#------------------------------------------------------------------------------ #$Date: 2016-02-20 16:35:30 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176787 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/45/2214502.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2214502 loop_ _publ_author_name 'Guo-Ming Wang' 'Jin-Hua Li' 'Jing Han' 'Hui-Luan Liu' _publ_section_title ; A new vanadate containing helical chains ; _journal_coeditor_code BG2076 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m2189 _journal_page_last m2189 _journal_paper_doi 10.1107/S160053680703471X _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '(C6 H16 N4 O2) [V2 O6]' _chemical_formula_moiety 'C6 H16 N4 O2 2+, O6 V2 2-' _chemical_formula_sum 'C6 H16 N4 O8 V2' _chemical_formula_weight 374.11 _chemical_name_systematic ; catena-poly[N,N'-bis(2-ammonioethyl)oxamide [dioxidovanadate-\m-oxido-dioxidovanadate-\m-oxido]], ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 100.114(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.7453(3) _cell_length_b 5.50870(10) _cell_length_c 18.1775(2) _cell_measurement_reflns_used 4832 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 25.99 _cell_measurement_theta_min 3.08 _cell_volume 664.94(3) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Siemems SMART CCD' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 4832 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_min 3.08 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_T_max 0.8929 _exptl_absorpt_correction_T_min 0.7604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 380 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.339 _refine_diff_density_min -0.362 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1300 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.110 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0293 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.6776P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0780 _reflns_number_gt 1217 _reflns_number_total 1300 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bg2076.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2214502 _cod_database_fobs_code 2214502 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' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy V V 0.65928(5) 0.70817(7) 0.20100(2) 0.01778(15) Uani d . 1 O O1 0.7174(3) 0.6053(4) 0.12407(10) 0.0363(5) Uani d . 1 O O2 0.4226(3) 0.7879(4) 0.18675(13) 0.0411(5) Uani d . 1 O O3 0.8179(3) 0.9687(3) 0.23015(10) 0.0291(4) Uani d . 1 O O4 0.2428(2) 0.9303(3) -0.01377(9) 0.0256(4) Uani d . 1 C C1 0.3990(3) 1.0441(4) 0.00875(12) 0.0188(5) Uani d . 1 C C2 0.2333(4) 1.3726(5) 0.06245(14) 0.0263(5) Uani d . 1 H H2A 0.1252 1.3422 0.0207 0.032 Uiso calc R 1 H H2B 0.2613 1.5454 0.0635 0.032 Uiso calc R 1 C C3 0.1615(4) 1.3043(5) 0.13401(15) 0.0295(6) Uani d . 1 H H3A 0.2711 1.3257 0.1758 0.035 Uiso calc R 1 H H3B 0.0530 1.4122 0.1413 0.035 Uiso calc R 1 N N1 0.4117(3) 1.2438(4) 0.04932(11) 0.0217(4) Uani d . 1 H H1A 0.5286 1.2992 0.0685 0.026 Uiso calc R 1 N N2 0.0899(3) 1.0505(4) 0.13286(11) 0.0242(4) Uani d . 1 H H2C 0.0491 1.0172 0.1757 0.036 Uiso calc R 1 H H2D 0.1898 0.9508 0.1271 0.036 Uiso calc R 1 H H2E -0.0123 1.0308 0.0951 0.036 Uiso calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V 0.0180(2) 0.0148(2) 0.0203(2) 0.00000(14) 0.00284(15) 0.00046(14) O1 0.0497(12) 0.0343(11) 0.0263(9) -0.0053(9) 0.0105(8) -0.0082(8) O2 0.0227(10) 0.0353(11) 0.0626(14) 0.0066(8) 0.0002(9) 0.0068(10) O3 0.0342(10) 0.0222(9) 0.0330(9) -0.0085(7) 0.0114(8) -0.0084(7) O4 0.0181(8) 0.0257(9) 0.0326(9) -0.0039(7) 0.0033(7) -0.0019(7) C1 0.0182(11) 0.0218(11) 0.0165(10) -0.0002(9) 0.0033(8) 0.0035(9) C2 0.0281(13) 0.0201(12) 0.0318(13) 0.0038(10) 0.0084(10) 0.0004(10) C3 0.0307(14) 0.0276(14) 0.0329(14) 0.0015(10) 0.0131(11) -0.0058(11) N1 0.0183(10) 0.0224(10) 0.0248(10) -0.0021(8) 0.0052(8) -0.0030(8) N2 0.0178(10) 0.0311(11) 0.0244(10) 0.0023(8) 0.0056(8) 0.0028(8) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 V O2 . . 109.60(11) no O1 V O3 . 2_645 109.79(9) no O2 V O3 . 2_645 105.57(10) no O1 V O3 . . 108.03(9) no O2 V O3 . . 110.13(9) no O3 V O3 2_645 . 113.68(3) no V O3 V 2_655 . 139.01(10) no O4 C1 N1 . . 125.3(2) no O4 C1 C1 . 3_675 120.6(3) no N1 C1 C1 . 3_675 114.1(2) no N1 C2 C3 . . 114.8(2) no N1 C2 H2A . . 108.6 no C3 C2 H2A . . 108.6 no N1 C2 H2B . . 108.6 no C3 C2 H2B . . 108.6 no H2A C2 H2B . . 107.5 no N2 C3 C2 . . 112.1(2) no N2 C3 H3A . . 109.2 no C2 C3 H3A . . 109.2 no N2 C3 H3B . . 109.2 no C2 C3 H3B . . 109.2 no H3A C3 H3B . . 107.9 no C1 N1 C2 . . 121.7(2) no C1 N1 H1A . . 119.2 no C2 N1 H1A . . 119.2 no C3 N2 H2C . . 109.5 no C3 N2 H2D . . 109.5 no H2C N2 H2D . . 109.5 no C3 N2 H2E . . 109.5 no H2C N2 H2E . . 109.5 no H2D N2 H2E . . 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V O1 . 1.6197(18) yes V O2 . 1.6322(19) yes V O3 2_645 1.8063(17) yes V O3 . 1.8127(17) yes O4 C1 . 1.232(3) no C1 N1 . 1.319(3) no C1 C1 3_675 1.532(4) no C2 N1 . 1.452(3) no C2 C3 . 1.513(3) no C2 H2A . 0.9700 no C2 H2B . 0.9700 no C3 N2 . 1.478(3) no C3 H3A . 0.9700 no C3 H3B . 0.9700 no N1 H1A . 0.8600 no N2 H2C . 0.8900 no N2 H2D . 0.8900 no N2 H2E . 0.8900 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O1 1_565 0.86 2.24 3.013(3) 148.9 yes N2 H2C O3 1_455 0.89 2.01 2.799(3) 147.8 yes N2 H2E O4 3_575 0.89 1.96 2.833(3) 166.6 yes N2 H2D O2 . 0.89 1.96 2.705(3) 140.0 yes