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_4128186
_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 H114 Gd N3 O9, 4(C5 H5 N)'
_chemical_formula_sum            'C104 H134 Gd N7 O9'
_chemical_formula_weight         1783.42
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.410(3)
_cell_length_b                   26.353(5)
_cell_length_c                   25.890(5)
_cell_measurement_reflns_used    87234
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.527
_cell_measurement_theta_min      2.226
_cell_volume                     9657(3)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev794 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            87234
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.527
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             3772
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.300
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_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         24266
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15214
_reflns_number_total             24266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10251_si_002.cif
_cod_data_source_block           SAP136
_cod_database_code               4128186
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.689
_shelx_estimated_absorpt_t_max   0.807
_shelx_res_checksum              62028
_shelx_hkl_checksum              84863