Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)2 followed by the formation of molecular poly-oxo cluster {U14} containing hemimellitate uranium(iv)
Dufaye, Maxime; Martin, Nicolas P.; Duval, Sylvain; Volkringer, Christophe; Ikeda-Ohno, Atsushi; Loiseau, Thierry; RSC Advances 9 (2019) 22795–; doi:10.1039/C9RA03707A

data_7234997
_publ_section_title
;
 Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)2
 followed by the formation of molecular poly-oxo cluster {U14} containing
 hemimellitate uranium(iv)
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              22795
_journal_paper_doi               10.1039/C9RA03707A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C88 H28 Cl8 O100 U14, 6(O4)'
_chemical_formula_sum            'C88 H28 Cl8 O124 U14'
_chemical_formula_weight         6685.12
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-11 deposited with the CCDC.	2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.247(2)
_cell_length_b                   18.247(2)
_cell_length_c                   29.034(3)
_cell_measurement_reflns_used    3826
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      16.39
_cell_measurement_theta_min      2.38
_cell_volume                     9667.0(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1273
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25791
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        16.588
_diffrn_reflns_theta_max         16.588
_diffrn_reflns_theta_min         1.318
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.890
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.5140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1250 before and 0.0792 after correction. The Ratio of minimum to maximum transmission is 0.6909. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_description       plate
_exptl_crystal_F_000             5944
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details
;
 Flack x determined using 891 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.552(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0791P)^2^+783.5139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2091
_reflns_number_total             2633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03707a2.cif
_cod_data_source_block           md200d125
_cod_original_cell_volume        9667(2)
_cod_database_code               7234997
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.648
_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. Restrained distances
 C16-O17
 1.22 with sigma of 0.02
 C16-O16
 1.28 with sigma of 0.02
 C15-C16
 1.5 with sigma of 0.02
 C18-C17
 1.5 with sigma of 0.02
 C7-C9
 1.5 with sigma of 0.02
 C22-C21
 1.5 with sigma of 0.02
 C10-O14
 1.25 with sigma of 0.02
 C19-O23
 1.22 with sigma of 0.02
 O22-C19
 1.28 with sigma of 0.02
 C20-C19
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: O7W(0.5) O4W(0.5) O5W(0.5) O9W(0.5) O1W(0.5) O2W(0.5) O8W(0.5)
 O11W(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C5(H5), C4(H4), C3(H3)
4.b Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C17,C11), C7(C6,C5,C4,C3,C2)
4.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              9436
_olex2_submission_special_instructions 'No special instructions were received'