#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012418.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_2012418 loop_ _publ_author_name 'Geupel, Sandra' 'Pilz, Katrin' 'van Smaalen, Sander' 'B\"ullesfeld, Frank' 'Prokofiev, Andrei' 'Assmus, Wolf' _publ_section_title ; Synchrotron-radiation study of the two-leg spin-ladder (VO)~2~P~2~O~7~ at 120K ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i9 _journal_page_last i13 _journal_paper_doi 10.1107/S0108270101017553 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '(V O)2 P2 O7' _chemical_formula_moiety '(V O 2+)2, (P2 O7 4-)' _chemical_formula_structural '(V O)2 P2 O7' _chemical_formula_sum 'O9 P2 V2' _chemical_formula_weight 307.82 _chemical_name_common 'Vanadyl pyrophosphate' _chemical_name_systematic 'Oxovanadium(IV) diphosphate' _space_group_IT_number 29 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 7.7004(4) _cell_length_b 9.5777(5) _cell_length_c 16.5825(8) _cell_measurement_reflns_used 25 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 16.1 _cell_volume 1222.99(11) _computing_cell_refinement 'MACH3 in CAD-4 UNIX Software (Enraf-Nonius, 1998)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 1999) and ORTEP-3 (Farrugia, 1997) ; _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 120(2) _diffrn_detector_area_resol_mean ; number of pixels: 1024 x 1024 (512 x 512 in binning mode), pixel size: 60 \mm x 60 \mm ; _diffrn_measured_fraction_theta_full .957 _diffrn_measured_fraction_theta_max .957 _diffrn_measurement_device_type ; Huber four-circle Kappa diffractometer with Siemens SMART CCD area detector and Oxford Cryostream Cooler ; _diffrn_measurement_method '\w and \f' _diffrn_radiation_monochromator 'Si (111)' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength .70843 _diffrn_reflns_av_R_equivalents .0600 _diffrn_reflns_av_sigmaI/netI .0551 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 11910 _diffrn_reflns_reduction_process ; Overloaded reflections were omitted in the data reduction process. ; _diffrn_reflns_theta_full 30.40 _diffrn_reflns_theta_max 30.40 _diffrn_reflns_theta_min 2.12 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_T_max .950 _exptl_absorpt_correction_T_min .804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 3.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rectangular prism' _exptl_crystal_F_000 1184 _exptl_crystal_size_max .100 _exptl_crystal_size_mid .040 _exptl_crystal_size_min .030 _refine_diff_density_max .813 _refine_diff_density_min -.669 _refine_ls_abs_structure_details 'Flack (1983), 1303 Friedel pairs' _refine_ls_abs_structure_Flack .00(13) _refine_ls_extinction_coef .0165(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref .877 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 237 _refine_ls_number_reflns 3149 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all .877 _refine_ls_R_factor_all .0352 _refine_ls_R_factor_gt .0306 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0302P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .0675 _refine_ls_wR_factor_ref .0684 _reflns_number_gt 2452 _reflns_number_total 3149 _reflns_threshold_expression I>2\s(I) _cod_data_source_file br1349.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012418 _cod_database_fobs_code 2012418 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x, -y, z+1/2' 3 '-x+1/2, y, z+1/2' 4 'x+1/2, -y, z' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol V1 .20343(11) .00936(7) .67906(5) .0037(2) Uani d . 1 . . V V2 .20820(11) .99768(7) .36924(5) .0029(2) Uani d . 1 . . V V3 .20639(11) .50028(6) .42979(5) .0035(2) Uani d . 1 . . V V4 .20815(11) .50132(6) .11893(5) .0031(2) Uani d . 1 . . V P1 .30947(17) .79399(12) .01948(9) .0035(3) Uani d . 1 . . P P2 .29951(16) .20942(12) .51845(9) .0029(3) Uani d . 1 . . P P3 .29602(17) .70759(11) .27490(8) .0031(3) Uani d . 1 . . P P4 .30314(17) .29872(12) .77388(8) .0028(3) Uani d . 1 . . P O1 .0006(4) .0417(3) .6832(2) .0060(6) Uani d . 1 . . O O2 .0042(7) .9676(3) .3636(2) .0069(6) Uani d . 1 . . O O3 .4989(8) .5125(3) .4331(2) .0061(7) Uani d . 1 . . O O4 .4999(5) .5137(3) .1150(2) .0070(6) Uani d . 1 . . O O5 .5041(4) .3281(2) .7746(2) .0097(5) Uani d . 1 . . O O6 .4952(4) .2136(3) .49010(16) .0057(5) Uani d . 1 . . O O7 .2821(6) .8695(3) .2747(2) .0043(9) Uani d . 1 . . O O8 .2782(7) .1377(3) .7743(2) .0057(9) Uani d . 1 . . O O9 .2463(8) .3657(3) .5257(2) .0048(7) Uani d . 1 . . O O10 .2517(8) .6384(3) .0244(2) .0044(7) Uani d . 1 . . O O11 .3019(4) .8583(3) .1010(2) .0069(8) Uani d . 1 . . O O12 .2926(4) .1392(3) .5986(2) .0052(8) Uani d . 1 . . O O13 .2858(5) .8699(3) .4540(2) .0052(8) Uani d . 1 . . O O14 .1984(4) .1434(3) .4514(2) .0061(8) Uani d . 1 . . O O15 .2310(5) .3601(3) .6981(2) .0071(7) Uani d . 1 . . O O16 .2191(4) .6471(3) .2000(2) .0059(7) Uani d . 1 . . O O17 .2308(6) .3612(4) .8496(2) .0062(7) Uani d . 1 . . O O18 .2228(5) .6521(3) .3514(2) .0070(8) Uani d . 1 . . O 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 V1 .0050(6) .0038(4) .0022(4) -.0001(3) .0000(4) .0003(3) V2 .0032(6) .0032(4) .0023(4) .0001(3) .0002(3) -.0001(3) V3 .0037(6) .0043(4) .0025(5) .0001(3) -.0001(4) .0000(3) V4 .0039(6) .0033(4) .0020(4) -.0003(3) -.0002(3) .0002(3) P1 .0038(8) .0034(5) .0033(7) .0000(4) -.0007(6) .0002(4) P2 .0044(9) .0029(5) .0014(6) -.0007(4) .0000(6) -.0002(4) P3 .0025(8) .0038(5) .0030(7) .0001(4) -.0002(6) -.0004(4) P4 .0030(7) .0030(5) .0025(7) -.0001(4) -.0004(6) .0001(4) O1 .0105(15) .0059(13) .0015(14) -.0013(14) .0005(14) -.0007(13) O2 .0063(15) .0077(13) .0066(16) -.0003(17) -.0017(18) -.0013(13) O3 .0081(16) .0068(15) .0035(16) .0005(12) -.0021(17) -.0027(11) O4 .0076(16) .0077(14) .0057(15) .0005(12) .0003(13) -.0015(12) O5 .0064(12) .0043(11) .0183(14) -.0002(10) -.0002(13) -.0016(14) O6 .0072(14) .0077(13) .0022(13) -.0009(10) -.0002(11) .0004(10) O7 .006(2) .0042(13) .0023(14) .0005(11) -.0026(15) -.0005(12) O8 .008(2) .0038(13) .0056(15) -.0003(12) -.0029(16) -.0007(13) O9 .0065(19) .0042(14) .0036(17) .0022(12) -.0008(13) -.0012(14) O10 .0066(17) .0028(14) .0039(17) -.0013(12) -.0012(13) .0001(14) O11 .009(2) .0048(13) .0065(15) .0010(11) -.0026(13) -.0026(10) O12 .005(2) .0072(14) .0035(14) -.0024(11) -.0012(13) .0016(10) O13 .005(2) .0046(13) .0062(17) -.0011(11) -.0011(14) .0000(11) O14 .007(2) .0046(13) .0070(17) -.0021(11) -.0001(13) -.0015(11) O15 .0109(19) .0058(13) .0044(16) .0011(12) -.0011(14) .0012(11) O16 .004(2) .0056(13) .0076(16) -.0012(11) -.0021(14) -.0015(11) O17 .0098(19) .0058(16) .0031(17) -.0017(12) .0027(14) -.0010(13) O18 .011(2) .0051(15) .0043(18) -.0004(12) .0017(14) .0000(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V .3025 .5303 'Brennan & Cowan (1992)' P P .1021 .0946 'Brennan & Cowan (1992)' O O .0108 .0061 'Brennan & Cowan (1992)' 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 V1 O11 . 3_545 98.77(15) no O1 V1 O12 . . 104.49(15) no O11 V1 O12 3_545 . 91.53(14) no O1 V1 O7 . 3_545 98.36(18) no O11 V1 O7 3_545 3_545 91.67(13) no O12 V1 O7 . 3_545 156.15(15) no O1 V1 O8 . . 97.11(19) no O11 V1 O8 3_545 . 162.03(15) no O12 V1 O8 . . 92.59(13) no O7 V1 O8 3_545 . 77.71(13) no O1 V1 O1 . 4 175.8(2) no O11 V1 O1 3_545 4 83.36(12) no O12 V1 O1 . 4 78.98(12) no O7 V1 O1 3_545 4 77.93(16) no O8 V1 O1 . 4 80.28(17) no O2 V2 O14 . 1_565 97.56(15) no O2 V2 O13 . . 103.25(16) no O14 V2 O13 1_565 . 87.59(14) no O2 V2 O8 . 3_564 97.0(2) no O14 V2 O8 1_565 3_564 93.98(14) no O13 V2 O8 . 3_564 159.30(17) no O2 V2 O7 . . 96.83(18) no O14 V2 O7 1_565 . 164.35(15) no O13 V2 O7 . . 95.09(14) no O8 V2 O7 3_564 . 78.15(12) no O2 V2 O2 . 4_575 174.0(2) no O14 V2 O2 1_565 4_575 87.89(13) no O13 V2 O2 . 4_575 79.47(13) no O8 V2 O2 3_564 4_575 79.96(17) no O7 V2 O2 . 4_575 77.48(16) no O3 V3 O17 4_465 3_554 102.66(18) no O3 V3 O18 4_465 . 98.27(17) no O17 V3 O18 3_554 . 92.23(15) no O3 V3 O9 4_465 . 94.2(2) no O17 V3 O9 3_554 . 93.55(13) no O18 V3 O9 . . 164.72(17) no O3 V3 O10 4_465 3 100.2(2) no O17 V3 O10 3_554 3 156.16(19) no O18 V3 O10 . 3 91.03(13) no O9 V3 O10 . 3 78.10(13) no O3 V3 O3 4_465 . 176.4(2) no O17 V3 O3 3_554 . 78.67(15) no O18 V3 O3 . . 85.01(14) no O9 V3 O3 . . 82.27(19) no O10 V3 O3 3 . 78.1(2) no O4 V4 O16 4_465 . 97.80(15) no O4 V4 O15 4_465 3_554 101.85(16) no O16 V4 O15 . 3_554 91.31(15) no O4 V4 O9 4_465 3_554 94.8(2) no O16 V4 O9 . 3_554 166.26(18) no O15 V4 O9 3_554 3_554 91.54(14) no O4 V4 O10 4_465 . 100.8(2) no O16 V4 O10 . . 93.49(13) no O15 V4 O10 3_554 . 156.0(2) no O9 V4 O10 3_554 . 78.65(13) no O4 V4 O4 4_465 . 175.5(2) no O16 V4 O4 . . 86.50(12) no O15 V4 O4 3_554 . 79.38(14) no O9 V4 O4 3_554 . 80.83(19) no O10 V4 O4 . . 77.46(19) no O11 P1 O13 . 3_554 116.0(2) no O11 P1 O10 . . 109.7(2) no O13 P1 O10 3_554 . 111.2(2) no O11 P1 O6 . 2_664 109.64(17) no O13 P1 O6 3_554 2_664 105.33(19) no O10 P1 O6 . 2_664 104.1(2) no O12 P2 O14 . . 116.9(2) no O12 P2 O9 . . 110.8(2) no O14 P2 O9 . . 109.1(2) no O12 P2 O6 . . 108.12(17) no O14 P2 O6 . . 106.61(18) no O9 P2 O6 . . 104.5(2) no O18 P3 O16 . . 114.9(2) no O18 P3 O7 . . 109.4(2) no O16 P3 O7 . . 111.0(2) no O18 P3 O5 . 2_664 107.2(2) no O16 P3 O5 . 2_664 107.49(19) no O7 P3 O5 . 2_664 106.5(2) no O15 P4 O17 . . 114.2(2) no O15 P4 O8 . . 110.4(2) no O17 P4 O8 . . 110.3(2) no O15 P4 O5 . . 107.6(2) no O17 P4 O5 . . 106.8(2) no O8 P4 O5 . . 107.4(2) no V1 O1 V1 . 4_455 156.36(16) no V2 O2 V2 . 4_475 160.47(18) no V3 O3 V3 4_565 . 171.92(19) no V4 O4 V4 4_565 . 170.90(18) no P4 O5 P3 . 2_665 157.20(17) yes P2 O6 P1 . 2_665 144.50(18) yes P3 O7 V2 . . 127.5(2) no P3 O7 V1 . 3_564 129.9(2) no V2 O7 V1 . 3_564 102.12(15) no P4 O8 V2 . 3_545 129.8(2) no P4 O8 V1 . . 128.1(2) no V2 O8 V1 3_545 . 102.02(15) no P2 O9 V4 . 3 128.5(3) no P2 O9 V3 . . 125.4(2) no V4 O9 V3 3 . 102.13(14) no P1 O10 V4 . . 133.8(2) no P1 O10 V3 . 3_554 121.7(3) no V4 O10 V3 . 3_554 101.11(14) no P1 O11 V1 . 3_564 156.3(2) no P2 O12 V1 . . 155.6(2) no P1 O13 V2 3 . 132.4(2) no P2 O14 V2 . 1_545 143.2(2) no P4 O15 V4 . 3 138.8(2) no P3 O16 V4 . . 150.8(2) no P4 O17 V3 . 3 139.0(3) no P3 O18 V3 . . 149.1(2) 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 V1 O1 . 1.594(3) yes V1 O11 3_545 1.941(3) yes V1 O12 . 1.949(3) yes V1 O7 3_545 2.079(4) yes V1 O8 . 2.083(4) yes V1 O1 4 2.341(3) yes V2 O2 . 1.600(5) yes V2 O14 1_565 1.951(4) yes V2 O13 . 1.957(4) yes V2 O8 3_564 2.071(4) yes V2 O7 . 2.071(4) yes V2 O2 4_575 2.305(5) yes V3 O3 4_465 1.603(6) yes V3 O17 3_554 1.944(4) yes V3 O18 . 1.954(4) yes V3 O9 . 2.070(4) yes V3 O10 3 2.077(4) yes V3 O3 . 2.256(6) yes V4 O4 4_465 1.612(4) yes V4 O16 . 1.940(3) yes V4 O15 3_554 1.942(3) yes V4 O9 3_554 2.050(4) yes V4 O10 . 2.073(4) yes V4 O4 . 2.250(4) yes P1 O11 . 1.487(4) yes P1 O13 3_554 1.499(4) yes P1 O10 . 1.557(4) yes P1 O6 2_664 1.583(3) yes P2 O12 . 1.490(3) yes P2 O14 . 1.498(4) yes P2 O9 . 1.556(3) yes P2 O6 . 1.579(3) yes P3 O18 . 1.487(4) yes P3 O16 . 1.494(3) yes P3 O7 . 1.554(3) yes P3 O5 2_664 1.576(3) yes P4 O15 . 1.495(4) yes P4 O17 . 1.498(4) yes P4 O8 . 1.554(3) yes P4 O5 . 1.573(3) yes 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O15 P4 O5 P3 2_665 -117.8(7) no O17 P4 O5 P3 2_665 119.2(7) no O8 P4 O5 P3 2_665 .9(7) no O12 P2 O6 P1 2_665 -21.2(4) no O14 P2 O6 P1 2_665 -147.7(3) no O9 P2 O6 P1 2_665 96.9(3) no