Isolable 1,1-disubstituted silole dianion: a homogeneous two-electron-transfer reducing reagent.
Han, Zhengang; Li, Jianfeng; Hu, Hongfan; Zhang, Jianying; Cui, Chunming; Inorganic chemistry 53 (2014) 5890–5892; doi:10.1021/ic500820v

data_4338676
_publ_section_title
;
 Isolable 1,1-disubstituted silole dianion: a homogeneous
 two-electron-transfer reducing reagent.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5890
_journal_page_last               5892
_journal_paper_doi               10.1021/ic500820v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C54 H66 Si3), 3(C7 H8)'
_chemical_formula_sum            'C129 H156 Si6'
_chemical_formula_weight         1875.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                84.56(3)
_cell_angle_beta                 79.12(3)
_cell_angle_gamma                81.76(3)
_cell_formula_units_Z            1
_cell_length_a                   11.813(2)
_cell_length_b                   15.658(3)
_cell_length_c                   16.713(3)
_cell_measurement_reflns_used    4459
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      26.0127
_cell_measurement_theta_min      1.3173
_cell_volume                     2997.2(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0362
_diffrn_orient_matrix_UB_12      -0.0094
_diffrn_orient_matrix_UB_13      0.0785
_diffrn_orient_matrix_UB_21      -0.0618
_diffrn_orient_matrix_UB_22      -0.0039
_diffrn_orient_matrix_UB_23      0.0188
_diffrn_orient_matrix_UB_31      0.0020
_diffrn_orient_matrix_UB_32      -0.0577
_diffrn_orient_matrix_UB_33      -0.0199
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.1201
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25180
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.24
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6091
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10492
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2410
_reflns_number_gt                5470
_reflns_number_total             10492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500820v_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338675--4338676.cif.
;
_cod_original_formula_sum        'C129 H156 Si6 '
_cod_database_code               4338676
_diffrn_number_total             11729
_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
 C80-C63
 1.5 with sigma of 0.02
 C1A-C9
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C81 \\sim C61 \\sim C19 \\sim C9 \\sim C8 \\sim C76 \\sim C1A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C63 \\sim C43 \\sim C73 \\sim C78 \\sim C55 \\sim C72 \\sim C80: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C81) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C80) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C19(0.75) H19(0.75) C61(0.75) H61(0.75) C81(0.75) H81(0.75)
 C76(0.75) H76(0.75) C8(0.75) H8(0.75) C9(0.75) C1A(0.75) H1AA(0.75) H1AB(0.75)
 H1AC(0.75) C78(0.75) H78(0.75) C55(0.75) H55(0.75) C72(0.75) H72(0.75)
 C63(0.75) C43(0.75) H43(0.75) C73(0.75) H73(0.75) C80(0.75) H80A(0.75)
 H80B(0.75) H80C(0.75)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C19(H19), C61(H61), C81(H81), C76(H76), C8(H8), C21(H21),
 C26(H26), C41(H41), C46(H46), C52(H52), C3(H3), C13(H13), C1E(H1E), C35(H35),
 C39(H39), C78(H78), C55(H55), C72(H72), C43(H43), C73(H73)
5.b Fitted hexagon refined as free rotating group:
 C19(C61,C81,C76,C8,C9), C78(C55,C72,C63,C43,C73)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C36(H36A,
 H36B,H36C), C40(H40A,H40B,H40C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C1A(H1AA,
 H1AB,H1AC), C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C1H(H1HA,H1HB,H1HC),
 C60(H60A,H60B,H60C), C66(H66A,H66B,H66C), C69(H69A,H69B,H69C), C80(H80A,H80B,
 H80C), C1B(H1BA,H1BB,H1BC)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'