.102 Uiso 0.50 1 calc PR C 1 C12' C 0.0564(7) 0.8889(17) 0.5410(8) 0.078(5) Uiso 0.50 1 d P C 2 H12D H 0.0562 0.8733 0.4983 0.094 Uiso 0.50 1 calc PR C 2 H12E H 0.0585 0.9825 0.5492 0.094 Uiso 0.50 1 calc PR C 2 H12F H 0.0207 0.8537 0.5470 0.094 Uiso 0.50 1 calc PR C 2 C13' C 0.1119(7) 0.8480(16) 0.6550(8) 0.066(4) Uiso 0.50 1 d P C 2 H13D H 0.1464 0.8057 0.6826 0.079 Uiso 0.50 1 calc PR C 2 H13E H 0.0769 0.8128 0.6626 0.079 Uiso 0.50 1 calc PR C 2 H13F H 0.1141 0.9418 0.6629 0.079 Uiso 0.50 1 calc PR C 2 C14 C 0.33087(15) 0.7231(4) 0.66794(16) 0.0228(8) Uani 1 1 d . . . C15 C 0.37368(16) 0.6256(4) 0.68390(16) 0.0243(8) Uani 1 1 d . C . C16 C 0.41378(17) 0.6292(4) 0.74268(18) 0.0327(9) Uani 1 1 d . . . H16 H 0.4429 0.5638 0.7544 0.039 Uiso 1 1 calc R C . C17 C 0.41205(19) 0.7258(5) 0.78426(19) 0.0382(10) Uani 1 1 d . C . H17 H 0.4398 0.7269 0.8242 0.046 Uiso 1 1 calc R . . C18 C 0.36983(19) 0.8209(4) 0.76767(18) 0.0357(10) Uani 1 1 d . . . H18 H 0.3688 0.8866 0.7968 0.043 Uiso 1 1 calc R C . C19 C 0.32866(17) 0.8230(4) 0.70930(17) 0.0280(8) Uani 1 1 d . C . C20 C 0.37535(17) 0.5129(4) 0.64101(18) 0.0285(8) Uani 1 1 d . . . H20 H 0.3511 0.5371 0.5983 0.034 Uiso 1 1 calc R C . C21 C 0.3483(2) 0.3934(5) 0.6607(2) 0.0508(13) Uani 1 1 d . C . H21A H 0.3723 0.3657 0.7018 0.061 Uiso 1 1 calc R . . H21B H 0.3463 0.3230 0.6309 0.061 Uiso 1 1 calc R . . H21C H 0.3090 0.4144 0.6619 0.061 Uiso 1 1 calc R . . C22 C 0.43648(19) 0.4831(5) 0.6388(2) 0.0443(11) Uani 1 1 d . C . H22A H 0.4536 0.5616 0.6270 0.053 Uiso 1 1 calc R . . H22B H 0.4348 0.4145 0.6082 0.053 Uiso 1 1 calc R . . H22C H 0.4605 0.4538 0.6796 0.053 Uiso 1 1 calc R . . C23 C 0.2847(2) 0.9330(4) 0.6936(2) 0.0390(10) Uani 1 1 d . . . H23 H 0.2614 0.9270 0.6490 0.047 Uiso 0.50 1 calc PR C 1 H23' H 0.2543 0.9118 0.6539 0.047 Uiso 0.50 1 d PR C 2 C24 C 0.2424(5) 0.9164(13) 0.7357(6) 0.054(3) Uiso 0.50 1 d P C 1 H24A H 0.2280 0.8269 0.7326 0.065 Uiso 0.50 1 calc PR C 1 H24B H 0.2095 0.9763 0.7213 0.065 Uiso 0.50 1 calc PR C 1 H24C H 0.2639 0.9360 0.7789 0.065 Uiso 0.50 1 calc PR C 1 C25 C 0.3126(7) 1.0656(17) 0.7063(8) 0.077(5) Uiso 0.50 1 d P C 1 H25A H 0.3387 1.0780 0.6809 0.092 Uiso 0.50 1 calc PR C 1 H25B H 0.3349 1.0723 0.7501 0.092 Uiso 0.50 1 calc PR C 1 H25C H 0.2823 1.1326 0.6961 0.092 Uiso 0.50 1 calc PR C 1 C24' C 0.2563(5) 0.9574(13) 0.7409(6) 0.052(3) Uiso 0.50 1 d P C 2 H24D H 0.2731 1.0351 0.7645 0.063 Uiso 0.50 1 calc PR C 2 H24E H 0.2621 0.8826 0.7689 0.063 Uiso 0.50 1 calc PR C 2 H24F H 0.2146 0.9708 0.7211 0.063 Uiso 0.50 1 calc PR C 2 C25' C 0.3155(6) 1.0592(13) 0.6846(7) 0.056(3) Uiso 0.50 1 d P C 2 H25D H 0.3386 1.0429 0.6564 0.067 Uiso 0.50 1 calc PR C 2 H25E H 0.3412 1.0887 0.7246 0.067 Uiso 0.50 1 calc PR C 2 H25F H 0.2864 1.1263 0.6671 0.067 Uiso 0.50 1 calc PR C 2 O5 O 0.0130(7) 0.2915(12) 0.2405(8) 0.129(5) Uiso 0.50 1 d P . -1 C30 C -0.0143(4) 0.5044(7) 0.2160(3) 0.088(2) Uani 1 1 d . . . H30A H -0.0498 0.5590 0.2054 0.105 Uiso 1 1 calc R . . H30B H 0.0124 0.5384 0.1941 0.105 Uiso 1 1 calc R . . C31 C -0.0292(4) 0.3700(8) 0.1991(4) 0.092(2) Uani 1 1 d . . . H31A H -0.0684 0.3498 0.2022 0.110 Uiso 1 1 calc R . . H31B H -0.0292 0.3539 0.1561 0.110 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 0.0233(3) 0.0297(4) 0.0169(3) 0.0048(2) 0.0075(2) -0.0011(3) N1 0.0376(18) 0.0228(17) 0.0224(16) 0.0052(13) 0.0177(14) 0.0065(14) N2 0.044(2) 0.105(4) 0.043(2) 0.033(2) 0.0134(18) 0.000(2) O3 0.044(2) 0.105(4) 0.043(2) 0.033(2) 0.0134(18) 0.000(2) N4 0.0201(15) 0.0281(16) 0.0171(14) 0.0010(13) 0.0081(12) -0.0024(13) N5 0.0216(15) 0.0260(16) 0.0151(14) 0.0010(12) 0.0040(12) -0.0016(13) C1 0.0249(18) 0.0204(17) 0.0154(16) 0.0016(14) 0.0080(14) 0.0030(15) C2 0.0222(19) 0.042(2) 0.0151(17) 0.0048(16) 0.0043(14) -0.0090(17) C3 0.040(2) 0.046(3) 0.021(2) 0.0019(18) 0.0061(17) -0.018(2) C4 0.055(3) 0.069(4) 0.030(2) 0.006(2) 0.006(2) -0.036(3) C5 0.033(3) 0.107(5) 0.036(3) 0.017(3) 0.008(2) -0.027(3) C6 0.028(2) 0.096(5) 0.041(3) 0.012(3) 0.015(2) -0.001(3) C7 0.026(2) 0.058(3) 0.030(2) 0.005(2) 0.0115(17) 0.001(2) C8 0.071(3) 0.037(3) 0.049(3) -0.009(2) 0.025(3) -0.018(2) C11 0.043(3) 0.051(3) 0.063(3) 0.000(2) 0.028(2) 0.012(2) C14 0.0225(18) 0.0277(19) 0.0176(17) 0.0042(15) 0.0050(14) -0.0043(15) C15 0.0247(19) 0.029(2) 0.0192(18) 0.0018(15) 0.0072(15) -0.0033(16) C16 0.028(2) 0.038(2) 0.027(2) 0.0045(18) 0.0007(17) 0.0037(18) C17 0.037(2) 0.048(3) 0.0207(19) -0.0026(19) -0.0046(17) -0.002(2) C18 0.044(2) 0.037(2) 0.024(2) -0.0068(18) 0.0071(18) -0.0020(19) C19 0.031(2) 0.030(2) 0.0238(19) 0.0005(16) 0.0104(16) -0.0021(17) C20 0.029(2) 0.031(2) 0.0246(19) -0.0004(16) 0.0058(16) 0.0011(17) C21 0.068(3) 0.040(3) 0.053(3) -0.013(2) 0.032(3) -0.014(2) C22 0.039(2) 0.050(3) 0.044(3) -0.005(2) 0.013(2) 0.007(2) C23 0.046(3) 0.034(2) 0.033(2) -0.0056(19) 0.0040(19) 0.007(2) C30 0.111(6) 0.087(5) 0.074(4) 0.001(4) 0.041(4) -0.003(4) C31 0.093(5) 0.092(6) 0.088(5) -0.017(4) 0.022(4) -0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr N1 1.841(3) 7_566 ? Cr N2 1.867(4) . ? Cr O4 1.954(8) . ? Cr N1 1.961(3) . ? Cr N5 2.021(3) 7_566 ? Cr N4 2.025(3) . ? Cr Cr 2.6252(12) 7_566 ? N1 O1' 1.147(11) . ? N1 O1 1.202(6) . ? N1 Cr 1.841(3) 7_566 ? N2 O2 1.079(8) . ? N3 O4 1.125(11) . ? N4 C1 1.325(4) . ? N4 C2 1.452(4) . ? N5 C1 1.321(5) . ? N5 C14 1.458(4) . ? N5 Cr 2.021(3) 7_566 ? C2 C3 1.395(6) . ? C2 C7 1.410(6) . ? C3 C4 1.402(6) . ? C3 C8 1.504(7) . ? C4 C5 1.366(8) . ? C5 C6 1.370(9) . ? C6 C7 1.389(6) . ? C7 C11 1.529(7) . ? C8 C10' 1.468(16) . ? C8 C9 1.487(19) . ? C8 C10 1.596(14) . ? C8 C9' 1.606(18) . ? C11 C12 1.481(17) . ? C11 C13 1.49(2) . ? C11 C12' 1.530(17) . ? C11 C13' 1.580(17) . ? C14 C19 1.403(5) . ? C14 C15 1.406(5) . ? C15 C16 1.391(5) . ? C15 C20 1.522(5) . ? C16 C17 1.379(6) . ? C17 C18 1.380(6) . ? C18 C19 1.395(6) . ? C19 C23 1.518(6) . ? C20 C21 1.519(6) . ? C20 C22 1.521(6) . ? C23 C24' 1.457(13) . ? C23 C25 1.509(17) . ? C23 C25' 1.539(14) . ? C23 C24 1.601(13) . ? O5 C31 1.411(17) . ? O5 C31 1.535(18) 2 ? C30 C31 1.451(10) . ? C30 C30 1.485(14) 2 ? C31 O5 1.535(18) 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 N1 Cr N2 108.75(19) 7_566 . ? N1 Cr O4 171.1(3) 7_566 . ? N2 Cr O4 62.4(3) . . ? N1 Cr N1 92.71(13) 7_566 . ? N2 Cr N1 158.53(19) . . ? O4 Cr N1 96.2(3) . . ? N1 Cr N5 88.06(13) 7_566 7_566 ? N2 Cr N5 94.19(14) . 7_566 ? O4 Cr N5 91.5(2) . 7_566 ? N1 Cr N5 86.88(12) . 7_566 ? N1 Cr N4 87.62(13) 7_566 . ? N2 Cr N4 93.41(14) . . ? O4 Cr N4 93.8(2) . . ? N1 Cr N4 86.78(12) . . ? N5 Cr N4 172.15(12) 7_566 . ? N1 Cr Cr 48.24(10) 7_566 7_566 ? N2 Cr Cr 156.99(17) . 7_566 ? O4 Cr Cr 140.6(2) . 7_566 ? N1 Cr Cr 44.47(10) . 7_566 ? N5 Cr Cr 86.31(9) 7_566 7_566 ? N4 Cr Cr 85.93(9) . 7_566 ? O1' N1 O1 28.4(5) . . ? O1' N1 Cr 168.5(7) . 7_566 ? O1 N1 Cr 140.2(4) . 7_566 ? O1' N1 Cr 104.2(6) . . ? O1 N1 Cr 132.5(4) . . ? Cr N1 Cr 87.29(13) 7_566 . ? O2 N2 Cr 168.7(6) . . ? N3 O4 Cr 99.8(8) . . ? C1 N4 C2 116.2(3) . . ? C1 N4 Cr 121.2(2) . . ? C2 N4 Cr 122.4(2) . . ? C1 N5 C14 115.4(3) . . ? C1 N5 Cr 121.1(2) . 7_566 ? C14 N5 Cr 123.5(2) . 7_566 ? N5 C1 N4 125.5(3) . . ? C3 C2 C7 121.6(4) . . ? C3 C2 N4 119.6(4) . . ? C7 C2 N4 118.8(4) . . ? C2 C3 C4 117.3(5) . . ? C2 C3 C8 123.1(4) . . ? C4 C3 C8 119.5(4) . . ? C5 C4 C3 121.7(5) . . ? C4 C5 C6 120.1(4) . . ? C5 C6 C7 121.4(5) . . ? C6 C7 C2 117.9(5) . . ? C6 C7 C11 119.0(4) . . ? C2 C7 C11 123.1(4) . . ? C10' C8 C9 110.2(10) . . ? C10' C8 C3 119.2(7) . . ? C9 C8 C3 108.4(8) . . ? C10' C8 C10 24.0(7) . . ? C9 C8 C10 98.3(9) . . ? C3 C8 C10 106.5(6) . . ? C10' C8 C9' 113.3(10) . . ? C9 C8 C9' 11.6(11) . . ? C3 C8 C9' 113.9(7) . . ? C10 C8 C9' 105.4(9) . . ? C12 C11 C13 102.6(11) . . ? C12 C11 C7 118.5(8) . . ? C13 C11 C7 115.9(9) . . ? C12 C11 C12' 20.1(9) . . ? C13 C11 C12' 95.2(10) . . ? C7 C11 C12' 107.0(8) . . ? C12 C11 C13' 118.7(10) . . ? C13 C11 C13' 16.2(11) . . ? C7 C11 C13' 105.8(7) . . ? C12' C11 C13' 110.9(10) . . ? C19 C14 C15 121.5(3) . . ? C19 C14 N5 119.8(3) . . ? C15 C14 N5 118.7(3) . . ? C16 C15 C14 118.2(4) . . ? C16 C15 C20 119.2(3) . . ? C14 C15 C20 122.5(3) . . ? C17 C16 C15 121.2(4) . . ? C16 C17 C18 119.8(4) . . ? C17 C18 C19 121.7(4) . . ? C18 C19 C14 117.6(4) . . ? C18 C19 C23 118.7(4) . . ? C14 C19 C23 123.7(3) . . ? C21 C20 C22 110.6(4) . . ? C21 C20 C15 109.5(3) . . ? C22 C20 C15 112.8(3) . . ? C24' C23 C25 89.2(9) . . ? C24' C23 C19 113.9(6) . . ? C25 C23 C19 113.0(7) . . ? C24' C23 C25' 107.8(8) . . ? C25 C23 C25' 19.7(8) . . ? C19 C23 C25' 109.3(6) . . ? C24' C23 C24 19.2(7) . . ? C25 C23 C24 108.1(9) . . ? C19 C23 C24 107.8(6) . . ? C25' C23 C24 126.0(8) . . ? C31 O5 C31 103.3(10) . 2 ? C31 C30 C30 105.9(4) . 2 ? O5 C31 C30 107.4(9) . . ? O5 C31 O5 33.6(10) . 2 ? C30 C31 O5 106.8(8) . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.435 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.080 data_a10393 _database_code_depnum_ccdc_archive 'CCDC 903293' #TrackingRef '16364_web_deposit_cif_file_3_Yi-ChouTsai_1356074359.compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety "C62 H78 Mo2 N6 O4', 0.7(C6 H14)" _chemical_formula_sum 'C66.20 H87.80 Mo2 N6 O4' _chemical_formula_weight 1223.50 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5514(13) _cell_length_b 13.6186(13) _cell_length_c 34.248(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.118(2) _cell_angle_gamma 90.00 _cell_volume 6240.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2572 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8053 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 40388 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.05 _reflns_number_total 10905 _reflns_number_gt 8751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0539P)^2^+4.4411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10905 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 C1 C 0.8141(2) 0.0968(2) 0.07216(8) 0.0281(7) Uani 1 1 d . . . C2 C 0.8708(2) 0.1820(3) 0.07147(9) 0.0329(8) Uani 1 1 d . . . C3 C 0.8915(2) 0.2548(3) 0.10522(10) 0.0358(8) Uani 1 1 d . . . H3 H 0.8626 0.2280 0.1281 0.043 Uiso 1 1 calc R . . C4 C 0.8451(3) 0.3548(3) 0.09479(11) 0.0511(10) Uani 1 1 d . . . H4A H 0.8592 0.3983 0.1178 0.077 Uiso 1 1 calc R . . H4B H 0.7726 0.3476 0.0872 0.077 Uiso 1 1 calc R . . H4C H 0.8736 0.3829 0.0727 0.077 Uiso 1 1 calc R . . C5 C 1.0058(3) 0.2704(3) 0.11863(11) 0.0483(10) Uani 1 1 d . . . H5A H 1.0378 0.2070 0.1258 0.072 Uiso 1 1 calc R . . H5B H 1.0166 0.3143 0.1416 0.072 Uiso 1 1 calc R . . H5C H 1.0350 0.2996 0.0969 0.072 Uiso 1 1 calc R . . C6 C 0.9171(3) 0.1988(3) 0.03813(10) 0.0423(9) Uani 1 1 d . . . H6 H 0.9555 0.2568 0.0369 0.051 Uiso 1 1 calc R . . C7 C 0.9082(3) 0.1335(3) 0.00729(11) 0.0501(10) Uani 1 1 d . . . H7 H 0.9394 0.1468 -0.0151 0.060 Uiso 1 1 calc R . . C8 C 0.8544(3) 0.0494(3) 0.00888(10) 0.0453(10) Uani 1 1 d . . . H8 H 0.8490 0.0045 -0.0126 0.054 Uiso 1 1 calc R . . C9 C 0.8069(2) 0.0276(3) 0.04122(9) 0.0346(8) Uani 1 1 d . . . C10 C 0.7554(3) -0.0714(3) 0.04232(10) 0.0396(9) Uani 1 1 d . . . H10 H 0.7393 -0.0807 0.0696 0.048 Uiso 1 1 calc R . . C11 C 0.6572(3) -0.0773(3) 0.01328(11) 0.0535(11) Uani 1 1 d . . . H11A H 0.6269 -0.1421 0.0153 0.080 Uiso 1 1 calc R . . H11B H 0.6707 -0.0673 -0.0137 0.080 Uiso 1 1 calc R . . H11C H 0.6113 -0.0264 0.0197 0.080 Uiso 1 1 calc R . . C12 C 0.8242(3) -0.1566(3) 0.03400(11) 0.0549(11) Uani 1 1 d . . . H12A H 0.7885 -0.2190 0.0347 0.082 Uiso 1 1 calc R . . H12B H 0.8842 -0.1571 0.0542 0.082 Uiso 1 1 calc R . . H12C H 0.8435 -0.1478 0.0078 0.082 Uiso 1 1 calc R . . C13 C 0.8157(2) 0.0484(2) 0.14014(8) 0.0254(7) Uani 1 1 d . . . C14 C 0.9277(2) 0.0386(2) 0.14646(9) 0.0279(7) Uani 1 1 d . . . C15 C 0.9812(2) -0.0014(3) 0.11899(10) 0.0362(8) Uani 1 1 d . . . H15 H 0.9463 -0.0261 0.0947 0.043 Uiso 1 1 calc R . . C16 C 1.0848(3) -0.0060(3) 0.12638(11) 0.0440(9) Uani 1 1 d . . . H16 H 1.1198 -0.0329 0.1070 0.053 Uiso 1 1 calc R . . C17 C 1.1375(3) 0.0281(3) 0.16149(11) 0.0438(9) Uani 1 1 d . . . H17 H 1.2083 0.0243 0.1666 0.053 Uiso 1 1 calc R . . C18 C 1.0850(3) 0.0679(3) 0.18915(11) 0.0398(9) Uani 1 1 d . . . H18 H 1.1204 0.0918 0.2135 0.048 Uiso 1 1 calc R . . C19 C 0.9819(2) 0.0736(2) 0.18199(9) 0.0310(8) Uani 1 1 d . . . H19 H 0.9474 0.1014 0.2014 0.037 Uiso 1 1 calc R . . C20 C 0.8077(2) -0.0332(2) 0.20233(8) 0.0260(7) Uani 1 1 d . . . C21 C 0.8338(2) -0.1306(3) 0.19389(9) 0.0320(8) Uani 1 1 d . . . C22 C 0.8228(3) -0.1790(3) 0.15380(11) 0.0432(9) Uani 1 1 d . . . H22 H 0.7963 -0.1296 0.1332 0.052 Uiso 1 1 calc R . . C23 C 0.9244(3) -0.2176(3) 0.14500(13) 0.0648(13) Uani 1 1 d . . . H23A H 0.9151 -0.2478 0.1187 0.097 Uiso 1 1 calc R . . H23B H 0.9507 -0.2665 0.1649 0.097 Uiso 1 1 calc R . . H23C H 0.9716 -0.1628 0.1458 0.097 Uiso 1 1 calc R . . C24 C 0.7501(3) -0.2658(3) 0.15122(14) 0.0713(14) Uani 1 1 d . . . H24A H 0.7437 -0.2955 0.1249 0.107 Uiso 1 1 calc R . . H24B H 0.6845 -0.2426 0.1559 0.107 Uiso 1 1 calc R . . H24C H 0.7756 -0.3148 0.1713 0.107 Uiso 1 1 calc R . . C25 C 0.8729(2) -0.1913(3) 0.22553(10) 0.0393(9) Uani 1 1 d . . . H25 H 0.8914 -0.2566 0.2201 0.047 Uiso 1 1 calc R . . C26 C 0.8855(3) -0.1602(3) 0.26393(10) 0.0417(9) Uani 1 1 d . . . H26 H 0.9125 -0.2031 0.2848 0.050 Uiso 1 1 calc R . . C27 C 0.8585(3) -0.0662(3) 0.27201(10) 0.0394(9) Uani 1 1 d . . . H27 H 0.8666 -0.0447 0.2987 0.047 Uiso 1 1 calc R . . C28 C 0.8194(2) -0.0011(3) 0.24181(9) 0.0309(8) Uani 1 1 d . . . C29 C 0.7889(3) 0.0990(3) 0.25421(9) 0.0341(8) Uani 1 1 d . . . H29 H 0.7685 0.1395 0.2299 0.041 Uiso 1 1 calc R . . C30 C 0.8734(3) 0.1523(3) 0.28072(10) 0.0522(10) Uani 1 1 d . . . H30A H 0.8503 0.2173 0.2876 0.078 Uiso 1 1 calc R . . H30B H 0.9306 0.1596 0.2667 0.078 Uiso 1 1 calc R . . H30C H 0.8936 0.1141 0.3049 0.078 Uiso 1 1 calc R . . C31 C 0.6992(3) 0.0891(3) 0.27575(11) 0.0494(10) Uani 1 1 d . . . H31A H 0.6789 0.1543 0.2836 0.074 Uiso 1 1 calc R . . H31B H 0.7174 0.0483 0.2993 0.074 Uiso 1 1 calc R . . H31C H 0.6437 0.0585 0.2581 0.074 Uiso 1 1 calc R . . C32 C 0.6032(2) 0.2740(2) 0.20450(8) 0.0248(7) Uani 1 1 d . . . C33 C 0.6873(2) 0.3320(2) 0.21750(8) 0.0288(7) Uani 1 1 d . . . C34 C 0.7629(2) 0.3627(2) 0.19152(9) 0.0329(8) Uani 1 1 d . . . H34 H 0.7407 0.3357 0.1644 0.039 Uiso 1 1 calc R . . C35 C 0.7675(3) 0.4760(3) 0.18841(11) 0.0466(9) Uani 1 1 d . . . H35A H 0.7009 0.5016 0.1781 0.070 Uiso 1 1 calc R . . H35B H 0.8142 0.4943 0.1705 0.070 Uiso 1 1 calc R . . H35C H 0.7904 0.5039 0.2147 0.070 Uiso 1 1 calc R . . C36 C 0.8677(3) 0.3254(3) 0.20615(11) 0.0476(10) Uani 1 1 d . . . H36A H 0.8669 0.2535 0.2076 0.071 Uiso 1 1 calc R . . H36B H 0.8916 0.3524 0.2325 0.071 Uiso 1 1 calc R . . H36C H 0.9124 0.3461 0.1878 0.071 Uiso 1 1 calc R . . C37 C 0.6996(3) 0.3705(3) 0.25579(9) 0.0380(8) Uani 1 1 d . . . H37 H 0.7578 0.4075 0.2653 0.046 Uiso 1 1 calc R . . C38 C 0.6291(3) 0.3559(3) 0.28010(10) 0.0421(9) Uani 1 1 d . . . H38 H 0.6393 0.3819 0.3062 0.051 Uiso 1 1 calc R . . C39 C 0.5443(3) 0.3036(3) 0.26652(9) 0.0377(9) Uani 1 1 d . . . H39 H 0.4950 0.2957 0.2832 0.045 Uiso 1 1 calc R . . C40 C 0.5281(2) 0.2616(2) 0.22876(8) 0.0288(7) Uani 1 1 d . . . C41 C 0.4298(2) 0.2094(2) 0.21530(9) 0.0329(8) Uani 1 1 d . . . H41 H 0.4253 0.1950 0.1864 0.040 Uiso 1 1 calc R . . C42 C 0.4223(3) 0.1119(3) 0.23671(11) 0.0500(10) Uani 1 1 d . . . H42A H 0.3580 0.0808 0.2269 0.075 Uiso 1 1 calc R . . H42B H 0.4275 0.1239 0.2652 0.075 Uiso 1 1 calc R . . H42C H 0.4768 0.0686 0.2318 0.075 Uiso 1 1 calc R . . C43 C 0.3396(3) 0.2733(3) 0.22066(11) 0.0503(10) Uani 1 1 d . . . H43A H 0.3431 0.3358 0.2068 0.075 Uiso 1 1 calc R . . H43B H 0.3403 0.2858 0.2489 0.075 Uiso 1 1 calc R . . H43C H 0.2778 0.2389 0.2098 0.075 Uiso 1 1 calc R . . C44 C 0.5626(2) 0.2794(2) 0.13307(8) 0.0232(6) Uani 1 1 d . . . C45 C 0.5467(2) 0.3883(2) 0.13346(8) 0.0254(7) Uani 1 1 d . . . C46 C 0.4961(2) 0.4370(2) 0.15984(9) 0.0302(7) Uani 1 1 d . . . H46 H 0.4691 0.4005 0.1793 0.036 Uiso 1 1 calc R . . C47 C 0.4841(3) 0.5377(3) 0.15830(10) 0.0374(8) Uani 1 1 d . . . H47 H 0.4477 0.5693 0.1762 0.045 Uiso 1 1 calc R . . C48 C 0.5247(3) 0.5931(3) 0.13086(10) 0.0397(9) Uani 1 1 d . . . H48 H 0.5171 0.6624 0.1299 0.048 Uiso 1 1 calc R . . C49 C 0.5764(3) 0.5452(3) 0.10488(10) 0.0370(8) Uani 1 1 d . . . H49 H 0.6049 0.5820 0.0859 0.044 Uiso 1 1 calc R . . C50 C 0.5872(2) 0.4454(2) 0.10615(9) 0.0313(8) Uani 1 1 d . . . H50 H 0.6233 0.4141 0.0880 0.038 Uiso 1 1 calc R . . C51 C 0.4898(2) 0.2763(2) 0.06430(8) 0.0268(7) Uani 1 1 d . . . C52 C 0.3887(2) 0.2989(2) 0.06630(9) 0.0297(7) Uani 1 1 d . . . C53 C 0.3310(2) 0.2715(3) 0.09963(9) 0.0341(8) Uani 1 1 d . . . H53 H 0.3786 0.2427 0.1220 0.041 Uiso 1 1 calc R . . C54 C 0.2786(3) 0.3601(3) 0.11497(11) 0.0506(10) Uani 1 1 d . . . H54A H 0.2426 0.3389 0.1362 0.076 Uiso 1 1 calc R . . H54B H 0.2312 0.3884 0.0933 0.076 Uiso 1 1 calc R . . H54C H 0.3285 0.4096 0.1252 0.076 Uiso 1 1 calc R . . C55 C 0.2497(3) 0.1949(3) 0.08514(10) 0.0435(9) Uani 1 1 d . . . H55A H 0.2136 0.1778 0.1068 0.065 Uiso 1 1 calc R . . H55B H 0.2809 0.1358 0.0762 0.065 Uiso 1 1 calc R . . H55C H 0.2027 0.2223 0.0631 0.065 Uiso 1 1 calc R . . C56 C 0.3316(3) 0.3466(3) 0.03415(10) 0.0405(9) Uani 1 1 d . . . H56 H 0.2642 0.3633 0.0356 0.049 Uiso 1 1 calc R . . C57 C 0.3703(3) 0.3698(3) 0.00079(10) 0.0492(10) Uani 1 1 d . . . H57 H 0.3311 0.4043 -0.0203 0.059 Uiso 1 1 calc R . . C58 C 0.4666(3) 0.3427(3) -0.00181(10) 0.0433(9) Uani 1 1 d . . . H58 H 0.4925 0.3568 -0.0254 0.052 Uiso 1 1 calc R . . C59 C 0.5274(2) 0.2951(3) 0.02898(9) 0.0326(8) Uani 1 1 d . . . C60 C 0.6296(3) 0.2651(3) 0.02130(9) 0.0387(9) Uani 1 1 d . . . H60 H 0.6690 0.2415 0.0467 0.046 Uiso 1 1 calc R . . C61 C 0.6872(3) 0.3492(3) 0.00568(12) 0.0584(12) Uani 1 1 d . . . H61A H 0.7528 0.3254 0.0012 0.088 Uiso 1 1 calc R . . H61B H 0.6960 0.4026 0.0251 0.088 Uiso 1 1 calc R . . H61C H 0.6496 0.3733 -0.0193 0.088 Uiso 1 1 calc R . . C62 C 0.6182(3) 0.1803(3) -0.00788(12) 0.0590(12) Uani 1 1 d . . . H62A H 0.6843 0.1594 -0.0128 0.089 Uiso 1 1 calc R . . H62B H 0.5780 0.2015 -0.0328 0.089 Uiso 1 1 calc R . . H62C H 0.5849 0.1253 0.0031 0.089 Uiso 1 1 calc R . . Mo1 Mo 0.597691(19) 0.07998(2) 0.099650(7) 0.02351(9) Uani 1 1 d . . . Mo2 Mo 0.607088(19) 0.067113(19) 0.160814(7) 0.02289(9) Uani 1 1 d . . . N1 N 0.76137(18) 0.07644(18) 0.10527(7) 0.0237(6) Uani 1 1 d . . . N2 N 0.76537(18) 0.03523(18) 0.17071(7) 0.0231(5) Uani 1 1 d . . . N3 N 0.59050(17) 0.22563(18) 0.16612(6) 0.0214(5) Uani 1 1 d . . . N4 N 0.55594(18) 0.23201(18) 0.09791(6) 0.0224(5) Uani 1 1 d . . . N5 N 0.5754(2) -0.1288(2) 0.12392(9) 0.0394(7) Uani 1 1 d . . . N6 N 0.3978(2) 0.0356(2) 0.11972(8) 0.0366(7) Uani 1 1 d . . . O1 O 0.58988(17) -0.07398(16) 0.09489(7) 0.0357(6) Uani 1 1 d . . . O2 O 0.59209(17) -0.08547(16) 0.15748(7) 0.0351(5) Uani 1 1 d . . . O3 O 0.45091(16) 0.04954(16) 0.15366(6) 0.0310(5) Uani 1 1 d . . . O4 O 0.44346(16) 0.05590(16) 0.09084(6) 0.0327(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0232(17) 0.037(2) 0.0246(15) 0.0036(13) 0.0045(12) 0.0067(15) C2 0.0262(19) 0.041(2) 0.0329(17) 0.0058(15) 0.0078(13) 0.0056(15) C3 0.034(2) 0.037(2) 0.0385(18) 0.0074(15) 0.0096(14) -0.0025(16) C4 0.050(3) 0.048(3) 0.055(2) 0.0056(19) 0.0072(18) 0.005(2) C5 0.034(2) 0.057(3) 0.054(2) 0.0083(19) 0.0065(16) -0.0058(19) C6 0.036(2) 0.052(3) 0.0418(19) 0.0138(18) 0.0138(15) 0.0041(18) C7 0.044(2) 0.072(3) 0.038(2) 0.011(2) 0.0204(17) 0.010(2) C8 0.043(2) 0.064(3) 0.0293(18) -0.0047(17) 0.0089(15) 0.016(2) C9 0.0291(19) 0.044(2) 0.0306(17) -0.0001(15) 0.0042(13) 0.0098(16) C10 0.042(2) 0.043(2) 0.0329(18) -0.0117(15) 0.0040(15) 0.0040(17) C11 0.048(3) 0.060(3) 0.049(2) -0.0138(19) -0.0044(18) 0.004(2) C12 0.060(3) 0.052(3) 0.051(2) -0.0157(19) 0.0021(19) 0.014(2) C13 0.0281(18) 0.0198(17) 0.0270(15) -0.0025(12) 0.0008(13) 0.0011(13) C14 0.0263(18) 0.0229(18) 0.0340(16) 0.0068(13) 0.0027(13) 0.0018(14) C15 0.030(2) 0.039(2) 0.0384(18) 0.0006(15) 0.0028(14) 0.0057(16) C16 0.036(2) 0.048(3) 0.050(2) 0.0054(18) 0.0149(17) 0.0126(18) C17 0.023(2) 0.049(2) 0.058(2) 0.0158(19) 0.0025(16) 0.0034(17) C18 0.030(2) 0.041(2) 0.044(2) 0.0086(16) -0.0052(15) -0.0079(16) C19 0.031(2) 0.0255(19) 0.0355(17) 0.0066(14) 0.0037(14) -0.0050(14) C20 0.0206(17) 0.0265(18) 0.0300(16) 0.0091(13) 0.0011(12) -0.0035(14) C21 0.0245(18) 0.033(2) 0.0388(18) 0.0067(15) 0.0049(13) -0.0005(15) C22 0.051(2) 0.024(2) 0.049(2) -0.0007(16) -0.0045(17) 0.0060(17) C23 0.085(3) 0.049(3) 0.063(3) 0.004(2) 0.019(2) 0.027(2) C24 0.072(3) 0.026(2) 0.102(4) -0.002(2) -0.030(3) 0.003(2) C25 0.030(2) 0.033(2) 0.055(2) 0.0150(17) 0.0076(16) 0.0044(16) C26 0.032(2) 0.047(3) 0.045(2) 0.0244(18) 0.0007(15) 0.0061(17) C27 0.036(2) 0.049(3) 0.0325(18) 0.0130(16) 0.0019(14) 0.0011(17) C28 0.0253(18) 0.038(2) 0.0286(16) 0.0073(14) 0.0017(13) -0.0041(15) C29 0.041(2) 0.035(2) 0.0249(16) 0.0048(14) 0.0011(14) -0.0016(16) C30 0.065(3) 0.048(3) 0.038(2) 0.0004(18) -0.0107(17) -0.010(2) C31 0.052(3) 0.055(3) 0.043(2) 0.0069(18) 0.0138(18) 0.010(2) C32 0.0329(18) 0.0211(17) 0.0201(14) -0.0010(12) 0.0033(12) 0.0025(14) C33 0.0351(19) 0.0233(18) 0.0270(15) -0.0005(13) 0.0016(13) 0.0025(15) C34 0.033(2) 0.031(2) 0.0327(17) -0.0033(14) 0.0002(14) -0.0054(15) C35 0.053(3) 0.034(2) 0.052(2) 0.0036(17) 0.0038(18) -0.0048(18) C36 0.040(2) 0.054(3) 0.048(2) 0.0066(19) 0.0038(17) -0.0004(19) C37 0.045(2) 0.029(2) 0.0370(18) -0.0064(15) -0.0042(15) -0.0007(16) C38 0.058(3) 0.040(2) 0.0284(17) -0.0095(15) 0.0047(16) 0.0045(19) C39 0.049(2) 0.039(2) 0.0269(16) 0.0001(15) 0.0119(15) 0.0073(18) C40 0.0351(19) 0.0268(19) 0.0247(15) 0.0037(13) 0.0055(13) 0.0059(15) C41 0.035(2) 0.037(2) 0.0291(16) 0.0034(14) 0.0106(13) -0.0019(16) C42 0.052(3) 0.052(3) 0.046(2) 0.0134(19) 0.0072(17) -0.015(2) C43 0.040(2) 0.064(3) 0.052(2) -0.003(2) 0.0211(17) 0.003(2) C44 0.0184(16) 0.0264(18) 0.0255(15) 0.0020(13) 0.0054(11) 0.0007(13) C45 0.0234(17) 0.0261(18) 0.0254(15) 0.0002(13) -0.0007(12) 0.0005(14) C46 0.0329(19) 0.0256(19) 0.0314(16) 0.0035(13) 0.0029(13) 0.0020(14) C47 0.037(2) 0.033(2) 0.0415(19) -0.0044(16) 0.0036(15) 0.0073(16) C48 0.041(2) 0.025(2) 0.050(2) 0.0035(16) -0.0010(16) 0.0003(16) C49 0.039(2) 0.033(2) 0.0382(18) 0.0086(15) 0.0028(15) -0.0037(16) C50 0.036(2) 0.029(2) 0.0286(16) 0.0030(14) 0.0037(13) -0.0020(15) C51 0.0288(18) 0.0257(18) 0.0248(15) 0.0000(13) 0.0006(12) 0.0001(14) C52 0.0298(19) 0.030(2) 0.0277(16) -0.0024(13) 0.0015(13) 0.0038(15) C53 0.0254(18) 0.047(2) 0.0300(16) -0.0009(15) 0.0029(13) 0.0044(16) C54 0.031(2) 0.067(3) 0.054(2) -0.018(2) 0.0055(16) 0.0061(19) C55 0.031(2) 0.052(3) 0.048(2) 0.0066(18) 0.0058(15) 0.0030(18) C56 0.033(2) 0.048(2) 0.0405(19) 0.0050(17) 0.0064(15) 0.0126(17) C57 0.048(2) 0.057(3) 0.040(2) 0.0219(18) -0.0012(17) 0.015(2) C58 0.043(2) 0.055(3) 0.0329(18) 0.0150(17) 0.0097(15) 0.0097(19) C59 0.035(2) 0.035(2) 0.0272(16) 0.0072(14) 0.0023(13) 0.0019(15) C60 0.036(2) 0.054(2) 0.0267(16) 0.0119(16) 0.0061(14) 0.0083(17) C61 0.048(3) 0.078(3) 0.051(2) 0.032(2) 0.0135(18) 0.002(2) C62 0.053(3) 0.069(3) 0.055(2) -0.005(2) 0.0083(19) 0.022(2) Mo1 0.02289(16) 0.02375(17) 0.02310(14) -0.00187(10) 0.00117(10) 0.00130(11) Mo2 0.02273(16) 0.02146(16) 0.02440(14) 0.00255(10) 0.00351(10) -0.00025(11) N1 0.0242(14) 0.0264(15) 0.0206(12) -0.0009(10) 0.0041(10) 0.0005(11) N2 0.0235(14) 0.0204(14) 0.0246(13) 0.0023(10) 0.0015(10) 0.0006(11) N3 0.0235(14) 0.0225(14) 0.0185(11) 0.0001(10) 0.0040(9) -0.0032(11) N4 0.0233(14) 0.0242(15) 0.0198(12) 0.0009(10) 0.0034(9) 0.0018(11) N5 0.0346(17) 0.0269(17) 0.0557(19) -0.0011(14) 0.0044(13) -0.0016(13) N6 0.0247(16) 0.0363(18) 0.0485(17) 0.0012(14) 0.0044(13) -0.0021(13) O1 0.0340(14) 0.0286(14) 0.0438(13) -0.0065(11) 0.0041(10) 0.0003(10) O2 0.0323(14) 0.0255(13) 0.0466(14) 0.0032(10) 0.0039(10) -0.0026(10) O3 0.0254(13) 0.0306(13) 0.0373(12) 0.0014(10) 0.0062(10) -0.0033(10) O4 0.0247(13) 0.0330(14) 0.0381(12) -0.0038(10) -0.0015(10) -0.0011(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.394(5) . ? C1 C9 1.410(4) . ? C1 N1 1.460(4) . ? C2 C6 1.406(4) . ? C2 C3 1.515(5) . ? C3 C4 1.518(5) . ? C3 C5 1.560(5) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.371(5) . ? C6 H6 0.9500 . ? C7 C8 1.363(6) . ? C7 H7 0.9500 . ? C8 C9 1.398(5) . ? C8 H8 0.9500 . ? C9 C10 1.521(5) . ? C10 C11 1.532(5) . ? C10 C12 1.543(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.349(4) . ? C13 N1 1.355(4) . ? C13 C14 1.504(4) . ? C14 C15 1.388(4) . ? C14 C19 1.401(4) . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.378(5) . ? C16 H16 0.9500 . ? C17 C18 1.382(5) . ? C17 H17 0.9500 . ? C18 C19 1.381(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C28 1.406(4) . ? C20 C21 1.414(5) . ? C20 N2 1.475(4) . ? C21 C25 1.398(4) . ? C21 C22 1.508(5) . ? C22 C24 1.533(5) . ? C22 C23 1.547(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.366(5) . ? C25 H25 0.9500 . ? C26 C27 1.370(5) . ? C26 H26 0.9500 . ? C27 C28 1.402(4) . ? C27 H27 0.9500 . ? C28 C29 1.505(5) . ? C29 C31 1.524(5) . ? C29 C30 1.527(5) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.400(4) . ? C32 C40 1.422(4) . ? C32 N3 1.456(3) . ? C33 C37 1.397(4) . ? C33 C34 1.518(4) . ? C34 C36 1.518(5) . ? C34 C35 1.549(5) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.377(5) . ? C37 H37 0.9500 . ? C38 C39 1.369(5) . ? C38 H38 0.9500 . ? C39 C40 1.399(4) . ? C39 H39 0.9500 . ? C40 C41 1.516(5) . ? C41 C42 1.528(5) . ? C41 C43 1.534(5) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 N3 1.351(4) . ? C44 N4 1.356(4) . ? C44 C45 1.499(4) . ? C45 C46 1.387(4) . ? C45 C50 1.394(4) . ? C46 C47 1.380(5) . ? C46 H46 0.9500 . ? C47 C48 1.385(5) . ? C47 H47 0.9500 . ? C48 C49 1.381(5) . ? C48 H48 0.9500 . ? C49 C50 1.367(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C59 1.408(4) . ? C51 C52 1.416(4) . ? C51 N4 1.472(4) . ? C52 C56 1.401(4) . ? C52 C53 1.528(4) . ? C53 C54 1.534(5) . ? C53 C55 1.541(5) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.368(5) . ? C56 H56 0.9500 . ? C57 C58 1.372(5) . ? C57 H57 0.9500 . ? C58 C59 1.391(4) . ? C58 H58 0.9500 . ? C59 C60 1.507(5) . ? C60 C62 1.519(5) . ? C60 C61 1.530(5) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? Mo1 Mo2 2.0857(4) . ? Mo1 O4 2.090(2) . ? Mo1 O1 2.105(2) . ? Mo1 N4 2.145(2) . ? Mo1 N1 2.196(2) . ? Mo2 O2 2.089(2) . ? Mo2 O3 2.105(2) . ? Mo2 N2 2.162(2) . ? Mo2 N3 2.181(2) . ? N5 O2 1.280(3) . ? N5 O1 1.283(3) . ? N6 O4 1.277(3) . ? N6 O3 1.281(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C9 121.1(3) . . ? C2 C1 N1 120.7(3) . . ? C9 C1 N1 118.2(3) . . ? C1 C2 C6 117.9(3) . . ? C1 C2 C3 124.6(3) . . ? C6 C2 C3 117.4(3) . . ? C2 C3 C4 112.8(3) . . ? C2 C3 C5 111.6(3) . . ? C4 C3 C5 107.6(3) . . ? C2 C3 H3 108.2 . . ? C4 C3 H3 108.2 . . ? C5 C3 H3 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.6(4) . . ? C7 C6 H6 119.2 . . ? C2 C6 H6 119.2 . . ? C8 C7 C6 119.8(3) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 121.8(3) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 C1 117.8(3) . . ? C8 C9 C10 118.6(3) . . ? C1 C9 C10 123.5(3) . . ? C9 C10 C11 112.7(3) . . ? C9 C10 C12 111.6(3) . . ? C11 C10 C12 109.1(3) . . ? C9 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 N1 116.8(3) . . ? N2 C13 C14 119.9(2) . . ? N1 C13 C14 123.2(3) . . ? C15 C14 C19 117.6(3) . . ? C15 C14 C13 124.1(3) . . ? C19 C14 C13 118.3(3) . . ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 118.6(3) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C19 C18 C17 121.0(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C14 120.8(3) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C28 C20 C21 119.7(3) . . ? C28 C20 N2 118.7(3) . . ? C21 C20 N2 121.6(3) . . ? C25 C21 C20 118.1(3) . . ? C25 C21 C22 114.7(3) . . ? C20 C21 C22 127.1(3) . . ? C21 C22 C24 111.0(3) . . ? C21 C22 C23 111.3(3) . . ? C24 C22 C23 108.1(3) . . ? C21 C22 H22 108.8 . . ? C24 C22 H22 108.8 . . ? C23 C22 H22 108.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C21 122.5(3) . . ? C26 C25 H25 118.8 . . ? C21 C25 H25 118.8 . . ? C25 C26 C27 119.1(3) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C28 121.6(3) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C20 119.0(3) . . ? C27 C28 C29 117.0(3) . . ? C20 C28 C29 124.0(3) . . ? C28 C29 C31 109.4(3) . . ? C28 C29 C30 112.6(3) . . ? C31 C29 C30 109.6(3) . . ? C28 C29 H29 108.4 . . ? C31 C29 H29 108.4 . . ? C30 C29 H29 108.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C40 120.2(3) . . ? C33 C32 N3 121.1(3) . . ? C40 C32 N3 118.7(3) . . ? C37 C33 C32 118.7(3) . . ? C37 C33 C34 117.1(3) . . ? C32 C33 C34 124.0(3) . . ? C36 C34 C33 113.5(3) . . ? C36 C34 C35 108.1(3) . . ? C33 C34 C35 110.7(3) . . ? C36 C34 H34 108.2 . . ? C33 C34 H34 108.2 . . ? C35 C34 H34 108.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C33 121.5(3) . . ? C38 C37 H37 119.2 . . ? C33 C37 H37 119.3 . . ? C39 C38 C37 119.7(3) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 121.8(3) . . ? C38 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C39 C40 C32 118.0(3) . . ? C39 C40 C41 118.3(3) . . ? C32 C40 C41 123.6(3) . . ? C40 C41 C42 112.5(3) . . ? C40 C41 C43 112.1(3) . . ? C42 C41 C43 108.7(3) . . ? C40 C41 H41 107.8 . . ? C42 C41 H41 107.8 . . ? C43 C41 H41 107.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N3 C44 N4 117.1(3) . . ? N3 C44 C45 123.4(3) . . ? N4 C44 C45 119.3(3) . . ? C46 C45 C50 117.3(3) . . ? C46 C45 C44 124.5(3) . . ? C50 C45 C44 118.2(3) . . ? C47 C46 C45 121.2(3) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 120.7(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 118.5(3) . . ? C49 C48 H48 120.8 . . ? C47 C48 H48 120.8 . . ? C50 C49 C48 120.8(3) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C45 121.6(3) . . ? C49 C50 H50 119.2 . . ? C45 C50 H50 119.2 . . ? C59 C51 C52 119.1(3) . . ? C59 C51 N4 119.2(3) . . ? C52 C51 N4 121.7(2) . . ? C56 C52 C51 118.7(3) . . ? C56 C52 C53 114.6(3) . . ? C51 C52 C53 126.6(3) . . ? C52 C53 C54 112.5(3) . . ? C52 C53 C55 110.4(3) . . ? C54 C53 C55 107.2(3) . . ? C52 C53 H53 108.9 . . ? C54 C53 H53 108.9 . . ? C55 C53 H53 108.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C52 121.8(3) . . ? C57 C56 H56 119.1 . . ? C52 C56 H56 119.1 . . ? C56 C57 C58 119.1(3) . . ? C56 C57 H57 120.4 . . ? C58 C57 H57 120.4 . . ? C57 C58 C59 122.1(3) . . ? C57 C58 H58 119.0 . . ? C59 C58 H58 119.0 . . ? C58 C59 C51 119.0(3) . . ? C58 C59 C60 116.4(3) . . ? C51 C59 C60 124.6(3) . . ? C59 C60 C62 108.7(3) . . ? C59 C60 C61 113.1(3) . . ? C62 C60 C61 110.1(3) . . ? C59 C60 H60 108.3 . . ? C62 C60 H60 108.3 . . ? C61 C60 H60 108.3 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Mo2 Mo1 O4 91.85(6) . . ? Mo2 Mo1 O1 89.34(6) . . ? O4 Mo1 O1 78.20(9) . . ? Mo2 Mo1 N4 94.75(6) . . ? O4 Mo1 N4 83.92(9) . . ? O1 Mo1 N4 161.79(9) . . ? Mo2 Mo1 N1 90.58(6) . . ? O4 Mo1 N1 169.19(9) . . ? O1 Mo1 N1 91.30(9) . . ? N4 Mo1 N1 106.38(9) . . ? Mo1 Mo2 O2 92.22(6) . . ? Mo1 Mo2 O3 89.57(6) . . ? O2 Mo2 O3 78.07(9) . . ? Mo1 Mo2 N2 94.33(6) . . ? O2 Mo2 N2 83.93(9) . . ? O3 Mo2 N2 161.73(9) . . ? Mo1 Mo2 N3 90.56(6) . . ? O2 Mo2 N3 168.13(9) . . ? O3 Mo2 N3 90.41(9) . . ? N2 Mo2 N3 107.37(9) . . ? C13 N1 C1 118.2(3) . . ? C13 N1 Mo1 118.94(19) . . ? C1 N1 Mo1 122.69(18) . . ? C13 N2 C20 117.9(2) . . ? C13 N2 Mo2 117.57(19) . . ? C20 N2 Mo2 120.20(18) . . ? C44 N3 C32 119.3(3) . . ? C44 N3 Mo2 119.05(19) . . ? C32 N3 Mo2 121.61(18) . . ? C44 N4 C51 116.5(2) . . ? C44 N4 Mo1 117.03(19) . . ? C51 N4 Mo1 122.89(18) . . ? O2 N5 O1 113.6(3) . . ? O4 N6 O3 113.5(2) . . ? N5 O1 Mo1 122.14(19) . . ? N5 O2 Mo2 120.65(19) . . ? N6 O3 Mo2 122.18(18) . . ? N6 O4 Mo1 121.23(18) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.958 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.112 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 495.0 68.2 2 0.000 0.000 0.500 494.9 69.4 _platon_squeeze_details ; The unit cell volume comprises a large region of disordered solvent which could not be modeled as discrete atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 137.6 electrons per unit cell, which were assigned to be 2.8 n-hexane molecules per unit cell. ;