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_7703568
_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         'C96 H38 O92 Si3 U12, (C15 H12 N2)5'
_chemical_formula_sum            'C171 H98 N10 O92 Si3 U12'
_chemical_formula_weight         6705.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc23bmgk
_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                90
_cell_angle_beta                 100.5790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1551(16)
_cell_length_b                   20.3001(12)
_cell_length_c                   50.380(3)
_cell_measurement_reflns_used    6890
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.661
_cell_measurement_theta_min      2.180
_cell_volume                     27300(3)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            75639
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.822
_exptl_absorpt_coefficient_mu    7.176
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0859 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.7779. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             12304
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;
TITL 1         C 1 2/c 1    R = 0.13
CELL   27.1551   20.3001   50.3800     90.00    100.58     90.00
SPGR C2/c
Q101 0.232 0.499 0.221 !       6.14 eA-3
C102 0.658 0.503 0.066 !       4.83 eA-3
C103 0.353 0.489 0.402 !       4.81 eA-3
C104 0.056 0.487 0.147 !       4.76 eA-3
Q105 0.268 0.106 0.282 !       4.66 eA-3
C106 0.975 0.436 0.192 !       4.55 eA-3
C107 0.110 0.502 0.106 !       4.54 eA-3
Q108 0.154 0.032 0.026 !       4.54 eA-3
C109 0.209 0.249 0.377 !       4.43 eA-3
C110 0.897 0.463 0.353 !       4.43 eA-3
C111 0.265 0.158 0.233 !       4.42 eA-3
C112 0.389 0.451 0.329 !       4.39 eA-3
C113 0.672 0.482 0.146 !       4.37 eA-3
C114 0.437 0.454 0.327 !       4.32 eA-3
C115 0.846 0.280 0.154 !       4.22 eA-3
C116 0.683 0.498 0.121 !       4.19 eA-3
C117 0.369 0.011 0.418 !       4.15 eA-3
C118 0.203 0.018 0.554 !       4.15 eA-3
Q119 0.079 0.049 0.389 !       4.06 eA-3
Q120 0.532 0.436 0.465 !       4.03 eA-3
C121 0.026 0.465 0.171 !       4.01 eA-3
C122 0.947 0.487 0.896 !       4.01 eA-3
C123 0.678 0.224 0.156 !       4.01 eA-3
C124 0.322 0.213 0.344 !       4.00 eA-3
C125 0.501 0.250 0.424 !       3.94 eA-3
C126 0.850 0.066 0.806 !       3.92 eA-3
C127 0.147 0.300 0.428 !       3.91 eA-3
Q128 0.406 0.436 0.104 !       3.87 eA-3
C129 0.805 0.364 0.748 !       3.85 eA-3
Q130 0.811 0.468 0.714 !       3.81 eA-3
C131 0.867 0.484 0.371 !       3.76 eA-3
C132 0.188 0.283 0.358 !       3.74 eA-3
Q133 0.852 0.405 0.124 !       3.74 eA-3
C134 0.593 0.449 0.120 !       3.73 eA-3
C135 0.311 0.500 0.470 !       3.70 eA-3
C136 0.744 0.251 0.097 !       3.68 eA-3
C137 0.334 0.188 0.253 !       3.67 eA-3
C138 0.625 0.468 0.149 !       3.65 eA-3
C139 0.579 0.204 0.997 !       3.56 eA-3
C140 0.376 0.233 0.364 !       3.55 eA-3
C141 0.041 0.203 0.515 !       3.53 eA-3
Q142 0.141 0.017 0.721 !       3.50 eA-3
C143 0.618 0.253 0.032 !       3.45 eA-3
C144 0.460 0.094 0.481 !       3.45 eA-3
C145 0.761 0.199 0.195 !       3.39 eA-3
Q146 0.319 0.405 0.069 !       3.37 eA-3
C147 0.460 0.013 0.809 !       3.37 eA-3
C148 0.031 0.503 0.120 !       3.37 eA-3
C149 0.445 0.448 0.299 !       3.36 eA-3
C150 0.186 0.187 0.568 !       3.34 eA-3
C151 0.165 0.278 0.449 !       3.31 eA-3
C152 0.305 0.204 0.437 !       3.31 eA-3
C153 0.696 0.159 0.153 !       3.30 eA-3
Q154 0.439 0.318 0.046 !       3.28 eA-3
C155 0.390 0.201 0.484 !       3.26 eA-3
C156 0.664 0.251 0.058 !       3.26 eA-3
C157 0.111 0.296 0.409 !       3.26 eA-3
C158 0.376 0.392 0.280 !       3.25 eA-3
Q159 0.264 0.466 0.141 !       3.24 eA-3
C160 0.538 0.254 0.093 !       3.20 eA-3
C161 0.913 0.236 0.083 !       3.16 eA-3
Q162 0.604 0.082 0.948 !       3.16 eA-3
C163 0.537 0.231 0.102 !       3.16 eA-3
C164 0.954 0.237 0.002 !       3.15 eA-3
C165 0.312 0.032 0.457 !       3.15 eA-3
C166 0.401 0.468 0.396 !       3.13 eA-3
C167 0.868 0.032 0.454 !       3.11 eA-3
C168 0.264 0.203 0.230 !       3.10 eA-3
Q169 0.071 0.453 0.530 !       3.08 eA-3
C170 0.585 0.433 0.221 !       3.05 eA-3
C171 0.476 0.314 0.075 !       3.05 eA-3
C172 0.310 0.265 0.328 !       3.04 eA-3
C173 0.889 0.187 0.059 !       3.04 eA-3
C174 0.259 0.235 0.310 !       3.03 eA-3
C175 0.637 0.278 0.854 !       3.01 eA-3
C176 0.280 0.201 0.410 !       3.01 eA-3
Q177 0.390 0.047 0.039 !       2.99 eA-3
C178 0.986 0.436 0.165 !       2.98 eA-3
C179 0.640 0.436 0.205 !       2.97 eA-3
C180 0.711 0.015 0.065 !       2.97 eA-3
C181 1.001 0.437 0.214 !       2.96 eA-3
C182 0.085 0.203 0.529 !       2.94 eA-3
C183 0.524 0.285 0.409 !       2.94 eA-3
Q184 0.482 0.327 0.451 !       2.92 eA-3
C185 0.328 0.013 0.418 !       2.92 eA-3
C186 0.500 0.469 0.251 !       2.91 eA-3
C187 0.897 0.283 0.078 !       2.90 eA-3
C188 0.289 0.309 0.392 !       2.88 eA-3
C189 0.698 0.256 0.960 !       2.86 eA-3
C190 0.802 0.244 0.040 !       2.86 eA-3
C191 0.470 0.255 0.281 !       2.85 eA-3
C192 0.435 0.204 0.406 !       2.84 eA-3
C193 0.174 0.200 0.377 !       2.78 eA-3
C194 0.674 0.700 0.377 !       2.78 eA-3
C195 0.124 0.302 0.720 !       2.77 eA-3
Q196 0.070 0.027 0.376 !       2.75 eA-3
Q197 0.976 0.173 0.565 !       2.71 eA-3
C198 0.310 0.234 0.245 !       2.71 eA-3
C199 0.087 0.217 0.644 !       2.70 eA-3
;
_refine_diff_density_max         2.495
_refine_diff_density_min         -3.730
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1044
_refine_ls_number_reflns         23927
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0890
_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^)+(0.0517P)^2^+2199.0215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16166
_reflns_number_total             23927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00379d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7703568--7703571.cif.'
_cod_database_code               7703568
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.222
_shelx_estimated_absorpt_t_min   0.124
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O22) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C42) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O19)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O31) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O22A) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O20) \\sim Ueq, Uanis(O20A) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O22A) \\sim Ueq,
Uanis(O26) \\sim Ueq, Uanis(O26A) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O23A)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O24A) \\sim Ueq, Uanis(O27) \\sim Ueq,
Uanis(O27A) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O28A) \\sim Ueq, Uanis(O25)
\\sim Ueq, Uanis(O25A) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O29A) \\sim Ueq,
Uanis(O30) \\sim Ueq, Uanis(O30A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 U2', U2, O1, O20, O21, O22, O1A, O20A, O22A, U1, U1', O25, O28, O25A, O28A,
 O26, O26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(U2')=Sof(U1')=Sof(O25A)=Sof(O24A)=Sof(O23A)=Sof(O1A)=Sof(O20A)=Sof(O22A)=
 Sof(O26A)=Sof(O27A)=Sof(O28A)=Sof(O29A)=Sof(O30A)=1-FVAR(1)
 Sof(U1)=Sof(U2)=Sof(O1)=Sof(O20)=Sof(O22)=Sof(O23)=Sof(O24)=Sof(O25)=Sof(O26)=
 Sof(O27)=Sof(O28)=Sof(O29)=Sof(O30)=FVAR(1)
 Sof(U3'A)=1-FVAR(2)
 Sof(U3')=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C15(H15), C16(H16), C18(H18), C20(H20), C22(H22),
 C24(H24), C25(H25), C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42),
  C44(H44), C46(H46)
5.b Idealised tetrahedral OH refined as rotating group:
 O41(H41)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'