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_4347184
_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         'C25 H40 Cl4 Li2 N2 O3 Th, C3'
_chemical_formula_sum            'C28 H40 Cl4 Li2 N2 O3 Th'
_chemical_formula_weight         840.34
_chemical_name_common            'Moris393 (Rami)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                74.50(3)
_cell_angle_beta                 76.40(4)
_cell_angle_gamma                67.87(6)
_cell_formula_units_Z            2
_cell_length_a                   8.745(18)
_cell_length_b                   9.35(4)
_cell_length_c                   15.89(5)
_cell_measurement_reflns_used    4299
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.4
_cell_volume                     1147(7)
_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 0.979
_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_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4058
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.399
_diffrn_source                   graphite
_exptl_absorpt_coefficient_mu    7.010
_exptl_absorpt_correction_T_max  0.5710
_exptl_absorpt_correction_T_min  0.3206
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.433
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_refine_diff_density_max         3.991
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4050
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1003P)^2^+70.6849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3893
_reflns_number_total             4050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02853_si_003.cif
_cod_data_source_block           Moris393
_cod_database_code               4347184
_shelx_estimated_absorpt_t_min   0.321
_shelx_estimated_absorpt_t_max   0.571
_diffrn_reflnslimit_h_min        0
_shelxl_version_number           2013-4
_shelx_res_checksum              86137
_shelx_hkl_checksum              28949