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_4347185
_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 Th'
_chemical_formula_sum            'C34 H48 Cl2 Li2 N4 O2 Th'
_chemical_formula_weight         861.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.180(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.753(4)
_cell_length_b                   10.150(6)
_cell_length_c                   17.081(3)
_cell_measurement_reflns_used    4477
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.17
_cell_volume                     3561(2)
_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 0.977
_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     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3147
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_min         2.608
_diffrn_source                   graphite
_exptl_absorpt_coefficient_mu    4.372
_exptl_absorpt_correction_T_max  0.229
_exptl_absorpt_correction_T_min  0.226
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.948
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+18.9441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.670
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2997
_reflns_number_total             3147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02853_si_001.cif
_cod_data_source_block           Moris395
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347185
_shelx_estimated_absorpt_t_min   0.226
_shelx_estimated_absorpt_t_max   0.269
_shelxl_version_number           2013-4
_shelx_res_checksum              40163
_shelx_hkl_checksum              71887