Synthesis of Coordination Polymers of Tetravalent Actinides (Uranium and Neptunium) with a Phthalate or Mellitate Ligand in an Aqueous Medium.
Martin, Nicolas P.; März, Juliane; Volkringer, Christophe; Henry, Natacha; Hennig, Christoph; Ikeda-Ohno, Atsushi; Loiseau, Thierry; Inorganic chemistry 56 (2017) 2902–2913; doi:10.1021/acs.inorgchem.6b02962

data_4345555
_publ_section_title
;
 Synthesis of Coordination Polymers of Tetravalent Actinides (Uranium and
 Neptunium) with a Phthalate or Mellitate Ligand in an Aqueous Medium.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2902
_journal_page_last               2913
_journal_paper_doi               10.1021/acs.inorgchem.6b02962
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         '2(U1 4+)2(O1 H1 1-)(C12 O12 6-)2(H2 O1)'
_chemical_formula_sum            'C12 H4 O16 U2'
_chemical_formula_weight         880.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.903(3)
_cell_length_b                   19.813(5)
_cell_length_c                   11.393(3)
_cell_measurement_reflns_used    2174
_cell_measurement_temperature    299.48
_cell_measurement_theta_max      19.506
_cell_measurement_theta_min      2.530
_cell_volume                     3138.3(13)
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      299.48
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13003
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.454
_diffrn_reflns_theta_min         2.530
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.714
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0916 before and 0.0729 after correction.
The Ratio of minimum to maximum transmission is 0.8103.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.726
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.057
_refine_diff_density_max         2.857
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.324
_refine_ls_abs_structure_details
;
 Flack x determined using 509 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.507(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1589
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0638P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                1274
_reflns_number_total             1589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02962_si_003.cif
_cod_data_source_block           nm653_a
_cod_original_cell_volume        3138.4(14)
_cod_database_code               4345555
_shelx_estimated_absorpt_t_max   0.385
_shelx_estimated_absorpt_t_min   0.254
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB)
;
_shelx_res_checksum              8175
_shelx_hkl_checksum              54309
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'