Molecular and Electronic Structures of Eight-Coordinate Uranium Bipyridine Complexes: A Rare Example of a Bipy(2-) Ligand Coordinated to a U(4+) Ion.
Rosenzweig, Michael W.; Heinemann, Frank W.; Maron, Laurent; Meyer, Karsten; Inorganic chemistry 56 (2017) 2792–2800; doi:10.1021/acs.inorgchem.6b02954

data_4345209
_publ_section_title
;
 Molecular and Electronic Structures of Eight-Coordinate Uranium
 Bipyridine Complexes: A Rare Example of a Bipy(2-) Ligand Coordinated to
 a U(4+) Ion.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2792
_journal_page_last               2800
_journal_paper_doi               10.1021/acs.inorgchem.6b02954
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C79 H104 N5 O3 U, C18 H36 K N2 O6, 2 (C5 H12)'
_chemical_formula_sum            'C107 H164 K N7 O9 U'
_chemical_formula_weight         1969.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.283(3)
_cell_length_b                   11.4771(9)
_cell_length_c                   27.246(2)
_cell_measurement_reflns_used    9589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.32
_cell_volume                     10095.1(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            398546
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1483 before and 0.1014 after correction.
The ratio of minimum to maximum transmission is 0.7932.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.707
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.082(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         22222
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+72.5667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                19464
_reflns_number_total             22222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02954_si_002.cif
_cod_data_source_block           mr1701
_cod_depositor_comments
'Adding full bibliography for 4345208--4345209.cif.'
_cod_original_cell_volume        10095.2(14)
_cod_database_code               4345209