Donor-Acceptor-Stabilized Silicon Analogue of an Acid Anhydride
Rajendra S. Ghadwal; Ramachandran Azhakar; Herbert W. Roesky; Kevin Pröpper; Birger Dittrich; Susanne Klein; Gernot Frenking; Journal of the American Chemical Society 133 (2011) 17552–17555; doi:10.1021/ja206702e

data_4107048
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie                            
Georg-August-Universit\"at G\"ottingen
Tammannstrasse 4, 37077 G\"ottingen (Germany)
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_name        'Herbert W. Roesky'
_publ_section_title
;
 Donor-Acceptor-Stabilized Silicon Analogue of an Acid Anhydride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17552
_journal_page_last               17555
_journal_paper_doi               10.1021/ja206702e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'2(C60.90 H43.90 B2 F30 N4 O3 Si2),3(C7 H8), 2(C6 H5)'
_chemical_formula_sum            'C154.8 H121.8 B4 F60 N8 O6 Si4'
_chemical_formula_weight         3485.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.8520(10)
_cell_angle_beta                 74.8960(10)
_cell_angle_gamma                77.0250(10)
_cell_formula_units_Z            1
_cell_length_a                   13.3606(2)
_cell_length_b                   13.8311(2)
_cell_length_c                   21.8530(4)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      143.705
_cell_measurement_theta_min      6.644
_cell_volume                     3749.34(11)
_computing_cell_refinement       'SAINT (Bruker 2009)'
_computing_data_collection       'APEX2 (Bruker 2009)'
_computing_data_reduction        'SAINT (Bruker 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            169031
_diffrn_reflns_theta_full        72.62
_diffrn_reflns_theta_max         72.62
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  0.4697
_exptl_absorpt_correction_T_min  0.3814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       bar
_exptl_crystal_F_000             1771
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         14362
_refine_ls_number_restraints     2911
_refine_ls_restrained_S_all      2.027
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0760P)^2^+3.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                12096
_reflns_number_total             14362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja206702e_si_002.cif
_cod_data_source_block           final7
_cod_original_cell_volume        3749.34(10)
_cod_original_formula_sum        'C154.80 H121.80 B4 F60 N8 O6 Si4'
_cod_database_code               4107048