# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 #TrackingRef '- 1_ccdc_deposit.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-12-02 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Rossin, A. et al.' # Name of author for correspondence _publ_contact_author_address ;ICCOM-CNR, Florence (Italy) ; # Address of author for correspondence _publ_contact_author_email a.rossin@iccom.cnr.it _publ_contact_author_fax 39(055)5225203 _publ_contact_author_phone 39(055)5225248 _publ_contact_letter ; Submission dated :2009-12-02 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as a personal communication This CIF is submitted as part of a journal submission Rossin A. et al. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_footnote _publ_author_address #<--'Last name, first name' ; ? ; ;ICCOM-CNR, Florence (Italy) ; loop_ _publ_author_name A.Rossin 'Barbara Di Credico' 'Giuliano Giambastiani' 'Maurizio Peruzzini' 'Gennaro Pescitelli' 'Gianna Reginato' 'Elisa Borfecchia' 'Diego Gianolio' 'Carlo Lamberti' 'Silvia Bordiga' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_1 _database_code_depnum_ccdc_archive 'CCDC 855629' #TrackingRef '- 1_ccdc_deposit.cif' _audit_creation_date 2009-12-02T15:49:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C5 H9 Co1 N O6 S' _chemical_formula_sum 'C5 H9 Co N O6 S' _chemical_formula_weight 270.13 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration rm #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 12.335(4) _cell_length_b 12.335(4) _cell_length_c 5.265(3) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 801.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2655 _cell_measurement_theta_min 3.845 _cell_measurement_theta_max 28.7561 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour magenta _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41' _symmetry_space_group_name_Hall 'P 4w' _symmetry_Int_Tables_number 76 _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90107 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 -0.0473610638 _diffrn_orient_matrix_ub_12 0.0321654793 _diffrn_orient_matrix_ub_13 -0.0068829195 _diffrn_orient_matrix_ub_21 -0.0307367067 _diffrn_orient_matrix_ub_22 -0.046522031 _diffrn_orient_matrix_ub_23 -0.0292392913 _diffrn_orient_matrix_ub_31 -0.0093862553 _diffrn_orient_matrix_ub_32 -0.0087646853 _diffrn_orient_matrix_ub_33 0.1307186508 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0445 _diffrn_reflns_number 4373 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 28.95 _diffrn_reflns_theta_full 28.95 _diffrn_measured_fraction_theta_full 0.874 _diffrn_measured_fraction_theta_max 0.874 _reflns_number_total 1769 _reflns_number_gt 1608 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1769 _refine_ls_number_parameters 131 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.061 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(17) _refine_diff_density_max 0.551 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2954(2) -0.2057(2) 0.7195(6) 0.0103(6) Uani 1 1 d . . . H1A H 0.2633 -0.1968 0.5464 0.012 Uiso 1 1 calc R . . C2 C 0.3448(3) -0.3186(2) 0.7393(6) 0.0126(7) Uani 1 1 d . . . H2A H 0.3824 -0.3386 0.58 0.015 Uiso 1 1 calc R . . H2B H 0.2883 -0.3735 0.7761 0.015 Uiso 1 1 calc R . . C3 C 0.4756(3) -0.1694(2) 0.9008(6) 0.0097(6) Uani 1 1 d . . . H3 H 0.5423 -0.1715 0.7927 0.012 Uiso 1 1 calc R . . C4 C 0.5016(3) 0.1048(3) 0.6402(6) 0.0105(6) Uani 1 1 d . . . C5 C 0.1866(2) 0.2062(2) 1.1684(6) 0.0092(6) Uani 1 1 d . . . N1 N 0.3837(2) -0.1259(2) 0.7506(5) 0.0097(6) Uani 1 1 d . . . H1 H 0.402(3) -0.103(3) 0.616(7) 0.012 Uiso 1 1 d . . . O1 O 0.41676(17) 0.12869(17) 0.7570(4) 0.0131(5) Uani 1 1 d . . . O2 O 0.43148(16) -0.03323(17) 1.2112(4) 0.0111(4) Uani 1 1 d . . . O3 O 0.20776(18) -0.10089(18) 1.0465(4) 0.0143(5) Uani 1 1 d . . . O4 O 0.2081(2) 0.0518(2) 0.6625(5) 0.0190(6) Uani 1 1 d D . . H4A H 0.1448(18) 0.027(3) 0.655(8) 0.023 Uiso 1 1 d D . . H4B H 0.223(3) 0.077(3) 0.524(5) 0.023 Uiso 1 1 d D . . O5 O 0.25686(17) 0.13228(17) 1.1920(5) 0.0122(4) Uani 1 1 d . . . O6 O 0.0026(7) -0.0137(6) 0.9637(17) 0.0575(18) Uiso 0.5 1 d P . . S1 S 0.43970(6) -0.30770(6) 0.99992(15) 0.01326(18) Uani 1 1 d . . . Co1 Co 0.32124(3) 0.01546(3) 0.94137(7) 0.00913(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0090(15) 0.0125(15) 0.0094(16) -0.0022(13) -0.0006(13) -0.0039(12) C2 0.0116(16) 0.0136(16) 0.0127(16) -0.0026(13) -0.0003(13) -0.0014(12) C3 0.0085(15) 0.0105(15) 0.0101(15) 0.0015(12) 0.0005(12) 0.0006(12) C4 0.0106(16) 0.0107(16) 0.0102(15) -0.0019(12) -0.0016(12) -0.0038(13) C5 0.0100(15) 0.0101(15) 0.0075(15) -0.0008(13) 0.0003(13) 0.0010(12) N1 0.0087(14) 0.0115(14) 0.0089(14) 0.0010(11) 0.0020(11) -0.0018(11) O1 0.0100(11) 0.0112(11) 0.0180(13) 0.0015(10) 0.0051(9) 0.0007(9) O2 0.0119(11) 0.0107(11) 0.0107(10) -0.0026(10) -0.0015(10) 0.0000(9) O3 0.0144(12) 0.0116(12) 0.0168(12) -0.0024(9) 0.0040(10) -0.0028(10) O4 0.0160(12) 0.0285(14) 0.0126(12) 0.0108(11) -0.0033(11) -0.0026(10) O5 0.0151(11) 0.0101(11) 0.0114(10) -0.0013(10) 0.0004(10) 0.0044(9) S1 0.0143(4) 0.0092(4) 0.0162(4) 0.0005(3) -0.0034(3) -0.0003(3) Co1 0.0081(2) 0.0092(2) 0.01004(19) 0.00029(17) 0.00046(17) -0.00044(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.477(4) . ? C1 C2 1.523(4) . ? C1 C5 1.537(4) 4_554 ? C1 H1A 1 . ? C2 S1 1.809(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 N1 1.483(4) . ? C3 C4 1.517(4) 2_655 ? C3 S1 1.839(3) . ? C3 H3 1 . ? C4 O1 1.250(4) . ? C4 O2 1.265(4) 2_654 ? C4 C3 1.517(4) 2_654 ? C5 O3 1.254(4) 3 ? C5 O5 1.264(4) . ? C5 C1 1.537(4) 3 ? N1 Co1 2.154(3) . ? N1 H1 0.80(4) . ? O1 Co1 2.069(2) . ? O2 C4 1.265(4) 2_655 ? O2 Co1 2.056(2) . ? O3 C5 1.254(4) 4_554 ? O3 Co1 2.080(2) . ? O4 Co1 2.075(3) . ? O4 H4A 0.840(19) . ? O4 H4B 0.812(19) . ? O5 Co1 2.109(2) . ? O6 O6 1.338(2) 3 ? O6 O6 1.338(2) 4_554 ? 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 N1 C1 C2 107.9(2) . . ? N1 C1 C5 110.5(2) . 4_554 ? C2 C1 C5 112.3(2) . 4_554 ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? C5 C1 H1A 108.7 4_554 . ? C1 C2 S1 104.0(2) . . ? C1 C2 H2A 111 . . ? S1 C2 H2A 111 . . ? C1 C2 H2B 111 . . ? S1 C2 H2B 111 . . ? H2A C2 H2B 109 . . ? N1 C3 C4 113.2(3) . 2_655 ? N1 C3 S1 107.6(2) . . ? C4 C3 S1 107.2(2) 2_655 . ? N1 C3 H3 109.6 . . ? C4 C3 H3 109.6 2_655 . ? S1 C3 H3 109.6 . . ? O1 C4 O2 124.4(3) . 2_654 ? O1 C4 C3 116.1(3) . 2_654 ? O2 C4 C3 119.4(3) 2_654 2_654 ? O3 C5 O5 122.4(3) 3 . ? O3 C5 C1 119.0(3) 3 3 ? O5 C5 C1 118.6(3) . 3 ? C1 N1 C3 112.4(2) . . ? C1 N1 Co1 109.11(19) . . ? C3 N1 Co1 108.53(19) . . ? C1 N1 H1 110(3) . . ? C3 N1 H1 113(3) . . ? Co1 N1 H1 103(3) . . ? C4 O1 Co1 123.3(2) . . ? C4 O2 Co1 115.5(2) 2_655 . ? C5 O3 Co1 116.7(2) 4_554 . ? Co1 O4 H4A 125(3) . . ? Co1 O4 H4B 124(3) . . ? H4A O4 H4B 108(4) . . ? C5 O5 Co1 133.6(2) . . ? O6 O6 O6 165.2(6) 3 4_554 ? C2 S1 C3 90.56(15) . . ? O2 Co1 O1 98.32(9) . . ? O2 Co1 O4 175.48(10) . . ? O1 Co1 O4 84.56(10) . . ? O2 Co1 O3 93.42(9) . . ? O1 Co1 O3 166.89(9) . . ? O4 Co1 O3 83.38(10) . . ? O2 Co1 O5 90.93(10) . . ? O1 Co1 O5 92.68(9) . . ? O4 Co1 O5 92.42(11) . . ? O3 Co1 O5 92.96(9) . . ? O2 Co1 N1 81.32(11) . . ? O1 Co1 N1 97.11(10) . . ? O4 Co1 N1 94.90(11) . . ? O3 Co1 N1 78.84(10) . . ? O5 Co1 N1 168.29(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.80(4) 2.32(4) 3.117(4) 173(4) 1_554 O4 H4A O6 0.840(19) 2.01(2) 2.830(8) 164(4) 4_554 O4 H4A O6 0.840(19) 2.09(3) 2.841(9) 149(4) 2_554 O4 H4A O6 0.840(19) 2.44(3) 3.098(9) 135(4) . O4 H4B O5 0.812(19) 1.924(19) 2.735(4) 178(4) 1_554 O4 H4B O3 0.812(19) 2.51(3) 3.027(4) 122(3) 3_554 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF