Occurrence of polyoxouranium motifs in uranyl organic networks constructed by using silicon-centered carboxylate linkers: structures, spectroscopy and computation.
Liu, Chao; Yang, Xin-Xue; Niu, Shuai; Yi, Xiao-Yi; Pan, Qing-Jiang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4155–4163; doi:10.1039/d0dt00379d

data_7703570
_publ_section_title
;
 Occurrence of polyoxouranium motifs in uranyl organic networks
 constructed by using silicon-centered carboxylate linkers: structures,
 spectroscopy and computation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4155
_journal_page_last               4163
_journal_paper_doi               10.1039/d0dt00379d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C54 H34 O27 Si2 U5'
_chemical_formula_sum            'C54 H34 O27 Si2 U5'
_chemical_formula_weight         2361.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc237ngh
_audit_creation_date             2020-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-19 deposited with the CCDC.	2020-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                76.477(2)
_cell_angle_beta                 81.425(2)
_cell_angle_gamma                73.681(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2639(13)
_cell_length_b                   16.2562(15)
_cell_length_c                   17.8214(16)
_cell_measurement_reflns_used    2016
_cell_measurement_temperature    150
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     3840.5(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24036
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.143
_diffrn_reflns_theta_min         1.333
_exptl_absorpt_coefficient_mu    10.605
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0925 before and 0.0374 after correction. The Ratio of minimum to maximum transmission is 0.5977. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_platon_squeeze_details
;
TITL 1         P -1         R = 0.06
CELL   14.2639   16.2562   17.8214     76.48     81.43     73.68
SPGR P-1
Q101 0.938 0.445 0.389 !       5.60 eA-3
C102 0.580 0.594 0.333 !       5.59 eA-3
C103 0.592 0.074 0.453 !       4.47 eA-3
C104 0.704 0.059 0.496 !       4.03 eA-3
Q105 0.801 0.186 0.378 !       3.90 eA-3
C106 0.545 0.056 0.501 !       3.69 eA-3
Q107 0.221 0.385 0.410 !       3.14 eA-3
Q108 0.286 0.343 0.427 !       3.11 eA-3
C109 0.748 0.470 0.392 !       2.99 eA-3
Q110 0.951 0.398 0.342 !       2.96 eA-3
C111 0.662 0.719 0.358 !       2.69 eA-3
C112 0.478 0.970 0.460 !       2.66 eA-3
Q113 0.382 0.045 0.471 !       2.59 eA-3
C114 0.403 0.045 0.315 !       2.59 eA-3
C115 0.469 0.232 0.279 !       2.44 eA-3
C116 0.526 0.979 0.400 !       2.41 eA-3
Q117 0.295 0.886 0.359 !       2.41 eA-3
C118 0.502 0.468 0.435 !       2.36 eA-3
Q119 0.238 0.681 0.255 !       2.28 eA-3
Q120 0.236 0.619 0.289 !       2.15 eA-3
C121 0.441 0.082 0.449 !       2.14 eA-3
C122 0.610 0.740 0.386 !       2.12 eA-3
C123 0.686 0.963 0.432 !       2.12 eA-3
C124 0.657 0.921 0.443 !       2.03 eA-3
Q125 0.945 0.707 0.441 !       1.99 eA-3
Q126 0.344 0.441 0.482 !       1.98 eA-3
Q127 0.201 0.467 0.413 !       1.86 eA-3
C128 0.377 0.862 0.369 !       1.85 eA-3
Q129 0.641 0.859 0.405 !       1.82 eA-3
C130 0.803 0.345 0.434 !       1.81 eA-3
Q131 0.423 0.783 0.090 !       1.81 eA-3
C132 0.429 0.168 0.238 !       1.80 eA-3
Q133 0.935 0.830 0.492 !       1.79 eA-3
Q134 0.793 0.395 0.466 !       1.79 eA-3
C135 0.534 0.754 0.393 !       1.78 eA-3
Q136 0.095 0.165 0.395 !       1.77 eA-3
C137 0.673 0.321 0.442 !       1.74 eA-3
C138 0.457 0.183 0.329 !       1.73 eA-3
C139 0.545 0.720 0.393 !       1.73 eA-3
Q140 0.063 0.578 0.404 !       1.72 eA-3
Q141 1.002 0.691 0.457 !       1.70 eA-3
C142 0.372 0.804 0.395 !       1.66 eA-3
C143 0.667 0.172 0.278 !       1.66 eA-3
Q144 0.779 0.305 0.469 !       1.66 eA-3
C145 0.514 0.314 0.455 !       1.65 eA-3
C146 0.393 0.009 0.352 !       1.59 eA-3
Q147 0.781 0.527 0.401 !       1.58 eA-3
C148 0.535 0.082 0.283 !       1.57 eA-3
Q149 0.792 0.491 0.421 !       1.57 eA-3
C150 0.440 0.942 0.392 !       1.57 eA-3
Q151 0.328 0.022 0.391 !       1.56 eA-3
Q152 0.248 0.066 0.371 !       1.52 eA-3
C153 0.643 0.089 0.347 !       1.52 eA-3
Q154 0.971 0.954 0.407 !       1.50 eA-3
C155 0.452 0.884 0.423 !       1.50 eA-3
Q156 0.653 0.446 0.438 !       1.50 eA-3
Q157 0.888 0.749 0.432 !       1.48 eA-3
Q158 0.358 0.245 0.373 !       1.42 eA-3
C159 0.394 0.746 0.459 !       1.42 eA-3
C160 0.560 0.055 0.312 !       1.41 eA-3
C161 0.765 0.206 0.233 !       1.39 eA-3
C162 0.458 0.155 0.377 !       1.39 eA-3
Q163 0.956 1.004 0.284 !       1.38 eA-3
C164 0.535 0.234 0.468 !       1.37 eA-3
C165 0.410 0.681 0.485 !       1.37 eA-3
C166 0.527 0.325 0.486 !       1.37 eA-3
Q167 0.281 0.928 0.215 !       1.37 eA-3
C168 0.439 0.826 0.469 !       1.36 eA-3
C169 0.548 0.195 0.424 !       1.36 eA-3
Q170 0.969 0.371 0.410 !       1.36 eA-3
C171 0.639 0.783 0.372 !       1.36 eA-3
Q172 0.715 0.199 0.498 !       1.35 eA-3
Q173 0.547 0.342 0.221 !       1.35 eA-3
Q174 0.816 0.643 0.456 !       1.35 eA-3
C175 0.488 0.392 0.502 !       1.35 eA-3
C176 0.578 1.000 0.428 !       1.35 eA-3
Q177 0.040 0.992 0.300 !       1.35 eA-3
Q178 0.148 0.433 0.406 !       1.33 eA-3
C179 0.373 0.810 0.459 !       1.33 eA-3
Q180 0.829 0.482 0.428 !       1.33 eA-3
Q181 0.271 0.740 0.468 !       1.33 eA-3
Q182 0.546 0.488 0.233 !       1.31 eA-3
C183 0.718 0.190 0.348 !       1.31 eA-3
C184 0.496 0.145 0.247 !       1.29 eA-3
Q185 0.125 0.108 0.125 !       1.28 eA-3
C186 0.563 0.031 0.375 !       1.27 eA-3
C187 0.702 0.249 0.370 !       1.27 eA-3
Q188 0.297 0.304 0.482 !       1.26 eA-3
Q189 0.348 0.777 0.405 !       1.26 eA-3
C190 0.647 0.090 0.374 !       1.25 eA-3
C191 0.520 0.216 0.377 !       1.25 eA-3
Q192 0.824 0.806 0.423 !       1.24 eA-3
Q193 0.030 0.636 0.429 !       1.24 eA-3
Q194 0.411 0.169 0.473 !       1.24 eA-3
C195 0.599 0.160 0.314 !       1.23 eA-3
C196 0.503 0.998 0.325 !       1.23 eA-3
Q197 0.286 0.574 0.075 !       1.22 eA-3
Q198 0.426 0.060 0.017 !       1.22 eA-3
C199 0.398 0.736 0.397 !       1.22 eA-3
;
_refine_diff_density_max         2.156
_refine_diff_density_min         -1.765
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         15127
_refine_ls_number_restraints     920
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10092
_reflns_number_total             15127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00379d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7703568--7703571.cif.'
_cod_database_code               7703570
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O23A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(U3A)=Sof(U5A)=Sof(O17A)=Sof(O21A)=Sof(O24A)=Sof(O25A)=Sof(O26A)=Sof(O27A)=
 1-FVAR(1)
 Sof(U3)=Sof(U5)=Sof(O17)=Sof(O21)=Sof(O24)=Sof(O25)=Sof(O26)=Sof(O27)=FVAR(1)
 Sof(O23A)=Sof(O22A)=Sof(O20A)=Sof(U1A)=1-FVAR(2)
 Sof(U1)=Sof(O20)=Sof(O22)=Sof(O23)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27),
  C29(H29), C32(H32), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50), C52(H52)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'