#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:46:34 +0100 (vie 25 de mar de 2016) $
#$Revision: 179935 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/30/7023055.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_7023055
loop_
_publ_author_name
'Sohail, M.'
'Panisch, R.'
'Bowden, A.'
'Bassindale, A. R.'
'Taylor, P. G.'
'Korlyukov, A. A.'
'Arkhipov, D. E.'
'Male, L.'
'Callear, S.'
'Coles, S. J.'
'Hursthouse, M. B.'
'Harrington, R. W.'
'Clegg, W.'
_publ_section_title
;
 Pentacoordinate silicon complexes with dynamic motion resembling a
 pendulum on the S(N)2 reaction pathway.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10971
_journal_page_last               10981
_journal_paper_doi               10.1039/c3dt50613d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C8 H14 I N O2 Si'
_chemical_formula_weight         311.19
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.079(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4342(3)
_cell_length_b                   7.2543(2)
_cell_length_c                   9.6610(3)
_cell_measurement_reflns_used    8450
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     575.77(3)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6956
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2582
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.7104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                2426
_reflns_number_total             2582
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt50613d.txt
_cod_data_source_block           2009src0169
_cod_original_cell_volume        575.73(3)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7023055
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
C2 C 1.0658(4) 0.2828(14) 0.3683(3) 0.0157(13) Uani 1 1 d .
C3 C 1.1481(5) 0.2637(6) 0.5196(4) 0.0224(13) Uani 1 1 d .
H3A H 1.1565 0.1315 0.5458 0.027 Uiso 1 1 calc R
H3B H 1.0831 0.3261 0.5791 0.027 Uiso 1 1 calc R
C4 C 1.3174(4) 0.3480(5) 0.5476(4) 0.0224(11) Uani 1 1 d .
H4A H 1.3088 0.4836 0.5372 0.027 Uiso 1 1 calc R
H4B H 1.3767 0.3197 0.6459 0.027 Uiso 1 1 calc R
C5 C 1.4095(4) 0.2709(9) 0.4436(4) 0.0216(15) Uani 1 1 d .
H5A H 1.5162 0.3338 0.4578 0.026 Uiso 1 1 calc R
H5B H 1.4305 0.1382 0.4638 0.026 Uiso 1 1 calc R
C6 C 1.3205(4) 0.2929(18) 0.2912(3) 0.0163(9) Uani 1 1 d .
C7 C 1.0460(3) 0.3053(19) 0.1184(3) 0.0151(6) Uani 1 1 d .
H7A H 1.0686 0.2002 0.0603 0.018 Uiso 1 1 calc R
H7B H 1.0668 0.4220 0.0723 0.018 Uiso 1 1 calc R
C8 C 0.7130(13) 0.0831(11) 0.1018(10) 0.0172(16) Uani 1 1 d .
H8A H 0.7839 -0.0234 0.1323 0.026 Uiso 1 1 calc R
H8B H 0.6679 0.0759 -0.0009 0.026 Uiso 1 1 calc R
H8C H 0.6239 0.0827 0.1517 0.026 Uiso 1 1 calc R
C9 C 0.7221(13) 0.5153(11) 0.1195(11) 0.023(2) Uani 1 1 d .
H9A H 0.6308 0.5098 0.1666 0.035 Uiso 1 1 calc R
H9B H 0.6806 0.5387 0.0178 0.035 Uiso 1 1 calc R
H9C H 0.7961 0.6149 0.1612 0.035 Uiso 1 1 calc R
N1 N 1.1457(3) 0.2937(14) 0.2658(2) 0.0139(7) Uani 1 1 d .
O2 O 0.9084(3) 0.2834(12) 0.3305(2) 0.0214(11) Uani 1 1 d .
O6 O 1.3820(2) 0.3013(11) 0.1909(2) 0.0211(5) Uani 1 1 d .
Si1 Si 0.83140(10) 0.2964(5) 0.14348(8) 0.0152(2) Uani 1 1 d .
I1 I 1.18985(2) -0.19733(3) 0.248333(18) 0.01931(7) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C2 0.0154(14) 0.015(4) 0.0169(14) -0.002(2) 0.0038(11) -0.003(2)
C3 0.0243(19) 0.028(4) 0.0129(15) 0.0029(15) 0.0010(13) -0.0001(16)
C4 0.0176(18) 0.028(3) 0.0175(17) -0.0053(14) -0.0045(14) -0.0010(14)
C5 0.0132(16) 0.028(5) 0.0194(15) -0.0016(17) -0.0048(12) 0.0030(16)
C6 0.0120(14) 0.013(3) 0.0241(14) 0.000(4) 0.0038(11) -0.006(3)
C7 0.0170(14) 0.0162(14) 0.0109(12) 0.000(5) 0.0006(10) -0.005(5)
C8 0.013(3) 0.021(3) 0.019(3) -0.002(2) 0.007(2) -0.004(3)
C9 0.021(4) 0.020(3) 0.025(4) 0.002(3) -0.001(3) -0.002(3)
N1 0.0123(11) 0.0138(18) 0.0148(11) -0.004(3) 0.0013(9) 0.002(3)
O2 0.0121(10) 0.036(3) 0.0161(10) 0.0050(19) 0.0039(8) 0.0007(19)
O6 0.0142(10) 0.0247(12) 0.0253(11) -0.002(4) 0.0062(9) 0.006(4)
Si1 0.0119(4) 0.0170(5) 0.0162(4) 0.0032(11) 0.0020(3) 0.0024(11)
I1 0.02050(11) 0.01563(10) 0.02004(10) -0.0010(2) 0.00093(7) -0.0005(3)
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 '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
O2 C2 N1 117.0(3)
O2 C2 C3 120.1(3)
N1 C2 C3 122.9(3)
C2 C3 C4 110.5(4)
C5 C4 C3 109.7(3)
C6 C5 C4 113.2(4)
O6 C6 N1 118.4(3)
O6 C6 C5 125.8(3)
N1 C6 C5 115.7(3)
N1 C7 Si1 103.13(18)
C2 N1 C6 123.3(3)
C2 N1 C7 116.7(2)
C6 N1 C7 120.0(2)
C2 O2 Si1 113.7(2)
O2 Si1 C9 103.5(4)
O2 Si1 C8 103.5(4)
C9 Si1 C8 118.13(16)
O2 Si1 C7 89.55(11)
C9 Si1 C7 115.3(6)
C8 Si1 C7 119.5(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C2 O2 1.295(4)
C2 N1 1.320(4)
C2 C3 1.476(4)
C3 C4 1.520(5)
C4 C5 1.510(5)
C5 C6 1.502(5)
C6 O6 1.200(4)
C6 N1 1.438(4)
C7 N1 1.484(3)
C7 Si1 1.881(3)
C8 Si1 1.837(9)
C9 Si1 1.824(9)
O2 Si1 1.779(2)
