#------------------------------------------------------------------------------
#$Date: 2016-02-13 13:50:18 +0100 (Sat 13 de Feb de 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/98/1519881.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_1519881
loop_
_publ_author_name
'Taylor, P. G.'
'Callear, Samantha K.'
'Hursthouse, Michael B.'
_publ_section_title
;
 C14H16Cl2N2O2Si
;
_journal_name_full               'Crystal Structure Report Archive'
_journal_page_first              619
_journal_year                    2008
_chemical_formula_sum            'C14 H16 Cl2 N2 O2 Si'
_chemical_formula_weight         343.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                109.321(2)
_cell_angle_beta                 103.396(2)
_cell_angle_gamma                100.002(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1291(3)
_cell_length_b                   10.8097(4)
_cell_length_c                   11.8595(5)
_cell_measurement_reflns_used    13677
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     920.42(7)
_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 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18586
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_correction_T_min  0.9129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.016(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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0880P)²+0.0104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1558
_reflns_number_gt                3002
_reflns_number_total             4196
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            eCrystal-619.cif
_cod_data_source_block           2008src0980
_cod_depositor_comments
;
Citation :
Taylor, P. G. and Callear, Samantha K. and Hursthouse, Michael B. (2008) 
University of Southampton, Crystal Structure Report Archive. 
(doi:10.5258/ecrystals/619)

More at:
http://ecrystals.chem.soton.ac.uk/619/
;
_cod_original_cell_volume        920.42(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1519881
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
C28 C 0.212(2) 0.2696(19) -0.2002(19) 0.024(3) Uani 0.447(6) 1 d PD A 1
H28A H 0.2361 0.2953 -0.2679 0.036 Uiso 0.447(6) 1 calc PR A 1
H28B H 0.1351 0.3205 -0.1649 0.036 Uiso 0.447(6) 1 calc PR A 1
H28C H 0.1550 0.1717 -0.2337 0.036 Uiso 0.447(6) 1 calc PR A 1
Cl26 Cl 0.1790(6) 0.2765(6) -0.2044(5) 0.0529(13) Uani 0.553(6) 1 d PD A 1
C8 C 0.2832(18) 0.4382(15) 0.5604(14) 0.056(6) Uani 0.618(6) 1 d PDU B 2
H8A H 0.2597 0.4802 0.6399 0.084 Uiso 0.618(6) 1 calc PR B 2
H8B H 0.3219 0.5089 0.5302 0.084 Uiso 0.618(6) 1 calc PR B 2
H8C H 0.3756 0.3924 0.5738 0.084 Uiso 0.618(6) 1 calc PR B 2
Cl6 Cl 0.2929(5) 0.4636(6) 0.5839(6) 0.0328(9) Uani 0.382(6) 1 d PD B 2
C2 C 0.0139(3) 0.1685(2) 0.2572(2) 0.0283(5) Uani 1 1 d U A .
C3 C -0.1549(3) 0.1400(3) 0.2689(3) 0.0346(6) Uani 1 1 d U . .
H3 H -0.2499 0.0725 0.2012 0.042 Uiso 1 1 calc R . .
C4 C -0.1801(3) 0.2114(3) 0.3801(3) 0.0381(6) Uani 1 1 d U . .
H4 H -0.2938 0.1926 0.3892 0.046 Uiso 1 1 calc R . .
C5 C -0.0422(4) 0.3108(3) 0.4798(3) 0.0367(6) Uani 1 1 d U B .
H5 H -0.0613 0.3594 0.5563 0.044 Uiso 1 1 calc R . .
C6 C 0.1214(3) 0.3378(2) 0.4662(2) 0.0300(5) Uani 1 1 d DU . .
C7 C 0.3176(3) 0.2860(3) 0.3325(2) 0.0299(5) Uani 1 1 d . . .
H7A H 0.4056 0.2667 0.3929 0.036 Uiso 1 1 calc R B .
H7B H 0.3606 0.3817 0.3427 0.036 Uiso 1 1 calc R . .
C22 C 0.5300(3) 0.2902(2) 0.0916(2) 0.0289(5) Uani 1 1 d . A .
C23 C 0.6904(3) 0.3472(3) 0.0797(3) 0.0343(6) Uani 1 1 d . . .
H23 H 0.7978 0.3637 0.1422 0.041 Uiso 1 1 calc R . .
C24 C 0.6909(4) 0.3787(3) -0.0220(3) 0.0402(7) Uani 1 1 d . . .
H24 H 0.7997 0.4169 -0.0303 0.048 Uiso 1 1 calc R . .
C25 C 0.5343(4) 0.3559(3) -0.1146(3) 0.0468(7) Uani 1 1 d . A .
H25 H 0.5364 0.3778 -0.1856 0.056 Uiso 1 1 calc R . .
C26 C 0.3778(4) 0.3016(3) -0.1017(3) 0.0383(6) Uani 1 1 d D . .
C27 C 0.2159(3) 0.2151(2) 0.0267(2) 0.0282(5) Uani 1 1 d . . .
H27A H 0.1381 0.1342 -0.0476 0.034 Uiso 1 1 calc R A .
H27B H 0.1508 0.2848 0.0456 0.034 Uiso 1 1 calc R . .
C31 C 0.3271(4) -0.0030(3) 0.1350(3) 0.0391(6) Uani 1 1 d . . .
H31A H 0.3995 -0.0040 0.2131 0.059 Uiso 1 1 calc R A .
H31B H 0.3889 -0.0214 0.0720 0.059 Uiso 1 1 calc R . .
H31C H 0.2150 -0.0732 0.1035 0.059 Uiso 1 1 calc R . .
N1 N 0.1482(3) 0.2645(2) 0.35650(18) 0.0269(5) Uani 1 1 d . A .
N21 N 0.3763(3) 0.2697(2) 0.00083(19) 0.0285(5) Uani 1 1 d . A .
O2 O 0.0520(2) 0.10772(17) 0.15633(15) 0.0315(4) Uani 1 1 d . . .
O22 O 0.5127(2) 0.25426(18) 0.18283(16) 0.0314(4) Uani 1 1 d . . .
Si1 Si 0.28511(8) 0.16674(7) 0.16595(6) 0.0274(2) Uani 1 1 d . A .
Cl2 Cl 1.15523(9) 0.51721(7) 0.24367(6) 0.0398(2) Uani 1 1 d . . .
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'
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
C26 C28 H28A 109.5 . .
C26 C28 H28B 109.5 . .
C26 C28 H28C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O2 C2 N1 116.9(2) . .
O2 C2 C3 123.7(2) . .
N1 C2 C3 119.4(2) . .
C4 C3 C2 118.7(2) . .
C4 C3 H3 120.7 . .
C2 C3 H3 120.7 . .
C3 C4 C5 121.2(2) . .
C3 C4 H4 119.4 . .
C5 C4 H4 119.4 . .
C6 C5 C4 119.2(2) . .
C6 C5 H5 120.4 . .
C4 C5 H5 120.4 . .
N1 C6 C5 119.8(2) . .
N1 C6 C8 112.9(7) . .
C5 C6 C8 127.3(7) . .
N1 C6 Cl6 119.4(3) . .
C5 C6 Cl6 120.8(3) . .
C8 C6 Cl6 6.8(9) . .
N1 C7 Si1 108.09(16) . .
N1 C7 H7A 110.1 . .
Si1 C7 H7A 110.1 . .
N1 C7 H7B 110.1 . .
Si1 C7 H7B 110.1 . .
H7A C7 H7B 108.4 . .
O22 C22 N21 115.8(2) . .
O22 C22 C23 125.2(2) . .
N21 C22 C23 119.0(2) . .
C24 C23 C22 119.4(3) . .
C24 C23 H23 120.3 . .
C22 C23 H23 120.3 . .
C23 C24 C25 121.1(3) . .
C23 C24 H24 119.4 . .
C25 C24 H24 119.4 . .
C26 C25 C24 119.2(3) . .
C26 C25 H25 120.4 . .
C24 C25 H25 120.4 . .
C25 C26 N21 120.0(3) . .
C25 C26 C28 120.5(10) . .
N21 C26 C28 119.4(10) . .
C25 C26 Cl26 123.3(3) . .
N21 C26 Cl26 116.6(3) . .
C28 C26 Cl26 6.1(10) . .
N21 C27 Si1 107.86(15) . .
N21 C27 H27A 110.1 . .
Si1 C27 H27A 110.1 . .
N21 C27 H27B 110.1 . .
Si1 C27 H27B 110.1 . .
H27A C27 H27B 108.4 . .
Si1 C31 H31A 109.5 . .
Si1 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
Si1 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C2 N1 C6 121.7(2) . .
C2 N1 C7 114.27(19) . .
C6 N1 C7 124.0(2) . .
C26 N21 C22 121.2(2) . .
C26 N21 C27 124.7(2) . .
C22 N21 C27 114.0(2) . .
C2 O2 Si1 114.76(15) . .
C22 O22 Si1 115.48(15) . .
O2 Si1 C31 94.97(10) . .
O2 Si1 O22 170.57(8) . .
C31 Si1 O22 94.43(10) . .
O2 Si1 C27 90.62(9) . .
C31 Si1 C27 117.38(12) . .
O22 Si1 C27 85.69(9) . .
O2 Si1 C7 86.00(9) . .
C31 Si1 C7 120.22(12) . .
O22 Si1 C7 88.65(9) . .
C27 Si1 C7 122.39(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C28 C26 1.462(15) .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
Cl26 C26 1.699(6) .
C8 C6 1.476(11) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
Cl6 C6 1.710(6) .
C2 O2 1.297(3) .
C2 N1 1.363(3) .
C2 C3 1.402(3) .
C3 C4 1.373(4) .
C3 H3 0.9500 .
C4 C5 1.391(4) .
C4 H4 0.9500 .
C5 C6 1.369(4) .
C5 H5 0.9500 .
C6 N1 1.370(3) .
C7 N1 1.465(3) .
C7 Si1 1.894(2) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C22 O22 1.292(3) .
C22 N21 1.375(3) .
C22 C23 1.401(3) .
C23 C24 1.358(4) .
C23 H23 0.9500 .
C24 C25 1.397(4) .
C24 H24 0.9500 .
C25 C26 1.370(4) .
C25 H25 0.9500 .
C26 N21 1.371(3) .
C27 N21 1.477(3) .
C27 Si1 1.887(3) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C31 Si1 1.857(3) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
O2 Si1 1.8553(17) .
O22 Si1 1.8584(17) .
