data_dimethyl substituted thiourea

Transcription

1 data_dimethyl substituted thiourea _audit_creation_method SHELXL _chemical_name_systematic? _chemical_name_common 4,5-Dimethylbenzimidazolene-2-thione _chemical_formula_moiety 'C9 H10 N2 S' _chemical_formula_structural? _chemical_formula_analytical? _chemical_formula_sum 'C9 H10 N2 S' _chemical_formula_weight _chemical_melting_point? _chemical_compound_source synthesis _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 'H' 'H' 'N' 'N' 'S' 'S' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m P 2(1/m) _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z'

2 'x, -y-1/2, z' _cell_length_a (11) _cell_length_b 8.320(2) _cell_length_c (2) _cell_angle_alpha _cell_angle_beta (3) _cell_angle_gamma _cell_volume 449.3(2) _cell_formula_units_z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 3 _cell_measurement_theta_max 57 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.8mm _exptl_crystal_size_mid 0.4mm _exptl_crystal_size_min 0.1mm _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn _exptl_crystal_density_method? _exptl_crystal_f_ _exptl_absorpt_coefficient_mu _exptl_absorpt_correction_type? _exptl_absorpt_correction_t_min? _exptl_absorpt_correction_t_max? _exptl_special_details? _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Siemens P4/RA

3 _diffrn_measurement_method\q-2\q _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time? _diffrn_standards_decay_% less than 1 _diffrn_reflns_number 645 _diffrn_reflns_av_r_equivalents _diffrn_reflns_av_sigmai/neti _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max _reflns_number_total 645 _reflns_number_observed 614 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction XDISK _computing_structure_solution 'SHELXS v.5.03 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXS v.5.03 (Sheldrick, 1994)' _computing_molecular_graphics XP _computing_publication_material XCIF _refine_special_details Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wr and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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.

4 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(fo^2^)+(0.2168p)^2^ p] 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 SHELXL _refine_ls_extinction_coef (111) _refine_ls_extinction_expression 'Fc^*^=kFc[ xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 645 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_r_factor_all _refine_ls_r_factor_obs _refine_ls_wr_factor_all _refine_ls_wr_factor_obs _refine_ls_goodness_of_fit_all _refine_ls_goodness_of_fit_obs _refine_ls_restrained_s_all _refine_ls_restrained_s_obs _refine_ls_shift/esd_max _refine_ls_shift/esd_mean _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S (3) (14) (10) Uani 1 d S.

5 N1 N (7) (5) (4) (13) Uani 1 d.. H1 H (92) (74) (50) Uiso 1 d.. C1 C (9) (7) (5) 0.032(2) Uani 1 d.. H1A H (13) (35) (24) Uiso 1 calc R. H1B H (50) (32) (7) Uiso 1 calc R. H1C H (57) (7) (27) Uiso 1 calc R. C2 C (8) (7) (4) (15) Uani 1 d.. C3 C (8) (6) (4) (14) Uani 1 d.. H3 H (8) (6) (4) Uiso 1 calc R. C4 C (8) (6) (4) (14) Uani 1 d.. C5 C (12) (6) 0.016(2) Uani 1 d S. _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 S (15) (14) (15) (9) N (2) 0.011(2) 0.020(2) (2) 0.014(2) 0.000(2) C (3) 0.047(4) 0.024(3) 0.012(3) 0.018(2) 0.000(2) C (2) 0.037(3) 0.011(2) 0.002(2) 0.005(2) (2) C (3) 0.023(3) 0.018(3) 0.003(2) 0.012(2) (2) C (3) 0.019(3) 0.016(3) 0.001(2) 0.008(2) 0.001(2) C (3) 0.014(4) 0.014(4) (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. _geom_bond_atom_site_label_1

6 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C (6). yes N1 C (6). yes N1 C (6). yes C1 C (7). yes C2 C (7). yes C2 C (11) 4_565 yes C3 C (7). yes C4 C (10) 4_565 yes C5 N (6) 4_565 yes _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 C5 N1 C (4).. yes C3 C2 C (3). 4_565 yes C3 C2 C (5).. yes C2 C2 C (3) 4_565. yes C4 C3 C (5).. yes C4 C4 C (3) 4_565. yes C4 C4 N (3) 4_565. yes C3 C4 N (5).. yes N1 C5 N (5). 4_565 yes N1 C5 S (3).. yes N1 C5 S (3) 4_565. yes _refine_diff_density_max _refine_diff_density_min _refine_diff_density_rms 0.200