#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1004032.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_global _audit_creation_date 'October, 8, 2001' # TITLE _publ_section_title ; Hydrothermal synthesis and characterization of the new layered fluorogallophosphate Mu-23 Chem. Eur. J. 2002, 8, 1614' ; _publ_contact_author_name 'Dr. Angelique Simon' _publ_contact_author_address ; Laboratoire de Materiaux Mineraux, Universite de Haute Alsace 3, rue Alfred Werner F-68093 MULHOUSE CEDEX, FRANCE ; _publ_contact_author_email 'a.simon@uha.fr' _publ_contact_author_fax '[033] 3 89336885' _publ_contact_author_phone '[033] 3 89336884' _publ_requested_journal 'Chemistry a European Journal' # AUTHOR LIST loop_ _publ_author_name 'L. Josien' 'A. Simon' 'V. Gramlich' 'J. Patarin' data_mu23 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H43 F6 Ga5 N4 O22 P4' _chemical_formula_weight 1181.98 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.735(11) _cell_length_b 8.864(5) _cell_length_c 12.636(10) _cell_angle_alpha 98.36(5) _cell_angle_beta 100.18(8) _cell_angle_gamma 115.84(7) _cell_volume 838.9(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'prism' _exptl_crystal_colour colourless _exptl_crystal_size_max .4 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.340 _exptl_crystal_density_method ? _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 4.280 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min .26 _exptl_absorpt_correction_T_max .46 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SYNTEX P21 4-circle diffractometer' _diffrn_measurement_method ' \w scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2975 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2975 _reflns_number_observed 2432 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SIEMENS SHELXTL Plus' _computing_cell_refinement 'SIEMENS SHELXTL Plus' _computing_data_reduction 'SIEMENS SHELXTL Plus' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXLTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2975 _refine_ls_number_parameters 247 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_obs 0.0255 _refine_ls_wR_factor_all 0.0652 _refine_ls_wR_factor_obs 0.0641 _refine_ls_goodness_of_fit_all 0.957 _refine_ls_goodness_of_fit_obs 1.050 _refine_ls_restrained_S_all 0.958 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max 0.021 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.0000 0.5000 0.0000 0.00893(12) Uani 1 d S . Ga2 Ga 0.27456(5) 0.03080(4) 0.00642(3) 0.00971(10) Uani 1 d . . Ga3 Ga 0.73844(5) 0.37774(5) -0.27681(3) 0.01065(11) Uani 1 d D . P1 P 0.60563(11) 0.22351(11) -0.07886(7) 0.0097(2) Uani 1 d . . P2 P 0.09343(11) 0.24599(10) 0.10892(7) 0.0093(2) Uani 1 d . . O4 O 0.1917(3) 0.1410(3) 0.0939(2) 0.0155(5) Uani 1 d . . O8 O 0.6693(4) 0.1434(3) -0.3506(2) 0.0177(5) Uani 1 d D . H8X H 0.6497(36) 0.0624(14) -0.3182(15) 0.040 Uiso 1 d D . H8Y H 0.6646(58) 0.1135(23) -0.4198(12) 0.040 Uiso 1 d D . O6 O 0.4394(3) 0.1950(3) -0.0410(2) 0.0148(5) Uani 1 d . . F2 F 0.9032(3) 0.4362(3) -0.3618(2) 0.0184(4) Uani 1 d . . F1 F 0.9331(2) 0.4031(2) -0.1601(2) 0.0136(4) Uani 1 d . . O3 O 0.1911(3) 0.3793(3) 0.2189(2) 0.0136(5) Uani 1 d . . O5 O 0.3882(3) -0.0501(3) 0.0988(2) 0.0151(5) Uani 1 d . . O9 O 0.2324(3) 0.6451(3) -0.0122(2) 0.0126(5) Uani 1 d . . O7 O 0.5859(3) 0.2800(3) -0.1855(2) 0.0142(5) Uani 1 d . . F3 F 0.5600(3) 0.3730(3) -0.3836(2) 0.0187(4) Uani 1 d . . O2 O -0.0936(3) 0.1177(3) 0.1159(2) 0.0127(5) Uani 1 d . . N1 N -0.1090(4) 0.7169(4) 0.3029(3) 0.0235(7) Uani 1 d . . H1A H -0.0390(4) 0.6667(4) 0.3020(3) 0.035 Uiso 0.50 d PR . O2W O 0.8770(4) 0.2280(4) 0.3290(3) 0.0399(8) Uani 1 d DU . H5W H 0.9416(4) 0.3390(4) 0.3470(3) 0.040 Uiso 1 d RD . H4W H 0.8568(4) 0.1897(4) 0.2582(3) 0.040 Uiso 1 d RD . O1W O 0.6952(4) 0.0253(4) 0.4511(2) 0.0311(7) Uani 1 d DU . H1W H 0.7530(4) 0.0892(4) 0.4115(2) 0.040 Uiso 1 d RD . H2W H 0.5845(4) -0.0403(4) 0.4167(2) 0.040 Uiso 1 d RD . N4 N -0.4156(4) 0.4343(4) 0.3329(3) 0.0203(7) Uani 1 d . . H4A H -0.4854(4) 0.4846(4) 0.3341(3) 0.030 Uiso 1 d R . C2 C -0.2720(5) 0.6120(5) 0.2109(3) 0.0261(9) Uani 1 d . . H2A H -0.2416(5) 0.6071(5) 0.1415(3) 0.039 Uiso 1 d R . H2B H -0.3463(5) 0.6661(5) 0.2096(3) 0.039 Uiso 1 d R . C5 C -0.2517(5) 0.5414(5) 0.4258(3) 0.0234(9) Uani 1 d . . H5C H -0.1767(5) 0.4881(5) 0.4274(3) 0.035 Uiso 1 d R . H5D H -0.2823(5) 0.5464(5) 0.4951(3) 0.035 Uiso 1 d R . C6 C -0.1551(5) 0.7212(5) 0.4114(3) 0.0249(9) Uani 1 d . . H6A H -0.2276(5) 0.7769(5) 0.4142(3) 0.037 Uiso 1 d R . H6B H -0.0488(5) 0.7876(5) 0.4709(3) 0.037 Uiso 1 d R . C3 C -0.3705(5) 0.4324(5) 0.2243(3) 0.0257(9) Uani 1 d . . H3A H -0.4768(5) 0.3680(5) 0.1646(3) 0.038 Uiso 1 d R . H3B H -0.2995(5) 0.3752(5) 0.2205(3) 0.038 Uiso 1 d R . C8 C -0.0124(6) 0.8945(6) 0.2886(4) 0.0417(12) Uani 1 d . . H8A H 0.0154(6) 0.8882(6) 0.2184(4) 0.063 Uiso 1 d R . H8B H -0.0848(6) 0.9505(6) 0.2905(4) 0.063 Uiso 1 d R . H8C H 0.0948(6) 0.9598(6) 0.3475(4) 0.063 Uiso 1 d R . C7 C -0.5160(6) 0.2550(5) 0.3455(4) 0.0326(10) Uani 1 d . . H7A H -0.6207(6) 0.1890(5) 0.2849(4) 0.049 Uiso 1 d R . H7B H -0.4419(6) 0.2007(5) 0.3462(4) 0.049 Uiso 1 d R . H7C H -0.5483(6) 0.2602(5) 0.4142(4) 0.049 Uiso 1 d R . O1 O 0.0718(3) 0.3216(3) 0.0113(2) 0.0121(5) Uani 1 d . . 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 0.0055(3) 0.0099(3) 0.0100(3) 0.0025(2) 0.0026(2) 0.0023(2) Ga2 0.0060(2) 0.0099(2) 0.0133(2) 0.00271(15) 0.00440(15) 0.0032(2) Ga3 0.0075(2) 0.0124(2) 0.0106(2) 0.00198(15) 0.00287(15) 0.0037(2) P1 0.0055(4) 0.0103(4) 0.0135(4) 0.0041(3) 0.0044(3) 0.0028(4) P2 0.0064(4) 0.0091(4) 0.0114(4) 0.0015(3) 0.0030(3) 0.0030(4) O4 0.0159(13) 0.0179(13) 0.0170(13) 0.0014(10) 0.0057(10) 0.0123(11) O8 0.031(2) 0.0094(12) 0.0149(13) 0.0014(10) 0.0102(12) 0.0110(12) O6 0.0092(12) 0.0163(12) 0.0216(13) 0.0082(11) 0.0084(10) 0.0058(10) F2 0.0162(11) 0.0253(11) 0.0189(11) 0.0067(9) 0.0114(9) 0.0115(9) F1 0.0101(10) 0.0177(10) 0.0122(10) 0.0015(8) 0.0031(8) 0.0067(9) O3 0.0142(13) 0.0119(12) 0.0123(12) -0.0004(10) 0.0014(10) 0.0060(10) O5 0.0165(13) 0.0133(12) 0.0158(13) 0.0008(10) 0.0009(10) 0.0095(11) O9 0.0056(11) 0.0142(12) 0.0143(12) 0.0037(10) 0.0036(10) 0.0011(10) O7 0.0098(12) 0.0189(12) 0.0162(13) 0.0075(10) 0.0063(10) 0.0070(11) F3 0.0143(10) 0.0254(11) 0.0146(10) 0.0012(9) 0.0005(8) 0.0103(9) O2 0.0069(12) 0.0137(12) 0.0143(12) 0.0017(10) 0.0053(10) 0.0019(10) N1 0.016(2) 0.028(2) 0.034(2) 0.012(2) 0.0112(15) 0.014(2) O2W 0.046(2) 0.028(2) 0.040(2) 0.0080(14) 0.030(2) 0.0066(15) O1W 0.026(2) 0.031(2) 0.026(2) 0.0022(13) 0.0093(13) 0.0046(13) N4 0.017(2) 0.026(2) 0.021(2) 0.0038(14) 0.0055(14) 0.0134(15) C2 0.027(2) 0.043(2) 0.018(2) 0.009(2) 0.008(2) 0.024(2) C5 0.022(2) 0.033(2) 0.018(2) 0.006(2) 0.004(2) 0.016(2) C6 0.023(2) 0.027(2) 0.023(2) 0.001(2) 0.006(2) 0.012(2) C3 0.027(2) 0.036(2) 0.017(2) 0.003(2) 0.007(2) 0.018(2) C8 0.040(3) 0.035(3) 0.067(3) 0.029(2) 0.025(3) 0.023(2) C7 0.028(2) 0.029(2) 0.036(2) 0.010(2) 0.006(2) 0.009(2) O1 0.0106(12) 0.0127(12) 0.0133(12) 0.0033(10) 0.0039(10) 0.0056(10) _refine_diff_density_max 0.659 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.106