#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238816.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_2238816 loop_ _publ_author_name 'Ould Saleck, Ahmed' 'Assani, Abderrazzak' 'Saadi, Mohamed' 'El Ammari, Lahcen' _publ_section_title ; A triclinic polymorph of dicadmium divanadate(V) ; _journal_coeditor_code WM2776 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i79 _journal_paper_doi 10.1107/S1600536813028869 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac 'Cd2 V2 O7' _chemical_formula_moiety 'Cd2 O7 V2' _chemical_formula_structural 'Cd2 V2 O7' _chemical_formula_sum 'Cd2 O7 V2' _chemical_formula_weight 438.68 _chemical_name_systematic ; Dicadmium divanadate(V) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 83.3250(10) _cell_angle_beta 63.8980(10) _cell_angle_gamma 80.1450(10) _cell_formula_units_Z 2 _cell_length_a 6.5974(2) _cell_length_b 6.8994(2) _cell_length_c 6.9961(2) _cell_measurement_reflns_used 2717 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 33.13 _cell_measurement_theta_min 3.00 _cell_volume 281.450(15) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)' _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method '\f and \w scans' _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 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 10113 _diffrn_reflns_theta_full 33.13 _diffrn_reflns_theta_max 33.13 _diffrn_reflns_theta_min 3.00 _exptl_absorpt_coefficient_mu 10.650 _exptl_absorpt_correction_T_max 0.3759 _exptl_absorpt_correction_T_min 0.1636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 5.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 396 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.696 _refine_diff_density_min -1.527 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 2134 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.206 _refine_ls_R_factor_all 0.0164 _refine_ls_R_factor_gt 0.0155 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+0.2572P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0374 _reflns_number_gt 2077 _reflns_number_total 2134 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL El13_D205_DRX3_S23 in P-1 CELL 0.71073 6.5974 6.8994 6.9961 83.325 63.898 80.145 ZERR 2.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC O V CD UNIT 14 4 4 MERG 2 SHEL 40 0.65 OMIT 2 0 0 OMIT 0 0 2 FMAP 2 PLAN 10 ACTA BOND L.S. 10 WGHT 0.014800 0.257200 FVAR 0.16175 CD1 3 0.242138 0.336697 0.832583 11.00000 0.00672 0.00774 = 0.00900 0.00047 -0.00431 -0.00006 CD2 3 0.749797 0.034380 0.757479 11.00000 0.00779 0.00795 = 0.00808 0.00069 -0.00277 0.00031 V1 2 0.710381 0.164502 0.258637 11.00000 0.00423 0.00515 = 0.00483 -0.00007 -0.00222 -0.00033 V2 2 0.228362 0.455174 0.344090 11.00000 0.00472 0.00635 = 0.00446 -0.00065 -0.00115 -0.00089 O1 1 0.861194 0.332841 0.081555 11.00000 0.00890 0.00960 = 0.00982 0.00231 -0.00253 -0.00313 O2 1 0.862190 0.043913 0.390716 11.00000 0.00798 0.01241 = 0.00898 0.00034 -0.00444 0.00090 O3 1 0.459176 0.289333 0.436292 11.00000 0.00700 0.01161 = 0.00787 -0.00130 -0.00322 0.00210 O4 1 0.654631 -0.006377 0.123319 11.00000 0.01100 0.00679 = 0.00947 -0.00137 -0.00542 -0.00123 O5 1 0.271365 0.294814 0.165970 11.00000 0.01283 0.00787 = 0.00831 -0.00154 -0.00570 0.00019 O6 1 0.383925 0.643814 0.243573 11.00000 0.00811 0.00790 = 0.01465 0.00141 -0.00457 -0.00209 O7 1 -0.049612 0.589249 0.367816 11.00000 0.00555 0.01567 = 0.00637 0.00039 -0.00205 0.00265 HKLF 4 REM El13_D205_DRX3_S23 in P-1 REM R1 = 0.0155 for 2077 Fo > 4sig(Fo) and 0.0164 for all 2134 data REM 100 parameters refined using 0 restraints END WGHT 0.0144 0.2603 REM Highest difference peak 0.696, deepest hole -1.527, 1-sigma level 0.245 Q1 1 0.8105 -0.1526 0.5681 11.00000 0.05 0.70 Q2 1 0.7490 0.2997 0.1298 11.00000 0.05 0.69 Q3 1 0.7454 0.4242 0.0805 11.00000 0.05 0.66 Q4 1 0.7425 0.3438 -0.0197 11.00000 0.05 0.65 Q5 1 0.7663 -0.0627 0.5036 11.00000 0.05 0.65 Q6 1 0.7319 -0.0947 0.4312 11.00000 0.05 0.65 Q7 1 0.3105 0.5792 0.2755 11.00000 0.05 0.64 Q8 1 0.7117 -0.0869 0.1577 11.00000 0.05 0.63 Q9 1 0.1648 0.6560 0.2657 11.00000 0.05 0.62 Q10 1 0.2150 0.2055 0.5257 11.00000 0.05 0.62 ; _cod_data_source_file wm2776.cif _cod_data_source_block I _cod_original_cell_volume 281.450(14) _cod_database_code 2238816 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_occupancy _atom_site_symmetry_multiplicity Cd Cd1 0.24214(2) 0.336697(18) 0.83258(2) 0.00767(4) Uani d 1 1 Cd Cd2 0.74980(2) 0.034380(18) 0.75748(2) 0.00845(4) Uani d 1 1 V V1 0.71038(5) 0.16450(4) 0.25864(4) 0.00469(5) Uani d 1 1 V V2 0.22836(5) 0.45517(4) 0.34409(5) 0.00542(5) Uani d 1 1 O O1 0.8612(2) 0.3328(2) 0.0816(2) 0.0100(2) Uani d 1 1 O O2 0.8622(2) 0.0439(2) 0.3907(2) 0.0099(2) Uani d 1 1 O O3 0.4592(2) 0.2893(2) 0.4363(2) 0.0092(2) Uani d 1 1 O O4 0.6546(2) -0.00638(19) 0.1233(2) 0.0086(2) Uani d 1 1 O O5 0.2714(2) 0.29481(19) 0.1660(2) 0.0093(2) Uani d 1 1 O O6 0.3839(2) 0.6438(2) 0.2436(2) 0.0104(2) Uani d 1 1 O O7 -0.0496(2) 0.5892(2) 0.3678(2) 0.0100(2) Uani d 1 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 Cd1 0.00672(6) 0.00774(6) 0.00900(6) -0.00006(4) -0.00431(4) 0.00047(4) Cd2 0.00779(6) 0.00795(6) 0.00808(6) 0.00031(4) -0.00277(4) 0.00069(4) V1 0.00423(11) 0.00515(11) 0.00483(11) -0.00033(8) -0.00222(9) -0.00007(9) V2 0.00472(11) 0.00635(12) 0.00446(11) -0.00089(9) -0.00115(9) -0.00065(9) O1 0.0089(5) 0.0096(5) 0.0098(5) -0.0031(4) -0.0025(5) 0.0023(4) O2 0.0080(5) 0.0124(6) 0.0090(5) 0.0009(4) -0.0044(4) 0.0003(4) O3 0.0070(5) 0.0116(6) 0.0079(5) 0.0021(4) -0.0032(4) -0.0013(4) O4 0.0110(6) 0.0068(5) 0.0095(5) -0.0012(4) -0.0054(5) -0.0014(4) O5 0.0128(6) 0.0079(5) 0.0083(5) 0.0002(4) -0.0057(5) -0.0015(4) O6 0.0081(5) 0.0079(5) 0.0147(6) -0.0021(4) -0.0046(5) 0.0014(4) O7 0.0056(5) 0.0157(6) 0.0064(5) 0.0026(4) -0.0020(4) 0.0004(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Cd Cd -0.8075 1.2024 '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 O7 Cd1 O4 2_566 2_656 114.29(5) O7 Cd1 O6 2_566 2_666 131.24(5) O4 Cd1 O6 2_656 2_666 83.66(5) O7 Cd1 O1 2_566 2_666 85.81(5) O4 Cd1 O1 2_656 2_666 157.35(5) O6 Cd1 O1 2_666 2_666 90.73(5) O7 Cd1 O1 2_566 1_456 76.73(5) O4 Cd1 O1 2_656 1_456 94.46(5) O6 Cd1 O1 2_666 1_456 149.98(5) O1 Cd1 O1 2_666 1_456 79.55(5) O7 Cd1 O5 2_566 1_556 153.49(5) O4 Cd1 O5 2_656 1_556 74.22(5) O6 Cd1 O5 2_666 1_556 73.06(5) O1 Cd1 O5 2_666 1_556 83.15(5) O1 Cd1 O5 1_456 1_556 77.60(5) O7 Cd1 O3 2_566 . 62.10(5) O4 Cd1 O3 2_656 . 86.49(5) O6 Cd1 O3 2_666 . 75.19(5) O1 Cd1 O3 2_666 . 113.31(5) O1 Cd1 O3 1_456 . 134.73(5) O5 Cd1 O3 1_556 . 144.28(4) O6 Cd2 O5 2_666 2_656 156.37(5) O6 Cd2 O2 2_666 2_756 116.20(5) O5 Cd2 O2 2_656 2_756 87.38(5) O6 Cd2 O2 2_666 . 88.75(5) O5 Cd2 O2 2_656 . 99.75(5) O2 Cd2 O2 2_756 . 74.71(5) O6 Cd2 O4 2_666 1_556 96.72(5) O5 Cd2 O4 2_656 1_556 75.42(5) O2 Cd2 O4 2_756 1_556 102.17(5) O2 Cd2 O4 . 1_556 174.49(5) O6 Cd2 O4 2_666 2_656 81.30(5) O5 Cd2 O4 2_656 2_656 75.69(5) O2 Cd2 O4 2_756 2_656 160.52(5) O2 Cd2 O4 . 2_656 98.40(5) O4 Cd2 O4 1_556 2_656 83.09(5) O1 V1 O2 . . 109.38(7) O1 V1 O3 . . 107.57(7) O2 V1 O3 . . 109.85(7) O1 V1 O4 . . 109.71(7) O2 V1 O4 . . 109.65(7) O3 V1 O4 . . 110.65(6) O5 V2 O6 . . 114.25(7) O5 V2 O7 . . 99.11(7) O6 V2 O7 . . 98.25(7) O5 V2 O7 . 2_566 121.64(7) O6 V2 O7 . 2_566 123.74(7) O7 V2 O7 . 2_566 79.57(6) O5 V2 O3 . . 92.06(6) O6 V2 O3 . . 93.85(6) O7 V2 O3 . . 158.40(6) O7 V2 O3 2_566 . 78.83(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cd1 O7 2_566 2.2401(13) Cd1 O4 2_656 2.2898(13) Cd1 O6 2_666 2.3083(14) Cd1 O1 2_666 2.3345(14) Cd1 O1 1_456 2.3476(13) Cd1 O5 1_556 2.4043(13) Cd1 O3 . 2.5300(13) Cd2 O6 2_666 2.2449(14) Cd2 O5 2_656 2.2858(13) Cd2 O2 2_756 2.2894(14) Cd2 O2 . 2.3327(14) Cd2 O4 1_556 2.3459(13) Cd2 O4 2_656 2.4562(14) V1 O1 . 1.6882(13) V1 O2 . 1.7028(14) V1 O3 . 1.7265(13) V1 O4 . 1.7708(13) V2 O5 . 1.6612(14) V2 O6 . 1.6885(14) V2 O7 . 1.8530(13) V2 O7 2_566 1.8535(13) V2 O3 . 2.0348(13) V2 V2 2_566 2.8482(6)