Covalency in Lanthanides. An X-ray Absorption Spectroscopy and Density Functional Theory Study of LnCl6(x-) (x = 3, 2).
Löble, Matthias W; Keith, Jason M.; Altman, Alison B.; Stieber, S Chantal E; Batista, Enrique R.; Boland, Kevin S.; Conradson, Steven D.; Clark, David L.; Lezama Pacheco, Juan; Kozimor, Stosh A.; Martin, Richard L.; Minasian, Stefan G.; Olson, Angela C.; Scott, Brian L.; Shuh, David K.; Tyliszczak, Tolek; Wilkerson, Marianne P.; Zehnder, Ralph A.; Journal of the American Chemical Society 137 (2015) 2506–2523; doi:10.1021/ja510067v

data_4123458
_publ_section_title
;
 Covalency in Lanthanides. An X-ray Absorption Spectroscopy and Density
 Functional Theory Study of LnCl6(x-) (x = 3, 2).
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2506
_journal_page_last               2523
_journal_paper_doi               10.1021/ja510067v
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C80 H72 Ce Cl6 N4 P3'
_chemical_formula_weight         1535.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.415(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4642(9)
_cell_length_b                   15.2500(9)
_cell_length_c                   16.0021(9)
_cell_measurement_temperature    140(1)
_cell_volume                     3772.6(4)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_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      140(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43037
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.9297
_exptl_absorpt_correction_T_min  0.8367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         17397
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                15944
_reflns_number_total             17397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja510067v_si_002.cif
_cod_data_source_block           apx1649
_cod_depositor_comments
'Adding full bibliography for 4123456--4123460.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4123458