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_7234996
_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         '0.125(C144 H64 O96 U8), 0.125(C8 N4)'
_chemical_formula_sum            'C19 H8 N0.5 O12 U'
_chemical_formula_weight         673.29
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-03
_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            8
_cell_length_a                   11.7099(16)
_cell_length_b                   11.7099(16)
_cell_length_c                   27.227(4)
_cell_measurement_reflns_used    8387
_cell_measurement_temperature    299.92
_cell_measurement_theta_max      26.146
_cell_measurement_theta_min      2.837
_cell_volume                     3733.4(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      299.92
_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 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0630
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            40345
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.361
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    8.769
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker, 2014/5) was used for absorption correction. wR2(int) was 0.1266 before and  0.0849 after correction. The Ratio of minimum to maximum transmission is 0.8675. The\I/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.396
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+10.1412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1660
_reflns_number_total             2335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03707a2.cif
_cod_data_source_block           tetrai41a
_cod_original_cell_volume        3733.4(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C19 H8 N0.50 O12 U'
_cod_database_code               7234996
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.499
_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. Others
 Fixed Sof: C10(0.25) C11(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9)
3.b Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              25413
_olex2_submission_special_instructions 'No special instructions were received'