 
data_lava19 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C19 H23 N S2'
_chemical_formula_sum             'C19 H23 N S2' 
_chemical_formula_weight          329.50 
_chemical_compound_source         'Synthesized by the authors. See text'

loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.3331   0.5567 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P21/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
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                    5.48322(9)
_cell_length_b                    41.7378(7)
_cell_length_c                    7.65094(13)
_cell_angle_alpha                 90
_cell_angle_beta                  107.1757(9)
_cell_angle_gamma                 90
_cell_volume                      1672.87(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100
_cell_measurement_reflns_used     12533
_cell_measurement_theta_min        4.24
_cell_measurement_theta_max       70.36
 
_exptl_crystal_description        'Plate'
_exptl_crystal_colour             'Colorless'
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas          ?
_exptl_crystal_density_diffrn     1.308 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              704 
_exptl_absorpt_coefficient_mu     2.830 
_exptl_absorpt_correction_Type    multi-scan
_exptl_absorpt_correction_T_min   0.8190
_exptl_absorpt_correction_T_max   0.9450
_exptl_absorpt_process_details    'Sadabs (Sheldrick, 2008)'
 
_exptl_special_details
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a graphite monochromator. The crystal-to-detector distance was 
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 10.0 degree
scan in 33 frames over four different parts of the reciprocal space
(132 frames total). 


;
 
_diffrn_ambient_temperature       100
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'Incoatec I\muS Microsource '
_diffrn_radiation_monochromator   'Quazar MX'
_diffrn_measurement_device_type   'Bruker APEX II'
_diffrn_measurement_method        'ω'
_diffrn_detector_area_resol_mean   8.3
_diffrn_reflns_number             34518
_diffrn_reflns_av_R_equivalents   0.030
_diffrn_reflns_av_sigmaI/netI     0.0137 
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -50
_diffrn_reflns_limit_k_max        51
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          2.12 
_diffrn_reflns_theta_max          70.84 
_reflns_number_total              3171
_reflns_number_gt                 3016
_reflns_threshold_expression      'I>2σ(I)'
 
_computing_data_collection        'APEX2  (Bruker AXS, 2009)'
_computing_cell_refinement        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_reduction         'SAINT V7.68A(Bruker AXS, 2009)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material   'UdMX (Maris, 2004)'
 
_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)+(0.0344P)²+1.4249P] 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          3171 
_refine_ls_number_parameters      225 
_refine_ls_number_restraints      22 
_refine_ls_R_factor_all           0.0414 
_refine_ls_R_factor_gt            0.0396 
_refine_ls_wR_factor_ref          0.0973 
_refine_ls_wR_factor_gt           0.0965 
_refine_ls_goodness_of_fit_ref    1.185 
_refine_ls_restrained_S_all       1.184 
_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 
S1 S 0.66269(13) 0.028637(14) 0.15356(9) 0.02320(16) Uani 0.9188(14) 1 d PD A 1 
C1 C 0.8814(4) 0.05754(5) 0.2555(3) 0.0229(4) Uani 0.9188(14) 1 d PD A 1 
H1 H 1.0555 0.0537 0.3200 0.027 Uiso 0.9188(14) 1 calc PR A 1 
C2 C 0.7668(4) 0.08689(5) 0.2296(3) 0.0190(4) Uani 0.9188(14) 1 d PD A 1 
C3 C 0.5024(4) 0.08608(5) 0.1274(5) 0.0198(5) Uani 0.9188(14) 1 d PD A 1 
C4 C 0.4181(5) 0.05554(5) 0.0755(5) 0.0229(5) Uani 0.9188(14) 1 d PD A 1 
H4 H 0.2488 0.0501 0.0064 0.027 Uiso 0.9188(14) 1 calc PR A 1 
S2 S 0.85724(10) 0.126176(11) 0.28754(7) 0.02068(16) Uani 0.9188(14) 1 d PD A 1 
N1 N 0.3796(4) 0.11549(4) 0.0977(3) 0.0194(4) Uani 0.9188(14) 1 d PD A 1 
C5 C 0.5366(5) 0.13810(5) 0.1742(3) 0.0171(5) Uani 0.9188(14) 1 d PD A 1 
S21 S 0.7479(16) 0.03475(19) 0.1835(12) 0.02320(16) Uani 0.0812(14) 1 d PD A 2 
C21 C 0.449(4) 0.0493(5) 0.092(8) 0.0229(4) Uani 0.0812(14) 1 d PD A 2 
H21 H 0.3024 0.0369 0.0340 0.027 Uiso 0.0812(14) 1 calc PR A 2 
C22 C 0.454(5) 0.0815(4) 0.115(7) 0.0190(4) Uani 0.0812(14) 1 d PD A 2 
C23 C 0.698(4) 0.0939(4) 0.211(4) 0.0198(5) Uani 0.0812(14) 1 d PD A 2 
C24 C 0.878(4) 0.0707(4) 0.260(4) 0.0229(5) Uani 0.0812(14) 1 d PD A 2 
H24 H 1.0518 0.0742 0.3278 0.027 Uiso 0.0812(14) 1 calc PR A 2 
S22 S 0.2470(14) 0.11391(13) 0.0455(9) 0.02068(16) Uani 0.0812(14) 1 d PD A 2 
N21 N 0.708(4) 0.1274(4) 0.241(2) 0.0194(4) Uani 0.0812(14) 1 d PD A 2 
C25 C 0.514(4) 0.1392(4) 0.125(4) 0.0171(5) Uani 0.0812(14) 1 d PD A 2 
C6 C 0.4720(3) 0.17245(4) 0.1608(2) 0.0198(4) Uani 1 1 d D . . 
C7 C 0.2242(4) 0.18257(5) 0.0679(3) 0.0220(4) Uani 1 1 d . A . 
H7 H 0.0955 0.1672 0.0153 0.026 Uiso 1 1 calc R . . 
C8 C 0.1669(4) 0.21482(5) 0.0527(3) 0.0221(4) Uani 1 1 d . . . 
H8 H -0.0025 0.2213 -0.0101 0.027 Uiso 1 1 calc R A . 
C9 C 0.3510(3) 0.23834(4) 0.1270(3) 0.0197(4) Uani 1 1 d . A . 
C10 C 0.5954(4) 0.22792(4) 0.2204(3) 0.0216(4) Uani 1 1 d . . . 
H10 H 0.7241 0.2433 0.2732 0.026 Uiso 1 1 calc R A . 
C11 C 0.6553(3) 0.19554(4) 0.2382(3) 0.0213(4) Uani 1 1 d . A . 
H11 H 0.8235 0.1891 0.3039 0.026 Uiso 1 1 calc R . . 
C12 C 0.2779(3) 0.27337(4) 0.0989(3) 0.0219(4) Uani 1 1 d . . . 
H12A H 0.1328 0.2772 0.1484 0.026 Uiso 1 1 calc R A . 
H12B H 0.2163 0.2775 -0.0343 0.026 Uiso 1 1 calc R . . 
C13 C 0.4858(4) 0.29783(4) 0.1847(3) 0.0210(4) Uani 1 1 d . A . 
H13A H 0.6360 0.2938 0.1411 0.025 Uiso 1 1 calc R . . 
H13B H 0.5399 0.2953 0.3193 0.025 Uiso 1 1 calc R . . 
C14 C 0.3925(4) 0.33212(4) 0.1362(3) 0.0221(4) Uani 1 1 d . . . 
H14A H 0.3240 0.3339 0.0015 0.026 Uiso 1 1 calc R A . 
H14B H 0.2505 0.3365 0.1882 0.026 Uiso 1 1 calc R . . 
C15 C 0.5973(4) 0.35761(4) 0.2048(3) 0.0221(4) Uani 1 1 d . A . 
H15A H 0.7438 0.3527 0.1585 0.027 Uiso 1 1 calc R . . 
H15B H 0.6587 0.3568 0.3401 0.027 Uiso 1 1 calc R . . 
C16 C 0.5008(4) 0.39131(4) 0.1444(3) 0.0222(4) Uani 1 1 d . . . 
H16A H 0.4328 0.3917 0.0093 0.027 Uiso 1 1 calc R A . 
H16B H 0.3578 0.3963 0.1943 0.027 Uiso 1 1 calc R . . 
C17 C 0.7024(4) 0.41747(4) 0.2045(3) 0.0223(4) Uani 1 1 d . A . 
H17A H 0.8511 0.4119 0.1622 0.027 Uiso 1 1 calc R . . 
H17B H 0.7611 0.4184 0.3398 0.027 Uiso 1 1 calc R . . 
C18 C 0.6018(4) 0.45029(4) 0.1291(3) 0.0226(4) Uani 1 1 d . . . 
H18A H 0.5364 0.4490 -0.0059 0.027 Uiso 1 1 calc R A . 
H18B H 0.4569 0.4561 0.1753 0.027 Uiso 1 1 calc R . . 
C19 C 0.8021(4) 0.47673(5) 0.1810(3) 0.0270(4) Uani 1 1 d . A . 
H19A H 0.8525 0.4801 0.3137 0.041 Uiso 1 1 calc R . . 
H19B H 0.7307 0.4966 0.1187 0.041 Uiso 1 1 calc R . . 
H19C H 0.9519 0.4705 0.1439 0.041 Uiso 1 1 calc R . . 
 
 
_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_site_symmetry_1            
        _geom_bond_site_symmetry_2            
        _geom_bond_distance                   
        _geom_bond_publ_flag                  
S1             C4             .              .                     1.716(2)   y
S1             C1             .              .                     1.717(2)   y
C1             C2             .              .                     1.364(3)   y
C1             H1             .              .                       0.9500   ?
C2             C3             .              .                     1.430(3)   y
C2             S2             .              .                     1.732(2)   y
C3             C4             .              .                     1.374(3)   y
C3             N1             .              .                     1.386(3)   y
C4             H4             .              .                       0.9500   ?
S2             C5             .              .                     1.786(2)   y
N1             C5             .              .                     1.295(3)   y
C5             C6             .              .                     1.473(3)   y
S21            C21            .              .                    1.691(18)   y
S21            C24            .              .                    1.693(16)   y
C21            C22            .              .                    1.358(18)   y
C21            H21            .              .                       0.9500   ?
C22            C23            .              .                    1.418(17)   y
C22            S22            .              .                    1.744(16)   y
C23            C24            .              .                    1.356(17)   y
C23            N21            .              .                    1.415(16)   y
C24            H24            .              .                       0.9500   ?
S22            C25            .              .                    1.763(19)   y
N21            C25            .              .                    1.266(18)   y
C25            C6             .              .                    1.446(16)   y
C6             C11            .              .                     1.392(3)   y
C6             C7             .              .                     1.400(3)   y
C7             C8             .              .                     1.379(3)   y
C7             H7             .              .                       0.9500   ?
C8             C9             .              .                     1.403(3)   y
C8             H8             .              .                       0.9500   ?
C9             C10            .              .                     1.389(3)   y
C9             C12            .              .                     1.514(3)   y
C10            C11            .              .                     1.388(3)   y
C10            H10            .              .                       0.9500   ?
C11            H11            .              .                       0.9500   ?
C12            C13            .              .                     1.527(3)   y
C12            H12a           .              .                       0.9900   ?
C12            H12b           .              .                       0.9900   ?
C13            C14            .              .                     1.528(2)   y
C13            H13a           .              .                       0.9900   ?
C13            H13b           .              .                       0.9900   ?
C14            C15            .              .                     1.523(3)   y
C14            H14a           .              .                       0.9900   ?
C14            H14b           .              .                       0.9900   ?
C15            C16            .              .                     1.526(2)   y
C15            H15a           .              .                       0.9900   ?
C15            H15b           .              .                       0.9900   ?
C16            C17            .              .                     1.525(3)   y
C16            H16a           .              .                       0.9900   ?
C16            H16b           .              .                       0.9900   ?
C17            C18            .              .                     1.525(3)   y
C17            H17a           .              .                       0.9900   ?
C17            H17b           .              .                       0.9900   ?
C18            C19            .              .                     1.525(3)   y
C18            H18a           .              .                       0.9900   ?
C18            H18b           .              .                       0.9900   ?
C19            H19a           .              .                       0.9800   ?
C19            H19b           .              .                       0.9800   ?
C19            H19c           .              .                       0.9800   ?

loop_                                         
        _geom_angle_atom_site_label_1         
        _geom_angle_atom_site_label_2         
        _geom_angle_atom_site_label_3         
        _geom_angle_site_symmetry_1           
        _geom_angle_site_symmetry_2           
        _geom_angle_site_symmetry_3           
        _geom_angle                           
        _geom_angle_publ_flag                 
C4        S1        C1        .         .         .          93.88(11)        y
C2        C1        S1        .         .         .         109.57(17)        y
C2        C1        H1        .         .         .              125.2        ?
S1        C1        H1        .         .         .              125.2        ?
C1        C2        C3        .         .         .           114.0(2)        y
C1        C2        S2        .         .         .         136.72(18)        y
C3        C2        S2        .         .         .         109.25(17)        y
C4        C3        N1        .         .         .           131.9(2)        y
C4        C3        C2        .         .         .           112.4(2)        y
N1        C3        C2        .         .         .         115.71(19)        y
C3        C4        S1        .         .         .         110.17(18)        y
C3        C4        H4        .         .         .              124.9        ?
S1        C4        H4        .         .         .              124.9        ?
C2        S2        C5        .         .         .          88.46(10)        y
C5        N1        C3        .         .         .           110.2(2)        y
N1        C5        C6        .         .         .           124.3(2)        y
N1        C5        S2        .         .         .         116.38(16)        y
C6        C5        S2        .         .         .         119.13(16)        y
C21       S21       C24       .         .         .           94.8(10)        y
C22       C21       S21       .         .         .          108.8(15)        y
C22       C21       H21       .         .         .              125.6        ?
S21       C21       H21       .         .         .              125.6        ?
C21       C22       C23       .         .         .          114.0(15)        y
C21       C22       S22       .         .         .          138.0(17)        y
C23       C22       S22       .         .         .          107.7(13)        y
C24       C23       N21       .         .         .          131.9(18)        y
C24       C23       C22       .         .         .          112.6(15)        y
N21       C23       C22       .         .         .          115.5(16)        y
C23       C24       S21       .         .         .          109.7(14)        y
C23       C24       H24       .         .         .              125.1        ?
S21       C24       H24       .         .         .              125.1        ?
C22       S22       C25       .         .         .           87.6(10)        y
C25       N21       C23       .         .         .          106.6(15)        y
N21       C25       C6        .         .         .          113.0(16)        y
N21       C25       S22       .         .         .          116.6(15)        y
C6        C25       S22       .         .         .          118.4(15)        y
C11       C6        C7        .         .         .         118.51(17)        y
C11       C6        C25       .         .         .           127.5(9)        y
C7        C6        C25       .         .         .           112.3(9)        y
C11       C6        C5        .         .         .         121.06(18)        y
C7        C6        C5        .         .         .         120.43(18)        y
C8        C7        C6        .         .         .         120.03(17)        y
C8        C7        H7        .         .         .              120.0        ?
C6        C7        H7        .         .         .              120.0        ?
C7        C8        C9        .         .         .         121.99(17)        y
C7        C8        H8        .         .         .              119.0        ?
C9        C8        H8        .         .         .              119.0        ?
C10       C9        C8        .         .         .         117.33(17)        y
C10       C9        C12       .         .         .         123.37(17)        y
C8        C9        C12       .         .         .         119.29(17)        y
C11       C10       C9        .         .         .         121.31(17)        y
C11       C10       H10       .         .         .              119.3        ?
C9        C10       H10       .         .         .              119.3        ?
C10       C11       C6        .         .         .         120.82(17)        y
C10       C11       H11       .         .         .              119.6        ?
C6        C11       H11       .         .         .              119.6        ?
C9        C12       C13       .         .         .         116.87(15)        y
C9        C12       H12A      .         .         .              108.1        ?
C13       C12       H12A      .         .         .              108.1        ?
C9        C12       H12B      .         .         .              108.1        ?
C13       C12       H12B      .         .         .              108.1        ?
H12A      C12       H12B      .         .         .              107.3        ?
C12       C13       C14       .         .         .         111.60(15)        y
C12       C13       H13A      .         .         .              109.3        ?
C14       C13       H13A      .         .         .              109.3        ?
C12       C13       H13B      .         .         .              109.3        ?
C14       C13       H13B      .         .         .              109.3        ?
H13A      C13       H13B      .         .         .              108.0        ?
C15       C14       C13       .         .         .         114.24(15)        y
C15       C14       H14A      .         .         .              108.7        ?
C13       C14       H14A      .         .         .              108.7        ?
C15       C14       H14B      .         .         .              108.7        ?
C13       C14       H14B      .         .         .              108.7        ?
H14A      C14       H14B      .         .         .              107.6        ?
C14       C15       C16       .         .         .         112.66(15)        y
C14       C15       H15A      .         .         .              109.1        ?
C16       C15       H15A      .         .         .              109.1        ?
C14       C15       H15B      .         .         .              109.1        ?
C16       C15       H15B      .         .         .              109.1        ?
H15A      C15       H15B      .         .         .              107.8        ?
C17       C16       C15       .         .         .         114.40(16)        y
C17       C16       H16A      .         .         .              108.7        ?
C15       C16       H16A      .         .         .              108.7        ?
C17       C16       H16B      .         .         .              108.7        ?
C15       C16       H16B      .         .         .              108.7        ?
H16A      C16       H16B      .         .         .              107.6        ?
C16       C17       C18       .         .         .         112.35(15)        y
C16       C17       H17A      .         .         .              109.1        ?
C18       C17       H17A      .         .         .              109.1        ?
C16       C17       H17B      .         .         .              109.1        ?
C18       C17       H17B      .         .         .              109.1        ?
H17A      C17       H17B      .         .         .              107.9        ?
C19       C18       C17       .         .         .         113.55(16)        y
C19       C18       H18A      .         .         .              108.9        ?
C17       C18       H18A      .         .         .              108.9        ?
C19       C18       H18B      .         .         .              108.9        ?
C17       C18       H18B      .         .         .              108.9        ?
H18A      C18       H18B      .         .         .              107.7        ?
C18       C19       H19A      .         .         .              109.5        ?
C18       C19       H19B      .         .         .              109.5        ?
H19A      C19       H19B      .         .         .              109.5        ?
C18       C19       H19C      .         .         .              109.5        ?
H19A      C19       H19C      .         .         .              109.5        ?
H19B      C19       H19C      .         .         .              109.5        ?

loop_                                         
        _geom_torsion_atom_site_label_1       
        _geom_torsion_atom_site_label_2       
        _geom_torsion_atom_site_label_3       
        _geom_torsion_atom_site_label_4       
        _geom_torsion_site_symmetry_1         
        _geom_torsion_site_symmetry_2         
        _geom_torsion_site_symmetry_3         
        _geom_torsion_site_symmetry_4         
        _geom_torsion                         
        _geom_torsion_publ_flag               
C4      S1      C1      C2      .       .       .       .            0.2(2)   y
S1      C1      C2      C3      .       .       .       .           -0.1(3)   y
S1      C1      C2      S2      .       .       .       .       -179.57(19)   y
C1      C2      C3      C4      .       .       .       .           -0.1(4)   y
S2      C2      C3      C4      .       .       .       .          179.5(3)   y
C1      C2      C3      N1      .       .       .       .         -179.8(3)   y
S2      C2      C3      N1      .       .       .       .           -0.1(4)   y
N1      C3      C4      S1      .       .       .       .          179.8(3)   y
C2      C3      C4      S1      .       .       .       .            0.3(4)   y
C1      S1      C4      C3      .       .       .       .           -0.3(3)   y
C1      C2      S2      C5      .       .       .       .         -179.7(3)   y
C3      C2      S2      C5      .       .       .       .            0.7(2)   y
C4      C3      N1      C5      .       .       .       .          179.6(4)   y
C2      C3      N1      C5      .       .       .       .           -0.8(4)   y
C3      N1      C5      C6      .       .       .       .          176.6(2)   y
C3      N1      C5      S2      .       .       .       .            1.4(3)   y
C2      S2      C5      N1      .       .       .       .         -1.32(17)   y
C2      S2      C5      C6      .       .       .       .       -176.74(17)   y
C24     S21     C21     C22     .       .       .       .              2(5)   y
S21     C21     C22     C23     .       .       .       .             -2(7)   y
S21     C21     C22     S22     .       .       .       .            172(5)   y
C21     C22     C23     C24     .       .       .       .              0(7)   y
S22     C22     C23     C24     .       .       .       .           -176(3)   y
C21     C22     C23     N21     .       .       .       .           -179(4)   y
S22     C22     C23     N21     .       .       .       .              6(5)   y
N21     C23     C24     S21     .       .       .       .            180(3)   y
C22     C23     C24     S21     .       .       .       .              2(5)   y
C21     S21     C24     C23     .       .       .       .             -2(3)   y
C21     C22     S22     C25     .       .       .       .           -167(7)   y
C23     C22     S22     C25     .       .       .       .              7(4)   y
C24     C23     N21     C25     .       .       .       .            161(4)   y
C22     C23     N21     C25     .       .       .       .            -21(4)   y
C23     N21     C25     C6      .       .       .       .            169(2)   y
C23     N21     C25     S22     .       .       .       .             27(3)   y
C22     S22     C25     N21     .       .       .       .            -21(3)   y
C22     S22     C25     C6      .       .       .       .           -161(3)   y
N21     C25     C6      C11     .       .       .       .             33(3)   y
S22     C25     C6      C11     .       .       .       .          174.1(9)   y
N21     C25     C6      C7      .       .       .       .        -162.6(19)   y
S22     C25     C6      C7      .       .       .       .            -21(2)   y
N21     C25     C6      C5      .       .       .       .            -35(3)   y
S22     C25     C6      C5      .       .       .       .            107(6)   y
N1      C5      C6      C11     .       .       .       .       -176.33(19)   y
S2      C5      C6      C11     .       .       .       .           -1.3(2)   y
N1      C5      C6      C7      .       .       .       .            3.0(3)   y
S2      C5      C6      C7      .       .       .       .        178.03(14)   y
N1      C5      C6      C25     .       .       .       .            -55(4)   y
S2      C5      C6      C25     .       .       .       .            120(5)   y
C11     C6      C7      C8      .       .       .       .            0.8(3)   y
C25     C6      C7      C8      .       .       .       .        -165.6(14)   y
C5      C6      C7      C8      .       .       .       .       -178.58(18)   y
C6      C7      C8      C9      .       .       .       .            0.4(3)   y
C7      C8      C9      C10     .       .       .       .           -1.0(3)   y
C7      C8      C9      C12     .       .       .       .        177.60(17)   y
C8      C9      C10     C11     .       .       .       .            0.5(3)   y
C12     C9      C10     C11     .       .       .       .       -178.10(18)   y
C9      C10     C11     C6      .       .       .       .            0.7(3)   y
C7      C6      C11     C10     .       .       .       .           -1.3(3)   y
C25     C6      C11     C10     .       .       .       .         162.7(16)   y
C5      C6      C11     C10     .       .       .       .        178.02(18)   y
C10     C9      C12     C13     .       .       .       .           -2.0(3)   y
C8      C9      C12     C13     .       .       .       .        179.43(16)   y
C9      C12     C13     C14     .       .       .       .        176.39(15)   y
C12     C13     C14     C15     .       .       .       .       -175.36(15)   y
C13     C14     C15     C16     .       .       .       .        176.72(15)   y
C14     C15     C16     C17     .       .       .       .       -177.93(16)   y
C15     C16     C17     C18     .       .       .       .        175.81(16)   y
C16     C17     C18     C19     .       .       .       .       -177.82(16)   y



_diffrn_measured_fraction_theta_max    0.985 
_diffrn_reflns_theta_full              70.84 
_diffrn_measured_fraction_theta_full   0.985 
_refine_diff_density_max               0.314
_refine_diff_density_min              -0.230
_refine_diff_density_rms               0.050
_iucr_refine_instructions
;
TITL lava19 in P2(1)/c
CELL 1.54178   5.4832  41.7378   7.6509  90.000 107.176  90.000
ZERR    4.00   0.0001   0.0007   0.0001   0.000   0.001   0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C  H  N  S
UNIT 76  92  4  8
 
SIZE  0.02  0.06  0.1
TEMP -173
 
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN -5
WPDB -1
CONF
WGHT    0.034400    1.424900
FVAR       0.17290   0.91879
PART 1
EADP S1 S21
EADP S2 S22
EADP C1 C21
EADP C2 C22
EADP C3 C23
EADP C4 C24
EADP N1 N21
EADP C5 C25
 
S1    4    0.662691    0.028637    0.153555    21.00000    0.02376    0.01830 =
         0.02766   -0.00333    0.00779   -0.00168
C1    1    0.881386    0.057537    0.255502    21.00000    0.02226    0.02101 =
         0.02632    0.00011    0.00858    0.00103
AFIX  43
H1    2    1.055479    0.053679    0.320012    21.00000   -1.20000
AFIX   0
C2    1    0.766771    0.086890    0.229645    21.00000    0.01710    0.02236 =
         0.01878    0.00043    0.00712   -0.00080
C3    1    0.502433    0.086080    0.127382    21.00000    0.01996    0.02178 =
         0.02036    0.00080    0.01008   -0.00142
C4    1    0.418095    0.055539    0.075498    21.00000    0.02116    0.02305 =
         0.02369   -0.00096    0.00548   -0.00190
AFIX  43
H4    2    0.248831    0.050106    0.006401    21.00000   -1.20000
AFIX   0
S2    4    0.857238    0.126176    0.287541    21.00000    0.01638    0.01870 =
         0.02458   -0.00003    0.00236   -0.00105
N1    3    0.379565    0.115488    0.097723    21.00000    0.01632    0.02266 =
         0.01815   -0.00103    0.00345   -0.00089
C5    1    0.536615    0.138098    0.174154    21.00000    0.01812    0.02342 =
         0.01027    0.00108    0.00495   -0.00107
SAME  .02 S1 > C5
SADI  .02 C5 C6 C25 C6
PART 2
S21   4    0.747869    0.034749    0.183533   -21.00000    0.02376    0.01830 =
         0.02766   -0.00333    0.00779   -0.00168
C21   1    0.449295    0.049251    0.092126   -21.00000    0.02226    0.02101 =
         0.02632    0.00011    0.00858    0.00103
AFIX  43
H21   2    0.302419    0.036852    0.034041   -21.00000   -1.20000
AFIX   0
C22   1    0.453876    0.081533    0.115363   -21.00000    0.01710    0.02236 =
         0.01878    0.00043    0.00712   -0.00080
C23   1    0.697662    0.093908    0.210928   -21.00000    0.01996    0.02178 =
         0.02036    0.00080    0.01008   -0.00142
C24   1    0.878309    0.070739    0.260304   -21.00000    0.02116    0.02305 =
         0.02369   -0.00096    0.00548   -0.00190
AFIX  43
H24   2    1.051849    0.074183    0.327782   -21.00000   -1.20000
AFIX   0
S22   4    0.247008    0.113910    0.045493   -21.00000    0.01638    0.01870 =
         0.02458   -0.00003    0.00236   -0.00105
N21   3    0.707924    0.127378    0.241331   -21.00000    0.01632    0.02266 =
         0.01815   -0.00103    0.00345   -0.00089
C25   1    0.514459    0.139213    0.125226   -21.00000    0.01812    0.02342 =
         0.01027    0.00108    0.00495   -0.00107
PART 0
C6    1    0.472027    0.172446    0.160818    11.00000    0.02105    0.02171 =
         0.01857    0.00011    0.00875   -0.00124
C7    1    0.224212    0.182575    0.067897    11.00000    0.01896    0.02608 =
         0.02079    0.00092    0.00564   -0.00506
AFIX  43
H7    2    0.095490    0.167230    0.015316    11.00000   -1.20000
AFIX   0
C8    1    0.166864    0.214824    0.052657    11.00000    0.01663    0.02929 =
         0.02043    0.00343    0.00538    0.00011
AFIX  43
H8    2   -0.002472    0.221304   -0.010103    11.00000   -1.20000
AFIX   0
C9    1    0.351043    0.238342    0.127036    11.00000    0.01997    0.02337 =
         0.01772    0.00081    0.00839    0.00137
C10   1    0.595404    0.227923    0.220420    11.00000    0.01961    0.02156 =
         0.02191   -0.00253    0.00351   -0.00192
AFIX  43
H10   2    0.724078    0.243264    0.273182    11.00000   -1.20000
AFIX   0
C11   1    0.655302    0.195543    0.238172    11.00000    0.01685    0.02403 =
         0.02092   -0.00178    0.00224    0.00084
AFIX  43
H11   2    0.823460    0.189060    0.303926    11.00000   -1.20000
AFIX   0
C12   1    0.277926    0.273368    0.098933    11.00000    0.01943    0.02526 =
         0.02050    0.00080    0.00500    0.00351
AFIX  23
H12A  2    0.132802    0.277192    0.148434    11.00000   -1.20000
H12B  2    0.216255    0.277508   -0.034328    11.00000   -1.20000
AFIX   0
C13   1    0.485816    0.297834    0.184664    11.00000    0.02054    0.02241 =
         0.02059    0.00200    0.00698    0.00285
AFIX  23
H13A  2    0.635983    0.293775    0.141072    11.00000   -1.20000
H13B  2    0.539933    0.295252    0.319292    11.00000   -1.20000
AFIX   0
C14   1    0.392514    0.332117    0.136164    11.00000    0.02130    0.02272 =
         0.02325    0.00307    0.00828    0.00388
AFIX  23
H14A  2    0.323989    0.333911    0.001470    11.00000   -1.20000
H14B  2    0.250536    0.336461    0.188160    11.00000   -1.20000
AFIX   0
C15   1    0.597264    0.357606    0.204798    11.00000    0.02145    0.02365 =
         0.02193    0.00312    0.00754    0.00339
AFIX  23
H15A  2    0.743773    0.352733    0.158516    11.00000   -1.20000
H15B  2    0.658677    0.356845    0.340099    11.00000   -1.20000
AFIX   0
C16   1    0.500776    0.391313    0.144427    11.00000    0.01999    0.02332 =
         0.02300    0.00100    0.00583    0.00152
AFIX  23
H16A  2    0.432780    0.391669    0.009321    11.00000   -1.20000
H16B  2    0.357782    0.396286    0.194295    11.00000   -1.20000
AFIX   0
C17   1    0.702370    0.417467    0.204493    11.00000    0.02128    0.02349 =
         0.02214    0.00146    0.00621    0.00163
AFIX  23
H17A  2    0.851147    0.411910    0.162175    11.00000   -1.20000
H17B  2    0.761090    0.418448    0.339795    11.00000   -1.20000
AFIX   0
C18   1    0.601798    0.450289    0.129145    11.00000    0.02124    0.02345 =
         0.02310    0.00016    0.00655    0.00048
AFIX  23
H18A  2    0.536403    0.448958   -0.005880    11.00000   -1.20000
H18B  2    0.456858    0.456076    0.175266    11.00000   -1.20000
AFIX   0
C19   1    0.802140    0.476733    0.180988    11.00000    0.02565    0.02451 =
         0.03065    0.00028    0.00792   -0.00119
AFIX 137
H19A  2    0.852530    0.480067    0.313659    11.00000   -1.50000
H19B  2    0.730716    0.496636    0.118689    11.00000   -1.50000
H19C  2    0.951939    0.470491    0.143937    11.00000   -1.50000
HKLF 4
 
REM  lava19 in P2(1)/c
REM R1 =  0.0396 for   3016 Fo > 4sig(Fo)  and  0.0414 for all   3171 data
REM    225 parameters refined using     22 restraints
 
END  
     
WGHT      0.0323      1.4403 
REM Highest difference peak  0.314,  deepest hole -0.230,  1-sigma level  0.050
Q1    1   0.8439  0.1045  0.2620  11.00000  0.05    0.31
Q2    1   0.6495  0.4328  0.1566  11.00000  0.05    0.31
Q3    1   0.6485  0.0881  0.1623  11.00000  0.05    0.31
Q4    1   0.8771  0.1286  0.1576  11.00000  0.05    0.28
Q5    1   0.3467  0.1776  0.1368  11.00000  0.05    0.27
;
