Synthesis, structure, and reactivity of zwitterionic divalent rare-Earth metal silanides.
Thalangamaarachchige, Vidura D.; Unruh, Daniel K.; Cordes, David B.; Krempner, Clemens; Inorganic chemistry 54 (2015) 4189–4191; doi:10.1021/acs.inorgchem.5b00542

data_4343245
_publ_section_title
;
 Synthesis, structure, and reactivity of zwitterionic divalent rare-Earth
 metal silanides.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4189
_journal_page_last               4191
_journal_paper_doi               10.1021/acs.inorgchem.5b00542
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C54 H84 B2 O6 Si8 Yb, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H100 B2 O8 Si8 Yb'
_chemical_formula_weight         1392.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.8720(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6349(13)
_cell_length_b                   20.318(2)
_cell_length_c                   13.6729(14)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.27
_cell_volume                     3502.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.986
_diffrn_reflns_theta_min         1.798
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         8419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0243P)^2^+1.6506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6981
_reflns_number_total             8419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00542_si_002.cif
_cod_data_source_block           Yb-4
_cod_database_code               4343245
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.888
_shelxl_version_number           2014-3
_shelx_res_checksum              97027
_shelx_hkl_checksum              6111