# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 906120' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H8 N2 O7 V2 Zn2 ' _chemical_formula_sum 'C2 H8 N2 O7 V2 Zn2 ' _chemical_formula_weight 404.76 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.0932(14) _cell_length_b 8.6150(17) _cell_length_c 8.1921(16) _cell_angle_alpha 90.00 _cell_angle_beta 112.18(3) _cell_angle_gamma 90.00 _cell_volume 463.56(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 7.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4164 _exptl_absorpt_correction_T_max 0.5097 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2618 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.09 _reflns_number_total 1589 _reflns_number_gt 1564 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0097P)^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 0.030(13) _refine_ls_number_reflns 1589 _refine_ls_number_parameters 136 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0401 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Zn1 Zn 0.45994(6) 0.56832(4) 0.76578(5) 0.01398(10) Uani 1 1 d . . . Zn2 Zn 0.77153(6) 1.28796(4) 0.76134(5) 0.01362(10) Uani 1 1 d . . . V1 V 0.61865(8) 0.88486(6) 0.60143(8) 0.01055(13) Uani 1 1 d . . . V2 V 0.97478(8) 1.15513(6) 1.19332(7) 0.01062(13) Uani 1 1 d . . . N1 N 0.5904(4) 0.5432(3) 1.0294(4) 0.0155(6) Uani 1 1 d . . . H1A H 0.4922 0.5316 1.0730 0.019 Uiso 1 1 calc R . . H1B H 0.6666 0.4563 1.0544 0.019 Uiso 1 1 calc R . . N2 N 1.0338(4) 0.7577(3) 1.3638(4) 0.0147(6) Uani 1 1 d . . . H2C H 1.1077 0.7371 1.4779 0.018 Uiso 1 1 calc R . . H2D H 0.9687 0.8481 1.3599 0.018 Uiso 1 1 calc R . . C1 C 0.7220(5) 0.6788(4) 1.1183(5) 0.0175(8) Uani 1 1 d . . . H1C H 0.6372 0.7615 1.1335 0.021 Uiso 1 1 calc R . . H1D H 0.7906 0.7176 1.0442 0.021 Uiso 1 1 calc R . . C2 C 0.8780(5) 0.6338(4) 1.2953(5) 0.0190(8) Uani 1 1 d . . . H2A H 0.8114 0.6167 1.3776 0.023 Uiso 1 1 calc R . . H2B H 0.9435 0.5377 1.2844 0.023 Uiso 1 1 calc R . . O1 O 0.5052(4) 0.3937(3) 0.6303(3) 0.0143(5) Uani 1 1 d . . . O2 O 0.1615(3) 0.5656(3) 0.7020(3) 0.0151(5) Uani 1 1 d . . . O3 O 0.4820(4) 0.7809(3) 0.6891(4) 0.0192(5) Uani 1 1 d . . . O4 O 0.8625(4) 0.7995(3) 0.6580(3) 0.0192(5) Uani 1 1 d . . . O5 O 0.6438(4) 1.0616(3) 0.6833(3) 0.0200(5) Uani 1 1 d . . . O6 O 0.8169(4) 1.2424(3) 1.0075(3) 0.0178(5) Uani 1 1 d . . . O7 O 0.8777(4) 1.5248(3) 0.8470(4) 0.0232(6) 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 Zn1 0.0181(2) 0.01093(18) 0.0129(2) -0.00080(16) 0.00585(16) -0.00034(16) Zn2 0.0145(2) 0.01436(19) 0.0124(2) 0.00199(16) 0.00560(16) 0.00329(17) V1 0.0123(3) 0.0081(2) 0.0108(3) 0.0004(2) 0.0038(2) -0.0003(2) V2 0.0125(3) 0.0092(3) 0.0106(3) 0.0010(2) 0.0048(2) 0.0002(2) N1 0.0209(15) 0.0161(15) 0.0110(16) -0.0020(12) 0.0077(12) -0.0036(13) N2 0.0165(15) 0.0137(15) 0.0137(16) 0.0003(12) 0.0056(12) 0.0023(12) C1 0.0223(19) 0.0120(16) 0.017(2) -0.0033(15) 0.0057(16) -0.0036(15) C2 0.0177(19) 0.0179(17) 0.019(2) 0.0039(16) 0.0042(15) -0.0037(15) O1 0.0138(12) 0.0157(11) 0.0109(13) -0.0026(10) 0.0017(9) 0.0041(10) O2 0.0134(11) 0.0153(11) 0.0183(13) -0.0017(11) 0.0080(9) 0.0010(11) O3 0.0226(13) 0.0143(12) 0.0236(15) 0.0024(11) 0.0120(11) -0.0017(11) O4 0.0161(12) 0.0208(12) 0.0199(14) 0.0033(11) 0.0059(10) 0.0041(11) O5 0.0248(14) 0.0115(11) 0.0237(14) -0.0033(11) 0.0091(11) -0.0004(12) O6 0.0224(13) 0.0177(12) 0.0102(13) 0.0033(10) 0.0025(11) 0.0011(10) O7 0.0326(16) 0.0160(14) 0.0287(17) -0.0047(11) 0.0205(13) -0.0068(11) _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 Zn1 O3 1.961(3) . ? Zn1 O1 1.966(2) . ? Zn1 O2 1.980(2) . ? Zn1 N1 2.015(3) . ? Zn2 O6 1.958(2) . ? Zn2 O1 2.005(2) 1_565 ? Zn2 N2 2.024(3) 2_757 ? Zn2 O5 2.144(3) . ? Zn2 O7 2.196(2) . ? V1 O5 1.646(3) . ? V1 O3 1.668(2) . ? V1 O1 1.767(3) 2_656 ? V1 O4 1.773(2) . ? V2 O7 1.651(2) 2_747 ? V2 O6 1.688(2) . ? V2 O2 1.700(2) 2_657 ? V2 O4 1.817(3) 2_757 ? N1 C1 1.501(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.485(4) . ? N2 Zn2 2.024(3) 2_747 ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? C1 C2 1.505(5) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O1 V1 1.767(3) 2_646 ? O1 Zn2 2.005(2) 1_545 ? O2 V2 1.700(2) 2_647 ? O4 V2 1.817(3) 2_747 ? O7 V2 1.651(2) 2_757 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 118.94(11) . . ? O3 Zn1 O2 97.64(10) . . ? O1 Zn1 O2 103.19(10) . . ? O3 Zn1 N1 112.58(12) . . ? O1 Zn1 N1 114.57(12) . . ? O2 Zn1 N1 107.12(12) . . ? O6 Zn2 O1 113.43(10) . 1_565 ? O6 Zn2 N2 128.15(11) . 2_757 ? O1 Zn2 N2 118.21(11) 1_565 2_757 ? O6 Zn2 O5 90.65(10) . . ? O1 Zn2 O5 92.69(10) 1_565 . ? N2 Zn2 O5 91.37(10) 2_757 . ? O6 Zn2 O7 87.38(10) . . ? O1 Zn2 O7 83.63(10) 1_565 . ? N2 Zn2 O7 93.69(11) 2_757 . ? O5 Zn2 O7 174.74(9) . . ? O5 V1 O3 108.23(13) . . ? O5 V1 O1 109.35(12) . 2_656 ? O3 V1 O1 110.57(13) . 2_656 ? O5 V1 O4 109.39(13) . . ? O3 V1 O4 109.46(13) . . ? O1 V1 O4 109.81(12) 2_656 . ? O7 V2 O6 112.18(13) 2_747 . ? O7 V2 O2 108.44(12) 2_747 2_657 ? O6 V2 O2 110.29(12) . 2_657 ? O7 V2 O4 108.03(13) 2_747 2_757 ? O6 V2 O4 109.70(12) . 2_757 ? O2 V2 O4 108.08(12) 2_657 2_757 ? C1 N1 Zn1 112.7(2) . . ? C1 N1 H1A 109.0 . . ? Zn1 N1 H1A 109.0 . . ? C1 N1 H1B 109.0 . . ? Zn1 N1 H1B 109.0 . . ? H1A N1 H1B 107.8 . . ? C2 N2 Zn2 117.0(2) . 2_747 ? C2 N2 H2C 108.1 . . ? Zn2 N2 H2C 108.1 2_747 . ? C2 N2 H2D 108.1 . . ? Zn2 N2 H2D 108.1 2_747 . ? H2C N2 H2D 107.3 . . ? N1 C1 C2 111.3(3) . . ? N1 C1 H1C 109.4 . . ? C2 C1 H1C 109.4 . . ? N1 C1 H1D 109.4 . . ? C2 C1 H1D 109.4 . . ? H1C C1 H1D 108.0 . . ? N2 C2 C1 110.5(3) . . ? N2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? V1 O1 Zn1 121.21(13) 2_646 . ? V1 O1 Zn2 122.78(13) 2_646 1_545 ? Zn1 O1 Zn2 111.54(12) . 1_545 ? V2 O2 Zn1 128.04(14) 2_647 . ? V1 O3 Zn1 140.24(15) . . ? V1 O4 V2 140.28(15) . 2_747 ? V1 O5 Zn2 158.71(14) . . ? V2 O6 Zn2 144.39(15) . . ? V2 O7 Zn2 137.29(15) 2_757 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 N1 C1 -13.1(3) . . . . ? O1 Zn1 N1 C1 127.0(2) . . . . ? O2 Zn1 N1 C1 -119.2(2) . . . . ? Zn1 N1 C1 C2 -157.3(2) . . . . ? Zn2 N2 C2 C1 -70.0(3) 2_747 . . . ? N1 C1 C2 N2 167.8(3) . . . . ? O3 Zn1 O1 V1 -49.37(18) . . . 2_646 ? O2 Zn1 O1 V1 57.22(17) . . . 2_646 ? N1 Zn1 O1 V1 173.30(14) . . . 2_646 ? O3 Zn1 O1 Zn2 107.52(13) . . . 1_545 ? O2 Zn1 O1 Zn2 -145.88(12) . . . 1_545 ? N1 Zn1 O1 Zn2 -29.81(16) . . . 1_545 ? O3 Zn1 O2 V2 -74.04(19) . . . 2_647 ? O1 Zn1 O2 V2 163.76(17) . . . 2_647 ? N1 Zn1 O2 V2 42.5(2) . . . 2_647 ? O5 V1 O3 Zn1 -145.8(2) . . . . ? O1 V1 O3 Zn1 94.5(3) 2_656 . . . ? O4 V1 O3 Zn1 -26.6(3) . . . . ? O1 Zn1 O3 V1 -36.6(3) . . . . ? O2 Zn1 O3 V1 -146.3(3) . . . . ? N1 Zn1 O3 V1 101.5(3) . . . . ? O5 V1 O4 V2 105.5(3) . . . 2_747 ? O3 V1 O4 V2 -12.9(3) . . . 2_747 ? O1 V1 O4 V2 -134.5(2) 2_656 . . 2_747 ? O3 V1 O5 Zn2 157.0(4) . . . . ? O1 V1 O5 Zn2 -82.5(4) 2_656 . . . ? O4 V1 O5 Zn2 37.8(5) . . . . ? O6 Zn2 O5 V1 -118.6(4) . . . . ? O1 Zn2 O5 V1 127.9(4) 1_565 . . . ? N2 Zn2 O5 V1 9.6(4) 2_757 . . . ? O7 Zn2 O5 V1 173.5(9) . . . . ? O7 V2 O6 Zn2 -20.1(3) 2_747 . . . ? O2 V2 O6 Zn2 -141.1(2) 2_657 . . . ? O4 V2 O6 Zn2 100.0(3) 2_757 . . . ? O1 Zn2 O6 V2 175.0(2) 1_565 . . . ? N2 Zn2 O6 V2 -10.5(3) 2_757 . . . ? O5 Zn2 O6 V2 81.8(3) . . . . ? O7 Zn2 O6 V2 -103.1(3) . . . . ? O6 Zn2 O7 V2 138.3(2) . . . 2_757 ? O1 Zn2 O7 V2 -107.8(2) 1_565 . . 2_757 ? N2 Zn2 O7 V2 10.2(2) 2_757 . . 2_757 ? O5 Zn2 O7 V2 -153.7(10) . . . 2_757 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O5 0.90 2.54 3.358(4) 151.9 2_647 N1 H1B O6 0.90 2.23 3.090(4) 158.6 1_545 N2 H2C O2 0.90 2.27 3.056(4) 145.1 1_656 N2 H2C O3 0.90 2.59 3.294(4) 135.5 1_656 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.425 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.104