Synthesis, Structure, and Reactivity of Disiloxa[3]tetrelocenophanes.
Wirtz, Lisa; Jourdain, Matthias; Huch, Volker; Zimmer, Michael; Schäfer, André; ACS omega 4 (2019) 18355–18360; doi:10.1021/acsomega.9b02605

data_4516992
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Disiloxa[3]tetrelocenophanes.
;
_journal_issue                   19
_journal_name_full               'ACS omega'
_journal_page_first              18355
_journal_page_last               18360
_journal_paper_doi               10.1021/acsomega.9b02605
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C21 H32 N2 O Pb Si2'
_chemical_formula_sum            'C21 H32 N2 O Pb Si2'
_chemical_formula_weight         591.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8368(12)
_cell_length_b                   12.0431(8)
_cell_length_c                   11.5413(9)
_cell_measurement_reflns_used    4320
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.42
_cell_volume                     2340.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0823
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33867
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.683
_diffrn_reflns_theta_min         2.419
_exptl_absorpt_coefficient_mu    7.325
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.5701
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.366
_refine_diff_density_min         -2.970
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+18.1844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2647
_reflns_number_total             3147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b02605_si_007.cif
_cod_data_source_block           sh4177
_cod_database_code               4516992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.322
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              98825
_shelx_hkl_checksum              4474