Addition of Small Electrophiles to N-Heterocyclic-Carbene-Stabilized Disilicon(0): A Revisit of the Isolobal Concept in Low-Valent Silicon Chemistry.
Arz, Marius I.; Straßmann, Martin; Geiß, Daniel; Schnakenburg, Gregor; Filippou, Alexander C.; Journal of the American Chemical Society 138 (2016) 4589–4600; doi:10.1021/jacs.6b01018

data_4124997
_publ_section_title
;
 Addition of Small Electrophiles to N-Heterocyclic-Carbene-Stabilized
 Disilicon(0): A Revisit of the Isolobal Concept in Low-Valent Silicon
 Chemistry.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4589
_journal_page_last               4600
_journal_paper_doi               10.1021/jacs.6b01018
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C32 H12 B F24, C54 H72 N4 Na Si2'
_chemical_formula_sum            'C86 H84 B F24 N4 Na Si2'
_chemical_formula_weight         1719.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.132(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9849(6)
_cell_length_b                   22.4945(10)
_cell_length_c                   21.3530(7)
_cell_measurement_reflns_used    6940
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.55
_cell_volume                     8604.0(6)
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1949
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44493
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.553
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9580
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.698
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         44493
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      0.710
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0515P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16344
_reflns_number_total             44493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01018_si_001.cif
_cod_data_source_block           3622
_cod_depositor_comments
'Adding full bibliography for 4124995--4124999.cif.'
_cod_database_code               4124997
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1S-F2S \\sim F2S-F3S \\sim F3S-F1S
 with sigma of 0.001
 F1-F2 \\sim F2-F3 \\sim F3-F1
 with sigma of 0.001
3. Rigid bond restraints
 C30, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F7) \\sim Ueq, Uanis(F7S) \\sim Ueq, Uanis(F7T) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F8S) \\sim Ueq, Uanis(F8T) \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F9S) \\sim Ueq, Uanis(F9T) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F2S) \\sim Ueq, Uanis(F3S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F4) \\sim Ueq, Uanis(F4S) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5S)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6S) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
5. Others
 1*[Sof(F7)+Sof(F8)+Sof(F9)]+1*[Sof(F7T)+Sof(F8T)+Sof(F9T)]+1*[Sof(F7S)+
 Sof(F8S)+Sof(F9S)]=1 with esd of 0.0001
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F4S)=Sof(F5S)=Sof(F6S)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F1S)=Sof(F2S)=Sof(F3S)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Sof(F7T)=Sof(F8T)=Sof(F9T)=FVAR(4)
 Sof(F7S)=Sof(F8S)=Sof(F9S)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
6.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C31(H31), C33(H33), C37(H37), C39(H39), C41(H41), C2(H2), C3(H3),
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'