Iodine-doped sumanene and its application for the synthesis of chalcogenasumanenes and silasumanenes
Tan, Qitao; Zhou, Dandan; Zhang, Tao; Liu, Bingxin; Xu, Bin; Chemical Communications 53 (2017) 10279–10282; doi:10.1039/C7CC05885C

data_1546838
_publ_section_title
;
 Iodine-doped sumanene and its application for the synthesis of
 chalcogenasumanenes and silasumanenes
;
_journal_issue                   74
_journal_name_full               'Chemical Communications'
_journal_page_first              10279
_journal_page_last               10282
_journal_paper_doi               10.1039/C7CC05885C
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         C24H24Si3
_chemical_formula_sum            'C24 H24 Si3'
_chemical_formula_weight         396.70
_chemical_name_common            Si-Sum
_chemical_name_systematic        Si-Sumanene
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-08-21 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.345(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.0400(14)
_cell_length_b                   20.685(2)
_cell_length_c                   18.893(2)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.19
_cell_volume                     4697.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens SMART CCD'
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29232
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_preparation       ', Luminescent,Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1675P)^2^+0.4879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.2445
_reflns_number_gt                5090
_reflns_number_total             10867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc05885c2.cif
_cod_data_source_block           ZDD-Si-Sum
_cod_original_cell_volume        4697.4(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1546838