#------------------------------------------------------------------------------ #$Date: 2011-01-03 14:48:23 +0200 (Mon, 03 Jan 2011) $ #$Revision: 5312 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000194.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_4000194 loop_ _publ_author_name 'Choi, C' 'Anokhina, E V' 'Taullelle, F' 'Zhao, Y' 'Lachgar, A' _publ_section_title ; (C10H28N4)[Ga6(OH)2(PO4)2(HPO4)4(C2O4)3].3.5H2O Preparation, Crystal Structure, NMR Spectroscopy, and Thermal Stability of a Novel Gallium Phosphatooxalate with pendant Oxalate ligands ; _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_formula_structural 'C8 H20.50 Ga3 N2 O20.75 P3' _chemical_formula_sum 'C16 H41 Ga6 N4 O41.5 P6' _chemical_formula_weight 778.83 _chemical_name_systematic 'Gallium Phosphatooxalate' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 73.988(9) _cell_angle_beta 79.199(7) _cell_angle_gamma 78.775(7) _cell_formula_units_Z 2 _cell_length_a 9.0220(7) _cell_length_b 9.1864(9) _cell_length_c 13.4912(9) _cell_measurement_reflns_used 40 _cell_measurement_temperature 228(2) _cell_measurement_theta_max 12.90 _cell_measurement_theta_min 3.82 _cell_volume 1043.55(15) _diffrn_ambient_temperature 228(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 7155 _diffrn_reflns_theta_max 30.20 _diffrn_reflns_theta_min 2.32 _diffrn_standards_decay_% ? _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.187 _exptl_absorpt_correction_T_max 0.9742 _exptl_absorpt_correction_T_min 0.5793 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 773 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 364 _refine_ls_number_reflns 6075 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0301 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+1.3168P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.0657 _reflns_number_gt 4981 _reflns_number_total 6075 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4000194 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ga1 Ga 0.10385(3) 0.14220(3) 0.24218(2) 0.00981(6) Uani 1 1 d . . . Ga2 Ga 0.39918(3) 0.70671(3) 0.02524(2) 0.00990(6) Uani 1 1 d . . . Ga3 Ga 0.48262(3) 0.11052(3) 0.29716(2) 0.00920(6) Uani 1 1 d . . . P1 P 0.32790(7) 0.38726(8) 0.13373(5) 0.01022(12) Uani 1 1 d . . . P2 P 0.37903(8) -0.08789(8) 0.18120(5) 0.01135(12) Uani 1 1 d . . . P3 P -0.21680(8) 0.21610(9) 0.15774(5) 0.01343(13) Uani 1 1 d . . . O11 O 0.2985(2) 0.5629(2) 0.11930(15) 0.0170(4) Uani 1 1 d . . . O12 O 0.4069(2) 0.3575(2) 0.02728(14) 0.0158(4) Uani 1 1 d . . . O13 O 0.1735(2) 0.3328(2) 0.15917(14) 0.0143(4) Uani 1 1 d . . . O14 O 0.4321(2) 0.3161(2) 0.21597(14) 0.0136(4) Uani 1 1 d . . . O21 O 0.2320(2) 0.0148(2) 0.15318(14) 0.0143(4) Uani 1 1 d . . . O22 O 0.5012(2) -0.0020(2) 0.19091(14) 0.0127(4) Uani 1 1 d . . . O23 O 0.3435(3) -0.2158(3) 0.28432(17) 0.0227(4) Uani 1 1 d D . . H23 H 0.317(7) -0.180(7) 0.333(4) 0.090(16) Uiso 1 1 d D . . O24 O 0.4479(2) -0.1727(3) 0.09696(18) 0.0248(5) Uani 1 1 d . . . O31 O -0.2579(3) 0.3927(3) 0.14620(19) 0.0262(5) Uani 1 1 d D . . H31 H -0.302(7) 0.423(7) 0.191(4) 0.090(16) Uiso 1 1 d D . . O32 O -0.0457(2) 0.1715(2) 0.14738(14) 0.0166(4) Uani 1 1 d . . . O33 O 0.6985(2) 0.1310(2) 0.25893(14) 0.0135(4) Uani 1 1 d . . . O34 O -0.2667(2) 0.1831(3) 0.06294(15) 0.0207(4) Uani 1 1 d . . . O1 O -0.0413(2) 0.2475(2) 0.33839(14) 0.0147(4) Uani 1 1 d . . . O2 O 0.0160(2) -0.0416(2) 0.33118(14) 0.0138(4) Uani 1 1 d . . . O3 O -0.2102(3) 0.1958(3) 0.48343(17) 0.0260(5) Uani 1 1 d . . . O4 O -0.1489(2) -0.1105(2) 0.47331(15) 0.0186(4) Uani 1 1 d . . . C1 C -0.1181(3) 0.1577(3) 0.4120(2) 0.0145(5) Uani 1 1 d . . . C2 C -0.0841(3) -0.0117(3) 0.40646(19) 0.0136(5) Uani 1 1 d . . . O5 O 0.4672(2) 0.1889(2) 0.42628(13) 0.0139(4) Uani 1 1 d . . . O6 O 0.5340(2) -0.0953(2) 0.40121(13) 0.0134(4) Uani 1 1 d . . . C3 C 0.4812(3) 0.0820(3) 0.50745(19) 0.0123(5) Uani 1 1 d . . . O7 O 0.2675(2) 0.0917(2) 0.32850(14) 0.0117(3) Uani 1 1 d . . . H7 H 0.240(5) 0.084(5) 0.386(3) 0.033(11) Uiso 1 1 d . . . N1 N -0.2236(3) -0.1493(4) 0.0650(2) 0.0269(6) Uani 1 1 d D . . H1N1 H -0.268(5) -0.233(5) 0.068(3) 0.049(14) Uiso 1 1 d D . . H1N2 H -0.197(6) -0.107(6) -0.006(3) 0.076(18) Uiso 1 1 d D . . H1N3 H -0.298(7) -0.084(8) 0.100(5) 0.12(3) Uiso 1 1 d D . . N2 N -0.0017(3) -0.3919(3) 0.39736(18) 0.0169(5) Uani 1 1 d . . . H2N1 H -0.011(4) -0.310(5) 0.419(3) 0.027(10) Uiso 1 1 d . . . C11 C -0.0896(4) -0.2044(6) 0.1209(3) 0.0482(13) Uani 1 1 d . . . H11A H -0.0300 -0.1208 0.1079 0.058 Uiso 1 1 calc R . . H11B H -0.0244 -0.2875 0.0938 0.058 Uiso 1 1 calc R . . C12 C -0.1348(3) -0.2618(4) 0.2371(2) 0.0202(6) Uani 1 1 d . . . H12A H -0.2172 -0.3233 0.2511 0.024 Uiso 1 1 calc R . . H12B H -0.1703 -0.1754 0.2692 0.024 Uiso 1 1 calc R . . C13 C 0.0065(4) -0.3589(4) 0.2807(2) 0.0220(6) Uani 1 1 d . . . H13A H 0.0243 -0.4566 0.2611 0.026 Uiso 1 1 calc R . . H13B H 0.0947 -0.3065 0.2478 0.026 Uiso 1 1 calc R . . C14 C -0.1416(3) -0.4562(4) 0.4557(2) 0.0195(6) Uani 1 1 d . . . H14A H -0.1487 -0.5478 0.4341 0.023 Uiso 1 1 calc R . . H14B H -0.2321 -0.3807 0.4391 0.023 Uiso 1 1 calc R . . C15 C 0.1379(3) -0.5024(4) 0.4280(2) 0.0212(6) Uani 1 1 d . . . H15A H 0.2291 -0.4569 0.3917 0.025 Uiso 1 1 calc R . . H15B H 0.1408 -0.5960 0.4057 0.025 Uiso 1 1 calc R . . O1W O 0.5865(5) 0.4929(6) 0.3217(3) 0.0855(15) Uani 1 1 d . . . H1W1 H 0.5017 0.5233 0.3618 0.128 Uiso 0.50 1 d P . . H1W2 H 0.5742 0.5661 0.2682 0.128 Uiso 1 1 d . . . O2W O -0.0467(6) 0.5350(7) 0.0370(4) 0.0434(14) Uani 0.50 1 d P . . H2W H 0.0600 0.4895 0.0340 0.065 Uiso 1 1 d . . . O3W O 0.531(4) 0.454(4) 0.5000 0.153(11) Uiso 0.25 1 d P . . H3W H 0.5116 0.5042 0.4409 0.229 Uiso 0.50 1 d P . . 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 Ga1 0.00776(12) 0.01351(13) 0.00843(11) -0.00127(9) -0.00160(9) -0.00395(10) Ga2 0.01130(13) 0.01085(13) 0.00890(12) -0.00295(9) -0.00195(9) -0.00369(10) Ga3 0.00865(12) 0.01315(13) 0.00712(11) -0.00228(9) -0.00148(9) -0.00480(10) P1 0.0098(3) 0.0101(3) 0.0094(3) -0.0005(2) 0.0011(2) -0.0034(2) P2 0.0103(3) 0.0137(3) 0.0127(3) -0.0057(2) -0.0017(2) -0.0043(2) P3 0.0086(3) 0.0205(3) 0.0103(3) 0.0023(2) -0.0034(2) -0.0070(3) O11 0.0191(10) 0.0100(9) 0.0182(9) -0.0018(7) 0.0054(7) -0.0042(7) O12 0.0148(9) 0.0183(9) 0.0125(8) -0.0047(7) 0.0020(7) -0.0008(7) O13 0.0113(9) 0.0152(9) 0.0148(8) 0.0029(7) -0.0033(7) -0.0061(7) O14 0.0118(9) 0.0150(9) 0.0145(8) -0.0006(7) -0.0031(7) -0.0063(7) O21 0.0105(8) 0.0222(10) 0.0119(8) -0.0062(7) -0.0036(7) -0.0017(7) O22 0.0104(8) 0.0195(9) 0.0120(8) -0.0075(7) -0.0005(6) -0.0073(7) O23 0.0240(11) 0.0166(10) 0.0250(11) 0.0023(8) -0.0036(9) -0.0078(9) O24 0.0143(10) 0.0358(13) 0.0364(12) -0.0289(10) -0.0018(9) -0.0055(9) O31 0.0221(11) 0.0204(11) 0.0288(12) 0.0038(9) -0.0001(9) -0.0040(9) O32 0.0099(9) 0.0280(11) 0.0126(8) -0.0016(8) -0.0044(7) -0.0070(8) O33 0.0092(8) 0.0207(10) 0.0111(8) 0.0007(7) -0.0040(6) -0.0077(7) O34 0.0120(9) 0.0367(13) 0.0129(9) 0.0000(8) -0.0066(7) -0.0070(9) O1 0.0140(9) 0.0139(9) 0.0160(8) -0.0029(7) -0.0002(7) -0.0045(7) O2 0.0129(9) 0.0158(9) 0.0136(8) -0.0038(7) -0.0005(7) -0.0059(7) O3 0.0243(11) 0.0250(11) 0.0247(11) -0.0073(9) 0.0087(9) -0.0043(9) O4 0.0212(10) 0.0195(10) 0.0153(9) -0.0015(8) 0.0001(8) -0.0102(8) C1 0.0118(11) 0.0153(12) 0.0156(11) -0.0004(9) -0.0027(9) -0.0045(10) C2 0.0129(12) 0.0163(12) 0.0128(11) -0.0007(9) -0.0047(9) -0.0068(10) O5 0.0167(9) 0.0173(9) 0.0089(8) -0.0011(7) -0.0020(7) -0.0082(8) O6 0.0162(9) 0.0159(9) 0.0085(8) -0.0024(7) -0.0025(7) -0.0037(7) C3 0.0096(11) 0.0177(13) 0.0115(10) -0.0031(9) -0.0025(8) -0.0061(9) O7 0.0091(8) 0.0189(9) 0.0078(8) -0.0025(7) -0.0011(6) -0.0048(7) N1 0.0234(14) 0.0341(16) 0.0204(12) -0.0010(11) -0.0072(11) -0.0023(12) N2 0.0190(12) 0.0154(11) 0.0159(10) -0.0037(9) -0.0026(9) -0.0019(9) C11 0.0176(16) 0.087(4) 0.0229(16) 0.0111(19) -0.0030(13) -0.0028(19) C12 0.0197(14) 0.0236(14) 0.0174(12) -0.0040(11) -0.0045(10) -0.0031(11) C13 0.0208(14) 0.0262(15) 0.0151(12) -0.0030(11) -0.0016(10) 0.0019(12) C14 0.0191(14) 0.0210(14) 0.0186(12) -0.0028(10) -0.0044(10) -0.0047(11) C15 0.0165(13) 0.0247(15) 0.0188(13) -0.0018(11) -0.0032(10) 0.0009(11) O1W 0.096(3) 0.117(4) 0.065(2) -0.036(2) 0.010(2) -0.070(3) O2W 0.035(3) 0.045(3) 0.044(3) 0.005(3) -0.010(2) -0.012(3) loop_ _atom_type_symbol _atom_type_oxidation_number Ga 3.0 P 5.0 O -2.0 N -3