data_global _journal_coden_Cambridge 182 loop_ _publ_author_name ; D. O'Hare ; 'Kim, Jong-Young' 'Norquist, Alexander J.' _publ_contact_author_name ; Prof Dermot O'Hare ; _publ_contact_author_address ; Inorganic Chemistry Lab University of Oxford South Parks Rd Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email 'DERMOT.OHARE@CHEM.OX.AC.UK' _publ_requested_journal 'Chemical Communications' _publ_section_title ; The First Organically Templated Thorium Compounds, [C4N2H12]0.5[ThF5] and [C5N2H14][ThF6]*0.5H2O ; data_CRYSTALS_cifa _database_code_CSD 189998 _audit_creation_date 02-05-04 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 8.9255(3) _cell_angle_alpha 90 _cell_length_b 7.2633(3) _cell_angle_beta 105.054(2) _cell_length_c 8.9504(4) _cell_angle_gamma 90 _cell_volume 560.3 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Th ' -8.1270 8.8700 35.5645 0.5634 23.4219 3.4620 12.7473 17.8309 4.8070 99.1722 13.4314 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C2 H6 F5 N1 Th1 ' _chemical_formula_moiety ' C2 H6 F5 N1 Th1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 371.10 _cell_measurement_reflns_used 1212 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.06 _exptl_crystal_density_diffrn 4.399 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 608.716 _exptl_absorpt_coefficient_mu 26.630 # Sheldrick geometric definitions 0.34 0.34 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.34 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 2356 _reflns_number_total 1265 _diffrn_reflns_av_R_equivalents 0.04 # Number of reflections with Friedels Law is 1265 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1279 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_gt 1031 _diffrn_reflns_theta_min 5.47 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _refine_diff_density_min -1.62 _refine_diff_density_max 1.30 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 1031 _refine_ls_number_parameters 83 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0607 _refine_ls_goodness_of_fit_ref 0.8263 _refine_ls_shift/su_max 0.000191 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 8.34 12.1 6.37 2.23 0.586 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type TH1 TH 0.43082(3) 0.35332(4) 0.15524(3) 0.0046 1.0000 Uani F4 F 0.3924(6) 0.2969(7) 0.4041(6) 0.0125 1.0000 Uani F2 F 0.3773(6) 0.0373(7) 0.1777(5) 0.0112 1.0000 Uani F1 F 0.6352(6) 0.4259(7) 0.0446(6) 0.0111 1.0000 Uani F3 F 0.6486(6) 0.1540(7) 0.2633(6) 0.0110 1.0000 Uani F5 F 0.1664(6) 0.3520(7) 0.0829(6) 0.0152 1.0000 Uani N1 N 0.0826(9) -0.1636(11) 0.0685(9) 0.0151 1.0000 Uani C2 C 0.0304(9) -0.0253(12) 0.1671(9) 0.0100 1.0000 Uani C1 C -0.113(1) 0.0752(13) 0.0727(9) 0.0125 1.0000 Uani H5 H 0.0054 -0.0890 0.2571 0.0113 1.0000 Uiso H6 H 0.1158 0.0662 0.2074 0.0113 1.0000 Uiso H4 H -0.1441 0.1721 0.1380 0.0160 1.0000 Uiso H3 H -0.1999 -0.0157 0.0388 0.0160 1.0000 Uiso H1 H 0.1766 -0.2298 0.1309 0.0188 1.0000 Uiso H2 H -0.0025 -0.2555 0.0288 0.0188 1.0000 Uiso 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 Th1 0.00585(18) 0.00427(18) 0.00399(18) 0.00022(11) 0.0018(1) -0.00009(12) F4 0.014(2) 0.009(2) 0.015(2) -0.000(2) 0.006(2) -0.002(2) F2 0.012(2) 0.009(2) 0.010(2) -0.0014(19) -0.0019(18) 0.001(2) F1 0.011(2) 0.008(2) 0.015(2) 0.006(2) 0.0047(18) 0.005(2) F3 0.012(2) 0.008(2) 0.013(2) -0.0010(19) 0.0044(18) -0.003(2) F5 0.017(3) 0.011(2) 0.018(3) -0.001(2) 0.007(2) -0.001(2) N1 0.015(4) 0.014(4) 0.016(4) 0.004(3) 0.004(3) 0.006(3) C2 0.007(4) 0.011(4) 0.009(4) -0.004(3) -0.003(3) -0.001(3) C1 0.014(4) 0.016(4) 0.010(4) 0.000(3) 0.006(3) -0.006(4) _refine_ls_extinction_coef 3.9(7) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Th1 . Th1 2_665 3.9459(5) yes Th1 . F4 . 2.376(5) yes Th1 . F4 4_554 2.441(5) yes Th1 . F2 . 2.364(5) yes Th1 . F2 3_655 2.371(5) yes Th1 . F1 . 2.351(5) yes Th1 . F1 2_665 2.360(5) yes Th1 . F3 . 2.415(5) yes Th1 . F3 3_655 2.464(5) yes Th1 . F5 . 2.279(5) yes N1 . C2 . 1.489(11) yes N1 . C1 2_555 1.502(11) yes N1 . H1 . 1.002 no N1 . H2 . 1.005 no C2 . C1 . 1.523(12) yes C2 . H5 . 1.003 no C2 . H6 . 1.005 no C1 . H4 . 1.000 no C1 . H3 . 1.005 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Th1 2_665 Th1 . F4 . 154.32(12) yes Th1 2_665 Th1 . F4 4_554 65.66(12) yes F4 . Th1 . F4 4_554 140.0(1) yes Th1 2_665 Th1 . F2 . 133.75(12) yes F4 . Th1 . F2 . 70.80(17) yes F4 4_554 Th1 . F2 . 70.19(17) yes Th1 2_665 Th1 . F2 3_655 80.38(12) yes F4 . Th1 . F2 3_655 76.27(17) yes F4 4_554 Th1 . F2 3_655 137.57(17) yes F2 . Th1 . F2 3_655 128.48(12) yes Th1 2_665 Th1 . F1 . 33.18(12) yes F4 . Th1 . F1 . 138.65(17) yes F4 4_554 Th1 . F1 . 69.58(17) yes F2 . Th1 . F1 . 116.72(18) yes F2 3_655 Th1 . F1 . 68.09(18) yes Th1 2_665 Th1 . F1 2_665 33.03(11) yes F4 . Th1 . F1 2_665 139.39(17) yes F4 4_554 Th1 . F1 2_665 70.03(17) yes F2 . Th1 . F1 2_665 135.09(17) yes F2 3_655 Th1 . F1 2_665 95.29(17) yes Th1 2_665 Th1 . F3 . 103.84(12) yes F4 . Th1 . F3 . 79.53(17) yes F4 4_554 Th1 . F3 . 90.39(17) yes F2 . Th1 . F3 . 62.82(16) yes F2 3_655 Th1 . F3 . 73.20(17) yes Th1 2_665 Th1 . F3 3_655 84.06(11) yes F4 . Th1 . F3 3_655 75.68(17) yes F4 4_554 Th1 . F3 3_655 133.32(17) yes F2 . Th1 . F3 3_655 139.06(17) yes F2 3_655 Th1 . F3 3_655 61.98(17) yes Th1 2_665 Th1 . F5 . 107.01(13) yes F4 . Th1 . F5 . 82.80(18) yes F4 4_554 Th1 . F5 . 81.31(17) yes F2 . Th1 . F5 . 78.64(17) yes F2 3_655 Th1 . F5 . 134.94(18) yes F1 . Th1 . F1 2_665 66.22(19) yes F1 . Th1 . F3 . 70.81(16) yes F1 2_665 Th1 . F3 . 136.67(16) yes F1 . Th1 . F3 3_655 103.91(17) yes F1 2_665 Th1 . F3 3_655 65.64(17) yes F3 . Th1 . F3 3_655 132.55(9) yes F1 . Th1 . F5 . 137.80(18) yes F1 2_665 Th1 . F5 . 75.59(17) yes F3 . Th1 . F5 . 141.03(17) yes F3 3_655 Th1 . F5 . 74.42(17) yes Th1 . F4 . Th1 4_555 157.0(2) yes Th1 . F2 . Th1 3_645 118.2(2) yes Th1 . F1 . Th1 2_665 113.78(19) yes Th1 . F3 . Th1 3_645 112.7(2) yes C2 . N1 . C1 2_555 111.2(7) yes C2 . N1 . H1 . 109.790 no C1 2_555 N1 . H1 . 111.541 no C2 . N1 . H2 . 109.490 no C1 2_555 N1 . H2 . 105.709 no H1 . N1 . H2 . 108.967 no N1 . C2 . C1 . 109.9(7) yes N1 . C2 . H5 . 109.507 no C1 . C2 . H5 . 109.683 no N1 . C2 . H6 . 109.536 no C1 . C2 . H6 . 109.334 no H5 . C2 . H6 . 108.850 no N1 2_555 C1 . C2 . 111.3(7) yes N1 2_555 C1 . H4 . 109.257 no C2 . C1 . H4 . 109.554 no N1 2_555 C1 . H3 . 108.710 no C2 . C1 . H3 . 108.938 no H4 . C1 . H3 . 109.004 no data_CRYSTALS_cif _database_code_CSD 189999 _audit_creation_date 02-12-08 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================= _cell_length_a 6.8048(2) _cell_angle_alpha 90 _cell_length_b 17.6478(6) _cell_angle_beta 90 _cell_length_c 17.7611(7) _cell_angle_gamma 90 _cell_volume 2132.9 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P c n b ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y,z+1/2' 'x+1/2,-y,-z+1/2' 'x+1/2,-y+1/2,z+1/2' '-x+1/2,y+1/2,-z+1/2' '-x,-y+1/2,z' 'x,y+1/2,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Th ' -8.1270 8.8700 35.5645 0.5634 23.4219 3.4620 12.7473 17.8309 4.8070 99.1722 13.4314 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C5 H14 F6 N2 O0.50 Th1 ' _chemical_formula_moiety ' C5 H14 F6 N2 O0.50 Th1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 456.21 _cell_measurement_reflns_used 2682 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' colorless ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 2.841 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1585.162 _exptl_absorpt_coefficient_mu 14.039 # Sheldrick geometric definitions 0.33 0.76 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.76 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 4797 _reflns_number_total 2423 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 2423 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2441 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_gt 1683 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _refine_diff_density_min -1.41 _refine_diff_density_max 1.72 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 1683 _refine_ls_number_parameters 142 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0739 _refine_ls_goodness_of_fit_ref 0.8380 _refine_ls_shift/su_max 0.000128 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 11.9 17.8 10.2 3.88 1.13 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type TH1 TH 0.07915(4) 0.035451(15) 0.282378(15) 0.0154 1.0000 Uani F2 F 0.3752(7) 0.0789(3) 0.2239(3) 0.0244 1.0000 Uani F1 F 0.0204(8) -0.0114(4) 0.4021(3) 0.0401 1.0000 Uani F4 F -0.2608(8) 0.0555(3) 0.3006(3) 0.0243 1.0000 Uani F5 F 0.3754(7) -0.0194(3) 0.3305(3) 0.0235 1.0000 Uani F3 F 0.0202(9) 0.1511(3) 0.2244(4) 0.0395 1.0000 Uani F6 F 0.1612(11) 0.1276(4) 0.3633(4) 0.0562 1.0000 Uani O1 O 0.0000 0.2500 0.4374(9) 0.1645 1.0000 Uani N1 N -0.2964(14) 0.2367(5) 0.2374(6) 0.0478 1.0000 Uani N2 N -0.2948(16) 0.0008(9) 0.4871(6) 0.0702 1.0000 Uani C1 C -0.4109(17) 0.2254(6) 0.3048(6) 0.0393 1.0000 Uani C4 C -0.409(2) 0.0687(8) 0.4739(6) 0.0488 1.0000 Uani C2 C -0.4038(16) 0.2273(5) 0.1650(6) 0.0369 1.0000 Uani C5 C -0.4028(16) -0.0717(8) 0.4824(6) 0.0456 1.0000 Uani C3 C -0.277(5) 0.2414(16) 0.1044(13) 0.0630 0.5000 Uani C6 C -0.315(7) 0.129(3) 0.4890(19) 0.1197 0.5000 Uani H6 H -0.3282 0.2373 0.3503 0.0483 1.0000 Uiso H5 H -0.4522 0.1708 0.3075 0.0483 1.0000 Uiso H1 H -0.2389 0.2892 0.2392 0.0393 1.0000 Uiso H2 H -0.1825 0.1993 0.2384 0.0393 1.0000 Uiso H11 H -0.4385 0.0642 0.4187 0.0605 1.0000 Uiso H7 H -0.4528 0.1738 0.1583 0.0462 1.0000 Uiso H13 H -0.3171 -0.1139 0.5032 0.0576 1.0000 Uiso H12 H -0.4310 -0.0834 0.4282 0.0576 1.0000 Uiso H8 H -0.3428 0.2340 0.0548 0.0771 0.5000 Uiso H9 H -0.2182 0.2929 0.1073 0.0771 0.5000 Uiso H10 H -0.1607 0.2031 0.1062 0.0771 0.5000 Uiso H14 H -0.1804 0.1331 0.4603 0.1162 0.5000 Uiso H15 H -0.2812 0.1369 0.5436 0.1162 0.5000 Uiso H16 H -0.3881 0.1779 0.4721 0.1162 0.5000 Uiso H3 H -0.2349 0.0051 0.5391 0.0600 1.0000 Uiso H4 H -0.1826 -0.0001 0.4496 0.0600 1.0000 Uiso H17 H 0.0425 0.2043 0.4111 0.0500 1.0000 Uiso 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 Th1 0.00749(17) 0.01761(18) 0.02103(18) 0.00004(12) 0.00034(13) 0.00013(11) F2 0.016(2) 0.019(2) 0.039(3) 0.006(2) -0.001(2) 0.0030(18) F1 0.019(3) 0.078(4) 0.023(3) 0.008(3) -0.002(2) -0.006(3) F4 0.013(2) 0.029(2) 0.031(2) -0.004(2) 0.003(2) -0.000(2) F5 0.019(2) 0.026(3) 0.025(2) 0.0030(19) 0.0035(19) 0.0008(19) F3 0.020(3) 0.025(3) 0.074(4) 0.012(3) 0.001(3) -0.001(2) F6 0.056(4) 0.051(4) 0.062(4) -0.032(4) -0.004(4) -0.003(3) O1 0.31(3) 0.147(17) 0.040(8) 0.0000 0.0000 0.18(2) N1 0.030(5) 0.035(5) 0.078(7) 0.000(5) 0.005(5) 0.004(4) N2 0.032(6) 0.129(11) 0.049(6) 0.011(7) 0.011(5) 0.014(7) C1 0.037(6) 0.031(5) 0.050(6) -0.001(4) -0.014(5) 0.003(5) C4 0.045(7) 0.074(8) 0.027(5) -0.001(5) -0.001(6) -0.006(7) C2 0.034(5) 0.028(5) 0.049(6) -0.005(4) 0.001(5) -0.001(4) C5 0.023(5) 0.075(8) 0.039(6) 0.004(6) 0.003(5) 0.010(6) C3 0.09(2) 0.064(15) 0.039(11) 0.017(12) -0.005(15) -0.004(17) C6 0.09(3) 0.22(5) 0.046(17) 0.03(3) -0.025(18) -0.04(4) _refine_ls_extinction_coef 18.9(35) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Th1 . Th1 4_455 3.8033(2) yes Th1 . Th1 4_555 3.8033(2) yes Th1 . F2 . 2.393(5) yes Th1 . F2 4_455 2.452(5) yes Th1 . F1 . 2.316(5) yes Th1 . F4 . 2.362(5) yes Th1 . F4 4_555 2.436(5) yes Th1 . F5 . 2.394(5) yes Th1 . F5 4_455 2.454(5) yes Th1 . F3 . 2.322(6) yes Th1 . F6 . 2.241(6) yes O1 . H17 . 0.976 no O1 . H17 7_555 0.976 no N1 . C1 . 1.442(15) yes N1 . C2 . 1.487(15) yes N1 . H1 . 1.007 no N1 . H2 . 1.018 no N2 . C4 . 1.449(19) yes N2 . C5 . 1.477(19) yes N2 . H3 . 1.013 no N2 . H4 . 1.014 no C1 . C1 7_455 1.49(2) yes C1 . H6 . 1.007 no C1 . H5 . 1.005 no C4 . C5 2_456 1.498(16) yes C4 . C6 . 1.27(5) yes C4 . H11 . 1.004 no C2 . C2 7_455 1.53(2) yes C2 . C3 . 1.40(3) yes C2 . H7 . 1.010 no C5 . H13 . 1.016 no C5 . H12 . 1.003 no C3 . H8 . 0.995 no C3 . H9 . 0.996 no C3 . H10 . 1.044 no C6 . H14 . 1.050 no C6 . H15 . 1.007 no C6 . H16 . 1.039 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Th1 4_455 Th1 . Th1 4_555 126.914(15) yes Th1 4_455 Th1 . F2 . 136.67(13) yes Th1 4_555 Th1 . F2 . 38.84(11) yes Th1 4_455 Th1 . F2 4_455 37.73(12) yes Th1 4_555 Th1 . F2 4_455 102.81(12) yes F2 . Th1 . F2 4_455 136.12(9) yes Th1 4_455 Th1 . F1 . 90.33(14) yes Th1 4_555 Th1 . F1 . 108.34(15) yes F2 . Th1 . F1 . 131.17(19) yes F2 4_455 Th1 . F1 . 69.5(2) yes Th1 4_455 Th1 . F4 . 38.26(12) yes Th1 4_555 Th1 . F4 . 165.17(12) yes F2 . Th1 . F4 . 146.67(16) yes F2 4_455 Th1 . F4 . 64.88(17) yes F1 . Th1 . F4 . 76.06(19) yes Th1 4_455 Th1 . F4 4_555 90.01(12) yes Th1 4_555 Th1 . F4 4_555 36.90(12) yes F2 . Th1 . F4 4_555 64.69(17) yes F2 4_455 Th1 . F4 4_555 71.52(17) yes F1 . Th1 . F4 4_555 113.4(2) yes Th1 4_455 Th1 . F5 . 136.74(12) yes Th1 4_555 Th1 . F5 . 38.89(12) yes F2 . Th1 . F5 . 64.89(17) yes F2 4_455 Th1 . F5 . 99.21(16) yes F1 . Th1 . F5 . 70.93(19) yes Th1 4_455 Th1 . F5 4_455 37.77(12) yes Th1 4_555 Th1 . F5 4_455 102.73(12) yes F2 . Th1 . F5 4_455 99.10(17) yes F2 4_455 Th1 . F5 4_455 63.13(17) yes F1 . Th1 . F5 4_455 127.68(18) yes Th1 4_455 Th1 . F3 . 90.04(15) yes Th1 4_555 Th1 . F3 . 108.04(15) yes F2 . Th1 . F3 . 70.78(19) yes F2 4_455 Th1 . F3 . 127.30(19) yes F1 . Th1 . F3 . 133.7(2) yes Th1 4_455 Th1 . F6 . 131.0(2) yes Th1 4_555 Th1 . F6 . 102.1(2) yes F2 . Th1 . F6 . 80.6(2) yes F2 4_455 Th1 . F6 . 140.1(2) yes F1 . Th1 . F6 . 73.3(3) yes F4 . Th1 . F4 4_555 128.27(15) yes F4 . Th1 . F5 . 146.76(16) yes F4 4_555 Th1 . F5 . 64.72(17) yes F4 . Th1 . F5 4_455 64.90(17) yes F4 4_555 Th1 . F5 4_455 71.48(17) yes F5 . Th1 . F5 4_455 136.1(1) yes F4 . Th1 . F3 . 76.09(19) yes F4 4_555 Th1 . F3 . 112.9(2) yes F5 . Th1 . F3 . 131.25(18) yes F5 4_455 Th1 . F3 . 69.0(2) yes F4 . Th1 . F6 . 92.7(2) yes F4 4_555 Th1 . F6 . 139.0(2) yes F5 . Th1 . F6 . 81.6(2) yes F5 4_455 Th1 . F6 . 138.5(2) yes F3 . Th1 . F6 . 71.9(3) yes Th1 . F2 . Th1 4_555 103.43(18) yes Th1 . F4 . Th1 4_455 104.84(19) yes Th1 . F5 . Th1 4_555 103.35(18) yes H17 . O1 . H17 7_555 122.800 no C1 . N1 . C2 . 115.8(9) yes C1 . N1 . H1 . 108.019 no C2 . N1 . H1 . 108.727 no C1 . N1 . H2 . 107.876 no C2 . N1 . H2 . 108.574 no H1 . N1 . H2 . 107.507 no C4 . N2 . C5 . 116.1(10) yes C4 . N2 . H3 . 107.603 no C5 . N2 . H3 . 108.527 no C4 . N2 . H4 . 108.102 no C5 . N2 . H4 . 108.881 no H3 . N2 . H4 . 107.316 no N1 . C1 . C1 7_455 111.1(7) yes N1 . C1 . H6 . 109.615 no C1 7_455 C1 . H6 . 109.445 no N1 . C1 . H5 . 108.844 no C1 7_455 C1 . H5 . 109.328 no H6 . C1 . H5 . 108.513 no N2 . C4 . C5 2_456 113.8(11) yes N2 . C4 . C6 . 112.8(25) yes C5 2_456 C4 . C6 . 106.9(24) yes N2 . C4 . H11 . 101.561 no C5 2_456 C4 . H11 . 109.927 no C6 . C4 . H11 . 111.797 no N1 . C2 . C2 7_455 111.2(6) yes N1 . C2 . C3 . 110.1(14) yes C2 7_455 C2 . C3 . 115.6(14) yes N1 . C2 . H7 . 111.574 no C2 7_455 C2 . H7 . 101.882 no C3 . C2 . H7 . 106.147 no N2 . C5 . C4 2_456 111.3(11) yes N2 . C5 . H13 . 109.191 no C4 2_456 C5 . H13 . 109.079 no N2 . C5 . H12 . 109.172 no C4 2_456 C5 . H12 . 109.982 no H13 . C5 . H12 . 108.003 no C2 . C3 . H8 . 112.540 no C2 . C3 . H9 . 111.763 no H8 . C3 . H9 . 110.190 no C2 . C3 . H10 . 109.227 no H8 . C3 . H10 . 106.449 no H9 . C3 . H10 . 106.337 no C4 . C6 . H14 . 113.188 no C4 . C6 . H15 . 115.577 no H14 . C6 . H15 . 105.104 no C4 . C6 . H16 . 113.027 no H14 . C6 . H16 . 102.866 no H15 . C6 . H16 . 105.926 no