 
data_Br_293K 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C3 Cd N3 S3, C7 H17 Br N' 
_chemical_formula_sum 
 'C10 H17 Br Cd N4 S3' 
_chemical_formula_weight          481.77 
 
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' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cd'  'Cd'  -0.8075   1.2024 
 '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 b c a' 
_symmetry_space_group_name_HALL   '-P 2ac 2ab' 
 
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                    18.702(2) 
_cell_length_b                    17.0024(18) 
_cell_length_c                    10.8512(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3450.5(6) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     2153 
_cell_measurement_theta_min       2.18 
_cell_measurement_theta_max       25.00 
 
_exptl_crystal_description        columnar 
_exptl_crystal_colour             colorless  
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.855 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1888 
_exptl_absorpt_coefficient_mu     3.937 
_exptl_absorpt_correction_type    'Multi-scan'  
_exptl_absorpt_correction_T_min   0.5065 
_exptl_absorpt_correction_T_max   0.5065 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             17800 
_diffrn_reflns_av_R_equivalents   0.0444 
_diffrn_reflns_av_sigmaI/netI     0.0367 
_diffrn_reflns_limit_h_min        -22 
_diffrn_reflns_limit_h_max        21 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.18 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3034 
_reflns_number_gt                 2153 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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)+(0.0814P)²+18.9787P] where P=(Fo²+2Fc²)/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_number_reflns          3022 
_refine_ls_number_parameters      160 
_refine_ls_number_restraints      108 
_refine_ls_R_factor_all           0.1010 
_refine_ls_R_factor_gt            0.0698 
_refine_ls_wR_factor_ref          0.1793 
_refine_ls_wR_factor_gt           0.1638 
_refine_ls_goodness_of_fit_ref    1.044 
_refine_ls_restrained_S_all       1.042 
_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 
C9 C 0.3768(4) 0.1325(4) 0.2923(6) 0.0553(18) Uani 1 1 d U . . 
S3 S 0.49393(11) 0.17699(14) -0.09225(16) 0.0786(6) Uani 1 1 d U . . 
Cd1 Cd 0.37585(3) 0.23759(3) 0.02418(4) 0.05607(16) Uani 1 1 d U . . 
S1 S 0.36857(15) 0.09840(13) 0.15159(19) 0.0887(8) Uani 1 1 d U . . 
N4 N 0.3832(3) 0.1529(4) 0.3940(5) 0.0723(19) Uani 1 1 d U . . 
C8 C 0.4672(3) 0.1960(4) -0.2328(6) 0.0519(18) Uani 1 1 d U . . 
N2 N 0.4486(3) 0.2922(4) 0.1683(5) 0.0655(16) Uani 1 1 d U . . 
S2 S 0.25588(12) 0.29732(16) 0.13225(18) 0.0843(7) Uani 1 1 d U . . 
C10 C 0.2840(3) 0.3071(4) 0.2726(6) 0.0541(18) Uani 1 1 d U . . 
N3 N 0.2981(3) 0.1820(4) -0.1233(5) 0.0718(18) Uani 1 1 d U . . 
N1 N 0.6156(7) 0.0598(6) 0.2943(11) 0.167(3) Uani 1 1 d U . . 
C4 C 0.6331(7) 0.1741(7) 0.1609(13) 0.171(5) Uani 1 1 d U . . 
H4A H 0.6111 0.2036 0.2261 0.256 Uiso 1 1 calc R . . 
H4B H 0.5984 0.1636 0.0978 0.256 Uiso 1 1 calc R . . 
H4C H 0.6719 0.2039 0.1266 0.256 Uiso 1 1 calc R . . 
C6 C 0.5770(10) 0.1022(9) 0.3810(13) 0.191(4) Uani 1 1 d U . . 
H6A H 0.5379 0.0689 0.4079 0.229 Uiso 1 1 calc R . . 
H6B H 0.5557 0.1465 0.3383 0.229 Uiso 1 1 calc R . . 
C7 C 0.6117(8) 0.1336(8) 0.4933(12) 0.167(3) Uani 1 1 d U . . 
H7A H 0.5885 0.1832 0.5116 0.201 Uiso 1 1 calc R . . 
H7B H 0.6607 0.1459 0.4710 0.201 Uiso 1 1 calc R . . 
Br1 Br 0.61568(6) 0.07865(8) 0.63808(12) 0.1210(4) Uani 1 1 d U . . 
C3 C 0.6606(9) 0.0991(7) 0.2102(12) 0.147(4) Uani 1 1 d U . . 
H3A H 0.7012 0.1154 0.2613 0.176 Uiso 1 1 calc R . . 
C5 C 0.6951(9) 0.0522(9) 0.1100(15) 0.210(6) Uani 1 1 d U . . 
H5A H 0.7130 0.0038 0.1433 0.315 Uiso 1 1 calc R . . 
H5B H 0.7339 0.0818 0.0751 0.315 Uiso 1 1 calc R . . 
H5C H 0.6605 0.0410 0.0470 0.315 Uiso 1 1 calc R . . 
C1 C 0.6473(8) -0.0097(7) 0.3483(12) 0.167(3) Uani 1 1 d U . . 
H1A H 0.6809 0.0056 0.4108 0.251 Uiso 1 1 calc R . . 
H1B H 0.6716 -0.0392 0.2856 0.251 Uiso 1 1 calc R . . 
H1C H 0.6106 -0.0416 0.3845 0.251 Uiso 1 1 calc R . . 
C2 C 0.5642(9) 0.0207(11) 0.1977(17) 0.245(6) Uani 1 1 d U . . 
H2A H 0.5390 0.0610 0.1533 0.368 Uiso 1 1 calc R . . 
H2B H 0.5304 -0.0123 0.2398 0.368 Uiso 1 1 calc R . . 
H2C H 0.5916 -0.0104 0.1411 0.368 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_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
C9 N4 1.163(9) . ? 
C9 S1 1.640(7) . ? 
S3 C8 1.637(7) . ? 
S3 Cd1 2.745(2) . ? 
Cd1 N2 2.272(6) . ? 
Cd1 N4 2.341(6) 7_565 ? 
Cd1 N3 2.360(6) . ? 
Cd1 S2 2.728(2) . ? 
Cd1 S1 2.744(2) . ? 
N4 Cd1 2.341(6) 7_566 ? 
C8 N2 1.146(8) 7_565 ? 
N2 C8 1.146(8) 7_566 ? 
S2 C10 1.620(7) . ? 
C10 N3 1.175(8) 7_566 ? 
N3 C10 1.175(8) 7_565 ? 
N1 C6 1.388(17) . ? 
N1 C3 1.410(18) . ? 
N1 C1 1.447(16) . ? 
N1 C2 1.570(19) . ? 
C4 C3 1.476(16) . ? 
C4 H4A 0.9600 . ? 
C4 H4B 0.9600 . ? 
C4 H4C 0.9600 . ? 
C6 C7 1.480(19) . ? 
C6 H6A 0.9700 . ? 
C6 H6B 0.9700 . ? 
C7 Br1 1.829(13) . ? 
C7 H7A 0.9700 . ? 
C7 H7B 0.9700 . ? 
C3 C5 1.494(18) . ? 
C3 H3A 0.9800 . ? 
C5 H5A 0.9600 . ? 
C5 H5B 0.9600 . ? 
C5 H5C 0.9600 . ? 
C1 H1A 0.9600 . ? 
C1 H1B 0.9600 . ? 
C1 H1C 0.9600 . ? 
C2 H2A 0.9600 . ? 
C2 H2B 0.9600 . ? 
C2 H2C 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 
N4 C9 S1 176.6(6) . . ? 
C8 S3 Cd1 96.3(2) . . ? 
N2 Cd1 N4 93.1(2) . 7_565 ? 
N2 Cd1 N3 178.8(2) . . ? 
N4 Cd1 N3 86.9(2) 7_565 . ? 
N2 Cd1 S2 92.56(16) . . ? 
N4 Cd1 S2 90.68(16) 7_565 . ? 
N3 Cd1 S2 86.20(16) . . ? 
N2 Cd1 S1 92.05(16) . . ? 
N4 Cd1 S1 173.09(16) 7_565 . ? 
N3 Cd1 S1 88.03(17) . . ? 
S2 Cd1 S1 93.65(8) . . ? 
N2 Cd1 S3 89.33(16) . . ? 
N4 Cd1 S3 88.47(16) 7_565 . ? 
N3 Cd1 S3 91.92(16) . . ? 
S2 Cd1 S3 177.97(6) . . ? 
S1 Cd1 S3 87.03(7) . . ? 
C9 S1 Cd1 99.1(2) . . ? 
C9 N4 Cd1 143.5(6) . 7_566 ? 
N2 C8 S3 178.7(7) 7_565 . ? 
C8 N2 Cd1 153.9(5) 7_566 . ? 
C10 S2 Cd1 100.1(3) . . ? 
N3 C10 S2 173.4(6) 7_566 . ? 
C10 N3 Cd1 136.7(6) 7_565 . ? 
C6 N1 C3 120.2(11) . . ? 
C6 N1 C1 111.3(12) . . ? 
C3 N1 C1 113.8(12) . . ? 
C6 N1 C2 110.7(14) . . ? 
C3 N1 C2 97.7(12) . . ? 
C1 N1 C2 100.2(11) . . ? 
C3 C4 H4A 109.5 . . ? 
C3 C4 H4B 109.5 . . ? 
H4A C4 H4B 109.5 . . ? 
C3 C4 H4C 109.5 . . ? 
H4A C4 H4C 109.5 . . ? 
H4B C4 H4C 109.5 . . ? 
N1 C6 C7 121.1(15) . . ? 
N1 C6 H6A 107.0 . . ? 
C7 C6 H6A 107.0 . . ? 
N1 C6 H6B 107.0 . . ? 
C7 C6 H6B 107.0 . . ? 
H6A C6 H6B 106.8 . . ? 
C6 C7 Br1 122.8(11) . . ? 
C6 C7 H7A 106.6 . . ? 
Br1 C7 H7A 106.6 . . ? 
C6 C7 H7B 106.6 . . ? 
Br1 C7 H7B 106.6 . . ? 
H7A C7 H7B 106.6 . . ? 
N1 C3 C4 115.8(13) . . ? 
N1 C3 C5 118.5(11) . . ? 
C4 C3 C5 110.3(12) . . ? 
N1 C3 H3A 103.3 . . ? 
C4 C3 H3A 103.3 . . ? 
C5 C3 H3A 103.3 . . ? 
C3 C5 H5A 109.5 . . ? 
C3 C5 H5B 109.5 . . ? 
H5A C5 H5B 109.5 . . ? 
C3 C5 H5C 109.5 . . ? 
H5A C5 H5C 109.5 . . ? 
H5B C5 H5C 109.5 . . ? 
N1 C1 H1A 109.5 . . ? 
N1 C1 H1B 109.5 . . ? 
H1A C1 H1B 109.5 . . ? 
N1 C1 H1C 109.5 . . ? 
H1A C1 H1C 109.5 . . ? 
H1B C1 H1C 109.5 . . ? 
N1 C2 H2A 109.5 . . ? 
N1 C2 H2B 109.5 . . ? 
H2A C2 H2B 109.5 . . ? 
N1 C2 H2C 109.5 . . ? 
H2A C2 H2C 109.5 . . ? 
H2B C2 H2C 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 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C8 S3 Cd1 N2 -138.5(3) . . . . ? 
C8 S3 Cd1 N4 -45.4(3) . . . 7_565 ? 
C8 S3 Cd1 N3 41.5(3) . . . . ? 
C8 S3 Cd1 S2 20(2) . . . . ? 
C8 S3 Cd1 S1 129.4(3) . . . . ? 
N4 C9 S1 Cd1 -167(11) . . . . ? 
N2 Cd1 S1 C9 30.8(3) . . . . ? 
N4 Cd1 S1 C9 169.5(13) 7_565 . . . ? 
N3 Cd1 S1 C9 -147.9(3) . . . . ? 
S2 Cd1 S1 C9 -61.9(3) . . . . ? 
S3 Cd1 S1 C9 120.1(3) . . . . ? 
S1 C9 N4 Cd1 -175(100) . . . 7_566 ? 
Cd1 S3 C8 N2 -122(28) . . . 7_565 ? 
N4 Cd1 N2 C8 144.8(14) 7_565 . . 7_566 ? 
N3 Cd1 N2 C8 54(11) . . . 7_566 ? 
S2 Cd1 N2 C8 54.0(14) . . . 7_566 ? 
S1 Cd1 N2 C8 -39.8(14) . . . 7_566 ? 
S3 Cd1 N2 C8 -126.8(14) . . . 7_566 ? 
N2 Cd1 S2 C10 -25.0(3) . . . . ? 
N4 Cd1 S2 C10 -118.2(3) 7_565 . . . ? 
N3 Cd1 S2 C10 155.0(3) . . . . ? 
S1 Cd1 S2 C10 67.2(3) . . . . ? 
S3 Cd1 S2 C10 177(46) . . . . ? 
Cd1 S2 C10 N3 172(6) . . . 7_566 ? 
N2 Cd1 N3 C10 109(10) . . . 7_565 ? 
N4 Cd1 N3 C10 17.7(8) 7_565 . . 7_565 ? 
S2 Cd1 N3 C10 108.6(8) . . . 7_565 ? 
S1 Cd1 N3 C10 -157.6(8) . . . 7_565 ? 
S3 Cd1 N3 C10 -70.7(8) . . . 7_565 ? 
C3 N1 C6 C7 -77.5(19) . . . . ? 
C1 N1 C6 C7 59.3(19) . . . . ? 
C2 N1 C6 C7 169.8(13) . . . . ? 
N1 C6 C7 Br1 -91.3(17) . . . . ? 
C6 N1 C3 C4 -39(2) . . . . ? 
C1 N1 C3 C4 -174.8(11) . . . . ? 
C2 N1 C3 C4 80.4(14) . . . . ? 
C6 N1 C3 C5 -173.6(14) . . . . ? 
C1 N1 C3 C5 50.6(19) . . . . ? 
C2 N1 C3 C5 -54.1(17) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    1.093 
_refine_diff_density_min   -0.968 
_refine_diff_density_rms    0.149 
