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_4346457
_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         'C54 H80 N6 O2 U'
_chemical_formula_sum            'C54 H80 N6 O2 U'
_chemical_formula_weight         1083.27
_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                103.1520(10)
_cell_angle_beta                 109.5310(10)
_cell_angle_gamma                106.6290(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3031(2)
_cell_length_b                   13.9263(2)
_cell_length_c                   16.7844(3)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.67
_cell_volume                     2622.03(8)
_computing_cell_refinement       'Bruker SAINT, (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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35967
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    3.139
_exptl_absorpt_correction_T_max  0.6019
_exptl_absorpt_correction_T_min  0.3028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2004'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
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_refine_diff_density_max         1.524
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0241P)^2^+1.8148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0493
_reflns_number_gt                9046
_reflns_number_total             9668
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           comp6
_cod_original_cell_volume        2622.03(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4346457