 
data_2007src0237r
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr P. G. Taylor
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C21 H28 N2 O2 Si2'
_chemical_formula_weight          396.63
 
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'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'P 2(1)/c'

loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    10.72290(10)
_cell_length_b                    10.23950(10)
_cell_length_c                    20.1530(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  92.7121(7)
_cell_angle_gamma                 90.00
_cell_volume                      2210.26(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     55769
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.16
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.192
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              848
_exptl_absorpt_coefficient_mu     0.178
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.9721
_exptl_absorpt_correction_T_max   0.9894
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)'
 
_exptl_special_details
;
 SADABS was used to perform the Absorption correction
Parameter refinement on 37920 reflections reduced R(int) from 0.1173 to 0.0347
Ratio of minimum to maximum apparent transmission: 0.934560
The given Tmin and Tmax were generated using the SHELX SIZE command.
;
 
_diffrn_ambient_temperature        120(2)
_diffrn_radiation_wavelength       0.71073
_diffrn_radiation_type             MoK\a
_diffrn_radiation_source           'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type    
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method         'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             38821
_diffrn_reflns_av_R_equivalents   0.0341
_diffrn_reflns_av_sigmaI/netI     0.0211
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          3.36
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5047
_reflns_number_gt                 4629
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution    
;
Sir2004 (Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., 
Cascarano, G., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R., 
2004)
;
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     
'PLATON/PLUTON (Spek, A. L., 1998)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0346P)²+1.2007P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5047
_refine_ls_number_parameters      250
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0380
_refine_ls_R_factor_gt            0.0338
_refine_ls_wR_factor_ref          0.0874
_refine_ls_wR_factor_gt           0.0839
_refine_ls_goodness_of_fit_ref    1.063
_refine_ls_restrained_S_all       1.063
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
C1 C 0.67147(10) -0.20036(11) 0.13977(6) 0.0167(2) Uani 1 1 d . . .
C2 C 0.78764(11) -0.02301(11) 0.10273(6) 0.0177(2) Uani 1 1 d . . .
C3 C 0.82346(11) -0.15197(12) 0.06866(6) 0.0186(2) Uani 1 1 d . . .
C4 C 0.73554(11) 0.06775(12) 0.04754(6) 0.0193(2) Uani 1 1 d . . .
C5 C 0.61014(11) 0.10230(12) 0.04189(6) 0.0210(2) Uani 1 1 d . . .
H5 H 0.5546 0.0724 0.0740 0.025 Uiso 1 1 calc R . .
C6 C 0.56541(12) 0.18051(13) -0.01059(7) 0.0254(3) Uani 1 1 d . . .
H6 H 0.4797 0.2043 -0.0137 0.030 Uiso 1 1 calc R . .
C7 C 0.64435(13) 0.22374(13) -0.05812(7) 0.0286(3) Uani 1 1 d . . .
H7 H 0.6134 0.2771 -0.0938 0.034 Uiso 1 1 calc R . .
C8 C 0.76947(14) 0.18837(15) -0.05323(7) 0.0312(3) Uani 1 1 d . . .
H8 H 0.8244 0.2176 -0.0858 0.037 Uiso 1 1 calc R . .
C9 C 0.81478(12) 0.11058(14) -0.00118(7) 0.0270(3) Uani 1 1 d . . .
H9 H 0.9003 0.0862 0.0014 0.032 Uiso 1 1 calc R . .
C10 C 0.90358(11) 0.02911(12) 0.14185(6) 0.0198(2) Uani 1 1 d . . .
C11 C 0.94395(13) 0.15738(13) 0.13767(7) 0.0281(3) Uani 1 1 d . . .
H11 H 0.8995 0.2170 0.1092 0.034 Uiso 1 1 calc R . .
C12 C 1.04909(13) 0.19958(15) 0.17487(8) 0.0323(3) Uani 1 1 d . . .
H12 H 1.0755 0.2878 0.1718 0.039 Uiso 1 1 calc R . .
C13 C 1.11519(13) 0.11429(15) 0.21617(7) 0.0309(3) Uani 1 1 d . . .
H13 H 1.1872 0.1434 0.2412 0.037 Uiso 1 1 calc R . .
C14 C 1.07574(13) -0.01440(15) 0.22083(7) 0.0312(3) Uani 1 1 d . . .
H14 H 1.1208 -0.0738 0.2491 0.037 Uiso 1 1 calc R . .
C15 C 0.97026(12) -0.05639(13) 0.18404(7) 0.0253(3) Uani 1 1 d . . .
H15 H 0.9433 -0.1444 0.1877 0.030 Uiso 1 1 calc R . .
C16 C 0.64555(17) -0.51865(14) 0.09623(8) 0.0391(4) Uani 1 1 d . . .
H16A H 0.6596 -0.5210 0.1446 0.059 Uiso 1 1 calc R . .
H16B H 0.6512 -0.6074 0.0784 0.059 Uiso 1 1 calc R . .
H16C H 0.5624 -0.4828 0.0850 0.059 Uiso 1 1 calc R . .
C17 C 0.74088(14) -0.40517(15) -0.03180(7) 0.0306(3) Uani 1 1 d . . .
H17A H 0.6552 -0.3768 -0.0431 0.046 Uiso 1 1 calc R . .
H17B H 0.7548 -0.4915 -0.0511 0.046 Uiso 1 1 calc R . .
H17C H 0.7998 -0.3424 -0.0495 0.046 Uiso 1 1 calc R . .
C18 C 0.92603(14) -0.46760(15) 0.08466(8) 0.0343(3) Uani 1 1 d . . .
H18A H 0.9863 -0.4062 0.0671 0.051 Uiso 1 1 calc R . .
H18B H 0.9408 -0.5550 0.0669 0.051 Uiso 1 1 calc R . .
H18C H 0.9360 -0.4698 0.1332 0.051 Uiso 1 1 calc R . .
C19 C 0.67429(15) 0.18415(14) 0.21797(8) 0.0358(3) Uani 1 1 d . . .
H19A H 0.7623 0.1847 0.2334 0.054 Uiso 1 1 calc R . .
H19B H 0.6251 0.2338 0.2491 0.054 Uiso 1 1 calc R . .
H19C H 0.6657 0.2242 0.1738 0.054 Uiso 1 1 calc R . .
C20 C 0.65974(15) -0.07026(16) 0.29305(7) 0.0340(3) Uani 1 1 d . . .
H20A H 0.6351 -0.1623 0.2899 0.051 Uiso 1 1 calc R . .
H20B H 0.6165 -0.0284 0.3292 0.051 Uiso 1 1 calc R . .
H20C H 0.7502 -0.0643 0.3021 0.051 Uiso 1 1 calc R . .
C21 C 0.44523(12) 0.01311(14) 0.19696(7) 0.0261(3) Uani 1 1 d . . .
H21A H 0.4235 0.0722 0.1600 0.039 Uiso 1 1 calc R . .
H21B H 0.4041 0.0425 0.2367 0.039 Uiso 1 1 calc R . .
H21C H 0.4173 -0.0755 0.1855 0.039 Uiso 1 1 calc R . .
N1 N 0.74878(9) -0.25060(10) 0.09086(5) 0.0175(2) Uani 1 1 d . . .
N2 N 0.69210(9) -0.06913(10) 0.14780(5) 0.0173(2) Uani 1 1 d . . .
O1 O 0.59892(8) -0.26553(8) 0.17064(4) 0.02150(19) Uani 1 1 d . . .
O2 O 0.90366(9) -0.16520(9) 0.02883(5) 0.0267(2) Uani 1 1 d . . .
Si1 Si 0.76528(3) -0.41435(3) 0.059749(17) 0.02070(9) Uani 1 1 d . . .
Si2 Si 0.61704(3) 0.01346(3) 0.213497(17) 0.01965(9) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.2179(14) . ?
C1 N2 1.3701(15) . ?
C1 N1 1.4146(14) . ?
C2 N2 1.4785(14) . ?
C2 C4 1.5343(17) . ?
C2 C10 1.5360(16) . ?
C2 C3 1.5451(16) . ?
C3 O2 1.2115(15) . ?
C3 N1 1.3767(15) . ?
C4 C5 1.3899(17) . ?
C4 C9 1.3990(17) . ?
C5 C6 1.3935(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.3808(19) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.3867(19) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.3867(18) . ?
C10 C15 1.3939(18) . ?
C11 C12 1.3928(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.3909(19) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 Si1 1.8490(15) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si1 1.8536(14) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 Si1 1.8544(15) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 Si2 1.8531(15) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 Si2 1.8562(15) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 Si2 1.8567(13) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N1 Si1 1.8018(11) . ?
N2 Si2 1.7935(10) . ?
 
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
 _geom_angle_publ_flag
O1 C1 N2 125.49(11) . . ?
O1 C1 N1 124.49(11) . . ?
N2 C1 N1 110.01(10) . . ?
N2 C2 C4 113.56(9) . . ?
N2 C2 C10 111.29(10) . . ?
C4 C2 C10 114.82(10) . . ?
N2 C2 C3 101.19(9) . . ?
C4 C2 C3 106.57(10) . . ?
C10 C2 C3 108.23(9) . . ?
O2 C3 N1 125.13(11) . . ?
O2 C3 C2 126.10(11) . . ?
N1 C3 C2 108.78(10) . . ?
C5 C4 C9 118.69(12) . . ?
C5 C4 C2 122.09(11) . . ?
C9 C4 C2 119.09(11) . . ?
C4 C5 C6 120.36(12) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 120.69(12) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 119.29(12) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C9 C8 C7 120.41(13) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C4 120.55(12) . . ?
C8 C9 H9 119.7 . . ?
C4 C9 H9 119.7 . . ?
C11 C10 C15 118.64(12) . . ?
C11 C10 C2 123.04(11) . . ?
C15 C10 C2 118.31(11) . . ?
C10 C11 C12 120.54(13) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 120.54(13) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.49(13) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C13 C14 C15 120.01(13) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C10 120.77(13) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 N1 C1 109.20(10) . . ?
C3 N1 Si1 120.09(8) . . ?
C1 N1 Si1 130.64(8) . . ?
C1 N2 C2 110.70(9) . . ?
C1 N2 Si2 118.30(8) . . ?
C2 N2 Si2 130.63(8) . . ?
N1 Si1 C16 108.52(6) . . ?
N1 Si1 C17 106.72(6) . . ?
C16 Si1 C17 110.92(8) . . ?
N1 Si1 C18 106.54(6) . . ?
C16 Si1 C18 112.12(8) . . ?
C17 Si1 C18 111.72(7) . . ?
N2 Si2 C19 108.75(6) . . ?
N2 Si2 C20 108.59(6) . . ?
C19 Si2 C20 109.02(8) . . ?
N2 Si2 C21 110.04(6) . . ?
C19 Si2 C21 109.52(7) . . ?
C20 Si2 C21 110.87(7) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.349
_refine_diff_density_min   -0.245
_refine_diff_density_rms    0.045
