#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/27/2012720.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012720 loop_ _publ_author_name 'Hill, Nicholas J.' 'Leung, Lai-Shi' 'Levason, William' 'Webster, Michael' _publ_section_title ; Tetraaquatetrakis(trimethylphosphine oxide-\kO)cerium(III) trichloride trihydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m295 _journal_page_last m296 _journal_paper_doi 10.1107/S0108270102004766 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Ce (C3 H9 O P)4 (H2 O)4] Cl3 , 3H2 O' _chemical_formula_moiety 'C12 H44 Ce O8 P4 3+ , 3Cl - , 3H2 O' _chemical_formula_sum 'C12 H50 Ce Cl3 O11 P4' _chemical_formula_weight 740.87 _chemical_name_systematic ; Tetraaquatetrakis(trimethylphosphine oxide-\kO)cerium(III) trichloride trihydrate ; _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 _audit_creation_method 'SHELXL97 + template + hand edit' _cell_angle_alpha 70.406(10) _cell_angle_beta 82.483(10) _cell_angle_gamma 74.161(10) _cell_formula_units_Z 2 _cell_length_a 10.2753(10) _cell_length_b 11.1003(10) _cell_length_c 15.6822(15) _cell_measurement_reflns_used 12600 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 1619.6(3) _computing_cell_refinement 'COLLECT and DENZO' _computing_data_collection 'COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'COLLECT and DENZO' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.955 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_sigmaI/netI 0.055 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 18262 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 3.15 _exptl_absorpt_coefficient_mu 1.889 _exptl_absorpt_correction_T_max 0.739 _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 758 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.61 _refine_diff_density_min -0.88 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 281 _refine_ls_number_reflns 5444 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.6782P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.061 _refine_ls_wR_factor_ref 0.064 _reflns_number_gt 4908 _reflns_number_total 5444 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1541.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2012720 _cod_database_fobs_code 2012720 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ce1 0.170923(14) 0.447541(15) 0.236975(10) 0.00969(7) Uani d . 1 . . Ce Cl1 0.66467(8) 0.13714(8) 0.95434(5) 0.02455(18) Uani d . 1 . . Cl Cl2 0.79567(7) 0.46661(8) 0.46286(5) 0.02255(18) Uani d . 1 . . Cl Cl3 0.81261(8) 0.15098(7) 0.27890(5) 0.02305(18) Uani d . 1 . . Cl P1 0.45924(7) 0.53612(8) 0.30830(5) 0.01389(17) Uani d . 1 . . P P2 0.13475(8) 0.27826(8) 0.07704(5) 0.01521(17) Uani d . 1 . . P P3 0.21974(8) 0.12407(8) 0.43087(5) 0.01755(18) Uani d . 1 . . P P4 -0.02876(8) 0.78827(7) 0.21972(5) 0.01511(17) Uani d . 1 . . P O1 0.31975(19) 0.54269(19) 0.28467(13) 0.0167(4) Uani d . 1 . . O O2 0.1148(2) 0.38855(19) 0.11687(13) 0.0178(5) Uani d . 1 . . O O3 0.2181(2) 0.2225(2) 0.33801(13) 0.0205(5) Uani d . 1 . . O O4 0.0266(2) 0.66530(18) 0.19285(13) 0.0171(4) Uani d . 1 . . O O5 0.2950(2) 0.57446(19) 0.09564(13) 0.0172(5) Uani d . 1 . . O O6 -0.0693(2) 0.3978(2) 0.28078(13) 0.0194(5) Uani d . 1 . . O O7 0.0860(2) 0.4750(2) 0.38972(13) 0.0215(5) Uani d . 1 . . O O8 0.3968(2) 0.30949(19) 0.20133(14) 0.0207(5) Uani d . 1 . . O O9 0.6418(2) 0.3001(2) 0.09643(14) 0.0236(5) Uani d . 1 . . O O10 0.5393(2) 0.0538(2) 0.28094(14) 0.0250(5) Uani d . 1 . . O O11 0.4524(2) 0.0460(2) 0.86491(15) 0.0305(6) Uani d . 1 . . O C1 0.5285(3) 0.3828(3) 0.3900(2) 0.0238(7) Uani d . 1 . . C H1A 0.4672 0.3691 0.4439 0.0419 Uiso calc R 1 . . H H1B 0.6167 0.3835 0.4069 0.0419 Uiso calc R 1 . . H H1C 0.5399 0.3112 0.3643 0.0419 Uiso calc R 1 . . H C2 0.5748(3) 0.5549(3) 0.2123(2) 0.0227(7) Uani d . 1 . . C H2A 0.5398 0.6390 0.1658 0.0419 Uiso calc R 1 . . H H2B 0.5853 0.4822 0.1878 0.0419 Uiso calc R 1 . . H H2C 0.6628 0.5540 0.2305 0.0419 Uiso calc R 1 . . H C3 0.4572(3) 0.6642(3) 0.3538(2) 0.0220(7) Uani d . 1 . . C H3A 0.4194 0.7501 0.3099 0.0419 Uiso calc R 1 . . H H3B 0.5498 0.6595 0.3662 0.0419 Uiso calc R 1 . . H H3C 0.4012 0.6532 0.4102 0.0419 Uiso calc R 1 . . H C4 0.1849(3) 0.1205(3) 0.1596(2) 0.0269(8) Uani d . 1 . . C H4A 0.2697 0.1136 0.1852 0.0419 Uiso calc R 1 . . H H4B 0.1983 0.0516 0.1310 0.0419 Uiso calc R 1 . . H H4C 0.1142 0.1095 0.2080 0.0419 Uiso calc R 1 . . H C5 -0.0185(3) 0.2855(3) 0.0333(2) 0.0238(7) Uani d . 1 . . C H5A -0.0895 0.2798 0.0817 0.0419 Uiso calc R 1 . . H H5B -0.0055 0.2118 0.0094 0.0419 Uiso calc R 1 . . H H5C -0.0454 0.3690 -0.0155 0.0419 Uiso calc R 1 . . H C6 0.2602(4) 0.2892(4) -0.0131(3) 0.0413(10) Uani d . 1 . . C H6A 0.3463 0.2853 0.0094 0.0419 Uiso calc R 1 . . H H6B 0.2317 0.3728 -0.0615 0.0419 Uiso calc R 1 . . H H6C 0.2716 0.2155 -0.0368 0.0419 Uiso calc R 1 . . H C7 0.2723(3) -0.0406(3) 0.4263(2) 0.0251(7) Uani d . 1 . . C H7A 0.2114 -0.0532 0.3885 0.0419 Uiso calc R 1 . . H H7B 0.2693 -0.1027 0.4876 0.0419 Uiso calc R 1 . . H H7C 0.3649 -0.0565 0.4001 0.0419 Uiso calc R 1 . . H C8 0.0585(4) 0.1418(3) 0.4892(2) 0.0331(9) Uani d . 1 . . C H8A -0.0083 0.1347 0.4530 0.0419 Uiso calc R 1 . . H H8B 0.0311 0.2282 0.4988 0.0419 Uiso calc R 1 . . H H8C 0.0639 0.0721 0.5479 0.0419 Uiso calc R 1 . . H C9 0.3347(4) 0.1376(4) 0.5003(2) 0.0327(9) Uani d . 1 . . C H9A 0.4253 0.1281 0.4707 0.0419 Uiso calc R 1 . . H H9B 0.3372 0.0682 0.5590 0.0419 Uiso calc R 1 . . H H9C 0.3050 0.2242 0.5097 0.0419 Uiso calc R 1 . . H C10 -0.0588(3) 0.9334(3) 0.1237(2) 0.0219(7) Uani d . 1 . . C H10A 0.0254 0.9383 0.0867 0.0419 Uiso calc R 1 . . H H10B -0.0903 1.0113 0.1441 0.0419 Uiso calc R 1 . . H H10C -0.1280 0.9303 0.0875 0.0419 Uiso calc R 1 . . H C11 0.0850(3) 0.8126(3) 0.2858(2) 0.0225(7) Uani d . 1 . . C H11A 0.1724 0.8139 0.2525 0.0419 Uiso calc R 1 . . H H11B 0.0976 0.7405 0.3433 0.0419 Uiso calc R 1 . . H H11C 0.0472 0.8968 0.2979 0.0419 Uiso calc R 1 . . H C12 -0.1849(3) 0.7866(3) 0.2831(2) 0.0285(8) Uani d . 1 . . C H12A -0.1729 0.7079 0.3367 0.0419 Uiso calc R 1 . . H H12B -0.2531 0.7851 0.2454 0.0419 Uiso calc R 1 . . H H12C -0.2148 0.8657 0.3022 0.0419 Uiso calc R 1 . . H H5X 0.3027 0.6592 0.0926 0.030 Uiso d . 1 . . H H5Y 0.2778 0.5928 0.0405 0.030 Uiso d . 1 . . H H6X -0.1092 0.4167 0.3234 0.030 Uiso d . 1 . . H H6Y -0.0969 0.3283 0.2802 0.030 Uiso d . 1 . . H H7X 0.0018 0.4834 0.4183 0.030 Uiso d . 1 . . H H7Y 0.1436 0.4850 0.4297 0.030 Uiso d . 1 . . H H8X 0.4244 0.2223 0.2363 0.030 Uiso d . 1 . . H H8Y 0.4698 0.3282 0.1634 0.030 Uiso d . 1 . . H H9X 0.6823 0.2483 0.1518 0.030 Uiso d . 1 . . H H9Y 0.6558 0.2215 0.0834 0.030 Uiso d . 1 . . H H10X 0.6168 0.0787 0.2753 0.030 Uiso d . 1 . . H H10Y 0.5488 0.0223 0.2325 0.030 Uiso d . 1 . . H H11X 0.4221 -0.0040 0.9144 0.030 Uiso d . 1 . . H H11Y 0.5332 0.0363 0.8929 0.030 Uiso d . 1 . . 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 Ce1 0.00884(11) 0.01139(10) 0.01005(10) -0.00222(6) -0.00039(6) -0.00514(7) Cl1 0.0271(5) 0.0225(4) 0.0279(4) -0.0097(3) 0.0001(3) -0.0104(3) Cl2 0.0144(4) 0.0417(5) 0.0187(4) -0.0116(3) 0.0030(3) -0.0163(4) Cl3 0.0224(4) 0.0231(4) 0.0274(4) -0.0058(3) -0.0008(3) -0.0126(3) P1 0.0103(4) 0.0203(4) 0.0143(4) -0.0066(3) 0.0004(3) -0.0077(3) P2 0.0155(4) 0.0194(4) 0.0157(4) -0.0070(3) 0.0026(3) -0.0109(3) P3 0.0192(5) 0.0146(4) 0.0155(4) -0.0039(3) 0.0027(3) -0.0019(3) P4 0.0154(4) 0.0127(4) 0.0168(4) -0.0002(3) -0.0013(3) -0.0065(3) O1 0.0105(11) 0.0263(12) 0.0193(11) -0.0070(9) 0.0016(8) -0.0138(9) O2 0.0235(12) 0.0175(11) 0.0168(11) -0.0050(8) -0.0040(9) -0.0099(9) O3 0.0187(12) 0.0170(11) 0.0177(11) 0.0007(8) 0.0025(9) -0.0004(9) O4 0.0196(12) 0.0123(11) 0.0205(11) 0.0002(8) -0.0039(9) -0.0085(9) O5 0.0236(12) 0.0164(11) 0.0115(10) -0.0082(9) 0.0009(8) -0.0024(9) O6 0.0155(12) 0.0266(12) 0.0230(12) -0.0097(9) 0.0041(9) -0.0149(10) O7 0.0163(12) 0.0406(14) 0.0178(11) -0.0156(10) 0.0067(8) -0.0182(10) O8 0.0124(12) 0.0158(11) 0.0264(12) 0.0009(8) 0.0076(9) -0.0035(9) O9 0.0251(13) 0.0254(12) 0.0199(12) -0.0063(9) 0.0040(9) -0.0082(10) O10 0.0203(13) 0.0239(12) 0.0269(13) -0.0014(9) 0.0005(9) -0.0065(10) O11 0.0337(15) 0.0392(15) 0.0224(13) -0.0162(11) -0.0049(10) -0.0073(11) C1 0.0238(19) 0.0272(19) 0.0211(17) -0.0111(14) -0.0079(14) -0.0021(14) C2 0.0167(18) 0.0309(19) 0.0208(17) -0.0081(13) 0.0044(13) -0.0088(15) C3 0.0184(18) 0.0321(19) 0.0252(18) -0.0123(14) 0.0018(13) -0.0176(15) C4 0.0264(19) 0.0191(18) 0.038(2) -0.0005(14) -0.0096(15) -0.0130(15) C5 0.029(2) 0.0237(18) 0.0216(17) -0.0098(14) -0.0082(14) -0.0055(14) C6 0.039(2) 0.058(3) 0.040(2) -0.0261(19) 0.0216(17) -0.030(2) C7 0.0264(19) 0.0177(17) 0.0301(19) -0.0046(13) -0.0001(14) -0.0071(15) C8 0.029(2) 0.0250(19) 0.033(2) -0.0040(15) 0.0158(15) -0.0027(16) C9 0.047(2) 0.030(2) 0.0212(18) -0.0129(17) -0.0093(16) -0.0023(16) C10 0.0262(19) 0.0161(17) 0.0217(17) -0.0006(13) -0.0039(13) -0.0062(14) C11 0.031(2) 0.0150(16) 0.0238(18) -0.0025(13) -0.0077(14) -0.0092(14) C12 0.023(2) 0.0257(19) 0.0297(19) 0.0009(14) 0.0048(14) -0.0076(15) 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 '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 _geom_angle_publ_flag O2 Ce1 O4 95.04(7) ? O2 Ce1 O1 145.66(7) y O4 Ce1 O1 85.72(7) ? O2 Ce1 O3 93.30(7) ? O4 Ce1 O3 149.91(7) y O1 Ce1 O3 103.12(7) ? O2 Ce1 O8 79.32(7) ? O4 Ce1 O8 143.01(6) ? O1 Ce1 O8 79.73(7) ? O3 Ce1 O8 67.02(6) y O2 Ce1 O7 142.93(7) ? O4 Ce1 O7 78.93(7) ? O1 Ce1 O7 70.96(6) y O3 Ce1 O7 77.05(7) ? O8 Ce1 O7 126.33(7) ? O2 Ce1 O5 75.65(7) ? O4 Ce1 O5 75.84(7) y O1 Ce1 O5 71.26(6) ? O3 Ce1 O5 134.25(7) ? O8 Ce1 O5 67.32(6) y O7 Ce1 O5 135.61(6) ? O2 Ce1 O6 73.50(7) y O4 Ce1 O6 78.80(7) ? O1 Ce1 O6 139.51(6) ? O3 Ce1 O6 75.99(7) ? O8 Ce1 O6 132.16(7) ? O7 Ce1 O6 69.45(6) y O5 Ce1 O6 137.71(6) ? O1 P1 C1 111.31(13) ? O1 P1 C2 112.50(13) ? C1 P1 C2 107.30(16) ? O1 P1 C3 111.37(13) ? C1 P1 C3 107.75(16) ? C2 P1 C3 106.32(15) ? O2 P2 C5 110.01(14) ? O2 P2 C6 111.54(16) ? C5 P2 C6 107.84(18) ? O2 P2 C4 111.84(14) ? C5 P2 C4 107.58(15) ? C6 P2 C4 107.85(19) ? O3 P3 C9 111.92(14) ? O3 P3 C8 112.77(14) ? C9 P3 C8 106.80(19) ? O3 P3 C7 111.25(14) ? C9 P3 C7 106.34(17) ? C8 P3 C7 107.40(16) ? O4 P4 C12 112.02(15) ? O4 P4 C10 112.05(13) ? C12 P4 C10 106.79(15) ? O4 P4 C11 112.62(13) ? C12 P4 C11 107.56(17) ? C10 P4 C11 105.37(15) ? P1 O1 Ce1 149.58(12) y P2 O2 Ce1 144.83(12) y P3 O3 Ce1 151.31(13) y P4 O4 Ce1 144.27(12) y Ce1 O5 H5X 117.6 ? Ce1 O5 H5Y 127.2 ? H5X O5 H5Y 97.5 ? Ce1 O6 H6X 116.9 ? Ce1 O6 H6Y 129.1 ? H6X O6 H6Y 104.6 ? Ce1 O7 H7X 132.4 ? Ce1 O7 H7Y 122.4 ? H7X O7 H7Y 105.1 ? Ce1 O8 H8X 119.6 ? Ce1 O8 H8Y 133.9 ? H8X O8 H8Y 105.9 ? H9X O9 H9Y 86.5 ? H10X O10 H10Y 101.2 ? H11X O11 H11Y 91.3 ? P1 C1 H1A 109.5 ? P1 C1 H1B 109.5 ? H1A C1 H1B 109.5 ? P1 C1 H1C 109.5 ? H1A C1 H1C 109.5 ? H1B C1 H1C 109.5 ? P1 C2 H2A 109.5 ? P1 C2 H2B 109.5 ? H2A C2 H2B 109.5 ? P1 C2 H2C 109.5 ? H2A C2 H2C 109.5 ? H2B C2 H2C 109.5 ? P1 C3 H3A 109.5 ? P1 C3 H3B 109.5 ? H3A C3 H3B 109.5 ? P1 C3 H3C 109.5 ? H3A C3 H3C 109.5 ? H3B C3 H3C 109.5 ? P2 C4 H4A 109.5 ? P2 C4 H4B 109.5 ? H4A C4 H4B 109.5 ? P2 C4 H4C 109.5 ? H4A C4 H4C 109.5 ? H4B C4 H4C 109.5 ? P2 C5 H5A 109.5 ? P2 C5 H5B 109.5 ? H5A C5 H5B 109.5 ? P2 C5 H5C 109.5 ? H5A C5 H5C 109.5 ? H5B C5 H5C 109.5 ? P2 C6 H6A 109.5 ? P2 C6 H6B 109.5 ? H6A C6 H6B 109.5 ? P2 C6 H6C 109.5 ? H6A C6 H6C 109.5 ? H6B C6 H6C 109.5 ? P3 C7 H7A 109.5 ? P3 C7 H7B 109.5 ? H7A C7 H7B 109.5 ? P3 C7 H7C 109.5 ? H7A C7 H7C 109.5 ? H7B C7 H7C 109.5 ? P3 C8 H8A 109.5 ? P3 C8 H8B 109.5 ? H8A C8 H8B 109.5 ? P3 C8 H8C 109.5 ? H8A C8 H8C 109.5 ? H8B C8 H8C 109.5 ? P3 C9 H9A 109.5 ? P3 C9 H9B 109.5 ? H9A C9 H9B 109.5 ? P3 C9 H9C 109.5 ? H9A C9 H9C 109.5 ? H9B C9 H9C 109.5 ? P4 C10 H10A 109.5 ? P4 C10 H10B 109.5 ? H10A C10 H10B 109.5 ? P4 C10 H10C 109.5 ? H10A C10 H10C 109.5 ? H10B C10 H10C 109.5 ? P4 C11 H11A 109.5 ? P4 C11 H11B 109.5 ? H11A C11 H11B 109.5 ? P4 C11 H11C 109.5 ? H11A C11 H11C 109.5 ? H11B C11 H11C 109.5 ? P4 C12 H12A 109.5 ? P4 C12 H12B 109.5 ? H12A C12 H12B 109.5 ? P4 C12 H12C 109.5 ? H12A C12 H12C 109.5 ? H12B C12 H12C 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 Ce1 O1 . 2.3926(19) y Ce1 O2 . 2.372(2) y Ce1 O3 . 2.4230(19) y Ce1 O4 . 2.3896(19) y Ce1 O5 . 2.5827(18) y Ce1 O6 . 2.6300(19) y Ce1 O7 . 2.528(2) y Ce1 O8 . 2.518(2) y P1 O1 . 1.503(2) ? P1 C1 . 1.778(3) ? P1 C2 . 1.782(3) ? P1 C3 . 1.786(3) ? P2 O2 . 1.508(2) ? P2 C5 . 1.770(3) ? P2 C6 . 1.780(3) ? P2 C4 . 1.780(3) ? P3 O3 . 1.498(2) ? P3 C9 . 1.774(3) ? P3 C8 . 1.779(3) ? P3 C7 . 1.783(3) ? P4 O4 . 1.505(2) ? P4 C12 . 1.774(3) ? P4 C10 . 1.784(3) ? P4 C11 . 1.786(3) ? O5 H5X . 0.9502 ? O5 H5Y . 0.8502 ? O6 H6X . 0.7960 ? O6 H6Y . 0.8949 ? O7 H7X . 0.9166 ? O7 H7Y . 0.9675 ? O8 H8X . 0.9235 ? O8 H8Y . 0.9195 ? O9 H9X . 0.9420 ? O9 H9Y . 0.9314 ? O10 H10X . 0.8966 ? O10 H10Y . 0.9215 ? O11 H11X . 0.8661 ? O11 H11Y . 0.9526 ? C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? C1 H1C . 0.9800 ? C2 H2A . 0.9800 ? C2 H2B . 0.9800 ? C2 H2C . 0.9800 ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C4 H4C . 0.9800 ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C5 H5C . 0.9800 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? C7 H7A . 0.9800 ? C7 H7B . 0.9800 ? C7 H7C . 0.9800 ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? C10 H10A . 0.9800 ? C10 H10B . 0.9800 ? C10 H10C . 0.9800 ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O5 H5X Cl1 2_666 0.95 2.24 3.161(2) 164 y O5 H5Y O9 2_665 0.85 2.25 2.933(3) 137 y O6 H6X Cl2 1_455 0.80 2.45 3.242(2) 173 y O6 H6Y Cl3 1_455 0.89 2.40 3.295(2) 176 y O7 H7X Cl2 1_455 0.92 2.18 3.067(2) 163 y O7 H7Y Cl2 2_666 0.97 2.14 3.068(2) 160 y O8 H8X O10 . 0.92 1.87 2.755(3) 159 y O8 H8Y O9 . 0.92 1.94 2.818(3) 160 y O9 H9X Cl3 . 0.94 2.32 3.250(2) 168 y O9 H9Y Cl1 1_554 0.93 2.48 3.260(2) 141 y O10 H10X Cl3 . 0.90 2.37 3.265(2) 172 y O10 H10Y O11 2_656 0.92 1.92 2.840(3) 173 y O11 H11X Cl1 2_657 0.87 2.33 3.193(2) 179 y O11 H11Y Cl1 . 0.95 2.43 3.271(2) 147 y 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 C1 P1 O1 Ce1 -52.0(3) C2 P1 O1 Ce1 68.5(3) C3 P1 O1 Ce1 -172.3(2) O2 Ce1 O1 P1 -66.8(3) O4 Ce1 O1 P1 -159.4(2) O3 Ce1 O1 P1 49.7(2) O8 Ce1 O1 P1 -13.6(2) O7 Ce1 O1 P1 120.8(2) O5 Ce1 O1 P1 -82.9(2) O6 Ce1 O1 P1 133.4(2) C5 P2 O2 Ce1 141.6(2) C6 P2 O2 Ce1 -98.8(2) C4 P2 O2 Ce1 22.1(3) O4 Ce1 O2 P2 -175.4(2) O1 Ce1 O2 P2 94.8(2) O3 Ce1 O2 P2 -24.4(2) O8 Ce1 O2 P2 41.5(2) O7 Ce1 O2 P2 -97.1(2) O5 Ce1 O2 P2 110.6(2) O6 Ce1 O2 P2 -98.7(2) C9 P3 O3 Ce1 -65.7(3) C8 P3 O3 Ce1 54.8(3) C7 P3 O3 Ce1 175.5(2) O2 Ce1 O3 P3 -147.3(3) O4 Ce1 O3 P3 -41.3(3) O1 Ce1 O3 P3 63.1(3) O8 Ce1 O3 P3 135.8(3) O7 Ce1 O3 P3 -3.5(3) O5 Ce1 O3 P3 139.6(2) O6 Ce1 O3 P3 -75.2(3) C12 P4 O4 Ce1 -91.7(2) C10 P4 O4 Ce1 148.4(2) C11 P4 O4 Ce1 29.8(3) O2 Ce1 O4 P4 174.0(2) O1 Ce1 O4 P4 -40.5(2) O3 Ce1 O4 P4 68.4(3) O8 Ce1 O4 P4 -107.1(2) O7 Ce1 O4 P4 30.9(2) O5 Ce1 O4 P4 -112.2(2) O6 Ce1 O4 P4 101.9(2)