Uranium(III) Coordination Chemistry and Oxidation in a Flexible Small-Cavity Macrocycle
Arnold, Polly L.; Farnaby, Joy H.; Gardiner, Michael G.; Love, Jason B.; Organometallics 34 (2015) 2114–; doi:10.1021/om5012193

data_4085358
_publ_section_title
;
 Uranium(III) Coordination Chemistry and Oxidation in a Flexible
 Small-Cavity Macrocycle
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2114
_journal_paper_doi               10.1021/om5012193
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C38 H54 N3 Si2 U'
_chemical_formula_sum            'C38 H54 N3 Si2 U'
_chemical_formula_weight         847.05
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 122.539(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.993(5)
_cell_length_b                   13.296(5)
_cell_length_c                   24.124(5)
_cell_measurement_reflns_used    15310
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.3450
_cell_measurement_theta_min      3.6380
_cell_volume                     3513(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    ortep
_computing_publication_material  mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    4.719
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.1096
_exptl_crystal_size_mid          0.1052
_exptl_crystal_size_min          0.0557
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8505
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0168P)^2^+5.6231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                7673
_reflns_number_total             8505
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5012193_si_001.cif
_cod_data_source_block           po4033_tri_refinalized
_cod_depositor_comments
'Adding full bibliography for 4085357--4085359.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4085358