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_1549391
_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         'C40 H52 Cl4 O12 U2, 0.5(C3 H8 O)'
_chemical_formula_sum            'C41.5 H56 Cl4 O12.5 U2'
_chemical_formula_weight         1372.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                67.493(9)
_cell_angle_beta                 86.541(10)
_cell_angle_gamma                76.417(10)
_cell_formula_units_Z            1
_cell_length_a                   10.683(2)
_cell_length_b                   11.322(2)
_cell_length_c                   11.736(2)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.963
_cell_measurement_theta_min      2.460
_cell_volume                     1274.0(4)
_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      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38899
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.612
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1067 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.8742. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       plate
_exptl_crystal_F_000             657
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          5.384
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5011
_reflns_number_total             5575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00752g2.cif
_cod_data_source_block           1481p-1_a-copy
_cod_depositor_comments
'Adding full bibliography for 1549391--1549392.cif.'
_cod_original_cell_volume        1273.9(4)
_cod_original_formula_sum        'C41.50 H56 Cl4 O12.50 U2'
_cod_database_code               1549391
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.558
_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
 O1-H1
 0.85 with sigma of 0.01
 O5A-H5AA
 0.85 with sigma of 0.01
 O5B-H5BA
 0.85 with sigma of 0.01
 C2S-O1S
 1.4248 with sigma of 0.02
 C2-H1
 1.930116 with sigma of 0.02
 U1-H1
 2.98425 with sigma of 0.02
 C6A-H5AA
 1.884884 with sigma of 0.02
 U1-H5AA
 2.945822 with sigma of 0.02
 C6B-H5BA
 1.855728 with sigma of 0.02
 U1-H5BA
 2.686081 with sigma of 0.02
 O1S-C4S
 2.3732 with sigma of 0.04
 O1S-C3S
 2.4353 with sigma of 0.04
 C3S-C4S
 2.5114 with sigma of 0.04
 U1-O5A \\sim U1-O5B
 with sigma of 0.02
 O5A-C6A \\sim O5B-C6B
 with sigma of 0.02
 C6A-H6A \\sim C6B-H6B
 with sigma of 0.02
 C6A-C8A \\sim C6B-C7B
 with sigma of 0.02
 C6A-C7A \\sim C6B-C8B
 with sigma of 0.02
 C8A-H8AA \\sim C7B-H7BC
 with sigma of 0.02
 C8A-H8AB \\sim C7B-H7BA
 with sigma of 0.02
 C8A-H8AC \\sim C7B-H7BB
 with sigma of 0.02
 C7A-H7AA \\sim C8B-H8BA
 with sigma of 0.02
 C7A-H7AB \\sim C8B-H8BB
 with sigma of 0.02
 C7A-H7AC \\sim C8B-H8BC
 with sigma of 0.02
 U1-C6A \\sim U1-C6B
 with sigma of 0.04
 O5A-H6A \\sim O5B-H6B
 with sigma of 0.04
 O5A-C8A \\sim O5B-C7B
 with sigma of 0.04
 O5A-C7A \\sim O5B-C8B
 with sigma of 0.04
 C6A-H8AA \\sim C6B-H7BC
 with sigma of 0.04
 C6A-H8AB \\sim C6B-H7BA
 with sigma of 0.04
 C6A-H8AC \\sim C6B-H7BB
 with sigma of 0.04
 C6A-H7AA \\sim C6B-H8BA
 with sigma of 0.04
 C6A-H7AB \\sim C6B-H8BB
 with sigma of 0.04
 C6A-H7AC \\sim C6B-H8BC
 with sigma of 0.04
 H6A-C8A \\sim H6B-C7B
 with sigma of 0.04
 H6A-C7A \\sim H6B-C8B
 with sigma of 0.04
 C8A-C7A \\sim C7B-C8B
 with sigma of 0.04
 H8AA-H8AB \\sim H7BC-H7BA
 with sigma of 0.04
 H8AA-H8AC \\sim H7BC-H7BB
 with sigma of 0.04
 H8AB-H8AC \\sim H7BA-H7BB
 with sigma of 0.04
 H7AA-H7AB \\sim H8BA-H8BB
 with sigma of 0.04
 H7AA-H7AC \\sim H8BA-H8BC
 with sigma of 0.04
 H7AB-H7AC \\sim H8BB-H8BC
 with sigma of 0.04
 C2S-C3S \\sim C2S-C4S
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O5B, C6B, C7B, C8B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Fixed Sof: O5A(0.75) H5AA(0.75) C6A(0.75) H6A(0.75) C8A(0.75) H8AA(0.75)
 H8AB(0.75) H8AC(0.75) C7A(0.75) H7AA(0.75) H7AB(0.75) H7AC(0.75) O5B(0.25)
 H5BA(0.25) C6B(0.25) H6B(0.25) C7B(0.25) H7BA(0.25) H7BB(0.25) H7BC(0.25)
 C8B(0.25) H8BA(0.25) H8BB(0.25) H8BC(0.25) O1S(0.25) H1S(0.25) C2S(0.25)
 H2S(0.25) C3S(0.25) H3SA(0.25) H3SB(0.25) H3SC(0.25) C4S(0.25) H4SA(0.25)
 H4SB(0.25) H4SC(0.25)
5.a Riding coordinates:
 C7B(H7BA,H7BB,H7BC), O1S(H1S)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C6A(H6A), C2S(H2S)
5.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C0AA(H0AA), C4A(H4A), C5A(H5A), C1AA(H1AA), C5B(H5B), C3A(H3A),
 C2B(H2B), C4B(H4B), C3B(H3BA)
5.d Idealised Me refined as rotating group:
 C3(H3B,H3C,H3D), C4(H4C,H4D,H4E), C8A(H8AA,H8AB,H8AC), C7A(H7AA,H7AB,H7AC),
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              89522
_olex2_submission_special_instructions 'No special instructions were received'