Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Modec, Barbara' 'Brencic, Jurij V.' 'Zubieta, Jon' _publ_contact_author_name 'Dr Barbara Modec' _publ_contact_author_address ; Department of Chemistry University of Ljubljana Askerceva 5 Ljubljana 1000 SLOVENIA ; _publ_contact_author_email 'BARBARA.MODEC@UNI-LJ.SI' _publ_section_title ; A Templated Synthesis of Tetranuclear Polyoxoalkoxymolybdates(V). Bromo Coordinated Oxomolybdenum(V) Clusters: Known Core Structure with New Ligands. Oxidation to the Lindquist Anion. ; data_1a _database_code_CSD 173626 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dipyridinium tetrachloro-di-\m~2~-methoxo-dimethanol-di- \m~3~-oxo-di-\m~2~-oxo-tetraoxotetramolybdate(V) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 Cl4 Mo4 N2 O12' _chemical_formula_weight 939.93 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0503(9) _cell_length_b 9.2675(9) _cell_length_c 9.7103(9) _cell_angle_alpha 109.404(2) _cell_angle_beta 110.841(2) _cell_angle_gamma 98.077(2) _cell_volume 686.30(11) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.274 _exptl_crystal_density_method ? _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 2.232 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS' _exptl_absorpt_correction_T_min 0.7083 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4663 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.26 _reflns_number_total 3166 _reflns_number_gt 2711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SMART (Siemens, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0522P)^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 3166 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.51542(3) 0.34434(3) -0.66240(3) 0.01248(9) Uani 1 d . . . Mo2 Mo -0.26294(3) 0.38688(3) -0.40138(3) 0.01299(9) Uani 1 d . . . Cl1 Cl -0.78216(10) 0.13621(9) -0.82852(10) 0.01824(17) Uani 1 d . . . Cl2 Cl -0.20129(10) 0.23236(10) -0.24200(10) 0.01893(17) Uani 1 d . . . O1 O -0.4392(3) 0.2884(3) -0.7997(3) 0.0178(5) Uani 1 d . . . O2 O -0.1271(3) 0.3435(3) -0.4785(3) 0.0181(5) Uani 1 d . . . O3 O -0.4685(3) 0.2160(3) -0.5380(3) 0.0146(5) Uani 1 d . . . O4 O -0.3498(3) 0.5430(3) -0.4820(3) 0.0138(4) Uani 1 d . . . O5 O -0.6298(3) 0.4953(3) -0.7568(3) 0.0145(5) Uani 1 d . . . O6 O -0.0565(3) 0.5913(3) -0.1983(3) 0.0176(5) Uani 1 d . . . H6 H -0.0931 0.6678 -0.1771 0.026 Uiso 1 calc R . . N N 0.3763(4) 0.1344(3) -0.3647(4) 0.0211(6) Uani 1 d . . . H H 0.4410 0.1480 -0.4091 0.025 Uiso 1 calc R . . C51 C -0.6710(4) 0.4760(4) -0.9203(4) 0.0188(7) Uani 1 d . . . H51A H -0.6182 0.4036 -0.9664 0.028 Uiso 1 calc R . . H51B H -0.6336 0.5780 -0.9208 0.028 Uiso 1 calc R . . H51C H -0.7887 0.4336 -0.9829 0.028 Uiso 1 calc R . . C61 C 0.1036(4) 0.6436(5) -0.1939(4) 0.0237(8) Uani 1 d . . . H61A H 0.1474 0.5544 -0.2168 0.036 Uiso 1 calc R . . H61B H 0.1772 0.7250 -0.0884 0.036 Uiso 1 calc R . . H61C H 0.0928 0.6861 -0.2735 0.036 Uiso 1 calc R . . C1 C 0.2388(5) 0.1797(4) -0.4058(4) 0.0261(8) Uani 1 d . . . H1 H 0.2158 0.2264 -0.4793 0.031 Uiso 1 calc R . . C2 C 0.1317(4) 0.1567(4) -0.3388(4) 0.0220(7) Uani 1 d . . . H2 H 0.0359 0.1881 -0.3659 0.026 Uiso 1 calc R . . C3 C 0.1688(4) 0.0861(4) -0.2301(4) 0.0200(7) Uani 1 d . . . H3 H 0.0972 0.0690 -0.1843 0.024 Uiso 1 calc R . . C4 C 0.3123(4) 0.0412(4) -0.1900(4) 0.0196(7) Uani 1 d . . . H4 H 0.3374 -0.0071 -0.1180 0.024 Uiso 1 calc R . . C5 C 0.4180(4) 0.0690(4) -0.2580(4) 0.0217(7) Uani 1 d . . . H5 H 0.5167 0.0425 -0.2299 0.026 Uiso 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 0.01227(15) 0.01445(15) 0.01348(15) 0.00730(11) 0.00681(11) 0.00462(11) Mo2 0.01222(15) 0.01616(15) 0.01458(15) 0.00860(12) 0.00738(11) 0.00572(11) Cl1 0.0169(4) 0.0175(4) 0.0189(4) 0.0077(3) 0.0070(3) 0.0026(3) Cl2 0.0203(4) 0.0233(4) 0.0213(4) 0.0149(3) 0.0109(3) 0.0105(3) O1 0.0173(12) 0.0204(12) 0.0176(12) 0.0078(10) 0.0089(10) 0.0068(10) O2 0.0176(12) 0.0241(13) 0.0193(12) 0.0129(10) 0.0102(10) 0.0095(10) O3 0.0157(11) 0.0138(11) 0.0166(11) 0.0073(9) 0.0081(9) 0.0052(9) O4 0.0126(11) 0.0155(11) 0.0153(11) 0.0082(9) 0.0066(9) 0.0035(9) O5 0.0149(11) 0.0173(11) 0.0142(11) 0.0088(9) 0.0067(9) 0.0057(9) O6 0.0131(11) 0.0205(12) 0.0194(12) 0.0081(10) 0.0078(10) 0.0039(9) N 0.0250(16) 0.0194(14) 0.0241(15) 0.0075(12) 0.0181(13) 0.0049(12) C51 0.0238(18) 0.0229(17) 0.0149(16) 0.0104(14) 0.0104(14) 0.0096(14) C61 0.0142(17) 0.033(2) 0.0255(19) 0.0144(16) 0.0098(14) 0.0040(15) C1 0.032(2) 0.0244(18) 0.0229(18) 0.0135(16) 0.0107(16) 0.0057(16) C2 0.0204(18) 0.0229(18) 0.0241(18) 0.0110(15) 0.0095(15) 0.0077(14) C3 0.0194(17) 0.0187(16) 0.0218(18) 0.0076(14) 0.0106(14) 0.0021(14) C4 0.0223(18) 0.0173(16) 0.0187(17) 0.0085(14) 0.0075(14) 0.0054(14) C5 0.0178(17) 0.0150(16) 0.0299(19) 0.0064(15) 0.0099(15) 0.0068(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.678(2) . ? Mo1 O3 1.946(2) . ? Mo1 O4 1.980(2) . ? Mo1 O5 2.110(2) . ? Mo1 O4 2.269(2) 2_464 ? Mo1 Cl1 2.4502(8) . ? Mo1 Mo2 2.6005(4) . ? Mo2 O2 1.682(2) . ? Mo2 O3 1.936(2) . ? Mo2 O4 1.990(2) . ? Mo2 O5 2.176(2) 2_464 ? Mo2 O6 2.2070(23) . ? Mo2 Cl2 2.4166(8) . ? O4 Mo1 2.269(2) 2_464 ? O5 C51 1.437(4) . ? O5 Mo2 2.176(2) 2_464 ? O6 C61 1.443(4) . ? O6 H6 0.8200 . ? N C5 1.337(5) . ? N C1 1.337(5) . ? N H 0.8600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C1 C2 1.376(5) . ? C1 H1 0.9300 . ? C2 C3 1.386(5) . ? C2 H2 0.9300 . ? C3 C4 1.382(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O3 107.24(10) . . ? O1 Mo1 O4 106.20(10) . . ? O3 Mo1 O4 93.76(9) . . ? O1 Mo1 O5 93.79(10) . . ? O3 Mo1 O5 158.02(9) . . ? O4 Mo1 O5 86.26(9) . . ? O1 Mo1 O4 164.04(10) . 2_464 ? O3 Mo1 O4 88.50(8) . 2_464 ? O4 Mo1 O4 74.60(9) . 2_464 ? O5 Mo1 O4 70.28(8) . 2_464 ? O1 Mo1 Cl1 95.37(8) . . ? O3 Mo1 Cl1 84.59(7) . . ? O4 Mo1 Cl1 157.81(7) . . ? O5 Mo1 Cl1 87.18(6) . . ? O4 Mo1 Cl1 83.23(6) 2_464 . ? O1 Mo1 Mo2 100.64(8) . . ? O3 Mo1 Mo2 47.78(6) . . ? O4 Mo1 Mo2 49.24(6) . . ? O5 Mo1 Mo2 135.41(6) . . ? O4 Mo1 Mo2 91.86(6) 2_464 . ? Cl1 Mo1 Mo2 132.30(2) . . ? O2 Mo2 O3 107.42(10) . . ? O2 Mo2 O4 105.04(10) . . ? O3 Mo2 O4 93.73(9) . . ? O2 Mo2 O5 161.92(10) . 2_464 ? O3 Mo2 O5 90.60(9) . 2_464 ? O4 Mo2 O5 74.41(9) . 2_464 ? O2 Mo2 Cl2 94.17(8) . . ? O3 Mo2 Cl2 85.13(7) . . ? O4 Mo2 Cl2 160.13(7) . . ? O5 Mo2 Cl2 85.76(6) 2_464 . ? O2 Mo2 Mo1 99.89(8) . . ? O3 Mo2 Mo1 48.09(6) . . ? O4 Mo2 Mo1 48.90(6) . . ? O5 Mo2 Mo1 93.18(6) 2_464 . ? Cl2 Mo2 Mo1 133.22(2) . . ? Mo2 O3 Mo1 84.13(9) . . ? Mo1 O4 Mo2 81.86(8) . . ? Mo1 O4 Mo1 105.40(9) . 2_464 ? Mo2 O4 Mo1 107.86(9) . 2_464 ? C51 O5 Mo1 122.20(19) . . ? C51 O5 Mo2 127.81(19) . 2_464 ? Mo1 O5 Mo2 107.01(9) . 2_464 ? C61 O6 H6 109.5 . . ? C5 N C1 123.2(3) . . ? C5 N H 118.4 . . ? C1 N H 118.4 . . ? O5 C51 H51A 109.5 . . ? O5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O6 C61 H61A 109.5 . . ? O6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N C1 C2 119.6(3) . . ? N C1 H1 120.2 . . ? C2 C1 H1 120.2 . . ? C1 C2 C3 119.0(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N C5 C4 119.0(3) . . ? N C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.983 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.142 #===END data_1b _database_code_CSD 173627 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dipyridinium tetrachloro-di-\m~2~-ethoxo-diethanol-di-\m~3~- oxo-di-\m~2~-oxo-tetraoxotetramolybdate(V) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H34 Cl4 Mo4 N2 O12' _chemical_formula_weight 996.03 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1930(10) _cell_length_b 9.7236(9) _cell_length_c 10.441(2) _cell_angle_alpha 110.690(10) _cell_angle_beta 104.24(2) _cell_angle_gamma 100.200(10) _cell_volume 809.63(19) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63 _cell_measurement_theta_min 4.57 _cell_measurement_theta_max 14.74 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.043 _exptl_crystal_density_method ? _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 1.898 _exptl_absorpt_correction_type 'psi scan' _exptl_abosrpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_T_max 0.825 _exptl_special_details ; ? ; _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 'Enraf Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5069 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.94 _reflns_number_total 3882 _reflns_number_gt 3387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.3121P] 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 SHELXL _refine_ls_extinction_coef 0.0191(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3882 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.10044(2) -0.03065(2) 1.14411(2) 0.02916(7) Uani 1 d . . . Mo2 Mo 1.14933(2) -0.18588(2) 0.90591(2) 0.03103(7) Uani 1 d . . . Cl1 Cl 0.94473(8) -0.11431(8) 1.27717(8) 0.04588(15) Uani 1 d . . . Cl2 Cl 1.07470(9) -0.45762(7) 0.75125(9) 0.05164(17) Uani 1 d . . . O1 O 1.2766(2) 0.0132(2) 1.2664(2) 0.0435(4) Uani 1 d . . . O2 O 1.3394(2) -0.1712(2) 0.9769(2) 0.0431(4) Uani 1 d . . . O3 O 1.04211(19) -0.25008(18) 1.02289(19) 0.0339(3) Uani 1 d . . . O4 O 1.13802(17) 0.02885(17) 0.98969(17) 0.0293(3) Uani 1 d . . . O5 O 1.06690(19) 0.18595(18) 1.23725(17) 0.0335(3) Uani 1 d . . . O6 O 1.2144(2) -0.1344(2) 0.7348(2) 0.0479(5) Uani 1 d . . . H6 H 1.1795 -0.0686 0.7172 0.072 Uiso 1 calc R . . N N 0.7457(3) -0.4344(3) 0.9140(3) 0.0555(6) Uani 1 d . . . H H 0.8399 -0.3739 0.9568 0.067 Uiso 1 calc R . . C1 C 0.7252(4) -0.5828(4) 0.8563(4) 0.0617(9) Uani 1 d . . . H1 H 0.8116 -0.6205 0.8617 0.074 Uiso 1 calc R . . C2 C 0.5785(4) -0.6814(4) 0.7888(4) 0.0589(8) Uani 1 d . . . H2 H 0.5629 -0.7870 0.7477 0.071 Uiso 1 calc R . . C3 C 0.4520(4) -0.6219(4) 0.7822(3) 0.0555(8) Uani 1 d . . . H3 H 0.3502 -0.6877 0.7365 0.067 Uiso 1 calc R . . C4 C 0.4769(4) -0.4664(4) 0.8429(3) 0.0525(7) Uani 1 d . . . H4 H 0.3927 -0.4254 0.8390 0.063 Uiso 1 calc R . . C5 C 0.6268(4) -0.3728(3) 0.9092(3) 0.0536(7) Uani 1 d . . . H5 H 0.6464 -0.2667 0.9509 0.064 Uiso 1 calc R . . C51 C 1.1415(3) 0.2795(3) 1.3922(3) 0.0426(6) Uani 1 d . . . H51A H 1.1575 0.2136 1.4424 0.051 Uiso 1 calc R . . H51B H 1.0737 0.3376 1.4285 0.051 Uiso 1 calc R . . C52 C 1.2963(4) 0.3880(4) 1.4227(3) 0.0603(8) Uani 1 d . . . H52A H 1.3651 0.3305 1.3909 0.090 Uiso 1 calc R . . H52B H 1.3422 0.4511 1.5252 0.090 Uiso 1 calc R . . H52C H 1.2806 0.4521 1.3716 0.090 Uiso 1 calc R . . C61 C 1.3498(4) -0.1408(5) 0.6935(4) 0.0681(10) Uani 1 d . . . H61A H 1.3767 -0.2328 0.6936 0.082 Uiso 1 calc R . . H61B H 1.4371 -0.0527 0.7643 0.082 Uiso 1 calc R . . C62 C 1.3257(5) -0.1417(6) 0.5475(4) 0.0817(12) Uani 1 d . . . H62A H 1.4148 -0.1585 0.5187 0.123 Uiso 1 calc R . . H62B H 1.3136 -0.0446 0.5505 0.123 Uiso 1 calc R . . H62C H 1.2330 -0.2224 0.4787 0.123 Uiso 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 0.02401(11) 0.03171(11) 0.03368(11) 0.01413(8) 0.00970(8) 0.01144(7) Mo2 0.02538(11) 0.03095(11) 0.03910(12) 0.01330(8) 0.01327(8) 0.01290(8) Cl1 0.0486(4) 0.0521(4) 0.0529(4) 0.0308(3) 0.0267(3) 0.0198(3) Cl2 0.0498(4) 0.0345(3) 0.0625(4) 0.0078(3) 0.0193(3) 0.0183(3) O1 0.0309(9) 0.0534(11) 0.0435(10) 0.0188(8) 0.0071(7) 0.0166(8) O2 0.0283(8) 0.0466(10) 0.0568(11) 0.0202(9) 0.0149(8) 0.0186(7) O3 0.0307(8) 0.0319(8) 0.0424(9) 0.0165(7) 0.0138(7) 0.0123(6) O4 0.0226(7) 0.0293(7) 0.0362(8) 0.0130(6) 0.0101(6) 0.0091(6) O5 0.0281(8) 0.0341(8) 0.0326(8) 0.0081(6) 0.0079(6) 0.0110(6) O6 0.0439(11) 0.0614(12) 0.0614(12) 0.0341(10) 0.0332(10) 0.0295(9) N 0.0329(12) 0.0711(17) 0.0559(15) 0.0327(13) 0.0057(10) -0.0007(11) C1 0.0572(19) 0.082(2) 0.079(2) 0.054(2) 0.0309(17) 0.0429(18) C2 0.077(2) 0.0436(15) 0.0611(19) 0.0245(14) 0.0263(17) 0.0176(15) C3 0.0408(15) 0.0651(19) 0.0488(16) 0.0243(14) 0.0090(12) -0.0046(13) C4 0.0430(15) 0.0698(19) 0.0580(17) 0.0313(15) 0.0230(13) 0.0292(14) C5 0.0633(19) 0.0422(14) 0.0527(16) 0.0176(13) 0.0210(15) 0.0117(13) C51 0.0401(13) 0.0450(13) 0.0329(12) 0.0083(10) 0.0086(10) 0.0111(11) C52 0.0515(18) 0.0556(17) 0.0464(16) 0.0098(13) 0.0014(13) -0.0033(14) C61 0.0508(18) 0.109(3) 0.077(2) 0.052(2) 0.0432(18) 0.0404(19) C62 0.074(3) 0.124(4) 0.061(2) 0.040(2) 0.039(2) 0.035(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.6701(18) . ? Mo1 O3 1.9479(17) . ? Mo1 O4 1.9789(16) . ? Mo1 O5 2.0993(16) . ? Mo1 O4 2.2982(16) 2_757 ? Mo1 Cl1 2.4506(7) . ? Mo1 Mo2 2.6083(5) . ? Mo2 O2 1.6805(17) . ? Mo2 O3 1.9407(17) . ? Mo2 O4 1.9916(15) . ? Mo2 O5 2.1731(17) 2_757 ? Mo2 O6 2.2025(19) . ? Mo2 Cl2 2.4203(8) . ? O4 Mo1 2.2982(16) 2_757 ? O5 C51 1.452(3) . ? O5 Mo2 2.1731(17) 2_757 ? O6 C61 1.419(3) . ? N C1 1.309(5) . ? N C5 1.335(4) . ? C1 C2 1.354(5) . ? C2 C3 1.385(5) . ? C3 C4 1.367(5) . ? C4 C5 1.360(4) . ? C51 C52 1.499(4) . ? C61 C62 1.482(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 O1 Mo1 O3 106.34(8) . . ? O1 Mo1 O4 106.32(8) . . ? O3 Mo1 O4 93.80(7) . . ? O1 Mo1 O5 95.38(9) . . ? O3 Mo1 O5 157.16(7) . . ? O4 Mo1 O5 86.65(7) . . ? O1 Mo1 O4 165.70(8) . 2_757 ? O3 Mo1 O4 87.85(7) . 2_757 ? O4 Mo1 O4 73.74(7) . 2_757 ? O5 Mo1 O4 70.32(6) . 2_757 ? O1 Mo1 Cl1 96.97(7) . . ? O3 Mo1 Cl1 83.41(5) . . ? O4 Mo1 Cl1 156.34(5) . . ? O5 Mo1 Cl1 87.08(5) . . ? O4 Mo1 Cl1 82.67(4) 2_757 . ? O1 Mo1 Mo2 100.39(7) . . ? O3 Mo1 Mo2 47.76(5) . . ? O4 Mo1 Mo2 49.15(5) . . ? O5 Mo1 Mo2 135.61(5) . . ? O4 Mo1 Mo2 90.39(4) 2_757 . ? Cl1 Mo1 Mo2 130.98(2) . . ? O2 Mo2 O3 106.60(8) . . ? O2 Mo2 O4 104.30(8) . . ? O3 Mo2 O4 93.62(7) . . ? O2 Mo2 O5 160.92(8) . 2_757 ? O3 Mo2 O5 92.45(7) . 2_757 ? O4 Mo2 O5 74.93(6) . 2_757 ? O2 Mo2 Cl2 94.87(7) . . ? O3 Mo2 Cl2 84.93(5) . . ? O4 Mo2 Cl2 160.33(5) . . ? O5 Mo2 Cl2 85.51(5) 2_757 . ? O2 Mo2 Mo1 99.06(7) . . ? O3 Mo2 Mo1 47.99(5) . . ? O4 Mo2 Mo1 48.72(5) . . ? O5 Mo2 Mo1 94.50(5) 2_757 . ? Cl2 Mo2 Mo1 132.92(2) . . ? Mo2 O3 Mo1 84.25(6) . . ? Mo1 O4 Mo2 82.13(6) . . ? Mo1 O4 Mo1 106.26(7) . 2_757 ? Mo2 O4 Mo1 106.69(7) . 2_757 ? C51 O5 Mo1 119.78(15) . . ? C51 O5 Mo2 127.89(15) . 2_757 ? Mo1 O5 Mo2 107.53(7) . 2_757 ? C1 N C5 122.9(3) . . ? N C1 C2 120.2(3) . . ? C1 C2 C3 118.6(3) . . ? C4 C3 C2 120.0(3) . . ? C3 C4 C5 118.9(3) . . ? N C5 C4 119.5(3) . . ? O5 C51 C52 110.7(2) . . ? O6 C61 C62 112.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.663 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.122 #===END data_1c _database_code_CSD 173628 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dipyridinium tetrabromo-di-\m~2~-ethoxo-diethanol-di-\m~3~- oxo-di-\m~2~-oxo-tetraoxotetramolybdate(V) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H34 Br4 Mo4 N2 O12' _chemical_formula_weight 1173.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.21240(10) _cell_length_b 9.84160(10) _cell_length_c 10.43200(10) _cell_angle_alpha 110.8365(6) _cell_angle_beta 104.1747(6) _cell_angle_gamma 99.9521(6) _cell_volume 821.026(15) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3676 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.374 _exptl_crystal_density_method ? _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 6.414 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7160 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3742 _reflns_number_gt 3237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.9532P] 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 SHELXL _refine_ls_extinction_coef 0.0021(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3742 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.10167(3) -0.02968(3) 1.14326(3) 0.01829(8) Uani 1 d . . . Mo2 Mo 1.14845(3) -0.18487(3) 0.90398(3) 0.01957(8) Uani 1 d . . . Br1 Br 0.94516(4) -0.11748(4) 1.28887(4) 0.03127(10) Uani 1 d . . . Br2 Br 1.07030(4) -0.47145(4) 0.74428(4) 0.03363(11) Uani 1 d . . . O1 O 1.2781(3) 0.0144(3) 1.2649(2) 0.0279(5) Uani 1 d . . . O2 O 1.3377(2) -0.1715(3) 0.9732(2) 0.0273(5) Uani 1 d . . . O3 O 1.0441(2) -0.2464(2) 1.0227(2) 0.0211(4) Uani 1 d . . . O4 O 1.1365(2) 0.0274(2) 0.9873(2) 0.0190(4) Uani 1 d . . . O5 O 1.0677(2) 0.1848(2) 1.2383(2) 0.0209(4) Uani 1 d . . . O6 O 1.2108(3) -0.1425(3) 0.7282(3) 0.0298(5) Uani 1 d . . . H6 H 1.1751 -0.0777 0.7110 0.045 Uiso 1 calc R . . N N 0.7528(3) -0.4374(3) 0.9154(3) 0.0332(7) Uani 1 d . . . H0 H 0.8480 -0.3810 0.9570 0.040 Uiso 1 calc R . . C1 C 0.7263(5) -0.5854(5) 0.8578(4) 0.0390(9) Uani 1 d . . . H1 H 0.8098 -0.6268 0.8626 0.047 Uiso 1 calc R . . C2 C 0.5765(5) -0.6788(4) 0.7909(4) 0.0393(9) Uani 1 d . . . H2 H 0.5570 -0.7837 0.7501 0.047 Uiso 1 calc R . . C3 C 0.4549(4) -0.6140(5) 0.7853(4) 0.0383(9) Uani 1 d . . . H3 H 0.3520 -0.6751 0.7400 0.046 Uiso 1 calc R . . C4 C 0.4870(4) -0.4581(4) 0.8474(4) 0.0352(8) Uani 1 d . . . H4 H 0.4061 -0.4131 0.8450 0.042 Uiso 1 calc R . . C5 C 0.6383(4) -0.3709(4) 0.9121(4) 0.0329(8) Uani 1 d . . . H5 H 0.6619 -0.2656 0.9537 0.040 Uiso 1 calc R . . C51 C 1.1446(4) 0.2778(4) 1.3931(3) 0.0284(7) Uani 1 d . . . H51A H 1.1624 0.2130 1.4434 0.034 Uiso 1 calc R . . H51B H 1.0775 0.3354 1.4311 0.034 Uiso 1 calc R . . C52 C 1.2978(4) 0.3847(4) 1.4206(4) 0.0386(9) Uani 1 d . . . H52A H 1.3643 0.3276 1.3835 0.058 Uiso 1 calc R . . H52B H 1.3473 0.4446 1.5233 0.058 Uiso 1 calc R . . H52C H 1.2798 0.4503 1.3726 0.058 Uiso 1 calc R . . C61 C 1.3536(5) -0.1395(5) 0.6969(4) 0.0452(10) Uani 1 d . . . H61A H 1.3872 -0.2258 0.7028 0.054 Uiso 1 calc R . . H61B H 1.4339 -0.0479 0.7690 0.054 Uiso 1 calc R . . C62 C 1.3348(5) -0.1441(6) 0.5491(4) 0.0508(11) Uani 1 d . . . H62A H 1.4317 -0.1443 0.5304 0.076 Uiso 1 calc R . . H62B H 1.3056 -0.0565 0.5442 0.076 Uiso 1 calc R . . H62C H 1.2548 -0.2344 0.4775 0.076 Uiso 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 0.01621(14) 0.01894(14) 0.01958(15) 0.00771(11) 0.00542(11) 0.00616(11) Mo2 0.01717(15) 0.01925(14) 0.02291(15) 0.00767(11) 0.00789(11) 0.00735(11) Br1 0.0346(2) 0.0329(2) 0.0329(2) 0.01758(16) 0.01566(16) 0.01071(16) Br2 0.0334(2) 0.02347(18) 0.0386(2) 0.00544(15) 0.01206(16) 0.01124(15) O1 0.0226(12) 0.0330(13) 0.0245(12) 0.0107(10) 0.0028(10) 0.0092(10) O2 0.0203(12) 0.0284(12) 0.0340(13) 0.0114(10) 0.0099(10) 0.0109(10) O3 0.0189(11) 0.0206(11) 0.0248(12) 0.0096(9) 0.0068(9) 0.0082(9) O4 0.0179(10) 0.0173(10) 0.0201(11) 0.0059(9) 0.0061(9) 0.0054(8) O5 0.0202(11) 0.0207(11) 0.0180(11) 0.0041(9) 0.0050(9) 0.0074(9) O6 0.0287(13) 0.0357(14) 0.0360(14) 0.0194(11) 0.0185(11) 0.0149(11) N 0.0195(15) 0.0399(18) 0.0340(17) 0.0185(14) 0.0008(13) -0.0015(13) C1 0.039(2) 0.051(3) 0.045(2) 0.032(2) 0.0180(19) 0.027(2) C2 0.055(3) 0.0275(19) 0.038(2) 0.0169(17) 0.0161(19) 0.0094(18) C3 0.0239(19) 0.049(2) 0.033(2) 0.0173(18) 0.0047(16) -0.0041(17) C4 0.0293(19) 0.046(2) 0.038(2) 0.0212(18) 0.0150(17) 0.0175(17) C5 0.041(2) 0.0265(18) 0.0312(19) 0.0129(16) 0.0121(16) 0.0083(16) C51 0.0315(19) 0.0252(17) 0.0189(16) 0.0027(14) 0.0041(14) 0.0053(14) C52 0.036(2) 0.032(2) 0.029(2) 0.0045(16) 0.0009(16) -0.0019(16) C61 0.033(2) 0.070(3) 0.046(2) 0.030(2) 0.0241(19) 0.021(2) C62 0.032(2) 0.088(4) 0.036(2) 0.026(2) 0.0193(18) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.672(2) . ? Mo1 O3 1.946(2) . ? Mo1 O4 1.977(2) . ? Mo1 O5 2.104(2) . ? Mo1 O4 2.290(2) 2_757 ? Mo1 Br1 2.5902(4) . ? Mo1 Mo2 2.6060(4) . ? Mo2 O2 1.678(2) . ? Mo2 O3 1.934(2) . ? Mo2 O4 1.992(2) . ? Mo2 O5 2.173(2) 2_757 ? Mo2 O6 2.2007(22) . ? Mo2 Br2 2.5722(4) . ? O4 Mo1 2.290(2) 2_757 ? O5 C51 1.453(4) . ? O5 Mo2 2.173(2) 2_757 ? O6 C61 1.429(4) . ? N C1 1.313(5) . ? N C5 1.334(5) . ? C1 C2 1.367(5) . ? C2 C3 1.381(5) . ? C3 C4 1.380(5) . ? C4 C5 1.360(5) . ? C51 C52 1.503(5) . ? C61 C62 1.492(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 O1 Mo1 O3 106.45(10) . . ? O1 Mo1 O4 106.42(10) . . ? O3 Mo1 O4 93.71(9) . . ? O1 Mo1 O5 95.03(10) . . ? O3 Mo1 O5 157.26(8) . . ? O4 Mo1 O5 87.15(8) . . ? O1 Mo1 O4 165.29(9) . 2_757 ? O3 Mo1 O4 88.12(8) . 2_757 ? O4 Mo1 O4 73.93(9) . 2_757 ? O5 Mo1 O4 70.26(8) . 2_757 ? O1 Mo1 Br1 95.86(8) . . ? O3 Mo1 Br1 83.09(6) . . ? O4 Mo1 Br1 157.44(6) . . ? O5 Mo1 Br1 87.45(6) . . ? O4 Mo1 Br1 83.64(5) 2_757 . ? O1 Mo1 Mo2 100.54(8) . . ? O3 Mo1 Mo2 47.61(6) . . ? O4 Mo1 Mo2 49.20(6) . . ? O5 Mo1 Mo2 136.18(6) . . ? O4 Mo1 Mo2 90.75(5) 2_757 . ? Br1 Mo1 Mo2 130.605(14) . . ? O2 Mo2 O3 106.44(10) . . ? O2 Mo2 O4 104.65(10) . . ? O3 Mo2 O4 93.61(8) . . ? O2 Mo2 O5 160.82(10) . 2_757 ? O3 Mo2 O5 92.70(8) . 2_757 ? O4 Mo2 O5 74.78(8) . 2_757 ? O2 Mo2 Br2 94.28(8) . . ? O3 Mo2 Br2 84.20(6) . . ? O4 Mo2 Br2 160.75(6) . . ? O5 Mo2 Br2 86.20(5) 2_757 . ? O2 Mo2 Mo1 99.18(8) . . ? O3 Mo2 Mo1 48.00(6) . . ? O4 Mo2 Mo1 48.71(6) . . ? O5 Mo2 Mo1 94.58(5) 2_757 . ? Br2 Mo2 Mo1 132.196(14) . . ? Mo2 O3 Mo1 84.39(8) . . ? Mo1 O4 Mo2 82.09(8) . . ? Mo1 O4 Mo1 106.07(9) . 2_757 ? Mo2 O4 Mo1 106.97(9) . 2_757 ? C51 O5 Mo1 119.81(18) . . ? C51 O5 Mo2 128.43(18) . 2_757 ? Mo1 O5 Mo2 107.35(9) . 2_757 ? C1 N C5 122.8(3) . . ? N C1 C2 120.3(3) . . ? C1 C2 C3 118.6(3) . . ? C4 C3 C2 119.6(3) . . ? C5 C4 C3 119.2(3) . . ? N C5 C4 119.5(3) . . ? O5 C51 C52 110.6(3) . . ? O6 C61 C62 111.5(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.723 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.109 #===END data_2a _database_code_CSD 173629 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dibromo-di-\m~2~-ethoxo-di-\m~3~- oxo-di-\m~2~-oxo-tetraoxotetrapyridine tetramolybdenum(V) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Br2 Mo4 N4 O10' _chemical_formula_weight 1078.10 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8953(3) _cell_length_b 16.9472(4) _cell_length_c 14.4907(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.3770(10) _cell_angle_gamma 90.00 _cell_volume 3375.96(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7426 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method ? _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 3.874 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13525 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7607 _reflns_number_gt 5919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+9.4586P] 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 SHELXL _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7607 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.97954(4) -0.59073(3) 1.03831(3) 0.03619(15) Uani 1 d . . . Mo2 Mo -0.85490(4) -0.55421(3) 0.92970(3) 0.04169(16) Uani 1 d . . . Mo3 Mo -0.43140(4) -0.01083(3) 0.91871(3) 0.03648(15) Uani 1 d . . . Mo4 Mo -0.36114(4) 0.10151(3) 1.02939(4) 0.04034(15) Uani 1 d . . . O1 O -0.9931(3) -0.6875(3) 1.0141(3) 0.0515(11) Uani 1 d . . . O2 O -0.8455(4) -0.6453(3) 0.8851(3) 0.0573(12) Uani 1 d . . . O3 O -0.4064(3) 0.0231(3) 0.8159(3) 0.0469(10) Uani 1 d . . . O4 O -0.3251(4) 0.1591(3) 0.9461(3) 0.0518(11) Uani 1 d . . . O5 O -1.1278(3) -0.5744(3) 1.0493(3) 0.0423(9) Uani 1 d . . . O6 O -0.8423(3) -0.5692(3) 1.0633(3) 0.0448(10) Uani 1 d . . . O7 O -0.9978(3) -0.5339(2) 0.9174(3) 0.0384(8) Uani 1 d . . . O8 O -0.3142(3) -0.0037(2) 1.0071(3) 0.0444(9) Uani 1 d . . . O9 O -0.5677(3) -0.0558(3) 0.8558(3) 0.0431(9) Uani 1 d . . . O10 O -0.4993(3) 0.0759(2) 0.9767(3) 0.0371(8) Uani 1 d . . . N1 N -0.9607(4) -0.6196(3) 1.1901(3) 0.0432(11) Uani 1 d . . . N2 N -0.8647(4) -0.5154(4) 0.7789(4) 0.0544(14) Uani 1 d . . . N3 N -0.3649(4) -0.1256(3) 0.8891(4) 0.0465(12) Uani 1 d . . . N4 N -0.4153(4) 0.2164(3) 1.0840(4) 0.0485(12) Uani 1 d . . . Br2 Br -0.67309(7) -0.52960(7) 0.94898(9) 0.0903(3) Uani 1 d . . . Br4 Br -0.20248(7) 0.12077(6) 1.14324(7) 0.0758(3) Uani 1 d . . . C11 C -0.9054(5) -0.5758(4) 1.2526(4) 0.0484(14) Uani 1 d . . . H11 H -0.8791 -0.5290 1.2338 0.058 Uiso 1 calc R . . C12 C -0.8857(6) -0.5984(6) 1.3464(5) 0.067(2) Uani 1 d . . . H12 H -0.8455 -0.5680 1.3894 0.081 Uiso 1 calc R . . C13 C -0.9272(6) -0.6667(5) 1.3736(5) 0.066(2) Uani 1 d . . . H13 H -0.9149 -0.6831 1.4354 0.079 Uiso 1 calc R . . C14 C -0.9854(7) -0.7096(5) 1.3107(5) 0.067(2) Uani 1 d . . . H14 H -1.0148 -0.7551 1.3290 0.080 Uiso 1 calc R . . C15 C -1.0014(6) -0.6859(4) 1.2189(5) 0.0559(17) Uani 1 d . . . H15 H -1.0412 -0.7163 1.1756 0.067 Uiso 1 calc R . . C21 C -0.8213(6) -0.4499(6) 0.7516(6) 0.072(2) Uani 1 d . . . H21 H -0.7876 -0.4167 0.7961 0.087 Uiso 1 calc R . . C22 C -0.8266(7) -0.4316(8) 0.6571(7) 0.088(3) Uani 1 d . . . H22 H -0.7971 -0.3860 0.6393 0.106 Uiso 1 calc R . . C23 C -0.8742(9) -0.4797(9) 0.5909(7) 0.102(4) Uani 1 d . . . H23 H -0.8762 -0.4681 0.5279 0.122 Uiso 1 calc R . . C24 C -0.9193(9) -0.5453(8) 0.6186(6) 0.095(4) Uani 1 d . . . H24 H -0.9529 -0.5789 0.5745 0.114 Uiso 1 calc R . . C25 C -0.9146(7) -0.5617(7) 0.7131(6) 0.075(2) Uani 1 d . . . H25 H -0.9468 -0.6058 0.7314 0.090 Uiso 1 calc R . . C31 C -0.3474(7) -0.1429(5) 0.8024(6) 0.068(2) Uani 1 d . . . H31 H -0.3702 -0.1086 0.7540 0.082 Uiso 1 calc R . . C32 C -0.2970(8) -0.2094(6) 0.7825(8) 0.088(3) Uani 1 d . . . H32 H -0.2844 -0.2194 0.7223 0.106 Uiso 1 calc R . . C33 C -0.2655(7) -0.2614(5) 0.8561(8) 0.081(3) Uani 1 d . . . H33 H -0.2318 -0.3071 0.8454 0.098 Uiso 1 calc R . . C34 C -0.2848(7) -0.2441(5) 0.9440(8) 0.081(3) Uani 1 d . . . H34 H -0.2652 -0.2779 0.9937 0.097 Uiso 1 calc R . . C35 C -0.3339(6) -0.1755(5) 0.9570(6) 0.0614(18) Uani 1 d . . . H35 H -0.3459 -0.1635 1.0169 0.074 Uiso 1 calc R . . C41 C -0.4527(6) 0.2701(4) 1.0208(6) 0.0622(19) Uani 1 d . . . H41 H -0.4620 0.2561 0.9581 0.075 Uiso 1 calc R . . C42 C -0.4777(7) 0.3445(5) 1.0448(7) 0.075(2) Uani 1 d . . . H42 H -0.5054 0.3801 0.9996 0.090 Uiso 1 calc R . . C43 C -0.4613(7) 0.3652(5) 1.1360(8) 0.082(3) Uani 1 d . . . H43 H -0.4758 0.4160 1.1538 0.098 Uiso 1 calc R . . C44 C -0.4247(8) 0.3131(5) 1.1998(7) 0.078(3) Uani 1 d . . . H44 H -0.4147 0.3271 1.2626 0.094 Uiso 1 calc R . . C45 C -0.4013(7) 0.2375(5) 1.1731(6) 0.067(2) Uani 1 d . . . H45 H -0.3755 0.2013 1.2183 0.080 Uiso 1 calc R . . C51 C -1.1977(6) -0.6358(5) 1.0197(6) 0.069(2) Uani 1 d . . . H51A H -1.2574 -0.6256 1.0448 0.082 Uiso 1 calc R . . H51B H -1.1722 -0.6863 1.0436 0.082 Uiso 1 calc R . . C52 C -1.2183(8) -0.6389(9) 0.9162(8) 0.105(4) Uani 1 d . . . H52A H -1.2438 -0.5890 0.8927 0.158 Uiso 1 calc R . . H52B H -1.2652 -0.6796 0.8975 0.158 Uiso 1 calc R . . H52C H -1.1593 -0.6501 0.8915 0.158 Uiso 1 calc R . . C91 C -0.6090(6) -0.0302(5) 0.7651(5) 0.0616(19) Uani 1 d . . . H91A H -0.6629 -0.0645 0.7415 0.074 Uiso 1 calc R . . H91B H -0.5606 -0.0343 0.7235 0.074 Uiso 1 calc R . . C92 C -0.6445(7) 0.0529(6) 0.7654(7) 0.084(3) Uani 1 d . . . H92A H -0.6749 0.0670 0.7039 0.125 Uiso 1 calc R . . H92B H -0.5906 0.0875 0.7844 0.125 Uiso 1 calc R . . H92C H -0.6908 0.0576 0.8082 0.125 Uiso 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 0.0392(3) 0.0386(3) 0.0305(2) 0.00381(18) 0.00429(18) 0.00343(19) Mo2 0.0408(3) 0.0486(3) 0.0367(3) 0.0069(2) 0.0090(2) 0.0082(2) Mo3 0.0442(3) 0.0313(2) 0.0346(3) 0.00043(18) 0.00768(19) 0.00617(19) Mo4 0.0461(3) 0.0337(3) 0.0418(3) -0.0027(2) 0.0081(2) 0.0032(2) O1 0.061(3) 0.047(3) 0.046(2) -0.001(2) 0.009(2) 0.005(2) O2 0.061(3) 0.059(3) 0.054(3) 0.004(2) 0.017(2) 0.011(2) O3 0.060(3) 0.042(2) 0.041(2) 0.0024(18) 0.0153(19) 0.0051(19) O4 0.066(3) 0.040(2) 0.054(3) -0.0012(19) 0.022(2) 0.001(2) O5 0.039(2) 0.044(2) 0.044(2) 0.0000(18) 0.0059(17) 0.0000(17) O6 0.041(2) 0.055(3) 0.037(2) 0.0091(19) 0.0035(17) 0.0088(19) O7 0.039(2) 0.045(2) 0.0310(18) 0.0051(16) 0.0052(15) 0.0040(17) O8 0.046(2) 0.041(2) 0.047(2) -0.0034(18) 0.0085(18) 0.0087(18) O9 0.047(2) 0.044(2) 0.037(2) -0.0015(18) 0.0025(17) 0.0018(18) O10 0.043(2) 0.0311(18) 0.0367(19) 0.0011(15) 0.0043(16) 0.0069(16) N1 0.044(3) 0.052(3) 0.034(2) 0.009(2) 0.004(2) 0.009(2) N2 0.055(3) 0.068(4) 0.045(3) 0.013(3) 0.022(3) 0.013(3) N3 0.045(3) 0.039(3) 0.056(3) -0.008(2) 0.008(2) 0.007(2) N4 0.048(3) 0.040(3) 0.058(3) -0.010(2) 0.012(2) 0.000(2) Br2 0.0557(5) 0.1067(8) 0.1097(8) 0.0295(6) 0.0164(5) 0.0104(5) Br4 0.0663(5) 0.0779(6) 0.0800(6) -0.0105(5) -0.0001(4) -0.0004(4) C11 0.050(3) 0.058(4) 0.038(3) 0.004(3) 0.007(3) 0.004(3) C12 0.074(5) 0.088(6) 0.037(3) 0.004(4) -0.001(3) 0.002(4) C13 0.072(5) 0.084(6) 0.041(4) 0.027(4) 0.009(3) 0.014(4) C14 0.086(6) 0.063(5) 0.055(4) 0.027(4) 0.022(4) 0.006(4) C15 0.065(4) 0.055(4) 0.047(4) 0.013(3) 0.007(3) -0.004(3) C21 0.056(4) 0.105(7) 0.060(4) 0.022(5) 0.021(4) 0.006(4) C22 0.069(5) 0.130(9) 0.073(6) 0.046(6) 0.035(5) 0.012(6) C23 0.092(7) 0.170(13) 0.048(5) 0.032(7) 0.027(5) 0.056(8) C24 0.103(8) 0.134(10) 0.046(5) 0.000(6) 0.004(5) 0.029(7) C25 0.079(6) 0.096(7) 0.047(4) -0.007(4) 0.001(4) 0.008(5) C31 0.090(6) 0.054(4) 0.064(5) -0.010(4) 0.028(4) 0.013(4) C32 0.100(7) 0.080(6) 0.094(7) -0.020(5) 0.048(6) 0.015(5) C33 0.066(5) 0.048(4) 0.130(9) -0.018(5) 0.017(5) 0.016(4) C34 0.076(6) 0.049(4) 0.114(8) 0.014(5) 0.003(5) 0.023(4) C35 0.073(5) 0.051(4) 0.059(4) 0.005(3) 0.006(4) 0.014(4) C41 0.065(4) 0.046(4) 0.074(5) -0.003(3) 0.006(4) 0.010(3) C42 0.084(6) 0.050(4) 0.093(6) 0.002(4) 0.018(5) 0.022(4) C43 0.091(7) 0.051(5) 0.112(8) -0.024(5) 0.044(6) 0.001(4) C44 0.108(7) 0.058(5) 0.075(6) -0.028(4) 0.031(5) -0.009(5) C45 0.087(6) 0.054(4) 0.062(4) -0.012(4) 0.021(4) 0.007(4) C51 0.055(4) 0.072(5) 0.076(5) 0.011(4) 0.000(4) -0.004(4) C52 0.082(7) 0.130(10) 0.095(8) -0.009(7) -0.019(6) -0.016(7) C91 0.058(4) 0.080(5) 0.043(4) 0.016(3) -0.004(3) -0.014(4) C92 0.077(6) 0.090(7) 0.082(6) 0.035(5) 0.006(5) 0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.682(5) . ? Mo1 O6 1.924(4) . ? Mo1 O7 1.983(4) . ? Mo1 O5 2.107(4) . ? Mo1 N1 2.232(5) . ? Mo1 O7 2.243(4) 3_347 ? Mo1 Mo2 2.5795(7) . ? Mo2 O2 1.686(5) . ? Mo2 O6 1.935(4) . ? Mo2 O7 1.998(4) . ? Mo2 O5 2.218(4) 3_347 ? Mo2 N2 2.267(5) . ? Mo2 Br2 2.5355(11) . ? Mo3 O3 1.679(4) . ? Mo3 O8 1.924(4) . ? Mo3 O10 1.997(4) . ? Mo3 O9 2.121(4) . ? Mo3 O10 2.206(4) 3_457 ? Mo3 N3 2.222(5) . ? Mo3 Mo4 2.5872(7) . ? Mo4 O4 1.684(5) . ? Mo4 O8 1.941(4) . ? Mo4 O10 2.008(4) . ? Mo4 O9 2.197(4) 3_457 ? Mo4 N4 2.271(5) . ? Mo4 Br4 2.5747(10) . ? O5 C51 1.446(9) . ? O5 Mo2 2.218(4) 3_347 ? O7 Mo1 2.243(4) 3_347 ? O9 C91 1.423(8) . ? O9 Mo4 2.197(4) 3_457 ? O10 Mo3 2.206(4) 3_457 ? N1 C11 1.327(9) . ? N1 C15 1.351(9) . ? N2 C21 1.349(11) . ? N2 C25 1.346(11) . ? N3 C35 1.320(9) . ? N3 C31 1.347(9) . ? N4 C45 1.326(9) . ? N4 C41 1.342(10) . ? C11 C12 1.400(9) . ? C12 C13 1.376(12) . ? C13 C14 1.340(13) . ? C14 C15 1.376(10) . ? C21 C22 1.395(12) . ? C22 C23 1.354(18) . ? C23 C24 1.365(19) . ? C24 C25 1.389(12) . ? C31 C32 1.379(12) . ? C32 C33 1.404(15) . ? C33 C34 1.372(14) . ? C34 C35 1.374(11) . ? C41 C42 1.367(11) . ? C42 C43 1.354(14) . ? C43 C44 1.325(14) . ? C44 C45 1.390(11) . ? C51 C52 1.486(13) . ? C91 C92 1.492(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O6 107.6(2) . . ? O1 Mo1 O7 107.1(2) . . ? O6 Mo1 O7 94.01(17) . . ? O1 Mo1 O5 93.6(2) . . ? O6 Mo1 O5 156.05(18) . . ? O7 Mo1 O5 90.11(16) . . ? O1 Mo1 N1 89.2(2) . . ? O6 Mo1 N1 83.40(18) . . ? O7 Mo1 N1 163.53(19) . . ? O5 Mo1 N1 86.00(17) . . ? O1 Mo1 O7 164.09(19) . 3_347 ? O6 Mo1 O7 86.78(17) . 3_347 ? O7 Mo1 O7 77.89(17) . 3_347 ? O5 Mo1 O7 71.03(16) . 3_347 ? N1 Mo1 O7 85.72(17) . 3_347 ? O1 Mo1 Mo2 99.89(16) . . ? O6 Mo1 Mo2 48.24(12) . . ? O7 Mo1 Mo2 49.86(11) . . ? O5 Mo1 Mo2 139.90(12) . . ? N1 Mo1 Mo2 131.39(14) . . ? O7 Mo1 Mo2 94.78(10) 3_347 . ? O2 Mo2 O6 105.2(2) . . ? O2 Mo2 O7 104.8(2) . . ? O6 Mo2 O7 93.22(16) . . ? O2 Mo2 O5 165.5(2) . 3_347 ? O6 Mo2 O5 89.25(18) . 3_347 ? O7 Mo2 O5 73.52(16) . 3_347 ? O2 Mo2 N2 83.9(2) . . ? O6 Mo2 N2 170.5(2) . . ? O7 Mo2 N2 86.83(18) . . ? O5 Mo2 N2 81.7(2) 3_347 . ? O2 Mo2 Br2 93.53(18) . . ? O6 Mo2 Br2 88.14(13) . . ? O7 Mo2 Br2 160.57(13) . . ? O5 Mo2 Br2 87.12(11) 3_347 . ? N2 Mo2 Br2 88.70(16) . . ? O2 Mo2 Mo1 96.33(17) . . ? O6 Mo2 Mo1 47.88(13) . . ? O7 Mo2 Mo1 49.37(11) . . ? O5 Mo2 Mo1 93.20(11) 3_347 . ? N2 Mo2 Mo1 134.95(16) . . ? Br2 Mo2 Mo1 135.97(4) . . ? O3 Mo3 O8 107.7(2) . . ? O3 Mo3 O10 107.00(19) . . ? O8 Mo3 O10 94.57(16) . . ? O3 Mo3 O9 91.6(2) . . ? O8 Mo3 O9 157.76(18) . . ? O10 Mo3 O9 89.91(16) . . ? O3 Mo3 O10 161.4(2) . 3_457 ? O8 Mo3 O10 89.20(17) . 3_457 ? O10 Mo3 O10 78.39(17) . 3_457 ? O9 Mo3 O10 70.37(15) . 3_457 ? O3 Mo3 N3 89.0(2) . . ? O8 Mo3 N3 81.27(19) . . ? O10 Mo3 N3 163.93(19) . . ? O9 Mo3 N3 88.43(18) . . ? O10 Mo3 N3 86.01(18) 3_457 . ? O3 Mo3 Mo4 100.93(16) . . ? O8 Mo3 Mo4 48.27(12) . . ? O10 Mo3 Mo4 49.94(12) . . ? O9 Mo3 Mo4 139.82(12) . . ? O10 Mo3 Mo4 96.03(10) 3_457 . ? N3 Mo3 Mo4 129.34(14) . . ? O4 Mo4 O8 105.7(2) . . ? O4 Mo4 O10 102.7(2) . . ? O8 Mo4 O10 93.69(17) . . ? O4 Mo4 O9 163.88(19) . 3_457 ? O8 Mo4 O9 90.10(17) . 3_457 ? O10 Mo4 O9 72.60(15) . 3_457 ? O4 Mo4 N4 84.3(2) . . ? O8 Mo4 N4 169.0(2) . . ? O10 Mo4 N4 88.32(18) . . ? O9 Mo4 N4 80.17(18) 3_457 . ? O4 Mo4 Br4 93.99(18) . . ? O8 Mo4 Br4 86.88(14) . . ? O10 Mo4 Br4 162.42(11) . . ? O9 Mo4 Br4 89.84(11) 3_457 . ? N4 Mo4 Br4 87.95(15) . . ? O4 Mo4 Mo3 96.16(16) . . ? O8 Mo4 Mo3 47.70(13) . . ? O10 Mo4 Mo3 49.58(11) . . ? O9 Mo4 Mo3 92.26(11) 3_457 . ? N4 Mo4 Mo3 137.11(14) . . ? Br4 Mo4 Mo3 134.51(3) . . ? C51 O5 Mo1 120.3(5) . . ? C51 O5 Mo2 131.8(4) . 3_347 ? Mo1 O5 Mo2 105.47(18) . 3_347 ? Mo1 O6 Mo2 83.88(16) . . ? Mo1 O7 Mo2 80.78(14) . . ? Mo1 O7 Mo1 102.11(17) . 3_347 ? Mo2 O7 Mo1 108.41(18) . 3_347 ? Mo3 O8 Mo4 84.04(17) . . ? C91 O9 Mo3 120.2(4) . . ? C91 O9 Mo4 129.9(4) . 3_457 ? Mo3 O9 Mo4 105.85(17) . 3_457 ? Mo3 O10 Mo4 80.49(14) . . ? Mo3 O10 Mo3 101.61(17) . 3_457 ? Mo4 O10 Mo3 109.61(17) . 3_457 ? C11 N1 C15 118.8(6) . . ? C11 N1 Mo1 121.6(4) . . ? C15 N1 Mo1 119.5(5) . . ? C21 N2 C25 118.5(7) . . ? C21 N2 Mo2 123.7(6) . . ? C25 N2 Mo2 117.8(6) . . ? C35 N3 C31 118.2(6) . . ? C35 N3 Mo3 121.1(5) . . ? C31 N3 Mo3 120.5(5) . . ? C45 N4 C41 118.0(7) . . ? C45 N4 Mo4 124.2(5) . . ? C41 N4 Mo4 117.3(5) . . ? N1 C11 C12 121.3(7) . . ? C13 C12 C11 118.6(8) . . ? C14 C13 C12 119.8(7) . . ? C13 C14 C15 119.7(8) . . ? N1 C15 C14 121.6(7) . . ? N2 C21 C22 120.6(10) . . ? C23 C22 C21 120.8(11) . . ? C22 C23 C24 118.6(9) . . ? C23 C24 C25 119.6(11) . . ? N2 C25 C24 121.8(11) . . ? N3 C31 C32 122.6(9) . . ? C31 C32 C33 117.8(9) . . ? C34 C33 C32 119.3(8) . . ? C35 C34 C33 118.4(9) . . ? N3 C35 C34 123.7(8) . . ? N4 C41 C42 122.7(8) . . ? C43 C42 C41 118.3(9) . . ? C44 C43 C42 120.2(8) . . ? C43 C44 C45 120.0(9) . . ? N4 C45 C44 120.9(9) . . ? O5 C51 C52 110.3(8) . . ? O9 C91 C92 112.0(7) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.324 _refine_diff_density_min -2.065 _refine_diff_density_rms 0.145 #===END data_2b _database_code_CSD 173630 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dibromo-di-\m~2~-ethoxo-di-\m~3~- oxo-di-\m~2~-oxo-tetraoxotetrapyridine tetramolybdenum(V).acetonitrile (1/2) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Br2 Mo4 N6 O10' _chemical_formula_weight 1160.21 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4794(2) _cell_length_b 12.75790(10) _cell_length_c 13.5427(2) _cell_angle_alpha 67.5773(5) _cell_angle_beta 82.6479(5) _cell_angle_gamma 70.4822(5) _cell_volume 1878.60(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7397 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14962 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.31 _reflns_number_total 8344 _reflns_number_gt 7481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+12.6347P] 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 8344 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.11789(3) 0.44557(4) 0.94226(3) 0.01350(10) Uani 1 d . . . Mo2 Mo 0.10281(3) 0.65816(4) 0.92654(3) 0.01491(10) Uani 1 d . . . Mo3 Mo -0.53108(3) 0.45423(3) 1.62636(3) 0.01070(9) Uani 1 d . . . Mo4 Mo -0.43301(3) 0.26985(3) 1.57193(3) 0.01278(10) Uani 1 d . . . Br2 Br 0.08020(6) 0.85653(5) 0.77101(5) 0.03479(15) Uani 1 d . . . Br4 Br -0.24223(5) 0.10610(5) 1.61793(5) 0.03388(15) Uani 1 d . . . O1 O 0.2598(3) 0.3816(3) 0.9501(3) 0.0193(7) Uani 1 d . . . O2 O 0.2427(3) 0.6309(3) 0.9392(3) 0.0224(7) Uani 1 d . . . O3 O -0.6225(3) 0.4057(3) 1.7205(3) 0.0171(7) Uani 1 d . . . O4 O -0.5097(3) 0.1831(3) 1.6512(3) 0.0204(7) Uani 1 d . . . O5 O 0.0850(3) 0.2926(3) 1.0575(3) 0.0163(7) Uani 1 d . . . C51 C 0.1622(4) 0.2272(5) 1.1471(4) 0.0221(10) Uani 1 d . . . H51A H 0.1210 0.1933 1.2105 0.027 Uiso 1 calc R . . H51B H 0.1927 0.2815 1.1601 0.027 Uiso 1 calc R . . C52 C 0.2589(5) 0.1284(5) 1.1266(5) 0.0351(14) Uani 1 d . . . H52A H 0.3089 0.0867 1.1871 0.053 Uiso 1 calc R . . H52B H 0.3003 0.1620 1.0643 0.053 Uiso 1 calc R . . H52C H 0.2289 0.0737 1.1152 0.053 Uiso 1 calc R . . O6 O 0.0882(3) 0.5946(3) 0.8223(3) 0.0179(7) Uani 1 d . . . O7 O 0.0702(3) 0.5237(3) 1.0498(3) 0.0148(6) Uani 1 d . . . O8 O -0.3849(3) 0.3330(3) 1.6621(3) 0.0155(6) Uani 1 d . . . O9 O -0.6503(3) 0.6267(3) 1.5658(3) 0.0132(6) Uani 1 d . . . C91 C -0.7694(4) 0.6424(5) 1.5872(4) 0.0188(10) Uani 1 d . . . H91A H -0.8089 0.7256 1.5762 0.023 Uiso 1 calc R . . H91B H -0.7793 0.5955 1.6614 0.023 Uiso 1 calc R . . C92 C -0.8214(4) 0.6049(5) 1.5160(5) 0.0245(11) Uani 1 d . . . H92A H -0.9008 0.6170 1.5325 0.037 Uiso 1 calc R . . H92B H -0.7836 0.5221 1.5279 0.037 Uiso 1 calc R . . H92C H -0.8128 0.6520 1.4426 0.037 Uiso 1 calc R . . O10 O -0.5521(3) 0.4252(3) 1.4971(2) 0.0116(6) Uani 1 d . . . N1 N 0.1105(4) 0.3784(4) 0.8160(3) 0.0179(8) Uani 1 d . . . C11 C 0.0243(5) 0.4352(5) 0.7465(4) 0.0238(11) Uani 1 d . . . H11 H -0.0348 0.4981 0.7562 0.029 Uiso 1 calc R . . C12 C 0.0201(6) 0.4033(6) 0.6608(5) 0.0325(13) Uani 1 d . . . H12 H -0.0419 0.4425 0.6148 0.039 Uiso 1 calc R . . C13 C 0.1086(7) 0.3132(7) 0.6445(5) 0.0410(16) Uani 1 d . . . H13 H 0.1079 0.2918 0.5861 0.049 Uiso 1 calc R . . C14 C -0.3244(5) 0.5705(5) 1.7831(4) 0.0245(11) Uani 1 d . . . H14 H -0.2506 0.5747 1.7745 0.029 Uiso 1 calc R . . C15 C 0.1966(5) 0.2887(5) 0.8008(4) 0.0236(11) Uani 1 d . . . H15 H 0.2565 0.2488 0.8493 0.028 Uiso 1 calc R . . N2 N 0.0795(4) 0.7592(4) 1.0389(3) 0.0180(8) Uani 1 d . . . C21 C 0.1690(5) 0.7344(5) 1.1008(4) 0.0246(11) Uani 1 d . . . H21 H 0.2370 0.6783 1.0942 0.029 Uiso 1 calc R . . C22 C 0.1636(5) 0.7884(5) 1.1727(5) 0.0265(11) Uani 1 d . . . H22 H 0.2261 0.7677 1.2147 0.032 Uiso 1 calc R . . C23 C 0.0645(5) 0.8734(5) 1.1814(4) 0.0256(11) Uani 1 d . . . H23 H 0.0590 0.9114 1.2292 0.031 Uiso 1 calc R . . C24 C -0.0271(5) 0.9017(5) 1.1177(4) 0.0245(11) Uani 1 d . . . H24 H -0.0949 0.9595 1.1218 0.029 Uiso 1 calc R . . C25 C -0.0164(4) 0.8428(4) 1.0482(4) 0.0196(10) Uani 1 d . . . H25 H -0.0785 0.8620 1.0061 0.023 Uiso 1 calc R . . N3 N -0.4708(3) 0.5218(3) 1.7301(3) 0.0141(7) Uani 1 d . . . C31 C -0.5396(4) 0.5571(5) 1.8029(4) 0.0247(11) Uani 1 d . . . H31 H -0.6132 0.5527 1.8097 0.030 Uiso 1 calc R . . C32 C -0.5045(5) 0.6002(6) 1.8685(5) 0.0314(13) Uani 1 d . . . H32 H -0.5542 0.6247 1.9185 0.038 Uiso 1 calc R . . C33 C -0.3959(5) 0.6065(5) 1.8592(4) 0.0252(11) Uani 1 d . . . H33 H -0.3707 0.6345 1.9032 0.030 Uiso 1 calc R . . C34 C 0.1990(6) 0.2539(6) 0.7152(5) 0.0337(14) Uani 1 d . . . H34 H 0.2598 0.1924 0.7054 0.040 Uiso 1 calc R . . C35 C -0.3646(4) 0.5281(5) 1.7202(4) 0.0204(10) Uani 1 d . . . H35 H -0.3166 0.5033 1.6695 0.024 Uiso 1 calc R . . N4 N -0.4532(4) 0.1962(4) 1.4473(3) 0.0176(8) Uani 1 d . . . C41 C -0.3677(5) 0.1626(5) 1.3836(4) 0.0250(11) Uani 1 d . . . H41 H -0.3005 0.1791 1.3837 0.030 Uiso 1 calc R . . C42 C -0.3750(5) 0.1049(5) 1.3183(5) 0.0315(13) Uani 1 d . . . H42 H -0.3136 0.0824 1.2759 0.038 Uiso 1 calc R . . C43 C -0.4743(5) 0.0808(5) 1.3166(4) 0.0267(12) Uani 1 d . . . H43 H -0.4811 0.0415 1.2733 0.032 Uiso 1 calc R . . C44 C -0.5634(5) 0.1161(5) 1.3803(5) 0.0285(12) Uani 1 d . . . H44 H -0.6316 0.1015 1.3806 0.034 Uiso 1 calc R . . C45 C -0.5497(5) 0.1738(5) 1.4438(4) 0.0229(11) Uani 1 d . . . H45 H -0.6105 0.1982 1.4861 0.028 Uiso 1 calc R . . N6 N -0.8479(6) 0.2812(7) 1.3949(5) 0.0491(15) Uani 1 d . . . C61 C -0.8890(5) 0.2081(7) 1.4324(5) 0.0359(14) Uani 1 d . . . C62 C -0.9433(6) 0.1158(7) 1.4823(7) 0.0464(17) Uani 1 d . . . H62A H -0.8867 0.0408 1.5162 0.070 Uiso 1 calc R . . H62B H -0.9821 0.1097 1.4288 0.070 Uiso 1 calc R . . H62C H -0.9970 0.1359 1.5347 0.070 Uiso 1 calc R . . N7 N -0.3568(8) 1.0261(8) 1.0817(6) 0.076(2) Uani 1 d . . . C71 C -0.4045(7) 1.0919(7) 1.0061(6) 0.0455(17) Uani 1 d . . . C72 C -0.4656(7) 1.1761(8) 0.9087(6) 0.059(2) Uani 1 d . . . H72A H -0.4985 1.1357 0.8800 0.088 Uiso 1 calc R . . H72B H -0.4139 1.2095 0.8576 0.088 Uiso 1 calc R . . H72C H -0.5247 1.2387 0.9242 0.088 Uiso 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 0.01259(19) 0.0189(2) 0.01340(19) -0.00983(16) 0.00352(14) -0.00704(15) Mo2 0.01434(19) 0.0191(2) 0.0159(2) -0.00994(16) 0.00442(15) -0.00828(15) Mo3 0.01105(18) 0.01315(18) 0.00991(18) -0.00548(14) 0.00178(13) -0.00539(14) Mo4 0.01451(19) 0.01202(18) 0.01312(19) -0.00563(15) 0.00150(14) -0.00504(14) Br2 0.0414(3) 0.0303(3) 0.0331(3) -0.0107(3) 0.0057(3) -0.0146(3) Br4 0.0329(3) 0.0293(3) 0.0352(3) -0.0124(3) -0.0022(2) -0.0027(2) O1 0.0165(16) 0.0264(18) 0.0198(17) -0.0142(15) 0.0049(13) -0.0079(14) O2 0.0195(17) 0.0277(19) 0.0278(19) -0.0162(16) 0.0059(14) -0.0119(15) O3 0.0185(16) 0.0205(17) 0.0139(16) -0.0063(13) 0.0039(13) -0.0097(14) O4 0.0264(19) 0.0163(16) 0.0210(18) -0.0092(14) 0.0066(14) -0.0094(14) O5 0.0167(16) 0.0206(17) 0.0143(16) -0.0070(13) 0.0017(13) -0.0090(13) C51 0.024(3) 0.028(3) 0.016(2) -0.008(2) -0.0018(19) -0.010(2) C52 0.031(3) 0.028(3) 0.033(3) -0.003(3) -0.006(2) 0.001(2) O6 0.0197(17) 0.0233(17) 0.0148(16) -0.0101(14) 0.0046(13) -0.0098(14) O7 0.0117(15) 0.0223(17) 0.0142(15) -0.0098(13) 0.0024(12) -0.0069(13) O8 0.0163(16) 0.0156(15) 0.0149(16) -0.0068(13) -0.0002(12) -0.0037(13) O9 0.0107(15) 0.0162(15) 0.0143(15) -0.0077(13) 0.0034(12) -0.0050(12) C91 0.011(2) 0.021(2) 0.024(2) -0.011(2) 0.0035(18) -0.0023(18) C92 0.013(2) 0.031(3) 0.034(3) -0.015(2) 0.001(2) -0.010(2) O10 0.0120(14) 0.0126(14) 0.0123(15) -0.0054(12) 0.0026(11) -0.0064(12) N1 0.019(2) 0.025(2) 0.017(2) -0.0125(17) 0.0062(16) -0.0134(17) C11 0.028(3) 0.034(3) 0.017(2) -0.011(2) 0.004(2) -0.018(2) C12 0.045(4) 0.042(3) 0.023(3) -0.016(3) -0.002(2) -0.023(3) C13 0.061(4) 0.057(4) 0.029(3) -0.028(3) 0.011(3) -0.037(4) C14 0.019(2) 0.032(3) 0.030(3) -0.015(2) -0.003(2) -0.012(2) C15 0.024(3) 0.028(3) 0.029(3) -0.018(2) 0.010(2) -0.015(2) N2 0.019(2) 0.020(2) 0.019(2) -0.0095(17) 0.0015(16) -0.0078(16) C21 0.021(3) 0.028(3) 0.026(3) -0.013(2) -0.004(2) -0.004(2) C22 0.028(3) 0.030(3) 0.025(3) -0.013(2) -0.004(2) -0.010(2) C23 0.034(3) 0.028(3) 0.023(3) -0.014(2) 0.000(2) -0.014(2) C24 0.026(3) 0.023(3) 0.027(3) -0.014(2) 0.004(2) -0.006(2) C25 0.019(2) 0.021(2) 0.020(2) -0.011(2) 0.0012(19) -0.0047(19) N3 0.0136(18) 0.0148(18) 0.0155(19) -0.0061(15) -0.0004(14) -0.0055(15) C31 0.018(2) 0.043(3) 0.026(3) -0.024(2) 0.006(2) -0.014(2) C32 0.029(3) 0.047(4) 0.031(3) -0.029(3) 0.007(2) -0.014(3) C33 0.025(3) 0.031(3) 0.028(3) -0.016(2) -0.005(2) -0.010(2) C34 0.041(3) 0.042(3) 0.038(3) -0.031(3) 0.019(3) -0.024(3) C35 0.018(2) 0.027(3) 0.021(2) -0.013(2) 0.0045(19) -0.009(2) N4 0.021(2) 0.0150(19) 0.019(2) -0.0094(16) -0.0003(16) -0.0050(16) C41 0.026(3) 0.030(3) 0.027(3) -0.017(2) 0.004(2) -0.011(2) C42 0.038(3) 0.034(3) 0.033(3) -0.026(3) 0.008(3) -0.012(3) C43 0.040(3) 0.021(2) 0.025(3) -0.012(2) -0.004(2) -0.012(2) C44 0.031(3) 0.027(3) 0.032(3) -0.012(2) -0.006(2) -0.010(2) C45 0.023(3) 0.025(3) 0.026(3) -0.013(2) -0.002(2) -0.007(2) N6 0.044(3) 0.068(4) 0.039(3) -0.026(3) 0.013(3) -0.019(3) C61 0.029(3) 0.053(4) 0.026(3) -0.024(3) 0.005(2) -0.004(3) C62 0.036(4) 0.044(4) 0.064(5) -0.029(4) 0.004(3) -0.008(3) N7 0.090(6) 0.066(5) 0.043(4) -0.013(4) -0.006(4) 0.004(4) C71 0.049(4) 0.046(4) 0.031(4) -0.010(3) 0.003(3) -0.009(3) C72 0.045(4) 0.070(6) 0.034(4) 0.007(4) -0.002(3) -0.013(4) _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 O1 1.682(3) . ? Mo1 O6 1.928(4) . ? Mo1 O7 1.990(3) . ? Mo1 O5 2.112(3) . ? Mo1 N1 2.209(4) . ? Mo1 O7 2.243(3) 2_567 ? Mo1 Mo2 2.5817(6) . ? Mo2 O2 1.680(4) . ? Mo2 O6 1.929(3) . ? Mo2 O7 2.000(3) . ? Mo2 O5 2.219(3) 2_567 ? Mo2 N2 2.279(4) . ? Mo2 Br2 2.5553(7) . ? Mo3 O3 1.676(3) . ? Mo3 O8 1.930(3) . ? Mo3 O10 1.987(3) . ? Mo3 O9 2.116(3) . ? Mo3 O10 2.213(3) 2_468 ? Mo3 N3 2.216(4) . ? Mo3 Mo4 2.5966(5) . ? Mo4 O4 1.683(3) . ? Mo4 O8 1.939(3) . ? Mo4 O10 2.012(3) . ? Mo4 O9 2.201(3) 2_468 ? Mo4 N4 2.296(4) . ? Mo4 Br4 2.5464(7) . ? O5 C51 1.445(6) . ? O5 Mo2 2.219(3) 2_567 ? C51 C52 1.513(8) . ? O7 Mo1 2.243(3) 2_567 ? O9 C91 1.438(5) . ? O9 Mo4 2.201(3) 2_468 ? C91 C92 1.516(7) . ? O10 Mo3 2.213(3) 2_468 ? N1 C11 1.337(7) . ? N1 C15 1.345(7) . ? C11 C12 1.380(7) . ? C12 C13 1.368(10) . ? C13 C34 1.384(10) . ? C14 C35 1.382(7) . ? C14 C33 1.387(8) . ? C15 C34 1.385(8) . ? N2 C25 1.341(6) . ? N2 C21 1.360(7) . ? C21 C22 1.375(8) . ? C22 C23 1.371(8) . ? C23 C24 1.385(8) . ? C24 C25 1.382(7) . ? N3 C31 1.332(6) . ? N3 C35 1.341(6) . ? C31 C32 1.385(7) . ? C32 C33 1.372(8) . ? N4 C45 1.338(7) . ? N4 C41 1.344(7) . ? C41 C42 1.376(8) . ? C42 C43 1.379(8) . ? C43 C44 1.379(9) . ? C44 C45 1.384(8) . ? N6 C61 1.132(10) . ? C61 C62 1.453(10) . ? N7 C71 1.129(10) . ? C71 C72 1.450(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O6 106.93(16) . . ? O1 Mo1 O7 108.29(15) . . ? O6 Mo1 O7 93.86(14) . . ? O1 Mo1 O5 93.69(16) . . ? O6 Mo1 O5 157.41(14) . . ? O7 Mo1 O5 88.15(13) . . ? O1 Mo1 N1 90.30(16) . . ? O6 Mo1 N1 81.60(15) . . ? O7 Mo1 N1 161.37(14) . . ? O5 Mo1 N1 89.34(14) . . ? O1 Mo1 O7 163.61(15) . 2_567 ? O6 Mo1 O7 87.11(13) . 2_567 ? O7 Mo1 O7 78.41(13) . 2_567 ? O5 Mo1 O7 71.24(13) . 2_567 ? N1 Mo1 O7 83.30(14) . 2_567 ? O1 Mo1 Mo2 100.44(12) . . ? O6 Mo1 Mo2 48.00(10) . . ? O7 Mo1 Mo2 49.86(10) . . ? O5 Mo1 Mo2 137.99(9) . . ? N1 Mo1 Mo2 129.51(11) . . ? O7 Mo1 Mo2 95.25(9) 2_567 . ? O2 Mo2 O6 106.41(16) . . ? O2 Mo2 O7 102.89(16) . . ? O6 Mo2 O7 93.49(14) . . ? O2 Mo2 O5 166.43(15) . 2_567 ? O6 Mo2 O5 87.03(13) . 2_567 ? O7 Mo2 O5 73.77(13) . 2_567 ? O2 Mo2 N2 85.39(16) . . ? O6 Mo2 N2 167.23(15) . . ? O7 Mo2 N2 88.47(14) . . ? O5 Mo2 N2 81.40(14) 2_567 . ? O2 Mo2 Br2 93.43(13) . . ? O6 Mo2 Br2 86.70(11) . . ? O7 Mo2 Br2 162.89(10) . . ? O5 Mo2 Br2 89.17(9) 2_567 . ? N2 Mo2 Br2 87.74(11) . . ? O2 Mo2 Mo1 95.95(13) . . ? O6 Mo2 Mo1 47.97(10) . . ? O7 Mo2 Mo1 49.50(9) . . ? O5 Mo2 Mo1 91.67(9) 2_567 . ? N2 Mo2 Mo1 137.29(11) . . ? Br2 Mo2 Mo1 134.51(2) . . ? O3 Mo3 O8 106.81(15) . . ? O3 Mo3 O10 108.60(15) . . ? O8 Mo3 O10 94.51(13) . . ? O3 Mo3 O9 91.62(15) . . ? O8 Mo3 O9 158.48(13) . . ? O10 Mo3 O9 89.87(12) . . ? O3 Mo3 O10 161.25(14) . 2_468 ? O8 Mo3 O10 89.32(13) . 2_468 ? O10 Mo3 O10 78.82(13) . 2_468 ? O9 Mo3 O10 70.85(12) . 2_468 ? O3 Mo3 N3 91.22(16) . . ? O8 Mo3 N3 82.48(14) . . ? O10 Mo3 N3 159.90(14) . . ? O9 Mo3 N3 86.19(13) . . ? O10 Mo3 N3 81.27(13) 2_468 . ? O3 Mo3 Mo4 101.93(12) . . ? O8 Mo3 Mo4 47.99(10) . . ? O10 Mo3 Mo4 49.93(9) . . ? O9 Mo3 Mo4 139.76(9) . . ? O10 Mo3 Mo4 95.96(8) 2_468 . ? N3 Mo3 Mo4 130.47(10) . . ? O4 Mo4 O8 105.76(16) . . ? O4 Mo4 O10 103.40(15) . . ? O8 Mo4 O10 93.47(13) . . ? O4 Mo4 O9 164.32(15) . 2_468 ? O8 Mo4 O9 89.79(13) . 2_468 ? O10 Mo4 O9 73.01(12) . 2_468 ? O4 Mo4 N4 84.65(16) . . ? O8 Mo4 N4 167.66(15) . . ? O10 Mo4 N4 90.43(14) . . ? O9 Mo4 N4 80.16(13) 2_468 . ? O4 Mo4 Br4 95.05(12) . . ? O8 Mo4 Br4 85.72(10) . . ? O10 Mo4 Br4 161.00(9) . . ? O9 Mo4 Br4 88.00(8) 2_468 . ? N4 Mo4 Br4 86.79(10) . . ? O4 Mo4 Mo3 97.18(12) . . ? O8 Mo4 Mo3 47.71(10) . . ? O10 Mo4 Mo3 49.11(9) . . ? O9 Mo4 Mo3 91.78(8) 2_468 . ? N4 Mo4 Mo3 138.97(10) . . ? Br4 Mo4 Mo3 133.42(2) . . ? C51 O5 Mo1 116.1(3) . . ? C51 O5 Mo2 123.7(3) . 2_567 ? Mo1 O5 Mo2 105.46(14) . 2_567 ? O5 C51 C52 111.2(4) . . ? Mo1 O6 Mo2 84.03(13) . . ? Mo1 O7 Mo2 80.64(12) . . ? Mo1 O7 Mo1 101.59(13) . 2_567 ? Mo2 O7 Mo1 108.54(14) . 2_567 ? Mo3 O8 Mo4 84.30(13) . . ? C91 O9 Mo3 119.6(3) . . ? C91 O9 Mo4 129.5(3) . 2_468 ? Mo3 O9 Mo4 105.74(13) . 2_468 ? O9 C91 C92 112.0(4) . . ? Mo3 O10 Mo4 80.97(12) . . ? Mo3 O10 Mo3 101.18(13) . 2_468 ? Mo4 O10 Mo3 108.99(14) . 2_468 ? C11 N1 C15 118.8(5) . . ? C11 N1 Mo1 119.6(4) . . ? C15 N1 Mo1 121.3(4) . . ? N1 C11 C12 122.0(6) . . ? C13 C12 C11 119.1(6) . . ? C12 C13 C34 119.7(5) . . ? C35 C14 C33 118.9(5) . . ? N1 C15 C34 122.1(6) . . ? C25 N2 C21 117.0(4) . . ? C25 N2 Mo2 124.7(3) . . ? C21 N2 Mo2 118.3(3) . . ? N2 C21 C22 123.1(5) . . ? C23 C22 C21 119.0(5) . . ? C22 C23 C24 118.9(5) . . ? C25 C24 C23 119.1(5) . . ? N2 C25 C24 122.8(5) . . ? C31 N3 C35 119.1(4) . . ? C31 N3 Mo3 120.5(3) . . ? C35 N3 Mo3 120.4(3) . . ? N3 C31 C32 121.9(5) . . ? C33 C32 C31 119.5(5) . . ? C32 C33 C14 118.7(5) . . ? C13 C34 C15 118.3(6) . . ? N3 C35 C14 122.0(5) . . ? C45 N4 C41 117.2(4) . . ? C45 N4 Mo4 119.6(3) . . ? C41 N4 Mo4 122.8(3) . . ? N4 C41 C42 123.0(5) . . ? C41 C42 C43 119.2(5) . . ? C42 C43 C44 118.5(5) . . ? C43 C44 C45 119.0(5) . . ? N4 C45 C44 123.0(5) . . ? N6 C61 C62 178.5(7) . . ? N7 C71 C72 179.8(9) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.180 _refine_diff_density_min -2.362 _refine_diff_density_rms 0.176 #===END data_3 _database_code_CSD 173631 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetramethylpyrazinium(2+) nonadecaoxohexamolybdate(VI). tetrametyhlpyrazine.ethanol (1/1/2) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H38 Mo6 N4 O21' _chemical_formula_weight 1246.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.66390(10) _cell_length_b 10.82010(10) _cell_length_c 11.05740(10) _cell_angle_alpha 77.6940(4) _cell_angle_beta 67.0360(4) _cell_angle_gamma 67.1440(4) _cell_volume 877.163(15) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3997 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'yellow white' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.359 _exptl_crystal_density_method ? _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 2.168 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7765 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4020 _reflns_number_gt 3608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.5839P] 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 SHELXL _refine_ls_extinction_coef 0.0042(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4020 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo01 Mo 0.91659(3) 0.18264(2) 0.11829(2) 0.02265(7) Uani 1 d . . . Mo02 Mo 1.09686(3) -0.14447(2) 0.16299(2) 0.02353(7) Uani 1 d . . . Mo03 Mo 1.28185(3) 0.01677(2) -0.10686(2) 0.02234(7) Uani 1 d . . . O1 O 0.8637(3) 0.31426(19) 0.20258(19) 0.0346(4) Uani 1 d . . . O2 O 1.1681(3) -0.25025(19) 0.28082(18) 0.0349(4) Uani 1 d . . . O3 O 1.4871(2) 0.02592(19) -0.18872(18) 0.0322(4) Uani 1 d . . . O4 O 0.7087(2) 0.13749(17) 0.18329(17) 0.0254(4) Uani 1 d . . . O5 O 0.8608(2) 0.26507(16) -0.03845(18) 0.0272(4) Uani 1 d . . . O6 O 1.0185(2) 0.03049(18) 0.22529(17) 0.0272(4) Uani 1 d . . . O7 O 1.1663(2) 0.15734(18) 0.00537(18) 0.0277(4) Uani 1 d . . . O8 O 1.0000 0.0000 0.0000 0.0176(4) Uani 1 d S . . O9 O 0.8490(2) -0.12550(17) 0.22163(17) 0.0265(4) Uani 1 d . . . O10 O 1.3082(2) -0.10920(18) 0.04162(17) 0.0268(4) Uani 1 d . . . N1 N 1.5522(3) -0.47551(19) -0.1316(2) 0.0220(4) Uani 1 d . . . H1 H 1.5857 -0.4598 -0.2158 0.026 Uiso 1 calc R . . C11 C 1.6000(3) -0.4193(2) -0.0618(2) 0.0217(5) Uani 1 d . . . C12 C 1.4536(3) -0.5558(2) -0.0746(2) 0.0214(5) Uani 1 d . . . C13 C 1.7109(4) -0.3319(3) -0.1334(3) 0.0324(6) Uani 1 d . . . H13A H 1.8238 -0.3710 -0.1200 0.049 Uiso 1 calc R . . H13B H 1.6504 -0.2442 -0.1003 0.049 Uiso 1 calc R . . H13C H 1.7297 -0.3245 -0.2257 0.049 Uiso 1 calc R . . C14 C 1.4054(4) -0.6144(3) -0.1598(3) 0.0279(5) Uani 1 d . . . H14A H 1.2781 -0.5883 -0.1323 0.042 Uiso 1 calc R . . H14B H 1.4563 -0.7107 -0.1521 0.042 Uiso 1 calc R . . H14C H 1.4508 -0.5820 -0.2498 0.042 Uiso 1 calc R . . N2 N 1.5670(3) -0.1345(2) -0.47521(18) 0.0235(4) Uani 1 d . . . C21 C 1.5854(3) 0.0816(2) -0.4983(2) 0.0233(5) Uani 1 d . . . C22 C 1.6554(3) -0.0568(2) -0.4730(2) 0.0231(5) Uani 1 d . . . C23 C 1.6722(4) 0.1753(3) -0.4930(3) 0.0322(6) Uani 1 d . . . H23A H 1.7953 0.1457 -0.5479 0.048 Uiso 1 calc R . . H23B H 1.6638 0.1756 -0.4038 0.048 Uiso 1 calc R . . H23C H 1.6130 0.2645 -0.5237 0.048 Uiso 1 calc R . . C24 C 1.8256(3) -0.1225(3) -0.4439(3) 0.0304(6) Uani 1 d . . . H24A H 1.8093 -0.0965 -0.3608 0.046 Uiso 1 calc R . . H24B H 1.9182 -0.0946 -0.5120 0.046 Uiso 1 calc R . . H24C H 1.8585 -0.2184 -0.4402 0.046 Uiso 1 calc R . . O11 O 1.3234(3) -0.5933(2) 0.4009(2) 0.0424(5) Uani 1 d . . . H11 H 1.3706 -0.6709 0.4261 0.064 Uiso 1 calc R . . C1 C 1.2564(4) -0.5070(3) 0.5052(3) 0.0324(6) Uani 1 d . . . H1A H 1.1897 -0.4171 0.4785 0.039 Uiso 1 calc R . . H1B H 1.3556 -0.5018 0.5219 0.039 Uiso 1 calc R . . C2 C 1.1388(4) -0.5572(3) 0.6286(3) 0.0376(6) Uani 1 d . . . H2A H 1.0388 -0.5601 0.6130 0.056 Uiso 1 calc R . . H2B H 1.0972 -0.4979 0.6967 0.056 Uiso 1 calc R . . H2C H 1.2049 -0.6459 0.6556 0.056 Uiso 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 Mo01 0.02665(12) 0.01877(12) 0.02290(12) -0.00752(8) -0.00598(9) -0.00746(8) Mo02 0.02639(12) 0.02196(12) 0.01889(12) 0.00141(8) -0.00957(9) -0.00441(9) Mo03 0.01952(11) 0.02427(12) 0.02255(12) -0.00372(8) -0.00338(8) -0.00951(8) O1 0.0390(11) 0.0291(10) 0.0360(11) -0.0135(8) -0.0075(9) -0.0114(8) O2 0.0378(11) 0.0340(10) 0.0267(10) 0.0053(8) -0.0154(8) -0.0053(8) O3 0.0244(9) 0.0391(11) 0.0321(10) -0.0061(8) -0.0022(8) -0.0152(8) O4 0.0240(9) 0.0240(9) 0.0233(9) -0.0066(7) -0.0024(7) -0.0064(7) O5 0.0320(9) 0.0157(8) 0.0290(9) 0.0000(7) -0.0101(8) -0.0042(7) O6 0.0320(9) 0.0297(9) 0.0206(9) -0.0060(7) -0.0107(7) -0.0074(7) O7 0.0280(9) 0.0273(9) 0.0317(10) -0.0084(7) -0.0060(8) -0.0143(7) O8 0.0204(11) 0.0158(11) 0.0162(11) -0.0019(8) -0.0060(9) -0.0056(9) O9 0.0280(9) 0.0251(9) 0.0217(9) 0.0023(7) -0.0048(7) -0.0101(7) O10 0.0230(9) 0.0297(9) 0.0274(9) -0.0013(7) -0.0114(7) -0.0063(7) N1 0.0254(10) 0.0198(10) 0.0201(10) -0.0026(8) -0.0080(8) -0.0060(8) C11 0.0205(11) 0.0185(11) 0.0254(12) -0.0038(9) -0.0073(9) -0.0054(9) C12 0.0214(11) 0.0157(11) 0.0266(12) -0.0053(9) -0.0098(10) -0.0025(9) C13 0.0363(15) 0.0362(15) 0.0293(14) -0.0065(11) -0.0035(11) -0.0225(12) C14 0.0338(14) 0.0275(13) 0.0290(13) -0.0035(10) -0.0151(11) -0.0122(11) N2 0.0259(10) 0.0258(10) 0.0167(10) -0.0037(8) -0.0029(8) -0.0098(8) C21 0.0265(12) 0.0267(12) 0.0181(11) -0.0031(9) -0.0042(10) -0.0131(10) C22 0.0235(12) 0.0283(13) 0.0154(11) -0.0047(9) -0.0039(9) -0.0077(10) C23 0.0366(15) 0.0295(14) 0.0369(15) -0.0042(11) -0.0116(12) -0.0176(12) C24 0.0273(13) 0.0322(14) 0.0289(14) -0.0021(11) -0.0087(11) -0.0081(11) O11 0.0540(13) 0.0354(11) 0.0337(11) -0.0107(9) -0.0158(10) -0.0060(10) C1 0.0440(16) 0.0213(12) 0.0348(15) -0.0012(11) -0.0189(12) -0.0088(11) C2 0.0397(16) 0.0429(16) 0.0332(15) -0.0096(12) -0.0104(12) -0.0156(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 Mo01 O1 1.6828(18) . ? Mo01 O4 1.8773(17) . ? Mo01 O5 1.9217(18) . ? Mo01 O6 1.9353(18) . ? Mo01 O7 1.9725(17) . ? Mo01 O8 2.32238(19) . ? Mo02 O2 1.6826(18) . ? Mo02 O9 1.9237(17) . ? Mo02 O10 1.9253(17) . ? Mo02 O6 1.9266(17) . ? Mo02 O5 1.9323(18) 2_755 ? Mo02 O8 2.3143(2) . ? Mo03 O3 1.6837(17) . ? Mo03 O7 1.8730(17) . ? Mo03 O10 1.9242(17) . ? Mo03 O9 1.9314(17) 2_755 ? Mo03 O4 1.9868(17) 2_755 ? Mo03 O8 2.3224(2) . ? O4 Mo03 1.9868(17) 2_755 ? O5 Mo02 1.9323(18) 2_755 ? O8 Mo02 2.3143(2) 2_755 ? O8 Mo01 2.32238(19) 2_755 ? O8 Mo03 2.3224(2) 2_755 ? O9 Mo03 1.9314(17) 2_755 ? N1 C11 1.335(3) . ? N1 C12 1.344(3) . ? C11 C12 1.393(3) 2_845 ? C11 C13 1.495(3) . ? C12 C11 1.393(3) 2_845 ? C12 C14 1.494(3) . ? N2 C21 1.342(3) 2_854 ? N2 C22 1.348(3) . ? C21 N2 1.342(3) 2_854 ? C21 C22 1.392(3) . ? C21 C23 1.499(3) . ? C22 C24 1.497(3) . ? O11 C1 1.434(3) . ? C1 C2 1.491(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 O1 Mo01 O4 104.14(9) . . ? O1 Mo01 O5 103.67(9) . . ? O4 Mo01 O5 89.09(8) . . ? O1 Mo01 O6 102.84(9) . . ? O4 Mo01 O6 88.60(8) . . ? O5 Mo01 O6 153.14(7) . . ? O1 Mo01 O7 102.60(8) . . ? O4 Mo01 O7 153.26(7) . . ? O5 Mo01 O7 85.29(8) . . ? O6 Mo01 O7 84.83(8) . . ? O1 Mo01 O8 178.02(7) . . ? O4 Mo01 O8 77.75(5) . . ? O5 Mo01 O8 76.84(5) . . ? O6 Mo01 O8 76.52(5) . . ? O7 Mo01 O8 75.51(5) . . ? O2 Mo02 O9 103.35(9) . . ? O2 Mo02 O10 103.15(9) . . ? O9 Mo02 O10 153.49(7) . . ? O2 Mo02 O6 103.45(9) . . ? O9 Mo02 O6 86.87(8) . . ? O10 Mo02 O6 87.48(8) . . ? O2 Mo02 O5 102.82(9) . 2_755 ? O9 Mo02 O5 87.30(8) . 2_755 ? O10 Mo02 O5 86.40(8) . 2_755 ? O6 Mo02 O5 153.73(7) . 2_755 ? O2 Mo02 O8 179.64(7) . . ? O9 Mo02 O8 76.78(5) . . ? O10 Mo02 O8 76.71(5) . . ? O6 Mo02 O8 76.88(5) . . ? O5 Mo02 O8 76.85(5) 2_755 . ? O3 Mo03 O7 104.59(8) . . ? O3 Mo03 O10 104.14(9) . . ? O7 Mo03 O10 89.34(8) . . ? O3 Mo03 O9 102.73(9) . 2_755 ? O7 Mo03 O9 88.90(8) . 2_755 ? O10 Mo03 O9 152.63(7) . 2_755 ? O3 Mo03 O4 102.35(8) . 2_755 ? O7 Mo03 O4 153.06(7) . 2_755 ? O10 Mo03 O4 84.69(8) . 2_755 ? O9 Mo03 O4 84.60(8) 2_755 2_755 ? O3 Mo03 O8 177.95(6) . . ? O7 Mo03 O8 77.32(5) . . ? O10 Mo03 O8 76.53(5) . . ? O9 Mo03 O8 76.44(5) 2_755 . ? O4 Mo03 O8 75.74(5) 2_755 . ? Mo01 O4 Mo03 116.46(8) . 2_755 ? Mo01 O5 Mo02 116.37(8) . 2_755 ? Mo02 O6 Mo01 116.40(8) . . ? Mo03 O7 Mo01 117.22(8) . . ? Mo02 O8 Mo02 180.0 . 2_755 ? Mo02 O8 Mo01 89.874(7) . 2_755 ? Mo02 O8 Mo01 90.126(7) 2_755 2_755 ? Mo02 O8 Mo01 90.126(7) . . ? Mo02 O8 Mo01 89.874(7) 2_755 . ? Mo01 O8 Mo01 180.0 2_755 . ? Mo02 O8 Mo03 90.063(7) . 2_755 ? Mo02 O8 Mo03 89.937(7) 2_755 2_755 ? Mo01 O8 Mo03 89.956(7) 2_755 2_755 ? Mo01 O8 Mo03 90.044(7) . 2_755 ? Mo02 O8 Mo03 89.937(7) . . ? Mo02 O8 Mo03 90.063(7) 2_755 . ? Mo01 O8 Mo03 90.044(7) 2_755 . ? Mo01 O8 Mo03 89.956(7) . . ? Mo03 O8 Mo03 180.0 2_755 . ? Mo02 O9 Mo03 116.63(8) . 2_755 ? Mo03 O10 Mo02 116.69(8) . . ? C11 N1 C12 122.1(2) . . ? N1 C11 C12 119.3(2) . 2_845 ? N1 C11 C13 118.6(2) . . ? C12 C11 C13 122.1(2) 2_845 . ? N1 C12 C11 118.6(2) . 2_845 ? N1 C12 C14 118.8(2) . . ? C11 C12 C14 122.6(2) 2_845 . ? C21 N2 C22 121.6(2) 2_854 . ? N2 C21 C22 119.6(2) 2_854 . ? N2 C21 C23 118.4(2) 2_854 . ? C22 C21 C23 122.0(2) . . ? N2 C22 C21 118.8(2) . . ? N2 C22 C24 118.9(2) . . ? C21 C22 C24 122.3(2) . . ? O11 C1 C2 111.4(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.641 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.089