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_4516991
_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         'C14 H20 O Pb Si2'
_chemical_formula_sum            'C14 H20 O Pb Si2'
_chemical_formula_weight         467.67
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.897(2)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   14.6027(5)
_cell_length_b                   21.7849(9)
_cell_length_c                   31.2862(13)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    172(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.29
_cell_volume                     9833.0(7)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      172(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0688
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            195438
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.011
_diffrn_reflns_theta_min         1.144
_exptl_absorpt_coefficient_mu    10.428
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4948
_exptl_absorpt_correction_type   multi-scan
_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            yellow
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_description       needle
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.505
_refine_diff_density_min         -2.128
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         23667
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+46.7597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17032
_reflns_number_total             23667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b02605_si_005.cif
_cod_data_source_block           sh3801c
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4516991
_shelx_estimated_absorpt_t_min   0.195
_shelx_estimated_absorpt_t_max   0.674
_shelxl_version_number           2014/6
_shelx_res_checksum              15144