Uranium(III) redox chemistry assisted by a hemilabile bis(phenolate) cyclam ligand: uranium-nitrogen multiple bond formation comprising a trans-{RN═U(VI)═NR}(2+) complex.
Maria, Leonor; Santos, Isabel C.; Sousa, Vânia R; Marçalo, Joaquim; Inorganic chemistry 54 (2015) 9115–9126; doi:10.1021/acs.inorgchem.5b01547

data_4346459
_publ_section_title
;
 Uranium(III) redox chemistry assisted by a hemilabile bis(phenolate)
 cyclam ligand: uranium-nitrogen multiple bond formation comprising a
 trans-{RN&#x2550;U(VI)&#x2550;NR}(2+) complex.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9115
_journal_page_last               9126
_journal_paper_doi               10.1021/acs.inorgchem.5b01547
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C46 H70 N6 O2 U, 2(C24 H20 B), C H2 Cl2'
_chemical_formula_sum            'C95 H112 B2 Cl2 N6 O2 U'
_chemical_formula_weight         1700.46
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_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                 91.769(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6810(15)
_cell_length_b                   13.7702(10)
_cell_length_c                   30.849(2)
_cell_measurement_reflns_used    2063
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.51
_cell_measurement_theta_min      2.24
_cell_volume                     8781.0(11)
_computing_cell_refinement       'Bruker SMART, (Bruker, 2004)'
_computing_data_collection       'Bruker SMART, (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2004)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1652
_diffrn_reflns_av_sigmaI/netI    0.3022
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40485
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.5910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.870
_refine_diff_density_min         -2.099
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       0.0044(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         15346
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.2635
_refine_ls_R_factor_gt           0.1469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+0.9198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3091
_refine_ls_wR_factor_ref         0.3498
_reflns_number_gt                6718
_reflns_number_total             15346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01547_si_002.cif
_cod_data_source_block           comp3
_cod_original_cell_volume        8781.1(11)
_cod_original_sg_symbol_H-M      p_2/n
_cod_database_code               4346459