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_4345219
_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 2-)2(C8 O4 H4 2-)2(H2 O1), H2 O1'
_chemical_formula_sum            'C16 H12 O13 U2'
_chemical_formula_weight         888.32
_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             2016-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                77.492(6)
_cell_angle_beta                 86.775(5)
_cell_angle_gamma                83.487(5)
_cell_formula_units_Z            2
_cell_length_a                   7.8178(7)
_cell_length_b                   9.5870(9)
_cell_length_c                   13.2310(13)
_cell_measurement_reflns_used    6113
_cell_measurement_temperature    299.82
_cell_measurement_theta_max      26.159
_cell_measurement_theta_min      2.411
_cell_volume                     961.36(16)
_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      299.82
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         1.577
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.896
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0778 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8362.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.069
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0199P)^2^+0.3620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3122
_reflns_number_total             3929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02962_si_001.cif
_cod_data_source_block           nm669_a
_cod_depositor_comments          'Adding full bibliography for 4345219.cif.'
_cod_database_code               4345219
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
2.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C6A(H6A), C5A(H5A), C5B(H5B), C4B(H4B), C6B(H6B), C3B(H3B)
;
_shelx_res_checksum              26934
_shelx_hkl_checksum              71423
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'