Silicon in a Negatively Charged Shell: Anions of Spirosilabifluorene
Zabula, Alexander V.; Rogachev, Andrey Yu.; Guzei, Ilia A.; West, Robert; Organometallics 32 (2013) 3760–; doi:10.1021/om400419a

data_4089543
_publ_section_title
;
 Silicon in a Negatively Charged Shell: Anions of Spirosilabifluorene
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3760
_journal_paper_doi               10.1021/om400419a
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C24 H16 Si, C16 H32 Li O4'
_chemical_formula_sum            'C40 H48 Li O4 Si'
_chemical_formula_weight         627.81
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2012-12-03
_audit_creation_method
;
  Olex2 1.2-dev
  (compiled Nov 28 2012 18:15:36, GUI svn.r4378)
;
_cell_angle_alpha                114.311(15)
_cell_angle_beta                 97.232(15)
_cell_angle_gamma                106.991(16)
_cell_formula_units_Z            1
_cell_length_a                   9.002(4)
_cell_length_b                   10.248(4)
_cell_length_c                   10.991(4)
_cell_measurement_reflns_used    7636
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.424
_cell_measurement_theta_min      2.308
_cell_volume                     847.7(6)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21722
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.737
_diffrn_reflns_theta_min         2.120
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1179 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.8374.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             337
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.05(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9056
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.2429P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                8048
_reflns_number_total             9056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400419a_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        847.8(6)
_cod_database_code               4089543
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H31A,H31B} of C31, {H32A,H32B} of C32, {H33A,H33B} of C33, {H34A,H34B} of
  C34, {H35A,H35B} of C35, {H36A,H36B} of C36, {H37A,H37B} of C37, H3 of C3, H2
  of C2, {H38A,H38B,H38C,H38D} of C38, {H39A,H39B} of C39, {H40A,H40B} of C40,
  {H39C,H39D} of C39A, {H40C,H40D} of C40A, {H30A,H30B} of C30, {H29A,H29B} of
  C29, {H28A,H28B} of C28, {H27A,H27B} of C27, {H26A,H26B} of C26, {H25A,H25B}
  of C25, H23 of C23, H4 of C4, H5 of C5, H8 of C8, H9 of C9, H10 of C10, H11
  of C11, H14 of C14, H15 of C15, H16 of C16, H17 of C17, H20 of C20, H21 of
  C21, H22 of C22
2. Restrained distances
 O4-C40A ~ O4-C40 ~ O4-C37
 with sigma of 0.01
 C39-C38 ~ C39A-C38
 with sigma of 0.01
 C40A-C39A ~ C40-C39 ~ C38-C37
 with sigma of 0.01
3. Others
 Sof(H38A)=Sof(H38B)=1-Sof(H38B)=1-Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=1-Sof(H38B)=1-Sof(H38B)=1-Sof(H38B)=1-Sof(H38B)=1-
 Sof(H38B)=1-Sof(H38B)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C38(H38C,H38D), C39(H39A,H39B), C40(H40A,H40B), C39A(H39C,H39D), C40A(H40C,
 H40D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.957
_shelx_hkl_checksum              20024
_shelx_res_checksum              12259
_shelxl_version_number           2012-6