# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_added_by_encifer _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _data_manuscript_title ; 'Molybdenum- and Tungsten(II) Monometallic 3-(2-Pyridyl)pyrazole and Bimetallic 3-(2-Pyridyl)pyrazolate Complexes' ; _audit_creation_method SHELXL _pub_requested_journal 'Dalton Transactions' _publ_contact_author ; FERNANDO VILLAFA\~NE IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_phone +34-983-184620 _publ_contact_author_fax +34-983-423013 _publ_contact_author_email fervilla@qi.uva.es loop_ _publ_author_name _publ_author_address 'Marta Arroyo' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Daniel Miguel' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; F.Villafane ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Elisabete C. B. Alegria' ; Centro de Qu\'imica Estrutural, Complexo I, Instituto Superior T\'ecnico, Technical University of Lisbon, 1049-001 Lisboa, Portugal ; 'Armando J. L. Pombeiro' ; Centro de Qu\'imica Estrutural, Complexo I, Instituto Superior T\'ecnico, Technical University of Lisbon, 1049-001 Lisboa, Portugal ; _publ_contact_author_name 'FERNANDO VILLAFANE' #---------data section of block ----------------------- data_Compound_1_ma3am _database_code_depnum_ccdc_archive 'CCDC 858711' #TrackingRef '- Molybdenum_and_tungsten_REVISED_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H7 Mo N3 O4' _chemical_formula_weight 353.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 6.790(5) _cell_length_b 15.749(10) _cell_length_c 12.449(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.396(13) _cell_angle_gamma 90.00 _cell_volume 1330.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 377 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 16.50 _exptl_crystal_description PRISM _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.457967 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS - Bruker area detector absorption corrections #----------------------------------------------------- Laue group number 2 selected Laue group numbers: [1] -1 [8] -3m (rhombohedral axes) [2] 2/m (Y unique) [9] -31m (Z unique) [3] mmm [10] -3m1 (Z unique) [4] 4/m (Z unique) [11] 6/m (Z unique) [5] 4/mmm (Z unique) [12] 6/mmm (Z unique) [6] -3 (rhombohedral axes) [13] m3 [7] -3 (Z unique) [14] m3m Friedel opposites treated as equivalent for parameter fitting Reading batch 1 from file MA3A1.raw Reading batch 2 from file MA3A2.raw Reading batch 3 from file MA3A3.raw Mean and maximum errors in direction cosine check function = 0.001 0.003 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Maximum 2-theta = 46.67 degrees 3125 Reflections of which 1939 unique; 4.91 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 918 856 165 0 0 0 0 0 0 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 774 317 221 123 83 257 71 37 56 Settings for parameter refinement: (Intensity/sigma) threshold = 5.000 (Intensity+sigma)/(Mean Intensity) threshold = 0.250 Savitsky-Golay smoothing applied to incident beam correction Maximum odd and even order spherical harmonic coefficients = 1 4 Sigma(I) values NOT rescaled 708 Reflections employed for parameter determination Effective data to parameter ratio = 1.18 R(int) = 0.0748 before parameter refinement Cycle R(decay) R(absor) 1 0.0606 0.0523 2 0.0490 0.0478 3 0.0463 0.0460 4 0.0451 0.0453 5 0.0447 0.0449 6 0.0446 0.0448 7 0.0446 0.0449 8 0.0447 0.0449 9 0.0448 0.0451 10 0.0450 0.0452 R(int) = 0.0452 after parameter refinement Batch R(int) Factor range Sigma(ib) Sigma(db) K(sigI) Total I>2sig(I) 1 0.0876 0.627 - 1.357 0.0700 0.0864 1.000 1500 525 2 0.0910 0.520 - 1.667 0.0934 0.1018 1.000 1078 411 3 0.0943 0.782 - 1.599 0.0832 0.0969 1.000 547 278 Sigma(ib) and sigma(db) are the square roots of the variances of the normalized incident and diffracted beam correction factors. K(sigI) multiplies the sigma(I) values for the batch in question. Background contribution to sig(I) = 0.0000 times mean intensity 2-theta dependent absorption corrections not applied 3125 Corrected reflections written to file MA3AM.HKL Maximum and minimum effective transmission: 1.000000 0.457967 ; _diffrn_ambient_temperature 299(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3004 _diffrn_reflns_av_R_equivalents 0.1173 _diffrn_reflns_av_sigmaI/netI 0.1348 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 23.17 _reflns_number_total 952 _reflns_number_gt 576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; There is a disorder which exchanges the pyridine and pyrazole rings by the symmetry operation -x+1,y,-z+1/2. The rings were modeled with occupancy 0.5 and with constraints to maintain the geometry and to avoid the ellipsoids to become non-positive-definite. 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^)+(0.0618P)^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 952 _refine_ls_number_parameters 116 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 0.926 _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 0.5000 0.31521(7) 0.2500 0.0494(5) Uani 1 2 d S . . C1 C 0.2472(16) 0.3085(6) 0.1663(8) 0.050(2) Uani 1 1 d . A . O1 O 0.0988(12) 0.2983(5) 0.1185(7) 0.089(3) Uani 1 1 d . . . C2 C 0.5973(14) 0.2274(7) 0.1605(9) 0.053(3) Uani 1 1 d . A . O2 O 0.6588(11) 0.1746(5) 0.1071(7) 0.090(3) Uani 1 1 d . . . N1 N 0.4047(10) 0.4375(4) 0.3306(6) 0.056(5) Uani 0.50 1 d PGU A 1 C11 C 0.2993(9) 0.4423(4) 0.4185(6) 0.056(5) Uani 0.50 1 d PGU A 1 H11 H 0.2601 0.3929 0.4525 0.067 Uiso 0.50 1 calc PR A 1 C12 C 0.2502(11) 0.5179(5) 0.4576(7) 0.061(6) Uani 0.50 1 d PGU A 1 H12 H 0.1768 0.5212 0.5189 0.073 Uiso 0.50 1 calc PR A 1 C13 C 0.3065(13) 0.5887(5) 0.4088(8) 0.062(5) Uani 0.50 1 d PGU A 1 H13 H 0.2723 0.6414 0.4361 0.074 Uiso 0.50 1 calc PR A 1 C14 C 0.4118(14) 0.5840(5) 0.3209(8) 0.049(4) Uani 0.50 1 d PGU . 1 H14 H 0.4510 0.6334 0.2869 0.059 Uiso 0.50 1 calc PR A 1 C15 C 0.4609(12) 0.5084(5) 0.2818(7) 0.046(5) Uani 0.50 1 d PGU . 1 N2 N 0.3925(10) 0.4263(4) 0.3438(6) 0.048(5) Uani 0.50 1 d PGU A 2 N3 N 0.2847(11) 0.4291(4) 0.4324(6) 0.064(5) Uani 0.50 1 d PGU A 2 H3 H 0.2451 0.3860 0.4680 0.077 Uiso 0.50 1 calc PR A 2 C18 C 0.2498(11) 0.5114(5) 0.4552(6) 0.066(6) Uani 0.50 1 d PGU A 2 H18 H 0.1788 0.5314 0.5122 0.079 Uiso 0.50 1 calc PR A 2 C17 C 0.3361(10) 0.5594(4) 0.3807(6) 0.066(5) Uani 0.50 1 d PGU A 2 H17 H 0.3350 0.6184 0.3774 0.079 Uiso 0.50 1 calc PR A 2 C16 C 0.4243(10) 0.5068(4) 0.3118(6) 0.055(5) Uani 0.50 1 d PGU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0586(8) 0.0343(7) 0.0550(9) 0.000 -0.0012(6) 0.000 C1 0.066(7) 0.040(5) 0.042(6) 0.008(5) -0.009(6) 0.012(6) O1 0.076(6) 0.086(6) 0.101(7) 0.015(5) -0.023(5) -0.005(5) C2 0.045(6) 0.062(6) 0.051(7) 0.008(6) -0.002(6) 0.001(5) O2 0.096(6) 0.085(6) 0.090(6) -0.033(5) 0.015(5) 0.019(5) N1 0.064(11) 0.047(7) 0.056(10) -0.008(9) -0.002(9) 0.011(10) C11 0.056(12) 0.046(7) 0.064(12) 0.006(9) 0.004(9) 0.011(10) C12 0.060(12) 0.061(9) 0.063(12) -0.011(9) 0.015(10) 0.009(10) C13 0.065(11) 0.048(8) 0.074(12) -0.008(9) 0.018(9) 0.014(9) C14 0.068(12) 0.040(7) 0.039(10) -0.015(8) -0.002(8) 0.014(8) C15 0.051(13) 0.039(7) 0.045(13) -0.013(8) -0.010(9) 0.008(9) N2 0.059(11) 0.034(6) 0.051(10) -0.005(8) -0.001(9) 0.011(8) N3 0.069(11) 0.047(7) 0.078(11) 0.003(8) 0.020(9) -0.006(8) C18 0.060(12) 0.067(10) 0.072(12) -0.021(10) 0.012(10) 0.018(11) C17 0.085(13) 0.029(7) 0.084(13) -0.015(8) 0.003(10) 0.008(9) C16 0.078(12) 0.035(8) 0.053(10) -0.004(8) -0.002(9) 0.000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.912(11) . ? Mo1 C2 1.912(11) 2_655 ? Mo1 C1 1.973(11) 2_655 ? Mo1 C1 1.973(11) . ? Mo1 N2 2.242(12) 2_655 ? Mo1 N2 2.242(6) . ? Mo1 N1 2.278(5) 2_655 ? Mo1 N1 2.278(5) . ? C1 O1 1.160(10) . ? C2 O2 1.153(10) . ? N1 C11 1.334(4) . ? N1 C15 1.334(4) . ? C11 C12 1.334(4) . ? C12 C13 1.334(4) . ? C13 C14 1.334(4) . ? C14 C15 1.334(4) . ? C15 C16 1.429(8) 2_655 ? N2 C16 1.350(4) . ? N2 N3 1.350(4) . ? N3 C18 1.350(4) . ? C18 C17 1.350(4) . ? C17 C16 1.350(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C2 87.3(6) . 2_655 ? C2 Mo1 C1 87.4(4) . 2_655 ? C2 Mo1 C1 88.1(4) 2_655 2_655 ? C2 Mo1 C1 88.1(4) . . ? C2 Mo1 C1 87.4(4) 2_655 . ? C1 Mo1 C1 173.9(5) 2_655 . ? C2 Mo1 N2 97.6(4) . 2_655 ? C2 Mo1 N2 175.0(5) 2_655 2_655 ? C1 Mo1 N2 91.2(5) 2_655 2_655 ? C1 Mo1 N2 93.5(5) . 2_655 ? C2 Mo1 N2 97.6(3) 2_655 . ? C1 Mo1 N2 93.5(3) 2_655 . ? C2 Mo1 N1 104.1(3) . 2_655 ? C2 Mo1 N1 168.6(4) 2_655 2_655 ? C1 Mo1 N1 91.2(3) 2_655 2_655 ? C1 Mo1 N1 94.0(3) . 2_655 ? C2 Mo1 N1 168.6(4) . . ? C2 Mo1 N1 104.1(3) 2_655 . ? C1 Mo1 N1 94.0(3) 2_655 . ? C1 Mo1 N1 91.2(3) . . ? N2 Mo1 N1 71.0(5) 2_655 . ? O1 C1 Mo1 175.0(9) . . ? O2 C2 Mo1 178.9(9) . . ? C11 N1 C15 120.0 . . ? C11 N1 Mo1 125.5(4) . . ? C15 N1 Mo1 114.5(4) . . ? N1 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 N1 120.0 . . ? C15 C16 N2 110.9(4) 2_655 . ? N1 C15 C16 122.2(5) . 2_655 ? C14 C15 C16 117.8(6) . 2_655 ? C16 N2 N3 108.0 . . ? C16 N2 Mo1 121.4(4) . . ? N3 N2 Mo1 130.6(4) . . ? C18 N3 N2 108.0 . . ? N3 C18 C17 108.0 . . ? C16 C17 C18 108.0 . . ? N2 C16 C17 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.17 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.536 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.121 #===END data_compound_2_ma105am _database_code_depnum_ccdc_archive 'CCDC 858712' #TrackingRef '- Molybdenum_and_tungsten_REVISED_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14.50 H15 Br Mo N3 O2.50' _chemical_formula_weight 447.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.917(18) _cell_length_b 7.033(4) _cell_length_c 18.237(11) _cell_angle_alpha 90.00 _cell_angle_beta 121.470(9) _cell_angle_gamma 90.00 _cell_volume 3273(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 3.004 _cell_measurement_theta_max 23.307 _exptl_crystal_description PRISM _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 3.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.660350 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS - Bruker area detector absorption corrections #----------------------------------------------------- Laue group number 2 selected Laue group numbers: [1] -1 [8] -3m (rhombohedral axes) [2] 2/m (Y unique) [9] -31m (Z unique) [3] mmm [10] -3m1 (Z unique) [4] 4/m (Z unique) [11] 6/m (Z unique) [5] 4/mmm (Z unique) [12] 6/mmm (Z unique) [6] -3 (rhombohedral axes) [13] m3 [7] -3 (Z unique) [14] m3m Friedel opposites treated as equivalent for parameter fitting Reading batch 1 from file MA105A1.raw Reading batch 2 from file MA105A2.raw Reading batch 3 from file MA105A3.raw Mean and maximum errors in direction cosine check function = 0.000 0.002 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Maximum 2-theta = 46.59 degrees 7401 Reflections of which 2591 unique; 5.89 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 160 871 897 550 70 43 0 0 0 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 363 155 104 87 87 373 235 177 1010 Settings for parameter refinement: (Intensity/sigma) threshold = 5.000 (Intensity+sigma)/(Mean Intensity) threshold = 0.250 Savitsky-Golay smoothing applied to incident beam correction Maximum odd and even order spherical harmonic coefficients = 1 4 Sigma(I) values NOT rescaled 5318 Reflections employed for parameter determination Effective data to parameter ratio = 5.56 R(int) = 0.1160 before parameter refinement Cycle R(decay) R(absor) 1 0.0664 0.0425 2 0.0355 0.0313 3 0.0292 0.0271 4 0.0260 0.0248 5 0.0241 0.0234 6 0.0229 0.0225 7 0.0222 0.0219 8 0.0217 0.0216 9 0.0214 0.0213 10 0.0212 0.0211 R(int) = 0.0211 after parameter refinement Batch R(int) Factor range Sigma(ib) Sigma(db) K(sigI) Total I>2sig(I) 1 0.0214 0.679 - 1.262 0.1184 0.0636 1.000 3555 2927 2 0.0231 0.802 - 1.585 0.0983 0.0977 1.000 2535 2059 3 0.0228 0.747 - 1.734 0.1738 0.0752 1.000 1311 1058 Sigma(ib) and sigma(db) are the square roots of the variances of the normalized incident and diffracted beam correction factors. K(sigI) multiplies the sigma(I) values for the batch in question. Background contribution to sig(I) = 0.0000 times mean intensity 2-theta dependent absorption corrections not applied 7401 Corrected reflections written to file MA105AM.HKL Maximum and minimum effective transmission: 1.000000 0.660350 ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6959 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 23.36 _reflns_number_total 2365 _reflns_number_gt 2124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; A molecule of acetone lies in a twofold axis and therefore only one half was refined, the other half being generated by the symmetry operation -x,y,-z-1/2. 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^)+(0.0275P)^2^+2.6391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2365 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0497 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C52 C 0.04922(16) -0.2347(6) -0.2180(3) 0.0733(11) Uani 1 1 d . . . H52A H 0.0499 -0.2883 -0.2658 0.110 Uiso 1 1 calc R . . H52B H 0.0509 -0.3349 -0.1809 0.110 Uiso 1 1 calc R . . H52C H 0.0787 -0.1513 -0.1866 0.110 Uiso 1 1 calc R . . C51 C 0.0000 -0.1257(7) -0.2500 0.0488(11) Uani 1 2 d S . . O51 O 0.0000 0.0467(5) -0.2500 0.0505(8) Uani 1 2 d S . . Mo1 Mo 0.106951(9) 0.18715(3) 0.017814(15) 0.03138(9) Uani 1 1 d . . . Br1 Br 0.169630(12) -0.09644(5) 0.03750(2) 0.04982(12) Uani 1 1 d . . . C1 C 0.04943(12) 0.0038(5) -0.03831(18) 0.0378(7) Uani 1 1 d . . . O1 O 0.01663(9) -0.1078(3) -0.06779(15) 0.0561(6) Uani 1 1 d . . . C2 C 0.10501(11) 0.0817(5) 0.1146(2) 0.0469(8) Uani 1 1 d . . . O2 O 0.10243(9) 0.0116(5) 0.16964(16) 0.0770(8) Uani 1 1 d . . . N1 N 0.18355(9) 0.3509(3) 0.08093(15) 0.0388(6) Uani 1 1 d . . . N2 N 0.12219(9) 0.2779(3) -0.08454(15) 0.0371(6) Uani 1 1 d . . . N3 N 0.09755(12) 0.2587(4) -0.17040(17) 0.0461(7) Uani 1 1 d . . . C3 C 0.02928(12) 0.3505(5) -0.0683(2) 0.0510(9) Uani 1 1 d . . . H3A H 0.0193 0.3737 -0.1273 0.061 Uiso 1 1 calc R . . H3B H 0.0001 0.3193 -0.0614 0.061 Uiso 1 1 calc R . . C4 C 0.06819(13) 0.4660(5) -0.0058(2) 0.0499(8) Uani 1 1 d . . . H4 H 0.0812 0.5784 -0.0207 0.060 Uiso 1 1 calc R . . C5 C 0.08365(14) 0.4243(5) 0.0790(2) 0.0587(10) Uani 1 1 d . . . H5A H 0.0561 0.3949 0.0902 0.070 Uiso 1 1 calc R . . H5B H 0.1119 0.5003 0.1235 0.070 Uiso 1 1 calc R . . C11 C 0.21529(13) 0.3761(5) 0.1659(2) 0.0489(8) Uani 1 1 d . . . H11 H 0.2037 0.3367 0.2018 0.059 Uiso 1 1 calc R . . C12 C 0.26400(13) 0.4572(5) 0.2023(2) 0.0593(9) Uani 1 1 d . . . H12 H 0.2853 0.4699 0.2616 0.071 Uiso 1 1 calc R . . C13 C 0.28052(13) 0.5187(5) 0.1495(2) 0.0619(10) Uani 1 1 d . . . H13 H 0.3133 0.5750 0.1727 0.074 Uiso 1 1 calc R . . C14 C 0.24925(12) 0.4980(5) 0.0633(2) 0.0526(9) Uani 1 1 d . . . H14 H 0.2602 0.5412 0.0270 0.063 Uiso 1 1 calc R . . C15 C 0.20099(11) 0.4123(4) 0.0298(2) 0.0384(7) Uani 1 1 d . . . C16 C 0.16606(11) 0.3762(4) -0.0612(2) 0.0387(7) Uani 1 1 d . . . C17 C 0.16865(15) 0.4189(5) -0.1344(2) 0.0544(9) Uani 1 1 d . . . H17 H 0.1947 0.4862 -0.1366 0.065 Uiso 1 1 calc R . . C18 C 0.12469(15) 0.3398(5) -0.2012(2) 0.0545(9) Uani 1 1 d . . . H18 H 0.1152 0.3420 -0.2586 0.065 Uiso 1 1 calc R . . H3 H 0.0708(13) 0.199(5) -0.193(2) 0.041(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C52 0.084(3) 0.063(3) 0.079(3) 0.009(2) 0.047(2) 0.017(2) C51 0.063(3) 0.046(3) 0.038(2) 0.000 0.027(2) 0.000 O51 0.0529(19) 0.042(2) 0.0441(18) 0.000 0.0168(15) 0.000 Mo1 0.02830(14) 0.03210(16) 0.03816(15) 0.00432(11) 0.02042(12) 0.00404(10) Br1 0.0450(2) 0.0376(2) 0.0768(2) 0.00845(16) 0.03874(18) 0.01153(14) C1 0.0341(16) 0.0402(18) 0.0438(17) 0.0082(15) 0.0236(14) 0.0079(15) O1 0.0429(13) 0.0521(15) 0.0700(16) -0.0034(12) 0.0270(12) -0.0132(12) C2 0.0283(16) 0.068(2) 0.0417(18) 0.0084(16) 0.0161(15) 0.0076(15) O2 0.0547(15) 0.127(3) 0.0553(15) 0.0420(16) 0.0326(13) 0.0160(16) N1 0.0380(13) 0.0346(15) 0.0428(15) -0.0035(11) 0.0204(12) -0.0002(11) N2 0.0394(14) 0.0360(14) 0.0399(14) 0.0038(11) 0.0234(12) 0.0046(12) N3 0.0530(18) 0.0426(17) 0.0413(16) 0.0025(13) 0.0238(15) -0.0007(15) C3 0.0420(18) 0.048(2) 0.064(2) 0.0194(17) 0.0282(18) 0.0209(16) C4 0.051(2) 0.0340(18) 0.073(2) 0.0084(17) 0.0381(19) 0.0139(16) C5 0.058(2) 0.058(2) 0.076(3) -0.0140(19) 0.045(2) 0.0073(17) C11 0.0471(19) 0.049(2) 0.051(2) -0.0020(16) 0.0254(17) 0.0014(16) C12 0.046(2) 0.056(2) 0.057(2) -0.0103(18) 0.0137(18) -0.0047(17) C13 0.0372(19) 0.057(2) 0.074(3) -0.007(2) 0.0162(19) -0.0051(17) C14 0.0417(18) 0.045(2) 0.080(3) 0.0022(18) 0.0383(19) -0.0001(16) C15 0.0346(16) 0.0274(16) 0.060(2) 0.0010(14) 0.0293(16) 0.0033(12) C16 0.0421(18) 0.0302(16) 0.0545(19) 0.0066(14) 0.0326(16) 0.0072(14) C17 0.068(2) 0.045(2) 0.071(2) 0.0041(18) 0.051(2) 0.0000(18) C18 0.081(3) 0.051(2) 0.0464(19) 0.0069(17) 0.044(2) 0.0042(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C52 C51 1.483(5) . ? C51 O51 1.213(5) . ? C51 C52 1.483(5) 2_554 ? Mo1 C2 1.944(3) . ? Mo1 C1 1.958(3) . ? Mo1 C4 2.203(3) . ? Mo1 N2 2.233(2) . ? Mo1 N1 2.269(3) . ? Mo1 C5 2.308(3) . ? Mo1 C3 2.318(3) . ? Mo1 Br1 2.6306(12) . ? C1 O1 1.148(4) . ? C2 O2 1.156(4) . ? N1 C11 1.340(4) . ? N1 C15 1.355(4) . ? N2 C16 1.341(4) . ? N2 N3 1.345(3) . ? N3 C18 1.333(4) . ? C3 C4 1.388(5) . ? C4 C5 1.394(5) . ? C11 C12 1.371(5) . ? C12 C13 1.362(5) . ? C13 C14 1.354(5) . ? C14 C15 1.379(4) . ? C15 C16 1.449(4) . ? C16 C17 1.410(4) . ? C17 C18 1.360(5) . ? 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 O51 C51 C52 121.1(2) . 2_554 ? O51 C51 C52 121.1(2) . . ? C52 C51 C52 117.8(5) 2_554 . ? C2 Mo1 C1 77.80(13) . . ? C2 Mo1 C4 104.75(13) . . ? C1 Mo1 C4 104.76(13) . . ? C2 Mo1 N2 169.80(11) . . ? C1 Mo1 N2 104.98(11) . . ? C4 Mo1 N2 84.19(11) . . ? C2 Mo1 N1 103.53(11) . . ? C1 Mo1 N1 168.20(10) . . ? C4 Mo1 N1 86.36(12) . . ? N2 Mo1 N1 71.72(9) . . ? C2 Mo1 C5 71.14(14) . . ? C1 Mo1 C5 108.89(13) . . ? C4 Mo1 C5 35.90(13) . . ? N2 Mo1 C5 116.27(11) . . ? N1 Mo1 C5 82.40(12) . . ? C2 Mo1 C3 108.02(12) . . ? C1 Mo1 C3 71.07(13) . . ? C4 Mo1 C3 35.65(12) . . ? N2 Mo1 C3 82.09(11) . . ? N1 Mo1 C3 118.80(12) . . ? C5 Mo1 C3 61.32(13) . . ? C2 Mo1 Br1 86.79(10) . . ? C1 Mo1 Br1 86.65(10) . . ? C4 Mo1 Br1 165.12(9) . . ? N2 Mo1 Br1 83.61(6) . . ? N1 Mo1 Br1 81.74(8) . . ? C5 Mo1 Br1 148.85(10) . . ? C3 Mo1 Br1 149.23(9) . . ? O1 C1 Mo1 177.0(3) . . ? O2 C2 Mo1 176.6(3) . . ? C11 N1 C15 117.3(3) . . ? C11 N1 Mo1 124.9(2) . . ? C15 N1 Mo1 117.54(19) . . ? C16 N2 N3 105.8(2) . . ? C16 N2 Mo1 118.33(19) . . ? N3 N2 Mo1 135.9(2) . . ? C18 N3 N2 111.3(3) . . ? C4 C3 Mo1 67.65(18) . . ? C3 C4 C5 116.0(3) . . ? C3 C4 Mo1 76.70(19) . . ? C5 C4 Mo1 76.13(19) . . ? C4 C5 Mo1 67.97(18) . . ? N1 C11 C12 123.2(3) . . ? C13 C12 C11 118.4(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 119.4(3) . . ? N1 C15 C14 121.7(3) . . ? N1 C15 C16 115.2(2) . . ? C14 C15 C16 123.1(3) . . ? N2 C16 C17 109.7(3) . . ? N2 C16 C15 117.1(2) . . ? C17 C16 C15 133.2(3) . . ? C18 C17 C16 104.8(3) . . ? N3 C18 C17 108.3(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.446 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.056 #===END data_c_3_thf_ma111cm _database_code_depnum_ccdc_archive 'CCDC 858713' #TrackingRef '- Molybdenum_and_tungsten_REVISED_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Cl Mo N3 O3' _chemical_formula_weight 459.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.104(3) _cell_length_b 10.941(4) _cell_length_c 12.147(4) _cell_angle_alpha 80.805(5) _cell_angle_beta 72.521(4) _cell_angle_gamma 82.904(5) _cell_volume 1010.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 899 _cell_measurement_theta_min 3.372 _cell_measurement_theta_max 23.233 _exptl_crystal_description PRISM _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805495 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS - Bruker area detector absorption corrections #----------------------------------------------------- Laue group number 1 selected Laue group numbers: [1] -1 [8] -3m (rhombohedral axes) [2] 2/m (Y unique) [9] -31m (Z unique) [3] mmm [10] -3m1 (Z unique) [4] 4/m (Z unique) [11] 6/m (Z unique) [5] 4/mmm (Z unique) [12] 6/mmm (Z unique) [6] -3 (rhombohedral axes) [13] m3 [7] -3 (Z unique) [14] m3m Friedel opposites treated as equivalent for parameter fitting Reading batch 1 from file MA111C1.raw Reading batch 2 from file MA111C2.raw Reading batch 3 from file MA111C3.raw Mean and maximum errors in direction cosine check function = 0.001 0.003 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Maximum 2-theta = 46.56 degrees 4614 Reflections of which 2874 unique; 7.23 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 1379 1250 245 0 0 0 0 0 0 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 167 64 66 47 49 286 286 297 1612 Settings for parameter refinement: (Intensity/sigma) threshold = 5.000 (Intensity+sigma)/(Mean Intensity) threshold = 0.250 Savitsky-Golay smoothing applied to incident beam correction Maximum odd and even order spherical harmonic coefficients = 1 4 Sigma(I) values NOT rescaled 2872 Reflections employed for parameter determination Effective data to parameter ratio = 4.60 R(int) = 0.0401 before parameter refinement Cycle R(decay) R(absor) 1 0.0250 0.0207 2 0.0184 0.0179 3 0.0171 0.0170 4 0.0165 0.0165 5 0.0162 0.0163 6 0.0160 0.0162 7 0.0160 0.0162 8 0.0160 0.0162 9 0.0160 0.0162 10 0.0160 0.0162 R(int) = 0.0162 after parameter refinement Batch R(int) Factor range Sigma(ib) Sigma(db) K(sigI) Total I>2sig(I) 1 0.0159 0.813 - 1.092 0.0524 0.0364 1.000 2204 1271 2 0.0157 0.869 - 1.285 0.0547 0.0372 1.000 1592 1050 3 0.0181 0.856 - 1.058 0.0305 0.0341 1.000 818 672 Sigma(ib) and sigma(db) are the square roots of the variances of the normalized incident and diffracted beam correction factors. K(sigI) multiplies the sigma(I) values for the batch in question. Background contribution to sig(I) = 0.0000 times mean intensity 2-theta dependent absorption corrections not applied 4614 Corrected reflections written to file MA111CM.HKL Maximum and minimum effective transmission: 1.000000 0.805495 ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4614 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2874 _reflns_number_gt 2656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.3162P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2874 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.55168(3) 0.752781(18) 0.797471(17) 0.03386(10) Uani 1 1 d . . . Cl1 Cl 0.75237(9) 0.74737(6) 0.59665(5) 0.04519(17) Uani 1 1 d . . . N1 N 0.5718(3) 0.96016(19) 0.74269(18) 0.0379(5) Uani 1 1 d . . . N2 N 0.3580(3) 0.82200(18) 0.70220(17) 0.0363(5) Uani 1 1 d . . . N3 N 0.2297(3) 0.7730(2) 0.6797(2) 0.0438(6) Uani 1 1 d . . . C1 C 0.5602(4) 0.5723(3) 0.8044(2) 0.0476(7) Uani 1 1 d . . . O1 O 0.5720(3) 0.46544(19) 0.8062(2) 0.0714(6) Uani 1 1 d . . . C2 C 0.7541(4) 0.7089(3) 0.8557(2) 0.0516(7) Uani 1 1 d . . . O2 O 0.8743(3) 0.6814(3) 0.8901(2) 0.0839(8) Uani 1 1 d . . . C3 C 0.3131(4) 0.6775(3) 0.9399(2) 0.0524(7) Uani 1 1 d . . . H3A H 0.2116 0.6700 0.9156 0.063 Uiso 1 1 calc R . . H3B H 0.3357 0.6092 0.9965 0.063 Uiso 1 1 calc R . . C4 C 0.3402(4) 0.7970(3) 0.9563(2) 0.0491(7) Uani 1 1 d . . . C5 C 0.4960(4) 0.8040(3) 0.9830(2) 0.0531(7) Uani 1 1 d . . . H5A H 0.5241 0.7395 1.0408 0.064 Uiso 1 1 calc R . . H5B H 0.5236 0.8859 0.9891 0.064 Uiso 1 1 calc R . . C6 C 0.2106(4) 0.9083(3) 0.9492(3) 0.0672(9) Uani 1 1 d . . . H6A H 0.1468 0.8975 0.8968 0.101 Uiso 1 1 calc R . . H6B H 0.2712 0.9822 0.9210 0.101 Uiso 1 1 calc R . . H6C H 0.1318 0.9155 1.0251 0.101 Uiso 1 1 calc R . . C11 C 0.6881(4) 1.0266(3) 0.7607(3) 0.0520(7) Uani 1 1 d . . . H11 H 0.7616 0.9872 0.8037 0.062 Uiso 1 1 calc R . . C12 C 0.7028(5) 1.1492(3) 0.7187(3) 0.0648(9) Uani 1 1 d . . . H12 H 0.7837 1.1920 0.7343 0.078 Uiso 1 1 calc R . . C13 C 0.5988(5) 1.2089(3) 0.6537(3) 0.0636(9) Uani 1 1 d . . . H13 H 0.6074 1.2927 0.6251 0.076 Uiso 1 1 calc R . . C14 C 0.4811(4) 1.1433(2) 0.6311(2) 0.0489(7) Uani 1 1 d . . . H14 H 0.4103 1.1815 0.5858 0.059 Uiso 1 1 calc R . . C15 C 0.4697(3) 1.0193(2) 0.6771(2) 0.0372(6) Uani 1 1 d . . . C16 C 0.3467(3) 0.9423(2) 0.6603(2) 0.0356(6) Uani 1 1 d . . . C17 C 0.2089(4) 0.9698(3) 0.6115(3) 0.0497(7) Uani 1 1 d . . . H17 H 0.1731 1.0465 0.5769 0.060 Uiso 1 1 calc R . . C18 C 0.1383(4) 0.8594(3) 0.6258(3) 0.0525(7) Uani 1 1 d . . . H18 H 0.0434 0.8464 0.6022 0.063 Uiso 1 1 calc R . . O90 O 0.2087(4) 0.5186(2) 0.7097(2) 0.0849(8) Uani 1 1 d . . . C91 C 0.1581(6) 0.4275(4) 0.8070(4) 0.0924(13) Uani 1 1 d . . . H91A H 0.0910 0.4660 0.8751 0.111 Uiso 1 1 calc R . . H91B H 0.2592 0.3804 0.8238 0.111 Uiso 1 1 calc R . . C92 C 0.0509(6) 0.3450(4) 0.7756(4) 0.1065(16) Uani 1 1 d . . . H92A H 0.1101 0.2628 0.7686 0.128 Uiso 1 1 calc R . . H92B H -0.0600 0.3377 0.8346 0.128 Uiso 1 1 calc R . . C93 C 0.0255(6) 0.4032(5) 0.6634(4) 0.1061(16) Uani 1 1 d . . . H93A H 0.0346 0.3410 0.6127 0.127 Uiso 1 1 calc R . . H93B H -0.0872 0.4492 0.6746 0.127 Uiso 1 1 calc R . . C94 C 0.1641(7) 0.4860(4) 0.6147(4) 0.0937(13) Uani 1 1 d . . . H94A H 0.2637 0.4446 0.5635 0.112 Uiso 1 1 calc R . . H94B H 0.1250 0.5597 0.5703 0.112 Uiso 1 1 calc R . . H3 H 0.225(4) 0.696(3) 0.698(2) 0.050(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03478(15) 0.03276(14) 0.03603(14) -0.00271(9) -0.01407(10) -0.00264(9) Cl1 0.0444(4) 0.0495(4) 0.0403(4) -0.0064(3) -0.0104(3) -0.0020(3) N1 0.0385(12) 0.0358(12) 0.0433(12) -0.0105(9) -0.0137(10) -0.0060(10) N2 0.0335(12) 0.0343(12) 0.0435(12) -0.0029(9) -0.0140(10) -0.0073(9) N3 0.0431(14) 0.0413(14) 0.0524(14) 0.0009(11) -0.0215(11) -0.0133(11) C1 0.0473(17) 0.0457(19) 0.0509(17) -0.0012(13) -0.0183(14) -0.0030(13) O1 0.0851(17) 0.0333(13) 0.0968(18) 0.0000(11) -0.0342(14) 0.0006(11) C2 0.0501(18) 0.0588(19) 0.0467(16) -0.0032(13) -0.0169(14) -0.0049(14) O2 0.0526(15) 0.123(2) 0.0809(17) 0.0026(15) -0.0397(13) 0.0038(14) C3 0.0465(17) 0.064(2) 0.0428(15) 0.0030(13) -0.0087(13) -0.0125(14) C4 0.0452(17) 0.0586(19) 0.0400(15) -0.0101(13) -0.0063(13) -0.0007(14) C5 0.063(2) 0.0585(19) 0.0395(15) -0.0111(13) -0.0160(14) -0.0031(15) C6 0.059(2) 0.077(2) 0.0560(19) -0.0149(16) -0.0072(16) 0.0161(17) C11 0.0541(18) 0.0534(18) 0.0574(18) -0.0123(14) -0.0223(15) -0.0148(15) C12 0.074(2) 0.058(2) 0.072(2) -0.0138(17) -0.0219(19) -0.0325(18) C13 0.083(2) 0.0379(17) 0.070(2) -0.0039(15) -0.0172(19) -0.0205(17) C14 0.0583(18) 0.0374(15) 0.0518(16) -0.0053(12) -0.0168(14) -0.0050(13) C15 0.0393(15) 0.0322(14) 0.0388(14) -0.0074(11) -0.0081(12) -0.0018(11) C16 0.0358(14) 0.0314(14) 0.0385(13) -0.0021(10) -0.0101(11) -0.0034(11) C17 0.0442(17) 0.0461(17) 0.0593(18) 0.0066(13) -0.0234(14) -0.0014(13) C18 0.0443(17) 0.0624(19) 0.0585(18) 0.0023(14) -0.0284(14) -0.0116(15) O90 0.123(2) 0.0544(14) 0.0956(18) 0.0050(13) -0.0542(17) -0.0360(15) C91 0.117(4) 0.063(2) 0.109(3) 0.013(2) -0.053(3) -0.028(2) C92 0.106(4) 0.092(3) 0.110(4) -0.014(3) 0.003(3) -0.051(3) C93 0.083(3) 0.143(4) 0.097(3) -0.061(3) 0.000(3) -0.033(3) C94 0.135(4) 0.068(2) 0.088(3) -0.011(2) -0.037(3) -0.029(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.953(3) . ? Mo1 C1 1.957(3) . ? Mo1 N2 2.212(2) . ? Mo1 C4 2.236(3) . ? Mo1 N1 2.272(2) . ? Mo1 C5 2.307(3) . ? Mo1 C3 2.311(3) . ? Mo1 Cl1 2.4976(9) . ? N1 C11 1.345(3) . ? N1 C15 1.355(3) . ? N2 C16 1.336(3) . ? N2 N3 1.341(3) . ? N3 C18 1.339(4) . ? C1 O1 1.158(3) . ? C2 O2 1.160(4) . ? C3 C4 1.407(4) . ? C4 C5 1.408(4) . ? C4 C6 1.515(4) . ? C11 C12 1.363(4) . ? C12 C13 1.363(5) . ? C13 C14 1.375(4) . ? C14 C15 1.385(4) . ? C15 C16 1.459(4) . ? C16 C17 1.395(4) . ? C17 C18 1.365(4) . ? O90 C91 1.411(4) . ? O90 C94 1.416(5) . ? C91 C92 1.490(6) . ? C92 C93 1.471(6) . ? C93 C94 1.454(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 81.82(12) . . ? C2 Mo1 N2 168.85(10) . . ? C1 Mo1 N2 103.36(10) . . ? C2 Mo1 C4 103.07(12) . . ? C1 Mo1 C4 104.48(11) . . ? N2 Mo1 C4 85.35(10) . . ? C2 Mo1 N1 100.76(10) . . ? C1 Mo1 N1 166.12(10) . . ? N2 Mo1 N1 71.87(7) . . ? C4 Mo1 N1 88.32(9) . . ? C2 Mo1 C5 68.82(12) . . ? C1 Mo1 C5 109.40(11) . . ? N2 Mo1 C5 117.56(10) . . ? C4 Mo1 C5 36.06(10) . . ? N1 Mo1 C5 84.08(9) . . ? C2 Mo1 C3 107.92(12) . . ? C1 Mo1 C3 70.16(11) . . ? N2 Mo1 C3 83.19(10) . . ? C4 Mo1 C3 35.99(10) . . ? N1 Mo1 C3 121.06(9) . . ? C5 Mo1 C3 61.58(11) . . ? C2 Mo1 Cl1 87.80(9) . . ? C1 Mo1 Cl1 85.48(8) . . ? N2 Mo1 Cl1 82.84(6) . . ? C4 Mo1 Cl1 166.07(8) . . ? N1 Mo1 Cl1 81.02(5) . . ? C5 Mo1 Cl1 149.31(8) . . ? C3 Mo1 Cl1 148.13(8) . . ? C11 N1 C15 117.2(2) . . ? C11 N1 Mo1 125.17(19) . . ? C15 N1 Mo1 117.29(15) . . ? C16 N2 N3 105.6(2) . . ? C16 N2 Mo1 118.98(16) . . ? N3 N2 Mo1 135.20(17) . . ? C18 N3 N2 111.2(2) . . ? O1 C1 Mo1 177.3(3) . . ? O2 C2 Mo1 179.2(3) . . ? C4 C3 Mo1 69.12(15) . . ? C3 C4 C5 114.3(3) . . ? C3 C4 C6 123.0(3) . . ? C5 C4 C6 122.8(3) . . ? C3 C4 Mo1 74.90(16) . . ? C5 C4 Mo1 74.71(16) . . ? C6 C4 Mo1 120.2(2) . . ? C4 C5 Mo1 69.22(15) . . ? N1 C11 C12 122.8(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C14 118.9(3) . . ? C13 C14 C15 118.9(3) . . ? N1 C15 C14 122.2(2) . . ? N1 C15 C16 114.7(2) . . ? C14 C15 C16 123.1(2) . . ? N2 C16 C17 110.5(2) . . ? N2 C16 C15 116.9(2) . . ? C17 C16 C15 132.5(2) . . ? C18 C17 C16 104.7(2) . . ? N3 C18 C17 107.9(2) . . ? C91 O90 C94 109.5(3) . . ? O90 C91 C92 106.2(3) . . ? C93 C92 C91 106.3(3) . . ? C94 C93 C92 104.5(4) . . ? O90 C94 C93 106.8(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.233 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.065 #===END data_C_5_ma116am _database_code_depnum_ccdc_archive 'CCDC 858714' #TrackingRef '- Molybdenum_and_tungsten_REVISED_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H15 I2 N3 O4 W' _chemical_formula_weight 738.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.875(7) _cell_length_b 10.711(4) _cell_length_c 11.668(8) _cell_angle_alpha 78.737(18) _cell_angle_beta 81.722(19) _cell_angle_gamma 78.658(18) _cell_volume 1060.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 970 _cell_measurement_theta_min 2.795 _cell_measurement_theta_max 23.689 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 8.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603004 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS - Bruker area detector absorption corrections #----------------------------------------------------- Laue group number 1 selected Laue group numbers: [1] -1 [8] -3m (rhombohedral axes) [2] 2/m (Y unique) [9] -31m (Z unique) [3] mmm [10] -3m1 (Z unique) [4] 4/m (Z unique) [11] 6/m (Z unique) [5] 4/mmm (Z unique) [12] 6/mmm (Z unique) [6] -3 (rhombohedral axes) [13] m3 [7] -3 (Z unique) [14] m3m Friedel opposites treated as equivalent for parameter fitting Reading batch 1 from file MA116A1.raw Reading batch 2 from file MA116A2.raw Reading batch 3 from file MA116A3.raw Mean and maximum errors in direction cosine check function = 0.004 0.016 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Maximum 2-theta = 47.01 degrees 4808 Reflections of which 3086 unique; 3.84 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 1562 1326 198 0 0 0 0 0 0 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 292 153 105 112 91 516 346 272 1199 Settings for parameter refinement: (Intensity/sigma) threshold = 5.000 (Intensity+sigma)/(Mean Intensity) threshold = 0.250 Savitsky-Golay smoothing applied to incident beam correction Maximum odd and even order spherical harmonic coefficients = 1 4 Sigma(I) values NOT rescaled 2591 Reflections employed for parameter determination Effective data to parameter ratio = 2.14 R(int) = 0.1132 before parameter refinement Cycle R(decay) R(absor) 1 0.0732 0.0500 2 0.0407 0.0350 3 0.0326 0.0298 4 0.0287 0.0272 5 0.0265 0.0256 6 0.0251 0.0246 7 0.0242 0.0239 8 0.0236 0.0233 9 0.0232 0.0229 10 0.0228 0.0226 R(int) = 0.0226 after parameter refinement Batch R(int) Factor range Sigma(ib) Sigma(db) K(sigI) Total I>2sig(I) 1 0.0247 0.594 - 1.395 0.0635 0.0927 1.000 2325 1233 2 0.0223 0.733 - 1.768 0.0997 0.0983 1.000 1644 993 3 0.0267 0.808 - 2.077 0.1412 0.1259 1.000 839 620 Sigma(ib) and sigma(db) are the square roots of the variances of the normalized incident and diffracted beam correction factors. K(sigI) multiplies the sigma(I) values for the batch in question. Background contribution to sig(I) = 0.0000 times mean intensity 2-theta dependent absorption corrections not applied 4808 Corrected reflections written to file MA116AM.HKL Maximum and minimum effective transmission: 1.000000 0.603004 ; _diffrn_ambient_temperature 299(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4808 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.89 _reflns_number_total 3186 _reflns_number_gt 2668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3086 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 W1 W 0.32936(4) 0.30745(3) 0.21350(3) 0.04416(17) Uani 1 1 d . . . I1 I 0.24031(10) 0.05711(7) 0.25011(7) 0.0773(3) Uani 1 1 d . . . I2 I 0.16815(7) 0.33635(6) 0.44196(5) 0.0583(2) Uani 1 1 d . . . N1 N 0.5452(8) 0.2353(7) 0.3104(6) 0.0495(18) Uani 1 1 d . . . N2 N 0.4083(8) 0.4724(6) 0.2524(6) 0.0474(17) Uani 1 1 d . . . N3 N 0.3455(11) 0.6021(8) 0.2357(7) 0.065(2) Uani 1 1 d . . . H3 H 0.237(13) 0.627(11) 0.199(10) 0.078 Uiso 1 1 d . . . C1 C 0.4663(11) 0.2153(10) 0.0906(9) 0.060(2) Uani 1 1 d . . . O1 O 0.5488(11) 0.1643(10) 0.0221(8) 0.102(3) Uani 1 1 d . . . C2 C 0.3276(11) 0.4273(10) 0.0639(8) 0.059(2) Uani 1 1 d . . . O2 O 0.3254(9) 0.4995(8) -0.0254(6) 0.082(2) Uani 1 1 d . . . C3 C 0.1057(12) 0.3456(10) 0.1753(9) 0.059(2) Uani 1 1 d . . . O3 O -0.0192(9) 0.3653(9) 0.1536(8) 0.092(3) Uani 1 1 d . . . C11 C 0.6101(12) 0.1102(10) 0.3395(10) 0.068(3) Uani 1 1 d . . . H11 H 0.5678 0.0478 0.3158 0.082 Uiso 1 1 calc R . . C12 C 0.7386(13) 0.0691(11) 0.4040(11) 0.077(3) Uani 1 1 d . . . H12 H 0.7792 -0.0182 0.4239 0.093 Uiso 1 1 calc R . . C13 C 0.8022(13) 0.1625(14) 0.4366(11) 0.083(4) Uani 1 1 d . . . H13 H 0.8878 0.1382 0.4786 0.100 Uiso 1 1 calc R . . C14 C 0.7406(11) 0.2916(11) 0.4076(8) 0.063(3) Uani 1 1 d . . . H14 H 0.7847 0.3549 0.4281 0.076 Uiso 1 1 calc R . . C15 C 0.6100(10) 0.3248(9) 0.3467(8) 0.051(2) Uani 1 1 d . . . C16 C 0.5294(10) 0.4586(9) 0.3132(7) 0.048(2) Uani 1 1 d . . . C17 C 0.5444(13) 0.5782(10) 0.3373(9) 0.064(3) Uani 1 1 d . . . H17 H 0.6171 0.5956 0.3793 0.076 Uiso 1 1 calc R . . C18 C 0.4275(14) 0.6642(10) 0.2850(10) 0.072(3) Uani 1 1 d . . . H18 H 0.4086 0.7529 0.2841 0.087 Uiso 1 1 calc R . . O90 O 1.0688(10) 0.6970(9) 0.1438(8) 0.097(3) Uani 1 1 d . . . C91 C 0.926(3) 0.679(2) 0.2067(19) 0.214(15) Uani 1 1 d . . . H91A H 0.9388 0.6478 0.2891 0.257 Uiso 1 1 calc R . . H91B H 0.8865 0.6138 0.1776 0.257 Uiso 1 1 calc R . . C92 C 0.818(2) 0.7978(16) 0.1940(18) 0.146(8) Uani 1 1 d . . . H92A H 0.7216 0.7853 0.1711 0.176 Uiso 1 1 calc R . . H92B H 0.7958 0.8313 0.2672 0.176 Uiso 1 1 calc R . . C93 C 0.888(2) 0.880(2) 0.108(2) 0.167(9) Uani 1 1 d . . . H93A H 0.8955 0.9570 0.1382 0.201 Uiso 1 1 calc R . . H93B H 0.8273 0.9070 0.0420 0.201 Uiso 1 1 calc R . . C94 C 1.0466(15) 0.8129(14) 0.0693(12) 0.097(4) Uani 1 1 d . . . H94A H 1.0529 0.7997 -0.0113 0.116 Uiso 1 1 calc R . . H94B H 1.1240 0.8635 0.0745 0.116 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0405(2) 0.0460(3) 0.0473(2) -0.01055(16) -0.00521(15) -0.00776(16) I1 0.0938(6) 0.0549(4) 0.0922(5) -0.0175(4) -0.0146(4) -0.0264(4) I2 0.0508(4) 0.0725(4) 0.0547(4) -0.0182(3) 0.0038(3) -0.0185(3) N1 0.035(4) 0.056(5) 0.056(4) -0.008(4) -0.002(3) -0.008(3) N2 0.052(4) 0.039(4) 0.052(4) -0.003(3) -0.003(3) -0.016(3) N3 0.080(6) 0.049(5) 0.065(5) -0.006(4) -0.009(4) -0.012(4) C1 0.052(6) 0.070(6) 0.057(5) -0.018(5) 0.002(5) -0.012(5) O1 0.094(6) 0.119(7) 0.093(6) -0.052(6) 0.011(5) 0.002(5) C2 0.053(6) 0.074(7) 0.050(5) -0.011(5) 0.000(4) -0.017(5) O2 0.088(5) 0.101(6) 0.055(4) 0.007(4) -0.012(4) -0.030(5) C3 0.051(6) 0.065(6) 0.063(6) -0.018(5) -0.005(5) -0.013(5) O3 0.046(4) 0.126(7) 0.107(6) -0.023(5) -0.026(4) -0.006(4) C11 0.061(6) 0.055(6) 0.086(7) -0.021(5) -0.012(5) 0.006(5) C12 0.069(7) 0.065(7) 0.089(8) -0.005(6) -0.022(6) 0.009(6) C13 0.051(6) 0.107(10) 0.086(8) -0.001(7) -0.022(6) -0.005(6) C14 0.045(5) 0.084(8) 0.062(6) 0.001(5) -0.014(4) -0.021(5) C15 0.038(5) 0.060(6) 0.056(5) -0.008(4) 0.002(4) -0.014(4) C16 0.047(5) 0.055(5) 0.044(5) -0.001(4) -0.001(4) -0.020(4) C17 0.075(7) 0.059(6) 0.068(6) -0.012(5) -0.015(5) -0.030(5) C18 0.092(8) 0.051(6) 0.078(7) -0.017(5) -0.008(6) -0.016(6) O90 0.077(5) 0.086(6) 0.099(6) 0.017(5) 0.009(5) 0.004(4) C91 0.21(2) 0.144(16) 0.169(18) 0.075(15) 0.100(18) 0.055(16) C92 0.111(14) 0.107(13) 0.177(18) 0.025(13) 0.039(13) -0.004(11) C93 0.120(15) 0.134(15) 0.19(2) 0.048(15) -0.002(14) 0.020(12) C94 0.082(9) 0.111(11) 0.081(8) 0.012(8) 0.011(7) -0.022(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. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C2 1.955(10) . ? W1 C1 2.022(10) . ? W1 C3 2.042(10) . ? W1 N2 2.170(7) . ? W1 N1 2.290(7) . ? W1 I1 2.8785(13) . ? W1 I2 2.8807(18) . ? N1 C11 1.349(12) . ? N1 C15 1.369(12) . ? N2 C16 1.340(11) . ? N2 N3 1.379(10) . ? N3 C18 1.328(14) . ? C1 O1 1.148(12) . ? C2 O2 1.170(11) . ? C3 O3 1.143(12) . ? C11 C12 1.407(15) . ? C12 C13 1.377(17) . ? C13 C14 1.378(16) . ? C14 C15 1.397(13) . ? C15 C16 1.475(13) . ? C16 C17 1.399(13) . ? C17 C18 1.372(15) . ? O90 C94 1.366(15) . ? O90 C91 1.40(2) . ? C91 C92 1.43(2) . ? C92 C93 1.37(2) . ? C93 C94 1.50(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 W1 C1 72.3(4) . . ? C2 W1 C3 74.3(4) . . ? C1 W1 C3 109.7(4) . . ? C2 W1 N2 76.8(3) . . ? C1 W1 N2 115.7(3) . . ? C3 W1 N2 113.9(3) . . ? C2 W1 N1 123.1(3) . . ? C1 W1 N1 81.1(3) . . ? C3 W1 N1 162.3(3) . . ? N2 W1 N1 71.1(3) . . ? C2 W1 I1 124.0(3) . . ? C1 W1 I1 75.1(3) . . ? C3 W1 I1 75.6(3) . . ? N2 W1 I1 159.20(18) . . ? N1 W1 I1 94.50(19) . . ? C2 W1 I2 130.8(3) . . ? C1 W1 I2 156.8(3) . . ? C3 W1 I2 79.6(3) . . ? N2 W1 I2 76.85(19) . . ? N1 W1 I2 85.33(18) . . ? I1 W1 I2 87.34(3) . . ? C11 N1 C15 117.0(8) . . ? C11 N1 W1 125.0(7) . . ? C15 N1 W1 118.0(6) . . ? C16 N2 N3 106.4(7) . . ? C16 N2 W1 122.0(6) . . ? N3 N2 W1 131.3(6) . . ? C18 N3 N2 109.0(9) . . ? O1 C1 W1 177.4(9) . . ? O2 C2 W1 179.5(9) . . ? O3 C3 W1 179.1(9) . . ? N1 C11 C12 123.4(10) . . ? C13 C12 C11 117.8(10) . . ? C12 C13 C14 120.8(10) . . ? C13 C14 C15 118.2(10) . . ? N1 C15 C14 122.9(9) . . ? N1 C15 C16 113.1(7) . . ? C14 C15 C16 124.0(9) . . ? N2 C16 C17 110.2(8) . . ? N2 C16 C15 115.7(8) . . ? C17 C16 C15 134.0(9) . . ? C18 C17 C16 104.4(9) . . ? N3 C18 C17 110.0(9) . . ? C94 O90 C91 107.8(10) . . ? O90 C91 C92 110.1(15) . . ? C93 C92 C91 105.3(15) . . ? C92 C93 C94 109.0(15) . . ? O90 C94 C93 105.9(11) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 23.89 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.502 _refine_diff_density_min -1.964 _refine_diff_density_rms 0.184 #===END data_Compound_6_ma1691am _database_code_depnum_ccdc_archive 'CCDC 858715' #TrackingRef '- Molybdenum_and_tungsten_REVISED_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Mo2 N6 O4' _chemical_formula_weight 674.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 18.316(10) _cell_length_b 18.316(9) _cell_length_c 42.269(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12280(14) _cell_formula_units_Z 18 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 743 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.39 _exptl_crystal_description PRISM _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6048 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.718393 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS - Bruker Nonius area detector scaling and absorption correction - V2.05 #----------------------------------------------------------------------------- Equivalent reflections defined according to point group -31m Reading batch 1 from file ma1691a1.raw Reading batch 2 from file ma1691a2.raw Reading batch 3 from file ma1691a3.raw Mean and maximum errors in direction cosine check function = 0.000 0.000 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Maximum 2-theta = 46.57 deg. Approximate wavelength = 0.71068 Angstroms #============================================================================= PART 1 - Refinement of parameters to model systematic errors Thresholds should now be specified for excluding reflections from the parameter refinement; these reflections may still be corrected and included in the final output .hkl file 18893 Reflections of which 3455 unique; 15.15 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 35 43 660 493 772 705 248 160 339 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 1623 487 363 214 143 385 104 58 78 Settings for parameter refinement: Maximum resolution = 0.1000 A (Intensity/sigma) threshold = 3.000 Restraint esd for equal adjacent scale factors = 0.0050 Maximum odd and even orders for spherical harmonics = 3 6 5828 Reflections employed for parameter determination Effective data to parameter ratio = 3.65 R(int) = 0.1210 (selected reflections only, before parameter refinement) Cycle R(incid) R(diffr) Mean wt. 1 0.1156 0.1139 0.8737 2 0.1132 0.1129 0.8769 3 0.1129 0.1128 0.8774 4 0.1129 0.1128 0.8776 5 0.1129 0.1128 0.8777 6 0.1129 0.1128 0.8777 7 0.1129 0.1128 0.8777 8 0.1129 0.1128 0.8777 9 0.1129 0.1128 0.8777 10 0.1129 0.1128 0.8777 11 0.1129 0.1129 0.8777 12 0.1129 0.1129 0.8777 13 0.1129 0.1129 0.8777 14 0.1129 0.1129 0.8778 15 0.1129 0.1129 0.8778 R(int) = 0.1129 (selected reflections only, after parameter refinement) #============================================================================= PART 2 - Reject outliers and establish error model Rejected reflections are ignored in the statistics and Postscript plots (except the detector diagnostics) and in the output .hkl file Before applying rejections there are: 18893 total and 3455 unique reflections assuming Friedel's law. Reflections rejected for which |I-|/su > 4.00 Where: su^2 = sigma(I)^2 + ( 0.02000 )^2 (sigma(I) from SAINT) 18296 total and 3429 unique reflections left after |I-|/su test ** Impossible to obtain satisfactory error model ** g = 0.0500 gave best error model; g set to 0.0500 for statistics and data output Run 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 -28.0 0.1567 0.757 - 0.866 0.900 - 1.183 0.898 8785 3946 2 -28.0 0.1576 1.389 - 1.611 0.870 - 1.080 0.804 6237 2758 3 -28.0 0.1551 0.691 - 0.823 0.895 - 1.211 0.809 3274 1400 su = K * Sqrt[ sigma^2(I) + (g)^2 ] where sigma(I) is estimated by SAINT The above statistics are based on all non-rejected data, ignoring reflections without equivalents when estimating R(int) and K. #============================================================================= PART 3 - Output Postscript diagnostics and corrected data Diagnostic plots written to Postscript file sad.eps 18296 Corrected reflections written to file ma1691am.hkl Ratio of minimum to maximum apparent transmission: 0.718393 Lambda/2 correction factor = 0.0015 ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17301 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.44 _reflns_number_total 1967 _reflns_number_gt 1295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Several small peaks were found which probably correspond to solvent or adventitious water disordered in the void along the trigonal axis. Despite repeated attempts it was not possible to obtain a sensible model for this electron density. 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^)+(0.1013P)^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 1967 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 0.79156(6) 0.76857(6) 0.07399(2) 0.0332(4) Uani 1 1 d . . . N2 N 0.6843(5) 0.6515(5) 0.0510(2) 0.033(2) Uani 1 1 d . . . N1 N 0.8422(6) 0.6844(6) 0.0549(2) 0.042(2) Uani 1 1 d . . . N3 N 0.5997(5) 0.6117(5) 0.0533(2) 0.033(2) Uani 1 1 d . . . C1 C 0.8866(8) 0.8421(8) 0.1003(4) 0.062(4) Uani 1 1 d . . . O1 O 0.9402(7) 0.8818(6) 0.1188(4) 0.107(5) Uani 1 1 d . . . C2 C 0.7560(7) 0.8406(7) 0.0937(3) 0.038(3) Uani 1 1 d . . . O2 O 0.7440(5) 0.8915(5) 0.1062(2) 0.057(2) Uani 1 1 d . . . C3 C 0.9023(9) 0.8639(9) 0.0419(4) 0.068(4) Uani 1 1 d . . . H3A H 0.9247 0.9233 0.0463 0.04(3) Uiso 1 1 calc R . . H3B H 0.9451 0.8496 0.0366 0.06(4) Uiso 1 1 calc R . . C4 C 0.8274(9) 0.8233(9) 0.0249(3) 0.058(4) Uani 1 1 d . . . H4 H 0.8207 0.7883 0.0063 0.15(8) Uiso 1 1 calc R . . C5 C 0.7652(8) 0.8402(8) 0.0345(3) 0.049(3) Uani 1 1 d . . . H5A H 0.7112 0.8095 0.0238 0.12(6) Uiso 1 1 calc R . . H5B H 0.7826 0.8987 0.0387 0.03(3) Uiso 1 1 calc R . . C11 C 0.9220(8) 0.7010(9) 0.0578(3) 0.054(4) Uani 1 1 d . . . H11 H 0.9576 0.7442 0.0714 0.02(3) Uiso 1 1 calc R . . C12 C 0.9534(10) 0.6592(10) 0.0423(4) 0.066(4) Uani 1 1 d . . . H12 H 1.0089 0.6725 0.0454 0.05(4) Uiso 1 1 calc R . . C13 C 0.9043(11) 0.5989(11) 0.0225(3) 0.071(5) Uani 1 1 d . . . H13 H 0.9255 0.5706 0.0108 0.06(4) Uiso 1 1 calc R . . C14 C 0.8231(10) 0.5785(9) 0.0194(3) 0.057(4) Uani 1 1 d . . . H14 H 0.7876 0.5348 0.0060 0.03(3) Uiso 1 1 calc R . . C15 C 0.7926(8) 0.6218(8) 0.0360(3) 0.043(3) Uani 1 1 d . . . C16 C 0.7051(8) 0.6015(7) 0.0351(3) 0.038(3) Uani 1 1 d . . . C17 C 0.6311(8) 0.5290(7) 0.0256(3) 0.051(3) Uani 1 1 d . . . H17 H 0.6264 0.4842 0.0137 0.03(3) Uiso 1 1 calc R . . C18 C 0.5693(8) 0.5382(8) 0.0375(3) 0.047(3) Uani 1 1 d . . . H18 H 0.5123 0.4991 0.0352 0.04(3) 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 0.0257(6) 0.0280(6) 0.0447(7) 0.0009(4) 0.0025(4) 0.0125(5) N2 0.030(5) 0.036(5) 0.035(6) 0.004(4) 0.005(4) 0.019(5) N1 0.041(6) 0.040(6) 0.050(6) 0.003(5) 0.008(5) 0.024(5) N3 0.026(5) 0.031(5) 0.040(6) -0.003(4) -0.001(4) 0.012(4) C1 0.035(8) 0.044(8) 0.104(12) -0.014(8) -0.015(8) 0.017(7) O1 0.072(8) 0.069(8) 0.177(14) -0.053(8) -0.064(9) 0.033(7) C2 0.035(7) 0.036(7) 0.046(7) 0.000(6) -0.004(5) 0.019(6) O2 0.059(6) 0.046(5) 0.071(6) -0.007(5) 0.000(5) 0.031(5) C3 0.045(9) 0.041(8) 0.113(13) 0.018(8) 0.031(9) 0.016(7) C4 0.066(10) 0.052(9) 0.058(9) 0.020(7) 0.029(7) 0.031(8) C5 0.056(9) 0.036(7) 0.053(8) 0.015(6) 0.004(7) 0.023(7) C11 0.045(8) 0.059(9) 0.072(10) 0.019(8) 0.008(7) 0.037(8) C12 0.071(11) 0.089(12) 0.073(11) 0.022(9) 0.023(9) 0.065(10) C13 0.107(14) 0.099(13) 0.053(10) 0.013(9) 0.034(9) 0.085(12) C14 0.072(10) 0.060(9) 0.055(9) 0.004(7) 0.013(7) 0.045(8) C15 0.054(8) 0.047(8) 0.039(7) 0.007(6) 0.009(6) 0.033(7) C16 0.063(8) 0.032(6) 0.026(6) 0.001(5) 0.008(5) 0.028(6) C17 0.060(9) 0.037(8) 0.057(8) -0.016(6) -0.003(7) 0.024(7) C18 0.052(8) 0.034(7) 0.049(8) -0.008(6) -0.002(6) 0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.928(12) . ? Mo1 C1 1.933(14) . ? Mo1 N3 2.205(9) 18_654 ? Mo1 C4 2.255(13) . ? Mo1 N2 2.278(9) . ? Mo1 N1 2.306(9) . ? Mo1 C5 2.317(12) . ? Mo1 C3 2.337(13) . ? N2 C16 1.335(14) . ? N2 N3 1.345(11) . ? N1 C15 1.318(15) . ? N1 C11 1.341(15) . ? N3 C18 1.349(14) . ? N3 Mo1 2.205(9) 18_654 ? C1 O1 1.179(16) . ? C2 O2 1.183(13) . ? C3 C4 1.39(2) . ? C4 C5 1.383(18) . ? C11 C12 1.335(18) . ? C12 C13 1.32(2) . ? C13 C14 1.35(2) . ? C14 C15 1.370(17) . ? C15 C16 1.453(16) . ? C16 C17 1.402(17) . ? C17 C18 1.323(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 76.6(5) . . ? C2 Mo1 N3 89.1(4) . 18_654 ? C1 Mo1 N3 90.9(5) . 18_654 ? C2 Mo1 C4 102.5(5) . . ? C1 Mo1 C4 105.0(6) . . ? N3 Mo1 C4 162.0(5) 18_654 . ? C2 Mo1 N2 113.6(4) . . ? C1 Mo1 N2 162.5(5) . . ? N3 Mo1 N2 75.7(3) 18_654 . ? C4 Mo1 N2 87.0(5) . . ? C2 Mo1 N1 174.2(4) . . ? C1 Mo1 N1 98.3(5) . . ? N3 Mo1 N1 88.2(3) 18_654 . ? C4 Mo1 N1 81.4(4) . . ? N2 Mo1 N1 70.6(3) . . ? C2 Mo1 C5 71.8(5) . . ? C1 Mo1 C5 113.0(6) . . ? N3 Mo1 C5 143.9(4) 18_654 . ? C4 Mo1 C5 35.2(4) . . ? N2 Mo1 C5 84.2(4) . . ? N1 Mo1 C5 113.2(4) . . ? C2 Mo1 C3 101.7(5) . . ? C1 Mo1 C3 70.8(6) . . ? N3 Mo1 C3 155.5(5) 18_654 . ? C4 Mo1 C3 35.2(5) . . ? N2 Mo1 C3 118.3(5) . . ? N1 Mo1 C3 78.9(4) . . ? C5 Mo1 C3 60.5(5) . . ? C16 N2 N3 108.1(9) . . ? C16 N2 Mo1 116.8(7) . . ? N3 N2 Mo1 134.2(7) . . ? C15 N1 C11 116.9(11) . . ? C15 N1 Mo1 117.4(8) . . ? C11 N1 Mo1 125.0(9) . . ? N2 N3 C18 107.1(9) . . ? N2 N3 Mo1 119.2(6) . 18_654 ? C18 N3 Mo1 128.8(8) . 18_654 ? O1 C1 Mo1 173.5(15) . . ? O2 C2 Mo1 172.2(10) . . ? C4 C3 Mo1 69.2(7) . . ? C5 C4 C3 115.5(14) . . ? C5 C4 Mo1 74.9(7) . . ? C3 C4 Mo1 75.6(8) . . ? C4 C5 Mo1 69.9(7) . . ? C12 C11 N1 123.9(15) . . ? C13 C12 C11 118.9(15) . . ? C12 C13 C14 119.3(13) . . ? C13 C14 C15 120.3(15) . . ? N1 C15 C14 120.6(12) . . ? N1 C15 C16 115.5(10) . . ? C14 C15 C16 123.8(12) . . ? N2 C16 C17 108.8(10) . . ? N2 C16 C15 118.0(10) . . ? C17 C16 C15 132.1(11) . . ? C18 C17 C16 104.7(11) . . ? C17 C18 N3 111.3(11) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 23.44 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.782 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.180 #===END data_C_7_ma119am _database_code_depnum_ccdc_archive 'CCDC 858716' #TrackingRef '- Molybdenum_and_tungsten_REVISED_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.50 H27 Cl Mo2 N6 O4' _chemical_formula_weight 744.89 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 30.973(12) _cell_length_b 13.498(5) _cell_length_c 15.162(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.442(8) _cell_angle_gamma 90.00 _cell_volume 6213(4) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 852 _cell_measurement_theta_min 2.229 _cell_measurement_theta_max 21.518 _exptl_crystal_description PLATE _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.606560 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; SADABS - Bruker area detector absorption corrections #----------------------------------------------------- Laue group number 2 selected Laue group numbers: [1] -1 [8] -3m (rhombohedral axes) [2] 2/m (Y unique) [9] -31m (Z unique) [3] mmm [10] -3m1 (Z unique) [4] 4/m (Z unique) [11] 6/m (Z unique) [5] 4/mmm (Z unique) [12] 6/mmm (Z unique) [6] -3 (rhombohedral axes) [13] m3 [7] -3 (Z unique) [14] m3m Friedel opposites treated as equivalent for parameter fitting Reading batch 1 from file MA119A1.raw Reading batch 2 from file MA119A2.raw Reading batch 3 from file MA119A3.raw Mean and maximum errors in direction cosine check function = 0.001 0.007 The mean error should not exceed 0.005, and is usually caused by matrix changes during data processing. Maximum 2-theta = 46.80 degrees 14081 Reflections of which 4692 unique; 11.20 data per frame Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 246 1197 1755 1299 190 5 0 0 0 Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf Number of groups: 1203 648 511 392 290 893 305 147 303 Settings for parameter refinement: (Intensity/sigma) threshold = 5.000 (Intensity+sigma)/(Mean Intensity) threshold = 0.250 Savitsky-Golay smoothing applied to incident beam correction Maximum odd and even order spherical harmonic coefficients = 1 4 Sigma(I) values NOT rescaled 5404 Reflections employed for parameter determination Effective data to parameter ratio = 5.92 R(int) = 0.0616 before parameter refinement Cycle R(decay) R(absor) 1 0.0544 0.0529 2 0.0519 0.0519 3 0.0516 0.0517 4 0.0515 0.0516 5 0.0514 0.0515 6 0.0514 0.0515 7 0.0514 0.0515 8 0.0514 0.0515 9 0.0515 0.0515 10 0.0515 0.0515 R(int) = 0.0515 after parameter refinement Batch R(int) Factor range Sigma(ib) Sigma(db) K(sigI) Total I>2sig(I) 1 0.0819 0.776 - 1.346 0.0496 0.0548 1.000 6795 4436 2 0.0716 0.773 - 1.133 0.0753 0.0618 1.000 4796 2975 3 0.0810 0.780 - 1.184 0.0769 0.0717 1.000 2490 1497 Sigma(ib) and sigma(db) are the square roots of the variances of the normalized incident and diffracted beam correction factors. K(sigI) multiplies the sigma(I) values for the batch in question. Background contribution to sig(I) = 0.0000 times mean intensity 2-theta dependent absorption corrections not applied 14081 Corrected reflections written to file MA119AM.HKL Maximum and minimum effective transmission: 1.000000 0.606560 ; _diffrn_ambient_temperature 299(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13725 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 23.33 _reflns_number_total 6888 _reflns_number_gt 4831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(6) _refine_ls_number_reflns 6888 _refine_ls_number_parameters 752 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 0.39733(4) 0.38842(9) 0.31842(7) 0.0347(3) Uani 1 1 d . . . Mo2 Mo 0.33093(5) 0.17130(10) 0.15575(7) 0.0403(4) Uani 1 1 d . . . N1 N 0.4112(4) 0.3484(9) 0.4678(8) 0.042(3) Uani 1 1 d . . . N2 N 0.3451(3) 0.2768(8) 0.3407(7) 0.032(3) Uani 1 1 d . . . N3 N 0.3143(4) 0.2212(9) 0.2861(8) 0.039(3) Uani 1 1 d . . . N4 N 0.3404(4) 0.0187(8) 0.2204(8) 0.044(3) Uani 1 1 d . . . N5 N 0.3976(4) 0.1693(9) 0.2553(7) 0.038(3) Uani 1 1 d . . . N6 N 0.4262(4) 0.2396(9) 0.2952(7) 0.041(3) Uani 1 1 d . . . C1 C 0.4512(6) 0.4615(12) 0.3191(10) 0.050(4) Uani 1 1 d . . . O1 O 0.4837(4) 0.5065(10) 0.3176(8) 0.078(4) Uani 1 1 d . . . C2 C 0.3966(5) 0.4114(11) 0.1906(10) 0.042(4) Uani 1 1 d . . . O2 O 0.4005(4) 0.4281(9) 0.1177(7) 0.066(3) Uani 1 1 d . . . C3 C 0.3951(6) 0.5494(12) 0.3819(10) 0.058(5) Uani 1 1 d . . . H3A H 0.4059 0.5556 0.4462 0.070 Uiso 1 1 calc R . . H3B H 0.4029 0.6047 0.3472 0.070 Uiso 1 1 calc R . . C4 C 0.3529(5) 0.5084(10) 0.3538(10) 0.038(4) Uani 1 1 d . . . C5 C 0.3417(6) 0.4959(12) 0.2616(11) 0.057(5) Uani 1 1 d . . . H5A H 0.3492 0.5498 0.2250 0.068 Uiso 1 1 calc R . . H5B H 0.3131 0.4668 0.2382 0.068 Uiso 1 1 calc R . . C6 C 0.2695(7) 0.1556(11) 0.1038(12) 0.060(5) Uani 1 1 d . . . O6 O 0.2309(5) 0.1497(9) 0.0713(9) 0.083(4) Uani 1 1 d . . . C7 C 0.3127(5) 0.3037(11) 0.1098(9) 0.042(4) Uani 1 1 d . . . O7 O 0.2976(4) 0.3769(8) 0.0774(7) 0.058(3) Uani 1 1 d . . . C8 C 0.3198(9) 0.0853(15) 0.0211(12) 0.096(8) Uani 1 1 d . . . H8A H 0.3115 0.0162 0.0231 0.116 Uiso 1 1 calc R . . H8B H 0.3042 0.1201 -0.0317 0.116 Uiso 1 1 calc R . . C9 C 0.3649(8) 0.1078(15) 0.0495(11) 0.069(5) Uani 1 1 d . . . C10 C 0.3714(7) 0.2111(14) 0.0484(11) 0.068(5) Uani 1 1 d . . . H10A H 0.3560 0.2463 -0.0043 0.081 Uiso 1 1 calc R . . H10B H 0.4012 0.2346 0.0703 0.081 Uiso 1 1 calc R . . C11 C 0.4454(5) 0.3779(10) 0.5292(9) 0.041(4) Uani 1 1 d . . . H11 H 0.4665 0.4173 0.5104 0.049 Uiso 1 1 calc R . . C12 C 0.4514(5) 0.3543(11) 0.6174(9) 0.048(4) Uani 1 1 d . . . H12 H 0.4759 0.3777 0.6577 0.057 Uiso 1 1 calc R . . C13 C 0.4219(6) 0.2969(12) 0.6460(9) 0.052(4) Uani 1 1 d . . . H13 H 0.4261 0.2791 0.7063 0.062 Uiso 1 1 calc R . . C14 C 0.3852(5) 0.2641(13) 0.5861(10) 0.055(4) Uani 1 1 d . . . H14 H 0.3643 0.2250 0.6056 0.066 Uiso 1 1 calc R . . C15 C 0.3803(5) 0.2905(10) 0.4964(9) 0.042(4) Uani 1 1 d . . . C16 C 0.3449(5) 0.2533(10) 0.4266(9) 0.041(4) Uani 1 1 d . . . C17 C 0.3118(5) 0.1849(10) 0.4267(9) 0.043(4) Uani 1 1 d . . . H17 H 0.3035 0.1563 0.4766 0.052 Uiso 1 1 calc R . . C18 C 0.2935(5) 0.1677(11) 0.3368(10) 0.045(4) Uani 1 1 d . . . H18 H 0.2702 0.1249 0.3158 0.054 Uiso 1 1 calc R . . C19 C 0.3223(6) 0.4866(12) 0.4161(11) 0.058(5) Uani 1 1 d . . . H19A H 0.3059 0.5452 0.4238 0.086 Uiso 1 1 calc R . . H19B H 0.3390 0.4660 0.4734 0.086 Uiso 1 1 calc R . . H19C H 0.3024 0.4347 0.3911 0.086 Uiso 1 1 calc R . . C21 C 0.3096(6) -0.0531(12) 0.2076(11) 0.060(5) Uani 1 1 d . . . H21 H 0.2822 -0.0398 0.1718 0.072 Uiso 1 1 calc R . . C22 C 0.3174(8) -0.1474(11) 0.2464(12) 0.061(5) Uani 1 1 d . . . H22 H 0.2956 -0.1956 0.2348 0.073 Uiso 1 1 calc R . . C23 C 0.3548(8) -0.1675(14) 0.2982(13) 0.068(6) Uani 1 1 d . . . H23 H 0.3594 -0.2295 0.3252 0.081 Uiso 1 1 calc R . . C24 C 0.3879(7) -0.0975(12) 0.3137(11) 0.058(5) Uani 1 1 d . . . H24 H 0.4153 -0.1123 0.3492 0.070 Uiso 1 1 calc R . . C25 C 0.3792(6) -0.0013(11) 0.2737(11) 0.045(4) Uani 1 1 d . . . C26 C 0.4106(5) 0.0830(10) 0.2938(10) 0.043(4) Uani 1 1 d . . . C27 C 0.4492(6) 0.0948(13) 0.3524(12) 0.062(5) Uani 1 1 d . . . H27 H 0.4661 0.0457 0.3857 0.074 Uiso 1 1 calc R . . C28 C 0.4583(6) 0.1920(13) 0.3526(11) 0.053(5) Uani 1 1 d . . . H28 H 0.4829 0.2221 0.3873 0.063 Uiso 1 1 calc R . . C29 C 0.4028(9) 0.0321(18) 0.0725(14) 0.117(11) Uani 1 1 d . . . H29A H 0.4125 0.0135 0.0185 0.176 Uiso 1 1 calc R . . H29B H 0.3925 -0.0256 0.0992 0.176 Uiso 1 1 calc R . . H29C H 0.4268 0.0612 0.1141 0.176 Uiso 1 1 calc R . . Mo51 Mo 0.12106(4) 0.88405(10) 0.20060(7) 0.0408(4) Uani 1 1 d . . . Mo52 Mo 0.18989(4) 0.66710(11) 0.09900(7) 0.0398(4) Uani 1 1 d . . . N51 N 0.1093(4) 0.8476(9) 0.3407(8) 0.043(3) Uani 1 1 d . . . N52 N 0.1741(4) 0.7791(8) 0.2685(7) 0.035(3) Uani 1 1 d . . . N53 N 0.2052(4) 0.7229(9) 0.2402(8) 0.040(3) Uani 1 1 d . . . N54 N 0.1807(4) 0.5147(9) 0.1587(7) 0.046(3) Uani 1 1 d . . . N55 N 0.1242(4) 0.6633(9) 0.1440(7) 0.048(3) Uani 1 1 d . . . N56 N 0.0943(4) 0.7322(9) 0.1604(8) 0.048(3) Uani 1 1 d . . . C51 C 0.1221(5) 0.9023(13) 0.0736(11) 0.050(5) Uani 1 1 d . . . O51 O 0.1182(4) 0.9196(9) -0.0030(7) 0.067(4) Uani 1 1 d . . . C52 C 0.0648(7) 0.9471(14) 0.1517(11) 0.064(5) Uani 1 1 d . . . O52 O 0.0318(5) 0.9837(13) 0.1174(10) 0.111(6) Uani 1 1 d . . . C53 C 0.1765(6) 0.9943(14) 0.1885(11) 0.065(5) Uani 1 1 d . . . H53A H 0.2056 0.9665 0.1918 0.078 Uiso 1 1 calc R . . H53B H 0.1692 1.0459 0.1434 0.078 Uiso 1 1 calc R . . C54 C 0.1632(7) 1.0106(12) 0.2714(10) 0.056(5) Uani 1 1 d . . . C55 C 0.1177(6) 1.0453(11) 0.2566(13) 0.070(5) Uani 1 1 d . . . H55A H 0.1096 1.0976 0.2125 0.084 Uiso 1 1 calc R . . H55B H 0.1048 1.0527 0.3095 0.084 Uiso 1 1 calc R . . C56 C 0.2535(6) 0.6558(10) 0.0970(10) 0.047(4) Uani 1 1 d . . . O56 O 0.2903(4) 0.6510(9) 0.0972(9) 0.072(4) Uani 1 1 d . . . C57 C 0.2064(5) 0.7989(13) 0.0650(9) 0.050(4) Uani 1 1 d . . . O57 O 0.2221(4) 0.8736(8) 0.0457(7) 0.056(3) Uani 1 1 d . . . C58 C 0.1497(6) 0.7002(14) -0.0438(10) 0.067(5) Uani 1 1 d . . . H58A H 0.1195 0.7218 -0.0477 0.081 Uiso 1 1 calc R . . H58B H 0.1650 0.7352 -0.0844 0.081 Uiso 1 1 calc R . . C59 C 0.1576(7) 0.5984(13) -0.0342(10) 0.060(5) Uani 1 1 d . . . C60 C 0.2032(9) 0.5744(15) -0.0240(11) 0.094(8) Uani 1 1 d . . . H60A H 0.2193 0.6072 -0.0643 0.113 Uiso 1 1 calc R . . H60B H 0.2112 0.5054 -0.0127 0.113 Uiso 1 1 calc R . . C61 C 0.0731(5) 0.8782(12) 0.3718(10) 0.057(4) Uani 1 1 d . . . H61 H 0.0515 0.9148 0.3342 0.069 Uiso 1 1 calc R . . C62 C 0.0679(6) 0.8562(13) 0.4566(11) 0.061(5) Uani 1 1 d . . . H62 H 0.0431 0.8785 0.4763 0.073 Uiso 1 1 calc R . . C63 C 0.0993(6) 0.8011(15) 0.5141(11) 0.068(5) Uani 1 1 d . . . H63 H 0.0955 0.7849 0.5717 0.082 Uiso 1 1 calc R . . C64 C 0.1361(6) 0.7711(12) 0.4839(10) 0.055(4) Uani 1 1 d . . . H64 H 0.1583 0.7364 0.5219 0.065 Uiso 1 1 calc R . . C65 C 0.1402(5) 0.7932(11) 0.3946(9) 0.043(4) Uani 1 1 d . . . C66 C 0.1764(5) 0.7562(10) 0.3557(8) 0.038(4) Uani 1 1 d . . . C67 C 0.2083(6) 0.6917(11) 0.3867(10) 0.052(4) Uani 1 1 d . . . H67 H 0.2159 0.6653 0.4444 0.063 Uiso 1 1 calc R . . C68 C 0.2278(5) 0.6726(11) 0.3126(9) 0.049(4) Uani 1 1 d . . . H68 H 0.2522 0.6322 0.3129 0.059 Uiso 1 1 calc R . . C69 C 0.1906(7) 0.9996(14) 0.3612(11) 0.072(6) Uani 1 1 d . . . H69A H 0.2095 0.9432 0.3620 0.109 Uiso 1 1 calc R . . H69B H 0.1720 0.9902 0.4043 0.109 Uiso 1 1 calc R . . H69C H 0.2081 1.0581 0.3762 0.109 Uiso 1 1 calc R . . C71 C 0.2123(6) 0.4438(12) 0.1700(10) 0.060(5) Uani 1 1 d . . . H71 H 0.2391 0.4576 0.1542 0.073 Uiso 1 1 calc R . . C72 C 0.2055(8) 0.3494(11) 0.2052(10) 0.060(5) Uani 1 1 d . . . H72 H 0.2278 0.3023 0.2157 0.073 Uiso 1 1 calc R . . C73 C 0.1662(8) 0.3306(15) 0.2226(11) 0.070(6) Uani 1 1 d . . . H73 H 0.1605 0.2678 0.2428 0.084 Uiso 1 1 calc R . . C74 C 0.1330(8) 0.4011(15) 0.2119(11) 0.071(6) Uani 1 1 d . . . H74 H 0.1056 0.3859 0.2246 0.085 Uiso 1 1 calc R . . C75 C 0.1414(6) 0.4938(13) 0.1821(11) 0.053(4) Uani 1 1 d . . . C76 C 0.1117(5) 0.5753(11) 0.1734(10) 0.043(4) Uani 1 1 d . . . C77 C 0.0715(6) 0.5864(13) 0.2040(11) 0.060(5) Uani 1 1 d . . . H77 H 0.0550 0.5376 0.2252 0.072 Uiso 1 1 calc R . . C78 C 0.0628(5) 0.6851(14) 0.1949(11) 0.056(5) Uani 1 1 d . . . H78 H 0.0385 0.7161 0.2104 0.068 Uiso 1 1 calc R . . C79 C 0.1205(8) 0.5229(19) -0.0380(13) 0.105(9) Uani 1 1 d . . . H79A H 0.1315 0.4661 -0.0024 0.158 Uiso 1 1 calc R . . H79B H 0.1100 0.5029 -0.0993 0.158 Uiso 1 1 calc R . . H79C H 0.0969 0.5523 -0.0148 0.158 Uiso 1 1 calc R . . C90 C 0.0180(9) 0.767(3) 0.9414(18) 0.182(15) Uani 1 1 d . . . H90A H 0.0429 0.7443 0.9861 0.218 Uiso 1 1 calc R . . H90B H 0.0211 0.8382 0.9363 0.218 Uiso 1 1 calc R . . Cl91 Cl -0.0240(3) 0.7476(12) 0.9791(8) 0.242(6) Uani 1 1 d . . . Cl92 Cl 0.0230(4) 0.7150(13) 0.8385(8) 0.282(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0383(8) 0.0348(8) 0.0313(7) 0.0027(6) 0.0079(6) -0.0029(6) Mo2 0.0491(10) 0.0363(8) 0.0350(7) -0.0018(7) 0.0071(6) -0.0024(7) N1 0.034(8) 0.051(8) 0.044(8) 0.000(6) 0.013(6) 0.002(6) N2 0.030(7) 0.037(7) 0.029(6) -0.004(5) 0.005(5) -0.008(5) N3 0.034(8) 0.033(7) 0.049(7) 0.009(6) 0.007(6) -0.001(6) N4 0.051(9) 0.029(7) 0.054(8) -0.008(6) 0.018(7) -0.001(6) N5 0.029(7) 0.043(7) 0.044(7) -0.004(6) 0.008(5) -0.003(6) N6 0.029(8) 0.050(8) 0.045(7) -0.002(6) 0.013(6) -0.005(6) C1 0.065(13) 0.047(10) 0.041(9) 0.007(8) 0.019(8) -0.003(9) O1 0.057(9) 0.079(9) 0.099(10) 0.023(7) 0.017(7) -0.006(7) C2 0.052(12) 0.030(10) 0.046(10) -0.011(7) 0.011(9) -0.008(7) O2 0.087(10) 0.078(9) 0.038(6) 0.000(6) 0.026(6) -0.019(7) C3 0.071(14) 0.052(11) 0.050(10) 0.014(8) 0.011(9) -0.008(9) C4 0.047(10) 0.027(8) 0.044(9) 0.000(7) 0.019(7) 0.004(7) C5 0.068(13) 0.045(11) 0.061(12) 0.006(9) 0.021(9) 0.006(9) C6 0.095(17) 0.032(9) 0.052(10) 0.025(8) 0.015(11) 0.014(9) O6 0.060(10) 0.087(10) 0.091(10) 0.016(7) -0.010(8) -0.010(7) C7 0.053(11) 0.045(10) 0.031(8) -0.020(7) 0.016(7) -0.022(8) O7 0.076(9) 0.043(7) 0.053(7) 0.014(6) 0.007(6) 0.010(6) C8 0.19(3) 0.058(14) 0.051(11) -0.027(10) 0.037(14) -0.018(14) C9 0.103(17) 0.061(14) 0.047(10) -0.010(10) 0.027(11) 0.001(12) C10 0.090(15) 0.077(15) 0.046(10) -0.011(9) 0.034(10) 0.001(11) C11 0.032(9) 0.040(9) 0.044(9) -0.008(7) -0.009(7) -0.001(7) C12 0.049(11) 0.062(11) 0.028(8) -0.005(7) -0.002(7) -0.007(8) C13 0.068(13) 0.059(11) 0.021(8) 0.000(7) -0.012(8) 0.000(9) C14 0.047(11) 0.077(13) 0.045(10) 0.016(9) 0.022(8) -0.002(9) C15 0.045(10) 0.038(9) 0.043(9) 0.006(7) 0.006(7) -0.004(7) C16 0.044(10) 0.034(9) 0.039(9) 0.004(7) -0.005(7) -0.001(7) C17 0.061(11) 0.031(9) 0.040(9) 0.022(7) 0.015(7) -0.004(7) C18 0.036(10) 0.043(9) 0.058(10) 0.002(8) 0.014(8) -0.015(7) C19 0.069(14) 0.040(10) 0.067(11) -0.009(8) 0.023(9) 0.014(8) C21 0.065(13) 0.049(11) 0.070(11) -0.023(9) 0.021(9) -0.011(9) C22 0.122(19) 0.025(10) 0.050(10) -0.005(8) 0.048(12) -0.024(10) C23 0.12(2) 0.023(10) 0.070(13) -0.002(10) 0.048(13) -0.004(12) C24 0.078(15) 0.049(12) 0.044(10) -0.010(9) 0.004(9) 0.017(10) C25 0.051(12) 0.034(9) 0.054(9) -0.008(8) 0.020(8) 0.007(8) C26 0.049(11) 0.029(9) 0.051(10) 0.010(7) 0.010(8) 0.010(7) C27 0.052(12) 0.056(13) 0.070(12) 0.011(9) -0.003(9) 0.020(9) C28 0.045(11) 0.058(13) 0.057(10) -0.006(9) 0.014(9) 0.008(9) C29 0.20(3) 0.11(2) 0.072(15) 0.007(14) 0.088(17) 0.06(2) Mo51 0.0450(9) 0.0427(8) 0.0367(8) 0.0063(7) 0.0130(6) 0.0143(7) Mo52 0.0413(9) 0.0422(8) 0.0361(7) 0.0004(7) 0.0087(6) 0.0082(7) N51 0.034(8) 0.056(8) 0.041(7) -0.012(6) 0.015(6) 0.013(6) N52 0.029(7) 0.038(7) 0.040(7) -0.003(6) 0.008(5) 0.002(5) N53 0.039(8) 0.042(8) 0.042(7) 0.016(6) 0.013(6) 0.012(6) N54 0.054(9) 0.042(8) 0.037(7) -0.002(6) 0.000(6) 0.003(7) N55 0.064(9) 0.042(8) 0.034(7) -0.002(6) 0.001(6) 0.009(7) N56 0.035(8) 0.056(9) 0.055(8) 0.002(7) 0.013(6) 0.021(7) C51 0.045(12) 0.054(13) 0.058(12) 0.006(9) 0.023(9) 0.018(8) O51 0.095(10) 0.074(9) 0.037(7) 0.017(6) 0.021(6) 0.012(6) C52 0.069(14) 0.086(14) 0.045(10) 0.002(9) 0.026(9) 0.010(11) O52 0.064(10) 0.170(16) 0.098(10) 0.044(10) 0.013(8) 0.065(10) C53 0.068(14) 0.070(13) 0.062(12) 0.005(10) 0.026(10) 0.006(10) C54 0.091(15) 0.046(10) 0.035(9) -0.007(8) 0.025(9) -0.024(10) C55 0.091(16) 0.032(10) 0.095(14) 0.002(9) 0.039(12) 0.021(9) C56 0.069(13) 0.024(8) 0.051(10) 0.003(7) 0.017(9) 0.009(8) O56 0.043(8) 0.088(10) 0.091(9) 0.011(7) 0.027(7) 0.015(7) C57 0.049(11) 0.074(13) 0.031(8) 0.011(8) 0.018(7) 0.026(9) O57 0.057(8) 0.053(7) 0.061(7) 0.008(6) 0.017(6) -0.002(6) C58 0.062(13) 0.098(16) 0.038(9) -0.010(9) -0.001(8) 0.013(10) C59 0.076(15) 0.056(12) 0.041(9) -0.010(8) -0.005(9) 0.013(10) C60 0.16(2) 0.068(14) 0.047(11) -0.026(10) 0.002(12) 0.032(14) C61 0.040(10) 0.076(12) 0.059(10) 0.007(9) 0.019(8) 0.013(9) C62 0.057(12) 0.076(13) 0.061(11) -0.021(9) 0.038(10) -0.009(9) C63 0.067(14) 0.097(15) 0.047(10) 0.009(10) 0.025(10) -0.015(11) C64 0.069(13) 0.061(11) 0.034(9) 0.012(8) 0.010(8) 0.003(9) C65 0.051(11) 0.046(9) 0.030(8) -0.009(7) 0.006(7) -0.010(8) C66 0.051(10) 0.034(9) 0.025(8) 0.002(6) 0.000(7) 0.008(7) C67 0.076(13) 0.037(10) 0.040(9) -0.003(7) 0.002(9) -0.013(8) C68 0.050(11) 0.056(10) 0.036(8) 0.007(8) -0.003(7) 0.015(8) C69 0.103(16) 0.054(11) 0.064(12) -0.019(9) 0.024(11) -0.039(10) C71 0.056(12) 0.059(12) 0.062(10) -0.013(9) 0.000(9) 0.023(9) C72 0.108(17) 0.025(9) 0.044(10) 0.015(7) 0.005(10) 0.026(9) C73 0.12(2) 0.042(12) 0.044(11) -0.001(10) 0.004(11) 0.000(13) C74 0.100(18) 0.072(15) 0.046(11) -0.015(10) 0.025(11) -0.003(13) C75 0.056(13) 0.047(11) 0.055(10) -0.003(9) 0.013(8) -0.007(9) C76 0.050(11) 0.032(9) 0.042(9) -0.006(7) 0.001(8) -0.004(7) C77 0.056(13) 0.053(12) 0.072(12) 0.004(9) 0.016(10) -0.010(9) C78 0.026(10) 0.084(15) 0.059(10) 0.014(10) 0.009(8) 0.004(9) C79 0.12(2) 0.14(2) 0.048(13) -0.017(14) -0.008(12) -0.021(18) C90 0.052(18) 0.37(5) 0.12(2) -0.01(3) 0.011(15) 0.01(2) Cl91 0.111(8) 0.40(2) 0.210(11) 0.022(12) 0.014(7) -0.034(10) Cl92 0.169(11) 0.48(2) 0.170(10) 0.008(12) -0.030(8) 0.094(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.936(18) . ? Mo1 C2 1.959(16) . ? Mo1 N6 2.254(12) . ? Mo1 C4 2.258(14) . ? Mo1 N2 2.284(11) . ? Mo1 N1 2.284(12) . ? Mo1 C5 2.285(17) . ? Mo1 C3 2.382(16) . ? Mo2 C6 1.92(2) . ? Mo2 C7 1.960(17) . ? Mo2 N3 2.243(12) . ? Mo2 C9 2.261(17) . ? Mo2 N4 2.275(12) . ? Mo2 N5 2.303(11) . ? Mo2 C10 2.307(16) . ? Mo2 C8 2.314(17) . ? N1 C11 1.324(17) . ? N1 C15 1.372(18) . ? N2 C16 1.341(16) . ? N2 N3 1.359(15) . ? N3 C18 1.313(17) . ? N4 C25 1.34(2) . ? N4 C21 1.347(19) . ? N5 C26 1.329(17) . ? N5 N6 1.356(15) . ? N6 C28 1.348(19) . ? C1 O1 1.179(18) . ? C2 O2 1.157(16) . ? C3 C4 1.41(2) . ? C4 C5 1.38(2) . ? C4 C19 1.49(2) . ? C6 O6 1.20(2) . ? C7 O7 1.159(17) . ? C8 C9 1.41(3) . ? C9 C10 1.41(2) . ? C9 C29 1.54(3) . ? C11 C12 1.352(19) . ? C12 C13 1.33(2) . ? C13 C14 1.38(2) . ? C14 C15 1.385(19) . ? C15 C16 1.453(19) . ? C16 C17 1.38(2) . ? C17 C18 1.387(19) . ? C21 C22 1.40(2) . ? C22 C23 1.29(3) . ? C23 C24 1.38(3) . ? C24 C25 1.44(2) . ? C25 C26 1.49(2) . ? C26 C27 1.35(2) . ? C27 C28 1.34(2) . ? Mo51 C51 1.948(16) . ? Mo51 C52 1.95(2) . ? Mo51 N56 2.249(13) . ? Mo51 N52 2.256(11) . ? Mo51 N51 2.279(12) . ? Mo51 C54 2.284(16) . ? Mo51 C53 2.307(18) . ? Mo51 C55 2.346(15) . ? Mo52 C57 1.949(19) . ? Mo52 C56 1.983(19) . ? Mo52 N53 2.229(12) . ? Mo52 C59 2.266(15) . ? Mo52 N55 2.272(13) . ? Mo52 N54 2.287(12) . ? Mo52 C58 2.317(16) . ? Mo52 C60 2.349(17) . ? N51 C65 1.348(18) . ? N51 C61 1.363(18) . ? N52 C66 1.346(16) . ? N52 N53 1.362(15) . ? N53 C68 1.361(17) . ? N54 C71 1.356(18) . ? N54 C75 1.36(2) . ? N55 C76 1.352(18) . ? N55 N56 1.369(16) . ? N56 C78 1.353(19) . ? C51 O51 1.167(16) . ? C52 O52 1.16(2) . ? C53 C54 1.41(2) . ? C54 C55 1.46(2) . ? C54 C69 1.46(2) . ? C56 O56 1.141(18) . ? C57 O57 1.181(18) . ? C58 C59 1.40(2) . ? C59 C60 1.43(3) . ? C59 C79 1.53(3) . ? C61 C62 1.36(2) . ? C62 C63 1.39(2) . ? C63 C64 1.37(2) . ? C64 C65 1.417(19) . ? C65 C66 1.45(2) . ? C66 C67 1.33(2) . ? C67 C68 1.40(2) . ? C71 C72 1.41(2) . ? C72 C73 1.32(3) . ? C73 C74 1.39(3) . ? C74 C75 1.37(2) . ? C75 C76 1.42(2) . ? C76 C77 1.42(2) . ? C77 C78 1.36(2) . ? C90 Cl91 1.55(3) . ? C90 Cl92 1.74(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 76.4(6) . . ? C1 Mo1 N6 95.0(6) . . ? C2 Mo1 N6 85.0(5) . . ? C1 Mo1 C4 101.4(6) . . ? C2 Mo1 C4 103.5(6) . . ? N6 Mo1 C4 162.8(5) . . ? C1 Mo1 N2 165.9(5) . . ? C2 Mo1 N2 112.4(5) . . ? N6 Mo1 N2 75.5(4) . . ? C4 Mo1 N2 87.5(5) . . ? C1 Mo1 N1 97.1(5) . . ? C2 Mo1 N1 168.9(5) . . ? N6 Mo1 N1 86.7(4) . . ? C4 Mo1 N1 86.5(5) . . ? N2 Mo1 N1 72.3(4) . . ? C1 Mo1 C5 105.2(7) . . ? C2 Mo1 C5 70.5(6) . . ? N6 Mo1 C5 143.0(5) . . ? C4 Mo1 C5 35.4(5) . . ? N2 Mo1 C5 88.4(5) . . ? N1 Mo1 C5 120.2(5) . . ? C1 Mo1 C3 68.1(6) . . ? C2 Mo1 C3 105.1(6) . . ? N6 Mo1 C3 156.9(5) . . ? C4 Mo1 C3 35.1(5) . . ? N2 Mo1 C3 117.6(5) . . ? N1 Mo1 C3 80.2(5) . . ? C5 Mo1 C3 59.6(6) . . ? C6 Mo2 C7 76.3(6) . . ? C6 Mo2 N3 90.8(6) . . ? C7 Mo2 N3 86.5(5) . . ? C6 Mo2 C9 103.3(8) . . ? C7 Mo2 C9 103.6(6) . . ? N3 Mo2 C9 164.3(6) . . ? C6 Mo2 N4 96.3(5) . . ? C7 Mo2 N4 169.2(5) . . ? N3 Mo2 N4 85.7(4) . . ? C9 Mo2 N4 85.7(6) . . ? C6 Mo2 N5 162.5(5) . . ? C7 Mo2 N5 113.6(5) . . ? N3 Mo2 N5 76.0(4) . . ? C9 Mo2 N5 88.8(6) . . ? N4 Mo2 N5 71.6(4) . . ? C6 Mo2 C10 111.6(7) . . ? C7 Mo2 C10 72.3(6) . . ? N3 Mo2 C10 143.5(5) . . ? C9 Mo2 C10 35.9(6) . . ? N4 Mo2 C10 118.2(6) . . ? N5 Mo2 C10 85.6(6) . . ? C6 Mo2 C8 67.7(9) . . ? C7 Mo2 C8 99.3(7) . . ? N3 Mo2 C8 155.2(7) . . ? C9 Mo2 C8 36.0(7) . . ? N4 Mo2 C8 84.8(6) . . ? N5 Mo2 C8 122.0(8) . . ? C10 Mo2 C8 60.1(7) . . ? C11 N1 C15 117.4(13) . . ? C11 N1 Mo1 126.3(10) . . ? C15 N1 Mo1 116.3(9) . . ? C16 N2 N3 108.8(11) . . ? C16 N2 Mo1 116.1(9) . . ? N3 N2 Mo1 135.0(8) . . ? C18 N3 N2 108.3(11) . . ? C18 N3 Mo2 125.2(10) . . ? N2 N3 Mo2 116.5(9) . . ? C25 N4 C21 117.9(14) . . ? C25 N4 Mo2 117.8(10) . . ? C21 N4 Mo2 124.2(12) . . ? C26 N5 N6 107.6(12) . . ? C26 N5 Mo2 116.9(10) . . ? N6 N5 Mo2 134.8(9) . . ? C28 N6 N5 106.7(12) . . ? C28 N6 Mo1 126.0(10) . . ? N5 N6 Mo1 116.7(9) . . ? O1 C1 Mo1 178.6(14) . . ? O2 C2 Mo1 173.1(13) . . ? C4 C3 Mo1 67.6(9) . . ? C5 C4 C3 112.7(14) . . ? C5 C4 C19 123.5(15) . . ? C3 C4 C19 123.7(14) . . ? C5 C4 Mo1 73.4(9) . . ? C3 C4 Mo1 77.3(10) . . ? C19 C4 Mo1 120.1(10) . . ? C4 C5 Mo1 71.2(9) . . ? O6 C6 Mo2 177.5(14) . . ? O7 C7 Mo2 172.1(12) . . ? C9 C8 Mo2 70.0(10) . . ? C10 C9 C8 110.1(18) . . ? C10 C9 C29 124(2) . . ? C8 C9 C29 126(2) . . ? C10 C9 Mo2 73.8(9) . . ? C8 C9 Mo2 74.1(11) . . ? C29 C9 Mo2 122.1(12) . . ? C9 C10 Mo2 70.3(10) . . ? N1 C11 C12 124.0(15) . . ? C13 C12 C11 119.3(14) . . ? C12 C13 C14 120.1(13) . . ? C13 C14 C15 118.7(15) . . ? N1 C15 C14 120.6(14) . . ? N1 C15 C16 116.1(12) . . ? C14 C15 C16 123.2(14) . . ? N2 C16 C17 107.8(12) . . ? N2 C16 C15 118.5(13) . . ? C17 C16 C15 133.1(13) . . ? C16 C17 C18 105.7(12) . . ? N3 C18 C17 109.2(13) . . ? N4 C21 C22 122.3(17) . . ? C23 C22 C21 120.3(18) . . ? C22 C23 C24 120.4(19) . . ? C23 C24 C25 118.4(18) . . ? N4 C25 C24 120.6(15) . . ? N4 C25 C26 116.3(13) . . ? C24 C25 C26 123.0(16) . . ? N5 C26 C27 109.7(14) . . ? N5 C26 C25 116.8(14) . . ? C27 C26 C25 133.1(15) . . ? C28 C27 C26 105.9(14) . . ? C27 C28 N6 109.7(15) . . ? C51 Mo51 C52 76.0(6) . . ? C51 Mo51 N56 85.7(6) . . ? C52 Mo51 N56 92.4(6) . . ? C51 Mo51 N52 112.1(5) . . ? C52 Mo51 N52 164.3(6) . . ? N56 Mo51 N52 75.4(4) . . ? C51 Mo51 N51 170.3(6) . . ? C52 Mo51 N51 98.7(5) . . ? N56 Mo51 N51 86.4(4) . . ? N52 Mo51 N51 71.1(4) . . ? C51 Mo51 C54 104.4(7) . . ? C52 Mo51 C54 103.7(8) . . ? N56 Mo51 C54 162.6(6) . . ? N52 Mo51 C54 87.6(6) . . ? N51 Mo51 C54 84.6(5) . . ? C51 Mo51 C53 71.4(7) . . ? C52 Mo51 C53 108.1(7) . . ? N56 Mo51 C53 143.7(5) . . ? N52 Mo51 C53 87.4(6) . . ? N51 Mo51 C53 118.2(5) . . ? C54 Mo51 C53 35.9(5) . . ? C51 Mo51 C55 104.5(7) . . ? C52 Mo51 C55 68.4(7) . . ? N56 Mo51 C55 154.6(6) . . ? N52 Mo51 C55 119.9(6) . . ? N51 Mo51 C55 80.6(5) . . ? C54 Mo51 C55 36.7(6) . . ? C53 Mo51 C55 61.1(6) . . ? C57 Mo52 C56 75.7(6) . . ? C57 Mo52 N53 85.9(5) . . ? C56 Mo52 N53 91.0(6) . . ? C57 Mo52 C59 103.3(6) . . ? C56 Mo52 C59 102.6(7) . . ? N53 Mo52 C59 165.0(6) . . ? C57 Mo52 N55 113.4(5) . . ? C56 Mo52 N55 162.8(5) . . ? N53 Mo52 N55 75.6(4) . . ? C59 Mo52 N55 89.7(6) . . ? C57 Mo52 N54 170.2(5) . . ? C56 Mo52 N54 98.0(5) . . ? N53 Mo52 N54 86.7(4) . . ? C59 Mo52 N54 85.3(5) . . ? N55 Mo52 N54 70.8(5) . . ? C57 Mo52 C58 72.3(7) . . ? C56 Mo52 C58 110.6(7) . . ? N53 Mo52 C58 143.6(5) . . ? C59 Mo52 C58 35.5(6) . . ? N55 Mo52 C58 86.4(6) . . ? N54 Mo52 C58 117.2(6) . . ? C57 Mo52 C60 100.4(7) . . ? C56 Mo52 C60 67.4(8) . . ? N53 Mo52 C60 154.8(6) . . ? C59 Mo52 C60 36.0(6) . . ? N55 Mo52 C60 122.4(7) . . ? N54 Mo52 C60 83.7(6) . . ? C58 Mo52 C60 60.5(7) . . ? C65 N51 C61 119.4(13) . . ? C65 N51 Mo51 117.1(9) . . ? C61 N51 Mo51 123.5(10) . . ? C66 N52 N53 106.1(11) . . ? C66 N52 Mo51 119.0(9) . . ? N53 N52 Mo51 134.7(8) . . ? C68 N53 N52 107.8(11) . . ? C68 N53 Mo52 125.7(10) . . ? N52 N53 Mo52 117.5(8) . . ? C71 N54 C75 118.7(15) . . ? C71 N54 Mo52 122.8(12) . . ? C75 N54 Mo52 118.5(10) . . ? C76 N55 N56 106.9(13) . . ? C76 N55 Mo52 116.7(10) . . ? N56 N55 Mo52 135.8(10) . . ? C78 N56 N55 108.4(13) . . ? C78 N56 Mo51 125.3(11) . . ? N55 N56 Mo51 116.3(10) . . ? O51 C51 Mo51 172.0(13) . . ? O52 C52 Mo51 175.8(15) . . ? C54 C53 Mo51 71.2(10) . . ? C53 C54 C55 110.8(16) . . ? C53 C54 C69 126.5(19) . . ? C55 C54 C69 122.6(16) . . ? C53 C54 Mo51 72.9(10) . . ? C55 C54 Mo51 74.0(10) . . ? C69 C54 Mo51 122.2(11) . . ? C54 C55 Mo51 69.3(8) . . ? O56 C56 Mo52 178.4(14) . . ? O57 C57 Mo52 170.9(13) . . ? C59 C58 Mo52 70.3(9) . . ? C58 C59 C60 112.5(18) . . ? C58 C59 C79 122.5(19) . . ? C60 C59 C79 124.9(19) . . ? C58 C59 Mo52 74.2(9) . . ? C60 C59 Mo52 75.2(9) . . ? C79 C59 Mo52 120.2(12) . . ? C59 C60 Mo52 68.9(9) . . ? C62 C61 N51 121.4(15) . . ? C61 C62 C63 120.9(16) . . ? C64 C63 C62 118.2(15) . . ? C63 C64 C65 119.7(15) . . ? N51 C65 C64 120.4(14) . . ? N51 C65 C66 117.0(12) . . ? C64 C65 C66 122.6(14) . . ? C67 C66 N52 112.9(13) . . ? C67 C66 C65 131.2(14) . . ? N52 C66 C65 115.1(12) . . ? C66 C67 C68 104.2(13) . . ? N53 C68 C67 108.8(14) . . ? N54 C71 C72 121.8(17) . . ? C73 C72 C71 117.4(17) . . ? C72 C73 C74 122(2) . . ? C75 C74 C73 119(2) . . ? N54 C75 C74 120.8(17) . . ? N54 C75 C76 114.2(15) . . ? C74 C75 C76 125.0(18) . . ? N55 C76 C77 110.0(13) . . ? N55 C76 C75 119.2(15) . . ? C77 C76 C75 130.1(15) . . ? C78 C77 C76 103.8(14) . . ? N56 C78 C77 110.8(15) . . ? Cl91 C90 Cl92 120(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.757 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.117 #===END