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_4348493
_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
'3(U1 O2 2+)(O1 2-)3(O1 H1 1-)(C7 N2 H7 O4 1-) , 2(H2 O1)'
_chemical_formula_sum            'C7 H7 N2 O16 U3'
_chemical_formula_weight         1089.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.723(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.761(2)
_cell_length_b                   12.5678(11)
_cell_length_c                   15.5142(15)
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    299.37
_cell_measurement_theta_max      25.843
_cell_measurement_theta_min      2.682
_cell_volume                     3772.6(6)
_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      299.37
_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 0.983
_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  0.0835
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.620
_diffrn_reflns_theta_min         1.932
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.773
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1114 before and 0.0772 after correction.
The Ratio of minimum to maximum transmission is 0.6626.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.835
_exptl_crystal_description       needle
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0250P)^2^+31.0970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3141
_reflns_number_total             3903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01232_si_004.cif
_cod_data_source_block           monoc2c
_cod_original_cell_volume        3772.7(6)
_cod_database_code               4348493
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C3(H3)
 Thermal parameters of the two water molecules O1W and O2W are large,
 probably due to their positions within voids of the structure. This may
 reflect a slight disordered situation for them. Moreover, a Alert A is 
 related to short inter-atomic distances (2.46 &#x0081;) between these two
 water molecules.
;
_shelx_res_checksum              72082
_shelx_hkl_checksum              73900
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'