data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_cambridge 1326 _journal_year 2010 _journal_volume 12 _journal_page_first 0 loop_ _publ_author_name F.D.Montigny R.Bast A.S.P.Gomes G.Pilet N.Vanthuyne C.Roussel ; L.Guy ; P.Schwerdtfeger T.Saue J.Crassous _publ_contact_author_name 'Guillaume Pilet' _publ_contact_author_email guillaume.pilet@univ-lyon1.fr data_1 _database_code_depnum_ccdc_archive 'CCDC 753444' _audit_creation_date 10-03-15 _audit_creation_method CRYSTALS_ver_12.86 #_oxford_structure_analysis_title 'import in P 21 21 21' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 8.9219(2) _cell_length_b 10.0914(2) _cell_length_c 13.6763(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1231.34(5) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C6 H12 I1 O1 Re1 S3 # Dc = 2.75 Fooo = 928.00 Mu = 128.43 M = 509.46 # Found Formula = C6 H12 I1 O1 Re1 S3 # Dc = 2.75 FOOO = 928.00 Mu = 128.43 M = 509.46 _chemical_formula_sum 'C6 H12 I1 O1 Re1 S3' _chemical_formula_moiety 'C6 H12 I1 O1 Re1 S3' _chemical_compound_source ? _chemical_formula_weight 509.46 _cell_measurement_reflns_used 1713 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.98 _exptl_crystal_density_diffrn 2.748 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 12.843 # Sheldrick geometric approximatio 0.30 0.41 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.41 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 2958 _reflns_number_total 2936 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 1700 # Number of reflections without Friedels Law is 2936 # Theoretical number of reflections is about 1469 _diffrn_reflns_theta_min 2.508 _diffrn_reflns_theta_max 27.904 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.904 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.18 _refine_diff_density_max 1.22 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 2236 _refine_ls_number_restraints 0 _refine_ls_number_parameters 111 _oxford_refine_ls_R_factor_ref 0.0314 _refine_ls_wR_factor_ref 0.0342 _refine_ls_goodness_of_fit_ref 1.0952 _refine_ls_shift/su_max 0.000306 # The values computed from all data _oxford_reflns_number_all 2927 _refine_ls_R_factor_all 0.0453 _refine_ls_wR_factor_all 0.0528 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2389 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_gt 0.0363 _refine_ls_abs_structure_Flack 0.026(17) _refine_ls_abs_structure_details 'Flack (1983), 1236 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.258 0.121 0.552E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Re1 Re 0.33019(3) 0.19807(3) 0.75175(4) 0.0382 1.0000 Uani . . . . . . . O1 O 0.2458(8) 0.3442(7) 0.7312(6) 0.0603 1.0000 Uani . . . . . . . I1 I 0.09663(6) 0.02792(7) 0.75301(9) 0.0648 1.0000 Uani . . . . . . . S2 S 0.5812(2) 0.2615(2) 0.7620(2) 0.0422 1.0000 Uani . . . . . . . S3 S 0.4043(3) 0.0824(3) 0.61709(17) 0.0413 1.0000 Uani . . . . . . . S4 S 0.3586(4) 0.1382(3) 0.9119(2) 0.0591 1.0000 Uani . . . . . . . C3 C 0.5387(15) 0.2094(15) 0.9531(7) 0.0632 1.0000 Uani . . . . . . . C4 C 0.6544(14) 0.1953(15) 0.8771(8) 0.0627 1.0000 Uani . . . . . . . C5 C 0.6839(11) 0.1682(11) 0.6724(8) 0.0469 1.0000 Uani . . . . . . . C6 C 0.5915(11) 0.1501(10) 0.5797(7) 0.0396 1.0000 Uani . . . . . . . C7 C 0.6634(12) 0.0485(12) 0.5141(8) 0.0545 1.0000 Uani . . . . . . . C8 C 0.5688(14) 0.2798(13) 0.5253(8) 0.0592 1.0000 Uani . . . . . . . H131 H 0.5035 0.2662 0.4676 0.0697 1.0000 Uiso R . . . . . . H132 H 0.5160 0.3473 0.5707 0.0697 1.0000 Uiso R . . . . . . H133 H 0.6662 0.3197 0.5055 0.0697 1.0000 Uiso R . . . . . . H101 H 0.6012 0.0381 0.4537 0.0629 1.0000 Uiso R . . . . . . H102 H 0.7669 0.0780 0.4950 0.0629 1.0000 Uiso R . . . . . . H103 H 0.6702 -0.0386 0.5487 0.0629 1.0000 Uiso R . . . . . . H71 H 0.7520 0.2472 0.8910 0.0771 1.0000 Uiso R . . . . . . H72 H 0.6852 0.1010 0.8642 0.0771 1.0000 Uiso R . . . . . . H111 H 0.5743 0.1655 1.0141 0.0679 1.0000 Uiso R . . . . . . H112 H 0.5251 0.3082 0.9679 0.0679 1.0000 Uiso R . . . . . . H41 H 0.7795 0.2166 0.6564 0.0570 1.0000 Uiso R . . . . . . H42 H 0.7103 0.0791 0.7004 0.0570 1.0000 Uiso R . . . . . . 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 Re1 0.03194(15) 0.04221(17) 0.04044(17) 0.0034(3) 0.0024(3) 0.00851(12) I1 0.0354(3) 0.0784(4) 0.0805(5) 0.0112(7) 0.0098(5) -0.0064(3) O1 0.044(4) 0.052(3) 0.085(6) 0.016(4) -0.005(4) 0.020(3) S3 0.0354(11) 0.0462(12) 0.0423(11) -0.0034(10) 0.0022(9) -0.0042(10) S2 0.0385(10) 0.0428(10) 0.0452(14) -0.0070(11) -0.0051(11) 0.0030(8) S4 0.0661(19) 0.0697(18) 0.0413(13) 0.0094(13) 0.0070(12) 0.0106(15) C7 0.043(5) 0.063(6) 0.058(6) -0.015(5) 0.012(5) -0.008(5) C8 0.056(7) 0.070(8) 0.052(6) 0.010(5) 0.015(5) -0.009(6) C6 0.032(5) 0.050(5) 0.037(4) 0.003(4) 0.007(4) -0.007(4) C5 0.030(5) 0.050(6) 0.061(6) -0.004(5) 0.005(4) -0.005(4) C4 0.055(7) 0.086(8) 0.048(5) 0.005(6) -0.019(6) 0.019(7) C3 0.079(9) 0.078(8) 0.033(5) 0.004(5) -0.006(5) 0.012(8) _refine_ls_extinction_coef 22(2) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.1192(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . I1 . 2.7001(7) yes Re1 . O1 . 1.679(6) yes Re1 . S3 . 2.278(2) yes Re1 . S2 . 2.334(2) yes Re1 . S4 . 2.286(3) yes S3 . C6 . 1.876(9) yes S2 . C5 . 1.796(10) yes S2 . C4 . 1.831(11) yes S4 . C3 . 1.848(14) yes C7 . C6 . 1.506(13) yes C7 . H101 . 1.001 no C7 . H102 . 1.005 no C7 . H103 . 1.000 no C8 . C6 . 1.519(15) yes C8 . H131 . 0.991 no C8 . H132 . 1.035 no C8 . H133 . 0.995 no C6 . C5 . 1.524(14) yes C5 . H41 . 1.007 no C5 . H42 . 1.005 no C4 . C3 . 1.471(16) yes C4 . H71 . 1.034 no C4 . H72 . 1.007 no C3 . H111 . 0.996 no C3 . H112 . 1.025 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I1 . Re1 . O1 . 102.3(3) yes I1 . Re1 . S3 . 84.46(6) yes O1 . Re1 . S3 . 116.4(3) yes I1 . Re1 . S2 . 156.18(6) yes O1 . Re1 . S2 . 101.5(3) yes S3 . Re1 . S2 . 84.86(9) yes I1 . Re1 . S4 . 84.92(9) yes O1 . Re1 . S4 . 116.2(3) yes S3 . Re1 . S4 . 127.38(12) yes S2 . Re1 . S4 . 84.76(11) yes Re1 . S3 . C6 . 107.0(3) yes Re1 . S2 . C5 . 107.7(3) yes Re1 . S2 . C4 . 107.1(5) yes C5 . S2 . C4 . 102.3(6) yes Re1 . S4 . C3 . 106.6(4) yes C6 . C7 . H101 . 109.1 no C6 . C7 . H102 . 110.1 no H101 . C7 . H102 . 109.0 no C6 . C7 . H103 . 110.0 no H101 . C7 . H103 . 109.4 no H102 . C7 . H103 . 109.1 no C6 . C8 . H131 . 110.5 no C6 . C8 . H132 . 109.6 no H131 . C8 . H132 . 107.4 no C6 . C8 . H133 . 111.5 no H131 . C8 . H133 . 110.7 no H132 . C8 . H133 . 107.1 no S3 . C6 . C8 . 109.2(7) yes S3 . C6 . C7 . 107.1(7) yes C8 . C6 . C7 . 110.6(8) yes S3 . C6 . C5 . 107.3(6) yes C8 . C6 . C5 . 112.1(9) yes C7 . C6 . C5 . 110.3(9) yes C6 . C5 . S2 . 110.8(7) yes C6 . C5 . H41 . 109.5 no S2 . C5 . H41 . 109.1 no C6 . C5 . H42 . 109.7 no S2 . C5 . H42 . 109.2 no H41 . C5 . H42 . 108.5 no S2 . C4 . C3 . 108.8(8) yes S2 . C4 . H71 . 105.9 no C3 . C4 . H71 . 114.4 no S2 . C4 . H72 . 106.9 no C3 . C4 . H72 . 114.0 no H71 . C4 . H72 . 106.3 no S4 . C3 . C4 . 110.9(9) yes S4 . C3 . H111 . 111.1 no C4 . C3 . H111 . 109.0 no S4 . C3 . H112 . 109.5 no C4 . C3 . H112 . 108.4 no H111 . C3 . H112 . 107.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C5 . H42 . O1 3_646 175 1.00 2.58 3.581(16) yes data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 753445' _audit_creation_date 06-11-15 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'import in P 21 21 21' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.1147(3) _cell_length_b 10.5897(4) _cell_length_c 16.4388(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1412.62(9) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C8 H17 O1 Re1 S4 # Dc = 2.09 Fooo = 848.00 Mu = 91.64 M = 443.69 # Found Formula = C8 H17 O1 Re1 S4 # Dc = 2.09 FOOO = 848.00 Mu = 91.64 M = 443.69 _chemical_formula_sum 'C8 H17 O1 Re1 S4' _chemical_formula_moiety 'C8 H17 O1 Re1 S4' _chemical_compound_source ? _chemical_formula_weight 443.69 _cell_measurement_reflns_used 1941 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 9.164 # Sheldrick geometric approximatio 0.57 0.75 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.5666 _exptl_absorpt_correction_T_max 0.7458 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 3381 _reflns_number_total 3358 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 1940 # Number of reflections without Friedels Law is 3358 # Theoretical number of reflections is about 1680 _diffrn_reflns_theta_min 2.288 _diffrn_reflns_theta_max 27.870 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.870 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.85 _refine_diff_density_max 1.42 _refine_ls_number_reflns 2400 _refine_ls_number_restraints 0 _refine_ls_number_parameters 128 #_refine_ls_R_factor_ref 0.0325 _refine_ls_wR_factor_ref 0.0290 _refine_ls_goodness_of_fit_ref 1.0960 #_reflns_number_all 3346 _refine_ls_R_factor_all 0.0555 _refine_ls_wR_factor_all 0.0469 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 2400 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_gt 0.0290 _refine_ls_shift/su_max 0.000333 _refine_ls_abs_structure_Flack 0.008(14) _refine_ls_abs_structure_details 'Flack (1983), 1418 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.214 -0.374E-01 0.326E-01 ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Re1 Re 0.31039(4) 0.07384(3) 0.13947(2) 0.0465 1.0000 Uani . . . . . . S1 S 0.1299(3) -0.0200(3) 0.04932(18) 0.0652 1.0000 Uani . . . . . . S2 S 0.4848(3) 0.2391(3) 0.18684(16) 0.0591 1.0000 Uani . . . . . . S3 S 0.1102(2) 0.2257(2) 0.14111(18) 0.0534 1.0000 Uani . . . . . . S4 S 0.5165(3) 0.0435(3) 0.04690(18) 0.0756 1.0000 Uani . . . . . . O1 O 0.3122(10) -0.0216(6) 0.2217(4) 0.0652 1.0000 Uani . . . . . . C1 C 0.271(2) -0.2578(12) 0.0445(12) 0.1266 1.0000 Uani . . . . . . C2 C 0.2284(16) -0.1484(13) -0.0081(8) 0.0905 1.0000 Uani . . . . . . C3 C 0.6933(15) 0.1379(11) 0.0794(7) 0.0758 1.0000 Uani . . . . . . C4 C 0.6414(12) 0.2659(11) 0.1105(7) 0.0723 1.0000 Uani . . . . . . C5 C 0.3620(12) 0.3814(9) 0.1831(6) 0.0641 1.0000 Uani . . . . . . C6 C 0.1870(15) 0.3556(8) 0.2067(5) 0.0567 1.0000 Uani . . . . . . C7 C 0.0786(15) 0.4711(11) 0.1907(7) 0.0790 1.0000 Uani . . . . . . C8 C 0.177(2) 0.3122(11) 0.2974(6) 0.0908 1.0000 Uani . . . . . . H131 H 0.3244 -0.3281 0.0131 0.1390 1.0000 Uiso . . . . . . H132 H 0.3461 -0.2316 0.0899 0.1390 1.0000 Uiso . . . . . . H133 H 0.1658 -0.2926 0.0698 0.1390 1.0000 Uiso . . . . . . H91 H 0.3352 -0.1137 -0.0351 0.0985 1.0000 Uiso . . . . . . H92 H 0.1549 -0.1748 -0.0552 0.0985 1.0000 Uiso . . . . . . H81 H 0.7562 0.0923 0.1237 0.0923 1.0000 Uiso . . . . . . H82 H 0.7729 0.1486 0.0316 0.0923 1.0000 Uiso . . . . . . H121 H 0.7397 0.3120 0.1338 0.0880 1.0000 Uiso . . . . . . H122 H 0.5977 0.3174 0.0635 0.0880 1.0000 Uiso . . . . . . H151 H 0.0638 0.2904 0.3139 0.1189 1.0000 Uiso . . . . . . H152 H 0.2240 0.3780 0.3347 0.1189 1.0000 Uiso . . . . . . H153 H 0.2493 0.2321 0.3051 0.1189 1.0000 Uiso . . . . . . H141 H 0.1126 0.5441 0.2252 0.0955 1.0000 Uiso . . . . . . H142 H -0.0416 0.4503 0.2047 0.0955 1.0000 Uiso . . . . . . H143 H 0.0818 0.4960 0.1320 0.0955 1.0000 Uiso . . . . . . H101 H 0.4109 0.4498 0.2197 0.0811 1.0000 Uiso . . . . . . H102 H 0.3649 0.4196 0.1250 0.0811 1.0000 Uiso . . . . . . 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 Re1 0.04053(13) 0.04923(16) 0.04960(15) 0.00480(19) 0.00078(18) -0.00066(18) S1 0.0567(14) 0.0668(16) 0.0721(16) -0.0150(13) 0.0021(12) -0.0123(12) S2 0.0474(13) 0.0643(16) 0.0656(15) 0.0015(12) -0.0119(11) -0.0062(12) S3 0.0405(10) 0.0567(13) 0.0630(13) -0.0064(14) -0.0018(12) 0.0003(9) S4 0.0558(14) 0.088(2) 0.0832(18) -0.0184(16) 0.0214(13) -0.0049(14) O1 0.069(4) 0.066(4) 0.061(4) 0.025(3) -0.005(4) -0.002(4) C1 0.121(14) 0.050(7) 0.209(18) -0.026(9) 0.006(12) 0.007(8) C2 0.083(9) 0.094(9) 0.095(9) -0.052(7) 0.020(7) -0.016(7) C3 0.047(5) 0.090(7) 0.090(7) 0.008(6) 0.012(7) -0.009(6) C4 0.051(6) 0.074(7) 0.092(8) 0.012(6) 0.001(5) -0.012(5) C5 0.068(7) 0.053(6) 0.072(6) -0.012(5) -0.019(5) 0.006(5) C6 0.061(5) 0.048(5) 0.061(5) -0.009(4) -0.008(6) -0.001(6) C7 0.088(8) 0.063(7) 0.086(8) -0.010(6) 0.005(6) 0.018(6) C8 0.128(11) 0.085(8) 0.059(6) -0.014(6) 0.008(8) 0.007(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12402(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . S1 . 2.308(3) yes Re1 . S2 . 2.382(3) yes Re1 . S3 . 2.286(2) yes Re1 . S4 . 2.284(3) yes Re1 . O1 . 1.687(5) yes S1 . C2 . 1.838(12) yes S2 . C4 . 1.808(10) yes S2 . C5 . 1.808(10) yes S3 . C6 . 1.856(9) yes S4 . C3 . 1.829(12) yes C1 . C2 . 1.486(19) yes C1 . H131 . 1.005 no C1 . H132 . 1.003 no C1 . H133 . 1.017 no C2 . H91 . 1.041 no C2 . H92 . 1.017 no C3 . C4 . 1.508(15) yes C3 . H81 . 1.012 no C3 . H82 . 1.024 no C4 . H121 . 1.010 no C4 . H122 . 1.011 no C5 . C6 . 1.498(15) yes C5 . H101 . 1.021 no C5 . H102 . 1.037 no C6 . C7 . 1.529(14) yes C6 . C8 . 1.562(14) yes C7 . H141 . 0.997 no C7 . H142 . 1.026 no C7 . H143 . 1.001 no C8 . H151 . 0.982 no C8 . H152 . 1.005 no C8 . H153 . 1.041 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Re1 . S2 . 154.57(10) yes S1 . Re1 . S3 . 81.92(10) yes S2 . Re1 . S3 . 84.34(8) yes S1 . Re1 . S4 . 88.64(10) yes S2 . Re1 . S4 . 83.46(10) yes S3 . Re1 . S4 . 128.85(11) yes S1 . Re1 . O1 . 105.2(3) yes S2 . Re1 . O1 . 100.0(2) yes S3 . Re1 . O1 . 114.7(3) yes S4 . Re1 . O1 . 116.3(3) yes Re1 . S1 . C2 . 111.8(4) yes Re1 . S2 . C4 . 107.8(4) yes Re1 . S2 . C5 . 105.9(3) yes C4 . S2 . C5 . 103.5(5) yes Re1 . S3 . C6 . 106.9(4) yes Re1 . S4 . C3 . 107.6(4) yes C2 . C1 . H131 . 112.3 no C2 . C1 . H132 . 111.0 no H131 . C1 . H132 . 108.8 no C2 . C1 . H133 . 109.1 no H131 . C1 . H133 . 107.7 no H132 . C1 . H133 . 107.9 no S1 . C2 . C1 . 112.3(9) yes S1 . C2 . H91 . 108.7 no C1 . C2 . H91 . 109.3 no S1 . C2 . H92 . 109.9 no C1 . C2 . H92 . 111.4 no H91 . C2 . H92 . 105.0 no S4 . C3 . C4 . 111.8(8) yes S4 . C3 . H81 . 110.2 no C4 . C3 . H81 . 109.0 no S4 . C3 . H82 . 109.3 no C4 . C3 . H82 . 109.7 no H81 . C3 . H82 . 106.7 no C3 . C4 . S2 . 106.9(7) yes C3 . C4 . H121 . 110.0 no S2 . C4 . H121 . 111.6 no C3 . C4 . H122 . 108.9 no S2 . C4 . H122 . 111.6 no H121 . C4 . H122 . 107.8 no S2 . C5 . C6 . 111.2(7) yes S2 . C5 . H101 . 110.9 no C6 . C5 . H101 . 110.1 no S2 . C5 . H102 . 110.1 no C6 . C5 . H102 . 109.3 no H101 . C5 . H102 . 105.0 no S3 . C6 . C5 . 107.6(7) yes S3 . C6 . C7 . 107.4(7) yes C5 . C6 . C7 . 110.8(9) yes S3 . C6 . C8 . 108.6(7) yes C5 . C6 . C8 . 110.6(10) yes C7 . C6 . C8 . 111.6(9) yes C6 . C7 . H141 . 111.3 no C6 . C7 . H142 . 109.7 no H141 . C7 . H142 . 107.6 no C6 . C7 . H143 . 111.2 no H141 . C7 . H143 . 109.6 no H142 . C7 . H143 . 107.3 no C6 . C8 . H151 . 112.5 no C6 . C8 . H152 . 111.0 no H151 . C8 . H152 . 110.6 no C6 . C8 . H153 . 109.0 no H151 . C8 . H153 . 107.6 no H152 . C8 . H153 . 105.9 no data_3 _database_code_depnum_ccdc_archive 'CCDC 753446' _audit_creation_date 10-02-08 _audit_creation_method CRYSTALS_ver_12.87 _oxford_structure_analysis_title 'import in P 21/n' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 8.1618(5) _cell_length_b 16.1619(6) _cell_length_c 10.9861(6) _cell_angle_alpha 90 _cell_angle_beta 102.115(2) _cell_angle_gamma 90 _cell_volume 1416.90(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C8 H17 O1 Re1 S4 # Dc = 2.08 Fooo = 848.00 Mu = 91.36 M = 443.69 # Found Formula = C8 H17 O1 Re1 S4 # Dc = 2.08 FOOO = 848.00 Mu = 91.36 M = 443.69 _chemical_formula_sum 'C8 H17 O1 Re1 S4' _chemical_formula_moiety 'C8 H17 O1 Re1 S4' _chemical_compound_source ? _chemical_formula_weight 443.69 _cell_measurement_reflns_used 15807 _cell_measurement_theta_min 1 _cell_measurement_theta_max 29 _cell_measurement_temperature 293 _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_min 0.165 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_max 0.231 _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 9.136 # Sheldrick geometric approximatio 0.21 0.22 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.13 _exptl_absorpt_correction_T_max 0.22 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 9209 _reflns_number_total 3617 _diffrn_reflns_av_R_equivalents 0.162 # Number of reflections without Friedels Law is 3617 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 3768 _diffrn_reflns_theta_min 2.277 _diffrn_reflns_theta_max 29.077 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.006 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -3.83 _refine_diff_density_max 1.95 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 1735 _refine_ls_number_restraints 0 _refine_ls_number_parameters 128 _oxford_refine_ls_R_factor_ref 0.0570 _refine_ls_wR_factor_ref 0.0644 _refine_ls_goodness_of_fit_ref 1.0655 _refine_ls_shift/su_max 0.0001248 _refine_ls_shift/su_mean 1.5418822 # The values computed from all data _oxford_reflns_number_all 3605 _refine_ls_R_factor_all 0.1061 _refine_ls_wR_factor_all 0.1126 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2017 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_gt 0.0694 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.20 0.463 0.724 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Re1 Re 0.12817(6) 0.14451(3) 0.17389(5) 0.0478 1.0000 Uani . . . . . . . O1 O 0.1436(14) 0.2298(7) 0.2643(11) 0.0752 1.0000 Uani . . . . . . . S1 S 0.3341(5) 0.0553(3) 0.2754(4) 0.0635 1.0000 Uani . . . . . . . S2 S -0.0847(4) 0.1900(2) 0.0040(4) 0.0558 1.0000 Uani . . . . . . . S3 S 0.2940(4) 0.1444(3) 0.0294(4) 0.0603 1.0000 Uani . . . . . . . S4 S -0.0675(5) 0.0492(3) 0.2012(4) 0.0636 1.0000 Uani . . . . . . . C1 C 0.231(3) 0.0546(16) 0.5012(16) 0.0996 1.0000 Uani . . . . . . . C2 C 0.267(3) -0.0006(13) 0.3988(17) 0.0847 1.0000 Uani . . . . . . . C3 C -0.2677(16) 0.0805(10) 0.1021(16) 0.0647 1.0000 Uani . . . . . . . C4 C -0.2446(18) 0.1083(11) -0.0235(16) 0.0677 1.0000 Uani . . . . . . . C5 C 0.006(2) 0.1831(11) -0.1348(14) 0.0646 1.0000 Uani . . . . . . . C6 C 0.186(2) 0.2094(11) -0.1045(15) 0.0680 1.0000 Uani . . . . . . . C7 C 0.210(3) 0.2976(13) -0.067(2) 0.0964 1.0000 Uani . . . . . . . C8 C 0.262(3) 0.1864(14) -0.2145(19) 0.0913 1.0000 Uani . . . . . . . H31 H -0.3167 0.1269 0.1403 0.0781 1.0000 Uiso . . . . . . . H32 H -0.3468 0.0344 0.0919 0.0781 1.0000 Uiso . . . . . . . H41 H -0.3505 0.1283 -0.0731 0.0811 1.0000 Uiso . . . . . . . H42 H -0.2082 0.0608 -0.0678 0.0810 1.0000 Uiso . . . . . . . H51 H -0.0579 0.2180 -0.2004 0.0780 1.0000 Uiso . . . . . . . H52 H -0.0022 0.1250 -0.1647 0.0781 1.0000 Uiso . . . . . . . H81 H 0.3809 0.1965 -0.1952 0.1331 1.0000 Uiso . . . . . . . H82 H 0.2116 0.2185 -0.2869 0.1330 1.0000 Uiso . . . . . . . H83 H 0.2433 0.1284 -0.2340 0.1330 1.0000 Uiso . . . . . . . H73 H 0.3259 0.3147 -0.0638 0.1420 1.0000 Uiso . . . . . . . H72 H 0.1379 0.3335 -0.1251 0.1420 1.0000 Uiso . . . . . . . H71 H 0.1865 0.3063 0.0149 0.1420 1.0000 Uiso . . . . . . . H21 H 0.3548 -0.0393 0.4360 0.1029 1.0000 Uiso . . . . . . . H22 H 0.1655 -0.0321 0.3637 0.1030 1.0000 Uiso . . . . . . . H11 H 0.1887 0.0214 0.5616 0.1440 1.0000 Uiso . . . . . . . H12 H 0.3307 0.0819 0.5418 0.1440 1.0000 Uiso . . . . . . . H13 H 0.1474 0.0946 0.4668 0.1440 1.0000 Uiso . . . . . . . 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 Re1 0.0395(3) 0.0516(3) 0.0483(3) -0.0065(3) 0.00030(19) -0.0017(3) O1 0.066(6) 0.068(7) 0.081(8) -0.027(6) -0.010(6) -0.001(5) S4 0.0528(19) 0.071(3) 0.064(2) 0.0058(19) 0.0048(17) -0.0060(18) C3 0.041(7) 0.066(9) 0.085(11) -0.008(8) 0.010(7) -0.004(6) C4 0.046(8) 0.085(11) 0.066(9) 0.001(8) -0.004(7) -0.008(8) S2 0.0429(16) 0.059(2) 0.061(2) -0.0004(16) 0.0002(15) 0.0096(15) C5 0.063(9) 0.075(10) 0.051(8) 0.014(7) -0.001(7) 0.016(8) C6 0.067(9) 0.072(10) 0.066(10) 0.016(8) 0.015(8) 0.006(8) S3 0.0416(16) 0.073(2) 0.066(2) 0.0123(19) 0.0099(15) 0.0085(17) C8 0.085(12) 0.113(16) 0.083(13) 0.039(12) 0.035(11) 0.013(12) C7 0.093(14) 0.085(14) 0.109(16) 0.007(12) 0.017(12) -0.007(11) S1 0.0500(18) 0.072(2) 0.063(2) 0.012(2) 0.0002(16) 0.0094(18) C2 0.090(13) 0.083(12) 0.070(11) 0.028(10) -0.008(9) -0.018(10) C1 0.105(15) 0.15(2) 0.051(10) 0.012(12) 0.026(10) 0.000(14) _refine_ls_extinction_coef 23(8) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2190(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . O1 . 1.689(10) yes Re1 . S4 . 2.283(4) yes Re1 . S2 . 2.384(3) yes Re1 . S3 . 2.292(4) yes Re1 . S1 . 2.315(4) yes S4 . C3 . 1.834(15) yes C3 . C4 . 1.50(2) yes C3 . H31 . 0.984 no C3 . H32 . 0.976 no C4 . S2 . 1.836(16) yes C4 . H41 . 0.975 no C4 . H42 . 0.988 no S2 . C5 . 1.832(17) yes C5 . C6 . 1.50(2) yes C5 . H51 . 0.976 no C5 . H52 . 0.992 no C6 . S3 . 1.871(16) yes C6 . C8 . 1.51(3) yes C6 . C7 . 1.48(3) yes C8 . H81 . 0.967 no C8 . H82 . 0.965 no C8 . H83 . 0.967 no C7 . H73 . 0.976 no C7 . H72 . 0.968 no C7 . H71 . 0.971 no S1 . C2 . 1.806(19) yes C2 . C1 . 1.51(3) yes C2 . H21 . 0.971 no C2 . H22 . 0.983 no C1 . H11 . 0.970 no C1 . H12 . 0.954 no C1 . H13 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Re1 . S4 . 116.2(5) yes O1 . Re1 . S2 . 99.3(4) yes S4 . Re1 . S2 . 84.02(13) yes O1 . Re1 . S3 . 115.2(5) yes S4 . Re1 . S3 . 128.44(15) yes S2 . Re1 . S3 . 84.09(13) yes O1 . Re1 . S1 . 105.6(4) yes S4 . Re1 . S1 . 88.51(14) yes S2 . Re1 . S1 . 154.86(15) yes S3 . Re1 . S1 . 81.88(14) yes Re1 . S4 . C3 . 107.3(5) yes S4 . C3 . C4 . 111.1(10) yes S4 . C3 . H31 . 110.3 no C4 . C3 . H31 . 107.7 no S4 . C3 . H32 . 110.1 no C4 . C3 . H32 . 109.3 no H31 . C3 . H32 . 108.2 no C3 . C4 . S2 . 106.7(11) yes C3 . C4 . H41 . 110.3 no S2 . C4 . H41 . 111.7 no C3 . C4 . H42 . 109.2 no S2 . C4 . H42 . 111.3 no H41 . C4 . H42 . 107.7 no C4 . S2 . Re1 . 106.4(5) yes C4 . S2 . C5 . 102.5(8) yes Re1 . S2 . C5 . 106.1(5) yes S2 . C5 . C6 . 110.3(12) yes S2 . C5 . H51 . 109.4 no C6 . C5 . H51 . 110.3 no S2 . C5 . H52 . 108.8 no C6 . C5 . H52 . 109.7 no H51 . C5 . H52 . 108.2 no C5 . C6 . S3 . 107.0(11) yes C5 . C6 . C8 . 107.3(15) yes S3 . C6 . C8 . 106.6(12) yes C5 . C6 . C7 . 113.7(15) yes S3 . C6 . C7 . 107.9(13) yes C8 . C6 . C7 . 113.8(16) yes C6 . S3 . Re1 . 107.2(5) yes C6 . C8 . H81 . 110.2 no C6 . C8 . H82 . 110.7 no H81 . C8 . H82 . 108.8 no C6 . C8 . H83 . 110.3 no H81 . C8 . H83 . 108.3 no H82 . C8 . H83 . 108.6 no C6 . C7 . H73 . 110.8 no C6 . C7 . H72 . 111.4 no H73 . C7 . H72 . 107.8 no C6 . C7 . H71 . 110.8 no H73 . C7 . H71 . 107.8 no H72 . C7 . H71 . 108.1 no Re1 . S1 . C2 . 111.8(7) yes S1 . C2 . C1 . 113.6(14) yes S1 . C2 . H21 . 109.1 no C1 . C2 . H21 . 108.0 no S1 . C2 . H22 . 109.1 no C1 . C2 . H22 . 108.2 no H21 . C2 . H22 . 108.5 no C2 . C1 . H11 . 109.7 no C2 . C1 . H12 . 109.7 no H11 . C1 . H12 . 109.0 no C2 . C1 . H13 . 110.0 no H11 . C1 . H13 . 108.7 no H12 . C1 . H13 . 109.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C5 . H51 . O1 4_454 131 0.98 2.53 3.25(3) yes C8 . H81 . O1 4_554 152 0.97 2.57 3.45(3) yes data_4 _database_code_depnum_ccdc_archive 'CCDC 753447' _audit_creation_date 10-03-15 _audit_creation_method CRYSTALS_ver_12.86 #_oxford_structure_analysis_title 'import in P 21 21 21' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 8.9219(2) _cell_length_b 10.0914(2) _cell_length_c 13.6763(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1231.34(5) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C6 H12 I1 O1 Re1 S3 # Dc = 2.75 Fooo = 928.00 Mu = 128.43 M = 509.46 # Found Formula = C6 H12 I1 O1 Re1 S3 # Dc = 2.75 FOOO = 928.00 Mu = 128.43 M = 509.46 _chemical_formula_sum 'C6 H12 I1 O1 Re1 S3' _chemical_formula_moiety 'C6 H12 I1 O1 Re1 S3' _chemical_compound_source ? _chemical_formula_weight 509.46 _cell_measurement_reflns_used 1713 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.98 _exptl_crystal_density_diffrn 2.748 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 12.843 # Sheldrick geometric approximatio 0.30 0.41 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.41 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 2958 _reflns_number_total 2936 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 1700 # Number of reflections without Friedels Law is 2936 # Theoretical number of reflections is about 1469 _diffrn_reflns_theta_min 2.508 _diffrn_reflns_theta_max 27.904 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.904 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.18 _refine_diff_density_max 1.22 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 2236 _refine_ls_number_restraints 0 _refine_ls_number_parameters 111 _oxford_refine_ls_R_factor_ref 0.0314 _refine_ls_wR_factor_ref 0.0342 _refine_ls_goodness_of_fit_ref 1.0952 _refine_ls_shift/su_max 0.000306 # The values computed from all data _oxford_reflns_number_all 2927 _refine_ls_R_factor_all 0.0453 _refine_ls_wR_factor_all 0.0528 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2389 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_gt 0.0363 _refine_ls_abs_structure_Flack 0.026(17) _refine_ls_abs_structure_details 'Flack (1983), 1236 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.258 0.121 0.552E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Re1 Re 0.33019(3) 0.19807(3) 0.75175(4) 0.0382 1.0000 Uani . . . . . . . O1 O 0.2458(8) 0.3442(7) 0.7312(6) 0.0603 1.0000 Uani . . . . . . . I1 I 0.09663(6) 0.02792(7) 0.75301(9) 0.0648 1.0000 Uani . . . . . . . S2 S 0.5812(2) 0.2615(2) 0.7620(2) 0.0422 1.0000 Uani . . . . . . . S3 S 0.4043(3) 0.0824(3) 0.61709(17) 0.0413 1.0000 Uani . . . . . . . S4 S 0.3586(4) 0.1382(3) 0.9119(2) 0.0591 1.0000 Uani . . . . . . . C3 C 0.5387(15) 0.2094(15) 0.9531(7) 0.0632 1.0000 Uani . . . . . . . C4 C 0.6544(14) 0.1953(15) 0.8771(8) 0.0627 1.0000 Uani . . . . . . . C5 C 0.6839(11) 0.1682(11) 0.6724(8) 0.0469 1.0000 Uani . . . . . . . C6 C 0.5915(11) 0.1501(10) 0.5797(7) 0.0396 1.0000 Uani . . . . . . . C7 C 0.6634(12) 0.0485(12) 0.5141(8) 0.0545 1.0000 Uani . . . . . . . C8 C 0.5688(14) 0.2798(13) 0.5253(8) 0.0592 1.0000 Uani . . . . . . . H131 H 0.5035 0.2662 0.4676 0.0697 1.0000 Uiso R . . . . . . H132 H 0.5160 0.3473 0.5707 0.0697 1.0000 Uiso R . . . . . . H133 H 0.6662 0.3197 0.5055 0.0697 1.0000 Uiso R . . . . . . H101 H 0.6012 0.0381 0.4537 0.0629 1.0000 Uiso R . . . . . . H102 H 0.7669 0.0780 0.4950 0.0629 1.0000 Uiso R . . . . . . H103 H 0.6702 -0.0386 0.5487 0.0629 1.0000 Uiso R . . . . . . H71 H 0.7520 0.2472 0.8910 0.0771 1.0000 Uiso R . . . . . . H72 H 0.6852 0.1010 0.8642 0.0771 1.0000 Uiso R . . . . . . H111 H 0.5743 0.1655 1.0141 0.0679 1.0000 Uiso R . . . . . . H112 H 0.5251 0.3082 0.9679 0.0679 1.0000 Uiso R . . . . . . H41 H 0.7795 0.2166 0.6564 0.0570 1.0000 Uiso R . . . . . . H42 H 0.7103 0.0791 0.7004 0.0570 1.0000 Uiso R . . . . . . 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 Re1 0.03194(15) 0.04221(17) 0.04044(17) 0.0034(3) 0.0024(3) 0.00851(12) I1 0.0354(3) 0.0784(4) 0.0805(5) 0.0112(7) 0.0098(5) -0.0064(3) O1 0.044(4) 0.052(3) 0.085(6) 0.016(4) -0.005(4) 0.020(3) S3 0.0354(11) 0.0462(12) 0.0423(11) -0.0034(10) 0.0022(9) -0.0042(10) S2 0.0385(10) 0.0428(10) 0.0452(14) -0.0070(11) -0.0051(11) 0.0030(8) S4 0.0661(19) 0.0697(18) 0.0413(13) 0.0094(13) 0.0070(12) 0.0106(15) C7 0.043(5) 0.063(6) 0.058(6) -0.015(5) 0.012(5) -0.008(5) C8 0.056(7) 0.070(8) 0.052(6) 0.010(5) 0.015(5) -0.009(6) C6 0.032(5) 0.050(5) 0.037(4) 0.003(4) 0.007(4) -0.007(4) C5 0.030(5) 0.050(6) 0.061(6) -0.004(5) 0.005(4) -0.005(4) C4 0.055(7) 0.086(8) 0.048(5) 0.005(6) -0.019(6) 0.019(7) C3 0.079(9) 0.078(8) 0.033(5) 0.004(5) -0.006(5) 0.012(8) _refine_ls_extinction_coef 22(2) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.1192(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . I1 . 2.7001(7) yes Re1 . O1 . 1.679(6) yes Re1 . S3 . 2.278(2) yes Re1 . S2 . 2.334(2) yes Re1 . S4 . 2.286(3) yes S3 . C6 . 1.876(9) yes S2 . C5 . 1.796(10) yes S2 . C4 . 1.831(11) yes S4 . C3 . 1.848(14) yes C7 . C6 . 1.506(13) yes C7 . H101 . 1.001 no C7 . H102 . 1.005 no C7 . H103 . 1.000 no C8 . C6 . 1.519(15) yes C8 . H131 . 0.991 no C8 . H132 . 1.035 no C8 . H133 . 0.995 no C6 . C5 . 1.524(14) yes C5 . H41 . 1.007 no C5 . H42 . 1.005 no C4 . C3 . 1.471(16) yes C4 . H71 . 1.034 no C4 . H72 . 1.007 no C3 . H111 . 0.996 no C3 . H112 . 1.025 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I1 . Re1 . O1 . 102.3(3) yes I1 . Re1 . S3 . 84.46(6) yes O1 . Re1 . S3 . 116.4(3) yes I1 . Re1 . S2 . 156.18(6) yes O1 . Re1 . S2 . 101.5(3) yes S3 . Re1 . S2 . 84.86(9) yes I1 . Re1 . S4 . 84.92(9) yes O1 . Re1 . S4 . 116.2(3) yes S3 . Re1 . S4 . 127.38(12) yes S2 . Re1 . S4 . 84.76(11) yes Re1 . S3 . C6 . 107.0(3) yes Re1 . S2 . C5 . 107.7(3) yes Re1 . S2 . C4 . 107.1(5) yes C5 . S2 . C4 . 102.3(6) yes Re1 . S4 . C3 . 106.6(4) yes C6 . C7 . H101 . 109.1 no C6 . C7 . H102 . 110.1 no H101 . C7 . H102 . 109.0 no C6 . C7 . H103 . 110.0 no H101 . C7 . H103 . 109.4 no H102 . C7 . H103 . 109.1 no C6 . C8 . H131 . 110.5 no C6 . C8 . H132 . 109.6 no H131 . C8 . H132 . 107.4 no C6 . C8 . H133 . 111.5 no H131 . C8 . H133 . 110.7 no H132 . C8 . H133 . 107.1 no S3 . C6 . C8 . 109.2(7) yes S3 . C6 . C7 . 107.1(7) yes C8 . C6 . C7 . 110.6(8) yes S3 . C6 . C5 . 107.3(6) yes C8 . C6 . C5 . 112.1(9) yes C7 . C6 . C5 . 110.3(9) yes C6 . C5 . S2 . 110.8(7) yes C6 . C5 . H41 . 109.5 no S2 . C5 . H41 . 109.1 no C6 . C5 . H42 . 109.7 no S2 . C5 . H42 . 109.2 no H41 . C5 . H42 . 108.5 no S2 . C4 . C3 . 108.8(8) yes S2 . C4 . H71 . 105.9 no C3 . C4 . H71 . 114.4 no S2 . C4 . H72 . 106.9 no C3 . C4 . H72 . 114.0 no H71 . C4 . H72 . 106.3 no S4 . C3 . C4 . 110.9(9) yes S4 . C3 . H111 . 111.1 no C4 . C3 . H111 . 109.0 no S4 . C3 . H112 . 109.5 no C4 . C3 . H112 . 108.4 no H111 . C3 . H112 . 107.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C5 . H42 . O1 3_646 175 1.00 2.58 3.581(16) yes