#------------------------------------------------------------------------------
#$Date: 2016-03-21 12:10:46 +0100 (lun 21 de mar de 2016) $
#$Revision: 178692 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/03/4080367.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_4080367
loop_
_publ_author_name
'Sohail, Muhammad'
'Bassindale, Alan R.'
'Taylor, Peter G.'
'Korlyukov, Alexander A.'
'Arkhipov, Dmitry E.'
'Male, Louise'
'Coles, Simon J.'
'Hursthouse, Michael B.'
_publ_section_title
;
 Synthesis and Hydrolysis--Condensation Study of Water-Soluble
 Self-Assembled Pentacoordinate Polysilylamides
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1721
_journal_paper_doi               10.1021/om301137b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C8 H10 Cl3 N O Si'
_chemical_formula_sum            'C8 H10 Cl3 N O Si'
_chemical_formula_weight         270.61
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.293(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6868(7)
_cell_length_b                   14.4742(12)
_cell_length_c                   9.3571(8)
_cell_measurement_reflns_used    4358
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      2.66
_cell_volume                     1134.85(16)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Smart 1000 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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12701
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0423
_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)+(0.0200P)²+2.23P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                2383
_reflns_number_total             3251
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            om301137b_si_002.cif
_cod_data_source_block           109cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4080367
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 0.20398(8) 0.47059(5) 0.29263(7) 0.02121(14) Uani 1 1 d .
Cl1 Cl 0.22432(8) 0.44310(5) 0.53805(6) 0.03158(15) Uani 1 1 d .
Cl2 Cl 0.03926(8) 0.29977(4) 0.13924(8) 0.03434(15) Uani 1 1 d .
Cl3 Cl 0.66667(7) 0.27860(5) 0.30389(7) 0.03230(15) Uani 1 1 d .
O1 O 0.21990(19) 0.48292(12) 0.09350(16) 0.0229(3) Uani 1 1 d .
N1 N 0.4300(2) 0.38795(13) 0.1760(2) 0.0201(4) Uani 1 1 d .
C1 C 0.3957(3) 0.40160(17) 0.3206(2) 0.0233(5) Uani 1 1 d .
H1A H 0.4849 0.4352 0.3884 0.028 Uiso 1 1 calc R
H1B H 0.3839 0.3410 0.3656 0.028 Uiso 1 1 calc R
C2 C 0.3283(3) 0.43370(15) 0.0611(2) 0.0188(4) Uani 1 1 d .
C3 C 0.3500(3) 0.42448(17) -0.0826(2) 0.0232(5) Uani 1 1 d .
H3A H 0.2813 0.4558 -0.1641 0.028 Uiso 1 1 calc R
C4 C 0.4706(3) 0.37010(17) -0.1032(3) 0.0255(5) Uani 1 1 d .
H4A H 0.4852 0.3638 -0.1999 0.031 Uiso 1 1 calc R
C5 C 0.5733(3) 0.32348(17) 0.0150(3) 0.0273(5) Uani 1 1 d .
H5A H 0.6571 0.2858 -0.0001 0.033 Uiso 1 1 calc R
C6 C 0.5498(3) 0.33365(16) 0.1528(3) 0.0230(4) Uani 1 1 d .
C7 C 0.0087(3) 0.40785(17) 0.2232(3) 0.0253(5) Uani 1 1 d .
H7A H -0.0387 0.3961 0.3067 0.030 Uiso 1 1 calc R
H7B H -0.0664 0.4467 0.1495 0.030 Uiso 1 1 calc R
C8 C 0.1875(3) 0.59775(18) 0.3119(3) 0.0320(6) Uani 1 1 d .
H8A H 0.1492 0.6257 0.2135 0.048 Uiso 1 1 calc R
H8B H 0.2924 0.6233 0.3616 0.048 Uiso 1 1 calc R
H8C H 0.1121 0.6114 0.3707 0.048 Uiso 1 1 calc R
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
Si1 0.0226(3) 0.0255(3) 0.0147(3) 0.0008(2) 0.0034(2) 0.0024(2)
Cl1 0.0339(3) 0.0466(4) 0.0143(2) 0.0024(2) 0.0064(2) 0.0042(3)
Cl2 0.0376(3) 0.0285(3) 0.0380(3) -0.0043(3) 0.0119(3) -0.0033(3)
Cl3 0.0266(3) 0.0384(3) 0.0304(3) 0.0095(3) 0.0047(2) 0.0094(2)
O1 0.0239(8) 0.0292(9) 0.0152(7) 0.0034(6) 0.0047(6) 0.0053(7)
N1 0.0215(9) 0.0227(9) 0.0158(8) 0.0014(7) 0.0042(7) -0.0001(7)
C1 0.0238(11) 0.0317(12) 0.0135(9) 0.0035(9) 0.0035(8) 0.0021(9)
C2 0.0199(10) 0.0202(10) 0.0153(9) 0.0005(8) 0.0029(8) -0.0020(8)
C3 0.0266(11) 0.0266(12) 0.0147(9) -0.0016(8) 0.0023(8) -0.0013(9)
C4 0.0288(12) 0.0288(12) 0.0213(11) -0.0047(9) 0.0107(9) -0.0050(10)
C5 0.0272(12) 0.0274(12) 0.0301(12) -0.0061(10) 0.0123(10) -0.0010(10)
C6 0.0200(10) 0.0223(11) 0.0246(11) 0.0014(9) 0.0025(9) -0.0015(9)
C7 0.0235(11) 0.0310(12) 0.0210(10) -0.0017(9) 0.0053(9) 0.0013(9)
C8 0.0427(15) 0.0285(13) 0.0259(12) -0.0019(10) 0.0109(11) 0.0042(11)
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
C8 Si1 C7 115.20(12)
C8 Si1 C1 126.47(12)
C7 Si1 C1 118.12(11)
C8 Si1 O1 91.67(10)
C7 Si1 O1 89.94(9)
C1 Si1 O1 84.12(8)
C8 Si1 Cl1 93.58(8)
C7 Si1 Cl1 94.96(8)
C1 Si1 Cl1 86.41(7)
O1 Si1 Cl1 170.51(6)
C2 O1 Si1 115.21(14)
C6 N1 C2 120.95(19)
C6 N1 C1 124.75(19)
C2 N1 C1 114.29(18)
N1 C1 Si1 109.04(14)
N1 C1 H1A 109.9
Si1 C1 H1A 109.9
N1 C1 H1B 109.9
Si1 C1 H1B 109.9
H1A C1 H1B 108.3
O1 C2 N1 116.47(18)
O1 C2 C3 124.7(2)
N1 C2 C3 118.8(2)
C4 C3 C2 119.3(2)
C4 C3 H3A 120.4
C2 C3 H3A 120.4
C3 C4 C5 121.3(2)
C3 C4 H4A 119.3
C5 C4 H4A 119.3
C6 C5 C4 118.2(2)
C6 C5 H5A 120.9
C4 C5 H5A 120.9
N1 C6 C5 121.4(2)
N1 C6 Cl3 116.69(17)
C5 C6 Cl3 121.86(19)
Cl2 C7 Si1 110.29(12)
Cl2 C7 H7A 109.6
Si1 C7 H7A 109.6
Cl2 C7 H7B 109.6
Si1 C7 H7B 109.6
H7A C7 H7B 108.1
Si1 C8 H8A 109.5
Si1 C8 H8B 109.5
H8A C8 H8B 109.5
Si1 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si1 C8 1.859(3)
Si1 C7 1.882(2)
Si1 C1 1.899(2)
Si1 O1 1.9128(16)
Si1 Cl1 2.2911(8)
Cl2 C7 1.801(3)
Cl3 C6 1.705(2)
O1 C2 1.280(3)
N1 C6 1.366(3)
N1 C2 1.369(3)
N1 C1 1.474(3)
C1 H1A 0.9900
C1 H1B 0.9900
C2 C3 1.412(3)
C3 C4 1.365(3)
C3 H3A 0.9500
C4 C5 1.398(3)
C4 H4A 0.9500
C5 C6 1.366(3)
C5 H5A 0.9500
C7 H7A 0.9900
C7 H7B 0.9900
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
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
C8 Si1 O1 C2 135.25(17)
C7 Si1 O1 C2 -109.54(17)
C1 Si1 O1 C2 8.75(17)
C6 N1 C1 Si1 -173.18(18)
C2 N1 C1 Si1 5.7(2)
C8 Si1 C1 N1 -95.07(19)
C7 Si1 C1 N1 79.42(18)
O1 Si1 C1 N1 -7.35(15)
Cl1 Si1 C1 N1 173.13(16)
Si1 O1 C2 N1 -7.6(2)
Si1 O1 C2 C3 172.95(18)
C6 N1 C2 O1 -180.0(2)
C1 N1 C2 O1 1.1(3)
C6 N1 C2 C3 -0.5(3)
C1 N1 C2 C3 -179.4(2)
O1 C2 C3 C4 179.7(2)
N1 C2 C3 C4 0.3(3)
C2 C3 C4 C5 -0.1(4)
C3 C4 C5 C6 0.0(4)
C2 N1 C6 C5 0.5(3)
C1 N1 C6 C5 179.2(2)
C2 N1 C6 Cl3 -178.92(16)
C1 N1 C6 Cl3 -0.2(3)
C4 C5 C6 N1 -0.2(4)
C4 C5 C6 Cl3 179.14(18)
C8 Si1 C7 Cl2 156.56(12)
C1 Si1 C7 Cl2 -18.55(17)
O1 Si1 C7 Cl2 64.74(12)
Cl1 Si1 C7 Cl2 -107.12(11)
