#------------------------------------------------------------------------------ #$Date: 2015-02-05 10:50:53 +0200 (Thu, 05 Feb 2015) $ #$Revision: 131180 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/06/4030615.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4030615 loop_ _publ_author_name 'Riou, D.' 'Ferey, G' _publ_section_title ; The structure of the intercalate VOPO4, 0.5 piperazin ; _journal_name_full 'European Journal of Solid State and Inorganic Chemistry' _journal_page_first 25 _journal_page_last 35 _journal_volume 31 _journal_year 1994 _chemical_formula_sum 'C2 H6 N O5 P V' _chemical_formula_weight 205.99 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 111.14(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7906(4) _cell_length_b 8.2757(5) _cell_length_c 8.5617(4) _cell_volume 580.93(6) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 1.941 _exptl_crystal_density_diffrn 2.355 _exptl_crystal_F_000 412 _refine_ls_number_parameters 111 _refine_ls_number_reflns 1583 _refine_ls_R_factor_gt 0.024 _refine_ls_wR_factor_gt 0.025 _[local]_cod_data_source_file EJSSIC-1994-31-25-35.cif _[local]_cod_data_source_block VOPO4-half-piperazin _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; small difference in the abstract and in the table II about the beta angle, 111.13(1) and 111.14(1) ; _cod_database_code 4030615 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv V V Uiso 0.65750(10) 0.03400(10) 0.82250(10) 1.000 0.0079(1) P P Uiso 0.44280(10) 0.23430(10) 0.47960(10) 1.000 0.0077(3) O1 O Uiso 0.3540(2) 0.3833(2) 0.5111(2) 1.000 0.0141(9) O2 O Uiso 0.3230(2) 0.1496(2) 0.3243(2) 1.000 0.0124(8) O3 O Uiso 0.6005(2) 0.2865(2) 0.4545(2) 1.000 0.0131(8) O4 O Uiso 0.4878(2) 0.1181(2) 0.6291(2) 1.000 0.0131(8) O5 O Uiso 0.8374(2) 0.1025(2) 0.8594(2) 1.000 0.0179(9) N N Uiso 0.8587(2) 0.0703(2) 0.5216(2) 1.000 0.0147(10) C1 C Uiso 0.8510(3) 0.0064(3) 0.3557(3) 1.000 0.0165(11) C2 C Uiso 0.0272(3) 0.1281(3) 0.6220(3) 1.000 0.0161(11) H1 H Uiso 0.047(3) 0.284(3) 0.066(4) 1.000 0.018(4) H2 H Uiso 0.027(3) 0.158(3) 0.721(4) 1.000 0.018(4) H3 H Uiso 0.750(4) 0.968(4) 0.297(4) 1.000 0.018(4) H4 H Uiso 0.872(3) 0.095(4) 0.293(4) 1.000 0.018(4) H5 H Uiso 0.828(4) -0.003(4) 0.572(4) 1.000 0.018(4) H6 H Uiso 0.784(4) 0.145(4) 0.508(4) 1.000 0.018(4) 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' P P 0.1023 0.0942 ' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 V O5 116.61(9) . . yes O1 V O4 130.04(9) 2_646 . yes O2 V O4 87.12(8) 3_656 . yes O3 V O4 86.78(8) 4_555 . yes O1 V O5 113.30(9) 2_646 . yes O2 V O5 95.15(9) 3_656 . yes O3 V O5 93.18(9) 4_555 . yes O1 V O2 90.69(8) 2_646 3_656 yes O1 V O3 88.44(8) 2_646 4_555 yes O2 V O3 171.26(9) 3_656 4_555 yes O1 P O2 106.59(11) . . yes O1 P O3 109.87(11) . . yes O1 P O4 110.58(10) . . yes O2 P O3 112.22(10) . . yes O2 P O4 109.04(10) . . yes O3 P O4 108.55(11) . . yes V O1 P 144.81(11) 2_656 . yes V O2 P 134.20(12) 3_656 . yes V O3 P 134.17(11) 4_554 . yes V O4 P 146.60(13) . . yes C1 N C2 110.79(19) . 1_655 yes C1 N H6 110(2) . . no H5 N H6 102(3) . . no C1 N H5 109(2) . . no C2 N H6 113(2) 1_655 . no C2 N H5 112(2) 1_655 . no N C1 C2 110.74(19) . 3_656 yes N C2 C1 110.30(19) 1_455 3_656 yes N C1 H4 107.9(19) . . no N C1 H3 111(2) . 1_545 no H3 C1 H4 108(3) 1_545 . no C2 C1 H4 111.2(18) 3_656 . no C2 C1 H3 109(2) 3_656 1_545 no N C2 H2 107.2(19) 1_455 . no C1 C2 H2 109.4(18) 3_656 . no H1 C2 H2 110(2) 4_555 . no N C2 H1 106.7(19) 1_455 4_555 no C1 C2 H1 112.9(18) 3_656 4_555 no 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 V O4 1.9157(19) . yes V O5 1.601(2) . yes V O1 1.9233(18) 2_646 yes V O2 2.0182(19) 3_656 yes V O3 2.0355(19) 4_555 yes P O1 1.5344(19) . yes P O2 1.5357(18) . yes P O3 1.539(2) . yes P O4 1.5344(18) . yes N C1 1.494(3) . yes N C2 1.498(3) 1_655 yes N H5 0.84(3) . no N H6 0.88(4) . no C1 C2 1.508(4) 3_656 no C1 H4 0.97(3) . no C1 H3 0.91(3) 1_545 no C2 H2 0.88(3) . no C2 H1 0.92(3) 4_555 no 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 _geom_hbond_publ_flag N H5 O5 0.84(3) 2.58(3) 2.977(2) 110(3) . yes N H5 O2 0.84(3) 2.21(4) 3.021(2) 162(3) 3_656 yes N H6 O3 0.88(4) 1.91(4) 2.783(3) 172(3) . yes N H6 O5 0.88(4) 2.58(3) 3.018(2) 112(3) 4_554 yes C2_l H1 O5 0.92(3) 2.54(3) 3.179(3) 127(2) 1_454 yes C2 H2 O5 0.88(3) 2.41(3) 3.067(3) 131(2) 1_455 yes C1_h H3 O4 0.91(3) 2.50(4) 3.198(3) 135(3) 3_666 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 V O4 P -0.7(2) . . . no O1 V O4 P 176.46(17) 2_646 . . no O2 V O4 P -95.1(2) 3_656 . . no O3 V O4 P 91.2(2) 4_555 . . no O4 V O1 P 33.3(3) . 2_646 2_646 no O5 V O1 P -149.43(19) . 2_646 2_646 no O4 V O2 P -29.27(16) . 3_656 3_656 no O5 V O2 P -145.74(15) . 3_656 3_656 no O4 V O3 P 55.86(15) . 4_555 4_555 no O5 V O3 P 172.36(15) . 4_555 4_555 no O2 P O1 V 155.15(19) . . 2_656 no O3 P O1 V -83.0(2) . . 2_656 no O4 P O1 V 36.8(2) . . 2_656 no O1 P O2 V 170.80(13) . . 3_656 no O3 P O2 V 50.49(18) . . 3_656 no O4 P O2 V -69.81(17) . . 3_656 no O1 P O3 V -44.28(17) . . 4_554 no O2 P O3 V 74.11(16) . . 4_554 no O4 P O3 V -165.31(13) . . 4_554 no O1 P O4 V -105.0(2) . . . no O2 P O4 V 138.10(19) . . . no O3 P O4 V 15.6(2) . . . no C2 N C1 C2 57.3(2) 1_655 . 3_656 no