The "Wanderlust" of Me<sub>3</sub>Si groups in rare-earth triple-decker complexes: a combined experimental and computational study.
Lorenz, Volker; Liebing, Phil; Bathelier, Adrien; Engelhardt, Felix; Maron, Laurent; Hilfert, Liane; Busse, Sabine; Edelmann, Frank T.; Chemical communications (Cambridge, England) 54 (2018) 10280–10283; doi:10.1039/c8cc05317k

data_7122215
_publ_section_title
;
 The &quot;Wanderlust&quot; of Me<sub>3</sub>Si groups in rare-earth
 triple-decker complexes: a combined experimental and computational study.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10280
_journal_page_last               10283
_journal_paper_doi               10.1039/c8cc05317k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C42 H72 La2 Si6'
_chemical_formula_weight         1023.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-04-25 deposited with the CCDC.
2018-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.11(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.747(5)
_cell_length_b                   20.280(4)
_cell_length_c                   20.734(8)
_cell_measurement_reflns_used    33493
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.203
_cell_measurement_theta_min      1.935
_cell_volume                     4927(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      ' 143 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33493
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.203
_diffrn_reflns_theta_max         25.203
_diffrn_reflns_theta_min         1.935
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.7567
_exptl_absorpt_correction_T_min  0.6186
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.673
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 6705 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(11)
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         33493
_refine_ls_number_restraints     2200
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0889P)^2^+35.5807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                32468
_reflns_number_total             33493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05317k2.cif
_cod_data_source_block           fe0160_a
_cod_depositor_comments
'Adding full bibliography for 7122212--7122216.cif.'
_cod_database_code               7122215
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details   'STOE X-RED'
_shelx_res_checksum              27695