####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data___Sulflower _audit_block_doi 10.5517/ccqlsbd _database_code_depnum_ccdc_archive 'CCDC 673454' loop_ _citation_id _citation_doi _citation_year 1 10.1002/chem.200800519 2008 _audit_update_record ; 2008-01-09 deposited with the CCDC. 2020-11-05 downloaded from the CCDC. ; #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 S8 ' _chemical_formula_moiety 'C16 S8 ' _chemical_formula_weight 448.66 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 3.869(2) _cell_length_b 16.529(9) _cell_length_c 11.146(6) _cell_angle_alpha 90.0000 _cell_angle_beta 94.023(10) _cell_angle_gamma 90.0000 _cell_volume 711.0(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1586 _cell_measurement_theta_min 3.7 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.096 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448.00 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.883 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 5559 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1604 _reflns_number_gt 1185 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1681 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 1604 _refine_ls_number_parameters 110 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.87 _refine_diff_density_min -0.53 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) S 0.0558(3) 0.77124(7) 1.05779(11) 0.0155(3) Uani 1.00 1 d . . . S(2) S 0.1788(3) 0.80258(7) 0.77939(11) 0.0157(3) Uani 1.00 1 d . . . S(3) S 0.4920(3) 0.94902(8) 0.62818(11) 0.0176(3) Uani 1.00 1 d . . . S(4) S 0.8132(3) 1.12604(7) 0.69541(11) 0.0164(3) Uani 1.00 1 d . . . C(1) C 0.1850(11) 0.8532(2) 1.1501(4) 0.0145(9) Uani 1.00 1 d . . . C(2) C 0.3166(11) 0.9157(2) 1.0862(4) 0.0129(9) Uani 1.00 1 d . . . C(3) C 0.1852(11) 0.8245(3) 0.9333(4) 0.0142(9) Uani 1.00 1 d . . . C(4) C 0.3182(11) 0.8994(2) 0.9620(4) 0.0135(9) Uani 1.00 1 d . . . C(5) C 0.3622(12) 0.8980(2) 0.7542(4) 0.0146(9) Uani 1.00 1 d . . . C(6) C 0.4235(12) 0.9423(2) 0.8589(4) 0.0157(10) Uani 1.00 1 d . . . C(7) C 0.6251(12) 1.0307(2) 0.7198(4) 0.0158(10) Uani 1.00 1 d . . . C(8) C 0.5749(12) 1.0183(2) 0.8379(4) 0.0131(9) Uani 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0155(6) 0.0164(6) 0.0143(6) -0.0015(4) -0.0011(4) 0.0019(4) S(2) 0.0200(6) 0.0141(5) 0.0125(6) -0.0024(4) -0.0018(4) 0.0004(4) S(3) 0.0244(6) 0.0183(6) 0.0100(6) -0.0023(5) -0.0001(4) 0.0009(4) S(4) 0.0203(6) 0.0168(6) 0.0120(6) -0.0007(4) 0.0006(4) 0.0027(4) C(1) 0.012(2) 0.019(2) 0.013(2) 0.0036(19) 0.0015(17) -0.0022(18) C(2) 0.013(2) 0.016(2) 0.010(2) -0.0012(19) 0.0028(17) -0.0002(18) C(3) 0.012(2) 0.018(2) 0.012(2) 0.0005(18) 0.0012(18) 0.0006(18) C(4) 0.010(2) 0.015(2) 0.015(2) -0.0001(18) -0.0007(18) -0.0003(18) C(5) 0.016(2) 0.015(2) 0.013(2) 0.0011(19) 0.0007(18) 0.0000(18) C(6) 0.015(2) 0.017(2) 0.014(2) 0.0058(19) -0.0039(18) 0.0022(18) C(7) 0.019(2) 0.019(2) 0.010(2) 0.002(2) -0.0001(18) 0.0022(18) C(8) 0.015(2) 0.013(2) 0.012(2) 0.0051(18) 0.0042(17) 0.0001(18) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S(1) C(1) 1.752(4) yes . . S(1) C(3) 1.746(4) yes . . S(2) C(3) 1.752(4) yes . . S(2) C(5) 1.760(4) yes . . S(3) C(5) 1.742(5) yes . . S(3) C(7) 1.748(4) yes . . S(4) C(1) 1.755(4) yes . 3_677 S(4) C(7) 1.765(4) yes . . C(1) C(2) 1.373(6) yes . . C(2) C(4) 1.411(6) yes . . C(2) C(8) 1.425(6) yes . 3_677 C(3) C(4) 1.369(6) yes . . C(4) C(6) 1.434(6) yes . . C(5) C(6) 1.385(6) yes . . C(6) C(8) 1.413(6) yes . . C(7) C(8) 1.360(6) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(1) S(1) C(3) 89.5(2) yes . . . C(3) S(2) C(5) 89.6(2) yes . . . C(5) S(3) C(7) 89.6(2) yes . . . C(1) S(4) C(7) 89.8(2) yes 3_677 . . S(1) C(1) S(4) 135.1(2) yes . . 3_677 S(1) C(1) C(2) 112.2(3) yes . . . S(4) C(1) C(2) 112.6(3) yes 3_677 . . C(1) C(2) C(4) 113.1(4) yes . . . C(1) C(2) C(8) 111.9(4) yes . . 3_677 C(4) C(2) C(8) 135.0(4) yes . . 3_677 S(1) C(3) S(2) 133.5(2) yes . . . S(1) C(3) C(4) 113.2(3) yes . . . S(2) C(3) C(4) 113.3(3) yes . . . C(2) C(4) C(3) 112.0(4) yes . . . C(2) C(4) C(6) 135.4(4) yes . . . C(3) C(4) C(6) 112.5(4) yes . . . S(2) C(5) S(3) 134.8(2) yes . . . S(2) C(5) C(6) 112.7(3) yes . . . S(3) C(5) C(6) 112.4(3) yes . . . C(4) C(6) C(5) 111.8(4) yes . . . C(4) C(6) C(8) 135.9(4) yes . . . C(5) C(6) C(8) 112.3(4) yes . . . S(3) C(7) S(4) 135.0(2) yes . . . S(3) C(7) C(8) 113.1(3) yes . . . S(4) C(7) C(8) 111.8(3) yes . . . C(2) C(8) C(6) 133.6(4) yes 3_677 . . C(2) C(8) C(7) 113.8(4) yes 3_677 . . C(6) C(8) C(7) 112.5(4) yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) S(1) C(3) S(2) -179.4(3) ? . . . . C(1) S(1) C(3) C(4) 0.2(3) ? . . . . C(3) S(1) C(1) C(2) 0.0(3) ? . . . . C(3) S(1) C(1) S(4) -179.8(2) ? . . . 3_677 C(3) S(2) C(5) S(3) 179.0(4) ? . . . . C(3) S(2) C(5) C(6) 0.3(3) ? . . . . C(5) S(2) C(3) S(1) 179.6(3) ? . . . . C(5) S(2) C(3) C(4) 0.0(3) ? . . . . C(5) S(3) C(7) S(4) -179.9(3) ? . . . . C(5) S(3) C(7) C(8) 0.6(3) ? . . . . C(7) S(3) C(5) S(2) -179.1(4) ? . . . . C(7) S(3) C(5) C(6) -0.5(3) ? . . . . C(1) S(4) C(7) S(3) -179.9(2) ? 3_677 . . . C(1) S(4) C(7) C(8) -0.4(3) ? 3_677 . . . C(7) S(4) C(1) S(1) -179.2(3) ? . . 3_677 3_677 C(7) S(4) C(1) C(2) 0.5(3) ? . . 3_677 3_677 S(1) C(1) C(2) C(4) -0.2(4) ? . . . . S(1) C(1) C(2) C(8) -179.3(3) ? . . . 3_677 S(4) C(1) C(2) C(4) 179.6(3) ? 3_677 . . . S(4) C(1) C(2) C(8) 0.6(5) ? 3_677 . . 3_677 C(1) C(2) C(4) C(3) 0.4(5) ? . . . . C(1) C(2) C(4) C(6) 180.0(4) ? . . . . C(1) C(2) C(8) C(6) 179.3(5) ? . . 3_677 3_677 C(1) C(2) C(8) C(7) -0.3(5) ? . . 3_677 3_677 C(4) C(2) C(8) C(6) 0.6(9) ? . . 3_677 3_677 C(4) C(2) C(8) C(7) -179.1(5) ? . . 3_677 3_677 C(8) C(2) C(4) C(3) 179.1(5) ? 3_677 . . . C(8) C(2) C(4) C(6) -1.3(9) ? 3_677 . . . S(1) C(3) C(4) C(2) -0.3(5) ? . . . . S(1) C(3) C(4) C(6) 180.0(2) ? . . . . S(2) C(3) C(4) C(2) 179.4(3) ? . . . . S(2) C(3) C(4) C(6) -0.3(5) ? . . . . C(2) C(4) C(6) C(5) -179.0(5) ? . . . . C(2) C(4) C(6) C(8) 1.2(9) ? . . . . C(3) C(4) C(6) C(5) 0.6(5) ? . . . . C(3) C(4) C(6) C(8) -179.2(5) ? . . . . S(2) C(5) C(6) C(4) -0.6(5) ? . . . . S(2) C(5) C(6) C(8) 179.2(3) ? . . . . S(3) C(5) C(6) C(4) -179.5(3) ? . . . . S(3) C(5) C(6) C(8) 0.3(5) ? . . . . C(4) C(6) C(8) C(2) -0.5(8) ? . . . 3_677 C(4) C(6) C(8) C(7) 179.9(4) ? . . . . C(5) C(6) C(8) C(2) 179.8(4) ? . . . 3_677 C(5) C(6) C(8) C(7) 0.1(4) ? . . . . S(3) C(7) C(8) C(2) 179.8(3) ? . . . 3_677 S(3) C(7) C(8) C(6) -0.5(5) ? . . . . S(4) C(7) C(8) C(2) 0.1(4) ? . . . 3_677 S(4) C(7) C(8) C(6) 179.8(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S(1) S(2) 3.1972(17) ? . 4_465 S(1) S(2) 3.5446(16) ? . 4_565 S(2) S(1) 3.5446(16) ? . 4_464 S(2) S(1) 3.1972(17) ? . 4_564 S(2) S(4) 3.5059(16) ? . 2_546 S(2) S(4) 3.5185(16) ? . 2_646 S(2) C(1) 3.459(4) ? . 4_464 S(2) C(1) 3.597(4) ? . 4_564 S(2) C(5) 3.524(4) ? . 1_455 S(3) S(3) 3.3217(17) ? . 3_676 S(4) S(2) 3.5059(16) ? . 2_556 S(4) S(2) 3.5185(16) ? . 2_656 S(4) C(7) 3.508(5) ? . 1_655 C(1) S(2) 3.597(4) ? . 4_465 C(1) S(2) 3.459(4) ? . 4_565 C(1) C(2) 3.539(6) ? . 1_455 C(2) C(1) 3.539(6) ? . 1_655 C(3) C(6) 3.581(6) ? . 1_455 C(5) S(2) 3.524(4) ? . 1_655 C(5) C(7) 3.597(6) ? . 1_455 C(6) C(3) 3.581(6) ? . 1_655 C(6) C(8) 3.508(6) ? . 1_455 C(7) S(4) 3.508(5) ? . 1_455 C(7) C(5) 3.597(6) ? . 1_655 C(8) C(6) 3.508(6) ? . 1_655 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================

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