#============================================================================= _audit_creation_method SHELXL #============================================================================= # PROCESSING SUMMARY _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? # SUBMISSION DETAILS _publ_contact_author_name ; Prof. Dr. G. Meyer ; _publ_contact_author_address ; Institut f\"ur Anorganische Chemie Universit\"at zu K\"oln Greinstra\&se 6 D-50939 K\"oln Germany ; _publ_contact_author_phone '+49 221 470 3262' _publ_contact_author_fax '+49 221 470 4899' _publ_contact_author_email 'ac118@uni-koeln.de' _publ_requested_category FM _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a regular structural paper in Crystals. ; # TITEL AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_address 'Walbaum, Christine' ; Institut f\"ur Anorganische Chemie Universit\"at zu K\"oln Greinstra\&se 6 D-50939 K\"oln Germany ; 'Pantenburg, Ingo' ; Institut f\"ur Anorganische Chemie Universit\"at zu K\"oln Greinstra\&se 6 D-50939 K\"oln Germany ; 'Meyer, Gerd' ; Institut f\"ur Anorganische Chemie Universit\"at zu K\"oln Greinstra\&se 6 D-50939 K\"oln Germany ; data_cw136 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 O8, I2' _chemical_formula_sum 'C24 H32 I2 O8' _chemical_formula_weight 702.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.8499(11) _cell_length_b 12.037(3) _cell_length_c 12.804(2) _cell_angle_alpha 64.561(15) _cell_angle_beta 86.815(17) _cell_angle_gamma 83.893(17) _cell_volume 671.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5536 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 29.66 _exptl_crystal_description collumn _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 2.387 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5359 _exptl_absorpt_correction_T_max 0.7874 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 13396 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.66 _reflns_number_total 3765 _reflns_number_gt 1965 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0377P)^2^+0.0000P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 'not measured' _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3765 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.835 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.95821(7) -0.52957(3) 1.41265(2) 0.06788(13) Uani 1 1 d . . . O4 O 0.8827(6) -0.6376(2) 1.2515(2) 0.0655(7) Uani 1 1 d . . . O1 O 0.7483(5) -0.8678(2) 1.23802(19) 0.0528(6) Uani 1 1 d . . . O10 O 0.5675(5) -0.1379(2) 0.92057(19) 0.0555(6) Uani 1 1 d . . . O7 O 0.7943(6) -0.3747(2) 1.0986(2) 0.0733(8) Uani 1 1 d . . . C16 C 0.3984(7) -0.0309(3) 0.7313(3) 0.0456(7) Uani 1 1 d . . . C11 C 0.5698(7) -0.0343(3) 0.8169(3) 0.0451(7) Uani 1 1 d . . . C2 C 0.9112(8) -0.8624(3) 1.3249(3) 0.0558(9) Uani 1 1 d . . . H00A H 1.0459 -0.9340 1.3549 0.071(3) Uiso 1 1 calc R . . H00B H 0.7931 -0.8617 1.3884 0.071(3) Uiso 1 1 calc R . . C3 C 1.0563(8) -0.7466(4) 1.2711(4) 0.0632(10) Uani 1 1 d . . . H00C H 1.2065 -0.7532 1.3210 0.071(3) Uiso 1 1 calc R . . H00D H 1.1375 -0.7397 1.1978 0.071(3) Uiso 1 1 calc R . . C12 C 0.7276(8) 0.0632(3) 0.7937(3) 0.0558(9) Uani 1 1 d . . . H010 H 0.8447 0.0612 0.8497 0.077(6) Uiso 1 1 calc R . . C14 C 0.5410(8) 0.1690(3) 0.6038(3) 0.0631(10) Uani 1 1 d . . . H011 H 0.5286 0.2379 0.5328 0.077(6) Uiso 1 1 calc R . . C15 C 0.3846(8) 0.0705(3) 0.6252(3) 0.0576(9) Uani 1 1 d . . . H012 H 0.2708 0.0731 0.5680 0.077(6) Uiso 1 1 calc R . . C13 C 0.7102(9) 0.1643(3) 0.6858(3) 0.0638(10) Uani 1 1 d . . . H013 H 0.8170 0.2295 0.6703 0.077(6) Uiso 1 1 calc R . . C5 C 0.7368(9) -0.5836(3) 1.1469(3) 0.0629(10) Uani 1 1 d . . . H01A H 0.5992 -0.6369 1.1478 0.071(3) Uiso 1 1 calc R . . H01B H 0.8640 -0.5733 1.0828 0.071(3) Uiso 1 1 calc R . . C6 C 0.5985(9) -0.4615(4) 1.1316(4) 0.0695(11) Uani 1 1 d . . . H01C H 0.4572 -0.4345 1.0729 0.071(3) Uiso 1 1 calc R . . H01D H 0.5091 -0.4684 1.2036 0.071(3) Uiso 1 1 calc R . . C8 C 0.7047(11) -0.2659(3) 1.1126(3) 0.0737(12) Uani 1 1 d . . . H01E H 0.8003 -0.2662 1.1772 0.071(3) Uiso 1 1 calc R . . H01F H 0.5074 -0.2643 1.1298 0.071(3) Uiso 1 1 calc R . . C9 C 0.7610(9) -0.1530(3) 1.0057(3) 0.0615(10) Uani 1 1 d . . . H01G H 0.7422 -0.0812 1.0224 0.071(3) Uiso 1 1 calc R . . H01H H 0.9485 -0.1621 0.9780 0.071(3) Uiso 1 1 calc 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 I1 0.0930(2) 0.06316(17) 0.04721(14) -0.02027(10) -0.00849(11) -0.01641(13) O4 0.0864(19) 0.0615(15) 0.0564(14) -0.0345(12) -0.0222(13) 0.0132(14) O1 0.0565(15) 0.0527(13) 0.0498(12) -0.0200(10) -0.0067(11) -0.0125(11) O10 0.0672(16) 0.0502(13) 0.0458(12) -0.0149(10) -0.0070(11) -0.0130(12) O7 0.090(2) 0.0483(14) 0.0784(18) -0.0257(13) 0.0134(16) -0.0067(14) C16 0.0422(19) 0.0441(17) 0.0502(17) -0.0207(14) 0.0029(15) -0.0016(15) C11 0.049(2) 0.0407(16) 0.0458(16) -0.0196(13) 0.0029(14) -0.0018(15) C2 0.053(2) 0.063(2) 0.0555(19) -0.0300(17) -0.0082(17) -0.0008(18) C3 0.060(2) 0.069(2) 0.073(2) -0.040(2) -0.0141(19) -0.003(2) C12 0.061(2) 0.0509(19) 0.058(2) -0.0247(16) 0.0028(18) -0.0124(17) C14 0.067(3) 0.0470(19) 0.058(2) -0.0077(16) 0.007(2) -0.0030(18) C15 0.052(2) 0.060(2) 0.0511(19) -0.0161(16) -0.0042(17) 0.0022(18) C13 0.066(3) 0.049(2) 0.073(2) -0.0232(18) 0.013(2) -0.0141(19) C5 0.074(3) 0.061(2) 0.058(2) -0.0258(17) -0.0115(19) -0.016(2) C6 0.065(3) 0.075(3) 0.066(2) -0.027(2) -0.021(2) 0.000(2) C8 0.109(4) 0.057(2) 0.051(2) -0.0223(17) -0.007(2) 0.004(2) C9 0.084(3) 0.0506(19) 0.0543(19) -0.0262(16) -0.0163(19) 0.0000(19) _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 I1 I1 2.6839(7) 2_748 ? O4 C5 1.407(4) . ? O4 C3 1.414(5) . ? O1 C16 1.374(4) 2_647 ? O1 C2 1.427(4) . ? O10 C11 1.377(4) . ? O10 C9 1.417(4) . ? O7 C6 1.399(5) . ? O7 C8 1.417(5) . ? C16 O1 1.374(4) 2_647 ? C16 C15 1.381(5) . ? C16 C11 1.397(5) . ? C11 C12 1.384(5) . ? C2 C3 1.497(5) . ? C12 C13 1.394(5) . ? C14 C13 1.348(5) . ? C14 C15 1.395(5) . ? C5 C6 1.485(6) . ? C8 C9 1.494(5) . ? 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 O4 C3 116.0(3) . . ? C16 O1 C2 117.7(3) 2_647 . ? C11 O10 C9 118.1(3) . . ? C6 O7 C8 114.6(3) . . ? O1 C16 C15 125.0(3) 2_647 . ? O1 C16 C11 115.4(3) 2_647 . ? C15 C16 C11 119.7(3) . . ? O10 C11 C12 124.7(3) . . ? O10 C11 C16 115.8(3) . . ? C12 C11 C16 119.5(3) . . ? O1 C2 C3 108.1(3) . . ? O4 C3 C2 114.2(3) . . ? C11 C12 C13 119.7(4) . . ? C13 C14 C15 120.0(3) . . ? C16 C15 C14 120.2(4) . . ? C14 C13 C12 121.0(3) . . ? O4 C5 C6 109.3(3) . . ? O7 C6 C5 109.8(3) . . ? O7 C8 C9 111.1(3) . . ? O10 C9 C8 108.3(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.66 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.641 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.079