Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Morris, R.' 'Slawin, A.' 'Wragg, David S.' _publ_contact_author_name 'Prof Russell E. Morris' _publ_contact_author_address ; Prof R Morris School of Chemistry Purdie Building University of St Andrews St Andrews FIFE KY16 9ST UK ; _publ_contact_author_email 'rem1@st-andrews.ac.uk' _publ_section_title ; The Synthesis of Gallium Phosphate Frameworks with and without Fluoride Ions Present: Attempts to Direct the Synthesis of Double Four Ring-Containing Materials ; data_[pyr,F]-GaPO-1 _database_code_CSD 135560 _audit_creation_date 1999-08-06T10:42:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H14 F2 Ga6 N2 O25 P6' _chemical_formula_weight 1204.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.391(4) _cell_length_b 12.414(3) _cell_length_c 12.846(4) _cell_angle_alpha 71.04(3) _cell_angle_beta 68.39(2) _cell_angle_gamma 66.88(2) _cell_volume 1518.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.63 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.682 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6849 _diffrn_radiation_monochromator graphite _diffrn_reflns_number 14097 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.025 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.833 _diffrn_measured_fraction_theta_max 0.833 _reflns_number_total 7704 _reflns_number_gt 7319 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7704 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.207 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 1.766 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.39573(4) 0.70795(4) 0.24627(3) 0.00568(10) Uani 1 1 d . . . Ga2 Ga -0.19857(4) 1.27875(4) 0.06357(3) 0.00597(10) Uani 1 1 d . . . Ga3 Ga 0.10635(4) 0.82590(4) 0.25664(3) 0.00521(10) Uani 1 1 d . . . Ga4 Ga 0.31605(4) 0.77747(4) 0.58054(3) 0.00597(10) Uani 1 1 d . . . Ga5 Ga -0.26798(4) 0.92923(4) 0.16611(3) 0.00509(10) Uani 1 1 d . . . Ga6 Ga -0.21515(4) 0.55445(4) 0.33519(3) 0.00604(10) Uani 1 1 d . . . P7 P 0.18746(9) 0.68039(8) 0.48269(8) 0.00568(18) Uani 1 1 d . . . P8 P 0.55422(9) 0.78938(8) 0.34998(8) 0.00549(17) Uani 1 1 d . . . P9 P 0.31354(9) 0.85102(9) 0.02035(8) 0.00611(18) Uani 1 1 d . . . P10 P 0.63685(9) 0.45695(8) 0.23003(8) 0.00541(17) Uani 1 1 d . . . P11 P -0.13467(9) 1.06137(8) 0.24828(8) 0.00546(17) Uani 1 1 d . . . P12 P -0.03521(9) 0.70646(8) 0.17018(8) 0.00568(18) Uani 1 1 d . . . F1 F 0.2490(2) 0.6744(2) 0.2311(2) 0.0089(4) Uani 1 1 d . . . F2 F 0.2527(2) 0.8597(2) 0.2736(2) 0.0085(4) Uani 1 1 d . . . O3 O 0.4201(3) 0.7868(3) 0.0850(2) 0.0089(5) Uani 1 1 d . . . O4 O 0.3308(3) 0.6477(3) 0.4093(2) 0.0096(5) Uani 1 1 d . . . O5 O 0.5225(3) 0.7652(3) 0.2569(2) 0.0103(5) Uani 1 1 d . . . O6 O 0.5117(3) 0.5585(3) 0.2143(3) 0.0116(5) Uani 1 1 d . . . O7 O -0.1071(3) 1.1779(3) 0.1683(2) 0.0100(5) Uani 1 1 d . . . O8 O -0.3263(3) 1.2300(3) 0.0561(2) 0.0089(5) Uani 1 1 d . . . O9 O -0.0885(3) 1.3277(3) -0.0721(2) 0.0105(5) Uani 1 1 d . . . O10 O -0.2926(3) 1.4163(3) 0.1156(3) 0.0156(6) Uani 1 1 d . . . O11 O -0.0142(3) 0.9770(2) 0.2888(2) 0.0084(5) Uani 1 1 d . . . O12 O 0.1705(3) 0.8871(3) 0.0945(2) 0.0087(5) Uani 1 1 d . . . O13 O -0.0182(3) 0.7639(3) 0.2488(2) 0.0093(5) Uani 1 1 d . . . O14 O 0.0808(3) 0.7519(3) 0.4193(2) 0.0091(5) Uani 1 1 d . . . O15 O 0.1757(3) 0.7524(3) 0.5668(2) 0.0109(5) Uani 1 1 d . . . O16 O 0.4338(3) 0.8254(3) 0.4503(2) 0.0106(5) Uani 1 1 d . . . O17 O 0.3995(3) 0.6469(3) 0.6740(3) 0.0130(6) Uani 1 1 d . . . O18 O 0.2531(3) 0.9060(3) 0.6479(3) 0.0128(6) Uani 1 1 d . . . O19 O -0.1712(3) 1.0056(3) 0.1803(3) 0.0117(5) Uani 1 1 d . . . O20 O -0.3510(3) 1.0356(2) 0.0598(2) 0.0090(5) Uani 1 1 d . . . O21 O -0.1535(3) 0.7907(2) 0.1210(3) 0.0098(5) Uani 1 1 d . . . O22 O -0.3915(3) 0.8967(3) 0.3001(3) 0.0135(6) Uani 1 1 d . . . O23 O -0.0641(3) 0.5879(2) 0.2384(2) 0.0099(5) Uani 1 1 d . . . O24 O -0.3403(3) 0.6787(3) 0.3965(3) 0.0131(6) Uani 1 1 d . . . O25 O -0.1505(3) 0.4346(3) 0.4455(2) 0.0105(5) Uani 1 1 d . . . O26 O -0.2655(3) 0.4960(3) 0.2530(3) 0.0172(6) Uani 1 1 d . . . C1 C 0.0889(6) 1.2741(8) 0.2046(6) 0.0439(17) Uani 1 1 d . . . H1 H 0.0051 1.3033 0.2563 0.053 Uiso 1 1 calc R . . N1 N 0.1584(9) 1.1569(8) 0.2239(7) 0.072(3) Uani 1 1 d . . . H1A H 0.1264 1.1067 0.2839 0.087 Uiso 1 1 calc R . . C5 C 0.2829(10) 1.1156(6) 0.1468(9) 0.055(2) Uani 1 1 d . . . H5 H 0.3325 1.0329 0.1578 0.066 Uiso 1 1 calc R . . C2 C 0.1393(6) 1.3521(5) 0.1097(6) 0.0366(14) Uani 1 1 d . . . H2 H 0.0914 1.435 0.0942 0.044 Uiso 1 1 calc R . . C4 C 0.3298(6) 1.1928(7) 0.0596(5) 0.0413(17) Uani 1 1 d . . . H4 H 0.4163 1.1656 0.0105 0.05 Uiso 1 1 calc R . . C3 C 0.2617(7) 1.3048(7) 0.0388(5) 0.0475(19) Uani 1 1 d . . . H3 H 0.2975 1.3563 -0.0281 0.057 Uiso 1 1 calc R . . C7 C -0.6294(7) 1.1620(6) 0.3807(7) 0.0407(16) Uani 1 1 d . . . H7 H -0.5691 1.0829 0.3847 0.049 Uiso 1 1 calc R . . C9 C -0.8338(7) 1.2911(10) 0.4537(6) 0.059(3) Uani 1 1 d . . . H9 H -0.9194 1.3012 0.5069 0.07 Uiso 1 1 calc R . . C6 C -0.5991(7) 1.2585(11) 0.2932(6) 0.059(3) Uani 1 1 d . . . H6 H -0.5169 1.2458 0.2353 0.071 Uiso 1 1 calc R . . C8 C -0.7507(8) 1.1885(9) 0.4599(6) 0.055(2) Uani 1 1 d . . . H8 H -0.7727 1.1262 0.5221 0.066 Uiso 1 1 calc R . . N2 N -0.6873(12) 1.3684(9) 0.2926(9) 0.095(4) Uani 1 1 d . . . H2A H -0.6703 1.4304 0.2396 0.114 Uiso 1 1 calc R . . C10 C -0.8098(10) 1.3814(9) 0.3807(11) 0.072(3) Uani 1 1 d . . . H10 H -0.8734 1.4585 0.3842 0.086 Uiso 1 1 calc R . . O31 O 0.0894(10) 1.0300(7) 0.4524(7) 0.0335(19) Uani 0.5 1 d P . . O32 O -0.4336(13) 1.5253(11) -0.0594(10) 0.059(3) Uani 0.5 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 0.00428(18) 0.00686(19) 0.00328(18) -0.00082(14) -0.00094(13) 0.00063(14) Ga2 0.00713(18) 0.00536(18) 0.00316(18) -0.00125(14) 0.00044(14) -0.00109(14) Ga3 0.00433(18) 0.00593(18) 0.00308(18) -0.00088(14) -0.00094(14) 0.00058(14) Ga4 0.00601(18) 0.00540(18) 0.00363(18) -0.00130(14) 0.00080(14) -0.00057(14) Ga5 0.00647(18) 0.00465(18) 0.00340(18) -0.00068(14) -0.00098(14) -0.00145(14) Ga6 0.00695(18) 0.00490(18) 0.00536(19) 0.00036(14) -0.00223(14) -0.00161(14) P7 0.0049(4) 0.0067(4) 0.0030(4) 0.0005(3) -0.0010(3) -0.0006(3) P8 0.0056(4) 0.0047(4) 0.0037(4) -0.0011(3) 0.0006(3) -0.0007(3) P9 0.0054(4) 0.0076(4) 0.0032(4) 0.0001(3) -0.0013(3) -0.0008(3) P10 0.0060(4) 0.0043(4) 0.0049(4) -0.0023(3) -0.0017(3) 0.0008(3) P11 0.0057(4) 0.0036(4) 0.0060(4) -0.0019(3) -0.0017(3) 0.0004(3) P12 0.0060(4) 0.0045(4) 0.0043(4) -0.0018(3) 0.0008(3) -0.0007(3) F1 0.0077(10) 0.0089(10) 0.0084(10) -0.0028(8) -0.0023(8) -0.0001(8) F2 0.0064(9) 0.0101(10) 0.0072(10) -0.0027(8) -0.0019(8) -0.0002(8) O3 0.0069(11) 0.0114(12) 0.0043(11) 0.0002(10) -0.0012(9) -0.0005(10) O4 0.0049(11) 0.0139(13) 0.0044(11) 0.0001(10) -0.0012(9) 0.0009(10) O5 0.0074(12) 0.0165(13) 0.0068(12) -0.0035(10) -0.0010(9) -0.0036(10) O6 0.0097(12) 0.0099(12) 0.0103(13) -0.0024(10) -0.0031(10) 0.0024(10) O7 0.0115(12) 0.0093(12) 0.0097(13) 0.0018(10) -0.0052(10) -0.0047(10) O8 0.0079(12) 0.0100(12) 0.0083(12) -0.0038(10) -0.0001(10) -0.0028(10) O9 0.0098(12) 0.0097(12) 0.0065(12) -0.0017(10) 0.0035(10) -0.0028(10) O10 0.0217(15) 0.0095(13) 0.0088(13) -0.0066(11) 0.0003(11) 0.0017(11) O11 0.0088(12) 0.0067(11) 0.0086(12) -0.0024(10) -0.0052(10) 0.0019(10) O12 0.0056(11) 0.0118(12) 0.0027(11) 0.0016(9) -0.0008(9) 0.0004(10) O13 0.0088(12) 0.0111(12) 0.0078(12) -0.0041(10) -0.0011(10) -0.0021(10) O14 0.0051(11) 0.0135(13) 0.0042(11) 0.0010(10) -0.0020(9) 0.0002(10) O15 0.0075(12) 0.0158(13) 0.0092(13) -0.0076(11) -0.0008(10) -0.0007(10) O16 0.0115(12) 0.0099(12) 0.0064(12) -0.0031(10) 0.0038(10) -0.0042(10) O17 0.0118(13) 0.0122(13) 0.0101(13) 0.0042(11) -0.0029(10) -0.0042(11) O18 0.0101(12) 0.0105(13) 0.0136(14) -0.0088(11) 0.0044(10) -0.0012(10) O19 0.0165(13) 0.0087(12) 0.0123(13) -0.0020(10) -0.0061(11) -0.0047(11) O20 0.0105(12) 0.0084(12) 0.0080(12) 0.0025(10) -0.0052(10) -0.0038(10) O21 0.0090(12) 0.0084(12) 0.0120(13) -0.0061(10) -0.0058(10) 0.0030(10) O22 0.0178(14) 0.0118(13) 0.0074(12) -0.0042(10) 0.0067(11) -0.0090(11) O23 0.0083(12) 0.0059(12) 0.0107(13) -0.0026(10) 0.0035(10) -0.0023(10) O24 0.0113(13) 0.0129(13) 0.0087(13) -0.0043(11) -0.0036(10) 0.0051(11) O25 0.0105(12) 0.0092(12) 0.0091(12) 0.0047(10) -0.0044(10) -0.0041(10) O26 0.0179(15) 0.0154(14) 0.0239(16) -0.0059(12) -0.0126(13) -0.0032(12) C1 0.023(3) 0.080(5) 0.033(3) -0.025(3) 0.007(2) -0.023(3) N1 0.106(7) 0.087(6) 0.058(4) 0.044(4) -0.051(5) -0.085(6) C5 0.077(6) 0.020(3) 0.092(7) -0.009(3) -0.064(5) -0.004(3) C2 0.035(3) 0.017(2) 0.046(4) -0.008(2) -0.009(3) 0.002(2) C4 0.028(3) 0.055(4) 0.025(3) -0.025(3) -0.008(2) 0.018(3) C3 0.045(4) 0.050(4) 0.020(3) 0.013(3) 0.003(3) -0.015(3) C7 0.033(3) 0.035(3) 0.064(5) -0.029(3) -0.025(3) 0.005(3) C9 0.023(3) 0.105(7) 0.026(3) -0.028(4) -0.009(2) 0.016(4) C6 0.025(3) 0.130(9) 0.030(3) -0.025(4) 0.009(3) -0.040(4) C8 0.042(4) 0.093(7) 0.027(3) 0.022(4) -0.017(3) -0.038(4) N2 0.145(9) 0.086(6) 0.107(7) 0.066(6) -0.102(7) -0.097(7) C10 0.066(6) 0.055(5) 0.116(9) -0.054(6) -0.065(6) 0.025(5) O31 0.050(5) 0.024(4) 0.022(4) -0.006(3) -0.010(4) -0.006(4) O32 0.066(8) 0.066(8) 0.044(6) 0.012(5) -0.030(5) -0.023(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 O6 1.878(3) . ? Ga1 O5 1.904(3) . ? Ga1 O4 1.942(3) . ? Ga1 O3 1.949(3) . ? Ga1 F1 1.960(2) . ? Ga1 F2 1.982(2) . ? Ga1 Ga3 3.0068(13) . ? Ga2 O9 1.811(3) . ? Ga2 O10 1.813(3) . ? Ga2 O8 1.823(3) . ? Ga2 O7 1.838(3) . ? Ga3 O13 1.905(3) . ? Ga3 O11 1.908(3) . ? Ga3 O12 1.933(3) . ? Ga3 O14 1.952(3) . ? Ga3 F2 1.969(2) . ? Ga3 F1 1.974(2) . ? Ga4 O16 1.811(3) . ? Ga4 O15 1.821(3) . ? Ga4 O17 1.827(3) . ? Ga4 O18 1.830(3) . ? Ga5 O19 1.796(3) . ? Ga5 O20 1.817(3) . ? Ga5 O22 1.821(3) . ? Ga5 O21 1.823(3) . ? Ga6 O26 1.800(3) . ? Ga6 O24 1.808(3) . ? Ga6 O25 1.818(3) . ? Ga6 O23 1.825(3) . ? P7 O4 1.521(3) . ? P7 O14 1.529(3) . ? P7 O25 1.548(3) 2_566 ? P7 O15 1.553(3) . ? P8 O5 1.512(3) . ? P8 O16 1.527(3) . ? P8 O22 1.539(3) 1_655 ? P8 O24 1.546(3) 1_655 ? P9 O12 1.525(3) . ? P9 O3 1.533(3) . ? P9 O8 1.555(3) 2_575 ? P9 O20 1.560(3) 2_575 ? P10 O6 1.515(3) . ? P10 O26 1.522(3) 1_655 ? P10 O10 1.534(3) 1_645 ? P10 O17 1.538(3) 2_666 ? P11 O11 1.514(3) . ? P11 O19 1.518(3) . ? P11 O18 1.536(3) 2_576 ? P11 O7 1.549(3) . ? P12 O13 1.512(3) . ? P12 O9 1.524(3) 2_575 ? P12 O23 1.540(3) . ? P12 O21 1.550(3) . ? O8 P9 1.555(3) 2_575 ? O9 P12 1.524(3) 2_575 ? O10 P10 1.534(3) 1_465 ? O17 P10 1.538(3) 2_666 ? O18 P11 1.536(3) 2_576 ? O20 P9 1.560(3) 2_575 ? O22 P8 1.539(3) 1_455 ? O24 P8 1.546(3) 1_455 ? O25 P7 1.548(3) 2_566 ? O26 P10 1.522(3) 1_455 ? C1 N1 1.346(12) . ? C1 C2 1.380(10) . ? N1 C5 1.407(13) . ? C5 C4 1.312(12) . ? C2 C3 1.374(9) . ? C4 C3 1.293(10) . ? C7 C8 1.369(10) . ? C7 C6 1.408(12) . ? C9 C8 1.252(13) . ? C9 C10 1.257(15) . ? C6 N2 1.339(14) . ? N2 C10 1.425(16) . ? 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 O6 Ga1 O5 97.69(14) . . ? O6 Ga1 O4 95.17(13) . . ? O5 Ga1 O4 96.48(13) . . ? O6 Ga1 O3 93.53(13) . . ? O5 Ga1 O3 91.20(12) . . ? O4 Ga1 O3 167.52(12) . . ? O6 Ga1 F1 90.36(12) . . ? O5 Ga1 F1 171.39(11) . . ? O4 Ga1 F1 85.79(11) . . ? O3 Ga1 F1 85.23(11) . . ? O6 Ga1 F2 170.89(12) . . ? O5 Ga1 F2 91.27(12) . . ? O4 Ga1 F2 85.45(11) . . ? O3 Ga1 F2 84.56(11) . . ? F1 Ga1 F2 80.61(10) . . ? O6 Ga1 Ga3 130.65(10) . . ? O5 Ga1 Ga3 131.47(9) . . ? O4 Ga1 Ga3 84.61(9) . . ? O3 Ga1 Ga3 82.93(9) . . ? F1 Ga1 Ga3 40.32(7) . . ? F2 Ga1 Ga3 40.29(7) . . ? O9 Ga2 O10 102.75(14) . . ? O9 Ga2 O8 116.19(14) . . ? O10 Ga2 O8 103.38(15) . . ? O9 Ga2 O7 111.90(14) . . ? O10 Ga2 O7 106.17(14) . . ? O8 Ga2 O7 114.73(13) . . ? O13 Ga3 O11 97.87(12) . . ? O13 Ga3 O12 97.76(13) . . ? O11 Ga3 O12 94.85(12) . . ? O13 Ga3 O14 91.00(12) . . ? O11 Ga3 O14 92.03(12) . . ? O12 Ga3 O14 168.00(12) . . ? O13 Ga3 F2 169.73(11) . . ? O11 Ga3 F2 91.18(11) . . ? O12 Ga3 F2 86.23(11) . . ? O14 Ga3 F2 83.81(11) . . ? O13 Ga3 F1 90.20(11) . . ? O11 Ga3 F1 171.59(11) . . ? O12 Ga3 F1 86.36(11) . . ? O14 Ga3 F1 85.43(11) . . ? F2 Ga3 F1 80.58(10) . . ? O13 Ga3 Ga1 130.07(9) . . ? O11 Ga3 Ga1 131.77(9) . . ? O12 Ga3 Ga1 84.78(9) . . ? O14 Ga3 Ga1 83.31(8) . . ? F2 Ga3 Ga1 40.60(7) . . ? F1 Ga3 Ga1 39.99(7) . . ? O16 Ga4 O15 117.79(14) . . ? O16 Ga4 O17 111.43(14) . . ? O15 Ga4 O17 109.74(14) . . ? O16 Ga4 O18 100.77(13) . . ? O15 Ga4 O18 108.50(14) . . ? O17 Ga4 O18 107.82(15) . . ? O19 Ga5 O20 103.85(13) . . ? O19 Ga5 O22 111.69(14) . . ? O20 Ga5 O22 109.53(14) . . ? O19 Ga5 O21 107.52(14) . . ? O20 Ga5 O21 113.79(13) . . ? O22 Ga5 O21 110.31(14) . . ? O26 Ga6 O24 115.53(15) . . ? O26 Ga6 O25 110.08(15) . . ? O24 Ga6 O25 110.50(14) . . ? O26 Ga6 O23 104.36(15) . . ? O24 Ga6 O23 114.09(14) . . ? O25 Ga6 O23 101.21(13) . . ? O4 P7 O14 116.73(16) . . ? O4 P7 O25 110.10(17) . 2_566 ? O14 P7 O25 105.04(17) . 2_566 ? O4 P7 O15 107.87(17) . . ? O14 P7 O15 108.81(17) . . ? O25 P7 O15 107.99(17) 2_566 . ? O5 P8 O16 114.21(17) . . ? O5 P8 O22 109.05(18) . 1_655 ? O16 P8 O22 104.97(16) . 1_655 ? O5 P8 O24 110.46(18) . 1_655 ? O16 P8 O24 108.83(17) . 1_655 ? O22 P8 O24 109.09(19) 1_655 1_655 ? O12 P9 O3 115.86(16) . . ? O12 P9 O8 108.89(17) . 2_575 ? O3 P9 O8 108.94(16) . 2_575 ? O12 P9 O20 110.12(16) . 2_575 ? O3 P9 O20 104.68(16) . 2_575 ? O8 P9 O20 108.07(16) 2_575 2_575 ? O6 P10 O26 113.06(18) . 1_655 ? O6 P10 O10 106.55(18) . 1_645 ? O26 P10 O10 106.1(2) 1_655 1_645 ? O6 P10 O17 109.92(17) . 2_666 ? O26 P10 O17 110.86(18) 1_655 2_666 ? O10 P10 O17 110.22(18) 1_645 2_666 ? O11 P11 O19 111.53(17) . . ? O11 P11 O18 109.55(17) . 2_576 ? O19 P11 O18 109.26(18) . 2_576 ? O11 P11 O7 110.81(16) . . ? O19 P11 O7 106.81(16) . . ? O18 P11 O7 108.81(17) 2_576 . ? O13 P12 O9 113.95(17) . 2_575 ? O13 P12 O23 109.36(17) . . ? O9 P12 O23 105.15(16) 2_575 . ? O13 P12 O21 110.03(16) . . ? O9 P12 O21 109.47(17) 2_575 . ? O23 P12 O21 108.67(17) . . ? Ga1 F1 Ga3 99.69(11) . . ? Ga3 F2 Ga1 99.11(11) . . ? P9 O3 Ga1 127.65(17) . . ? P7 O4 Ga1 126.81(17) . . ? P8 O5 Ga1 137.20(18) . . ? P10 O6 Ga1 146.6(2) . . ? P11 O7 Ga2 124.63(18) . . ? P9 O8 Ga2 128.79(17) 2_575 . ? P12 O9 Ga2 147.85(19) 2_575 . ? P10 O10 Ga2 139.1(2) 1_465 . ? P11 O11 Ga3 132.10(18) . . ? P9 O12 Ga3 126.49(16) . . ? P12 O13 Ga3 139.58(18) . . ? P7 O14 Ga3 127.80(17) . . ? P7 O15 Ga4 124.15(17) . . ? P8 O16 Ga4 147.30(19) . . ? P10 O17 Ga4 137.0(2) 2_666 . ? P11 O18 Ga4 130.67(19) 2_576 . ? P11 O19 Ga5 152.6(2) . . ? P9 O20 Ga5 125.28(18) 2_575 . ? P12 O21 Ga5 124.56(18) . . ? P8 O22 Ga5 129.79(19) 1_455 . ? P12 O23 Ga6 132.43(18) . . ? P8 O24 Ga6 132.3(2) 1_455 . ? P7 O25 Ga6 131.95(19) 2_566 . ? P10 O26 Ga6 153.7(2) 1_455 . ? N1 C1 C2 120.1(6) . . ? C1 N1 C5 119.1(6) . . ? C4 C5 N1 119.2(6) . . ? C3 C2 C1 117.2(6) . . ? C3 C4 C5 121.9(7) . . ? C4 C3 C2 122.4(6) . . ? C8 C7 C6 116.3(7) . . ? C8 C9 C10 123.4(8) . . ? N2 C6 C7 119.3(7) . . ? C9 C8 C7 122.8(7) . . ? C6 N2 C10 117.7(7) . . ? C9 C10 N2 120.1(8) . . ? #===END data_[pyr,F]-GaPO-2 _database_code_CSD 156915 _audit_creation_date 1999-09-14T10:05:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H14 F2 Ga6 N2 O25 P6' _chemical_formula_weight 1204.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.265(5) _cell_length_b 9.397(8) _cell_length_c 9.238(5) _cell_angle_alpha 94.36(6) _cell_angle_beta 90.64(5) _cell_angle_gamma 103.67(5) _cell_volume 778.9(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_diffrn 2.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 582 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.538 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 2730 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2730 _reflns_number_gt 2518 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2730 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.015 _refine_diff_density_max 0.548 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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' 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 0.13908(4) 0.08599(4) 0.43565(4) 0.01163(12) Uani 1 1 d . . . Ga2 Ga 0.60890(4) 0.34138(4) 0.39230(4) 0.01249(13) Uani 1 1 d . . . Ga3 Ga 0.62500(4) -0.07859(4) 0.15717(4) 0.01277(13) Uani 1 1 d . . . P4 P 0.37722(10) 0.09021(10) 0.18526(10) 0.0118(2) Uani 1 1 d . . . P5 P 0.37956(10) 0.32951(10) 0.62664(10) 0.0116(2) Uani 1 1 d . . . P6 P 0.83224(10) 0.14986(10) 0.35659(10) 0.0131(2) Uani 1 1 d . . . F1 F -0.0201(2) -0.0906(2) 0.3875(2) 0.0157(4) Uani 1 1 d . . . O1 O 0.4394(3) -0.0469(3) 0.1776(4) 0.0296(7) Uani 1 1 d . . . O2 O 0.2712(3) 0.2667(3) 0.5023(3) 0.0180(6) Uani 1 1 d . . . O3 O 0.5396(3) 0.3462(3) 0.5747(3) 0.0225(6) Uani 1 1 d . . . O4 O 0.7686(3) 0.0884(3) 0.2025(3) 0.0196(6) Uani 1 1 d . . . O5 O 0.7891(3) 0.2975(3) 0.3915(3) 0.0189(6) Uani 1 1 d . . . O6 O 0.2367(3) -0.0403(3) 0.5361(3) 0.0179(6) Uani 1 1 d . . . O7 O 0.2276(3) 0.0597(3) 0.2551(3) 0.0190(6) Uani 1 1 d . . . O8 O 0.6427(3) -0.2405(3) 0.2413(3) 0.0194(6) Uani 1 1 d . . . O9 O 0.0016(3) 0.1882(3) 0.3533(3) 0.0163(6) Uani 1 1 d . . . O10 O 0.4877(3) 0.2185(4) 0.2622(4) 0.0350(8) Uani 1 1 d . . . O11 O 0.3589(4) 0.4812(3) 0.6819(3) 0.0238(6) Uani 1 1 d . . . O12 O 0.3543(4) 0.1329(4) 0.0320(3) 0.0320(7) Uani 1 1 d . . . C1 C 0.8795(9) 0.5342(14) 0.7574(11) 0.089(3) Uani 1 1 d . . . H1 H 0.9137 0.6047 0.6924 0.107 Uiso 1 1 calc R . . C2 C 0.9200(11) 0.4161(17) 0.7428(10) 0.106(4) Uani 1 1 d . . . H2 H 0.9758 0.3988 0.6631 0.127 Uiso 1 1 calc R . . C3 C 0.8862(11) 0.3151(9) 0.8369(16) 0.097(3) Uani 1 1 d . . . H3 H 0.9195 0.2291 0.8242 0.116 Uiso 1 1 calc R . . N1 N 0.7559(9) 0.4692(12) 0.9607(9) 0.118(3) Uani 1 1 d . . . H1A H 0.7028 0.4911 1.0309 0.141 Uiso 1 1 calc R . . C5 C 0.8011(11) 0.5605(10) 0.8485(14) 0.098(3) Uani 1 1 d . . . H5 H 0.7671 0.6459 0.8464 0.117 Uiso 1 1 calc R . . C4 C 0.8060(13) 0.3366(10) 0.9475(11) 0.100(4) Uani 1 1 d . . . H4 H 0.7821 0.2677 1.0159 0.119 Uiso 1 1 calc R . . O21 O -0.0181(12) -0.0896(12) 0.0258(11) 0.079(3) Uani 0.5 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 0.0091(2) 0.0131(2) 0.0135(2) 0.00366(16) 0.00424(15) 0.00323(15) Ga2 0.0120(2) 0.0108(2) 0.0157(2) 0.00083(16) 0.00277(16) 0.00451(16) Ga3 0.0145(2) 0.0122(2) 0.0131(2) 0.00380(16) 0.00349(16) 0.00529(16) P4 0.0118(5) 0.0136(4) 0.0105(4) 0.0000(4) 0.0041(3) 0.0039(4) P5 0.0140(5) 0.0102(4) 0.0115(4) 0.0021(3) 0.0038(3) 0.0042(4) P6 0.0105(5) 0.0129(4) 0.0175(5) 0.0044(4) 0.0035(3) 0.0047(4) F1 0.0152(11) 0.0167(11) 0.0152(11) 0.0012(9) 0.0046(8) 0.0036(9) O1 0.0187(15) 0.0204(15) 0.053(2) 0.0083(14) 0.0102(14) 0.0095(12) O2 0.0153(14) 0.0182(13) 0.0181(14) 0.0042(11) -0.0017(11) -0.0019(11) O3 0.0152(14) 0.0386(17) 0.0148(14) 0.0040(12) 0.0036(11) 0.0079(12) O4 0.0172(14) 0.0205(14) 0.0195(14) 0.0046(11) -0.0005(11) 0.0001(11) O5 0.0126(13) 0.0125(13) 0.0329(16) 0.0013(11) 0.0029(11) 0.0059(10) O6 0.0134(13) 0.0195(13) 0.0234(14) 0.0113(11) 0.0062(11) 0.0060(11) O7 0.0132(14) 0.0259(14) 0.0188(14) 0.0021(11) 0.0069(11) 0.0058(11) O8 0.0283(16) 0.0157(13) 0.0161(14) 0.0061(11) 0.0059(11) 0.0074(11) O9 0.0093(13) 0.0172(13) 0.0244(14) 0.0083(11) 0.0028(10) 0.0047(10) O10 0.0177(16) 0.0385(19) 0.0418(19) -0.0214(15) -0.0004(14) 0.0009(14) O11 0.0413(18) 0.0130(13) 0.0193(15) 0.0011(11) 0.0059(13) 0.0106(13) O12 0.048(2) 0.0392(18) 0.0125(14) 0.0089(13) 0.0093(13) 0.0150(16) C1 0.048(5) 0.141(9) 0.085(6) 0.077(7) 0.013(4) 0.014(5) C2 0.064(6) 0.169(11) 0.061(5) -0.041(7) 0.015(4) -0.007(7) C3 0.084(7) 0.045(4) 0.153(10) -0.036(6) -0.009(7) 0.014(4) N1 0.097(6) 0.163(9) 0.078(5) -0.024(6) 0.033(5) 0.008(6) C5 0.077(6) 0.077(6) 0.155(10) 0.055(6) 0.005(7) 0.035(5) C4 0.124(9) 0.058(5) 0.091(7) 0.045(5) -0.030(6) -0.040(5) O21 0.063(6) 0.105(8) 0.072(7) -0.003(6) 0.001(5) 0.032(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 O7 1.892(3) . ? Ga1 O2 1.898(3) . ? Ga1 O6 1.935(3) . ? Ga1 O9 1.947(3) . ? Ga1 F1 1.960(3) . ? Ga1 F1 1.985(2) 2_556 ? Ga1 Ga1 3.010(2) 2_556 ? Ga2 O10 1.785(3) . ? Ga2 O5 1.811(3) . ? Ga2 O3 1.811(3) . ? Ga2 O11 1.811(3) 2_666 ? Ga3 O8 1.800(3) . ? Ga3 O12 1.808(3) 2_655 ? Ga3 O4 1.819(3) . ? Ga3 O1 1.823(3) . ? P4 O7 1.510(3) . ? P4 O10 1.509(3) . ? P4 O12 1.527(3) . ? P4 O1 1.528(3) . ? P5 O2 1.505(3) . ? P5 O8 1.520(3) 2_656 ? P5 O11 1.533(3) . ? P5 O3 1.540(3) . ? P6 O6 1.519(3) 2_656 ? P6 O9 1.526(3) 1_655 ? P6 O5 1.545(3) . ? P6 O4 1.550(3) . ? F1 Ga1 1.985(2) 2_556 ? O6 P6 1.519(3) 2_656 ? O8 P5 1.520(3) 2_656 ? O9 P6 1.526(3) 1_455 ? O11 Ga2 1.811(3) 2_666 ? O12 Ga3 1.808(3) 2_655 ? C1 C5 1.168(13) . ? C1 C2 1.252(14) . ? C2 C3 1.321(15) . ? C3 C4 1.302(14) . ? N1 C5 1.400(13) . ? N1 C4 1.427(13) . ? O21 O21 1.74(2) 2 ? 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 O7 Ga1 O2 97.29(13) . . ? O7 Ga1 O6 95.55(13) . . ? O2 Ga1 O6 96.88(13) . . ? O7 Ga1 O9 92.84(12) . . ? O2 Ga1 O9 91.40(13) . . ? O6 Ga1 O9 167.36(11) . . ? O7 Ga1 F1 90.99(12) . . ? O2 Ga1 F1 170.88(10) . . ? O6 Ga1 F1 86.06(12) . . ? O9 Ga1 F1 84.35(12) . . ? O7 Ga1 F1 171.35(10) . 2_556 ? O2 Ga1 F1 91.05(12) . 2_556 ? O6 Ga1 F1 85.70(11) . 2_556 ? O9 Ga1 F1 84.62(11) . 2_556 ? F1 Ga1 F1 80.54(11) . 2_556 ? O7 Ga1 Ga1 131.54(10) . 2_556 ? O2 Ga1 Ga1 130.92(9) . 2_556 ? O6 Ga1 Ga1 84.59(10) . 2_556 ? O9 Ga1 Ga1 82.76(9) . 2_556 ? F1 Ga1 Ga1 40.57(7) . 2_556 ? F1 Ga1 Ga1 39.96(7) 2_556 2_556 ? O10 Ga2 O5 109.13(14) . . ? O10 Ga2 O3 114.80(15) . . ? O5 Ga2 O3 110.74(13) . . ? O10 Ga2 O11 104.78(17) . 2_666 ? O5 Ga2 O11 104.47(14) . 2_666 ? O3 Ga2 O11 112.27(14) . 2_666 ? O8 Ga3 O12 101.19(15) . 2_655 ? O8 Ga3 O4 116.91(14) . . ? O12 Ga3 O4 106.57(15) 2_655 . ? O8 Ga3 O1 111.45(14) . . ? O12 Ga3 O1 108.04(16) 2_655 . ? O4 Ga3 O1 111.68(14) . . ? O7 P4 O10 112.76(17) . . ? O7 P4 O12 107.36(18) . . ? O10 P4 O12 106.4(2) . . ? O7 P4 O1 110.32(17) . . ? O10 P4 O1 110.15(19) . . ? O12 P4 O1 109.70(19) . . ? O2 P5 O8 114.12(17) . 2_656 ? O2 P5 O11 109.55(17) . . ? O8 P5 O11 104.80(16) 2_656 . ? O2 P5 O3 109.68(16) . . ? O8 P5 O3 109.67(17) 2_656 . ? O11 P5 O3 108.82(18) . . ? O6 P6 O9 115.96(16) 2_656 1_655 ? O6 P6 O5 110.27(17) 2_656 . ? O9 P6 O5 105.48(16) 1_655 . ? O6 P6 O4 108.37(16) 2_656 . ? O9 P6 O4 108.81(16) 1_655 . ? O5 P6 O4 107.65(17) . . ? Ga1 F1 Ga1 99.46(11) . 2_556 ? P4 O1 Ga3 133.99(19) . . ? P5 O2 Ga1 139.28(18) . . ? P5 O3 Ga2 130.05(18) . . ? P6 O4 Ga3 126.44(18) . . ? P6 O5 Ga2 130.66(17) . . ? P6 O6 Ga1 126.85(17) 2_656 . ? P4 O7 Ga1 141.12(18) . . ? P5 O8 Ga3 148.60(18) 2_656 . ? P6 O9 Ga1 128.27(16) 1_455 . ? P4 O10 Ga2 165.0(3) . . ? P5 O11 Ga2 134.64(18) . 2_666 ? P4 O12 Ga3 142.2(2) . 2_655 ? C5 C1 C2 123.4(9) . . ? C1 C2 C3 122.2(9) . . ? C4 C3 C2 119.5(9) . . ? C5 N1 C4 113.7(8) . . ? C1 C5 N1 122.9(9) . . ? C3 C4 N1 117.9(8) . . ? #===END data_[pyr,F]-GaPO-3 _database_code_CSD 156916 _audit_creation_date 1999-08-11T09:58:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H13 F2 Ga4 N2 O17 P4' _chemical_formula_weight 873.95 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.157(3) _cell_length_b 14.202(3) _cell_length_c 13.065(5) _cell_angle_alpha 90 _cell_angle_beta 91.848(2) _cell_angle_gamma 90 _cell_volume 2254.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.12 _exptl_absorpt_correction_T_min 0.9045 _exptl_absorpt_correction_T_max 0.9045 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 3964 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 3964 _reflns_number_gt 3079 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3964 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.116 _refine_ls_shift/su_mean 0.007 _refine_diff_density_max 1.35 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.219 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' O O 0.0106 0.006 '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' 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' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.11264(7) 0.77351(6) 0.38530(6) 0.0109(2) Uani 1 1 d . . . Ga2 Ga 0.35502(7) 0.62105(6) 0.26319(6) 0.0109(2) Uani 1 1 d . . . Ga3 Ga -0.03735(7) 0.73407(6) 0.15808(6) 0.0114(2) Uani 1 1 d . . . Ga4 Ga 0.36466(7) 0.86522(6) 0.20668(6) 0.0112(2) Uani 1 1 d . . . P1 P 0.10976(17) 0.57910(13) 0.27150(15) 0.0113(4) Uani 1 1 d . . . P2 P 0.12192(17) 0.90733(13) 0.19360(15) 0.0113(4) Uani 1 1 d . . . P3 P 0.37279(17) 0.78009(13) 0.42586(15) 0.0110(4) Uani 1 1 d . . . P4 P 0.51615(17) 0.70903(14) 0.11160(15) 0.0127(4) Uani 1 1 d . . . F1 F -0.0269(4) 0.7632(3) 0.3060(3) 0.0131(9) Uani 1 1 d . . . F2 F 0.2863(4) 0.7407(3) 0.2230(3) 0.0149(10) Uani 1 1 d . . . O1 O 0.1369(4) 0.8811(3) 0.3083(4) 0.0133(12) Uani 1 1 d . . . O2 O 0.2338(4) 0.9020(4) 0.1426(4) 0.0142(12) Uani 1 1 d . . . O3 O 0.4441(5) 0.6307(4) 0.1513(4) 0.0187(13) Uani 1 1 d . . . O4 O 0.0313(5) 0.6211(3) 0.1887(4) 0.0157(12) Uani 1 1 d . . . O5 O -0.1816(5) 0.7609(4) 0.1689(4) 0.0151(12) Uiso 1 1 d . . . H5' H -0.2157 0.7122 0.1794 0.023 Uiso 1 1 calc R . . O6 O 0.4350(4) 0.9845(3) 0.1939(4) 0.0136(12) Uani 1 1 d . . . O7 O 0.1255(4) 0.6445(4) 0.3644(4) 0.0161(12) Uani 1 1 d . . . O8 O 0.2537(5) 0.7808(4) 0.4544(4) 0.0146(12) Uani 1 1 d . . . O9 O 0.2223(4) 0.5633(4) 0.2235(4) 0.0140(12) Uani 1 1 d . . . O10 O 0.0414(5) 0.8435(4) 0.1348(4) 0.0160(12) Uani 1 1 d . . . O11 O 0.3968(5) 0.8577(4) 0.3461(4) 0.0171(12) Uani 1 1 d . . . O12 O 0.4488(4) 0.8009(4) 0.5181(4) 0.0151(12) Uani 1 1 d . . . O13 O 0.5341(5) 0.6926(4) -0.0013(4) 0.0169(12) Uani 1 1 d . . . O14 O 0.4061(5) 0.6823(4) 0.3820(4) 0.0162(12) Uani 1 1 d . . . O15 O 0.0773(5) 1.0080(4) 0.1840(4) 0.0155(12) Uani 1 1 d . . . O16 O 0.4685(5) 0.8066(4) 0.1270(5) 0.0266(15) Uani 1 1 d . . . O17 O 0.6254(5) 0.6981(5) 0.1765(5) 0.0382(17) Uani 1 1 d . . . H17 H 0.6699 0.7376 0.1585 0.057 Uiso 1 1 calc R . . C9 C 0.1551(14) 0.5417(12) -0.0242(14) 0.076(5) Uani 1 1 d . . . H9 H 0.0949 0.541 0.018 0.092 Uiso 1 1 calc R . . C5 C -0.1578(11) 0.5728(19) 0.4253(10) 0.094(8) Uani 1 1 d . . . H5 H -0.0813 0.5758 0.4282 0.112 Uiso 1 1 calc R . . C4 C -0.2167(16) 0.6456(14) 0.4086(10) 0.082(6) Uani 1 1 d . . . H4 H -0.1822 0.7032 0.3986 0.099 Uiso 1 1 calc R . . C8 C 0.2409(16) 0.5124(9) 0.0073(9) 0.054(4) Uani 1 1 d . . . H8 H 0.239 0.4872 0.0729 0.065 Uiso 1 1 calc R . . C10 C 0.3410(11) 0.5374(10) -0.1152(15) 0.064(4) Uani 1 1 d . . . H10 H 0.4104 0.5346 -0.1428 0.077 Uiso 1 1 calc R . . N1 N -0.219(3) 0.4810(14) 0.4403(9) 0.171(12) Uani 1 1 d . . . H21 H -0.1875 0.4275 0.4519 0.205 Uiso 1 1 calc R . . C7 C 0.3293(19) 0.5091(9) -0.0296(16) 0.092(7) Uani 1 1 d . . . H7A H 0.3891 0.4848 0.0079 0.111 Uiso 1 1 calc R . . N18 N 0.250(2) 0.5756(8) -0.1768(8) 0.130(9) Uani 1 1 d . . . H18 H 0.2564 0.5956 -0.2385 0.156 Uiso 1 1 calc R . . C6 C 0.1430(15) 0.5761(10) -0.1198(16) 0.088(6) Uani 1 1 d . . . H6 H 0.0765 0.5977 -0.148 0.106 Uiso 1 1 calc R . . C2 C -0.3729(9) 0.5773(10) 0.4162(8) 0.044(3) Uani 1 1 d . . . H2 H -0.4488 0.5857 0.413 0.053 Uiso 1 1 calc R . . C3 C -0.3191(14) 0.6420(11) 0.4051(10) 0.067(4) Uani 1 1 d . . . H3 H -0.3557 0.6984 0.3921 0.08 Uiso 1 1 calc R . . C1 C -0.3374(19) 0.4960(13) 0.4323(10) 0.096(7) Uani 1 1 d . . . H1 H -0.3858 0.4458 0.439 0.115 Uiso 1 1 calc R . . 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 0.0114(5) 0.0118(4) 0.0094(4) -0.0003(3) 0.0018(3) -0.0004(3) Ga2 0.0107(5) 0.0109(4) 0.0112(4) 0.0001(3) 0.0026(3) -0.0003(3) Ga3 0.0102(5) 0.0127(4) 0.0113(5) -0.0003(3) -0.0001(3) -0.0006(3) Ga4 0.0117(5) 0.0113(4) 0.0107(4) 0.0007(3) 0.0020(3) 0.0001(3) P1 0.0129(11) 0.0097(9) 0.0113(10) 0.0009(8) 0.0002(8) -0.0002(8) P2 0.0117(11) 0.0096(9) 0.0129(10) 0.0002(8) 0.0025(8) 0.0005(8) P3 0.0118(11) 0.0126(10) 0.0085(9) 0.0000(8) -0.0019(8) 0.0008(8) P4 0.0105(10) 0.0170(10) 0.0107(10) 0.0001(8) 0.0037(8) 0.0003(8) F1 0.009(2) 0.018(2) 0.013(2) 0.0000(18) 0.0013(17) 0.0007(18) F2 0.017(2) 0.013(2) 0.014(2) 0.0043(18) -0.0001(19) -0.0007(19) O1 0.015(3) 0.009(3) 0.015(3) 0.003(2) 0.002(2) 0.001(2) O2 0.010(3) 0.017(3) 0.016(3) 0.007(2) 0.001(2) 0.003(2) O3 0.020(3) 0.019(3) 0.017(3) 0.006(2) 0.004(2) 0.006(2) O4 0.019(3) 0.013(3) 0.014(3) 0.002(2) -0.005(2) 0.003(2) O6 0.011(3) 0.011(3) 0.020(3) 0.001(2) 0.008(2) 0.001(2) O7 0.016(3) 0.013(3) 0.019(3) 0.001(2) -0.004(2) 0.000(2) O8 0.014(3) 0.019(3) 0.011(3) -0.002(2) -0.003(2) -0.003(2) O9 0.014(3) 0.016(3) 0.012(3) -0.002(2) -0.001(2) -0.002(2) O10 0.021(3) 0.014(3) 0.013(3) 0.000(2) 0.000(2) -0.004(2) O11 0.022(3) 0.014(3) 0.015(3) -0.001(2) 0.000(2) -0.008(2) O12 0.015(3) 0.017(3) 0.013(3) 0.000(2) -0.002(2) 0.000(2) O13 0.022(3) 0.019(3) 0.010(3) 0.001(2) 0.009(2) 0.000(2) O14 0.024(3) 0.011(3) 0.015(3) 0.002(2) 0.000(2) 0.007(2) O15 0.015(3) 0.013(3) 0.018(3) 0.000(2) -0.004(2) -0.001(2) O16 0.032(4) 0.015(3) 0.034(4) 0.002(3) 0.024(3) -0.001(3) O17 0.021(4) 0.063(5) 0.030(4) 0.005(3) -0.005(3) -0.014(3) C9 0.054(10) 0.089(12) 0.088(13) -0.034(10) 0.040(9) -0.013(9) C5 0.021(7) 0.23(2) 0.032(8) -0.061(12) -0.007(6) 0.030(11) C4 0.090(13) 0.124(15) 0.035(7) 0.001(8) 0.025(9) -0.063(12) C8 0.098(13) 0.039(7) 0.026(6) -0.002(5) 0.025(8) -0.017(8) C10 0.033(7) 0.059(9) 0.100(13) -0.015(9) -0.003(8) 0.001(6) N1 0.36(3) 0.120(14) 0.025(6) -0.039(8) -0.053(13) 0.168(18) C7 0.15(2) 0.025(7) 0.099(15) -0.005(8) -0.065(14) 0.002(9) N18 0.32(3) 0.042(7) 0.024(6) 0.005(5) 0.010(11) -0.049(12) C6 0.097(13) 0.048(8) 0.113(14) -0.033(9) -0.082(11) 0.039(9) C2 0.030(6) 0.076(9) 0.027(6) 0.018(6) -0.007(5) -0.026(6) C3 0.091(12) 0.072(10) 0.037(7) 0.017(7) 0.007(8) 0.032(10) C1 0.17(2) 0.081(12) 0.032(7) -0.009(8) 0.003(10) -0.093(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 O13 1.851(5) 4_576 ? Ga1 O1 1.858(5) . ? Ga1 O7 1.860(5) . ? Ga1 O8 1.915(6) . ? Ga1 F1 1.965(5) . ? Ga2 O3 1.852(5) . ? Ga2 O14 1.868(5) . ? Ga2 O9 1.869(5) . ? Ga2 O15 1.923(5) 2_545 ? Ga2 F2 1.957(4) . ? Ga3 O5 1.804(6) . ? Ga3 O4 1.846(5) . ? Ga3 O10 1.855(5) . ? Ga3 O12 1.898(5) 4_575 ? Ga3 F1 1.976(4) . ? Ga4 O2 1.849(5) . ? Ga4 O11 1.854(5) . ? Ga4 O16 1.859(6) . ? Ga4 O6 1.908(5) . ? Ga4 F2 2.023(4) . ? P1 O6 1.523(5) 2_545 ? P1 O7 1.535(6) . ? P1 O4 1.540(6) . ? P1 O9 1.540(6) . ? P2 O10 1.524(6) . ? P2 O15 1.533(5) . ? P2 O2 1.536(5) . ? P2 O1 1.549(5) . ? P3 O8 1.507(6) . ? P3 O12 1.523(6) . ? P3 O11 1.552(6) . ? P3 O14 1.561(5) . ? P4 O13 1.516(5) . ? P4 O3 1.517(6) . ? P4 O16 1.517(6) . ? P4 O17 1.561(7) . ? O6 P1 1.523(5) 2 ? O12 Ga3 1.898(5) 4_676 ? O13 Ga1 1.851(5) 4_675 ? O15 Ga2 1.923(5) 2 ? C9 C8 1.19(2) . ? C9 C6 1.34(2) . ? C5 C4 1.27(2) . ? C5 N1 1.52(3) . ? C4 C3 1.25(2) . ? C8 C7 1.19(2) . ? C10 C7 1.20(2) . ? C10 N18 1.45(2) . ? N1 C1 1.46(3) . ? N18 C6 1.52(2) . ? C2 C3 1.141(19) . ? C2 C1 1.25(2) . ? 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 O13 Ga1 O1 108.4(2) 4_576 . ? O13 Ga1 O7 114.9(2) 4_576 . ? O1 Ga1 O7 135.6(2) . . ? O13 Ga1 O8 94.9(2) 4_576 . ? O1 Ga1 O8 93.2(2) . . ? O7 Ga1 O8 92.5(2) . . ? O13 Ga1 F1 89.0(2) 4_576 . ? O1 Ga1 F1 85.7(2) . . ? O7 Ga1 F1 85.7(2) . . ? O8 Ga1 F1 176.1(2) . . ? O3 Ga2 O14 115.7(3) . . ? O3 Ga2 O9 109.6(2) . . ? O14 Ga2 O9 134.1(2) . . ? O3 Ga2 O15 95.2(2) . 2_545 ? O14 Ga2 O15 87.9(2) . 2_545 ? O9 Ga2 O15 95.1(2) . 2_545 ? O3 Ga2 F2 88.8(2) . . ? O14 Ga2 F2 86.9(2) . . ? O9 Ga2 F2 87.1(2) . . ? O15 Ga2 F2 174.5(2) 2_545 . ? O5 Ga3 O4 126.9(2) . . ? O5 Ga3 O10 110.1(2) . . ? O4 Ga3 O10 122.1(3) . . ? O5 Ga3 O12 94.3(2) . 4_575 ? O4 Ga3 O12 90.4(2) . 4_575 ? O10 Ga3 O12 95.2(2) . 4_575 ? O5 Ga3 F1 84.9(2) . . ? O4 Ga3 F1 87.5(2) . . ? O10 Ga3 F1 88.2(2) . . ? O12 Ga3 F1 176.6(2) 4_575 . ? O2 Ga4 O11 127.8(2) . . ? O2 Ga4 O16 117.6(3) . . ? O11 Ga4 O16 113.5(3) . . ? O2 Ga4 O6 95.2(2) . . ? O11 Ga4 O6 93.2(2) . . ? O16 Ga4 O6 92.0(2) . . ? O2 Ga4 F2 83.9(2) . . ? O11 Ga4 F2 86.1(2) . . ? O16 Ga4 F2 89.9(2) . . ? O6 Ga4 F2 178.15(19) . . ? O6 P1 O7 109.6(3) 2_545 . ? O6 P1 O4 109.3(3) 2_545 . ? O7 P1 O4 112.3(3) . . ? O6 P1 O9 108.8(3) 2_545 . ? O7 P1 O9 108.7(3) . . ? O4 P1 O9 108.0(3) . . ? O10 P2 O15 107.1(3) . . ? O10 P2 O2 108.4(3) . . ? O15 P2 O2 109.1(3) . . ? O10 P2 O1 113.5(3) . . ? O15 P2 O1 109.5(3) . . ? O2 P2 O1 109.3(3) . . ? O8 P3 O12 111.5(3) . . ? O8 P3 O11 111.4(3) . . ? O12 P3 O11 105.7(3) . . ? O8 P3 O14 111.1(3) . . ? O12 P3 O14 107.8(3) . . ? O11 P3 O14 109.2(3) . . ? O13 P4 O3 108.8(3) . . ? O13 P4 O16 109.7(3) . . ? O3 P4 O16 113.4(3) . . ? O13 P4 O17 111.5(4) . . ? O3 P4 O17 103.4(4) . . ? O16 P4 O17 109.9(4) . . ? Ga1 F1 Ga3 123.9(2) . . ? Ga2 F2 Ga4 126.1(2) . . ? P2 O1 Ga1 134.9(3) . . ? P2 O2 Ga4 125.3(3) . . ? P4 O3 Ga2 133.1(4) . . ? P1 O4 Ga3 139.0(3) . . ? P1 O6 Ga4 126.3(3) 2 . ? P1 O7 Ga1 134.6(3) . . ? P3 O8 Ga1 137.4(3) . . ? P1 O9 Ga2 126.4(3) . . ? P2 O10 Ga3 137.9(3) . . ? P3 O11 Ga4 131.5(3) . . ? P3 O12 Ga3 138.1(3) . 4_676 ? P4 O13 Ga1 146.4(4) . 4_675 ? P3 O14 Ga2 129.5(3) . . ? P2 O15 Ga2 127.1(3) . 2 ? P4 O16 Ga4 138.8(3) . . ? C8 C9 C6 121.2(15) . . ? C4 C5 N1 116.6(14) . . ? C3 C4 C5 122.0(17) . . ? C9 C8 C7 131.9(16) . . ? C7 C10 N18 122.1(17) . . ? C1 N1 C5 110.5(11) . . ? C8 C7 C10 119.9(18) . . ? C10 N18 C6 112.2(11) . . ? C9 C6 N18 112.5(13) . . ? C3 C2 C1 124.8(15) . . ? C2 C3 C4 127.3(17) . . ? C2 C1 N1 118.9(14) . . ? #===END data_[pyr,O]-GaPO-4 _database_code_CSD 155357 _audit_creation_date 2001-01-16T09:29:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C20 H40 F0 Ga8 N4 O42 P8' _chemical_formula_weight 1814.08 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z' '-x, y, -z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 13.016(3) _cell_length_b 13.016(3) _cell_length_c 7.356(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1246.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 2.417 _exptl_crystal_F_000 892 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.333 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 562 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.8 _diffrn_reflns_theta_max 60.14 _reflns_number_total 302 _reflns_number_gt 265 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1584P)^2^+1.7040P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 302 _refine_ls_number_parameters 59 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.079 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_gt 0.1838 _refine_ls_wR_factor_all 0.1953 _refine_ls_goodness_of_fit_gt 1.111 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_restrained_S_gt 1.111 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.013 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.5(4) _refine_diff_density_max 0.589 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.173 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O5 O 0.5 0.5 0 0.036(6) Uani 1 d S . Ga1 Ga 0.40764(12) 0.40764(12) 0.1639(4) 0.0537(12) Uani 1 d S . P1 P 0.3704(3) 0.3704(3) 0.7627(8) 0.078(3) Uani 1 d S . O1 O 0.3482(11) 0.3482(11) 0.962(2) 0.121(10) Uani 1 d S . O2 O 0.4859(15) 0.3482(12) 0.729(2) 0.105(6) Uani 1 d . . O3 O 0.3056(9) 0.3056(9) 0.645(3) 0.131(12) Uani 1 d S . O4 O 0.3174(9) 0.3174(9) 0.309(2) 0.128(12) Uani 1 d S . C1 C 0.4511(17) 0.0895(16) 1.004(4) 0.101(8) Uani 1 d . . H1 H 0.4153(17) 0.1512(16) 1.012(4) 0.18(13) Uiso 1 calc R . C2 C 0.5 0.100(3) 0.5 0.120(13) Uani 1 d S . H2 H 0.5 0.171(3) 0.5 0.14(15) Uiso 1 calc SR . 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 O5 0.037(8) 0.037(8) 0.033(14) 0 0 0 Ga1 0.0659(14) 0.0659(14) 0.0293(14) -0.0002(9) -0.0002(9) -0.0286(13) P1 0.106(4) 0.106(4) 0.023(3) 0.001(2) 0.001(2) -0.071(5) O1 0.172(15) 0.172(15) 0.018(9) 0.008(6) 0.008(6) -0.12(2) O2 0.093(11) 0.120(10) 0.103(12) -0.079(10) 0.015(10) -0.014(11) O3 0.180(19) 0.180(19) 0.033(8) -0.009(7) -0.009(7) -0.15(2) O4 0.181(19) 0.181(19) 0.021(8) 0.004(5) 0.004(5) -0.16(2) C1 0.14(2) 0.093(13) 0.073(13) -0.012(18) -0.01(2) 0.035(16) C2 0.20(5) 0.10(3) 0.054(17) 0 0.00(3) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O5 Ga1 2.084(2) 3_665 ? O5 Ga1 2.084(2) 4_655 ? O5 Ga1 2.084(2) . ? O5 Ga1 2.084(2) 2_565 ? Ga1 O2 1.77(2) 4_656 ? Ga1 O2 1.77(2) 7_566 ? Ga1 O1 1.84(2) 1_554 ? Ga1 O4 1.97(2) . ? P1 O3 1.48(2) . ? P1 O1 1.52(2) . ? P1 O2 1.55(2) . ? P1 O2 1.55(2) 8 ? O1 Ga1 1.84(2) 1_556 ? O2 Ga1 1.77(2) 4_656 ? C1 C1 1.27(4) 4_657 ? C1 C2 1.34(3) 13 ? C2 C1 1.34(3) 15_556 ? C2 C1 1.34(3) 13_554 ? 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 Ga1 O5 Ga1 109.54(7) 3_665 4_655 ? Ga1 O5 Ga1 109.32(14) 3_665 . ? Ga1 O5 Ga1 109.55(7) 4_655 . ? Ga1 O5 Ga1 109.55(7) 3_665 2_565 ? Ga1 O5 Ga1 109.32(14) 4_655 2_565 ? Ga1 O5 Ga1 109.54(7) . 2_565 ? O2 Ga1 O2 119.1(13) 4_656 7_566 ? O2 Ga1 O1 120.1(6) 4_656 1_554 ? O2 Ga1 O1 120.1(6) 7_566 1_554 ? O2 Ga1 O4 88.0(6) 4_656 . ? O2 Ga1 O4 88.0(6) 7_566 . ? O1 Ga1 O4 86.3(8) 1_554 . ? O2 Ga1 O5 93.3(5) 4_656 . ? O2 Ga1 O5 93.3(5) 7_566 . ? O1 Ga1 O5 91.1(6) 1_554 . ? O4 Ga1 O5 177.4(5) . . ? O3 P1 O1 110.4(11) . . ? O3 P1 O2 110.8(7) . . ? O1 P1 O2 107.5(8) . . ? O3 P1 O2 110.8(7) . 8 ? O1 P1 O2 107.5(8) . 8 ? O2 P1 O2 109.7(14) . 8 ? P1 O1 Ga1 128.0(13) . 1_556 ? P1 O2 Ga1 127.3(9) . 4_656 ? C1 C1 C2 119.5(19) 4_657 13 ? C1 C2 C1 121(4) 15_556 13_554 ?