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_4346455
_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         'C42 H70 N10 O2 U, C2 H3 N'
_chemical_formula_sum            'C44 H73 N11 O2 U'
_chemical_formula_weight         1026.16
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.143(2)
_cell_angle_beta                 75.293(2)
_cell_angle_gamma                69.7870(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1487(2)
_cell_length_b                   13.5956(2)
_cell_length_c                   19.218(4)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.31
_cell_volume                     2335.8(5)
_computing_cell_refinement       'Bruker SMART, (Bruker, 2005)'
_computing_data_collection       'Bruker SMART, (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT, (Bruker, 2005)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32494
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    3.522
_exptl_absorpt_correction_T_max  0.7196
_exptl_absorpt_correction_T_min  0.3332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8849
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+1.3469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                8208
_reflns_number_total             8849
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b01547_si_001.cif
_cod_data_source_block           Comp4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4346455