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_7120449
_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 Eu3 N2 O11 Si6'
_chemical_formula_weight         2016.52
_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
_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                112.016(3)
_cell_angle_beta                 94.082(3)
_cell_angle_gamma                104.427(3)
_cell_formula_units_Z            4
_cell_length_a                   16.608(3)
_cell_length_b                   24.187(4)
_cell_length_c                   27.710(4)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.31
_cell_volume                     9825(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_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            162625
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.752
_diffrn_reflns_theta_min         1.288
_diffrn_source                   'Micro Focus Rotating Anode'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  0.4903
_exptl_absorpt_correction_T_min  0.3774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0910 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.7723.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             4180
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.880
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1985
_refine_ls_number_reflns         37495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+13.8065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26135
_reflns_number_total             37495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04396a2.cif
_cod_data_source_block           evans3
_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               7120449
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.889
_shelx_res_checksum              12960