Synthesis of Coordinatively Unsaturated Tetravalent Actinide Complexes with η(5) Coordination of Pyrrole.
Batrice, Rami J.; Fridman, Natalia; Eisen, Moris S.; Inorganic chemistry 55 (2016) 2998–3006; doi:10.1021/acs.inorgchem.5b02853

data_4347183
_publ_section_title
;
 Synthesis of Coordinatively Unsaturated Tetravalent Actinide Complexes
 with \h(5) Coordination of Pyrrole.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2998
_journal_page_last               3006
_journal_paper_doi               10.1021/acs.inorgchem.5b02853
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C34 H48 Cl2 Li2 N4 O2 U'
_chemical_formula_sum            'C34 H48 Cl2 Li2 N4 O2 U'
_chemical_formula_weight         867.57
_chemical_name_common            Moris407
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.7620(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3080(8)
_cell_length_b                   11.5880(5)
_cell_length_c                   17.4560(10)
_cell_measurement_reflns_used    5207
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.49
_cell_measurement_theta_min      1.19
_cell_volume                     3469.0(3)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Mercury 3.5'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.817
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.817
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5119
_diffrn_reflns_point_group_measured_fraction_full 0.817
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.490
_diffrn_reflns_theta_min         1.187
_diffrn_source                   graphite
_exptl_absorpt_coefficient_mu    4.869
_exptl_absorpt_correction_T_max  0.2320
_exptl_absorpt_correction_T_min  0.1890
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+23.2210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3799
_reflns_number_total             5119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02853_si_002.cif
_cod_data_source_block           Moris407
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347183
_shelx_estimated_absorpt_t_min   0.218
_shelx_estimated_absorpt_t_max   0.323
_shelxl_version_number           2013-4
_shelx_res_checksum              56310
_shelx_hkl_checksum              38108