 
data_2007jmw0002

#twin data
#180 deg rotation about -2 0 -1 axis
#hklf5 file format does not allow for proper merging of data
#hence completeness is overestimated and figures for observed
#and unique data are wrong  

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 2,3-Dihydrothieno[3,4-B][1,4]dioxine-5-carbaldehyde
;
_chemical_name_common             ?
_chemical_melting_point           '138 - 140'
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C7 H6 O3 S'
_chemical_formula_weight          170.18
 
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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(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                    10.0118(8)
_cell_length_b                    4.3353(3)
_cell_length_c                    16.6170(14)
_cell_angle_alpha                 90.00
_cell_angle_beta                  106.290(2)
_cell_angle_gamma                 90.00
_cell_volume                      692.29(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     1605
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        lath
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.633
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              352
_exptl_absorpt_coefficient_mu     0.412
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9039
_exptl_absorpt_correction_T_max   0.9959
_exptl_absorpt_process_details    
'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_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 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             4406
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0667
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -5
_diffrn_reflns_limit_k_max        5
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          3.75
_diffrn_reflns_theta_max          25.00
_reflns_number_total              4407
_reflns_number_gt                 3616
_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     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_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 > 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)+(0.0578P)²+3.0732P] 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      SHELXL
_refine_ls_extinction_coef        0.024(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4407
_refine_ls_number_parameters      102
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0913
_refine_ls_R_factor_gt            0.0727
_refine_ls_wR_factor_ref          0.1854
_refine_ls_wR_factor_gt           0.1614
_refine_ls_goodness_of_fit_ref    1.094
_refine_ls_restrained_S_all       1.094
_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 0.2263(3) 0.8896(7) 0.25538(17) 0.0219(7) Uani 1 1 d . . .
C2 C 0.2279(3) 0.9268(7) 0.33793(17) 0.0191(7) Uani 1 1 d . . .
C3 C 0.1391(3) 1.0354(7) 0.45091(17) 0.0238(7) Uani 1 1 d . . .
H3A H 0.0912 0.8381 0.4543 0.029 Uiso 1 1 calc R . .
H3B H 0.0897 1.2014 0.4719 0.029 Uiso 1 1 calc R . .
C4 C 0.2868(3) 1.0178(7) 0.50455(18) 0.0256(8) Uani 1 1 d . . .
H4A H 0.3345 1.2147 0.5005 0.031 Uiso 1 1 calc R . .
H4B H 0.2877 0.9882 0.5638 0.031 Uiso 1 1 calc R . .
C5 C 0.3388(3) 0.7652(7) 0.39396(16) 0.0206(7) Uani 1 1 d . . .
C6 C 0.4197(3) 0.6086(7) 0.35371(18) 0.0238(7) Uani 1 1 d . . .
H6 H 0.4984 0.4880 0.3814 0.029 Uiso 1 1 calc R . .
C7 C 0.1317(3) 1.0287(8) 0.18282(18) 0.0267(8) Uani 1 1 d . . .
H7 H 0.0595 1.1555 0.1913 0.032 Uiso 1 1 calc R . .
O1 O 0.1343(2) 1.0977(5) 0.36360(12) 0.0231(5) Uani 1 1 d . . .
O2 O 0.3616(2) 0.7660(5) 0.47910(11) 0.0234(5) Uani 1 1 d . . .
O3 O 0.1385(2) 0.9942(5) 0.11087(12) 0.0303(6) Uani 1 1 d . . .
S1 S 0.36147(8) 0.65683(18) 0.24693(4) 0.0229(3) Uani 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
C1 0.0221(17) 0.0282(18) 0.0137(15) -0.0010(13) 0.0022(12) -0.0016(14)
C2 0.0186(17) 0.0218(16) 0.0160(15) -0.0016(13) 0.0035(12) -0.0059(13)
C3 0.0259(18) 0.0357(19) 0.0096(15) -0.0010(13) 0.0046(12) -0.0034(15)
C4 0.0317(19) 0.0287(19) 0.0139(15) -0.0025(13) 0.0023(13) -0.0007(15)
C5 0.0212(16) 0.0264(17) 0.0101(13) 0.0023(13) -0.0024(11) -0.0051(14)
C6 0.0202(17) 0.0288(18) 0.0192(16) 0.0026(13) 0.0006(13) 0.0020(14)
C7 0.0229(18) 0.039(2) 0.0163(17) -0.0008(14) 0.0025(12) -0.0031(15)
O1 0.0225(12) 0.0331(13) 0.0131(10) 0.0017(9) 0.0040(8) 0.0035(10)
O2 0.0282(12) 0.0280(12) 0.0125(10) 0.0030(9) 0.0030(8) 0.0041(10)
O3 0.0359(14) 0.0404(15) 0.0114(11) 0.0013(10) 0.0014(9) -0.0024(11)
S1 0.0221(5) 0.0328(5) 0.0129(4) -0.0009(3) 0.0032(3) -0.0003(3)
 
_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 C2 1.377(4) . ?
C1 C7 1.440(4) . ?
C1 S1 1.725(3) . ?
C2 O1 1.354(3) . ?
C2 C5 1.418(4) . ?
C3 O1 1.463(3) . ?
C3 C4 1.499(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O2 1.452(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.367(4) . ?
C5 O2 1.368(3) . ?
C6 S1 1.718(3) . ?
C6 H6 0.9500 . ?
C7 O3 1.225(4) . ?
C7 H7 0.9500 . ?
 
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
C2 C1 C7 127.3(3) . . ?
C2 C1 S1 111.1(2) . . ?
C7 C1 S1 121.5(2) . . ?
O1 C2 C1 124.2(3) . . ?
O1 C2 C5 123.2(2) . . ?
C1 C2 C5 112.6(3) . . ?
O1 C3 C4 110.6(2) . . ?
O1 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
O1 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
O2 C4 C3 111.6(2) . . ?
O2 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
O2 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C6 C5 O2 123.9(2) . . ?
C6 C5 C2 112.7(2) . . ?
O2 C5 C2 123.4(3) . . ?
C5 C6 S1 111.6(2) . . ?
C5 C6 H6 124.2 . . ?
S1 C6 H6 124.2 . . ?
O3 C7 C1 124.2(3) . . ?
O3 C7 H7 117.9 . . ?
C1 C7 H7 117.9 . . ?
C2 O1 C3 112.2(2) . . ?
C5 O2 C4 110.6(2) . . ?
C6 S1 C1 91.94(14) . . ?
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    0.525
_refine_diff_density_min   -1.033
_refine_diff_density_rms    0.121
