# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_020jart13 #TrackingRef '2a.cif' _audit_creation_date 13-03-25 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '020jart13 At 23:14 on 13/ 1' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 8.10950(10) _cell_length_b 15.6301(3) _cell_length_c 16.3634(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2074.10(6) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c 21 n ' _symmetry_space_group_name_Hall 'P -2n -2ac' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,-z+1/2 -x+1/2,y,z+1/2 -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C22 H28 Al1 N2 # Dc = 1.11 Fooo = 760.00 Mu = 1.04 M = 347.46 # Found Formula = C22 H31 Al1 N2 # Dc = 1.12 FOOO = 760.00 Mu = 1.04 M = 350.48 _chemical_formula_sum 'C22 H31 Al1 N2' _chemical_formula_moiety 'C22 H31 Al1 N2' _chemical_compound_source . _chemical_formula_weight 350.48 _cell_measurement_reflns_used 2595 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.210 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_max 0.330 _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.104 # Sheldrick geometric approximatio 0.97 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.98 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 23363 _reflns_number_total 2447 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections without Friedels Law is 4315 # Number of reflections with Friedels Law is 2447 # Theoretical number of reflections is about 2380 _diffrn_reflns_theta_min 5.152 _diffrn_reflns_theta_max 27.488 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.664 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.38 _oxford_diffrn_Wilson_scale 3.34 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.29 _refine_diff_density_max 0.27 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 2447 _refine_ls_number_restraints 1 _refine_ls_number_parameters 238 _oxford_refine_ls_R_factor_ref 0.0507 _refine_ls_wR_factor_ref 0.1008 _refine_ls_goodness_of_fit_ref 0.9516 _refine_ls_shift/su_max 0.0004174 _refine_ls_shift/su_mean 0.0000311 # The values computed with all filters except I/sigma _oxford_reflns_number_all 2447 _refine_ls_R_factor_all 0.0507 _refine_ls_wR_factor_all 0.1008 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2140 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_gt 0.0889 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 43.2 71.9 44.9 19.6 4.87 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Al1 Al 0.71359(8) 0.60749(9) 0.24530(4) 0.0274 1.0000 Uani . . . . . . C2 C 0.4583(3) 0.59320(16) 0.23707(14) 0.0220 1.0000 Uani . . . . . . N3 N 0.3741(2) 0.54744(15) 0.29197(12) 0.0240 1.0000 Uani . . . . . . C4 C 0.4573(3) 0.50952(17) 0.36139(14) 0.0240 1.0000 Uani . . . . . . C5 C 0.4922(3) 0.55921(17) 0.42995(15) 0.0248 1.0000 Uani . . . . . . C6 C 0.4482(4) 0.65254(18) 0.43370(17) 0.0332 1.0000 Uani . . . . . . C7 C 0.5717(3) 0.5195(2) 0.49557(15) 0.0273 1.0000 Uani . . . . . . C8 C 0.6122(3) 0.43305(19) 0.49458(15) 0.0289 1.0000 Uani . . . . . . C9 C 0.5733(3) 0.38582(19) 0.42533(16) 0.0299 1.0000 Uani . . . . . . C10 C 0.4963(3) 0.42244(18) 0.35818(15) 0.0267 1.0000 Uani . . . . . . C11 C 0.4624(4) 0.3702(2) 0.28261(17) 0.0380 1.0000 Uani . . . . . . C12 C 0.6921(4) 0.3904(2) 0.56760(18) 0.0377 1.0000 Uani . . . . . . C13 C 0.1941(3) 0.5319(2) 0.28745(16) 0.0304 1.0000 Uani . . . . . . C14 C 0.1420(3) 0.53140(19) 0.19850(17) 0.0289 1.0000 Uani . . . . . . C15 C 0.1958(3) 0.6152(2) 0.16050(16) 0.0303 1.0000 Uani . . . . . . N16 N 0.3739(2) 0.62838(15) 0.17487(12) 0.0244 1.0000 Uani . . . . . . C17 C 0.4567(3) 0.68285(17) 0.11638(14) 0.0239 1.0000 Uani . . . . . . C18 C 0.4818(3) 0.76854(18) 0.13441(14) 0.0265 1.0000 Uani . . . . . . C19 C 0.4297(4) 0.8084(2) 0.21495(17) 0.0355 1.0000 Uani . . . . . . C20 C 0.5630(3) 0.81891(18) 0.07581(16) 0.0288 1.0000 Uani . . . . . . C21 C 0.6157(3) 0.78562(18) 0.00205(15) 0.0258 1.0000 Uani . . . . . . C22 C 0.5852(3) 0.69904(17) -0.01473(15) 0.0252 1.0000 Uani . . . . . . C23 C 0.5047(3) 0.64694(17) 0.04129(16) 0.0245 1.0000 Uani . . . . . . C24 C 0.4769(4) 0.55388(18) 0.02199(18) 0.0335 1.0000 Uani . . . . . . C25 C 0.7020(4) 0.8404(2) -0.05962(18) 0.0345 1.0000 Uani . . . . . . H61 H 0.4924 0.6762 0.4838 0.0502 1.0000 Uiso R . . . . . H63 H 0.4905 0.6847 0.3867 0.0502 1.0000 Uiso R . . . . . H62 H 0.3308 0.6594 0.4365 0.0506 1.0000 Uiso R . . . . . H71 H 0.5970 0.5524 0.5403 0.0329 1.0000 Uiso R . . . . . H91 H 0.6003 0.3277 0.4237 0.0362 1.0000 Uiso R . . . . . H111 H 0.4862 0.3114 0.2919 0.0571 1.0000 Uiso R . . . . . H112 H 0.5322 0.3896 0.2393 0.0574 1.0000 Uiso R . . . . . H113 H 0.3505 0.3765 0.2666 0.0573 1.0000 Uiso R . . . . . H122 H 0.7963 0.3627 0.5510 0.0575 1.0000 Uiso R . . . . . H121 H 0.7184 0.4318 0.6102 0.0571 1.0000 Uiso R . . . . . H123 H 0.6196 0.3480 0.5915 0.0573 1.0000 Uiso R . . . . . H132 H 0.1372 0.5774 0.3188 0.0355 1.0000 Uiso R . . . . . H131 H 0.1719 0.4764 0.3126 0.0362 1.0000 Uiso R . . . . . H141 H 0.0223 0.5245 0.1930 0.0351 1.0000 Uiso R . . . . . H142 H 0.1975 0.4838 0.1702 0.0347 1.0000 Uiso R . . . . . H152 H 0.1361 0.6636 0.1848 0.0353 1.0000 Uiso R . . . . . H151 H 0.1754 0.6145 0.1010 0.0356 1.0000 Uiso R . . . . . H191 H 0.3950 0.8670 0.2087 0.0534 1.0000 Uiso R . . . . . H193 H 0.5220 0.8089 0.2523 0.0534 1.0000 Uiso R . . . . . H192 H 0.3420 0.7758 0.2391 0.0532 1.0000 Uiso R . . . . . H201 H 0.5785 0.8777 0.0861 0.0350 1.0000 Uiso R . . . . . H221 H 0.6202 0.6757 -0.0645 0.0301 1.0000 Uiso R . . . . . H242 H 0.5405 0.5363 -0.0253 0.0503 1.0000 Uiso R . . . . . H241 H 0.5097 0.5206 0.0680 0.0504 1.0000 Uiso R . . . . . H243 H 0.3602 0.5437 0.0115 0.0497 1.0000 Uiso R . . . . . H252 H 0.7688 0.8052 -0.0944 0.0525 1.0000 Uiso R . . . . . H251 H 0.7696 0.8817 -0.0319 0.0521 1.0000 Uiso R . . . . . H253 H 0.6201 0.8705 -0.0920 0.0525 1.0000 Uiso R . . . . . H1 H 0.775(4) 0.620(3) 0.1635(19) 0.046(9) 1.0000 Uiso . . . . . . H2 H 0.782(5) 0.527(3) 0.294(3) 0.073(13) 1.0000 Uiso . . . . . . H5 H 0.737(6) 0.688(3) 0.292(3) 0.071(13) 1.0000 Uiso . . . . . . 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 Al1 0.0191(3) 0.0386(4) 0.0244(3) 0.0028(3) -0.0004(3) -0.0005(4) C2 0.0220(9) 0.0217(12) 0.0223(10) 0.0004(9) 0.0017(8) 0.0010(9) N3 0.0195(10) 0.0288(11) 0.0237(10) 0.0056(9) -0.0001(8) 0.0001(8) C4 0.0230(11) 0.0288(12) 0.0202(11) 0.0058(10) 0.0005(9) -0.0012(10) C5 0.0243(12) 0.0261(12) 0.0238(12) 0.0014(10) 0.0034(10) 0.0012(10) C6 0.0408(16) 0.0285(13) 0.0304(13) -0.0016(11) 0.0055(12) -0.0002(12) C7 0.0265(12) 0.0351(14) 0.0202(10) -0.0003(10) 0.0012(10) -0.0019(11) C8 0.0241(12) 0.0347(14) 0.0278(13) 0.0089(11) 0.0008(10) -0.0019(11) C9 0.0324(14) 0.0261(13) 0.0313(13) 0.0046(11) -0.0005(11) 0.0005(10) C10 0.0262(12) 0.0290(12) 0.0250(12) 0.0006(10) 0.0008(10) -0.0002(10) C11 0.0480(17) 0.0326(14) 0.0334(14) -0.0057(12) -0.0086(13) 0.0049(13) C12 0.0363(16) 0.0483(18) 0.0285(13) 0.0098(13) -0.0059(12) -0.0010(14) C13 0.0215(12) 0.0401(15) 0.0297(13) 0.0037(12) 0.0032(10) -0.0037(11) C14 0.0204(11) 0.0344(14) 0.0318(12) 0.0036(11) 0.0007(10) -0.0019(11) C15 0.0201(11) 0.0375(13) 0.0334(12) 0.0085(12) -0.0037(9) 0.0002(11) N16 0.0191(9) 0.0296(11) 0.0245(10) 0.0066(8) -0.0007(8) -0.0012(8) C17 0.0208(11) 0.0290(13) 0.0219(10) 0.0031(10) -0.0004(9) 0.0012(10) C18 0.0300(13) 0.0266(12) 0.0228(11) 0.0007(10) -0.0009(10) 0.0024(10) C19 0.0436(16) 0.0330(14) 0.0300(14) -0.0065(11) 0.0039(13) 0.0007(12) C20 0.0357(15) 0.0211(12) 0.0296(12) 0.0012(10) -0.0004(11) -0.0024(11) C21 0.0275(13) 0.0256(12) 0.0242(12) 0.0035(10) -0.0014(10) 0.0000(10) C22 0.0279(13) 0.0253(12) 0.0225(11) 0.0015(9) 0.0009(9) 0.0002(10) C23 0.0230(12) 0.0238(12) 0.0267(12) 0.0026(10) -0.0037(10) 0.0005(10) C24 0.0388(15) 0.0250(13) 0.0368(14) -0.0002(12) -0.0024(12) -0.0020(12) C25 0.0384(16) 0.0326(14) 0.0324(14) 0.0065(12) 0.0037(12) 0.0005(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5293(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Al1 . C2 . 2.086(2) yes Al1 . H1 . 1.44(3) no Al1 . H2 . 1.58(5) no Al1 . H5 . 1.48(5) no C2 . N3 . 1.336(3) yes C2 . N16 . 1.344(3) yes N3 . C4 . 1.448(3) yes N3 . C13 . 1.481(3) yes C4 . C5 . 1.394(3) yes C4 . C10 . 1.398(4) yes C5 . C6 . 1.503(4) yes C5 . C7 . 1.397(4) yes C6 . H61 . 0.969 no C6 . H63 . 0.980 no C6 . H62 . 0.959 no C7 . C8 . 1.391(4) yes C7 . H71 . 0.917 no C8 . C9 . 1.389(4) yes C8 . C12 . 1.514(4) yes C9 . C10 . 1.387(4) yes C9 . H91 . 0.935 no C10 . C11 . 1.507(4) yes C11 . H111 . 0.951 no C11 . H112 . 0.956 no C11 . H113 . 0.950 no C12 . H122 . 0.987 no C12 . H121 . 0.975 no C12 . H123 . 0.968 no C13 . C14 . 1.516(4) yes C13 . H132 . 0.991 no C13 . H131 . 0.977 no C14 . C15 . 1.515(4) yes C14 . H141 . 0.981 no C14 . H142 . 0.984 no C15 . N16 . 1.477(3) yes C15 . H152 . 0.982 no C15 . H151 . 0.987 no N16 . C17 . 1.446(3) yes C17 . C18 . 1.386(4) yes C17 . C23 . 1.406(3) yes C18 . C19 . 1.518(3) yes C18 . C20 . 1.405(4) yes C19 . H191 . 0.964 no C19 . H193 . 0.966 no C19 . H192 . 0.960 no C20 . C21 . 1.382(4) yes C20 . H201 . 0.943 no C21 . C22 . 1.403(4) yes C21 . C25 . 1.498(4) yes C22 . C23 . 1.389(4) yes C22 . H221 . 0.937 no C23 . C24 . 1.505(4) yes C24 . H242 . 0.970 no C24 . H241 . 0.954 no C24 . H243 . 0.974 no C25 . H252 . 0.960 no C25 . H251 . 0.960 no C25 . H253 . 0.971 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . Al1 . H1 . 107.4(13) no C2 . Al1 . H2 . 107.2(16) no H1 . Al1 . H2 . 117(2) no C2 . Al1 . H5 . 104.6(18) no H1 . Al1 . H5 . 109(2) no H2 . Al1 . H5 . 111(2) no Al1 . C2 . N3 . 121.41(17) yes Al1 . C2 . N16 . 120.69(17) yes N3 . C2 . N16 . 117.9(2) yes C2 . N3 . C4 . 120.6(2) yes C2 . N3 . C13 . 123.9(2) yes C4 . N3 . C13 . 115.5(2) yes N3 . C4 . C5 . 119.9(2) yes N3 . C4 . C10 . 118.3(2) yes C5 . C4 . C10 . 121.8(2) yes C4 . C5 . C6 . 121.7(2) yes C4 . C5 . C7 . 117.7(2) yes C6 . C5 . C7 . 120.6(3) yes C5 . C6 . H61 . 108.5 no C5 . C6 . H63 . 112.5 no H61 . C6 . H63 . 109.8 no C5 . C6 . H62 . 110.3 no H61 . C6 . H62 . 106.5 no H63 . C6 . H62 . 109.1 no C5 . C7 . C8 . 122.1(2) yes C5 . C7 . H71 . 117.9 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 118.2(2) yes C7 . C8 . C12 . 121.3(3) yes C9 . C8 . C12 . 120.4(3) yes C8 . C9 . C10 . 121.9(3) yes C8 . C9 . H91 . 119.1 no C10 . C9 . H91 . 119.0 no C4 . C10 . C9 . 118.3(2) yes C4 . C10 . C11 . 121.1(2) yes C9 . C10 . C11 . 120.5(3) yes C10 . C11 . H111 . 110.8 no C10 . C11 . H112 . 109.1 no H111 . C11 . H112 . 107.8 no C10 . C11 . H113 . 110.1 no H111 . C11 . H113 . 109.8 no H112 . C11 . H113 . 109.2 no C8 . C12 . H122 . 110.0 no C8 . C12 . H121 . 111.4 no H122 . C12 . H121 . 107.5 no C8 . C12 . H123 . 111.1 no H122 . C12 . H123 . 109.3 no H121 . C12 . H123 . 107.4 no N3 . C13 . C14 . 108.9(2) yes N3 . C13 . H132 . 108.4 no C14 . C13 . H132 . 111.8 no N3 . C13 . H131 . 107.8 no C14 . C13 . H131 . 110.4 no H132 . C13 . H131 . 109.5 no C13 . C14 . C15 . 108.0(2) yes C13 . C14 . H141 . 111.4 no C15 . C14 . H141 . 110.0 no C13 . C14 . H142 . 109.1 no C15 . C14 . H142 . 109.2 no H141 . C14 . H142 . 109.0 no C14 . C15 . N16 . 109.7(2) yes C14 . C15 . H152 . 110.9 no N16 . C15 . H152 . 108.1 no C14 . C15 . H151 . 110.3 no N16 . C15 . H151 . 108.8 no H152 . C15 . H151 . 108.9 no C15 . N16 . C2 . 124.2(2) yes C15 . N16 . C17 . 115.48(19) yes C2 . N16 . C17 . 120.4(2) yes N16 . C17 . C18 . 119.7(2) yes N16 . C17 . C23 . 118.2(2) yes C18 . C17 . C23 . 122.1(2) yes C17 . C18 . C19 . 122.7(2) yes C17 . C18 . C20 . 117.7(2) yes C19 . C18 . C20 . 119.6(2) yes C18 . C19 . H191 . 112.2 no C18 . C19 . H193 . 109.7 no H191 . C19 . H193 . 106.6 no C18 . C19 . H192 . 110.2 no H191 . C19 . H192 . 109.4 no H193 . C19 . H192 . 108.5 no C18 . C20 . C21 . 122.0(3) yes C18 . C20 . H201 . 119.1 no C21 . C20 . H201 . 118.8 no C20 . C21 . C22 . 118.7(2) yes C20 . C21 . C25 . 121.2(3) yes C22 . C21 . C25 . 120.2(2) yes C21 . C22 . C23 . 121.3(2) yes C21 . C22 . H221 . 119.5 no C23 . C22 . H221 . 119.2 no C17 . C23 . C22 . 118.2(2) yes C17 . C23 . C24 . 121.8(2) yes C22 . C23 . C24 . 119.9(2) yes C23 . C24 . H242 . 111.2 no C23 . C24 . H241 . 108.7 no H242 . C24 . H241 . 109.1 no C23 . C24 . H243 . 109.9 no H242 . C24 . H243 . 109.2 no H241 . C24 . H243 . 108.8 no C21 . C25 . H252 . 109.6 no C21 . C25 . H251 . 109.4 no H252 . C25 . H251 . 110.1 no C21 . C25 . H253 . 109.0 no H252 . C25 . H253 . 109.9 no H251 . C25 . H253 . 108.9 no _iucr_refine_instruction_details_constraints ; # # Punched on 25/03/13 at 13:32:43 # #LIST 12 BLOCK SCALE X'S, U'S CONT H ( 1,X'S,U[ISO]) H(2,X'S,U[ISO]) H (5,X'S,U[ISO]) REM RIDE AL ( 1,X'S) H ( 1,X'S) H ( 2,X'S) H ( 5,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 63,X'S) H ( 62,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 122,X'S) H ( 121,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 24,X'S) H ( 242,X'S) H ( 241,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 252,X'S) H ( 251,X'S) H ( 253,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/03/13 at 13:32:43 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 931225' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment '2b.cif' data_009jart12 #TrackingRef '2b.cif' _audit_creation_date 13-03-25 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '009jart12 At 15:25 on 27/10' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 10.65680(10) _cell_length_b 19.2990(2) _cell_length_c 16.7649(2) _cell_angle_alpha 90 _cell_angle_beta 105.3598(5) _cell_angle_gamma 90 _cell_volume 3324.81(6) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C42 H55.50 Al1.50 N3 # Dc = 1.28 Fooo = 1152.00 Mu = 1.11 M = 642.90 # Found Formula = C35 H51 Al1 N2 # Dc = 1.05 FOOO = 1152.00 Mu = 0.85 M = 526.78 _chemical_formula_sum 'C35 H51 Al1 N2' _chemical_formula_moiety 'C35 H51 Al1 N2' _chemical_compound_source . _chemical_formula_weight 526.78 _cell_measurement_reflns_used 7697 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.210 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_max 0.450 _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.085 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.98 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 73798 _reflns_number_total 7562 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections without Friedels Law is 13798 # Number of reflections with Friedels Law is 7562 # Theoretical number of reflections is about 7626 _diffrn_reflns_theta_min 5.154 _diffrn_reflns_theta_max 27.485 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.485 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.50 _oxford_diffrn_Wilson_scale 4.15 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.28 _refine_diff_density_max 0.36 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 7561 _refine_ls_number_restraints 256 _refine_ls_number_parameters 418 _oxford_refine_ls_R_factor_ref 0.0611 _refine_ls_wR_factor_ref 0.1109 _refine_ls_goodness_of_fit_ref 0.9276 _refine_ls_shift/su_max 0.0044486 _refine_ls_shift/su_mean 0.0003953 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7562 _refine_ls_R_factor_all 0.0612 _refine_ls_wR_factor_all 0.1110 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6121 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_gt 0.1010 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 20.3 29.7 14.6 3.74 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C2 C 0.41659(11) 0.24472(6) 0.46948(7) 0.0220 1.0000 Uani . . . . . . C4 C 0.40559(13) 0.13462(6) 0.53488(7) 0.0240 1.0000 Uani . . . . . . C5 C 0.28952(13) 0.12169(7) 0.55661(8) 0.0268 1.0000 Uani . . . . . . C6 C 0.29845(15) 0.08402(8) 0.62900(9) 0.0337 1.0000 Uani . . . . . . C7 C 0.41631(16) 0.05903(8) 0.67598(9) 0.0384 1.0000 Uani . . . . . . C8 C 0.52864(15) 0.06999(8) 0.65113(9) 0.0346 1.0000 Uani . . . . . . C9 C 0.52590(13) 0.10819(7) 0.58007(8) 0.0271 1.0000 Uani . . . . . . C10 C 0.65065(13) 0.12010(7) 0.55404(9) 0.0307 1.0000 Uani . . . . . . C11 C 0.70458(16) 0.05119(9) 0.53191(11) 0.0436 1.0000 Uani . . . . . . C12 C 0.75295(15) 0.15857(9) 0.62052(11) 0.0437 1.0000 Uani . . . . . . C13 C 0.15875(13) 0.14811(8) 0.50517(9) 0.0326 1.0000 Uani . . . . . . C14 C 0.11651(18) 0.21295(9) 0.54305(13) 0.0513 1.0000 Uani . . . . . . C15 C 0.05307(16) 0.09281(10) 0.49280(13) 0.0496 1.0000 Uani . . . . . . C16 C 0.38992(14) 0.13560(7) 0.38539(8) 0.0284 1.0000 Uani . . . . . . C17 C 0.44641(15) 0.17664(7) 0.32617(8) 0.0316 1.0000 Uani . . . . . . C18 C 0.38804(15) 0.24846(7) 0.31782(8) 0.0317 1.0000 Uani . . . . . . C20 C 0.42344(12) 0.35550(6) 0.40191(7) 0.0233 1.0000 Uani . . . . . . C21 C 0.54683(13) 0.38521(7) 0.41163(8) 0.0257 1.0000 Uani . . . . . . C22 C 0.55305(15) 0.45740(7) 0.40707(8) 0.0317 1.0000 Uani . . . . . . C23 C 0.44173(16) 0.49771(7) 0.39223(9) 0.0347 1.0000 Uani . . . . . . C24 C 0.32156(15) 0.46699(7) 0.38297(9) 0.0335 1.0000 Uani . . . . . . C25 C 0.30957(13) 0.39525(7) 0.38816(8) 0.0279 1.0000 Uani . . . . . . C26 C 0.17650(14) 0.36291(8) 0.37911(10) 0.0363 1.0000 Uani . . . . . . C27 C 0.09936(17) 0.40075(12) 0.43082(12) 0.0533 1.0000 Uani . . . . . . C28 C 0.09847(16) 0.35985(10) 0.28850(11) 0.0452 1.0000 Uani . . . . . . C29 C 0.67001(13) 0.34222(8) 0.42556(9) 0.0332 1.0000 Uani . . . . . . C30 C 0.71388(17) 0.33658(11) 0.34577(11) 0.0473 1.0000 Uani . . . . . . C31 C 0.78095(15) 0.37082(11) 0.49560(10) 0.0468 1.0000 Uani . . . . . . C40 C 0.8070(8) 0.3698(5) 0.7818(6) 0.0931 0.3784 Uani D . . 1 1 . C41 C 0.9288(8) 0.3862(4) 0.7562(7) 0.0749 0.3784 Uani D . . 1 1 . C42 C 0.9787(8) 0.3397(4) 0.7096(6) 0.0816 0.3784 Uani D . . 1 1 . C43 C 1.0858(8) 0.3569(5) 0.6823(6) 0.0775 0.3784 Uani D . . 1 1 . C44 C 1.1430(10) 0.4200(5) 0.6989(8) 0.0742 0.3784 Uani D . . 1 1 . C45 C 1.0936(13) 0.4665(5) 0.7443(11) 0.0762 0.3784 Uani D . . 1 1 . C46 C 0.9913(12) 0.4490(5) 0.7757(9) 0.0705 0.3784 Uani D . . 1 1 . C50 C 0.8474(5) 0.3441(2) 0.7726(3) 0.0676 0.6216 Uani D . . 1 2 . C51 C 0.9597(4) 0.37596(17) 0.7471(4) 0.0460 0.6216 Uani D . . 1 2 . C52 C 1.0292(3) 0.33801(16) 0.7021(3) 0.0437 0.6216 Uani D . . 1 2 . C53 C 1.1312(4) 0.3681(2) 0.6779(3) 0.0475 0.6216 Uani D . . 1 2 . C54 C 1.1660(5) 0.4360(2) 0.6971(4) 0.0459 0.6216 Uani D . . 1 2 . C55 C 1.0997(6) 0.4734(2) 0.7425(5) 0.0441 0.6216 Uani D . . 1 2 . C56 C 0.9958(6) 0.4447(2) 0.7661(5) 0.0433 0.6216 Uani D . . 1 2 . Al1 Al 0.45587(4) 0.29611(2) 0.58392(2) 0.0285 1.0000 Uani . . . . . . N3 N 0.40139(10) 0.17572(5) 0.46230(6) 0.0231 1.0000 Uani . . . . . . N19 N 0.41155(10) 0.28066(5) 0.40047(6) 0.0236 1.0000 Uani . . . . . . H61 H 0.2201 0.0750 0.6453 0.0399 1.0000 Uiso R . . . . . H71 H 0.4190 0.0341 0.7254 0.0466 1.0000 Uiso R . . . . . H81 H 0.6115 0.0514 0.6843 0.0426 1.0000 Uiso R . . . . . H101 H 0.6285 0.1492 0.5048 0.0367 1.0000 Uiso R . . . . . H112 H 0.7799 0.0604 0.5100 0.0645 1.0000 Uiso R . . . . . H111 H 0.7306 0.0217 0.5820 0.0647 1.0000 Uiso R . . . . . H113 H 0.6381 0.0270 0.4895 0.0641 1.0000 Uiso R . . . . . H121 H 0.8300 0.1663 0.6008 0.0646 1.0000 Uiso R . . . . . H123 H 0.7786 0.1311 0.6715 0.0652 1.0000 Uiso R . . . . . H122 H 0.7198 0.2025 0.6329 0.0645 1.0000 Uiso R . . . . . H131 H 0.1690 0.1604 0.4497 0.0385 1.0000 Uiso R . . . . . H142 H 0.0322 0.2284 0.5083 0.0759 1.0000 Uiso R . . . . . H141 H 0.1070 0.2010 0.5982 0.0759 1.0000 Uiso R . . . . . H143 H 0.1822 0.2501 0.5466 0.0761 1.0000 Uiso R . . . . . H151 H -0.0279 0.1097 0.4555 0.0724 1.0000 Uiso R . . . . . H153 H 0.0367 0.0820 0.5465 0.0731 1.0000 Uiso R . . . . . H152 H 0.0806 0.0506 0.4705 0.0738 1.0000 Uiso R . . . . . H161 H 0.4376 0.0922 0.4005 0.0342 1.0000 Uiso R . . . . . H162 H 0.2976 0.1248 0.3597 0.0343 1.0000 Uiso R . . . . . H171 H 0.5419 0.1788 0.3479 0.0379 1.0000 Uiso R . . . . . H172 H 0.4242 0.1543 0.2718 0.0381 1.0000 Uiso R . . . . . H181 H 0.4263 0.2780 0.2850 0.0388 1.0000 Uiso R . . . . . H182 H 0.2926 0.2450 0.2931 0.0386 1.0000 Uiso R . . . . . H221 H 0.6356 0.4794 0.4151 0.0378 1.0000 Uiso R . . . . . H231 H 0.4469 0.5474 0.3890 0.0420 1.0000 Uiso R . . . . . H241 H 0.2440 0.4950 0.3737 0.0407 1.0000 Uiso R . . . . . H261 H 0.1916 0.3152 0.4001 0.0431 1.0000 Uiso R . . . . . H271 H 0.0195 0.3751 0.4290 0.0792 1.0000 Uiso R . . . . . H272 H 0.1507 0.4041 0.4881 0.0783 1.0000 Uiso R . . . . . H273 H 0.0761 0.4476 0.4093 0.0786 1.0000 Uiso R . . . . . H281 H 0.0141 0.3383 0.2842 0.0685 1.0000 Uiso R . . . . . H282 H 0.0828 0.4072 0.2657 0.0667 1.0000 Uiso R . . . . . H283 H 0.1453 0.3343 0.2552 0.0674 1.0000 Uiso R . . . . . H291 H 0.6499 0.2952 0.4404 0.0398 1.0000 Uiso R . . . . . H301 H 0.7908 0.3064 0.3545 0.0697 1.0000 Uiso R . . . . . H302 H 0.7375 0.3836 0.3300 0.0699 1.0000 Uiso R . . . . . H303 H 0.6445 0.3173 0.3008 0.0700 1.0000 Uiso R . . . . . H311 H 0.8534 0.3384 0.5057 0.0687 1.0000 Uiso R . . . . . H312 H 0.8102 0.4160 0.4795 0.0691 1.0000 Uiso R . . . . . H313 H 0.7520 0.3765 0.5459 0.0688 1.0000 Uiso R . . . . . H401 H 0.7788 0.4106 0.8061 0.1397 0.3784 Uiso R . . 1 1 . H402 H 0.8254 0.3330 0.8226 0.1398 0.3784 Uiso R . . 1 1 . H403 H 0.7386 0.3561 0.7342 0.1399 0.3784 Uiso R . . 1 1 . H421 H 0.9396 0.2963 0.6971 0.0982 0.3784 Uiso R . . 1 1 . H431 H 1.1194 0.3249 0.6522 0.0934 0.3784 Uiso R . . 1 1 . H441 H 1.2159 0.4318 0.6805 0.0902 0.3784 Uiso R . . 1 1 . H451 H 1.1299 0.5109 0.7542 0.0922 0.3784 Uiso R . . 1 1 . H461 H 0.9633 0.4795 0.8110 0.0852 0.3784 Uiso R . . 1 1 . H501 H 0.8154 0.3753 0.8096 0.1025 0.6216 Uiso R . . 1 2 . H502 H 0.8777 0.3032 0.8025 0.1023 0.6216 Uiso R . . 1 2 . H503 H 0.7778 0.3308 0.7258 0.1023 0.6216 Uiso R . . 1 2 . H521 H 1.0064 0.2920 0.6877 0.0523 0.6216 Uiso R . . 1 2 . H531 H 1.1783 0.3415 0.6482 0.0575 0.6216 Uiso R . . 1 2 . H541 H 1.2347 0.4560 0.6800 0.0551 0.6216 Uiso R . . 1 2 . H551 H 1.1250 0.5196 0.7576 0.0534 0.6216 Uiso R . . 1 2 . H561 H 0.9485 0.4713 0.7948 0.0527 0.6216 Uiso R . . 1 2 . H1 H 0.4429(18) 0.2437(10) 0.6516(11) 0.054(5) 1.0000 Uiso . . . . . . H2 H 0.5949(18) 0.3228(10) 0.5964(11) 0.051(5) 1.0000 Uiso . . . . . . H3 H 0.3548(19) 0.3529(10) 0.5748(12) 0.054(5) 1.0000 Uiso . . . . . . 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 C2 0.0229(6) 0.0226(6) 0.0218(5) -0.0005(4) 0.0085(4) -0.0017(4) C4 0.0312(6) 0.0209(6) 0.0211(6) -0.0015(4) 0.0091(5) -0.0038(5) C5 0.0316(7) 0.0235(6) 0.0274(6) -0.0032(5) 0.0114(5) -0.0026(5) C6 0.0406(8) 0.0346(7) 0.0304(7) -0.0001(6) 0.0174(6) -0.0078(6) C7 0.0511(9) 0.0398(8) 0.0251(7) 0.0072(6) 0.0114(6) -0.0065(7) C8 0.0388(8) 0.0358(7) 0.0262(6) 0.0051(5) 0.0033(6) -0.0028(6) C9 0.0302(6) 0.0257(6) 0.0247(6) -0.0011(5) 0.0060(5) -0.0041(5) C10 0.0275(6) 0.0307(7) 0.0336(7) 0.0016(5) 0.0074(5) -0.0024(5) C11 0.0385(8) 0.0421(9) 0.0534(10) -0.0073(7) 0.0178(7) -0.0012(7) C12 0.0319(8) 0.0433(9) 0.0531(10) -0.0093(7) 0.0065(7) -0.0070(6) C13 0.0289(7) 0.0346(7) 0.0374(7) 0.0009(6) 0.0142(6) -0.0001(6) C14 0.0448(9) 0.0372(9) 0.0748(13) -0.0052(8) 0.0208(9) 0.0058(7) C15 0.0329(8) 0.0444(9) 0.0687(12) -0.0037(8) 0.0087(8) -0.0044(7) C16 0.0412(7) 0.0225(6) 0.0228(6) -0.0047(5) 0.0105(5) -0.0031(5) C17 0.0440(8) 0.0291(7) 0.0244(6) -0.0040(5) 0.0141(6) -0.0002(6) C18 0.0487(8) 0.0276(6) 0.0197(6) -0.0017(5) 0.0107(6) -0.0026(6) C20 0.0290(6) 0.0223(6) 0.0202(5) 0.0009(4) 0.0094(5) -0.0013(5) C21 0.0295(6) 0.0284(6) 0.0200(5) 0.0012(5) 0.0080(5) -0.0028(5) C22 0.0392(7) 0.0306(7) 0.0256(6) -0.0008(5) 0.0088(5) -0.0113(6) C23 0.0544(9) 0.0229(6) 0.0279(7) -0.0009(5) 0.0129(6) -0.0031(6) C24 0.0433(8) 0.0280(7) 0.0310(7) 0.0017(5) 0.0127(6) 0.0077(6) C25 0.0305(7) 0.0295(7) 0.0254(6) 0.0016(5) 0.0102(5) 0.0017(5) C26 0.0273(7) 0.0399(8) 0.0432(8) 0.0076(6) 0.0121(6) 0.0027(6) C27 0.0357(8) 0.0767(13) 0.0531(10) 0.0059(9) 0.0217(8) 0.0095(9) C28 0.0344(8) 0.0479(9) 0.0494(9) 0.0000(7) 0.0040(7) 0.0012(7) C29 0.0270(6) 0.0379(7) 0.0364(7) 0.0036(6) 0.0115(6) -0.0006(6) C30 0.0395(8) 0.0639(11) 0.0421(9) -0.0064(8) 0.0173(7) 0.0051(8) C31 0.0291(7) 0.0704(12) 0.0404(8) 0.0004(8) 0.0082(6) -0.0013(7) C40 0.102(6) 0.077(5) 0.077(5) 0.013(4) -0.018(4) -0.017(4) C41 0.091(5) 0.061(3) 0.050(4) 0.004(3) -0.021(3) 0.004(3) C42 0.096(5) 0.062(4) 0.065(4) -0.012(3) -0.015(4) -0.003(4) C43 0.094(6) 0.062(4) 0.062(4) -0.017(4) -0.006(4) 0.009(4) C44 0.086(5) 0.067(5) 0.054(4) 0.001(4) -0.010(4) 0.016(4) C45 0.090(6) 0.062(5) 0.062(5) 0.000(4) -0.007(4) 0.018(4) C46 0.089(6) 0.054(4) 0.053(5) -0.005(3) -0.009(4) 0.011(4) C50 0.063(2) 0.072(3) 0.067(2) 0.000(2) 0.0153(19) -0.019(2) C51 0.0528(19) 0.0445(18) 0.0366(16) 0.0015(14) 0.0046(14) -0.0078(15) C52 0.054(2) 0.0335(15) 0.0388(15) -0.0029(12) 0.0044(17) -0.0046(14) C53 0.053(2) 0.049(2) 0.0385(15) -0.0016(14) 0.0084(16) 0.0019(16) C54 0.0442(17) 0.048(2) 0.0431(18) 0.0114(17) 0.0074(14) 0.0005(15) C55 0.043(2) 0.0310(16) 0.053(2) 0.0030(16) 0.0026(17) 0.0006(15) C56 0.0453(19) 0.038(2) 0.046(2) -0.0041(16) 0.0104(17) 0.0031(16) Al1 0.0405(2) 0.02500(19) 0.02207(18) -0.00341(15) 0.01170(16) -0.00449(16) N3 0.0302(5) 0.0205(5) 0.0199(5) -0.0012(4) 0.0088(4) -0.0025(4) N19 0.0299(5) 0.0216(5) 0.0205(5) -0.0007(4) 0.0088(4) -0.0007(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5836(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C2 . Al1 . 2.1012(12) yes C2 . N3 . 1.3429(16) yes C2 . N19 . 1.3378(15) yes C4 . C5 . 1.4013(18) yes C4 . C9 . 1.4011(18) yes C4 . N3 . 1.4433(15) yes C5 . C6 . 1.3960(18) yes C5 . C13 . 1.5197(19) yes C6 . C7 . 1.381(2) yes C6 . H61 . 0.961 no C7 . C8 . 1.384(2) yes C7 . H71 . 0.951 no C8 . C9 . 1.3948(18) yes C8 . H81 . 0.978 no C9 . C10 . 1.5225(18) yes C10 . C11 . 1.533(2) yes C10 . C12 . 1.529(2) yes C10 . H101 . 0.974 no C11 . H112 . 0.983 no C11 . H111 . 0.990 no C11 . H113 . 0.979 no C12 . H121 . 0.975 no C12 . H123 . 0.981 no C12 . H122 . 0.962 no C13 . C14 . 1.524(2) yes C13 . C15 . 1.525(2) yes C13 . H131 . 0.993 no C14 . H142 . 0.979 no C14 . H141 . 0.984 no C14 . H143 . 0.992 no C15 . H151 . 0.977 no C15 . H153 . 0.983 no C15 . H152 . 0.974 no C16 . C17 . 1.5139(18) yes C16 . N3 . 1.4811(15) yes C16 . H161 . 0.977 no C16 . H162 . 0.987 no C17 . C18 . 1.511(2) yes C17 . H171 . 0.987 no C17 . H172 . 0.979 no C18 . N19 . 1.4782(15) yes C18 . H181 . 0.955 no C18 . H182 . 0.993 no C20 . C21 . 1.4040(18) yes C20 . C25 . 1.4021(18) yes C20 . N19 . 1.4496(16) yes C21 . C22 . 1.3978(19) yes C21 . C29 . 1.5178(19) yes C22 . C23 . 1.385(2) yes C22 . H221 . 0.954 no C23 . C24 . 1.382(2) yes C23 . H231 . 0.964 no C24 . C25 . 1.3952(19) yes C24 . H241 . 0.966 no C25 . C26 . 1.5197(19) yes C26 . C27 . 1.529(2) yes C26 . C28 . 1.528(2) yes C26 . H261 . 0.983 no C27 . H271 . 0.978 no C27 . H272 . 0.973 no C27 . H273 . 0.981 no C28 . H281 . 0.976 no C28 . H282 . 0.987 no C28 . H283 . 0.975 no C29 . C30 . 1.533(2) yes C29 . C31 . 1.532(2) yes C29 . H291 . 0.981 no C30 . H301 . 0.984 no C30 . H302 . 0.996 no C30 . H303 . 0.979 no C31 . H311 . 0.973 no C31 . H312 . 0.988 no C31 . H313 . 0.978 no C40 . C41 . 1.505(6) yes C40 . H401 . 0.969 no C40 . H402 . 0.969 no C40 . H403 . 0.965 no C41 . C42 . 1.385(5) yes C41 . C46 . 1.380(5) yes C42 . C43 . 1.377(5) yes C42 . H421 . 0.935 no C43 . C44 . 1.358(5) yes C43 . H431 . 0.928 no C44 . C45 . 1.368(5) yes C44 . H441 . 0.937 no C45 . C46 . 1.373(5) yes C45 . H451 . 0.938 no C46 . H461 . 0.938 no C50 . C51 . 1.505(4) yes C50 . H501 . 0.988 no C50 . H502 . 0.946 no C50 . H503 . 0.960 no C51 . C52 . 1.395(3) yes C51 . C56 . 1.394(3) yes C52 . C53 . 1.385(3) yes C52 . H521 . 0.935 no C53 . C54 . 1.376(3) yes C53 . H531 . 0.946 no C54 . C55 . 1.373(3) yes C54 . H541 . 0.938 no C55 . C56 . 1.387(3) yes C55 . H551 . 0.946 no C56 . H561 . 0.937 no Al1 . H1 . 1.554(19) no Al1 . H2 . 1.530(19) no Al1 . H3 . 1.52(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Al1 . C2 . N3 . 122.68(9) yes Al1 . C2 . N19 . 119.84(9) yes N3 . C2 . N19 . 117.42(11) yes C5 . C4 . C9 . 122.61(12) yes C5 . C4 . N3 . 118.99(11) yes C9 . C4 . N3 . 118.39(11) yes C4 . C5 . C6 . 117.20(12) yes C4 . C5 . C13 . 122.18(12) yes C6 . C5 . C13 . 120.61(12) yes C5 . C6 . C7 . 121.34(13) yes C5 . C6 . H61 . 118.5 no C7 . C6 . H61 . 120.1 no C6 . C7 . C8 . 120.23(13) yes C6 . C7 . H71 . 119.1 no C8 . C7 . H71 . 120.7 no C7 . C8 . C9 . 120.92(14) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 119.4 no C4 . C9 . C8 . 117.60(12) yes C4 . C9 . C10 . 122.25(11) yes C8 . C9 . C10 . 120.15(12) yes C9 . C10 . C11 . 110.51(12) yes C9 . C10 . C12 . 111.87(12) yes C11 . C10 . C12 . 110.92(13) yes C9 . C10 . H101 . 107.2 no C11 . C10 . H101 . 108.4 no C12 . C10 . H101 . 107.7 no C10 . C11 . H112 . 109.2 no C10 . C11 . H111 . 109.4 no H112 . C11 . H111 . 110.3 no C10 . C11 . H113 . 110.1 no H112 . C11 . H113 . 108.6 no H111 . C11 . H113 . 109.2 no C10 . C12 . H121 . 109.2 no C10 . C12 . H123 . 110.7 no H121 . C12 . H123 . 108.3 no C10 . C12 . H122 . 110.7 no H121 . C12 . H122 . 109.2 no H123 . C12 . H122 . 108.7 no C5 . C13 . C14 . 111.51(13) yes C5 . C13 . C15 . 112.05(13) yes C14 . C13 . C15 . 110.00(13) yes C5 . C13 . H131 . 107.4 no C14 . C13 . H131 . 108.2 no C15 . C13 . H131 . 107.4 no C13 . C14 . H142 . 109.2 no C13 . C14 . H141 . 108.3 no H142 . C14 . H141 . 108.9 no C13 . C14 . H143 . 109.7 no H142 . C14 . H143 . 109.7 no H141 . C14 . H143 . 111.0 no C13 . C15 . H151 . 110.4 no C13 . C15 . H153 . 109.2 no H151 . C15 . H153 . 108.4 no C13 . C15 . H152 . 110.5 no H151 . C15 . H152 . 109.8 no H153 . C15 . H152 . 108.6 no C17 . C16 . N3 . 110.00(10) yes C17 . C16 . H161 . 110.4 no N3 . C16 . H161 . 107.8 no C17 . C16 . H162 . 110.4 no N3 . C16 . H162 . 109.5 no H161 . C16 . H162 . 108.8 no C16 . C17 . C18 . 108.38(11) yes C16 . C17 . H171 . 109.3 no C18 . C17 . H171 . 110.8 no C16 . C17 . H172 . 109.9 no C18 . C17 . H172 . 109.0 no H171 . C17 . H172 . 109.5 no C17 . C18 . N19 . 109.60(11) yes C17 . C18 . H181 . 111.9 no N19 . C18 . H181 . 107.2 no C17 . C18 . H182 . 109.2 no N19 . C18 . H182 . 108.6 no H181 . C18 . H182 . 110.2 no C21 . C20 . C25 . 122.61(12) yes C21 . C20 . N19 . 118.94(11) yes C25 . C20 . N19 . 118.32(11) yes C20 . C21 . C22 . 117.21(12) yes C20 . C21 . C29 . 122.68(12) yes C22 . C21 . C29 . 120.11(12) yes C21 . C22 . C23 . 121.26(13) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 119.3 no C22 . C23 . C24 . 120.22(13) yes C22 . C23 . H231 . 120.7 no C24 . C23 . H231 . 119.1 no C23 . C24 . C25 . 121.08(13) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 118.5 no C20 . C25 . C24 . 117.62(12) yes C20 . C25 . C26 . 122.40(12) yes C24 . C25 . C26 . 119.99(13) yes C25 . C26 . C27 . 112.01(14) yes C25 . C26 . C28 . 111.28(12) yes C27 . C26 . C28 . 110.46(13) yes C25 . C26 . H261 . 106.8 no C27 . C26 . H261 . 107.8 no C28 . C26 . H261 . 108.3 no C26 . C27 . H271 . 109.5 no C26 . C27 . H272 . 110.2 no H271 . C27 . H272 . 108.7 no C26 . C27 . H273 . 110.6 no H271 . C27 . H273 . 108.8 no H272 . C27 . H273 . 108.9 no C26 . C28 . H281 . 109.8 no C26 . C28 . H282 . 109.9 no H281 . C28 . H282 . 108.0 no C26 . C28 . H283 . 111.2 no H281 . C28 . H283 . 110.1 no H282 . C28 . H283 . 107.8 no C21 . C29 . C30 . 110.84(12) yes C21 . C29 . C31 . 112.43(13) yes C30 . C29 . C31 . 110.03(12) yes C21 . C29 . H291 . 107.9 no C30 . C29 . H291 . 107.1 no C31 . C29 . H291 . 108.4 no C29 . C30 . H301 . 110.2 no C29 . C30 . H302 . 108.9 no H301 . C30 . H302 . 108.7 no C29 . C30 . H303 . 110.9 no H301 . C30 . H303 . 108.5 no H302 . C30 . H303 . 109.5 no C29 . C31 . H311 . 108.5 no C29 . C31 . H312 . 110.1 no H311 . C31 . H312 . 108.7 no C29 . C31 . H313 . 110.2 no H311 . C31 . H313 . 109.8 no H312 . C31 . H313 . 109.4 no C41 . C40 . H401 . 109.6 no C41 . C40 . H402 . 109.0 no H401 . C40 . H402 . 109.1 no C41 . C40 . H403 . 109.9 no H401 . C40 . H403 . 108.7 no H402 . C40 . H403 . 110.5 no C40 . C41 . C42 . 120.98(6) yes C40 . C41 . C46 . 120.99(6) yes C42 . C41 . C46 . 117.98(6) yes C41 . C42 . C43 . 120.52(7) yes C41 . C42 . H421 . 119.4 no C43 . C42 . H421 . 120.0 no C42 . C43 . C44 . 120.93(7) yes C42 . C43 . H431 . 119.6 no C44 . C43 . H431 . 119.4 no C43 . C44 . C45 . 118.94(7) yes C43 . C44 . H441 . 121.1 no C45 . C44 . H441 . 120.0 no C44 . C45 . C46 . 120.92(7) yes C44 . C45 . H451 . 119.8 no C46 . C45 . H451 . 119.3 no C41 . C46 . C45 . 120.50(7) yes C41 . C46 . H461 . 119.2 no C45 . C46 . H461 . 120.3 no C51 . C50 . H501 . 111.2 no C51 . C50 . H502 . 107.8 no H501 . C50 . H502 . 107.6 no C51 . C50 . H503 . 112.2 no H501 . C50 . H503 . 110.8 no H502 . C50 . H503 . 106.9 no C50 . C51 . C52 . 120.98(6) yes C50 . C51 . C56 . 120.99(6) yes C52 . C51 . C56 . 118.02(5) yes C51 . C52 . C53 . 120.54(6) yes C51 . C52 . H521 . 120.0 no C53 . C52 . H521 . 119.5 no C52 . C53 . C54 . 120.96(6) yes C52 . C53 . H531 . 119.7 no C54 . C53 . H531 . 119.3 no C53 . C54 . C55 . 118.97(6) yes C53 . C54 . H541 . 120.4 no C55 . C54 . H541 . 120.6 no C54 . C55 . C56 . 120.93(6) yes C54 . C55 . H551 . 119.6 no C56 . C55 . H551 . 119.5 no C51 . C56 . C55 . 120.53(6) yes C51 . C56 . H561 . 119.1 no C55 . C56 . H561 . 120.4 no C2 . Al1 . H1 . 108.9(7) no C2 . Al1 . H2 . 103.6(7) no H1 . Al1 . H2 . 113.0(10) no C2 . Al1 . H3 . 106.5(7) no H1 . Al1 . H3 . 110.3(10) no H2 . Al1 . H3 . 114.0(10) no C16 . N3 . C4 . 115.07(10) yes C16 . N3 . C2 . 125.20(10) yes C4 . N3 . C2 . 119.56(10) yes C18 . N19 . C20 . 115.27(10) yes C18 . N19 . C2 . 123.42(10) yes C20 . N19 . C2 . 121.26(10) yes _iucr_refine_instruction_details_constraints ; # # Punched on 25/03/13 at 13:40:19 # #LIST 12 BLOCK SCALE X'S, U'S CONT H (1,X'S,U[ISO]) H(2,X'S,U[ISO]) H(3,X'S,U[ISO]) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 111,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 123,X'S) H ( 122,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 142,X'S) H ( 141,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 153,X'S) H ( 152,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) H ( 273,X'S) RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) H ( 283,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) H ( 313,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 402,X'S) H ( 403,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) H ( 503,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) REM RIDE AL ( 1,X'S) H ( 1,X'S) H ( 2,X'S) H ( 3,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/03/13 at 13:40:19 # #LIST 16 SAME C(40) C(41) C(42) C(43) C(44) C(45) C(46) C(41) AND CONT C(40) C(41) C(46) C(45) C(44) C(43) C(42) C(41) AND CONT C(50) C(51) C(52) C(53) C(54) C(55) C(56) C(51) AND CONT C(50) C(51) C(56) C(55) C(54) C(53) C(52) C(51) SIMU 0.01 C(40) C(41) C(42) C(43) C(44) C(45) C(46) C(41) AND CONT C(40) C(41) C(46) C(45) C(44) C(43) C(42) C(41) AND CONT C(50) C(51) C(52) C(53) C(54) C(55) C(56) C(51) AND CONT C(50) C(51) C(56) C(55) C(54) C(53) C(52) C(51) DELU 0.01 C(40) C(41) C(42) C(43) C(44) C(45) C(46) C(41) AND CONT C(40) C(41) C(46) C(45) C(44) C(43) C(42) C(41) AND CONT C(50) C(51) C(52) C(53) C(54) C(55) C(56) C(51) AND CONT C(50) C(51) C(56) C(55) C(54) C(53) C(52) C(51) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 931226' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment '3a.cif' data_1 #TrackingRef '3a.cif' _audit_creation_date 13-03-25 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '005rtrt12 At 23: 7 on 28/ 8' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.80680(10) _cell_length_b 17.0565(2) _cell_length_c 18.6455(2) _cell_angle_alpha 75.1194(4) _cell_angle_beta 88.9465(4) _cell_angle_gamma 85.7380(4) _cell_volume 3005.89(6) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C50 H60 Al2 F0.50 Mo2 N4 O8 # Dc = 1.22 Fooo = 1252.00 Mu = 4.95 M = 1100.39 # Found Formula = C58 H67 Al2 F1 Mo2 N4 O8 # Dc = 1.34 FOOO = 1252.00 Mu = 5.03 M = 1213.03 _chemical_formula_sum 'C58 H67 Al2 F1 Mo2 N4 O8' _chemical_formula_moiety 'C58 H67 Al2 F1 Mo2 N4 O8' _chemical_compound_source . _chemical_formula_weight 1213.03 _cell_measurement_reflns_used 12963 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.130 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_max 0.240 _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.503 # Sheldrick geometric approximatio 0.93 0.94 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.94 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 100852 _reflns_number_total 13693 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections without Friedels Law is 24053 # Number of reflections with Friedels Law is 13693 # Theoretical number of reflections is about 13794 _diffrn_reflns_theta_min 5.122 _diffrn_reflns_theta_max 27.488 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.938 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -21 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.38 _oxford_diffrn_Wilson_scale 13.96 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.88 _refine_diff_density_max 1.08 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 13693 _refine_ls_number_restraints 256 _refine_ls_number_parameters 763 _oxford_refine_ls_R_factor_ref 0.0592 _refine_ls_wR_factor_ref 0.1098 _refine_ls_goodness_of_fit_ref 0.9335 _refine_ls_shift/su_max 0.0094287 _refine_ls_shift/su_mean 0.0003675 # The values computed with all filters except I/sigma _oxford_reflns_number_all 13693 _refine_ls_R_factor_all 0.0592 _refine_ls_wR_factor_all 0.1098 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10735 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_gt 0.0917 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 16.0 23.0 11.0 2.84 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mo1 Mo 0.46820(3) 0.711805(16) 0.251878(13) 0.0270 1.0000 Uani . . . . . . Al2 Al 0.67823(9) 0.74614(5) 0.32026(5) 0.0268 1.0000 Uani . . . . . . C3 C 0.7159(3) 0.69518(17) 0.43063(15) 0.0245 1.0000 Uani . . . . . . N4 N 0.7892(2) 0.62411(14) 0.45317(13) 0.0248 1.0000 Uani . . . . . . C5 C 0.8155(3) 0.58262(18) 0.53202(15) 0.0283 1.0000 Uani . . . . . . C6 C 0.7021(4) 0.6084(2) 0.57936(17) 0.0353 1.0000 Uani . . . . . . C7 C 0.6837(3) 0.7005(2) 0.56143(16) 0.0339 1.0000 Uani . . . . . . N8 N 0.6649(2) 0.73317(14) 0.48047(13) 0.0251 1.0000 Uani . . . . . . C9 C 0.5942(3) 0.81322(17) 0.45598(15) 0.0265 1.0000 Uani . . . . . . C10 C 0.4509(3) 0.81991(19) 0.45686(16) 0.0303 1.0000 Uani . . . . . . C11 C 0.3851(3) 0.8977(2) 0.43618(17) 0.0338 1.0000 Uani . . . . . . C12 C 0.4565(4) 0.9671(2) 0.41524(17) 0.0350 1.0000 Uani . . . . . . C13 C 0.3819(4) 1.0506(2) 0.3934(2) 0.0458 1.0000 Uani . . . . . . C14 C 0.5985(4) 0.9581(2) 0.41555(18) 0.0354 1.0000 Uani . . . . . . C15 C 0.6704(3) 0.88185(19) 0.43631(17) 0.0314 1.0000 Uani . . . . . . C16 C 0.8243(3) 0.8757(2) 0.4389(2) 0.0406 1.0000 Uani . . . . . . C17 C 0.3695(3) 0.7461(2) 0.4786(2) 0.0388 1.0000 Uani . . . . . . C18 C 0.8612(3) 0.58931(17) 0.39918(15) 0.0249 1.0000 Uani . . . . . . C19 C 0.9795(3) 0.62417(18) 0.36590(16) 0.0275 1.0000 Uani . . . . . . C20 C 1.0473(3) 0.58951(19) 0.31340(16) 0.0294 1.0000 Uani . . . . . . C21 C 1.0025(3) 0.5216(2) 0.29543(17) 0.0312 1.0000 Uani . . . . . . C22 C 0.8865(3) 0.48770(18) 0.33061(17) 0.0305 1.0000 Uani . . . . . . C23 C 0.8138(3) 0.52037(17) 0.38229(16) 0.0270 1.0000 Uani . . . . . . C24 C 0.6884(3) 0.4815(2) 0.4189(2) 0.0381 1.0000 Uani . . . . . . C25 C 1.0779(4) 0.4847(2) 0.23934(19) 0.0400 1.0000 Uani . . . . . . C26 C 1.0375(3) 0.6945(2) 0.38656(19) 0.0344 1.0000 Uani . . . . . . C27 C 0.4016(3) 0.6285(2) 0.34077(18) 0.0338 1.0000 Uani . . . . . . O28 O 0.3627(3) 0.57885(16) 0.38923(15) 0.0489 1.0000 Uani . . . . . . C29 C 0.4257(4) 0.6388(2) 0.1902(2) 0.0416 1.0000 Uani . . . . . . O30 O 0.3970(3) 0.5979(2) 0.15274(19) 0.0667 1.0000 Uani . . . . . . C31 C 0.2807(3) 0.7645(2) 0.23215(18) 0.0368 1.0000 Uani . . . . . . O32 O 0.1711(3) 0.79416(18) 0.22086(16) 0.0544 1.0000 Uani . . . . . . C33 C 0.5392(4) 0.7859(2) 0.15721(19) 0.0409 1.0000 Uani . . . . . . O34 O 0.5783(4) 0.8233(2) 0.10185(16) 0.0657 1.0000 Uani . . . . . . Mo35 Mo 0.92110(3) 0.224830(16) 0.293435(14) 0.0295 1.0000 Uani . . . . . . Al36 Al 0.87355(9) 0.27932(6) 0.15051(5) 0.0307 1.0000 Uani . . . . . . C37 C 0.6835(3) 0.29526(19) 0.10293(16) 0.0287 1.0000 Uani . . . . . . N38 N 0.6170(3) 0.36867(16) 0.08858(15) 0.0314 1.0000 Uani . . . . . . C39 C 0.6864(3) 0.43788(18) 0.09660(17) 0.0305 1.0000 Uani . . . . . . C40 C 0.7716(3) 0.47655(19) 0.03940(17) 0.0305 1.0000 Uani . . . . . . C41 C 0.7970(4) 0.4466(2) -0.02940(18) 0.0383 1.0000 Uani . . . . . . C42 C 0.8302(3) 0.5461(2) 0.04615(18) 0.0340 1.0000 Uani . . . . . . C43 C 0.8051(3) 0.5779(2) 0.10739(19) 0.0354 1.0000 Uani . . . . . . C44 C 0.8667(4) 0.6545(2) 0.1125(2) 0.0492 1.0000 Uani . . . . . . C45 C 0.7212(4) 0.5371(2) 0.16344(19) 0.0375 1.0000 Uani . . . . . . C46 C 0.6604(3) 0.46700(19) 0.15964(17) 0.0336 1.0000 Uani . . . . . . C47 C 0.5707(4) 0.4244(2) 0.2214(2) 0.0465 1.0000 Uani . . . . . . C48 C 0.4766(3) 0.3867(2) 0.0582(2) 0.0424 1.0000 Uani . . . . . . C49 C 0.4011(4) 0.3098(2) 0.0795(2) 0.0480 1.0000 Uani . . . . . . C50 C 0.4841(4) 0.2432(2) 0.0557(2) 0.0483 1.0000 Uani . . . . . . N51 N 0.6234(3) 0.23445(16) 0.08707(15) 0.0329 1.0000 Uani . . . . . . C52 C 0.6964(3) 0.15529(19) 0.09813(17) 0.0319 1.0000 Uani . . . . . . C53 C 0.6698(3) 0.0945(2) 0.16157(18) 0.0351 1.0000 Uani . . . . . . C54 C 0.5690(4) 0.1093(3) 0.2186(2) 0.0487 1.0000 Uani . . . . . . C55 C 0.7417(4) 0.0188(2) 0.17063(19) 0.0403 1.0000 Uani . . . . . . C56 C 0.8330(4) 0.0027(2) 0.1182(2) 0.0456 1.0000 Uani . . . . . . C57 C 0.9113(5) -0.0794(3) 0.1296(3) 0.0654 1.0000 Uani . . . . . . C58 C 0.8534(4) 0.0646(2) 0.0545(2) 0.0485 1.0000 Uani . . . . . . C59 C 0.7860(4) 0.1417(2) 0.04269(18) 0.0381 1.0000 Uani . . . . . . C60 C 0.8096(5) 0.2060(2) -0.0278(2) 0.0517 1.0000 Uani . . . . . . C61 C 0.9444(3) 0.2710(2) 0.37832(18) 0.0357 1.0000 Uani . . . . . . O62 O 0.9561(3) 0.29665(18) 0.42943(14) 0.0502 1.0000 Uani . . . . . . C63 C 1.1224(4) 0.2388(2) 0.27073(19) 0.0414 1.0000 Uani . . . . . . O64 O 1.2374(3) 0.2472(2) 0.26337(19) 0.0678 1.0000 Uani . . . . . . C65 C 0.9710(4) 0.1141(2) 0.3562(2) 0.0494 1.0000 Uani . . . . . . O66 O 1.0017(4) 0.0500(2) 0.3921(2) 0.0822 1.0000 Uani . . . . . . C67 C 0.7249(4) 0.2149(2) 0.32885(19) 0.0409 1.0000 Uani . . . . . . O68 O 0.6173(3) 0.2114(2) 0.35395(17) 0.0622 1.0000 Uani . . . . . . F69 F 1.1346(8) 0.1625(4) 0.0473(4) 0.1140 0.6018 Uani D . . 1 1 . F70 F 1.1939(13) 0.1510(7) 0.0200(6) 0.1174 0.3982 Uani D . . 1 2 . C71 C 1.2012(8) 0.0945(4) 0.0926(3) 0.0714 0.6018 Uani D . . 1 1 . C72 C 1.2252(11) 0.0915(6) 0.0839(5) 0.0885 0.3982 Uani D . . 1 2 . C73 C 1.1552(8) 0.0725(5) 0.1622(4) 0.0666 0.6018 Uani D . . 1 1 . C74 C 1.1578(13) 0.0992(7) 0.1433(6) 0.0865 0.3982 Uani D . . 1 2 . C75 C 1.1871(13) 0.0365(7) 0.2080(5) 0.0773 0.3982 Uani D . . 1 2 . C76 C 1.2294(8) 0.0056(4) 0.2094(3) 0.0602 0.6018 Uani D . . 1 1 . C77 C 1.2923(14) -0.0221(7) 0.2100(5) 0.0754 0.3982 Uani D . . 1 2 . C78 C 1.3407(7) -0.0334(4) 0.1841(4) 0.0596 0.6018 Uani D . . 1 1 . C79 C 1.3762(8) -0.0057(5) 0.1098(4) 0.0701 0.6018 Uani D . . 1 1 . C80 C 1.3616(14) -0.0212(8) 0.1449(7) 0.0774 0.3982 Uani D . . 1 2 . C81 C 1.2996(9) 0.0588(5) 0.0615(3) 0.0722 0.6018 Uani D . . 1 1 . C82 C 1.3268(16) 0.0377(9) 0.0785(6) 0.0787 0.3982 Uani D . . 1 2 . H51 H 0.9015 0.5977 0.5462 0.0344 1.0000 Uiso R . . . . . H52 H 0.8191 0.5244 0.5387 0.0341 1.0000 Uiso R . . . . . H61 H 0.7251 0.5859 0.6317 0.0420 1.0000 Uiso R . . . . . H62 H 0.6168 0.5877 0.5691 0.0415 1.0000 Uiso R . . . . . H71 H 0.7639 0.7224 0.5767 0.0411 1.0000 Uiso R . . . . . H72 H 0.6028 0.7178 0.5865 0.0408 1.0000 Uiso R . . . . . H111 H 0.2900 0.9031 0.4365 0.0406 1.0000 Uiso R . . . . . H131 H 0.4355 1.0903 0.4059 0.0694 1.0000 Uiso R . . . . . H132 H 0.2961 1.0506 0.4182 0.0686 1.0000 Uiso R . . . . . H133 H 0.3653 1.0659 0.3414 0.0692 1.0000 Uiso R . . . . . H141 H 0.6473 1.0046 0.4021 0.0431 1.0000 Uiso R . . . . . H161 H 0.8561 0.9241 0.4467 0.0613 1.0000 Uiso R . . . . . H162 H 0.8581 0.8305 0.4774 0.0614 1.0000 Uiso R . . . . . H163 H 0.8602 0.8692 0.3930 0.0616 1.0000 Uiso R . . . . . H171 H 0.2740 0.7613 0.4800 0.0582 1.0000 Uiso R . . . . . H172 H 0.3954 0.7144 0.5268 0.0587 1.0000 Uiso R . . . . . H173 H 0.3832 0.7132 0.4451 0.0584 1.0000 Uiso R . . . . . H201 H 1.1257 0.6124 0.2899 0.0352 1.0000 Uiso R . . . . . H221 H 0.8544 0.4423 0.3185 0.0371 1.0000 Uiso R . . . . . H241 H 0.6396 0.4613 0.3849 0.0578 1.0000 Uiso R . . . . . H242 H 0.7142 0.4374 0.4611 0.0579 1.0000 Uiso R . . . . . H243 H 0.6298 0.5198 0.4363 0.0575 1.0000 Uiso R . . . . . H251 H 1.0986 0.4277 0.2600 0.0605 1.0000 Uiso R . . . . . H252 H 1.1612 0.5104 0.2238 0.0600 1.0000 Uiso R . . . . . H253 H 1.0204 0.4914 0.1968 0.0603 1.0000 Uiso R . . . . . H263 H 1.1342 0.6929 0.3805 0.0520 1.0000 Uiso R . . . . . H262 H 1.0171 0.6940 0.4367 0.0522 1.0000 Uiso R . . . . . H261 H 0.9974 0.7445 0.3558 0.0523 1.0000 Uiso R . . . . . H411 H 0.8429 0.4862 -0.0663 0.0573 1.0000 Uiso R . . . . . H412 H 0.8534 0.3966 -0.0180 0.0569 1.0000 Uiso R . . . . . H413 H 0.7125 0.4377 -0.0500 0.0571 1.0000 Uiso R . . . . . H421 H 0.8862 0.5720 0.0084 0.0414 1.0000 Uiso R . . . . . H441 H 0.8145 0.6794 0.1457 0.0747 1.0000 Uiso R . . . . . H442 H 0.9593 0.6426 0.1304 0.0743 1.0000 Uiso R . . . . . H443 H 0.8667 0.6924 0.0651 0.0744 1.0000 Uiso R . . . . . H451 H 0.7037 0.5576 0.2048 0.0450 1.0000 Uiso R . . . . . H471 H 0.5587 0.4548 0.2581 0.0701 1.0000 Uiso R . . . . . H472 H 0.6102 0.3711 0.2441 0.0704 1.0000 Uiso R . . . . . H473 H 0.4823 0.4197 0.2022 0.0701 1.0000 Uiso R . . . . . H481 H 0.4313 0.4278 0.0800 0.0508 1.0000 Uiso R . . . . . H482 H 0.4803 0.4064 0.0050 0.0509 1.0000 Uiso R . . . . . H491 H 0.3884 0.2940 0.1332 0.0577 1.0000 Uiso R . . . . . H492 H 0.3126 0.3194 0.0551 0.0579 1.0000 Uiso R . . . . . H501 H 0.4907 0.2573 0.0019 0.0579 1.0000 Uiso R . . . . . H502 H 0.4416 0.1913 0.0728 0.0581 1.0000 Uiso R . . . . . H541 H 0.5829 0.0693 0.2643 0.0729 1.0000 Uiso R . . . . . H542 H 0.5769 0.1616 0.2274 0.0727 1.0000 Uiso R . . . . . H543 H 0.4781 0.1081 0.2020 0.0731 1.0000 Uiso R . . . . . H551 H 0.7270 -0.0219 0.2136 0.0477 1.0000 Uiso R . . . . . H571 H 0.8922 -0.1031 0.0897 0.0982 1.0000 Uiso R . . . . . H572 H 1.0077 -0.0741 0.1306 0.0980 1.0000 Uiso R . . . . . H573 H 0.8858 -0.1151 0.1748 0.0982 1.0000 Uiso R . . . . . H581 H 0.9142 0.0542 0.0185 0.0577 1.0000 Uiso R . . . . . H601 H 0.8463 0.1816 -0.0651 0.0773 1.0000 Uiso R . . . . . H602 H 0.8731 0.2425 -0.0193 0.0775 1.0000 Uiso R . . . . . H603 H 0.7258 0.2365 -0.0452 0.0777 1.0000 Uiso R . . . . . H731 H 1.0787 0.0985 0.1789 0.0802 0.6018 Uiso R . . 1 1 . H741 H 1.0952 0.1433 0.1426 0.1041 0.3982 Uiso R . . 1 2 . H751 H 1.1343 0.0344 0.2503 0.0931 0.3982 Uiso R . . 1 2 . H761 H 1.2035 -0.0147 0.2603 0.0712 0.6018 Uiso R . . 1 1 . H771 H 1.3148 -0.0609 0.2542 0.0902 0.3982 Uiso R . . 1 2 . H781 H 1.3914 -0.0771 0.2154 0.0713 0.6018 Uiso R . . 1 1 . H791 H 1.4522 -0.0298 0.0905 0.0842 0.6018 Uiso R . . 1 1 . H801 H 1.4330 -0.0601 0.1452 0.0931 0.3982 Uiso R . . 1 2 . H811 H 1.3167 0.0752 0.0108 0.0871 0.6018 Uiso R . . 1 1 . H821 H 1.3729 0.0382 0.0341 0.0941 0.3982 Uiso R . . 1 2 . H1 H 0.514(4) 0.781(2) 0.312(2) 0.037(9) 1.0000 Uiso . . . . . . H3 H 0.869(4) 0.322(3) 0.222(2) 0.053(12) 1.0000 Uiso . . . . . . H4 H 0.651(4) 0.673(2) 0.281(2) 0.037(9) 1.0000 Uiso . . . . . . H5 H 0.891(4) 0.187(2) 0.211(2) 0.046(11) 1.0000 Uiso . . . . . . H6 H 0.784(4) 0.802(2) 0.288(2) 0.046(11) 1.0000 Uiso . . . . . . H7 H 0.980(4) 0.305(3) 0.091(2) 0.055(12) 1.0000 Uiso . . . . . . 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 0.02696(13) 0.03134(13) 0.02269(12) -0.00721(10) -0.00431(9) 0.00008(10) Al2 0.0278(4) 0.0297(4) 0.0220(4) -0.0043(3) -0.0015(3) -0.0045(3) C3 0.0228(13) 0.0272(13) 0.0247(13) -0.0080(11) 0.0010(10) -0.0056(10) N4 0.0267(11) 0.0270(12) 0.0201(11) -0.0044(9) -0.0010(9) -0.0033(9) C5 0.0312(15) 0.0308(15) 0.0204(13) -0.0024(11) -0.0051(11) 0.0005(12) C6 0.0406(17) 0.0396(17) 0.0224(14) -0.0023(12) 0.0006(12) -0.0004(14) C7 0.0382(16) 0.0417(17) 0.0234(14) -0.0121(12) 0.0009(12) 0.0001(13) N8 0.0277(12) 0.0259(12) 0.0217(11) -0.0064(9) 0.0007(9) -0.0014(9) C9 0.0305(14) 0.0281(14) 0.0224(13) -0.0090(11) 0.0003(11) -0.0032(11) C10 0.0314(15) 0.0369(16) 0.0259(14) -0.0138(12) -0.0003(11) -0.0045(12) C11 0.0289(15) 0.0418(17) 0.0331(15) -0.0160(13) -0.0013(12) 0.0042(13) C12 0.0432(18) 0.0352(16) 0.0262(14) -0.0091(12) -0.0009(13) 0.0047(13) C13 0.054(2) 0.0385(18) 0.0419(19) -0.0097(15) 0.0009(16) 0.0120(16) C14 0.0444(18) 0.0298(15) 0.0322(16) -0.0079(12) 0.0018(13) -0.0036(13) C15 0.0340(15) 0.0313(15) 0.0305(15) -0.0100(12) -0.0005(12) -0.0045(12) C16 0.0341(17) 0.0353(17) 0.054(2) -0.0129(15) -0.0003(15) -0.0079(13) C17 0.0342(16) 0.0462(19) 0.0423(18) -0.0202(15) 0.0044(14) -0.0118(14) C18 0.0247(13) 0.0268(13) 0.0235(13) -0.0073(10) -0.0039(10) 0.0001(10) C19 0.0251(13) 0.0314(14) 0.0271(14) -0.0091(11) -0.0015(11) -0.0027(11) C20 0.0247(13) 0.0375(16) 0.0275(14) -0.0107(12) 0.0003(11) -0.0027(12) C21 0.0276(14) 0.0398(16) 0.0273(14) -0.0115(12) -0.0047(11) 0.0023(12) C22 0.0331(15) 0.0291(14) 0.0309(15) -0.0107(12) -0.0054(12) -0.0009(12) C23 0.0270(14) 0.0259(13) 0.0272(14) -0.0050(11) -0.0039(11) -0.0015(11) C24 0.0359(17) 0.0362(17) 0.0436(18) -0.0104(14) 0.0035(14) -0.0123(13) C25 0.0374(17) 0.049(2) 0.0385(17) -0.0208(15) -0.0011(14) 0.0016(15) C26 0.0289(15) 0.0399(17) 0.0389(17) -0.0163(14) 0.0040(12) -0.0098(13) C27 0.0286(15) 0.0346(16) 0.0386(17) -0.0101(13) -0.0068(12) 0.0000(12) O28 0.0473(15) 0.0437(14) 0.0479(15) 0.0043(12) 0.0020(12) -0.0104(12) C29 0.0348(17) 0.050(2) 0.0429(19) -0.0180(16) -0.0133(14) 0.0054(15) O30 0.0627(19) 0.076(2) 0.078(2) -0.0517(18) -0.0330(16) 0.0111(16) C31 0.0353(17) 0.0409(18) 0.0299(15) -0.0012(13) -0.0013(13) -0.0037(14) O32 0.0334(13) 0.0627(18) 0.0557(17) 0.0026(13) -0.0043(12) 0.0079(12) C33 0.0440(19) 0.048(2) 0.0295(16) -0.0099(14) -0.0014(14) 0.0030(15) O34 0.080(2) 0.071(2) 0.0364(15) 0.0026(14) 0.0157(14) -0.0065(17) Mo35 0.02941(13) 0.03261(14) 0.02676(13) -0.00729(10) -0.00594(10) -0.00276(10) Al36 0.0253(4) 0.0394(5) 0.0272(4) -0.0094(4) -0.0042(3) 0.0022(4) C37 0.0267(14) 0.0337(15) 0.0260(14) -0.0091(11) -0.0031(11) 0.0011(11) N38 0.0246(12) 0.0350(13) 0.0340(13) -0.0087(11) -0.0056(10) 0.0034(10) C39 0.0286(14) 0.0299(15) 0.0325(15) -0.0087(12) -0.0050(12) 0.0057(12) C40 0.0242(14) 0.0377(16) 0.0293(14) -0.0099(12) -0.0064(11) 0.0062(12) C41 0.0363(17) 0.051(2) 0.0294(16) -0.0138(14) -0.0045(13) 0.0016(14) C42 0.0280(15) 0.0389(17) 0.0325(15) -0.0054(13) -0.0043(12) 0.0017(12) C43 0.0346(16) 0.0322(16) 0.0393(17) -0.0104(13) -0.0085(13) 0.0040(13) C44 0.053(2) 0.0390(19) 0.059(2) -0.0175(17) -0.0051(18) -0.0025(16) C45 0.0421(18) 0.0386(17) 0.0340(16) -0.0164(14) -0.0030(13) 0.0089(14) C46 0.0349(16) 0.0332(16) 0.0307(15) -0.0077(12) -0.0015(12) 0.0087(13) C47 0.056(2) 0.0428(19) 0.0384(18) -0.0098(15) 0.0091(16) 0.0056(17) C48 0.0289(16) 0.0435(19) 0.053(2) -0.0098(16) -0.0117(15) 0.0043(14) C49 0.0266(16) 0.052(2) 0.061(2) -0.0061(18) -0.0117(15) -0.0002(15) C50 0.0383(19) 0.048(2) 0.059(2) -0.0139(18) -0.0206(17) -0.0040(16) N51 0.0298(13) 0.0348(14) 0.0342(14) -0.0088(11) -0.0087(10) -0.0003(10) C52 0.0323(15) 0.0332(15) 0.0307(15) -0.0094(12) -0.0072(12) -0.0006(12) C53 0.0349(16) 0.0401(17) 0.0318(15) -0.0107(13) -0.0006(13) -0.0076(13) C54 0.055(2) 0.052(2) 0.042(2) -0.0169(17) 0.0121(17) -0.0122(18) C55 0.0460(19) 0.0375(17) 0.0329(16) 0.0002(13) 0.0002(14) -0.0064(15) C56 0.053(2) 0.0358(18) 0.044(2) -0.0051(15) 0.0005(16) 0.0058(16) C57 0.073(3) 0.043(2) 0.066(3) 0.006(2) 0.021(2) 0.011(2) C58 0.059(2) 0.0417(19) 0.0405(19) -0.0064(15) 0.0152(17) 0.0067(17) C59 0.0462(19) 0.0386(17) 0.0275(15) -0.0054(13) -0.0002(13) -0.0003(14) C60 0.071(3) 0.044(2) 0.0334(18) -0.0017(15) 0.0074(17) 0.0059(19) C61 0.0337(16) 0.0419(18) 0.0323(16) -0.0091(13) -0.0046(13) -0.0079(13) O62 0.0598(17) 0.0614(17) 0.0359(13) -0.0200(12) -0.0066(12) -0.0187(14) C63 0.0353(18) 0.052(2) 0.0353(17) -0.0082(15) -0.0064(14) -0.0025(15) O64 0.0353(15) 0.101(3) 0.065(2) -0.0161(18) -0.0003(13) -0.0088(16) C65 0.048(2) 0.043(2) 0.053(2) -0.0014(17) -0.0152(17) -0.0105(16) O66 0.086(3) 0.0467(18) 0.095(3) 0.0199(17) -0.030(2) -0.0114(17) C67 0.0400(18) 0.055(2) 0.0335(16) -0.0191(15) -0.0033(14) -0.0091(15) O68 0.0469(16) 0.095(2) 0.0572(18) -0.0384(17) 0.0154(13) -0.0211(16) F69 0.103(5) 0.085(4) 0.136(5) -0.002(4) -0.018(4) 0.021(3) F70 0.114(7) 0.119(7) 0.115(7) -0.022(5) 0.014(6) -0.011(6) C71 0.069(4) 0.052(3) 0.092(4) -0.017(3) -0.015(3) 0.000(3) C72 0.085(6) 0.083(6) 0.104(6) -0.034(5) 0.012(5) -0.014(5) C73 0.056(4) 0.054(4) 0.091(4) -0.026(3) 0.001(3) 0.012(3) C74 0.078(6) 0.077(6) 0.112(6) -0.040(5) 0.014(5) -0.003(5) C75 0.077(6) 0.068(6) 0.102(6) -0.051(5) 0.015(5) -0.004(5) C76 0.056(4) 0.054(4) 0.076(4) -0.028(3) 0.003(3) 0.001(3) C77 0.078(6) 0.060(5) 0.099(6) -0.039(5) 0.011(5) -0.008(5) C78 0.060(4) 0.043(3) 0.078(4) -0.022(3) -0.001(3) 0.007(3) C79 0.065(4) 0.059(4) 0.085(4) -0.019(4) 0.015(4) 0.001(3) C80 0.079(6) 0.063(6) 0.100(7) -0.039(5) 0.021(6) -0.004(5) C81 0.071(4) 0.058(4) 0.087(4) -0.015(3) 0.003(4) -0.013(3) C82 0.078(6) 0.074(6) 0.094(6) -0.038(5) 0.020(5) -0.015(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.27859(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . Al2 . 2.6211(9) yes Mo1 . C27 . 2.020(3) yes Mo1 . C29 . 1.969(4) yes Mo1 . C31 . 1.983(3) yes Mo1 . C33 . 2.034(4) yes Mo1 . H1 . 1.91(4) no Mo1 . H4 . 1.90(4) no Al2 . C3 . 2.047(3) yes Al2 . H1 . 1.67(4) no Al2 . H4 . 1.63(4) no Al2 . H6 . 1.47(4) no C3 . N4 . 1.335(4) yes C3 . N8 . 1.333(4) yes N4 . C5 . 1.477(3) yes N4 . C18 . 1.443(4) yes C5 . C6 . 1.517(4) yes C5 . H51 . 0.961 no C5 . H52 . 0.967 no C6 . C7 . 1.516(5) yes C6 . H61 . 0.977 no C6 . H62 . 0.972 no C7 . N8 . 1.479(4) yes C7 . H71 . 0.973 no C7 . H72 . 0.978 no N8 . C9 . 1.451(4) yes C9 . C10 . 1.401(4) yes C9 . C15 . 1.401(4) yes C10 . C11 . 1.394(4) yes C10 . C17 . 1.504(4) yes C11 . C12 . 1.386(5) yes C11 . H111 . 0.930 no C12 . C13 . 1.514(5) yes C12 . C14 . 1.389(5) yes C13 . H131 . 0.963 no C13 . H132 . 0.952 no C13 . H133 . 0.952 no C14 . C15 . 1.398(4) yes C14 . H141 . 0.933 no C15 . C16 . 1.506(4) yes C16 . H161 . 0.948 no C16 . H162 . 0.952 no C16 . H163 . 0.949 no C17 . H171 . 0.955 no C17 . H172 . 0.950 no C17 . H173 . 0.943 no C18 . C19 . 1.403(4) yes C18 . C23 . 1.405(4) yes C19 . C20 . 1.402(4) yes C19 . C26 . 1.503(4) yes C20 . C21 . 1.388(4) yes C20 . H201 . 0.938 no C21 . C22 . 1.391(4) yes C21 . C25 . 1.509(4) yes C22 . C23 . 1.392(4) yes C22 . H221 . 0.937 no C23 . C24 . 1.509(4) yes C24 . H241 . 0.946 no C24 . H242 . 0.961 no C24 . H243 . 0.953 no C25 . H251 . 0.958 no C25 . H252 . 0.961 no C25 . H253 . 0.960 no C26 . H263 . 0.952 no C26 . H262 . 0.951 no C26 . H261 . 0.958 no C27 . O28 . 1.150(4) yes C29 . O30 . 1.158(4) yes C31 . O32 . 1.153(4) yes C33 . O34 . 1.142(4) yes Mo35 . Al36 . 2.6252(9) yes Mo35 . C61 . 1.964(3) yes Mo35 . C63 . 2.030(4) yes Mo35 . C65 . 1.981(4) yes Mo35 . C67 . 2.028(4) yes Mo35 . H3 . 1.88(4) no Mo35 . H5 . 1.85(4) no Al36 . C37 . 2.049(3) yes Al36 . H3 . 1.68(4) no Al36 . H5 . 1.69(4) no Al36 . H7 . 1.51(4) no C37 . N38 . 1.333(4) yes C37 . N51 . 1.329(4) yes N38 . C39 . 1.447(4) yes N38 . C48 . 1.479(4) yes C39 . C40 . 1.399(4) yes C39 . C46 . 1.401(4) yes C40 . C41 . 1.509(4) yes C40 . C42 . 1.391(5) yes C41 . H411 . 0.962 no C41 . H412 . 0.959 no C41 . H413 . 0.958 no C42 . C43 . 1.395(5) yes C42 . H421 . 0.924 no C43 . C44 . 1.506(5) yes C43 . C45 . 1.391(5) yes C44 . H441 . 0.956 no C44 . H442 . 0.963 no C44 . H443 . 0.953 no C45 . C46 . 1.393(5) yes C45 . H451 . 0.934 no C46 . C47 . 1.502(5) yes C47 . H471 . 0.961 no C47 . H472 . 0.954 no C47 . H473 . 0.960 no C48 . C49 . 1.514(5) yes C48 . H481 . 0.973 no C48 . H482 . 0.963 no C49 . C50 . 1.503(6) yes C49 . H491 . 0.975 no C49 . H492 . 0.970 no C50 . N51 . 1.478(4) yes C50 . H501 . 0.970 no C50 . H502 . 0.982 no N51 . C52 . 1.448(4) yes C52 . C53 . 1.393(4) yes C52 . C59 . 1.398(5) yes C53 . C54 . 1.495(5) yes C53 . C55 . 1.397(5) yes C54 . H541 . 0.950 no C54 . H542 . 0.956 no C54 . H543 . 0.952 no C55 . C56 . 1.379(5) yes C55 . H551 . 0.932 no C56 . C57 . 1.514(5) yes C56 . C58 . 1.393(5) yes C57 . H571 . 0.960 no C57 . H572 . 0.958 no C57 . H573 . 0.946 no C58 . C59 . 1.393(5) yes C58 . H581 . 0.932 no C59 . C60 . 1.507(5) yes C60 . H601 . 0.950 no C60 . H602 . 0.956 no C60 . H603 . 0.955 no C61 . O62 . 1.157(4) yes C63 . O64 . 1.148(4) yes C65 . O66 . 1.148(5) yes C67 . O68 . 1.146(4) yes F69 . C71 . 1.375(5) yes F70 . C72 . 1.374(6) yes C71 . C73 . 1.334(5) yes C71 . C81 . 1.309(5) yes C72 . C74 . 1.310(6) yes C72 . C82 . 1.324(6) yes C73 . C76 . 1.410(5) yes C73 . H731 . 0.933 no C74 . C75 . 1.408(6) yes C74 . H741 . 0.933 no C75 . C77 . 1.377(5) yes C75 . H751 . 0.930 no C76 . C78 . 1.375(5) yes C76 . H761 . 0.959 no C77 . C80 . 1.377(6) yes C77 . H771 . 0.933 no C78 . C79 . 1.390(5) yes C78 . H781 . 0.935 no C79 . C81 . 1.408(5) yes C79 . H791 . 0.935 no C80 . C82 . 1.409(6) yes C80 . H801 . 0.927 no C81 . H811 . 0.930 no C82 . H821 . 0.935 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Al2 . Mo1 . C27 . 95.19(9) yes Al2 . Mo1 . C29 . 139.03(10) yes C27 . Mo1 . C29 . 88.11(15) yes Al2 . Mo1 . C31 . 132.20(11) yes C27 . Mo1 . C31 . 90.98(13) yes C29 . Mo1 . C31 . 88.42(14) yes Al2 . Mo1 . C33 . 87.37(10) yes C27 . Mo1 . C33 . 173.99(14) yes C29 . Mo1 . C33 . 86.41(16) yes C31 . Mo1 . C33 . 91.32(14) yes Al2 . Mo1 . H1 . 39.5(11) no C27 . Mo1 . H1 . 92.0(11) no C29 . Mo1 . H1 . 178.5(11) no C31 . Mo1 . H1 . 93.1(11) no C33 . Mo1 . H1 . 93.4(11) no Al2 . Mo1 . H4 . 38.4(11) no C27 . Mo1 . H4 . 88.7(11) no C29 . Mo1 . H4 . 101.2(11) no C31 . Mo1 . H4 . 170.4(11) no C33 . Mo1 . H4 . 89.9(11) no H1 . Mo1 . H4 . 77.4(15) no Mo1 . Al2 . C3 . 122.34(8) yes Mo1 . Al2 . H1 . 46.6(12) no C3 . Al2 . H1 . 107.5(12) no Mo1 . Al2 . H4 . 46.2(13) no C3 . Al2 . H4 . 108.1(13) no H1 . Al2 . H4 . 92.2(18) no Mo1 . Al2 . H6 . 127.4(15) no C3 . Al2 . H6 . 110.3(16) no H1 . Al2 . H6 . 118.9(20) no H4 . Al2 . H6 . 118(2) no Al2 . C3 . N4 . 120.8(2) yes Al2 . C3 . N8 . 119.3(2) yes N4 . C3 . N8 . 119.8(2) yes C3 . N4 . C5 . 123.5(2) yes C3 . N4 . C18 . 119.6(2) yes C5 . N4 . C18 . 116.5(2) yes N4 . C5 . C6 . 109.4(2) yes N4 . C5 . H51 . 108.9 no C6 . C5 . H51 . 109.6 no N4 . C5 . H52 . 109.6 no C6 . C5 . H52 . 109.8 no H51 . C5 . H52 . 109.6 no C5 . C6 . C7 . 109.9(3) yes C5 . C6 . H61 . 109.2 no C7 . C6 . H61 . 110.4 no C5 . C6 . H62 . 109.7 no C7 . C6 . H62 . 108.7 no H61 . C6 . H62 . 108.9 no C6 . C7 . N8 . 109.1(2) yes C6 . C7 . H71 . 110.4 no N8 . C7 . H71 . 108.9 no C6 . C7 . H72 . 110.5 no N8 . C7 . H72 . 108.5 no H71 . C7 . H72 . 109.4 no C7 . N8 . C3 . 123.4(2) yes C7 . N8 . C9 . 116.5(2) yes C3 . N8 . C9 . 119.9(2) yes N8 . C9 . C10 . 118.8(3) yes N8 . C9 . C15 . 119.3(3) yes C10 . C9 . C15 . 121.8(3) yes C9 . C10 . C11 . 117.8(3) yes C9 . C10 . C17 . 121.6(3) yes C11 . C10 . C17 . 120.6(3) yes C10 . C11 . C12 . 122.2(3) yes C10 . C11 . H111 . 118.8 no C12 . C11 . H111 . 119.0 no C11 . C12 . C13 . 120.9(3) yes C11 . C12 . C14 . 118.4(3) yes C13 . C12 . C14 . 120.8(3) yes C12 . C13 . H131 . 110.5 no C12 . C13 . H132 . 110.6 no H131 . C13 . H132 . 108.9 no C12 . C13 . H133 . 109.7 no H131 . C13 . H133 . 108.8 no H132 . C13 . H133 . 108.3 no C12 . C14 . C15 . 122.1(3) yes C12 . C14 . H141 . 118.8 no C15 . C14 . H141 . 119.1 no C9 . C15 . C14 . 117.7(3) yes C9 . C15 . C16 . 122.3(3) yes C14 . C15 . C16 . 120.0(3) yes C15 . C16 . H161 . 110.2 no C15 . C16 . H162 . 111.2 no H161 . C16 . H162 . 109.2 no C15 . C16 . H163 . 109.8 no H161 . C16 . H163 . 107.9 no H162 . C16 . H163 . 108.5 no C10 . C17 . H171 . 111.0 no C10 . C17 . H172 . 110.2 no H171 . C17 . H172 . 107.5 no C10 . C17 . H173 . 111.5 no H171 . C17 . H173 . 108.1 no H172 . C17 . H173 . 108.5 no N4 . C18 . C19 . 119.0(2) yes N4 . C18 . C23 . 119.6(3) yes C19 . C18 . C23 . 121.4(3) yes C18 . C19 . C20 . 117.9(3) yes C18 . C19 . C26 . 122.5(3) yes C20 . C19 . C26 . 119.5(3) yes C19 . C20 . C21 . 121.9(3) yes C19 . C20 . H201 . 119.4 no C21 . C20 . H201 . 118.7 no C20 . C21 . C22 . 118.5(3) yes C20 . C21 . C25 . 121.1(3) yes C22 . C21 . C25 . 120.4(3) yes C21 . C22 . C23 . 122.0(3) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 118.6 no C18 . C23 . C22 . 118.2(3) yes C18 . C23 . C24 . 121.8(3) yes C22 . C23 . C24 . 120.0(3) yes C23 . C24 . H241 . 110.3 no C23 . C24 . H242 . 110.2 no H241 . C24 . H242 . 109.1 no C23 . C24 . H243 . 110.7 no H241 . C24 . H243 . 109.1 no H242 . C24 . H243 . 107.4 no C21 . C25 . H251 . 110.1 no C21 . C25 . H252 . 111.2 no H251 . C25 . H252 . 109.3 no C21 . C25 . H253 . 109.0 no H251 . C25 . H253 . 108.1 no H252 . C25 . H253 . 109.0 no C19 . C26 . H263 . 111.0 no C19 . C26 . H262 . 111.1 no H263 . C26 . H262 . 108.4 no C19 . C26 . H261 . 109.4 no H263 . C26 . H261 . 109.3 no H262 . C26 . H261 . 107.6 no Mo1 . C27 . O28 . 176.8(3) yes Mo1 . C29 . O30 . 177.5(3) yes Mo1 . C31 . O32 . 179.2(3) yes Mo1 . C33 . O34 . 175.4(3) yes Al36 . Mo35 . C61 . 137.32(10) yes Al36 . Mo35 . C63 . 87.85(10) yes C61 . Mo35 . C63 . 87.77(14) yes Al36 . Mo35 . C65 . 131.81(13) yes C61 . Mo35 . C65 . 90.52(16) yes C63 . Mo35 . C65 . 89.04(16) yes Al36 . Mo35 . C67 . 98.48(10) yes C61 . Mo35 . C67 . 84.69(13) yes C63 . Mo35 . C67 . 172.37(14) yes C65 . Mo35 . C67 . 89.87(16) yes Al36 . Mo35 . H3 . 39.6(13) no C61 . Mo35 . H3 . 98.2(13) no C63 . Mo35 . H3 . 91.8(13) no C65 . Mo35 . H3 . 171.2(13) no C67 . Mo35 . H3 . 90.4(13) no Al36 . Mo35 . H5 . 39.7(12) no C61 . Mo35 . H5 . 176.3(12) no C63 . Mo35 . H5 . 94.0(12) no C65 . Mo35 . H5 . 92.7(12) no C67 . Mo35 . H5 . 93.6(12) no H3 . Mo35 . H5 . 78.5(18) no Mo35 . Al36 . C37 . 124.53(9) yes Mo35 . Al36 . H3 . 45.6(14) no C37 . Al36 . H3 . 109.1(14) no Mo35 . Al36 . H5 . 44.6(13) no C37 . Al36 . H5 . 109.1(13) no H3 . Al36 . H5 . 89.3(20) no Mo35 . Al36 . H7 . 125.8(16) no C37 . Al36 . H7 . 109.6(16) no H3 . Al36 . H7 . 118(2) no H5 . Al36 . H7 . 120(2) no Al36 . C37 . N38 . 118.9(2) yes Al36 . C37 . N51 . 122.1(2) yes N38 . C37 . N51 . 118.9(3) yes C37 . N38 . C39 . 119.9(2) yes C37 . N38 . C48 . 124.0(3) yes C39 . N38 . C48 . 115.9(3) yes N38 . C39 . C40 . 119.1(3) yes N38 . C39 . C46 . 118.9(3) yes C40 . C39 . C46 . 121.9(3) yes C39 . C40 . C41 . 122.0(3) yes C39 . C40 . C42 . 118.1(3) yes C41 . C40 . C42 . 119.9(3) yes C40 . C41 . H411 . 110.0 no C40 . C41 . H412 . 110.5 no H411 . C41 . H412 . 108.5 no C40 . C41 . H413 . 110.7 no H411 . C41 . H413 . 108.4 no H412 . C41 . H413 . 108.8 no C40 . C42 . C43 . 121.8(3) yes C40 . C42 . H421 . 118.4 no C43 . C42 . H421 . 119.8 no C42 . C43 . C44 . 120.9(3) yes C42 . C43 . C45 . 118.3(3) yes C44 . C43 . C45 . 120.9(3) yes C43 . C44 . H441 . 110.2 no C43 . C44 . H442 . 110.4 no H441 . C44 . H442 . 108.9 no C43 . C44 . H443 . 110.3 no H441 . C44 . H443 . 108.1 no H442 . C44 . H443 . 108.8 no C43 . C45 . C46 . 122.3(3) yes C43 . C45 . H451 . 119.1 no C46 . C45 . H451 . 118.6 no C39 . C46 . C45 . 117.7(3) yes C39 . C46 . C47 . 121.6(3) yes C45 . C46 . C47 . 120.8(3) yes C46 . C47 . H471 . 110.2 no C46 . C47 . H472 . 110.4 no H471 . C47 . H472 . 109.4 no C46 . C47 . H473 . 109.9 no H471 . C47 . H473 . 108.3 no H472 . C47 . H473 . 108.7 no N38 . C48 . C49 . 109.0(3) yes N38 . C48 . H481 . 107.8 no C49 . C48 . H481 . 109.7 no N38 . C48 . H482 . 109.6 no C49 . C48 . H482 . 110.1 no H481 . C48 . H482 . 110.6 no C48 . C49 . C50 . 109.0(3) yes C48 . C49 . H491 . 109.4 no C50 . C49 . H491 . 109.6 no C48 . C49 . H492 . 109.6 no C50 . C49 . H492 . 109.8 no H491 . C49 . H492 . 109.6 no C49 . C50 . N51 . 109.5(3) yes C49 . C50 . H501 . 109.4 no N51 . C50 . H501 . 108.7 no C49 . C50 . H502 . 110.7 no N51 . C50 . H502 . 109.1 no H501 . C50 . H502 . 109.4 no C50 . N51 . C37 . 123.3(3) yes C50 . N51 . C52 . 116.6(3) yes C37 . N51 . C52 . 120.0(3) yes N51 . C52 . C53 . 119.0(3) yes N51 . C52 . C59 . 118.5(3) yes C53 . C52 . C59 . 122.4(3) yes C52 . C53 . C54 . 121.6(3) yes C52 . C53 . C55 . 117.6(3) yes C54 . C53 . C55 . 120.8(3) yes C53 . C54 . H541 . 110.9 no C53 . C54 . H542 . 111.0 no H541 . C54 . H542 . 108.3 no C53 . C54 . H543 . 110.3 no H541 . C54 . H543 . 108.7 no H542 . C54 . H543 . 107.5 no C53 . C55 . C56 . 122.1(3) yes C53 . C55 . H551 . 118.5 no C56 . C55 . H551 . 119.4 no C55 . C56 . C57 . 121.2(3) yes C55 . C56 . C58 . 118.4(3) yes C57 . C56 . C58 . 120.5(4) yes C56 . C57 . H571 . 109.9 no C56 . C57 . H572 . 110.6 no H571 . C57 . H572 . 108.4 no C56 . C57 . H573 . 110.7 no H571 . C57 . H573 . 108.6 no H572 . C57 . H573 . 108.6 no C56 . C58 . C59 . 122.3(3) yes C56 . C58 . H581 . 119.1 no C59 . C58 . H581 . 118.6 no C52 . C59 . C58 . 117.1(3) yes C52 . C59 . C60 . 122.6(3) yes C58 . C59 . C60 . 120.2(3) yes C59 . C60 . H601 . 110.3 no C59 . C60 . H602 . 110.3 no H601 . C60 . H602 . 108.2 no C59 . C60 . H603 . 110.4 no H601 . C60 . H603 . 109.1 no H602 . C60 . H603 . 108.5 no Mo35 . C61 . O62 . 178.3(3) yes Mo35 . C63 . O64 . 174.8(3) yes Mo35 . C65 . O66 . 179.0(4) yes Mo35 . C67 . O68 . 174.2(3) yes F69 . C71 . C73 . 115.79(6) yes F69 . C71 . C81 . 115.73(6) yes C73 . C71 . C81 . 128.47(6) yes F70 . C72 . C74 . 115.67(7) yes F70 . C72 . C82 . 115.70(7) yes C74 . C72 . C82 . 128.40(7) yes C71 . C73 . C76 . 115.30(7) yes C71 . C73 . H731 . 123.0 no C76 . C73 . H731 . 121.7 no C72 . C74 . C75 . 115.32(7) yes C72 . C74 . H741 . 122.0 no C75 . C74 . H741 . 122.6 no C74 . C75 . C77 . 121.42(7) yes C74 . C75 . H751 . 119.6 no C77 . C75 . H751 . 119.0 no C73 . C76 . C78 . 121.38(7) yes C73 . C76 . H761 . 121.2 no C78 . C76 . H761 . 117.4 no C75 . C77 . C80 . 117.66(7) yes C75 . C77 . H771 . 120.4 no C80 . C77 . H771 . 121.9 no C76 . C78 . C79 . 117.68(7) yes C76 . C78 . H781 . 121.7 no C79 . C78 . H781 . 120.6 no C78 . C79 . C81 . 121.46(7) yes C78 . C79 . H791 . 120.6 no C81 . C79 . H791 . 118.0 no C77 . C80 . C82 . 121.40(7) yes C77 . C80 . H801 . 119.0 no C82 . C80 . H801 . 119.6 no C79 . C81 . C71 . 115.35(7) yes C79 . C81 . H811 . 122.8 no C71 . C81 . H811 . 121.8 no C80 . C82 . C72 . 115.30(7) yes C80 . C82 . H821 . 121.8 no C72 . C82 . H821 . 122.9 no Mo1 . H1 . Al2 . 93.9(17) no Mo35 . H3 . Al36 . 94.9(20) no Mo1 . H4 . Al2 . 95.4(17) no Mo35 . H5 . Al36 . 95.7(19) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C5 . H51 . O62 2_766 149.63(10) 0.961 2.494 3.359(7) yes C26 . H262 . O62 2_766 161.23(9) 0.951 2.560 3.474(7) yes C41 . H413 . O30 2_665 145.97(11) 0.958 2.441 3.280(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 25/03/13 at 13:52:02 # #LIST 12 BLOCK SCALE X'S, U'S CONT H ( 1,X'S,U[ISO]) H ( 4,X'S,U[ISO]) H ( 6,X'S,U[ISO]) CONT H ( 3,X'S,U[ISO]) H ( 5,X'S,U[ISO]) H ( 7,X'S,U[ISO]) REM RIDE MO ( 1,X'S) H ( 1,X'S) H ( 4,X'S) REM RIDE AL ( 2,X'S) H ( 1,X'S) H ( 4,X'S) H ( 6,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S) RIDE C ( 26,X'S) H ( 263,X'S) H ( 262,X'S) H ( 261,X'S) REM RIDE MO ( 35,X'S) H ( 3,X'S) H ( 5,X'S) REM RIDE AL ( 36,X'S) H ( 3,X'S) H ( 5,X'S) H ( 7,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) H ( 473,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) RIDE C ( 54,X'S) H ( 541,X'S) H ( 542,X'S) H ( 543,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 57,X'S) H ( 571,X'S) H ( 572,X'S) H ( 573,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S) RIDE C ( 73,X'S) H ( 731,X'S) RIDE C ( 74,X'S) H ( 741,X'S) RIDE C ( 75,X'S) H ( 751,X'S) RIDE C ( 76,X'S) H ( 761,X'S) RIDE C ( 77,X'S) H ( 771,X'S) RIDE C ( 78,X'S) H ( 781,X'S) RIDE C ( 79,X'S) H ( 791,X'S) RIDE C ( 80,X'S) H ( 801,X'S) RIDE C ( 81,X'S) H ( 811,X'S) RIDE C ( 82,X'S) H ( 821,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/03/13 at 13:52:02 # #LIST 16 SAME F(69) C(71) C(73) C(76) C(78) C(79) C(81) AND CONT F(69) C(71) C(81) C(79) C(78) C(76) C(73) AND CONT F(70) C(72) C(74) C(75) C(77) C(80) C(82) AND CONT F(70) C(72) C(82) C(80) C(77) C(75) C(74) SIMU 0.01 F(69) C(71) C(73) C(76) C(78) C(79) C(81) AND CONT F(69) C(71) C(81) C(79) C(78) C(76) C(73) AND CONT F(70) C(72) C(74) C(75) C(77) C(80) C(82) AND CONT F(70) C(72) C(82) C(80) C(77) C(75) C(74) DELU 0.01 F(69) C(71) C(73) C(76) C(78) C(79) C(81) AND CONT F(69) C(71) C(81) C(79) C(78) C(76) C(73) AND CONT F(70) C(72) C(74) C(75) C(77) C(80) C(82) AND CONT F(70) C(72) C(82) C(80) C(77) C(75) C(74) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 931227' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global _audit_creation_date 13-03-25 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 077janp12 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 15.66060(10) _cell_length_b 10.52320(10) _cell_length_c 23.2731(2) _cell_angle_alpha 90 _cell_angle_beta 98.8379(4) _cell_angle_gamma 90 _cell_volume 3789.86(5) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C38 H47 Al1 F2 Mo1 N2 O4 # Dc = 1.33 Fooo = 1576.00 Mu = 4.19 M = 756.72 # Found Formula = C38 H47 Al1 F2 Mo1 N2 O4 # Dc = 1.33 FOOO = 1576.00 Mu = 4.19 M = 756.72 _chemical_formula_sum 'C38 H47 Al1 F2 Mo1 N2 O4' _chemical_formula_moiety 'C32 H43 Al Mo N2 O4, C6 H4 F2' _chemical_compound_source . _chemical_formula_weight 756.72 _cell_measurement_reflns_used 9042 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.180 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_max 0.380 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.419 # Sheldrick geometric approximatio 0.88 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.93 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 76494 _reflns_number_total 8607 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections without Friedels Law is 15640 # Number of reflections with Friedels Law is 8607 # Theoretical number of reflections is about 8678 _diffrn_reflns_theta_min 5.113 _diffrn_reflns_theta_max 27.467 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.918 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _oxford_diffrn_Wilson_B_factor 2.27 _oxford_diffrn_Wilson_scale 32.76 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.89 _refine_diff_density_max 0.64 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 8607 _refine_ls_number_restraints 0 _refine_ls_number_parameters 442 _oxford_refine_ls_R_factor_ref 0.0616 _refine_ls_wR_factor_ref 0.1092 _refine_ls_goodness_of_fit_ref 0.9145 _refine_ls_shift/su_max 0.0010938 _refine_ls_shift/su_mean 0.0000270 # The values computed from all data _oxford_reflns_number_all 8607 _refine_ls_R_factor_all 0.0616 _refine_ls_wR_factor_all 0.1092 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6878 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_gt 0.0939 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 11.4 16.5 7.79 1.93 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mo1 Mo 0.721771(15) 0.61505(2) 0.383730(10) 0.0247 1.0000 Uani . . . . . . Al2 Al 0.73835(5) 0.42494(8) 0.45553(4) 0.0244 1.0000 Uani . . . . . . C3 C 0.73293(17) 0.2391(3) 0.43039(11) 0.0218 1.0000 Uani . . . . . . N4 N 0.80569(14) 0.1782(2) 0.42388(10) 0.0240 1.0000 Uani . . . . . . C5 C 0.88879(17) 0.2383(3) 0.44277(12) 0.0247 1.0000 Uani . . . . . . C6 C 0.93343(17) 0.2916(3) 0.40024(13) 0.0272 1.0000 Uani . . . . . . C7 C 1.0124(2) 0.3500(3) 0.41975(15) 0.0379 1.0000 Uani . . . . . . C8 C 1.0464(2) 0.3541(4) 0.47792(16) 0.0448 1.0000 Uani . . . . . . C9 C 1.0027(2) 0.2981(4) 0.51838(15) 0.0435 1.0000 Uani . . . . . . C10 C 0.92356(19) 0.2368(3) 0.50203(13) 0.0328 1.0000 Uani . . . . . . C11 C 0.8825(2) 0.1662(4) 0.54772(14) 0.0451 1.0000 Uani . . . . . . C12 C 0.9281(3) 0.0374(5) 0.5611(2) 0.0618 1.0000 Uani . . . . . . C13 C 0.8843(3) 0.2420(6) 0.60400(17) 0.0710 1.0000 Uani . . . . . . C14 C 0.9022(2) 0.2835(3) 0.33527(13) 0.0320 1.0000 Uani . . . . . . C15 C 0.9527(3) 0.1795(3) 0.30824(15) 0.0444 1.0000 Uani . . . . . . C16 C 0.9133(2) 0.4093(3) 0.30406(15) 0.0414 1.0000 Uani . . . . . . C17 C 0.80685(19) 0.0468(3) 0.40120(15) 0.0337 1.0000 Uani . . . . . . C18 C 0.7217(2) 0.0207(3) 0.36258(15) 0.0347 1.0000 Uani . . . . . . C19 C 0.64896(19) 0.0470(3) 0.39718(14) 0.0306 1.0000 Uani . . . . . . N20 N 0.65717(14) 0.1795(2) 0.41844(10) 0.0231 1.0000 Uani . . . . . . C21 C 0.57938(17) 0.2399(3) 0.43209(12) 0.0246 1.0000 Uani . . . . . . C22 C 0.51782(18) 0.2852(3) 0.38602(13) 0.0281 1.0000 Uani . . . . . . C23 C 0.5271(2) 0.2729(3) 0.32234(13) 0.0337 1.0000 Uani . . . . . . C24 C 0.4686(3) 0.1665(4) 0.29285(17) 0.0499 1.0000 Uani . . . . . . C25 C 0.5048(2) 0.3963(4) 0.28832(16) 0.0440 1.0000 Uani . . . . . . C26 C 0.44411(19) 0.3441(3) 0.40076(15) 0.0363 1.0000 Uani . . . . . . C27 C 0.4317(2) 0.3552(4) 0.45825(16) 0.0439 1.0000 Uani . . . . . . C28 C 0.4916(2) 0.3061(4) 0.50229(15) 0.0411 1.0000 Uani . . . . . . C29 C 0.56610(19) 0.2456(3) 0.49050(13) 0.0313 1.0000 Uani . . . . . . C30 C 0.6272(2) 0.1849(4) 0.54024(14) 0.0418 1.0000 Uani . . . . . . C31 C 0.5929(3) 0.0545(4) 0.55574(19) 0.0582 1.0000 Uani . . . . . . C32 C 0.6423(3) 0.2681(5) 0.59465(15) 0.0570 1.0000 Uani . . . . . . C33 C 0.62047(19) 0.7223(3) 0.35398(12) 0.0289 1.0000 Uani . . . . . . O34 O 0.55988(14) 0.7845(2) 0.33982(10) 0.0374 1.0000 Uani . . . . . . C35 C 0.80978(19) 0.7176(3) 0.35173(13) 0.0311 1.0000 Uani . . . . . . O36 O 0.86435(15) 0.7736(2) 0.33515(11) 0.0450 1.0000 Uani . . . . . . C37 C 0.73849(19) 0.7300(3) 0.45371(13) 0.0303 1.0000 Uani . . . . . . O38 O 0.74734(17) 0.8033(2) 0.49095(10) 0.0437 1.0000 Uani . . . . . . C39 C 0.7080(2) 0.5120(3) 0.30806(14) 0.0354 1.0000 Uani . . . . . . O40 O 0.70280(17) 0.4606(3) 0.26453(12) 0.0590 1.0000 Uani . . . . . . F41 F 0.8377(3) 0.8800(3) 0.78011(12) 0.0954 1.0000 Uani . . . . . . C42 C 0.8212(3) 0.7976(5) 0.73552(16) 0.0574 1.0000 Uani . . . . . . C43 C 0.8369(4) 0.6704(5) 0.74377(19) 0.0681 1.0000 Uani . . . . . . C44 C 0.8191(3) 0.5893(6) 0.6968(2) 0.0719 1.0000 Uani . . . . . . C45 C 0.7884(3) 0.6366(7) 0.6426(2) 0.0773 1.0000 Uani . . . . . . C46 C 0.7744(3) 0.7644(7) 0.63460(19) 0.0744 1.0000 Uani . . . . . . C47 C 0.7902(3) 0.8441(5) 0.68157(18) 0.0560 1.0000 Uani . . . . . . F48 F 0.7779(2) 0.9707(3) 0.67613(14) 0.0906 1.0000 Uani . . . . . . H71 H 1.0431 0.3873 0.3929 0.0460 1.0000 Uiso R . . . . . H81 H 1.0996 0.3956 0.4902 0.0540 1.0000 Uiso R . . . . . H91 H 1.0262 0.3000 0.5580 0.0523 1.0000 Uiso R . . . . . H111 H 0.8219 0.1487 0.5316 0.0539 1.0000 Uiso R . . . . . H121 H 0.9018 -0.0077 0.5894 0.0929 1.0000 Uiso R . . . . . H122 H 0.9878 0.0501 0.5764 0.0927 1.0000 Uiso R . . . . . H123 H 0.9241 -0.0147 0.5264 0.0928 1.0000 Uiso R . . . . . H131 H 0.8516 0.1975 0.6291 0.1068 1.0000 Uiso R . . . . . H132 H 0.9432 0.2500 0.6234 0.1068 1.0000 Uiso R . . . . . H133 H 0.8606 0.3255 0.5953 0.1066 1.0000 Uiso R . . . . . H141 H 0.8409 0.2612 0.3288 0.0377 1.0000 Uiso R . . . . . H151 H 0.9330 0.1724 0.2669 0.0670 1.0000 Uiso R . . . . . H153 H 1.0139 0.2014 0.3144 0.0670 1.0000 Uiso R . . . . . H152 H 0.9452 0.0984 0.3261 0.0667 1.0000 Uiso R . . . . . H161 H 0.8827 0.4061 0.2653 0.0619 1.0000 Uiso R . . . . . H163 H 0.9737 0.4234 0.3022 0.0616 1.0000 Uiso R . . . . . H162 H 0.8918 0.4800 0.3244 0.0617 1.0000 Uiso R . . . . . H171 H 0.8164 -0.0126 0.4333 0.0399 1.0000 Uiso R . . . . . H172 H 0.8537 0.0408 0.3783 0.0404 1.0000 Uiso R . . . . . H181 H 0.7201 -0.0671 0.3498 0.0420 1.0000 Uiso R . . . . . H182 H 0.7153 0.0754 0.3282 0.0417 1.0000 Uiso R . . . . . H192 H 0.6522 -0.0110 0.4297 0.0371 1.0000 Uiso R . . . . . H191 H 0.5938 0.0368 0.3724 0.0371 1.0000 Uiso R . . . . . H231 H 0.5871 0.2509 0.3200 0.0394 1.0000 Uiso R . . . . . H242 H 0.4768 0.1595 0.2527 0.0746 1.0000 Uiso R . . . . . H241 H 0.4819 0.0864 0.3119 0.0752 1.0000 Uiso R . . . . . H243 H 0.4092 0.1866 0.2946 0.0748 1.0000 Uiso R . . . . . H252 H 0.5214 0.3895 0.2499 0.0659 1.0000 Uiso R . . . . . H251 H 0.5346 0.4676 0.3085 0.0658 1.0000 Uiso R . . . . . H253 H 0.4433 0.4107 0.2839 0.0656 1.0000 Uiso R . . . . . H261 H 0.4030 0.3777 0.3710 0.0441 1.0000 Uiso R . . . . . H271 H 0.3819 0.3966 0.4669 0.0532 1.0000 Uiso R . . . . . H281 H 0.4823 0.3133 0.5406 0.0494 1.0000 Uiso R . . . . . H301 H 0.6831 0.1713 0.5274 0.0500 1.0000 Uiso R . . . . . H311 H 0.6352 0.0135 0.5844 0.0867 1.0000 Uiso R . . . . . H312 H 0.5396 0.0630 0.5712 0.0869 1.0000 Uiso R . . . . . H313 H 0.5829 0.0015 0.5216 0.0868 1.0000 Uiso R . . . . . H321 H 0.6864 0.2312 0.6227 0.0848 1.0000 Uiso R . . . . . H322 H 0.6605 0.3520 0.5850 0.0848 1.0000 Uiso R . . . . . H323 H 0.5901 0.2747 0.6122 0.0843 1.0000 Uiso R . . . . . H431 H 0.8586 0.6380 0.7810 0.0825 1.0000 Uiso R . . . . . H441 H 0.8284 0.5016 0.7014 0.0858 1.0000 Uiso R . . . . . H451 H 0.7768 0.5819 0.6111 0.0931 1.0000 Uiso R . . . . . H461 H 0.7546 0.7971 0.5975 0.0891 1.0000 Uiso R . . . . . H23 H 0.652(2) 0.504(3) 0.4188(15) 0.0360 1.0000 Uiso . . . . . . H21 H 0.755(2) 0.442(4) 0.5191(16) 0.0424 1.0000 Uiso . . . . . . H22 H 0.807(2) 0.503(3) 0.4177(15) 0.0370 1.0000 Uiso . . . . . . 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 0.02586(12) 0.02190(11) 0.02619(12) -0.00030(9) 0.00350(8) 0.00000(10) Al2 0.0265(4) 0.0218(4) 0.0249(4) -0.0031(3) 0.0038(3) -0.0004(3) C3 0.0219(12) 0.0237(13) 0.0200(12) 0.0042(10) 0.0037(9) -0.0002(10) N4 0.0206(10) 0.0211(11) 0.0311(12) -0.0001(9) 0.0059(9) 0.0011(9) C5 0.0203(12) 0.0245(13) 0.0296(14) -0.0003(10) 0.0051(10) 0.0016(10) C6 0.0204(12) 0.0289(14) 0.0326(14) 0.0009(11) 0.0051(11) 0.0014(11) C7 0.0269(15) 0.0389(17) 0.0484(19) 0.0008(14) 0.0068(13) -0.0062(13) C8 0.0281(15) 0.051(2) 0.052(2) -0.0096(16) -0.0043(14) -0.0072(14) C9 0.0317(16) 0.059(2) 0.0360(17) -0.0097(16) -0.0071(13) 0.0042(15) C10 0.0259(14) 0.0419(17) 0.0299(15) 0.0004(13) 0.0023(11) 0.0083(13) C11 0.0322(16) 0.072(3) 0.0314(16) 0.0137(16) 0.0063(13) 0.0167(16) C12 0.055(2) 0.074(3) 0.060(3) 0.033(2) 0.0169(19) 0.015(2) C13 0.067(3) 0.113(4) 0.035(2) 0.011(2) 0.0144(19) 0.035(3) C14 0.0299(14) 0.0364(16) 0.0297(14) 0.0042(12) 0.0050(11) -0.0026(12) C15 0.057(2) 0.043(2) 0.0353(17) 0.0032(14) 0.0141(15) 0.0057(17) C16 0.0406(17) 0.044(2) 0.0427(18) 0.0128(15) 0.0171(14) 0.0073(14) C17 0.0288(14) 0.0199(14) 0.0542(19) -0.0032(13) 0.0123(13) 0.0030(11) C18 0.0335(15) 0.0248(14) 0.0474(17) -0.0089(13) 0.0114(13) -0.0017(12) C19 0.0265(14) 0.0208(14) 0.0454(17) -0.0057(12) 0.0085(12) -0.0020(11) N20 0.0212(10) 0.0197(11) 0.0292(11) -0.0016(9) 0.0067(9) 0.0003(8) C21 0.0230(12) 0.0223(13) 0.0294(14) -0.0022(10) 0.0065(10) -0.0035(10) C22 0.0229(13) 0.0280(14) 0.0339(15) 0.0012(11) 0.0059(11) 0.0001(11) C23 0.0277(14) 0.0407(17) 0.0326(15) -0.0001(13) 0.0039(12) 0.0039(13) C24 0.056(2) 0.048(2) 0.0427(19) -0.0070(16) -0.0001(17) -0.0029(18) C25 0.0355(16) 0.051(2) 0.0438(18) 0.0123(16) 0.0012(14) 0.0016(15) C26 0.0234(14) 0.0433(17) 0.0421(17) 0.0010(14) 0.0050(12) 0.0046(13) C27 0.0302(16) 0.054(2) 0.0494(19) -0.0062(16) 0.0127(14) 0.0119(15) C28 0.0334(16) 0.057(2) 0.0358(16) -0.0076(15) 0.0140(13) 0.0009(15) C29 0.0259(14) 0.0383(16) 0.0308(15) -0.0033(12) 0.0076(11) -0.0020(12) C30 0.0282(15) 0.067(2) 0.0307(16) 0.0037(15) 0.0047(12) -0.0004(15) C31 0.061(2) 0.057(3) 0.054(2) 0.016(2) -0.0010(19) 0.003(2) C32 0.055(2) 0.088(3) 0.0284(17) 0.0010(18) 0.0071(16) -0.017(2) C33 0.0330(15) 0.0288(15) 0.0255(13) -0.0031(11) 0.0064(11) -0.0042(12) O34 0.0321(11) 0.0371(12) 0.0416(12) -0.0002(10) 0.0015(9) 0.0070(10) C35 0.0327(15) 0.0273(14) 0.0332(15) 0.0031(12) 0.0049(12) 0.0048(12) O36 0.0384(13) 0.0422(14) 0.0565(15) 0.0166(12) 0.0141(11) -0.0012(11) C37 0.0330(15) 0.0294(15) 0.0276(14) 0.0047(12) 0.0020(11) -0.0012(12) O38 0.0648(16) 0.0340(12) 0.0314(11) -0.0048(10) 0.0042(11) -0.0024(11) C39 0.0270(14) 0.0393(17) 0.0400(17) -0.0058(14) 0.0055(12) 0.0005(13) O40 0.0457(14) 0.083(2) 0.0486(15) -0.0325(15) 0.0076(12) -0.0028(14) F41 0.161(3) 0.073(2) 0.0469(14) -0.0081(14) -0.0007(17) -0.003(2) C42 0.073(3) 0.068(3) 0.0323(18) -0.0013(18) 0.0111(18) -0.011(2) C43 0.099(4) 0.065(3) 0.042(2) 0.005(2) 0.018(2) -0.005(3) C44 0.061(3) 0.082(4) 0.077(3) -0.018(3) 0.025(2) -0.007(2) C45 0.033(2) 0.129(5) 0.070(3) -0.046(3) 0.0076(19) -0.002(3) C46 0.042(2) 0.142(5) 0.037(2) -0.004(3) -0.0014(17) 0.010(3) C47 0.046(2) 0.078(3) 0.045(2) 0.013(2) 0.0090(17) 0.007(2) F48 0.106(2) 0.091(2) 0.0742(19) 0.0307(17) 0.0150(17) 0.0192(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17586(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . Al2 . 2.5939(9) yes Mo1 . C33 . 1.983(3) yes Mo1 . C35 . 1.983(3) yes Mo1 . C37 . 2.013(3) yes Mo1 . C39 . 2.051(3) yes Mo1 . H23 . 1.88(3) no Mo1 . H22 . 1.86(4) no Al2 . C3 . 2.039(3) yes Al2 . H23 . 1.70(3) no Al2 . H21 . 1.47(4) no Al2 . H22 . 1.70(3) no C3 . N4 . 1.336(3) yes C3 . N20 . 1.333(3) yes N4 . C5 . 1.453(3) yes N4 . C17 . 1.481(4) yes C5 . C6 . 1.413(4) yes C5 . C10 . 1.403(4) yes C6 . C7 . 1.393(4) yes C6 . C14 . 1.518(4) yes C7 . C8 . 1.377(5) yes C7 . H71 . 0.931 no C8 . C9 . 1.378(5) yes C8 . H81 . 0.945 no C9 . C10 . 1.397(5) yes C9 . H91 . 0.938 no C10 . C11 . 1.518(5) yes C11 . C12 . 1.541(6) yes C11 . C13 . 1.530(6) yes C11 . H111 . 0.983 no C12 . H121 . 0.956 no C12 . H122 . 0.958 no C12 . H123 . 0.970 no C13 . H131 . 0.957 no C13 . H132 . 0.966 no C13 . H133 . 0.963 no C14 . C15 . 1.541(5) yes C14 . C16 . 1.533(4) yes C14 . H141 . 0.977 no C15 . H151 . 0.967 no C15 . H153 . 0.974 no C15 . H152 . 0.964 no C16 . H161 . 0.956 no C16 . H163 . 0.965 no C16 . H162 . 0.969 no C17 . C18 . 1.514(4) yes C17 . H171 . 0.967 no C17 . H172 . 0.973 no C18 . C19 . 1.518(4) yes C18 . H181 . 0.970 no C18 . H182 . 0.979 no C19 . N20 . 1.479(3) yes C19 . H192 . 0.967 no C19 . H191 . 0.969 no N20 . C21 . 1.452(3) yes C21 . C22 . 1.410(4) yes C21 . C29 . 1.408(4) yes C22 . C23 . 1.517(4) yes C22 . C26 . 1.398(4) yes C23 . C24 . 1.539(5) yes C23 . C25 . 1.533(5) yes C23 . H231 . 0.978 no C24 . H242 . 0.966 no C24 . H241 . 0.960 no C24 . H243 . 0.961 no C25 . H252 . 0.971 no C25 . H251 . 0.968 no C25 . H253 . 0.964 no C26 . C27 . 1.386(5) yes C26 . H261 . 0.940 no C27 . C28 . 1.380(5) yes C27 . H271 . 0.941 no C28 . C29 . 1.393(4) yes C28 . H281 . 0.929 no C29 . C30 . 1.524(4) yes C30 . C31 . 1.537(6) yes C30 . C32 . 1.528(5) yes C30 . H301 . 0.978 no C31 . H311 . 0.967 no C31 . H312 . 0.963 no C31 . H313 . 0.964 no C32 . H321 . 0.957 no C32 . H322 . 0.966 no C32 . H323 . 0.970 no C33 . O34 . 1.158(4) yes C35 . O36 . 1.153(4) yes C37 . O38 . 1.153(4) yes C39 . O40 . 1.140(4) yes F41 . C42 . 1.347(5) yes C42 . C43 . 1.369(7) yes C42 . C47 . 1.365(6) yes C43 . C44 . 1.382(7) yes C43 . H431 . 0.944 no C44 . C45 . 1.372(8) yes C44 . H441 . 0.938 no C45 . C46 . 1.371(8) yes C45 . H451 . 0.926 no C46 . C47 . 1.370(7) yes C46 . H461 . 0.938 no C47 . F48 . 1.350(6) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Al2 . Mo1 . C33 . 131.25(9) yes Al2 . Mo1 . C35 . 130.91(9) yes C33 . Mo1 . C35 . 97.13(12) yes Al2 . Mo1 . C37 . 87.39(8) yes C33 . Mo1 . C37 . 86.46(12) yes C35 . Mo1 . C37 . 88.02(12) yes Al2 . Mo1 . C39 . 97.60(10) yes C33 . Mo1 . C39 . 91.61(12) yes C35 . Mo1 . C39 . 87.29(13) yes C37 . Mo1 . C39 . 174.66(13) yes Al2 . Mo1 . H23 . 41.0(11) no C33 . Mo1 . H23 . 91.0(11) no C35 . Mo1 . H23 . 171.9(11) no C37 . Mo1 . H23 . 92.1(11) no C39 . Mo1 . H23 . 92.9(11) no Al2 . Mo1 . H22 . 40.9(11) no C33 . Mo1 . H22 . 172.1(11) no C35 . Mo1 . H22 . 90.6(11) no C37 . Mo1 . H22 . 92.4(11) no C39 . Mo1 . H22 . 90.2(11) no H23 . Mo1 . H22 . 81.3(15) no Mo1 . Al2 . C3 . 124.00(8) yes Mo1 . Al2 . H23 . 46.3(12) no C3 . Al2 . H23 . 109.1(12) no Mo1 . Al2 . H21 . 122.7(15) no C3 . Al2 . H21 . 113.3(15) no H23 . Al2 . H21 . 116.6(19) no Mo1 . Al2 . H22 . 45.8(12) no C3 . Al2 . H22 . 108.5(12) no H23 . Al2 . H22 . 91.3(17) no H21 . Al2 . H22 . 116.0(19) no Al2 . C3 . N4 . 119.60(19) yes Al2 . C3 . N20 . 120.50(19) yes N4 . C3 . N20 . 119.9(2) yes C3 . N4 . C5 . 119.8(2) yes C3 . N4 . C17 . 123.1(2) yes C5 . N4 . C17 . 117.1(2) yes N4 . C5 . C6 . 118.5(2) yes N4 . C5 . C10 . 119.1(2) yes C6 . C5 . C10 . 122.3(3) yes C5 . C6 . C7 . 117.2(3) yes C5 . C6 . C14 . 123.8(3) yes C7 . C6 . C14 . 118.9(3) yes C6 . C7 . C8 . 121.6(3) yes C6 . C7 . H71 . 119.4 no C8 . C7 . H71 . 119.0 no C7 . C8 . C9 . 120.1(3) yes C7 . C8 . H81 . 120.1 no C9 . C8 . H81 . 119.9 no C8 . C9 . C10 . 121.6(3) yes C8 . C9 . H91 . 120.0 no C10 . C9 . H91 . 118.4 no C5 . C10 . C9 . 117.2(3) yes C5 . C10 . C11 . 123.5(3) yes C9 . C10 . C11 . 119.2(3) yes C10 . C11 . C12 . 109.8(3) yes C10 . C11 . C13 . 113.0(4) yes C12 . C11 . C13 . 109.8(3) yes C10 . C11 . H111 . 108.2 no C12 . C11 . H111 . 107.6 no C13 . C11 . H111 . 108.3 no C11 . C12 . H121 . 110.0 no C11 . C12 . H122 . 110.4 no H121 . C12 . H122 . 108.2 no C11 . C12 . H123 . 111.2 no H121 . C12 . H123 . 108.3 no H122 . C12 . H123 . 108.8 no C11 . C13 . H131 . 109.1 no C11 . C13 . H132 . 109.7 no H131 . C13 . H132 . 108.6 no C11 . C13 . H133 . 109.8 no H131 . C13 . H133 . 110.5 no H132 . C13 . H133 . 109.1 no C6 . C14 . C15 . 109.8(3) yes C6 . C14 . C16 . 112.3(3) yes C15 . C14 . C16 . 108.5(3) yes C6 . C14 . H141 . 109.1 no C15 . C14 . H141 . 108.7 no C16 . C14 . H141 . 108.3 no C14 . C15 . H151 . 110.8 no C14 . C15 . H153 . 109.0 no H151 . C15 . H153 . 108.8 no C14 . C15 . H152 . 110.3 no H151 . C15 . H152 . 108.7 no H153 . C15 . H152 . 109.2 no C14 . C16 . H161 . 109.9 no C14 . C16 . H163 . 109.7 no H161 . C16 . H163 . 108.3 no C14 . C16 . H162 . 111.0 no H161 . C16 . H162 . 109.1 no H163 . C16 . H162 . 108.7 no N4 . C17 . C18 . 108.9(2) yes N4 . C17 . H171 . 109.7 no C18 . C17 . H171 . 111.0 no N4 . C17 . H172 . 107.9 no C18 . C17 . H172 . 109.4 no H171 . C17 . H172 . 109.9 no C17 . C18 . C19 . 108.4(3) yes C17 . C18 . H181 . 109.6 no C19 . C18 . H181 . 110.5 no C17 . C18 . H182 . 110.5 no C19 . C18 . H182 . 109.6 no H181 . C18 . H182 . 108.3 no C18 . C19 . N20 . 108.4(2) yes C18 . C19 . H192 . 110.3 no N20 . C19 . H192 . 110.0 no C18 . C19 . H191 . 109.7 no N20 . C19 . H191 . 109.1 no H192 . C19 . H191 . 109.3 no C19 . N20 . C3 . 122.8(2) yes C19 . N20 . C21 . 116.9(2) yes C3 . N20 . C21 . 119.9(2) yes N20 . C21 . C22 . 118.7(2) yes N20 . C21 . C29 . 118.9(2) yes C22 . C21 . C29 . 122.3(3) yes C21 . C22 . C23 . 123.9(3) yes C21 . C22 . C26 . 117.2(3) yes C23 . C22 . C26 . 119.0(3) yes C22 . C23 . C24 . 111.0(3) yes C22 . C23 . C25 . 112.6(3) yes C24 . C23 . C25 . 108.2(3) yes C22 . C23 . H231 . 108.2 no C24 . C23 . H231 . 108.4 no C25 . C23 . H231 . 108.4 no C23 . C24 . H242 . 109.2 no C23 . C24 . H241 . 111.1 no H242 . C24 . H241 . 109.1 no C23 . C24 . H243 . 109.6 no H242 . C24 . H243 . 109.4 no H241 . C24 . H243 . 108.4 no C23 . C25 . H252 . 109.9 no C23 . C25 . H251 . 110.6 no H252 . C25 . H251 . 109.1 no C23 . C25 . H253 . 109.4 no H252 . C25 . H253 . 108.5 no H251 . C25 . H253 . 109.2 no C22 . C26 . C27 . 121.2(3) yes C22 . C26 . H261 . 119.0 no C27 . C26 . H261 . 119.8 no C26 . C27 . C28 . 120.3(3) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 120.4 no C27 . C28 . C29 . 121.3(3) yes C27 . C28 . H281 . 119.6 no C29 . C28 . H281 . 119.1 no C21 . C29 . C28 . 117.5(3) yes C21 . C29 . C30 . 123.1(3) yes C28 . C29 . C30 . 119.3(3) yes C29 . C30 . C31 . 110.6(3) yes C29 . C30 . C32 . 112.8(3) yes C31 . C30 . C32 . 109.4(3) yes C29 . C30 . H301 . 108.4 no C31 . C30 . H301 . 107.7 no C32 . C30 . H301 . 107.8 no C30 . C31 . H311 . 109.5 no C30 . C31 . H312 . 111.0 no H311 . C31 . H312 . 109.0 no C30 . C31 . H313 . 109.9 no H311 . C31 . H313 . 108.6 no H312 . C31 . H313 . 108.8 no C30 . C32 . H321 . 109.7 no C30 . C32 . H322 . 110.2 no H321 . C32 . H322 . 108.7 no C30 . C32 . H323 . 111.0 no H321 . C32 . H323 . 108.0 no H322 . C32 . H323 . 109.2 no Mo1 . C33 . O34 . 176.0(2) yes Mo1 . C35 . O36 . 176.2(3) yes Mo1 . C37 . O38 . 174.9(3) yes Mo1 . C39 . O40 . 175.8(3) yes F41 . C42 . C43 . 120.8(4) yes F41 . C42 . C47 . 118.5(4) yes C43 . C42 . C47 . 120.7(4) yes C42 . C43 . C44 . 118.9(5) yes C42 . C43 . H431 . 120.9 no C44 . C43 . H431 . 120.2 no C43 . C44 . C45 . 120.2(5) yes C43 . C44 . H441 . 120.5 no C45 . C44 . H441 . 119.3 no C44 . C45 . C46 . 120.4(5) yes C44 . C45 . H451 . 119.9 no C46 . C45 . H451 . 119.7 no C45 . C46 . C47 . 119.2(5) yes C45 . C46 . H461 . 120.5 no C47 . C46 . H461 . 120.3 no C46 . C47 . C42 . 120.6(5) yes C46 . C47 . F48 . 121.6(4) yes C42 . C47 . F48 . 117.8(4) yes Mo1 . H23 . Al2 . 92.6(16) no Mo1 . H22 . Al2 . 93.3(16) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C30 . H301 . C3 . 129 0.98 2.60 3.302(5) yes C46 . H461 . O38 . 153 0.94 2.47 3.330(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 25/03/13 at 17:39:57 # #LIST 12 BLOCK SCALE X'S, U'S H(21, X'S) H(22, X'S) H(23, X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 153,X'S) H ( 152,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 163,X'S) H ( 162,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) RIDE C ( 19,X'S) H ( 192,X'S) H ( 191,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 242,X'S) H ( 241,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 252,X'S) H ( 251,X'S) H ( 253,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) H ( 313,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/03/13 at 17:39:57 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 931228' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4a _audit_creation_date 13-03-25 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 072janp12 _chemical_name_systematic . _chemical_melting_point . _refine_special_details ; The difference map indicated the presence of diffuse electron density believed to be disordered difluorobenzene. SQUEEZE was used leaving a void from which the electron density was removed. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.001 1165 151 ' ' 2 0.500 0.500 0.784 1165 151 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _cell_length_a 29.5361(2) _cell_length_b 19.9130(2) _cell_length_c 26.0448(2) _cell_angle_alpha 90 _cell_angle_beta 124.3299(4) _cell_angle_gamma 90 _cell_volume 12649.92(19) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C224 H264 Al8 F8 Mo8 N16 O24 # Dc = 2.47 Fooo = 4848.00 Mu = 9.51 M = 2350.01 # Found Formula = C112 H132 Al4 F4 Mo4 N8 O12 # Dc = 1.23 FOOO = 4848.00 Mu = 4.76 M = 1175.00 _chemical_formula_sum 'C119.8 H1137.2 Al4 F6.6 Mo4 N8 O12' _chemical_formula_moiety 'C100 H124 Al4 Mo4 N8 O12, 3.3(C6 H4 F2)' _chemical_compound_source . _chemical_formula_weight 2498.33 _cell_measurement_reflns_used 14763 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.240 _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5149.602 _exptl_absorpt_coefficient_mu 0.483 # Sheldrick geometric approximatio 0.91 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.93 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 122049 _reflns_number_total 14393 _diffrn_reflns_av_R_equivalents 0.047 # Number of reflections without Friedels Law is 14393 # Number of reflections with Friedels Law is 14393 # Theoretical number of reflections is about 14519 _diffrn_reflns_theta_min 5.110 _diffrn_reflns_theta_max 27.492 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.943 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _reflns_limit_h_min -38 _reflns_limit_h_max 31 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 33 _oxford_diffrn_Wilson_B_factor 2.03 _oxford_diffrn_Wilson_scale 772.41 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.16 _refine_diff_density_max 2.53 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 14392 _refine_ls_number_restraints 0 _refine_ls_number_parameters 664 _oxford_refine_ls_R_factor_ref 0.0950 _refine_ls_wR_factor_ref 0.1758 _refine_ls_goodness_of_fit_ref 0.9861 _refine_ls_shift/su_max 0.0014180 _refine_ls_shift/su_mean 0.0000151 # The values computed from all data _oxford_reflns_number_all 14393 _refine_ls_R_factor_all 0.0951 _refine_ls_wR_factor_all 0.1759 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9525 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_gt 0.1360 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 12.8 19.2 9.32 2.40 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mo1 Mo -0.085939(15) 0.43420(2) -0.105644(17) 0.0223 1.0000 Uani . . . . . . Al2 Al -0.10083(6) 0.48821(7) -0.01683(6) 0.0237 1.0000 Uani . . . . . . H22 H -0.088(2) 0.416(3) -0.036(3) 0.0387 1.0000 Uiso . . . . . . Mo3 Mo -0.167499(16) 0.56276(2) -0.121695(18) 0.0251 1.0000 Uani . . . . . . H21 H -0.162(2) 0.518(3) -0.061(3) 0.0296 1.0000 Uiso . . . . . . Al4 Al -0.20414(6) 0.45193(8) -0.20730(7) 0.0303 1.0000 Uani . . . . . . H43 H -0.219(3) 0.500(3) -0.170(3) 0.0414 1.0000 Uiso . . . . . . H41 H -0.160(2) 0.396(3) -0.164(3) 0.0318 1.0000 Uiso . . . . . . C5 C -0.27318(19) 0.3882(2) -0.2604(2) 0.0258 1.0000 Uani . . . . . . N6 N -0.26890(17) 0.3389(2) -0.2929(2) 0.0298 1.0000 Uani . . . . . . C7 C -0.3148(2) 0.2951(3) -0.3387(3) 0.0439 1.0000 Uani . . . . . . C8 C -0.3591(3) 0.2927(4) -0.3268(4) 0.0633 1.0000 Uani . . . . . . C9 C -0.3735(2) 0.3641(3) -0.3217(3) 0.0477 1.0000 Uani . . . . . . N10 N -0.32316(18) 0.3999(2) -0.2729(2) 0.0326 1.0000 Uani . . . . . . C11 C -0.3324(2) 0.4480(3) -0.2383(2) 0.0316 1.0000 Uani . . . . . . C12 C -0.3426(2) 0.5150(3) -0.2566(3) 0.0365 1.0000 Uani . . . . . . C13 C -0.3392(3) 0.5408(4) -0.3089(4) 0.0543 1.0000 Uani . . . . . . H133 H -0.3637 0.5779 -0.3293 0.0811 1.0000 Uiso R . . . . . H131 H -0.3500 0.5056 -0.3391 0.0810 1.0000 Uiso R . . . . . H132 H -0.3026 0.5545 -0.2936 0.0811 1.0000 Uiso R . . . . . C14 C -0.3560(2) 0.5581(3) -0.2249(3) 0.0474 1.0000 Uani . . . . . . C15 C -0.3595(3) 0.5359(4) -0.1768(3) 0.0573 1.0000 Uani . . . . . . C16 C -0.3753(3) 0.5839(6) -0.1439(4) 0.0890 1.0000 Uani . . . . . . H162 H -0.3712 0.5620 -0.1084 0.1340 1.0000 Uiso R . . . . . H163 H -0.4132 0.5974 -0.1720 0.1340 1.0000 Uiso R . . . . . H161 H -0.3523 0.6229 -0.1303 0.1342 1.0000 Uiso R . . . . . C17 C -0.3493(3) 0.4700(4) -0.1603(3) 0.0559 1.0000 Uani . . . . . . C18 C -0.3354(2) 0.4247(3) -0.1900(3) 0.0427 1.0000 Uani . . . . . . C19 C -0.3247(4) 0.3515(4) -0.1718(4) 0.0673 1.0000 Uani . . . . . . H192 H -0.3178 0.3466 -0.1314 0.1010 1.0000 Uiso R . . . . . H193 H -0.3561 0.3251 -0.2013 0.1009 1.0000 Uiso R . . . . . H191 H -0.2929 0.3366 -0.1706 0.1010 1.0000 Uiso R . . . . . H171 H -0.3519 0.4548 -0.1282 0.0669 1.0000 Uiso R . . . . . H141 H -0.3631 0.6032 -0.2365 0.0571 1.0000 Uiso R . . . . . H92 H -0.3998 0.3632 -0.3102 0.0582 1.0000 Uiso R . . . . . H91 H -0.3895 0.3869 -0.3610 0.0581 1.0000 Uiso R . . . . . H82 H -0.3912 0.2698 -0.3611 0.0760 1.0000 Uiso R . . . . . H81 H -0.3456 0.2688 -0.2879 0.0762 1.0000 Uiso R . . . . . H71 H -0.3013 0.2507 -0.3352 0.0533 1.0000 Uiso R . . . . . H72 H -0.3298 0.3118 -0.3799 0.0533 1.0000 Uiso R . . . . . C20 C -0.2175(2) 0.3229(3) -0.2841(2) 0.0307 1.0000 Uani . . . . . . C21 C -0.1844(2) 0.2741(3) -0.2401(2) 0.0326 1.0000 Uani . . . . . . C22 C -0.1993(3) 0.2430(3) -0.1985(3) 0.0430 1.0000 Uani . . . . . . H221 H -0.1711 0.2115 -0.1703 0.0649 1.0000 Uiso R . . . . . H222 H -0.2334 0.2189 -0.2229 0.0651 1.0000 Uiso R . . . . . H223 H -0.2026 0.2766 -0.1747 0.0649 1.0000 Uiso R . . . . . C23 C -0.1367(2) 0.2555(3) -0.2348(3) 0.0374 1.0000 Uani . . . . . . C24 C -0.1226(2) 0.2822(3) -0.2733(3) 0.0404 1.0000 Uani . . . . . . C25 C -0.0702(3) 0.2610(4) -0.2667(4) 0.0574 1.0000 Uani . . . . . . H253 H -0.0751 0.2631 -0.3063 0.0861 1.0000 Uiso R . . . . . H252 H -0.0611 0.2160 -0.2514 0.0862 1.0000 Uiso R . . . . . H251 H -0.0406 0.2898 -0.2380 0.0862 1.0000 Uiso R . . . . . C26 C -0.1574(3) 0.3284(3) -0.3181(3) 0.0445 1.0000 Uani . . . . . . C27 C -0.2054(2) 0.3497(3) -0.3244(3) 0.0366 1.0000 Uani . . . . . . C28 C -0.2428(3) 0.3995(3) -0.3748(3) 0.0473 1.0000 Uani . . . . . . H283 H -0.2476 0.3869 -0.4133 0.0713 1.0000 Uiso R . . . . . H282 H -0.2776 0.3996 -0.3801 0.0713 1.0000 Uiso R . . . . . H281 H -0.2268 0.4434 -0.3627 0.0711 1.0000 Uiso R . . . . . H261 H -0.1492 0.3457 -0.3451 0.0540 1.0000 Uiso R . . . . . H231 H -0.1136 0.2246 -0.2049 0.0452 1.0000 Uiso R . . . . . H42 H -0.2033 0.4775 -0.2660 0.0445 1.0000 Uiso R . . . . . H23 H -0.100(3) 0.521(4) -0.090(3) 0.0642 1.0000 Uiso . . . . . . C29 C -0.1676(2) 0.6045(3) -0.1899(2) 0.0359 1.0000 Uani . . . . . . O30 O -0.1648(2) 0.6308(2) -0.2279(2) 0.0523 1.0000 Uani . . . . . . C31 C -0.1197(2) 0.6386(3) -0.0704(2) 0.0327 1.0000 Uani . . . . . . O32 O -0.09512(17) 0.6860(2) -0.04546(19) 0.0434 1.0000 Uani . . . . . . C33 C -0.2286(2) 0.6215(3) -0.1387(2) 0.0346 1.0000 Uani . . . . . . O34 O -0.26066(17) 0.6608(2) -0.1466(2) 0.0463 1.0000 Uani . . . . . . O35 O -0.03724(13) 0.53346(18) 0.03694(16) 0.0308 1.0000 Uani . . . . . . C36 C 0.0114(2) 0.5425(2) 0.0596(2) 0.0250 1.0000 Uani . . . . . . C37 C -0.10414(19) 0.4547(3) 0.0587(2) 0.0271 1.0000 Uani . . . . . . N38 N -0.11850(18) 0.4974(2) 0.08704(19) 0.0301 1.0000 Uani . . . . . . C39 C -0.1356(2) 0.5646(3) 0.0648(2) 0.0299 1.0000 Uani . . . . . . C40 C -0.0970(2) 0.6169(3) 0.0916(3) 0.0356 1.0000 Uani . . . . . . C41 C -0.0389(3) 0.6040(4) 0.1456(3) 0.0478 1.0000 Uani . . . . . . H411 H -0.0140 0.6360 0.1461 0.0719 1.0000 Uiso R . . . . . H412 H -0.0367 0.6081 0.1835 0.0718 1.0000 Uiso R . . . . . H413 H -0.0275 0.5597 0.1431 0.0719 1.0000 Uiso R . . . . . C42 C -0.1148(3) 0.6812(3) 0.0678(3) 0.0489 1.0000 Uani . . . . . . C43 C -0.1690(3) 0.6953(3) 0.0216(3) 0.0510 1.0000 Uani . . . . . . C44 C -0.2068(3) 0.6430(3) -0.0010(3) 0.0480 1.0000 Uani . . . . . . C45 C -0.1913(2) 0.5771(3) 0.0193(3) 0.0372 1.0000 Uani . . . . . . C46 C -0.2330(2) 0.5222(4) -0.0077(3) 0.0465 1.0000 Uani . . . . . . H461 H -0.2665 0.5385 -0.0144 0.0701 1.0000 Uiso R . . . . . H463 H -0.2203 0.4843 0.0200 0.0702 1.0000 Uiso R . . . . . H462 H -0.2401 0.5089 -0.0470 0.0703 1.0000 Uiso R . . . . . H441 H -0.2437 0.6522 -0.0307 0.0579 1.0000 Uiso R . . . . . C47 C -0.1866(5) 0.7646(4) -0.0055(5) 0.0834 1.0000 Uani . . . . . . H471 H -0.2253 0.7695 -0.0257 0.1251 1.0000 Uiso R . . . . . H473 H -0.1676 0.7972 0.0272 0.1250 1.0000 Uiso R . . . . . H472 H -0.1772 0.7717 -0.0350 0.1250 1.0000 Uiso R . . . . . H421 H -0.0895 0.7160 0.0834 0.0589 1.0000 Uiso R . . . . . C48 C -0.1182(3) 0.4800(3) 0.1427(3) 0.0436 1.0000 Uani . . . . . . C49 C -0.0763(3) 0.4270(3) 0.1797(3) 0.0530 1.0000 Uani . . . . . . C50 C -0.0857(3) 0.3689(3) 0.1381(3) 0.0468 1.0000 Uani . . . . . . N51 N -0.08904(18) 0.3930(2) 0.0818(2) 0.0321 1.0000 Uani . . . . . . C52 C -0.0809(2) 0.3400(3) 0.0502(2) 0.0303 1.0000 Uani . . . . . . C53 C -0.1271(2) 0.3081(3) 0.0006(3) 0.0346 1.0000 Uani . . . . . . C54 C -0.1190(3) 0.2524(3) -0.0256(3) 0.0385 1.0000 Uani . . . . . . C55 C -0.0675(3) 0.2293(3) -0.0047(3) 0.0444 1.0000 Uani . . . . . . C56 C -0.0224(3) 0.2633(3) 0.0432(3) 0.0452 1.0000 Uani . . . . . . C57 C -0.0278(2) 0.3195(3) 0.0722(3) 0.0360 1.0000 Uani . . . . . . C58 C 0.0219(3) 0.3564(4) 0.1229(3) 0.0548 1.0000 Uani . . . . . . H583 H 0.0508 0.3252 0.1481 0.0821 1.0000 Uiso R . . . . . H581 H 0.0136 0.3806 0.1485 0.0820 1.0000 Uiso R . . . . . H582 H 0.0339 0.3878 0.1049 0.0820 1.0000 Uiso R . . . . . H561 H 0.0127 0.2484 0.0568 0.0539 1.0000 Uiso R . . . . . C59 C -0.0608(4) 0.1676(4) -0.0343(4) 0.0623 1.0000 Uani . . . . . . H593 H -0.0271 0.1461 -0.0045 0.0939 1.0000 Uiso R . . . . . H592 H -0.0903 0.1368 -0.0479 0.0940 1.0000 Uiso R . . . . . H591 H -0.0596 0.1805 -0.0690 0.0939 1.0000 Uiso R . . . . . H541 H -0.1494 0.2300 -0.0582 0.0459 1.0000 Uiso R . . . . . C60 C -0.1839(2) 0.3357(3) -0.0275(3) 0.0473 1.0000 Uani . . . . . . H601 H -0.2101 0.3035 -0.0559 0.0711 1.0000 Uiso R . . . . . H602 H -0.1895 0.3445 0.0046 0.0709 1.0000 Uiso R . . . . . H603 H -0.1881 0.3768 -0.0491 0.0708 1.0000 Uiso R . . . . . H501 H -0.1194 0.3461 0.1254 0.0560 1.0000 Uiso R . . . . . H502 H -0.0554 0.3376 0.1605 0.0560 1.0000 Uiso R . . . . . H491 H -0.0791 0.4130 0.2132 0.0639 1.0000 Uiso R . . . . . H492 H -0.0404 0.4454 0.1968 0.0638 1.0000 Uiso R . . . . . H481 H -0.1539 0.4637 0.1298 0.0521 1.0000 Uiso R . . . . . H482 H -0.1086 0.5197 0.1686 0.0519 1.0000 Uiso R . . . . . C61 C -0.0853(2) 0.4604(3) -0.1789(2) 0.0320 1.0000 Uani . . . . . . O62 O -0.08185(18) 0.4780(3) -0.21869(19) 0.0489 1.0000 Uani . . . . . . C63 C -0.0570(2) 0.3431(3) -0.1029(2) 0.0325 1.0000 Uani . . . . . . O64 O -0.03550(17) 0.2931(2) -0.0989(2) 0.0437 1.0000 Uani . . . . . . F65 F 0.1342(2) 0.9212(3) -0.0363(3) 0.0942 1.0000 Uani . . . . . . C66 C 0.1793(3) 0.8992(4) 0.0161(3) 0.0537 1.0000 Uani . . . . . . C67 C 0.2085(3) 0.8460(4) 0.0152(3) 0.0532 1.0000 Uani . . . . . . F68 F 0.1901(2) 0.8149(3) -0.0383(2) 0.0872 1.0000 Uani . . . . . . C69 C 0.2551(3) 0.8242(3) 0.0690(3) 0.0498 1.0000 Uani . . . . . . C70 C 0.2720(3) 0.8550(3) 0.1244(3) 0.0476 1.0000 Uani . . . . . . C71 C 0.2433(3) 0.9079(4) 0.1258(3) 0.0546 1.0000 Uani . . . . . . C72 C 0.1962(3) 0.9309(4) 0.0717(4) 0.0572 1.0000 Uani . . . . . . H721 H 0.1751 0.9683 0.0718 0.0682 1.0000 Uiso R . . . . . H711 H 0.2551 0.9286 0.1636 0.0659 1.0000 Uiso R . . . . . H701 H 0.3033 0.8400 0.1611 0.0570 1.0000 Uiso R . . . . . H691 H 0.2761 0.7870 0.0682 0.0586 1.0000 Uiso 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 0.02190(19) 0.02398(19) 0.02060(18) -0.00057(15) 0.01176(15) -0.00128(15) Al2 0.0237(7) 0.0256(7) 0.0219(6) -0.0009(5) 0.0129(6) -0.0007(5) Mo3 0.0244(2) 0.0249(2) 0.0226(2) 0.00071(16) 0.01106(16) 0.00079(16) Al4 0.0280(7) 0.0327(8) 0.0277(7) -0.0002(6) 0.0142(6) -0.0010(6) C5 0.026(2) 0.026(2) 0.025(2) 0.0001(18) 0.0144(19) -0.0023(18) N6 0.026(2) 0.029(2) 0.033(2) -0.0070(17) 0.0153(18) -0.0054(16) C7 0.034(3) 0.043(3) 0.044(3) -0.017(3) 0.015(3) -0.010(2) C8 0.044(4) 0.053(4) 0.084(5) -0.027(4) 0.030(4) -0.018(3) C9 0.024(3) 0.051(4) 0.056(4) -0.021(3) 0.015(3) -0.012(2) N10 0.030(2) 0.031(2) 0.035(2) -0.0046(18) 0.0175(19) -0.0041(17) C11 0.022(2) 0.039(3) 0.034(3) -0.003(2) 0.015(2) 0.0001(19) C12 0.025(2) 0.040(3) 0.039(3) 0.001(2) 0.015(2) 0.001(2) C13 0.052(4) 0.048(4) 0.066(4) 0.018(3) 0.036(4) 0.007(3) C14 0.030(3) 0.046(3) 0.053(4) -0.007(3) 0.015(3) 0.007(2) C15 0.034(3) 0.081(5) 0.050(4) -0.016(4) 0.020(3) 0.011(3) C16 0.060(5) 0.136(9) 0.058(5) -0.030(5) 0.025(4) 0.038(5) C17 0.040(3) 0.097(6) 0.032(3) 0.002(3) 0.022(3) 0.009(4) C18 0.036(3) 0.056(4) 0.034(3) 0.006(3) 0.019(2) 0.003(3) C19 0.069(5) 0.076(5) 0.055(4) 0.030(4) 0.034(4) 0.013(4) C20 0.032(2) 0.032(3) 0.028(2) -0.009(2) 0.016(2) -0.006(2) C21 0.034(3) 0.030(3) 0.030(3) -0.005(2) 0.016(2) -0.004(2) C22 0.050(3) 0.042(3) 0.041(3) 0.007(3) 0.028(3) 0.004(3) C23 0.037(3) 0.033(3) 0.038(3) -0.004(2) 0.018(2) 0.001(2) C24 0.034(3) 0.039(3) 0.053(3) -0.014(3) 0.028(3) -0.009(2) C25 0.046(4) 0.062(4) 0.076(5) -0.011(4) 0.041(4) 0.002(3) C26 0.053(4) 0.040(3) 0.057(4) -0.008(3) 0.041(3) -0.005(3) C27 0.042(3) 0.035(3) 0.038(3) -0.002(2) 0.025(3) -0.004(2) C28 0.056(4) 0.046(3) 0.041(3) 0.004(3) 0.028(3) -0.003(3) C29 0.037(3) 0.034(3) 0.029(3) -0.003(2) 0.014(2) -0.004(2) O30 0.068(3) 0.051(3) 0.035(2) 0.0060(19) 0.027(2) -0.012(2) C31 0.031(3) 0.034(3) 0.033(3) 0.003(2) 0.018(2) 0.002(2) O32 0.047(2) 0.037(2) 0.042(2) -0.0115(18) 0.0232(19) -0.0132(18) C33 0.034(3) 0.033(3) 0.034(3) 0.003(2) 0.016(2) 0.000(2) O34 0.039(2) 0.042(2) 0.054(3) 0.0066(19) 0.024(2) 0.0144(18) O35 0.0214(16) 0.0373(19) 0.0299(18) -0.0066(15) 0.0122(14) -0.0056(14) C36 0.031(2) 0.027(2) 0.019(2) 0.0011(17) 0.0148(19) 0.0010(18) C37 0.024(2) 0.034(2) 0.024(2) 0.0024(18) 0.0137(19) -0.0021(18) N38 0.034(2) 0.036(2) 0.026(2) 0.0010(17) 0.0204(18) 0.0024(18) C39 0.032(2) 0.034(3) 0.028(2) -0.002(2) 0.020(2) 0.001(2) C40 0.043(3) 0.040(3) 0.035(3) -0.004(2) 0.029(3) -0.004(2) C41 0.043(3) 0.060(4) 0.046(3) -0.019(3) 0.028(3) -0.012(3) C42 0.078(5) 0.034(3) 0.063(4) -0.005(3) 0.057(4) -0.003(3) C43 0.078(5) 0.044(3) 0.059(4) 0.015(3) 0.056(4) 0.023(3) C44 0.055(4) 0.054(4) 0.047(3) 0.012(3) 0.035(3) 0.023(3) C45 0.034(3) 0.050(3) 0.035(3) -0.001(2) 0.024(2) 0.005(2) C46 0.031(3) 0.067(4) 0.041(3) -0.009(3) 0.020(3) -0.006(3) C47 0.141(9) 0.052(5) 0.108(7) 0.031(5) 0.101(7) 0.041(5) C48 0.062(4) 0.045(3) 0.035(3) 0.002(2) 0.034(3) 0.005(3) C49 0.075(5) 0.057(4) 0.031(3) 0.009(3) 0.032(3) 0.010(3) C50 0.068(4) 0.049(4) 0.036(3) 0.013(3) 0.037(3) 0.011(3) N51 0.035(2) 0.034(2) 0.029(2) 0.0029(18) 0.0192(19) 0.0055(18) C52 0.033(3) 0.030(2) 0.033(3) 0.004(2) 0.021(2) 0.002(2) C53 0.037(3) 0.037(3) 0.036(3) 0.006(2) 0.025(2) -0.002(2) C54 0.047(3) 0.032(3) 0.042(3) -0.001(2) 0.028(3) -0.008(2) C55 0.061(4) 0.034(3) 0.056(4) 0.003(3) 0.043(3) 0.001(3) C56 0.046(3) 0.043(3) 0.056(4) 0.011(3) 0.034(3) 0.017(3) C57 0.032(3) 0.036(3) 0.039(3) 0.009(2) 0.020(2) 0.006(2) C58 0.033(3) 0.059(4) 0.051(4) -0.002(3) 0.010(3) 0.004(3) C59 0.084(5) 0.041(4) 0.085(5) -0.002(3) 0.062(5) 0.006(3) C60 0.037(3) 0.046(3) 0.057(4) -0.004(3) 0.025(3) -0.006(3) C61 0.028(2) 0.037(3) 0.027(2) 0.002(2) 0.014(2) 0.000(2) O62 0.046(2) 0.071(3) 0.034(2) 0.014(2) 0.0253(19) 0.004(2) C63 0.033(3) 0.030(3) 0.030(3) -0.004(2) 0.015(2) -0.006(2) O64 0.046(2) 0.030(2) 0.050(2) -0.0005(17) 0.024(2) 0.0080(17) F65 0.092(4) 0.117(5) 0.066(3) 0.010(3) 0.041(3) 0.007(3) C66 0.055(4) 0.061(4) 0.049(4) 0.003(3) 0.031(3) -0.007(3) C67 0.065(4) 0.067(4) 0.043(3) -0.016(3) 0.040(3) -0.020(4) F68 0.104(4) 0.111(4) 0.059(3) -0.021(3) 0.053(3) -0.010(3) C69 0.065(4) 0.049(4) 0.058(4) -0.009(3) 0.048(4) -0.015(3) C70 0.054(4) 0.051(4) 0.043(3) -0.009(3) 0.031(3) -0.013(3) C71 0.067(4) 0.056(4) 0.050(4) -0.017(3) 0.038(4) -0.017(3) C72 0.067(4) 0.046(4) 0.073(5) -0.007(3) 0.049(4) -0.010(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.043051(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . C36 2_565 1.877(5) yes Mo1 . Al2 . 2.8015(14) yes Mo1 . H22 . 1.88(6) no Mo1 . Mo3 . 3.3758(5) yes Mo1 . Al4 . 2.9829(16) yes Mo1 . H41 . 1.98(6) no Mo1 . H23 . 1.87(8) no Mo1 . C61 . 1.988(5) yes Mo1 . C63 . 1.989(5) yes Al2 . H22 . 1.64(6) no Al2 . Mo3 . 2.7340(14) yes Al2 . H21 . 1.62(6) no Al2 . H23 . 2.02(7) no Al2 . O35 . 1.826(4) yes Al2 . C37 . 2.132(5) yes Mo3 . H21 . 1.75(5) no Mo3 . Al4 . 2.8794(16) yes Mo3 . H43 . 1.82(6) no Mo3 . H23 . 1.87(7) no Mo3 . C29 . 1.959(6) yes Mo3 . C31 . 1.982(5) yes Mo3 . C33 . 1.978(6) yes Al4 . H43 . 1.58(6) no Al4 . H41 . 1.61(6) no Al4 . C5 . 2.121(5) yes Al4 . H42 . 1.625 no C5 . N6 . 1.348(6) yes C5 . N10 . 1.341(6) yes N6 . C7 . 1.483(6) yes N6 . C20 . 1.439(7) yes C7 . C8 . 1.507(10) yes C7 . H71 . 0.954 no C7 . H72 . 0.961 no C8 . C9 . 1.512(10) yes C8 . H82 . 0.975 no C8 . H81 . 0.978 no C9 . N10 . 1.483(7) yes C9 . H92 . 0.976 no C9 . H91 . 0.966 no N10 . C11 . 1.442(7) yes C11 . C12 . 1.392(8) yes C11 . C18 . 1.393(8) yes C12 . C13 . 1.510(9) yes C12 . C14 . 1.394(8) yes C13 . H133 . 0.960 no C13 . H131 . 0.962 no C13 . H132 . 0.957 no C14 . C15 . 1.386(11) yes C14 . H141 . 0.933 no C15 . C16 . 1.522(9) yes C15 . C17 . 1.362(11) yes C16 . H162 . 0.968 no C16 . H163 . 0.968 no C16 . H161 . 0.958 no C17 . C18 . 1.391(9) yes C17 . H171 . 0.930 no C18 . C19 . 1.510(10) yes C19 . H192 . 0.957 no C19 . H193 . 0.961 no C19 . H191 . 0.968 no C20 . C21 . 1.397(7) yes C20 . C27 . 1.391(7) yes C21 . C22 . 1.513(8) yes C21 . C23 . 1.386(8) yes C22 . H221 . 0.967 no C22 . H222 . 0.962 no C22 . H223 . 0.954 no C23 . C24 . 1.390(8) yes C23 . H231 . 0.924 no C24 . C25 . 1.515(8) yes C24 . C26 . 1.383(9) yes C25 . H253 . 0.958 no C25 . H252 . 0.955 no C25 . H251 . 0.956 no C26 . C27 . 1.398(8) yes C26 . H261 . 0.929 no C27 . C28 . 1.513(8) yes C28 . H283 . 0.963 no C28 . H282 . 0.956 no C28 . H281 . 0.958 no C29 . O30 . 1.165(7) yes C31 . O32 . 1.145(6) yes C33 . O34 . 1.156(7) yes O35 . C36 . 1.220(6) yes C37 . N38 . 1.342(6) yes C37 . N51 . 1.328(7) yes N38 . C39 . 1.433(7) yes N38 . C48 . 1.487(6) yes C39 . C40 . 1.404(8) yes C39 . C45 . 1.405(7) yes C40 . C41 . 1.506(8) yes C40 . C42 . 1.391(8) yes C41 . H411 . 0.968 no C41 . H412 . 0.956 no C41 . H413 . 0.960 no C42 . C43 . 1.383(10) yes C42 . H421 . 0.929 no C43 . C44 . 1.393(10) yes C43 . C47 . 1.503(9) yes C44 . C45 . 1.393(8) yes C44 . H441 . 0.931 no C45 . C46 . 1.493(8) yes C46 . H461 . 0.958 no C46 . H463 . 0.963 no C46 . H462 . 0.959 no C47 . H471 . 0.958 no C47 . H473 . 0.961 no C47 . H472 . 0.962 no C48 . C49 . 1.493(9) yes C48 . H481 . 0.963 no C48 . H482 . 0.972 no C49 . C50 . 1.499(9) yes C49 . H491 . 0.964 no C49 . H492 . 0.963 no C50 . N51 . 1.493(7) yes C50 . H501 . 0.966 no C50 . H502 . 0.970 no N51 . C52 . 1.438(6) yes C52 . C53 . 1.396(8) yes C52 . C57 . 1.395(7) yes C53 . C54 . 1.391(8) yes C53 . C60 . 1.505(8) yes C54 . C55 . 1.373(9) yes C54 . H541 . 0.931 no C55 . C56 . 1.385(9) yes C55 . C59 . 1.521(9) yes C56 . C57 . 1.407(8) yes C56 . H561 . 0.933 no C57 . C58 . 1.501(8) yes C58 . H583 . 0.956 no C58 . H581 . 0.959 no C58 . H582 . 0.961 no C59 . H593 . 0.953 no C59 . H592 . 0.956 no C59 . H591 . 0.959 no C60 . H601 . 0.955 no C60 . H602 . 0.956 no C60 . H603 . 0.961 no C61 . O62 . 1.152(6) yes C63 . O64 . 1.154(6) yes F65 . C66 . 1.334(9) yes C66 . C67 . 1.374(11) yes C66 . C72 . 1.390(10) yes C67 . F68 . 1.330(7) yes C67 . C69 . 1.368(10) yes C69 . C70 . 1.375(9) yes C69 . H691 . 0.975 no C70 . C71 . 1.367(10) yes C70 . H701 . 0.927 no C71 . C72 . 1.386(11) yes C71 . H711 . 0.934 no C72 . H721 . 0.970 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C36 2_565 Mo1 . Al2 . 92.96(14) yes C36 2_565 Mo1 . H22 . 95.5(18) no Al2 . Mo1 . H22 . 34.3(19) no C36 2_565 Mo1 . Mo3 . 112.94(15) yes Al2 . Mo1 . Mo3 . 51.52(3) yes H22 . Mo1 . Mo3 . 81.8(19) no C36 2_565 Mo1 . Al4 . 154.40(14) yes Al2 . Mo1 . Al4 . 92.13(4) yes H22 . Mo1 . Al4 . 102.7(18) no Mo3 . Mo1 . Al4 . 53.42(3) yes C36 2_565 Mo1 . H41 . 167.2(16) no Al2 . Mo1 . H41 . 99.1(16) no H22 . Mo1 . H41 . 92(2) no Mo3 . Mo1 . H41 . 78.2(17) no Al4 . Mo1 . H41 . 30.0(17) no C36 2_565 Mo1 . H23 . 88(2) no Al2 . Mo1 . H23 . 46(2) no H22 . Mo1 . H23 . 80(3) no Mo3 . Mo1 . H23 . 26(2) no Al4 . Mo1 . H23 . 78(2) no C36 2_565 Mo1 . C61 . 84.5(2) yes Al2 . Mo1 . C61 . 141.49(16) yes H22 . Mo1 . C61 . 175.8(19) no Mo3 . Mo1 . C61 . 94.28(16) yes Al4 . Mo1 . C61 . 75.96(15) yes C36 2_565 Mo1 . C63 . 82.9(2) yes Al2 . Mo1 . C63 . 125.76(16) yes H22 . Mo1 . C63 . 92.0(19) no Mo3 . Mo1 . C63 . 163.36(15) yes Al4 . Mo1 . C63 . 113.84(15) yes H41 . Mo1 . H23 . 104(3) no H41 . Mo1 . C61 . 88.6(16) no H23 . Mo1 . C61 . 95(2) no H41 . Mo1 . C63 . 86.6(17) no H23 . Mo1 . C63 . 167(2) no C61 . Mo1 . C63 . 92.2(2) yes Mo1 . Al2 . H22 . 40(2) no Mo1 . Al2 . Mo3 . 75.15(4) yes H22 . Al2 . Mo3 . 109(2) no Mo1 . Al2 . H21 . 101.2(19) no H22 . Al2 . H21 . 118(3) no Mo3 . Al2 . H21 . 37.5(19) no Mo1 . Al2 . H23 . 42(2) no H22 . Al2 . H23 . 82(3) no Mo3 . Al2 . H23 . 43(2) no H21 . Al2 . H23 . 80(3) no Mo1 . Al2 . O35 . 104.49(12) yes H22 . Al2 . O35 . 111(2) no Mo3 . Al2 . O35 . 110.37(13) yes H21 . Al2 . O35 . 128.4(20) no H23 . Al2 . O35 . 91(2) no Mo1 . Al2 . C37 . 138.76(15) yes H22 . Al2 . C37 . 99(2) no Mo3 . Al2 . C37 . 135.25(14) yes H21 . Al2 . C37 . 98.5(19) no H23 . Al2 . C37 . 178(2) no O35 . Al2 . C37 . 90.55(18) yes Mo1 . H22 . Al2 . 105(3) no Mo1 . Mo3 . Al2 . 53.34(3) yes Mo1 . Mo3 . H21 . 79.1(18) no Al2 . Mo3 . H21 . 34.2(18) no Mo1 . Mo3 . Al4 . 56.29(3) yes Al2 . Mo3 . Al4 . 95.84(4) yes H21 . Mo3 . Al4 . 96.5(18) no Mo1 . Mo3 . H43 . 79.8(20) no Al2 . Mo3 . H43 . 100.0(19) no H21 . Mo3 . H43 . 84(3) no Al4 . Mo3 . H43 . 29.7(19) no Mo1 . Mo3 . H23 . 26(2) no Al2 . Mo3 . H23 . 48(2) no H21 . Mo3 . H23 . 81(3) no Al4 . Mo3 . H23 . 81(2) no H43 . Mo3 . H23 . 105(3) no Mo1 . Mo3 . C29 . 93.98(17) yes Al2 . Mo3 . C29 . 140.13(17) yes H21 . Mo3 . C29 . 173.0(18) no Al4 . Mo3 . C29 . 79.35(16) yes H43 . Mo3 . C29 . 94.8(19) no Mo1 . Mo3 . C31 . 107.88(15) yes Al2 . Mo3 . C31 . 84.41(15) yes H21 . Mo3 . C31 . 96.5(18) no Al4 . Mo3 . C31 . 156.83(15) yes H43 . Mo3 . C31 . 172.3(20) no Mo1 . Mo3 . C33 . 166.54(16) yes Al2 . Mo3 . C33 . 126.65(16) yes H21 . Mo3 . C33 . 96.1(18) no Al4 . Mo3 . C33 . 112.46(16) yes H43 . Mo3 . C33 . 87.2(20) no H23 . Mo3 . C29 . 93(2) no H23 . Mo3 . C31 . 82(2) no C29 . Mo3 . C31 . 85.7(2) yes H23 . Mo3 . C33 . 167(2) no C29 . Mo3 . C33 . 90.7(2) yes C31 . Mo3 . C33 . 85.1(2) yes Mo3 . H21 . Al2 . 108(3) no Mo1 . Al4 . Mo3 . 70.29(4) yes Mo1 . Al4 . H43 . 97(2) no Mo3 . Al4 . H43 . 35(2) no Mo1 . Al4 . H41 . 38(2) no Mo3 . Al4 . H41 . 101(2) no H43 . Al4 . H41 . 113(3) no Mo1 . Al4 . C5 . 136.19(15) yes Mo3 . Al4 . C5 . 140.07(15) yes H43 . Al4 . C5 . 105(2) no H41 . Al4 . C5 . 98(2) no Mo1 . Al4 . H42 . 103.9 no Mo3 . Al4 . H42 . 106.8 no H43 . Al4 . H42 . 122.4 no H41 . Al4 . H42 . 116.6 no C5 . Al4 . H42 . 95.3 no Mo3 . H43 . Al4 . 116(4) no Mo1 . H41 . Al4 . 112(3) no Al4 . C5 . N6 . 116.7(3) yes Al4 . C5 . N10 . 125.2(4) yes N6 . C5 . N10 . 117.0(4) yes C5 . N6 . C7 . 124.5(4) yes C5 . N6 . C20 . 121.7(4) yes C7 . N6 . C20 . 113.7(4) yes N6 . C7 . C8 . 111.0(5) yes N6 . C7 . H71 . 109.0 no C8 . C7 . H71 . 108.5 no N6 . C7 . H72 . 109.4 no C8 . C7 . H72 . 109.6 no H71 . C7 . H72 . 109.4 no C7 . C8 . C9 . 108.0(6) yes C7 . C8 . H82 . 109.5 no C9 . C8 . H82 . 110.2 no C7 . C8 . H81 . 109.6 no C9 . C8 . H81 . 109.7 no H82 . C8 . H81 . 109.9 no C8 . C9 . N10 . 109.3(5) yes C8 . C9 . H92 . 108.7 no N10 . C9 . H92 . 109.6 no C8 . C9 . H91 . 110.0 no N10 . C9 . H91 . 109.6 no H92 . C9 . H91 . 109.7 no C9 . N10 . C5 . 124.1(4) yes C9 . N10 . C11 . 113.7(4) yes C5 . N10 . C11 . 122.2(4) yes N10 . C11 . C12 . 120.3(5) yes N10 . C11 . C18 . 118.4(5) yes C12 . C11 . C18 . 121.1(5) yes C11 . C12 . C13 . 121.5(5) yes C11 . C12 . C14 . 117.8(6) yes C13 . C12 . C14 . 120.7(6) yes C12 . C13 . H133 . 110.4 no C12 . C13 . H131 . 109.2 no H133 . C13 . H131 . 108.0 no C12 . C13 . H132 . 110.8 no H133 . C13 . H132 . 109.4 no H131 . C13 . H132 . 109.0 no C12 . C14 . C15 . 122.0(6) yes C12 . C14 . H141 . 119.3 no C15 . C14 . H141 . 118.7 no C14 . C15 . C16 . 120.8(8) yes C14 . C15 . C17 . 118.6(6) yes C16 . C15 . C17 . 120.6(8) yes C15 . C16 . H162 . 110.2 no C15 . C16 . H163 . 109.9 no H162 . C16 . H163 . 108.2 no C15 . C16 . H161 . 109.7 no H162 . C16 . H161 . 109.4 no H163 . C16 . H161 . 109.4 no C15 . C17 . C18 . 122.0(6) yes C15 . C17 . H171 . 118.9 no C18 . C17 . H171 . 119.1 no C11 . C18 . C17 . 118.5(6) yes C11 . C18 . C19 . 119.7(6) yes C17 . C18 . C19 . 121.7(6) yes C18 . C19 . H192 . 108.7 no C18 . C19 . H193 . 110.0 no H192 . C19 . H193 . 109.5 no C18 . C19 . H191 . 109.6 no H192 . C19 . H191 . 109.3 no H193 . C19 . H191 . 109.7 no N6 . C20 . C21 . 118.1(5) yes N6 . C20 . C27 . 119.5(5) yes C21 . C20 . C27 . 121.9(5) yes C20 . C21 . C22 . 121.4(5) yes C20 . C21 . C23 . 117.9(5) yes C22 . C21 . C23 . 120.7(5) yes C21 . C22 . H221 . 109.6 no C21 . C22 . H222 . 110.4 no H221 . C22 . H222 . 108.1 no C21 . C22 . H223 . 110.8 no H221 . C22 . H223 . 108.8 no H222 . C22 . H223 . 109.1 no C21 . C23 . C24 . 121.9(5) yes C21 . C23 . H231 . 119.1 no C24 . C23 . H231 . 119.0 no C23 . C24 . C25 . 120.9(6) yes C23 . C24 . C26 . 118.6(5) yes C25 . C24 . C26 . 120.5(6) yes C24 . C25 . H253 . 110.0 no C24 . C25 . H252 . 109.7 no H253 . C25 . H252 . 109.0 no C24 . C25 . H251 . 110.2 no H253 . C25 . H251 . 109.4 no H252 . C25 . H251 . 108.5 no C24 . C26 . C27 . 121.6(6) yes C24 . C26 . H261 . 119.8 no C27 . C26 . H261 . 118.7 no C26 . C27 . C20 . 118.0(5) yes C26 . C27 . C28 . 119.7(5) yes C20 . C27 . C28 . 122.3(5) yes C27 . C28 . H283 . 109.9 no C27 . C28 . H282 . 109.1 no H283 . C28 . H282 . 109.4 no C27 . C28 . H281 . 109.2 no H283 . C28 . H281 . 109.7 no H282 . C28 . H281 . 109.6 no Mo1 . H23 . Mo3 . 129(4) no Mo1 . H23 . Al2 . 92(3) no Mo3 . H23 . Al2 . 89(3) no Mo3 . C29 . O30 . 176.2(5) yes Mo3 . C31 . O32 . 173.7(5) yes Mo3 . C33 . O34 . 173.4(5) yes Al2 . O35 . C36 . 149.9(3) yes O35 . C36 . Mo1 2_565 169.3(4) yes Al2 . C37 . N38 . 120.1(4) yes Al2 . C37 . N51 . 121.9(4) yes N38 . C37 . N51 . 117.8(4) yes C37 . N38 . C39 . 121.2(4) yes C37 . N38 . C48 . 124.0(4) yes C39 . N38 . C48 . 114.8(4) yes N38 . C39 . C40 . 119.3(5) yes N38 . C39 . C45 . 118.9(5) yes C40 . C39 . C45 . 121.6(5) yes C39 . C40 . C41 . 121.1(5) yes C39 . C40 . C42 . 117.7(6) yes C41 . C40 . C42 . 121.2(6) yes C40 . C41 . H411 . 111.0 no C40 . C41 . H412 . 109.1 no H411 . C41 . H412 . 108.9 no C40 . C41 . H413 . 110.6 no H411 . C41 . H413 . 108.2 no H412 . C41 . H413 . 109.0 no C40 . C42 . C43 . 122.3(6) yes C40 . C42 . H421 . 118.9 no C43 . C42 . H421 . 118.7 no C42 . C43 . C44 . 118.4(6) yes C42 . C43 . C47 . 121.2(8) yes C44 . C43 . C47 . 120.3(7) yes C43 . C44 . C45 . 122.0(6) yes C43 . C44 . H441 . 119.2 no C45 . C44 . H441 . 118.8 no C39 . C45 . C44 . 117.7(6) yes C39 . C45 . C46 . 122.1(5) yes C44 . C45 . C46 . 120.2(6) yes C45 . C46 . H461 . 109.3 no C45 . C46 . H463 . 110.6 no H461 . C46 . H463 . 109.2 no C45 . C46 . H462 . 109.3 no H461 . C46 . H462 . 108.5 no H463 . C46 . H462 . 110.0 no C43 . C47 . H471 . 110.0 no C43 . C47 . H473 . 109.3 no H471 . C47 . H473 . 109.7 no C43 . C47 . H472 . 109.3 no H471 . C47 . H472 . 109.8 no H473 . C47 . H472 . 108.7 no N38 . C48 . C49 . 109.8(5) yes N38 . C48 . H481 . 109.5 no C49 . C48 . H481 . 109.5 no N38 . C48 . H482 . 108.9 no C49 . C48 . H482 . 108.5 no H481 . C48 . H482 . 110.7 no C48 . C49 . C50 . 109.4(5) yes C48 . C49 . H491 . 108.9 no C50 . C49 . H491 . 110.8 no C48 . C49 . H492 . 109.1 no C50 . C49 . H492 . 109.6 no H491 . C49 . H492 . 109.0 no C49 . C50 . N51 . 110.1(5) yes C49 . C50 . H501 . 110.2 no N51 . C50 . H501 . 109.3 no C49 . C50 . H502 . 109.2 no N51 . C50 . H502 . 108.9 no H501 . C50 . H502 . 109.1 no C50 . N51 . C37 . 124.2(4) yes C50 . N51 . C52 . 112.7(4) yes C37 . N51 . C52 . 122.7(4) yes N51 . C52 . C53 . 118.3(5) yes N51 . C52 . C57 . 119.5(5) yes C53 . C52 . C57 . 122.1(5) yes C52 . C53 . C54 . 117.9(5) yes C52 . C53 . C60 . 121.5(5) yes C54 . C53 . C60 . 120.4(5) yes C53 . C54 . C55 . 122.1(6) yes C53 . C54 . H541 . 119.0 no C55 . C54 . H541 . 118.9 no C54 . C55 . C56 . 118.8(6) yes C54 . C55 . C59 . 120.1(6) yes C56 . C55 . C59 . 121.1(6) yes C55 . C56 . C57 . 121.9(5) yes C55 . C56 . H561 . 119.1 no C57 . C56 . H561 . 119.0 no C56 . C57 . C52 . 117.1(5) yes C56 . C57 . C58 . 120.8(5) yes C52 . C57 . C58 . 122.1(5) yes C57 . C58 . H583 . 109.6 no C57 . C58 . H581 . 110.7 no H583 . C58 . H581 . 109.0 no C57 . C58 . H582 . 109.6 no H583 . C58 . H582 . 109.1 no H581 . C58 . H582 . 108.7 no C55 . C59 . H593 . 109.1 no C55 . C59 . H592 . 110.7 no H593 . C59 . H592 . 109.2 no C55 . C59 . H591 . 110.3 no H593 . C59 . H591 . 108.0 no H592 . C59 . H591 . 109.5 no C53 . C60 . H601 . 109.0 no C53 . C60 . H602 . 109.7 no H601 . C60 . H602 . 109.7 no C53 . C60 . H603 . 109.7 no H601 . C60 . H603 . 109.7 no H602 . C60 . H603 . 109.0 no Mo1 . C61 . O62 . 175.5(5) yes Mo1 . C63 . O64 . 173.6(5) yes F65 . C66 . C67 . 120.6(7) yes F65 . C66 . C72 . 118.8(7) yes C67 . C66 . C72 . 120.6(7) yes C66 . C67 . F68 . 119.1(7) yes C66 . C67 . C69 . 120.4(6) yes F68 . C67 . C69 . 120.5(7) yes C67 . C69 . C70 . 119.6(7) yes C67 . C69 . H691 . 120.2 no C70 . C69 . H691 . 120.2 no C69 . C70 . C71 . 120.6(7) yes C69 . C70 . H701 . 120.0 no C71 . C70 . H701 . 119.4 no C70 . C71 . C72 . 120.6(6) yes C70 . C71 . H711 . 120.1 no C72 . C71 . H711 . 119.3 no C66 . C72 . C71 . 118.2(7) yes C66 . C72 . H721 . 119.9 no C71 . C72 . H721 . 121.9 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C48 . H482 . O62 5_565 125.83(18) 0.972 2.575 3.241(10) yes C70 . H701 . O30 7_565 127.78(19) 0.927 2.551 3.203(10) yes _iucr_refine_instruction_details_constraints ; # # Punched on 25/03/13 at 17:56:14 # #LIST 12 BLOCK SCALE X'S, U'S H(21, X'S) H(22, X'S) H(23, X'S) H(41, X'S) H(43, X'S) RIDE AL ( 4,X'S) H ( 42,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 92,X'S) H ( 91,X'S) RIDE C ( 13,X'S) H ( 133,X'S) H ( 131,X'S) H ( 132,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 16,X'S) H ( 162,X'S) H ( 163,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 192,X'S) H ( 193,X'S) H ( 191,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) H ( 223,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 25,X'S) H ( 253,X'S) H ( 252,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 283,X'S) H ( 282,X'S) H ( 281,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 463,X'S) H ( 462,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 473,X'S) H ( 472,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 50,X'S) H ( 501,X'S) H ( 502,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 58,X'S) H ( 583,X'S) H ( 581,X'S) H ( 582,X'S) RIDE C ( 59,X'S) H ( 593,X'S) H ( 592,X'S) H ( 591,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S) RIDE C ( 69,X'S) H ( 691,X'S) RIDE C ( 70,X'S) H ( 701,X'S) RIDE C ( 71,X'S) H ( 711,X'S) RIDE C ( 72,X'S) H ( 721,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/03/13 at 17:56:14 # #LIST 16 REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # start Validation Reply Form _vrf_CHEMW01_4a ; PROBLEM: The ratio of given/expected molecular weight as calculated RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_CHEMW03_4a ; PROBLEM: WARNING: The ratio of given/expected molecular weight as RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_ABSMU01_4a ; PROBLEM: The ratio of given/expected absorption coefficient lies RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_PLAT041_4a ; PROBLEM: Calc. and Reported SumFormula Strings Differ ? RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_PLAT068_4a ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_FORMU01_4a ; PROBLEM: There is a discrepancy between the atom counts in the RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_CELLZ01_4a ; PROBLEM: Difference between formula and atom_site contents detected. RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_PLAT042_4a ; PROBLEM: Calc. and Reported MoietyFormula Strings Differ ? RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; _vrf_PLAT044_4a ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: The value was calculated to include the solvent removed by SQUEEZE. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 931229'