#------------------------------------------------------------------------------ #$Date: 2021-12-09 02:04:17 +0200 (Thu, 09 Dec 2021) $ #$Revision: 271281 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/90/7709042.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7709042 loop_ _publ_author_name 'Hou, Xiaomin' 'Tang, Sifu' _publ_section_title ; Lanthanide-uranyl Phosphonates Constructed from Diethyl ((phenylsulfonyl)methyl)phosphonate ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03596G _journal_year 2022 _chemical_formula_sum 'C14 H22 O18 P2 S2 U2' _chemical_formula_weight 1080.43 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2021-12-04 deposited with the CCDC. 2021-12-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.939(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.1219(7) _cell_length_b 9.0241(6) _cell_length_c 12.5490(8) _cell_measurement_reflns_used 16724 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.999 _cell_measurement_theta_min 3.208 _cell_volume 1370.92(15) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_unetI/netI 0.0234 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 17147 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.208 _exptl_absorpt_coefficient_mu 12.144 _exptl_absorpt_correction_T_max 0.145 _exptl_absorpt_correction_T_min 0.067 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.617 _exptl_crystal_description block _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.351 _exptl_crystal_size_mid 0.201 _exptl_crystal_size_min 0.159 _refine_diff_density_max 1.047 _refine_diff_density_min -1.171 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2405 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0218 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+6.8060P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0541 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2059 _reflns_number_total 2405 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03596g2.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7709042 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL 1 in P2(1)/c CELL 0.71073 12.1219 9.0241 12.5490 90.000 92.939 90.000 ZERR 2.00 0.0007 0.0006 0.0008 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O P S U UNIT 28 44 36 4 4 4 L.S. 10 BOND acta OMIT -3 50 OMIT -4 1 3 OMIT -5 0 4 OMIT 1 1 1 OMIT -6 3 2 OMIT 6 1 2 OMIT -6 1 2 OMIT -3 3 3 FMAP 2 PLAN 10 WGHT 0.018700 6.806000 FVAR 0.08143 U1 6 0.961700 0.254494 0.123414 11.00000 0.01720 0.01680 = 0.00987 -0.00036 0.00238 -0.00046 P1 4 0.869221 0.420863 -0.126196 11.00000 0.01855 0.01917 = 0.01015 -0.00186 0.00384 -0.00322 S1 5 0.648997 0.272001 -0.180992 11.00000 0.01807 0.03475 = 0.02152 -0.00429 -0.00055 -0.00340 O1 3 0.900950 0.575156 -0.090096 11.00000 0.02484 0.02175 = 0.01463 -0.00321 0.00493 -0.00435 O1W 3 1.061626 0.311505 0.295109 11.00000 0.03418 0.02820 = 0.02012 -0.00052 -0.00051 -0.01062 AFIX 3 H1W 2 1.017086 0.297925 0.344299 11.00000 -1.50000 H2W 2 1.090946 0.396795 0.301229 11.00000 -1.50000 AFIX 0 O2 3 0.889033 0.395009 -0.243176 11.00000 0.02681 0.02130 = 0.00965 -0.00243 0.00197 0.00170 O2W 3 0.803893 0.095480 0.058956 11.00000 0.04060 0.04327 = 0.02515 0.00572 -0.00662 -0.02343 AFIX 3 H3W 2 0.795823 0.010870 0.087176 11.00000 -1.50000 H4W 2 0.754623 0.121000 0.012046 11.00000 -1.50000 AFIX 0 O3 3 0.922335 0.299043 -0.058597 11.00000 0.02636 0.02530 = 0.01482 0.00066 0.00058 -0.00152 O4 3 0.644125 0.308705 -0.293144 11.00000 0.02921 0.06644 = 0.02131 0.00155 -0.00271 -0.01019 O5 3 0.696680 0.133029 -0.146905 11.00000 0.02970 0.03088 = 0.04229 -0.00838 -0.00592 0.00225 O6 3 1.053691 0.111603 0.093155 11.00000 0.03091 0.02290 = 0.02824 -0.00104 0.00236 0.00514 O7 3 0.869122 0.397562 0.150737 11.00000 0.02788 0.02385 = 0.02629 0.00069 0.00475 0.00723 C1 1 0.432899 0.355070 -0.197361 11.00000 0.03642 0.05197 = 0.04586 0.01162 0.00399 0.00965 AFIX 43 H1A 2 0.451145 0.405832 -0.258505 11.00000 -1.20000 AFIX 0 C2 1 0.325786 0.355769 -0.166596 11.00000 0.03020 0.07445 = 0.06601 0.00140 -0.00320 0.01468 AFIX 43 H2A 2 0.270889 0.404101 -0.207780 11.00000 -1.20000 AFIX 0 C3 1 0.300519 0.283808 -0.073713 11.00000 0.02078 0.07397 = 0.05388 -0.02117 0.01097 -0.00249 AFIX 43 H3A 2 0.228225 0.284488 -0.052234 11.00000 -1.20000 AFIX 0 C4 1 0.379892 0.212248 -0.013554 11.00000 0.04178 0.07984 = 0.04253 0.00723 0.00973 -0.01836 AFIX 43 H4A 2 0.361860 0.166144 0.049509 11.00000 -1.20000 AFIX 0 C5 1 0.487540 0.207242 -0.045220 11.00000 0.02623 0.07281 = 0.04129 0.01836 -0.00013 -0.00258 AFIX 43 H5A 2 0.541721 0.156237 -0.004921 11.00000 -1.20000 AFIX 0 C6 1 0.513019 0.279864 -0.138322 11.00000 0.01873 0.03678 = 0.03466 -0.00257 0.00193 -0.00572 C7 1 0.720228 0.416540 -0.110503 11.00000 0.02207 0.02859 = 0.02630 -0.00558 0.00545 -0.00525 AFIX 23 H7A 2 0.707193 0.406624 -0.035215 11.00000 -1.20000 H7B 2 0.689167 0.510636 -0.134363 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0218 for 2059 Fo > 4sig(Fo) and 0.0282 for all 2405 data REM 172 parameters refined using 0 restraints END WGHT 0.0190 6.8285 REM Highest difference peak 1.047, deepest hole -1.171, 1-sigma level 0.140 Q1 1 0.9470 0.3326 0.1604 11.00000 0.05 1.05 Q2 1 0.9739 0.3268 0.0782 11.00000 0.05 0.91 Q3 1 0.9633 0.1038 0.1195 11.00000 0.05 0.72 Q4 1 1.1294 -0.0781 0.1260 11.00000 0.05 0.56 Q5 1 0.8014 0.2023 0.1179 11.00000 0.05 0.55 Q6 1 0.9743 0.1652 0.0760 11.00000 0.05 0.52 Q7 1 0.9581 0.4077 0.1176 11.00000 0.05 0.50 Q8 1 0.8101 0.3030 0.1180 11.00000 0.05 0.48 Q9 1 0.8064 0.1906 0.0646 11.00000 0.05 0.47 Q10 1 0.9580 0.1741 0.1790 11.00000 0.05 0.46 ; _shelx_res_checksum 38832 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.96170(2) 0.25449(2) 0.12341(2) 0.01457(8) Uani 1 1 d . . . . . P1 P 0.86922(11) 0.42086(14) -0.12620(10) 0.0159(3) Uani 1 1 d . . . . . S1 S 0.64900(11) 0.27200(16) -0.18099(11) 0.0248(3) Uani 1 1 d . . . . . O1 O 0.9009(3) 0.5752(4) -0.0901(3) 0.0203(8) Uani 1 1 d . . . . . O1W O 1.0616(3) 0.3115(4) 0.2951(3) 0.0276(9) Uani 1 1 d . . . . . H1W H 1.0171 0.2979 0.3443 0.041 Uiso 1 1 d R U . . . H2W H 1.0909 0.3968 0.3012 0.041 Uiso 1 1 d R U . . . O2 O 0.8890(3) 0.3950(4) -0.2432(2) 0.0192(8) Uani 1 1 d . . . . . O2W O 0.8039(3) 0.0955(5) 0.0590(3) 0.0366(10) Uani 1 1 d . . . . . H3W H 0.7958 0.0109 0.0872 0.055 Uiso 1 1 d R U . . . H4W H 0.7546 0.1210 0.0120 0.055 Uiso 1 1 d R U . . . O3 O 0.9223(3) 0.2990(4) -0.0586(3) 0.0222(8) Uani 1 1 d . . . . . O4 O 0.6441(3) 0.3087(6) -0.2931(3) 0.0391(11) Uani 1 1 d . . . . . O5 O 0.6967(3) 0.1330(4) -0.1469(3) 0.0346(10) Uani 1 1 d . . . . . O6 O 1.0537(3) 0.1116(4) 0.0932(3) 0.0273(9) Uani 1 1 d . . . . . O7 O 0.8691(3) 0.3976(4) 0.1507(3) 0.0259(9) Uani 1 1 d . . . . . C1 C 0.4329(5) 0.3551(8) -0.1974(6) 0.0447(17) Uani 1 1 d . . . . . H1A H 0.4511 0.4058 -0.2585 0.054 Uiso 1 1 calc R U . . . C2 C 0.3258(6) 0.3558(9) -0.1666(7) 0.057(2) Uani 1 1 d . . . . . H2A H 0.2709 0.4041 -0.2078 0.068 Uiso 1 1 calc R U . . . C3 C 0.3005(5) 0.2838(9) -0.0737(6) 0.0492(19) Uani 1 1 d . . . . . H3A H 0.2282 0.2845 -0.0522 0.059 Uiso 1 1 calc R U . . . C4 C 0.3799(6) 0.2122(10) -0.0136(6) 0.054(2) Uani 1 1 d . . . . . H4A H 0.3619 0.1661 0.0495 0.065 Uiso 1 1 calc R U . . . C5 C 0.4875(5) 0.2072(9) -0.0452(6) 0.0468(18) Uani 1 1 d . . . . . H5A H 0.5417 0.1562 -0.0049 0.056 Uiso 1 1 calc R U . . . C6 C 0.5130(5) 0.2799(7) -0.1383(5) 0.0300(13) Uani 1 1 d . . . . . C7 C 0.7202(4) 0.4165(6) -0.1105(4) 0.0255(12) Uani 1 1 d . . . . . H7A H 0.7072 0.4066 -0.0352 0.031 Uiso 1 1 calc R U . . . H7B H 0.6892 0.5106 -0.1344 0.031 Uiso 1 1 calc R U . . . 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 U1 0.01720(12) 0.01680(12) 0.00987(11) -0.00036(7) 0.00238(7) -0.00046(8) P1 0.0186(6) 0.0192(6) 0.0102(6) -0.0019(5) 0.0038(5) -0.0032(5) S1 0.0181(6) 0.0348(8) 0.0215(7) -0.0043(6) -0.0006(5) -0.0034(6) O1 0.0248(19) 0.0217(18) 0.0146(17) -0.0032(15) 0.0049(15) -0.0043(16) O1W 0.034(2) 0.028(2) 0.0201(19) -0.0005(17) -0.0005(17) -0.0106(18) O2 0.0268(19) 0.0213(18) 0.0096(17) -0.0024(14) 0.0020(15) 0.0017(16) O2W 0.041(2) 0.043(3) 0.025(2) 0.0057(19) -0.0066(18) -0.023(2) O3 0.026(2) 0.0253(19) 0.0148(18) 0.0007(16) 0.0006(16) -0.0015(16) O4 0.029(2) 0.066(3) 0.021(2) 0.002(2) -0.0027(18) -0.010(2) O5 0.030(2) 0.031(2) 0.042(2) -0.008(2) -0.0059(19) 0.0022(18) O6 0.031(2) 0.023(2) 0.028(2) -0.0010(17) 0.0024(17) 0.0051(17) O7 0.028(2) 0.024(2) 0.026(2) 0.0007(16) 0.0048(17) 0.0072(17) C1 0.036(4) 0.052(4) 0.046(4) 0.012(3) 0.004(3) 0.010(3) C2 0.030(4) 0.074(6) 0.066(5) 0.001(4) -0.003(4) 0.015(4) C3 0.021(3) 0.074(5) 0.054(5) -0.021(4) 0.011(3) -0.002(3) C4 0.042(4) 0.080(6) 0.043(4) 0.007(4) 0.010(4) -0.018(4) C5 0.026(3) 0.073(5) 0.041(4) 0.018(4) 0.000(3) -0.003(3) C6 0.019(3) 0.037(3) 0.035(3) -0.003(3) 0.002(3) -0.006(2) C7 0.022(3) 0.029(3) 0.026(3) -0.006(2) 0.005(2) -0.005(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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 U1 O6 178.79(16) . . ? O7 U1 O1 91.13(15) . 3_765 ? O6 U1 O1 88.74(16) . 3_765 ? O7 U1 O3 87.93(15) . . ? O6 U1 O3 90.86(15) . . ? O1 U1 O3 79.80(12) 3_765 . ? O7 U1 O2 90.93(15) . 4_566 ? O6 U1 O2 89.88(15) . 4_566 ? O1 U1 O2 143.66(12) 3_765 4_566 ? O3 U1 O2 136.54(12) . 4_566 ? O7 U1 O1W 88.07(15) . . ? O6 U1 O1W 93.04(16) . . ? O1 U1 O1W 72.24(12) 3_765 . ? O3 U1 O1W 151.65(13) . . ? O2 U1 O1W 71.58(12) 4_566 . ? O7 U1 O2W 89.95(16) . . ? O6 U1 O2W 89.56(16) . . ? O1 U1 O2W 150.33(12) 3_765 . ? O3 U1 O2W 70.61(12) . . ? O2 U1 O2W 65.94(12) 4_566 . ? O1W U1 O2W 137.43(12) . . ? O1 P1 O3 114.1(2) . . ? O1 P1 O2 112.5(2) . . ? O3 P1 O2 110.3(2) . . ? O1 P1 C7 103.0(2) . . ? O3 P1 C7 108.6(2) . . ? O2 P1 C7 107.9(2) . . ? O5 S1 O4 119.1(3) . . ? O5 S1 C6 108.3(3) . . ? O4 S1 C6 107.2(3) . . ? O5 S1 C7 108.4(3) . . ? O4 S1 C7 108.2(3) . . ? C6 S1 C7 104.9(3) . . ? P1 O1 U1 137.1(2) . 3_765 ? P1 O2 U1 149.2(2) . 4_565 ? P1 O3 U1 137.0(2) . . ? C6 C1 C2 120.3(7) . . ? C1 C2 C3 119.2(7) . . ? C4 C3 C2 120.8(6) . . ? C3 C4 C5 120.5(7) . . ? C4 C5 C6 118.7(7) . . ? C1 C6 C5 120.4(6) . . ? C1 C6 S1 120.3(5) . . ? C5 C6 S1 119.3(5) . . ? S1 C7 P1 114.8(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O7 1.756(4) . ? U1 O6 1.759(4) . ? U1 O1 2.320(3) 3_765 ? U1 O3 2.344(3) . ? U1 O2 2.356(3) 4_566 ? U1 O1W 2.471(4) . ? U1 O2W 2.493(4) . ? P1 O1 1.508(4) . ? P1 O3 1.512(4) . ? P1 O2 1.518(3) . ? P1 C7 1.827(5) . ? S1 O5 1.437(4) . ? S1 O4 1.444(4) . ? S1 C6 1.760(6) . ? S1 C7 1.775(5) . ? O1 U1 2.320(3) 3_765 ? O2 U1 2.356(3) 4_565 ? C1 C6 1.371(9) . ? C1 C2 1.373(9) . ? C2 C3 1.382(11) . ? C3 C4 1.356(11) . ? C4 C5 1.384(10) . ? C5 C6 1.388(9) . ?