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_7120450
_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            'C86 H154 N2 O11 Si6 Sm3'
_chemical_formula_weight         2011.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                112.1043(15)
_cell_angle_beta                 94.4050(16)
_cell_angle_gamma                104.1064(16)
_cell_formula_units_Z            4
_cell_length_a                   16.635(2)
_cell_length_b                   24.176(3)
_cell_length_c                   27.798(4)
_cell_measurement_reflns_used    5507
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.31
_cell_volume                     9867(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.1569
_diffrn_reflns_av_unetI/netI     0.2057
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            100892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.696
_diffrn_reflns_theta_min         1.285
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.660
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1975
_refine_ls_number_reflns         37384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17221
_reflns_number_total             37384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04396a2.cif
_cod_data_source_block           dnh16
_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_database_code               7120450
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.792
_shelx_res_checksum              86613