Synthesis and Characterization of Tris-chelate Complexes for Understanding f-Orbital Bonding in Later Actinides.
Galley, Shane S.; Pattenaude, Scott A.; Gaggioli, Carlo Alberto; Qiao, Yusen; Sperling, Joseph M.; Zeller, Matthias; Pakhira, Srimanta; Mendoza-Cortes, Jose L; Schelter, Eric J.; Albrecht-Schmitt, Thomas E; Gagliardi, Laura; Bart, Suzanne C.; Journal of the American Chemical Society 141 (2019) 2356–2366; doi:10.1021/jacs.8b10251

data_4128191
_publ_section_title
;
 Synthesis and Characterization of Tris-chelate Complexes for
 Understanding f-Orbital Bonding in Later Actinides.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2356
_journal_page_last               2366
_journal_paper_doi               10.1021/jacs.8b10251
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C84 H104 Cf N3 O9, 4(C5 H5 N)'
_chemical_formula_sum            'C104 H134 Cf N7 O9'
_chemical_formula_weight         1875.17
_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-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 100.6914(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3744(7)
_cell_length_b                   26.2457(12)
_cell_length_c                   25.7763(12)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    131(2)
_cell_measurement_theta_max      27.5596
_cell_measurement_theta_min      2.3589
_cell_volume                     9555.7(8)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex2 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      131(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker ApexII CCD diffractometer'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            148384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.
(2015). J. Appl. Cryst. 48 3-10.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             3908
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.075
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         22211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+15.4457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17559
_reflns_number_total             22211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10251_si_006.cif
_cod_data_source_block           TrisDopoCf
_cod_database_code               4128191
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              70285
_shelx_hkl_checksum              90560