Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_isk32 _database_code_CSD 167561 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'M. Ishaque Khan' 'Sabri Cevik' 'Robert J. Doedens' _publ_contact_author_name 'Prof. M. Ishaque Khan' _publ_contact_author_address ; Prof. M. Ishaque Khan Department of Biological, Chemical, and Physical Sciences Illinois Institute of Technology, Chicago, IL 60616, USA ; _publ_contact_author_email 'khan@iit.edu' _publ_section_title ; Inorganic-organic hybrid materials derived from oxovanadium sulfate motifs: synthesis and characterization of [VIV2O2(SO4)2(2,2'-bpy)2] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 N2 O5 S V' _chemical_formula_weight 319.18 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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.4102(6) _cell_length_b 16.4887(16) _cell_length_c 10.2176(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.417(2) _cell_angle_gamma 90.00 _cell_volume 1065.40(18) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 3036 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 23.25 _exptl_crystal_description Needle _exptl_crystal_colour Green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7865 _exptl_absorpt_correction_T_max 0.9664 _exptl_absorpt_process_details 'computed via SADABS' _exptl_special_details ; Crystal orientation and preliminary unit cell constants were obtained from reflections gathered from three sets of 15 frames each, chosen to cover a wide range of reciprocal space. Refined cell parameters were computed after data collection on the basis of the setting angles of 3036 reflections with a resolution limit of 0.90 Angstroms. ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '30s frames at 0.3 deg. omega increments' _diffrn_standards_number 'n/a' _diffrn_standards_interval_count 'n/a' _diffrn_standards_interval_time 'n/a' _diffrn_standards_decay_% none _diffrn_reflns_number 7756 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 23.27 _diffrn_special_details ; A full sphere of data was collected by use of 0.3 degree omega increments and 30s frame counting times. The first 50 frames were remeasured at the end of data collection and no evidence of decay was observed. To a limiting resolution of 0.90 A, the completeness of coverage was 100.00%, the average redundancy was 5.0, and R(sym) for the uncorrected data was 0.056. ; _reflns_number_total 1530 _reflns_number_gt 1284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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. Hydrogen atoms were included at idealized positions and refined by use of the riding model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.04P)^2^+10.0P] 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 n/a _refine_ls_number_reflns 1530 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.220 _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 V1 V 0.20839(18) 0.93655(7) 0.87461(11) 0.0094(4) Uani 1 1 d . . . S1 S 0.2979(3) 1.03224(10) 1.15162(16) 0.0096(4) Uani 1 1 d . . . N1 N 0.1818(9) 0.8698(3) 0.6938(5) 0.0123(13) Uani 1 1 d . . . N2 N 0.2003(8) 0.8042(3) 0.9308(5) 0.0104(13) Uani 1 1 d . . . O1 O 0.1831(8) 1.0228(3) 0.8062(5) 0.0162(11) Uani 1 1 d . . . O2 O 0.2585(7) 0.9567(3) 1.0696(4) 0.0130(11) Uani 1 1 d . . . O3 O 0.3475(8) 1.0100(3) 1.2897(4) 0.0154(11) Uani 1 1 d . . . O4 O 0.4716(7) 1.0789(3) 1.1084(5) 0.0128(11) Uani 1 1 d . . . O5 O 0.1078(7) 1.0847(3) 1.1225(4) 0.0134(11) Uani 1 1 d . . . C1 C 0.1719(11) 0.9075(4) 0.5761(7) 0.0137(16) Uani 1 1 d . . . H1A H 0.1711 0.9651 0.5741 0.016 Uiso 1 1 calc R . . C2 C 0.1627(11) 0.8658(5) 0.4579(7) 0.0162(16) Uani 1 1 d . . . H2A H 0.1513 0.8939 0.3760 0.019 Uiso 1 1 calc R . . C3 C 0.1706(11) 0.7814(5) 0.4620(7) 0.0184(17) Uani 1 1 d . . . H3A H 0.1684 0.7512 0.3826 0.022 Uiso 1 1 calc R . . C4 C 0.1817(11) 0.7420(5) 0.5815(7) 0.0144(16) Uani 1 1 d . . . H4A H 0.1894 0.6845 0.5857 0.017 Uiso 1 1 calc R . . C5 C 0.1813(10) 0.7877(4) 0.6974(7) 0.0110(15) Uani 1 1 d . . . C6 C 0.1775(10) 0.7508(4) 0.8290(7) 0.0100(15) Uani 1 1 d . . . C7 C 0.1467(11) 0.6687(4) 0.8484(7) 0.0149(16) Uani 1 1 d . . . H7A H 0.1219 0.6328 0.7747 0.018 Uiso 1 1 calc R . . C8 C 0.1525(11) 0.6395(4) 0.9750(7) 0.0167(17) Uani 1 1 d . . . H8A H 0.1378 0.5831 0.9902 0.020 Uiso 1 1 calc R . . C9 C 0.1803(11) 0.6940(4) 1.0805(7) 0.0147(16) Uani 1 1 d . . . H9A H 0.1851 0.6755 1.1690 0.018 Uiso 1 1 calc R . . C10 C 0.2007(10) 0.7749(4) 1.0538(7) 0.0118(15) Uani 1 1 d . . . H10A H 0.2159 0.8121 1.1258 0.014 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0084(6) 0.0081(6) 0.0119(6) -0.0027(5) 0.0018(5) -0.0008(5) S1 0.0079(9) 0.0109(9) 0.0099(9) -0.0050(7) 0.0016(7) -0.0014(7) N1 0.008(3) 0.012(3) 0.016(3) 0.001(3) 0.002(2) 0.000(2) N2 0.008(3) 0.007(3) 0.017(3) -0.002(3) 0.003(2) -0.001(2) O1 0.013(3) 0.015(3) 0.020(3) -0.001(2) 0.001(2) -0.001(2) O2 0.015(3) 0.009(2) 0.016(2) -0.004(2) 0.005(2) 0.000(2) O3 0.019(3) 0.014(3) 0.012(2) -0.001(2) 0.001(2) -0.001(2) O4 0.013(3) 0.009(2) 0.018(3) -0.004(2) 0.005(2) -0.002(2) O5 0.013(3) 0.010(3) 0.017(3) 0.0000(19) 0.001(2) 0.002(2) C1 0.008(4) 0.017(4) 0.015(4) 0.002(3) -0.001(3) -0.002(3) C2 0.011(4) 0.023(4) 0.015(4) 0.000(3) 0.005(3) -0.004(3) C3 0.009(4) 0.030(5) 0.018(4) -0.008(3) 0.007(3) -0.006(3) C4 0.008(4) 0.018(4) 0.017(4) -0.001(3) -0.001(3) -0.001(3) C5 0.005(3) 0.011(4) 0.018(4) -0.004(3) 0.001(3) 0.001(3) C6 0.006(4) 0.008(3) 0.015(4) -0.002(3) -0.001(3) 0.004(3) C7 0.010(4) 0.011(4) 0.023(4) -0.007(3) 0.002(3) -0.003(3) C8 0.012(4) 0.010(4) 0.029(4) 0.011(3) 0.006(3) 0.005(3) C9 0.008(4) 0.018(4) 0.018(4) 0.002(3) 0.002(3) 0.000(3) C10 0.009(4) 0.013(4) 0.014(4) 0.000(3) 0.003(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.582(5) . ? V1 O2 1.994(5) . ? V1 O4 2.046(5) 3_677 ? V1 O5 2.062(5) 3_577 ? V1 N1 2.133(6) . ? V1 N2 2.259(6) . ? S1 O3 1.442(5) . ? S1 O4 1.479(5) . ? S1 O5 1.484(5) . ? S1 O2 1.499(5) . ? N1 C1 1.346(9) . ? N1 C5 1.353(9) . ? N2 C10 1.346(9) . ? N2 C6 1.352(9) . ? O4 V1 2.046(5) 3_677 ? O5 V1 2.062(5) 3_577 ? C1 C2 1.382(10) . ? C2 C3 1.393(11) . ? C3 C4 1.375(10) . ? C4 C5 1.404(10) . ? C5 C6 1.481(10) . ? C6 C7 1.387(10) . ? C7 C8 1.375(10) . ? C8 C9 1.391(10) . ? C9 C10 1.372(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 V1 O2 106.2(2) . . ? O1 V1 O4 100.3(2) . 3_677 ? O2 V1 O4 86.59(19) . 3_677 ? O1 V1 O5 97.4(2) . 3_577 ? O2 V1 O5 90.68(19) . 3_577 ? O4 V1 O5 162.15(19) 3_677 3_577 ? O1 V1 N1 95.4(2) . . ? O2 V1 N1 158.2(2) . . ? O4 V1 N1 86.9(2) 3_677 . ? O5 V1 N1 89.2(2) 3_577 . ? O1 V1 N2 167.5(2) . . ? O2 V1 N2 85.03(19) . . ? O4 V1 N2 85.55(19) 3_677 . ? O5 V1 N2 76.64(19) 3_577 . ? N1 V1 N2 73.7(2) . . ? O3 S1 O4 111.6(3) . . ? O3 S1 O5 112.7(3) . . ? O4 S1 O5 105.7(3) . . ? O3 S1 O2 109.0(3) . . ? O4 S1 O2 109.4(3) . . ? O5 S1 O2 108.3(3) . . ? C1 N1 C5 119.0(6) . . ? C1 N1 V1 121.4(5) . . ? C5 N1 V1 119.6(4) . . ? C10 N2 C6 117.9(6) . . ? C10 N2 V1 126.0(4) . . ? C6 N2 V1 115.9(4) . . ? S1 O2 V1 133.0(3) . . ? S1 O4 V1 134.7(3) . 3_677 ? S1 O5 V1 132.5(3) . 3_577 ? N1 C1 C2 122.7(7) . . ? C1 C2 C3 118.3(7) . . ? C4 C3 C2 119.7(7) . . ? C3 C4 C5 119.2(7) . . ? N1 C5 C4 121.0(6) . . ? N1 C5 C6 115.8(6) . . ? C4 C5 C6 123.2(6) . . ? N2 C6 C7 121.7(6) . . ? N2 C6 C5 114.5(6) . . ? C7 C6 C5 123.7(6) . . ? C8 C7 C6 119.5(7) . . ? C7 C8 C9 118.9(7) . . ? C10 C9 C8 118.6(7) . . ? N2 C10 C9 123.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.826 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.134