Highly Selective Addition of Cyclosilanes to Alkynes Enabling New Conjugated Materials
Jiang, Qifeng; Gittens, Alexandra; Wong, Sydnee; Siegler, Maxime A.; Klausen, Rebekka S.; Chemical Science  (2022) –; doi:10.1039/D2SC01690G

data_1567070
_publ_section_title
;
 Highly Selective Addition of Cyclosilanes to Alkynes Enabling New
 Conjugated Materials
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01690G
_journal_year                    2022
_chemical_formula_moiety         'C30 H58 Si10'
_chemical_formula_sum            'C30 H58 Si10'
_chemical_formula_weight         699.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-15 deposited with the CCDC.	2022-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                86.116(2)
_cell_angle_beta                 83.625(2)
_cell_angle_gamma                81.600(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8909(3)
_cell_length_b                   13.8639(4)
_cell_length_c                   37.0010(12)
_cell_measurement_reflns_used    7055
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.8340
_cell_measurement_theta_min      3.3460
_cell_volume                     4477.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            55290
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.248
_diffrn_reflns_theta_max         67.248
_diffrn_reflns_theta_min         2.406
_exptl_absorpt_coefficient_mu    2.897
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         16062
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+4.5564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13297
_reflns_number_total             16062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01690g2.cif
_cod_data_source_block           3a
_cod_database_code               1567070
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.694
_oxdiff_exptl_absorpt_empirical_full_max 1.503
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_shelx_res_checksum              5171
_shelx_hkl_checksum              59200