Synthesis, Characterization, and Density Functional Theory Analysis of Uranium and Thorium Complexes Containing Nitrogen-Rich 5-Methyltetrazolate Ligands.
Browne, Kevin P.; Maerzke, Katie A.; Travia, Nicholas E.; Morris, David E.; Scott, Brian L.; Henson, Neil J.; Yang, Ping; Kiplinger, Jaqueline L.; Veauthier, Jacqueline M.; Inorganic chemistry 55 (2016) 4941–4950; doi:10.1021/acs.inorgchem.6b00492

data_4347704
_publ_section_title
;
 Synthesis, Characterization, and Density Functional Theory Analysis of
 Uranium and Thorium Complexes Containing Nitrogen-Rich
 5-Methyltetrazolate Ligands.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4941
_journal_page_last               4950
_journal_paper_doi               10.1021/acs.inorgchem.6b00492
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C24 H36 N8 U'
_chemical_formula_weight         674.64
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/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                 115.120(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.226(5)
_cell_length_b                   10.8224(14)
_cell_length_c                   15.090(2)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      35.09
_cell_measurement_theta_min      2.68
_cell_volume                     5208.7(12)
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15232
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.27
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.260
_exptl_absorpt_correction_T_max  0.4744
_exptl_absorpt_correction_T_min  0.4341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2014/3 (Bruker AXS, 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.294
_refine_diff_density_min         -3.955
_refine_diff_density_rms         0.639
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         10184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                8679
_reflns_number_total             10184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00492_si_004.cif
_cod_data_source_block           dq0289
_cod_original_cell_volume        5208.6(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347704