Thermally Stable Uranium Dinitrogen Complex with Siloxide Supporting Ligands
Mansell, Stephen M.; Farnaby, Joy H.; Germeroth, Anne I.; Arnold, Polly L.; Organometallics 32 (2013) 4214–; doi:10.1021/om4003957

data_4081054
_publ_section_title
;
 Thermally Stable Uranium Dinitrogen Complex with Siloxide Supporting
 Ligands
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4214
_journal_paper_doi               10.1021/om4003957
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C162 H198 N2 O6 Si6 U2'
_chemical_formula_sum            'C162 H198 N2 O6 Si6 U2'
_chemical_formula_weight         2913.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.943(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.2851(19)
_cell_length_b                   17.6856(10)
_cell_length_c                   29.4728(17)
_cell_measurement_reflns_used    8275
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      21.9810
_cell_measurement_theta_min      2.9296
_cell_volume                     15182.6(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2808
_diffrn_reflns_av_sigmaI/netI    0.2548
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79581
_diffrn_reflns_theta_full        22.03
_diffrn_reflns_theta_max         22.03
_diffrn_reflns_theta_min         2.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6000
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.049
_refine_diff_density_min         -2.920
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         15834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.3565
_refine_ls_R_factor_gt           0.2573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+3134.7124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5214
_refine_ls_wR_factor_ref         0.5687
_reflns_number_gt                7595
_reflns_number_total             15834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4003957_si_002.cif
_cod_data_source_block           1E_vacuum
_cod_database_code               4081054