Differential uranyl(v) oxo-group bonding between the uranium and metal cations from groups 1, 2, 4, and 12; a high energy resolution X-ray absorption, computational, and synthetic study
Zegke, Markus; Zhang, Xiaobin; Pidchenko, Ivan; Hlina, Johann A.; Lord, Rianne M.; Purkis, Jamie; Nichol, Gary S.; Magnani, Nicola; Schreckenbach, Georg; Vitova, Tonya; Love, Jason B.; Arnold, Polly L.; Chemical Science 10 (2019) 9740–; doi:10.1039/C8SC05717F

data_1554601
_publ_section_title
;
 Differential uranyl(v) oxo-group bonding between the uranium and metal
 cations from groups 1, 2, 4, and 12; a high energy resolution X-ray
 absorption, computational, and synthetic study
;
_journal_issue                   42
_journal_name_full               'Chemical Science'
_journal_page_first              9740
_journal_paper_doi               10.1039/C8SC05717F
_journal_volume                  10
_journal_year                    2019
_chemical_formula_sum            'C65 H73 Ca I N11 O4 U'
_chemical_formula_weight         1477.35
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.157(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4073(7)
_cell_length_b                   15.5310(4)
_cell_length_c                   33.3439(15)
_cell_measurement_reflns_used    25595
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.9330
_cell_measurement_theta_min      3.2350
_cell_volume                     8225.2(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 8.0521
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            130415
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    2.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.6567
_exptl_crystal_size_mid          0.5351
_exptl_crystal_size_min          0.2440
_refine_diff_density_max         3.217
_refine_diff_density_min         -9.138
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11791
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.1207
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1017.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2758
_refine_ls_wR_factor_ref         0.2816
_reflns_number_gt                10091
_reflns_number_total             11791
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8sc05717f2.cif
_cod_data_source_block           p14107_reint_ref-sr
_cod_original_cell_volume        8225.2(5)
_cod_database_code               1554601