Heterocyclopentanediyls vs Heterocyclopentadienes: A Question of Silyl Group Migration.
Beer, Henrik; Bresien, Jonas; Michalik, Dirk; Rölke, Anne-Kristin; Schulz, Axel; Villinger, Alexander; Wustrack, Ronald; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c00460

data_4038438
_publ_section_title
;
 Heterocyclopentanediyls vs Heterocyclopentadienes: A Question of Silyl
 Group Migration.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00460
_journal_year                    2020
_chemical_formula_moiety         'C28 H65 N3 P2 Si8'
_chemical_formula_sum            'C28 H65 N3 P2 Si8'
_chemical_formula_weight         730.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.309(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.0404(12)
_cell_length_b                   9.6147(4)
_cell_length_c                   32.3626(14)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.61
_cell_volume                     8715.5(6)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            73168
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.494
_diffrn_reflns_theta_min         2.195
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       needle
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         15706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0389P)^2^+2.8291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9727
_reflns_number_total             15706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c00460_si_002.cif
_cod_data_source_block           is_ar7_33a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4038438
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2013-4
_shelx_res_checksum              81697
_shelx_hkl_checksum              50589