#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:03:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180001 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/95/7029588.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_7029588
loop_
_publ_author_name
'Kociok-Köhn, Gabriele'
'Mahon, Mary F.'
'Molloy, Kieran C.'
'Price, Gareth J.'
'Prior, Timothy J.'
'Smith, Douglas R. G.'
_publ_section_title
;
 Biomimetic polyorganosiloxanes: model compounds for new materials.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7734
_journal_page_last               7746
_journal_paper_doi               10.1039/c4dt00554f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C17 H24 N2 O2 Si'
_chemical_formula_sum            'C17 H24 N2 O2 Si'
_chemical_formula_weight         316.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.284(3)
_cell_angle_beta                 92.095(3)
_cell_angle_gamma                99.840(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0964(4)
_cell_length_b                   8.3765(5)
_cell_length_c                   13.0731(7)
_cell_measurement_reflns_used    16108
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     862.75(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL-2012 (Sheldrick, 2012)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '143 2.0 degree images with ω 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  0.0449
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9597
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         5.533
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0507P)²+0.4022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3247
_reflns_number_total             3883
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt00554f1.cif
_cod_data_source_block           Compound-5-k04kcm13
_cod_depositor_comments
'Adding full bibliography for 7029587--7029593.cif.'
_cod_database_code               7029588
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Si Si -0.17479(6) 0.24545(6) 0.06680(4) 0.03045(15) Uani 1 1 d . .
O1 O 0.98461(14) 0.28759(14) 0.48220(10) 0.0289(3) Uani 1 1 d . .
O2 O 0.57788(15) 0.56988(14) 0.40160(9) 0.0301(3) Uani 1 1 d . .
N1 N 0.77960(16) 0.42408(16) 0.43811(10) 0.0234(3) Uani 1 1 d . .
H1 H 0.851(3) 0.516(3) 0.4578(17) 0.034(5) Uiso 1 1 d . .
N2 N 0.51139(16) 0.28970(17) 0.37729(10) 0.0248(3) Uani 1 1 d . .
C1 C 0.83892(19) 0.28155(19) 0.44763(12) 0.0232(3) Uani 1 1 d . .
C2 C 0.7204(2) 0.13103(19) 0.41593(13) 0.0259(3) Uani 1 1 d . .
C3 C 0.5632(2) 0.14330(19) 0.38329(12) 0.0263(3) Uani 1 1 d . .
H3 H 0.4841 0.0450 0.3634 0.032 Uiso 1 1 calc R U
C4 C 0.61845(19) 0.43695(19) 0.40499(12) 0.0236(3) Uani 1 1 d . .
C5 C 0.7767(2) -0.0293(2) 0.42047(18) 0.0397(4) Uani 1 1 d . .
H5A H 0.6805 -0.1191 0.4033 0.059 Uiso 1 1 calc R U
H5B H 0.8238 -0.0304 0.4904 0.059 Uiso 1 1 calc R U
H5C H 0.8625 -0.0434 0.3706 0.059 Uiso 1 1 calc R U
C6 C 0.3335(2) 0.2905(2) 0.34814(13) 0.0282(3) Uani 1 1 d . .
H6A H 0.3062 0.3984 0.3765 0.034 Uiso 1 1 calc R U
H6B H 0.2618 0.2061 0.3805 0.034 Uiso 1 1 calc R U
C7 C 0.2911(2) 0.2583(2) 0.23244(13) 0.0286(3) Uani 1 1 d . .
H7A H 0.3146 0.1492 0.2034 0.034 Uiso 1 1 calc R U
H7B H 0.3623 0.3418 0.1991 0.034 Uiso 1 1 calc R U
C8 C 0.1063(2) 0.2643(2) 0.20954(13) 0.0301(4) Uani 1 1 d . .
H8A H 0.0821 0.3698 0.2448 0.036 Uiso 1 1 calc R U
H8B H 0.0366 0.1752 0.2391 0.036 Uiso 1 1 calc R U
C9 C 0.0548(2) 0.2470(2) 0.09417(13) 0.0334(4) Uani 1 1 d . .
H9A H 0.0834 0.1439 0.0583 0.040 Uiso 1 1 calc R U
H9B H 0.1207 0.3389 0.0652 0.040 Uiso 1 1 calc R U
C10 C -0.3010(2) 0.0588(3) 0.10621(16) 0.0407(4) Uani 1 1 d . .
H10A H -0.2726 0.0552 0.1793 0.061 Uiso 1 1 calc R U
H10B H -0.2759 -0.0392 0.0635 0.061 Uiso 1 1 calc R U
H10C H -0.4209 0.0624 0.0966 0.061 Uiso 1 1 calc R U
C11 C -0.2385(3) 0.4307(3) 0.14010(15) 0.0419(4) Uani 1 1 d . .
H11A H -0.3595 0.4257 0.1272 0.063 Uiso 1 1 calc R U
H11B H -0.1770 0.5293 0.1173 0.063 Uiso 1 1 calc R U
H11C H -0.2126 0.4346 0.2143 0.063 Uiso 1 1 calc R U
C12 C -0.2199(2) 0.2474(2) -0.07516(13) 0.0295(3) Uani 1 1 d . .
C13 C -0.1080(2) 0.2116(2) -0.15074(14) 0.0362(4) Uani 1 1 d . .
H13 H -0.0052 0.1808 -0.1310 0.043 Uiso 1 1 calc R U
C14 C -0.1456(3) 0.2205(3) -0.25500(15) 0.0409(4) Uani 1 1 d . .
H14 H -0.0675 0.1968 -0.3050 0.049 Uiso 1 1 calc R U
C15 C -0.2935(2) 0.2629(2) -0.28546(14) 0.0353(4) Uani 1 1 d . .
H15 H -0.3172 0.2703 -0.3562 0.042 Uiso 1 1 calc R U
C16 C -0.4089(2) 0.2952(2) -0.21257(14) 0.0355(4) Uani 1 1 d . .
H16 H -0.5138 0.3205 -0.2336 0.043 Uiso 1 1 calc R U
C17 C -0.3702(2) 0.2904(2) -0.10844(14) 0.0341(4) Uani 1 1 d . .
H17 H -0.4479 0.3169 -0.0588 0.041 Uiso 1 1 calc R U
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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 '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
C11 Si C10 108.89(10)
C11 Si C9 110.55(9)
C10 Si C9 109.67(9)
C11 Si C12 107.86(9)
C10 Si C12 109.74(8)
C9 Si C12 110.11(8)
C1 N1 C4 126.83(14)
C1 N1 H1 116.3(14)
C4 N1 H1 116.8(14)
C4 N2 C3 121.48(13)
C4 N2 C6 118.77(13)
C3 N2 C6 119.59(13)
O1 C1 N1 120.31(14)
O1 C1 C2 124.05(14)
N1 C1 C2 115.64(13)
C3 C2 C1 117.59(14)
C3 C2 C5 123.44(15)
C1 C2 C5 118.97(14)
C2 C3 N2 123.80(15)
C2 C3 H3 118.1
N2 C3 H3 118.1
O2 C4 N2 123.82(14)
O2 C4 N1 121.56(14)
N2 C4 N1 114.63(13)
C2 C5 H5A 109.5
C2 C5 H5B 109.5
H5A C5 H5B 109.5
C2 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
N2 C6 C7 113.86(13)
N2 C6 H6A 108.8
C7 C6 H6A 108.8
N2 C6 H6B 108.8
C7 C6 H6B 108.8
H6A C6 H6B 107.7
C6 C7 C8 110.25(13)
C6 C7 H7A 109.6
C8 C7 H7A 109.6
C6 C7 H7B 109.6
C8 C7 H7B 109.6
H7A C7 H7B 108.1
C7 C8 C9 114.09(14)
C7 C8 H8A 108.7
C9 C8 H8A 108.7
C7 C8 H8B 108.7
C9 C8 H8B 108.7
H8A C8 H8B 107.6
C8 C9 Si 113.66(12)
C8 C9 H9A 108.8
Si C9 H9A 108.8
C8 C9 H9B 108.8
Si C9 H9B 108.8
H9A C9 H9B 107.7
Si C10 H10A 109.5
Si C10 H10B 109.5
H10A C10 H10B 109.5
Si C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
Si C11 H11A 109.5
Si C11 H11B 109.5
H11A C11 H11B 109.5
Si C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
C17 C12 C13 117.22(16)
C17 C12 Si 119.44(13)
C13 C12 Si 123.32(13)
C12 C13 C14 120.93(17)
C12 C13 H13 119.5
C14 C13 H13 119.5
C15 C14 C13 120.65(18)
C15 C14 H14 119.7
C13 C14 H14 119.7
C14 C15 C16 119.74(17)
C14 C15 H15 120.1
C16 C15 H15 120.1
C15 C16 C17 119.71(17)
C15 C16 H16 120.1
C17 C16 H16 120.1
C16 C17 C12 121.70(17)
C16 C17 H17 119.2
C12 C17 H17 119.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si C11 1.864(2)
Si C10 1.865(2)
Si C9 1.8772(18)
Si C12 1.8812(18)
O1 C1 1.2378(19)
O2 C4 1.2198(19)
N1 C1 1.381(2)
N1 C4 1.3862(19)
N1 H1 0.88(2)
N2 C4 1.374(2)
N2 C3 1.374(2)
N2 C6 1.4778(19)
C1 C2 1.445(2)
C2 C3 1.353(2)
C2 C5 1.499(2)
C3 H3 0.9500
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 C7 1.514(2)
C6 H6A 0.9900
C6 H6B 0.9900
C7 C8 1.526(2)
C7 H7A 0.9900
C7 H7B 0.9900
C8 C9 1.530(2)
C8 H8A 0.9900
C8 H8B 0.9900
C9 H9A 0.9900
C9 H9B 0.9900
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 H11A 0.9800
C11 H11B 0.9800
C11 H11C 0.9800
C12 C17 1.398(2)
C12 C13 1.400(2)
C13 C14 1.401(3)
C13 H13 0.9500
C14 C15 1.368(3)
C14 H14 0.9500
C15 C16 1.390(3)
C15 H15 0.9500
C16 C17 1.394(2)
C16 H16 0.9500
C17 H17 0.9500
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.88(2) 1.97(2) 2.8490(18) 173(2) 2_766
