# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1643 data_pn1030699 #------------------------------------------------------------------------------ _audit_creation_date '1999-09-22' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_contact_author_name ' PROF. COLIN L RASTON ' _publ_contact_author_address ; DEPT. OF CHEMISTRY MONASH UNIVERSITY CLAYTON, MELBOURNE, VICTORIA 3168 AUSTRALIA ; _publ_contact_author_email ' c.raston@sci.monash.edu.au ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 16.3050(3) _cell_length_b 17.6498(3) _cell_length_c 15.9096(2) _cell_angle_alpha 90 _cell_angle_beta 100.7773(11) _cell_angle_gamma 90 _cell_volume 4497.7(1) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 939.13 _chemical_formula_analytical ? _chemical_formula_sum 'C48 H57 Ga3 O6 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1944.00 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; There is 50% disorder about a C2 symmetry axis for C25 and C24 ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Enraf Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 6400 _reflns_number_total 33253 _reflns_number_gt 4917 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga 0 12 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 192 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 228 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 24 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ga(1) -0.09760(4) 0.31866(3) 0.18913(3) 0.0139(2) 1.000 . Uani d ? Ga(2) 0.0000 0.15064(4) 0.2500 0.0144(2) 0.500 ST Uani d ? O(1) -0.0463(2) 0.2253(2) 0.1676(2) 0.017(1) 1.000 . Uani d ? O(2) 0.0000 0.3687(3) 0.2500 0.018(1) 0.500 ST Uani d ? O(3) 0.0620(3) 0.1830(2) 0.4939(2) 0.032(1) 1.000 . Uani d ? O(4) 0.0000 0.5211(3) 0.2500 0.074(2) 0.500 ST Uani d ? C(1) -0.1362(3) 0.3667(3) 0.0752(3) 0.016(1) 1.000 . Uani d ? C(2) -0.0895(4) 0.4189(4) 0.0424(4) 0.054(2) 1.000 . Uani d ? C(3) -0.1140(5) 0.4498(6) -0.0365(5) 0.087(3) 1.000 . Uani d ? C(4) -0.1924(4) 0.4312(5) -0.0844(4) 0.053(2) 1.000 . Uani d ? C(5) -0.2391(4) 0.3801(4) -0.0539(3) 0.029(2) 1.000 . Uani d ? C(6) -0.2093(3) 0.3483(3) 0.0262(3) 0.025(2) 1.000 . Uani d ? C(7) -0.1715(3) 0.3063(3) 0.2736(3) 0.022(2) 1.000 . Uani d ? C(8) -0.2471(4) 0.2678(4) 0.2547(4) 0.036(2) 1.000 . Uani d ? C(9) -0.2986(5) 0.2610(4) 0.3143(6) 0.059(3) 1.000 . Uani d ? C(10) -0.2780(5) 0.2936(6) 0.3933(5) 0.066(3) 1.000 . Uani d ? C(11) -0.2035(6) 0.3340(7) 0.4122(4) 0.086(3) 1.000 . Uani d ? C(12) -0.1504(4) 0.3383(5) 0.3530(4) 0.047(2) 1.000 . Uani d ? C(13) 0.0885(3) 0.0927(3) 0.2111(3) 0.020(1) 1.000 . Uani d ? C(14) 0.1131(4) 0.0234(3) 0.2530(4) 0.029(2) 1.000 . Uani d ? C(15) 0.1753(4) -0.0214(4) 0.2278(5) 0.045(2) 1.000 . Uani d ? C(16) 0.2132(4) 0.0006(4) 0.1633(5) 0.042(2) 1.000 . Uani d ? C(17) 0.1912(4) 0.0686(4) 0.1206(4) 0.044(2) 1.000 . Uani d ? C(18) 0.1289(3) 0.1140(3) 0.1448(3) 0.027(2) 1.000 . Uani d ? C(19) 0.0286(5) 0.2283(4) 0.5562(4) 0.044(2) 1.000 . Uani d ? C(20) 0.0184(5) 0.1722(4) 0.6271(4) 0.043(2) 1.000 . Uani d ? C(21) -0.0002(4) 0.0988(4) 0.5775(4) 0.031(2) 1.000 . Uani d ? C(22) 0.0558(4) 0.1030(3) 0.5120(4) 0.031(2) 1.000 . Uani d ? C(23) -0.0708(5) 0.5579(4) 0.2173(5) 0.058(3) 1.000 . Uani d ? C(24) -0.0359(8) 0.6067(7) 0.1545(7) 0.032(4) 0.500 . Uani d ? C(25) 0.0357(9) 0.6338(8) 0.2151(8) 0.043(4) 0.500 . Uani d ? H(1) -0.0378 0.4343 0.0759 0.064 1.000 . Uiso c ? H(2) -0.0784 0.4838 -0.0590 0.104 1.000 . Uiso c ? H(3) -0.2120 0.4547 -0.1380 0.063 1.000 . Uiso c ? H(4) -0.2918 0.3655 -0.0861 0.035 1.000 . Uiso c ? H(5) -0.2429 0.3115 0.0472 0.030 1.000 . Uiso c ? H(6) -0.2638 0.2458 0.1997 0.043 1.000 . Uiso c ? H(7) -0.3491 0.2332 0.3000 0.071 1.000 . Uiso c ? H(8) -0.3135 0.2888 0.4341 0.080 1.000 . Uiso c ? H(9) -0.1887 0.3589 0.4659 0.103 1.000 . Uiso c ? H(10) -0.0986 0.3640 0.3682 0.056 1.000 . Uiso c ? H(11) 0.0872 0.0070 0.2986 0.035 1.000 . Uiso c ? H(12) 0.1911 -0.0678 0.2565 0.054 1.000 . Uiso c ? H(13) 0.2551 -0.0305 0.1470 0.050 1.000 . Uiso c ? H(14) 0.2181 0.0841 0.0754 0.053 1.000 . Uiso c ? H(15) 0.1138 0.1603 0.1154 0.032 1.000 . Uiso c ? H(16) 0.0663 0.2676 0.5782 0.053 1.000 . Uiso c ? H(17) -0.0238 0.2497 0.5311 0.053 1.000 . Uiso c ? H(18) 0.0682 0.1683 0.6688 0.052 1.000 . Uiso c ? H(19) -0.0265 0.1862 0.6542 0.052 1.000 . Uiso c ? H(20) 0.0134 0.0561 0.6139 0.037 1.000 . Uiso c ? H(21) -0.0572 0.0962 0.5506 0.037 1.000 . Uiso c ? H(22) 0.0318 0.0761 0.4616 0.037 1.000 . Uiso c ? H(23) 0.1093 0.0826 0.5345 0.037 1.000 . Uiso c ? H(24) -0.1134 0.5247 0.1898 0.070 1.000 . Uiso c ? H(25) -0.0914 0.5871 0.2591 0.070 1.000 . Uiso c ? H(26) -0.0205 0.5782 0.1092 0.039 0.500 . Uiso d ? H(27) -0.0727 0.6463 0.1314 0.039 0.500 . Uiso d ? H(28) 0.0195 0.6744 0.2477 0.052 0.500 . Uiso d ? H(29) 0.0778 0.6507 0.1855 0.052 0.500 . Uiso d ? H(30) -0.0434 0.2148 0.1097 0.020 1.000 . Uiso c ? H(31) 0.0000(3) 0.4225(3) 0.2500(3) 0.022(1) 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ga(1) 0.0134(3) 0.0136(3) 0.0146(3) 0.0027(2) 0.0024(2) 0.0002(2) Ga(1*) 0.0133(3) 0.0135(3) 0.0146(3) -0.0026(2) 0.0024(2) -0.0001(2) Ga(2) 0.0191(5) 0.0094(4) 0.0144(4) 0.0000 0.0028(3) 0.0000 O(1*) 0.022(2) 0.014(2) 0.016(2) -0.004(2) 0.005(2) -0.002(1) O(1) 0.022(2) 0.014(2) 0.016(2) 0.003(2) 0.005(2) 0.001(1) O(2) 0.017(3) 0.014(3) 0.020(3) 0.0000 -0.002(2) 0.0000 O(3) 0.053(3) 0.027(2) 0.018(2) -0.007(2) 0.010(2) 0.001(2) O(4) 0.054(5) 0.002(3) 0.137(7) -0.0012 -0.057(5) -0.0072 C(1) 0.015(3) 0.017(3) 0.017(3) 0.004(2) 0.007(2) -0.004(2) C(2) 0.040(4) 0.065(5) 0.043(4) -0.016(4) -0.027(3) 0.029(4) C(3) 0.060(6) 0.123(8) 0.065(5) -0.050(6) -0.025(4) 0.072(5) C(4) 0.042(5) 0.082(6) 0.030(4) 0.000(4) -0.003(3) 0.037(4) C(5) 0.025(3) 0.042(4) 0.017(3) 0.004(3) -0.002(2) -0.001(3) C(6) 0.023(3) 0.030(4) 0.020(3) -0.009(3) -0.001(2) 0.003(2) C(7) 0.011(3) 0.028(3) 0.029(3) 0.009(2) 0.005(2) 0.006(2) C(8) 0.032(4) 0.026(4) 0.054(4) 0.010(3) 0.020(3) 0.011(3) C(9) 0.057(5) 0.030(4) 0.109(7) 0.022(4) 0.063(5) 0.036(4) C(10) 0.044(5) 0.113(8) 0.052(5) 0.047(5) 0.036(4) 0.056(5) C(11) 0.057(6) 0.18(1) 0.024(4) 0.060(7) 0.019(4) 0.030(5) C(12) 0.023(4) 0.099(6) 0.020(3) 0.013(4) 0.009(3) -0.007(3) C(13*) 0.018(3) 0.024(3) 0.013(3) -0.001(2) -0.005(2) 0.007(2) C(13) 0.019(3) 0.024(3) 0.013(3) 0.000(2) -0.005(2) -0.008(2) C(14) 0.025(3) 0.022(3) 0.037(3) 0.007(3) -0.004(3) -0.005(3) C(15) 0.032(4) 0.020(4) 0.071(5) 0.014(3) -0.018(4) -0.017(3) C(16) 0.018(3) 0.035(4) 0.068(5) 0.010(3) -0.004(3) -0.031(4) C(17) 0.026(4) 0.057(5) 0.053(4) -0.009(4) 0.017(3) -0.031(4) C(18) 0.022(3) 0.026(3) 0.031(3) 0.005(3) 0.002(3) -0.013(3) C(19) 0.073(5) 0.026(4) 0.030(3) 0.008(4) 0.003(3) 0.001(3) C(20) 0.051(5) 0.057(5) 0.027(3) 0.015(4) 0.023(3) 0.005(3) C(21) 0.026(3) 0.036(4) 0.031(3) -0.003(3) 0.006(3) 0.020(3) C(22) 0.037(4) 0.023(4) 0.030(3) 0.010(3) 0.002(3) 0.009(3) C(23) 0.041(5) 0.030(4) 0.102(6) 0.019(4) 0.006(4) -0.007(4) C(23*) 0.042(5) 0.029(4) 0.097(6) -0.023(4) 0.002(4) -0.002(4) C(24) 0.029(7) 0.045(9) 0.023(6) 0.002(6) 0.008(5) 0.008(6) C(25) 0.051(9) 0.032(8) 0.048(8) -0.003(7) 0.013(7) 0.012(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4917 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_all 0.0824 _refine_ls_wR_factor_ref 0.0824 _refine_ls_goodness_of_fit_all 5.863 _refine_ls_goodness_of_fit_ref 5.863 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.75 _refine_diff_density_max 1.05 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 O3 2.642(5) . 2 no O1 C22 3.562(6) . 2 no O2 O4 2.691(7) . . no O2 C23 3.541(8) . . no O2 C23 3.541(8) . 2 no O3 H4 3.0280 . 8 no C1 H13 2.9145 . 5_455 no C3 H26 2.7104 . 3_565 no C3 C24 3.49(2) . 3_565 no C4 H29 3.0491 . 3_565 no C6 H13 3.0030 . 5_455 no C14 H20 2.8576 . 4_554 no C15 H3 2.8015 . 8 no C15 H20 2.9743 . 4_554 no C16 H24 2.8123 . 5_545 no C16 H23 2.8150 . 4_554 no C18 H22 2.9187 . 2 no C18 C22 3.538(8) . 2 no C19 H29 2.9694 . 4_565 no C19 C25 3.49(1) . 4_565 no C19 C24 3.56(1) . 4_565 no C25 H7 2.7348 . 5 no C25 H16 2.9023 . 4_564 no H1 H2 2.4375 . 3_565 no H1 H26 2.5991 . . no H2 H26 2.2175 . 3_565 no H5 H5 2.6249 . 7_455 no H7 H27 2.3844 . 6_445 no H7 H28 2.3848 . 5_445 no H7 H29 2.4582 . 5_445 no H7 H19 2.6855 . 7_456 no H11 H20 2.5933 . 3_556 no H13 H24 2.3378 . 5_545 no H16 H29 2.2151 . 4_565 no H17 H27 2.6515 . 4_565 no H20 H22 2.6654 . 3_556 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #===END data_pn2291098 #------------------------------------------------------------------------------ _audit_creation_date '19100-03-20' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_contact_author_name ' PROF. COLIN L RASTON ' _publ_contact_author_address ; DEPT. OF CHEMISTRY MONASH UNIVERSITY CLAYTON, MELBOURNE, VICTORIA 3168 AUSTRALIA ; _publ_contact_author_email ' c.raston@sci.monash.edu.au ' _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 22.5232(2) _cell_length_b 22.5232(2) _cell_length_c 20.8835(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 9174.7(1) _cell_formula_units_Z 6 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 ' _symmetry_Int_Tables_number 148 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '2/3+x,1/3+y,1/3+z' '1/3+x,2/3+y,2/3+z' ' -y, +x-y, +z' '2/3-y,1/3+x-y,1/3+z' '1/3-y,2/3+x-y,2/3+z' ' -x+y, -x, +z' '2/3-x+y,1/3-x,1/3+z' '1/3-x+y,2/3-x,2/3+z' ' -x, -y, -z' '2/3-x,1/3-y,1/3-z' '1/3-x,2/3-y,2/3-z' ' +y, -x+y, -z' '2/3+y,1/3-x+y,1/3-z' '1/3+y,2/3-x+y,2/3-z' ' +x-y, +x, -z' '2/3+x-y,1/3+x,1/3-z' '1/3+x-y,2/3+x,2/3-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'chunk' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1121.37 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H78 Ga6 O9 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3456.00 _exptl_absorpt_coefficient_mu 2.642 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Enraf Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 5967 _reflns_number_total 45092 _reflns_number_gt 3576 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga 0 36 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 54 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 240 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 468 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ga(1) 0.61131(3) 0.24235(3) 0.11453(3) 0.0233(2) 1.000 . Uani d ? Ga(2) 0.57702(4) 0.30792(3) -0.00455(4) 0.0403(2) 1.000 . Uani d ? O(1) 0.6054(2) 0.2482(2) 0.0251(2) 0.0153(9) 1.000 . Uani d ? O(2) 0.6667 0.3333 0.1422(3) 0.0168(9) 0.333 ST Uani d ? O(9) 0.5438(2) 0.3017(2) 0.0965(2) 0.025(1) 1.000 . Uani d ? O(10) 0.6667 0.3333 -0.0797(4) 0.046(2) 0.333 ST Uani d ? O(11) 0.832(1) 0.1625(6) 0.1358(8) 0.091(6) 0.250 . Uani d ? C(1) 0.5470(2) 0.1695(2) 0.1700(3) 0.017(1) 1.000 . Uani d ? C(2) 0.4821(3) 0.1195(2) 0.1479(3) 0.019(2) 1.000 . Uani d ? C(3) 0.4362(3) 0.0698(3) 0.1906(3) 0.027(2) 1.000 . Uani d ? C(4) 0.4527(3) 0.0681(3) 0.2539(3) 0.030(2) 1.000 . Uani d ? C(5) 0.5176(3) 0.1163(3) 0.2743(3) 0.028(2) 1.000 . Uani d ? C(6) 0.5652(3) 0.1667(2) 0.2335(3) 0.020(2) 1.000 . Uani d ? C(7) 0.3745(3) 0.2464(3) -0.1239(3) 0.032(2) 1.000 . Uani d ? C(8) 0.4086(3) 0.2095(3) -0.1294(3) 0.034(2) 1.000 . Uani d ? C(9) 0.4681(3) 0.2280(3) -0.0957(3) 0.022(2) 1.000 . Uani d ? C(10) 0.4958(3) 0.2849(3) -0.0550(2) 0.020(2) 1.000 . Uani d ? C(11) 0.4621(3) 0.3229(3) -0.0503(3) 0.023(2) 1.000 . Uani d ? C(12) 0.4021(3) 0.3026(3) -0.0842(3) 0.028(2) 1.000 . Uani d ? C(13) 0.4891(3) 0.3858(3) -0.0085(3) 0.040(2) 1.000 . Uani d ? C(14) 0.5030(3) 0.1857(3) -0.1047(3) 0.036(2) 1.000 . Uani d ? C(15) 0.3100(3) 0.2268(3) -0.1623(4) 0.056(2) 1.000 . Uani d ? C(16) 0.4610(3) 0.1173(3) 0.0796(3) 0.029(2) 1.000 . Uani d ? C(17) 0.6354(3) 0.2166(3) 0.2592(3) 0.027(2) 1.000 . Uani d ? C(18) 0.4023(3) 0.0137(3) 0.2990(3) 0.051(2) 1.000 . Uani d ? C(19) 0.7598(6) 0.1715(5) 0.1355(5) 0.025(3) 0.500 . Uani d ? C(20) 0.7939(6) 0.1790(6) 0.2017(6) 0.042(4) 0.500 . Uani d ? C(22) 0.7885(7) 0.1429(6) 0.0965(8) 0.054(5) 0.500 . Uani d ? H(1) 0.3919 0.0362 0.1755 0.033 1.000 . Uiso c ? H(2) 0.5298 0.1155 0.3179 0.034 1.000 . Uiso c ? H(3) 0.3903 0.1706 -0.1570 0.040 1.000 . Uiso c ? H(4) 0.3793 0.3287 -0.0800 0.035 1.000 . Uiso c ? H(5) 0.4212 0.1224 0.0779 0.034 1.000 . Uiso c ? H(6) 0.4970 0.1537 0.0565 0.034 1.000 . Uiso c ? H(7) 0.4502 0.0747 0.0608 0.034 1.000 . Uiso c ? H(8) 0.6567 0.1923 0.2735 0.032 1.000 . Uiso c ? H(9) 0.6615 0.2475 0.2261 0.032 1.000 . Uiso c ? H(10) 0.6309 0.2417 0.2938 0.032 1.000 . Uiso c ? H(11) 0.3920 0.0352 0.3336 0.059 1.000 . Uiso c ? H(12) 0.3607 -0.0153 0.2766 0.059 1.000 . Uiso c ? H(13) 0.4206 -0.0126 0.3156 0.059 1.000 . Uiso c ? H(14) 0.5302 0.3926 0.0126 0.048 1.000 . Uiso c ? H(15) 0.5012 0.4250 -0.0347 0.048 1.000 . Uiso c ? H(16) 0.4567 0.3807 0.0221 0.048 1.000 . Uiso c ? H(18) 0.5159 0.1879 -0.1481 0.040 1.000 . Uiso c ? H(19) 0.5422 0.2033 -0.0780 0.040 1.000 . Uiso c ? H(20) 0.2736 0.2176 -0.1345 0.067 1.000 . Uiso c ? H(21) 0.3185 0.2634 -0.1904 0.067 1.000 . Uiso c ? H(22) 0.2990 0.1869 -0.1872 0.067 1.000 . Uiso c ? H(23) 0.4719 0.1392 -0.0933 0.040 1.000 . Uiso c ? Ga(2*) 0.69208(4) 0.26910(3) -0.00455(4) 0.0403(2) 1.000 . Uani d ? O(9*) 0.6983(2) 0.2421(2) 0.0965(2) 0.025(1) 1.000 . Uani d ? Ga(1*) 0.63105(3) 0.38869(3) 0.11453(3) 0.0233(2) 1.000 . Uani d ? O(1*) 0.6428(2) 0.3946(2) 0.0251(2) 0.0153(9) 1.000 . Uani d ? Ga(1*) 0.75765(3) 0.36895(3) 0.11453(3) 0.0233(2) 1.000 . Uani d ? O(11*) 0.835(1) 0.1708(6) 0.1975(8) 0.091(6) 0.250 . Uani d ? C(20*) 0.8727(6) 0.1543(6) 0.1316(6) 0.042(4) 0.500 . Uani d ? O(1*) 0.7518(2) 0.3572(2) 0.0251(2) 0.0153(9) 1.000 . Uani d ? C(10*) 0.7151(3) 0.2109(3) -0.0550(2) 0.020(2) 1.000 . Uani d ? C(1*) 0.6224(2) 0.4530(2) 0.1700(3) 0.017(1) 1.000 . Uani d ? Ga(2*) 0.73090(4) 0.42298(3) -0.00455(4) 0.0403(2) 1.000 . Uani d ? O(9*) 0.7579(2) 0.4562(2) 0.0965(2) 0.025(1) 1.000 . Uani d ? C(1*) 0.8305(2) 0.3776(2) 0.1700(3) 0.017(1) 1.000 . Uani d ? C(19*) 0.9068(6) 0.1618(5) 0.1978(5) 0.025(3) 0.500 . Uani d ? C(22*) 0.8781(7) 0.1905(6) 0.2368(8) 0.054(5) 0.500 . Uani d ? C(9*) 0.7720(3) 0.2401(3) -0.0957(3) 0.022(2) 1.000 . Uani d ? C(11*) 0.6771(3) 0.1392(3) -0.0503(3) 0.023(2) 1.000 . Uani d ? C(2*) 0.6374(3) 0.5179(2) 0.1479(3) 0.019(2) 1.000 . Uani d ? C(6*) 0.6015(3) 0.4348(2) 0.2335(3) 0.020(2) 1.000 . Uani d ? C(10*) 0.7891(3) 0.5042(3) -0.0550(2) 0.020(2) 1.000 . Uani d ? C(2*) 0.8805(3) 0.3626(2) 0.1479(3) 0.019(2) 1.000 . Uani d ? C(6*) 0.8333(3) 0.3985(2) 0.2335(3) 0.020(2) 1.000 . Uani d ? C(8*) 0.7905(3) 0.1991(3) -0.1294(3) 0.034(2) 1.000 . Uani d ? C(14*) 0.8143(3) 0.3173(3) -0.1047(3) 0.036(2) 1.000 . Uani d ? C(12*) 0.6974(3) 0.0994(3) -0.0842(3) 0.028(2) 1.000 . Uani d ? C(13*) 0.6142(3) 0.1033(3) -0.0085(3) 0.040(2) 1.000 . Uani d ? C(3*) 0.6337(3) 0.5638(3) 0.1906(3) 0.027(2) 1.000 . Uani d ? C(16*) 0.6563(3) 0.5390(3) 0.0796(3) 0.029(2) 1.000 . Uani d ? C(5*) 0.5986(3) 0.4824(3) 0.2743(3) 0.028(2) 1.000 . Uani d ? C(17*) 0.5812(3) 0.3646(3) 0.2592(3) 0.027(2) 1.000 . Uani d ? C(9*) 0.7599(3) 0.5319(3) -0.0957(3) 0.022(2) 1.000 . Uani d ? C(11*) 0.8608(3) 0.5379(3) -0.0503(3) 0.023(2) 1.000 . Uani d ? C(3*) 0.9302(3) 0.3663(3) 0.1906(3) 0.027(2) 1.000 . Uani d ? C(16*) 0.8827(3) 0.3437(3) 0.0796(3) 0.029(2) 1.000 . Uani d ? C(5*) 0.8837(3) 0.4014(3) 0.2743(3) 0.028(2) 1.000 . Uani d ? C(17*) 0.7834(3) 0.4188(3) 0.2592(3) 0.027(2) 1.000 . Uani d ? C(7*) 0.7536(3) 0.1282(3) -0.1239(3) 0.032(2) 1.000 . Uani d ? H(3*) 0.8294 0.2197 -0.1570 0.040 1.000 . Uiso c ? H(18*) 0.8121 0.3281 -0.1481 0.040 1.000 . Uiso c ? H(19*) 0.7967 0.3389 -0.0780 0.040 1.000 . Uiso c ? H(23*) 0.8608 0.3327 -0.0933 0.040 1.000 . Uiso c ? H(4*) 0.6713 0.0506 -0.0800 0.035 1.000 . Uiso c ? H(14*) 0.6074 0.1375 0.0126 0.048 1.000 . Uiso c ? H(15*) 0.5750 0.0762 -0.0347 0.048 1.000 . Uiso c ? H(16*) 0.6193 0.0759 0.0221 0.048 1.000 . Uiso c ? C(4*) 0.6154(3) 0.5473(3) 0.2539(3) 0.030(2) 1.000 . Uani d ? H(1*) 0.6443 0.6081 0.1755 0.033 1.000 . Uiso c ? H(5*) 0.7011 0.5788 0.0779 0.034 1.000 . Uiso c ? H(6*) 0.6566 0.5030 0.0565 0.034 1.000 . Uiso c ? H(7*) 0.6245 0.5498 0.0608 0.034 1.000 . Uiso c ? H(2*) 0.5857 0.4702 0.3179 0.034 1.000 . Uiso c ? H(8*) 0.5356 0.3433 0.2735 0.032 1.000 . Uiso c ? H(9*) 0.5860 0.3385 0.2261 0.032 1.000 . Uiso c ? H(10*) 0.6108 0.3691 0.2938 0.032 1.000 . Uiso c ? C(8*) 0.8009(3) 0.5914(3) -0.1294(3) 0.034(2) 1.000 . Uani d ? C(14*) 0.6827(3) 0.4970(3) -0.1047(3) 0.036(2) 1.000 . Uani d ? C(12*) 0.9006(3) 0.5979(3) -0.0842(3) 0.028(2) 1.000 . Uani d ? C(13*) 0.8967(3) 0.5109(3) -0.0085(3) 0.040(2) 1.000 . Uani d ? C(4*) 0.9319(3) 0.3846(3) 0.2539(3) 0.030(2) 1.000 . Uani d ? H(1*) 0.9638 0.3557 0.1755 0.033 1.000 . Uiso c ? H(5*) 0.8776 0.2989 0.0779 0.034 1.000 . Uiso c ? H(6*) 0.8463 0.3434 0.0565 0.034 1.000 . Uiso c ? H(7*) 0.9253 0.3755 0.0608 0.034 1.000 . Uiso c ? H(2*) 0.8845 0.4143 0.3179 0.034 1.000 . Uiso c ? H(8*) 0.8077 0.4644 0.2735 0.032 1.000 . Uiso c ? H(9*) 0.7525 0.4140 0.2261 0.032 1.000 . Uiso c ? H(10*) 0.7583 0.3892 0.2938 0.032 1.000 . Uiso c ? C(15*) 0.7732(3) 0.0832(3) -0.1623(4) 0.056(2) 1.000 . Uani d ? C(18*) 0.6114(3) 0.5977(3) 0.2990(3) 0.051(2) 1.000 . Uani d ? C(7*) 0.8718(3) 0.6255(3) -0.1239(3) 0.032(2) 1.000 . Uani d ? H(3*) 0.7803 0.6097 -0.1570 0.040 1.000 . Uiso c ? H(18*) 0.6719 0.4841 -0.1481 0.040 1.000 . Uiso c ? H(19*) 0.6611 0.4578 -0.0780 0.040 1.000 . Uiso c ? H(23*) 0.6673 0.5281 -0.0933 0.040 1.000 . Uiso c ? H(4*) 0.9494 0.6207 -0.0800 0.035 1.000 . Uiso c ? H(14*) 0.8625 0.4698 0.0126 0.048 1.000 . Uiso c ? H(15*) 0.9238 0.4988 -0.0347 0.048 1.000 . Uiso c ? H(16*) 0.9241 0.5433 0.0221 0.048 1.000 . Uiso c ? C(18*) 0.9863(3) 0.3886(3) 0.2990(3) 0.051(2) 1.000 . Uani d ? H(20*) 0.7824 0.0560 -0.1345 0.067 1.000 . Uiso c ? H(21*) 0.7366 0.0552 -0.1904 0.067 1.000 . Uiso c ? H(22*) 0.8131 0.1121 -0.1872 0.067 1.000 . Uiso c ? H(11*) 0.6432 0.6080 0.3336 0.059 1.000 . Uiso c ? H(12*) 0.6240 0.6393 0.2766 0.059 1.000 . Uiso c ? H(13*) 0.5668 0.5794 0.3156 0.059 1.000 . Uiso c ? C(15*) 0.9168(3) 0.6900(3) -0.1623(4) 0.056(2) 1.000 . Uani d ? H(11*) 0.9648 0.3568 0.3336 0.059 1.000 . Uiso c ? H(12*) 1.0153 0.3760 0.2766 0.059 1.000 . Uiso c ? H(13*) 1.0126 0.4332 0.3156 0.059 1.000 . Uiso c ? H(20*) 0.9440 0.7264 -0.1345 0.067 1.000 . Uiso c ? H(21*) 0.9448 0.6815 -0.1904 0.067 1.000 . Uiso c ? H(22*) 0.8879 0.7010 -0.1872 0.067 1.000 . Uiso c ? 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 Ga(1) 0.0235(4) 0.0205(3) 0.0133(3) 0.0015(3) 0.0015(3) -0.0004(3) Ga(2) 0.0445(4) 0.0241(4) 0.0597(6) 0.0228(3) -0.0375(4) -0.0193(3) O(1) 0.018(2) 0.017(2) 0.011(2) 0.009(2) -0.002(1) -0.001(1) O(2) 0.018(2) 0.0176 0.015(4) 0.0088 0.0000 0.0000 O(9) 0.030(2) 0.019(2) 0.019(2) 0.006(2) -0.002(2) -0.003(2) O(10) 0.026(3) 0.0262 0.085(7) 0.0131 0.0000 0.0000 O(11) 0.15(1) 0.005(6) 0.10(1) 0.023(8) -0.11(1) 0.018(7) C(1) 0.019(3) 0.018(3) 0.016(3) 0.010(2) 0.005(2) 0.001(2) C(2) 0.020(3) 0.019(3) 0.018(3) 0.010(3) 0.001(2) -0.002(2) C(3) 0.020(3) 0.024(3) 0.032(4) 0.008(3) 0.003(3) 0.000(3) C(4) 0.033(4) 0.023(3) 0.027(4) 0.009(3) 0.009(3) 0.003(3) C(5) 0.041(4) 0.028(3) 0.013(3) 0.015(3) 0.002(3) 0.003(3) C(6) 0.025(3) 0.019(3) 0.015(3) 0.010(3) 0.002(2) 0.000(2) C(7) 0.020(3) 0.023(3) 0.038(4) 0.000(3) -0.009(3) 0.011(3) C(8) 0.039(4) 0.018(3) 0.033(4) 0.004(3) -0.017(3) -0.001(3) C(9) 0.026(3) 0.020(3) 0.021(3) 0.012(3) -0.006(2) 0.003(2) C(10) 0.020(3) 0.023(3) 0.013(3) 0.009(2) -0.001(2) 0.000(2) C(11) 0.024(3) 0.025(3) 0.020(3) 0.011(3) 0.004(3) 0.004(2) C(12) 0.022(3) 0.032(3) 0.031(4) 0.015(3) 0.002(3) 0.010(3) C(13) 0.048(4) 0.053(4) 0.038(4) 0.039(4) -0.010(3) -0.014(3) C(14) 0.049(4) 0.035(4) 0.026(4) 0.023(3) -0.015(3) -0.015(3) C(15) 0.043(4) 0.037(4) 0.076(6) 0.012(3) -0.029(4) 0.004(4) C(16) 0.023(3) 0.028(3) 0.026(4) 0.005(3) -0.003(3) 0.002(3) C(17) 0.029(3) 0.027(3) 0.017(3) 0.008(3) -0.004(3) 0.001(3) C(18) 0.051(4) 0.042(4) 0.037(5) 0.006(4) 0.019(3) 0.015(3) C(19) 0.039(7) 0.037(7) 0.022(7) 0.036(6) 0.008(5) 0.020(5) C(20) 0.060(8) 0.046(9) 0.018(8) 0.026(7) 0.025(6) 0.021(6) C(22) 0.043(8) 0.034(8) 0.10(1) 0.027(7) 0.014(8) 0.021(8) Ga(2*) 0.0241(4) 0.0231(4) 0.0597(6) 0.0014(3) 0.0193(4) -0.0182(3) O(9*) 0.019(2) 0.037(2) 0.019(2) 0.013(2) 0.003(2) 0.001(2) Ga(1*) 0.0409(4) 0.0235(3) 0.0133(3) 0.0220(3) -0.0019(3) -0.0015(3) O(1*) 0.017(2) 0.018(2) 0.011(2) 0.009(2) 0.002(1) 0.002(1) Ga(1*) 0.0205(4) 0.0409(3) 0.0133(3) 0.0190(3) 0.0004(3) 0.0019(3) O(11*) 0.15(1) 0.005(6) 0.10(1) 0.023(8) -0.11(1) 0.018(7) C(20*) 0.060(8) 0.046(9) 0.018(8) 0.026(7) 0.025(6) 0.021(6) O(1*) 0.017(2) 0.017(2) 0.011(2) 0.008(2) 0.001(1) -0.002(1) C(10*) 0.023(3) 0.025(3) 0.013(3) 0.014(2) 0.000(2) -0.001(2) C(1*) 0.017(3) 0.019(3) 0.016(3) 0.009(2) -0.004(2) -0.005(2) Ga(2*) 0.0231(4) 0.0445(4) 0.0597(6) 0.0217(3) 0.0182(4) 0.0375(3) O(9*) 0.037(2) 0.030(2) 0.019(2) 0.024(2) -0.001(2) 0.002(2) C(1*) 0.018(3) 0.017(3) 0.016(3) 0.008(2) -0.001(2) 0.004(2) C(19*) 0.039(7) 0.037(7) 0.022(7) 0.036(6) 0.008(5) 0.020(5) C(22*) 0.043(8) 0.034(8) 0.10(1) 0.027(7) 0.014(8) 0.021(8) C(9*) 0.020(3) 0.023(3) 0.021(3) 0.008(3) -0.003(2) -0.009(2) C(11*) 0.025(3) 0.027(3) 0.020(3) 0.014(3) -0.004(3) 0.000(2) C(2*) 0.020(3) 0.020(3) 0.018(3) 0.011(3) -0.003(2) -0.001(2) C(6*) 0.024(3) 0.025(3) 0.015(3) 0.015(3) -0.002(2) -0.002(2) C(10*) 0.025(3) 0.020(3) 0.013(3) 0.011(2) 0.001(2) 0.001(2) C(2*) 0.019(3) 0.020(3) 0.018(3) 0.009(3) 0.002(2) 0.003(2) C(6*) 0.019(3) 0.024(3) 0.015(3) 0.009(3) 0.000(2) 0.002(2) C(8*) 0.018(4) 0.047(3) 0.033(4) 0.013(3) 0.001(3) -0.016(3) C(14*) 0.035(4) 0.038(4) 0.026(4) 0.012(3) 0.015(3) 0.001(3) C(12*) 0.032(3) 0.023(3) 0.031(4) 0.016(3) -0.010(3) -0.008(3) C(13*) 0.053(4) 0.023(4) 0.038(4) 0.014(4) 0.014(3) 0.004(3) C(3*) 0.028(3) 0.020(3) 0.032(4) 0.012(3) -0.004(3) -0.003(3) C(16*) 0.040(3) 0.023(3) 0.026(4) 0.017(3) 0.005(3) 0.003(3) C(5*) 0.038(4) 0.041(3) 0.013(3) 0.026(3) 0.000(3) -0.002(3) C(17*) 0.041(3) 0.029(3) 0.017(3) 0.021(3) 0.005(3) 0.004(3) C(9*) 0.023(3) 0.026(3) 0.021(3) 0.015(3) 0.009(2) 0.006(2) C(11*) 0.027(3) 0.024(3) 0.020(3) 0.013(3) 0.000(3) -0.004(2) C(3*) 0.024(3) 0.028(3) 0.032(4) 0.016(3) 0.000(3) 0.004(3) C(16*) 0.028(3) 0.040(3) 0.026(4) 0.022(3) -0.002(3) -0.005(3) C(5*) 0.028(4) 0.038(3) 0.013(3) 0.013(3) -0.003(3) 0.000(3) C(17*) 0.027(3) 0.041(3) 0.017(3) 0.020(3) -0.001(3) -0.005(3) C(7*) 0.023(3) 0.042(3) 0.038(4) 0.022(3) -0.011(3) -0.020(3) C(4*) 0.037(4) 0.033(3) 0.027(4) 0.024(3) -0.006(3) -0.009(3) C(8*) 0.047(4) 0.039(3) 0.033(4) 0.034(3) 0.016(3) 0.017(3) C(14*) 0.038(4) 0.049(4) 0.026(4) 0.026(3) -0.001(3) 0.015(3) C(12*) 0.023(3) 0.022(3) 0.031(4) 0.007(3) 0.008(3) -0.002(3) C(13*) 0.023(4) 0.048(4) 0.038(4) 0.009(4) -0.004(3) 0.010(3) C(4*) 0.023(4) 0.037(3) 0.027(4) 0.013(3) -0.003(3) 0.006(3) C(15*) 0.037(4) 0.057(4) 0.076(6) 0.025(3) -0.004(4) -0.034(4) C(18*) 0.081(4) 0.051(4) 0.037(5) 0.045(4) -0.004(3) -0.019(3) C(7*) 0.042(3) 0.020(3) 0.038(4) 0.020(3) 0.020(3) 0.009(3) C(18*) 0.042(4) 0.081(4) 0.037(5) 0.036(4) -0.015(3) 0.004(3) C(15*) 0.057(4) 0.043(4) 0.076(6) 0.031(3) 0.034(4) 0.029(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3576 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_number_constraints 4 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_all 0.0599 _refine_ls_wR_factor_ref 0.0599 _refine_ls_goodness_of_fit_all 4.550 _refine_ls_goodness_of_fit_ref 4.550 _refine_ls_shift/su_max 4.5750 _refine_ls_shift/su_mean 0.3150 _refine_diff_density_min -1.97 _refine_diff_density_max 2.60 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag GA1 GA2 2.9599(9) . 2_655 yes GA1 O1 1.881(3) . . yes GA1 O2 1.879(2) . . yes GA1 O9 1.998(3) . 2_655 yes GA1 C1 1.938(5) . . yes GA2 O1 1.860(3) . . yes GA2 O1 1.870(3) . 3_665 yes GA2 O9 2.219(4) . . yes GA2 C10 1.944(5) . . yes O11 O11 1.30(4) . 10_655 yes O11 C19 1.73(2) . . yes O11 C20 1.75(3) . . yes O11 C20 1.03(2) . 10_655 yes O11 C22 1.18(2) . . yes C1 C2 1.404(7) . . yes C1 C6 1.399(7) . . yes C2 C3 1.400(7) . . yes C2 C16 1.497(7) . . yes C3 C4 1.378(8) . . yes C3 H1 0.95 . . no C4 C5 1.381(8) . . yes C4 C18 1.512(8) . . yes C5 C6 1.395(7) . . yes C5 H2 0.95 . . no C6 C17 1.507(7) . . yes C7 C8 1.389(8) . . yes C7 C12 1.375(8) . . yes C7 C15 1.519(8) . . yes C8 C9 1.381(7) . . yes C8 H3 0.95 . . no C9 C10 1.398(7) . . yes C9 C14 1.521(7) . . yes C10 C11 1.404(7) . . yes C11 C12 1.387(7) . . yes C11 C13 1.508(8) . . yes C12 H4 0.96 . . no C13 H14 0.96 . . no C13 H15 0.95 . . no C13 H16 0.93 . . no C14 H18 0.94 . . no C14 H19 0.95 . . no C14 H23 0.95 . . no C15 H20 0.94 . . no C15 H21 0.95 . . no C15 H22 0.96 . . no C16 H5 0.96 . . no C16 H6 0.95 . . no C16 H7 0.95 . . no C17 H8 0.94 . . no C17 H9 0.95 . . no C17 H10 0.95 . . no C18 H11 0.96 . . no C18 H12 0.95 . . no C18 H13 0.94 . . no C19 C20 1.55(2) . . yes C19 C22 1.38(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag GA2 GA1 O1 37.78(9) 2_655 . . yes GA2 GA1 O2 91.8(2) 2_655 . . yes GA2 GA1 O9 48.6(1) 2_655 . 2_655 yes GA2 GA1 C1 142.9(1) 2_655 . . yes O1 GA1 O2 105.1(2) . . . yes O1 GA1 O9 85.2(1) . . 2_655 yes O1 GA1 C1 127.1(2) . . . yes O2 GA1 O9 86.8(1) . . 2_655 yes O2 GA1 C1 123.2(2) . . . yes O9 GA1 C1 115.4(2) 2_655 . . yes GA1 GA2 O1 88.9(1) 3_665 . . yes GA1 GA2 O1 38.0(1) 3_665 . 3_665 yes GA1 GA2 O9 42.45(9) 3_665 . . yes GA1 GA2 C10 131.5(2) 3_665 . . yes O1 GA2 O1 105.3(2) . . 3_665 yes O1 GA2 O9 82.2(1) . . . yes O1 GA2 C10 127.3(2) . . . yes O1 GA2 O9 79.5(1) 3_665 . . yes O1 GA2 C10 127.4(2) 3_665 . . yes O9 GA2 C10 104.9(2) . . . yes GA1 O1 GA2 116.3(2) . . . yes GA1 O1 GA2 104.2(1) . . 2_655 yes GA2 O1 GA2 113.6(2) . . 2_655 yes GA1 O2 GA1 111.0(2) . . 2_655 yes GA1 O2 GA1 111.0(2) . . 3_665 yes GA1 O2 GA1 111.0(2) 2_655 . 3_665 yes GA1 O9 GA2 89.0(1) 3_665 . . yes O11 O11 C19 88(2) 10_655 . . yes O11 O11 C20 36(1) 10_655 . . yes O11 O11 C20 97(1) 10_655 . 10_655 yes O11 O11 C22 136(3) 10_655 . . yes C19 O11 C20 53(1) . . . yes C19 O11 C20 174(2) . . 10_655 yes C19 O11 C22 53(1) . . . yes C20 O11 C20 133(1) . . 10_655 yes C20 O11 C22 103(2) . . . yes C20 O11 C22 121(2) 10_655 . . yes GA1 C1 C2 121.3(4) . . . yes GA1 C1 C6 119.5(4) . . . yes C2 C1 C6 119.1(5) . . . yes C1 C2 C3 119.2(5) . . . yes C1 C2 C16 121.7(5) . . . yes C3 C2 C16 119.0(5) . . . yes C2 C3 C4 122.1(5) . . . yes C2 C3 H1 119.0 . . . no C4 C3 H1 119.0 . . . no C3 C4 C5 117.9(5) . . . yes C3 C4 C18 121.0(5) . . . yes C5 C4 C18 121.0(6) . . . yes C4 C5 C6 122.1(5) . . . yes C4 C5 H2 118.8 . . . no C6 C5 H2 119.1 . . . no C1 C6 C5 119.4(5) . . . yes C1 C6 C17 121.7(5) . . . yes C5 C6 C17 118.9(5) . . . yes C8 C7 C12 118.2(5) . . . yes C8 C7 C15 121.1(6) . . . yes C12 C7 C15 120.7(6) . . . yes C7 C8 C9 121.3(5) . . . yes C7 C8 H3 119.0 . . . no C9 C8 H3 119.6 . . . no C8 C9 C10 120.5(5) . . . yes C8 C9 C14 118.5(5) . . . yes C10 C9 C14 121.0(5) . . . yes GA2 C10 C9 120.3(4) . . . yes GA2 C10 C11 121.5(4) . . . yes C9 C10 C11 118.2(5) . . . yes C10 C11 C12 119.9(5) . . . yes C10 C11 C13 121.8(5) . . . yes C12 C11 C13 118.3(5) . . . yes C7 C12 C11 121.9(5) . . . yes C7 C12 H4 119.2 . . . no C11 C12 H4 118.9 . . . no C11 C13 H14 108.5 . . . no C11 C13 H15 109.4 . . . no C11 C13 H16 110.9 . . . no H14 C13 H15 107.9 . . . no H14 C13 H16 109.5 . . . no H15 C13 H16 110.5 . . . no C9 C14 H18 109.1 . . . no C9 C14 H19 109.3 . . . no C9 C14 H23 109.3 . . . no H18 C14 H19 110.2 . . . no H18 C14 H23 109.6 . . . no H19 C14 H23 109.4 . . . no C7 C15 H20 109.9 . . . no C7 C15 H21 109.0 . . . no C7 C15 H22 108.8 . . . no H20 C15 H21 110.4 . . . no H20 C15 H22 109.9 . . . no H21 C15 H22 108.9 . . . no C2 C16 H5 109.3 . . . no C2 C16 H6 109.6 . . . no C2 C16 H7 110.1 . . . no H5 C16 H6 109.0 . . . no H5 C16 H7 108.9 . . . no H6 C16 H7 109.9 . . . no C6 C17 H8 109.2 . . . no C6 C17 H9 108.9 . . . no C6 C17 H10 109.2 . . . no H8 C17 H9 110.4 . . . no H8 C17 H10 109.9 . . . no H9 C17 H10 109.2 . . . no C4 C18 H11 109.5 . . . no C4 C18 H12 109.5 . . . no C4 C18 H13 110.6 . . . no H11 C18 H12 108.1 . . . no H11 C18 H13 109.3 . . . no H12 C18 H13 109.9 . . . no O11 C19 C20 64.3(8) . . . yes O11 C19 C22 42.7(9) . . . yes C20 C19 C22 105(1) . . . yes O11 C20 O11 47(1) . . 10_655 yes O11 C20 C19 62.9(7) . . . yes O11 C20 C19 110(2) 10_655 . . yes O11 C22 C19 85(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag GA2 O10 2.390(6) . . no O1 O10 2.779(7) . . no O9 C19 2.70(1) . 3_665 no O10 C10 3.474(5) . . no O10 C10 3.474(5) . 2_655 no O10 C10 3.474(5) . 3_665 no O10 C14 3.558(6) . . no O10 C14 3.558(6) . 2_655 no O10 C14 3.558(6) . 3_665 no C4 C8 3.564(8) . 9 no C8 C14 3.544(8) . 17_554 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ #===END