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# 
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#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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data_PC-X1720f2-shelxl
# COM648 Secant Lam Sze Kui's PC-X1720f2 (collected at PolyU) 15-Jun-2011 

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_absolute_configuration rmad
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H17 N O4 S'
_chemical_formula_sum            'C15 H17 N O4 S'
_chemical_formula_weight         307.36

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   5.0949(2)
_cell_length_b                   12.0655(4)
_cell_length_c                   24.2090(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1488.19(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11344
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      25.02

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9210
_exptl_absorpt_correction_T_max  0.9638
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11344
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2616
_reflns_number_gt                2306
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'APEX (Bruker AXS Inc, 2007)'
_computing_cell_refinement       'SAINT v7.34A (Bruker AXS Inc, 2007)'
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0361P)^2^+0.1990P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack (1983). 1054 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_number_reflns         2616
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_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
S1 S 0.87519(11) 0.38532(5) 0.40888(2) 0.04290(17) Uani 1 1 d . . .
O1 O 0.9715(3) 0.55905(13) 0.23178(6) 0.0487(4) Uani 1 1 d . . .
O2 O 0.4293(4) 0.75312(14) 0.29953(8) 0.0729(6) Uani 1 1 d . . .
O3 O 1.1392(3) 0.41462(16) 0.39465(7) 0.0636(5) Uani 1 1 d . . .
O4 O 0.8054(4) 0.27188(12) 0.41694(7) 0.0592(5) Uani 1 1 d . . .
N1 N 0.6927(4) 0.43064(16) 0.35866(8) 0.0383(4) Uani 1 1 d . . .
C1 C 0.7853(4) 0.46089(18) 0.46825(9) 0.0400(5) Uani 1 1 d . . .
C2 C 0.5843(5) 0.42179(19) 0.50105(9) 0.0465(6) Uani 1 1 d . . .
H2 H 0.5081 0.3534 0.4936 0.056 Uiso 1 1 calc R . .
C3 C 0.4971(6) 0.4847(2) 0.54491(9) 0.0519(6) Uani 1 1 d . . .
H3 H 0.3636 0.4574 0.5673 0.062 Uiso 1 1 calc R . .
C4 C 0.6046(5) 0.58763(19) 0.55620(9) 0.0488(6) Uani 1 1 d . . .
C5 C 0.8073(5) 0.6251(2) 0.52321(10) 0.0548(6) Uani 1 1 d . . .
H5 H 0.8835 0.6936 0.5306 0.066 Uiso 1 1 calc R . .
C6 C 0.8986(5) 0.56248(19) 0.47944(10) 0.0519(6) Uani 1 1 d . . .
H6 H 1.0356 0.5886 0.4576 0.062 Uiso 1 1 calc R . .
C7 C 0.7175(5) 0.54775(17) 0.34314(9) 0.0407(5) Uani 1 1 d . . .
H7A H 0.9018 0.5675 0.3409 0.049 Uiso 1 1 calc R . .
H7B H 0.6367 0.5937 0.3713 0.049 Uiso 1 1 calc R . .
C8 C 0.5854(4) 0.56933(16) 0.28751(8) 0.0348(5) Uani 1 1 d . . .
H8 H 0.4022 0.5449 0.2896 0.042 Uiso 1 1 calc R . .
C9 C 0.5916(5) 0.69510(18) 0.27763(9) 0.0433(6) Uani 1 1 d . . .
C10 C 0.8088(5) 0.74267(19) 0.24330(11) 0.0569(7) Uani 1 1 d . . .
H10A H 0.9515 0.7655 0.2673 0.068 Uiso 1 1 calc R . .
H10B H 0.7451 0.8078 0.2240 0.068 Uiso 1 1 calc R . .
C11 C 0.9115(5) 0.6590(2) 0.20125(10) 0.0546(7) Uani 1 1 d . . .
H11 H 1.0632 0.6870 0.1807 0.066 Uiso 1 1 calc R . .
C12 C 0.6942(5) 0.6215(2) 0.16399(10) 0.0581(7) Uani 1 1 d . . .
H12 H 0.6473 0.6541 0.1306 0.070 Uiso 1 1 calc R . .
C13 C 0.5816(5) 0.5350(2) 0.18658(9) 0.0499(6) Uani 1 1 d . . .
H13 H 0.4400 0.4959 0.1721 0.060 Uiso 1 1 calc R . .
C14 C 0.7198(4) 0.50975(18) 0.23959(9) 0.0381(5) Uani 1 1 d . . .
H14 H 0.7328 0.4298 0.2461 0.046 Uiso 1 1 calc R . .
C15 C 0.5020(7) 0.6561(2) 0.60355(10) 0.0725(9) Uani 1 1 d . . .
H15A H 0.5239 0.6160 0.6375 0.087 Uiso 1 1 calc R . .
H15B H 0.3191 0.6715 0.5978 0.087 Uiso 1 1 calc R . .
H15C H 0.5976 0.7246 0.6055 0.087 Uiso 1 1 calc R . .
H1 H 0.545(5) 0.4161(18) 0.3655(9) 0.042(7) Uiso 1 1 d . . .

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
S1 0.0417(3) 0.0487(3) 0.0383(3) 0.0036(3) 0.0021(3) 0.0116(3)
O1 0.0337(8) 0.0571(10) 0.0554(10) 0.0117(8) 0.0074(8) 0.0069(7)
O2 0.0854(15) 0.0518(10) 0.0814(13) -0.0066(9) 0.0122(12) 0.0291(11)
O3 0.0374(8) 0.0946(14) 0.0589(11) 0.0032(10) 0.0026(8) 0.0164(9)
O4 0.0883(13) 0.0385(9) 0.0508(10) 0.0049(8) 0.0030(10) 0.0169(9)
N1 0.0360(10) 0.0420(11) 0.0370(11) 0.0045(8) 0.0030(8) -0.0007(8)
C1 0.0413(12) 0.0452(12) 0.0335(12) 0.0055(10) -0.0043(10) 0.0046(10)
C2 0.0593(15) 0.0417(12) 0.0386(13) 0.0015(10) 0.0003(11) -0.0042(12)
C3 0.0637(15) 0.0561(15) 0.0359(14) 0.0044(11) 0.0066(12) -0.0021(13)
C4 0.0639(15) 0.0474(14) 0.0349(12) 0.0005(10) -0.0111(12) 0.0068(13)
C5 0.0658(16) 0.0415(12) 0.0571(16) -0.0035(12) -0.0114(14) -0.0048(13)
C6 0.0484(13) 0.0555(14) 0.0518(15) 0.0051(12) 0.0010(13) -0.0079(13)
C7 0.0454(12) 0.0391(12) 0.0376(12) -0.0015(10) -0.0018(10) -0.0004(10)
C8 0.0319(11) 0.0375(11) 0.0350(11) 0.0008(9) -0.0006(9) 0.0025(10)
C9 0.0501(13) 0.0367(12) 0.0430(13) -0.0011(10) -0.0101(12) 0.0099(12)
C10 0.0623(16) 0.0395(13) 0.0687(18) 0.0091(12) -0.0047(14) -0.0053(12)
C11 0.0480(15) 0.0568(15) 0.0591(15) 0.0223(12) 0.0090(13) -0.0010(12)
C12 0.0668(16) 0.0692(17) 0.0384(14) 0.0116(13) 0.0068(12) 0.0158(15)
C13 0.0558(15) 0.0570(15) 0.0369(13) -0.0083(11) -0.0041(12) 0.0025(13)
C14 0.0385(11) 0.0351(11) 0.0407(13) -0.0001(10) 0.0026(10) 0.0009(9)
C15 0.096(2) 0.0696(19) 0.0520(17) -0.0140(13) -0.0023(17) 0.0169(17)

_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
S1 O4 1.4275(16) . ?
S1 O3 1.4330(17) . ?
S1 N1 1.6252(19) . ?
S1 C1 1.763(2) . ?
O1 C14 1.426(3) . ?
O1 C11 1.447(3) . ?
O2 C9 1.206(3) . ?
N1 C7 1.467(3) . ?
N1 H1 0.79(2) . ?
C1 C2 1.379(3) . ?
C1 C6 1.382(3) . ?
C2 C3 1.379(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(3) . ?
C4 C15 1.507(3) . ?
C5 C6 1.382(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.528(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C14 1.527(3) . ?
C8 C9 1.537(3) . ?
C8 H8 0.9800 . ?
C9 C10 1.498(3) . ?
C10 C11 1.526(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.498(4) . ?
C11 H11 0.9800 . ?
C12 C13 1.311(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.495(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?

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
O4 S1 O3 120.21(11) . . ?
O4 S1 N1 106.40(11) . . ?
O3 S1 N1 105.91(10) . . ?
O4 S1 C1 108.65(11) . . ?
O3 S1 C1 108.21(11) . . ?
N1 S1 C1 106.69(10) . . ?
C14 O1 C11 103.02(16) . . ?
C7 N1 S1 117.79(15) . . ?
C7 N1 H1 110.5(16) . . ?
S1 N1 H1 108.2(16) . . ?
C2 C1 C6 120.1(2) . . ?
C2 C1 S1 119.05(17) . . ?
C6 C1 S1 120.66(18) . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 121.2(2) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 C15 121.3(2) . . ?
C3 C4 C15 120.3(3) . . ?
C4 C5 C6 121.1(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.6(2) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
N1 C7 C8 110.60(17) . . ?
N1 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C14 C8 C7 113.08(17) . . ?
C14 C8 C9 109.71(17) . . ?
C7 C8 C9 107.25(16) . . ?
C14 C8 H8 108.9 . . ?
C7 C8 H8 108.9 . . ?
C9 C8 H8 108.9 . . ?
O2 C9 C10 121.9(2) . . ?
O2 C9 C8 119.4(2) . . ?
C10 C9 C8 118.68(19) . . ?
C9 C10 C11 111.7(2) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
O1 C11 C12 102.26(19) . . ?
O1 C11 C10 106.44(19) . . ?
C12 C11 C10 110.4(2) . . ?
O1 C11 H11 112.4 . . ?
C12 C11 H11 112.4 . . ?
C10 C11 H11 112.4 . . ?
C13 C12 C11 108.2(2) . . ?
C13 C12 H12 125.9 . . ?
C11 C12 H12 125.9 . . ?
C12 C13 C14 108.3(2) . . ?
C12 C13 H13 125.8 . . ?
C14 C13 H13 125.8 . . ?
O1 C14 C13 102.99(18) . . ?
O1 C14 C8 107.90(17) . . ?
C13 C14 C8 110.20(17) . . ?
O1 C14 H14 111.8 . . ?
C13 C14 H14 111.8 . . ?
C8 C14 H14 111.8 . . ?
C4 C15 H15A 109.5 . . ?
C4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

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 O3 0.79(2) 2.19(2) 2.958(3) 166(2) 1_455

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.034
_database_code_depnum_ccdc_archive 'CCDC 976137'