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_4089545
_publ_section_title
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 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         'C64 H64 K4 O4 Si2'
_chemical_formula_sum            'C64 H64 K4 O4 Si2'
_chemical_formula_weight         1109.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2012-12-13
_audit_creation_method
;
  Olex2 1.2-dev
  (compiled Dec  4 2012 21:23:29, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.469(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.193(7)
_cell_length_b                   10.599(3)
_cell_length_c                   24.462(8)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.352
_cell_measurement_theta_min      2.554
_cell_volume                     5516(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            143180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.422
_diffrn_reflns_theta_min         1.681
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.8039
_exptl_absorpt_correction_T_min  0.7686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0658 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.9561.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         15236
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+4.7372P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11846
_reflns_number_total             15236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400419a_si_002.cif
_cod_data_source_block           compound_4
_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_database_code               4089545
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H29 of C29, H28 of C28, H27 of C27, H26 of C26, H23 of C23, H22 of C22, H21
  of C21, H20 of C20, 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,
  H32 of C32, H33 of C33, H34 of C34, H35 of C35, H38 of C38, H39 of C39, H40
  of C40, H41 of C41, H44 of C44, H45 of C45, H46 of C46, H47 of C47, {H49A,
  H49B} of C49, {H50A,H50B,H50C,H50D} of C50, {H51A,H51B} of C51, {H1,H52} of
  C52, {H53A,H53B} of C53, {H54A,H54B} of C54, {H55A,H55B} of C55, {H56A,H56B}
  of C56, {H53C,H53D} of C53A, {H54C,H54D} of C54A, {H55C,H55D} of C55A, {H56C,
  H56D} of C56A, {H57A,H57B} of C57, {H58A,H58B} of C58, {H59A,H59B} of C59,
  {H60A,H60B} of C60, {H61A,H61B} of C61, {H62A,H62B} of C62, {H63A,H63B} of
  C63, {H64A,H64B} of C64, {H51C,H51D} of C51A, {H52A,H52B} of C52A
2. Restrained distances
 O1-C49 ~ O1-C52A ~ O1-C52 ~ O2A-C56A ~ O2A-C53A ~ O2-C53 ~ O2-C56
 with sigma of 0.01
 C50-C49 ~ C52-C51 ~ C52A-C51A ~ C54-C53 ~ C56-C55 ~ C54A-C53A ~ C56A-C55A
 with sigma of 0.01
 C55-C54 ~ C55A-C54A ~ C51-C50 ~ C51A-C50
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C52) = Uanis(C52A)
Uanis(C51) = Uanis(C51A)
Uanis(C53A) = Uanis(C53)
Uanis(O2A) = Uanis(O2)
4. Others
 Sof(O2)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=1-Sof(C53)=1-Sof(C53)=1-
 Sof(C53)=1-Sof(C53)=1-Sof(C53)=1-Sof(C53)=1-Sof(C53)=1-Sof(C53)=1-Sof(C53)=1-
 Sof(C53)=1-Sof(C53)=1-Sof(C53)=1-Sof(C53)
 Sof(H50A)=Sof(H50B)=1-Sof(H50B)=1-Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 Sof(C52)=Sof(H1)=Sof(H52)=1-Sof(H50B)=1-Sof(H50B)=1-Sof(H50B)=1-Sof(H50B)=1-
 Sof(H50B)=1-Sof(H50B)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C50(H50C,H50D), C51(H51A,H51B), C52(H1,H52),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C53A(H53C,
 H53D), C54A(H54C,H54D), C55A(H55C,H55D), C56A(H56C,H56D), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B), C51A(H51C,H51D), C52A(H52A,H52B)
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), C26(H26),
  C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35),
 C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47)
;
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.933
_shelx_hkl_checksum              1756
_shelx_res_checksum              82783
_shelxl_version_number           2012-6