Synthesis of Rare-Earth-Metal-in-Cryptand Dications, [Ln(2.2.2-cryptand)]2+, from Sm2+, Eu2+, and Yb2+ Silyl Metallocenes (C5H4SiMe3)2Ln(THF)2
Huh, Daniel N.; Kotyk, Christopher Matthew; Gembicky, Milan; Rheingold, Arnold L.; Ziller, Joseph W.; Evans, William J.; Chem. Commun.  (2017) –; doi:10.1039/C7CC04396A

data_7120447
_publ_section_title
;
 Synthesis of Rare-Earth-Metal-in-Cryptand Dications,
 [Ln(2.2.2-cryptand)]2+, from Sm2+, Eu2+, and Yb2+ Silyl Metallocenes
 (C5H4SiMe3)2Ln(THF)2
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04396A
_journal_year                    2017
_chemical_formula_sum            'C87 H138 N2 O6 Si6 Yb3'
_chemical_formula_weight         1995.65
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-19 deposited with the CCDC.
2017-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8892(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6054(13)
_cell_length_b                   25.418(2)
_cell_length_c                   23.8913(19)
_cell_measurement_reflns_used    9574
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      2.24
_cell_volume                     9442.2(13)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART 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  0.0452
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            115724
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.134
_diffrn_reflns_theta_min         1.535
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.070
_exptl_absorpt_correction_T_max  0.6946
_exptl_absorpt_correction_T_min  0.4909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.474
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.151
_refine_diff_density_max         2.082
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         24068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0359P)^2^+38.8227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19184
_reflns_number_total             24068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04396a2.cif
_cod_data_source_block           dnh30
_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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        9442.3(13)
_cod_database_code               7120447
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.324
_shelx_estimated_absorpt_t_max   0.654
_shelx_res_checksum              9601