# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '1a_AGK15-1b_sanz.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-07-06 _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 'Sanz Miguel, Pablo J.' _publ_contact_author_address ;Department of Bioinorganic Chemistry TU Dortmund University Otto-Hahn-Strasse 6 44227 Dortmund, Germany ; # Address of author for correspondence _publ_contact_author_email pablo.sanz@uni-dortmund.de _publ_contact_author_fax 49(231)7553797 _publ_contact_author_phone 49(231)7555034 _publ_contact_letter ; Submission dated :2010-07-06 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 ; #============================================================================== # # 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 'Agnes Kozma' ; ? ; ;Department of Bioinorganic Chemistry TU Dortmund University Otto-Hahn-Strasse 6 44227 Dortmund, Germany ; 'Susana Ibanez' '' '' 'Pablo J. Sanz Miguel' '' '' 'Deepali Gupta' '' '' 'Bernhard Lippert' '' '' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_1a_AGK15-1b_sanz _database_code_depnum_ccdc_archive 'CCDC 831963' #TrackingRef '1a_AGK15-1b_sanz.cif' _audit_creation_date 2010-07-06T11:06:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 N5 O, N O3' _chemical_formula_sum 'C6 H8 N6 O4' _chemical_formula_weight 228.18 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3469(7) _cell_length_b 6.6534(7) _cell_length_c 10.9527(13) _cell_angle_alpha 88.543(10) _cell_angle_beta 89.933(9) _cell_angle_gamma 72.034(10) _cell_volume 439.81(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1713 _cell_measurement_theta_min 3.2114 _cell_measurement_theta_max 29.1421 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 236 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_unetI/netI 0.0674 _diffrn_reflns_number 3362 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.822 _reflns_number_total 1962 _reflns_number_gt 1337 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1962 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.496 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # 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' 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 N1 N 0.1950(3) 0.1435(3) 0.46059(16) 0.0152(4) Uani 1 1 d . . . H1A H 0.0914 0.148 0.5149 0.018 Uiso 1 1 calc R . . C2 C 0.3096(4) 0.2860(3) 0.4715(2) 0.0152(5) Uani 1 1 d . . . N2 N 0.2541(3) 0.4179(3) 0.56271(17) 0.0197(4) Uani 1 1 d . . . H2A H 0.3242 0.5115 0.5736 0.024 Uiso 1 1 calc R . . H2B H 0.1472 0.4122 0.6126 0.024 Uiso 1 1 calc R . . N3 N 0.4707(3) 0.2953(3) 0.39685(17) 0.0162(4) Uani 1 1 d . . . C4 C 0.5084(4) 0.1501(4) 0.3096(2) 0.0154(5) Uani 1 1 d . . . C5 C 0.4009(4) 0.0037(4) 0.2910(2) 0.0156(5) Uani 1 1 d . . . C6 C 0.2278(4) -0.0079(3) 0.3711(2) 0.0145(5) Uani 1 1 d . . . O6 O 0.1172(3) -0.1295(3) 0.36910(14) 0.0208(4) Uani 1 1 d . . . N7 N 0.4971(3) -0.1133(3) 0.19262(17) 0.0165(4) Uani 1 1 d . . . C7 C 0.4301(4) -0.2843(4) 0.1405(2) 0.0211(5) Uani 1 1 d . . . H7A H 0.537 -0.354 0.0783 0.032 Uiso 1 1 calc R . . H7B H 0.2829 -0.2263 0.1031 0.032 Uiso 1 1 calc R . . H7C H 0.4256 -0.3873 0.2052 0.032 Uiso 1 1 calc R . . C8 C 0.6574(4) -0.0412(4) 0.1530(2) 0.0185(5) Uani 1 1 d . . . H8A H 0.7512 -0.0947 0.0859 0.022 Uiso 1 1 calc R . . N9 N 0.6673(3) 0.1185(3) 0.22186(17) 0.0168(4) Uani 1 1 d . . . H9A H 0.7609 0.1914 0.2122 0.02 Uiso 1 1 calc R . . N10 N 1.0556(3) 0.3213(3) 0.12523(16) 0.0170(4) Uani 1 1 d . . . O11 O 1.2013(3) 0.3968(3) 0.09489(16) 0.0295(5) Uani 1 1 d . . . O12 O 1.0275(3) 0.1685(3) 0.07247(16) 0.0271(4) Uani 1 1 d . . . O13 O 0.9298(3) 0.3933(3) 0.21447(16) 0.0294(5) 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 N1 0.0142(9) 0.0174(10) 0.0139(9) -0.0045(8) 0.0075(7) -0.0047(8) C2 0.0141(11) 0.0149(11) 0.0157(11) 0.0004(9) -0.0024(9) -0.0033(9) N2 0.0213(10) 0.0234(10) 0.0174(10) -0.0060(8) 0.0054(8) -0.0109(9) N3 0.0175(10) 0.0167(10) 0.0160(9) -0.0036(8) 0.0027(8) -0.0073(8) C4 0.0142(11) 0.0187(11) 0.0144(11) 0.0012(9) 0.0013(9) -0.0067(10) C5 0.0156(11) 0.0158(11) 0.0160(11) -0.0020(9) 0.0027(9) -0.0057(10) C6 0.0153(11) 0.0163(11) 0.0119(10) -0.0044(9) 0.0039(9) -0.0047(10) O6 0.0251(9) 0.0237(9) 0.0201(9) -0.0111(7) 0.0108(7) -0.0161(8) N7 0.0164(10) 0.0170(10) 0.0163(10) -0.0021(8) 0.0014(8) -0.0055(8) C7 0.0271(13) 0.0199(12) 0.0176(11) -0.0108(10) 0.0047(10) -0.0084(11) C8 0.0154(11) 0.0201(12) 0.0183(12) -0.0007(10) 0.0027(9) -0.0033(10) N9 0.0155(10) 0.0211(10) 0.0162(9) -0.0030(8) 0.0051(8) -0.0091(9) N10 0.0166(10) 0.0206(10) 0.0135(10) 0.0007(8) 0.0012(8) -0.0055(8) O11 0.0300(10) 0.0384(11) 0.0288(10) 0.0012(8) 0.0035(8) -0.0233(9) O12 0.0314(10) 0.0253(9) 0.0299(10) -0.0084(8) 0.0058(8) -0.0162(9) O13 0.0294(10) 0.0346(11) 0.0242(9) -0.0137(8) 0.0111(8) -0.0086(9) #----------------------------------------------------------------------------# # 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 N1 C2 1.368(3) . ? N1 C6 1.393(3) . ? N1 H1A 0.88 . ? C2 N3 1.324(3) . ? C2 N2 1.321(3) . ? N2 H2A 0.88 . ? N2 H2B 0.88 . ? N3 C4 1.345(3) . ? C4 N9 1.365(3) . ? C4 C5 1.369(3) . ? C5 N7 1.374(3) . ? C5 C6 1.424(3) . ? C6 O6 1.224(2) . ? N7 C8 1.320(3) . ? N7 C7 1.460(3) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 N9 1.336(3) . ? C8 H8A 0.95 . ? N9 H9A 0.88 . ? N10 O11 1.223(2) . ? N10 O12 1.242(2) . ? N10 O13 1.268(2) . ? 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 C2 N1 C6 125.77(19) . . ? C2 N1 H1A 117.1 . . ? C6 N1 H1A 117.1 . . ? N3 C2 N2 119.7(2) . . ? N3 C2 N1 123.4(2) . . ? N2 C2 N1 116.9(2) . . ? C2 N2 H2A 120 . . ? C2 N2 H2B 120 . . ? H2A N2 H2B 120 . . ? C2 N3 C4 112.54(19) . . ? N3 C4 N9 125.81(19) . . ? N3 C4 C5 128.0(2) . . ? N9 C4 C5 106.2(2) . . ? C4 C5 N7 107.7(2) . . ? C4 C5 C6 119.8(2) . . ? N7 C5 C6 132.4(2) . . ? O6 C6 N1 121.0(2) . . ? O6 C6 C5 128.5(2) . . ? N1 C6 C5 110.44(19) . . ? C8 N7 C5 107.86(18) . . ? C8 N7 C7 126.4(2) . . ? C5 N7 C7 125.70(18) . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N7 C8 N9 109.4(2) . . ? N7 C8 H8A 125.3 . . ? N9 C8 H8A 125.3 . . ? C8 N9 C4 108.81(17) . . ? C8 N9 H9A 125.6 . . ? C4 N9 H9A 125.6 . . ? O11 N10 O12 121.8(2) . . ? O11 N10 O13 121.04(19) . . ? O12 N10 O13 117.10(17) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 N3 -0.6(3) . . . . ? C6 N1 C2 N2 179.9(2) . . . . ? N2 C2 N3 C4 179.5(2) . . . . ? N1 C2 N3 C4 0.1(3) . . . . ? C2 N3 C4 N9 -178.3(2) . . . . ? C2 N3 C4 C5 0.7(3) . . . . ? N3 C4 C5 N7 -179.1(2) . . . . ? N9 C4 C5 N7 0.1(2) . . . . ? N3 C4 C5 C6 -0.9(3) . . . . ? N9 C4 C5 C6 178.23(19) . . . . ? C2 N1 C6 O6 179.7(2) . . . . ? C2 N1 C6 C5 0.4(3) . . . . ? C4 C5 C6 O6 -178.9(2) . . . . ? N7 C5 C6 O6 -1.3(4) . . . . ? C4 C5 C6 N1 0.3(3) . . . . ? N7 C5 C6 N1 177.9(2) . . . . ? C4 C5 N7 C8 0.1(2) . . . . ? C6 C5 N7 C8 -177.7(2) . . . . ? C4 C5 N7 C7 -178.9(2) . . . . ? C6 C5 N7 C7 3.2(4) . . . . ? C5 N7 C8 N9 -0.3(2) . . . . ? C7 N7 C8 N9 178.74(19) . . . . ? N7 C8 N9 C4 0.3(2) . . . . ? N3 C4 N9 C8 178.9(2) . . . . ? C5 C4 N9 C8 -0.2(2) . . . . ? # 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 # Attachment '1b_AGK18_sanz.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-04 at 18:09:34 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_1b_AGK18_sanz _database_code_depnum_ccdc_archive 'CCDC 831964' #TrackingRef '1b_AGK18_sanz.cif' _audit_creation_date 2010-08-04T18:09:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 N5 O, Cl O4' _chemical_formula_sum 'C6 H8 Cl N5 O5' _chemical_formula_weight 265.62 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6936(9) _cell_length_b 10.0818(9) _cell_length_c 13.2751(16) _cell_angle_alpha 86.629(8) _cell_angle_beta 89.408(10) _cell_angle_gamma 72.912(9) _cell_volume 982.51(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2629 _cell_measurement_theta_min 2.5375 _cell_measurement_theta_max 29.0192 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.1095 _diffrn_reflns_number 7871 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.08 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.849 _reflns_number_total 4478 _reflns_number_gt 2586 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4478 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.34 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 N1A N 0.7496(3) -0.02590(19) 0.39042(16) 0.0199(5) Uani 1 1 d . . . H1A H 0.7885 -0.0767 0.4464 0.024 Uiso 1 1 calc R . . C2A C 0.6483(3) 0.1104(2) 0.3997(2) 0.0195(6) Uani 1 1 d . . . N2A N 0.6117(3) 0.1501(2) 0.49370(16) 0.0288(6) Uani 1 1 d . . . H21A H 0.5478 0.2361 0.504 0.035 Uiso 1 1 calc R . . H22A H 0.6514 0.0903 0.5453 0.035 Uiso 1 1 calc R . . N3A N 0.5888(3) 0.19985(19) 0.32299(16) 0.0170(5) Uani 1 1 d . . . C4A C 0.6349(3) 0.1422(2) 0.2336(2) 0.0171(6) Uani 1 1 d . . . C5A C 0.7333(3) 0.0083(2) 0.2176(2) 0.0142(6) Uani 1 1 d . . . C6A C 0.7955(3) -0.0900(2) 0.29988(19) 0.0158(6) Uani 1 1 d . . . O6A O 0.8802(2) -0.21363(15) 0.29883(13) 0.0206(4) Uani 1 1 d . . . N7A N 0.7442(3) -0.00395(19) 0.11424(16) 0.0158(5) Uani 1 1 d . . . C7A C 0.8320(3) -0.1305(2) 0.06231(19) 0.0229(7) Uani 1 1 d . . . H71A H 0.8392 -0.107 -0.01 0.034 Uiso 1 1 calc R . . H72A H 0.7607 -0.1963 0.0724 0.034 Uiso 1 1 calc R . . H73A H 0.9549 -0.1729 0.0898 0.034 Uiso 1 1 calc R . . C8A C 0.6589(3) 0.1185(2) 0.0702(2) 0.0196(6) Uani 1 1 d . . . H8A H 0.6464 0.1391 -0.0006 0.024 Uiso 1 1 calc R . . N9A N 0.5927(3) 0.20895(19) 0.14089(16) 0.0194(5) Uani 1 1 d . . . H9A H 0.5318 0.2972 0.1294 0.023 Uiso 1 1 calc R . . N1B N 0.8969(2) 0.36826(18) 0.54192(16) 0.0171(5) Uani 1 1 d . . . H1B H 0.9496 0.3239 0.5978 0.021 Uiso 1 1 calc R . . C2B C 0.7562(3) 0.4884(2) 0.5516(2) 0.0160(6) Uani 1 1 d . . . N2B N 0.7134(3) 0.5262(2) 0.64464(16) 0.0220(5) Uani 1 1 d . . . H21B H 0.6256 0.6028 0.6548 0.026 Uiso 1 1 calc R . . H22B H 0.7728 0.4748 0.6964 0.026 Uiso 1 1 calc R . . N3B N 0.6666(3) 0.56606(19) 0.47402(16) 0.0168(5) Uani 1 1 d . . . C4B C 0.7298(3) 0.5151(2) 0.38508(19) 0.0140(6) Uani 1 1 d . . . C5B C 0.8695(3) 0.3967(2) 0.3690(2) 0.0155(6) Uani 1 1 d . . . C6B C 0.9621(3) 0.3117(2) 0.45136(19) 0.0188(6) Uani 1 1 d . . . O6B O 1.0862(2) 0.20101(16) 0.44882(13) 0.0275(5) Uani 1 1 d . . . C7B C 1.0221(3) 0.2750(2) 0.21585(19) 0.0219(6) Uani 1 1 d . . . H71B H 1.0162 0.2969 0.1428 0.033 Uiso 1 1 calc R . . H72B H 0.9958 0.1865 0.2303 0.033 Uiso 1 1 calc R . . H73B H 1.1441 0.2678 0.2409 0.033 Uiso 1 1 calc R . . N7B N 0.8871(3) 0.38604(19) 0.26619(16) 0.0158(5) Uani 1 1 d . . . C8B C 0.7642(3) 0.4913(2) 0.2215(2) 0.0172(6) Uani 1 1 d . . . H8B H 0.748 0.5089 0.1506 0.021 Uiso 1 1 calc R . . N9B N 0.6651(3) 0.57014(19) 0.29153(16) 0.0183(5) Uani 1 1 d . . . H9B H 0.5731 0.6453 0.2793 0.022 Uiso 1 1 calc R . . Cl1 Cl 0.24331(8) 0.52810(6) 0.07600(5) 0.01768(16) Uani 1 1 d . . . O11 O 0.2246(2) 0.64449(15) 0.00556(13) 0.0276(5) Uani 1 1 d . . . O12 O 0.0989(2) 0.55960(16) 0.14774(13) 0.0243(4) Uani 1 1 d . . . O13 O 0.4159(2) 0.49707(15) 0.12980(13) 0.0245(5) Uani 1 1 d . . . O14 O 0.2420(2) 0.40823(16) 0.02340(13) 0.0283(5) Uani 1 1 d . . . Cl2 Cl 0.31280(8) 0.89141(6) 0.23027(5) 0.01919(16) Uani 1 1 d . . . O21 O 0.1507(2) 0.94741(16) 0.17171(14) 0.0311(5) Uani 1 1 d . . . O22 O 0.4660(2) 0.84590(18) 0.16488(15) 0.0354(5) Uani 1 1 d . . . O23 O 0.3023(2) 0.77238(16) 0.29225(14) 0.0327(5) Uani 1 1 d . . . O24 O 0.3405(2) 0.99335(16) 0.29360(14) 0.0281(5) 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 N1A 0.0251(13) 0.0149(11) 0.0153(14) 0.0016(10) 0.0001(11) 0.0004(9) C2A 0.0192(15) 0.0179(14) 0.0209(18) -0.0042(13) 0.0011(13) -0.0041(11) N2A 0.0452(16) 0.0195(12) 0.0139(15) -0.0023(11) 0.0001(12) 0.0028(11) N3A 0.0256(13) 0.0125(11) 0.0110(14) 0.0003(10) -0.0002(11) -0.0025(9) C4A 0.0189(15) 0.0164(14) 0.0158(17) 0.0008(12) -0.0014(13) -0.0054(11) C5A 0.0133(14) 0.0158(13) 0.0133(16) -0.0005(11) 0.0025(12) -0.0040(11) C6A 0.0153(15) 0.0210(15) 0.0117(16) -0.0022(12) -0.0003(12) -0.0062(11) O6A 0.0266(10) 0.0132(9) 0.0167(11) 0.0008(8) -0.0019(9) 0.0022(8) N7A 0.0200(12) 0.0128(11) 0.0134(14) -0.0018(10) 0.0011(10) -0.0027(9) C7A 0.0329(17) 0.0167(14) 0.0154(17) -0.0067(12) 0.0016(14) -0.0004(12) C8A 0.0265(16) 0.0196(15) 0.0127(16) -0.0002(12) 0.0010(13) -0.0069(12) N9A 0.0261(13) 0.0112(11) 0.0148(14) 0.0023(10) 0.0007(11) 0.0033(9) N1B 0.0236(13) 0.0146(11) 0.0087(13) 0.0022(10) -0.0032(10) 0.0008(9) C2B 0.0186(15) 0.0147(14) 0.0156(17) -0.0034(12) 0.0022(13) -0.0062(11) N2B 0.0280(14) 0.0212(12) 0.0111(14) -0.0020(10) -0.0012(11) 0.0020(10) N3B 0.0195(12) 0.0167(11) 0.0113(14) -0.0004(10) 0.0010(10) -0.0007(9) C4B 0.0147(14) 0.0161(13) 0.0116(16) 0.0010(11) -0.0040(12) -0.0053(11) C5B 0.0183(15) 0.0127(13) 0.0148(17) -0.0026(12) 0.0045(13) -0.0031(11) C6B 0.0237(15) 0.0185(14) 0.0147(17) -0.0015(13) -0.0003(13) -0.0069(12) O6B 0.0352(11) 0.0209(10) 0.0146(12) -0.0002(9) -0.0001(9) 0.0100(8) C7B 0.0259(16) 0.0223(14) 0.0137(17) -0.0034(12) 0.0009(13) -0.0006(11) N7B 0.0202(13) 0.0138(11) 0.0123(14) 0.0004(10) -0.0005(10) -0.0034(9) C8B 0.0219(15) 0.0197(14) 0.0091(16) -0.0005(12) -0.0012(13) -0.0049(12) N9B 0.0198(12) 0.0146(11) 0.0152(15) 0.0017(10) -0.0021(11) 0.0028(9) Cl1 0.0208(4) 0.0170(3) 0.0137(4) 0.0000(3) -0.0003(3) -0.0031(3) O11 0.0350(12) 0.0201(10) 0.0229(13) 0.0097(9) 0.0056(10) -0.0030(8) O12 0.0200(10) 0.0325(11) 0.0173(12) 0.0037(9) 0.0059(9) -0.0040(8) O13 0.0208(11) 0.0245(10) 0.0263(13) -0.0038(9) -0.0078(9) -0.0031(8) O14 0.0418(12) 0.0215(10) 0.0242(13) -0.0095(9) -0.0003(10) -0.0118(9) Cl2 0.0193(4) 0.0190(4) 0.0176(4) -0.0004(3) -0.0014(3) -0.0030(3) O21 0.0227(11) 0.0318(11) 0.0343(14) 0.0016(9) -0.0146(10) -0.0012(8) O22 0.0226(11) 0.0530(13) 0.0317(14) -0.0157(11) 0.0099(10) -0.0105(10) O23 0.0453(12) 0.0217(10) 0.0312(14) 0.0094(9) -0.0055(10) -0.0121(9) O24 0.0343(11) 0.0215(10) 0.0293(13) -0.0080(9) -0.0027(10) -0.0083(9) #----------------------------------------------------------------------------# # 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 N1A C2A 1.378(3) . ? N1A C6A 1.391(3) . ? N1A H1A 0.88 . ? C2A N3A 1.312(3) . ? C2A N2A 1.334(3) . ? N2A H21A 0.88 . ? N2A H22A 0.88 . ? N3A C4A 1.350(3) . ? C4A N9A 1.362(3) . ? C4A C5A 1.368(3) . ? C5A N7A 1.384(3) . ? C5A C6A 1.417(3) . ? C6A O6A 1.226(3) . ? N7A C8A 1.320(3) . ? N7A C7A 1.465(3) . ? C7A H71A 0.98 . ? C7A H72A 0.98 . ? C7A H73A 0.98 . ? C8A N9A 1.338(3) . ? C8A H8A 0.95 . ? N9A H9A 0.88 . ? N1B C2B 1.378(3) . ? N1B C6B 1.387(3) . ? N1B H1B 0.88 . ? C2B N3B 1.323(3) . ? C2B N2B 1.324(3) . ? N2B H21B 0.88 . ? N2B H22B 0.88 . ? N3B C4B 1.344(3) . ? C4B N9B 1.367(3) . ? C4B C5B 1.377(3) . ? C5B N7B 1.378(3) . ? C5B C6B 1.409(3) . ? C6B O6B 1.239(3) . ? C7B N7B 1.472(3) . ? C7B H71B 0.98 . ? C7B H72B 0.98 . ? C7B H73B 0.98 . ? N7B C8B 1.312(3) . ? C8B N9B 1.339(3) . ? C8B H8B 0.95 . ? N9B H9B 0.88 . ? Cl1 O11 1.4306(17) . ? Cl1 O12 1.4314(17) . ? Cl1 O14 1.4334(15) . ? Cl1 O13 1.4559(16) . ? Cl2 O21 1.4261(17) . ? Cl2 O24 1.4292(15) . ? Cl2 O22 1.4354(17) . ? Cl2 O23 1.4363(17) . ? 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 C2A N1A C6A 125.5(2) . . ? C2A N1A H1A 117.3 . . ? C6A N1A H1A 117.3 . . ? N3A C2A N2A 119.8(2) . . ? N3A C2A N1A 124.0(2) . . ? N2A C2A N1A 116.2(3) . . ? C2A N2A H21A 120 . . ? C2A N2A H22A 120 . . ? H21A N2A H22A 120 . . ? C2A N3A C4A 112.2(2) . . ? N3A C4A N9A 125.8(2) . . ? N3A C4A C5A 127.6(3) . . ? N9A C4A C5A 106.7(2) . . ? C4A C5A N7A 107.2(2) . . ? C4A C5A C6A 120.7(2) . . ? N7A C5A C6A 132.0(2) . . ? O6A C6A N1A 121.0(2) . . ? O6A C6A C5A 129.0(2) . . ? N1A C6A C5A 109.9(2) . . ? C8A N7A C5A 107.9(2) . . ? C8A N7A C7A 125.7(2) . . ? C5A N7A C7A 126.3(2) . . ? N7A C7A H71A 109.5 . . ? N7A C7A H72A 109.5 . . ? H71A C7A H72A 109.5 . . ? N7A C7A H73A 109.5 . . ? H71A C7A H73A 109.5 . . ? H72A C7A H73A 109.5 . . ? N7A C8A N9A 109.3(2) . . ? N7A C8A H8A 125.3 . . ? N9A C8A H8A 125.3 . . ? C8A N9A C4A 108.9(2) . . ? C8A N9A H9A 125.6 . . ? C4A N9A H9A 125.6 . . ? C2B N1B C6B 125.3(2) . . ? C2B N1B H1B 117.4 . . ? C6B N1B H1B 117.4 . . ? N3B C2B N2B 119.8(2) . . ? N3B C2B N1B 123.7(2) . . ? N2B C2B N1B 116.5(2) . . ? C2B N2B H21B 120 . . ? C2B N2B H22B 120 . . ? H21B N2B H22B 120 . . ? C2B N3B C4B 112.3(2) . . ? N3B C4B N9B 126.5(2) . . ? N3B C4B C5B 127.6(3) . . ? N9B C4B C5B 105.9(2) . . ? C4B C5B N7B 107.4(2) . . ? C4B C5B C6B 120.3(2) . . ? N7B C5B C6B 132.3(2) . . ? O6B C6B N1B 121.6(2) . . ? O6B C6B C5B 127.7(2) . . ? N1B C6B C5B 110.8(2) . . ? N7B C7B H71B 109.5 . . ? N7B C7B H72B 109.5 . . ? H71B C7B H72B 109.5 . . ? N7B C7B H73B 109.5 . . ? H71B C7B H73B 109.5 . . ? H72B C7B H73B 109.5 . . ? C8B N7B C5B 108.4(2) . . ? C8B N7B C7B 126.2(2) . . ? C5B N7B C7B 125.4(2) . . ? N7B C8B N9B 109.3(2) . . ? N7B C8B H8B 125.3 . . ? N9B C8B H8B 125.3 . . ? C8B N9B C4B 109.0(2) . . ? C8B N9B H9B 125.5 . . ? C4B N9B H9B 125.5 . . ? O11 Cl1 O12 109.89(11) . . ? O11 Cl1 O14 109.86(11) . . ? O12 Cl1 O14 110.45(10) . . ? O11 Cl1 O13 109.71(10) . . ? O12 Cl1 O13 108.69(11) . . ? O14 Cl1 O13 108.21(10) . . ? O21 Cl2 O24 110.45(10) . . ? O21 Cl2 O22 109.89(12) . . ? O24 Cl2 O22 109.65(10) . . ? O21 Cl2 O23 110.51(10) . . ? O24 Cl2 O23 108.95(11) . . ? O22 Cl2 O23 107.32(11) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A N1A C2A N3A -3.4(4) . . . . ? C6A N1A C2A N2A 176.8(2) . . . . ? N2A C2A N3A C4A -178.9(2) . . . . ? N1A C2A N3A C4A 1.3(3) . . . . ? C2A N3A C4A N9A -179.9(2) . . . . ? C2A N3A C4A C5A -0.7(3) . . . . ? N3A C4A C5A N7A 179.1(2) . . . . ? N9A C4A C5A N7A -1.6(2) . . . . ? N3A C4A C5A C6A 1.9(4) . . . . ? N9A C4A C5A C6A -178.7(2) . . . . ? C2A N1A C6A O6A -177.1(2) . . . . ? C2A N1A C6A C5A 4.0(3) . . . . ? C4A C5A C6A O6A 177.9(2) . . . . ? N7A C5A C6A O6A 1.6(4) . . . . ? C4A C5A C6A N1A -3.2(3) . . . . ? N7A C5A C6A N1A -179.6(2) . . . . ? C4A C5A N7A C8A 1.1(3) . . . . ? C6A C5A N7A C8A 177.9(2) . . . . ? C4A C5A N7A C7A -177.91(19) . . . . ? C6A C5A N7A C7A -1.2(4) . . . . ? C5A N7A C8A N9A -0.2(3) . . . . ? C7A N7A C8A N9A 178.80(19) . . . . ? N7A C8A N9A C4A -0.7(3) . . . . ? N3A C4A N9A C8A -179.2(2) . . . . ? C5A C4A N9A C8A 1.4(3) . . . . ? C6B N1B C2B N3B -0.8(4) . . . . ? C6B N1B C2B N2B -179.9(2) . . . . ? N2B C2B N3B C4B 178.38(19) . . . . ? N1B C2B N3B C4B -0.7(3) . . . . ? C2B N3B C4B N9B 179.2(2) . . . . ? C2B N3B C4B C5B 0.4(3) . . . . ? N3B C4B C5B N7B -179.7(2) . . . . ? N9B C4B C5B N7B 1.4(2) . . . . ? N3B C4B C5B C6B 1.3(4) . . . . ? N9B C4B C5B C6B -177.69(19) . . . . ? C2B N1B C6B O6B -178.0(2) . . . . ? C2B N1B C6B C5B 2.3(3) . . . . ? C4B C5B C6B O6B 177.9(2) . . . . ? N7B C5B C6B O6B -0.9(4) . . . . ? C4B C5B C6B N1B -2.4(3) . . . . ? N7B C5B C6B N1B 178.8(2) . . . . ? C4B C5B N7B C8B -0.5(3) . . . . ? C6B C5B N7B C8B 178.4(2) . . . . ? C4B C5B N7B C7B 179.30(19) . . . . ? C6B C5B N7B C7B -1.8(4) . . . . ? C5B N7B C8B N9B -0.6(3) . . . . ? C7B N7B C8B N9B 179.59(18) . . . . ? N7B C8B N9B C4B 1.5(3) . . . . ? N3B C4B N9B C8B 179.2(2) . . . . ? C5B C4B N9B C8B -1.8(2) . . . . ? # 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 # Attachment '1c_AGK23.1_sanz.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-04-28 at 18:02:56 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_1c_AGK23.1_sanz _database_code_depnum_ccdc_archive 'CCDC 831965' #TrackingRef '1c_AGK23.1_sanz.cif' _audit_creation_date 2011-04-28T18:02:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H8 N5 O, B F4' _chemical_formula_sum 'C6 H8 B F4 N5 O' _chemical_formula_weight 252.98 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5337(7) _cell_length_b 10.0931(8) _cell_length_c 13.1155(8) _cell_angle_alpha 86.712(6) _cell_angle_beta 89.796(6) _cell_angle_gamma 72.735(8) _cell_volume 950.68(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2964 _cell_measurement_theta_min 2.5469 _cell_measurement_theta_max 28.9714 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0822 _diffrn_reflns_number 7492 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 29.04 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.854 _reflns_number_total 4326 _reflns_number_gt 2481 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4326 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.372 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.07 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 N1A N 0.2489(3) 0.52441(19) 0.11100(14) 0.0200(5) Uani 1 1 d . . . H1A H 0.209 0.5758 0.0544 0.024 Uiso 1 1 calc R . . C2A C 0.3523(3) 0.3892(2) 0.10020(18) 0.0183(5) Uani 1 1 d . . . N2A N 0.3896(3) 0.3493(2) 0.00622(16) 0.0292(6) Uani 1 1 d . . . H21A H 0.4548 0.2631 -0.0038 0.035 Uiso 1 1 calc R . . H22A H 0.3493 0.409 -0.0463 0.035 Uiso 1 1 calc R . . N3A N 0.4136(3) 0.29858(19) 0.17927(15) 0.0198(5) Uani 1 1 d . . . C4A C 0.3654(3) 0.3564(2) 0.26895(18) 0.0182(5) Uani 1 1 d . . . C5A C 0.2665(3) 0.4905(2) 0.28560(17) 0.0169(5) Uani 1 1 d . . . C6A C 0.2012(3) 0.5877(2) 0.20133(18) 0.0186(5) Uani 1 1 d . . . O6A O 0.1164(2) 0.71193(16) 0.20383(12) 0.0244(4) Uani 1 1 d . . . C7A C 0.1633(4) 0.6292(3) 0.44272(19) 0.0257(6) Uani 1 1 d . . . H71A H 0.1431 0.6045 0.5143 0.038 Uiso 1 1 calc R . . H72A H 0.0436 0.6774 0.4093 0.038 Uiso 1 1 calc R . . H73A H 0.2432 0.6902 0.4396 0.038 Uiso 1 1 calc R . . N7A N 0.2532(3) 0.50273(19) 0.39040(15) 0.0195(5) Uani 1 1 d . . . C8A C 0.3392(4) 0.3792(2) 0.43421(18) 0.0227(6) Uani 1 1 d . . . H8A H 0.3496 0.3577 0.5058 0.027 Uiso 1 1 calc R . . N9A N 0.4088(3) 0.2897(2) 0.36400(15) 0.0220(5) Uani 1 1 d . . . H9A H 0.4726 0.2019 0.3762 0.026 Uiso 1 1 calc R . . N1B N 0.8975(3) -0.13474(19) 0.04110(14) 0.0194(5) Uani 1 1 d . . . H1B H 0.9499 -0.1811 0.0975 0.023 Uiso 1 1 calc R . . C2B C 0.7575(3) -0.0136(2) 0.05191(18) 0.0181(5) Uani 1 1 d . . . N2B N 0.7132(3) 0.0236(2) 0.14560(15) 0.0239(5) Uani 1 1 d . . . H21B H 0.6246 0.101 0.1556 0.029 Uiso 1 1 calc R . . H22B H 0.7723 -0.0289 0.1982 0.029 Uiso 1 1 calc R . . N3B N 0.6672(3) 0.06663(19) -0.02756(14) 0.0177(5) Uani 1 1 d . . . C4B C 0.7313(3) 0.0153(2) -0.11729(18) 0.0157(5) Uani 1 1 d . . . C5B C 0.8712(3) -0.1030(2) -0.13368(18) 0.0171(5) Uani 1 1 d . . . C6B C 0.9637(4) -0.1906(2) -0.04997(18) 0.0195(6) Uani 1 1 d . . . O6B O 1.0881(3) -0.30185(17) -0.05375(13) 0.0309(5) Uani 1 1 d . . . N7B N 0.8918(3) -0.11346(19) -0.23826(14) 0.0182(5) Uani 1 1 d . . . C7B C 1.0284(4) -0.2236(3) -0.28918(19) 0.0258(6) Uani 1 1 d . . . H71B H 1.0153 -0.2047 -0.3633 0.039 Uiso 1 1 calc R . . H72B H 1.0075 -0.3132 -0.2708 0.039 Uiso 1 1 calc R . . H73B H 1.154 -0.2266 -0.2675 0.039 Uiso 1 1 calc R . . C8B C 0.7681(3) -0.0052(2) -0.28293(18) 0.0201(6) Uani 1 1 d . . . H8B H 0.7522 0.014 -0.3546 0.024 Uiso 1 1 calc R . . N9B N 0.6685(3) 0.0734(2) -0.21237(14) 0.0202(5) Uani 1 1 d . . . H9B H 0.577 0.1504 -0.2248 0.024 Uiso 1 1 calc R . . B1 B 0.7528(4) -0.0273(3) 0.4244(2) 0.0219(7) Uani 1 1 d . . . F11 F 0.8948(2) -0.05797(15) 0.35520(11) 0.0318(4) Uani 1 1 d . . . F12 F 0.7512(2) 0.08837(14) 0.47628(11) 0.0322(4) Uani 1 1 d . . . F13 F 0.5840(2) 0.00344(14) 0.36961(11) 0.0315(4) Uani 1 1 d . . . F14 F 0.7682(2) -0.13962(14) 0.49297(11) 0.0320(4) Uani 1 1 d . . . B2 B 0.3172(4) 0.3904(3) -0.2685(2) 0.0221(7) Uani 1 1 d . . . F21 F 0.3465(2) 0.48584(14) -0.20494(11) 0.0327(4) Uani 1 1 d . . . F22 F 0.4698(2) 0.34311(16) -0.33169(12) 0.0375(4) Uani 1 1 d . . . F23 F 0.3032(2) 0.27468(15) -0.20912(12) 0.0368(4) Uani 1 1 d . . . F24 F 0.1590(2) 0.44750(15) -0.32781(12) 0.0345(4) 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 N1A 0.0255(13) 0.0162(10) 0.0122(11) 0.0056(8) -0.0036(9) 0.0022(10) C2A 0.0195(14) 0.0155(12) 0.0172(13) 0.0001(10) -0.0030(11) -0.0013(11) N2A 0.0423(16) 0.0200(11) 0.0158(12) 0.0005(9) -0.0025(10) 0.0050(11) N3A 0.0248(13) 0.0172(10) 0.0136(11) 0.0009(9) -0.0005(9) -0.0008(10) C4A 0.0170(13) 0.0155(12) 0.0195(13) 0.0041(10) -0.0038(10) -0.0019(11) C5A 0.0162(13) 0.0163(12) 0.0142(13) 0.0022(10) -0.0023(10) 0.0009(11) C6A 0.0175(14) 0.0149(12) 0.0221(14) 0.0005(11) -0.0022(11) -0.0031(11) O6A 0.0310(11) 0.0152(9) 0.0200(10) 0.0043(7) -0.0058(8) 0.0027(8) C7A 0.0326(16) 0.0230(13) 0.0169(14) -0.0034(11) 0.0018(12) -0.0011(13) N7A 0.0223(12) 0.0161(10) 0.0156(11) 0.0006(9) -0.0005(9) 0.0006(10) C8A 0.0277(16) 0.0221(13) 0.0143(13) 0.0045(11) -0.0037(11) -0.0022(12) N9A 0.0295(13) 0.0143(10) 0.0153(11) 0.0055(9) -0.0026(9) 0.0031(10) N1B 0.0245(12) 0.0140(10) 0.0129(11) 0.0046(8) -0.0035(9) 0.0040(9) C2B 0.0193(14) 0.0160(12) 0.0174(13) 0.0009(10) -0.0008(10) -0.0030(11) N2B 0.0263(13) 0.0208(11) 0.0162(12) 0.0017(9) -0.0030(10) 0.0055(10) N3B 0.0179(12) 0.0152(10) 0.0149(11) -0.0008(9) -0.0010(9) 0.0029(9) C4B 0.0149(13) 0.0149(12) 0.0158(13) 0.0032(10) -0.0038(10) -0.0029(11) C5B 0.0177(13) 0.0147(12) 0.0162(13) -0.0015(10) -0.0020(10) -0.0006(11) C6B 0.0226(14) 0.0168(12) 0.0161(13) 0.0022(10) -0.0011(11) -0.0016(12) O6B 0.0385(12) 0.0195(9) 0.0191(10) 0.0035(8) -0.0030(9) 0.0145(9) N7B 0.0216(12) 0.0161(10) 0.0131(11) 0.0014(8) -0.0006(9) -0.0003(9) C7B 0.0276(16) 0.0253(14) 0.0190(14) -0.0022(11) 0.0019(12) 0.0004(13) C8B 0.0235(14) 0.0181(12) 0.0151(13) 0.0051(10) -0.0047(11) -0.0019(12) N9B 0.0220(12) 0.0170(10) 0.0144(11) 0.0036(9) -0.0058(9) 0.0044(9) B1 0.0235(17) 0.0179(14) 0.0200(16) 0.0075(12) -0.0047(13) -0.0011(13) F11 0.0282(9) 0.0317(8) 0.0283(9) 0.0053(7) 0.0066(7) 0.0006(7) F12 0.0454(11) 0.0249(8) 0.0250(8) -0.0028(7) -0.0040(7) -0.0081(8) F13 0.0265(9) 0.0281(8) 0.0334(9) -0.0001(7) -0.0103(7) 0.0014(7) F14 0.0403(10) 0.0227(8) 0.0261(9) 0.0111(7) 0.0008(7) -0.0013(8) B2 0.0225(17) 0.0214(15) 0.0172(16) 0.0050(12) -0.0043(13) 0.0003(14) F21 0.0397(10) 0.0274(8) 0.0274(9) -0.0030(7) -0.0049(7) -0.0040(8) F22 0.0298(10) 0.0475(10) 0.0323(9) -0.0086(8) 0.0041(8) -0.0059(8) F23 0.0443(11) 0.0252(8) 0.0352(10) 0.0128(7) -0.0061(8) -0.0042(8) F24 0.0292(9) 0.0316(9) 0.0345(9) 0.0068(7) -0.0146(7) 0.0023(8) #----------------------------------------------------------------------------# # 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 N1A C2A 1.371(3) . ? N1A C6A 1.374(3) . ? N1A H1A 0.88 . ? C2A N2A 1.322(3) . ? C2A N3A 1.330(3) . ? N2A H21A 0.88 . ? N2A H22A 0.88 . ? N3A C4A 1.344(3) . ? C4A C5A 1.367(3) . ? C4A N9A 1.375(3) . ? C5A N7A 1.388(3) . ? C5A C6A 1.421(3) . ? C6A O6A 1.229(3) . ? C7A N7A 1.464(3) . ? C7A H71A 0.98 . ? C7A H72A 0.98 . ? C7A H73A 0.98 . ? N7A C8A 1.321(3) . ? C8A N9A 1.323(3) . ? C8A H8A 0.95 . ? N9A H9A 0.88 . ? N1B C2B 1.371(3) . ? N1B C6B 1.378(3) . ? N1B H1B 0.88 . ? C2B N2B 1.318(3) . ? C2B N3B 1.336(3) . ? N2B H21B 0.88 . ? N2B H22B 0.88 . ? N3B C4B 1.343(3) . ? C4B C5B 1.365(3) . ? C4B N9B 1.370(3) . ? C5B N7B 1.386(3) . ? C5B C6B 1.415(3) . ? C6B O6B 1.234(3) . ? N7B C8B 1.316(3) . ? N7B C7B 1.464(3) . ? C7B H71B 0.98 . ? C7B H72B 0.98 . ? C7B H73B 0.98 . ? C8B N9B 1.332(3) . ? C8B H8B 0.95 . ? N9B H9B 0.88 . ? B1 F11 1.376(3) . ? B1 F12 1.382(3) . ? B1 F14 1.384(3) . ? B1 F13 1.406(3) . ? B2 F21 1.376(3) . ? B2 F24 1.380(3) . ? B2 F22 1.396(3) . ? B2 F23 1.397(3) . ? 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 C2A N1A C6A 126.5(2) . . ? C2A N1A H1A 116.8 . . ? C6A N1A H1A 116.8 . . ? N2A C2A N3A 119.7(2) . . ? N2A C2A N1A 117.3(2) . . ? N3A C2A N1A 122.9(2) . . ? C2A N2A H21A 120 . . ? C2A N2A H22A 120 . . ? H21A N2A H22A 120 . . ? C2A N3A C4A 112.05(19) . . ? N3A C4A C5A 128.2(2) . . ? N3A C4A N9A 125.8(2) . . ? C5A C4A N9A 106.0(2) . . ? C4A C5A N7A 107.8(2) . . ? C4A C5A C6A 119.9(2) . . ? N7A C5A C6A 132.3(2) . . ? O6A C6A N1A 122.1(2) . . ? O6A C6A C5A 127.5(2) . . ? N1A C6A C5A 110.3(2) . . ? N7A C7A H71A 109.5 . . ? N7A C7A H72A 109.5 . . ? H71A C7A H72A 109.5 . . ? N7A C7A H73A 109.5 . . ? H71A C7A H73A 109.5 . . ? H72A C7A H73A 109.5 . . ? C8A N7A C5A 107.1(2) . . ? C8A N7A C7A 126.4(2) . . ? C5A N7A C7A 126.50(19) . . ? N7A C8A N9A 110.2(2) . . ? N7A C8A H8A 124.9 . . ? N9A C8A H8A 124.9 . . ? C8A N9A C4A 108.9(2) . . ? C8A N9A H9A 125.5 . . ? C4A N9A H9A 125.5 . . ? C2B N1B C6B 126.0(2) . . ? C2B N1B H1B 117 . . ? C6B N1B H1B 117 . . ? N2B C2B N3B 119.7(2) . . ? N2B C2B N1B 117.4(2) . . ? N3B C2B N1B 122.9(2) . . ? C2B N2B H21B 120 . . ? C2B N2B H22B 120 . . ? H21B N2B H22B 120 . . ? C2B N3B C4B 112.1(2) . . ? N3B C4B C5B 128.0(2) . . ? N3B C4B N9B 126.3(2) . . ? C5B C4B N9B 105.7(2) . . ? C4B C5B N7B 108.0(2) . . ? C4B C5B C6B 120.2(2) . . ? N7B C5B C6B 131.8(2) . . ? O6B C6B N1B 122.4(2) . . ? O6B C6B C5B 126.9(2) . . ? N1B C6B C5B 110.7(2) . . ? C8B N7B C5B 107.4(2) . . ? C8B N7B C7B 126.5(2) . . ? C5B N7B C7B 126.1(2) . . ? N7B C7B H71B 109.5 . . ? N7B C7B H72B 109.5 . . ? H71B C7B H72B 109.5 . . ? N7B C7B H73B 109.5 . . ? H71B C7B H73B 109.5 . . ? H72B C7B H73B 109.5 . . ? N7B C8B N9B 109.7(2) . . ? N7B C8B H8B 125.1 . . ? N9B C8B H8B 125.1 . . ? C8B N9B C4B 109.2(2) . . ? C8B N9B H9B 125.4 . . ? C4B N9B H9B 125.4 . . ? F11 B1 F12 111.3(2) . . ? F11 B1 F14 110.5(2) . . ? F12 B1 F14 109.9(2) . . ? F11 B1 F13 107.8(2) . . ? F12 B1 F13 107.8(2) . . ? F14 B1 F13 109.5(2) . . ? F21 B2 F24 111.0(2) . . ? F21 B2 F22 110.3(2) . . ? F24 B2 F22 109.5(2) . . ? F21 B2 F23 108.7(2) . . ? F24 B2 F23 110.8(2) . . ? F22 B2 F23 106.5(2) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A N1A C2A N2A -177.3(2) . . . . ? C6A N1A C2A N3A 3.2(4) . . . . ? N2A C2A N3A C4A 179.3(2) . . . . ? N1A C2A N3A C4A -1.3(3) . . . . ? C2A N3A C4A C5A -0.2(4) . . . . ? C2A N3A C4A N9A -179.7(2) . . . . ? N3A C4A C5A N7A -179.1(2) . . . . ? N9A C4A C5A N7A 0.5(3) . . . . ? N3A C4A C5A C6A 0.0(4) . . . . ? N9A C4A C5A C6A 179.6(2) . . . . ? C2A N1A C6A O6A 175.9(2) . . . . ? C2A N1A C6A C5A -3.1(3) . . . . ? C4A C5A C6A O6A -177.4(2) . . . . ? N7A C5A C6A O6A 1.5(5) . . . . ? C4A C5A C6A N1A 1.5(3) . . . . ? N7A C5A C6A N1A -179.6(2) . . . . ? C4A C5A N7A C8A -0.9(3) . . . . ? C6A C5A N7A C8A -179.9(3) . . . . ? C4A C5A N7A C7A 178.2(2) . . . . ? C6A C5A N7A C7A -0.8(4) . . . . ? C5A N7A C8A N9A 1.0(3) . . . . ? C7A N7A C8A N9A -178.2(2) . . . . ? N7A C8A N9A C4A -0.7(3) . . . . ? N3A C4A N9A C8A 179.7(2) . . . . ? C5A C4A N9A C8A 0.1(3) . . . . ? C6B N1B C2B N2B -179.8(2) . . . . ? C6B N1B C2B N3B -0.3(4) . . . . ? N2B C2B N3B C4B 178.8(2) . . . . ? N1B C2B N3B C4B -0.7(3) . . . . ? C2B N3B C4B C5B -0.2(3) . . . . ? C2B N3B C4B N9B -179.7(2) . . . . ? N3B C4B C5B N7B -178.9(2) . . . . ? N9B C4B C5B N7B 0.7(3) . . . . ? N3B C4B C5B C6B 2.0(4) . . . . ? N9B C4B C5B C6B -178.4(2) . . . . ? C2B N1B C6B O6B -178.5(2) . . . . ? C2B N1B C6B C5B 1.9(3) . . . . ? C4B C5B C6B O6B 177.9(2) . . . . ? N7B C5B C6B O6B -0.9(4) . . . . ? C4B C5B C6B N1B -2.6(3) . . . . ? N7B C5B C6B N1B 178.6(2) . . . . ? C4B C5B N7B C8B -0.2(3) . . . . ? C6B C5B N7B C8B 178.7(2) . . . . ? C4B C5B N7B C7B 178.8(2) . . . . ? C6B C5B N7B C7B -2.3(4) . . . . ? C5B N7B C8B N9B -0.5(3) . . . . ? C7B N7B C8B N9B -179.4(2) . . . . ? N7B C8B N9B C4B 0.9(3) . . . . ? N3B C4B N9B C8B 178.6(2) . . . . ? C5B C4B N9B C8B -1.0(3) . . . . ? # 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 # Attachment '4_AGK1702_sanz.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-08-24 at 16:08:13 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_4_AGK1702_sanz _database_code_depnum_ccdc_archive 'CCDC 831966' #TrackingRef '4_AGK1702_sanz.cif' _audit_creation_date 2010-08-24T16:08:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H20 N12 O2 Pt, 2(Cl O4)' _chemical_formula_sum 'C12 H20 Cl2 N12 O10 Pt' _chemical_formula_weight 758.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5564(7) _cell_length_b 12.7157(7) _cell_length_c 9.7164(7) _cell_angle_alpha 90 _cell_angle_beta 108.876(8) _cell_angle_gamma 90 _cell_volume 1117.20(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2175 _cell_measurement_theta_min 2.2107 _cell_measurement_theta_max 28.8995 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.6 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_T_max 0.517 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0994 _diffrn_reflns_number 4892 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.96 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.872 _reflns_number_total 2578 _reflns_number_gt 1589 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2578 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.165 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.175 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 Pt1 Pt 0 0 0.5 0.01470(8) Uani 1 2 d S . . N11 N -0.2125(4) 0.0489(3) 0.4172(4) 0.0199(11) Uani 1 1 d . . . H11A H -0.2691 -0.0041 0.3647 0.03 Uiso 1 1 calc R . . H11B H -0.2174 0.1054 0.3584 0.03 Uiso 1 1 calc R . . H11C H -0.2465 0.0673 0.4911 0.03 Uiso 1 1 calc R . . N1 N 0.3663(4) 0.1890(3) 0.2332(4) 0.0166(10) Uani 1 1 d . . . H1A H 0.4298 0.2002 0.1864 0.02 Uiso 1 1 calc R . . C2 C 0.3392(6) 0.0859(4) 0.2605(6) 0.0190(13) Uani 1 1 d . . . N2 N 0.4170(4) 0.0144(4) 0.2174(4) 0.0257(12) Uani 1 1 d . . . H2A H 0.4046 -0.0528 0.2313 0.031 Uiso 1 1 calc R . . H2B H 0.4812 0.0343 0.1748 0.031 Uiso 1 1 calc R . . N3 N 0.2447(5) 0.0565(3) 0.3233(5) 0.0179(11) Uani 1 1 d . . . C4 C 0.1750(5) 0.1397(4) 0.3629(5) 0.0131(12) Uani 1 1 d . . . C5 C 0.1953(8) 0.2426(4) 0.3386(7) 0.0170(16) Uani 1 1 d . . . C6 C 0.3021(6) 0.2765(4) 0.2731(6) 0.0169(12) Uani 1 1 d . . . O6 O 0.3381(4) 0.3649(3) 0.2518(4) 0.0259(10) Uani 1 1 d . . . N7 N 0.1064(5) 0.2999(3) 0.3980(4) 0.0133(10) Uani 1 1 d . . . C7 C 0.0809(7) 0.4132(4) 0.3918(6) 0.0288(16) Uani 1 1 d . . . H7A H 0.0106 0.4305 0.4428 0.043 Uiso 1 1 calc R . . H7B H 0.0404 0.4355 0.29 0.043 Uiso 1 1 calc R . . H7C H 0.1746 0.4497 0.4384 0.043 Uiso 1 1 calc R . . C8 C 0.0342(6) 0.2309(4) 0.4504(5) 0.0168(12) Uani 1 1 d . . . H8A H -0.0372 0.2489 0.4954 0.02 Uiso 1 1 calc R . . N9 N 0.0741(5) 0.1314(3) 0.4322(4) 0.0149(10) Uani 1 1 d . . . Cl1 Cl 0.67683(16) 0.21481(11) 0.05811(15) 0.0240(3) Uani 1 1 d . . . O11 O 0.8186(6) 0.2352(5) 0.1570(5) 0.063(2) Uani 1 1 d . . . O12 O 0.6823(4) 0.2125(3) -0.0864(4) 0.0250(9) Uani 1 1 d . . . O13 O 0.5770(5) 0.2946(4) 0.0700(4) 0.0631(15) Uani 1 1 d . . . O14 O 0.6259(6) 0.1171(4) 0.0934(5) 0.0702(17) 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 Pt1 0.01421(14) 0.01327(13) 0.01938(14) 0.0032(3) 0.00925(10) 0.0005(3) N11 0.020(3) 0.014(2) 0.026(3) 0.005(2) 0.008(2) 0.001(2) N1 0.014(3) 0.021(2) 0.021(3) 0.004(2) 0.014(2) 0.002(2) C2 0.011(3) 0.022(3) 0.027(3) -0.004(3) 0.010(3) 0.003(3) N2 0.029(3) 0.006(3) 0.052(3) -0.002(3) 0.026(2) -0.002(2) N3 0.018(3) 0.014(2) 0.028(3) -0.002(2) 0.015(2) 0.000(2) C4 0.010(3) 0.012(3) 0.016(3) 0.001(3) 0.002(2) 0.003(2) C5 0.018(4) 0.009(3) 0.023(4) -0.008(3) 0.004(3) -0.002(3) C6 0.011(3) 0.022(3) 0.016(3) 0.001(3) 0.002(2) 0.003(3) O6 0.022(2) 0.014(2) 0.046(3) 0.013(2) 0.016(2) -0.0002(18) N7 0.012(3) 0.012(2) 0.017(2) -0.002(2) 0.006(2) 0.004(2) C7 0.040(4) 0.015(3) 0.039(4) 0.001(3) 0.023(3) 0.009(3) C8 0.015(3) 0.020(3) 0.018(3) 0.000(3) 0.009(2) 0.003(3) N9 0.014(3) 0.016(2) 0.015(2) 0.003(2) 0.006(2) -0.005(2) Cl1 0.0194(8) 0.0343(8) 0.0221(8) 0.0047(8) 0.0119(6) -0.0014(7) O11 0.026(4) 0.139(6) 0.025(3) -0.006(3) 0.007(3) -0.016(3) O12 0.023(2) 0.037(2) 0.018(2) -0.003(2) 0.0101(18) -0.0051(19) O13 0.067(4) 0.088(4) 0.041(3) 0.004(3) 0.027(3) 0.041(3) O14 0.106(5) 0.058(3) 0.064(4) 0.011(3) 0.051(4) -0.035(3) #----------------------------------------------------------------------------# # 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 Pt1 N9 2.007(4) . ? Pt1 N9 2.007(4) 3_556 ? Pt1 N11 2.025(4) 3_556 ? Pt1 N11 2.025(4) . ? N11 H11A 0.91 . ? N11 H11B 0.91 . ? N11 H11C 0.91 . ? N1 C2 1.379(6) . ? N1 C6 1.385(6) . ? N1 H1A 0.88 . ? C2 N3 1.298(6) . ? C2 N2 1.325(6) . ? N2 H2A 0.88 . ? N2 H2B 0.88 . ? N3 C4 1.370(6) . ? C4 N9 1.348(6) . ? C4 C5 1.354(7) . ? C5 N7 1.379(7) . ? C5 C6 1.433(8) . ? C6 O6 1.213(6) . ? N7 C8 1.316(6) . ? N7 C7 1.460(6) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 N9 1.349(6) . ? C8 H8A 0.95 . ? Cl1 O11 1.408(5) . ? Cl1 O14 1.416(4) . ? Cl1 O12 1.422(3) . ? Cl1 O13 1.423(4) . ? 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 N9 Pt1 N9 179.9990(10) . 3_556 ? N9 Pt1 N11 88.33(16) . 3_556 ? N9 Pt1 N11 91.67(16) 3_556 3_556 ? N9 Pt1 N11 91.67(16) . . ? N9 Pt1 N11 88.33(16) 3_556 . ? N11 Pt1 N11 180 3_556 . ? Pt1 N11 H11A 109.5 . . ? Pt1 N11 H11B 109.5 . . ? H11A N11 H11B 109.5 . . ? Pt1 N11 H11C 109.5 . . ? H11A N11 H11C 109.5 . . ? H11B N11 H11C 109.5 . . ? C2 N1 C6 125.7(4) . . ? C2 N1 H1A 117.2 . . ? C6 N1 H1A 117.2 . . ? N3 C2 N2 119.9(5) . . ? N3 C2 N1 124.5(5) . . ? N2 C2 N1 115.6(4) . . ? C2 N2 H2A 120 . . ? C2 N2 H2B 120 . . ? H2A N2 H2B 120 . . ? C2 N3 C4 112.7(4) . . ? N9 C4 C5 109.2(5) . . ? N9 C4 N3 124.8(4) . . ? C5 C4 N3 126.0(5) . . ? C4 C5 N7 107.2(5) . . ? C4 C5 C6 122.1(6) . . ? N7 C5 C6 130.6(5) . . ? O6 C6 N1 121.4(5) . . ? O6 C6 C5 129.6(5) . . ? N1 C6 C5 109.0(5) . . ? C8 N7 C5 106.3(4) . . ? C8 N7 C7 124.9(4) . . ? C5 N7 C7 128.4(4) . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N7 C8 N9 111.7(4) . . ? N7 C8 H8A 124.2 . . ? N9 C8 H8A 124.2 . . ? C4 N9 C8 105.6(4) . . ? C4 N9 Pt1 128.0(3) . . ? C8 N9 Pt1 126.4(3) . . ? O11 Cl1 O14 109.0(3) . . ? O11 Cl1 O12 110.0(3) . . ? O14 Cl1 O12 110.3(3) . . ? O11 Cl1 O13 109.6(3) . . ? O14 Cl1 O13 108.3(3) . . ? O12 Cl1 O13 109.6(2) . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 N3 2.7(9) . . . . ? C6 N1 C2 N2 -177.6(5) . . . . ? N2 C2 N3 C4 179.2(5) . . . . ? N1 C2 N3 C4 -1.1(8) . . . . ? C2 N3 C4 N9 -178.7(5) . . . . ? C2 N3 C4 C5 1.6(8) . . . . ? N9 C4 C5 N7 1.4(7) . . . . ? N3 C4 C5 N7 -178.8(5) . . . . ? N9 C4 C5 C6 176.7(5) . . . . ? N3 C4 C5 C6 -3.6(10) . . . . ? C2 N1 C6 O6 175.9(5) . . . . ? C2 N1 C6 C5 -3.9(7) . . . . ? C4 C5 C6 O6 -175.6(6) . . . . ? N7 C5 C6 O6 -1.5(12) . . . . ? C4 C5 C6 N1 4.2(8) . . . . ? N7 C5 C6 N1 178.3(6) . . . . ? C4 C5 N7 C8 -2.0(7) . . . . ? C6 C5 N7 C8 -176.7(7) . . . . ? C4 C5 N7 C7 -175.4(5) . . . . ? C6 C5 N7 C7 9.9(11) . . . . ? C5 N7 C8 N9 1.8(7) . . . . ? C7 N7 C8 N9 175.5(5) . . . . ? C5 C4 N9 C8 -0.4(6) . . . . ? N3 C4 N9 C8 179.9(5) . . . . ? C5 C4 N9 Pt1 -179.0(4) . . . . ? N3 C4 N9 Pt1 1.2(8) . . . . ? N7 C8 N9 C4 -0.9(6) . . . . ? N7 C8 N9 Pt1 177.8(3) . . . . ? N11 Pt1 N9 C4 46.0(4) 3_556 . . . ? N11 Pt1 N9 C4 -134.0(4) . . . . ? N11 Pt1 N9 C8 -132.4(4) 3_556 . . . ? N11 Pt1 N9 C8 47.6(4) . . . . ? # 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 # Attachment '5_AGK10_sanz.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-06-08 at 11:21:04 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : 1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_5_AGK10_sanz _database_code_depnum_ccdc_archive 'CCDC 831967' #TrackingRef '5_AGK10_sanz.cif' _audit_creation_date 2011-06-08T11:21:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H20 N12 O2 Pt, 2(Cl O4), 3(H2 O)' _chemical_formula_sum 'C12 H26 Cl2 N12 O13 Pt' _chemical_formula_weight 812.44 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3162(4) _cell_length_b 10.4184(5) _cell_length_c 13.6046(6) _cell_angle_alpha 76.664(4) _cell_angle_beta 83.274(4) _cell_angle_gamma 77.138(4) _cell_volume 1249.60(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4995 _cell_measurement_theta_min 2.2432 _cell_measurement_theta_max 29.1156 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_T_max 0.553 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unetI/netI 0.0906 _diffrn_reflns_number 9990 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.18 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.841 _reflns_number_total 5680 _reflns_number_gt 4409 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5680 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0438 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.401 _refine_diff_density_min -1.604 _refine_diff_density_rms 0.148 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 Pt1 Pt 0.546887(19) 0.74464(2) 0.741570(15) 0.01820(5) Uani 1 1 d . . . N11 N 0.4864(3) 0.7811(4) 0.5964(3) 0.0308(11) Uani 1 1 d . . . H111 H 0.4842 0.7017 0.5798 0.046 Uiso 1 1 calc R . . H112 H 0.5528 0.8222 0.5532 0.046 Uiso 1 1 calc R . . H113 H 0.3952 0.8354 0.5914 0.046 Uiso 1 1 calc R . . N12 N 0.5964(3) 0.7127(4) 0.8877(2) 0.0236(10) Uani 1 1 d . . . H121 H 0.5766 0.7927 0.9079 0.035 Uiso 1 1 calc R . . H122 H 0.6938 0.6747 0.8931 0.035 Uiso 1 1 calc R . . H123 H 0.5409 0.6565 0.9277 0.035 Uiso 1 1 calc R . . N1A N -0.0346(4) 0.8082(4) 0.8922(3) 0.0268(11) Uani 1 1 d . . . H1A H -0.1248 0.842 0.9137 0.032 Uiso 1 1 calc R . . C2A C 0.0620(5) 0.8947(5) 0.8658(3) 0.0272(13) Uani 1 1 d . . . N2A N 0.0125(4) 1.0213(4) 0.8743(3) 0.0381(12) Uani 1 1 d . . . H21A H 0.0709 1.0797 0.8564 0.046 Uiso 1 1 calc R . . H22A H -0.0789 1.0471 0.898 0.046 Uiso 1 1 calc R . . N3A N 0.1998(3) 0.8569(4) 0.8300(3) 0.0226(10) Uani 1 1 d . . . C4A C 0.2349(5) 0.7269(5) 0.8236(3) 0.0232(12) Uani 1 1 d . . . C5A C 0.1449(4) 0.6335(5) 0.8503(3) 0.0206(12) Uani 1 1 d . . . C6A C -0.0036(4) 0.6711(5) 0.8885(3) 0.0232(12) Uani 1 1 d . . . O6A O -0.0975(3) 0.6031(3) 0.9145(2) 0.0295(9) Uani 1 1 d . . . N7A N 0.2265(4) 0.5142(4) 0.8326(3) 0.0206(10) Uani 1 1 d . . . C7A C 0.1790(4) 0.3842(5) 0.8472(3) 0.0300(14) Uani 1 1 d . . . H71A H 0.266 0.3116 0.8452 0.045 Uiso 1 1 calc R . . H72A H 0.1162 0.3882 0.7931 0.045 Uiso 1 1 calc R . . H73A H 0.1234 0.3666 0.9129 0.045 Uiso 1 1 calc R . . C8A C 0.3619(4) 0.5341(5) 0.7971(3) 0.0212(12) Uani 1 1 d . . . H8A H 0.4414 0.4665 0.7799 0.025 Uiso 1 1 calc R . . N9A N 0.3689(3) 0.6637(4) 0.7893(3) 0.0207(10) Uani 1 1 d . . . N1B N 0.9840(4) 0.7862(4) 0.6320(3) 0.0215(10) Uani 1 1 d . . . H1B H 1.0623 0.7278 0.6161 0.026 Uiso 1 1 calc R . . C2B C 0.8577(5) 0.7383(5) 0.6653(3) 0.0212(12) Uani 1 1 d . . . N2B N 0.8672(4) 0.6083(4) 0.6706(3) 0.0313(12) Uani 1 1 d . . . H21B H 0.7899 0.5716 0.6929 0.038 Uiso 1 1 calc R . . H22B H 0.9508 0.5586 0.6519 0.038 Uiso 1 1 calc R . . N3B N 0.7344(3) 0.8162(4) 0.6926(3) 0.0180(10) Uani 1 1 d . . . C4B C 0.7430(4) 0.9491(5) 0.6836(3) 0.0199(12) Uani 1 1 d . . . C5B C 0.8696(5) 0.9986(5) 0.6514(3) 0.0226(12) Uani 1 1 d . . . C6B C 1.0006(5) 0.9178(5) 0.6208(3) 0.0244(12) Uani 1 1 d . . . O6B O 1.1214(3) 0.9474(3) 0.5885(2) 0.0335(9) Uani 1 1 d . . . N7B N 0.8308(4) 1.1343(4) 0.6512(3) 0.0266(10) Uani 1 1 d . . . C7B C 0.9284(5) 1.2298(5) 0.6313(3) 0.0361(14) Uani 1 1 d . . . H71B H 0.8695 1.3214 0.6255 0.054 Uiso 1 1 calc R . . H72B H 0.9884 1.2228 0.5678 0.054 Uiso 1 1 calc R . . H73B H 0.9932 1.2097 0.687 0.054 Uiso 1 1 calc R . . C8B C 0.6873(5) 1.1568(5) 0.6825(3) 0.0326(14) Uani 1 1 d . . . H8B H 0.6322 1.2432 0.6891 0.039 Uiso 1 1 calc R . . N9B N 0.6291(4) 1.0475(4) 0.7035(3) 0.0288(11) Uani 1 1 d . . . Cl1 Cl 0.70084(12) 0.32551(12) 0.89578(9) 0.0252(3) Uani 1 1 d . . . O11 O 0.6357(3) 0.4141(3) 0.9624(2) 0.0298(9) Uani 1 1 d . . . O12 O 0.7057(3) 0.3999(3) 0.7935(2) 0.0272(8) Uani 1 1 d . . . O13 O 0.8446(3) 0.2592(4) 0.9225(2) 0.0500(12) Uani 1 1 d . . . O14 O 0.6094(4) 0.2289(4) 0.9034(2) 0.0503(11) Uani 1 1 d . . . Cl2 Cl 0.72591(12) 0.52291(14) 0.44047(9) 0.0316(3) Uani 1 1 d . . . O21 O 0.7371(3) 0.3929(3) 0.4136(2) 0.0358(9) Uani 1 1 d . . . O22 O 0.8715(3) 0.5534(4) 0.4268(3) 0.0458(11) Uani 1 1 d . . . O23 O 0.6292(3) 0.6242(3) 0.3751(2) 0.0434(10) Uani 1 1 d . . . O24 O 0.6696(3) 0.5167(4) 0.5444(2) 0.0462(11) Uani 1 1 d . . . O1W O 0.3541(3) 1.0593(3) 0.8273(3) 0.0494(11) Uani 1 1 d . . . H1W H 0.4372 1.0639 0.7948 0.074 Uiso 1 1 d R . . H2W H 0.3183 1.0026 0.8069 0.074 Uiso 1 1 d R . . O2W O -0.3119(3) 0.9376(3) 0.9692(2) 0.0416(10) Uani 1 1 d . . . H3W H -0.3479 1.0183 0.9409 0.062 Uiso 1 1 d R . . H4W H -0.3195 0.9328 1.0327 0.062 Uiso 1 1 d R . . O3W O 1.3266(4) 1.1031(4) 0.5675(3) 0.0627(13) Uani 1 1 d . . . H5W H 1.2421 1.0864 0.5645 0.094 Uiso 1 1 d R . . H6W H 1.3168 1.1575 0.6068 0.094 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 Pt1 0.01753(9) 0.01927(10) 0.01836(10) -0.00444(7) 0.00087(6) -0.00552(7) N11 0.026(2) 0.040(3) 0.024(2) 0.000(2) 0.0024(17) -0.0099(19) N12 0.0145(19) 0.028(3) 0.028(2) -0.0041(19) 0.0012(16) -0.0067(16) N1A 0.017(2) 0.037(3) 0.023(2) -0.010(2) 0.0004(16) 0.0039(19) C2A 0.035(3) 0.028(3) 0.017(3) -0.005(2) -0.009(2) 0.000(2) N2A 0.038(2) 0.027(3) 0.047(3) -0.014(2) -0.002(2) 0.003(2) N3A 0.0145(19) 0.029(3) 0.023(2) -0.0078(19) -0.0019(16) 0.0005(17) C4A 0.018(2) 0.029(3) 0.021(3) -0.002(2) -0.003(2) -0.003(2) C5A 0.015(2) 0.027(3) 0.017(3) -0.004(2) -0.0014(19) -0.001(2) C6A 0.018(2) 0.031(3) 0.017(3) -0.006(2) -0.005(2) 0.006(2) O6A 0.0136(16) 0.038(2) 0.036(2) -0.0068(18) 0.0045(14) -0.0070(15) N7A 0.020(2) 0.020(2) 0.021(2) -0.0035(19) -0.0029(17) -0.0044(18) C7A 0.024(3) 0.034(3) 0.031(3) -0.007(3) 0.010(2) -0.008(2) C8A 0.014(2) 0.035(3) 0.015(3) -0.006(2) 0.0007(19) -0.008(2) N9A 0.019(2) 0.018(2) 0.025(2) -0.0033(19) -0.0059(16) -0.0033(17) N1B 0.020(2) 0.023(2) 0.022(2) -0.0095(19) 0.0022(16) -0.0034(17) C2B 0.028(3) 0.025(3) 0.012(3) -0.003(2) 0.000(2) -0.011(2) N2B 0.020(2) 0.033(3) 0.044(3) -0.011(2) 0.0066(18) -0.0107(18) N3B 0.016(2) 0.023(3) 0.015(2) -0.0057(19) 0.0016(16) -0.0046(17) C4B 0.025(3) 0.021(3) 0.016(3) -0.006(2) 0.002(2) -0.009(2) C5B 0.026(3) 0.021(3) 0.018(3) -0.001(2) 0.003(2) -0.005(2) C6B 0.031(3) 0.032(3) 0.011(3) -0.004(2) 0.000(2) -0.010(2) O6B 0.0308(18) 0.043(2) 0.031(2) -0.0058(18) 0.0066(15) -0.0253(16) N7B 0.035(2) 0.030(3) 0.020(2) -0.006(2) 0.0020(18) -0.016(2) C7B 0.053(3) 0.028(3) 0.033(3) -0.001(3) 0.004(2) -0.028(3) C8B 0.038(3) 0.027(3) 0.030(3) -0.006(3) 0.004(2) -0.005(2) N9B 0.030(2) 0.020(2) 0.036(3) -0.007(2) 0.0074(18) -0.0082(19) Cl1 0.0297(6) 0.0192(7) 0.0233(7) -0.0029(5) -0.0004(5) -0.0005(5) O11 0.0285(17) 0.029(2) 0.029(2) -0.0078(16) 0.0050(14) -0.0015(15) O12 0.0337(17) 0.024(2) 0.0201(18) 0.0018(15) 0.0023(13) -0.0069(14) O13 0.042(2) 0.052(3) 0.048(2) -0.023(2) -0.0207(17) 0.0286(19) O14 0.081(3) 0.034(2) 0.043(2) -0.0078(19) 0.0152(19) -0.035(2) Cl2 0.0253(6) 0.0405(9) 0.0327(8) -0.0164(6) -0.0002(5) -0.0062(6) O21 0.0349(19) 0.034(2) 0.046(2) -0.0216(18) -0.0037(16) -0.0074(16) O22 0.0193(18) 0.054(3) 0.070(3) -0.027(2) 0.0031(17) -0.0093(17) O23 0.0365(19) 0.042(3) 0.048(2) -0.012(2) -0.0128(17) 0.0073(17) O24 0.049(2) 0.067(3) 0.026(2) -0.022(2) 0.0028(16) -0.0095(19) O1W 0.047(2) 0.041(3) 0.068(3) -0.032(2) 0.0203(18) -0.0177(18) O2W 0.0342(19) 0.034(2) 0.051(2) -0.0128(19) 0.0064(16) 0.0036(16) O3W 0.073(3) 0.089(4) 0.051(3) -0.030(2) 0.018(2) -0.064(2) #----------------------------------------------------------------------------# # 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 Pt1 N9A 2.001(4) . ? Pt1 N12 2.029(3) . ? Pt1 N3B 2.032(3) . ? Pt1 N11 2.046(3) . ? N11 H111 0.91 . ? N11 H112 0.91 . ? N11 H113 0.91 . ? N12 H121 0.91 . ? N12 H122 0.91 . ? N12 H123 0.91 . ? N1A C2A 1.373(6) . ? N1A C6A 1.404(6) . ? N1A H1A 0.88 . ? C2A N2A 1.325(6) . ? C2A N3A 1.325(5) . ? N2A H21A 0.88 . ? N2A H22A 0.88 . ? N3A C4A 1.341(6) . ? C4A N9A 1.360(5) . ? C4A C5A 1.383(6) . ? C5A N7A 1.363(6) . ? C5A C6A 1.421(5) . ? C6A O6A 1.217(5) . ? N7A C8A 1.340(5) . ? N7A C7A 1.480(6) . ? C7A H71A 0.98 . ? C7A H72A 0.98 . ? C7A H73A 0.98 . ? C8A N9A 1.345(6) . ? C8A H8A 0.95 . ? N1B C2B 1.369(5) . ? N1B C6B 1.385(6) . ? N1B H1B 0.88 . ? C2B N3B 1.319(5) . ? C2B N2B 1.322(6) . ? N2B H21B 0.88 . ? N2B H22B 0.88 . ? N3B C4B 1.380(6) . ? C4B N9B 1.351(6) . ? C4B C5B 1.376(6) . ? C5B N7B 1.379(6) . ? C5B C6B 1.399(6) . ? C6B O6B 1.237(5) . ? N7B C8B 1.341(5) . ? N7B C7B 1.453(5) . ? C7B H71B 0.98 . ? C7B H72B 0.98 . ? C7B H73B 0.98 . ? C8B N9B 1.327(6) . ? C8B H8B 0.95 . ? Cl1 O13 1.411(3) . ? Cl1 O12 1.429(3) . ? Cl1 O11 1.432(3) . ? Cl1 O14 1.436(4) . ? Cl2 O23 1.430(3) . ? Cl2 O24 1.441(3) . ? Cl2 O22 1.443(3) . ? Cl2 O21 1.461(4) . ? O1W H1W 0.85 . ? O1W H2W 0.8499 . ? O2W H3W 0.85 . ? O2W H4W 0.85 . ? O3W H5W 0.8501 . ? O3W H6W 0.85 . ? 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 N9A Pt1 N12 89.21(14) . . ? N9A Pt1 N3B 176.73(17) . . ? N12 Pt1 N3B 90.78(13) . . ? N9A Pt1 N11 88.89(14) . . ? N12 Pt1 N11 177.12(14) . . ? N3B Pt1 N11 91.24(14) . . ? Pt1 N11 H111 109.5 . . ? Pt1 N11 H112 109.5 . . ? H111 N11 H112 109.5 . . ? Pt1 N11 H113 109.5 . . ? H111 N11 H113 109.5 . . ? H112 N11 H113 109.5 . . ? Pt1 N12 H121 109.5 . . ? Pt1 N12 H122 109.5 . . ? H121 N12 H122 109.5 . . ? Pt1 N12 H123 109.5 . . ? H121 N12 H123 109.5 . . ? H122 N12 H123 109.5 . . ? C2A N1A C6A 126.5(4) . . ? C2A N1A H1A 116.8 . . ? C6A N1A H1A 116.8 . . ? N2A C2A N3A 119.5(5) . . ? N2A C2A N1A 117.9(4) . . ? N3A C2A N1A 122.6(5) . . ? C2A N2A H21A 120 . . ? C2A N2A H22A 120 . . ? H21A N2A H22A 120 . . ? C2A N3A C4A 113.5(4) . . ? N3A C4A N9A 125.0(4) . . ? N3A C4A C5A 127.2(4) . . ? N9A C4A C5A 107.8(5) . . ? N7A C5A C4A 107.2(4) . . ? N7A C5A C6A 132.1(5) . . ? C4A C5A C6A 120.6(5) . . ? O6A C6A N1A 121.1(4) . . ? O6A C6A C5A 129.3(5) . . ? N1A C6A C5A 109.6(4) . . ? C8A N7A C5A 107.6(4) . . ? C8A N7A C7A 124.4(4) . . ? C5A N7A C7A 128.0(4) . . ? N7A C7A H71A 109.5 . . ? N7A C7A H72A 109.5 . . ? H71A C7A H72A 109.5 . . ? N7A C7A H73A 109.5 . . ? H71A C7A H73A 109.5 . . ? H72A C7A H73A 109.5 . . ? N7A C8A N9A 110.1(4) . . ? N7A C8A H8A 124.9 . . ? N9A C8A H8A 124.9 . . ? C8A N9A C4A 107.3(4) . . ? C8A N9A Pt1 125.9(3) . . ? C4A N9A Pt1 126.8(4) . . ? C2B N1B C6B 126.3(4) . . ? C2B N1B H1B 116.9 . . ? C6B N1B H1B 116.9 . . ? N3B C2B N2B 121.9(4) . . ? N3B C2B N1B 122.1(5) . . ? N2B C2B N1B 116.0(4) . . ? C2B N2B H21B 120 . . ? C2B N2B H22B 120 . . ? H21B N2B H22B 120 . . ? C2B N3B C4B 114.8(4) . . ? C2B N3B Pt1 121.9(4) . . ? C4B N3B Pt1 123.3(3) . . ? N9B C4B C5B 111.2(5) . . ? N9B C4B N3B 124.9(4) . . ? C5B C4B N3B 123.9(4) . . ? C4B C5B N7B 105.6(4) . . ? C4B C5B C6B 122.0(5) . . ? N7B C5B C6B 132.2(4) . . ? O6B C6B N1B 119.3(4) . . ? O6B C6B C5B 129.8(5) . . ? N1B C6B C5B 110.9(4) . . ? C8B N7B C5B 105.5(4) . . ? C8B N7B C7B 127.2(4) . . ? C5B N7B C7B 127.1(4) . . ? N7B C7B H71B 109.5 . . ? N7B C7B H72B 109.5 . . ? H71B C7B H72B 109.5 . . ? N7B C7B H73B 109.5 . . ? H71B C7B H73B 109.5 . . ? H72B C7B H73B 109.5 . . ? N9B C8B N7B 114.0(4) . . ? N9B C8B H8B 123 . . ? N7B C8B H8B 123 . . ? C8B N9B C4B 103.7(4) . . ? O13 Cl1 O12 109.91(19) . . ? O13 Cl1 O11 110.3(2) . . ? O12 Cl1 O11 110.02(19) . . ? O13 Cl1 O14 110.2(2) . . ? O12 Cl1 O14 108.1(2) . . ? O11 Cl1 O14 108.2(2) . . ? O23 Cl2 O24 109.8(2) . . ? O23 Cl2 O22 109.8(2) . . ? O24 Cl2 O22 109.9(2) . . ? O23 Cl2 O21 109.1(2) . . ? O24 Cl2 O21 110.1(2) . . ? O22 Cl2 O21 108.0(2) . . ? H1W O1W H2W 107.7 . . ? H3W O2W H4W 107.7 . . ? H5W O3W H6W 107.7 . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A N1A C2A N2A 179.9(4) . . . . ? C6A N1A C2A N3A 1.7(7) . . . . ? N2A C2A N3A C4A -178.9(4) . . . . ? N1A C2A N3A C4A -0.7(6) . . . . ? C2A N3A C4A N9A 179.9(4) . . . . ? C2A N3A C4A C5A -0.5(7) . . . . ? N3A C4A C5A N7A -179.1(5) . . . . ? N9A C4A C5A N7A 0.5(5) . . . . ? N3A C4A C5A C6A 0.8(7) . . . . ? N9A C4A C5A C6A -179.6(4) . . . . ? C2A N1A C6A O6A 179.5(4) . . . . ? C2A N1A C6A C5A -1.3(6) . . . . ? N7A C5A C6A O6A -1.0(8) . . . . ? C4A C5A C6A O6A 179.2(5) . . . . ? N7A C5A C6A N1A 179.9(5) . . . . ? C4A C5A C6A N1A 0.2(6) . . . . ? C4A C5A N7A C8A 0.5(5) . . . . ? C6A C5A N7A C8A -179.3(4) . . . . ? C4A C5A N7A C7A -178.7(4) . . . . ? C6A C5A N7A C7A 1.5(8) . . . . ? C5A N7A C8A N9A -1.3(5) . . . . ? C7A N7A C8A N9A 177.9(4) . . . . ? N7A C8A N9A C4A 1.7(5) . . . . ? N7A C8A N9A Pt1 179.3(3) . . . . ? N3A C4A N9A C8A 178.3(5) . . . . ? C5A C4A N9A C8A -1.3(5) . . . . ? N3A C4A N9A Pt1 0.6(7) . . . . ? C5A C4A N9A Pt1 -179.0(3) . . . . ? N12 Pt1 N9A C8A -94.3(4) . . . . ? N11 Pt1 N9A C8A 87.9(4) . . . . ? N12 Pt1 N9A C4A 83.0(4) . . . . ? N11 Pt1 N9A C4A -94.9(4) . . . . ? C6B N1B C2B N3B -1.0(7) . . . . ? C6B N1B C2B N2B -179.6(4) . . . . ? N2B C2B N3B C4B 179.3(4) . . . . ? N1B C2B N3B C4B 0.8(6) . . . . ? N2B C2B N3B Pt1 -1.7(6) . . . . ? N1B C2B N3B Pt1 179.8(3) . . . . ? N12 Pt1 N3B C2B 94.7(3) . . . . ? N11 Pt1 N3B C2B -87.4(4) . . . . ? N12 Pt1 N3B C4B -86.4(4) . . . . ? N11 Pt1 N3B C4B 91.5(4) . . . . ? C2B N3B C4B N9B 177.4(4) . . . . ? Pt1 N3B C4B N9B -1.6(6) . . . . ? C2B N3B C4B C5B -1.7(7) . . . . ? Pt1 N3B C4B C5B 179.4(3) . . . . ? N9B C4B C5B N7B -0.3(6) . . . . ? N3B C4B C5B N7B 178.8(4) . . . . ? N9B C4B C5B C6B -176.4(4) . . . . ? N3B C4B C5B C6B 2.7(7) . . . . ? C2B N1B C6B O6B -179.1(4) . . . . ? C2B N1B C6B C5B 1.8(6) . . . . ? C4B C5B C6B O6B 178.5(5) . . . . ? N7B C5B C6B O6B 3.5(9) . . . . ? C4B C5B C6B N1B -2.5(6) . . . . ? N7B C5B C6B N1B -177.5(5) . . . . ? C4B C5B N7B C8B 0.1(5) . . . . ? C6B C5B N7B C8B 175.6(5) . . . . ? C4B C5B N7B C7B 174.4(4) . . . . ? C6B C5B N7B C7B -10.0(8) . . . . ? C5B N7B C8B N9B 0.2(5) . . . . ? C7B N7B C8B N9B -174.1(4) . . . . ? N7B C8B N9B C4B -0.4(5) . . . . ? C5B C4B N9B C8B 0.4(5) . . . . ? N3B C4B N9B C8B -178.7(4) . . . . ? # 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