#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:10:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178692 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/03/4080371.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_4080371
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
'C15 H19 N2 O2 Si +, 0.75 H3 O +, 1.75 Cl -, 0.25 H2 O'
_chemical_formula_sum            'C15 H21.75 Cl1.75 N2 O3 Si'
_chemical_formula_weight         368.22
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.673(12)
_cell_angle_beta                 71.708(11)
_cell_angle_gamma                71.435(12)
_cell_formula_units_Z            2
_cell_length_a                   7.941(3)
_cell_length_b                   10.448(5)
_cell_length_c                   12.404(6)
_cell_measurement_reflns_used    2202
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      1.68
_cell_volume                     922.9(7)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type
'Crystal Logics diffractometer with Rigaku Saturn 724 CCD detector'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Diamond I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8082
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             387
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0545
_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)+(0.0952P)²+0.7114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                2873
_reflns_number_total             3438
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om301137b_si_002.cif
_cod_data_source_block           ssh0985
_cod_database_code               4080371
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
Si Si 0.73278(10) 0.38493(6) 0.15305(6) 0.0139(2) Uani 1 1 d .
O1 O 0.4803(3) 0.40383(17) 0.17836(14) 0.0162(4) Uani 1 1 d .
N1 N 0.4379(3) 0.5427(2) 0.32864(17) 0.0142(5) Uani 1 1 d .
C1 C 0.6447(4) 0.4957(2) 0.2916(2) 0.0170(6) Uani 1 1 d .
H1A H 0.6901 0.4431 0.3502 0.020 Uiso 1 1 calc R
H1B H 0.6911 0.5740 0.2797 0.020 Uiso 1 1 calc R
C2 C 0.3624(4) 0.4872(2) 0.2653(2) 0.0140(5) Uani 1 1 d .
C3 C 0.1669(4) 0.5252(3) 0.2962(2) 0.0189(6) Uani 1 1 d .
H3 H 0.1105 0.4868 0.2543 0.023 Uiso 1 1 calc R
C4 C 0.0568(4) 0.6186(3) 0.3879(2) 0.0231(6) Uani 1 1 d .
H4 H -0.0760 0.6450 0.4084 0.028 Uiso 1 1 calc R
C5 C 0.1381(4) 0.6760(3) 0.4523(2) 0.0226(6) Uani 1 1 d .
C6 C 0.3292(4) 0.6354(3) 0.4201(2) 0.0199(6) Uani 1 1 d .
H6 H 0.3878 0.6719 0.4617 0.024 Uiso 1 1 calc R
C7 C 0.0195(5) 0.7807(3) 0.5514(3) 0.0365(8) Uani 1 1 d .
H7A H 0.1013 0.8079 0.5845 0.055 Uiso 1 1 calc R
H7B H -0.0625 0.7423 0.6092 0.055 Uiso 1 1 calc R
H7C H -0.0573 0.8601 0.5247 0.055 Uiso 1 1 calc R
O2 O 0.9784(3) 0.35225(16) 0.15301(15) 0.0172(4) Uani 1 1 d .
N2 N 0.9880(3) 0.1342(2) 0.14388(18) 0.0159(5) Uani 1 1 d .
C8 C 0.7908(4) 0.1938(2) 0.1500(2) 0.0180(6) Uani 1 1 d .
H8A H 0.7084 0.1694 0.2196 0.022 Uiso 1 1 calc R
H8B H 0.7710 0.1593 0.0828 0.022 Uiso 1 1 calc R
C9 C 1.0781(4) 0.2252(2) 0.1456(2) 0.0150(5) Uani 1 1 d .
C10 C 1.2654(4) 0.1774(3) 0.1419(2) 0.0176(6) Uani 1 1 d .
H10 H 1.3315 0.2389 0.1422 0.021 Uiso 1 1 calc R
C11 C 1.3534(4) 0.0393(3) 0.1376(2) 0.0207(6) Uani 1 1 d .
H11 H 1.4810 0.0060 0.1348 0.025 Uiso 1 1 calc R
C12 C 1.2571(4) -0.0528(3) 0.1375(2) 0.0213(6) Uani 1 1 d .
C13 C 1.0746(4) -0.0028(2) 0.1405(2) 0.0195(6) Uani 1 1 d .
H13 H 1.0070 -0.0632 0.1402 0.023 Uiso 1 1 calc R
C14 C 1.3507(5) -0.2043(3) 0.1350(3) 0.0309(7) Uani 1 1 d .
H14A H 1.2559 -0.2495 0.1499 0.046 Uiso 1 1 calc R
H14B H 1.4123 -0.2229 0.1935 0.046 Uiso 1 1 calc R
H14C H 1.4445 -0.2382 0.0599 0.046 Uiso 1 1 calc R
C15 C 0.7693(4) 0.4669(3) 0.0172(2) 0.0197(6) Uani 1 1 d .
H15A H 0.7953 0.5507 0.0274 0.030 Uiso 1 1 calc R
H15B H 0.6560 0.4882 -0.0050 0.030 Uiso 1 1 calc R
H15C H 0.8759 0.4052 -0.0424 0.030 Uiso 1 1 calc R
Cl1 Cl 0.54508(11) 0.78553(7) 0.56898(6) 0.0266(2) Uani 1 1 d .
Cl2 Cl 0.78533(15) 0.80101(9) 0.17260(9) 0.0306(4) Uani 0.740(4) 1 d P
O3 O 0.4937(6) 0.9299(4) 0.3667(3) 0.0435(12) Uani 0.679(7) 1 d PU
O3A O 0.708(3) 0.9322(16) 0.3871(15) 0.042(3) Uani 0.141(6) 1 d PU
O3B O 0.643(3) 0.9001(14) 0.3104(14) 0.048(2) Uani 0.182(6) 1 d PU
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
O1 Si C1 85.90(10)
O1 Si O2 169.64(9)
O1 Si C8 89.54(10)
O1 Si C15 96.33(11)
C1 Si O2 88.82(10)
C1 Si C8 121.94(12)
C1 Si C15 118.41(12)
O2 Si C8 85.70(10)
O2 Si C15 94.02(11)
C8 Si C15 119.62(12)
Si O1 C2 114.60(16)
C1 N1 C2 115.1(2)
C1 N1 C6 122.6(2)
C2 N1 C6 122.3(2)
Si C1 N1 107.42(16)
O1 C2 N1 116.4(2)
O1 C2 C3 125.1(2)
N1 C2 C3 118.5(2)
C2 C3 C4 119.5(2)
C3 C4 C5 121.1(3)
C4 C5 C6 117.6(2)
C4 C5 C7 121.8(3)
C6 C5 C7 120.6(3)
N1 C6 C5 121.0(2)
Si O2 C9 115.12(17)
C8 N2 C9 115.1(2)
C8 N2 C13 122.7(2)
C9 N2 C13 122.1(2)
Si C8 N2 107.88(17)
O2 C9 N2 116.1(2)
O2 C9 C10 124.9(2)
N2 C9 C10 119.0(2)
C9 C10 C11 119.0(2)
C10 C11 C12 121.1(3)
C11 C12 C13 118.4(2)
C11 C12 C14 121.7(3)
C13 C12 C14 119.9(3)
N2 C13 C12 120.3(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si O1 1.874(2)
Si C1 1.898(3)
Si O2 1.870(2)
Si C8 1.899(3)
Si C15 1.855(3)
O1 C2 1.300(3)
N1 C1 1.474(4)
N1 C2 1.360(3)
N1 C6 1.368(3)
C2 C3 1.398(4)
C3 C4 1.376(4)
C4 C5 1.416(4)
C5 C6 1.364(4)
C5 C7 1.508(4)
O2 C9 1.299(3)
N2 C8 1.467(4)
N2 C9 1.364(3)
N2 C13 1.372(3)
C9 C10 1.396(4)
C10 C11 1.383(4)
C11 C12 1.407(4)
C12 C13 1.364(4)
C12 C14 1.515(4)
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
C15 Si O1 C2 -112.29(18)
O2 Si O1 C2 65.5(5)
C1 Si O1 C2 5.87(17)
C8 Si O1 C2 127.95(17)
C2 N1 C1 Si 6.5(2)
C6 N1 C1 Si -173.56(18)
C15 Si C1 N1 88.56(19)
O2 Si C1 N1 -177.50(16)
O1 Si C1 N1 -6.42(15)
C8 Si C1 N1 -93.32(18)
Si O1 C2 N1 -3.4(3)
Si O1 C2 C3 175.20(19)
C6 N1 C2 O1 177.8(2)
C1 N1 C2 O1 -2.3(3)
C6 N1 C2 C3 -0.9(3)
C1 N1 C2 C3 179.0(2)
O1 C2 C3 C4 -177.5(2)
N1 C2 C3 C4 1.1(4)
C2 C3 C4 C5 -0.6(4)
C3 C4 C5 C6 0.0(4)
C3 C4 C5 C7 178.6(3)
C4 C5 C6 N1 0.2(4)
C7 C5 C6 N1 -178.5(3)
C2 N1 C6 C5 0.3(4)
C1 N1 C6 C5 -179.6(2)
C15 Si O2 C9 -116.31(18)
O1 Si O2 C9 65.9(5)
C1 Si O2 C9 125.29(18)
C8 Si O2 C9 3.14(18)
C9 N2 C8 Si 2.0(3)
C13 N2 C8 Si 179.93(19)
C15 Si C8 N2 89.5(2)
O2 Si C8 N2 -2.65(17)
O1 Si C8 N2 -173.45(17)
C1 Si C8 N2 -88.6(2)
Si O2 C9 N2 -2.7(3)
Si O2 C9 C10 178.68(19)
C13 N2 C9 O2 -177.6(2)
C8 N2 C9 O2 0.4(3)
C13 N2 C9 C10 1.1(4)
C8 N2 C9 C10 179.1(2)
O2 C9 C10 C11 177.9(2)
N2 C9 C10 C11 -0.6(4)
C9 C10 C11 C12 -0.2(4)
C10 C11 C12 C13 0.7(4)
C10 C11 C12 C14 -178.9(3)
C11 C12 C13 N2 -0.2(4)
C14 C12 C13 N2 179.4(2)
C9 N2 C13 C12 -0.7(4)
C8 N2 C13 C12 -178.5(2)
