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_7120448
_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_absolute_configuration unk
_chemical_formula_sum            'C42 H82 N2 O7 Si4 Sm2'
_chemical_formula_weight         1140.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 96.6221(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0618(16)
_cell_length_b                   17.0180(16)
_cell_length_c                   39.546(4)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.39
_cell_volume                     11405.9(19)
_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      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.920
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            55033
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.879
_diffrn_reflns_theta_min         1.696
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.225
_refine_diff_density_max         3.373
_refine_diff_density_min         -3.291
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         25579
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+312.3864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                22978
_reflns_number_total             25579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04396a2.cif
_cod_data_source_block           cmk30
_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        11406.0(19)
_cod_database_code               7120448
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.642
_shelx_res_checksum              61978
_shelx_fab_checksum              91595