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_4089544
_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         'C40 H48 Na2 O4 Si'
_chemical_formula_sum            'C40 H48 Na2 O4 Si'
_chemical_formula_weight         666.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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             2013-03-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                67.78(2)
_cell_angle_beta                 77.033(11)
_cell_angle_gamma                68.282(9)
_cell_formula_units_Z            2
_cell_length_a                   10.553(5)
_cell_length_b                   13.798(5)
_cell_length_c                   13.945(5)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.23
_cell_volume                     1737.9(12)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29018
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.303
_diffrn_reflns_theta_min         1.585
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.807354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.1260 before and 0.0416 after correction.
The Ratio of minimum to maximum transmission is 0.8074.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0437P)^2^+1.0552P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5950
_reflns_number_total             6987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400419a_si_002.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        1737.9(13)
_cod_database_code               4089544
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H27A,H27B,H27C,H27D} of C27, {H28A,H28B} of C28, {H29A,H29B} of C29, {H30A,
  H30B} of C30, {H31A,H31B} of C31, {H32A,H32B} of C32, {H33A,H33B} of C33,
  {H34A,H34B,H34C,H34D} of C34, {H35A,H35B} of C35, H17 of C17, H16 of C16, H15
  of C15, H14 of C14, H11 of C11, H10 of C10, H9 of C9, H8 of C8, H5 of C5, H4
  of C4, H3 of C3, H2 of C2, {H39A,H39B} of C39, {H39C,H39D} of C39A, {H40A,
  H40B} of C40, {H40C,H40D} of C40A, {H38C,H38D} of C38A, {H38A,H38B} of C38,
  {H37C,H37D} of C37A, {H37A,H37B} of C37, {H36C,H36D} of C36A, {H36A,H36B} of
  C36, {H35C,H35D} of C35A, H20 of C20, H21 of C21, H22 of C22, H23 of C23,
  {H25A,H25B,H25C,H25D} of C25, {H26A,H26B} of C26, {H26C,H26D} of C26A
2. Restrained distances
 C40A-C39A
 1.52 with sigma of 0.01
 C27-C26 ~ C26A-C25 ~ C26-C25
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C36) = Uanis(C36A)
Uanis(C35) = Uanis(C35A)
Uanis(C26) = Uanis(C26A)
Uanis(C39) = Uanis(C39A)
Uanis(C37) = Uanis(C37A)
Uanis(C38) = Uanis(C38A)
Uanis(C40) = Uanis(C40A)
4. Others
 Sof(H25A)=Sof(H25B)=1-Sof(H25B)=1-Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=1-
 Sof(H25B)=1-Sof(H25B)=1-Sof(H25B)=Sof(H27A)=Sof(H27B)=1-Sof(H25B)=1-Sof(H25B)
 Sof(H34A)=Sof(H34B)=1-Sof(H34B)=1-Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=1-
 Sof(H34B)=1-Sof(H34B)=1-Sof(H34B)=Sof(C36)=Sof(H36A)=Sof(H36B)=1-Sof(H34B)=1-
 Sof(H34B)=1-Sof(H34B)
 Sof(C37)=Sof(H37A)=Sof(H37B)=1-Sof(H37A)=1-Sof(H37A)=1-Sof(H37A)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=1-Sof(H37A)=1-Sof(H37A)=1-Sof(H37A)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=1-Sof(H37A)=1-Sof(H37A)=1-Sof(H37A)=Sof(C40)=Sof(H40A)=Sof(H40B)=1-
 Sof(H37A)=1-Sof(H37A)=1-Sof(H37A)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25(H25C,H25D), C26(H26A,H26B), C26A(H26C,H26D), C27(H27A,
 H27B), C27(H27C,H27D), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C34(H34C,H34D),
  C35(H35A,H35B), C35A(H35C,H35D), C36(H36A,H36B), C36A(H36C,H36D), C37(H37A,
 H37B), C37A(H37C,H37D), C38(H38A,H38B), C38A(H38C,H38D), C39(H39A,H39B),
 C39A(H39C,H39D), C40(H40A,H40B), C40A(H40C,H40D)
5.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   0.989
_shelx_estimated_absorpt_t_min   0.942
_shelx_hkl_checksum              98577
_shelx_res_checksum              80251
_shelxl_version_number           2012-9