# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '7071_web_deposit_cif_file_0_Liu,Yen-Hsiang_1315361790.ccdc_deposit_HT18A.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-01-26 _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 'Liu, Yen-Hsiang' # Name of author for correspondence _publ_contact_author_address ;Department of Chemistry Fu Jen Catholic University New Taipei City 24205, Taiwan ; # Address of author for correspondence _publ_contact_author_email chem2022@mails.fju.edu.tw _publ_contact_author_fax 886(2)29023209 _publ_contact_author_phone 886(2)29053570 _publ_contact_letter ; Submission dated :2011-09-07 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 part of a journal submission Liu, Yen-Hsiang ; #============================================================================== # # 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_name _publ_author_footnote _publ_author_address #<--'Last name, first name' 'Liu, Yen-Hsiang' ; ? ; ;Department of Chemistry Fu Jen Catholic University New Taipei City 24205, Taiwan ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_p-1 _database_code_depnum_ccdc_archive 'CCDC 843261' #TrackingRef '7071_web_deposit_cif_file_0_Liu,Yen-Hsiang_1315361790.ccdc_deposit_HT18A.cif' _audit_creation_date 2011-01-26T15:02:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common HT18A _chemical_formula_moiety 'C9 H8 Co O8, H2 O' _chemical_formula_sum 'C9 H10 Co O9' _chemical_formula_weight 321.1 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9177(5) _cell_length_b 7.2342(4) _cell_length_c 12.4632(10) _cell_angle_alpha 78.221(2) _cell_angle_beta 89.685(2) _cell_angle_gamma 64.885(5) _cell_volume 550.53(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 17986 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 326 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.6342 _exptl_absorpt_correction_T_max 0.9230 _exptl_special_details ; Comment on transmission values: The program SADABS (v2.06) outputs the ratio of minimum to maximum apparent transmission (0.687109). We have set T(max) to the expected value, i.e. exp(-r_min*mu) and we calculate T(min) from the minimum to maximum apparent transmission given by SADABS. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.756915E-1 _diffrn_orient_matrix_ub_12 -0.621955E-1 _diffrn_orient_matrix_ub_13 0.538584E-1 _diffrn_orient_matrix_ub_21 0.138657 _diffrn_orient_matrix_ub_22 -0.901653E-1 _diffrn_orient_matrix_ub_23 0.463189E-1 _diffrn_orient_matrix_ub_31 -0.273659E-1 _diffrn_orient_matrix_ub_32 0.111925 _diffrn_orient_matrix_ub_33 0.415742E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_unetI/netI 0.0781 _diffrn_reflns_number 7386 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.32 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 1999 _reflns_number_gt 1552 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1331P)^2^+1.8675P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1999 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.108 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.2399 _refine_ls_wR_factor_gt 0.2266 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.768 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.223 #----------------------------------------------------------------------------# # 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' Co Co 0.3494 0.9721 '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' 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 Co1 Co 0 0.5 0 0.0230(5) Uani 1 2 d S . . Co2 Co -0.5 1 0 0.0227(5) Uani 1 2 d S . . O1 O 0.0357(10) 0.7053(11) 0.6585(5) 0.0459(16) Uani 1 1 d . . . O2 O -0.2704(9) 0.7845(10) 0.5611(5) 0.0386(15) Uani 1 1 d . . . H2 H -0.3169 0.7763 0.6235 0.058 Uiso 1 1 calc R . . O3 O 0.4953(9) 0.5829(9) 0.1560(5) 0.0364(14) Uani 1 1 d . . . O4 O 0.2943(8) 0.9246(8) 0.1019(4) 0.0250(12) Uani 1 1 d . . . O5 O 0.0144(8) 0.6805(9) 0.1021(4) 0.0280(12) Uani 1 1 d . . . O6 O -0.2993(8) 0.9153(8) 0.1446(4) 0.0260(12) Uani 1 1 d . . . O81 O 0.0373(9) 0.7125(8) -0.1247(5) 0.0324(13) Uani 1 1 d . . . H81A H -0.0571 0.826 -0.1135 0.049 Uiso 1 1 d R . . H81B H 0.0346 0.7309 -0.1942 0.049 Uiso 1 1 d R . . O82 O -0.3431(8) 0.6781(8) -0.0211(4) 0.0260(12) Uani 1 1 d . . . H82A H -0.3717 0.582 0.0178 0.039 Uiso 1 1 d R . . H82B H -0.3695 0.6754 -0.0875 0.039 Uiso 1 1 d R . . O91 O -0.4697(10) 0.7740(10) 0.7424(6) 0.0429(16) Uani 1 1 d . . . H91A H -0.5618 0.8843 0.7591 0.064 Uiso 1 1 d R . . H91B H -0.537 0.7063 0.7289 0.064 Uiso 1 1 d R . . C1 C -0.0681(14) 0.7465(13) 0.5719(7) 0.0314(19) Uani 1 1 d . . . C2 C 0.0290(12) 0.7574(12) 0.4638(7) 0.0273(17) Uani 1 1 d . . . C3 C 0.2418(13) 0.7292(13) 0.4651(7) 0.0335(19) Uani 1 1 d . . . H3 H 0.3183 0.7096 0.5336 0.04 Uiso 1 1 d R . . C4 C 0.3410(13) 0.7246(13) 0.3696(7) 0.0307(18) Uani 1 1 d . . . H4 H 0.4863 0.7081 0.3701 0.037 Uiso 1 1 d R . . C5 C 0.2303(12) 0.7500(12) 0.2708(6) 0.0259(17) Uani 1 1 d . . . C6 C 0.3457(12) 0.7502(12) 0.1679(7) 0.0255(17) Uani 1 1 d . . . C7 C 0.0165(12) 0.7817(12) 0.2694(7) 0.0261(17) Uani 1 1 d . . . C8 C -0.0983(12) 0.7944(11) 0.1630(6) 0.0247(16) Uani 1 1 d . . . C9 C -0.0836(12) 0.7849(11) 0.3650(7) 0.0251(16) Uani 1 1 d . . . H9 H -0.2306 0.807 0.364 0.03 Uiso 1 1 d 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 Co1 0.0245(8) 0.0206(8) 0.0180(8) -0.0045(6) 0.0017(5) -0.0041(6) Co2 0.0232(8) 0.0199(8) 0.0194(8) -0.0025(6) 0.0022(5) -0.0049(6) O1 0.049(4) 0.058(4) 0.025(4) -0.008(3) 0.005(3) -0.019(3) O2 0.038(3) 0.052(4) 0.022(3) -0.008(3) 0.008(3) -0.016(3) O3 0.034(3) 0.023(3) 0.036(4) 0.004(3) 0.012(2) -0.002(2) O4 0.029(3) 0.021(3) 0.017(3) 0.001(2) 0.002(2) -0.005(2) O5 0.032(3) 0.034(3) 0.021(3) -0.015(2) 0.006(2) -0.012(2) O6 0.022(3) 0.030(3) 0.020(3) -0.007(2) 0.001(2) -0.005(2) O81 0.038(3) 0.023(3) 0.025(3) -0.001(2) 0.008(2) -0.004(2) O82 0.027(3) 0.023(3) 0.023(3) -0.007(2) 0.003(2) -0.005(2) O91 0.044(3) 0.034(3) 0.048(4) -0.016(3) 0.013(3) -0.012(3) C1 0.044(5) 0.026(4) 0.020(5) -0.004(3) 0.001(4) -0.013(4) C2 0.036(4) 0.023(4) 0.020(4) -0.005(3) 0.005(3) -0.010(3) C3 0.037(5) 0.032(4) 0.025(5) -0.003(4) -0.007(3) -0.012(4) C4 0.030(4) 0.033(4) 0.021(4) 0.001(3) -0.001(3) -0.009(3) C5 0.029(4) 0.023(4) 0.023(4) -0.008(3) 0.004(3) -0.008(3) C6 0.024(4) 0.025(4) 0.024(4) -0.004(3) 0.002(3) -0.008(3) C7 0.030(4) 0.021(4) 0.025(4) -0.010(3) 0.005(3) -0.007(3) C8 0.031(4) 0.020(4) 0.020(4) 0.001(3) 0.004(3) -0.011(3) C9 0.029(4) 0.019(4) 0.022(4) -0.004(3) -0.001(3) -0.006(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Co1 O5 2.031(5) . ? Co1 O5 2.031(5) 2_565 ? Co1 O81 2.050(6) . ? Co1 O81 2.050(6) 2_565 ? Co1 O82 2.153(5) 2_565 ? Co1 O82 2.153(5) . ? Co2 O4 2.071(5) 1_455 ? Co2 O4 2.071(5) 2_575 ? Co2 O6 2.099(5) . ? Co2 O6 2.099(5) 2_475 ? Co2 O82 2.184(5) 2_475 ? Co2 O82 2.184(5) . ? O1 C1 1.210(11) . ? O2 C1 1.309(10) . ? O2 H2 0.84 . ? O3 C6 1.251(9) . ? O4 C6 1.262(9) . ? O4 Co2 2.071(5) 1_655 ? O5 C8 1.251(9) . ? O6 C8 1.281(9) . ? O81 H81A 0.8427 . ? O81 H81B 0.8481 . ? O82 H82A 0.8578 . ? O82 H82B 0.8545 . ? O91 H91A 0.8488 . ? O91 H91B 0.8443 . ? C1 C2 1.505(11) . ? C2 C9 1.393(11) . ? C2 C3 1.397(12) . ? C3 C4 1.370(12) . ? C3 H3 0.9596 . ? C4 C5 1.391(11) . ? C4 H4 0.9605 . ? C5 C7 1.397(11) . ? C5 C6 1.508(11) . ? C7 C9 1.375(11) . ? C7 C8 1.515(11) . ? C9 H9 0.9597 . ? 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 O5 Co1 O5 180.0(2) . 2_565 ? O5 Co1 O81 86.6(2) . . ? O5 Co1 O81 93.4(2) 2_565 . ? O5 Co1 O81 93.4(2) . 2_565 ? O5 Co1 O81 86.6(2) 2_565 2_565 ? O81 Co1 O81 180.0(4) . 2_565 ? O5 Co1 O82 91.3(2) . 2_565 ? O5 Co1 O82 88.7(2) 2_565 2_565 ? O81 Co1 O82 88.7(2) . 2_565 ? O81 Co1 O82 91.3(2) 2_565 2_565 ? O5 Co1 O82 88.7(2) . . ? O5 Co1 O82 91.3(2) 2_565 . ? O81 Co1 O82 91.3(2) . . ? O81 Co1 O82 88.7(2) 2_565 . ? O82 Co1 O82 180.00(15) 2_565 . ? O4 Co2 O4 180.0(4) 1_455 2_575 ? O4 Co2 O6 85.6(2) 1_455 . ? O4 Co2 O6 94.4(2) 2_575 . ? O4 Co2 O6 94.4(2) 1_455 2_475 ? O4 Co2 O6 85.6(2) 2_575 2_475 ? O6 Co2 O6 180 . 2_475 ? O4 Co2 O82 89.78(19) 1_455 2_475 ? O4 Co2 O82 90.22(19) 2_575 2_475 ? O6 Co2 O82 89.9(2) . 2_475 ? O6 Co2 O82 90.1(2) 2_475 2_475 ? O4 Co2 O82 90.22(19) 1_455 . ? O4 Co2 O82 89.78(19) 2_575 . ? O6 Co2 O82 90.1(2) . . ? O6 Co2 O82 89.9(2) 2_475 . ? O82 Co2 O82 180.0(3) 2_475 . ? C1 O2 H2 109.5 . . ? C6 O4 Co2 124.6(5) . 1_655 ? C8 O5 Co1 141.1(5) . . ? C8 O6 Co2 128.3(5) . . ? Co1 O81 H81A 101 . . ? Co1 O81 H81B 135.2 . . ? H81A O81 H81B 104.6 . . ? Co1 O82 Co2 122.3(2) . . ? Co1 O82 H82A 96.1 . . ? Co2 O82 H82A 120.9 . . ? Co1 O82 H82B 100.7 . . ? Co2 O82 H82B 109.6 . . ? H82A O82 H82B 104.2 . . ? H91A O91 H91B 106.4 . . ? O1 C1 O2 125.1(8) . . ? O1 C1 C2 121.8(8) . . ? O2 C1 C2 113.1(7) . . ? C9 C2 C3 120.0(7) . . ? C9 C2 C1 121.9(7) . . ? C3 C2 C1 118.0(7) . . ? C4 C3 C2 120.0(8) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 119.5 . . ? C4 C5 C7 119.6(7) . . ? C4 C5 C6 117.9(7) . . ? C7 C5 C6 122.5(7) . . ? O3 C6 O4 123.7(7) . . ? O3 C6 C5 118.9(7) . . ? O4 C6 C5 117.2(6) . . ? C9 C7 C5 120.4(7) . . ? C9 C7 C8 120.2(7) . . ? C5 C7 C8 119.2(7) . . ? O5 C8 O6 126.2(7) . . ? O5 C8 C7 115.8(6) . . ? O6 C8 C7 118.0(7) . . ? C7 C9 C2 119.6(7) . . ? C7 C9 H9 120.4 . . ? C2 C9 H9 119.9 . . ? 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 O2 H2 O91 0.84 1.82 2.645(9) 168.2 . O81 H81A O4 0.84 1.89 2.724(7) 172 2_575 O81 H81B O1 0.85 1.88 2.713(9) 166.2 1_554 O82 H82A O3 0.86 1.95 2.570(8) 128.3 1_455 O82 H82A O81 0.86 2.52 2.938(7) 110.9 2_565 O82 H82B O91 0.85 2.11 2.934(9) 161.5 1_554 O91 H91A O6 0.85 2 2.794(8) 156.4 2_476 O91 H91B O3 0.84 2.19 2.711(9) 120.1 2_566 # 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