Bonding analysis in ytterbium(ii) distannyl and related tetryls
Chapple, Peter M.; Cartron, Julien; Hamdoun, Ghanem; Cordier, Marie; Kahlal, Samia; Oulyadi, Hassan; Carpentier, Jean-François; Saillard, Jean-Yves; Sarazin, Yann; Dalton Transactions  (2021) –; doi:10.1039/D1DT02355A

data_7708404
_publ_section_title
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 Bonding analysis in ytterbium(ii) distannyl and related tetryls
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02355A
_journal_year                    2021
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H78 Ge2 O3 Si6 Yb'
_chemical_formula_sum            'C30 H78 Ge2 O3 Si6 Yb'
_chemical_formula_weight         973.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-02-01 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.943(3)
_cell_length_b                   15.0354(17)
_cell_length_c                   17.129(2)
_cell_measurement_reflns_used    9733
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5049
_cell_measurement_theta_min      2.8061
_cell_measurement_wavelength     0.710730
_cell_volume                     4878.6(11)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155'
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0406018
_diffrn_orient_matrix_UB_12      0.0419516
_diffrn_orient_matrix_UB_13      0.0175852
_diffrn_orient_matrix_UB_21      -0.0129965
_diffrn_orient_matrix_UB_22      -0.0317715
_diffrn_orient_matrix_UB_23      0.0430703
_diffrn_orient_matrix_UB_31      0.0510504
_diffrn_orient_matrix_UB_32      0.0252769
_diffrn_orient_matrix_UB_33      0.0249509
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48766
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         2.099
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.297
_exptl_absorpt_correction_T_max  0.384
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.301(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         11236
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0140P)^2^+3.6204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                10170
_reflns_number_total             11236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt02355a3.cif
_cod_data_source_block           PC05078
_cod_database_code               7708404
_shelx_res_checksum              94532
_shelx_hkl_checksum              17370