data_global #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Bloggs, Joe J.' # Name of author for correspondence _publ_contact_author_address ;Department of Chemistry University of Anywhere Sometown Somewhere, UK ; # Address of author for correspondence _publ_contact_author_email j.bloggs@anywhere.ac.uk _publ_contact_author_fax '00(000)0000000' _publ_contact_author_phone '00(000)0000000' _publ_contact_letter ; Submission dated :2010-08-xx Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as a personal communication This CIF is submitted as part of a journal submission Bloggs, Joe J. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Bloggs, Joe J.' #<--'Last name, first name' ; ? ; ;Department of Chemistry University of Anywhere Sometown Somewhere, UK ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_i12610 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C17 H18 O S' _chemical_formula_sum 'C17 H18 O S' _chemical_formula_weight 270.37 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.2731(16) _cell_length_b 5.6491(5) _cell_length_c 12.1122(8) _cell_angle_alpha 90 _cell_angle_beta 98.130(2) _cell_angle_gamma 90 _cell_volume 1440.94(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100.00(10) _cell_measurement_reflns_used 1130 _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 24.9 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_absorpt_correction_T_min 0.6515 _exptl_absorpt_correction_T_max 0.7454 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100.00(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_unetI/netI 0.0811 _diffrn_reflns_number 5749 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 2713 _reflns_number_gt 2083 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0089(10) _refine_ls_number_reflns 2713 _refine_ls_number_parameters 177 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(10) _refine_diff_density_max 0.264 _refine_diff_density_min -0.25 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 S S 0.07067(3) 0.30529(16) 0.88428(6) 0.0272(2) Uani 1 1 d . . . O O 0.11884(9) 0.7239(4) 0.75957(17) 0.0225(5) Uani 1 1 d . . . C1 C 0.14155(13) 0.4974(6) 0.7287(2) 0.0178(7) Uani 1 1 d . . . C2 C 0.09192(12) 0.3058(7) 0.74126(19) 0.0198(6) Uani 1 1 d . . . H2 H 0.11 0.1512 0.7269 0.024 Uiso 1 1 calc R . . C3 C 0.02915(12) 0.3346(7) 0.6646(2) 0.0260(8) Uani 1 1 d . . . H3A H 0.0183 0.501 0.6557 0.031 Uiso 1 1 calc R . . H3B H 0.0324 0.2687 0.5916 0.031 Uiso 1 1 calc R . . C4 C -0.02122(13) 0.2045(6) 0.7177(2) 0.0306(9) Uani 1 1 d . . . H4A H -0.0144 0.0349 0.7156 0.037 Uiso 1 1 calc R . . H4B H -0.0632 0.2399 0.6788 0.037 Uiso 1 1 calc R . . C5 C -0.01463(13) 0.2919(9) 0.8377(2) 0.0378(9) Uani 1 1 d . . . H5A H -0.0349 0.1832 0.8836 0.045 Uiso 1 1 calc R . . H5B H -0.0338 0.447 0.8414 0.045 Uiso 1 1 calc R . . C6 C 0.15038(13) 0.5150(6) 0.6060(2) 0.0176(7) Uani 1 1 d . . . C7 C 0.18205(12) 0.3323(6) 0.5587(2) 0.0200(7) Uani 1 1 d . . . H7 H 0.1971 0.2033 0.6024 0.024 Uiso 1 1 calc R . . C8 C 0.19143(13) 0.3404(6) 0.4476(2) 0.0236(8) Uani 1 1 d . . . H8 H 0.2125 0.2178 0.4171 0.028 Uiso 1 1 calc R . . C9 C 0.16888(13) 0.5343(6) 0.3820(2) 0.0226(8) Uani 1 1 d . . . H9 H 0.1753 0.5422 0.3077 0.027 Uiso 1 1 calc R . . C10 C 0.13736(13) 0.7126(6) 0.4277(2) 0.0269(8) Uani 1 1 d . . . H10 H 0.1221 0.8407 0.3836 0.032 Uiso 1 1 calc R . . C11 C 0.12765(13) 0.7050(6) 0.5396(2) 0.0228(7) Uani 1 1 d . . . H11 H 0.106 0.8272 0.5694 0.027 Uiso 1 1 calc R . . C12 C 0.20626(13) 0.4462(6) 0.7984(2) 0.0184(7) Uani 1 1 d . . . C13 C 0.22137(12) 0.2377(6) 0.8564(2) 0.0193(7) Uani 1 1 d . . . H13 H 0.1907 0.1201 0.856 0.023 Uiso 1 1 calc R . . C14 C 0.28192(13) 0.2012(6) 0.9154(2) 0.0218(7) Uani 1 1 d . . . H14 H 0.2913 0.0608 0.9544 0.026 Uiso 1 1 calc R . . C15 C 0.32799(14) 0.3750(6) 0.9158(2) 0.0231(8) Uani 1 1 d . . . H15 H 0.3684 0.3509 0.9545 0.028 Uiso 1 1 calc R . . C16 C 0.31363(14) 0.5842(6) 0.8586(2) 0.0237(8) Uani 1 1 d . . . H16 H 0.3445 0.7006 0.8587 0.028 Uiso 1 1 calc R . . C17 C 0.25342(13) 0.6212(6) 0.8009(2) 0.0207(7) Uani 1 1 d . . . H17 H 0.2441 0.7634 0.7635 0.025 Uiso 1 1 calc R . . H1 H 0.1063(13) 0.697(6) 0.822(2) 0.024(9) 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 S 0.0240(4) 0.0395(6) 0.0189(4) 0.0019(4) 0.0052(3) -0.0015(5) O 0.0273(12) 0.0209(14) 0.0197(11) -0.0013(10) 0.0047(9) 0.0032(10) C1 0.0222(16) 0.0165(18) 0.0144(14) -0.0026(13) 0.0010(12) 0.0029(15) C2 0.0191(14) 0.0243(18) 0.0156(13) -0.0012(17) 0.0009(10) -0.0012(17) C3 0.0221(15) 0.030(2) 0.0226(15) -0.0021(17) -0.0062(12) 0.0010(17) C4 0.0195(16) 0.035(2) 0.0347(18) 0.0048(17) -0.0032(14) -0.0022(16) C5 0.0258(16) 0.055(3) 0.0334(17) 0.000(2) 0.0075(13) -0.001(2) C6 0.0181(15) 0.0194(19) 0.0144(14) -0.0022(14) -0.0009(11) -0.0009(14) C7 0.0219(14) 0.0202(19) 0.0165(13) 0.0011(15) -0.0024(11) 0.0001(16) C8 0.0267(15) 0.026(2) 0.0177(13) -0.0036(16) 0.0033(11) 0.0005(17) C9 0.0241(17) 0.030(2) 0.0127(15) 0.0019(15) 0.0006(12) -0.0044(16) C10 0.0280(17) 0.032(2) 0.0196(15) 0.0056(15) -0.0013(13) 0.0015(16) C11 0.0219(16) 0.0235(19) 0.0226(16) 0.0018(15) 0.0015(13) 0.0030(15) C12 0.0189(16) 0.024(2) 0.0130(14) -0.0025(14) 0.0051(11) -0.0018(15) C13 0.0182(15) 0.023(2) 0.0167(14) -0.0019(14) 0.0032(12) -0.0027(14) C14 0.0269(17) 0.024(2) 0.0143(14) -0.0002(14) 0.0007(13) 0.0013(16) C15 0.0209(16) 0.033(2) 0.0139(14) 0.0002(14) -0.0007(11) 0.0030(15) C16 0.0204(17) 0.029(2) 0.0217(16) -0.0024(16) 0.0038(13) -0.0051(15) C17 0.0242(17) 0.025(2) 0.0139(14) -0.0027(14) 0.0051(12) 0.0006(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S C5 1.824(3) . ? S C2 1.851(2) . ? O C1 1.436(3) . ? O H1 0.85(3) . ? C1 C6 1.527(4) . ? C1 C2 1.534(4) . ? C1 C12 1.537(4) . ? C2 C3 1.524(3) . ? C2 H2 0.98 . ? C3 C4 1.516(4) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.523(4) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C11 1.386(4) . ? C6 C7 1.399(4) . ? C7 C8 1.389(3) . ? C7 H7 0.93 . ? C8 C9 1.398(4) . ? C8 H8 0.93 . ? C9 C10 1.369(4) . ? C9 H9 0.93 . ? C10 C11 1.401(4) . ? C10 H10 0.93 . ? C11 H11 0.93 . ? C12 C13 1.386(4) . ? C12 C17 1.406(4) . ? C13 C14 1.397(3) . ? C13 H13 0.93 . ? C14 C15 1.387(4) . ? C14 H14 0.93 . ? C15 C16 1.382(4) . ? C15 H15 0.93 . ? C16 C17 1.385(4) . ? C16 H16 0.93 . ? C17 H17 0.93 . ? 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 C5 S C2 94.29(12) . . ? C1 O H1 103(2) . . ? O C1 C6 106.7(2) . . ? O C1 C2 109.9(2) . . ? C6 C1 C2 108.9(2) . . ? O C1 C12 109.4(2) . . ? C6 C1 C12 108.8(2) . . ? C2 C1 C12 112.8(2) . . ? C3 C2 C1 114.8(3) . . ? C3 C2 S 105.16(17) . . ? C1 C2 S 110.89(19) . . ? C3 C2 H2 108.6 . . ? C1 C2 H2 108.6 . . ? S C2 H2 108.6 . . ? C4 C3 C2 107.5(2) . . ? C4 C3 H3A 110.2 . . ? C2 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? C2 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 C5 105.8(3) . . ? C3 C4 H4A 110.6 . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4B 110.6 . . ? C5 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? C4 C5 S 105.2(2) . . ? C4 C5 H5A 110.7 . . ? S C5 H5A 110.7 . . ? C4 C5 H5B 110.7 . . ? S C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C11 C6 C7 118.9(3) . . ? C11 C6 C1 122.3(3) . . ? C7 C6 C1 118.9(3) . . ? C8 C7 C6 121.1(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 119.4(3) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.1(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C6 C11 C10 119.8(3) . . ? C6 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C17 118.2(3) . . ? C13 C12 C1 124.3(3) . . ? C17 C12 C1 117.4(3) . . ? C12 C13 C14 121.0(3) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.3(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.7(3) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF