#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:47:27 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178916 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/45/4114567.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4114567
loop_
_publ_author_name
'Yuxia Liu'
'Thomas C. Stringfellow'
'David Ballweg'
'Ilia A. Guzei'
'Robert West'
_publ_contact_author
; 
   Prof. Robert West 
   Department of Chemistry 
   University of Wisconsin 
   1101 University Ave. 
   Madison, WI  53706-1396  USA 
;
_publ_contact_author_email       west@chem.wisc.edu
_publ_contact_author_fax         1(608)2620381
_publ_contact_author_phone       1(608)2621873
_publ_section_title
;
 Structure and Chemistry of 1-Silafluorenyl Dianion, Its Derivatives, and
 an Organosilicon Diradical Dianion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              49
_journal_page_last               57
_journal_paper_doi               10.1021/ja011821m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C28 H24 Si2'
_chemical_formula_weight         416.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.365(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4399(13)
_cell_length_b                   7.1505(10)
_cell_length_c                   16.647(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1123.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1980
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9350
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0544
_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/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                1304
_reflns_number_total             1980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011821m_6.cif
_cod_data_source_block           west04
_cod_database_code               4114567
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.11583(9) 0.14440(10) 0.55059(4) 0.0591(3) Uani 1 1 d .
C1 C 0.0334(3) 0.2721(4) 0.63497(15) 0.0576(7) Uani 1 1 d .
C2 C -0.1008(4) 0.2659(4) 0.66615(17) 0.0718(9) Uani 1 1 d .
H2 H -0.1708 0.1871 0.6420 0.086 Uiso 1 1 calc R
C3 C -0.1345(4) 0.3740(5) 0.73260(19) 0.0871(10) Uani 1 1 d .
H3 H -0.2269 0.3689 0.7539 0.104 Uiso 1 1 calc R
C4 C -0.0322(5) 0.4892(5) 0.76728(19) 0.0870(11) Uani 1 1 d .
H4 H -0.0551 0.5627 0.8127 0.104 Uiso 1 1 calc R
C5 C 0.1014(4) 0.4990(4) 0.73733(18) 0.0765(9) Uani 1 1 d .
H5 H 0.1699 0.5799 0.7615 0.092 Uiso 1 1 calc R
C6 C 0.1367(3) 0.3907(3) 0.67166(15) 0.0607(8) Uani 1 1 d .
C7 C 0.2788(3) 0.3835(4) 0.63591(16) 0.0634(8) Uani 1 1 d .
C8 C 0.3971(4) 0.4875(4) 0.66293(19) 0.0754(9) Uani 1 1 d .
H8 H 0.3891 0.5724 0.7065 0.090 Uiso 1 1 calc R
C9 C 0.5245(5) 0.4650(5) 0.6257(3) 0.0957(11) Uani 1 1 d .
H9 H 0.6042 0.5362 0.6435 0.115 Uiso 1 1 calc R
C10 C 0.5385(4) 0.3423(6) 0.5634(2) 0.0930(11) Uani 1 1 d .
H10 H 0.6277 0.3271 0.5389 0.112 Uiso 1 1 calc R
C11 C 0.4215(4) 0.2395(4) 0.5360(2) 0.0817(10) Uani 1 1 d .
H11 H 0.4313 0.1554 0.4923 0.098 Uiso 1 1 calc R
C12 C 0.2907(3) 0.2584(4) 0.57177(16) 0.0626(8) Uani 1 1 d .
C13 C 0.1129(3) -0.1156(3) 0.56418(15) 0.0649(8) Uani 1 1 d .
H13A H 0.1788 -0.1734 0.5260 0.078 Uiso 1 1 calc R
H13B H 0.1472 -0.1462 0.6193 0.078 Uiso 1 1 calc R
C14 C 0.0357(3) 0.2004(4) 0.44935(15) 0.0659(8) Uani 1 1 d .
H14A H 0.0294 0.3380 0.4434 0.079 Uiso 1 1 calc R
H14B H 0.0989 0.1530 0.4074 0.079 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
C1 Si1 C12 91.55(13) .
C1 Si1 C13 112.84(13) .
C12 Si1 C13 115.22(13) .
C1 Si1 C14 113.99(12) .
C12 Si1 C14 114.38(13) .
C13 Si1 C14 108.30(12) .
C2 C1 C6 119.0(2) .
C2 C1 Si1 132.2(2) .
C6 C1 Si1 108.8(2) .
C1 C2 C3 120.6(3) .
C4 C3 C2 119.4(4) .
C5 C4 C3 121.2(3) .
C4 C5 C6 120.0(3) .
C5 C6 C1 119.8(3) .
C5 C6 C7 125.0(3) .
C1 C6 C7 115.2(2) .
C12 C7 C8 120.3(3) .
C12 C7 C6 114.7(3) .
C8 C7 C6 124.9(3) .
C9 C8 C7 119.3(3) .
C10 C9 C8 121.2(4) .
C9 C10 C11 119.7(4) .
C12 C11 C10 120.9(3) .
C11 C12 C7 118.5(3) .
C11 C12 Si1 131.8(2) .
C7 C12 Si1 109.7(2) .
C14 C13 Si1 112.91(19) 3_556
C13 C14 Si1 113.22(18) 3_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.861(3) .
Si1 C12 1.867(3) .
Si1 C13 1.873(3) .
Si1 C14 1.874(3) .
C1 C2 1.381(4) .
C1 C6 1.420(4) .
C2 C3 1.393(4) .
C3 C4 1.385(5) .
C4 C5 1.369(5) .
C5 C6 1.387(4) .
C6 C7 1.481(4) .
C7 C12 1.399(4) .
C7 C8 1.406(4) .
C8 C9 1.376(5) .
C9 C10 1.366(5) .
C10 C11 1.395(5) .
C11 C12 1.390(4) .
C13 C14 1.540(4) 3_556
C14 C13 1.540(4) 3_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C12 Si1 C1 C2 -177.0(3) .
C13 Si1 C1 C2 -58.7(3) .
C14 Si1 C1 C2 65.3(3) .
C12 Si1 C1 C6 1.08(18) .
C13 Si1 C1 C6 119.36(18) .
C14 Si1 C1 C6 -116.56(19) .
C6 C1 C2 C3 0.0(4) .
Si1 C1 C2 C3 177.9(2) .
C1 C2 C3 C4 0.2(5) .
C2 C3 C4 C5 0.2(5) .
C3 C4 C5 C6 -0.7(5) .
C4 C5 C6 C1 0.9(4) .
C4 C5 C6 C7 -177.5(3) .
C2 C1 C6 C5 -0.5(4) .
Si1 C1 C6 C5 -178.9(2) .
C2 C1 C6 C7 178.0(2) .
Si1 C1 C6 C7 -0.4(3) .
C5 C6 C7 C12 177.6(2) .
C1 C6 C7 C12 -0.9(3) .
C5 C6 C7 C8 -1.0(4) .
C1 C6 C7 C8 -179.4(2) .
C12 C7 C8 C9 0.0(4) .
C6 C7 C8 C9 178.5(3) .
C7 C8 C9 C10 -0.6(5) .
C8 C9 C10 C11 1.0(5) .
C9 C10 C11 C12 -0.7(5) .
C10 C11 C12 C7 0.1(4) .
C10 C11 C12 Si1 -180.0(2) .
C8 C7 C12 C11 0.2(4) .
C6 C7 C12 C11 -178.4(2) .
C8 C7 C12 Si1 -179.71(19) .
C6 C7 C12 Si1 1.7(3) .
C1 Si1 C12 C11 178.5(3) .
C13 Si1 C12 C11 62.3(3) .
C14 Si1 C12 C11 -64.2(3) .
C1 Si1 C12 C7 -1.57(18) .
C13 Si1 C12 C7 -117.79(19) .
C14 Si1 C12 C7 115.74(19) .
C1 Si1 C13 C14 73.3(2) 3_556
C12 Si1 C13 C14 176.68(17) 3_556
C14 Si1 C13 C14 -53.8(3) 3_556
C1 Si1 C14 C13 -72.5(2) 3_556
C12 Si1 C14 C13 -176.04(19) 3_556
C13 Si1 C14 C13 54.0(3) 3_556
