Formation of a new type of uranium(iv) poly-oxo cluster {U<sub>38</sub>} based on a controlled release of water <i>via</i> esterification reaction.
Martin, Nicolas P.; Volkringer, Christophe; Henry, Natacha; Trivelli, Xavier; Stoclet, Grégory; Ikeda-Ohno, Atsushi; Loiseau, Thierry; Chemical science 9 (2018) 5021–5032; doi:10.1039/c8sc00752g

data_1549392
_publ_section_title
;
 Formation of a new type of uranium(iv) poly-oxo cluster {U<sub>38</sub>}
 based on a controlled release of water <i>via</i> esterification
 reaction.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              5021
_journal_page_last               5032
_journal_paper_doi               10.1039/c8sc00752g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C60 H148 Cl42 O76 U38'
_chemical_formula_sum            'C60 H148 Cl42 O76 U38'
_chemical_formula_weight         12619.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-06 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6962(7)
_cell_length_b                   19.6962(7)
_cell_length_c                   29.9535(13)
_cell_measurement_reflns_used    5027
_cell_measurement_temperature    299.43
_cell_measurement_theta_max      28.070
_cell_measurement_theta_min      2.287
_cell_volume                     11620.2(8)
_computing_cell_refinement       '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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299.43
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            47568
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.270
_diffrn_reflns_theta_min         1.360
_exptl_absorpt_coefficient_mu    26.904
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1441 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.5285.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.607
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             10652
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.083
_refine_diff_density_max         3.030
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+91.8596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3990
_reflns_number_total             7301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00752g2.cif
_cod_data_source_block           996tetrai4m_a
_cod_depositor_comments
'Adding full bibliography for 1549391--1549392.cif.'
_cod_original_cell_volume        11620.2(10)
_cod_database_code               1549392
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1SA-H1SA
 0.85 with sigma of 0.01
 O1SB-H1SB
 0.85 with sigma of 0.01
 C2SA-H1SA
 1.952929 with sigma of 0.02
 U2-H1SA
 2.922887 with sigma of 0.02
 C2SB-H1SB
 1.97052 with sigma of 0.02
 U3-H1SB
 2.896145 with sigma of 0.02
3. Others
 Fixed Sof: H2SC(0.5) C3SC(0.5) H3SG(0.5) H3SH(0.5) H3SI(0.5) C5SC(0.5)
 H5SA(0.5) H5SB(0.5) H5SC(0.5) C4SC(0.5) H4SD(0.5) H4SE(0.5) H4SF(0.5)
 C6SC(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5)
4.a Ternary CH refined with riding coordinates:
 C2SB(H2SB), C2SA(H2SA), C2SC(H2SC)
4.b Idealised Me refined as rotating group:
 C4SA(H4SA,H4SB,H4SC), C3SA(H3SA,H3SB,H3SC), C3SB(H3SD,H3SE,H3SF), C3SC(H3SG,
 H3SH,H3SI), C5SC(H5SA,H5SB,H5SC), C4SC(H4SD,H4SE,H4SF), C6SC(H6SA,H6SB,H6SC)
;
_shelx_res_checksum              79368
_olex2_submission_special_instructions 'No special instructions were received'