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#$Date: 2016-03-25 11:30:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179793 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008913.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_7008913
loop_
_publ_author_name
'Choi, Seok-Bong'
'Boudjouk, Philip'
_publ_section_title
;
 A novel α,ω silyl dianionic salt. The synthesis and characterization
 of remotely connected benzannulated silole monoanions
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              841
_journal_paper_doi               10.1039/a906915a
_journal_year                    2000
_chemical_formula_sum            'C19 H20 Cl Si'
_chemical_formula_weight         311.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.377(2)
_cell_angle_beta                 112.958(2)
_cell_angle_gamma                96.817(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9575(10)
_cell_length_b                   9.4809(11)
_cell_length_c                   11.2364(13)
_cell_measurement_temperature    298(2)
_cell_volume                     853.00(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_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  0.1995
_diffrn_reflns_av_sigmaI/netI    0.1164
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3754
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.286
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             330
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0696
_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)+(0.0462P)²+2.3558P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                1988
_reflns_number_total             2724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a906915a.txt
_cod_data_source_block           j
_cod_database_code               7008913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.12407(16) 0.04702(13) 0.72375(12) 0.0368(4) Uani 1 1 d . . .
Cl1 Cl 0.36751(16) 0.04016(15) 0.83768(14) 0.0561(4) Uani 1 1 d . . .
C1 C 0.0729(6) 0.2224(5) 0.7756(4) 0.0384(11) Uani 1 1 d . . .
C2 C -0.0484(6) 0.1959(5) 0.8177(4) 0.0346(10) Uani 1 1 d . . .
C3 C -0.0990(6) 0.0396(5) 0.8216(4) 0.0373(11) Uani 1 1 d . . .
C4 C -0.0224(5) -0.0596(5) 0.7719(4) 0.0334(10) Uani 1 1 d . . .
C5 C 0.1511(6) 0.3672(5) 0.7699(5) 0.0430(12) Uani 1 1 d . . .
C6 C 0.1401(8) 0.3991(6) 0.6505(6) 0.0627(17) Uani 1 1 d . . .
H6A H 0.0781 0.3308 0.5725 0.075 Uiso 1 1 calc R . .
C7 C 0.2200(9) 0.5312(7) 0.6456(7) 0.080(2) Uani 1 1 d . . .
H7A H 0.2080 0.5525 0.5645 0.096 Uiso 1 1 calc R . .
C8 C 0.3165(8) 0.6304(6) 0.7601(8) 0.0701(19) Uani 1 1 d . . .
H8A H 0.3738 0.7175 0.7574 0.084 Uiso 1 1 calc R . .
C9 C 0.3281(8) 0.6008(6) 0.8777(8) 0.076(2) Uani 1 1 d . . .
H9A H 0.3908 0.6693 0.9554 0.091 Uiso 1 1 calc R . .
C10 C 0.2471(7) 0.4690(6) 0.8828(6) 0.0563(14) Uani 1 1 d . . .
H10A H 0.2583 0.4495 0.9644 0.068 Uiso 1 1 calc R . .
C11 C -0.1379(6) 0.3080(5) 0.8550(5) 0.0459(12) Uani 1 1 d . . .
H11A H -0.0777 0.4042 0.8649 0.055 Uiso 1 1 calc R . .
H11B H -0.1388 0.3001 0.9399 0.055 Uiso 1 1 calc R . .
C12 C -0.3152(7) 0.2915(7) 0.7535(6) 0.0585(15) Uani 1 1 d . . .
H12A H -0.3754 0.1961 0.7456 0.070 Uiso 1 1 calc R . .
H12B H -0.3669 0.3629 0.7861 0.070 Uiso 1 1 calc R . .
C13 C -0.3316(8) 0.3091(8) 0.6193(6) 0.080(2) Uani 1 1 d . . .
H13A H -0.2721 0.2433 0.5895 0.096 Uiso 1 1 calc R . .
H13B H -0.2798 0.4074 0.6257 0.096 Uiso 1 1 calc R . .
C14 C -0.5101(10) 0.2797(12) 0.5160(8) 0.127(4) Uani 1 1 d . . .
H14A H -0.5114 0.2918 0.4323 0.190 Uiso 1 1 calc R . .
H14B H -0.5690 0.3468 0.5429 0.190 Uiso 1 1 calc R . .
H14C H -0.5621 0.1821 0.5080 0.190 Uiso 1 1 calc R . .
C15 C -0.2091(6) -0.0075(6) 0.8727(5) 0.0466(13) Uani 1 1 d . . .
H15A H -0.2602 0.0579 0.9059 0.056 Uiso 1 1 calc R . .
C16 C -0.2422(6) -0.1553(6) 0.8736(5) 0.0519(14) Uani 1 1 d . . .
H16A H -0.3149 -0.1876 0.9090 0.062 Uiso 1 1 calc R . .
C17 C -0.1701(7) -0.2531(6) 0.8238(5) 0.0549(15) Uani 1 1 d . . .
H17A H -0.1959 -0.3511 0.8234 0.066 Uiso 1 1 calc R . .
C18 C -0.0584(7) -0.2057(5) 0.7739(5) 0.0486(13) Uani 1 1 d . . .
H18A H -0.0073 -0.2719 0.7417 0.058 Uiso 1 1 calc R . .
C19 C 0.0899(6) -0.0001(5) 0.5468(4) 0.0431(12) Uani 1 1 d . . .
H19A H 0.1644 0.0695 0.5305 0.052 Uiso 1 1 calc R . .
H19C H 0.1148 -0.0956 0.5284 0.052 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1 C4 93.5(2) . . ?
C1 Si1 C19 115.6(2) . . ?
C4 Si1 C19 116.4(2) . . ?
C1 Si1 Cl1 110.94(15) . . ?
C4 Si1 Cl1 112.43(15) . . ?
C19 Si1 Cl1 107.53(17) . . ?
C2 C1 C5 126.2(5) . . ?
C2 C1 Si1 108.5(3) . . ?
C5 C1 Si1 125.3(4) . . ?
C1 C2 C3 115.7(4) . . ?
C1 C2 C11 125.3(4) . . ?
C3 C2 C11 119.0(4) . . ?
C4 C3 C15 120.3(4) . . ?
C4 C3 C2 115.3(4) . . ?
C15 C3 C2 124.4(5) . . ?
C3 C4 C18 119.5(4) . . ?
C3 C4 Si1 106.9(3) . . ?
C18 C4 Si1 133.5(4) . . ?
C10 C5 C6 117.7(5) . . ?
C10 C5 C1 121.2(4) . . ?
C6 C5 C1 120.9(4) . . ?
C5 C6 C7 121.0(6) . . ?
C8 C7 C6 120.0(6) . . ?
C9 C8 C7 119.6(5) . . ?
C8 C9 C10 120.5(6) . . ?
C5 C10 C9 121.1(6) . . ?
C2 C11 C12 113.1(4) . . ?
C13 C12 C11 114.6(5) . . ?
C12 C13 C14 113.9(6) . . ?
C3 C15 C16 118.7(5) . . ?
C17 C16 C15 121.5(5) . . ?
C16 C17 C18 119.8(5) . . ?
C17 C18 C4 120.2(5) . . ?
C19 C19 Si1 111.5(4) 2_556 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.850(5) . ?
Si1 C4 1.853(4) . ?
Si1 C19 1.865(5) . ?
Si1 Cl1 2.0684(19) . ?
C1 C2 1.355(6) . ?
C1 C5 1.487(6) . ?
C2 C3 1.510(6) . ?
C2 C11 1.511(7) . ?
C3 C4 1.402(7) . ?
C3 C15 1.384(7) . ?
C4 C18 1.391(6) . ?
C5 C10 1.370(7) . ?
C5 C6 1.387(7) . ?
C6 C7 1.387(7) . ?
C7 C8 1.369(9) . ?
C8 C9 1.357(10) . ?
C9 C10 1.390(8) . ?
C11 C12 1.525(7) . ?
C12 C13 1.493(8) . ?
C13 C14 1.528(9) . ?
C15 C16 1.400(7) . ?
C16 C17 1.365(8) . ?
C17 C18 1.386(7) . ?
C19 C19 1.542(9) 2_556 ?
