Structural, Spectroscopic, and Theoretical Comparison of Traditional vs Recently Discovered Ln(2+) Ions in the [K(2.2.2-cryptand)][(C5H4SiMe3)3Ln] Complexes: The Variable Nature of Dy(2+) and Nd(2+).
Fieser, Megan E.; MacDonald, Matthew R.; Krull, Brandon T.; Bates, Jefferson E.; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Journal of the American Chemical Society 137 (2015) 369–382; doi:10.1021/ja510831n

data_4123168
_publ_section_title
;
 Structural, Spectroscopic, and Theoretical Comparison of Traditional vs
 Recently Discovered Ln(2+) Ions in the
 [K(2.2.2-cryptand)][(C5H4SiMe3)3Ln] Complexes: The Variable Nature of
 Dy(2+) and Nd(2+).
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              369
_journal_page_last               382
_journal_paper_doi               10.1021/ja510831n
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C46 H83 K N2 O7 Si3 Sm'
_chemical_formula_weight         1049.86
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.6567(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0764(7)
_cell_length_b                   24.4921(10)
_cell_length_c                   13.7530(6)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.53
_cell_volume                     5414.8(4)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2012.4-0, 2012'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55567
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         1.515
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.8970
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         10283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0200P)^2^+21.1276P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9521
_reflns_number_total             10283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510831n_si_003.cif
_cod_data_source_block           mrm66
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4123164--4123176.cif.
;
_cod_database_code               4123168
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.890
_shelxl_version_number           2013-2
_shelx_res_checksum              80127
_shelx_hkl_checksum              9937