# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1762 #=============================================================================== data_global #=============================================================================== _audit_creation_date 09-05-00 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; ; _publ_contact_author_address # Address of author for correspondance ; ; _publ_contact_author_phone 'xxxxxxxxxx' _publ_contact_author_fax 'xxxxxxxxxx' _publ_contact_author_email xxx@xx.xx.xx _publ_requested_journal 'Acta Crystallographica C' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # 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_address 'Dupont Karl' #<--'Last name, first name' ; Research School of Chemistry National Laboratory Ouchnock Islandia ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st614 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H24 Cl2 Co N2 O2 S2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H24 Cl2 Co N2 O2 S2' _chemical_formula_weight 494.37 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Co ? 0.299 0.973 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2-y,1/2+z -x,+y,1/2-z 1/2+x,1/2-y,-z -x,-y,-z 1/2+x,1/2+y,1/2-z +x,-y,1/2+z 1/2-x,1/2+y,+z _cell_length_a 13.3874(4) _cell_length_b 13.9184(7) _cell_length_c 12.0950(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2253.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 4941 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 4941 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 40 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 68 frames Set 2 Theta = -5.20 Kappa = -140.00 Phi = 0.00 16 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4941 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2903 _reflns_number_gt 1739 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1739 _refine_ls_number_parameters 120 _refine_ls_number_restraints 28 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_all 0.125 _refine_ls_wR_factor_ref 0.075 _refine_ls_goodness_of_fit_all 2.209 _refine_ls_goodness_of_fit_ref 1.376 _refine_ls_shift/su_max 0.002 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.870 _refine_diff_density_min -0.756 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CO 0.5000 0.30583(4) 0.2500 0.0153(3) 0.500 Uani ? ? Co CL 0.62650(7) 0.30771(7) 0.10642(6) 0.0275(4) 1.000 Uani ? ? Cl N1 0.5000 0.1536(3) 0.2500 0.020(2) 0.500 Uani ? ? N C1 0.5397(3) 0.1042(3) 0.3354(3) 0.023(2) 1.000 Uani ? ? C C2 0.5426(3) 0.0043(3) 0.3373(3) 0.025(2) 1.000 Uani ? ? C C3 0.5000 -0.0476(4) 0.2500 0.023(2) 0.500 Uani ? ? C C4 0.5758(3) 0.1616(3) 0.4348(3) 0.026(2) 1.000 Uani ? ? C S 0.62017(7) 0.28126(7) 0.40454(7) 0.0248(4) 1.000 Uani ? ? S C5 0.7421(3) 0.2569(4) 0.3473(3) 0.048(2) 1.000 Uani ? ? C N2 0.5000 0.4579(3) 0.2500 0.019(2) 0.500 Uani ? ? N C6 0.5259(3) 0.5090(3) 0.3402(3) 0.023(2) 1.000 Uani ? ? C C7 0.5266(3) 0.6078(3) 0.3441(3) 0.023(2) 1.000 Uani ? ? C C8 0.5000 0.6598(4) 0.2500 0.021(2) 0.500 Uani ? ? C C9 0.5000 0.7629(4) 0.2500 0.025(3) 0.500 Uani ? ? C C10 0.5000 -0.1504(4) 0.2500 0.025(3) 0.500 Uani ? ? C C11 0.2538(3) 0.0504(4) 0.3892(4) 0.057(1) 1.000 Uiso ? ? C O2 0.2373(4) -0.0040(4) 0.4819(4) 0.056(1) 0.600 Uiso ? ? O O2a 0.3274(7) 0.0871(6) 0.4503(7) 0.076(3) 0.400 Uiso ? ? O H1 0.5733 -0.0285 0.3972 0.0344 1.000 Uiso calc C2 H H2 0.6289 0.1269 0.4683 0.0398 1.000 Uiso calc C4 H H3 0.5219 0.1669 0.4854 0.0398 1.000 Uiso calc C4 H H4 0.7735 0.3157 0.3278 0.0681 1.000 Uiso calc C5 H H5 0.7816 0.2243 0.4006 0.0681 1.000 Uiso calc C5 H H6 0.7353 0.2178 0.2833 0.0681 1.000 Uiso calc C5 H H7 0.5448 0.4748 0.4048 0.0313 1.000 Uiso calc C6 H H8 0.5450 0.6402 0.4102 0.0318 1.000 Uiso calc C7 H 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 _atom_site_aniso_type_symbol CO 0.0247(3) 0.0090(3) 0.0161(3) 0.0000 -0.0014(2) 0.0000 Co CL 0.0336(5) 0.0280(5) 0.0220(4) 0.0037(4) 0.0038(4) 0.0023(3) Cl N1 0.029(2) 0.013(2) 0.020(2) 0.0000 -0.000(2) 0.0000 N C1 0.034(2) 0.017(2) 0.023(2) 0.000(2) 0.001(2) 0.001(1) C C2 0.036(2) 0.016(2) 0.027(2) 0.004(2) 0.001(2) 0.004(1) C C3 0.032(3) 0.014(2) 0.027(2) 0.0000 0.006(2) 0.0000 C C4 0.052(2) 0.014(2) 0.026(2) 0.002(2) -0.008(2) 0.004(1) C S 0.0331(5) 0.0184(4) 0.0251(4) -0.0010(4) -0.0064(4) -0.0012(4) S C5 0.030(2) 0.081(3) 0.046(2) 0.011(2) -0.006(2) 0.011(2) C N2 0.026(2) 0.015(2) 0.016(2) 0.0000 0.000(2) 0.0000 N C6 0.034(2) 0.018(2) 0.020(2) 0.002(2) -0.003(1) 0.002(1) C C7 0.034(2) 0.017(2) 0.023(2) -0.000(2) -0.003(1) -0.004(1) C C8 0.025(2) 0.014(2) 0.026(2) 0.0000 -0.000(2) 0.0000 C C9 0.029(3) 0.020(3) 0.026(3) 0.0000 0.002(2) 0.0000 C C10 0.028(3) 0.017(2) 0.032(3) 0.0000 0.000(2) 0.0000 C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CO CL 2.4258(9) . . ? CO CL 2.4258(9) . 3_655 ? CO N1 2.119(4) . . ? CO N1 2.119(4) . 3_655 ? CO S 2.4897(9) . . ? CO S 2.4897(9) . 3_655 ? CO N2 2.117(4) . . ? CO N2 2.117(4) . 3_655 ? N1 C1 1.350(4) . . ? N1 C1 1.350(4) . 3_655 ? C1 C2 1.391(5) . . ? C1 C4 1.522(5) . . ? C2 C3 1.400(5) . . ? C2 C3 1.400(5) . 3_655 ? C3 C10 1.430(8) . . ? C3 C10 1.430(8) . 3_655 ? C4 S 1.806(4) . . ? S C5 1.805(4) . . ? N2 C6 1.347(4) . . ? N2 C6 1.347(4) . 3_655 ? C6 C7 1.376(5) . . ? C7 C8 1.396(5) . . ? C7 C8 1.396(5) . 3_655 ? C8 C9 1.434(7) . . ? C8 C9 1.434(7) . 3_655 ? C9 C10 1.208(9) . ._565 ? C9 C10 1.208(9) . 3_665 ? C11 O2 1.371(7) . . ? C11 O2a 1.333(9) . . ? O2 O2a 1.79(1) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL CO CL 178.77(5) . . 3_655 ? CL CO N1 90.62(3) . . . ? CL CO S 95.04(3) . . . ? CL CO S 85.13(3) . . 3_655 ? CL CO N2 89.38(3) . . . ? CL CO N1 90.62(3) . 3_655 . ? CL CO S 85.13(3) . 3_655 . ? CL CO S 95.04(3) . 3_655 3_655 ? CL CO N2 89.38(3) . 3_655 . ? N1 CO S 82.11(3) . . . ? N1 CO S 82.11(3) . . 3_655 ? N1 CO N2 180.00 . . . ? S CO S 164.21(5) . . 3_655 ? S CO N2 97.89(3) . . . ? S CO N2 97.89(3) . 3_655 . ? C1 N1 C1 118.8(5) . . 3_655 ? N1 C1 C2 122.2(3) . . . ? N1 C1 C4 117.5(3) . . . ? C2 C1 C4 120.2(3) . . . ? C1 C2 C3 119.5(4) . . . ? C2 C3 C2 117.9(5) . . 3_655 ? C2 C3 C10 121.1(2) . . . ? C2 C3 C10 121.1(2) . 3_655 . ? C1 C4 S 115.4(2) . . . ? C4 S C5 101.6(2) . . . ? C6 N2 C6 116.3(4) . . 3_655 ? N2 C6 C7 123.9(3) . . . ? C6 C7 C8 119.3(3) . . . ? C7 C8 C7 117.4(5) . . 3_655 ? C7 C8 C9 121.3(2) . . . ? C7 C8 C9 121.3(2) . 3_655 . ? C8 C9 C10 180.00 . . ._565 ? C3 C10 C9 180.00 . . ._545 ? O2 C11 O2a 82.9(5) . . . ? C11 O2 O2a 47.6(4) . . . ? C11 O2a O2 49.4(4) . . . ?