Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Malcolm Chisholm' _publ_contact_author_address ; Department of Chemistry The Ohio State University 100 West 18th Avenue Columbus Ohio 43210-1185 UNITED STATES OF AMERICA ; _publ_contact_author_email CHISHOLM@CHEMISTRY.OHIO-STATE.EDU _publ_section_title ; Amidinate-Carboxylate Complexes of Dimolybdenum and Ditungsten: M2(O2CR)2((NPri)2CR?)2. Preparations, Molecular and Electronic Structures and Reactions. ; _publ_requested_category FM loop_ _publ_author_name 'Douglas J. Brown' 'Malcolm Chisholm' 'Judith C. Gallucci' data_Chisholm1141 _database_code_depnum_ccdc_archive 'CCDC 637924' _audit_creation_date 2007-01-24T14:50:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1141' _chemical_formula_moiety 'C38 H54 Li2 N4 O2' _chemical_formula_sum 'C38 H54 Li2 N4 O2' _chemical_formula_weight 612.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7238(10) _cell_length_b 10.0080(10) _cell_length_c 19.713(2) _cell_angle_alpha 93.575(5) _cell_angle_beta 91.225(5) _cell_angle_gamma 90.848(4) _cell_volume 1914.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6721 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_special_details ;All work was done at 200 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 2.7, which means that 90% of the reflections were measured at least 2.7 times. A combination of phi and omega scans with a frame width of 1.0 degree was used. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.210858E-1 _diffrn_orient_matrix_ub_12 0.357859E-1 _diffrn_orient_matrix_ub_13 -0.449322E-1 _diffrn_orient_matrix_ub_21 -0.991601E-1 _diffrn_orient_matrix_ub_22 -0.104748E-1 _diffrn_orient_matrix_ub_23 -0.141132E-1 _diffrn_orient_matrix_ub_31 -0.175051E-1 _diffrn_orient_matrix_ub_32 0.929261E-1 _diffrn_orient_matrix_ub_33 0.191469E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 36676 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 6769 _reflns_number_gt 5267 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The structure is a Li dimer which contains a crystallographic inversion center. There are two independent half molecules in the asymmetric unit, and these are labeled as molecules A and B. One of the carbon atoms of a THF ligand in molecule A is disordered over two sites: C(19A) and C(19C). SADI restraints were used for the C-C and O-C bonds with the following pairs of bond lengths restrained to be equal: C(19A)-C(18A) and C(19C)-C(18A), and a second pair consisting of O(1A)-C(19A) and O(1A)-C(19C). The occupancy factor for C(19A) was refined and that for C(19C) was restricted accordingly. Atom C(19A) was refined anisotropically, and C(19C) was kept isotropic. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H)=1.5*Ueq(bonded atom). The torsion angle, which defines the orientation of each methyl group about the C-C bond, was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H)=1.2*Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.5717P] 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_number_reflns 6769 _refine_ls_number_parameters 428 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_gt 0.1348 _refine_ls_wR_factor_all 0.1471 _refine_ls_goodness_of_fit_gt 1.055 _refine_ls_goodness_of_fit_all 1.007 _refine_ls_restrained_S_all 1.009 _refine_ls_restrained_S_gt 1.056 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.184 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.034 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1A O 0.65708(13) 0.2185(2) 0.06883(6) 0.0669(4) Uani 1 d D . N1A N 0.56084(13) 0.13669(14) -0.09361(7) 0.0421(3) Uani 1 d . . N2A N 0.63922(14) -0.05576(15) -0.05041(7) 0.0492(4) Uani 1 d . . C1A C 0.6453(2) 0.0346(2) -0.09731(8) 0.0397(4) Uani 1 d . . C2A C 0.5576(2) 0.2306(2) -0.14715(8) 0.0456(4) Uani 1 d . . H2A H 0.6498 0.2327 -0.16857 0.055 Uiso 1 calc R . C3A C 0.5275(2) 0.3691(2) -0.11593(10) 0.0583(5) Uani 1 d . . H3A1 H 0.5290 0.4336 -0.1513 0.087 Uiso 1 calc R . H3A2 H 0.5975 0.3948 -0.0808 0.087 Uiso 1 calc R . H3A3 H 0.4365 0.3684 -0.0955 0.087 Uiso 1 calc R . C4A C 0.4494(2) 0.1878(2) -0.20152(9) 0.0618(5) Uani 1 d . . H4A1 H 0.4470 0.2536 -0.2363 0.093 Uiso 1 calc R . H4A2 H 0.3591 0.1824 -0.1807 0.093 Uiso 1 calc R . H4A3 H 0.4726 0.0999 -0.2225 0.093 Uiso 1 calc R . C5A C 0.7510(2) -0.1520(2) -0.04641(10) 0.0613(6) Uani 1 d . . H5A H 0.8158 -0.1388 -0.08425 0.074 Uiso 1 calc R . C6A C 0.8275(3) -0.1294(2) 0.0198(2) 0.1025(10) Uani 1 d . . H6A1 H 0.8666 -0.0383 0.0236 0.154 Uiso 1 calc R . H6A2 H 0.9018 -0.1942 0.0222 0.154 Uiso 1 calc R . H6A3 H 0.7644 -0.141 0.0572 0.154 Uiso 1 calc R . C7A C 0.6958(3) -0.2936(3) -0.0527(2) 0.1106(11) Uani 1 d . . H7A1 H 0.7724 -0.3560 -0.0507 0.166 Uiso 1 calc R . H7A2 H 0.646 -0.3094 -0.0962 0.166 Uiso 1 calc R . H7A3 H 0.633 -0.3078 -0.0153 0.166 Uiso 1 calc R . C8A C 0.7465(2) 0.0214(2) -0.15157(8) 0.0413(4) Uani 1 d . . C9A C 0.8295(2) 0.0088(2) -0.19530(8) 0.0401(4) Uani 1 d . . C10A C 0.9318(2) -0.0052(2) -0.24687(8) 0.0382(4) Uani 1 d . . C11A C 1.0201(2) 0.1010(2) -0.25761(9) 0.0522(5) Uani 1 d . . H11A H 1.0122 0.1830 -0.23114 0.063 Uiso 1 calc R . C12A C 1.1195(2) 0.0885(2) -0.30644(10) 0.0646(6) Uani 1 d . . H12A H 1.1795 0.1619 -0.31340 0.078 Uiso 1 calc R . C13A C 1.1319(2) -0.0288(3) -0.34475(10) 0.0668(6) Uani 1 d . . H13A H 1.2004 -0.0369 -0.37831 0.08 Uiso 1 calc R . C14A C 1.0453(2) -0.1354(2) -0.33492(10) 0.0644(6) Uani 1 d . . H14A H 1.0545 -0.2169 -0.36168 0.077 Uiso 1 calc R . C15A C 0.9446(2) -0.1245(2) -0.28609(9) 0.0509(4) Uani 1 d . . H15A H 0.8847 -0.1983 -0.27953 0.061 Uiso 1 calc R . C16A C 0.7978(2) 0.2523(2) 0.05728(11) 0.0675(6) Uani 1 d . . H16A H 0.8084 0.3494 0.05145 0.081 Uiso 1 calc R . H16B H 0.8304 0.2025 0.01585 0.081 Uiso 1 calc R . C17A C 0.8793(2) 0.2135(2) 0.11945(11) 0.0683(6) Uani 1 d . . H17A H 0.9375 0.1351 0.10823 0.082 Uiso 1 calc R . H17B H 0.9388 0.2888 0.13795 0.082 Uiso 1 calc R . C18A C 0.7711(2) 0.1799(3) 0.16934(12) 0.0819(7) Uani 1 d D . H18A H 0.7657 0.0821 0.17407 0.098 Uiso 0.790(12) calc PR 1 H18B H 0.7919 0.2252 0.21455 0.098 Uiso 0.790(12) calc PR 1 H18C H 0.7997 0.1012 0.19395 0.098 Uiso 0.210(12) calc PR 2 H18D H 0.7604 0.2563 0.20307 0.098 Uiso 0.210(12) calc PR 2 C19A C 0.6413(3) 0.2285(6) 0.14068(12) 0.0620(13) Uani 0.790(12) d PD 1 H19A H 0.5625 0.1725 0.15374 0.074 Uiso 0.790(12) calc PR 1 H19B H 0.6257 0.3224 0.15708 0.074 Uiso 0.790(12) calc PR 1 C19C C 0.6474(12) 0.152(2) 0.1353(6) 0.065(4) Uiso 0.210(12) d PD 2 H19C H 0.5700 0.189 0.1621 0.079 Uiso 0.210(12) calc PR 2 H19D H 0.6332 0.054 0.1271 0.079 Uiso 0.210(12) calc PR 2 Li1A Li 0.5361(3) 0.1197(3) 0.00555(15) 0.0535(7) Uani 1 d . . O1B O 0.5952(2) 0.24254(15) 0.54539(7) 0.0711(4) Uani 1 d . . N1B N 0.34457(14) 0.46413(14) 0.53779(7) 0.0442(3) Uani 1 d . . N2B N 0.45572(14) 0.62565(14) 0.60677(6) 0.0420(3) Uani 1 d . . C1B C 0.3542(2) 0.5374(2) 0.59686(8) 0.0385(4) Uani 1 d . . C2B C 0.2153(2) 0.3915(2) 0.51985(9) 0.0564(5) Uani 1 d . . H2B H 0.1461 0.4151 0.55527 0.068 Uiso 1 calc R . C3B C 0.2369(3) 0.2411(2) 0.5169(2) 0.0912(8) Uani 1 d . . H3B1 H 0.1490 0.1944 0.5062 0.137 Uiso 1 calc R . H3B2 H 0.273 0.2153 0.5610 0.137 Uiso 1 calc R . H3B3 H 0.3030 0.2166 0.4816 0.137 Uiso 1 calc R . C4B C 0.1619(2) 0.4341(3) 0.45197(12) 0.0844(7) Uani 1 d . . H4B1 H 0.0760 0.3854 0.4395 0.127 Uiso 1 calc R . H4B2 H 0.2303 0.4139 0.4172 0.127 Uiso 1 calc R . H4B3 H 0.1449 0.5305 0.4552 0.127 Uiso 1 calc R . C5B C 0.4760(2) 0.6981(2) 0.67289(8) 0.0475(4) Uani 1 d . . H5B H 0.3850 0.7076 0.69519 0.057 Uiso 1 calc R . C6B C 0.5345(2) 0.8360(2) 0.66263(11) 0.0694(6) Uani 1 d . . H6B1 H 0.5463 0.8859 0.70678 0.104 Uiso 1 calc R . H6B2 H 0.4712 0.8838 0.6337 0.104 Uiso 1 calc R . H6B3 H 0.6238 0.8277 0.6408 0.104 Uiso 1 calc R . C7B C 0.5715(2) 0.6226(2) 0.71811(10) 0.0685(6) Uani 1 d . . H7B1 H 0.5882 0.6753 0.7612 0.103 Uiso 1 calc R . H7B2 H 0.6590 0.6075 0.6953 0.103 Uiso 1 calc R . H7B3 H 0.5290 0.5363 0.7271 0.103 Uiso 1 calc R . C8B C 0.2545(2) 0.5177(2) 0.65039(8) 0.0428(4) Uani 1 d . . C9B C 0.1787(2) 0.4980(2) 0.69590(8) 0.0416(4) Uani 1 d . . C10B C 0.0918(2) 0.4725(2) 0.75189(8) 0.0384(4) Uani 1 d . . C11B C 0.1497(2) 0.4363(2) 0.81288(9) 0.0488(4) Uani 1 d . . H11B H 0.2467 0.4294 0.81772 0.059 Uiso 1 calc R . C12B C 0.0662(2) 0.4102(2) 0.86674(9) 0.0577(5) Uani 1 d . . H12B H 0.1062 0.3853 0.90841 0.069 Uiso 1 calc R . C13B C -0.0739(2) 0.4200(2) 0.86017(10) 0.0594(5) Uani 1 d . . H13B H -0.1307 0.4009 0.89708 0.071 Uiso 1 calc R . C14B C -0.1320(2) 0.4572(2) 0.80060(10) 0.0586(5) Uani 1 d . . H14B H -0.2290 0.4651 0.79650 0.07 Uiso 1 calc R . C15B C -0.0501(2) 0.4835(2) 0.74622(9) 0.0484(4) Uani 1 d . . H15B H -0.0911 0.5092 0.70494 0.058 Uiso 1 calc R . C16B C 0.5830(4) 0.2420(3) 0.61701(12) 0.1103(11) Uani 1 d . . H16C H 0.5071 0.1808 0.62830 0.132 Uiso 1 calc R . H16D H 0.5623 0.3330 0.63620 0.132 Uiso 1 calc R . C17B C 0.7109(3) 0.1980(3) 0.64526(13) 0.0972(8) Uani 1 d . . H17C H 0.6938 0.1279 0.67750 0.117 Uiso 1 calc R . H17D H 0.7607 0.2739 0.66985 0.117 Uiso 1 calc R . C18B C 0.7911(4) 0.1448(4) 0.5887(2) 0.1242(13) Uani 1 d . . H18E H 0.8085 0.0485 0.5931 0.149 Uiso 1 calc R . H18F H 0.8806 0.1929 0.5877 0.149 Uiso 1 calc R . C19B C 0.7096(3) 0.1641(3) 0.52583(13) 0.1030(10) Uani 1 d . . H19E H 0.7657 0.2107 0.49299 0.124 Uiso 1 calc R . H19F H 0.6782 0.0766 0.50429 0.124 Uiso 1 calc R . Li1B Li 0.5124(3) 0.3765(3) 0.49305(14) 0.0478(7) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0506(8) 0.1030(11) 0.0468(7) 0.0002(7) 0.0062(6) 0.0038(7) N1A 0.0401(7) 0.0486(8) 0.0393(7) 0.0116(6) 0.0108(6) 0.0081(6) N2A 0.0425(8) 0.0594(9) 0.0492(8) 0.0222(7) 0.0189(6) 0.0177(7) C1A 0.0322(8) 0.0500(10) 0.0380(8) 0.0067(7) 0.0089(6) 0.0027(7) C2A 0.0435(9) 0.0498(10) 0.0457(9) 0.0146(8) 0.0136(7) 0.0077(7) C3A 0.0622(12) 0.0490(11) 0.0651(12) 0.0112(9) 0.0075(9) 0.0053(9) C4A 0.0782(14) 0.0630(12) 0.0452(10) 0.0078(9) 0.0000(9) 0.0132(10) C5A 0.0515(11) 0.0760(14) 0.0622(12) 0.0338(10) 0.0285(9) 0.0286(10) C6A 0.078(2) 0.0631(15) 0.164(3) 0.003(2) -0.052(2) 0.0183(12) C7A 0.115(2) 0.068(2) 0.144(3) -0.029(2) -0.036(2) 0.046(2) C8A 0.0405(9) 0.0441(9) 0.0404(9) 0.0083(7) 0.0075(7) 0.0037(7) C9A 0.0381(9) 0.0431(9) 0.0401(9) 0.0084(7) 0.0069(7) 0.0047(7) C10A 0.0360(8) 0.0449(9) 0.0343(8) 0.0046(7) 0.0062(6) 0.0062(7) C11A 0.0564(11) 0.0506(10) 0.0497(10) 0.0000(8) 0.0185(8) -0.0034(8) C12A 0.0579(12) 0.0783(14) 0.0585(12) 0.0055(10) 0.0244(10) -0.0105(10) C13A 0.0522(11) 0.101(2) 0.0471(11) -0.0023(11) 0.0207(9) 0.0085(11) C14A 0.0663(13) 0.0744(14) 0.0503(11) -0.0201(10) 0.0071(10) 0.0169(11) C15A 0.0487(10) 0.0519(10) 0.0512(10) -0.0041(8) 0.0036(8) 0.0014(8) C16A 0.0651(13) 0.0751(14) 0.0614(12) -0.0017(10) 0.0115(10) -0.0137(11) C17A 0.0502(11) 0.0810(15) 0.0723(14) -0.0076(11) 0.0025(10) 0.0028(10) C18A 0.0619(14) 0.121(2) 0.0646(14) 0.0177(13) 0.0017(11) 0.0085(13) C19A 0.057(2) 0.084(3) 0.0445(15) -0.0033(14) 0.0103(11) 0.0064(15) Li1A 0.050(2) 0.067(2) 0.045(2) 0.0103(14) 0.0127(13) 0.0054(14) O1B 0.0957(11) 0.0738(9) 0.0466(7) 0.0146(7) 0.0132(7) 0.0357(8) N1B 0.0390(7) 0.0551(9) 0.0383(7) -0.0019(6) 0.0093(6) -0.0017(6) N2B 0.0408(7) 0.0500(8) 0.0353(7) 0.0020(6) 0.0081(6) -0.0011(6) C1B 0.0363(8) 0.0446(9) 0.0359(8) 0.0075(7) 0.0091(6) 0.0071(7) C2B 0.0459(10) 0.0721(13) 0.0495(11) -0.0103(9) 0.0140(8) -0.0120(9) C3B 0.089(2) 0.071(2) 0.113(2) 0.0062(14) 0.0042(15) -0.0303(13) C4B 0.0650(14) 0.108(2) 0.078(2) -0.0005(14) -0.0184(12) -0.0130(13) C5B 0.0445(9) 0.0558(11) 0.0414(9) -0.0051(8) 0.0101(7) -0.0008(8) C6B 0.0777(15) 0.0600(13) 0.0689(13) -0.0081(10) 0.0050(11) -0.0090(11) C7B 0.0806(15) 0.0831(15) 0.0415(10) 0.0010(10) -0.0030(10) 0.0092(12) C8B 0.0420(9) 0.0445(9) 0.0420(9) 0.0012(7) 0.0085(7) 0.0035(7) C9B 0.0427(9) 0.0406(9) 0.0416(9) 0.0008(7) 0.0104(7) 0.0017(7) C10B 0.0411(9) 0.0348(8) 0.0394(9) 0.0010(6) 0.0115(7) -0.0007(7) C11B 0.0456(10) 0.0520(10) 0.0496(10) 0.0079(8) 0.0050(8) 0.0031(8) C12B 0.0742(14) 0.0590(12) 0.0417(10) 0.0140(8) 0.0064(9) 0.0028(10) C13B 0.0677(13) 0.0592(12) 0.0534(11) 0.0117(9) 0.0283(10) 0.0004(10) C14B 0.0435(10) 0.0666(12) 0.0682(13) 0.0166(10) 0.0194(9) 0.0023(9) C15B 0.0431(10) 0.0570(11) 0.0462(10) 0.0110(8) 0.0070(8) 0.0002(8) C16B 0.151(3) 0.138(3) 0.0478(13) 0.0311(14) 0.0179(15) 0.076(2) C17B 0.107(2) 0.115(2) 0.070(2) 0.0086(15) -0.0128(15) 0.006(2) C18B 0.116(2) 0.164(3) 0.097(2) 0.027(2) 0.000(2) 0.076(2) C19B 0.131(2) 0.107(2) 0.073(2) 0.0017(14) 0.012(2) 0.070(2) Li1B 0.050(2) 0.053(2) 0.0409(15) 0.0058(12) 0.0104(12) 0.0067(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1A C19A 1.425(3) . ? O1A C16A 1.431(2) . ? O1A C19C 1.510(11) . ? O1A Li1A 1.914(3) . ? N1A C1A 1.320(2) . ? N1A C2A 1.456(2) . ? N1A Li1A 1.992(3) . ? N2A C1A 1.335(2) . ? N2A C5A 1.467(2) . ? N2A Li1A 2.050(3) 2_655 ? N2A Li1A 2.272(3) . ? C1A C8A 1.470(2) . ? C1A Li1A 2.422(3) . ? C2A C3A 1.516(3) . ? C2A C4A 1.523(3) . ? C2A H2A 1 . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C4A H4A1 0.98 . ? C4A H4A2 0.98 . ? C4A H4A3 0.98 . ? C5A C6A 1.492(3) . ? C5A C7A 1.505(4) . ? C5A H5A 1 . ? C6A H6A1 0.98 . ? C6A H6A2 0.98 . ? C6A H6A3 0.98 . ? C7A H7A1 0.98 . ? C7A H7A2 0.98 . ? C7A H7A3 0.98 . ? C8A C9A 1.195(2) . ? C9A C10A 1.440(2) . ? C10A C11A 1.386(2) . ? C10A C15A 1.390(2) . ? C11A C12A 1.380(2) . ? C11A H11A 0.95 . ? C12A C13A 1.364(3) . ? C12A H12A 0.95 . ? C13A C14A 1.374(3) . ? C13A H13A 0.95 . ? C14A C15A 1.389(3) . ? C14A H14A 0.95 . ? C15A H15A 0.95 . ? C16A C17A 1.519(3) . ? C16A H16A 0.99 . ? C16A H16B 0.99 . ? C17A C18A 1.504(3) . ? C17A H17A 0.99 . ? C17A H17B 0.99 . ? C18A C19C 1.380(11) . ? C18A C19A 1.473(4) . ? C18A H18A 0.99 . ? C18A H18B 0.99 . ? C18A H18C 0.99 . ? C18A H18D 0.99 . ? C19A H19A 0.99 . ? C19A H19B 0.99 . ? C19C Li1A 2.755(12) . ? C19C H19C 0.99 . ? C19C H19D 0.99 . ? Li1A N2A 2.050(3) 2_655 ? Li1A Li1A 2.483(7) 2_655 ? O1B C19B 1.417(3) . ? O1B C16B 1.420(3) . ? O1B Li1B 1.919(3) . ? N1B C1B 1.338(2) . ? N1B C2B 1.469(2) . ? N1B Li1B 2.053(3) . ? N1B Li1B 2.222(3) 2_666 ? N2B C1B 1.318(2) . ? N2B C5B 1.460(2) . ? N2B Li1B 1.997(3) 2_666 ? C1B C8B 1.469(2) . ? C1B Li1B 2.413(3) 2_666 ? C2B C4B 1.513(3) . ? C2B C3B 1.521(3) . ? C2B H2B 1 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C5B C6B 1.512(3) . ? C5B C7B 1.515(3) . ? C5B H5B 1 . ? C6B H6B1 0.98 . ? C6B H6B2 0.98 . ? C6B H6B3 0.98 . ? C7B H7B1 0.98 . ? C7B H7B2 0.98 . ? C7B H7B3 0.98 . ? C8B C9B 1.197(2) . ? C9B C10B 1.437(2) . ? C10B C11B 1.387(2) . ? C10B C15B 1.389(2) . ? C11B C12B 1.385(3) . ? C11B H11B 0.95 . ? C12B C13B 1.371(3) . ? C12B H12B 0.95 . ? C13B C14B 1.367(3) . ? C13B H13B 0.95 . ? C14B C15B 1.385(2) . ? C14B H14B 0.95 . ? C15B H15B 0.95 . ? C16B C17B 1.438(4) . ? C16B H16C 0.99 . ? C16B H16D 0.99 . ? C17B C18B 1.453(4) . ? C17B H17C 0.99 . ? C17B H17D 0.99 . ? C18B C19B 1.481(4) . ? C18B H18E 0.99 . ? C18B H18F 0.99 . ? C19B H19E 0.99 . ? C19B H19F 0.99 . ? Li1B N2B 1.997(3) 2_666 ? Li1B N1B 2.222(3) 2_666 ? Li1B C1B 2.413(3) 2_666 ? Li1B Li1B 2.485(6) 2_666 ? 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 C19A O1A C16A 106.3(2) . . ? C16A O1A C19C 109.3(5) . . ? C19A O1A Li1A 124.8(2) . . ? C16A O1A Li1A 125.48(14) . . ? C19C O1A Li1A 106.5(6) . . ? C1A N1A C2A 120.16(13) . . ? C1A N1A Li1A 91.72(13) . . ? C2A N1A Li1A 143.81(14) . . ? C1A N2A C5A 118.40(13) . . ? C1A N2A Li1A 125.69(14) . 2_655 ? C5A N2A Li1A 112.34(14) . 2_655 ? C1A N2A Li1A 79.77(12) . . ? C5A N2A Li1A 144.2(2) . . ? Li1A N2A Li1A 69.90(15) 2_655 . ? N1A C1A N2A 119.09(13) . . ? N1A C1A C8A 120.67(14) . . ? N2A C1A C8A 120.24(14) . . ? N1A C1A Li1A 55.28(11) . . ? N2A C1A Li1A 67.40(11) . . ? C8A C1A Li1A 159.44(14) . . ? N1A C2A C3A 108.93(14) . . ? N1A C2A C4A 110.77(15) . . ? C3A C2A C4A 110.5(2) . . ? N1A C2A H2A 108.9 . . ? C3A C2A H2A 108.9 . . ? C4A C2A H2A 108.9 . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4A H4A1 109.5 . . ? C2A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C2A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? N2A C5A C6A 109.9(2) . . ? N2A C5A C7A 111.0(2) . . ? C6A C5A C7A 109.0(2) . . ? N2A C5A H5A 109.0 . . ? C6A C5A H5A 109.0 . . ? C7A C5A H5A 109.0 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C9A C8A C1A 179.0(2) . . ? C8A C9A C10A 178.7(2) . . ? C11A C10A C15A 119.02(15) . . ? C11A C10A C9A 119.95(14) . . ? C15A C10A C9A 121.03(15) . . ? C12A C11A C10A 120.6(2) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C13A C12A C11A 120.2(2) . . ? C13A C12A H12A 119.9 . . ? C11A C12A H12A 119.9 . . ? C12A C13A C14A 120.2(2) . . ? C12A C13A H13A 119.9 . . ? C14A C13A H13A 119.9 . . ? C13A C14A C15A 120.4(2) . . ? C13A C14A H14A 119.8 . . ? C15A C14A H14A 119.8 . . ? C14A C15A C10A 119.6(2) . . ? C14A C15A H15A 120.2 . . ? C10A C15A H15A 120.2 . . ? O1A C16A C17A 106.4(2) . . ? O1A C16A H16A 110.4 . . ? C17A C16A H16A 110.4 . . ? O1A C16A H16B 110.4 . . ? C17A C16A H16B 110.4 . . ? H16A C16A H16B 108.6 . . ? C18A C17A C16A 104.2(2) . . ? C18A C17A H17A 110.9 . . ? C16A C17A H17A 110.9 . . ? C18A C17A H17B 110.9 . . ? C16A C17A H17B 110.9 . . ? H17A C17A H17B 108.9 . . ? C19C C18A C17A 109.8(5) . . ? C19A C18A C17A 105.2(2) . . ? C19A C18A H18A 110.7 . . ? C17A C18A H18A 110.7 . . ? C19A C18A H18B 110.7 . . ? C17A C18A H18B 110.7 . . ? H18A C18A H18B 108.8 . . ? C19C C18A H18C 109.7 . . ? C17A C18A H18C 109.7 . . ? C19C C18A H18D 109.7 . . ? C17A C18A H18D 109.7 . . ? H18C C18A H18D 108.2 . . ? O1A C19A C18A 105.4(2) . . ? O1A C19A H19A 110.7 . . ? C18A C19A H19A 110.7 . . ? O1A C19A H19B 110.7 . . ? C18A C19A H19B 110.7 . . ? H19A C19A H19B 108.8 . . ? C18A C19C O1A 105.7(8) . . ? C18A C19C H19C 110.6 . . ? O1A C19C H19C 110.6 . . ? C18A C19C H19D 110.6(9) . . ? O1A C19C H19D 110.6(8) . . ? H19C C19C H19D 108.7 . . ? O1A Li1A N1A 118.9(2) . . ? O1A Li1A N2A 112.16(15) . 2_655 ? N1A Li1A N2A 126.1(2) . 2_655 ? O1A Li1A N2A 113.2(2) . . ? N1A Li1A N2A 64.51(10) . . ? N2A Li1A N2A 110.10(15) 2_655 . ? O1A Li1A C1A 114.32(14) . . ? N1A Li1A C1A 33.00(7) . . ? N2A Li1A C1A 130.1(2) 2_655 . ? N2A Li1A C1A 32.83(7) . . ? O1A Li1A Li1A 132.2(2) . 2_655 ? N1A Li1A Li1A 95.3(2) . 2_655 ? N2A Li1A Li1A 59.26(12) 2_655 2_655 ? N2A Li1A Li1A 50.84(11) . 2_655 ? C1A Li1A Li1A 76.26(14) . 2_655 ? O1A Li1A C19C 31.7(3) . . ? N1A Li1A C19C 147.8(3) . . ? N2A Li1A C19C 86.1(3) 2_655 . ? N2A Li1A C19C 108.7(4) . . ? C1A Li1A C19C 128.3(4) . . ? Li1A Li1A C19C 103.7(4) 2_655 . ? C19B O1B C16B 108.5(2) . . ? C19B O1B Li1B 125.6(2) . . ? C16B O1B Li1B 122.5(2) . . ? C1B N1B C2B 118.82(13) . . ? C1B N1B Li1B 122.31(14) . . ? C2B N1B Li1B 112.87(14) . . ? C1B N1B Li1B 81.24(12) . 2_666 ? C2B N1B Li1B 144.21(14) . 2_666 ? Li1B N1B Li1B 70.95(13) . 2_666 ? C1B N2B C5B 120.21(13) . . ? C1B N2B Li1B 91.03(13) . 2_666 ? C5B N2B Li1B 146.54(14) . 2_666 ? N2B C1B N1B 119.11(13) . . ? N2B C1B C8B 120.53(14) . . ? N1B C1B C8B 120.35(14) . . ? N2B C1B Li1B 55.86(11) . 2_666 ? N1B C1B Li1B 65.54(11) . 2_666 ? C8B C1B Li1B 165.21(13) . 2_666 ? N1B C2B C4B 109.1(2) . . ? N1B C2B C3B 110.7(2) . . ? C4B C2B C3B 110.5(2) . . ? N1B C2B H2B 108.8 . . ? C4B C2B H2B 108.8 . . ? C3B C2B H2B 108.8 . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B H4B1 109.5 . . ? C2B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C2B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? N2B C5B C6B 109.07(15) . . ? N2B C5B C7B 110.70(15) . . ? C6B C5B C7B 110.5(2) . . ? N2B C5B H5B 108.8 . . ? C6B C5B H5B 108.8 . . ? C7B C5B H5B 108.8 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C5B C7B H7B1 109.5 . . ? C5B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C5B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C9B C8B C1B 176.3(2) . . ? C8B C9B C10B 178.0(2) . . ? C11B C10B C15B 118.97(15) . . ? C11B C10B C9B 119.91(15) . . ? C15B C10B C9B 121.12(15) . . ? C12B C11B C10B 120.1(2) . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C13B C12B C11B 120.3(2) . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C14B C13B C12B 120.1(2) . . ? C14B C13B H13B 119.9 . . ? C12B C13B H13B 119.9 . . ? C13B C14B C15B 120.3(2) . . ? C13B C14B H14B 119.8 . . ? C15B C14B H14B 119.8 . . ? C14B C15B C10B 120.2(2) . . ? C14B C15B H15B 119.9 . . ? C10B C15B H15B 119.9 . . ? O1B C16B C17B 108.4(2) . . ? O1B C16B H16C 110.0 . . ? C17B C16B H16C 110.0 . . ? O1B C16B H16D 110.0 . . ? C17B C16B H16D 110.0 . . ? H16C C16B H16D 108.4 . . ? C16B C17B C18B 106.9(2) . . ? C16B C17B H17C 110.3 . . ? C18B C17B H17C 110.3 . . ? C16B C17B H17D 110.3 . . ? C18B C17B H17D 110.3 . . ? H17C C17B H17D 108.6 . . ? C17B C18B C19B 106.9(2) . . ? C17B C18B H18E 110.3 . . ? C19B C18B H18E 110.3 . . ? C17B C18B H18F 110.3 . . ? C19B C18B H18F 110.3 . . ? H18E C18B H18F 108.6 . . ? O1B C19B C18B 106.6(2) . . ? O1B C19B H19E 110.4 . . ? C18B C19B H19E 110.4 . . ? O1B C19B H19F 110.4 . . ? C18B C19B H19F 110.4 . . ? H19E C19B H19F 108.6 . . ? O1B Li1B N2B 119.39(15) . 2_666 ? O1B Li1B N1B 113.72(14) . . ? N2B Li1B N1B 123.0(2) 2_666 . ? O1B Li1B N1B 115.1(2) . 2_666 ? N2B Li1B N1B 65.47(10) 2_666 2_666 ? N1B Li1B N1B 109.05(13) . 2_666 ? O1B Li1B C1B 117.33(14) . 2_666 ? N2B Li1B C1B 33.10(7) 2_666 2_666 ? N1B Li1B C1B 126.65(14) . 2_666 ? N1B Li1B C1B 33.22(6) 2_666 2_666 ? O1B Li1B Li1B 135.4(2) . 2_666 ? N2B Li1B Li1B 94.5(2) 2_666 2_666 ? N1B Li1B Li1B 57.69(11) . 2_666 ? N1B Li1B Li1B 51.36(11) 2_666 2_666 ? C1B Li1B Li1B 75.24(14) 2_666 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A N1A C1A N2A -175.0(2) . . . . ? Li1A N1A C1A N2A 23.0(2) . . . . ? C2A N1A C1A C8A 6.0(2) . . . . ? Li1A N1A C1A C8A -156.0(2) . . . . ? C2A N1A C1A Li1A 162.0(2) . . . . ? Li1A N1A C1A Li1A 0 . . . . ? C5A N2A C1A N1A -167.4(2) . . . . ? Li1A N2A C1A N1A 35.6(3) 2_655 . . . ? Li1A N2A C1A N1A -20.4(2) . . . . ? C5A N2A C1A C8A 11.6(3) . . . . ? Li1A N2A C1A C8A -145.4(2) 2_655 . . . ? Li1A N2A C1A C8A 158.6(2) . . . . ? C5A N2A C1A Li1A -147.0(2) . . . . ? Li1A N2A C1A Li1A 56.0(2) 2_655 . . . ? Li1A N2A C1A Li1A 0 . . . . ? C1A N1A C2A C3A -146.3(2) . . . . ? Li1A N1A C2A C3A 2.2(3) . . . . ? C1A N1A C2A C4A 91.9(2) . . . . ? Li1A N1A C2A C4A -119.6(2) . . . . ? C1A N2A C5A C6A 114.9(2) . . . . ? Li1A N2A C5A C6A -85.2(2) 2_655 . . . ? Li1A N2A C5A C6A 1.1(3) . . . . ? C1A N2A C5A C7A -124.5(2) . . . . ? Li1A N2A C5A C7A 35.5(2) 2_655 . . . ? Li1A N2A C5A C7A 121.7(3) . . . . ? C15A C10A C11A C12A -0.1(3) . . . . ? C9A C10A C11A C12A 179.4(2) . . . . ? C10A C11A C12A C13A 0.0(3) . . . . ? C11A C12A C13A C14A 0.0(3) . . . . ? C12A C13A C14A C15A 0.1(3) . . . . ? C13A C14A C15A C10A -0.2(3) . . . . ? C11A C10A C15A C14A 0.2(3) . . . . ? C9A C10A C15A C14A -179.3(2) . . . . ? C19A O1A C16A C17A 28.5(3) . . . . ? C19C O1A C16A C17A -3.0(9) . . . . ? Li1A O1A C16A C17A -131.3(2) . . . . ? O1A C16A C17A C18A -9.5(2) . . . . ? C16A C17A C18A C19C 20.1(10) . . . . ? C16A C17A C18A C19A -12.1(3) . . . . ? C16A O1A C19A C18A -36.7(4) . . . . ? C19C O1A C19A C18A 63.9(9) . . . . ? Li1A O1A C19A C18A 123.3(3) . . . . ? C19C C18A C19A O1A -73.3(10) . . . . ? C17A C18A C19A O1A 29.8(4) . . . . ? C19A C18A C19C O1A 64.9(10) . . . . ? C17A C18A C19C O1A -21.9(14) . . . . ? C19A C18A C19C Li1A 92.8(17) . . . . ? C17A C18A C19C Li1A 6(2) . . . . ? C19A O1A C19C C18A -73.7(12) . . . . ? C16A O1A C19C C18A 15.6(15) . . . . ? Li1A O1A C19C C18A 153.8(10) . . . . ? C19A O1A C19C Li1A 132.5(7) . . . . ? C16A O1A C19C Li1A -138.1(5) . . . . ? Li1A O1A C19C Li1A 0 . . . . ? C19A O1A Li1A N1A 172.1(3) . . . . ? C16A O1A Li1A N1A -31.7(3) . . . . ? C19C O1A Li1A N1A -161.0(8) . . . . ? C19A O1A Li1A N2A 10.1(3) . . . 2_655 ? C16A O1A Li1A N2A 166.3(2) . . . 2_655 ? C19C O1A Li1A N2A 37.0(8) . . . 2_655 ? C19A O1A Li1A N2A -115.2(3) . . . . ? C16A O1A Li1A N2A 41.0(3) . . . . ? C19C O1A Li1A N2A -88.4(8) . . . . ? C19A O1A Li1A C1A -151.2(3) . . . . ? C16A O1A Li1A C1A 5.0(3) . . . . ? C19C O1A Li1A C1A -124.3(8) . . . . ? C19A O1A Li1A Li1A -57.8(4) . . . 2_655 ? C16A O1A Li1A Li1A 98.3(3) . . . 2_655 ? C19C O1A Li1A Li1A -31.0(8) . . . 2_655 ? C19A O1A Li1A C19C -26.8(6) . . . . ? C16A O1A Li1A C19C 129.3(8) . . . . ? C19C O1A Li1A C19C 0 . . . . ? C1A N1A Li1A O1A 90.7(2) . . . . ? C2A N1A Li1A O1A -62.4(3) . . . . ? C1A N1A Li1A N2A -110.0(2) . . . 2_655 ? C2A N1A Li1A N2A 96.9(3) . . . 2_655 ? C1A N1A Li1A N2A -12.84(10) . . . . ? C2A N1A Li1A N2A -166.0(2) . . . . ? C1A N1A Li1A C1A 0 . . . . ? C2A N1A Li1A C1A -153.1(3) . . . . ? C1A N1A Li1A Li1A -54.5(2) . . . 2_655 ? C2A N1A Li1A Li1A 152.3(2) . . . 2_655 ? C1A N1A Li1A C19C 72.0(9) . . . . ? C2A N1A Li1A C19C -81.2(9) . . . . ? C1A N2A Li1A O1A -99.4(2) . . . . ? C5A N2A Li1A O1A 25.8(3) . . . . ? Li1A N2A Li1A O1A 126.4(2) 2_655 . . . ? C1A N2A Li1A N1A 12.90(10) . . . . ? C5A N2A Li1A N1A 138.0(2) . . . . ? Li1A N2A Li1A N1A -121.3(2) 2_655 . . . ? C1A N2A Li1A N2A 134.2(2) . . . 2_655 ? C5A N2A Li1A N2A -100.6(2) . . . 2_655 ? Li1A N2A Li1A N2A 0 2_655 . . 2_655 ? C1A N2A Li1A C1A 0 . . . . ? C5A N2A Li1A C1A 125.2(3) . . . . ? Li1A N2A Li1A C1A -134.2(2) 2_655 . . . ? C1A N2A Li1A Li1A 134.2(2) . . . 2_655 ? C5A N2A Li1A Li1A -100.6(2) . . . 2_655 ? Li1A N2A Li1A Li1A 0 2_655 . . 2_655 ? C1A N2A Li1A C19C -133.1(3) . . . . ? C5A N2A Li1A C19C -7.9(4) . . . . ? Li1A N2A Li1A C19C 92.7(3) 2_655 . . . ? N1A C1A Li1A O1A -106.2(2) . . . . ? N2A C1A Li1A O1A 95.5(2) . . . . ? C8A C1A Li1A O1A -20.8(5) . . . . ? N1A C1A Li1A N1A 0 . . . . ? N2A C1A Li1A N1A -158.3(2) . . . . ? C8A C1A Li1A N1A 85.4(4) . . . . ? N1A C1A Li1A N2A 96.7(2) . . . 2_655 ? N2A C1A Li1A N2A -61.6(2) . . . 2_655 ? C8A C1A Li1A N2A -177.9(3) . . . 2_655 ? N1A C1A Li1A N2A 158.3(2) . . . . ? N2A C1A Li1A N2A 0 . . . . ? C8A C1A Li1A N2A -116.3(4) . . . . ? N1A C1A Li1A Li1A 123.4(2) . . . 2_655 ? N2A C1A Li1A Li1A -34.90(14) . . . 2_655 ? C8A C1A Li1A Li1A -151.2(4) . . . 2_655 ? N1A C1A Li1A C19C -139.8(5) . . . . ? N2A C1A Li1A C19C 61.9(5) . . . . ? C8A C1A Li1A C19C -54.4(7) . . . . ? C18A C19C Li1A O1A -42.6(14) . . . . ? O1A C19C Li1A O1A 0 . . . . ? C18A C19C Li1A N1A -10(3) . . . . ? O1A C19C Li1A N1A 32.3(13) . . . . ? C18A C19C Li1A N2A 171(2) . . . 2_655 ? O1A C19C Li1A N2A -146.1(7) . . . 2_655 ? C18A C19C Li1A N2A 61(2) . . . . ? O1A C19C Li1A N2A 104.0(7) . . . . ? C18A C19C Li1A C1A 31(2) . . . . ? O1A C19C Li1A C1A 73.7(9) . . . . ? C18A C19C Li1A Li1A 114.3(19) . . . 2_655 ? O1A C19C Li1A Li1A 156.9(6) . . . 2_655 ? C5B N2B C1B N1B -174.39(15) . . . . ? Li1B N2B C1B N1B 18.2(2) 2_666 . . . ? C5B N2B C1B C8B 4.4(2) . . . . ? Li1B N2B C1B C8B -163.0(2) 2_666 . . . ? C5B N2B C1B Li1B 167.4(2) . . . 2_666 ? Li1B N2B C1B Li1B 0 2_666 . . 2_666 ? C2B N1B C1B N2B -164.9(2) . . . . ? Li1B N1B C1B N2B 44.3(2) . . . . ? Li1B N1B C1B N2B -16.5(2) 2_666 . . . ? C2B N1B C1B C8B 16.3(2) . . . . ? Li1B N1B C1B C8B -134.5(2) . . . . ? Li1B N1B C1B C8B 164.7(2) 2_666 . . . ? C2B N1B C1B Li1B -148.4(2) . . . 2_666 ? Li1B N1B C1B Li1B 60.8(2) . . . 2_666 ? Li1B N1B C1B Li1B 0 2_666 . . 2_666 ? C1B N1B C2B C4B 123.5(2) . . . . ? Li1B N1B C2B C4B -83.1(2) . . . . ? Li1B N1B C2B C4B 5.7(3) 2_666 . . . ? C1B N1B C2B C3B -114.7(2) . . . . ? Li1B N1B C2B C3B 38.7(2) . . . . ? Li1B N1B C2B C3B 127.5(2) 2_666 . . . ? C1B N2B C5B C6B -148.1(2) . . . . ? Li1B N2B C5B C6B 8.7(3) 2_666 . . . ? C1B N2B C5B C7B 90.1(2) . . . . ? Li1B N2B C5B C7B -113.1(3) 2_666 . . . ? C15B C10B C11B C12B 0.8(3) . . . . ? C9B C10B C11B C12B -179.3(2) . . . . ? C10B C11B C12B C13B -0.1(3) . . . . ? C11B C12B C13B C14B -0.8(3) . . . . ? C12B C13B C14B C15B 0.8(3) . . . . ? C13B C14B C15B C10B -0.1(3) . . . . ? C11B C10B C15B C14B -0.7(3) . . . . ? C9B C10B C15B C14B 179.4(2) . . . . ? C19B O1B C16B C17B 17.1(4) . . . . ? Li1B O1B C16B C17B -143.2(2) . . . . ? O1B C16B C17B C18B -11.8(4) . . . . ? C16B C17B C18B C19B 2.5(4) . . . . ? C16B O1B C19B C18B -15.1(4) . . . . ? Li1B O1B C19B C18B 144.3(3) . . . . ? C17B C18B C19B O1B 7.7(4) . . . . ? C19B O1B Li1B N2B 19.9(3) . . . 2_666 ? C16B O1B Li1B N2B 176.6(2) . . . 2_666 ? C19B O1B Li1B N1B 178.2(2) . . . . ? C16B O1B Li1B N1B -25.0(3) . . . . ? C19B O1B Li1B N1B -54.9(3) . . . 2_666 ? C16B O1B Li1B N1B 101.8(3) . . . 2_666 ? C19B O1B Li1B C1B -17.8(3) . . . 2_666 ? C16B O1B Li1B C1B 138.9(2) . . . 2_666 ? C19B O1B Li1B Li1B -114.5(3) . . . 2_666 ? C16B O1B Li1B Li1B 42.3(4) . . . 2_666 ? C1B N1B Li1B O1B 64.1(2) . . . . ? C2B N1B Li1B O1B -88.2(2) . . . . ? Li1B N1B Li1B O1B 130.0(2) 2_666 . . . ? C1B N1B Li1B N2B -138.4(2) . . . 2_666 ? C2B N1B Li1B N2B 69.2(2) . . . 2_666 ? Li1B N1B Li1B N2B -72.6(2) 2_666 . . 2_666 ? C1B N1B Li1B N1B -65.9(2) . . . 2_666 ? C2B N1B Li1B N1B 141.8(2) . . . 2_666 ? Li1B N1B Li1B N1B 0 2_666 . . 2_666 ? C1B N1B Li1B C1B -98.1(2) . . . 2_666 ? C2B N1B Li1B C1B 109.6(2) . . . 2_666 ? Li1B N1B Li1B C1B -32.20(11) 2_666 . . 2_666 ? C1B N1B Li1B Li1B -65.9(2) . . . 2_666 ? C2B N1B Li1B Li1B 141.8(2) . . . 2_666 ? Li1B N1B Li1B Li1B 0 2_666 . . 2_666 ? #END OF CIF#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-01-17 at 16:37:54 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1135 _database_code_depnum_ccdc_archive 'CCDC 637925' _audit_creation_date 2007-01-17T16:37:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1135' _chemical_formula_moiety 'C30 H50 Li2 N4 O2 S2' _chemical_formula_sum 'C30 H50 Li2 N4 O2 S2' _chemical_formula_weight 576.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 9.1730(1) _cell_length_b 10.9696(1) _cell_length_c 17.1896(2) _cell_angle_alpha 90 _cell_angle_beta 95.9532(7) _cell_angle_gamma 90 _cell_volume 1720.36(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3201 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'triangular plate' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_special_details ;All work was done at 200 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space witha redundancy factor of 4.5, which means that 90% of the reflections were measured at least 4.5 times. A combination of phi and omega scans with a frame width of one degree was used for data collection. Data integration was done with Denzo. Scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.297104E-1 _diffrn_orient_matrix_ub_12 0.643002E-1 _diffrn_orient_matrix_ub_13 -0.836445E-1 _diffrn_orient_matrix_ub_21 -0.785533E-1 _diffrn_orient_matrix_ub_22 -0.456899E-1 _diffrn_orient_matrix_ub_23 -0.72212E-2 _diffrn_orient_matrix_ub_31 -0.265986E-1 _diffrn_orient_matrix_ub_32 0.405648E-1 _diffrn_orient_matrix_ub_33 0.326819E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 27382 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 3031 _reflns_number_gt 2261 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The structure is a Li dimer which contains a crystallograpic inversion center. The thienyl ring is disordered by rotation about the C(1)-C(2) bond. This was initially evident in the U values for S(1) and C(3) of 0.095 and 0.009 Ang.^2^, respectively. This disorder was modeled with a second orientation of the ring, with atom C(2) common to both rings. The major orientation consists of atoms S(1), C(2), C(3), C(4) and C(5) with an occupancy factor of 0.599(4). The minor orientation contains S(1A), C(2), C(3A), C(5A) and C(4A) with an occupancy factor of 0.401(4). It was necessary to introduce restraints into the refinement of this disordered model. The DFIX restraint of 1.70(1) Ang. was used for all S-C bond lengths. SADI restraints were used for the C-C bonds with the following pairs of bond lengths restrained to be equal: C(2)-C(3A) and C(2)-C(3), C(3)-C(4) and C(3A)-C(5A), C(4)-C(5) and C(4A)-C(5A). The FLAT restraint was used to maintain the planarity of the minor ring orientation. Atoms C(3) and C(3A) were kept isotropic, while the rest of the atoms in the rings were refined anisotropically. The THF ligand is also disordered, with two positions for one of its atoms: C(14) and C(14A). The occupancy factor for C(14) was chosen such that the refined U(iso) value for this atom is comparable to those U(iso) values of the adjacent atoms, C(13) and C(15). As a result, the occupancy factor was fixed at 0.7 for C(14) and 0.3 for C(14A). For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded atom). The torsion angle, which defines the orientation of each methyl group about the C-C bond, was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 *Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+0.4112P] 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_number_reflns 3031 _refine_ls_number_parameters 221 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_gt 0.1249 _refine_ls_wR_factor_all 0.1361 _refine_ls_goodness_of_fit_gt 1.118 _refine_ls_goodness_of_fit_all 1.04 _refine_ls_restrained_S_all 1.05 _refine_ls_restrained_S_gt 1.131 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.189 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.036 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O O 0.2899(2) 0.20003(14) 0.00231(9) 0.0711(5) Uani 1 d . . N1 N 0.6498(2) 0.09802(14) 0.01962(8) 0.0413(4) Uani 1 d . . N2 N 0.5480(2) 0.08125(14) 0.13454(8) 0.0448(4) Uani 1 d . . C1 C 0.6536(2) 0.1236(2) 0.09578(9) 0.0377(4) Uani 1 d . . C2 C 0.7747(2) 0.1999(2) 0.13583(10) 0.0403(4) Uani 1 d D . S1 S 0.9391(2) 0.14446(15) 0.16475(9) 0.0565(4) Uani 0.599(4) d PD 1 C3 C 0.7696(12) 0.3217(8) 0.1582(6) 0.062(3) Uiso 0.599(4) d PD 1 H3 H 0.6826 0.3692 0.1520 0.075 Uiso 0.599(4) calc PR 1 C4 C 0.9060(15) 0.3678(16) 0.1910(11) 0.068(3) Uani 0.599(4) d PD 1 H4 H 0.9240 0.4509 0.2041 0.082 Uiso 0.599(4) calc PR 1 C5 C 1.0078(19) 0.2786(10) 0.2012(10) 0.060(3) Uani 0.599(4) d PD 1 H5 H 1.1046 0.2895 0.2256 0.072 Uiso 0.599(4) calc PR 1 S1A S 0.7591(4) 0.3457(3) 0.1519(2) 0.0568(8) Uani 0.401(4) d PD 2 C3A C 0.9122(14) 0.1561(16) 0.1661(10) 0.130(11) Uiso 0.401(4) d PD 2 H3A H 0.9433 0.0741 0.1616 0.156 Uiso 0.401(4) calc PR 2 C4A C 0.9260(16) 0.356(2) 0.2037(14) 0.062(5) Uani 0.401(4) d PD 2 H4A H 0.9636 0.428 0.2291 0.075 Uiso 0.401(4) calc PR 2 C5A C 0.999(3) 0.2492(17) 0.2044(17) 0.076(5) Uani 0.401(4) d PD 2 H5A H 1.097 0.2379 0.2276 0.091 Uiso 0.401(4) calc PR 2 C6 C 0.7413(2) 0.1692(2) -0.02867(10) 0.0517(5) Uani 1 d . . H6 H 0.8248 0.2050 0.00593 0.062 Uiso 1 calc R . C7 C 0.6531(3) 0.2715(3) -0.0689(2) 0.1191(13) Uani 1 d . . H7A H 0.7141 0.3165 -0.1026 0.179 Uiso 1 calc R . H7B H 0.620 0.3268 -0.0295 0.179 Uiso 1 calc R . H7C H 0.5677 0.2377 -0.1007 0.179 Uiso 1 calc R . C8 C 0.8021(4) 0.0872(3) -0.0875(2) 0.1103(12) Uani 1 d . . H8A H 0.861 0.1355 -0.1209 0.165 Uiso 1 calc R . H8B H 0.7212 0.0479 -0.1199 0.165 Uiso 1 calc R . H8C H 0.864 0.0247 -0.0602 0.165 Uiso 1 calc R . C9 C 0.5569(2) 0.0905(2) 0.21984(10) 0.0489(5) Uani 1 d . . H9 H 0.6251 0.1585 0.23752 0.059 Uiso 1 calc R . C10 C 0.4067(3) 0.1185(2) 0.24398(12) 0.0642(6) Uani 1 d . . H10A H 0.4132 0.1282 0.3009 0.096 Uiso 1 calc R . H10B H 0.3397 0.0514 0.2280 0.096 Uiso 1 calc R . H10C H 0.3698 0.1941 0.2187 0.096 Uiso 1 calc R . C11 C 0.6144(3) -0.0261(2) 0.25713(13) 0.0825(8) Uani 1 d . . H11A H 0.614 -0.0203 0.3140 0.124 Uiso 1 calc R . H11B H 0.7148 -0.0399 0.2444 0.124 Uiso 1 calc R . H11C H 0.5519 -0.0941 0.2373 0.124 Uiso 1 calc R . C12 C 0.1992(3) 0.2045(3) -0.0694(2) 0.0886(9) Uani 1 d . . H12A H 0.1212 0.1420 -0.0701 0.106 Uiso 1 calc R . H12B H 0.2577 0.1886 -0.1136 0.106 Uiso 1 calc R . C13 C 0.1341(4) 0.3271(3) -0.0765(2) 0.0925(9) Uani 1 d . . H13A H 0.1870 0.3788 -0.1115 0.111 Uiso 0.7 calc PR 1 H13B H 0.0297 0.3225 -0.0977 0.111 Uiso 0.7 calc PR 1 H13C H 0.0314 0.3267 -0.0636 0.111 Uiso 0.3 calc PR 2 H13D H 0.1372 0.3604 -0.1298 0.111 Uiso 0.3 calc PR 2 C14 C 0.1484(6) 0.3756(5) 0.0018(3) 0.0860(13) Uani 0.7 d P 1 H14A H 0.0617 0.3551 0.0291 0.103 Uiso 0.7 calc PR 1 H14B H 0.1605 0.4653 0.0013 0.103 Uiso 0.7 calc PR 1 C14A C 0.2335(13) 0.3991(9) -0.0162(8) 0.090(3) Uani 0.3 d P 2 H14C H 0.3158 0.4364 -0.0407 0.108 Uiso 0.3 calc PR 2 H14D H 0.1778 0.4644 0.0072 0.108 Uiso 0.3 calc PR 2 C15 C 0.2857(3) 0.3136(2) 0.0407(2) 0.0886(9) Uani 1 d . . H15A H 0.3742 0.3624 0.0336 0.106 Uiso 0.7 calc PR 1 H15B H 0.2791 0.3023 0.0974 0.106 Uiso 0.7 calc PR 1 H15C H 0.2196 0.3095 0.0827 0.106 Uiso 0.3 calc PR 2 H15D H 0.3849 0.3367 0.0644 0.106 Uiso 0.3 calc PR 2 Li Li 0.4165(3) 0.0640(3) 0.0337(2) 0.0522(8) Uani 1 d . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O 0.0712(10) 0.0612(10) 0.0758(10) -0.0172(8) -0.0167(8) 0.0169(8) N1 0.0422(8) 0.0466(9) 0.0348(8) -0.0032(6) 0.0022(6) -0.0070(7) N2 0.0479(9) 0.0513(10) 0.0348(8) -0.0020(7) 0.0017(7) -0.0102(7) C1 0.0376(9) 0.0360(9) 0.0382(9) 0.0006(7) -0.0024(7) -0.0001(8) C2 0.0409(10) 0.0444(11) 0.0348(9) -0.0013(7) 0.0007(7) -0.0019(8) S1 0.0423(6) 0.0599(7) 0.0637(7) -0.0034(4) -0.0120(4) 0.0037(5) C4 0.093(5) 0.054(4) 0.054(6) -0.010(4) -0.004(3) -0.021(4) C5 0.048(4) 0.080(5) 0.049(4) -0.005(4) -0.003(3) -0.024(4) S1A 0.0603(13) 0.0376(12) 0.0715(14) -0.0168(10) 0.0022(8) -0.0075(11) C4A 0.066(8) 0.083(13) 0.037(6) -0.022(7) 0.000(5) -0.035(7) C5A 0.039(6) 0.124(12) 0.061(7) 0.013(9) -0.010(4) -0.024(8) C6 0.0500(11) 0.0677(14) 0.0372(10) -0.0018(9) 0.0032(8) -0.0190(10) C7 0.089(2) 0.151(3) 0.118(2) 0.091(2) 0.010(2) -0.002(2) C8 0.114(2) 0.136(3) 0.092(2) -0.052(2) 0.065(2) -0.067(2) C9 0.0604(12) 0.0515(12) 0.0347(10) -0.0015(8) 0.0037(8) -0.0119(9) C10 0.0714(15) 0.0735(15) 0.0495(12) -0.0093(11) 0.0150(10) -0.0125(12) C11 0.113(2) 0.083(2) 0.0504(13) 0.0145(12) 0.0029(13) 0.019(2) C12 0.091(2) 0.083(2) 0.084(2) -0.0133(14) -0.0291(15) 0.013(2) C13 0.089(2) 0.074(2) 0.109(2) 0.014(2) -0.016(2) 0.006(2) C14 0.093(4) 0.065(3) 0.104(3) 0.008(2) 0.031(3) 0.028(3) C14A 0.083(8) 0.056(6) 0.130(10) 0.014(6) 0.002(7) 0.007(6) C15 0.113(2) 0.065(2) 0.084(2) -0.0220(14) -0.006(2) 0.014(2) Li 0.048(2) 0.054(2) 0.054(2) -0.0077(15) -0.0006(14) 0.0009(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O C15 1.413(3) . ? O C12 1.415(3) . ? O Li 1.933(4) . ? N1 C1 1.336(2) . ? N1 C6 1.465(2) . ? N1 Li 2.063(4) 3_655 ? N1 Li 2.210(4) . ? N2 C1 1.316(2) . ? N2 C9 1.464(2) . ? N2 Li 2.015(3) . ? C1 C2 1.500(2) . ? C1 Li 2.412(3) . ? C2 C3 1.392(9) . ? C2 C3A 1.398(11) . ? C2 S1A 1.632(4) . ? C2 S1 1.654(2) . ? S1 C5 1.695(8) . ? C3 C4 1.411(12) . ? C3 H3 0.95 . ? C4 C5 1.351(8) . ? C4 H4 0.95 . ? C5 H5 0.95 . ? S1A C4A 1.693(10) . ? C3A C5A 1.415(14) . ? C3A H3A 0.95 . ? C4A C5A 1.351(9) . ? C4A H4A 0.95 . ? C5A H5A 0.95 . ? C6 C8 1.504(3) . ? C6 C7 1.509(4) . ? C6 H6 1 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C11 1.502(3) . ? C9 C10 1.511(3) . ? C9 H9 1 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C13 1.471(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.441(5) . ? C13 C14A 1.528(12) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C13 H13C 0.99 . ? C13 H13D 0.99 . ? C14 C15 1.524(5) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C14A C15 1.403(11) . ? C14A H14C 0.99 . ? C14A H14D 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C15 H15C 0.99 . ? C15 H15D 0.99 . ? Li N1 2.063(4) 3_655 ? Li Li 2.456(6) 3_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 C15 O C12 109.5(2) . . ? C15 O Li 126.5(2) . . ? C12 O Li 123.5(2) . . ? C1 N1 C6 119.01(14) . . ? C1 N1 Li 126.39(15) . 3_655 ? C6 N1 Li 111.51(14) . 3_655 ? C1 N1 Li 81.68(13) . . ? C6 N1 Li 140.38(15) . . ? Li N1 Li 70.08(15) 3_655 . ? C1 N2 C9 121.02(15) . . ? C1 N2 Li 90.25(14) . . ? C9 N2 Li 146.5(2) . . ? N2 C1 N1 118.44(15) . . ? N2 C1 C2 120.90(15) . . ? N1 C1 C2 120.66(15) . . ? N2 C1 Li 56.68(11) . . ? N1 C1 Li 65.08(12) . . ? C2 C1 Li 160.96(15) . . ? C3 C2 C1 128.2(5) . . ? C3A C2 C1 125.1(8) . . ? C3A C2 S1A 111.4(8) . . ? C1 C2 S1A 123.4(2) . . ? C3 C2 S1 109.0(5) . . ? C1 C2 S1 122.76(14) . . ? C2 S1 C5 94.8(6) . . ? C2 C3 C4 113.6(10) . . ? C2 C3 H3 123.2 . . ? C4 C3 H3 123.2 . . ? C5 C4 C3 111.4(14) . . ? C5 C4 H4 124.3 . . ? C3 C4 H4 124.3 . . ? C4 C5 S1 110.8(13) . . ? C4 C5 H5 124.6 . . ? S1 C5 H5 124.6 . . ? C2 S1A C4A 93.7(9) . . ? C2 C3A C5A 111.6(15) . . ? C2 C3A H3A 124.2 . . ? C5A C3A H3A 124.2 . . ? C5A C4A S1A 111.5(19) . . ? C5A C4A H4A 124.2 . . ? S1A C4A H4A 124.2 . . ? C4A C5A C3A 112(2) . . ? C4A C5A H5A 124.2 . . ? C3A C5A H5A 124.2 . . ? N1 C6 C8 109.7(2) . . ? N1 C6 C7 110.1(2) . . ? C8 C6 C7 110.8(2) . . ? N1 C6 H6 108.7 . . ? C8 C6 H6 108.7 . . ? C7 C6 H6 108.7 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C11 110.4(2) . . ? N2 C9 C10 109.4(2) . . ? C11 C9 C10 110.2(2) . . ? N2 C9 H9 108.9 . . ? C11 C9 H9 108.9 . . ? C10 C9 H9 108.9 . . ? 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 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O C12 C13 107.6(2) . . ? O C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? O C12 H12B 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C14 C13 C12 105.2(3) . . ? C12 C13 C14A 101.9(4) . . ? C14 C13 H13A 110.7 . . ? C12 C13 H13A 110.7 . . ? C14 C13 H13B 110.7 . . ? C12 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C12 C13 H13C 111.4 . . ? C14A C13 H13C 111.4 . . ? C12 C13 H13D 111.4 . . ? C14A C13 H13D 111.4 . . ? H13C C13 H13D 109.2 . . ? C13 C14 C15 103.7(3) . . ? C13 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? C13 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109 . . ? C15 C14A C13 105.4(7) . . ? C15 C14A H14C 110.7 . . ? C13 C14A H14C 110.7 . . ? C15 C14A H14D 110.7 . . ? C13 C14A H14D 110.7 . . ? H14C C14A H14D 108.8 . . ? C14A C15 O 106.7(5) . . ? O C15 C14 104.5(3) . . ? O C15 H15A 110.9 . . ? C14 C15 H15A 110.9 . . ? O C15 H15B 110.9 . . ? C14 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? C14A C15 H15C 110.4 . . ? O C15 H15C 110.4 . . ? C14A C15 H15D 110.4 . . ? O C15 H15D 110.4 . . ? H15C C15 H15D 108.6 . . ? O Li N2 117.2(2) . . ? O Li N1 113.6(2) . 3_655 ? N2 Li N1 125.9(2) . 3_655 ? O Li N1 113.5(2) . . ? N2 Li N1 65.06(11) . . ? N1 Li N1 109.92(15) 3_655 . ? O Li C1 113.7(2) . . ? N2 Li C1 33.07(8) . . ? N1 Li C1 129.9(2) 3_655 . ? N1 Li C1 33.24(7) . . ? O Li Li 134.0(2) . 3_655 ? N2 Li Li 96.5(2) . 3_655 ? N1 Li Li 57.78(14) 3_655 3_655 ? N1 Li Li 52.13(12) . 3_655 ? C1 Li Li 77.6(2) . 3_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N2 C1 N1 170.9(2) . . . . ? Li N2 C1 N1 -21.7(2) . . . . ? C9 N2 C1 C2 -9.7(3) . . . . ? Li N2 C1 C2 157.7(2) . . . . ? C9 N2 C1 Li -167.4(2) . . . . ? Li N2 C1 Li 0 . . . . ? C6 N1 C1 N2 163.9(2) . . . . ? Li N1 C1 N2 -37.7(3) 3_655 . . . ? Li N1 C1 N2 19.9(2) . . . . ? C6 N1 C1 C2 -15.4(2) . . . . ? Li N1 C1 C2 142.9(2) 3_655 . . . ? Li N1 C1 C2 -159.4(2) . . . . ? C6 N1 C1 Li 144.0(2) . . . . ? Li N1 C1 Li -57.6(2) 3_655 . . . ? Li N1 C1 Li 0 . . . . ? N2 C1 C2 C3 -75.7(6) . . . . ? N1 C1 C2 C3 103.6(6) . . . . ? Li C1 C2 C3 1.1(8) . . . . ? N2 C1 C2 C3A 96.3(9) . . . . ? N1 C1 C2 C3A -84.4(9) . . . . ? Li C1 C2 C3A 173.1(9) . . . . ? N2 C1 C2 S1A -81.6(3) . . . . ? N1 C1 C2 S1A 97.7(3) . . . . ? Li C1 C2 S1A -4.8(5) . . . . ? N2 C1 C2 S1 100.9(2) . . . . ? N1 C1 C2 S1 -79.8(2) . . . . ? Li C1 C2 S1 177.7(4) . . . . ? C3 C2 S1 C5 -3.2(8) . . . . ? C3A C2 S1 C5 -57(10) . . . . ? C1 C2 S1 C5 179.6(7) . . . . ? S1A C2 S1 C5 1.8(7) . . . . ? C3A C2 C3 C4 10.1(14) . . . . ? C1 C2 C3 C4 -176.7(10) . . . . ? S1A C2 C3 C4 -130(6) . . . . ? S1 C2 C3 C4 6.3(12) . . . . ? C2 C3 C4 C5 -6.9(18) . . . . ? C3 C4 C5 S1 4.3(17) . . . . ? C2 S1 C5 C4 -0.6(12) . . . . ? C3 C2 S1A C4A 38(5) . . . . ? C3A C2 S1A C4A -3.3(12) . . . . ? C1 C2 S1A C4A 174.9(9) . . . . ? S1 C2 S1A C4A -7.4(9) . . . . ? C3 C2 C3A C5A -3.1(18) . . . . ? C1 C2 C3A C5A -176.5(14) . . . . ? S1A C2 C3A C5A 1.6(18) . . . . ? S1 C2 C3A C5A 124(11) . . . . ? C2 S1A C4A C5A 4.2(18) . . . . ? S1A C4A C5A C3A -4(3) . . . . ? C2 C3A C5A C4A 2(3) . . . . ? C1 N1 C6 C8 141.9(2) . . . . ? Li N1 C6 C8 -19.5(2) 3_655 . . . ? Li N1 C6 C8 -103.9(3) . . . . ? C1 N1 C6 C7 -95.9(2) . . . . ? Li N1 C6 C7 102.7(2) 3_655 . . . ? Li N1 C6 C7 18.3(3) . . . . ? C1 N2 C9 C11 -96.6(2) . . . . ? Li N2 C9 C11 106.7(3) . . . . ? C1 N2 C9 C10 141.9(2) . . . . ? Li N2 C9 C10 -14.8(4) . . . . ? C15 O C12 C13 -0.1(3) . . . . ? Li O C12 C13 -173.2(2) . . . . ? O C12 C13 C14 -19.2(4) . . . . ? O C12 C13 C14A 17.1(6) . . . . ? C12 C13 C14 C15 29.4(4) . . . . ? C14A C13 C14 C15 -59.8(7) . . . . ? C14 C13 C14A C15 71.1(9) . . . . ? C12 C13 C14A C15 -28.4(9) . . . . ? C13 C14A C15 O 29.3(9) . . . . ? C13 C14A C15 C14 -62.5(8) . . . . ? C12 O C15 C14A -18.9(6) . . . . ? Li O C15 C14A 153.9(6) . . . . ? C12 O C15 C14 18.3(4) . . . . ? Li O C15 C14 -168.9(3) . . . . ? C13 C14 C15 C14A 68.9(9) . . . . ? C13 C14 C15 O -29.7(4) . . . . ? C15 O Li N2 3.7(3) . . . . ? C12 O Li N2 175.5(2) . . . . ? C15 O Li N1 164.2(2) . . . 3_655 ? C12 O Li N1 -23.9(3) . . . 3_655 ? C15 O Li N1 -69.2(3) . . . . ? C12 O Li N1 102.6(2) . . . . ? C15 O Li C1 -32.9(3) . . . . ? C12 O Li C1 139.0(2) . . . . ? C15 O Li Li -128.5(3) . . . 3_655 ? C12 O Li Li 43.3(4) . . . 3_655 ? C1 N2 Li O -92.3(2) . . . . ? C9 N2 Li O 67.9(4) . . . . ? C1 N2 Li N1 109.8(2) . . . 3_655 ? C9 N2 Li N1 -90.0(3) . . . 3_655 ? C1 N2 Li N1 12.50(11) . . . . ? C9 N2 Li N1 172.7(3) . . . . ? C1 N2 Li C1 0 . . . . ? C9 N2 Li C1 160.2(3) . . . . ? C1 N2 Li Li 55.3(2) . . . 3_655 ? C9 N2 Li Li -144.5(2) . . . 3_655 ? C1 N1 Li O 97.8(2) . . . . ? C6 N1 Li O -28.4(3) . . . . ? Li N1 Li O -128.5(2) 3_655 . . . ? C1 N1 Li N2 -12.44(11) . . . . ? C6 N1 Li N2 -138.7(2) . . . . ? Li N1 Li N2 121.2(2) 3_655 . . . ? C1 N1 Li N1 -133.7(2) . . . 3_655 ? C6 N1 Li N1 100.0(2) . . . 3_655 ? Li N1 Li N1 0 3_655 . . 3_655 ? C1 N1 Li C1 0 . . . . ? C6 N1 Li C1 -126.3(2) . . . . ? Li N1 Li C1 133.7(2) 3_655 . . . ? C1 N1 Li Li -133.7(2) . . . 3_655 ? C6 N1 Li Li 100.0(2) . . . 3_655 ? Li N1 Li Li 0 3_655 . . 3_655 ? N2 C1 Li O 103.8(2) . . . . ? N1 C1 Li O -97.2(2) . . . . ? C2 C1 Li O 15.0(5) . . . . ? N2 C1 Li N2 0 . . . . ? N1 C1 Li N2 159.0(2) . . . . ? C2 C1 Li N2 -88.8(4) . . . . ? N2 C1 Li N1 -96.7(2) . . . 3_655 ? N1 C1 Li N1 62.3(2) . . . 3_655 ? C2 C1 Li N1 174.5(3) . . . 3_655 ? N2 C1 Li N1 -159.0(2) . . . . ? N1 C1 Li N1 0 . . . . ? C2 C1 Li N1 112.2(4) . . . . ? N2 C1 Li Li -123.3(2) . . . 3_655 ? N1 C1 Li Li 35.77(15) . . . 3_655 ? C2 C1 Li Li 148.0(4) . . . 3_655 ? #END OF CIF # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-04-18 at 14:13:51 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : shelx dreduc import struct data_Chisholm1328 _database_code_depnum_ccdc_archive 'CCDC 637926' _audit_creation_date 2005-04-18T14:13:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1328' _chemical_formula_moiety 'C20 H40 Mo2 N4 O4' _chemical_formula_sum 'C20 H40 Mo2 N4 O4' _chemical_formula_weight 592.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3023(10) _cell_length_b 9.0596(10) _cell_length_c 9.5252(10) _cell_angle_alpha 68.840(4) _cell_angle_beta 77.080(4) _cell_angle_gamma 65.805(5) _cell_volume 607.03(12) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2756 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_special_details ;The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.5, which means that 90% of the reflections were measured at least 3.5 times. A combination of phi and omega scans with a frame width of 1 degree was used. The Mo dimer contains a crystallographic inversion center. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.101108 _diffrn_orient_matrix_ub_12 0.179546E-1 _diffrn_orient_matrix_ub_13 -0.748511E-1 _diffrn_orient_matrix_ub_21 -0.206694E-1 _diffrn_orient_matrix_ub_22 -0.606251E-1 _diffrn_orient_matrix_ub_23 -0.596446E-1 _diffrn_orient_matrix_ub_31 -0.832203E-1 _diffrn_orient_matrix_ub_32 0.110115 _diffrn_orient_matrix_ub_33 -0.601158E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 17872 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2771 _reflns_number_gt 2673 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+0.4632P] 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_number_reflns 2771 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.018 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0432 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.345 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 Mo1 Mo 0.474197(16) 0.087368(16) 0.894156(13) 0.01039(5) Uani 1 1 d . . . O1 O 0.26733(14) 0.27210(14) 0.98836(12) 0.0139(2) Uani 1 1 d . . . O2 O 0.67581(14) -0.08160(14) 0.78439(12) 0.0143(2) Uani 1 1 d . . . N1 N 0.28619(17) -0.00366(16) 0.86615(14) 0.0120(3) Uani 1 1 d . . . N2 N 0.65974(17) 0.19339(16) 0.89850(14) 0.0122(3) Uani 1 1 d . . . C1 C 0.25547(19) -0.13395(19) 0.97694(17) 0.0123(3) Uani 1 1 d . . . C2 C 0.1310(2) -0.2108(2) 0.96334(18) 0.0161(3) Uani 1 1 d . . . H2A H 0.0817 -0.1512 0.8651 0.024 Uiso 1 1 calc R . . H2B H 0.0345 -0.2 1.0443 0.024 Uiso 1 1 calc R . . H2C H 0.1962 -0.3312 0.9718 0.024 Uiso 1 1 calc R . . C3 C 0.1973(2) 0.0697(2) 0.72529(17) 0.0149(3) Uani 1 1 d . . . H3 H 0.071 0.0779 0.7518 0.018 Uiso 1 1 calc R . . C4 C 0.2856(3) -0.0394(2) 0.61924(19) 0.0242(4) Uani 1 1 d . . . H4A H 0.2826 -0.1536 0.6706 0.036 Uiso 1 1 calc R . . H4B H 0.4089 -0.0467 0.5908 0.036 Uiso 1 1 calc R . . H4C H 0.2218 0.012 0.5282 0.036 Uiso 1 1 calc R . . C5 C 0.2008(2) 0.2483(2) 0.6462(2) 0.0220(4) Uani 1 1 d . . . H5A H 0.144 0.3177 0.7148 0.033 Uiso 1 1 calc R . . H5B H 0.1367 0.3001 0.5553 0.033 Uiso 1 1 calc R . . H5C H 0.3239 0.2418 0.6176 0.033 Uiso 1 1 calc R . . C6 C 0.6898(2) 0.3338(2) 0.76990(18) 0.0148(3) Uani 1 1 d . . . H6 H 0.8059 0.3383 0.7774 0.018 Uiso 1 1 calc R . . C7 C 0.6999(3) 0.3007(2) 0.62142(19) 0.0233(4) Uani 1 1 d . . . H7A H 0.7941 0.1914 0.6209 0.035 Uiso 1 1 calc R . . H7B H 0.7257 0.3915 0.5368 0.035 Uiso 1 1 calc R . . H7C H 0.5863 0.2981 0.6113 0.035 Uiso 1 1 calc R . . C8 C 0.5443(2) 0.5036(2) 0.7741(2) 0.0255(4) Uani 1 1 d . . . H8A H 0.54 0.5224 0.8702 0.038 Uiso 1 1 calc R . . H8B H 0.4298 0.5023 0.7647 0.038 Uiso 1 1 calc R . . H8C H 0.5696 0.5952 0.6903 0.038 Uiso 1 1 calc R . . C9 C 0.2372(2) 0.2271(2) 1.13159(18) 0.0139(3) Uani 1 1 d . . . C10 C 0.0943(2) 0.3497(2) 1.20642(19) 0.0187(3) Uani 1 1 d . . . H10A H 0.0382 0.456 1.1291 0.028 Uiso 1 1 calc R . . H10B H 0.1466 0.3726 1.2752 0.028 Uiso 1 1 calc R . . H10C H 0.0051 0.3004 1.2636 0.028 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 Mo1 0.01107(7) 0.01143(7) 0.00878(7) -0.00112(5) -0.00241(5) -0.00507(5) O1 0.0139(5) 0.0140(5) 0.0136(5) -0.0033(4) -0.0022(4) -0.0051(4) O2 0.0149(5) 0.0158(5) 0.0121(5) -0.0040(4) -0.0011(4) -0.0056(4) N1 0.0119(6) 0.0141(6) 0.0105(6) -0.0025(5) -0.0031(5) -0.0052(5) N2 0.0126(6) 0.0126(6) 0.0114(6) -0.0016(5) -0.0014(5) -0.0062(5) C1 0.0100(7) 0.0133(7) 0.0146(7) -0.0068(6) 0.0000(6) -0.0035(6) C2 0.0172(8) 0.0196(8) 0.0157(8) -0.0053(6) -0.0018(6) -0.0104(6) C3 0.0151(7) 0.0170(8) 0.0127(7) -0.0032(6) -0.0050(6) -0.0051(6) C4 0.0326(10) 0.0249(9) 0.0150(8) -0.0075(7) -0.0042(7) -0.0080(8) C5 0.0288(9) 0.0188(8) 0.0176(8) 0.0005(7) -0.0110(7) -0.0085(7) C6 0.0157(8) 0.0141(7) 0.0143(7) -0.0015(6) -0.0011(6) -0.0075(6) C7 0.0318(10) 0.0263(9) 0.0139(8) -0.0020(7) -0.0016(7) -0.0161(8) C8 0.0247(9) 0.0154(8) 0.0266(9) -0.0008(7) 0.0010(7) -0.0043(7) C9 0.0129(7) 0.0162(7) 0.0163(8) -0.0060(6) -0.0017(6) -0.0077(6) C10 0.0204(8) 0.0184(8) 0.0182(8) -0.0079(7) -0.0017(6) -0.0060(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Mo1 Mo1 2.0691(2) 2_657 ? Mo1 O2 2.1239(11) . ? Mo1 N2 2.1371(13) . ? Mo1 N1 2.1419(13) . ? Mo1 O1 2.1435(11) . ? O1 C9 1.2726(19) . ? O2 C9 1.2711(19) 2_657 ? N1 C1 1.341(2) . ? N1 C3 1.4775(19) . ? N2 C1 1.340(2) 2_657 ? N2 C6 1.4763(19) . ? C1 C2 1.512(2) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 C4 1.527(2) . ? C3 C5 1.528(2) . ? C3 H3 1 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C8 1.526(2) . ? C6 C7 1.526(2) . ? C6 H6 1 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 O2 1.2711(19) 2_657 ? C9 C10 1.504(2) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? 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 Mo1 Mo1 O2 92.41(3) 2_657 . ? Mo1 Mo1 N2 93.03(4) 2_657 . ? O2 Mo1 N2 89.66(5) . . ? Mo1 Mo1 N1 92.72(3) 2_657 . ? O2 Mo1 N1 89.17(5) . . ? N2 Mo1 N1 174.17(5) . . ? Mo1 Mo1 O1 91.95(3) 2_657 . ? O2 Mo1 O1 175.64(4) . . ? N2 Mo1 O1 89.89(4) . . ? N1 Mo1 O1 90.85(4) . . ? C9 O1 Mo1 116.20(10) . . ? C9 O2 Mo1 116.82(10) 2_657 . ? C1 N1 C3 120.24(13) . . ? C1 N1 Mo1 118.66(10) . . ? C3 N1 Mo1 121.05(10) . . ? C1 N2 C6 120.18(13) 2_657 . ? C1 N2 Mo1 118.63(10) 2_657 . ? C6 N2 Mo1 121.15(10) . . ? N2 C1 N1 116.86(13) 2_657 . ? N2 C1 C2 121.12(14) 2_657 . ? N1 C1 C2 122.03(14) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 111.85(13) . . ? N1 C3 C5 109.03(13) . . ? C4 C3 C5 109.90(14) . . ? N1 C3 H3 108.7 . . ? C4 C3 H3 108.7 . . ? C5 C3 H3 108.7 . . ? 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 . . ? N2 C6 C8 110.93(13) . . ? N2 C6 C7 109.89(13) . . ? C8 C6 C7 110.74(15) . . ? N2 C6 H6 108.4 . . ? C8 C6 H6 108.4 . . ? C7 C6 H6 108.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 O1 122.62(14) 2_657 . ? O2 C9 C10 117.95(14) 2_657 . ? O1 C9 C10 119.43(14) . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo1 Mo1 O1 C9 -0.37(10) 2_657 . . . ? N2 Mo1 O1 C9 -93.40(11) . . . . ? N1 Mo1 O1 C9 92.38(11) . . . . ? Mo1 Mo1 O2 C9 0.17(10) 2_657 . . 2_657 ? N2 Mo1 O2 C9 93.19(11) . . . 2_657 ? N1 Mo1 O2 C9 -92.52(11) . . . 2_657 ? Mo1 Mo1 N1 C1 -0.63(11) 2_657 . . . ? O2 Mo1 N1 C1 91.74(11) . . . . ? O1 Mo1 N1 C1 -92.62(11) . . . . ? Mo1 Mo1 N1 C3 -177.97(11) 2_657 . . . ? O2 Mo1 N1 C3 -85.60(11) . . . . ? O1 Mo1 N1 C3 90.04(11) . . . . ? Mo1 Mo1 N2 C1 -2.89(11) 2_657 . . 2_657 ? O2 Mo1 N2 C1 -95.28(11) . . . 2_657 ? O1 Mo1 N2 C1 89.06(11) . . . 2_657 ? Mo1 Mo1 N2 C6 179.45(11) 2_657 . . . ? O2 Mo1 N2 C6 87.05(11) . . . . ? O1 Mo1 N2 C6 -88.61(11) . . . . ? C3 N1 C1 N2 -179.76(13) . . . 2_657 ? Mo1 N1 C1 N2 2.88(18) . . . 2_657 ? C3 N1 C1 C2 0.1(2) . . . . ? Mo1 N1 C1 C2 -177.26(11) . . . . ? C1 N1 C3 C4 -78.37(18) . . . . ? Mo1 N1 C3 C4 98.93(14) . . . . ? C1 N1 C3 C5 159.89(14) . . . . ? Mo1 N1 C3 C5 -22.81(17) . . . . ? C1 N2 C6 C8 -97.55(17) 2_657 . . . ? Mo1 N2 C6 C8 80.08(15) . . . . ? C1 N2 C6 C7 139.66(15) 2_657 . . . ? Mo1 N2 C6 C7 -42.71(16) . . . . ? Mo1 O1 C9 O2 0.32(19) . . . 2_657 ? Mo1 O1 C9 C10 179.85(10) . . . . ? # END OF CIF data_Chisholm1144 _database_code_depnum_ccdc_archive 'CCDC 637927' _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H68 Mo2 N4 O7' _chemical_formula_weight 980.92 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.311(1) _cell_length_b 11.735(1) _cell_length_c 12.973(1) _cell_angle_alpha 66.083(3) _cell_angle_beta 74.895(3) _cell_angle_gamma 68.780(5) _cell_volume 1197.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5447 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method ? _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.874 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ;The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.1, which means that 90% of the reflections were measured at least 3.1 times. A combination of phi and omega scans with a frame width of 1 degree was used. The Mo dimer occupies an inversion center. There is a disordered molecule of THF in a general position and another one located about an inversion center. The THF molecule in the general position was modeled with atoms O(3A), C(24A), C(25), C(26A) and C(27A) for one orientation, and with atoms O(3B), C(24B), C(25), C(26B) and C(27B) for the second orientation. SADI restraints were used for this modeling and both molecules were refined only isotropically. Atom C(25) is common to both orientations. Modeling of the THF molecule disordered about an inversion center was too difficult to sort out. Instead of obtaining a reasonable looking THF molecule, this region was modeled with the following isotropic atoms: C(18), C(19), C(20), O(4A), C(19A), C(20A), C(21A) and C(22A). ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32426 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 5452 _reflns_number_gt 5005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;For each methyl group of the Mo dimer, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded atom). The torsion angle, which defines the orientation of the methyl group about the C-C bond, was refined. The remaining hydrogen atoms on the Mo dimer were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.8717P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5452 _refine_ls_number_parameters 273 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_all 0.0818 _refine_ls_wR_factor_ref 0.0797 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.071 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.03742(2) 0.03165(2) 0.049653(14) 0.02551(7) Uani 1 d . . O1 O 0.2655(2) 0.00280(15) -0.03929(14) 0.0344(3) Uani 1 d . . O2 O 0.1871(2) -0.06394(15) -0.14773(13) 0.0346(3) Uani 1 d . . N1 N 0.1084(2) -0.1584(2) 0.16965(15) 0.0280(4) Uani 1 d . . N2 N 0.0184(2) -0.2282(2) 0.06296(15) 0.0278(4) Uani 1 d . . C1 C 0.2903(3) -0.0381(2) -0.1208(2) 0.0375(5) Uani 1 d . . C2 C 0.4491(3) -0.0542(3) -0.1897(3) 0.0574(7) Uani 1 d . . H2A H 0.5285 -0.0927 -0.1386 0.086 Uiso 1 calc R . H2B H 0.4582 0.0311 -0.2434 0.086 Uiso 1 calc R . H2C H 0.4640 -0.1116 -0.2317 0.086 Uiso 1 calc R . C3 C 0.0827(2) -0.2555(2) 0.1546(2) 0.0282(4) Uani 1 d . . C4 C 0.1213(3) -0.3866(2) 0.2365(2) 0.0322(4) Uani 1 d . . C5 C 0.1506(3) -0.4948(2) 0.3050(2) 0.0339(5) Uani 1 d . . C6 C 0.1825(3) -0.6239(2) 0.3879(2) 0.0319(4) Uani 1 d . . C7 C 0.2228(3) -0.7323(2) 0.3548(2) 0.0403(5) Uani 1 d . . H7 H 0.2313 -0.7206 0.2768 0.048 Uiso 1 calc R . C8 C 0.2502(3) -0.8560(2) 0.4348(2) 0.0493(6) Uani 1 d . . H8 H 0.2784 -0.9292 0.4116 0.059 Uiso 1 calc R . C9 C 0.2371(3) -0.8742(2) 0.5490(2) 0.0492(6) Uani 1 d . . H9 H 0.2557 -0.9596 0.6040 0.059 Uiso 1 calc R . C10 C 0.1970(3) -0.7682(3) 0.5824(2) 0.0513(7) Uani 1 d . . H10 H 0.1873 -0.7807 0.6607 0.062 Uiso 1 calc R . C11 C 0.1707(3) -0.6433(2) 0.5027(2) 0.0425(6) Uani 1 d . . H11 H 0.1445 -0.5708 0.5264 0.051 Uiso 1 calc R . C12 C 0.1961(3) -0.1899(2) 0.2624(2) 0.0374(5) Uani 1 d . . H12 H 0.1619 -0.2587 0.3310 0.045 Uiso 1 calc R . C13 C 0.3700(3) -0.2408(3) 0.2283(3) 0.0555(7) Uani 1 d . . H13A H 0.4259 -0.2571 0.2895 0.083 Uiso 1 calc R . H13B H 0.4037 -0.1761 0.1587 0.083 Uiso 1 calc R . H13C H 0.3923 -0.3222 0.2145 0.083 Uiso 1 calc R . C14 C 0.1586(4) -0.0681(3) 0.2915(2) 0.0491(6) Uani 1 d . . H14A H 0.2097 -0.0894 0.3569 0.074 Uiso 1 calc R . H14B H 0.0459 -0.0349 0.3102 0.074 Uiso 1 calc R . H14C H 0.1962 -0.0014 0.2260 0.074 Uiso 1 calc R . C15 C -0.0296(3) -0.3302(2) 0.0544(2) 0.0368(5) Uani 1 d . . H15 H 0.0484 -0.4162 0.0855 0.044 Uiso 1 calc R . C16 C -0.1875(4) -0.3358(3) 0.1236(3) 0.0592(8) Uani 1 d . . H16A H -0.2182 -0.4031 0.1158 0.089 Uiso 1 calc R . H16B H -0.2646 -0.2511 0.0957 0.089 Uiso 1 calc R . H16C H -0.1816 -0.3566 0.2038 0.089 Uiso 1 calc R . C17 C -0.0311(4) -0.3039(3) -0.0703(2) 0.0554(8) Uani 1 d . . H17A H -0.0498 -0.3772 -0.0774 0.083 Uiso 1 calc R . H17B H 0.0695 -0.2935 -0.1137 0.083 Uiso 1 calc R . H17C H -0.1138 -0.2240 -0.1001 0.083 Uiso 1 calc R . C18 C 0.4572(26) 0.6068(22) -0.1014(19) 0.070(5) Uiso 0.25 d P . C19 C 0.3490(17) 0.5098(15) -0.0330(14) 0.061(3) Uiso 0.25 d P . C20 C 0.4419(33) 0.3972(25) 0.0222(21) 0.069(5) Uiso 0.25 d P . O3A O 0.6869(9) 0.4071(7) 0.4218(6) 0.114(3) Uiso 0.533(7) d PD 1 C24A C 0.5597(12) 0.3635(10) 0.4361(10) 0.105(3) Uiso 0.533(7) d PD 1 H24A H 0.5047 0.3515 0.5145 0.126 Uiso 0.533(7) calc PR 1 H24B H 0.4862 0.4296 0.3824 0.126 Uiso 0.533(7) calc PR 1 C26A C 0.7866(10) 0.2076(8) 0.3828(8) 0.077(2) Uiso 0.533(7) d PD 1 H26A H 0.8420 0.1387 0.4464 0.093 Uiso 0.533(7) calc PR 1 H26B H 0.8162 0.1803 0.3155 0.093 Uiso 0.533(7) calc PR 1 C27A C 0.8064(17) 0.3353(14) 0.3569(13) 0.136(5) Uiso 0.533(7) d PD 1 H27A H 0.9094 0.3232 0.3744 0.163 Uiso 0.533(7) calc PR 1 H27B H 0.8029 0.3857 0.2747 0.163 Uiso 0.533(7) calc PR 1 C25 C 0.6061(7) 0.2517(6) 0.4175(5) 0.121(2) Uiso 1 d D . H25A H 0.5531 0.2615 0.3561 0.145 Uiso 0.533(7) calc PR 1 H25B H 0.5760 0.1835 0.4873 0.145 Uiso 0.533(7) calc PR 1 H25C H 0.5218 0.2422 0.4824 0.145 Uiso 0.467(7) calc PR 2 H25D H 0.5787 0.2340 0.3578 0.145 Uiso 0.467(7) calc PR 2 O3B O 0.7248(6) 0.1702(5) 0.4488(5) 0.065(2) Uiso 0.467(7) d PD 2 C24B C 0.6114(14) 0.3954(11) 0.3697(12) 0.103(3) Uiso 0.467(7) d PD 2 H24C H 0.5365 0.4492 0.4140 0.123 Uiso 0.467(7) calc PR 2 H24D H 0.6009 0.4390 0.2877 0.123 Uiso 0.467(7) calc PR 2 C26B C 0.8493(11) 0.2267(10) 0.4016(9) 0.086(3) Uiso 0.467(7) d PD 2 H26C H 0.9360 0.1744 0.4475 0.104 Uiso 0.467(7) calc PR 2 H26D H 0.8873 0.2249 0.3234 0.104 Uiso 0.467(7) calc PR 2 C27B C 0.8076(11) 0.3440(9) 0.3988(10) 0.078(3) Uiso 0.467(7) d PD 2 H27C H 0.8715 0.3959 0.3375 0.093 Uiso 0.467(7) calc PR 2 H27D H 0.8118 0.3483 0.4726 0.093 Uiso 0.467(7) calc PR 2 O4A O 0.3989(14) 0.5020(11) -0.0780(10) 0.071(3) Uiso 0.25 d P . C19A C 0.4803(38) 0.5609(33) -0.0901(30) 0.117(11) Uiso 0.25 d P . C20A C 0.5008(32) 0.6070(26) -0.0004(21) 0.098(8) Uiso 0.25 d P . C21A C 0.4131(13) 0.5987(12) -0.0498(11) 0.094(3) Uiso 0.50 d P . C22A C 0.4253(20) 0.4320(17) 0.0342(14) 0.117(6) Uiso 0.50 d P . 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 Mo 0.03520(11) 0.01794(10) 0.02398(10) -0.00376(7) -0.00657(7) -0.01053(7) O1 0.0346(8) 0.0276(8) 0.0389(9) -0.0056(7) -0.0058(7) -0.0128(6) O2 0.0426(9) 0.0265(7) 0.0309(8) -0.0087(6) 0.0001(7) -0.0106(6) N1 0.0383(9) 0.0210(8) 0.0237(8) -0.0022(7) -0.0086(7) -0.0106(7) N2 0.0393(9) 0.0164(8) 0.0280(9) -0.0043(7) -0.0063(7) -0.0110(7) C1 0.0372(12) 0.0243(10) 0.0390(12) -0.0030(9) -0.0001(10) -0.0081(9) C2 0.0417(14) 0.054(2) 0.065(2) -0.0196(15) 0.0108(13) -0.0146(12) C3 0.0358(11) 0.0184(9) 0.0257(10) -0.0028(8) -0.0035(8) -0.0086(8) C4 0.0411(12) 0.0235(10) 0.0297(11) -0.0055(9) -0.0053(9) -0.0106(9) C5 0.0413(12) 0.0251(10) 0.0329(11) -0.0064(9) -0.0067(9) -0.0099(9) C6 0.0368(11) 0.0216(10) 0.0315(11) -0.0021(8) -0.0060(9) -0.0091(8) C7 0.0545(14) 0.0294(11) 0.0353(12) -0.0071(10) -0.0081(11) -0.0134(10) C8 0.066(2) 0.0239(11) 0.054(2) -0.0093(11) -0.0094(13) -0.0123(11) C9 0.060(2) 0.0246(11) 0.0431(14) 0.0056(10) -0.0072(12) -0.0098(11) C10 0.065(2) 0.0390(14) 0.0291(12) -0.0011(10) -0.0041(11) -0.0050(12) C11 0.0560(15) 0.0283(11) 0.0338(12) -0.0079(10) -0.0068(11) -0.0042(10) C12 0.0560(14) 0.0281(11) 0.0292(11) -0.0001(9) -0.0173(10) -0.0168(10) C13 0.051(2) 0.050(2) 0.066(2) -0.0137(14) -0.0289(14) -0.0074(13) C14 0.075(2) 0.0409(14) 0.0409(14) -0.0109(11) -0.0233(13) -0.0210(13) C15 0.0549(14) 0.0207(10) 0.0387(12) -0.0051(9) -0.0145(11) -0.0154(10) C16 0.068(2) 0.052(2) 0.070(2) -0.0159(15) -0.005(2) -0.0399(15) C17 0.097(2) 0.0358(13) 0.048(2) -0.0118(12) -0.024(2) -0.0281(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo Mo 2.0775(3) 2 ? Mo O1 2.115(2) . ? Mo N1 2.119(2) . ? Mo N2 2.126(2) 2 ? Mo O2 2.136(2) 2 ? O1 C1 1.268(3) . ? O2 C1 1.268(3) . ? O2 Mo 2.136(2) 2 ? N1 C3 1.340(3) . ? N1 C12 1.478(3) . ? N2 C3 1.341(3) . ? N2 C15 1.472(3) . ? N2 Mo 2.126(2) 2 ? C1 C2 1.505(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 C4 1.449(3) . ? C4 C5 1.199(3) . ? C5 C6 1.435(3) . ? C6 C11 1.393(3) . ? C6 C7 1.399(3) . ? C7 C8 1.377(3) . ? C7 H7 0.95 . ? C8 C9 1.387(4) . ? C8 H8 0.95 . ? C9 C10 1.375(4) . ? C9 H9 0.95 . ? C10 C11 1.386(3) . ? C10 H10 0.95 . ? C11 H11 0.95 . ? C12 C13 1.521(4) . ? C12 C14 1.522(3) . ? C12 H12 1.00 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.518(4) . ? C15 C17 1.522(3) . ? C15 H15 1.00 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C21A 0.68(2) . ? C18 C22A 1.41(3) 2_665 ? C18 O4A 1.41(2) . ? C18 C20A 1.47(3) . ? C18 C20 1.54(3) 2_665 ? C18 C19 1.63(3) . ? C19 O4A 0.66(2) . ? C19 C22A 1.14(2) . ? C19 C21A 1.30(2) . ? C19 C20 1.32(3) . ? C19 C19A 1.45(4) . ? C19 C20A 1.57(3) 2_665 ? C20 C20A 0.53(3) 2_665 ? C20 O4A 1.41(3) . ? C20 C21A 1.50(3) 2_665 ? C20 C18 1.54(3) 2_665 ? C20 C19A 1.57(4) 2_665 ? C20 C19A 1.97(4) . ? O3A C24A 1.395(11) . ? O3A C27A 1.437(14) . ? C24A C25 1.327(10) . ? C24A H24A 0.99 . ? C24A H24B 0.99 . ? C26A C27A 1.467(15) . ? C26A C25 1.569(10) . ? C26A H26A 0.99 . ? C26A H26B 0.99 . ? C27A H27A 0.99 . ? C27A H27B 0.99 . ? C25 O3B 1.206(7) . ? C25 C24B 1.559(12) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C25 H25C 0.99 . ? C25 H25D 0.99 . ? O3B C26B 1.419(10) . ? C24B C27B 1.80(2) . ? C24B H24C 0.99 . ? C24B H24D 0.99 . ? C26B C27B 1.276(13) . ? C26B H26C 0.99 . ? C26B H26D 0.99 . ? C27B H27C 0.99 . ? C27B H27D 0.99 . ? O4A C19A 1.14(3) . ? O4A C21A 1.38(2) . ? O4A C22A 1.39(2) . ? O4A C20A 1.46(3) 2_665 ? C19A C21A 0.82(3) . ? C19A C22A 1.32(3) 2_665 ? C19A C20A 1.54(4) . ? C19A C20 1.57(4) 2_665 ? C19A C20A 1.81(4) 2_665 ? C19A C22A 1.82(4) . ? C20A C20 0.53(3) 2_665 ? C20A C22A 0.81(3) 2_665 ? C20A C21A 1.21(3) . ? C20A O4A 1.46(3) 2_665 ? C20A C19 1.57(3) 2_665 ? C20A C19A 1.81(4) 2_665 ? C21A C22A 1.46(2) 2_665 ? C21A C20 1.50(3) 2_665 ? C21A C22A 1.79(2) . ? C22A C20A 0.81(3) 2_665 ? C22A C19A 1.32(3) 2_665 ? C22A C18 1.41(3) 2_665 ? C22A C21A 1.46(2) 2_665 ? 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 Mo Mo O1 92.69(5) 2 . ? Mo Mo N1 93.03(5) 2 . ? O1 Mo N1 89.25(6) . . ? Mo Mo N2 93.05(5) 2 2 ? O1 Mo N2 88.64(6) . 2 ? N1 Mo N2 173.65(6) . 2 ? Mo Mo O2 91.39(5) 2 2 ? O1 Mo O2 175.90(6) . 2 ? N1 Mo O2 90.09(6) . 2 ? N2 Mo O2 91.59(6) 2 2 ? C1 O1 Mo 116.37(15) . . ? C1 O2 Mo 116.51(15) . 2 ? C3 N1 C12 118.9(2) . . ? C3 N1 Mo 117.86(14) . . ? C12 N1 Mo 123.03(13) . . ? C3 N2 C15 118.5(2) . . ? C3 N2 Mo 117.46(13) . 2 ? C15 N2 Mo 123.43(14) . 2 ? O2 C1 O1 123.0(2) . . ? O2 C1 C2 118.9(2) . . ? O1 C1 C2 118.0(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 N2 118.5(2) . . ? N1 C3 C4 120.7(2) . . ? N2 C3 C4 120.8(2) . . ? C5 C4 C3 178.9(2) . . ? C4 C5 C6 178.9(2) . . ? C11 C6 C7 118.9(2) . . ? C11 C6 C5 120.7(2) . . ? C7 C6 C5 120.4(2) . . ? C8 C7 C6 120.3(2) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.4(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.5(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 120.2(2) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? N1 C12 C13 111.0(2) . . ? N1 C12 C14 108.7(2) . . ? C13 C12 C14 110.8(2) . . ? N1 C12 H12 108.8 . . ? C13 C12 H12 108.8 . . ? C14 C12 H12 108.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 110.7(2) . . ? N2 C15 C17 109.1(2) . . ? C16 C15 C17 111.4(2) . . ? N2 C15 H15 108.5 . . ? C16 C15 H15 108.5 . . ? C17 C15 H15 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21A C18 C22A 81.0(22) . 2_665 ? C21A C18 O4A 73.5(22) . . ? C22A C18 O4A 110.5(17) 2_665 . ? C21A C18 C20A 54.6(21) . . ? C22A C18 C20A 32.5(12) 2_665 . ? O4A C18 C20A 113.0(19) . . ? C21A C18 C20 74.2(23) . 2_665 ? C22A C18 C20 17.0(12) 2_665 2_665 ? O4A C18 C20 121.5(17) . 2_665 ? C20A C18 C20 20.1(12) . 2_665 ? C21A C18 C19 50.2(20) . . ? C22A C18 C19 106.2(15) 2_665 . ? O4A C18 C19 23.8(7) . . ? C20A C18 C19 96.5(19) . . ? C20 C18 C19 110.9(17) 2_665 . ? O4A C19 C22A 97.0(22) . . ? O4A C19 C21A 82.8(19) . . ? C22A C19 C21A 94.0(16) . . ? O4A C19 C20 83.8(22) . . ? C22A C19 C20 19.7(14) . . ? C21A C19 C20 106.8(16) . . ? O4A C19 C19A 50.1(20) . . ? C22A C19 C19A 88.2(17) . . ? C21A C19 C19A 34.3(13) . . ? C20 C19 C19A 90.9(20) . . ? O4A C19 C20A 67.8(19) . 2_665 ? C22A C19 C20A 29.6(12) . 2_665 ? C21A C19 C20A 94.7(14) . 2_665 ? C20 C19 C20A 18.6(13) . 2_665 ? C19A C19 C20A 73.5(18) . 2_665 ? O4A C19 C18 59.7(18) . . ? C22A C19 C18 100.7(16) . . ? C21A C19 C18 23.6(9) . . ? C20 C19 C18 106.3(16) . . ? C19A C19 C18 16.6(14) . . ? C20A C19 C18 89.5(16) 2_665 . ? C20A C20 C19 108.9(48) 2_665 . ? C20A C20 O4A 84.4(44) 2_665 . ? C19 C20 O4A 27.8(8) . . ? C20A C20 C21A 47.5(41) 2_665 2_665 ? C19 C20 C21A 116.5(18) . 2_665 ? O4A C20 C21A 109.2(17) . 2_665 ? C20A C20 C18 72.6(44) 2_665 2_665 ? C19 C20 C18 119.2(22) . 2_665 ? O4A C20 C18 124.7(18) . 2_665 ? C21A C20 C18 25.7(9) 2_665 2_665 ? C20A C20 C19A 77.0(46) 2_665 2_665 ? C19 C20 C19A 101.7(22) . 2_665 ? O4A C20 C19A 109.4(19) . 2_665 ? C21A C20 C19A 30.9(12) 2_665 2_665 ? C18 C20 C19A 17.5(14) 2_665 2_665 ? C20A C20 C19A 64.4(44) 2_665 . ? C19 C20 C19A 47.2(14) . . ? O4A C20 C19A 34.7(11) . . ? C21A C20 C19A 75.0(14) 2_665 . ? C18 C20 C19A 90.7(16) 2_665 . ? C19A C20 C19A 77.2(19) 2_665 . ? C24A O3A C27A 103.4(9) . . ? C25 C24A O3A 110.4(8) . . ? C25 C24A H24A 109.6 . . ? O3A C24A H24A 109.6 . . ? C25 C24A H24B 109.6 . . ? O3A C24A H24B 109.6 . . ? H24A C24A H24B 108.1 . . ? C27A C26A C25 94.8(8) . . ? C27A C26A H26A 112.7 . . ? C25 C26A H26A 112.8 . . ? C27A C26A H26B 112.8 . . ? C25 C26A H26B 112.8 . . ? H26A C26A H26B 110.2 . . ? O3A C27A C26A 111.2(10) . . ? O3A C27A H27A 109.4 . . ? C26A C27A H27A 109.4 . . ? O3A C27A H27B 109.3 . . ? C26A C27A H27B 109.4 . . ? H27A C27A H27B 108.0 . . ? O3B C25 C24B 115.4(7) . . ? C24A C25 C26A 111.6(7) . . ? C24A C25 H25A 109.3 . . ? C26A C25 H25A 109.3 . . ? C24A C25 H25B 109.3 . . ? C26A C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? O3B C25 H25C 108.4 . . ? C24B C25 H25C 108.4 . . ? O3B C25 H25D 108.4 . . ? C24B C25 H25D 108.4 . . ? H25C C25 H25D 107.5 . . ? C25 O3B C26B 109.0(6) . . ? C25 C24B C27B 91.3(7) . . ? C25 C24B H24C 113.4 . . ? C27B C24B H24C 113.4 . . ? C25 C24B H24D 113.4 . . ? C27B C24B H24D 113.4 . . ? H24C C24B H24D 110.7 . . ? C27B C26B O3B 111.7(8) . . ? C27B C26B H26C 109.3 . . ? O3B C26B H26C 109.3 . . ? C27B C26B H26D 109.3 . . ? O3B C26B H26D 109.3 . . ? H26C C26B H26D 107.9 . . ? C26B C27B C24B 99.9(8) . . ? C26B C27B H27C 111.8 . . ? C24B C27B H27C 111.8 . . ? C26B C27B H27D 111.8 . . ? C24B C27B H27D 111.8 . . ? H27C C27B H27D 109.5 . . ? C19 O4A C19A 103.7(27) . . ? C19 O4A C21A 68.9(18) . . ? C19A O4A C21A 36.5(17) . . ? C19 O4A C22A 54.8(17) . . ? C19A O4A C22A 91.3(19) . . ? C21A O4A C22A 80.5(12) . . ? C19 O4A C20 68.4(21) . . ? C19A O4A C20 100.8(22) . . ? C21A O4A C20 97.7(14) . . ? C22A O4A C20 18.7(13) . . ? C19 O4A C18 96.5(21) . . ? C19A O4A C18 17.8(19) . . ? C21A O4A C18 28.1(9) . . ? C22A O4A C18 100.5(14) . . ? C20 O4A C18 113.7(15) . . ? C19 O4A C20A 87.4(21) . 2_665 ? C19A O4A C20A 87.3(23) . 2_665 ? C21A O4A C20A 96.6(14) . 2_665 ? C22A O4A C20A 32.9(11) . 2_665 ? C20 O4A C20A 21.2(13) . 2_665 ? C18 O4A C20A 103.4(17) . 2_665 ? C21A C19A O4A 87.7(33) . . ? C21A C19A C22A 82.7(29) . 2_665 ? O4A C19A C22A 140.2(34) . 2_665 ? C21A C19A C19 62.9(26) . . ? O4A C19A C19 26.3(11) . . ? C22A C19A C19 122.5(28) 2_665 . ? C21A C19A C20A 51.2(22) . . ? O4A C19A C20A 126.4(30) . . ? C22A C19A C20A 31.6(14) 2_665 . ? C19 C19A C20A 101.1(24) . . ? C21A C19A C20 69.8(25) . 2_665 ? O4A C19A C20 142.4(30) . 2_665 ? C22A C19A C20 15.0(14) 2_665 2_665 ? C19 C19A C20 119.1(25) . 2_665 ? C20A C19A C20 19.5(12) . 2_665 ? C21A C19A C20A 100.4(36) . 2_665 ? O4A C19A C20A 53.5(18) . 2_665 ? C22A C19A C20A 90.4(21) 2_665 2_665 ? C19 C19A C20A 56.4(16) . 2_665 ? C20A C19A C20A 96.8(22) . 2_665 ? C20 C19A C20A 100.1(20) 2_665 2_665 ? C21A C19A C22A 74.9(31) . . ? O4A C19A C22A 49.8(16) . . ? C22A C19A C22A 90.5(23) 2_665 . ? C19 C19A C22A 38.9(11) . . ? C20A C19A C22A 83.5(19) . . ? C20 C19A C22A 94.3(20) 2_665 . ? C20A C19A C22A 25.7(10) 2_665 . ? C21A C19A C20 87.2(34) . . ? O4A C19A C20 44.5(15) . . ? C22A C19A C20 96.4(23) 2_665 . ? C19 C19A C20 41.9(14) . . ? C20A C19A C20 94.5(20) . . ? C20 C19A C20 102.8(19) 2_665 . ? C20A C19A C20 15.3(10) 2_665 . ? C22A C19A C20 13.0(10) . . ? C20 C20A C22A 32.0(37) 2_665 2_665 ? C20 C20A C21A 113.6(52) 2_665 . ? C22A C20A C21A 90.6(29) 2_665 . ? C20 C20A O4A 74.3(43) 2_665 2_665 ? C22A C20A O4A 68.9(20) 2_665 2_665 ? C21A C20A O4A 125.5(23) . 2_665 ? C20 C20A C18 87.3(47) 2_665 . ? C22A C20A C18 69.4(24) 2_665 . ? C21A C20A C18 27.1(10) . . ? O4A C20A C18 126.4(21) 2_665 . ? C20 C20A C19A 83.5(48) 2_665 . ? C22A C20A C19A 58.7(23) 2_665 . ? C21A C20A C19A 32.0(15) . . ? O4A C20A C19A 108.6(21) 2_665 . ? C18 C20A C19A 18.0(15) . . ? C20 C20A C19 52.5(41) 2_665 2_665 ? C22A C20A C19 44.4(17) 2_665 2_665 ? C21A C20A C19 118.8(21) . 2_665 ? O4A C20A C19 24.8(7) 2_665 2_665 ? C18 C20A C19 108.3(20) . 2_665 ? C19A C20A C19 92.4(19) . 2_665 ? C20 C20A C19A 100.3(49) 2_665 2_665 ? C22A C20A C19A 77.7(26) 2_665 2_665 ? C21A C20A C19A 88.4(20) . 2_665 ? O4A C20A C19A 39.2(13) 2_665 2_665 ? C18 C20A C19A 99.8(21) . 2_665 ? C19A C20A C19A 83.2(22) . 2_665 ? C19 C20A C19A 50.2(14) 2_665 2_665 ? C18 C21A C19A 35.3(29) . . ? C18 C21A C20A 98.3(25) . . ? C19A C21A C20A 96.8(28) . . ? C18 C21A C19 106.2(25) . . ? C19A C21A C19 82.8(28) . . ? C20A C21A C19 134.0(19) . . ? C18 C21A O4A 78.4(23) . . ? C19A C21A O4A 55.7(26) . . ? C20A C21A O4A 135.9(16) . . ? C19 C21A O4A 28.3(7) . . ? C18 C21A C22A 71.8(22) . 2_665 ? C19A C21A C22A 63.4(25) . 2_665 ? C20A C21A C22A 33.5(13) . 2_665 ? C19 C21A C22A 122.8(13) . 2_665 ? O4A C21A C22A 108.9(12) . 2_665 ? C18 C21A C20 80.1(23) . 2_665 ? C19A C21A C20 79.3(27) . 2_665 ? C20A C21A C20 18.8(15) . 2_665 ? C19 C21A C20 136.7(15) . 2_665 ? O4A C21A C20 126.4(15) . 2_665 ? C22A C21A C20 17.6(12) 2_665 2_665 ? C18 C21A C22A 113.6(26) . . ? C19A C21A C22A 78.7(29) . . ? C20A C21A C22A 95.0(15) . . ? C19 C21A C22A 39.6(9) . . ? O4A C21A C22A 49.9(8) . . ? C22A C21A C22A 87.2(11) 2_665 . ? C20 C21A C22A 98.0(13) 2_665 . ? C20A C22A C19 106.0(24) 2_665 . ? C20A C22A C19A 89.8(30) 2_665 2_665 ? C19 C22A C19A 131.8(25) . 2_665 ? C20A C22A O4A 78.2(21) 2_665 . ? C19 C22A O4A 28.2(9) . . ? C19A C22A O4A 128.4(22) 2_665 . ? C20A C22A C18 78.1(25) 2_665 2_665 ? C19 C22A C18 150.5(21) . 2_665 ? C19A C22A C18 19.8(16) 2_665 2_665 ? O4A C22A C18 138.3(17) . 2_665 ? C20A C22A C21A 55.9(24) 2_665 2_665 ? C19 C22A C21A 133.9(18) . 2_665 ? C19A C22A C21A 33.9(15) 2_665 2_665 ? O4A C22A C21A 112.7(14) . 2_665 ? C18 C22A C21A 27.2(9) 2_665 2_665 ? C20A C22A C21A 102.7(28) 2_665 . ? C19 C22A C21A 46.4(11) . . ? C19A C22A C21A 86.1(19) 2_665 . ? O4A C22A C21A 49.6(9) . . ? C18 C22A C21A 104.1(15) 2_665 . ? C21A C22A C21A 92.8(11) 2_665 . ? C20A C22A C19A 76.5(27) 2_665 . ? C19 C22A C19A 52.8(14) . . ? C19A C22A C19A 89.5(23) 2_665 . ? O4A C22A C19A 39.0(11) . . ? C18 C22A C19A 101.9(20) 2_665 . ? C21A C22A C19A 81.1(15) 2_665 . ? C21A C22A C19A 26.4(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo Mo O1 C1 1.17(15) 2 . . . ? N1 Mo O1 C1 94.2(2) . . . . ? N2 Mo O1 C1 -91.8(2) 2 . . . ? Mo Mo N1 C3 -2.8(2) 2 . . . ? O1 Mo N1 C3 -95.4(2) . . . . ? O2 Mo N1 C3 88.6(2) 2 . . . ? Mo Mo N1 C12 171.8(2) 2 . . . ? O1 Mo N1 C12 79.2(2) . . . . ? O2 Mo N1 C12 -96.8(2) 2 . . . ? Mo O2 C1 O1 1.1(3) 2 . . . ? Mo O2 C1 C2 -177.8(2) 2 . . . ? Mo O1 C1 O2 -1.6(3) . . . . ? Mo O1 C1 C2 177.3(2) . . . . ? C12 N1 C3 N2 -172.7(2) . . . . ? Mo N1 C3 N2 2.1(3) . . . . ? C12 N1 C3 C4 8.2(3) . . . . ? Mo N1 C3 C4 -176.9(2) . . . . ? C15 N2 C3 N1 -171.7(2) . . . . ? Mo N2 C3 N1 -0.3(3) 2 . . . ? C15 N2 C3 C4 7.4(3) . . . . ? Mo N2 C3 C4 178.8(2) 2 . . . ? C11 C6 C7 C8 0.0(4) . . . . ? C5 C6 C7 C8 -178.6(2) . . . . ? C6 C7 C8 C9 0.5(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C8 C9 C10 C11 -0.4(5) . . . . ? C9 C10 C11 C6 0.9(4) . . . . ? C7 C6 C11 C10 -0.7(4) . . . . ? C5 C6 C11 C10 177.9(2) . . . . ? C3 N1 C12 C13 79.1(3) . . . . ? Mo N1 C12 C13 -95.4(2) . . . . ? C3 N1 C12 C14 -158.8(2) . . . . ? Mo N1 C12 C14 26.7(3) . . . . ? C3 N2 C15 C16 81.6(3) . . . . ? Mo N2 C15 C16 -89.3(2) 2 . . . ? C3 N2 C15 C17 -155.5(2) . . . . ? Mo N2 C15 C17 33.6(3) 2 . . . ? C21A C18 C19 O4A -167.2(37) . . . . ? C22A C18 C19 O4A -104.2(26) 2_665 . . . ? O4A C18 C19 O4A 0.000(4) . . . . ? C20A C18 C19 O4A -135.9(26) . . . . ? C20 C18 C19 O4A -121.4(29) 2_665 . . . ? C21A C18 C19 C22A -75.3(30) . . . . ? C22A C18 C19 C22A -12.3(25) 2_665 . . . ? O4A C18 C19 C22A 91.9(23) . . . . ? C20A C18 C19 C22A -44.0(22) . . . . ? C20 C18 C19 C22A -29.5(26) 2_665 . . . ? C21A C18 C19 C21A 0.000(5) . . . . ? C22A C18 C19 C21A 63.0(22) 2_665 . . . ? O4A C18 C19 C21A 167.2(37) . . . . ? C20A C18 C19 C21A 31.3(20) . . . . ? C20 C18 C19 C21A 45.8(22) 2_665 . . . ? C21A C18 C19 C20 -94.8(32) . . . . ? C22A C18 C19 C20 -31.8(26) 2_665 . . . ? O4A C18 C19 C20 72.4(22) . . . . ? C20A C18 C19 C20 -63.5(24) . . . . ? C20 C18 C19 C20 -49.0(32) 2_665 . . . ? C21A C18 C19 C19A -117.2(72) . . . . ? C22A C18 C19 C19A -54.2(61) 2_665 . . . ? O4A C18 C19 C19A 50.0(67) . . . . ? C20A C18 C19 C19A -85.9(65) . . . . ? C20 C18 C19 C19A -71.5(63) 2_665 . . . ? C21A C18 C19 C20A -102.9(28) . . . 2_665 ? C22A C18 C19 C20A -39.9(20) 2_665 . . 2_665 ? O4A C18 C19 C20A 64.3(20) . . . 2_665 ? C20A C18 C19 C20A -71.6(20) . . . 2_665 ? C20 C18 C19 C20A -57.1(21) 2_665 . . 2_665 ? O4A C19 C20 C20A 29.6(60) . . . 2_665 ? C22A C19 C20 C20A -102.2(70) . . . 2_665 ? C21A C19 C20 C20A -50.9(62) . . . 2_665 ? C19A C19 C20 C20A -20.0(60) . . . 2_665 ? C20A C19 C20 C20A 0.000(1) 2_665 . . 2_665 ? C18 C19 C20 C20A -26.3(62) . . . 2_665 ? O4A C19 C20 O4A 0.000(2) . . . . ? C22A C19 C20 O4A -131.8(58) . . . . ? C21A C19 C20 O4A -80.5(20) . . . . ? C19A C19 C20 O4A -49.6(20) . . . . ? C20A C19 C20 O4A -29.6(60) 2_665 . . . ? C18 C19 C20 O4A -55.9(18) . . . . ? O4A C19 C20 C21A 80.8(29) . . . 2_665 ? C22A C19 C20 C21A -51.0(43) . . . 2_665 ? C21A C19 C20 C21A 0.3(31) . . . 2_665 ? C19A C19 C20 C21A 31.2(27) . . . 2_665 ? C20A C19 C20 C21A 51.2(45) 2_665 . . 2_665 ? C18 C19 C20 C21A 24.9(30) . . . 2_665 ? O4A C19 C20 C18 109.8(30) . . . 2_665 ? C22A C19 C20 C18 -22.1(40) . . . 2_665 ? C21A C19 C20 C18 29.2(32) . . . 2_665 ? C19A C19 C20 C18 60.1(27) . . . 2_665 ? C20A C19 C20 C18 80.2(52) 2_665 . . 2_665 ? C18 C19 C20 C18 53.9(32) . . . 2_665 ? O4A C19 C20 C19A 109.6(24) . . . 2_665 ? C22A C19 C20 C19A -22.2(46) . . . 2_665 ? C21A C19 C20 C19A 29.1(25) . . . 2_665 ? C19A C19 C20 C19A 60.0(27) . . . 2_665 ? C20A C19 C20 C19A 80.0(53) 2_665 . . 2_665 ? C18 C19 C20 C19A 53.8(22) . . . 2_665 ? O4A C19 C20 C19A 49.6(20) . . . . ? C22A C19 C20 C19A -82.2(55) . . . . ? C21A C19 C20 C19A -30.9(16) . . . . ? C19A C19 C20 C19A 0.0 . . . . ? C20A C19 C20 C19A 20.0(60) 2_665 . . . ? C18 C19 C20 C19A -6.3(20) . . . . ? C27A O3A C24A C25 18.5(12) . . . . ? C24A O3A C27A C26A -30.5(14) . . . . ? C25 C26A C27A O3A 27.2(12) . . . . ? O3A C24A C25 O3B 38.3(13) . . . . ? O3A C24A C25 C24B -52.7(10) . . . . ? O3A C24A C25 C26A -1.5(12) . . . . ? C27A C26A C25 O3B -128.0(11) . . . . ? C27A C26A C25 C24A -15.5(11) . . . . ? C27A C26A C25 C24B 10.4(9) . . . . ? C24A C25 O3B C26B -55.9(10) . . . . ? C24B C25 O3B C26B -17.5(10) . . . . ? C26A C25 O3B C26B 29.7(7) . . . . ? O3B C25 C24B C27B -2.0(10) . . . . ? C24A C25 C24B C27B 105.5(14) . . . . ? C26A C25 C24B C27B -28.0(7) . . . . ? C25 O3B C26B C27B 37.8(11) . . . . ? O3B C26B C27B C24B -35.2(11) . . . . ? C25 C24B C27B C26B 22.2(10) . . . . ? C22A C19 O4A C19A -81.8(22) . . . . ? C21A C19 O4A C19A 11.4(23) . . . . ? C20 C19 O4A C19A -96.4(23) . . . . ? C19A C19 O4A C19A 0.000(3) . . . . ? C20A C19 O4A C19A -86.6(24) 2_665 . . . ? C18 C19 O4A C19A 16.5(20) . . . . ? C22A C19 O4A C21A -93.2(16) . . . . ? C21A C19 O4A C21A 0.000(1) . . . . ? C20 C19 O4A C21A -107.9(14) . . . . ? C19A C19 O4A C21A -11.4(23) . . . . ? C20A C19 O4A C21A -98.1(14) 2_665 . . . ? C18 C19 O4A C21A 5.1(15) . . . . ? C22A C19 O4A C22A 0.0 . . . . ? C21A C19 O4A C22A 93.2(16) . . . . ? C20 C19 O4A C22A -14.7(17) . . . . ? C19A C19 O4A C22A 81.8(22) . . . . ? C20A C19 O4A C22A -4.9(21) 2_665 . . . ? C18 C19 O4A C22A 98.3(17) . . . . ? C22A C19 O4A C20 14.7(17) . . . . ? C21A C19 O4A C20 107.9(14) . . . . ? C20 C19 O4A C20 0.0 . . . . ? C19A C19 O4A C20 96.4(23) . . . . ? C20A C19 O4A C20 9.8(19) 2_665 . . . ? C18 C19 O4A C20 113.0(15) . . . . ? C22A C19 O4A C18 -98.3(17) . . . . ? C21A C19 O4A C18 -5.1(15) . . . . ? C20 C19 O4A C18 -113.0(15) . . . . ? C19A C19 O4A C18 -16.5(20) . . . . ? C20A C19 O4A C18 -103.2(17) 2_665 . . . ? C18 C19 O4A C18 0.000(1) . . . . ? C22A C19 O4A C20A 4.9(21) . . . 2_665 ? C21A C19 O4A C20A 98.1(14) . . . 2_665 ? C20 C19 O4A C20A -9.8(19) . . . 2_665 ? C19A C19 O4A C20A 86.6(24) . . . 2_665 ? C20A C19 O4A C20A 0.000(1) 2_665 . . 2_665 ? C18 C19 O4A C20A 103.2(17) . . . 2_665 ? C20A C20 O4A C19 -152.0(57) 2_665 . . . ? C19 C20 O4A C19 0.000(2) . . . . ? C21A C20 O4A C19 -110.8(27) 2_665 . . . ? C18 C20 O4A C19 -87.6(35) 2_665 . . . ? C19A C20 O4A C19 -78.0(28) 2_665 . . . ? C19A C20 O4A C19 -100.5(27) . . . . ? C20A C20 O4A C19A -51.5(57) 2_665 . . . ? C19 C20 O4A C19A 100.5(27) . . . . ? C21A C20 O4A C19A -10.2(30) 2_665 . . . ? C18 C20 O4A C19A 12.9(35) 2_665 . . . ? C19A C20 O4A C19A 22.6(37) 2_665 . . . ? C19A C20 O4A C19A 0.000(3) . . . . ? C20A C20 O4A C21A -88.3(53) 2_665 . . . ? C19 C20 O4A C21A 63.6(18) . . . . ? C21A C20 O4A C21A -47.1(23) 2_665 . . . ? C18 C20 O4A C21A -24.0(32) 2_665 . . . ? C19A C20 O4A C21A -14.3(25) 2_665 . . . ? C19A C20 O4A C21A -36.9(18) . . . . ? C20A C20 O4A C22A -111.8(66) 2_665 . . . ? C19 C20 O4A C22A 40.2(52) . . . . ? C21A C20 O4A C22A -70.6(44) 2_665 . . . ? C18 C20 O4A C22A -47.5(38) 2_665 . . . ? C19A C20 O4A C22A -37.8(40) 2_665 . . . ? C19A C20 O4A C22A -60.4(55) . . . . ? C20A C20 O4A C18 -64.3(58) 2_665 . . . ? C19 C20 O4A C18 87.7(23) . . . . ? C21A C20 O4A C18 -23.1(30) 2_665 . . . ? C18 C20 O4A C18 0.0(41) 2_665 . . . ? C19A C20 O4A C18 9.7(29) 2_665 . . . ? C19A C20 O4A C18 -12.9(23) . . . . ? C20A C20 O4A C20A 0.0 2_665 . . 2_665 ? C19 C20 O4A C20A 152.0(57) . . . 2_665 ? C21A C20 O4A C20A 41.2(39) 2_665 . . 2_665 ? C18 C20 O4A C20A 64.3(42) 2_665 . . 2_665 ? C19A C20 O4A C20A 74.0(45) 2_665 . . 2_665 ? C19A C20 O4A C20A 51.5(57) . . . 2_665 ? C21A C18 O4A C19 10.2(29) . . . . ? C22A C18 O4A C19 83.7(26) 2_665 . . . ? C20A C18 O4A C19 48.7(29) . . . . ? C20 C18 O4A C19 69.3(32) 2_665 . . . ? C19 C18 O4A C19 0.000(4) . . . . ? C21A C18 O4A C19A -104.8(80) . . . . ? C22A C18 O4A C19A -31.3(70) 2_665 . . . ? C20A C18 O4A C19A -66.3(74) . . . . ? C20 C18 O4A C19A -45.8(69) 2_665 . . . ? C19 C18 O4A C19A -115.0(82) . . . . ? C21A C18 O4A C21A 0.000(3) . . . . ? C22A C18 O4A C21A 73.5(22) 2_665 . . . ? C20A C18 O4A C21A 38.5(18) . . . . ? C20 C18 O4A C21A 59.0(24) 2_665 . . . ? C19 C18 O4A C21A -10.2(29) . . . . ? C21A C18 O4A C22A -45.1(25) . . . . ? C22A C18 O4A C22A 28.3(23) 2_665 . . . ? C20A C18 O4A C22A -6.6(24) . . . . ? C20 C18 O4A C22A 13.9(27) 2_665 . . . ? C19 C18 O4A C22A -55.3(18) . . . . ? C21A C18 O4A C20 -59.1(31) . . . . ? C22A C18 O4A C20 14.4(27) 2_665 . . . ? C20A C18 O4A C20 -20.6(31) . . . . ? C20 C18 O4A C20 0.0(40) 2_665 . . . ? C19 C18 O4A C20 -69.3(23) . . . . ? C21A C18 O4A C20A -78.7(27) . . . 2_665 ? C22A C18 O4A C20A -5.2(24) 2_665 . . 2_665 ? C20A C18 O4A C20A -40.2(29) . . . 2_665 ? C20 C18 O4A C20A -19.6(31) 2_665 . . 2_665 ? C19 C18 O4A C20A -88.9(22) . . . 2_665 ? C19 O4A C19A C21A -18.1(37) . . . . ? C21A O4A C19A C21A 0.000(3) . . . . ? C22A O4A C19A C21A -72.1(29) . . . . ? C20 O4A C19A C21A -88.3(33) . . . . ? C18 O4A C19A C21A 49.8(61) . . . . ? C20A O4A C19A C21A -104.8(30) 2_665 . . . ? C19 O4A C19A C22A 57.7(53) . . . 2_665 ? C21A O4A C19A C22A 75.8(50) . . . 2_665 ? C22A O4A C19A C22A 3.7(50) . . . 2_665 ? C20 O4A C19A C22A -12.5(52) . . . 2_665 ? C18 O4A C19A C22A 125.6(107) . . . 2_665 ? C20A O4A C19A C22A -29.0(47) 2_665 . . 2_665 ? C19 O4A C19A C19 0.000(5) . . . . ? C21A O4A C19A C19 18.1(37) . . . . ? C22A O4A C19A C19 -54.0(19) . . . . ? C20 O4A C19A C19 -70.2(23) . . . . ? C18 O4A C19A C19 67.9(82) . . . . ? C20A O4A C19A C19 -86.7(23) 2_665 . . . ? C19 O4A C19A C20A 18.0(41) . . . . ? C21A O4A C19A C20A 36.1(23) . . . . ? C22A O4A C19A C20A -36.0(34) . . . . ? C20 O4A C19A C20A -52.2(37) . . . . ? C18 O4A C19A C20A 85.9(79) . . . . ? C20A O4A C19A C20A -68.7(34) 2_665 . . . ? C19 O4A C19A C20 33.8(54) . . . 2_665 ? C21A O4A C19A C20 51.9(39) . . . 2_665 ? C22A O4A C19A C20 -20.2(48) . . . 2_665 ? C20 O4A C19A C20 -36.4(56) . . . 2_665 ? C18 O4A C19A C20 101.7(92) . . . 2_665 ? C20A O4A C19A C20 -52.9(47) 2_665 . . 2_665 ? C19 O4A C19A C20A 86.7(23) . . . 2_665 ? C21A O4A C19A C20A 104.8(30) . . . 2_665 ? C22A O4A C19A C20A 32.7(11) . . . 2_665 ? C20 O4A C19A C20A 16.5(17) . . . 2_665 ? C18 O4A C19A C20A 154.6(79) . . . 2_665 ? C20A O4A C19A C20A 0.000(2) 2_665 . . 2_665 ? C19 O4A C19A C22A 54.0(19) . . . . ? C21A O4A C19A C22A 72.1(29) . . . . ? C22A O4A C19A C22A 0.000(2) . . . . ? C20 O4A C19A C22A -16.2(16) . . . . ? C18 O4A C19A C22A 121.9(77) . . . . ? C20A O4A C19A C22A -32.7(11) 2_665 . . . ? C19 O4A C19A C20 70.2(23) . . . . ? C21A O4A C19A C20 88.3(33) . . . . ? C22A O4A C19A C20 16.2(16) . . . . ? C20 O4A C19A C20 0.000(2) . . . . ? C18 O4A C19A C20 138.1(78) . . . . ? C20A O4A C19A C20 -16.5(17) 2_665 . . . ? O4A C19 C19A C21A 159.6(41) . . . . ? C22A C19 C19A C21A -99.7(29) . . . . ? C21A C19 C19A C21A 0.000(3) . . . . ? C20 C19 C19A C21A -119.3(31) . . . . ? C20A C19 C19A C21A -125.8(29) 2_665 . . . ? C18 C19 C19A C21A 39.2(51) . . . . ? O4A C19 C19A O4A 0.000(6) . . . . ? C22A C19 C19A O4A 100.7(25) . . . . ? C21A C19 C19A O4A -159.6(41) . . . . ? C20 C19 C19A O4A 81.1(25) . . . . ? C20A C19 C19A O4A 74.5(25) 2_665 . . . ? C18 C19 C19A O4A -120.4(74) . . . . ? O4A C19 C19A C22A -140.1(41) . . . 2_665 ? C22A C19 C19A C22A -39.5(34) . . . 2_665 ? C21A C19 C19A C22A 60.3(28) . . . 2_665 ? C20 C19 C19A C22A -59.0(34) . . . 2_665 ? C20A C19 C19A C22A -65.6(29) 2_665 . . 2_665 ? C18 C19 C19A C22A 99.5(73) . . . 2_665 ? O4A C19 C19A C20A -165.3(34) . . . . ? C22A C19 C19A C20A -64.7(23) . . . . ? C21A C19 C19A C20A 35.1(19) . . . . ? C20 C19 C19A C20A -84.2(24) . . . . ? C20A C19 C19A C20A -90.8(21) 2_665 . . . ? C18 C19 C19A C20A 74.2(63) . . . . ? O4A C19 C19A C20 -157.2(38) . . . 2_665 ? C22A C19 C19A C20 -56.5(29) . . . 2_665 ? C21A C19 C19A C20 43.2(21) . . . 2_665 ? C20 C19 C19A C20 -76.1(31) . . . 2_665 ? C20A C19 C19A C20 -82.6(25) 2_665 . . 2_665 ? C18 C19 C19A C20 82.4(64) . . . 2_665 ? O4A C19 C19A C20A -74.5(25) . . . 2_665 ? C22A C19 C19A C20A 26.1(14) . . . 2_665 ? C21A C19 C19A C20A 125.8(29) . . . 2_665 ? C20 C19 C19A C20A 6.5(20) . . . 2_665 ? C20A C19 C19A C20A 0.0 2_665 . . 2_665 ? C18 C19 C19A C20A 165.0(69) . . . 2_665 ? O4A C19 C19A C22A -100.7(25) . . . . ? C22A C19 C19A C22A 0.000(1) . . . . ? C21A C19 C19A C22A 99.7(29) . . . . ? C20 C19 C19A C22A -19.6(15) . . . . ? C20A C19 C19A C22A -26.1(14) 2_665 . . . ? C18 C19 C19A C22A 138.9(67) . . . . ? O4A C19 C19A C20 -81.1(25) . . . . ? C22A C19 C19A C20 19.6(15) . . . . ? C21A C19 C19A C20 119.3(31) . . . . ? C20 C19 C19A C20 0.0 . . . . ? C20A C19 C19A C20 -6.5(20) 2_665 . . . ? C18 C19 C19A C20 158.5(67) . . . . ? C20A C20 C19A C21A -150.1(56) 2_665 . . . ? C19 C20 C19A C21A 51.0(25) . . . . ? O4A C20 C19A C21A 89.6(33) . . . . ? C21A C20 C19A C21A -100.4(26) 2_665 . . . ? C18 C20 C19A C21A -79.8(27) 2_665 . . . ? C19A C20 C19A C21A -68.6(25) 2_665 . . . ? C20A C20 C19A O4A 120.3(62) 2_665 . . . ? C19 C20 C19A O4A -38.6(15) . . . . ? O4A C20 C19A O4A 0.000(4) . . . . ? C21A C20 C19A O4A 170.0(29) 2_665 . . . ? C18 C20 C19A O4A -169.4(29) 2_665 . . . ? C19A C20 C19A O4A -158.2(36) 2_665 . . . ? C20A C20 C19A C22A -67.7(53) 2_665 . . 2_665 ? C19 C20 C19A C22A 133.3(29) . . . 2_665 ? O4A C20 C19A C22A 172.0(34) . . . 2_665 ? C21A C20 C19A C22A -18.0(19) 2_665 . . 2_665 ? C18 C20 C19A C22A 2.5(27) 2_665 . . 2_665 ? C19A C20 C19A C22A 13.8(15) 2_665 . . 2_665 ? C20A C20 C19A C19 158.9(62) 2_665 . . . ? C19 C20 C19A C19 0.0 . . . . ? O4A C20 C19A C19 38.6(15) . . . . ? C21A C20 C19A C19 -151.4(26) 2_665 . . . ? C18 C20 C19A C19 -130.8(26) 2_665 . . . ? C19A C20 C19A C19 -119.6(29) 2_665 . . . ? C20A C20 C19A C20A -99.4(50) 2_665 . . . ? C19 C20 C19A C20A 101.7(26) . . . . ? O4A C20 C19A C20A 140.3(32) . . . . ? C21A C20 C19A C20A -49.7(16) 2_665 . . . ? C18 C20 C19A C20A -29.1(22) 2_665 . . . ? C19A C20 C19A C20A -17.9(12) 2_665 . . . ? C20A C20 C19A C20 -81.5(48) 2_665 . . 2_665 ? C19 C20 C19A C20 119.6(29) . . . 2_665 ? O4A C20 C19A C20 158.2(36) . . . 2_665 ? C21A C20 C19A C20 -31.8(12) 2_665 . . 2_665 ? C18 C20 C19A C20 -11.2(19) 2_665 . . 2_665 ? C19A C20 C19A C20 0.000(4) 2_665 . . 2_665 ? C20A C20 C19A C20A 0.000(3) 2_665 . . 2_665 ? C19 C20 C19A C20A -158.9(62) . . . 2_665 ? O4A C20 C19A C20A -120.3(62) . . . 2_665 ? C21A C20 C19A C20A 49.7(45) 2_665 . . 2_665 ? C18 C20 C19A C20A 70.3(47) 2_665 . . 2_665 ? C19A C20 C19A C20A 81.5(48) 2_665 . . 2_665 ? C20A C20 C19A C22A -131.4(79) 2_665 . . . ? C19 C20 C19A C22A 69.6(52) . . . . ? O4A C20 C19A C22A 108.3(59) . . . . ? C21A C20 C19A C22A -81.7(50) 2_665 . . . ? C18 C20 C19A C22A -61.2(47) 2_665 . . . ? C19A C20 C19A C22A -49.9(47) 2_665 . . . ? C21A C18 C20A C20 166.6(61) . . . 2_665 ? C22A C18 C20A C20 27.2(38) 2_665 . . 2_665 ? O4A C18 C20A C20 119.5(51) . . . 2_665 ? C20 C18 C20A C20 0.000(4) 2_665 . . 2_665 ? C19 C18 C20A C20 137.3(50) . . . 2_665 ? C21A C18 C20A C22A 139.4(41) . . . 2_665 ? C22A C18 C20A C22A 0.000(1) 2_665 . . 2_665 ? O4A C18 C20A C22A 92.3(33) . . . 2_665 ? C20 C18 C20A C22A -27.2(38) 2_665 . . 2_665 ? C19 C18 C20A C22A 110.0(29) . . . 2_665 ? C21A C18 C20A C21A 0.000(4) . . . . ? C22A C18 C20A C21A -139.4(41) 2_665 . . . ? O4A C18 C20A C21A -47.1(22) . . . . ? C20 C18 C20A C21A -166.6(61) 2_665 . . . ? C19 C18 C20A C21A -29.3(21) . . . . ? C21A C18 C20A O4A 98.3(39) . . . 2_665 ? C22A C18 C20A O4A -41.0(21) 2_665 . . 2_665 ? O4A C18 C20A O4A 51.2(37) . . . 2_665 ? C20 C18 C20A O4A -68.2(43) 2_665 . . 2_665 ? C19 C18 C20A O4A 69.0(30) . . . 2_665 ? C21A C18 C20A C19A 89.3(61) . . . . ? C22A C18 C20A C19A -50.1(67) 2_665 . . . ? O4A C18 C20A C19A 42.2(54) . . . . ? C20 C18 C20A C19A -77.3(79) 2_665 . . . ? C19 C18 C20A C19A 60.0(58) . . . . ? C21A C18 C20A C19 117.7(33) . . . 2_665 ? C22A C18 C20A C19 -21.7(17) 2_665 . . 2_665 ? O4A C18 C20A C19 70.6(27) . . . 2_665 ? C20 C18 C20A C19 -48.9(40) 2_665 . . 2_665 ? C19 C18 C20A C19 88.4(21) . . . 2_665 ? C21A C18 C20A C19A 66.6(33) . . . 2_665 ? C22A C18 C20A C19A -72.8(27) 2_665 . . 2_665 ? O4A C18 C20A C19A 19.5(29) . . . 2_665 ? C20 C18 C20A C19A -100.0(50) 2_665 . . 2_665 ? C19 C18 C20A C19A 37.2(22) . . . 2_665 ? C21A C19A C20A C20 -160.8(59) . . . 2_665 ? O4A C19A C20A C20 150.2(51) . . . 2_665 ? C22A C19A C20A C20 21.5(41) 2_665 . . 2_665 ? C19 C19A C20A C20 158.2(47) . . . 2_665 ? C20 C19A C20A C20 0.000(4) 2_665 . . 2_665 ? C20A C19A C20A C20 101.3(47) 2_665 . . 2_665 ? C22A C19A C20A C20 123.4(48) . . . 2_665 ? C20 C19A C20A C20 116.5(43) . . . 2_665 ? C21A C19A C20A C22A 177.7(48) . . . 2_665 ? O4A C19A C20A C22A 128.7(44) . . . 2_665 ? C22A C19A C20A C22A 0.0 2_665 . . 2_665 ? C19 C19A C20A C22A 136.7(34) . . . 2_665 ? C20 C19A C20A C22A -21.5(41) 2_665 . . 2_665 ? C20A C19A C20A C22A 79.7(26) 2_665 . . 2_665 ? C22A C19A C20A C22A 101.8(29) . . . 2_665 ? C20 C19A C20A C22A 94.9(25) . . . 2_665 ? C21A C19A C20A C21A 0.000(1) . . . . ? O4A C19A C20A C21A -49.0(31) . . . . ? C22A C19A C20A C21A -177.7(48) 2_665 . . . ? C19 C19A C20A C21A -41.0(24) . . . . ? C20 C19A C20A C21A 160.8(59) 2_665 . . . ? C20A C19A C20A C21A -98.0(36) 2_665 . . . ? C22A C19A C20A C21A -75.9(30) . . . . ? C20 C19A C20A C21A -82.8(33) . . . . ? C21A C19A C20A O4A 128.2(36) . . . 2_665 ? O4A C19A C20A O4A 79.2(38) . . . 2_665 ? C22A C19A C20A O4A -49.5(22) 2_665 . . 2_665 ? C19 C19A C20A O4A 87.2(25) . . . 2_665 ? C20 C19A C20A O4A -71.0(42) 2_665 . . 2_665 ? C20A C19A C20A O4A 30.2(19) 2_665 . . 2_665 ? C22A C19A C20A O4A 52.3(21) . . . 2_665 ? C20 C19A C20A O4A 45.4(21) . . . 2_665 ? C21A C19A C20A C18 -59.5(49) . . . . ? O4A C19A C20A C18 -108.5(73) . . . . ? C22A C19A C20A C18 122.8(74) 2_665 . . . ? C19 C19A C20A C18 -100.5(64) . . . . ? C20 C19A C20A C18 101.3(77) 2_665 . . . ? C20A C19A C20A C18 -157.4(73) 2_665 . . . ? C22A C19A C20A C18 -135.3(68) . . . . ? C20 C19A C20A C18 -142.2(70) . . . . ? C21A C19A C20A C19 147.4(34) . . . 2_665 ? O4A C19A C20A C19 98.4(34) . . . 2_665 ? C22A C19A C20A C19 -30.3(20) 2_665 . . 2_665 ? C19 C19A C20A C19 106.4(20) . . . 2_665 ? C20 C19A C20A C19 -51.8(40) 2_665 . . 2_665 ? C20A C19A C20A C19 49.4(15) 2_665 . . 2_665 ? C22A C19A C20A C19 71.5(17) . . . 2_665 ? C20 C19A C20A C19 64.6(16) . . . 2_665 ? C21A C19A C20A C19A 98.0(36) . . . 2_665 ? O4A C19A C20A C19A 49.0(29) . . . 2_665 ? C22A C19A C20A C19A -79.7(26) 2_665 . . 2_665 ? C19 C19A C20A C19A 57.0(18) . . . 2_665 ? C20 C19A C20A C19A -101.3(47) 2_665 . . 2_665 ? C20A C19A C20A C19A 0.001(1) 2_665 . . 2_665 ? C22A C19A C20A C19A 22.1(10) . . . 2_665 ? C20 C19A C20A C19A 15.2(10) . . . 2_665 ? C22A C18 C21A C19A -69.4(56) 2_665 . . . ? O4A C18 C21A C19A 45.2(56) . . . . ? C20A C18 C21A C19A -90.2(60) . . . . ? C20 C18 C21A C19A -85.4(58) 2_665 . . . ? C19 C18 C21A C19A 50.5(62) . . . . ? C22A C18 C21A C20A 20.8(19) 2_665 . . . ? O4A C18 C21A C20A 135.3(17) . . . . ? C20A C18 C21A C20A 0.000(2) . . . . ? C20 C18 C21A C20A 4.8(22) 2_665 . . . ? C19 C18 C21A C20A 140.7(24) . . . . ? C22A C18 C21A C19 -119.9(14) 2_665 . . . ? O4A C18 C21A C19 -5.3(15) . . . . ? C20A C18 C21A C19 -140.7(24) . . . . ? C20 C18 C21A C19 -135.9(17) 2_665 . . . ? C19 C18 C21A C19 0.000(2) . . . . ? C22A C18 C21A O4A -114.6(13) 2_665 . . . ? O4A C18 C21A O4A 0.000(1) . . . . ? C20A C18 C21A O4A -135.3(17) . . . . ? C20 C18 C21A O4A -130.6(13) 2_665 . . . ? C19 C18 C21A O4A 5.3(15) . . . . ? C22A C18 C21A C22A 0.0 2_665 . . 2_665 ? O4A C18 C21A C22A 114.6(12) . . . 2_665 ? C20A C18 C21A C22A -20.8(19) . . . 2_665 ? C20 C18 C21A C22A -16.0(13) 2_665 . . 2_665 ? C19 C18 C21A C22A 119.9(14) . . . 2_665 ? C22A C18 C21A C20 16.0(13) 2_665 . . 2_665 ? O4A C18 C21A C20 130.6(13) . . . 2_665 ? C20A C18 C21A C20 -4.8(22) . . . 2_665 ? C20 C18 C21A C20 0.000(1) 2_665 . . 2_665 ? C19 C18 C21A C20 135.9(17) . . . 2_665 ? C22A C18 C21A C22A -78.4(18) 2_665 . . . ? O4A C18 C21A C22A 36.1(16) . . . . ? C20A C18 C21A C22A -99.2(21) . . . . ? C20 C18 C21A C22A -94.4(19) 2_665 . . . ? C19 C18 C21A C22A 41.5(13) . . . . ? O4A C19A C21A C18 -122.8(65) . . . . ? C22A C19A C21A C18 95.9(60) 2_665 . . . ? C19 C19A C21A C18 -131.7(59) . . . . ? C20A C19A C21A C18 94.7(58) . . . . ? C20 C19A C21A C18 88.0(57) 2_665 . . . ? C20A C19A C21A C18 -175.0(70) 2_665 . . . ? C22A C19A C21A C18 -171.6(62) . . . . ? C20 C19A C21A C18 -167.3(63) . . . . ? O4A C19A C21A C20A 142.5(19) . . . . ? C22A C19A C21A C20A 1.2(25) 2_665 . . . ? C19 C19A C21A C20A 133.7(19) . . . . ? C20A C19A C21A C20A 0.0 . . . . ? C20 C19A C21A C20A -6.7(20) 2_665 . . . ? C20A C19A C21A C20A 90.3(24) 2_665 . . . ? C22A C19A C21A C20A 93.8(17) . . . . ? C20 C19A C21A C20A 98.0(19) . . . . ? O4A C19A C21A C19 8.9(18) . . . . ? C22A C19A C21A C19 -132.4(17) 2_665 . . . ? C19 C19A C21A C19 0.000(2) . . . . ? C20A C19A C21A C19 -133.7(19) . . . . ? C20 C19A C21A C19 -140.4(13) 2_665 . . . ? C20A C19A C21A C19 -43.3(17) 2_665 . . . ? C22A C19A C21A C19 -39.9(10) . . . . ? C20 C19A C21A C19 -35.6(12) . . . . ? O4A C19A C21A O4A 0.000(2) . . . . ? C22A C19A C21A O4A -141.3(29) 2_665 . . . ? C19 C19A C21A O4A -8.9(18) . . . . ? C20A C19A C21A O4A -142.5(19) . . . . ? C20 C19A C21A O4A -149.3(21) 2_665 . . . ? C20A C19A C21A O4A -52.2(18) 2_665 . . . ? C22A C19A C21A O4A -48.8(15) . . . . ? C20 C19A C21A O4A -44.5(15) . . . . ? O4A C19A C21A C22A 141.3(29) . . . 2_665 ? C22A C19A C21A C22A 0.0 2_665 . . 2_665 ? C19 C19A C21A C22A 132.4(17) . . . 2_665 ? C20A C19A C21A C22A -1.2(25) . . . 2_665 ? C20 C19A C21A C22A -7.9(18) 2_665 . . 2_665 ? C20A C19A C21A C22A 89.1(21) 2_665 . . 2_665 ? C22A C19A C21A C22A 92.5(18) . . . 2_665 ? C20 C19A C21A C22A 96.8(19) . . . 2_665 ? O4A C19A C21A C20 149.3(21) . . . 2_665 ? C22A C19A C21A C20 7.9(18) 2_665 . . 2_665 ? C19 C19A C21A C20 140.4(13) . . . 2_665 ? C20A C19A C21A C20 6.7(20) . . . 2_665 ? C20 C19A C21A C20 0.000(1) 2_665 . . 2_665 ? C20A C19A C21A C20 97.1(20) 2_665 . . 2_665 ? C22A C19A C21A C20 100.5(14) . . . 2_665 ? C20 C19A C21A C20 104.8(13) . . . 2_665 ? O4A C19A C21A C22A 48.8(15) . . . . ? C22A C19A C21A C22A -92.5(18) 2_665 . . . ? C19 C19A C21A C22A 39.9(10) . . . . ? C20A C19A C21A C22A -93.8(17) . . . . ? C20 C19A C21A C22A -100.5(14) 2_665 . . . ? C20A C19A C21A C22A -3.4(14) 2_665 . . . ? C22A C19A C21A C22A 0.000(1) . . . . ? C20 C19A C21A C22A 4.3(11) . . . . ? C20 C20A C21A C18 -14.7(65) 2_665 . . . ? C22A C20A C21A C18 -37.6(37) 2_665 . . . ? O4A C20A C21A C18 -101.8(36) 2_665 . . . ? C18 C20A C21A C18 0.000(5) . . . . ? C19A C20A C21A C18 -35.6(30) . . . . ? C19 C20A C21A C18 -73.5(35) 2_665 . . . ? C19A C20A C21A C18 -115.3(32) 2_665 . . . ? C20 C20A C21A C19A 20.9(66) 2_665 . . . ? C22A C20A C21A C19A -2.0(41) 2_665 . . . ? O4A C20A C21A C19A -66.2(41) 2_665 . . . ? C18 C20A C21A C19A 35.6(30) . . . . ? C19A C20A C21A C19A 0.000(1) . . . . ? C19 C20A C21A C19A -37.9(39) 2_665 . . . ? C19A C20A C21A C19A -79.7(37) 2_665 . . . ? C20 C20A C21A C19 107.5(59) 2_665 . . . ? C22A C20A C21A C19 84.7(34) 2_665 . . . ? O4A C20A C21A C19 20.4(42) 2_665 . . . ? C18 C20A C21A C19 122.2(36) . . . . ? C19A C20A C21A C19 86.6(34) . . . . ? C19 C20A C21A C19 48.7(37) 2_665 . . . ? C19A C20A C21A C19 6.9(28) 2_665 . . . ? C20 C20A C21A O4A 67.2(68) 2_665 . . . ? C22A C20A C21A O4A 44.3(40) 2_665 . . . ? O4A C20A C21A O4A -19.9(44) 2_665 . . . ? C18 C20A C21A O4A 81.9(30) . . . . ? C19A C20A C21A O4A 46.3(29) . . . . ? C19 C20A C21A O4A 8.4(40) 2_665 . . . ? C19A C20A C21A O4A -33.4(30) 2_665 . . . ? C20 C20A C21A C22A 22.9(45) 2_665 . . 2_665 ? C22A C20A C21A C22A 0.0 2_665 . . 2_665 ? O4A C20A C21A C22A -64.3(25) 2_665 . . 2_665 ? C18 C20A C21A C22A 37.6(37) . . . 2_665 ? C19A C20A C21A C22A 2.0(41) . . . 2_665 ? C19 C20A C21A C22A -35.9(18) 2_665 . . 2_665 ? C19A C20A C21A C22A -77.7(26) 2_665 . . 2_665 ? C20 C20A C21A C20 0.000(3) 2_665 . . 2_665 ? C22A C20A C21A C20 -22.9(45) 2_665 . . 2_665 ? O4A C20A C21A C20 -87.2(58) 2_665 . . 2_665 ? C18 C20A C21A C20 14.7(65) . . . 2_665 ? C19A C20A C21A C20 -20.9(66) . . . 2_665 ? C19 C20A C21A C20 -58.8(50) 2_665 . . 2_665 ? C19A C20A C21A C20 -100.6(59) 2_665 . . 2_665 ? C20 C20A C21A C22A 100.1(58) 2_665 . . . ? C22A C20A C21A C22A 77.2(27) 2_665 . . . ? O4A C20A C21A C22A 13.0(26) 2_665 . . . ? C18 C20A C21A C22A 114.8(27) . . . . ? C19A C20A C21A C22A 79.2(30) . . . . ? C19 C20A C21A C22A 41.3(23) 2_665 . . . ? C19A C20A C21A C22A -0.5(15) 2_665 . . . ? O4A C19 C21A C18 11.1(32) . . . . ? C22A C19 C21A C18 107.7(29) . . . . ? C20 C19 C21A C18 92.3(33) . . . . ? C19A C19 C21A C18 26.7(32) . . . . ? C20A C19 C21A C18 78.0(29) 2_665 . . . ? C18 C19 C21A C18 0.000(4) . . . . ? O4A C19 C21A C19A -15.6(32) . . . . ? C22A C19 C21A C19A 80.9(30) . . . . ? C20 C19 C21A C19A 65.6(35) . . . . ? C19A C19 C21A C19A 0.000(3) . . . . ? C20A C19 C21A C19A 51.2(30) 2_665 . . . ? C18 C19 C21A C19A -26.7(33) . . . . ? O4A C19 C21A C20A -108.2(29) . . . . ? C22A C19 C21A C20A -11.7(30) . . . . ? C20 C19 C21A C20A -27.0(34) . . . . ? C19A C19 C21A C20A -92.6(34) . . . . ? C20A C19 C21A C20A -41.4(32) 2_665 . . . ? C18 C19 C21A C20A -119.3(36) . . . . ? O4A C19 C21A O4A 0.000(2) . . . . ? C22A C19 C21A O4A 96.6(22) . . . . ? C20 C19 C21A O4A 81.2(23) . . . . ? C19A C19 C21A O4A 15.6(32) . . . . ? C20A C19 C21A O4A 66.8(19) 2_665 . . . ? C18 C19 C21A O4A -11.1(32) . . . . ? O4A C19 C21A C22A -67.3(23) . . . 2_665 ? C22A C19 C21A C22A 29.2(24) . . . 2_665 ? C20 C19 C21A C22A 13.9(25) . . . 2_665 ? C19A C19 C21A C22A -51.7(26) . . . 2_665 ? C20A C19 C21A C22A -0.5(21) 2_665 . . 2_665 ? C18 C19 C21A C22A -78.4(27) . . . 2_665 ? O4A C19 C21A C20 -81.6(32) . . . 2_665 ? C22A C19 C21A C20 15.0(30) . . . 2_665 ? C20 C19 C21A C20 -0.3(41) . . . 2_665 ? C19A C19 C21A C20 -66.0(31) . . . 2_665 ? C20A C19 C21A C20 -14.7(30) 2_665 . . 2_665 ? C18 C19 C21A C20 -92.7(33) . . . 2_665 ? O4A C19 C21A C22A -96.6(22) . . . . ? C22A C19 C21A C22A 0.000(2) . . . . ? C20 C19 C21A C22A -15.3(18) . . . . ? C19A C19 C21A C22A -80.9(30) . . . . ? C20A C19 C21A C22A -29.7(12) 2_665 . . . ? C18 C19 C21A C22A -107.7(29) . . . . ? C19 O4A C21A C18 -169.1(31) . . . . ? C19A O4A C21A C18 29.7(36) . . . . ? C22A O4A C21A C18 135.0(25) . . . . ? C20 O4A C21A C18 127.6(28) . . . . ? C18 O4A C21A C18 0.000(3) . . . . ? C20A O4A C21A C18 106.2(28) 2_665 . . . ? C19 O4A C21A C19A 161.1(39) . . . . ? C19A O4A C21A C19A 0.000(4) . . . . ? C22A O4A C21A C19A 105.3(32) . . . . ? C20 O4A C21A C19A 97.9(37) . . . . ? C18 O4A C21A C19A -29.7(36) . . . . ? C20A O4A C21A C19A 76.5(36) 2_665 . . . ? C19 O4A C21A C20A 100.9(32) . . . . ? C19A O4A C21A C20A -60.3(35) . . . . ? C22A O4A C21A C20A 45.1(27) . . . . ? C20 O4A C21A C20A 37.6(34) . . . . ? C18 O4A C21A C20A -90.0(31) . . . . ? C20A O4A C21A C20A 16.2(37) 2_665 . . . ? C19 O4A C21A C19 0.000(3) . . . . ? C19A O4A C21A C19 -161.1(39) . . . . ? C22A O4A C21A C19 -55.8(18) . . . . ? C20 O4A C21A C19 -63.3(21) . . . . ? C18 O4A C21A C19 169.1(31) . . . . ? C20A O4A C21A C19 -84.7(21) 2_665 . . . ? C19 O4A C21A C22A 125.0(20) . . . 2_665 ? C19A O4A C21A C22A -36.2(30) . . . 2_665 ? C22A O4A C21A C22A 69.1(15) . . . 2_665 ? C20 O4A C21A C22A 61.7(17) . . . 2_665 ? C18 O4A C21A C22A -65.9(22) . . . 2_665 ? C20A O4A C21A C22A 40.3(17) 2_665 . . 2_665 ? C19 O4A C21A C20 122.6(26) . . . 2_665 ? C19A O4A C21A C20 -38.6(29) . . . 2_665 ? C22A O4A C21A C20 66.7(18) . . . 2_665 ? C20 O4A C21A C20 59.3(27) . . . 2_665 ? C18 O4A C21A C20 -68.3(24) . . . 2_665 ? C20A O4A C21A C20 37.9(24) 2_665 . . 2_665 ? C19 O4A C21A C22A 55.8(18) . . . . ? C19A O4A C21A C22A -105.3(32) . . . . ? C22A O4A C21A C22A 0.000(2) . . . . ? C20 O4A C21A C22A -7.5(17) . . . . ? C18 O4A C21A C22A -135.0(25) . . . . ? C20A O4A C21A C22A -28.8(14) 2_665 . . . ? O4A C19 C22A C20A -9.2(41) . . . 2_665 ? C21A C19 C22A C20A -92.4(36) . . . 2_665 ? C20 C19 C22A C20A 39.1(41) . . . 2_665 ? C19A C19 C22A C20A -58.6(37) . . . 2_665 ? C20A C19 C22A C20A 0.000(2) 2_665 . . 2_665 ? C18 C19 C22A C20A -69.5(37) . . . 2_665 ? O4A C19 C22A C19A 95.4(33) . . . 2_665 ? C21A C19 C22A C19A 12.1(33) . . . 2_665 ? C20 C19 C22A C19A 143.6(71) . . . 2_665 ? C19A C19 C22A C19A 46.0(39) . . . 2_665 ? C20A C19 C22A C19A 104.6(47) 2_665 . . 2_665 ? C18 C19 C22A C19A 35.0(31) . . . 2_665 ? O4A C19 C22A O4A 0.0 . . . . ? C21A C19 C22A O4A -83.2(20) . . . . ? C20 C19 C22A O4A 48.3(59) . . . . ? C19A C19 C22A O4A -49.4(21) . . . . ? C20A C19 C22A O4A 9.2(41) 2_665 . . . ? C18 C19 C22A O4A -60.4(19) . . . . ? O4A C19 C22A C18 84.9(45) . . . 2_665 ? C21A C19 C22A C18 1.7(44) . . . 2_665 ? C20 C19 C22A C18 133.2(76) . . . 2_665 ? C19A C19 C22A C18 35.5(43) . . . 2_665 ? C20A C19 C22A C18 94.1(52) 2_665 . . 2_665 ? C18 C19 C22A C18 24.5(48) . . . 2_665 ? O4A C19 C22A C21A 48.5(32) . . . 2_665 ? C21A C19 C22A C21A -34.7(28) . . . 2_665 ? C20 C19 C22A C21A 96.8(56) . . . 2_665 ? C19A C19 C22A C21A -0.9(29) . . . 2_665 ? C20A C19 C22A C21A 57.7(31) 2_665 . . 2_665 ? C18 C19 C22A C21A -11.8(29) . . . 2_665 ? O4A C19 C22A C21A 83.2(20) . . . . ? C21A C19 C22A C21A 0.000(1) . . . . ? C20 C19 C22A C21A 131.5(55) . . . . ? C19A C19 C22A C21A 33.8(14) . . . . ? C20A C19 C22A C21A 92.4(36) 2_665 . . . ? C18 C19 C22A C21A 22.9(10) . . . . ? O4A C19 C22A C19A 49.4(21) . . . . ? C21A C19 C22A C19A -33.8(14) . . . . ? C20 C19 C22A C19A 97.6(56) . . . . ? C19A C19 C22A C19A 0.000(1) . . . . ? C20A C19 C22A C19A 58.6(37) 2_665 . . . ? C18 C19 C22A C19A -11.0(18) . . . . ? C19 O4A C22A C20A 171.0(40) . . . 2_665 ? C19A O4A C22A C20A -83.1(36) . . . 2_665 ? C21A O4A C22A C20A -118.2(31) . . . 2_665 ? C20 O4A C22A C20A 38.2(41) . . . 2_665 ? C18 O4A C22A C20A -98.4(33) . . . 2_665 ? C20A O4A C22A C20A 0.000(2) 2_665 . . 2_665 ? C19 O4A C22A C19 0.000(1) . . . . ? C19A O4A C22A C19 105.9(27) . . . . ? C21A O4A C22A C19 70.8(20) . . . . ? C20 O4A C22A C19 -132.8(59) . . . . ? C18 O4A C22A C19 90.6(23) . . . . ? C20A O4A C22A C19 -171.0(40) 2_665 . . . ? C19 O4A C22A C19A -108.9(34) . . . 2_665 ? C19A O4A C22A C19A -3.0(41) . . . 2_665 ? C21A O4A C22A C19A -38.0(27) . . . 2_665 ? C20 O4A C22A C19A 118.4(60) . . . 2_665 ? C18 O4A C22A C19A -18.3(29) . . . 2_665 ? C20A O4A C22A C19A 80.1(36) 2_665 . . 2_665 ? C19 O4A C22A C18 -132.6(35) . . . 2_665 ? C19A O4A C22A C18 -26.7(33) . . . 2_665 ? C21A O4A C22A C18 -61.7(27) . . . 2_665 ? C20 O4A C22A C18 94.7(53) . . . 2_665 ? C18 O4A C22A C18 -42.0(34) . . . 2_665 ? C20A O4A C22A C18 56.4(31) 2_665 . . 2_665 ? C19 O4A C22A C21A -144.2(26) . . . 2_665 ? C19A O4A C22A C21A -38.3(24) . . . 2_665 ? C21A O4A C22A C21A -73.4(15) . . . 2_665 ? C20 O4A C22A C21A 83.1(48) . . . 2_665 ? C18 O4A C22A C21A -53.6(18) . . . 2_665 ? C20A O4A C22A C21A 44.8(26) 2_665 . . 2_665 ? C19 O4A C22A C21A -70.8(20) . . . . ? C19A O4A C22A C21A 35.0(17) . . . . ? C21A O4A C22A C21A 0.000(2) . . . . ? C20 O4A C22A C21A 156.4(53) . . . . ? C18 O4A C22A C21A 19.8(11) . . . . ? C20A O4A C22A C21A 118.2(31) 2_665 . . . ? C19 O4A C22A C19A -105.9(27) . . . . ? C19A O4A C22A C19A 0.000(3) . . . . ? C21A O4A C22A C19A -35.0(17) . . . . ? C20 O4A C22A C19A 121.4(55) . . . . ? C18 O4A C22A C19A -15.3(21) . . . . ? C20A O4A C22A C19A 83.1(36) 2_665 . . . ? C18 C21A C22A C20A 13.1(36) . . . 2_665 ? C19A C21A C22A C20A 7.8(31) . . . 2_665 ? C20A C21A C22A C20A -88.2(29) . . . 2_665 ? C19 C21A C22A C20A 100.2(31) . . . 2_665 ? O4A C21A C22A C20A 62.2(26) . . . 2_665 ? C22A C21A C22A C20A -55.6(25) 2_665 . . 2_665 ? C20 C21A C22A C20A -69.5(23) 2_665 . . 2_665 ? C18 C21A C22A C19 -87.1(29) . . . . ? C19A C21A C22A C19 -92.4(29) . . . . ? C20A C21A C22A C19 171.6(22) . . . . ? C19 C21A C22A C19 0.000(3) . . . . ? O4A C21A C22A C19 -38.0(12) . . . . ? C22A C21A C22A C19 -155.8(20) 2_665 . . . ? C20 C21A C22A C19 -169.7(21) 2_665 . . . ? C18 C21A C22A C19A 102.0(30) . . . 2_665 ? C19A C21A C22A C19A 96.7(30) . . . 2_665 ? C20A C21A C22A C19A 0.7(21) . . . 2_665 ? C19 C21A C22A C19A -171.0(25) . . . 2_665 ? O4A C21A C22A C19A 151.0(21) . . . 2_665 ? C22A C21A C22A C19A 33.3(15) 2_665 . . 2_665 ? C20 C21A C22A C19A 19.4(22) 2_665 . . 2_665 ? C18 C21A C22A O4A -49.1(26) . . . . ? C19A C21A C22A O4A -54.4(25) . . . . ? C20A C21A C22A O4A -150.4(18) . . . . ? C19 C21A C22A O4A 38.0(12) . . . . ? O4A C21A C22A O4A 0.000(2) . . . . ? C22A C21A C22A O4A -117.8(14) 2_665 . . . ? C20 C21A C22A O4A -131.7(16) 2_665 . . . ? C18 C21A C22A C18 93.8(26) . . . 2_665 ? C19A C21A C22A C18 88.5(28) . . . 2_665 ? C20A C21A C22A C18 -7.5(17) . . . 2_665 ? C19 C21A C22A C18 -179.1(23) . . . 2_665 ? O4A C21A C22A C18 142.9(18) . . . 2_665 ? C22A C21A C22A C18 25.1(11) 2_665 . . 2_665 ? C20 C21A C22A C18 11.2(19) 2_665 . . 2_665 ? C18 C21A C22A C21A 68.7(25) . . . 2_665 ? C19A C21A C22A C21A 63.4(25) . . . 2_665 ? C20A C21A C22A C21A -32.6(13) . . . 2_665 ? C19 C21A C22A C21A 155.8(20) . . . 2_665 ? O4A C21A C22A C21A 117.8(14) . . . 2_665 ? C22A C21A C22A C21A -0.001(1) 2_665 . . 2_665 ? C20 C21A C22A C21A -13.9(14) 2_665 . . 2_665 ? C18 C21A C22A C19A 5.3(39) . . . . ? C19A C21A C22A C19A 0.000(3) . . . . ? C20A C21A C22A C19A -96.0(29) . . . . ? C19 C21A C22A C19A 92.4(29) . . . . ? O4A C21A C22A C19A 54.4(25) . . . . ? C22A C21A C22A C19A -63.4(25) 2_665 . . . ? C20 C21A C22A C19A -77.3(27) 2_665 . . . ? C21A C19A C22A C20A -172.2(32) . . . 2_665 ? O4A C19A C22A C20A 87.8(32) . . . 2_665 ? C22A C19A C22A C20A -89.9(29) 2_665 . . 2_665 ? C19 C19A C22A C20A 122.5(32) . . . 2_665 ? C20A C19A C22A C20A -120.7(23) . . . 2_665 ? C20 C19A C22A C20A -104.5(23) 2_665 . . 2_665 ? C20A C19A C22A C20A 0.000(3) 2_665 . . 2_665 ? C20 C19A C22A C20A 27.1(46) . . . 2_665 ? C21A C19A C22A C19 65.3(25) . . . . ? O4A C19A C22A C19 -34.8(14) . . . . ? C22A C19A C22A C19 147.6(29) 2_665 . . . ? C19 C19A C22A C19 0.000(1) . . . . ? C20A C19A C22A C19 116.8(25) . . . . ? C20 C19A C22A C19 133.0(27) 2_665 . . . ? C20A C19A C22A C19 -122.5(32) 2_665 . . . ? C20 C19A C22A C19 -95.4(54) . . . . ? C21A C19A C22A C19A -82.3(27) . . . 2_665 ? O4A C19A C22A C19A 177.7(32) . . . 2_665 ? C22A C19A C22A C19A 0.000(4) 2_665 . . 2_665 ? C19 C19A C22A C19A -147.6(29) . . . 2_665 ? C20A C19A C22A C19A -30.8(13) . . . 2_665 ? C20 C19A C22A C19A -14.6(15) 2_665 . . 2_665 ? C20A C19A C22A C19A 89.9(29) 2_665 . . 2_665 ? C20 C19A C22A C19A 117.0(56) . . . 2_665 ? C21A C19A C22A O4A 100.0(30) . . . . ? O4A C19A C22A O4A 0.000(4) . . . . ? C22A C19A C22A O4A -177.7(32) 2_665 . . . ? C19 C19A C22A O4A 34.8(14) . . . . ? C20A C19A C22A O4A 151.5(28) . . . . ? C20 C19A C22A O4A 167.8(30) 2_665 . . . ? C20A C19A C22A O4A -87.8(32) 2_665 . . . ? C20 C19A C22A O4A -60.6(53) . . . . ? C21A C19A C22A C18 -97.7(24) . . . 2_665 ? O4A C19A C22A C18 162.2(22) . . . 2_665 ? C22A C19A C22A C18 -15.4(21) 2_665 . . 2_665 ? C19 C19A C22A C18 -163.0(22) . . . 2_665 ? C20A C19A C22A C18 -46.2(19) . . . 2_665 ? C20 C19A C22A C18 -30.0(22) 2_665 . . 2_665 ? C20A C19A C22A C18 74.5(27) 2_665 . . 2_665 ? C20 C19A C22A C18 101.6(53) . . . 2_665 ? C21A C19A C22A C21A -115.3(24) . . . 2_665 ? O4A C19A C22A C21A 144.6(22) . . . 2_665 ? C22A C19A C22A C21A -33.0(13) 2_665 . . 2_665 ? C19 C19A C22A C21A 179.4(21) . . . 2_665 ? C20A C19A C22A C21A -63.8(14) . . . 2_665 ? C20 C19A C22A C21A -47.6(15) 2_665 . . 2_665 ? C20A C19A C22A C21A 56.9(24) 2_665 . . 2_665 ? C20 C19A C22A C21A 84.0(51) . . . 2_665 ? C21A C19A C22A C21A 0.000(3) . . . . ? O4A C19A C22A C21A -100.0(30) . . . . ? C22A C19A C22A C21A 82.3(27) 2_665 . . . ? C19 C19A C22A C21A -65.3(25) . . . . ? C20A C19A C22A C21A 51.5(20) . . . . ? C20 C19A C22A C21A 67.7(24) 2_665 . . . ? C20A C19A C22A C21A 172.2(32) 2_665 . . . ? C20 C19A C22A C21A -160.7(52) . . . . ? _refine_diff_density_max 0.774 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.064 #END OF CIF # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-04-22 at 10:29:04 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : shelx dreduc import struct data_Chisholm1317 _database_code_depnum_ccdc_archive 'CCDC 637928' _audit_creation_date 2005-04-22T10:29:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1317' _chemical_formula_moiety 'C34 H44 N4 O4 W2' _chemical_formula_sum 'C34 H44 N4 O4 W2' _chemical_formula_weight 940.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.279(1) _cell_length_b 9.371(1) _cell_length_c 12.082(1) _cell_angle_alpha 75.741(6) _cell_angle_beta 71.498(6) _cell_angle_gamma 78.558(5) _cell_volume 854.12(16) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3907 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_special_details ;The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.6, which means that 90% of the reflections were measured at least 3.6 times. A combination of phi and omega scans with a frame width of 2 degrees was used. The W dimer contains a crystallographic inversion center. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.298 _exptl_absorpt_correction_T_max 0.444 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.127142 _diffrn_orient_matrix_ub_12 0.147258E-1 _diffrn_orient_matrix_ub_13 0.129484E-1 _diffrn_orient_matrix_ub_21 0.15212E-1 _diffrn_orient_matrix_ub_22 0.625797E-1 _diffrn_orient_matrix_ub_23 -0.817278E-1 _diffrn_orient_matrix_ub_31 0.104444E-1 _diffrn_orient_matrix_ub_32 -0.905542E-1 _diffrn_orient_matrix_ub_33 -0.328372E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 26489 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 3913 _reflns_number_gt 3686 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+0.1355P] 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_number_reflns 3913 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.019 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0404 _refine_ls_wR_factor_gt 0.0398 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.152 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 W1 W 0.441678(10) 0.082034(9) 0.555817(7) 0.01149(4) Uani 1 1 d . . . N1 N 0.3648(3) 0.2341(2) 0.41647(18) 0.0134(4) Uani 1 1 d . . . N2 N 0.5128(3) -0.0583(2) 0.70260(18) 0.0133(4) Uani 1 1 d . . . O1 O 0.6736(2) 0.17203(19) 0.50462(15) 0.0151(4) Uani 1 1 d . . . O2 O 0.2056(2) -0.00327(19) 0.61097(15) 0.0154(4) Uani 1 1 d . . . C1 C 0.8031(3) 0.1117(3) 0.4326(2) 0.0164(5) Uani 1 1 d . . . C2 C 0.9711(3) 0.1702(3) 0.3998(2) 0.0242(6) Uani 1 1 d . . . H2A H 1.0585 0.1134 0.3451 0.036 Uiso 1 1 calc R . . H2B H 1.0061 0.1604 0.4718 0.036 Uiso 1 1 calc R . . H2C H 0.9587 0.2751 0.361 0.036 Uiso 1 1 calc R . . C3 C 0.4031(3) 0.1944(3) 0.3102(2) 0.0137(5) Uani 1 1 d . . . C4 C 0.3516(3) 0.2970(3) 0.2131(2) 0.0167(5) Uani 1 1 d . . . C5 C 0.3034(3) 0.3911(3) 0.1397(2) 0.0196(5) Uani 1 1 d . . . C6 C 0.2443(3) 0.5126(3) 0.0566(2) 0.0198(5) Uani 1 1 d . . . C7 C 0.2482(4) 0.4956(3) -0.0561(3) 0.0310(7) Uani 1 1 d . . . H7 H 0.2891 0.402 -0.0789 0.037 Uiso 1 1 calc R . . C8 C 0.1927(4) 0.6145(4) -0.1338(3) 0.0390(8) Uani 1 1 d . . . H8 H 0.1965 0.6024 -0.2104 0.047 Uiso 1 1 calc R . . C9 C 0.1321(4) 0.7502(3) -0.1024(3) 0.0337(7) Uani 1 1 d . . . H9 H 0.0938 0.8313 -0.1569 0.04 Uiso 1 1 calc R . . C10 C 0.1267(4) 0.7688(3) 0.0088(3) 0.0344(7) Uani 1 1 d . . . H10 H 0.0847 0.8626 0.031 0.041 Uiso 1 1 calc R . . C11 C 0.1831(4) 0.6496(3) 0.0878(3) 0.0284(6) Uani 1 1 d . . . H11 H 0.1796 0.6625 0.1642 0.034 Uiso 1 1 calc R . . C12 C 0.2787(3) 0.3862(3) 0.4275(2) 0.0175(5) Uani 1 1 d . . . H12 H 0.1897 0.4123 0.3834 0.021 Uiso 1 1 calc R . . C13 C 0.4069(4) 0.4987(3) 0.3737(2) 0.0268(6) Uani 1 1 d . . . H13A H 0.4616 0.4951 0.2894 0.04 Uiso 1 1 calc R . . H13B H 0.4949 0.4746 0.4162 0.04 Uiso 1 1 calc R . . H13C H 0.3467 0.5986 0.3809 0.04 Uiso 1 1 calc R . . C14 C 0.1897(3) 0.3897(3) 0.5580(2) 0.0255(6) Uani 1 1 d . . . H14A H 0.1112 0.3142 0.5911 0.038 Uiso 1 1 calc R . . H14B H 0.1245 0.488 0.5653 0.038 Uiso 1 1 calc R . . H14C H 0.2759 0.3691 0.6017 0.038 Uiso 1 1 calc R . . C15 C 0.4828(3) -0.0137(3) 0.8171(2) 0.0193(5) Uani 1 1 d . . . H15 H 0.455 -0.1015 0.8829 0.023 Uiso 1 1 calc R . . C16 C 0.6416(4) 0.0405(3) 0.8230(2) 0.0308(6) Uani 1 1 d . . . H16A H 0.7392 -0.0385 0.8121 0.046 Uiso 1 1 calc R . . H16B H 0.619 0.0666 0.9007 0.046 Uiso 1 1 calc R . . H16C H 0.6686 0.1281 0.76 0.046 Uiso 1 1 calc R . . C17 C 0.3300(4) 0.1080(3) 0.8332(2) 0.0291(7) Uani 1 1 d . . . H17A H 0.2284 0.0713 0.831 0.044 Uiso 1 1 calc R . . H17B H 0.3555 0.1947 0.7689 0.044 Uiso 1 1 calc R . . H17C H 0.3078 0.1364 0.91 0.044 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 W1 0.01292(6) 0.01055(6) 0.01225(6) -0.00314(4) -0.00496(4) -0.00089(4) N1 0.0148(10) 0.0107(10) 0.0157(10) -0.0015(8) -0.0063(8) -0.0017(8) N2 0.0152(10) 0.0134(10) 0.0115(10) -0.0024(8) -0.0043(8) -0.0021(8) O1 0.0149(8) 0.0130(9) 0.0195(9) -0.0040(7) -0.0057(7) -0.0042(7) O2 0.0140(8) 0.0153(9) 0.0170(9) -0.0038(7) -0.0039(7) -0.0024(7) C1 0.0176(12) 0.0158(12) 0.0160(12) 0.0024(10) -0.0085(10) -0.0033(10) C2 0.0186(13) 0.0245(14) 0.0307(15) -0.0029(12) -0.0083(11) -0.0066(11) C3 0.0135(12) 0.0159(13) 0.0133(12) -0.0011(10) -0.0056(9) -0.0048(9) C4 0.0182(12) 0.0164(12) 0.0177(12) -0.0032(10) -0.0068(10) -0.0042(10) C5 0.0222(13) 0.0192(13) 0.0191(12) -0.0025(10) -0.0082(10) -0.0047(10) C6 0.0192(13) 0.0208(13) 0.0184(12) 0.0020(10) -0.0073(10) -0.0041(10) C7 0.0432(18) 0.0250(16) 0.0275(15) -0.0048(12) -0.0187(13) 0.0036(13) C8 0.052(2) 0.042(2) 0.0239(15) 0.0006(14) -0.0214(15) 0.0010(16) C9 0.0319(16) 0.0319(17) 0.0294(16) 0.0109(13) -0.0130(13) -0.0006(13) C10 0.0369(17) 0.0184(15) 0.0404(18) 0.0010(13) -0.0096(14) 0.0031(13) C11 0.0355(16) 0.0249(15) 0.0234(14) -0.0027(12) -0.0107(12) 0.0004(12) C12 0.0195(13) 0.0142(13) 0.0204(13) -0.0040(10) -0.0110(10) 0.0037(10) C13 0.0386(16) 0.0159(14) 0.0287(15) -0.0049(11) -0.0109(13) -0.0074(12) C14 0.0255(14) 0.0216(14) 0.0268(14) -0.0073(12) -0.0079(12) 0.0068(11) C15 0.0277(14) 0.0189(13) 0.0116(12) -0.0031(10) -0.0063(10) -0.0021(11) C16 0.0419(17) 0.0340(17) 0.0256(14) -0.0106(12) -0.0145(13) -0.0114(13) C17 0.0425(18) 0.0255(15) 0.0176(13) -0.0088(11) -0.0095(12) 0.0067(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 W1 N1 2.100(2) . ? W1 O1 2.1004(16) . ? W1 N2 2.104(2) . ? W1 O2 2.1056(17) . ? W1 W1 2.17294(17) 2_656 ? N1 C3 1.348(3) . ? N1 C12 1.479(3) . ? N2 C3 1.346(3) 2_656 ? N2 C15 1.475(3) . ? O1 C1 1.279(3) . ? O2 C1 1.278(3) 2_656 ? C1 O2 1.278(3) 2_656 ? C1 C2 1.496(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 N2 1.346(3) 2_656 ? C3 C4 1.443(3) . ? C4 C5 1.193(3) . ? C5 C6 1.439(3) . ? C6 C11 1.381(4) . ? C6 C7 1.399(4) . ? C7 C8 1.374(4) . ? C7 H7 0.95 . ? C8 C9 1.370(4) . ? C8 H8 0.95 . ? C9 C10 1.383(4) . ? C9 H9 0.95 . ? C10 C11 1.388(4) . ? C10 H10 0.95 . ? C11 H11 0.95 . ? C12 C14 1.519(4) . ? C12 C13 1.527(4) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.523(4) . ? C15 C16 1.528(4) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? 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 W1 O1 90.14(7) . . ? N1 W1 N2 175.92(7) . . ? O1 W1 N2 89.28(7) . . ? N1 W1 O2 89.91(7) . . ? O1 W1 O2 178.12(5) . . ? N2 W1 O2 90.54(7) . . ? N1 W1 W1 91.84(6) . 2_656 ? O1 W1 W1 91.12(5) . 2_656 ? N2 W1 W1 92.21(6) . 2_656 ? O2 W1 W1 90.75(5) . 2_656 ? C3 N1 C12 118.3(2) . . ? C3 N1 W1 118.69(17) . . ? C12 N1 W1 122.95(16) . . ? C3 N2 C15 118.0(2) 2_656 . ? C3 N2 W1 118.17(16) 2_656 . ? C15 N2 W1 123.74(16) . . ? C1 O1 W1 117.71(16) . . ? C1 O2 W1 117.83(15) 2_656 . ? O2 C1 O1 122.5(2) 2_656 . ? O2 C1 C2 119.2(2) 2_656 . ? O1 C1 C2 118.3(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 N1 119.1(2) 2_656 . ? N2 C3 C4 121.2(2) 2_656 . ? N1 C3 C4 119.7(2) . . ? C5 C4 C3 174.0(3) . . ? C4 C5 C6 175.6(3) . . ? C11 C6 C7 118.9(2) . . ? C11 C6 C5 119.6(2) . . ? C7 C6 C5 121.5(2) . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120 . . ? C6 C7 H7 120 . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C6 C11 C10 120.7(3) . . ? C6 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? N1 C12 C14 109.1(2) . . ? N1 C12 C13 111.0(2) . . ? C14 C12 C13 111.0(2) . . ? N1 C12 H12 108.5 . . ? C14 C12 H12 108.5 . . ? C13 C12 H12 108.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C17 109.2(2) . . ? N2 C15 C16 111.4(2) . . ? C17 C15 C16 110.2(2) . . ? N2 C15 H15 108.7 . . ? C17 C15 H15 108.7 . . ? C16 C15 H15 108.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 W1 N1 C3 91.14(18) . . . . ? O2 W1 N1 C3 -90.74(18) . . . . ? W1 W1 N1 C3 0.01(18) 2_656 . . . ? O1 W1 N1 C12 -85.36(18) . . . . ? O2 W1 N1 C12 92.76(18) . . . . ? W1 W1 N1 C12 -176.49(17) 2_656 . . . ? O1 W1 N2 C3 -92.25(18) . . . 2_656 ? O2 W1 N2 C3 89.62(18) . . . 2_656 ? W1 W1 N2 C3 -1.15(18) 2_656 . . 2_656 ? O1 W1 N2 C15 84.84(19) . . . . ? O2 W1 N2 C15 -93.29(19) . . . . ? W1 W1 N2 C15 175.93(18) 2_656 . . . ? N1 W1 O1 C1 -92.73(17) . . . . ? N2 W1 O1 C1 91.32(17) . . . . ? W1 W1 O1 C1 -0.88(16) 2_656 . . . ? N1 W1 O2 C1 90.70(17) . . . 2_656 ? N2 W1 O2 C1 -93.36(17) . . . 2_656 ? W1 W1 O2 C1 -1.14(16) 2_656 . . 2_656 ? W1 O1 C1 O2 2.0(3) . . . 2_656 ? W1 O1 C1 C2 -177.21(16) . . . . ? C12 N1 C3 N2 177.53(18) . . . 2_656 ? W1 N1 C3 N2 0.9(3) . . . 2_656 ? C12 N1 C3 C4 -3.3(3) . . . . ? W1 N1 C3 C4 -179.98(17) . . . . ? C11 C6 C7 C8 0.4(4) . . . . ? C5 C6 C7 C8 -179.2(3) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C7 C8 C9 C10 0.2(5) . . . . ? C8 C9 C10 C11 0.1(5) . . . . ? C7 C6 C11 C10 -0.2(4) . . . . ? C5 C6 C11 C10 179.5(3) . . . . ? C9 C10 C11 C6 -0.1(5) . . . . ? C3 N1 C12 C14 159.1(2) . . . . ? W1 N1 C12 C14 -24.4(3) . . . . ? C3 N1 C12 C13 -78.3(3) . . . . ? W1 N1 C12 C13 98.3(2) . . . . ? C3 N2 C15 C17 -156.8(2) 2_656 . . . ? W1 N2 C15 C17 26.1(3) . . . . ? C3 N2 C15 C16 81.3(3) 2_656 . . . ? W1 N2 C15 C16 -95.8(2) . . . . ? # END OF CIF data_Chisholm1272 _database_code_depnum_ccdc_archive 'CCDC 637929' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H52 Fe2 Mo2 N4 O4, 4(C4 H8 O)' _chemical_formula_sum 'C58 H84 Fe2 Mo2 N4 O8' _chemical_formula_weight 1268.87 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' Fe Fe 0.3463 0.8444 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1354(1) _cell_length_b 11.8625(1) _cell_length_c 12.3209(1) _cell_angle_alpha 67.157(1) _cell_angle_beta 78.161(1) _cell_angle_gamma 85.503(1) _cell_volume 1467.96(2) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6696 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'rhombus-shaped plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ;All work was done at 200 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.0, which means that 90% of the reflections were measured at least 3.0 times. A combination of phi and omega scans with a frame width of 1.0 degree was used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40640 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6736 _reflns_number_gt 5529 _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 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The two THF molecules are disordered and many restraints were used in their refinement, while trying to find suitable disordered models. These THF molecules were refined isotropically. 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 'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.9273P] 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 6736 _refine_ls_number_parameters 314 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.016 _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 Mo1 Mo 0.52169(2) 0.56297(2) 0.03264(2) 0.03029(10) Uani 1 1 d . . . Fe1 Fe 0.72737(4) -0.14793(4) 0.47636(4) 0.03327(12) Uani 1 1 d . . . N1 N 0.5930(2) 0.4266(2) 0.1748(2) 0.0313(5) Uani 1 1 d . . . N2 N 0.4552(2) 0.7134(2) -0.1031(2) 0.0314(5) Uani 1 1 d . . . O1 O 0.7001(2) 0.59191(19) -0.07631(19) 0.0381(5) Uani 1 1 d . . . O2 O 0.3460(2) 0.54364(19) 0.14580(18) 0.0382(5) Uani 1 1 d . . . C1 C 0.5920(3) 0.3105(3) 0.1831(2) 0.0294(6) Uani 1 1 d . . . C2 C 0.6406(3) 0.2132(3) 0.2779(3) 0.0329(6) Uani 1 1 d . . . C3 C 0.6804(3) 0.1308(3) 0.3546(3) 0.0337(6) Uani 1 1 d . . . C4 C 0.7247(3) 0.0327(3) 0.4500(3) 0.0337(6) Uani 1 1 d . . . C5 C 0.8468(3) -0.0131(3) 0.4490(3) 0.0427(7) Uani 1 1 d . . . H5 H 0.9148 0.0156 0.3847 0.051 Uiso 1 1 calc R . . C6 C 0.8481(3) -0.1099(3) 0.5622(3) 0.0490(8) Uani 1 1 d . . . H6 H 0.9179 -0.1566 0.5867 0.059 Uiso 1 1 calc R . . C7 C 0.7288(3) -0.1250(3) 0.6321(3) 0.0430(7) Uani 1 1 d . . . H7 H 0.7046 -0.1836 0.7112 0.052 Uiso 1 1 calc R . . C8 C 0.6514(3) -0.0377(3) 0.5640(3) 0.0371(7) Uani 1 1 d . . . H8 H 0.5661 -0.0276 0.5892 0.045 Uiso 1 1 calc R . . C9 C 0.6540(4) -0.1654(3) 0.3446(3) 0.0518(9) Uani 1 1 d . . . H9 H 0.6233 -0.1009 0.2823 0.062 Uiso 1 1 calc R . . C10 C 0.7749(4) -0.2081(4) 0.3393(4) 0.0628(11) Uani 1 1 d . . . H10 H 0.8403 -0.1776 0.2725 0.075 Uiso 1 1 calc R . . C11 C 0.7833(4) -0.3047(4) 0.4503(4) 0.0617(11) Uani 1 1 d . . . H11 H 0.8550 -0.3500 0.4713 0.074 Uiso 1 1 calc R . . C12 C 0.6654(4) -0.3210(3) 0.5237(3) 0.0539(9) Uani 1 1 d . . . H12 H 0.6432 -0.3797 0.6032 0.065 Uiso 1 1 calc R . . C13 C 0.5864(3) -0.2343(3) 0.4575(3) 0.0479(8) Uani 1 1 d . . . H13 H 0.5017 -0.2245 0.4851 0.057 Uiso 1 1 calc R . . C14 C 0.6499(3) 0.4544(3) 0.2605(3) 0.0368(7) Uani 1 1 d . . . H14 H 0.6321 0.3852 0.3403 0.044 Uiso 1 1 calc R . . C15 C 0.7883(4) 0.4670(4) 0.2189(4) 0.0631(11) Uani 1 1 d . . . H15A H 0.8223 0.3909 0.2117 0.095 Uiso 1 1 calc R . . H15B H 0.8244 0.4833 0.2776 0.095 Uiso 1 1 calc R . . H15C H 0.8073 0.5348 0.1408 0.095 Uiso 1 1 calc R . . C16 C 0.5927(4) 0.5693(3) 0.2739(4) 0.0567(10) Uani 1 1 d . . . H16A H 0.5039 0.5577 0.3015 0.085 Uiso 1 1 calc R . . H16B H 0.6093 0.6381 0.1962 0.085 Uiso 1 1 calc R . . H16C H 0.6279 0.5865 0.3325 0.085 Uiso 1 1 calc R . . C17 C 0.7288(3) 0.5301(3) -0.1425(3) 0.0394(7) Uani 1 1 d . . . C18 C 0.8529(3) 0.5462(4) -0.2203(3) 0.0552(9) Uani 1 1 d . . . H18A H 0.9000 0.6053 -0.2081 0.083 Uiso 1 1 calc R . . H18B H 0.8445 0.5765 -0.3046 0.083 Uiso 1 1 calc R . . H18C H 0.8958 0.4675 -0.1996 0.083 Uiso 1 1 calc R . . C19 C 0.4547(3) 0.8409(3) -0.1112(3) 0.0358(6) Uani 1 1 d . . . H19 H 0.4709 0.8966 -0.1978 0.043 Uiso 1 1 calc R . . C20 C 0.5571(4) 0.8574(3) -0.0531(3) 0.0515(9) Uani 1 1 d . . . H20A H 0.6359 0.8360 -0.0929 0.077 Uiso 1 1 calc R . . H20B H 0.5418 0.8040 0.0321 0.077 Uiso 1 1 calc R . . H20C H 0.5593 0.9428 -0.0613 0.077 Uiso 1 1 calc R . . C21 C 0.3309(4) 0.8738(3) -0.0515(3) 0.0526(9) Uani 1 1 d . . . H21A H 0.2665 0.8630 -0.0901 0.079 Uiso 1 1 calc R . . H21B H 0.3323 0.9593 -0.0596 0.079 Uiso 1 1 calc R . . H21C H 0.3143 0.8204 0.0338 0.079 Uiso 1 1 calc R . . O3 O 1.0344(6) 0.7049(6) -0.0312(6) 0.149(2) Uiso 1 1 d . A . C22 C 0.9880(6) 0.7618(6) 0.0587(6) 0.0912(16) Uiso 1 1 d D . . H22A H 1.0505 0.8151 0.0614 0.109 Uiso 0.35(3) 1 calc PR A 1 H22B H 0.9603 0.6993 0.1400 0.109 Uiso 0.35(3) 1 calc PR A 1 H22C H 1.0570 0.7816 0.0878 0.109 Uiso 0.65(3) 1 calc PR A 2 H22D H 0.9311 0.7055 0.1282 0.109 Uiso 0.65(3) 1 calc PR A 2 C23 C 1.0057(7) 0.7950(6) -0.1462(6) 0.1048(19) Uiso 1 1 d D . . H23A H 1.0729 0.8554 -0.1889 0.126 Uiso 0.35(3) 1 calc PR A 1 H23B H 0.9932 0.7534 -0.1988 0.126 Uiso 0.35(3) 1 calc PR A 1 H23C H 1.0817 0.8180 -0.2079 0.126 Uiso 0.65(3) 1 calc PR A 2 H23D H 0.9478 0.7586 -0.1747 0.126 Uiso 0.65(3) 1 calc PR A 2 C24 C 0.9063(15) 0.847(2) -0.1159(13) 0.091(7) Uiso 0.35(3) 1 d PD A 1 H24A H 0.8366 0.8128 -0.1314 0.110 Uiso 0.35(3) 1 calc PR A 1 H24B H 0.9116 0.9356 -0.1676 0.110 Uiso 0.35(3) 1 calc PR A 1 C25 C 0.8812(12) 0.8352(15) 0.0061(11) 0.069(5) Uiso 0.35(3) 1 d PD A 1 H25A H 0.8027 0.7915 0.0487 0.082 Uiso 0.35(3) 1 calc PR A 1 H25B H 0.8765 0.9164 0.0119 0.082 Uiso 0.35(3) 1 calc PR A 1 C24A C 0.9571(18) 0.8910(12) -0.1288(11) 0.126(5) Uiso 0.65(3) 1 d PD A 2 H24C H 0.8837 0.9143 -0.1665 0.152 Uiso 0.65(3) 1 calc PR A 2 H24D H 1.0165 0.9593 -0.1704 0.152 Uiso 0.65(3) 1 calc PR A 2 C25A C 0.922(2) 0.8773(18) -0.0066(13) 0.179(8) Uiso 0.65(3) 1 d PD A 2 H25C H 0.8318 0.8678 0.0205 0.215 Uiso 0.65(3) 1 calc PR A 2 H25D H 0.9485 0.9484 0.0057 0.215 Uiso 0.65(3) 1 calc PR A 2 O4 O 0.2695(12) 0.6652(12) 0.4148(11) 0.165(5) Uiso 0.520(12) 1 d PD B 3 C26 C 0.2898(10) 0.7779(10) 0.3126(10) 0.092(4) Uiso 0.520(12) 1 d PD B 3 H26A H 0.3523 0.7694 0.2463 0.110 Uiso 0.520(12) 1 calc PR B 3 H26B H 0.3138 0.8447 0.3332 0.110 Uiso 0.520(12) 1 calc PR B 3 C27 C 0.1599(12) 0.7972(13) 0.2825(15) 0.138(6) Uiso 0.520(12) 1 d PD B 3 H27A H 0.1184 0.8669 0.2999 0.166 Uiso 0.520(12) 1 calc PR B 3 H27B H 0.1632 0.8124 0.1971 0.166 Uiso 0.520(12) 1 calc PR B 3 C28 C 0.0945(11) 0.6781(11) 0.3637(10) 0.101(4) Uiso 0.520(12) 1 d PD B 3 H28A H 0.0052 0.6919 0.3829 0.121 Uiso 0.520(12) 1 calc PR B 3 H28B H 0.1079 0.6184 0.3242 0.121 Uiso 0.520(12) 1 calc PR B 3 C29 C 0.1479(13) 0.6312(19) 0.4758(12) 0.142(7) Uiso 0.520(12) 1 d PD B 3 H29A H 0.1157 0.6746 0.5301 0.171 Uiso 0.520(12) 1 calc PR B 3 H29B H 0.1378 0.5418 0.5199 0.171 Uiso 0.520(12) 1 calc PR B 3 O4A O 0.231(2) 0.721(2) 0.467(2) 0.299(13) Uiso 0.480(12) 1 d PD B 4 C26A C 0.313(2) 0.758(4) 0.352(3) 0.48(4) Uiso 0.480(12) 1 d PD B 4 H26C H 0.3341 0.6893 0.3247 0.578 Uiso 0.480(12) 1 calc PR B 4 H26D H 0.3886 0.7973 0.3508 0.578 Uiso 0.480(12) 1 calc PR B 4 C27A C 0.2234(13) 0.8489(14) 0.2835(13) 0.105(5) Uiso 0.480(12) 1 d PD B 4 H27C H 0.2357 0.9321 0.2798 0.126 Uiso 0.480(12) 1 calc PR B 4 H27D H 0.2333 0.8515 0.2008 0.126 Uiso 0.480(12) 1 calc PR B 4 C28A C 0.0997(12) 0.7994(15) 0.3556(15) 0.130(6) Uiso 0.480(12) 1 d PD B 4 H28C H 0.0478 0.7894 0.3036 0.156 Uiso 0.480(12) 1 calc PR B 4 H28D H 0.0580 0.8558 0.3930 0.156 Uiso 0.480(12) 1 calc PR B 4 C29A C 0.1216(19) 0.6759(16) 0.4518(18) 0.154(9) Uiso 0.480(12) 1 d PD B 4 H29C H 0.0561 0.6525 0.5244 0.184 Uiso 0.480(12) 1 calc PR B 4 H29D H 0.1374 0.6090 0.4216 0.184 Uiso 0.480(12) 1 calc PR B 4 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 Mo1 0.04046(17) 0.02427(14) 0.02813(15) -0.01037(10) -0.00857(10) -0.00388(10) Fe1 0.0361(2) 0.0295(2) 0.0333(2) -0.01057(18) -0.00671(18) -0.00193(17) N1 0.0399(14) 0.0269(11) 0.0290(12) -0.0105(9) -0.0092(10) -0.0048(10) N2 0.0413(14) 0.0232(11) 0.0300(12) -0.0097(9) -0.0072(10) -0.0034(10) O1 0.0408(12) 0.0353(11) 0.0355(11) -0.0091(9) -0.0075(9) -0.0074(9) O2 0.0452(12) 0.0367(11) 0.0329(11) -0.0140(9) -0.0066(9) 0.0008(9) C1 0.0343(15) 0.0266(13) 0.0251(13) -0.0085(11) -0.0027(11) -0.0037(11) C2 0.0387(16) 0.0284(14) 0.0320(14) -0.0112(12) -0.0064(12) -0.0046(12) C3 0.0391(16) 0.0311(15) 0.0325(14) -0.0128(12) -0.0064(12) -0.0069(12) C4 0.0413(16) 0.0276(14) 0.0343(14) -0.0104(12) -0.0128(12) -0.0043(12) C5 0.0347(17) 0.0403(17) 0.0499(19) -0.0111(14) -0.0107(14) -0.0065(13) C6 0.051(2) 0.0439(19) 0.056(2) -0.0140(16) -0.0289(17) 0.0009(15) C7 0.059(2) 0.0367(16) 0.0343(15) -0.0106(13) -0.0154(15) -0.0019(15) C8 0.0468(18) 0.0343(15) 0.0303(14) -0.0121(12) -0.0068(13) -0.0035(13) C9 0.078(3) 0.0425(18) 0.0451(19) -0.0211(16) -0.0254(18) -0.0014(18) C10 0.075(3) 0.069(3) 0.053(2) -0.040(2) 0.011(2) -0.019(2) C11 0.064(3) 0.047(2) 0.089(3) -0.040(2) -0.022(2) 0.0158(18) C12 0.079(3) 0.0328(17) 0.053(2) -0.0146(15) -0.0171(19) -0.0118(17) C13 0.0462(19) 0.0460(19) 0.063(2) -0.0306(17) -0.0130(17) -0.0058(15) C14 0.0466(17) 0.0349(15) 0.0324(15) -0.0126(12) -0.0125(13) -0.0080(13) C15 0.051(2) 0.082(3) 0.066(2) -0.035(2) -0.0121(19) -0.020(2) C16 0.080(3) 0.047(2) 0.061(2) -0.0320(18) -0.028(2) -0.0003(19) C17 0.0413(17) 0.0380(16) 0.0329(15) -0.0059(13) -0.0093(13) 0.0004(13) C18 0.045(2) 0.056(2) 0.054(2) -0.0127(18) -0.0037(16) 0.0016(17) C19 0.0481(18) 0.0276(14) 0.0337(15) -0.0131(12) -0.0084(13) -0.0020(12) C20 0.067(2) 0.0378(17) 0.061(2) -0.0248(16) -0.0240(19) -0.0024(16) C21 0.060(2) 0.0450(19) 0.056(2) -0.0265(17) -0.0055(17) 0.0060(17) _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 Mo1 Mo1 2.0779(4) 2_665 ? Mo1 N1 2.117(2) . ? Mo1 N2 2.125(2) . ? Mo1 O1 2.126(2) . ? Mo1 O2 2.128(2) . ? Fe1 C8 2.034(3) . ? Fe1 C11 2.037(4) . ? Fe1 C4 2.037(3) . ? Fe1 C10 2.038(4) . ? Fe1 C13 2.038(3) . ? Fe1 C12 2.040(3) . ? Fe1 C5 2.042(3) . ? Fe1 C7 2.043(3) . ? Fe1 C9 2.044(3) . ? Fe1 C6 2.044(3) . ? N1 C1 1.342(4) . ? N1 C14 1.484(4) . ? N2 C1 1.335(4) 2_665 ? N2 C19 1.476(4) . ? O1 C17 1.274(4) . ? O2 C17 1.272(4) 2_665 ? C1 N2 1.335(4) 2_665 ? C1 C2 1.450(4) . ? C2 C3 1.196(4) . ? C3 C4 1.437(4) . ? C4 C5 1.424(4) . ? C4 C8 1.436(4) . ? C5 C6 1.423(5) . ? C5 H5 0.9500 . ? C6 C7 1.408(5) . ? C6 H6 0.9500 . ? C7 C8 1.415(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.398(6) . ? C9 C13 1.398(5) . ? C9 H9 0.9500 . ? C10 C11 1.418(6) . ? C10 H10 0.9500 . ? C11 C12 1.414(6) . ? C11 H11 0.9500 . ? C12 C13 1.413(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C16 1.512(5) . ? C14 C15 1.520(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O2 1.272(4) 2_665 ? C17 C18 1.490(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.522(5) . ? C19 C20 1.526(5) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O3 C23 1.486(8) . ? O3 C22 1.497(8) . ? C22 C25A 1.516(11) . ? C22 C25 1.519(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 H22C 0.9900 . ? C22 H22D 0.9900 . ? C23 C24 1.286(10) . ? C23 C24A 1.297(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 H23C 0.9900 . ? C23 H23D 0.9900 . ? C24 C25 1.422(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C24A C25A 1.423(11) . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? O4 C29 1.412(9) . ? O4 C26 1.431(9) . ? C26 C27 1.545(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.514(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.504(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O4A C26A 1.437(10) . ? O4A C29A 1.447(10) . ? C26A C27A 1.534(10) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27A C28A 1.500(9) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C28A C29A 1.524(10) . ? C28A H28C 0.9900 . ? C28A H28D 0.9900 . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? 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 Mo1 Mo1 N1 92.90(6) 2_665 . ? Mo1 Mo1 N2 93.16(6) 2_665 . ? N1 Mo1 N2 173.94(8) . . ? Mo1 Mo1 O1 92.10(6) 2_665 . ? N1 Mo1 O1 89.85(9) . . ? N2 Mo1 O1 89.83(9) . . ? Mo1 Mo1 O2 91.92(6) 2_665 . ? N1 Mo1 O2 90.18(9) . . ? N2 Mo1 O2 89.71(9) . . ? O1 Mo1 O2 175.97(8) . . ? C8 Fe1 C11 158.93(16) . . ? C8 Fe1 C4 41.31(12) . . ? C11 Fe1 C4 158.51(16) . . ? C8 Fe1 C10 158.20(17) . . ? C11 Fe1 C10 40.72(18) . . ? C4 Fe1 C10 122.75(15) . . ? C8 Fe1 C13 106.97(14) . . ? C11 Fe1 C13 68.07(16) . . ? C4 Fe1 C13 123.51(14) . . ? C10 Fe1 C13 67.43(16) . . ? C8 Fe1 C12 122.40(15) . . ? C11 Fe1 C12 40.58(18) . . ? C4 Fe1 C12 159.51(15) . . ? C10 Fe1 C12 68.02(16) . . ? C13 Fe1 C12 40.55(15) . . ? C8 Fe1 C5 69.06(13) . . ? C11 Fe1 C5 122.58(16) . . ? C4 Fe1 C5 40.85(13) . . ? C10 Fe1 C5 108.64(16) . . ? C13 Fe1 C5 160.21(14) . . ? C12 Fe1 C5 157.98(15) . . ? C8 Fe1 C7 40.61(13) . . ? C11 Fe1 C7 123.17(16) . . ? C4 Fe1 C7 68.73(12) . . ? C10 Fe1 C7 160.45(18) . . ? C13 Fe1 C7 121.75(15) . . ? C12 Fe1 C7 106.81(14) . . ? C5 Fe1 C7 68.65(14) . . ? C8 Fe1 C9 122.15(15) . . ? C11 Fe1 C9 68.12(16) . . ? C4 Fe1 C9 108.02(13) . . ? C10 Fe1 C9 40.06(17) . . ? C13 Fe1 C9 40.06(15) . . ? C12 Fe1 C9 67.97(15) . . ? C5 Fe1 C9 124.46(15) . . ? C7 Fe1 C9 157.40(16) . . ? C8 Fe1 C6 68.21(15) . . ? C11 Fe1 C6 108.04(17) . . ? C4 Fe1 C6 68.37(13) . . ? C10 Fe1 C6 125.10(18) . . ? C13 Fe1 C6 157.43(15) . . ? C12 Fe1 C6 121.98(15) . . ? C5 Fe1 C6 40.77(14) . . ? C7 Fe1 C6 40.31(15) . . ? C9 Fe1 C6 161.15(16) . . ? C1 N1 C14 118.9(2) . . ? C1 N1 Mo1 117.86(18) . . ? C14 N1 Mo1 123.18(19) . . ? C1 N2 C19 118.7(2) 2_665 . ? C1 N2 Mo1 117.43(18) 2_665 . ? C19 N2 Mo1 123.87(19) . . ? C17 O1 Mo1 116.9(2) . . ? C17 O2 Mo1 117.1(2) 2_665 . ? N2 C1 N1 118.6(2) 2_665 . ? N2 C1 C2 120.9(2) 2_665 . ? N1 C1 C2 120.4(3) . . ? C3 C2 C1 178.2(3) . . ? C2 C3 C4 177.9(3) . . ? C5 C4 C8 107.8(3) . . ? C5 C4 C3 126.9(3) . . ? C8 C4 C3 125.3(3) . . ? C5 C4 Fe1 69.76(18) . . ? C8 C4 Fe1 69.23(17) . . ? C3 C4 Fe1 126.0(2) . . ? C6 C5 C4 107.3(3) . . ? C6 C5 Fe1 69.70(19) . . ? C4 C5 Fe1 69.40(17) . . ? C6 C5 H5 126.3 . . ? C4 C5 H5 126.3 . . ? Fe1 C5 H5 126.1 . . ? C7 C6 C5 108.9(3) . . ? C7 C6 Fe1 69.79(18) . . ? C5 C6 Fe1 69.53(18) . . ? C7 C6 H6 125.6 . . ? C5 C6 H6 125.6 . . ? Fe1 C6 H6 126.7 . . ? C6 C7 C8 108.2(3) . . ? C6 C7 Fe1 69.90(19) . . ? C8 C7 Fe1 69.37(18) . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe1 C7 H7 126.4 . . ? C7 C8 C4 107.8(3) . . ? C7 C8 Fe1 70.03(19) . . ? C4 C8 Fe1 69.46(17) . . ? C7 C8 H8 126.1 . . ? C4 C8 H8 126.1 . . ? Fe1 C8 H8 126.0 . . ? C10 C9 C13 108.0(3) . . ? C10 C9 Fe1 69.7(2) . . ? C13 C9 Fe1 69.73(19) . . ? C10 C9 H9 126.0 . . ? C13 C9 H9 126.0 . . ? Fe1 C9 H9 126.1 . . ? C9 C10 C11 108.5(4) . . ? C9 C10 Fe1 70.2(2) . . ? C11 C10 Fe1 69.6(2) . . ? C9 C10 H10 125.7 . . ? C11 C10 H10 125.7 . . ? Fe1 C10 H10 126.0 . . ? C12 C11 C10 107.3(4) . . ? C12 C11 Fe1 69.8(2) . . ? C10 C11 Fe1 69.7(2) . . ? C12 C11 H11 126.3 . . ? C10 C11 H11 126.3 . . ? Fe1 C11 H11 125.8 . . ? C13 C12 C11 107.6(3) . . ? C13 C12 Fe1 69.67(19) . . ? C11 C12 Fe1 69.6(2) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? Fe1 C12 H12 126.1 . . ? C9 C13 C12 108.6(3) . . ? C9 C13 Fe1 70.2(2) . . ? C12 C13 Fe1 69.8(2) . . ? C9 C13 H13 125.7 . . ? C12 C13 H13 125.7 . . ? Fe1 C13 H13 125.9 . . ? N1 C14 C16 109.1(3) . . ? N1 C14 C15 110.7(3) . . ? C16 C14 C15 111.6(3) . . ? N1 C14 H14 108.5 . . ? C16 C14 H14 108.5 . . ? C15 C14 H14 108.5 . . ? 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 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 O1 122.0(3) 2_665 . ? O2 C17 C18 118.7(3) 2_665 . ? O1 C17 C18 119.3(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C21 111.0(3) . . ? N2 C19 C20 109.2(3) . . ? C21 C19 C20 110.7(3) . . ? N2 C19 H19 108.6 . . ? C21 C19 H19 108.6 . . ? C20 C19 H19 108.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 O3 C22 105.0(5) . . ? O3 C22 C25A 105.7(7) . . ? O3 C22 C25 99.8(7) . . ? O3 C22 H22A 111.8 . . ? C25 C22 H22A 111.8 . . ? O3 C22 H22B 111.8 . . ? C25 C22 H22B 111.8 . . ? H22A C22 H22B 109.5 . . ? O3 C22 H22C 110.6 . . ? C25A C22 H22C 110.6 . . ? O3 C22 H22D 110.6 . . ? C25A C22 H22D 110.6 . . ? H22C C22 H22D 108.7 . . ? C24 C23 O3 104.9(9) . . ? C24A C23 O3 108.7(8) . . ? C24 C23 H23A 110.8 . . ? O3 C23 H23A 110.8 . . ? C24 C23 H23B 110.8 . . ? O3 C23 H23B 110.8 . . ? H23A C23 H23B 108.8 . . ? C24A C23 H23C 109.9 . . ? O3 C23 H23C 109.9 . . ? C24A C23 H23D 109.9 . . ? O3 C23 H23D 109.9 . . ? H23C C23 H23D 108.3 . . ? C23 C24 C25 114.5(12) . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24A 108.6 . . ? C23 C24 H24B 108.6 . . ? C25 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C22 105.0(10) . . ? C24 C25 H25A 110.7 . . ? C22 C25 H25A 110.7 . . ? C24 C25 H25B 110.7 . . ? C22 C25 H25B 110.7 . . ? H25A C25 H25B 108.8 . . ? C23 C24A C25A 115.3(11) . . ? C23 C24A H24C 108.4 . . ? C25A C24A H24C 108.4 . . ? C23 C24A H24D 108.4 . . ? C25A C24A H24D 108.4 . . ? H24C C24A H24D 107.5 . . ? C24A C25A C22 103.1(10) . . ? C24A C25A H25C 111.2 . . ? C22 C25A H25C 111.2 . . ? C24A C25A H25D 111.1 . . ? C22 C25A H25D 111.1 . . ? H25C C25A H25D 109.1 . . ? C29 O4 C26 118.7(12) . . ? O4 C26 C27 99.1(9) . . ? O4 C26 H26A 111.9 . . ? C27 C26 H26A 112.0 . . ? O4 C26 H26B 112.0 . . ? C27 C26 H26B 111.9 . . ? H26A C26 H26B 109.6 . . ? C28 C27 C26 103.8(10) . . ? C28 C27 H27A 111.0 . . ? C26 C27 H27A 111.0 . . ? C28 C27 H27B 111.0 . . ? C26 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? C29 C28 C27 106.4(12) . . ? C29 C28 H28A 110.5 . . ? C27 C28 H28A 110.5 . . ? C29 C28 H28B 110.4 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.6 . . ? O4 C29 C28 94.7(10) . . ? O4 C29 H29A 112.8 . . ? C28 C29 H29A 112.8 . . ? O4 C29 H29B 112.8 . . ? C28 C29 H29B 112.8 . . ? H29A C29 H29B 110.2 . . ? C26A O4A C29A 106.1(18) . . ? O4A C26A C27A 95.2(17) . . ? O4A C26A H26C 112.7 . . ? C27A C26A H26C 112.7 . . ? O4A C26A H26D 112.7 . . ? C27A C26A H26D 112.7 . . ? H26C C26A H26D 110.2 . . ? C28A C27A C26A 103.5(14) . . ? C28A C27A H27C 111.0 . . ? C26A C27A H27C 111.1 . . ? C28A C27A H27D 111.1 . . ? C26A C27A H27D 111.1 . . ? H27C C27A H27D 109.0 . . ? C27A C28A C29A 106.8(12) . . ? C27A C28A H28C 110.4 . . ? C29A C28A H28C 110.4 . . ? C27A C28A H28D 110.4 . . ? C29A C28A H28D 110.4 . . ? H28C C28A H28D 108.6 . . ? O4A C29A C28A 91.3(10) . . ? O4A C29A H29C 113.4 . . ? C28A C29A H29C 113.4 . . ? O4A C29A H29D 113.4 . . ? C28A C29A H29D 113.4 . . ? H29C C29A H29D 110.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo1 Mo1 N1 C1 0.4(2) 2_665 . . . ? O1 Mo1 N1 C1 -91.7(2) . . . . ? O2 Mo1 N1 C1 92.3(2) . . . . ? Mo1 Mo1 N1 C14 176.8(2) 2_665 . . . ? O1 Mo1 N1 C14 84.7(2) . . . . ? O2 Mo1 N1 C14 -91.3(2) . . . . ? Mo1 Mo1 N2 C1 0.6(2) 2_665 . . 2_665 ? O1 Mo1 N2 C1 92.7(2) . . . 2_665 ? O2 Mo1 N2 C1 -91.3(2) . . . 2_665 ? Mo1 Mo1 N2 C19 178.6(2) 2_665 . . . ? O1 Mo1 N2 C19 -89.3(2) . . . . ? O2 Mo1 N2 C19 86.7(2) . . . . ? Mo1 Mo1 O1 C17 -1.0(2) 2_665 . . . ? N1 Mo1 O1 C17 91.9(2) . . . . ? N2 Mo1 O1 C17 -94.1(2) . . . . ? Mo1 Mo1 O2 C17 -0.4(2) 2_665 . . 2_665 ? N1 Mo1 O2 C17 -93.3(2) . . . 2_665 ? N2 Mo1 O2 C17 92.7(2) . . . 2_665 ? C14 N1 C1 N2 -177.5(2) . . . 2_665 ? Mo1 N1 C1 N2 -1.0(4) . . . 2_665 ? C14 N1 C1 C2 2.9(4) . . . . ? Mo1 N1 C1 C2 179.4(2) . . . . ? C8 Fe1 C4 C5 119.2(3) . . . . ? C11 Fe1 C4 C5 -46.3(5) . . . . ? C10 Fe1 C4 C5 -80.6(2) . . . . ? C13 Fe1 C4 C5 -163.7(2) . . . . ? C12 Fe1 C4 C5 162.6(4) . . . . ? C7 Fe1 C4 C5 81.5(2) . . . . ? C9 Fe1 C4 C5 -122.2(2) . . . . ? C6 Fe1 C4 C5 38.1(2) . . . . ? C11 Fe1 C4 C8 -165.6(4) . . . . ? C10 Fe1 C4 C8 160.1(2) . . . . ? C13 Fe1 C4 C8 77.1(2) . . . . ? C12 Fe1 C4 C8 43.4(4) . . . . ? C5 Fe1 C4 C8 -119.2(3) . . . . ? C7 Fe1 C4 C8 -37.70(19) . . . . ? C9 Fe1 C4 C8 118.5(2) . . . . ? C6 Fe1 C4 C8 -81.2(2) . . . . ? C8 Fe1 C4 C3 -119.2(3) . . . . ? C11 Fe1 C4 C3 75.2(5) . . . . ? C10 Fe1 C4 C3 40.9(3) . . . . ? C13 Fe1 C4 C3 -42.1(3) . . . . ? C12 Fe1 C4 C3 -75.9(5) . . . . ? C5 Fe1 C4 C3 121.5(4) . . . . ? C7 Fe1 C4 C3 -156.9(3) . . . . ? C9 Fe1 C4 C3 -0.7(3) . . . . ? C6 Fe1 C4 C3 159.6(3) . . . . ? C8 C4 C5 C6 -0.6(4) . . . . ? C3 C4 C5 C6 179.9(3) . . . . ? Fe1 C4 C5 C6 -59.6(2) . . . . ? C8 C4 C5 Fe1 59.0(2) . . . . ? C3 C4 C5 Fe1 -120.4(3) . . . . ? C8 Fe1 C5 C6 80.5(2) . . . . ? C11 Fe1 C5 C6 -79.7(3) . . . . ? C4 Fe1 C5 C6 118.6(3) . . . . ? C10 Fe1 C5 C6 -122.5(3) . . . . ? C13 Fe1 C5 C6 162.4(4) . . . . ? C12 Fe1 C5 C6 -45.2(5) . . . . ? C7 Fe1 C5 C6 36.8(2) . . . . ? C9 Fe1 C5 C6 -164.1(2) . . . . ? C8 Fe1 C5 C4 -38.07(18) . . . . ? C11 Fe1 C5 C4 161.7(2) . . . . ? C10 Fe1 C5 C4 118.9(2) . . . . ? C13 Fe1 C5 C4 43.9(5) . . . . ? C12 Fe1 C5 C4 -163.8(4) . . . . ? C7 Fe1 C5 C4 -81.8(2) . . . . ? C9 Fe1 C5 C4 77.3(2) . . . . ? C6 Fe1 C5 C4 -118.6(3) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? Fe1 C5 C6 C7 -58.9(2) . . . . ? C4 C5 C6 Fe1 59.4(2) . . . . ? C8 Fe1 C6 C7 37.56(19) . . . . ? C11 Fe1 C6 C7 -120.4(2) . . . . ? C4 Fe1 C6 C7 82.2(2) . . . . ? C10 Fe1 C6 C7 -162.2(2) . . . . ? C13 Fe1 C6 C7 -44.2(5) . . . . ? C12 Fe1 C6 C7 -77.9(3) . . . . ? C5 Fe1 C6 C7 120.3(3) . . . . ? C9 Fe1 C6 C7 164.7(4) . . . . ? C8 Fe1 C6 C5 -82.8(2) . . . . ? C11 Fe1 C6 C5 119.3(2) . . . . ? C4 Fe1 C6 C5 -38.2(2) . . . . ? C10 Fe1 C6 C5 77.5(3) . . . . ? C13 Fe1 C6 C5 -164.6(3) . . . . ? C12 Fe1 C6 C5 161.7(2) . . . . ? C7 Fe1 C6 C5 -120.3(3) . . . . ? C9 Fe1 C6 C5 44.3(5) . . . . ? C5 C6 C7 C8 -0.3(4) . . . . ? Fe1 C6 C7 C8 -59.0(2) . . . . ? C5 C6 C7 Fe1 58.7(2) . . . . ? C8 Fe1 C7 C6 -119.6(3) . . . . ? C11 Fe1 C7 C6 78.6(3) . . . . ? C4 Fe1 C7 C6 -81.2(2) . . . . ? C10 Fe1 C7 C6 48.4(5) . . . . ? C13 Fe1 C7 C6 161.7(2) . . . . ? C12 Fe1 C7 C6 119.9(2) . . . . ? C5 Fe1 C7 C6 -37.2(2) . . . . ? C9 Fe1 C7 C6 -167.1(3) . . . . ? C11 Fe1 C7 C8 -161.9(2) . . . . ? C4 Fe1 C7 C8 38.33(19) . . . . ? C10 Fe1 C7 C8 168.0(4) . . . . ? C13 Fe1 C7 C8 -78.8(2) . . . . ? C12 Fe1 C7 C8 -120.5(2) . . . . ? C5 Fe1 C7 C8 82.3(2) . . . . ? C9 Fe1 C7 C8 -47.6(4) . . . . ? C6 Fe1 C7 C8 119.6(3) . . . . ? C6 C7 C8 C4 -0.1(4) . . . . ? Fe1 C7 C8 C4 -59.4(2) . . . . ? C6 C7 C8 Fe1 59.3(2) . . . . ? C5 C4 C8 C7 0.5(3) . . . . ? C3 C4 C8 C7 179.9(3) . . . . ? Fe1 C4 C8 C7 59.8(2) . . . . ? C5 C4 C8 Fe1 -59.3(2) . . . . ? C3 C4 C8 Fe1 120.1(3) . . . . ? C11 Fe1 C8 C7 46.4(5) . . . . ? C4 Fe1 C8 C7 -118.9(3) . . . . ? C10 Fe1 C8 C7 -169.2(4) . . . . ? C13 Fe1 C8 C7 119.3(2) . . . . ? C12 Fe1 C8 C7 77.7(2) . . . . ? C5 Fe1 C8 C7 -81.2(2) . . . . ? C9 Fe1 C8 C7 160.4(2) . . . . ? C6 Fe1 C8 C7 -37.3(2) . . . . ? C11 Fe1 C8 C4 165.3(4) . . . . ? C10 Fe1 C8 C4 -50.3(5) . . . . ? C13 Fe1 C8 C4 -121.81(19) . . . . ? C12 Fe1 C8 C4 -163.46(19) . . . . ? C5 Fe1 C8 C4 37.66(18) . . . . ? C7 Fe1 C8 C4 118.9(3) . . . . ? C9 Fe1 C8 C4 -80.7(2) . . . . ? C6 Fe1 C8 C4 81.6(2) . . . . ? C8 Fe1 C9 C10 163.0(2) . . . . ? C11 Fe1 C9 C10 -37.7(2) . . . . ? C4 Fe1 C9 C10 119.8(2) . . . . ? C13 Fe1 C9 C10 -119.2(3) . . . . ? C12 Fe1 C9 C10 -81.6(3) . . . . ? C5 Fe1 C9 C10 77.7(3) . . . . ? C7 Fe1 C9 C10 -162.4(3) . . . . ? C6 Fe1 C9 C10 44.1(5) . . . . ? C8 Fe1 C9 C13 -77.8(2) . . . . ? C11 Fe1 C9 C13 81.5(2) . . . . ? C4 Fe1 C9 C13 -121.0(2) . . . . ? C10 Fe1 C9 C13 119.2(3) . . . . ? C12 Fe1 C9 C13 37.6(2) . . . . ? C5 Fe1 C9 C13 -163.1(2) . . . . ? C7 Fe1 C9 C13 -43.2(5) . . . . ? C6 Fe1 C9 C13 163.3(4) . . . . ? C13 C9 C10 C11 -0.2(4) . . . . ? Fe1 C9 C10 C11 59.3(3) . . . . ? C13 C9 C10 Fe1 -59.4(2) . . . . ? C8 Fe1 C10 C9 -41.7(5) . . . . ? C11 Fe1 C10 C9 119.6(3) . . . . ? C4 Fe1 C10 C9 -78.9(3) . . . . ? C13 Fe1 C10 C9 37.5(2) . . . . ? C12 Fe1 C10 C9 81.5(2) . . . . ? C5 Fe1 C10 C9 -121.8(2) . . . . ? C7 Fe1 C10 C9 159.7(4) . . . . ? C6 Fe1 C10 C9 -164.1(2) . . . . ? C8 Fe1 C10 C11 -161.3(4) . . . . ? C4 Fe1 C10 C11 161.6(2) . . . . ? C13 Fe1 C10 C11 -82.1(3) . . . . ? C12 Fe1 C10 C11 -38.1(2) . . . . ? C5 Fe1 C10 C11 118.6(2) . . . . ? C7 Fe1 C10 C11 40.1(6) . . . . ? C9 Fe1 C10 C11 -119.6(3) . . . . ? C6 Fe1 C10 C11 76.3(3) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? Fe1 C10 C11 C12 59.9(3) . . . . ? C9 C10 C11 Fe1 -59.6(3) . . . . ? C8 Fe1 C11 C12 42.3(5) . . . . ? C4 Fe1 C11 C12 -164.9(3) . . . . ? C10 Fe1 C11 C12 -118.3(4) . . . . ? C13 Fe1 C11 C12 -37.9(2) . . . . ? C5 Fe1 C11 C12 160.9(2) . . . . ? C7 Fe1 C11 C12 76.6(3) . . . . ? C9 Fe1 C11 C12 -81.2(3) . . . . ? C6 Fe1 C11 C12 118.4(2) . . . . ? C8 Fe1 C11 C10 160.6(4) . . . . ? C4 Fe1 C11 C10 -46.6(5) . . . . ? C13 Fe1 C11 C10 80.4(3) . . . . ? C12 Fe1 C11 C10 118.3(4) . . . . ? C5 Fe1 C11 C10 -80.7(3) . . . . ? C7 Fe1 C11 C10 -165.1(2) . . . . ? C9 Fe1 C11 C10 37.1(2) . . . . ? C6 Fe1 C11 C10 -123.3(3) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? Fe1 C11 C12 C13 59.6(2) . . . . ? C10 C11 C12 Fe1 -59.8(3) . . . . ? C8 Fe1 C12 C13 77.9(3) . . . . ? C11 Fe1 C12 C13 -118.8(3) . . . . ? C4 Fe1 C12 C13 45.4(5) . . . . ? C10 Fe1 C12 C13 -80.5(3) . . . . ? C5 Fe1 C12 C13 -166.0(4) . . . . ? C7 Fe1 C12 C13 119.5(2) . . . . ? C9 Fe1 C12 C13 -37.2(2) . . . . ? C6 Fe1 C12 C13 160.9(2) . . . . ? C8 Fe1 C12 C11 -163.3(2) . . . . ? C4 Fe1 C12 C11 164.2(4) . . . . ? C10 Fe1 C12 C11 38.3(3) . . . . ? C13 Fe1 C12 C11 118.8(3) . . . . ? C5 Fe1 C12 C11 -47.2(5) . . . . ? C7 Fe1 C12 C11 -121.7(2) . . . . ? C9 Fe1 C12 C11 81.6(3) . . . . ? C6 Fe1 C12 C11 -80.3(3) . . . . ? C10 C9 C13 C12 0.0(4) . . . . ? Fe1 C9 C13 C12 -59.4(2) . . . . ? C10 C9 C13 Fe1 59.4(2) . . . . ? C11 C12 C13 C9 0.2(4) . . . . ? Fe1 C12 C13 C9 59.7(2) . . . . ? C11 C12 C13 Fe1 -59.5(3) . . . . ? C8 Fe1 C13 C9 120.1(2) . . . . ? C11 Fe1 C13 C9 -81.6(3) . . . . ? C4 Fe1 C13 C9 77.8(3) . . . . ? C10 Fe1 C13 C9 -37.5(2) . . . . ? C12 Fe1 C13 C9 -119.6(3) . . . . ? C5 Fe1 C13 C9 44.9(5) . . . . ? C7 Fe1 C13 C9 162.0(2) . . . . ? C6 Fe1 C13 C9 -166.0(4) . . . . ? C8 Fe1 C13 C12 -120.3(2) . . . . ? C11 Fe1 C13 C12 37.9(2) . . . . ? C4 Fe1 C13 C12 -162.6(2) . . . . ? C10 Fe1 C13 C12 82.1(3) . . . . ? C5 Fe1 C13 C12 164.5(4) . . . . ? C7 Fe1 C13 C12 -78.5(3) . . . . ? C9 Fe1 C13 C12 119.6(3) . . . . ? C6 Fe1 C13 C12 -46.4(5) . . . . ? C1 N1 C14 C16 -154.3(3) . . . . ? Mo1 N1 C14 C16 29.3(4) . . . . ? C1 N1 C14 C15 82.5(4) . . . . ? Mo1 N1 C14 C15 -93.9(3) . . . . ? Mo1 O1 C17 O2 1.5(4) . . . 2_665 ? Mo1 O1 C17 C18 -179.7(2) . . . . ? C1 N2 C19 C21 82.4(3) 2_665 . . . ? Mo1 N2 C19 C21 -95.6(3) . . . . ? C1 N2 C19 C20 -155.3(3) 2_665 . . . ? Mo1 N2 C19 C20 26.8(3) . . . . ? C23 O3 C22 C25A 6.0(14) . . . . ? C23 O3 C22 C25 30.7(9) . . . . ? C22 O3 C23 C24 -32.0(14) . . . . ? C22 O3 C23 C24A 2.9(13) . . . . ? C24A C23 C24 C25 -82(2) . . . . ? O3 C23 C24 C25 19(2) . . . . ? C23 C24 C25 C22 1(2) . . . . ? O3 C22 C25 C24 -20.0(14) . . . . ? C25A C22 C25 C24 86(2) . . . . ? C24 C23 C24A C25A 77.0(19) . . . . ? O3 C23 C24A C25A -11.9(18) . . . . ? C23 C24A C25A C22 15(2) . . . . ? O3 C22 C25A C24A -11.9(17) . . . . ? C25 C22 C25A C24A -91(2) . . . . ? C29 O4 C26 C27 -19.6(19) . . . . ? O4 C26 C27 C28 -9.0(16) . . . . ? C26 C27 C28 C29 32.0(17) . . . . ? C26 O4 C29 C28 38.1(19) . . . . ? C27 C28 C29 O4 -39.8(17) . . . . ? C29A O4A C26A C27A 57(3) . . . . ? O4A C26A C27A C28A -27(3) . . . . ? C26A C27A C28A C29A -7(3) . . . . ? C26A O4A C29A C28A -60(2) . . . . ? C27A C28A C29A O4A 37(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.232 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.090 #END OF CIF data_Chisholm1321 _database_code_depnum_ccdc_archive 'CCDC 637930' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H52 Fe2 N4 O4 W2, 4(C4 H8 O)' _chemical_formula_sum 'C58 H84 Fe2 N4 O8 W2' _chemical_formula_weight 1444.69 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' Fe Fe 0.3463 0.8444 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0512(1) _cell_length_b 11.8155(1) _cell_length_c 12.2514(1) _cell_angle_alpha 67.331(4) _cell_angle_beta 77.860(4) _cell_angle_gamma 85.531(4) _cell_volume 1443.13(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6595 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'triangular-shaped plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 4.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.342 _exptl_absorpt_correction_T_max 0.508 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a hemisphere of reciprocal space with a redundancy factor of 3.1, which means that 90% of the reflections were measured at least 3.1 times. A combination of phi and omega scans with a frame width of 1.0 degree was used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40553 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6607 _reflns_number_gt 5787 _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 (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The two THF molecules are disordered and bond length restraints (SADI) were used in their refinement. They were refined only isotropically. The largest peaks in the final difference map range from 2.02 to 1.03 e/A**3 and are in the immediate vicinity of these THF molecules. 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 'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+2.7915P] 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 6607 _refine_ls_number_parameters 284 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.002 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 W1 W 0.522527(16) 0.566043(14) 0.534492(14) 0.02364(7) Uani 1 1 d . . . Fe1 Fe 0.72781(6) -0.14673(6) 0.97595(6) 0.02546(14) Uani 1 1 d . . . N1 N 0.5927(3) 0.4288(3) 0.6743(3) 0.0232(7) Uani 1 1 d . . . N2 N 0.4558(3) 0.7121(3) 0.3988(3) 0.0241(7) Uani 1 1 d . . . O1 O 0.3461(3) 0.5441(3) 0.6460(3) 0.0292(7) Uani 1 1 d . . . O2 O 0.6997(3) 0.5925(3) 0.4246(3) 0.0292(7) Uani 1 1 d . . . C1 C 0.5919(4) 0.3115(4) 0.6825(4) 0.0228(8) Uani 1 1 d . . . C2 C 0.6404(4) 0.2150(4) 0.7767(4) 0.0270(9) Uani 1 1 d . . . C3 C 0.6806(4) 0.1320(4) 0.8540(4) 0.0278(9) Uani 1 1 d . . . C4 C 0.7248(4) 0.0348(4) 0.9493(4) 0.0270(9) Uani 1 1 d . . . C5 C 0.8481(4) -0.0119(4) 0.9490(5) 0.0335(10) Uani 1 1 d . . . H5 H 0.9171 0.0167 0.8843 0.040 Uiso 1 1 calc R . . C6 C 0.8492(5) -0.1081(5) 1.0620(5) 0.0381(11) Uani 1 1 d . . . H6 H 0.9197 -0.1546 1.0864 0.046 Uiso 1 1 calc R . . C7 C 0.7292(5) -0.1237(4) 1.1321(4) 0.0342(11) Uani 1 1 d . . . H7 H 0.7047 -0.1832 1.2113 0.041 Uiso 1 1 calc R . . C8 C 0.6508(4) -0.0362(4) 1.0649(4) 0.0285(9) Uani 1 1 d . . . H8 H 0.5649 -0.0259 1.0912 0.034 Uiso 1 1 calc R . . C9 C 0.6555(5) -0.1638(5) 0.8427(4) 0.0393(12) Uani 1 1 d . . . H9 H 0.6251 -0.0986 0.7805 0.047 Uiso 1 1 calc R . . C10 C 0.7767(6) -0.2065(5) 0.8365(5) 0.0477(14) Uani 1 1 d . . . H10 H 0.8430 -0.1759 0.7694 0.057 Uiso 1 1 calc R . . C11 C 0.7838(5) -0.3038(5) 0.9482(6) 0.0474(14) Uani 1 1 d . . . H11 H 0.8558 -0.3497 0.9691 0.057 Uiso 1 1 calc R . . C12 C 0.6640(5) -0.3204(4) 1.0232(5) 0.0390(12) Uani 1 1 d . . . H12 H 0.6414 -0.3792 1.1030 0.047 Uiso 1 1 calc R . . C13 C 0.5852(5) -0.2334(4) 0.9569(5) 0.0347(11) Uani 1 1 d . . . H13 H 0.4996 -0.2234 0.9844 0.042 Uiso 1 1 calc R . . C14 C 0.6483(4) 0.4552(4) 0.7616(4) 0.0283(9) Uani 1 1 d . . . H14 H 0.6285 0.3855 0.8414 0.034 Uiso 1 1 calc R . . C15 C 0.7878(5) 0.4666(6) 0.7221(5) 0.0475(14) Uani 1 1 d . . . H15A H 0.8219 0.3905 0.7139 0.071 Uiso 1 1 calc R . . H15B H 0.8229 0.4813 0.7826 0.071 Uiso 1 1 calc R . . H15C H 0.8089 0.5353 0.6444 0.071 Uiso 1 1 calc R . . C16 C 0.5927(6) 0.5709(5) 0.7758(5) 0.0420(12) Uani 1 1 d . . . H16A H 0.5027 0.5611 0.8021 0.063 Uiso 1 1 calc R . . H16B H 0.6119 0.6403 0.6984 0.063 Uiso 1 1 calc R . . H16C H 0.6273 0.5862 0.8362 0.063 Uiso 1 1 calc R . . C17 C 0.2703(4) 0.4689(4) 0.6433(4) 0.0301(10) Uani 1 1 d . . . C18 C 0.1459(5) 0.4503(5) 0.7223(5) 0.0455(13) Uani 1 1 d . . . H18A H 0.1367 0.5034 0.7683 0.068 Uiso 1 1 calc R . . H18B H 0.1364 0.3644 0.7782 0.068 Uiso 1 1 calc R . . H18C H 0.0823 0.4707 0.6727 0.068 Uiso 1 1 calc R . . C19 C 0.4552(4) 0.8413(4) 0.3895(4) 0.0285(9) Uani 1 1 d . . . H19 H 0.4721 0.8962 0.3022 0.034 Uiso 1 1 calc R . . C20 C 0.5568(5) 0.8601(5) 0.4470(5) 0.0378(11) Uani 1 1 d . . . H20A H 0.6368 0.8386 0.4075 0.057 Uiso 1 1 calc R . . H20B H 0.5410 0.8076 0.5329 0.057 Uiso 1 1 calc R . . H20C H 0.5583 0.9462 0.4377 0.057 Uiso 1 1 calc R . . C21 C 0.3294(5) 0.8745(5) 0.4485(5) 0.0395(12) Uani 1 1 d . . . H21A H 0.2653 0.8625 0.4095 0.059 Uiso 1 1 calc R . . H21B H 0.3302 0.9605 0.4396 0.059 Uiso 1 1 calc R . . H21C H 0.3118 0.8218 0.5344 0.059 Uiso 1 1 calc R . . O3 O 0.7347(12) 0.3180(12) 1.0706(12) 0.217(5) Uiso 1 1 d D . . C31 C 0.7155(12) 0.2135(12) 1.1895(12) 0.132(4) Uiso 1 1 d D . . H31A H 0.6728 0.2394 1.2556 0.159 Uiso 1 1 calc R . . H31B H 0.6685 0.1457 1.1889 0.159 Uiso 1 1 calc R . . C32 C 0.8398(14) 0.1808(15) 1.1979(15) 0.168(6) Uiso 1 1 d D . . H32A H 0.8723 0.1285 1.1518 0.202 Uiso 1 1 calc R . . H32B H 0.8480 0.1367 1.2830 0.202 Uiso 1 1 calc R . . C33 C 0.9029(14) 0.2957(14) 1.1466(13) 0.154(5) Uiso 1 1 d D . . H33A H 0.8739 0.3470 1.1946 0.185 Uiso 1 1 calc R . . H33B H 0.9936 0.2848 1.1389 0.185 Uiso 1 1 calc R . . C34 C 0.8688(13) 0.3455(14) 1.0338(13) 0.153(5) Uiso 1 1 d D . . H34A H 0.9114 0.3043 0.9797 0.184 Uiso 1 1 calc R . . H34B H 0.8851 0.4348 0.9943 0.184 Uiso 1 1 calc R . . O4 O 0.0374(7) 0.7018(7) 0.4695(6) 0.121(2) Uiso 1 1 d D . . C41 C 0.0092(8) 0.7880(8) 0.3541(8) 0.084(2) Uiso 1 1 d D . . H41A H 0.0867 0.8198 0.2948 0.100 Uiso 1 1 calc R . . H41B H -0.0395 0.7466 0.3211 0.100 Uiso 1 1 calc R . . C42 C -0.0568(12) 0.8809(11) 0.3764(11) 0.136(4) Uiso 1 1 d D . . H42A H -0.1312 0.8969 0.3398 0.163 Uiso 1 1 calc R . . H42B H -0.0059 0.9566 0.3402 0.163 Uiso 1 1 calc R . . C43 C -0.0937(13) 0.8474(12) 0.5073(12) 0.148(5) Uiso 1 1 d D . . H43A H -0.0908 0.9201 0.5281 0.178 Uiso 1 1 calc R . . H43B H -0.1790 0.8138 0.5363 0.178 Uiso 1 1 calc R . . C44 C -0.0097(7) 0.7589(7) 0.5595(7) 0.0708(19) Uiso 1 1 d D . . H44A H -0.0511 0.6971 0.6370 0.085 Uiso 1 1 calc R . . H44B H 0.0587 0.7972 0.5741 0.085 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 W1 0.03189(11) 0.01954(10) 0.02160(10) -0.00865(7) -0.00662(7) -0.00379(7) Fe1 0.0263(3) 0.0243(3) 0.0259(3) -0.0094(3) -0.0051(2) -0.0015(2) N1 0.0279(19) 0.0231(17) 0.0205(17) -0.0088(14) -0.0057(14) -0.0044(14) N2 0.033(2) 0.0189(17) 0.0211(17) -0.0083(14) -0.0038(14) -0.0039(14) O1 0.0330(18) 0.0304(16) 0.0243(15) -0.0107(13) -0.0060(13) 0.0015(13) O2 0.0291(17) 0.0274(16) 0.0283(16) -0.0062(13) -0.0066(13) -0.0056(13) C1 0.026(2) 0.020(2) 0.0197(19) -0.0054(16) -0.0020(16) -0.0039(16) C2 0.031(2) 0.025(2) 0.026(2) -0.0098(18) -0.0026(18) -0.0067(18) C3 0.032(2) 0.029(2) 0.026(2) -0.0139(19) -0.0046(18) -0.0077(18) C4 0.033(2) 0.023(2) 0.027(2) -0.0080(18) -0.0109(18) -0.0059(18) C5 0.027(2) 0.033(2) 0.041(3) -0.012(2) -0.010(2) -0.0085(19) C6 0.037(3) 0.034(3) 0.048(3) -0.015(2) -0.021(2) 0.000(2) C7 0.048(3) 0.028(2) 0.030(2) -0.0113(19) -0.014(2) -0.001(2) C8 0.035(3) 0.029(2) 0.023(2) -0.0108(18) -0.0070(18) -0.0032(19) C9 0.062(4) 0.031(2) 0.032(3) -0.014(2) -0.018(2) -0.003(2) C10 0.055(4) 0.050(3) 0.044(3) -0.032(3) 0.008(3) -0.011(3) C11 0.042(3) 0.042(3) 0.071(4) -0.033(3) -0.019(3) 0.014(2) C12 0.052(3) 0.027(2) 0.041(3) -0.013(2) -0.011(2) -0.008(2) C13 0.033(3) 0.035(3) 0.044(3) -0.023(2) -0.008(2) -0.004(2) C14 0.036(3) 0.028(2) 0.024(2) -0.0103(18) -0.0082(18) -0.0088(19) C15 0.039(3) 0.061(4) 0.050(3) -0.026(3) -0.009(2) -0.017(3) C16 0.061(4) 0.036(3) 0.044(3) -0.024(2) -0.023(3) 0.000(2) C17 0.032(3) 0.028(2) 0.023(2) -0.0031(18) -0.0057(18) 0.0012(19) C18 0.038(3) 0.052(3) 0.039(3) -0.010(3) -0.005(2) 0.004(2) C19 0.040(3) 0.020(2) 0.026(2) -0.0088(17) -0.0079(19) -0.0023(18) C20 0.049(3) 0.030(2) 0.043(3) -0.020(2) -0.013(2) -0.006(2) C21 0.046(3) 0.033(3) 0.040(3) -0.018(2) -0.005(2) 0.006(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 W1 N1 2.094(4) . ? W1 N2 2.096(4) . ? W1 O2 2.099(3) . ? W1 O1 2.102(3) . ? W1 W1 2.1708(3) 2_666 ? Fe1 C7 2.036(5) . ? Fe1 C5 2.038(5) . ? Fe1 C8 2.038(4) . ? Fe1 C4 2.040(4) . ? Fe1 C9 2.042(5) . ? Fe1 C11 2.040(5) . ? Fe1 C13 2.044(5) . ? Fe1 C10 2.047(5) . ? Fe1 C12 2.045(5) . ? Fe1 C6 2.045(5) . ? N1 C1 1.351(5) . ? N1 C14 1.476(5) . ? N2 C1 1.345(5) 2_666 ? N2 C19 1.486(5) . ? O1 C17 1.282(6) . ? O2 C17 1.281(6) 2_666 ? C1 N2 1.345(5) 2_666 ? C1 C2 1.438(6) . ? C2 C3 1.204(6) . ? C3 C4 1.428(6) . ? C4 C5 1.429(7) . ? C4 C8 1.443(6) . ? C5 C6 1.415(7) . ? C5 H5 0.9500 . ? C6 C7 1.402(7) . ? C6 H6 0.9500 . ? C7 C8 1.415(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.391(8) . ? C9 C13 1.411(7) . ? C9 H9 0.9500 . ? C10 C11 1.421(8) . ? C10 H10 0.9500 . ? C11 C12 1.423(8) . ? C11 H11 0.9500 . ? C12 C13 1.410(7) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C16 1.512(7) . ? C14 C15 1.516(7) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O2 1.281(6) 2_666 ? C17 C18 1.483(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.515(7) . ? C19 C21 1.523(7) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O3 C34 1.478(12) . ? O3 C31 1.489(12) . ? C31 C32 1.412(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.424(17) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.399(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O4 C41 1.469(8) . ? O4 C44 1.489(8) . ? C41 C42 1.354(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.467(16) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.396(11) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? 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 W1 N2 176.08(12) . . ? N1 W1 O2 89.86(13) . . ? N2 W1 O2 89.91(13) . . ? N1 W1 O1 90.32(13) . . ? N2 W1 O1 89.79(13) . . ? O2 W1 O1 178.21(11) . . ? N1 W1 W1 91.95(9) . 2_666 ? N2 W1 W1 91.97(9) . 2_666 ? O2 W1 W1 90.95(9) . 2_666 ? O1 W1 W1 90.83(9) . 2_666 ? C7 Fe1 C5 68.4(2) . . ? C7 Fe1 C8 40.64(18) . . ? C5 Fe1 C8 69.03(19) . . ? C7 Fe1 C4 68.95(18) . . ? C5 Fe1 C4 41.04(19) . . ? C8 Fe1 C4 41.45(17) . . ? C7 Fe1 C9 157.9(2) . . ? C5 Fe1 C9 124.2(2) . . ? C8 Fe1 C9 122.4(2) . . ? C4 Fe1 C9 107.66(19) . . ? C7 Fe1 C11 123.5(2) . . ? C5 Fe1 C11 122.7(2) . . ? C8 Fe1 C11 159.1(2) . . ? C4 Fe1 C11 158.4(2) . . ? C9 Fe1 C11 67.7(2) . . ? C7 Fe1 C13 121.9(2) . . ? C5 Fe1 C13 160.2(2) . . ? C8 Fe1 C13 106.9(2) . . ? C4 Fe1 C13 123.21(19) . . ? C9 Fe1 C13 40.4(2) . . ? C11 Fe1 C13 67.9(2) . . ? C7 Fe1 C10 160.4(2) . . ? C5 Fe1 C10 108.5(2) . . ? C8 Fe1 C10 158.1(2) . . ? C4 Fe1 C10 122.3(2) . . ? C9 Fe1 C10 39.8(2) . . ? C11 Fe1 C10 40.7(2) . . ? C13 Fe1 C10 67.6(2) . . ? C7 Fe1 C12 106.9(2) . . ? C5 Fe1 C12 158.2(2) . . ? C8 Fe1 C12 122.2(2) . . ? C4 Fe1 C12 159.2(2) . . ? C9 Fe1 C12 68.0(2) . . ? C11 Fe1 C12 40.8(2) . . ? C13 Fe1 C12 40.4(2) . . ? C10 Fe1 C12 68.3(2) . . ? C7 Fe1 C6 40.2(2) . . ? C5 Fe1 C6 40.6(2) . . ? C8 Fe1 C6 68.1(2) . . ? C4 Fe1 C6 68.52(19) . . ? C9 Fe1 C6 160.7(2) . . ? C11 Fe1 C6 108.4(2) . . ? C13 Fe1 C6 157.6(2) . . ? C10 Fe1 C6 125.0(2) . . ? C12 Fe1 C6 122.3(2) . . ? C1 N1 C14 118.2(4) . . ? C1 N1 W1 118.9(3) . . ? C14 N1 W1 122.9(3) . . ? C1 N2 C19 117.8(4) 2_666 . ? C1 N2 W1 118.9(3) 2_666 . ? C19 N2 W1 123.2(3) . . ? C17 O1 W1 118.4(3) . . ? C17 O2 W1 118.4(3) 2_666 . ? N2 C1 N1 118.3(4) 2_666 . ? N2 C1 C2 121.3(4) 2_666 . ? N1 C1 C2 120.4(4) . . ? C3 C2 C1 178.2(5) . . ? C2 C3 C4 177.7(5) . . ? C3 C4 C5 127.4(4) . . ? C3 C4 C8 125.6(4) . . ? C5 C4 C8 107.1(4) . . ? C3 C4 Fe1 125.9(3) . . ? C5 C4 Fe1 69.4(3) . . ? C8 C4 Fe1 69.2(2) . . ? C6 C5 C4 107.9(4) . . ? C6 C5 Fe1 70.0(3) . . ? C4 C5 Fe1 69.5(2) . . ? C6 C5 H5 126.1 . . ? C4 C5 H5 126.1 . . ? Fe1 C5 H5 126.0 . . ? C7 C6 C5 108.8(4) . . ? C7 C6 Fe1 69.6(3) . . ? C5 C6 Fe1 69.5(3) . . ? C7 C6 H6 125.6 . . ? C5 C6 H6 125.6 . . ? Fe1 C6 H6 127.0 . . ? C6 C7 C8 108.6(4) . . ? C6 C7 Fe1 70.2(3) . . ? C8 C7 Fe1 69.8(3) . . ? C6 C7 H7 125.7 . . ? C8 C7 H7 125.7 . . ? Fe1 C7 H7 125.9 . . ? C7 C8 C4 107.6(4) . . ? C7 C8 Fe1 69.6(3) . . ? C4 C8 Fe1 69.3(2) . . ? C7 C8 H8 126.2 . . ? C4 C8 H8 126.2 . . ? Fe1 C8 H8 126.5 . . ? C10 C9 C13 108.7(5) . . ? C10 C9 Fe1 70.3(3) . . ? C13 C9 Fe1 69.9(3) . . ? C10 C9 H9 125.7 . . ? C13 C9 H9 125.7 . . ? Fe1 C9 H9 125.7 . . ? C9 C10 C11 108.0(5) . . ? C9 C10 Fe1 69.9(3) . . ? C11 C10 Fe1 69.4(3) . . ? C9 C10 H10 126.0 . . ? C11 C10 H10 126.0 . . ? Fe1 C10 H10 126.2 . . ? C10 C11 C12 107.8(5) . . ? C10 C11 Fe1 69.9(3) . . ? C12 C11 Fe1 69.8(3) . . ? C10 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? Fe1 C11 H11 125.8 . . ? C13 C12 C11 107.3(5) . . ? C13 C12 Fe1 69.8(3) . . ? C11 C12 Fe1 69.4(3) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? Fe1 C12 H12 126.0 . . ? C9 C13 C12 108.3(5) . . ? C9 C13 Fe1 69.7(3) . . ? C12 C13 Fe1 69.9(3) . . ? C9 C13 H13 125.9 . . ? C12 C13 H13 125.9 . . ? Fe1 C13 H13 126.1 . . ? N1 C14 C16 109.7(4) . . ? N1 C14 C15 110.9(4) . . ? C16 C14 C15 110.9(4) . . ? N1 C14 H14 108.4 . . ? C16 C14 H14 108.4 . . ? C15 C14 H14 108.4 . . ? 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 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 O1 121.4(4) 2_666 . ? O2 C17 C18 119.1(4) 2_666 . ? O1 C17 C18 119.5(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C20 109.8(4) . . ? N2 C19 C21 110.7(4) . . ? C20 C19 C21 110.8(4) . . ? N2 C19 H19 108.5 . . ? C20 C19 H19 108.5 . . ? C21 C19 H19 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C34 O3 C31 107.2(12) . . ? C32 C31 O3 99.8(12) . . ? C32 C31 H31A 111.8 . . ? O3 C31 H31A 111.8 . . ? C32 C31 H31B 111.8 . . ? O3 C31 H31B 111.8 . . ? H31A C31 H31B 109.5 . . ? C31 C32 C33 103.7(13) . . ? C31 C32 H32A 111.0 . . ? C33 C32 H32A 111.0 . . ? C31 C32 H32B 111.0 . . ? C33 C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? C34 C33 C32 100.9(14) . . ? C34 C33 H33A 111.6 . . ? C32 C33 H33A 111.6 . . ? C34 C33 H33B 111.6 . . ? C32 C33 H33B 111.6 . . ? H33A C33 H33B 109.4 . . ? C33 C34 O3 99.9(12) . . ? C33 C34 H34A 111.8 . . ? O3 C34 H34A 111.8 . . ? C33 C34 H34B 111.8 . . ? O3 C34 H34B 111.8 . . ? H34A C34 H34B 109.5 . . ? C41 O4 C44 106.4(7) . . ? C42 C41 O4 107.0(8) . . ? C42 C41 H41A 110.3 . . ? O4 C41 H41A 110.3 . . ? C42 C41 H41B 110.3 . . ? O4 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C41 C42 C43 109.3(10) . . ? C41 C42 H42A 109.8 . . ? C43 C42 H42A 109.8 . . ? C41 C42 H42B 109.8 . . ? C43 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? C44 C43 C42 106.5(10) . . ? C44 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? C44 C43 H43B 110.4 . . ? C42 C43 H43B 110.5 . . ? H43A C43 H43B 108.6 . . ? C43 C44 O4 104.6(8) . . ? C43 C44 H44A 110.8 . . ? O4 C44 H44A 110.8 . . ? C43 C44 H44B 110.8 . . ? O4 C44 H44B 110.8 . . ? H44A C44 H44B 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 W1 N1 C1 -90.6(3) . . . . ? O1 W1 N1 C1 91.2(3) . . . . ? W1 W1 N1 C1 0.3(3) 2_666 . . . ? O2 W1 N1 C14 86.6(3) . . . . ? O1 W1 N1 C14 -91.6(3) . . . . ? W1 W1 N1 C14 177.6(3) 2_666 . . . ? O2 W1 N2 C1 91.7(3) . . . 2_666 ? O1 W1 N2 C1 -90.1(3) . . . 2_666 ? W1 W1 N2 C1 0.7(3) 2_666 . . 2_666 ? O2 W1 N2 C19 -90.0(3) . . . . ? O1 W1 N2 C19 88.2(3) . . . . ? W1 W1 N2 C19 179.0(3) 2_666 . . . ? N1 W1 O1 C17 -92.0(3) . . . . ? N2 W1 O1 C17 92.0(3) . . . . ? W1 W1 O1 C17 0.0(3) 2_666 . . . ? N1 W1 O2 C17 91.3(3) . . . 2_666 ? N2 W1 O2 C17 -92.6(3) . . . 2_666 ? W1 W1 O2 C17 -0.6(3) 2_666 . . 2_666 ? C14 N1 C1 N2 -178.3(4) . . . 2_666 ? W1 N1 C1 N2 -0.9(5) . . . 2_666 ? C14 N1 C1 C2 2.1(6) . . . . ? W1 N1 C1 C2 179.5(3) . . . . ? C7 Fe1 C4 C3 -157.2(5) . . . . ? C5 Fe1 C4 C3 121.9(5) . . . . ? C8 Fe1 C4 C3 -119.6(5) . . . . ? C9 Fe1 C4 C3 -0.3(5) . . . . ? C11 Fe1 C4 C3 73.6(7) . . . . ? C13 Fe1 C4 C3 -42.0(5) . . . . ? C10 Fe1 C4 C3 40.8(5) . . . . ? C12 Fe1 C4 C3 -74.9(7) . . . . ? C6 Fe1 C4 C3 159.6(5) . . . . ? C7 Fe1 C4 C5 80.9(3) . . . . ? C8 Fe1 C4 C5 118.5(4) . . . . ? C9 Fe1 C4 C5 -122.2(3) . . . . ? C11 Fe1 C4 C5 -48.3(7) . . . . ? C13 Fe1 C4 C5 -163.9(3) . . . . ? C10 Fe1 C4 C5 -81.1(3) . . . . ? C12 Fe1 C4 C5 163.2(5) . . . . ? C6 Fe1 C4 C5 37.7(3) . . . . ? C7 Fe1 C4 C8 -37.6(3) . . . . ? C5 Fe1 C4 C8 -118.5(4) . . . . ? C9 Fe1 C4 C8 119.2(3) . . . . ? C11 Fe1 C4 C8 -166.8(5) . . . . ? C13 Fe1 C4 C8 77.5(3) . . . . ? C10 Fe1 C4 C8 160.4(3) . . . . ? C12 Fe1 C4 C8 44.7(6) . . . . ? C6 Fe1 C4 C8 -80.9(3) . . . . ? C3 C4 C5 C6 -179.8(4) . . . . ? C8 C4 C5 C6 -0.5(5) . . . . ? Fe1 C4 C5 C6 -59.7(3) . . . . ? C3 C4 C5 Fe1 -120.1(4) . . . . ? C8 C4 C5 Fe1 59.2(3) . . . . ? C7 Fe1 C5 C6 36.7(3) . . . . ? C8 Fe1 C5 C6 80.5(3) . . . . ? C4 Fe1 C5 C6 119.0(4) . . . . ? C9 Fe1 C5 C6 -163.9(3) . . . . ? C11 Fe1 C5 C6 -80.1(4) . . . . ? C13 Fe1 C5 C6 162.1(5) . . . . ? C10 Fe1 C5 C6 -122.7(3) . . . . ? C12 Fe1 C5 C6 -45.0(7) . . . . ? C7 Fe1 C5 C4 -82.3(3) . . . . ? C8 Fe1 C5 C4 -38.5(3) . . . . ? C9 Fe1 C5 C4 77.1(3) . . . . ? C11 Fe1 C5 C4 160.9(3) . . . . ? C13 Fe1 C5 C4 43.1(7) . . . . ? C10 Fe1 C5 C4 118.3(3) . . . . ? C12 Fe1 C5 C4 -164.0(5) . . . . ? C6 Fe1 C5 C4 -119.0(4) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? Fe1 C5 C6 C7 -58.6(3) . . . . ? C4 C5 C6 Fe1 59.4(3) . . . . ? C5 Fe1 C6 C7 120.5(4) . . . . ? C8 Fe1 C6 C7 37.6(3) . . . . ? C4 Fe1 C6 C7 82.4(3) . . . . ? C9 Fe1 C6 C7 164.5(6) . . . . ? C11 Fe1 C6 C7 -120.4(3) . . . . ? C13 Fe1 C6 C7 -43.7(6) . . . . ? C10 Fe1 C6 C7 -162.4(3) . . . . ? C12 Fe1 C6 C7 -77.6(3) . . . . ? C7 Fe1 C6 C5 -120.5(4) . . . . ? C8 Fe1 C6 C5 -82.9(3) . . . . ? C4 Fe1 C6 C5 -38.1(3) . . . . ? C9 Fe1 C6 C5 44.0(8) . . . . ? C11 Fe1 C6 C5 119.1(3) . . . . ? C13 Fe1 C6 C5 -164.2(5) . . . . ? C10 Fe1 C6 C5 77.1(4) . . . . ? C12 Fe1 C6 C5 161.9(3) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? Fe1 C6 C7 C8 -59.4(3) . . . . ? C5 C6 C7 Fe1 58.5(3) . . . . ? C5 Fe1 C7 C6 -37.0(3) . . . . ? C8 Fe1 C7 C6 -119.5(4) . . . . ? C4 Fe1 C7 C6 -81.2(3) . . . . ? C9 Fe1 C7 C6 -166.4(5) . . . . ? C11 Fe1 C7 C6 78.8(4) . . . . ? C13 Fe1 C7 C6 161.9(3) . . . . ? C10 Fe1 C7 C6 47.6(7) . . . . ? C12 Fe1 C7 C6 120.4(3) . . . . ? C5 Fe1 C7 C8 82.5(3) . . . . ? C4 Fe1 C7 C8 38.3(3) . . . . ? C9 Fe1 C7 C8 -46.9(6) . . . . ? C11 Fe1 C7 C8 -161.7(3) . . . . ? C13 Fe1 C7 C8 -78.5(3) . . . . ? C10 Fe1 C7 C8 167.1(6) . . . . ? C12 Fe1 C7 C8 -120.1(3) . . . . ? C6 Fe1 C7 C8 119.5(4) . . . . ? C6 C7 C8 C4 0.6(5) . . . . ? Fe1 C7 C8 C4 -59.1(3) . . . . ? C6 C7 C8 Fe1 59.7(3) . . . . ? C3 C4 C8 C7 179.2(4) . . . . ? C5 C4 C8 C7 -0.1(5) . . . . ? Fe1 C4 C8 C7 59.3(3) . . . . ? C3 C4 C8 Fe1 120.0(4) . . . . ? C5 C4 C8 Fe1 -59.4(3) . . . . ? C5 Fe1 C8 C7 -80.9(3) . . . . ? C4 Fe1 C8 C7 -119.1(4) . . . . ? C9 Fe1 C8 C7 161.0(3) . . . . ? C11 Fe1 C8 C7 47.3(7) . . . . ? C13 Fe1 C8 C7 119.6(3) . . . . ? C10 Fe1 C8 C7 -168.5(5) . . . . ? C12 Fe1 C8 C7 78.1(3) . . . . ? C6 Fe1 C8 C7 -37.2(3) . . . . ? C7 Fe1 C8 C4 119.1(4) . . . . ? C5 Fe1 C8 C4 38.1(3) . . . . ? C9 Fe1 C8 C4 -79.9(3) . . . . ? C11 Fe1 C8 C4 166.4(5) . . . . ? C13 Fe1 C8 C4 -121.4(3) . . . . ? C10 Fe1 C8 C4 -49.4(7) . . . . ? C12 Fe1 C8 C4 -162.8(3) . . . . ? C6 Fe1 C8 C4 81.8(3) . . . . ? C7 Fe1 C9 C10 -163.0(5) . . . . ? C5 Fe1 C9 C10 77.4(4) . . . . ? C8 Fe1 C9 C10 162.8(3) . . . . ? C4 Fe1 C9 C10 119.6(3) . . . . ? C11 Fe1 C9 C10 -37.9(3) . . . . ? C13 Fe1 C9 C10 -119.6(5) . . . . ? C12 Fe1 C9 C10 -82.1(3) . . . . ? C6 Fe1 C9 C10 44.3(8) . . . . ? C7 Fe1 C9 C13 -43.5(6) . . . . ? C5 Fe1 C9 C13 -163.0(3) . . . . ? C8 Fe1 C9 C13 -77.7(3) . . . . ? C4 Fe1 C9 C13 -120.8(3) . . . . ? C11 Fe1 C9 C13 81.6(3) . . . . ? C10 Fe1 C9 C13 119.6(5) . . . . ? C12 Fe1 C9 C13 37.5(3) . . . . ? C6 Fe1 C9 C13 163.9(6) . . . . ? C13 C9 C10 C11 -0.4(6) . . . . ? Fe1 C9 C10 C11 59.2(4) . . . . ? C13 C9 C10 Fe1 -59.6(3) . . . . ? C7 Fe1 C10 C9 160.8(6) . . . . ? C5 Fe1 C10 C9 -121.7(3) . . . . ? C8 Fe1 C10 C9 -42.1(7) . . . . ? C4 Fe1 C10 C9 -78.6(4) . . . . ? C11 Fe1 C10 C9 119.2(5) . . . . ? C13 Fe1 C10 C9 37.6(3) . . . . ? C12 Fe1 C10 C9 81.3(3) . . . . ? C6 Fe1 C10 C9 -163.6(3) . . . . ? C7 Fe1 C10 C11 41.6(8) . . . . ? C5 Fe1 C10 C11 119.1(3) . . . . ? C8 Fe1 C10 C11 -161.3(5) . . . . ? C4 Fe1 C10 C11 162.2(3) . . . . ? C9 Fe1 C10 C11 -119.2(5) . . . . ? C13 Fe1 C10 C11 -81.7(4) . . . . ? C12 Fe1 C10 C11 -38.0(3) . . . . ? C6 Fe1 C10 C11 77.1(4) . . . . ? C9 C10 C11 C12 0.2(6) . . . . ? Fe1 C10 C11 C12 59.7(4) . . . . ? C9 C10 C11 Fe1 -59.5(4) . . . . ? C7 Fe1 C11 C10 -164.6(3) . . . . ? C5 Fe1 C11 C10 -80.2(4) . . . . ? C8 Fe1 C11 C10 160.4(5) . . . . ? C4 Fe1 C11 C10 -44.6(7) . . . . ? C9 Fe1 C11 C10 37.1(3) . . . . ? C13 Fe1 C11 C10 80.9(4) . . . . ? C12 Fe1 C11 C10 118.8(5) . . . . ? C6 Fe1 C11 C10 -122.7(4) . . . . ? C7 Fe1 C11 C12 76.6(4) . . . . ? C5 Fe1 C11 C12 160.9(3) . . . . ? C8 Fe1 C11 C12 41.6(7) . . . . ? C4 Fe1 C11 C12 -163.4(5) . . . . ? C9 Fe1 C11 C12 -81.7(3) . . . . ? C13 Fe1 C11 C12 -37.9(3) . . . . ? C10 Fe1 C11 C12 -118.8(5) . . . . ? C6 Fe1 C11 C12 118.5(3) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? Fe1 C11 C12 C13 59.8(3) . . . . ? C10 C11 C12 Fe1 -59.8(4) . . . . ? C7 Fe1 C12 C13 119.6(3) . . . . ? C5 Fe1 C12 C13 -166.2(5) . . . . ? C8 Fe1 C12 C13 77.8(3) . . . . ? C4 Fe1 C12 C13 44.4(7) . . . . ? C9 Fe1 C12 C13 -37.5(3) . . . . ? C11 Fe1 C12 C13 -118.4(5) . . . . ? C10 Fe1 C12 C13 -80.5(3) . . . . ? C6 Fe1 C12 C13 160.8(3) . . . . ? C7 Fe1 C12 C11 -122.0(3) . . . . ? C5 Fe1 C12 C11 -47.8(7) . . . . ? C8 Fe1 C12 C11 -163.7(3) . . . . ? C4 Fe1 C12 C11 162.9(5) . . . . ? C9 Fe1 C12 C11 80.9(4) . . . . ? C13 Fe1 C12 C11 118.4(5) . . . . ? C10 Fe1 C12 C11 37.9(3) . . . . ? C6 Fe1 C12 C11 -80.7(4) . . . . ? C10 C9 C13 C12 0.4(6) . . . . ? Fe1 C9 C13 C12 -59.5(3) . . . . ? C10 C9 C13 Fe1 59.8(4) . . . . ? C11 C12 C13 C9 -0.2(5) . . . . ? Fe1 C12 C13 C9 59.4(3) . . . . ? C11 C12 C13 Fe1 -59.6(3) . . . . ? C7 Fe1 C13 C9 162.2(3) . . . . ? C5 Fe1 C13 C9 45.5(7) . . . . ? C8 Fe1 C13 C9 120.4(3) . . . . ? C4 Fe1 C13 C9 77.9(3) . . . . ? C11 Fe1 C13 C9 -81.1(3) . . . . ? C10 Fe1 C13 C9 -37.0(3) . . . . ? C12 Fe1 C13 C9 -119.4(4) . . . . ? C6 Fe1 C13 C9 -166.1(5) . . . . ? C7 Fe1 C13 C12 -78.3(3) . . . . ? C5 Fe1 C13 C12 164.9(6) . . . . ? C8 Fe1 C13 C12 -120.2(3) . . . . ? C4 Fe1 C13 C12 -162.7(3) . . . . ? C9 Fe1 C13 C12 119.4(4) . . . . ? C11 Fe1 C13 C12 38.3(3) . . . . ? C10 Fe1 C13 C12 82.4(3) . . . . ? C6 Fe1 C13 C12 -46.6(7) . . . . ? C1 N1 C14 C16 -154.9(4) . . . . ? W1 N1 C14 C16 27.9(5) . . . . ? C1 N1 C14 C15 82.3(5) . . . . ? W1 N1 C14 C15 -95.0(4) . . . . ? W1 O1 C17 O2 0.5(6) . . . 2_666 ? W1 O1 C17 C18 179.1(3) . . . . ? C1 N2 C19 C20 -155.4(4) 2_666 . . . ? W1 N2 C19 C20 26.3(5) . . . . ? C1 N2 C19 C21 81.9(5) 2_666 . . . ? W1 N2 C19 C21 -96.4(4) . . . . ? C34 O3 C31 C32 -8.9(15) . . . . ? O3 C31 C32 C33 37.4(16) . . . . ? C31 C32 C33 C34 -55.0(17) . . . . ? C32 C33 C34 O3 45.6(15) . . . . ? C31 O3 C34 C33 -22.9(16) . . . . ? C44 O4 C41 C42 -4.6(11) . . . . ? O4 C41 C42 C43 -10.8(14) . . . . ? C41 C42 C43 C44 23.3(16) . . . . ? C42 C43 C44 O4 -24.8(13) . . . . ? C41 O4 C44 C43 18.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.022 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.138 #END OF CIF #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-02-03 at 16:46:50 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : shelxl dreduc import struct data_Chisholm1390 _database_code_depnum_ccdc_archive 'CCDC 637931' _audit_creation_date 2007-02-03T16:46:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common Chisholm1390 _chemical_formula_moiety 'C46 H52 Mo2 N4 O4, C4 H8 O1' _chemical_formula_sum 'C50 H60 Mo2 N4 O5' _chemical_formula_weight 988.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 21.482(2) _cell_length_b 9.609(1) _cell_length_c 22.527(3) _cell_angle_alpha 90 _cell_angle_beta 97.633(4) _cell_angle_gamma 90 _cell_volume 4608.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11211 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.346688E-1 _diffrn_orient_matrix_ub_12 -0.546249E-1 _diffrn_orient_matrix_ub_13 -0.232059E-1 _diffrn_orient_matrix_ub_21 0.27157E-1 _diffrn_orient_matrix_ub_22 -0.175401E-1 _diffrn_orient_matrix_ub_23 -0.319967E-1 _diffrn_orient_matrix_ub_31 0.163238E-1 _diffrn_orient_matrix_ub_32 -0.86833E-1 _diffrn_orient_matrix_ub_33 0.210616E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'one degree phi and omega scans' _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 82643 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 10574 _reflns_number_gt 6867 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;There is a solvent molecule of THF in the asymmetric unit. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded atom). The torsion angle, which defines the orientation of each methyl group about the C-C bond, was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 *Ueq(bonded C atom). 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 'w=1/[\s^2^(Fo^2^)+(0.0674P)^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_number_reflns 10574 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.085 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mo1 Mo 0.242263(15) 0.29898(3) 0.030868(14) 0.02343(10) Uani 1 1 d . . . Mo2 Mo 0.211675(14) 0.12650(3) 0.078945(14) 0.02294(10) Uani 1 1 d . . . O1 O 0.19427(11) 0.2215(3) -0.05057(11) 0.0262(6) Uani 1 1 d . . . O2 O 0.16527(11) 0.0395(3) -0.00010(11) 0.0256(6) Uani 1 1 d . . . O3 O 0.31974(11) 0.1854(3) 0.00883(11) 0.0244(6) Uani 1 1 d . . . O4 O 0.29027(11) 0.0094(3) 0.06219(10) 0.0245(6) Uani 1 1 d . . . N1 N 0.29493(15) 0.4582(3) 0.08383(14) 0.0302(8) Uani 1 1 d . . . N2 N 0.19497(15) 0.4870(3) 0.05180(15) 0.0313(8) Uani 1 1 d . . . N3 N 0.22369(14) 0.1638(3) 0.17429(14) 0.0275(7) Uani 1 1 d . . . N4 N 0.12922(14) 0.1585(3) 0.12272(14) 0.0274(7) Uani 1 1 d . . . C1 C 0.0066(2) 0.2637(6) -0.22811(19) 0.0483(13) Uani 1 1 d . . . H1 H -0.0231 0.3133 -0.2552 0.058 Uiso 1 1 calc R . . C2 C 0.0391(2) 0.3326(5) -0.1778(2) 0.0468(12) Uani 1 1 d . . . H2 H 0.0314 0.4285 -0.1714 0.056 Uiso 1 1 calc R . . C3 C 0.0174(2) 0.1286(6) -0.23771(18) 0.0462(13) Uani 1 1 d . . . H3 H -0.0046 0.0843 -0.272 0.055 Uiso 1 1 calc R . . C4 C 0.08138(18) 0.2623(5) -0.13854(18) 0.0353(10) Uani 1 1 d . . . H4 H 0.1029 0.3104 -0.1051 0.042 Uiso 1 1 calc R . . C5 C 0.06078(18) 0.0501(5) -0.19799(18) 0.0377(11) Uani 1 1 d . . . C6 C 0.09412(17) 0.1184(4) -0.14631(17) 0.0318(10) Uani 1 1 d . . . C7 C 0.0710(2) -0.0895(5) -0.20786(18) 0.0432(12) Uani 1 1 d . . . H7 H 0.0487 -0.1329 -0.2422 0.052 Uiso 1 1 calc R . . C8 C 0.13598(16) 0.0380(4) -0.10587(16) 0.0282(9) Uani 1 1 d . . . C9 C 0.11296(19) -0.1690(5) -0.16909(18) 0.0364(10) Uani 1 1 d . . . C10 C 0.14627(18) -0.1046(4) -0.11657(17) 0.0317(10) Uani 1 1 d . . . C11 C 0.1244(2) -0.3124(5) -0.1803(2) 0.0456(12) Uani 1 1 d . . . H11 H 0.1021 -0.3561 -0.2145 0.055 Uiso 1 1 calc R . . C12 C 0.19004(19) -0.1879(4) -0.07914(18) 0.0351(10) Uani 1 1 d . . . H12 H 0.213 -0.1475 -0.0444 0.042 Uiso 1 1 calc R . . C13 C 0.1662(2) -0.3871(5) -0.1432(2) 0.0489(12) Uani 1 1 d . . . H13 H 0.1732 -0.4823 -0.1516 0.059 Uiso 1 1 calc R . . C14 C 0.1997(2) -0.3245(5) -0.0920(2) 0.0442(12) Uani 1 1 d . . . H14 H 0.2292 -0.3778 -0.0662 0.053 Uiso 1 1 calc R . . C15 C 0.16684(16) 0.1044(4) -0.04927(16) 0.0265(9) Uani 1 1 d . . . C16 C 0.3792(2) -0.1078(5) -0.17700(19) 0.0432(11) Uani 1 1 d . . . H16 H 0.3795 -0.1265 -0.2184 0.052 Uiso 1 1 calc R . . C17 C 0.3301(2) -0.0297(5) -0.15809(19) 0.0419(11) Uani 1 1 d . . . H17 H 0.2972 0.0036 -0.187 0.05 Uiso 1 1 calc R . . C18 C 0.4256(2) -0.1558(5) -0.13657(19) 0.0390(11) Uani 1 1 d . . . H18 H 0.4587 -0.2078 -0.15 0.047 Uiso 1 1 calc R . . C19 C 0.32878(18) -0.0007(4) -0.09891(17) 0.0336(10) Uani 1 1 d . . . H19 H 0.2953 0.0527 -0.0871 0.04 Uiso 1 1 calc R . . C20 C 0.42683(18) -0.1310(4) -0.07424(17) 0.0313(9) Uani 1 1 d . . . C21 C 0.37728(17) -0.0502(4) -0.05478(17) 0.0282(9) Uani 1 1 d . . . C22 C 0.47412(19) -0.1851(4) -0.03174(19) 0.0333(10) Uani 1 1 d . . . H22 H 0.5072 -0.2374 -0.045 0.04 Uiso 1 1 calc R . . C23 C 0.37737(17) -0.0283(4) 0.00722(17) 0.0261(9) Uani 1 1 d . . . C24 C 0.47402(18) -0.1646(4) 0.02919(19) 0.0322(10) Uani 1 1 d . . . C25 C 0.42453(17) -0.0865(4) 0.05008(17) 0.0271(9) Uani 1 1 d . . . C26 C 0.52287(19) -0.2191(4) 0.0723(2) 0.0388(10) Uani 1 1 d . . . H26 H 0.5565 -0.269 0.0588 0.047 Uiso 1 1 calc R . . C27 C 0.42573(18) -0.0690(4) 0.11281(18) 0.0337(10) Uani 1 1 d . . . H27 H 0.393 -0.0184 0.1275 0.04 Uiso 1 1 calc R . . C28 C 0.52220(19) -0.2011(4) 0.13182(19) 0.0400(11) Uani 1 1 d . . . H28 H 0.5545 -0.2403 0.1597 0.048 Uiso 1 1 calc R . . C29 C 0.4732(2) -0.1238(4) 0.15238(19) 0.0422(11) Uani 1 1 d . . . H29 H 0.4733 -0.1098 0.1941 0.051 Uiso 1 1 calc R . . C30 C 0.32691(17) 0.0594(4) 0.02740(16) 0.0267(9) Uani 1 1 d . . . C31 C 0.06774(19) -0.0567(4) 0.1062(2) 0.0414(11) Uani 1 1 d . . . H31A H 0.0914 -0.0804 0.0732 0.062 Uiso 1 1 calc R . . H31B H 0.0251 -0.0944 0.0978 0.062 Uiso 1 1 calc R . . H31C H 0.0888 -0.0968 0.1436 0.062 Uiso 1 1 calc R . . C32 C 0.02749(19) 0.1654(5) 0.0581(2) 0.0444(12) Uani 1 1 d . . . H32A H 0.0262 0.2666 0.0632 0.067 Uiso 1 1 calc R . . H32B H -0.0154 0.1282 0.053 0.067 Uiso 1 1 calc R . . H32C H 0.0475 0.1433 0.0226 0.067 Uiso 1 1 calc R . . C33 C 0.06459(18) 0.1010(4) 0.11234(19) 0.0356(10) Uani 1 1 d . . . H33 H 0.0432 0.1231 0.148 0.043 Uiso 1 1 calc R . . C34 C 0.33195(18) 0.1175(4) 0.21353(17) 0.0377(10) Uani 1 1 d . . . H34A H 0.3249 0.0183 0.205 0.057 Uiso 1 1 calc R . . H34B H 0.3638 0.1282 0.2486 0.057 Uiso 1 1 calc R . . H34C H 0.3465 0.1627 0.1789 0.057 Uiso 1 1 calc R . . C35 C 0.2799(2) 0.3380(4) 0.2400(2) 0.0462(12) Uani 1 1 d . . . H35A H 0.2899 0.387 0.2043 0.069 Uiso 1 1 calc R . . H35B H 0.3145 0.3499 0.2726 0.069 Uiso 1 1 calc R . . H35C H 0.2412 0.3763 0.2521 0.069 Uiso 1 1 calc R . . C36 C 0.27084(18) 0.1846(4) 0.22602(16) 0.0304(9) Uani 1 1 d . . . H36 H 0.2565 0.1374 0.2614 0.036 Uiso 1 1 calc R . . C37 C 0.16264(19) 0.1623(4) 0.17679(18) 0.0308(9) Uani 1 1 d . . . C38 C 0.1330(2) 0.1643(5) 0.23442(18) 0.0397(11) Uani 1 1 d . . . H38A H 0.1003 0.2361 0.2317 0.06 Uiso 1 1 calc R . . H38B H 0.1652 0.1849 0.2683 0.06 Uiso 1 1 calc R . . H38C H 0.1142 0.0732 0.2404 0.06 Uiso 1 1 calc R . . C39 C 0.09109(18) 0.4960(5) -0.00659(19) 0.0447(12) Uani 1 1 d . . . H39A H 0.1101 0.5097 -0.0433 0.067 Uiso 1 1 calc R . . H39B H 0.0502 0.5427 -0.0105 0.067 Uiso 1 1 calc R . . H39C H 0.0854 0.3962 0 0.067 Uiso 1 1 calc R . . C40 C 0.1050(2) 0.5434(5) 0.1050(2) 0.0547(13) Uani 1 1 d . . . H40A H 0.0997 0.4448 0.1144 0.082 Uiso 1 1 calc R . . H40B H 0.0641 0.5899 0.1009 0.082 Uiso 1 1 calc R . . H40C H 0.1333 0.5872 0.1374 0.082 Uiso 1 1 calc R . . C41 C 0.13325(19) 0.5563(4) 0.04559(19) 0.0380(10) Uani 1 1 d . . . H41 H 0.1395 0.6573 0.0375 0.046 Uiso 1 1 calc R . . C42 C 0.3789(2) 0.5324(5) 0.02681(19) 0.0470(12) Uani 1 1 d . . . H42A H 0.371 0.4491 0.0019 0.071 Uiso 1 1 calc R . . H42B H 0.4237 0.5561 0.0306 0.071 Uiso 1 1 calc R . . H42C H 0.354 0.6102 0.0082 0.071 Uiso 1 1 calc R . . C43 C 0.40328(19) 0.3960(5) 0.12095(19) 0.0411(11) Uani 1 1 d . . . H43A H 0.3924 0.3823 0.1614 0.062 Uiso 1 1 calc R . . H43B H 0.447 0.4274 0.1234 0.062 Uiso 1 1 calc R . . H43C H 0.3983 0.308 0.0988 0.062 Uiso 1 1 calc R . . C44 C 0.36044(18) 0.5044(5) 0.08882(17) 0.0367(10) Uani 1 1 d . . . H44 H 0.3649 0.5927 0.1125 0.044 Uiso 1 1 calc R . . C45 C 0.2470(2) 0.5485(4) 0.07590(17) 0.0338(10) Uani 1 1 d . . . C46 C 0.2527(2) 0.6992(4) 0.0930(2) 0.0434(11) Uani 1 1 d . . . H46A H 0.2527 0.756 0.0569 0.065 Uiso 1 1 calc R . . H46B H 0.292 0.7142 0.1197 0.065 Uiso 1 1 calc R . . H46C H 0.2171 0.726 0.1136 0.065 Uiso 1 1 calc R . . O5 O 0.2328(2) -0.0439(5) -0.27853(17) 0.0919(14) Uani 1 1 d . . . C48 C 0.2177(3) -0.1658(6) -0.3119(2) 0.0669(16) Uani 1 1 d . . . H48A H 0.1889 -0.2252 -0.2922 0.08 Uiso 1 1 calc R . . H48B H 0.2561 -0.2197 -0.3163 0.08 Uiso 1 1 calc R . . C49 C 0.1864(2) -0.1170(5) -0.3721(2) 0.0455(12) Uani 1 1 d . . . H49A H 0.1576 -0.1885 -0.3918 0.055 Uiso 1 1 calc R . . H49B H 0.2178 -0.0924 -0.3989 0.055 Uiso 1 1 calc R . . C50 C 0.1507(2) 0.0109(5) -0.3553(2) 0.0569(13) Uani 1 1 d . . . H50A H 0.1475 0.0816 -0.3875 0.068 Uiso 1 1 calc R . . H50B H 0.108 -0.0142 -0.3471 0.068 Uiso 1 1 calc R . . C51 C 0.1904(3) 0.0629(6) -0.2994(2) 0.0640(16) Uani 1 1 d . . . H51A H 0.2138 0.1474 -0.3085 0.077 Uiso 1 1 calc R . . H51B H 0.1635 0.0866 -0.2685 0.077 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 Mo1 0.02310(18) 0.02312(19) 0.02393(18) 0.00121(14) 0.00266(13) -0.00075(14) Mo2 0.02220(18) 0.02401(19) 0.02282(18) 0.00061(14) 0.00378(13) -0.00099(14) O1 0.0239(14) 0.0272(15) 0.0270(14) 0.0023(12) 0.0015(11) -0.0033(12) O2 0.0223(13) 0.0302(15) 0.0248(14) 0.0008(12) 0.0047(11) -0.0009(12) O3 0.0198(13) 0.0253(15) 0.0274(14) 0.0020(12) 0.0001(11) 0.0003(11) O4 0.0254(14) 0.0245(14) 0.0244(13) 0.0029(11) 0.0068(11) -0.0001(11) N1 0.0307(18) 0.0268(19) 0.0328(18) 0.0000(15) 0.0028(15) -0.0016(15) N2 0.0337(19) 0.0218(18) 0.041(2) -0.0005(16) 0.0159(16) 0.0012(15) N3 0.0232(17) 0.0319(19) 0.0283(18) -0.0018(14) 0.0068(14) 0.0032(14) N4 0.0216(17) 0.0324(19) 0.0286(18) 0.0012(15) 0.0047(14) 0.0015(14) C1 0.025(2) 0.084(4) 0.035(3) 0.025(3) 0.001(2) 0.000(3) C2 0.034(3) 0.060(3) 0.048(3) 0.018(2) 0.010(2) 0.001(2) C3 0.030(2) 0.084(4) 0.024(2) 0.008(2) -0.0016(18) -0.006(3) C4 0.024(2) 0.045(3) 0.036(2) 0.008(2) 0.0014(18) -0.004(2) C5 0.026(2) 0.061(3) 0.026(2) 0.001(2) 0.0068(18) -0.009(2) C6 0.021(2) 0.048(3) 0.027(2) 0.006(2) 0.0072(17) -0.0097(19) C7 0.032(2) 0.073(4) 0.026(2) -0.009(2) 0.0076(19) -0.015(2) C8 0.0205(19) 0.040(3) 0.025(2) 0.0013(18) 0.0046(16) -0.0072(18) C9 0.031(2) 0.051(3) 0.029(2) -0.011(2) 0.0105(19) -0.013(2) C10 0.027(2) 0.039(3) 0.032(2) -0.0042(19) 0.0115(18) -0.0070(19) C11 0.043(3) 0.054(3) 0.043(3) -0.022(2) 0.014(2) -0.015(2) C12 0.034(2) 0.039(3) 0.034(2) -0.004(2) 0.0066(19) -0.002(2) C13 0.055(3) 0.041(3) 0.055(3) -0.011(2) 0.021(3) -0.008(2) C14 0.046(3) 0.039(3) 0.049(3) -0.002(2) 0.015(2) -0.005(2) C15 0.0163(19) 0.037(2) 0.026(2) -0.0022(18) 0.0017(16) 0.0046(18) C16 0.053(3) 0.049(3) 0.029(2) -0.008(2) 0.012(2) -0.005(2) C17 0.039(2) 0.048(3) 0.036(2) 0.002(2) -0.003(2) 0.000(2) C18 0.043(3) 0.040(3) 0.036(2) -0.004(2) 0.015(2) 0.002(2) C19 0.030(2) 0.041(3) 0.032(2) 0.000(2) 0.0076(18) 0.003(2) C20 0.034(2) 0.029(2) 0.032(2) 0.0023(18) 0.0078(18) -0.0040(19) C21 0.028(2) 0.027(2) 0.030(2) -0.0023(18) 0.0050(17) -0.0060(18) C22 0.030(2) 0.028(2) 0.045(3) 0.000(2) 0.015(2) 0.0034(19) C23 0.025(2) 0.022(2) 0.031(2) 0.0009(17) 0.0041(17) -0.0013(17) C24 0.024(2) 0.033(2) 0.040(2) 0.0016(19) 0.0060(18) -0.0039(18) C25 0.024(2) 0.026(2) 0.032(2) 0.0001(17) 0.0067(17) -0.0024(17) C26 0.031(2) 0.034(3) 0.051(3) 0.006(2) 0.007(2) 0.006(2) C27 0.030(2) 0.038(2) 0.033(2) 0.001(2) 0.0055(18) 0.0073(19) C28 0.033(2) 0.048(3) 0.039(3) 0.011(2) 0.002(2) 0.009(2) C29 0.045(3) 0.048(3) 0.032(2) 0.005(2) 0.002(2) 0.004(2) C30 0.023(2) 0.033(2) 0.0230(19) -0.0046(18) -0.0004(16) -0.0009(18) C31 0.034(2) 0.046(3) 0.046(3) 0.001(2) 0.011(2) -0.009(2) C32 0.025(2) 0.057(3) 0.050(3) 0.011(2) 0.000(2) 0.002(2) C33 0.026(2) 0.045(3) 0.038(2) -0.003(2) 0.0101(18) -0.0007(19) C34 0.033(2) 0.053(3) 0.027(2) 0.000(2) 0.0017(18) 0.001(2) C35 0.059(3) 0.043(3) 0.037(3) -0.011(2) 0.009(2) -0.013(2) C36 0.036(2) 0.038(2) 0.0181(19) -0.0035(17) 0.0074(17) -0.0029(19) C37 0.035(2) 0.027(2) 0.031(2) 0.0037(18) 0.0093(19) -0.0012(18) C38 0.038(3) 0.049(3) 0.035(2) 0.004(2) 0.014(2) 0.009(2) C39 0.031(2) 0.054(3) 0.051(3) 0.012(2) 0.009(2) 0.012(2) C40 0.058(3) 0.058(3) 0.054(3) 0.002(3) 0.027(3) 0.008(3) C41 0.043(3) 0.029(2) 0.042(3) 0.005(2) 0.008(2) 0.009(2) C42 0.045(3) 0.057(3) 0.038(3) 0.008(2) 0.004(2) -0.016(2) C43 0.033(2) 0.054(3) 0.036(2) 0.003(2) 0.0034(19) -0.010(2) C44 0.038(2) 0.042(3) 0.029(2) -0.003(2) 0.0002(19) -0.013(2) C45 0.046(3) 0.026(2) 0.030(2) 0.0011(18) 0.006(2) -0.005(2) C46 0.060(3) 0.024(2) 0.044(3) -0.001(2) -0.002(2) 0.003(2) O5 0.119(4) 0.091(3) 0.052(2) 0.003(2) -0.036(2) -0.041(3) C48 0.065(4) 0.073(4) 0.057(3) 0.015(3) -0.011(3) -0.024(3) C49 0.045(3) 0.049(3) 0.041(3) -0.007(2) 0.000(2) -0.007(2) C50 0.060(3) 0.060(3) 0.049(3) -0.007(3) 0.001(3) 0.002(3) C51 0.067(4) 0.084(4) 0.044(3) -0.021(3) 0.019(3) -0.021(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Mo1 O3 2.104(2) . ? Mo1 O1 2.117(2) . ? Mo1 Mo2 2.1308(4) . ? Mo1 N2 2.156(3) . ? Mo1 N1 2.165(3) . ? Mo1 C45 2.600(4) . ? Mo2 O2 2.096(2) . ? Mo2 O4 2.105(2) . ? Mo2 N3 2.159(3) . ? Mo2 N4 2.161(3) . ? Mo2 C37 2.589(4) . ? O1 C15 1.272(4) . ? O2 C15 1.276(4) . ? O3 C30 1.284(4) . ? O4 C30 1.276(4) . ? N1 C45 1.340(5) . ? N1 C44 1.466(5) . ? N2 C45 1.316(5) . ? N2 C41 1.473(5) . ? N3 C37 1.320(5) . ? N3 C36 1.453(5) . ? N4 C37 1.330(5) . ? N4 C33 1.484(5) . ? C1 C3 1.341(7) . ? C1 C2 1.415(6) . ? C1 H1 0.95 . ? C2 C4 1.360(6) . ? C2 H2 0.95 . ? C3 C5 1.420(6) . ? C3 H3 0.95 . ? C4 C6 1.425(6) . ? C4 H4 0.95 . ? C5 C7 1.382(6) . ? C5 C6 1.442(5) . ? C6 C8 1.421(5) . ? C7 C9 1.396(6) . ? C7 H7 0.95 . ? C8 C10 1.414(5) . ? C8 C15 1.500(5) . ? C9 C11 1.428(6) . ? C9 C10 1.438(5) . ? C10 C12 1.423(6) . ? C11 C13 1.350(6) . ? C11 H11 0.95 . ? C12 C14 1.366(6) . ? C12 H12 0.95 . ? C13 C14 1.410(6) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C16 C18 1.339(6) . ? C16 C17 1.407(6) . ? C16 H16 0.95 . ? C17 C19 1.366(5) . ? C17 H17 0.95 . ? C18 C20 1.421(5) . ? C18 H18 0.95 . ? C19 C21 1.423(5) . ? C19 H19 0.95 . ? C20 C22 1.400(5) . ? C20 C21 1.433(5) . ? C21 C23 1.412(5) . ? C22 C24 1.387(6) . ? C22 H22 0.95 . ? C23 C25 1.418(5) . ? C23 C30 1.490(5) . ? C24 C25 1.431(5) . ? C24 C26 1.431(6) . ? C25 C27 1.420(5) . ? C26 C28 1.354(6) . ? C26 H26 0.95 . ? C27 C29 1.367(5) . ? C27 H27 0.95 . ? C28 C29 1.416(6) . ? C28 H28 0.95 . ? C29 H29 0.95 . ? C31 C33 1.524(6) . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 C33 1.501(5) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33 1 . ? C34 C36 1.522(5) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.515(5) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36 1 . ? C37 C38 1.521(5) . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 C41 1.502(6) . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C41 1.546(6) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 H41 1 . ? C42 C44 1.526(5) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 C44 1.509(6) . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44 1 . ? C45 C46 1.499(5) . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? O5 C48 1.407(6) . ? O5 C51 1.410(6) . ? C48 C49 1.505(6) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 C50 1.523(6) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 C51 1.509(6) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mo1 O1 85.55(9) . . ? O3 Mo1 Mo2 91.35(7) . . ? O1 Mo1 Mo2 91.11(7) . . ? O3 Mo1 N2 153.76(11) . . ? O1 Mo1 N2 107.16(11) . . ? Mo2 Mo1 N2 110.77(8) . . ? O3 Mo1 N1 97.17(11) . . ? O1 Mo1 N1 152.26(11) . . ? Mo2 Mo1 N1 116.32(8) . . ? N2 Mo1 N1 60.92(12) . . ? O3 Mo1 C45 125.39(11) . . ? O1 Mo1 C45 130.68(11) . . ? Mo2 Mo1 C45 121.17(8) . . ? N2 Mo1 C45 30.34(12) . . ? N1 Mo1 C45 30.98(12) . . ? O2 Mo2 O4 86.37(9) . . ? O2 Mo2 Mo1 91.29(7) . . ? O4 Mo2 Mo1 90.91(7) . . ? O2 Mo2 N3 153.13(10) . . ? O4 Mo2 N3 105.93(10) . . ? Mo1 Mo2 N3 111.86(8) . . ? O2 Mo2 N4 96.79(10) . . ? O4 Mo2 N4 152.11(11) . . ? Mo1 Mo2 N4 116.62(8) . . ? N3 Mo2 N4 61.27(11) . . ? O2 Mo2 C37 125.10(11) . . ? O4 Mo2 C37 130.59(11) . . ? Mo1 Mo2 C37 121.14(9) . . ? N3 Mo2 C37 30.61(11) . . ? N4 Mo2 C37 30.87(12) . . ? C15 O1 Mo1 117.7(2) . . ? C15 O2 Mo2 118.6(2) . . ? C30 O3 Mo1 118.5(2) . . ? C30 O4 Mo2 118.9(2) . . ? C45 N1 C44 121.8(3) . . ? C45 N1 Mo1 92.8(2) . . ? C44 N1 Mo1 133.0(3) . . ? C45 N2 C41 122.7(3) . . ? C45 N2 Mo1 93.9(2) . . ? C41 N2 Mo1 143.3(3) . . ? C37 N3 C36 123.9(3) . . ? C37 N3 Mo2 93.0(2) . . ? C36 N3 Mo2 143.1(2) . . ? C37 N4 C33 122.3(3) . . ? C37 N4 Mo2 92.7(2) . . ? C33 N4 Mo2 133.0(2) . . ? C3 C1 C2 120.3(4) . . ? C3 C1 H1 119.8 . . ? C2 C1 H1 119.8 . . ? C4 C2 C1 120.3(5) . . ? C4 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C1 C3 C5 121.7(4) . . ? C1 C3 H3 119.1 . . ? C5 C3 H3 119.1 . . ? C2 C4 C6 121.7(4) . . ? C2 C4 H4 119.2 . . ? C6 C4 H4 119.2 . . ? C7 C5 C3 121.3(4) . . ? C7 C5 C6 120.0(4) . . ? C3 C5 C6 118.7(4) . . ? C8 C6 C4 124.4(4) . . ? C8 C6 C5 118.3(4) . . ? C4 C6 C5 117.3(4) . . ? C5 C7 C9 122.2(4) . . ? C5 C7 H7 118.9 . . ? C9 C7 H7 118.9 . . ? C10 C8 C6 121.2(4) . . ? C10 C8 C15 119.8(3) . . ? C6 C8 C15 118.9(4) . . ? C7 C9 C11 121.9(4) . . ? C7 C9 C10 119.3(4) . . ? C11 C9 C10 118.8(4) . . ? C8 C10 C12 123.3(4) . . ? C8 C10 C9 119.0(4) . . ? C12 C10 C9 117.6(4) . . ? C13 C11 C9 121.3(4) . . ? C13 C11 H11 119.4 . . ? C9 C11 H11 119.4 . . ? C14 C12 C10 121.4(4) . . ? C14 C12 H12 119.3 . . ? C10 C12 H12 119.3 . . ? C11 C13 C14 120.4(4) . . ? C11 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C12 C14 C13 120.5(5) . . ? C12 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? O1 C15 O2 121.2(3) . . ? O1 C15 C8 120.7(3) . . ? O2 C15 C8 118.0(3) . . ? C18 C16 C17 119.9(4) . . ? C18 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C19 C17 C16 121.2(4) . . ? C19 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C16 C18 C20 121.9(4) . . ? C16 C18 H18 119 . . ? C20 C18 H18 119 . . ? C17 C19 C21 120.4(4) . . ? C17 C19 H19 119.8 . . ? C21 C19 H19 119.8 . . ? C22 C20 C18 122.0(4) . . ? C22 C20 C21 119.5(4) . . ? C18 C20 C21 118.4(4) . . ? C23 C21 C19 123.1(3) . . ? C23 C21 C20 118.7(3) . . ? C19 C21 C20 118.2(3) . . ? C24 C22 C20 121.8(4) . . ? C24 C22 H22 119.1 . . ? C20 C22 H22 119.1 . . ? C21 C23 C25 121.4(3) . . ? C21 C23 C30 118.7(3) . . ? C25 C23 C30 119.9(3) . . ? C22 C24 C25 119.9(4) . . ? C22 C24 C26 121.5(4) . . ? C25 C24 C26 118.6(4) . . ? C23 C25 C27 123.2(3) . . ? C23 C25 C24 118.5(3) . . ? C27 C25 C24 118.2(4) . . ? C28 C26 C24 121.5(4) . . ? C28 C26 H26 119.3 . . ? C24 C26 H26 119.3 . . ? C29 C27 C25 121.1(4) . . ? C29 C27 H27 119.4 . . ? C25 C27 H27 119.4 . . ? C26 C28 C29 119.8(4) . . ? C26 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C27 C29 C28 120.7(4) . . ? C27 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? O4 C30 O3 119.9(3) . . ? O4 C30 C23 120.5(3) . . ? O3 C30 C23 119.6(3) . . ? C33 C31 H31A 109.5 . . ? C33 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C33 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 C32 111.1(3) . . ? N4 C33 C31 109.4(3) . . ? C32 C33 C31 111.1(4) . . ? N4 C33 H33 108.4 . . ? C32 C33 H33 108.4 . . ? C31 C33 H33 108.4 . . ? C36 C34 H34A 109.5 . . ? C36 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C36 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C35 110.9(3) . . ? N3 C36 C34 108.7(3) . . ? C35 C36 C34 111.1(3) . . ? N3 C36 H36 108.7 . . ? C35 C36 H36 108.7 . . ? C34 C36 H36 108.7 . . ? N3 C37 N4 112.3(3) . . ? N3 C37 C38 124.6(4) . . ? N4 C37 C38 123.1(4) . . ? N3 C37 Mo2 56.38(19) . . ? N4 C37 Mo2 56.47(19) . . ? C38 C37 Mo2 173.0(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 H39A 109.5 . . ? C41 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C41 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N2 C41 C39 110.0(3) . . ? N2 C41 C40 109.5(3) . . ? C39 C41 C40 112.4(4) . . ? N2 C41 H41 108.3 . . ? C39 C41 H41 108.3 . . ? C40 C41 H41 108.3 . . ? C44 C42 H42A 109.5 . . ? C44 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C44 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N1 C44 C43 110.2(3) . . ? N1 C44 C42 110.3(3) . . ? C43 C44 C42 110.2(4) . . ? N1 C44 H44 108.7 . . ? C43 C44 H44 108.7 . . ? C42 C44 H44 108.7 . . ? N2 C45 N1 111.1(3) . . ? N2 C45 C46 125.1(4) . . ? N1 C45 C46 123.8(4) . . ? N2 C45 Mo1 55.8(2) . . ? N1 C45 Mo1 56.3(2) . . ? C46 C45 Mo1 171.3(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 O5 C51 109.6(4) . . ? O5 C48 C49 105.4(4) . . ? O5 C48 H48A 110.7 . . ? C49 C48 H48A 110.7 . . ? O5 C48 H48B 110.7 . . ? C49 C48 H48B 110.7 . . ? H48A C48 H48B 108.8 . . ? C48 C49 C50 101.9(4) . . ? C48 C49 H49A 111.4 . . ? C50 C49 H49A 111.4 . . ? C48 C49 H49B 111.4 . . ? C50 C49 H49B 111.4 . . ? H49A C49 H49B 109.2 . . ? C51 C50 C49 103.1(4) . . ? C51 C50 H50A 111.1 . . ? C49 C50 H50A 111.1 . . ? C51 C50 H50B 111.1 . . ? C49 C50 H50B 111.1 . . ? H50A C50 H50B 109.1 . . ? O5 C51 C50 107.8(4) . . ? O5 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? O5 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mo1 Mo2 O2 -83.91(9) . . . . ? O1 Mo1 Mo2 O2 1.67(9) . . . . ? N2 Mo1 Mo2 O2 110.51(12) . . . . ? N1 Mo1 Mo2 O2 177.41(11) . . . . ? C45 Mo1 Mo2 O2 142.36(13) . . . . ? O3 Mo1 Mo2 O4 2.48(9) . . . . ? O1 Mo1 Mo2 O4 88.06(9) . . . . ? N2 Mo1 Mo2 O4 -163.10(12) . . . . ? N1 Mo1 Mo2 O4 -96.20(11) . . . . ? C45 Mo1 Mo2 O4 -131.25(13) . . . . ? O3 Mo1 Mo2 N3 110.06(11) . . . . ? O1 Mo1 Mo2 N3 -164.36(11) . . . . ? N2 Mo1 Mo2 N3 -55.52(13) . . . . ? N1 Mo1 Mo2 N3 11.39(13) . . . . ? C45 Mo1 Mo2 N3 -23.66(14) . . . . ? O3 Mo1 Mo2 N4 177.83(11) . . . . ? O1 Mo1 Mo2 N4 -96.59(11) . . . . ? N2 Mo1 Mo2 N4 12.25(14) . . . . ? N1 Mo1 Mo2 N4 79.16(13) . . . . ? C45 Mo1 Mo2 N4 44.11(14) . . . . ? O3 Mo1 Mo2 C37 142.82(13) . . . . ? O1 Mo1 Mo2 C37 -131.61(13) . . . . ? N2 Mo1 Mo2 C37 -22.76(15) . . . . ? N1 Mo1 Mo2 C37 44.14(14) . . . . ? C45 Mo1 Mo2 C37 9.09(16) . . . . ? O3 Mo1 O1 C15 87.8(2) . . . . ? Mo2 Mo1 O1 C15 -3.5(2) . . . . ? N2 Mo1 O1 C15 -115.6(2) . . . . ? N1 Mo1 O1 C15 -175.2(3) . . . . ? C45 Mo1 O1 C15 -137.8(2) . . . . ? O4 Mo2 O2 C15 -91.4(2) . . . . ? Mo1 Mo2 O2 C15 -0.6(2) . . . . ? N3 Mo2 O2 C15 149.7(3) . . . . ? N4 Mo2 O2 C15 116.4(3) . . . . ? C37 Mo2 O2 C15 129.8(2) . . . . ? O1 Mo1 O3 C30 -90.7(3) . . . . ? Mo2 Mo1 O3 C30 0.3(2) . . . . ? N2 Mo1 O3 C30 148.5(3) . . . . ? N1 Mo1 O3 C30 117.0(3) . . . . ? C45 Mo1 O3 C30 131.0(3) . . . . ? O2 Mo2 O4 C30 84.9(3) . . . . ? Mo1 Mo2 O4 C30 -6.4(2) . . . . ? N3 Mo2 O4 C30 -119.4(3) . . . . ? N4 Mo2 O4 C30 -177.5(3) . . . . ? C37 Mo2 O4 C30 -140.4(2) . . . . ? O3 Mo1 N1 C45 157.6(2) . . . . ? O1 Mo1 N1 C45 63.5(3) . . . . ? Mo2 Mo1 N1 C45 -107.3(2) . . . . ? N2 Mo1 N1 C45 -7.1(2) . . . . ? O3 Mo1 N1 C44 17.5(3) . . . . ? O1 Mo1 N1 C44 -76.6(4) . . . . ? Mo2 Mo1 N1 C44 112.6(3) . . . . ? N2 Mo1 N1 C44 -147.2(4) . . . . ? C45 Mo1 N1 C44 -140.1(5) . . . . ? O3 Mo1 N2 C45 -29.1(4) . . . . ? O1 Mo1 N2 C45 -145.4(2) . . . . ? Mo2 Mo1 N2 C45 116.6(2) . . . . ? N1 Mo1 N2 C45 7.2(2) . . . . ? O3 Mo1 N2 C41 147.4(4) . . . . ? O1 Mo1 N2 C41 31.1(4) . . . . ? Mo2 Mo1 N2 C41 -66.9(4) . . . . ? N1 Mo1 N2 C41 -176.3(5) . . . . ? C45 Mo1 N2 C41 176.5(6) . . . . ? O2 Mo2 N3 C37 -33.1(4) . . . . ? O4 Mo2 N3 C37 -147.8(2) . . . . ? Mo1 Mo2 N3 C37 114.6(2) . . . . ? N4 Mo2 N3 C37 5.3(2) . . . . ? O2 Mo2 N3 C36 146.2(4) . . . . ? O4 Mo2 N3 C36 31.5(4) . . . . ? Mo1 Mo2 N3 C36 -66.1(4) . . . . ? N4 Mo2 N3 C36 -175.4(5) . . . . ? C37 Mo2 N3 C36 179.3(6) . . . . ? O2 Mo2 N4 C37 158.3(2) . . . . ? O4 Mo2 N4 C37 63.2(3) . . . . ? Mo1 Mo2 N4 C37 -106.8(2) . . . . ? N3 Mo2 N4 C37 -5.2(2) . . . . ? O2 Mo2 N4 C33 17.6(3) . . . . ? O4 Mo2 N4 C33 -77.5(4) . . . . ? Mo1 Mo2 N4 C33 112.4(3) . . . . ? N3 Mo2 N4 C33 -146.0(4) . . . . ? C37 Mo2 N4 C33 -140.8(5) . . . . ? C3 C1 C2 C4 -0.4(6) . . . . ? C2 C1 C3 C5 0.7(7) . . . . ? C1 C2 C4 C6 -0.3(6) . . . . ? C1 C3 C5 C7 179.2(4) . . . . ? C1 C3 C5 C6 -0.3(6) . . . . ? C2 C4 C6 C8 -177.7(4) . . . . ? C2 C4 C6 C5 0.6(6) . . . . ? C7 C5 C6 C8 -1.4(5) . . . . ? C3 C5 C6 C8 178.1(3) . . . . ? C7 C5 C6 C4 -179.8(4) . . . . ? C3 C5 C6 C4 -0.3(5) . . . . ? C3 C5 C7 C9 -179.4(4) . . . . ? C6 C5 C7 C9 0.1(6) . . . . ? C4 C6 C8 C10 180.0(4) . . . . ? C5 C6 C8 C10 1.7(5) . . . . ? C4 C6 C8 C15 3.4(5) . . . . ? C5 C6 C8 C15 -174.9(3) . . . . ? C5 C7 C9 C11 -178.5(4) . . . . ? C5 C7 C9 C10 0.9(6) . . . . ? C6 C8 C10 C12 176.7(3) . . . . ? C15 C8 C10 C12 -6.8(6) . . . . ? C6 C8 C10 C9 -0.8(5) . . . . ? C15 C8 C10 C9 175.8(3) . . . . ? C7 C9 C10 C8 -0.5(5) . . . . ? C11 C9 C10 C8 178.9(4) . . . . ? C7 C9 C10 C12 -178.1(4) . . . . ? C11 C9 C10 C12 1.3(5) . . . . ? C7 C9 C11 C13 178.4(4) . . . . ? C10 C9 C11 C13 -1.0(6) . . . . ? C8 C10 C12 C14 -178.3(4) . . . . ? C9 C10 C12 C14 -0.8(6) . . . . ? C9 C11 C13 C14 0.2(7) . . . . ? C10 C12 C14 C13 0.0(6) . . . . ? C11 C13 C14 C12 0.3(7) . . . . ? Mo1 O1 C15 O2 3.8(4) . . . . ? Mo1 O1 C15 C8 -175.4(2) . . . . ? Mo2 O2 C15 O1 -2.0(4) . . . . ? Mo2 O2 C15 C8 177.2(2) . . . . ? C10 C8 C15 O1 133.8(4) . . . . ? C6 C8 C15 O1 -49.6(5) . . . . ? C10 C8 C15 O2 -45.5(5) . . . . ? C6 C8 C15 O2 131.1(4) . . . . ? C18 C16 C17 C19 0.3(7) . . . . ? C17 C16 C18 C20 0.5(7) . . . . ? C16 C17 C19 C21 -0.4(6) . . . . ? C16 C18 C20 C22 177.8(4) . . . . ? C16 C18 C20 C21 -1.1(6) . . . . ? C17 C19 C21 C23 -177.6(4) . . . . ? C17 C19 C21 C20 -0.3(6) . . . . ? C22 C20 C21 C23 -0.5(6) . . . . ? C18 C20 C21 C23 178.4(4) . . . . ? C22 C20 C21 C19 -177.9(4) . . . . ? C18 C20 C21 C19 1.0(5) . . . . ? C18 C20 C22 C24 -177.9(4) . . . . ? C21 C20 C22 C24 1.0(6) . . . . ? C19 C21 C23 C25 176.1(4) . . . . ? C20 C21 C23 C25 -1.2(6) . . . . ? C19 C21 C23 C30 -4.6(6) . . . . ? C20 C21 C23 C30 178.2(3) . . . . ? C20 C22 C24 C25 0.2(6) . . . . ? C20 C22 C24 C26 -179.4(4) . . . . ? C21 C23 C25 C27 -178.9(4) . . . . ? C30 C23 C25 C27 1.8(6) . . . . ? C21 C23 C25 C24 2.3(6) . . . . ? C30 C23 C25 C24 -177.0(3) . . . . ? C22 C24 C25 C23 -1.8(6) . . . . ? C26 C24 C25 C23 177.8(4) . . . . ? C22 C24 C25 C27 179.3(4) . . . . ? C26 C24 C25 C27 -1.1(6) . . . . ? C22 C24 C26 C28 -178.8(4) . . . . ? C25 C24 C26 C28 1.6(6) . . . . ? C23 C25 C27 C29 -178.1(4) . . . . ? C24 C25 C27 C29 0.7(6) . . . . ? C24 C26 C28 C29 -1.6(7) . . . . ? C25 C27 C29 C28 -0.8(6) . . . . ? C26 C28 C29 C27 1.2(7) . . . . ? Mo2 O4 C30 O3 8.0(4) . . . . ? Mo2 O4 C30 C23 -170.9(2) . . . . ? Mo1 O3 C30 O4 -5.3(4) . . . . ? Mo1 O3 C30 C23 173.6(2) . . . . ? C21 C23 C30 O4 120.8(4) . . . . ? C25 C23 C30 O4 -59.8(5) . . . . ? C21 C23 C30 O3 -58.1(5) . . . . ? C25 C23 C30 O3 121.3(4) . . . . ? C37 N4 C33 C32 153.6(4) . . . . ? Mo2 N4 C33 C32 -74.8(4) . . . . ? C37 N4 C33 C31 -83.4(4) . . . . ? Mo2 N4 C33 C31 48.3(5) . . . . ? C37 N3 C36 C35 -82.9(5) . . . . ? Mo2 N3 C36 C35 98.0(4) . . . . ? C37 N3 C36 C34 154.7(4) . . . . ? Mo2 N3 C36 C34 -24.4(6) . . . . ? C36 N3 C37 N4 172.4(3) . . . . ? Mo2 N3 C37 N4 -8.2(3) . . . . ? C36 N3 C37 C38 -7.8(6) . . . . ? Mo2 N3 C37 C38 171.7(3) . . . . ? C36 N3 C37 Mo2 -179.5(4) . . . . ? C33 N4 C37 N3 155.0(3) . . . . ? Mo2 N4 C37 N3 8.1(3) . . . . ? C33 N4 C37 C38 -24.9(6) . . . . ? Mo2 N4 C37 C38 -171.7(3) . . . . ? C33 N4 C37 Mo2 146.8(4) . . . . ? O2 Mo2 C37 N3 162.4(2) . . . . ? O4 Mo2 C37 N3 42.4(3) . . . . ? Mo1 Mo2 C37 N3 -80.4(2) . . . . ? N4 Mo2 C37 N3 -170.9(4) . . . . ? O2 Mo2 C37 N4 -26.6(3) . . . . ? O4 Mo2 C37 N4 -146.6(2) . . . . ? Mo1 Mo2 C37 N4 90.5(2) . . . . ? N3 Mo2 C37 N4 170.9(4) . . . . ? C45 N2 C41 C39 152.7(4) . . . . ? Mo1 N2 C41 C39 -23.2(6) . . . . ? C45 N2 C41 C40 -83.4(5) . . . . ? Mo1 N2 C41 C40 100.8(5) . . . . ? C45 N1 C44 C43 157.6(4) . . . . ? Mo1 N1 C44 C43 -71.4(4) . . . . ? C45 N1 C44 C42 -80.6(5) . . . . ? Mo1 N1 C44 C42 50.5(5) . . . . ? C41 N2 C45 N1 171.5(3) . . . . ? Mo1 N2 C45 N1 -11.0(3) . . . . ? C41 N2 C45 C46 -8.0(6) . . . . ? Mo1 N2 C45 C46 169.5(3) . . . . ? C41 N2 C45 Mo1 -177.5(4) . . . . ? C44 N1 C45 N2 157.4(3) . . . . ? Mo1 N1 C45 N2 10.9(3) . . . . ? C44 N1 C45 C46 -23.1(6) . . . . ? Mo1 N1 C45 C46 -169.6(3) . . . . ? C44 N1 C45 Mo1 146.5(4) . . . . ? O3 Mo1 C45 N2 164.7(2) . . . . ? O1 Mo1 C45 N2 45.7(3) . . . . ? Mo2 Mo1 C45 N2 -77.7(2) . . . . ? N1 Mo1 C45 N2 -167.6(4) . . . . ? O3 Mo1 C45 N1 -27.7(3) . . . . ? O1 Mo1 C45 N1 -146.7(2) . . . . ? Mo2 Mo1 C45 N1 89.9(2) . . . . ? N2 Mo1 C45 N1 167.6(4) . . . . ? C51 O5 C48 C49 27.3(6) . . . . ? O5 C48 C49 C50 -35.0(5) . . . . ? C48 C49 C50 C51 29.4(5) . . . . ? C48 O5 C51 C50 -7.7(6) . . . . ? C49 C50 C51 O5 -14.6(5) . . . . ? #END OF CIF