Synthesis, Structures, and Proton Self-Exchange Reaction of μ3-Oxido/Hydroxido Bridged Trinuclear Uranyl(VI) Complexes with Tridentate Schiff-Base Ligands.
Yoshimura, Takashi; Nakaguchi, Masayuki; Morimoto, Keisuke; Inorganic chemistry 56 (2017) 4057–4064; doi:10.1021/acs.inorgchem.6b03175

data_4345602
_publ_section_title
;
 Synthesis, Structures, and Proton Self-Exchange Reaction of
 \m3-Oxido/Hydroxido Bridged Trinuclear Uranyl(VI) Complexes with
 Tridentate Schiff-Base Ligands.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4057
_journal_page_last               4064
_journal_paper_doi               10.1021/acs.inorgchem.6b03175
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C82 H107 Cl2 N4 O13 U3'
_chemical_formula_sum            'C82 H107 Cl2 N4 O13 U3'
_chemical_formula_weight         2141.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.273(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   20.122(2)
_cell_length_b                   19.3936(19)
_cell_length_c                   23.387(2)
_cell_measurement_reflns_used    59487
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.99
_cell_volume                     9071.9(15)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1193
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            86549
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         2.990
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.459
_exptl_absorpt_correction_T_max  0.309
_exptl_absorpt_correction_T_min  0.039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4164.00
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.215
_refine_diff_density_max         5.92
_refine_diff_density_min         -1.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     910
_refine_ls_number_reflns         20712
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1046P)^2^+96.5626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2455
_reflns_number_gt                12863
_reflns_number_total             20712
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic6b03175_si_002.cif
_cod_data_source_block           Et3NH[1]
_cod_original_cell_volume        9071.7(16)
_cod_database_code               4345602