# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Professor Isabel Goncalves' _publ_contact_author_address ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; _publ_contact_author_email igoncalves@dq.ua.pt _publ_contact_author_fax '+351 234 370084' _publ_contact_author_phone '+351 234 378190' loop_ _publ_author_name _publ_author_footnote _publ_author_address C.A.Gamelas . ; Instituto de Tecnologia Quimica e Biologica Universidade Nova de Lisboa 2781-901 Oeiras Portugal and Escola Superior de Tecnologia Instituto Politecnico de Setubal 2910-761 Setubal Portugal ; A.C.Gomes . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; S.M.Bruno . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'F.A.Almeida Paz' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; A.A.Valente . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; ; M.Pillinger ; . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; C.C.Romao . ; Instituto de Tecnologia Quimica e Biologica Universidade Nova de Lisboa 2781-901 Oeiras Portugal and Alfama Ltd., Taguspark Nucleo Central 267 2740-122 Porto Salvo Portugal ; I.S.Goncalves . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; data_2c _database_code_depnum_ccdc_archive 'CCDC 830597' #TrackingRef '2c.cif' # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '18 June 2011' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H96 Mo8 N8 O24' _chemical_formula_sum 'C72 H96 Mo8 N8 O24' _chemical_formula_weight 2225.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # CRYSTAL DATA #============================================================================== _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.309(3) _cell_length_b 20.309(3) _cell_length_c 33.411(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13781(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9073 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.41 _exptl_crystal_description Prism _exptl_crystal_colour Pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8769 _exptl_absorpt_correction_T_max 0.9154 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; #============================================================================== # EXPERIMENTAL DATA #============================================================================== _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method '\w / \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 56059 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7885 _reflns_number_gt 4999 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'SAINT+ (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' #============================================================================== # REFINEMENT DATA #============================================================================== _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7885 _refine_ls_number_parameters 259 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.03956(2) 0.31676(2) 0.085006(11) 0.02729(14) Uani 1 1 d . . . Mo2 Mo -0.01102(2) 0.45991(2) 0.147803(12) 0.03244(15) Uani 1 1 d . . . O1 O 0.04066(16) 0.32139(17) 0.03416(9) 0.0341(8) Uani 1 1 d . . . O2 O 0.13513(15) 0.31070(16) 0.09248(9) 0.0320(8) Uani 1 1 d . . . O3 O -0.04689(15) 0.28810(15) 0.09444(9) 0.0278(7) Uani 1 1 d . . . O4 O 0.03326(16) 0.39963(16) 0.10018(9) 0.0323(8) Uani 1 1 d . . . O5 O 0.06039(18) 0.45681(18) 0.17492(10) 0.0414(9) Uani 1 1 d . . . O6 O -0.05673(18) 0.52011(17) 0.17046(11) 0.0444(9) Uani 1 1 d . . . N1 N -0.0708(2) 0.48028(19) 0.09051(11) 0.0328(9) Uani 1 1 d . . . N2 N 0.0389(2) 0.5385(2) 0.11112(12) 0.0345(10) Uani 1 1 d . . . C1 C -0.1254(2) 0.4467(2) 0.08245(15) 0.0357(12) Uani 1 1 d . . . H1 H -0.1359 0.4091 0.0982 0.043 Uiso 1 1 calc R . . C2 C -0.1672(3) 0.4649(3) 0.05186(16) 0.0392(12) Uani 1 1 d . . . H2 H -0.2067 0.4408 0.0478 0.047 Uiso 1 1 calc R . . C3 C -0.1531(3) 0.5176(2) 0.02698(14) 0.0362(12) Uani 1 1 d . . . C4 C -0.0926(3) 0.5494(2) 0.03456(14) 0.0342(11) Uani 1 1 d . . . H4 H -0.0791 0.5844 0.0176 0.041 Uiso 1 1 calc R . . C5 C -0.0519(3) 0.5305(2) 0.06648(15) 0.0345(11) Uani 1 1 d . . . C6 C 0.0100(3) 0.5619(2) 0.07792(15) 0.0322(11) Uani 1 1 d . . . C7 C 0.0392(3) 0.6140(3) 0.05638(16) 0.0401(13) Uani 1 1 d . . . H7 H 0.0192 0.6296 0.0325 0.048 Uiso 1 1 calc R . . C8 C 0.0976(3) 0.6427(3) 0.07014(16) 0.0407(13) Uani 1 1 d . . . C9 C 0.1240(3) 0.6176(3) 0.10533(16) 0.0411(13) Uani 1 1 d . . . H9 H 0.1632 0.6360 0.1161 0.049 Uiso 1 1 calc R . . C10 C 0.0938(3) 0.5668(3) 0.12428(15) 0.0384(12) Uani 1 1 d . . . H10 H 0.1129 0.5506 0.1483 0.046 Uiso 1 1 calc R . . C11 C -0.1983(3) 0.5439(3) -0.00624(16) 0.0424(13) Uani 1 1 d . . . C12 C -0.2638(3) 0.5057(4) -0.0073(2) 0.079(2) Uani 1 1 d . . . H12A H -0.2551 0.4592 -0.0130 0.119 Uiso 1 1 calc R . . H12B H -0.2922 0.5240 -0.0283 0.119 Uiso 1 1 calc R . . H12C H -0.2860 0.5096 0.0186 0.119 Uiso 1 1 calc R . . C13 C -0.1634(3) 0.5350(3) -0.04699(16) 0.0596(17) Uani 1 1 d . . . H13A H -0.1233 0.5618 -0.0476 0.089 Uiso 1 1 calc R . . H13B H -0.1929 0.5489 -0.0686 0.089 Uiso 1 1 calc R . . H13C H -0.1517 0.4885 -0.0507 0.089 Uiso 1 1 calc R . . C14 C -0.2116(3) 0.6154(3) 0.00147(19) 0.0623(18) Uani 1 1 d . . . H14A H -0.2282 0.6210 0.0288 0.093 Uiso 1 1 calc R . . H14B H -0.2445 0.6315 -0.0176 0.093 Uiso 1 1 calc R . . H14C H -0.1708 0.6405 -0.0017 0.093 Uiso 1 1 calc R . . C15 C 0.1298(3) 0.7010(3) 0.04818(18) 0.0482(14) Uani 1 1 d . . . C16 C 0.2063(5) 0.6982(7) 0.0540(5) 0.225(8) Uani 1 1 d U . . H16A H 0.2226 0.6548 0.0459 0.337 Uiso 1 1 calc R . . H16B H 0.2170 0.7059 0.0822 0.337 Uiso 1 1 calc R . . H16C H 0.2271 0.7323 0.0375 0.337 Uiso 1 1 calc R . . C17 C 0.1170(4) 0.6991(4) 0.00454(18) 0.073(2) Uani 1 1 d . . . H17A H 0.1419 0.7343 -0.0087 0.110 Uiso 1 1 calc R . . H17B H 0.0699 0.7053 -0.0004 0.110 Uiso 1 1 calc R . . H17C H 0.1309 0.6564 -0.0062 0.110 Uiso 1 1 calc R . . C18 C 0.1006(8) 0.7624(4) 0.0651(3) 0.184(7) Uani 1 1 d U . . H18A H 0.1153 0.8003 0.0493 0.276 Uiso 1 1 calc R . . H18B H 0.1150 0.7677 0.0929 0.276 Uiso 1 1 calc R . . H18C H 0.0525 0.7594 0.0642 0.276 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0287(2) 0.0314(3) 0.0218(2) 0.00199(16) -0.00142(16) -0.00200(17) Mo2 0.0377(3) 0.0298(3) 0.0298(3) 0.00267(18) -0.00139(19) 0.00002(19) O1 0.0346(19) 0.048(2) 0.0196(16) 0.0038(14) -0.0025(14) -0.0093(16) O2 0.0273(18) 0.0360(19) 0.0326(18) 0.0046(14) -0.0024(14) -0.0028(14) O3 0.0303(18) 0.0318(18) 0.0213(16) 0.0023(13) -0.0004(13) -0.0044(14) O4 0.037(2) 0.0306(18) 0.0294(17) 0.0028(14) 0.0020(15) -0.0021(15) O5 0.048(2) 0.042(2) 0.0346(19) 0.0067(16) -0.0113(16) -0.0057(18) O6 0.050(2) 0.037(2) 0.047(2) 0.0051(17) 0.0106(18) 0.0006(18) N1 0.035(2) 0.026(2) 0.038(2) 0.0040(18) 0.0010(18) 0.0007(18) N2 0.034(2) 0.032(2) 0.037(2) 0.0054(18) -0.0041(19) 0.0035(18) C1 0.033(3) 0.022(2) 0.053(3) 0.010(2) -0.005(2) -0.005(2) C2 0.035(3) 0.033(3) 0.050(3) 0.000(2) -0.006(2) -0.001(2) C3 0.046(3) 0.026(3) 0.037(3) 0.001(2) -0.008(2) -0.004(2) C4 0.045(3) 0.028(3) 0.030(3) 0.007(2) -0.002(2) -0.006(2) C5 0.037(3) 0.033(3) 0.034(3) 0.004(2) 0.004(2) 0.000(2) C6 0.039(3) 0.021(2) 0.036(3) 0.004(2) -0.006(2) 0.001(2) C7 0.036(3) 0.040(3) 0.044(3) 0.013(2) -0.011(2) -0.003(2) C8 0.042(3) 0.034(3) 0.046(3) 0.010(2) -0.007(2) -0.009(2) C9 0.040(3) 0.039(3) 0.045(3) 0.004(2) -0.015(2) -0.006(2) C10 0.045(3) 0.037(3) 0.034(3) 0.001(2) -0.007(2) -0.002(2) C11 0.036(3) 0.047(3) 0.044(3) 0.009(3) -0.011(2) -0.001(2) C12 0.053(4) 0.103(6) 0.080(5) 0.043(4) -0.031(4) -0.020(4) C13 0.076(5) 0.067(4) 0.035(3) 0.002(3) -0.004(3) -0.006(4) C14 0.069(5) 0.057(4) 0.060(4) 0.011(3) -0.018(3) 0.018(3) C15 0.044(3) 0.041(3) 0.059(4) 0.013(3) -0.004(3) -0.013(3) C16 0.101(8) 0.238(13) 0.335(17) 0.226(13) -0.091(10) -0.100(9) C17 0.097(6) 0.082(5) 0.040(3) -0.004(3) 0.015(4) -0.049(4) C18 0.387(18) 0.049(5) 0.117(8) -0.017(5) 0.143(10) -0.065(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #============================================================================== # GEOMETRY #============================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.702(3) . ? Mo1 O4 1.762(3) . ? Mo1 O3 1.876(3) . ? Mo1 O2 1.961(3) . ? Mo1 O3 2.158(3) 6_454 ? Mo1 O3 2.392(3) 15 ? Mo1 Mo1 3.1520(10) 6_454 ? Mo2 O5 1.711(3) . ? Mo2 O6 1.712(4) . ? Mo2 O2 1.852(3) 12_666 ? Mo2 O4 2.200(3) . ? Mo2 N2 2.253(4) . ? Mo2 N1 2.304(4) . ? O2 Mo2 1.852(3) 15 ? O3 Mo1 2.158(3) 6_454 ? O3 Mo1 2.392(3) 12_666 ? N1 C1 1.330(6) . ? N1 C5 1.352(6) . ? N2 C10 1.331(6) . ? N2 C6 1.341(6) . ? C1 C2 1.380(7) . ? C1 H1 0.9500 . ? C2 C3 1.385(7) . ? C2 H2 0.9500 . ? C3 C4 1.410(7) . ? C3 C11 1.537(7) . ? C4 C5 1.403(7) . ? C4 H4 0.9500 . ? C5 C6 1.462(7) . ? C6 C7 1.411(7) . ? C7 C8 1.399(7) . ? C7 H7 0.9500 . ? C8 C9 1.389(7) . ? C8 C15 1.539(7) . ? C9 C10 1.357(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C14 1.500(8) . ? C11 C12 1.540(8) . ? C11 C13 1.546(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.482(8) . ? C15 C18 1.491(11) . ? C15 C16 1.566(12) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O4 103.62(16) . . ? O1 Mo1 O3 101.37(14) . . ? O4 Mo1 O3 100.37(14) . . ? O1 Mo1 O2 96.75(14) . . ? O4 Mo1 O2 95.46(14) . . ? O3 Mo1 O2 152.29(14) . . ? O1 Mo1 O3 101.50(14) . 6_454 ? O4 Mo1 O3 154.88(13) . 6_454 ? O3 Mo1 O3 74.56(15) . 6_454 ? O2 Mo1 O3 81.44(12) . 6_454 ? O1 Mo1 O3 173.45(14) . 15 ? O4 Mo1 O3 82.92(13) . 15 ? O3 Mo1 O3 76.73(13) . 15 ? O2 Mo1 O3 82.89(12) . 15 ? O3 Mo1 O3 71.96(12) 6_454 15 ? O1 Mo1 Mo1 93.11(11) . 6_454 ? O4 Mo1 Mo1 141.68(11) . 6_454 ? O3 Mo1 Mo1 41.94(10) . 6_454 ? O2 Mo1 Mo1 116.78(10) . 6_454 ? O3 Mo1 Mo1 35.53(8) 6_454 6_454 ? O3 Mo1 Mo1 81.29(8) 15 6_454 ? O5 Mo2 O6 104.58(19) . . ? O5 Mo2 O2 109.80(16) . 12_666 ? O6 Mo2 O2 102.29(16) . 12_666 ? O5 Mo2 O4 90.92(16) . . ? O6 Mo2 O4 159.91(15) . . ? O2 Mo2 O4 83.87(13) 12_666 . ? O5 Mo2 N2 86.16(16) . . ? O6 Mo2 N2 88.76(16) . . ? O2 Mo2 N2 157.11(14) 12_666 . ? O4 Mo2 N2 79.45(14) . . ? O5 Mo2 N1 153.25(16) . . ? O6 Mo2 N1 87.33(16) . . ? O2 Mo2 N1 90.34(14) 12_666 . ? O4 Mo2 N1 73.41(13) . . ? N2 Mo2 N1 69.98(15) . . ? Mo2 O2 Mo1 150.26(19) 15 . ? Mo1 O3 Mo1 102.54(14) . 6_454 ? Mo1 O3 Mo1 108.64(14) . 12_666 ? Mo1 O3 Mo1 99.66(12) 6_454 12_666 ? Mo1 O4 Mo2 140.28(17) . . ? C1 N1 C5 120.2(4) . . ? C1 N1 Mo2 121.0(3) . . ? C5 N1 Mo2 118.6(3) . . ? C10 N2 C6 119.1(4) . . ? C10 N2 Mo2 120.2(3) . . ? C6 N2 Mo2 120.3(3) . . ? N1 C1 C2 121.7(5) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 121.6(5) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C2 C3 C4 115.2(5) . . ? C2 C3 C11 125.3(5) . . ? C4 C3 C11 119.4(4) . . ? C5 C4 C3 121.6(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? N1 C5 C4 119.4(5) . . ? N1 C5 C6 114.7(4) . . ? C4 C5 C6 125.9(4) . . ? N2 C6 C7 120.3(5) . . ? N2 C6 C5 116.0(4) . . ? C7 C6 C5 123.8(4) . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 116.9(5) . . ? C9 C8 C15 121.4(5) . . ? C7 C8 C15 121.6(5) . . ? C10 C9 C8 119.9(5) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? N2 C10 C9 123.6(5) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C14 C11 C3 108.6(4) . . ? C14 C11 C12 109.7(6) . . ? C3 C11 C12 111.0(5) . . ? C14 C11 C13 110.3(5) . . ? C3 C11 C13 108.7(5) . . ? C12 C11 C13 108.5(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C18 109.0(7) . . ? C17 C15 C8 112.0(5) . . ? C18 C15 C8 107.1(5) . . ? C17 C15 C16 107.2(8) . . ? C18 C15 C16 112.1(9) . . ? C8 C15 C16 109.5(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo1 O2 Mo2 -100.8(4) . . . 15 ? O4 Mo1 O2 Mo2 154.8(4) . . . 15 ? O3 Mo1 O2 Mo2 29.9(6) . . . 15 ? O3 Mo1 O2 Mo2 -0.1(4) 6_454 . . 15 ? O3 Mo1 O2 Mo2 72.6(4) 15 . . 15 ? Mo1 Mo1 O2 Mo2 -3.8(4) 6_454 . . 15 ? O1 Mo1 O3 Mo1 81.89(16) . . . 6_454 ? O4 Mo1 O3 Mo1 -171.79(13) . . . 6_454 ? O2 Mo1 O3 Mo1 -48.0(3) . . . 6_454 ? O3 Mo1 O3 Mo1 -17.06(16) 6_454 . . 6_454 ? O3 Mo1 O3 Mo1 -91.70(11) 15 . . 6_454 ? O1 Mo1 O3 Mo1 -173.25(15) . . . 12_666 ? O4 Mo1 O3 Mo1 -66.93(16) . . . 12_666 ? O2 Mo1 O3 Mo1 56.9(3) . . . 12_666 ? O3 Mo1 O3 Mo1 87.80(11) 6_454 . . 12_666 ? O3 Mo1 O3 Mo1 13.16(13) 15 . . 12_666 ? Mo1 Mo1 O3 Mo1 104.86(17) 6_454 . . 12_666 ? O1 Mo1 O4 Mo2 146.1(3) . . . . ? O3 Mo1 O4 Mo2 41.6(3) . . . . ? O2 Mo1 O4 Mo2 -115.6(3) . . . . ? O3 Mo1 O4 Mo2 -34.1(5) 6_454 . . . ? O3 Mo1 O4 Mo2 -33.4(3) 15 . . . ? Mo1 Mo1 O4 Mo2 32.8(4) 6_454 . . . ? O5 Mo2 O4 Mo1 93.9(3) . . . . ? O6 Mo2 O4 Mo1 -125.1(4) . . . . ? O2 Mo2 O4 Mo1 -15.9(3) 12_666 . . . ? N2 Mo2 O4 Mo1 179.8(3) . . . . ? N1 Mo2 O4 Mo1 -108.1(3) . . . . ? O5 Mo2 N1 C1 150.3(4) . . . . ? O6 Mo2 N1 C1 -91.9(4) . . . . ? O2 Mo2 N1 C1 10.4(4) 12_666 . . . ? O4 Mo2 N1 C1 93.9(4) . . . . ? N2 Mo2 N1 C1 178.5(4) . . . . ? O5 Mo2 N1 C5 -34.4(6) . . . . ? O6 Mo2 N1 C5 83.5(4) . . . . ? O2 Mo2 N1 C5 -174.3(4) 12_666 . . . ? O4 Mo2 N1 C5 -90.8(4) . . . . ? N2 Mo2 N1 C5 -6.2(3) . . . . ? O5 Mo2 N2 C10 -14.0(4) . . . . ? O6 Mo2 N2 C10 90.7(4) . . . . ? O2 Mo2 N2 C10 -149.6(4) 12_666 . . . ? O4 Mo2 N2 C10 -105.7(4) . . . . ? N1 Mo2 N2 C10 178.3(4) . . . . ? O5 Mo2 N2 C6 172.8(4) . . . . ? O6 Mo2 N2 C6 -82.5(4) . . . . ? O2 Mo2 N2 C6 37.2(6) 12_666 . . . ? O4 Mo2 N2 C6 81.2(4) . . . . ? N1 Mo2 N2 C6 5.1(4) . . . . ? C5 N1 C1 C2 -5.6(8) . . . . ? Mo2 N1 C1 C2 169.6(4) . . . . ? N1 C1 C2 C3 2.6(8) . . . . ? C1 C2 C3 C4 1.7(8) . . . . ? C1 C2 C3 C11 -176.4(5) . . . . ? C2 C3 C4 C5 -3.2(7) . . . . ? C11 C3 C4 C5 175.1(5) . . . . ? C1 N1 C5 C4 4.0(7) . . . . ? Mo2 N1 C5 C4 -171.3(4) . . . . ? C1 N1 C5 C6 -178.1(4) . . . . ? Mo2 N1 C5 C6 6.6(6) . . . . ? C3 C4 C5 N1 0.4(8) . . . . ? C3 C4 C5 C6 -177.2(5) . . . . ? C10 N2 C6 C7 2.7(7) . . . . ? Mo2 N2 C6 C7 175.9(4) . . . . ? C10 N2 C6 C5 -176.9(5) . . . . ? Mo2 N2 C6 C5 -3.7(6) . . . . ? N1 C5 C6 N2 -2.0(7) . . . . ? C4 C5 C6 N2 175.7(5) . . . . ? N1 C5 C6 C7 178.4(5) . . . . ? C4 C5 C6 C7 -3.9(8) . . . . ? N2 C6 C7 C8 -1.6(8) . . . . ? C5 C6 C7 C8 177.9(5) . . . . ? C6 C7 C8 C9 -0.3(8) . . . . ? C6 C7 C8 C15 -178.1(5) . . . . ? C7 C8 C9 C10 1.1(8) . . . . ? C15 C8 C9 C10 178.9(5) . . . . ? C6 N2 C10 C9 -1.9(8) . . . . ? Mo2 N2 C10 C9 -175.2(4) . . . . ? C8 C9 C10 N2 0.0(9) . . . . ? C2 C3 C11 C14 123.2(6) . . . . ? C4 C3 C11 C14 -54.9(7) . . . . ? C2 C3 C11 C12 2.5(8) . . . . ? C4 C3 C11 C12 -175.6(6) . . . . ? C2 C3 C11 C13 -116.8(6) . . . . ? C4 C3 C11 C13 65.2(6) . . . . ? C9 C8 C15 C17 151.6(6) . . . . ? C7 C8 C15 C17 -30.7(8) . . . . ? C9 C8 C15 C18 -89.0(9) . . . . ? C7 C8 C15 C18 88.7(9) . . . . ? C9 C8 C15 C16 32.8(11) . . . . ? C7 C8 C15 C16 -149.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.251 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.129 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.060 0.690 0.224 6480 3448 ' ' _platon_squeeze_details ; ; #============================================================================== # END #==============================================================================