#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000491.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_4000491 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm048820o _journal_year 2004 _chemical_formula_sum 'C3.25 H2.75 F Ga2.5 N1.5 O11 P2' _chemical_formula_weight 494.06 _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_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 111.9300(10) _cell_angle_beta 103.6550(10) _cell_angle_gamma 101.9030(10) _cell_formula_units_Z 2 _cell_length_a 8.1217(6) _cell_length_b 8.9601(6) _cell_length_c 10.4611(8) _cell_measurement_temperature 293(2) _cell_volume 648.59(8) _diffrn_ambient_temperature 293(2) _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 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4604 _diffrn_reflns_theta_max 29.73 _diffrn_reflns_theta_min 2.24 _exptl_absorpt_coefficient_mu 5.488 _exptl_crystal_density_diffrn 2.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 475 _refine_ls_extinction_coef 0.006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3247 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0598 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1568 _refine_ls_wR_factor_ref 0.1654 _reflns_number_gt 2470 _reflns_number_total 3247 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M P-1 _cod_original_formula_sum 'C3.25 H2.75 F Ga2.50 N1.50 O11 P2' _cod_database_code 4000491 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 0.19859(9) 0.35167(8) 0.36296(7) 0.0116(2) Uani 1 1 d . . . Ga2 Ga 0.72345(9) 0.00093(8) 0.44691(8) 0.0131(2) Uani 1 1 d . . . Ga3 Ga 0.0000 0.0000 0.0000 0.0157(3) Uani 1 2 d S . . P1 P 0.5492(2) 0.2743(2) 0.51644(18) 0.0125(3) Uani 1 1 d . . . P2 P 0.9909(2) -0.0298(2) 0.29119(17) 0.0122(3) Uani 1 1 d . . . F1 F 0.1449(5) 0.2270(5) 0.1580(4) 0.0185(8) Uani 1 1 d . . . O1 O -0.0319(6) 0.4086(6) 0.3139(5) 0.0184(10) Uani 1 1 d . . . O2 O 0.6784(6) 0.4429(6) 0.6417(5) 0.0178(10) Uani 1 1 d . . . O3 O 0.2094(6) 0.4835(6) 0.5703(5) 0.0155(9) Uani 1 1 d . . . O4 O 0.4102(6) 0.2945(6) 0.4065(5) 0.0204(10) Uani 1 1 d . . . O5 O 1.0531(7) 0.1615(6) 0.3744(5) 0.0207(10) Uani 1 1 d . . . O6 O 0.8061(6) -0.0989(6) 0.3001(6) 0.0220(11) Uani 1 1 d . . . O7 O 0.6503(6) 0.1741(6) 0.4280(5) 0.0169(10) Uani 1 1 d . . . O8 O 0.4713(7) 0.1733(6) 0.5912(6) 0.0215(10) Uani 1 1 d . . . O9 O 0.2134(7) -0.0536(6) -0.0038(6) 0.0232(11) Uani 1 1 d . . . O10 O 0.9782(8) -0.1004(6) 0.1321(5) 0.0249(11) Uani 1 1 d . . . O11 O 1.1203(7) -0.1011(6) 0.3666(6) 0.0245(11) Uani 1 1 d . . . C1 C -0.0693(8) 0.4778(8) 0.4255(7) 0.0144(12) Uani 1 1 d . . . N1 N 0.5464(14) 0.1967(13) 0.1374(11) 0.039(2) Uiso 0.75 1 d PD . . C2 C 0.494(3) 0.315(3) 0.068(2) 0.112(8) Uiso 0.75 1 d PD . . C3 C 0.562(3) 0.296(4) -0.060(3) 0.188(16) Uiso 0.75 1 d PD . . C4 C 0.766(3) 0.393(5) -0.002(3) 0.184(15) Uiso 0.75 1 d PD . . N2 N 0.8495(19) 0.3727(18) -0.1126(15) 0.067(4) Uiso 0.75 1 d PD . . 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 0.0087(3) 0.0088(3) 0.0172(4) 0.0058(3) 0.0055(3) 0.0011(2) Ga2 0.0093(3) 0.0101(4) 0.0225(4) 0.0091(3) 0.0076(3) 0.0021(3) Ga3 0.0171(5) 0.0128(5) 0.0153(5) 0.0056(4) 0.0067(4) 0.0008(4) P1 0.0085(7) 0.0094(7) 0.0206(8) 0.0078(6) 0.0067(6) 0.0010(6) P2 0.0113(7) 0.0097(7) 0.0148(8) 0.0052(6) 0.0063(6) 0.0001(6) F1 0.021(2) 0.0139(19) 0.0161(18) 0.0043(15) 0.0082(16) -0.0010(15) O1 0.015(2) 0.021(2) 0.019(2) 0.007(2) 0.0074(19) 0.0077(19) O2 0.017(2) 0.011(2) 0.021(2) 0.0072(19) 0.0053(19) -0.0023(18) O3 0.012(2) 0.015(2) 0.019(2) 0.0052(18) 0.0081(18) 0.0038(17) O4 0.015(2) 0.021(2) 0.027(3) 0.012(2) 0.005(2) 0.0075(19) O5 0.024(3) 0.012(2) 0.022(2) 0.005(2) 0.011(2) -0.0010(19) O6 0.015(2) 0.016(2) 0.029(3) 0.002(2) 0.013(2) 0.0017(19) O7 0.015(2) 0.015(2) 0.031(3) 0.015(2) 0.013(2) 0.0090(18) O8 0.017(2) 0.016(2) 0.031(3) 0.012(2) 0.011(2) -0.0015(19) O9 0.015(2) 0.020(2) 0.030(3) 0.003(2) 0.012(2) 0.007(2) O10 0.040(3) 0.016(2) 0.018(2) 0.009(2) 0.014(2) 0.002(2) O11 0.021(3) 0.026(3) 0.024(3) 0.010(2) 0.002(2) 0.009(2) C1 0.011(3) 0.013(3) 0.021(3) 0.010(3) 0.004(3) 0.003(2)