# om010559n.cif data_global #------------------ AUDIT DETAILS-------------------------------------------# _audit_creation_date 2001-03-01 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Spicer, Mark D.' _publ_contact_author_address ; Department of Pure and Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UK ; _publ_contact_author_email m.d.spicer@strath.ac.uk _publ_contact_author_fax '44(141)552 0876' _publ_contact_author_phone '44(141)548 2800' _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_struct _audit_creation_date 2001-03-01T16:22:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C17 H21 B1 Mo1 N6 O2 S3' _chemical_formula_sum 'C17 H21 B1 Mo1 N6 O2 S3' _chemical_formula_weight 544.33 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.8124(7) _cell_length_b 13.3494(4) _cell_length_c 12.7461(4) _cell_angle_alpha 90 _cell_angle_beta 115.9617(12) _cell_angle_gamma 90 _cell_volume 4407.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123K _cell_measurement_reflns_used 4337 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour golden-yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type none #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_reflns_number 8463 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 27.31 _reflns_number_total 4878 _reflns_number_gt 3743 _reflns_number_gt 6104 _reflns_threshold_expression I>2.5u(I) _reflns_threshold_expression >2sigma(I) #------------------ 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_solution 'SHELXS-86 (Sheldrick, 1986) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+1.9829P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_number_reflns 4878 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_gt 1.057 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.067 _refine_diff_density_max 0.507 _refine_diff_density_min -0.505 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol C H B Mo N O S 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.107358(8) 0.18347(2) 0.05513(2) 0.01415(7) Uani 1 d . . S1 S 0.06528(3) 0.28388(5) 0.17025(6) 0.01693(15) Uani 1 d . . S3 S 0.13491(3) 0.36033(5) 0.00814(6) 0.01662(15) Uani 1 d . . S2 S 0.19237(2) 0.18473(4) 0.24146(6) 0.01473(14) Uani 1 d . . O1 O 0.09423(7) -0.02651(13) 0.1444(2) 0.0274(5) Uani 1 d . . N4 N 0.26310(8) 0.29689(15) 0.2068(2) 0.0172(5) Uani 1 d . . O2 O 0.16877(7) 0.04786(14) -0.0379(2) 0.0285(5) Uani 1 d . . N3 N 0.21808(8) 0.38664(14) 0.2721(2) 0.0157(5) Uani 1 d . . N6 N 0.07547(8) 0.51741(15) 0.0112(2) 0.0172(5) Uani 1 d . . N1 N 0.15384(8) 0.35365(15) 0.3571(2) 0.0163(5) Uani 1 d . . N5 N 0.13222(8) 0.47802(14) 0.1868(2) 0.0145(5) Uani 1 d . . N2 N 0.11445(9) 0.2306(2) 0.3977(2) 0.0214(5) Uani 1 d . . C9 C 0.11394(10) 0.4526(2) 0.0722(2) 0.0144(5) Uani 1 d . . C6 C 0.25344(10) 0.4483(2) 0.2575(2) 0.0207(6) Uani 1 d . . H6 H 0.25729(10) 0.5166(2) 0.2732(2) 0.025 Uiso 1 calc R . C12 C 0.04524(10) 0.5184(2) -0.1153(2) 0.0227(6) Uani 1 d . . H12A H 0.0661(2) 0.5434(11) -0.1511(2) 0.034 Uiso 1 calc R . H12B H 0.0157(3) 0.5609(10) -0.1356(2) 0.034 Uiso 1 calc R . H12C H 0.0341(5) 0.4516(3) -0.1424(3) 0.034 Uiso 1 calc R . C13 C 0.06693(12) 0.1802(2) -0.1466(2) 0.0250(7) Uani 1 d . . C7 C 0.28114(10) 0.3940(2) 0.2174(2) 0.0214(6) Uani 1 d . . H7 H 0.30743(10) 0.4171(2) 0.2000(2) 0.026 Uiso 1 calc R . B1 B 0.17534(12) 0.4313(2) 0.2993(3) 0.0165(6) Uani 1 d . . C11 C 0.06913(10) 0.5834(2) 0.0866(2) 0.0214(6) Uani 1 d . . H11 H 0.04522(10) 0.6353(2) 0.0666(2) 0.026 Uiso 1 calc R . C8 C 0.28212(11) 0.2126(2) 0.1647(2) 0.0246(7) Uani 1 d . . H8A H 0.3002(6) 0.1672(7) 0.2280(4) 0.037 Uiso 1 calc R . H8B H 0.3052(5) 0.2364(2) 0.1341(14) 0.037 Uiso 1 calc R . H8C H 0.25356(12) 0.1785(8) 0.1044(10) 0.037 Uiso 1 calc R . C4 C 0.07770(12) 0.1509(2) 0.3840(3) 0.0309(7) Uani 1 d . . H4A H 0.0859(4) 0.1210(9) 0.4586(4) 0.046 Uiso 1 calc R . H4B H 0.0795(5) 0.1010(7) 0.3317(12) 0.046 Uiso 1 calc R . H4C H 0.04344(14) 0.1782(3) 0.3527(15) 0.046 Uiso 1 calc R . C1 C 0.11294(10) 0.2908(2) 0.3111(2) 0.0159(6) Uani 1 d . . C10 C 0.10388(10) 0.5590(2) 0.1946(2) 0.0192(6) Uani 1 d . . H10 H 0.10822(10) 0.5910(2) 0.2631(2) 0.023 Uiso 1 calc R . C2 C 0.18154(11) 0.3301(2) 0.4746(2) 0.0258(7) Uani 1 d . . H2 H 0.21148(11) 0.3617(2) 0.5272(2) 0.031 Uiso 1 calc R . C5 C 0.22452(10) 0.2934(2) 0.2404(2) 0.0145(6) Uani 1 d . . C15 C 0.02058(11) 0.1352(2) -0.0389(3) 0.0274(7) Uani 1 d . . C14 C 0.03267(10) 0.2093(2) -0.0997(2) 0.0226(6) Uani 1 d . . C3 C 0.15751(11) 0.2540(2) 0.4987(2) 0.0286(7) Uani 1 d . . H3 H 0.16799(11) 0.2226(2) 0.5707(2) 0.034 Uiso 1 calc R . C16 C 0.09845(10) 0.0524(2) 0.1114(2) 0.0188(6) Uani 1 d . . C17 C 0.14599(10) 0.1014(2) -0.0060(2) 0.0193(6) Uani 1 d . . H13A H 0.0635(11) 0.116(2) -0.178(2) 0.028(8) Uiso 1 d . . H1 H 0.1924(9) 0.4949(17) 0.3624(19) 0.014(6) Uiso 1 d . . H15A H 0.0023(11) 0.1530(18) 0.007(2) 0.024(7) Uiso 1 d . . H13B H 0.0787(10) 0.2252(18) -0.181(2) 0.014(7) Uiso 1 d . . H14 H 0.0250(10) 0.2772(19) -0.097(2) 0.020(7) Uiso 1 d . . H15B H 0.0171(10) 0.0646(19) -0.070(2) 0.025(7) Uiso 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 Mo1 0.01226(12) 0.01593(12) 0.01257(13) -0.00152(10) 0.00389(9) -0.00113(9) S1 0.0137(3) 0.0211(3) 0.0149(4) 0.0003(3) 0.0053(3) 0.0010(3) S3 0.0196(4) 0.0164(3) 0.0149(4) 0.0009(3) 0.0085(3) 0.0020(3) S2 0.0126(3) 0.0124(3) 0.0164(4) 0.0003(3) 0.0038(3) -0.0007(3) O1 0.0299(12) 0.0212(10) 0.0298(12) 0.0019(9) 0.0119(10) -0.0071(9) N4 0.0154(12) 0.0180(12) 0.0182(13) -0.0008(9) 0.0073(10) 0.0005(9) O2 0.0290(12) 0.0330(11) 0.0290(12) -0.0066(9) 0.0176(10) 0.0033(9) N3 0.0152(12) 0.0157(11) 0.0133(12) 0.0006(9) 0.0038(10) -0.0008(9) N6 0.0155(12) 0.0192(11) 0.0158(12) 0.0056(10) 0.0057(10) 0.0058(9) N1 0.0156(12) 0.0196(11) 0.0128(12) 0.0004(9) 0.0053(10) 0.0032(9) N5 0.0167(12) 0.0116(10) 0.0154(12) 0.0013(9) 0.0073(10) 0.0017(9) N2 0.0214(13) 0.0243(12) 0.0192(13) 0.0052(10) 0.0095(11) -0.0005(10) C9 0.0153(14) 0.0122(12) 0.0184(15) 0.0035(11) 0.0100(12) 0.0025(10) C6 0.021(2) 0.0168(14) 0.024(2) -0.0004(12) 0.0094(13) -0.0054(11) C12 0.021(2) 0.0255(15) 0.021(2) 0.0085(12) 0.0089(13) 0.0056(12) C13 0.022(2) 0.030(2) 0.016(2) -0.0025(14) 0.0026(13) -0.0018(14) C7 0.021(2) 0.0191(14) 0.026(2) 0.0002(12) 0.0120(13) -0.0072(12) B1 0.015(2) 0.017(2) 0.015(2) -0.0013(13) 0.0048(13) -0.0007(13) C11 0.0186(15) 0.0185(14) 0.030(2) 0.0019(12) 0.0137(13) 0.0070(11) C8 0.021(2) 0.0255(15) 0.031(2) -0.0031(13) 0.0156(14) 0.0006(12) C4 0.031(2) 0.032(2) 0.032(2) 0.0131(14) 0.0154(15) -0.0011(14) C1 0.0164(14) 0.0184(13) 0.0142(14) 0.0014(11) 0.0078(12) 0.0045(11) C10 0.023(2) 0.0151(13) 0.024(2) -0.0033(12) 0.0140(13) 0.0000(11) C2 0.021(2) 0.037(2) 0.0127(15) 0.0009(13) 0.0014(12) -0.0007(13) C5 0.0132(14) 0.0161(13) 0.0110(14) 0.0010(10) 0.0024(11) 0.0017(10) C15 0.014(2) 0.040(2) 0.024(2) -0.0120(15) 0.0041(13) -0.0081(13) C14 0.0136(15) 0.029(2) 0.017(2) -0.0011(13) -0.0003(12) 0.0022(12) C3 0.029(2) 0.040(2) 0.014(2) 0.0100(13) 0.0068(13) 0.0053(14) C16 0.0149(14) 0.0252(15) 0.0149(15) -0.0076(12) 0.0052(12) -0.0021(11) C17 0.020(2) 0.0202(14) 0.0148(15) -0.0020(12) 0.0056(12) -0.0054(12) #------------------ 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 Mo1 C16 1.950(3) . ? Mo1 C17 1.951(3) . ? Mo1 C14 2.220(3) . ? Mo1 C13 2.313(3) . ? Mo1 C15 2.341(3) . ? Mo1 S2 2.5588(7) . ? Mo1 S1 2.6415(7) . ? Mo1 S3 2.6418(7) . ? S1 C1 1.720(3) . ? S3 C9 1.727(2) . ? S2 C5 1.724(2) . ? O1 C16 1.160(3) . ? N4 C5 1.355(3) . ? N4 C7 1.381(3) . ? N4 C8 1.453(3) . ? O2 C17 1.158(3) . ? N3 C5 1.346(3) . ? N3 C6 1.384(3) . ? N3 B1 1.538(3) . ? N6 C9 1.352(3) . ? N6 C11 1.375(3) . ? N6 C12 1.459(3) . ? N1 C1 1.353(3) . ? N1 C2 1.390(3) . ? N1 B1 1.550(3) . ? N5 C9 1.361(3) . ? N5 C10 1.384(3) . ? N5 B1 1.558(3) . ? N2 C1 1.351(3) . ? N2 C3 1.377(3) . ? N2 C4 1.457(3) . ? C6 C7 1.334(3) . ? C13 C14 1.414(4) . ? C11 C10 1.340(4) . ? C2 C3 1.339(4) . ? C15 C14 1.392(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 C16 Mo1 C17 80.38(10) . . ? C16 Mo1 C14 103.54(11) . . ? C17 Mo1 C14 103.46(11) . . ? C16 Mo1 C13 107.98(11) . . ? C17 Mo1 C13 69.08(11) . . ? C14 Mo1 C13 36.29(10) . . ? C16 Mo1 C15 70.02(11) . . ? C17 Mo1 C15 108.00(11) . . ? C14 Mo1 C15 35.41(10) . . ? C13 Mo1 C15 61.32(11) . . ? C16 Mo1 S2 83.76(7) . . ? C17 Mo1 S2 83.84(8) . . ? C14 Mo1 S2 170.34(8) . . ? C13 Mo1 S2 147.53(8) . . ? C15 Mo1 S2 148.33(8) . . ? C16 Mo1 S1 94.87(7) . . ? C17 Mo1 S1 171.03(8) . . ? C14 Mo1 S1 85.00(8) . . ? C13 Mo1 S1 119.80(8) . . ? C15 Mo1 S1 77.12(8) . . ? S2 Mo1 S1 88.10(2) . . ? C16 Mo1 S3 170.48(8) . . ? C17 Mo1 S3 97.50(7) . . ? C14 Mo1 S3 85.98(8) . . ? C13 Mo1 S3 79.62(8) . . ? C15 Mo1 S3 119.30(8) . . ? S2 Mo1 S3 86.79(2) . . ? S1 Mo1 S3 85.93(2) . . ? C1 S1 Mo1 104.84(9) . . ? C9 S3 Mo1 109.15(8) . . ? C5 S2 Mo1 107.31(9) . . ? C5 N4 C7 109.1(2) . . ? C5 N4 C8 125.7(2) . . ? C7 N4 C8 125.2(2) . . ? C5 N3 C6 107.7(2) . . ? C5 N3 B1 130.9(2) . . ? C6 N3 B1 120.6(2) . . ? C9 N6 C11 109.5(2) . . ? C9 N6 C12 125.8(2) . . ? C11 N6 C12 124.7(2) . . ? C1 N1 C2 107.9(2) . . ? C1 N1 B1 131.5(2) . . ? C2 N1 B1 120.2(2) . . ? C9 N5 C10 108.0(2) . . ? C9 N5 B1 131.7(2) . . ? C10 N5 B1 120.3(2) . . ? C1 N2 C3 108.9(2) . . ? C1 N2 C4 125.1(2) . . ? C3 N2 C4 126.0(2) . . ? N6 C9 N5 107.0(2) . . ? N6 C9 S3 123.5(2) . . ? N5 C9 S3 129.4(2) . . ? C7 C6 N3 109.1(2) . . ? C14 C13 Mo1 68.3(2) . . ? C6 C7 N4 106.5(2) . . ? N3 B1 N1 112.0(2) . . ? N3 B1 N5 110.0(2) . . ? N1 B1 N5 112.4(2) . . ? C10 C11 N6 107.1(2) . . ? N2 C1 N1 107.7(2) . . ? N2 C1 S1 123.1(2) . . ? N1 C1 S1 129.2(2) . . ? C11 C10 N5 108.4(2) . . ? C3 C2 N1 108.0(2) . . ? N3 C5 N4 107.6(2) . . ? N3 C5 S2 129.1(2) . . ? N4 C5 S2 123.3(2) . . ? C14 C15 Mo1 67.5(2) . . ? C15 C14 C13 115.5(3) . . ? C15 C14 Mo1 77.0(2) . . ? C13 C14 Mo1 75.4(2) . . ? C2 C3 N2 107.6(2) . . ? O1 C16 Mo1 178.2(2) . . ? O2 C17 Mo1 175.7(2) . . ? --=====================_5448112==_ Content-Type: text/plain; charset="us-ascii" Content-Disposition: attachment; filename="wtmcco3i.cif.txt" # CIF produced by WinGX routine CIF_UPDATE # Created on 2001-06-20 at 10:37:32 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : wtmco3i dreduc struct import data_wtmco3i _audit_creation_date 2001-06-20T10:37:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Spicer, Mark D.' _publ_contact_author_address ; Department of Pure and Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UK ; _publ_contact_author_email m.d.spicer@strath.ac.uk _publ_contact_author_fax '44(141)552 0876' _publ_contact_author_phone '44(141)548 2800' _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common W(Tm)(CO)3I _chemical_formula_moiety 'C15 H16 B1 I1 N6 O3 S3 W1' _chemical_formula_structural 'C15 H16 B1 I1 N6 O3 S3 W1' _chemical_formula_sum 'C19 H26 B I N6 O4 S3 W' _chemical_formula_weight 820.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8780(2) _cell_length_b 15.3477(3) _cell_length_c 14.0110(3) _cell_angle_alpha 90 _cell_angle_beta 94.9750(10) _cell_angle_gamma 90 _cell_volume 2758.81(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6355 _cell_measurement_theta_min 5602 _cell_measurement_theta_max 5602 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.57 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(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_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.703058E-1 _diffrn_orient_matrix_ub_12 0.175037E-1 _diffrn_orient_matrix_ub_13 -0.185073E-1 _diffrn_orient_matrix_ub_21 -0.319364E-1 _diffrn_orient_matrix_ub_22 0.186701E-1 _diffrn_orient_matrix_ub_23 -0.643658E-1 _diffrn_orient_matrix_ub_31 -0.105877E-1 _diffrn_orient_matrix_ub_32 0.599144E-1 _diffrn_orient_matrix_ub_33 0.25464E-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 0.094 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_number 24967 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6168 _reflns_number_gt 5495 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # 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, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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^)+(0.0001P)^2^+323.8882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5420 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2259 _refine_ls_wR_factor_gt 0.2225 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 6.808 _refine_diff_density_min -3.659 _refine_diff_density_rms 0.425 #----------------------------------------------------------------------------# # 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5704(14) 0.3369(11) 0.2428(12) 0.018(4) Uani 1 1 d ' ' ' ' ' ' C2 C 0.7179(15) 0.2695(12) 0.2145(12) 0.021(4) Uani 1 1 d ' ' ' ' ' ' H2 H 0.7783 0.2338 0.2231 0.025 Uiso 1 1 calc R ' ' ' ' C3 C 0.6893(15) 0.3171(12) 0.1355(13) 0.022(4) Uani 1 1 d ' ' ' ' ' ' H3 H 0.7242 0.3207 0.0786 0.026 Uiso 1 1 calc R ' ' ' ' C4 C 0.5447(16) 0.4249(13) 0.0927(15) 0.027(4) Uani 1 1 d ' ' ' ' ' ' H4A H 0.5778 0.4284 0.0325 0.041 Uiso 1 1 calc R ' ' ' ' H4B H 0.5489 0.4818 0.1246 0.041 Uiso 1 1 calc R ' ' ' ' H4C H 0.4714 0.4083 0.0793 0.041 Uiso 1 1 calc R ' ' ' ' C5 C 0.5335(14) 0.1037(11) 0.3224(12) 0.016(3) Uani 1 1 d ' ' ' ' ' ' C6 C 0.6493(14) 0.0777(13) 0.4439(16) 0.027(4) Uani 1 1 d ' ' ' ' ' ' H6 H 0.704 0.0866 0.4929 0.033 Uiso 1 1 calc R ' ' ' ' C7 C 0.5972(17) 0.0038(13) 0.4280(14) 0.028(4) Uani 1 1 d ' ' ' ' ' ' H7 H 0.6081 -0.0493 0.4622 0.034 Uiso 1 1 calc R ' ' ' ' C8 C 0.4564(16) -0.0465(12) 0.3080(14) 0.025(4) Uani 1 1 d ' ' ' ' ' ' H8A H 0.4105 -0.0211 0.2559 0.038 Uiso 1 1 calc R ' ' ' ' H8B H 0.4142 -0.0712 0.3562 0.038 Uiso 1 1 calc R ' ' ' ' H8C H 0.4988 -0.0925 0.2823 0.038 Uiso 1 1 calc R ' ' ' ' C9 C 0.5229(14) 0.2930(11) 0.4969(13) 0.017(3) Uani 1 1 d ' ' ' ' ' ' C10 C 0.6752(15) 0.3597(13) 0.5014(14) 0.026 Uani 1 1 d ' ' ' ' ' ' H10 H 0.7431 0.3764 0.4869 0.031 Uiso 1 1 calc R ' ' ' ' C11 C 0.616(2) 0.4007(13) 0.5674(14) 0.046 Uani 1 1 d ' ' ' ' ' ' H11 H 0.6364 0.4472 0.6097 0.055 Uiso 1 1 calc R ' ' ' ' C12 C 0.4437(15) 0.3843(12) 0.6187(14) 0.024 Uani 1 1 d ' ' ' ' ' ' H12A H 0.4657 0.4353 0.6573 0.036 Uiso 1 1 calc R ' ' ' ' H12B H 0.4308 0.3354 0.661 0.036 Uiso 1 1 calc R ' ' ' ' H12C H 0.3796 0.3981 0.5786 0.036 Uiso 1 1 calc R ' ' ' ' C13 C 0.1865(16) 0.2559(12) 0.2462(13) 0.023(4) Uani 1 1 d ' ' ' ' ' ' C14 C 0.2611(15) 0.3596(14) 0.3701(14) 0.022 Uani 1 1 d ' ' ' ' ' ' C15 C 0.3269(19) 0.2934(14) 0.1664(13) 0.032(5) Uani 1 1 d ' ' ' ' ' ' C16 C 0.6484(17) 0.9905(14) 0.1271(15) 0.032(5) Uani 1 1 d ' ' ' ' ' ' H16A H 0.5876 1.0268 0.1402 0.039 Uiso 1 1 calc R ' ' ' ' H16B H 0.6722 1.0088 0.0648 0.039 Uiso 1 1 calc R ' ' ' ' C17 C 0.7358(17) 1.0028(14) 0.2062(15) 0.031(5) Uani 1 1 d ' ' ' ' ' ' H17A H 0.7558 1.0644 0.21 0.046 Uiso 1 1 calc R ' ' ' ' H17B H 0.796 0.9675 0.1922 0.046 Uiso 1 1 calc R ' ' ' ' H17C H 0.7117 0.9844 0.2676 0.046 Uiso 1 1 calc R ' ' ' ' C18 C 0.5357(18) 0.8846(19) 0.0548(17) 0.044(6) Uani 1 1 d ' ' ' ' ' ' H18A H 0.5562 0.8991 -0.0099 0.053 Uiso 1 1 calc R ' ' ' ' H18B H 0.4757 0.9217 0.0677 0.053 Uiso 1 1 calc R ' ' ' ' C19 C 0.5051(19) 0.790(2) 0.058(2) 0.055(8) Uani 1 1 d ' ' ' ' ' ' H19A H 0.4467 0.7789 0.0101 0.083 Uiso 1 1 calc R ' ' ' ' H19B H 0.4841 0.7762 0.122 0.083 Uiso 1 1 calc R ' ' ' ' H19C H 0.5646 0.7536 0.0447 0.083 Uiso 1 1 calc R ' ' ' ' B1 B 0.6600(16) 0.2346(12) 0.3804(14) 0.016(4) Uiso 1 1 d ' ' ' ' ' ' H1 H 0.710(17) 0.2305(19) 0.391(4) 0.019 Uiso 1 1 calc R ' ' ' ' I1 I 0.22779(10) 0.10181(8) 0.36004(9) 0.0251(3) Uani 1 1 d ' ' ' ' ' ' N1 N 0.6447(12) 0.2806(9) 0.2819(10) 0.015(3) Uani 1 1 d ' ' ' ' ' ' N2 N 0.5981(12) 0.3600(10) 0.1547(11) 0.019(3) Uani 1 1 d ' ' ' ' ' ' N3 N 0.6113(11) 0.1408(10) 0.3771(11) 0.017(3) Uani 1 1 d ' ' ' ' ' ' N4 N 0.5229(12) 0.0194(10) 0.3509(11) 0.021(3) Uani 1 1 d ' ' ' ' ' ' N5 N 0.6163(11) 0.2885(10) 0.4598(11) 0.019 Uani 1 1 d ' ' ' ' ' ' N6 N 0.5247(12) 0.3610(10) 0.5583(10) 0.019(3) Uani 1 1 d ' ' ' ' ' ' O1 O 0.1017(13) 0.2610(10) 0.2140(12) 0.038(4) Uani 1 1 d ' ' ' ' ' ' O2 O 0.2338(10) 0.4068(11) 0.4016(10) 0.029(3) Uani 1 1 d ' ' ' ' ' ' O3 O 0.3251(13) 0.3169(11) 0.0875(11) 0.040(4) Uani 1 1 d ' ' ' ' ' ' O4 O 0.6194(10) 0.9009(9) 0.1234(10) 0.027(3) Uani 1 1 d ' ' ' ' ' ' S1 S 0.4665(3) 0.3780(3) 0.2975(3) 0.0182(9) Uani 1 1 d ' ' ' ' ' ' S2 S 0.4562(4) 0.1495(3) 0.2282(3) 0.0188(9) Uani 1 1 d ' ' ' ' ' ' S3 S 0.4186(3) 0.2228(3) 0.4720(3) 0.0169(9) Uani 1 1 d ' ' ' ' ' ' W1 W 0.33290(5) 0.25772(4) 0.30159(5) 0.0161(2) Uani 1 1 d ' ' ' ' ' ' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(9) 0.017(9) 0.014(8) 0.001(7) 0.005(7) -0.004(7) C2 0.022(9) 0.027(10) 0.015(8) -0.003(7) 0.008(7) 0.003(7) C3 0.027(10) 0.019(9) 0.022(9) -0.003(7) 0.014(8) -0.005(7) C4 0.027(10) 0.024(10) 0.031(11) 0.010(8) 0.001(8) 0.001(8) C5 0.022(9) 0.011(8) 0.015(8) 0.000(6) 0.011(7) 0.006(7) C6 0.015(9) 0.024(10) 0.043(12) 0.013(9) 0.000(8) -0.008(8) C7 0.045(12) 0.022(10) 0.020(10) 0.010(8) 0.014(9) 0.009(9) C8 0.036(11) 0.015(9) 0.026(10) -0.003(8) 0.007(8) 0.000(8) C9 0.023(9) 0.009(8) 0.020(9) 0.002(7) 0.005(7) -0.002(7) C10 0.022(9) 0.029(9) 0.027(10) -0.001(8) 0.007(9) -0.024(9) C11 0.102(12) 0.015(10) 0.016(9) -0.011(8) -0.023(8) -0.008(8) C12 0.032(10) 0.016(9) 0.027(9) -0.004(8) 0.024(10) 0.006(9) C13 0.034(11) 0.020(9) 0.014(8) 0.000(7) -0.012(8) 0.002(8) C14 0.017(10) 0.025(10) 0.021(9) 0.007(8) 0.014(8) -0.017(9) C15 0.057(14) 0.032(11) 0.008(9) 0.002(8) 0.006(8) 0.018(10) C16 0.038(12) 0.029(11) 0.031(11) -0.001(9) 0.010(9) 0.009(9) C17 0.036(12) 0.023(10) 0.033(11) -0.002(9) 0.007(9) 0.001(9) C18 0.029(12) 0.067(17) 0.036(13) -0.008(12) 0.006(10) 0.007(12) C19 0.027(12) 0.08(2) 0.061(17) -0.037(16) 0.000(11) -0.008(13) I1 0.0246(6) 0.0253(6) 0.0259(6) -0.0022(5) 0.0047(5) -0.0070(5) N1 0.024(8) 0.011(7) 0.012(7) 0.003(5) 0.007(6) 0.001(6) N2 0.023(8) 0.016(7) 0.018(7) 0.000(6) 0.004(6) -0.002(6) N3 0.010(7) 0.016(7) 0.025(8) 0.005(6) 0.002(6) 0.004(6) N4 0.026(8) 0.016(7) 0.022(8) -0.004(6) 0.008(6) -0.001(6) N5 0.016(8) 0.024(7) 0.018(7) -0.007(6) 0.005(6) 0.003(6) N6 0.023(8) 0.019(7) 0.015(7) 0.002(6) 0.010(6) 0.015(6) O1 0.043(10) 0.026(8) 0.045(9) -0.002(7) -0.001(8) 0.007(7) O2 0.011(6) 0.048(9) 0.029(7) 0.005(7) 0.007(5) -0.003(6) O3 0.043(9) 0.051(10) 0.027(8) 0.001(7) 0.002(7) 0.018(8) O4 0.020(7) 0.033(8) 0.030(7) 0.001(6) 0.009(6) 0.003(6) S1 0.019(2) 0.014(2) 0.022(2) 0.0006(17) 0.0053(17) 0.0018(16) S2 0.024(2) 0.015(2) 0.018(2) -0.0033(16) 0.0050(17) 0.0014(17) S3 0.019(2) 0.014(2) 0.018(2) 0.0006(16) 0.0026(16) -0.0025(16) W1 0.0164(4) 0.0134(4) 0.0185(4) -0.0006(3) 0.0019(2) 0.0011(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 C1 N2 1.36(2) ' ' ? C1 N1 1.37(2) ' ' ? C1 S1 1.719(18) ' ' ? C2 C3 1.35(3) ' ' ? C2 N1 1.40(2) ' ' ? C3 N2 1.39(2) ' ' ? C4 N2 1.45(2) ' ' ? C5 N3 1.34(2) ' ' ? C5 N4 1.36(2) ' ' ? C5 S2 1.731(18) ' ' ? C6 C7 1.33(3) ' ' ? C6 N3 1.40(2) ' ' ? C7 N4 1.40(3) ' ' ? C8 N4 1.42(2) ' ' ? C9 N6 1.35(2) ' ' ? C9 N5 1.35(2) ' ' ? C9 S3 1.734(17) ' ' ? C10 C11 1.40(3) ' ' ? C10 N5 1.43(2) ' ' ? C11 N6 1.32(3) ' ' ? C12 N6 1.44(2) ' ' ? C13 O1 1.15(2) ' ' ? C13 W1 1.975(19) ' ' ? C14 O2 0.93(2) ' ' ? C14 W1 2.09(2) ' ' ? C15 O3 1.16(2) ' ' ? C15 W1 1.968(18) ' ' ? C16 O4 1.42(3) ' ' ? C16 C17 1.52(3) ' ' ? C18 O4 1.40(3) ' ' ? C18 C19 1.50(4) ' ' ? B1 N5 1.53(2) ' ' ? B1 N1 1.55(2) ' ' ? B1 N3 1.57(2) ' ' ? I1 W1 2.9019(14) ' ' ? S1 W1 2.528(4) ' ' ? S2 W1 2.573(4) ' ' ? S3 W1 2.597(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 N2 C1 N1 107.3(15) ' ' ' ' ? N2 C1 S1 125.8(14) ' ' ' ' ? N1 C1 S1 126.7(13) ' ' ' ' ? C3 C2 N1 109.6(16) ' ' ' ' ? C2 C3 N2 105.7(15) ' ' ' ' ? N3 C5 N4 109.0(15) ' ' ' ' ? N3 C5 S2 128.1(13) ' ' ' ' ? N4 C5 S2 122.9(14) ' ' ' ' ? C7 C6 N3 109.6(18) ' ' ' ' ? C6 C7 N4 106.6(17) ' ' ' ' ? N6 C9 N5 108.5(15) ' ' ' ' ? N6 C9 S3 125.3(13) ' ' ' ' ? N5 C9 S3 126.2(13) ' ' ' ' ? C11 C10 N5 108.2(16) ' ' ' ' ? N6 C11 C10 105.1(16) ' ' ' ' ? O1 C13 W1 175.2(17) ' ' ' ' ? O2 C14 W1 175.9(18) ' ' ' ' ? O3 C15 W1 178(2) ' ' ' ' ? O4 C16 C17 108.7(17) ' ' ' ' ? O4 C18 C19 110(2) ' ' ' ' ? N5 B1 N1 112.0(14) ' ' ' ' ? N5 B1 N3 110.2(14) ' ' ' ' ? N1 B1 N3 111.9(14) ' ' ' ' ? C1 N1 C2 107.2(14) ' ' ' ' ? C1 N1 B1 132.5(14) ' ' ' ' ? C2 N1 B1 120.3(15) ' ' ' ' ? C1 N2 C3 110.2(15) ' ' ' ' ? C1 N2 C4 124.9(16) ' ' ' ' ? C3 N2 C4 124.8(16) ' ' ' ' ? C5 N3 C6 106.8(15) ' ' ' ' ? C5 N3 B1 133.3(15) ' ' ' ' ? C6 N3 B1 119.9(15) ' ' ' ' ? C5 N4 C7 108.0(16) ' ' ' ' ? C5 N4 C8 128.5(17) ' ' ' ' ? C7 N4 C8 123.4(16) ' ' ' ' ? C9 N5 C10 105.3(14) ' ' ' ' ? C9 N5 B1 134.5(16) ' ' ' ' ? C10 N5 B1 119.6(15) ' ' ' ' ? C11 N6 C9 112.7(16) ' ' ' ' ? C11 N6 C12 120.6(17) ' ' ' ' ? C9 N6 C12 126.3(16) ' ' ' ' ? C18 O4 C16 112.4(18) ' ' ' ' ? C1 S1 W1 107.4(6) ' ' ' ' ? C5 S2 W1 106.9(5) ' ' ' ' ? C9 S3 W1 108.4(6) ' ' ' ' ? C15 W1 C13 70.7(9) ' ' ' ' ? C15 W1 C14 104.6(8) ' ' ' ' ? C13 W1 C14 75.3(7) ' ' ' ' ? C15 W1 S1 75.2(7) ' ' ' ' ? C13 W1 S1 129.0(6) ' ' ' ' ? C14 W1 S1 78.1(5) ' ' ' ' ? C15 W1 S2 76.6(6) ' ' ' ' ? C13 W1 S2 115.8(6) ' ' ' ' ? C14 W1 S2 168.1(5) ' ' ' ' ? S1 W1 S2 91.02(14) ' ' ' ' ? C15 W1 S3 157.0(7) ' ' ' ' ? C13 W1 S3 132.3(6) ' ' ' ' ? C14 W1 S3 84.4(5) ' ' ' ' ? S1 W1 S3 86.32(14) ' ' ' ' ? S2 W1 S3 90.35(14) ' ' ' ' ? C15 W1 I1 121.4(7) ' ' ' ' ? C13 W1 I1 69.3(6) ' ' ' ' ? C14 W1 I1 104.6(5) ' ' ' ' ? S1 W1 I1 160.69(11) ' ' ' ' ? S2 W1 I1 84.24(10) ' ' ' ' ? S3 W1 I1 75.03(10) ' ' ' ' ? #===END