Counter-ion control of structure in uranyl ion complexes with 2,5-thiophenedicarboxylate
Thuéry, Pierre; Harrowfield, Jack; CrystEngComm 18 (2016) 1550–; doi:10.1039/C5CE02294K

data_7224010
_publ_section_title
;
 Counter-ion control of structure in uranyl ion complexes with
 2,5-thiophenedicarboxylate
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1550
_journal_paper_doi               10.1039/C5CE02294K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C128 H96 Fe2 N18 O44 S6 U5'
_chemical_formula_weight         4084.43
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                68.574(3)
_cell_angle_beta                 70.094(3)
_cell_angle_gamma                76.948(3)
_cell_formula_units_Z            1
_cell_length_a                   13.7311(8)
_cell_length_b                   15.5105(9)
_cell_length_c                   17.8862(9)
_cell_measurement_reflns_used    156076
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.03
_cell_volume                     3311.7(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 \f and 11 \w scans with 2\% steps (630 frames)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            156076
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.031
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.492
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1950
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.489
_refine_diff_density_min         -6.563
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         12556
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0655P)^2^+42.4307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10361
_reflns_number_total             12556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02294k1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7224008--7224013.cif.'
_cod_database_code               7224010
_shelxl_version_number           2014-3
_shelx_res_checksum              76178