data_2100398 loop_ _publ_author_name 'M. Helliwell' 'D. Collison' 'G. H. John' 'I. May' 'M. J. Sarsfield' 'C. A. Sharrad' 'A. D. Sutton' _publ_section_title ; Temperature-resolved study of three [M(M'O4)4(TBPO)4] complexes (MM' = URe, ThRe, ThTc) ; _journal_coeditor_code WS5025 _journal_date_accepted 2005-11-09 _journal_date_recd_electronic 2005-02-24 _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section B' _journal_page_first 68 _journal_page_last 85 _journal_paper_category FA _journal_volume 62 _journal_year 2006 _chemical_formula_sum 'C48 H108 O20 P4 Re4 Th' _chemical_formula_weight 2106.06 _chemical_melting_point ? _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42m _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 15.5577(12) _cell_length_b 15.5577(12) _cell_length_c 14.8730(17) _cell_measurement_reflns_used 1544 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.51 _cell_measurement_theta_min 2.74 _cell_volume 3599.9(6) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5728 _diffrn_reflns_theta_full 26.39 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_theta_min 1.85 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 8.906 _exptl_absorpt_correction_T_max 0.4696 _exptl_absorpt_correction_T_min 0.2970 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2012 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.787 _refine_diff_density_min -0.591 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(4) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 102 _refine_ls_number_reflns 1932 _refine_ls_number_restraints 95 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0442 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.1166 _reflns_number_gt 1605 _reflns_number_total 1932 _reflns_threshold_expression >2sigma(I) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x, y, -z' 'x, -y, -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' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Th1 0.5000 0.5000 0.5000 0.0554(3) Uani d SU 1 . . Th Re1 0.35587(3) 0.35587(3) 0.67317(4) 0.0863(3) Uani d SU 1 . . Re P1 0.3470(3) 0.3470(3) 0.3806(4) 0.124(2) Uani d SDU 1 . . P O1 0.4278(6) 0.4278(6) 0.6242(9) 0.104(3) Uani d SU 1 . . O O2 0.2561(7) 0.3779(11) 0.6402(9) 0.156(4) Uani d U 1 . . O O3 0.3608(9) 0.3608(9) 0.7830(9) 0.152(6) Uani d SU 1 . . O O4 0.4019(5) 0.4019(5) 0.4429(10) 0.106(4) Uani d SU 1 . . O C1 0.2387(9) 0.3958(17) 0.3955(18) 0.209(10) Uani d DU 1 . . C H1A 0.2318 0.4086 0.4589 0.250 Uiso calc R 1 . . H H1B 0.2387 0.4504 0.3640 0.250 Uiso calc R 1 . . H C2 0.1629(11) 0.3490(17) 0.367(2) 0.222(10) Uani d DU 1 . . C H2A 0.1647 0.2904 0.3892 0.266 Uiso calc R 1 . . H H2B 0.1598 0.3473 0.3017 0.266 Uiso calc R 1 . . H C3 0.0842(13) 0.3970(17) 0.406(2) 0.217(11) Uani d DU 1 . . C H3A 0.0765 0.3852 0.4694 0.261 Uiso calc R 1 . . H H3B 0.0884 0.4586 0.3966 0.261 Uiso calc R 1 . . H C4 0.0121(14) 0.3571(17) 0.3490(16) 0.212(11) Uani d DU 1 . . C H4A -0.0424 0.3793 0.3684 0.318 Uiso calc R 1 . . H H4B 0.0128 0.2957 0.3562 0.318 Uiso calc R 1 . . H H4C 0.0209 0.3712 0.2868 0.318 Uiso calc R 1 . . H C5 0.3937(16) 0.3937(16) 0.2812(15) 0.31(2) Uani d SDU 1 . . C H5A 0.3837 0.4553 0.2801 0.367 Uiso calc PR 0.50 . . H H5B 0.4553 0.3837 0.2801 0.367 Uiso calc PR 0.50 . . H C6 0.3519(17) 0.3519(17) 0.2023(18) 0.32(2) Uani d SDU 1 . . C H6A 0.2903 0.3619 0.2036 0.382 Uiso calc PR 0.50 . . H H6B 0.3619 0.2903 0.2036 0.382 Uiso calc PR 0.50 . . H C7 0.3915(16) 0.3915(16) 0.1167(17) 0.30(2) Uani d SDU 1 . . C H7A 0.3814 0.4530 0.1149 0.354 Uiso calc PR 0.50 . . H H7B 0.4530 0.3814 0.1149 0.354 Uiso calc PR 0.50 . . H C8 0.347(2) 0.347(2) 0.037(2) 0.35(3) Uani d SDU 1 . . C H8A 0.3687 0.3705 -0.0181 0.528 Uiso calc SR 1 . . H H8B 0.2863 0.3566 0.0408 0.528 Uiso calc PR 0.50 . . H H8C 0.3587 0.2866 0.0393 0.528 Uiso calc PR 0.50 . . H 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 Th1 0.0521(3) 0.0521(3) 0.0620(5) 0.000 0.000 0.000 Re1 0.0868(4) 0.0868(4) 0.0853(4) -0.0083(4) 0.0170(3) 0.0170(3) P1 0.128(3) 0.128(3) 0.115(4) -0.060(4) -0.0159(19) -0.0159(19) O1 0.103(5) 0.103(5) 0.107(7) -0.013(7) 0.023(4) 0.023(4) O2 0.098(6) 0.191(12) 0.178(10) -0.002(7) 0.002(6) 0.019(10) O3 0.184(9) 0.184(9) 0.089(6) -0.006(15) 0.028(5) 0.028(5) O4 0.097(5) 0.097(5) 0.126(8) -0.038(7) -0.017(4) -0.017(4) C1 0.130(7) 0.29(3) 0.209(18) -0.032(11) -0.070(10) -0.048(19) C2 0.128(8) 0.24(2) 0.30(2) -0.018(12) 0.020(15) -0.097(19) C3 0.150(10) 0.20(2) 0.31(3) 0.004(15) 0.062(17) -0.085(19) C4 0.142(11) 0.25(3) 0.25(3) 0.017(16) 0.045(18) -0.04(3) C5 0.40(3) 0.40(3) 0.120(9) 0.10(4) 0.087(16) 0.087(16) C6 0.41(3) 0.41(3) 0.140(9) 0.12(4) 0.076(18) 0.076(18) C7 0.38(3) 0.38(3) 0.124(11) 0.14(4) 0.069(18) 0.069(18) C8 0.45(4) 0.45(4) 0.154(13) 0.08(6) 0.05(2) 0.05(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 Th1 O4 4_656 . 97.7(3) ? O4 Th1 O4 4_656 3_566 137.0(7) ? O4 Th1 O4 . 3_566 97.7(3) ? O4 Th1 O4 4_656 2_665 97.7(3) ? O4 Th1 O4 . 2_665 137.0(7) ? O4 Th1 O4 3_566 2_665 97.7(3) ? O4 Th1 O1 4_656 . 73.9(3) ? O4 Th1 O1 . . 70.8(5) ? O4 Th1 O1 3_566 . 73.9(3) ? O4 Th1 O1 2_665 . 152.2(5) ? O4 Th1 O1 4_656 4_656 70.8(5) ? O4 Th1 O1 . 4_656 73.9(3) ? O4 Th1 O1 3_566 4_656 152.2(5) ? O4 Th1 O1 2_665 4_656 73.9(3) ? O1 Th1 O1 . 4_656 125.1(4) ? O4 Th1 O1 4_656 2_665 73.9(3) ? O4 Th1 O1 . 2_665 152.2(5) ? O4 Th1 O1 3_566 2_665 73.9(3) ? O4 Th1 O1 2_665 2_665 70.8(5) ? O1 Th1 O1 . 2_665 81.4(7) ? O1 Th1 O1 4_656 2_665 125.1(4) ? O4 Th1 O1 4_656 3_566 152.2(5) ? O4 Th1 O1 . 3_566 73.9(3) ? O4 Th1 O1 3_566 3_566 70.8(5) ? O4 Th1 O1 2_665 3_566 73.9(3) ? O1 Th1 O1 . 3_566 125.1(4) ? O1 Th1 O1 4_656 3_566 81.4(7) ? O1 Th1 O1 2_665 3_566 125.1(4) ? O3 Re1 O2 . 8 109.2(6) ? O3 Re1 O2 . . 109.2(6) ? O2 Re1 O2 8 . 107.3(12) ? O3 Re1 O1 . . 110.9(8) ? O2 Re1 O1 8 . 110.1(6) ? O2 Re1 O1 . . 110.1(6) ? O4 P1 C5 . . 92.7(13) ? O4 P1 C1 . . 101.9(7) ? C5 P1 C1 . . 107.4(10) ? O4 P1 C1 . 8 101.9(7) ? C5 P1 C1 . 8 107.4(10) ? C1 P1 C1 . 8 136.4(18) ? Re1 O1 Th1 . . 155.4(8) ? P1 O4 Th1 . . 164.0(9) ? C2 C1 P1 . . 119.7(15) ? C2 C1 H1A . . 107.4 ? P1 C1 H1A . . 107.4 ? C2 C1 H1B . . 107.4 ? P1 C1 H1B . . 107.4 ? H1A C1 H1B . . 106.9 ? C1 C2 C3 . . 106.9(16) ? C1 C2 H2A . . 110.3 ? C3 C2 H2A . . 110.3 ? C1 C2 H2B . . 110.3 ? C3 C2 H2B . . 110.3 ? H2A C2 H2B . . 108.6 ? C4 C3 C2 . . 100.1(16) ? C4 C3 H3A . . 111.7 ? C2 C3 H3A . . 111.7 ? C4 C3 H3B . . 111.7 ? C2 C3 H3B . . 111.7 ? H3A C3 H3B . . 109.5 ? C3 C4 H4A . . 109.5 ? C3 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C3 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C6 C5 P1 . . 107(2) ? C6 C5 H5A . . 110.3 ? P1 C5 H5A . . 110.3 ? C6 C5 H5B . . 110.3 ? P1 C5 H5B . . 110.3 ? H5A C5 H5B . . 108.6 ? C5 C6 C7 . . 107(2) ? C5 C6 H6A . . 110.2 ? C7 C6 H6A . . 110.2 ? C5 C6 H6B . . 110.2 ? C7 C6 H6B . . 110.2 ? H6A C6 H6B . . 108.5 ? C8 C7 C6 . . 106(2) ? C8 C7 H7A . . 110.5 ? C6 C7 H7A . . 110.5 ? C8 C7 H7B . . 110.5 ? C6 C7 H7B . . 110.5 ? H7A C7 H7B . . 108.7 ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Th1 O4 4_656 2.320(11) ? Th1 O4 . 2.320(11) ? Th1 O4 3_566 2.320(11) ? Th1 O4 2_665 2.320(11) ? Th1 O1 . 2.436(11) ? Th1 O1 4_656 2.436(11) ? Th1 O1 2_665 2.436(11) ? Th1 O1 3_566 2.436(11) ? Re1 O3 . 1.637(14) ? Re1 O2 8 1.664(11) ? Re1 O2 . 1.664(11) ? Re1 O1 . 1.742(12) ? P1 O4 . 1.522(12) ? P1 C5 . 1.800(18) ? P1 C1 . 1.862(15) ? P1 C1 8 1.862(15) ? C1 C2 . 1.449(17) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 C3 . 1.548(17) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 C4 . 1.536(18) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? C5 C6 . 1.49(2) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 C7 . 1.544(19) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? C7 C8 . 1.53(2) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? 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 O3 Re1 O1 Th1 . . . . 180.000(2) ? O2 Re1 O1 Th1 8 . . . 59.1(6) ? O2 Re1 O1 Th1 . . . . -59.1(6) ? O4 Th1 O1 Re1 4_656 . . . -104.4(3) ? O4 Th1 O1 Re1 . . . . 0.000(2) ? O4 Th1 O1 Re1 3_566 . . . 104.4(3) ? O4 Th1 O1 Re1 2_665 . . . 179.9990(10) ? O1 Th1 O1 Re1 4_656 . . . -52.83(14) ? O1 Th1 O1 Re1 2_665 . . . 180.000(2) ? O1 Th1 O1 Re1 3_566 . . . 52.83(14) ? C5 P1 O4 Th1 . . . . 0.000(2) ? C1 P1 O4 Th1 . . . . -108.4(10) ? C1 P1 O4 Th1 8 . . . 108.4(10) ? O4 Th1 O4 P1 4_656 . . . -110.1(3) ? O4 Th1 O4 P1 3_566 . . . 110.1(3) ? O4 Th1 O4 P1 2_665 . . . 0.001(4) ? O1 Th1 O4 P1 . . . . 180.000(3) ? O1 Th1 O4 P1 4_656 . . . -42.7(3) ? O1 Th1 O4 P1 2_665 . . . 179.999(2) ? O1 Th1 O4 P1 3_566 . . . 42.7(3) ? O4 P1 C1 C2 . . . . -163(3) ? C5 P1 C1 C2 . . . . 100(3) ? C1 P1 C1 C2 8 . . . -42(4) ? P1 C1 C2 C3 . . . . 168(2) ? C1 C2 C3 C4 . . . . 164(3) ? O4 P1 C5 C6 . . . . 180.000(2) ? C1 P1 C5 C6 . . . . -76.6(8) ? C1 P1 C5 C6 8 . . . 76.6(8) ? P1 C5 C6 C7 . . . . 180.000(2) ? C5 C6 C7 C8 . . . . 180.000(3) ?