Hydrothermal Crystallization of Uranyl Coordination Polymers Involving an Imidazolium Dicarboxylate Ligand: Effect of pH on the Nuclearity of Uranyl-Centered Subunits.
Martin, Nicolas P.; Falaise, Clément; Volkringer, Christophe; Henry, Natacha; Farger, Pierre; Falk, Camille; Delahaye, Emilie; Rabu, Pierre; Loiseau, Thierry; Inorganic chemistry 55 (2016) 8697–8705; doi:10.1021/acs.inorgchem.6b01232

data_4348491
_publ_section_title
;
 Hydrothermal Crystallization of Uranyl Coordination Polymers Involving an
 Imidazolium Dicarboxylate Ligand: Effect of pH on the Nuclearity of
 Uranyl-Centered Subunits.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8697
_journal_page_last               8705
_journal_paper_doi               10.1021/acs.inorgchem.6b01232
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '0.5(C16 H16 N4 O16 U2), 1.5(O)'
_chemical_formula_sum            'C8 H8 N2 O9.5 U'
_chemical_formula_weight         522.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-11
_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            4
_cell_length_a                   5.7412(3)
_cell_length_b                   14.4322(6)
_cell_length_c                   15.7094(7)
_cell_measurement_reflns_used    2158
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.226
_cell_measurement_theta_min      2.593
_cell_volume                     1301.65(10)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.521
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0384 after correction.
The Ratio of minimum to maximum transmission is 0.6154.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.118
_refine_diff_density_max         3.097
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0524P)^2^+5.3671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1217
_reflns_number_total             1679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01232_si_002.cif
_cod_data_source_block           orthopnnm
_cod_original_formula_sum        'C8 H8 N2 O9.50 U'
_cod_database_code               4348491
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: N1(0.5) H4AB(0.5) H4AA(0.5) H4BC(0.5) H4BD(0.5) C3(0.5) H3(0.5)
 N2(0.5) C6(0.5) H6(0.5) O1AA(0.25) O0AA(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4AB,H4AA), C4(H4BC,H4BD)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C2(H2B), C3(H3), C6(H6)
 Thermal parameters of the two water molecules O1AA and O0AA are large,
 probably due to their positions within voids of the structure. This may
 reflect a slight disordered situation for them.
;
_shelx_res_checksum              24871
_shelx_hkl_checksum              9714
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'