 
data_2009src0345pbca
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C15 H19 Cl N4 O7 Si'
_chemical_formula_weight          430.88
 
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'
 
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    Pbca
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    6.8700(3)
_cell_length_b                    23.3867(14)
_cell_length_c                    24.3510(15)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3912.4(4)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     55702
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.17
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.463
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1792
_exptl_absorpt_coefficient_mu     0.302
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9504
_exptl_absorpt_correction_T_max   0.9851
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)' 
 
_exptl_special_details
;
 ?
;
 
_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             20043
_diffrn_reflns_av_R_equivalents   0.0832
_diffrn_reflns_av_sigmaI/netI     0.0715
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          3.05
_diffrn_reflns_theta_max          25.00
_reflns_number_total              3395
_reflns_number_gt                 2812
_reflns_threshold_expression      >2σ(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     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_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 > 2σ(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.

 Hydrogen atoms on water molecule O1w could not be located.
 High R values due to unresolved modulation. However strudcture can be used
 to obtain gross connectivity.
;
 
_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)+(0.0400P)²+71.9615P] 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          3395
_refine_ls_number_parameters      256
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1940
_refine_ls_R_factor_gt            0.1744
_refine_ls_wR_factor_ref          0.3534
_refine_ls_wR_factor_gt           0.3437
_refine_ls_goodness_of_fit_ref    1.271
_refine_ls_restrained_S_all       1.271
_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
C2 C 0.5853(15) 0.2356(4) 0.4566(5) 0.039(3) Uani 1 1 d . . .
H2 H 0.6128 0.2676 0.4793 0.047 Uiso 1 1 calc R . .
C3 C 0.5559(16) 0.2430(5) 0.4024(6) 0.049(3) Uani 1 1 d . . .
C4 C 0.5124(16) 0.1958(4) 0.3708(6) 0.041(3) Uani 1 1 d . . .
H4 H 0.4905 0.2003 0.3325 0.049 Uiso 1 1 calc R . .
C5 C 0.5003(15) 0.1424(5) 0.3938(5) 0.037(3) Uani 1 1 d . . .
C6 C 0.5364(14) 0.1340(5) 0.4497(5) 0.035(3) Uani 1 1 d . . .
C7 C 0.6149(17) 0.1721(4) 0.5368(5) 0.041(3) Uani 1 1 d . . .
H7A H 0.5267 0.1955 0.5598 0.049 Uiso 1 1 calc R . .
H7B H 0.7508 0.1827 0.5456 0.049 Uiso 1 1 calc R . .
C8 C 0.573(2) 0.3014(5) 0.3767(6) 0.058(4) Uani 1 1 d . . .
H8A H 0.5783 0.3305 0.4056 0.086 Uiso 1 1 calc R . .
H8B H 0.4606 0.3084 0.3530 0.086 Uiso 1 1 calc R . .
H8C H 0.6928 0.3032 0.3547 0.086 Uiso 1 1 calc R . .
C22 C 0.9485(14) -0.0192(5) 0.6181(5) 0.044(3) Uani 1 1 d . . .
H22 H 0.9884 -0.0445 0.5898 0.053 Uiso 1 1 calc R . .
C23 C 0.9980(17) -0.0315(6) 0.6707(5) 0.051(4) Uani 1 1 d . . .
C24 C 0.9463(16) 0.0093(6) 0.7101(5) 0.046(3) Uani 1 1 d . . .
H24 H 0.9858 0.0044 0.7472 0.056 Uiso 1 1 calc R . .
C25 C 0.8404(16) 0.0557(6) 0.6957(5) 0.045(3) Uani 1 1 d . . .
C26 C 0.7761(15) 0.0668(5) 0.6410(5) 0.037(3) Uani 1 1 d . . .
C27 C 0.7738(15) 0.0389(4) 0.5474(4) 0.034(2) Uani 1 1 d . . .
H27A H 0.7233 0.0031 0.5311 0.040 Uiso 1 1 calc R . .
H27B H 0.8821 0.0530 0.5242 0.040 Uiso 1 1 calc R . .
C28 C 1.1008(18) -0.0841(7) 0.6862(6) 0.070(5) Uani 1 1 d . . .
H28A H 1.0185 -0.1068 0.7108 0.105 Uiso 1 1 calc R . .
H28B H 1.2225 -0.0743 0.7049 0.105 Uiso 1 1 calc R . .
H28C H 1.1298 -0.1064 0.6531 0.105 Uiso 1 1 calc R . .
C31 C 0.3282(15) 0.0684(5) 0.5704(5) 0.038(3) Uani 1 1 d . . .
H31A H 0.2301 0.0885 0.5485 0.058 Uiso 1 1 calc R . .
H31B H 0.3055 0.0759 0.6095 0.058 Uiso 1 1 calc R . .
H31C H 0.3192 0.0272 0.5635 0.058 Uiso 1 1 calc R . .
N1 N 0.5756(12) 0.1823(4) 0.4789(4) 0.034(2) Uani 1 1 d . . .
N5 N 0.4520(13) 0.0942(4) 0.3573(4) 0.045(3) Uani 1 1 d . . .
N21 N 0.8435(12) 0.0283(4) 0.6043(4) 0.036(2) Uani 1 1 d . . .
N25 N 0.7937(17) 0.0974(7) 0.7386(6) 0.067(4) Uani 1 1 d . . .
O5A O 0.3785(14) 0.1055(4) 0.3124(4) 0.063(3) Uani 1 1 d . . .
O5B O 0.4884(12) 0.0465(3) 0.3740(3) 0.045(2) Uani 1 1 d . . .
O6 O 0.5337(10) 0.0871(3) 0.4754(3) 0.0331(18) Uani 1 1 d . . .
O25A O 0.7285(17) 0.1431(6) 0.7267(5) 0.092(4) Uani 1 1 d . . .
O25B O 0.814(2) 0.0834(5) 0.7854(5) 0.103(5) Uani 1 1 d . . .
O26 O 0.6652(11) 0.1067(4) 0.6239(3) 0.047(2) Uani 1 1 d . . .
Si1 Si 0.5746(4) 0.09417(13) 0.55109(14) 0.0378(8) Uani 1 1 d . . .
Cl2 Cl 0.0438(4) 0.14593(13) 0.45616(15) 0.0519(9) Uani 1 1 d . . .
O1W O 0.5334(19) 0.2664(5) 0.6528(9) 0.159(8) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C2 C3 1.346(18) . ?
C2 N1 1.361(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(18) . ?
C3 C8 1.506(15) . ?
C4 C5 1.371(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(16) . ?
C5 N5 1.473(16) . ?
C6 O6 1.263(12) . ?
C6 N1 1.362(14) . ?
C7 N1 1.456(14) . ?
C7 Si1 1.875(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C22 C23 1.357(17) . ?
C22 N21 1.366(14) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(19) . ?
C23 C28 1.468(18) . ?
C24 C25 1.352(18) . ?
C24 H24 0.9500 . ?
C25 C26 1.426(16) . ?
C25 N25 1.467(18) . ?
C26 O26 1.275(14) . ?
C26 N21 1.351(15) . ?
C27 N21 1.487(13) . ?
C27 Si1 1.884(10) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 Si1 1.858(11) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N5 O5B 1.213(12) . ?
N5 O5A 1.233(13) . ?
N25 O25A 1.195(17) . ?
N25 O25B 1.195(15) . ?
O6 Si1 1.872(8) . ?
O26 Si1 1.901(9) . ?
 
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
C3 C2 N1 120.1(11) . . ?
C3 C2 H2 119.9 . . ?
N1 C2 H2 119.9 . . ?
C2 C3 C4 118.5(11) . . ?
C2 C3 C8 120.9(13) . . ?
C4 C3 C8 120.7(13) . . ?
C5 C4 C3 120.9(12) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 121.1(12) . . ?
C4 C5 N5 117.6(11) . . ?
C6 C5 N5 121.3(10) . . ?
O6 C6 N1 117.7(10) . . ?
O6 C6 C5 127.1(11) . . ?
N1 C6 C5 115.2(10) . . ?
N1 C7 Si1 108.2(8) . . ?
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 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C23 C22 N21 122.5(13) . . ?
C23 C22 H22 118.7 . . ?
N21 C22 H22 118.7 . . ?
C22 C23 C24 116.0(13) . . ?
C22 C23 C28 122.7(14) . . ?
C24 C23 C28 121.3(12) . . ?
C25 C24 C23 120.4(11) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 123.7(13) . . ?
C24 C25 N25 117.8(12) . . ?
C26 C25 N25 118.5(12) . . ?
O26 C26 N21 118.4(10) . . ?
O26 C26 C25 128.6(12) . . ?
N21 C26 C25 113.0(11) . . ?
N21 C27 Si1 107.7(7) . . ?
N21 C27 H27A 110.2 . . ?
Si1 C27 H27A 110.2 . . ?
N21 C27 H27B 110.2 . . ?
Si1 C27 H27B 110.2 . . ?
H27A C27 H27B 108.5 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
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 124.1(10) . . ?
C2 N1 C7 121.9(10) . . ?
C6 N1 C7 113.9(9) . . ?
O5B N5 O5A 125.3(11) . . ?
O5B N5 C5 117.1(10) . . ?
O5A N5 C5 117.6(10) . . ?
C26 N21 C22 124.0(10) . . ?
C26 N21 C27 113.3(9) . . ?
C22 N21 C27 122.4(10) . . ?
O25A N25 O25B 121.4(17) . . ?
O25A N25 C25 120.3(14) . . ?
O25B N25 C25 118.1(15) . . ?
C6 O6 Si1 114.2(7) . . ?
C26 O26 Si1 112.8(8) . . ?
C31 Si1 O6 94.8(4) . . ?
C31 Si1 C7 119.8(5) . . ?
O6 Si1 C7 85.7(4) . . ?
C31 Si1 C27 116.8(5) . . ?
O6 Si1 C27 90.1(4) . . ?
C7 Si1 C27 123.4(5) . . ?
C31 Si1 O26 96.4(5) . . ?
O6 Si1 O26 168.7(4) . . ?
C7 Si1 O26 88.6(5) . . ?
C27 Si1 O26 85.0(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.989
_refine_diff_density_max    1.266
_refine_diff_density_min   -0.517
_refine_diff_density_rms    0.133
