# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- all7a.cif' #============================================================================== # SUBMISSION DETAILS # ================== _publ_contact_author_name 'Professor W. Levason' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3792' _publ_contact_letter ; February 2011 Dear Sirs, This file contains crystallographic data in cif format for seven structures. It is offered as supporting information to accompany a paper to be submitted shortly. William Levason ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Hybrid Dibismuthines and Distibines: Complexes of Antimony- and Bismuth-Oxygen, -Sulfur and -Nitrogen Donor Ligands with Chromium, Tungsten and Manganese Carbonyls ; loop_ _publ_author_name _publ_author_address S.L.Benjamin ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.C.Rogers ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # 10slb049a2.cif # 10slb096xb.cif # 10slbfaccr1.cif # 10slbCrSb2O1.cif # 10slb098x2.cif # 10mr328a.cif # 11slbcrsb2nxa.cif #============================================================================ # 10slb049a2.cif data_10slb049a _database_code_depnum_ccdc_archive 'CCDC 817769' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-07-18 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetracarbonyl(1,5-bis(dimethylstibino)-3-oxapentane-Sb,Sb')tungsten(0) ; # Me2Sb(CH2)2O(CH2)2SbMe2 = C8H20OSb2 # (oxydiethane-2,1-diyl)bis(dimethylstibine) (ACD iLab defaults) # (oxydiethane-2,1-diyl)bis(dimethylstibane) (iLab selected options) # 1,5-bis(dimethylstibino)-3-oxapentane (wl suggestion, see refcode RIPNOU) # 1,5-bis(dimethylstibanyl)-3-oxapentane (from above) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 O5 Sb2 W' _chemical_formula_sum 'C12 H20 O5 Sb2 W' _chemical_formula_structural '(C8 H20 O Sb2) (C O)4 W' _chemical_formula_weight 671.63 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' 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 7.229(2) _cell_length_b 14.047(5) _cell_length_c 18.191(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.26(2) _cell_angle_gamma 90.00 _cell_volume 1839.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2881 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 9.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5296 # 0.5275 _exptl_absorpt_correction_T_max 1.0000 # 0.8379 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13234 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3519 _reflns_number_gt 3025 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. C6 has been artificially split into two sites C6A C6B to allow the addition of H atoms in calc positions. C6A & C6B have the same coordinates and Uij values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+55.8528P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3519 _refine_ls_number_parameters 218 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 W1 W 1.02580(7) 0.67337(4) 0.17617(3) 0.03968(18) Uani 1 1 d . A . Sb1 Sb 0.94832(16) 0.86288(8) 0.18262(7) 0.0704(4) Uani 1 1 d D . . Sb2 Sb 1.12360(14) 0.68870(7) 0.03477(5) 0.0492(3) Uani 1 1 d . . . O1A O 0.922(3) 0.8833(16) -0.0065(12) 0.068(7) Uani 0.51(3) 1 d PDU A 1 O1B O 0.804(5) 0.832(2) 0.0295(15) 0.089(11) Uani 0.49(3) 1 d PDU A 2 O2 O 1.4343(15) 0.7237(9) 0.2438(6) 0.071(3) Uani 1 1 d . A . O3 O 0.902(2) 0.6462(13) 0.3344(7) 0.102(5) Uani 1 1 d . A . O4 O 1.123(2) 0.4558(9) 0.1712(8) 0.094(5) Uani 1 1 d . A . O5 O 0.6130(14) 0.6313(8) 0.1090(6) 0.062(3) Uani 1 1 d . A . C1 C 1.164(3) 0.9620(12) 0.1586(11) 0.092(7) Uani 1 1 d . A . H1A H 1.2817 0.9434 0.1859 0.138 Uiso 1 1 calc R . . H1B H 1.1301 1.0262 0.1735 0.138 Uiso 1 1 calc R . . H1C H 1.1781 0.9612 0.1055 0.138 Uiso 1 1 calc R . . C2 C 0.874(4) 0.914(2) 0.2846(17) 0.153(14) Uani 1 1 d . A . H2A H 0.9684 0.8951 0.3240 0.230 Uiso 1 1 calc R . . H2B H 0.7535 0.8883 0.2944 0.230 Uiso 1 1 calc R . . H2C H 0.8669 0.9841 0.2828 0.230 Uiso 1 1 calc R . . C3A C 0.750(6) 0.931(3) 0.103(2) 0.085(15) Uani 0.51(3) 1 d PDU A 1 H3A1 H 0.6239 0.9184 0.1188 0.103 Uiso 0.51(3) 1 calc PR A 1 H3A2 H 0.7704 1.0003 0.1068 0.103 Uiso 0.51(3) 1 calc PR A 1 C4A C 0.749(4) 0.902(4) 0.0224(17) 0.098(15) Uani 0.51(3) 1 d PDU A 1 H4A1 H 0.6705 0.8449 0.0146 0.118 Uiso 0.51(3) 1 calc PR A 1 H4A2 H 0.6869 0.9540 -0.0076 0.118 Uiso 0.51(3) 1 calc PR A 1 C5A C 0.927(7) 0.8228(15) -0.0699(16) 0.105(15) Uani 0.51(3) 1 d PDU A 1 H5A1 H 1.0420 0.8363 -0.0935 0.126 Uiso 0.51(3) 1 calc PR A 1 H5A2 H 0.8205 0.8393 -0.1059 0.126 Uiso 0.51(3) 1 calc PR A 1 C6A C 0.919(3) 0.7170(12) -0.0540(9) 0.077(5) Uani 0.51(3) 1 d PDU A 1 H6A1 H 0.9455 0.6800 -0.0982 0.092 Uiso 0.51(3) 1 calc PR A 1 H6A2 H 0.7945 0.6991 -0.0403 0.092 Uiso 0.51(3) 1 calc PR A 1 C3B C 0.687(5) 0.913(4) 0.130(3) 0.085(14) Uani 0.49(3) 1 d PDU A 2 H3B1 H 0.5868 0.8646 0.1295 0.102 Uiso 0.49(3) 1 calc PR A 2 H3B2 H 0.6453 0.9734 0.1515 0.102 Uiso 0.49(3) 1 calc PR A 2 C4B C 0.761(7) 0.926(3) 0.056(3) 0.105(16) Uani 0.49(3) 1 d PDU A 2 H4B1 H 0.6667 0.9573 0.0206 0.126 Uiso 0.49(3) 1 calc PR A 2 H4B2 H 0.8741 0.9662 0.0603 0.126 Uiso 0.49(3) 1 calc PR A 2 C5B C 0.813(6) 0.807(2) -0.0449(17) 0.077(10) Uani 0.49(3) 1 d PDU A 2 H5B1 H 0.8731 0.8598 -0.0702 0.092 Uiso 0.49(3) 1 calc PR A 2 H5B2 H 0.6852 0.7999 -0.0689 0.092 Uiso 0.49(3) 1 calc PR A 2 C6B C 0.919(3) 0.7170(12) -0.0540(9) 0.077(5) Uani 0.49(3) 1 d PDU A 2 H6B1 H 0.9807 0.7208 -0.1004 0.092 Uiso 0.49(3) 1 calc PR A 2 H6B2 H 0.8306 0.6631 -0.0588 0.092 Uiso 0.49(3) 1 calc PR A 2 C7 C 1.240(2) 0.5645(13) -0.0107(9) 0.069(5) Uani 1 1 d . A . H7A H 1.3404 0.5398 0.0241 0.104 Uiso 1 1 calc R . . H7B H 1.2901 0.5809 -0.0573 0.104 Uiso 1 1 calc R . . H7C H 1.1436 0.5158 -0.0196 0.104 Uiso 1 1 calc R . . C8 C 1.327(3) 0.7888(15) 0.0077(9) 0.083(6) Uani 1 1 d . A . H8A H 1.4346 0.7853 0.0444 0.124 Uiso 1 1 calc R . . H8B H 1.2739 0.8531 0.0075 0.124 Uiso 1 1 calc R . . H8C H 1.3654 0.7742 -0.0413 0.124 Uiso 1 1 calc R . . C9 C 1.288(2) 0.7045(10) 0.2180(7) 0.048(3) Uani 1 1 d . . . C10 C 0.944(2) 0.6549(13) 0.2776(9) 0.066(4) Uani 1 1 d . . . C11 C 1.084(3) 0.5389(11) 0.1739(9) 0.066(5) Uani 1 1 d . . . C12 C 0.761(2) 0.6469(9) 0.1329(8) 0.047(3) 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 W1 0.0477(3) 0.0396(3) 0.0313(3) -0.00323(19) 0.0009(2) -0.0005(2) Sb1 0.0661(7) 0.0463(6) 0.0936(9) -0.0297(6) -0.0210(6) 0.0146(5) Sb2 0.0564(6) 0.0606(6) 0.0295(4) -0.0019(4) -0.0027(4) 0.0027(4) O1A 0.061(12) 0.070(10) 0.067(14) 0.007(10) -0.030(10) -0.013(11) O1B 0.10(2) 0.088(19) 0.074(15) -0.005(14) -0.014(15) 0.015(17) O2 0.052(6) 0.092(9) 0.065(7) -0.019(6) -0.008(5) -0.001(6) O3 0.117(12) 0.151(14) 0.043(7) -0.012(8) 0.023(7) -0.042(10) O4 0.125(12) 0.052(7) 0.094(10) -0.013(6) -0.047(8) 0.013(7) O5 0.046(6) 0.065(7) 0.073(7) -0.011(5) -0.001(5) -0.004(5) C1 0.127(17) 0.048(9) 0.089(13) -0.002(9) -0.059(12) -0.021(10) C2 0.095(17) 0.18(3) 0.19(3) -0.14(3) 0.027(18) 0.016(18) C3A 0.05(2) 0.06(3) 0.14(3) -0.04(3) -0.02(2) 0.02(2) C4A 0.062(17) 0.17(4) 0.062(17) 0.085(19) -0.010(15) -0.01(2) C5A 0.12(4) 0.068(12) 0.11(3) -0.025(17) -0.08(2) 0.01(2) C6A 0.092(13) 0.080(9) 0.052(9) 0.000(7) -0.025(8) 0.009(9) C3B 0.06(3) 0.06(3) 0.13(3) -0.03(2) -0.01(2) 0.01(2) C4B 0.09(3) 0.11(3) 0.10(3) -0.05(2) -0.03(3) 0.01(3) C5B 0.09(3) 0.058(18) 0.082(17) -0.015(17) 0.00(2) -0.018(14) C6B 0.092(13) 0.080(9) 0.052(9) 0.000(7) -0.025(8) 0.009(9) C7 0.056(9) 0.088(12) 0.063(10) -0.039(9) 0.004(7) 0.015(9) C8 0.104(15) 0.096(14) 0.047(9) 0.023(9) 0.005(9) -0.033(12) C9 0.054(8) 0.054(8) 0.034(6) -0.002(6) -0.003(6) -0.002(6) C10 0.073(11) 0.077(11) 0.049(9) -0.010(8) 0.013(8) -0.029(9) C11 0.092(12) 0.041(8) 0.057(9) -0.006(7) -0.034(8) 0.005(8) C12 0.055(9) 0.039(7) 0.046(7) -0.006(6) 0.006(6) -0.001(6) _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 W1 C11 1.937(15) . ? W1 C10 2.004(16) . ? W1 C9 2.026(14) . ? W1 C12 2.036(15) . ? W1 Sb1 2.7250(14) . ? W1 Sb2 2.7378(13) . ? Sb1 C2 2.11(2) . ? Sb1 C3B 2.16(3) . ? Sb1 C1 2.16(2) . ? Sb1 C3A 2.16(3) . ? Sb2 C6A 2.124(15) . ? Sb2 C8 2.123(17) . ? Sb2 C7 2.136(15) . ? O1A C4A 1.426(19) . ? O1A C5A 1.434(19) . ? O1B C5B 1.405(19) . ? O1B C4B 1.448(19) . ? O2 C9 1.147(16) . ? O3 C10 1.112(19) . ? O4 C11 1.202(18) . ? O5 C12 1.139(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3A C4A 1.526(19) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.516(19) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C3B C4B 1.52(2) . ? C3B H3B1 0.9900 . ? C3B H3B2 0.9900 . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 C11 W1 C10 88.6(8) . . ? C11 W1 C9 91.2(6) . . ? C10 W1 C9 91.5(6) . . ? C11 W1 C12 90.7(6) . . ? C10 W1 C12 89.3(6) . . ? C9 W1 C12 178.0(6) . . ? C11 W1 Sb1 178.6(4) . . ? C10 W1 Sb1 90.5(5) . . ? C9 W1 Sb1 87.8(4) . . ? C12 W1 Sb1 90.3(4) . . ? C11 W1 Sb2 88.9(5) . . ? C10 W1 Sb2 176.3(4) . . ? C9 W1 Sb2 91.3(4) . . ? C12 W1 Sb2 88.1(4) . . ? Sb1 W1 Sb2 92.03(4) . . ? C2 Sb1 C3B 89.6(15) . . ? C2 Sb1 C1 101.7(10) . . ? C3B Sb1 C1 108.7(16) . . ? C2 Sb1 C3A 103.2(14) . . ? C3B Sb1 C3A 19.7(17) . . ? C1 Sb1 C3A 91.7(16) . . ? C2 Sb1 W1 116.4(10) . . ? C3B Sb1 W1 118.4(15) . . ? C1 Sb1 W1 117.7(6) . . ? C3A Sb1 W1 121.9(11) . . ? C6A Sb2 C8 98.5(8) . . ? C6A Sb2 C7 97.5(7) . . ? C8 Sb2 C7 98.3(8) . . ? C6A Sb2 W1 120.5(6) . . ? C8 Sb2 W1 120.9(5) . . ? C7 Sb2 W1 116.4(5) . . ? C4A O1A C5A 120(3) . . ? C5B O1B C4B 125(3) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4A C3A Sb1 118(2) . . ? C4A C3A H3A1 107.8 . . ? Sb1 C3A H3A1 107.8 . . ? C4A C3A H3A2 107.8 . . ? Sb1 C3A H3A2 107.8 . . ? H3A1 C3A H3A2 107.1 . . ? O1A C4A C3A 119(3) . . ? O1A C4A H4A1 107.6 . . ? C3A C4A H4A1 107.6 . . ? O1A C4A H4A2 107.6 . . ? C3A C4A H4A2 107.6 . . ? H4A1 C4A H4A2 107.1 . . ? O1A C5A C6A 115(2) . . ? O1A C5A H5A1 108.5 . . ? C6A C5A H5A1 108.5 . . ? O1A C5A H5A2 108.5 . . ? C6A C5A H5A2 108.5 . . ? H5A1 C5A H5A2 107.5 . . ? C5A C6A Sb2 107.1(16) . . ? C5A C6A H6A1 110.3 . . ? Sb2 C6A H6A1 110.3 . . ? C5A C6A H6A2 110.3 . . ? Sb2 C6A H6A2 110.3 . . ? H6A1 C6A H6A2 108.6 . . ? C4B C3B Sb1 94(3) . . ? C4B C3B H3B1 113.0 . . ? Sb1 C3B H3B1 113.0 . . ? C4B C3B H3B2 112.9 . . ? Sb1 C3B H3B2 112.9 . . ? H3B1 C3B H3B2 110.4 . . ? O1B C4B C3B 106(4) . . ? O1B C4B H4B1 110.4 . . ? C3B C4B H4B1 110.4 . . ? O1B C4B H4B2 110.4 . . ? C3B C4B H4B2 110.4 . . ? H4B1 C4B H4B2 108.6 . . ? O1B C5B H5B1 109.1 . . ? O1B C5B H5B2 109.1 . . ? H5B1 C5B H5B2 107.8 . . ? Sb2 C7 H7A 109.5 . . ? Sb2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Sb2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Sb2 C8 H8A 109.5 . . ? Sb2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Sb2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 W1 177.6(13) . . ? O3 C10 W1 178.4(15) . . ? O4 C11 W1 178.4(19) . . ? O5 C12 W1 179.4(14) . . ? 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 Sb1 C3A C4A O1A -37(6) . . . . ? C3A C4A O1A C5A 156(4) . . . . ? C4A O1A C5A C6A -80(4) . . . . ? O1A C5A C6A Sb2 -50(4) . . . . ? Sb1 C3B C4B O1B 67(4) . . . . ? C3B C4B O1B C5B 157(4) . . . . ? C4B O1B C5B C6B 161(4) . . . . ? O1B C5B C6B Sb2 -27(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 5.038 _refine_diff_density_min -3.015 _refine_diff_density_rms 0.254 #===END OF CIF ============================================================== # 10slb096xb.cif data_10slb096x _database_code_depnum_ccdc_archive 'CCDC 817770' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-11-19 _audit_author_name 'Benjamin, Sophie L.' _audit_update_record '2010-12-14 re-ordered atom list' _chemical_name_systematic ; tricarbonyl(bis[(2-dimethylstibino)benzyl]sulfide)manganese(I) trifluoromethanesulfonate ; # [{o-C6H4(SbMe2)(CH2)}2S] = [C18H24SSb2] # [thiobis(methylene-2,1-phenylene)]bis(dimethylstibine) (iLab defaults) # [sulfanediylbis(methanediylbenzene-2,1-diyl)]bis(dimethylstibane) # (iLab selected options) # bis[(2-dimethylstibino)benzyl]sulfide (based on slb suggestion) # bis[(2-dimethylstibanyl)benzyl]sulfane (based on slb suggestion) # [F3CSO3]- = triflate anion # trifluoromethanesulphonate (from CSD search - very few hits(2?)) # trifluoromethanesulfonate (from CSD search - many hits with 'f' spelling) # trifluoromethanesulfonate (iLab defaults & selected options) # (sodium) trifluoromethanesulfonate (chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 Mn O3 S Sb2 1+, C F3 O3 S 1-' _chemical_formula_sum 'C22 H24 F3 Mn O6 S2 Sb2' _chemical_formula_structural '((C18 H24 S Sb2) Mn (C O)3) (C F3 S O3)' _chemical_formula_weight 803.97 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/m' _space_group_name_Hall '-P 2yb' _space_group_IT_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.7926(10) _cell_length_b 14.589(2) _cell_length_c 11.1433(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.534(8) _cell_angle_gamma 90.00 _cell_volume 1370.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3146 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 2.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7585 # exptl Tmin _exptl_absorpt_correction_T_max 1.0000 # and Tmax _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14910 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.56 _reflns_number_total 3233 _reflns_number_gt 3030 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+2.0054P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3233 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.83571(6) 0.2500 0.83382(4) 0.01936(11) Uani 1 2 d S . . Sb1 Sb 0.78636(2) 0.120612(11) 0.670520(14) 0.02549(7) Uani 1 1 d . . . S1 S 0.56547(10) 0.2500 0.83018(8) 0.02696(19) Uani 1 2 d S . . S2 S 0.09710(12) 0.2500 0.46660(8) 0.0305(2) Uani 1 2 d S . . F1 F 0.0630(3) 0.2500 0.2249(2) 0.0388(5) Uani 1 2 d S . . F2 F -0.1189(2) 0.17640(13) 0.27852(15) 0.0438(4) Uani 1 1 d . . . O1 O 0.8967(3) 0.10308(14) 1.02526(17) 0.0366(5) Uani 1 1 d . . . O2 O 1.1758(3) 0.2500 0.8527(3) 0.0393(7) Uani 1 2 d S . . O3 O -0.0181(4) 0.2500 0.5368(2) 0.0362(6) Uani 1 2 d S . . O4 O 0.1856(3) 0.16625(16) 0.47522(19) 0.0464(5) Uani 1 1 d . . . C1 C 0.6519(4) 0.1246(2) 0.4789(3) 0.0444(8) Uani 1 1 d . . . H1A H 0.5568 0.1621 0.4698 0.067 Uiso 1 1 calc R . . H1B H 0.6206 0.0622 0.4495 0.067 Uiso 1 1 calc R . . H1C H 0.7164 0.1513 0.4291 0.067 Uiso 1 1 calc R . . C2 C 0.9814(4) 0.0376(2) 0.6672(3) 0.0417(7) Uani 1 1 d . . . H2A H 1.0551 0.0729 0.6339 0.062 Uiso 1 1 calc R . . H2B H 0.9438 -0.0159 0.6138 0.062 Uiso 1 1 calc R . . H2C H 1.0358 0.0172 0.7524 0.062 Uiso 1 1 calc R . . C3 C 0.6489(3) 0.0284(2) 0.7454(2) 0.0336(6) Uani 1 1 d . . . C4 C 0.6998(4) -0.0599(2) 0.7802(3) 0.0456(8) Uani 1 1 d . . . H4 H 0.7920 -0.0829 0.7621 0.055 Uiso 1 1 calc R . . C5 C 0.6169(6) -0.1153(2) 0.8416(4) 0.0610(11) Uani 1 1 d . . . H5 H 0.6525 -0.1759 0.8655 0.073 Uiso 1 1 calc R . . C6 C 0.4825(5) -0.0820(3) 0.8677(3) 0.0626(11) Uani 1 1 d . . . H6 H 0.4253 -0.1200 0.9090 0.075 Uiso 1 1 calc R . . C7 C 0.4314(4) 0.0059(3) 0.8341(3) 0.0503(9) Uani 1 1 d . . . H7 H 0.3393 0.0284 0.8529 0.060 Uiso 1 1 calc R . . C8 C 0.5131(3) 0.0625(2) 0.7729(2) 0.0370(7) Uani 1 1 d . . . C9 C 0.4515(3) 0.1566(2) 0.7337(3) 0.0376(7) Uani 1 1 d . . . H9A H 0.3402 0.1603 0.7365 0.045 Uiso 1 1 calc R . . H9B H 0.4514 0.1663 0.6457 0.045 Uiso 1 1 calc R . . C10 C 0.8706(3) 0.15979(18) 0.9516(2) 0.0253(5) Uani 1 1 d . . . C11 C 1.0416(4) 0.2500 0.8414(3) 0.0261(7) Uani 1 2 d S . . C12 C -0.0265(5) 0.2500 0.3040(3) 0.0295(8) Uani 1 2 d S . . 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 Mn1 0.0200(2) 0.0216(2) 0.0157(2) 0.000 0.00383(18) 0.000 Sb1 0.02991(11) 0.02582(10) 0.02123(10) -0.00533(6) 0.00808(7) -0.00423(6) S1 0.0221(4) 0.0349(5) 0.0240(4) 0.000 0.0067(3) 0.000 S2 0.0356(5) 0.0326(5) 0.0202(4) 0.000 0.0027(3) 0.000 F1 0.0448(14) 0.0477(14) 0.0260(11) 0.000 0.0132(10) 0.000 F2 0.0494(10) 0.0473(10) 0.0326(8) -0.0103(8) 0.0079(7) -0.0182(8) O1 0.0503(12) 0.0310(10) 0.0252(9) 0.0064(8) 0.0056(8) -0.0001(9) O2 0.0266(15) 0.0488(18) 0.0437(16) 0.000 0.0122(12) 0.000 O3 0.0509(18) 0.0347(15) 0.0243(13) 0.000 0.0131(12) 0.000 O4 0.0504(13) 0.0492(13) 0.0346(11) 0.0065(10) 0.0042(9) 0.0191(11) C1 0.0531(19) 0.055(2) 0.0222(13) -0.0099(12) 0.0055(12) -0.0168(15) C2 0.0493(18) 0.0304(15) 0.0522(18) -0.0033(13) 0.0255(15) 0.0050(13) C3 0.0391(15) 0.0341(14) 0.0284(13) -0.0073(11) 0.0108(11) -0.0132(12) C4 0.063(2) 0.0338(16) 0.0412(17) -0.0062(13) 0.0163(15) -0.0125(15) C5 0.096(3) 0.0376(19) 0.050(2) -0.0033(15) 0.021(2) -0.0253(19) C6 0.086(3) 0.065(3) 0.0414(18) -0.0107(17) 0.0257(19) -0.046(2) C7 0.0495(19) 0.066(2) 0.0387(16) -0.0151(16) 0.0179(14) -0.0307(17) C8 0.0360(15) 0.0467(17) 0.0273(13) -0.0124(12) 0.0072(11) -0.0172(13) C9 0.0223(13) 0.0566(19) 0.0319(14) -0.0112(13) 0.0044(10) -0.0099(12) C10 0.0281(12) 0.0275(12) 0.0193(11) -0.0041(10) 0.0050(9) -0.0019(10) C11 0.0287(19) 0.0282(18) 0.0221(16) 0.000 0.0088(14) 0.000 C12 0.033(2) 0.0296(19) 0.0238(17) 0.000 0.0052(14) 0.000 _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 Mn1 C11 1.788(4) . ? Mn1 C10 1.822(3) 4_565 ? Mn1 C10 1.822(3) . ? Mn1 S1 2.3649(11) . ? Mn1 Sb1 2.5716(4) . ? Mn1 Sb1 2.5716(4) 4_565 ? Sb1 C2 2.108(3) . ? Sb1 C1 2.127(3) . ? Sb1 C3 2.131(3) . ? S1 C9 1.844(3) . ? S1 C9 1.844(3) 4_565 ? S2 O4 1.437(2) 4_565 ? S2 O4 1.437(2) . ? S2 O3 1.445(3) . ? S2 C12 1.829(4) . ? F1 C12 1.337(4) . ? F2 C12 1.327(3) . ? O1 C10 1.142(3) . ? O2 C11 1.151(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.383(4) . ? C3 C8 1.405(4) . ? C4 C5 1.391(5) . ? C4 H4 0.9500 . ? C5 C6 1.383(6) . ? C5 H5 0.9500 . ? C6 C7 1.376(6) . ? C6 H6 0.9500 . ? C7 C8 1.394(4) . ? C7 H7 0.9500 . ? C8 C9 1.495(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C12 F2 1.327(3) 4_565 ? 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 C11 Mn1 C10 90.32(11) . 4_565 ? C11 Mn1 C10 90.32(11) . . ? C10 Mn1 C10 92.52(15) 4_565 . ? C11 Mn1 S1 178.36(11) . . ? C10 Mn1 S1 88.54(8) 4_565 . ? C10 Mn1 S1 88.54(8) . . ? C11 Mn1 Sb1 89.88(8) . . ? C10 Mn1 Sb1 179.01(8) 4_565 . ? C10 Mn1 Sb1 86.52(8) . . ? S1 Mn1 Sb1 91.23(2) . . ? C11 Mn1 Sb1 89.88(8) . 4_565 ? C10 Mn1 Sb1 86.52(8) 4_565 4_565 ? C10 Mn1 Sb1 179.01(8) . 4_565 ? S1 Mn1 Sb1 91.23(2) . 4_565 ? Sb1 Mn1 Sb1 94.45(2) . 4_565 ? C2 Sb1 C1 102.74(13) . . ? C2 Sb1 C3 101.48(12) . . ? C1 Sb1 C3 101.25(11) . . ? C2 Sb1 Mn1 117.38(9) . . ? C1 Sb1 Mn1 128.61(10) . . ? C3 Sb1 Mn1 100.75(7) . . ? C9 S1 C9 95.2(2) . 4_565 ? C9 S1 Mn1 112.72(10) . . ? C9 S1 Mn1 112.72(10) 4_565 . ? O4 S2 O4 116.4(2) 4_565 . ? O4 S2 O3 114.43(11) 4_565 . ? O4 S2 O3 114.43(11) . . ? O4 S2 C12 102.95(11) 4_565 . ? O4 S2 C12 102.95(11) . . ? O3 S2 C12 103.06(18) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 119.7(3) . . ? C4 C3 Sb1 121.6(2) . . ? C8 C3 Sb1 118.3(2) . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.9(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.8(4) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C3 119.1(3) . . ? C7 C8 C9 119.5(3) . . ? C3 C8 C9 121.4(3) . . ? C8 C9 S1 114.60(19) . . ? C8 C9 H9A 108.6 . . ? S1 C9 H9A 108.6 . . ? C8 C9 H9B 108.6 . . ? S1 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? O1 C10 Mn1 178.1(2) . . ? O2 C11 Mn1 176.6(3) . . ? F2 C12 F2 108.0(3) . 4_565 ? F2 C12 F1 107.4(2) . . ? F2 C12 F1 107.4(2) 4_565 . ? F2 C12 S2 111.51(19) . . ? F2 C12 S2 111.51(19) 4_565 . ? F1 C12 S2 110.9(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.681 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.077 #===END OF CIF ============================================================== # 10slbfaccr1.cif data_10slbfaccr _database_code_depnum_ccdc_archive 'CCDC 817771' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-09-26 _audit_author_name 'Benjamin, Sophie L.' _audit_update_record '2010-12-15 Revised numbering scheme (mw)' _chemical_name_systematic ; Tricarbonyl(bis[(2-dimethylstibino)benzyl]sulfide)chromium(0) ; # [{o-C6H4(SbMe2)(CH2)}2S] = [C18H24SSb2] # [thiobis(methylene-2,1-phenylene)]bis(dimethylstibine) (iLab defaults) # [sulfanediylbis(methanediylbenzene-2,1-diyl)]bis(dimethylstibane) # (iLab selected options) # bis[(2-dimethylstibino)benzyl]sulfide (based on slb suggestion) # bis[(2-dimethylstibanyl)benzyl]sulfane (based on slb suggestion) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 Cr O3 S Sb2' _chemical_formula_sum 'C21 H24 Cr O3 S Sb2' _chemical_formula_structural '(C18 H24 S Sb2) Cr (C O)3' _chemical_formula_weight 651.96 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 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 12.6781(10) _cell_length_b 11.2606(10) _cell_length_c 16.5520(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.357(5) _cell_angle_gamma 90.00 _cell_volume 2363.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23271 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rhombus _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 2.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8574 # Exptl Tmin _exptl_absorpt_correction_T_max 1.0000 # and Tmax _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29464 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5404 _reflns_number_gt 4746 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.1018P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5404 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.28764(4) 0.12582(5) 0.79887(3) 0.01925(12) Uani 1 1 d . . . Sb1 Sb 0.315430(18) 0.23729(2) 0.663225(14) 0.01941(7) Uani 1 1 d . . . Sb2 Sb 0.106127(18) 0.03685(2) 0.757348(15) 0.02182(7) Uani 1 1 d . . . S1 S 0.37245(7) -0.04540(8) 0.74067(5) 0.02001(18) Uani 1 1 d . . . O1 O 0.2681(3) 0.0074(3) 0.96016(17) 0.0430(8) Uani 1 1 d . . . O2 O 0.1991(2) 0.3538(3) 0.86330(18) 0.0361(7) Uani 1 1 d . . . O3 O 0.5014(2) 0.1976(3) 0.85955(19) 0.0389(7) Uani 1 1 d . . . C1 C 0.3377(3) 0.4247(3) 0.6657(3) 0.0315(9) Uani 1 1 d . . . H1A H 0.2750 0.4628 0.6884 0.047 Uiso 1 1 calc R . . H1B H 0.3490 0.4538 0.6106 0.047 Uiso 1 1 calc R . . H1C H 0.3993 0.4438 0.6993 0.047 Uiso 1 1 calc R . . C2 C 0.2121(3) 0.2263(4) 0.5609(2) 0.0337(9) Uani 1 1 d . . . H2A H 0.1412 0.2518 0.5764 0.051 Uiso 1 1 calc R . . H2B H 0.2095 0.1441 0.5415 0.051 Uiso 1 1 calc R . . H2C H 0.2384 0.2779 0.5178 0.051 Uiso 1 1 calc R . . C3 C 0.4602(3) 0.1776(3) 0.6125(2) 0.0225(8) Uani 1 1 d . . . C4 C 0.5394(3) 0.2561(4) 0.5898(2) 0.0256(8) Uani 1 1 d . . . H4 H 0.5258 0.3391 0.5892 0.031 Uiso 1 1 calc R . . C5 C 0.6377(3) 0.2144(4) 0.5680(2) 0.0292(9) Uani 1 1 d . . . H5 H 0.6906 0.2687 0.5514 0.035 Uiso 1 1 calc R . . C6 C 0.6594(3) 0.0945(4) 0.5702(2) 0.0292(9) Uani 1 1 d . . . H6 H 0.7278 0.0666 0.5568 0.035 Uiso 1 1 calc R . . C7 C 0.5813(3) 0.0144(4) 0.5920(2) 0.0256(8) Uani 1 1 d . . . H7 H 0.5961 -0.0683 0.5928 0.031 Uiso 1 1 calc R . . C8 C 0.4809(3) 0.0552(3) 0.6127(2) 0.0210(7) Uani 1 1 d . . . C9 C 0.3955(3) -0.0341(3) 0.6317(2) 0.0209(7) Uani 1 1 d . . . H9A H 0.4163 -0.1129 0.6106 0.025 Uiso 1 1 calc R . . H9B H 0.3293 -0.0102 0.6043 0.025 Uiso 1 1 calc R . . C10 C 0.2873(3) -0.1781(3) 0.7407(2) 0.0232(8) Uani 1 1 d . . . H10A H 0.3329 -0.2492 0.7362 0.028 Uiso 1 1 calc R . . H10B H 0.2512 -0.1824 0.7935 0.028 Uiso 1 1 calc R . . C11 C 0.2050(3) -0.1842(3) 0.6752(2) 0.0216(7) Uani 1 1 d . . . C12 C 0.2135(3) -0.2735(3) 0.6174(2) 0.0251(8) Uani 1 1 d . . . H12 H 0.2722 -0.3258 0.6188 0.030 Uiso 1 1 calc R . . C13 C 0.1373(3) -0.2868(4) 0.5581(2) 0.0324(9) Uani 1 1 d . . . H13 H 0.1424 -0.3501 0.5204 0.039 Uiso 1 1 calc R . . C14 C 0.0540(3) -0.2088(4) 0.5535(3) 0.0345(10) Uani 1 1 d . . . H14 H 0.0023 -0.2175 0.5121 0.041 Uiso 1 1 calc R . . C15 C 0.0457(3) -0.1175(4) 0.6092(2) 0.0298(9) Uani 1 1 d . . . H15 H -0.0112 -0.0629 0.6050 0.036 Uiso 1 1 calc R . . C16 C 0.1197(3) -0.1044(3) 0.6714(2) 0.0208(7) Uani 1 1 d . . . C17 C 0.0181(3) -0.0532(4) 0.8491(3) 0.0364(10) Uani 1 1 d . . . H17A H 0.0051 0.0013 0.8941 0.055 Uiso 1 1 calc R . . H17B H 0.0585 -0.1218 0.8686 0.055 Uiso 1 1 calc R . . H17C H -0.0494 -0.0802 0.8265 0.055 Uiso 1 1 calc R . . C18 C -0.0246(3) 0.1286(4) 0.7057(3) 0.0372(10) Uani 1 1 d . . . H18A H -0.0415 0.1979 0.7390 0.056 Uiso 1 1 calc R . . H18B H -0.0858 0.0754 0.7034 0.056 Uiso 1 1 calc R . . H18C H -0.0068 0.1546 0.6510 0.056 Uiso 1 1 calc R . . C19 C 0.2740(3) 0.0506(3) 0.8971(2) 0.0268(8) Uani 1 1 d . . . C20 C 0.2304(3) 0.2637(3) 0.8387(2) 0.0245(8) Uani 1 1 d . . . C21 C 0.4193(3) 0.1720(3) 0.8332(2) 0.0245(8) 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 Cr1 0.0221(3) 0.0184(3) 0.0173(3) -0.0004(2) 0.0018(2) -0.0030(2) Sb1 0.01977(12) 0.01861(12) 0.01987(12) 0.00275(9) -0.00008(9) -0.00023(9) Sb2 0.01971(12) 0.01850(13) 0.02733(14) -0.00298(9) 0.00560(9) -0.00187(9) S1 0.0199(4) 0.0199(4) 0.0203(4) 0.0016(3) -0.0010(3) -0.0015(3) O1 0.075(2) 0.0314(16) 0.0227(15) 0.0040(12) 0.0059(14) -0.0099(16) O2 0.0319(15) 0.0304(16) 0.0460(18) -0.0121(13) 0.0074(13) 0.0007(13) O3 0.0331(16) 0.0340(17) 0.0493(19) -0.0047(14) -0.0122(14) -0.0069(14) C1 0.032(2) 0.021(2) 0.042(2) 0.0026(17) 0.0013(18) 0.0006(17) C2 0.032(2) 0.040(2) 0.029(2) 0.0046(18) -0.0073(17) -0.0011(19) C3 0.0227(18) 0.031(2) 0.0141(17) 0.0019(14) 0.0010(13) 0.0007(16) C4 0.031(2) 0.026(2) 0.0195(18) -0.0004(15) 0.0015(15) -0.0079(16) C5 0.027(2) 0.039(2) 0.0223(19) -0.0021(17) 0.0068(15) -0.0118(18) C6 0.0205(18) 0.043(2) 0.025(2) -0.0064(17) 0.0049(15) -0.0019(17) C7 0.0272(19) 0.029(2) 0.0211(19) -0.0048(15) 0.0018(15) 0.0011(16) C8 0.0208(17) 0.028(2) 0.0140(17) -0.0004(14) -0.0017(13) 0.0002(15) C9 0.0222(18) 0.0198(18) 0.0206(18) -0.0016(14) 0.0010(14) 0.0010(15) C10 0.0233(18) 0.0190(18) 0.0272(19) 0.0071(15) 0.0008(15) -0.0030(15) C11 0.0217(17) 0.0169(17) 0.0262(19) 0.0028(14) 0.0027(14) -0.0036(15) C12 0.0205(18) 0.0232(19) 0.032(2) -0.0036(15) 0.0094(15) -0.0025(15) C13 0.029(2) 0.035(2) 0.034(2) -0.0115(18) 0.0056(17) -0.0071(18) C14 0.0223(19) 0.047(3) 0.034(2) -0.0115(19) -0.0060(17) -0.0051(19) C15 0.0182(18) 0.036(2) 0.035(2) -0.0087(18) -0.0016(16) -0.0009(17) C16 0.0173(17) 0.0179(17) 0.0274(19) -0.0011(14) 0.0047(14) -0.0028(14) C17 0.040(2) 0.029(2) 0.041(2) -0.0024(18) 0.0179(19) -0.0081(19) C18 0.031(2) 0.032(2) 0.049(3) -0.002(2) 0.0031(19) 0.0090(19) C19 0.036(2) 0.0194(19) 0.025(2) -0.0061(15) 0.0033(16) -0.0041(16) C20 0.0197(18) 0.029(2) 0.0248(19) -0.0030(16) 0.0046(14) -0.0056(16) C21 0.031(2) 0.0198(18) 0.0224(18) 0.0016(14) -0.0003(15) -0.0027(16) _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 Cr1 C21 1.835(4) . ? Cr1 C20 1.838(4) . ? Cr1 C19 1.842(4) . ? Cr1 S1 2.4114(11) . ? Cr1 Sb1 2.5982(6) . ? Cr1 Sb2 2.5985(6) . ? Sb1 C1 2.129(4) . ? Sb1 C3 2.131(4) . ? Sb1 C2 2.139(4) . ? Sb2 C18 2.128(4) . ? Sb2 C16 2.141(4) . ? Sb2 C17 2.145(4) . ? S1 C9 1.833(4) . ? S1 C10 1.844(4) . ? O1 C19 1.155(5) . ? O2 C20 1.164(5) . ? O3 C21 1.162(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.391(5) . ? C3 C8 1.403(5) . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.378(6) . ? C5 H5 0.9500 . ? C6 C7 1.388(5) . ? C6 H6 0.9500 . ? C7 C8 1.398(5) . ? C7 H7 0.9500 . ? C8 C9 1.512(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.501(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.392(5) . ? C11 C16 1.407(5) . ? C12 C13 1.381(5) . ? C12 H12 0.9500 . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 H14 0.9500 . ? C15 C16 1.397(5) . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 C21 Cr1 C20 90.54(16) . . ? C21 Cr1 C19 86.95(17) . . ? C20 Cr1 C19 91.86(17) . . ? C21 Cr1 S1 86.77(12) . . ? C20 Cr1 S1 175.42(12) . . ? C19 Cr1 S1 91.69(12) . . ? C21 Cr1 Sb1 90.16(12) . . ? C20 Cr1 Sb1 87.58(12) . . ? C19 Cr1 Sb1 177.05(12) . . ? S1 Cr1 Sb1 88.73(3) . . ? C21 Cr1 Sb2 173.46(12) . . ? C20 Cr1 Sb2 94.01(11) . . ? C19 Cr1 Sb2 88.20(12) . . ? S1 Cr1 Sb2 88.99(3) . . ? Sb1 Cr1 Sb2 94.72(2) . . ? C1 Sb1 C3 101.86(15) . . ? C1 Sb1 C2 98.81(16) . . ? C3 Sb1 C2 101.21(15) . . ? C1 Sb1 Cr1 118.73(12) . . ? C3 Sb1 Cr1 108.04(10) . . ? C2 Sb1 Cr1 124.82(12) . . ? C18 Sb2 C16 99.18(16) . . ? C18 Sb2 C17 96.12(18) . . ? C16 Sb2 C17 99.41(15) . . ? C18 Sb2 Cr1 127.26(12) . . ? C16 Sb2 Cr1 112.79(9) . . ? C17 Sb2 Cr1 117.30(13) . . ? C9 S1 C10 98.82(16) . . ? C9 S1 Cr1 114.32(12) . . ? C10 S1 Cr1 112.68(13) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 119.3(3) . . ? C4 C3 Sb1 122.1(3) . . ? C8 C3 Sb1 118.1(3) . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 119.6(3) . . ? C7 C8 C9 119.1(3) . . ? C3 C8 C9 121.3(3) . . ? C8 C9 S1 111.7(2) . . ? C8 C9 H9A 109.3 . . ? S1 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? S1 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C11 C10 S1 116.2(2) . . ? C11 C10 H10A 108.2 . . ? S1 C10 H10A 108.2 . . ? C11 C10 H10B 108.2 . . ? S1 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C16 119.6(3) . . ? C12 C11 C10 118.2(3) . . ? C16 C11 C10 122.2(3) . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.3(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 121.0(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 118.5(3) . . ? C15 C16 Sb2 120.8(3) . . ? C11 C16 Sb2 120.7(3) . . ? Sb2 C17 H17A 109.5 . . ? Sb2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Sb2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Sb2 C18 H18A 109.5 . . ? Sb2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Sb2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 Cr1 177.0(3) . . ? O2 C20 Cr1 176.6(3) . . ? O3 C21 Cr1 175.7(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.636 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.122 #===END OF CIF ============================================================== # 10slbCrSb2O1.cif data_10slbcrsb2o _database_code_depnum_ccdc_archive 'CCDC 817772' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-09-30 _audit_author_name 'Benjamin, Sophie L.' _audit_update_record ; 2010-12-16 Re-ordered atom list 2011-01-03 Added Sb...O1A/O1B contacts ; _chemical_name_systematic ; Tetracarbonyl(1,5-bis(dimethylstibino)-3-oxapentane)chromium(0) ; # Me2Sb(CH2)2O(CH2)2SbMe2 = C8H20OSb2 # (oxydiethane-2,1-diyl)bis(dimethylstibine) (ACD iLab defaults) # (oxydiethane-2,1-diyl)bis(dimethylstibane) (iLab selected options) # 1,5-bis(dimethylstibino)-3-oxapentane (wl suggestion, see refcode RIPNOU) # 1,5-bis(dimethylstibanyl)-3-oxapentane (from above) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 Cr O5 Sb2' _chemical_formula_sum 'C12 H20 Cr O5 Sb2' _chemical_formula_structural '((C8 H20 O Sb2) (C O)4 Cr)' _chemical_formula_weight 539.78 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _space_group_name_Hall '-P 2yn' _space_group_IT_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 7.2837(5) _cell_length_b 13.933(2) _cell_length_c 17.804(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.690(10) _cell_angle_gamma 90.00 _cell_volume 1800.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19979 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 3.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8040 # Exptl Tmin _exptl_absorpt_correction_T_max 1.0000 # and Tmax _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18994 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3512 _reflns_number_gt 3072 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+28.7248P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3512 _refine_ls_number_parameters 218 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.5219(2) 0.67566(11) 0.17577(8) 0.0393(4) Uani 1 1 d . . . Sb1 Sb 0.61989(9) 0.68929(5) 0.03893(3) 0.0410(2) Uani 1 1 d D . . Sb2 Sb 0.45542(11) 0.85771(5) 0.18377(5) 0.0648(3) Uani 1 1 d D . . O1A O 0.303(3) 0.8338(13) 0.0319(9) 0.070(4) Uani 0.50 1 d PDU A 1 O1B O 0.4208(17) 0.8844(9) -0.0077(7) 0.046(3) Uani 0.50 1 d PDU B 2 O2 O 0.9119(11) 0.7206(7) 0.2407(4) 0.066(2) Uani 1 1 d . . . O3 O 0.5984(17) 0.4648(6) 0.1719(5) 0.092(3) Uani 1 1 d . . . O4 O 0.1313(11) 0.6369(6) 0.1099(5) 0.064(2) Uani 1 1 d . . . O5 O 0.4045(17) 0.6477(9) 0.3308(5) 0.104(4) Uani 1 1 d . . . C1 C 0.7429(15) 0.5624(8) -0.0032(6) 0.054(3) Uani 1 1 d . . . H1A H 0.6634 0.5070 0.0042 0.081 Uiso 1 1 calc R . . H1B H 0.8637 0.5519 0.0240 0.081 Uiso 1 1 calc R . . H1C H 0.7578 0.5702 -0.0571 0.081 Uiso 1 1 calc R . . C2 C 0.825(2) 0.7898(10) 0.0127(7) 0.071(3) Uani 1 1 d . . . H2A H 0.7902 0.8541 0.0288 0.107 Uiso 1 1 calc R . . H2B H 0.8364 0.7898 -0.0417 0.107 Uiso 1 1 calc R . . H2C H 0.9435 0.7719 0.0391 0.107 Uiso 1 1 calc R . . C3A C 0.4213(17) 0.7182(8) -0.0543(6) 0.065(3) Uani 0.50 1 d PDU A 1 H3A1 H 0.4846 0.7219 -0.1013 0.078 Uiso 0.50 1 calc PR A 1 H3A2 H 0.3311 0.6650 -0.0596 0.078 Uiso 0.50 1 calc PR A 1 C4A C 0.322(3) 0.8107(12) -0.0428(10) 0.050(4) Uani 0.50 1 d PDU A 1 H4A1 H 0.3892 0.8633 -0.0659 0.061 Uiso 0.50 1 calc PR A 1 H4A2 H 0.1978 0.8069 -0.0698 0.061 Uiso 0.50 1 calc PR A 1 C5A C 0.256(4) 0.9285(16) 0.0574(16) 0.066(7) Uani 0.50 1 d PDU A 1 H5A1 H 0.1514 0.9549 0.0249 0.080 Uiso 0.50 1 calc PR A 1 H5A2 H 0.3627 0.9722 0.0550 0.080 Uiso 0.50 1 calc PR A 1 C6A C 0.205(3) 0.920(3) 0.1379(16) 0.087(9) Uani 0.50 1 d PDU A 1 H6A1 H 0.0976 0.8773 0.1424 0.104 Uiso 0.50 1 calc PR A 1 H6A2 H 0.1810 0.9834 0.1605 0.104 Uiso 0.50 1 calc PR A 1 C3B C 0.4213(17) 0.7182(8) -0.0543(6) 0.065(3) Uani 0.50 1 d PDU B 2 H3B1 H 0.4473 0.6783 -0.0982 0.078 Uiso 0.50 1 calc PR B 2 H3B2 H 0.2957 0.7030 -0.0404 0.078 Uiso 0.50 1 calc PR B 2 C4B C 0.435(3) 0.8258(11) -0.0740(10) 0.060(5) Uani 0.50 1 d PDU B 2 H4B1 H 0.5549 0.8384 -0.0950 0.072 Uiso 0.50 1 calc PR B 2 H4B2 H 0.3358 0.8430 -0.1128 0.072 Uiso 0.50 1 calc PR B 2 C5B C 0.243(3) 0.893(3) 0.0195(11) 0.068(7) Uani 0.50 1 d PDU B 2 H5B1 H 0.1787 0.8305 0.0151 0.082 Uiso 0.50 1 calc PR B 2 H5B2 H 0.1690 0.9403 -0.0117 0.082 Uiso 0.50 1 calc PR B 2 C6B C 0.258(3) 0.9261(16) 0.1027(13) 0.064(8) Uani 0.50 1 d PDU B 2 H6B1 H 0.1346 0.9187 0.1215 0.077 Uiso 0.50 1 calc PR B 2 H6B2 H 0.2859 0.9957 0.1032 0.077 Uiso 0.50 1 calc PR B 2 C7 C 0.670(2) 0.9589(8) 0.1606(7) 0.076(4) Uani 1 1 d . A . H7A H 0.7136 0.9451 0.1111 0.114 Uiso 1 1 calc R . . H7B H 0.7733 0.9529 0.1994 0.114 Uiso 1 1 calc R . . H7C H 0.6212 1.0243 0.1610 0.114 Uiso 1 1 calc R . . C8 C 0.393(3) 0.9091(17) 0.2880(14) 0.154(11) Uani 1 1 d . A . H8A H 0.2953 0.8699 0.3069 0.231 Uiso 1 1 calc R . . H8B H 0.3520 0.9759 0.2829 0.231 Uiso 1 1 calc R . . H8C H 0.5034 0.9058 0.3234 0.231 Uiso 1 1 calc R . . C9 C 0.7664(15) 0.7033(8) 0.2143(5) 0.048(2) Uani 1 1 d . . . C10 C 0.5706(18) 0.5468(8) 0.1726(6) 0.059(3) Uani 1 1 d . . . C11 C 0.2782(15) 0.6534(7) 0.1346(6) 0.048(2) Uani 1 1 d . . . C12 C 0.4501(19) 0.6597(10) 0.2718(6) 0.069(3) 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 Cr1 0.0500(8) 0.0392(8) 0.0291(7) -0.0037(6) 0.0051(6) -0.0031(6) Sb1 0.0494(4) 0.0468(4) 0.0260(3) -0.0011(2) -0.0019(2) 0.0057(3) Sb2 0.0555(5) 0.0472(4) 0.0901(6) -0.0338(4) -0.0049(4) 0.0088(3) O1A 0.068(11) 0.071(10) 0.069(8) -0.008(8) -0.008(8) 0.014(9) O1B 0.045(6) 0.040(5) 0.050(7) 0.008(5) -0.012(5) -0.011(5) O2 0.056(5) 0.088(6) 0.051(4) -0.010(4) -0.008(4) 0.003(4) O3 0.151(10) 0.042(5) 0.072(6) 0.002(4) -0.050(6) 0.001(5) O4 0.052(4) 0.062(5) 0.078(5) -0.009(4) 0.011(4) -0.014(4) O5 0.131(9) 0.145(10) 0.040(5) -0.009(5) 0.035(5) -0.061(8) C1 0.060(6) 0.052(6) 0.052(6) -0.021(5) 0.009(5) 0.014(5) C2 0.089(9) 0.078(8) 0.046(6) 0.006(6) 0.005(6) -0.018(7) C3A 0.089(8) 0.057(5) 0.045(6) -0.003(4) -0.024(5) 0.013(6) C4A 0.042(10) 0.046(9) 0.061(8) 0.010(8) -0.005(9) -0.011(7) C5A 0.059(14) 0.056(12) 0.078(15) -0.012(11) -0.038(14) 0.001(10) C6A 0.055(16) 0.10(2) 0.105(17) -0.020(14) 0.009(15) 0.041(16) C3B 0.089(8) 0.057(5) 0.045(6) -0.003(4) -0.024(5) 0.013(6) C4B 0.064(13) 0.058(8) 0.054(11) -0.004(8) -0.023(9) -0.006(11) C5B 0.046(10) 0.10(2) 0.053(12) 0.034(12) -0.009(9) 0.006(13) C6B 0.044(14) 0.039(12) 0.108(17) -0.042(16) 0.000(13) 0.019(10) C7 0.105(10) 0.047(6) 0.068(8) -0.010(6) -0.037(7) -0.006(6) C8 0.121(15) 0.155(19) 0.19(2) -0.125(18) 0.065(15) -0.010(14) C9 0.059(6) 0.054(6) 0.029(4) -0.002(4) 0.000(4) 0.008(5) C10 0.087(8) 0.045(6) 0.041(5) 0.003(4) -0.023(5) 0.003(5) C11 0.058(6) 0.043(5) 0.044(5) -0.006(4) 0.015(5) -0.003(4) C12 0.084(8) 0.081(8) 0.040(6) -0.012(6) 0.006(5) -0.035(7) _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 Cr1 C10 1.833(11) . ? Cr1 C12 1.842(12) . ? Cr1 C11 1.890(11) . ? Cr1 C9 1.895(11) . ? Cr1 Sb2 2.5884(17) . ? Cr1 Sb1 2.6011(15) . ? Sb1 C2 2.128(13) . ? Sb1 C1 2.145(9) . ? Sb1 C3A 2.148(8) . ? Sb2 C8 2.072(18) . ? Sb2 C6A 2.125(17) . ? Sb2 C7 2.171(14) . ? Sb2 C6B 2.173(16) . ? O1A C4A 1.386(16) . ? O1A C5A 1.445(18) . ? O1B C5B 1.426(17) . ? O1B C4B 1.445(16) . ? O2 C9 1.149(13) . ? O3 C10 1.160(14) . ? O4 C11 1.146(13) . ? O5 C12 1.140(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3A C4A 1.501(15) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.516(19) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C5B C6B 1.546(18) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 C10 Cr1 C12 88.9(6) . . ? C10 Cr1 C11 90.3(5) . . ? C12 Cr1 C11 90.7(5) . . ? C10 Cr1 C9 91.8(5) . . ? C12 Cr1 C9 91.0(5) . . ? C11 Cr1 C9 177.3(5) . . ? C10 Cr1 Sb2 178.6(3) . . ? C12 Cr1 Sb2 89.9(5) . . ? C11 Cr1 Sb2 90.5(3) . . ? C9 Cr1 Sb2 87.4(3) . . ? C10 Cr1 Sb1 88.5(4) . . ? C12 Cr1 Sb1 177.2(4) . . ? C11 Cr1 Sb1 88.3(3) . . ? C9 Cr1 Sb1 90.2(3) . . ? Sb2 Cr1 Sb1 92.69(5) . . ? C2 Sb1 C1 98.3(5) . . ? C2 Sb1 C3A 98.5(5) . . ? C1 Sb1 C3A 99.1(4) . . ? C2 Sb1 Cr1 120.3(3) . . ? C1 Sb1 Cr1 114.9(3) . . ? C3A Sb1 Cr1 121.2(4) . . ? C8 Sb2 C6A 87.6(11) . . ? C8 Sb2 C7 99.2(7) . . ? C6A Sb2 C7 105.8(11) . . ? C8 Sb2 C6B 105.2(10) . . ? C6A Sb2 C6B 20.6(9) . . ? C7 Sb2 C6B 92.2(9) . . ? C8 Sb2 Cr1 116.3(8) . . ? C6A Sb2 Cr1 122.6(11) . . ? C7 Sb2 Cr1 119.0(4) . . ? C6B Sb2 Cr1 120.7(6) . . ? C4A O1A C5A 124(2) . . ? C5B O1B C4B 117.1(18) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4A C3A Sb1 111.0(9) . . ? C4A C3A H3A1 109.4 . . ? Sb1 C3A H3A1 109.4 . . ? C4A C3A H3A2 109.4 . . ? Sb1 C3A H3A2 109.4 . . ? H3A1 C3A H3A2 108.0 . . ? O1A C4A C3A 114.7(15) . . ? O1A C4A H4A1 108.6 . . ? C3A C4A H4A1 108.6 . . ? O1A C4A H4A2 108.6 . . ? C3A C4A H4A2 108.6 . . ? H4A1 C4A H4A2 107.6 . . ? O1A C5A C6A 108(2) . . ? O1A C5A H5A1 110.1 . . ? C6A C5A H5A1 110.1 . . ? O1A C5A H5A2 110.1 . . ? C6A C5A H5A2 110.1 . . ? H5A1 C5A H5A2 108.4 . . ? C5A C6A Sb2 97.1(14) . . ? C5A C6A H6A1 112.3 . . ? Sb2 C6A H6A1 112.3 . . ? C5A C6A H6A2 112.3 . . ? Sb2 C6A H6A2 112.3 . . ? H6A1 C6A H6A2 109.9 . . ? O1B C4B H4B1 109.5 . . ? O1B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 108.1 . . ? O1B C5B C6B 111(2) . . ? O1B C5B H5B1 109.5 . . ? C6B C5B H5B1 109.5 . . ? O1B C5B H5B2 109.5 . . ? C6B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 108.1 . . ? C5B C6B Sb2 119.8(13) . . ? C5B C6B H6B1 107.4 . . ? Sb2 C6B H6B1 107.4 . . ? C5B C6B H6B2 107.4 . . ? Sb2 C6B H6B2 107.4 . . ? H6B1 C6B H6B2 106.9 . . ? Sb2 C7 H7A 109.5 . . ? Sb2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Sb2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Sb2 C8 H8A 109.5 . . ? Sb2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Sb2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 Cr1 177.1(9) . . ? O3 C10 Cr1 178.3(13) . . ? O4 C11 Cr1 177.9(9) . . ? O5 C12 Cr1 178.4(12) . . ? 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 Sb1 C3A C4A O1A -30(2) . . . . ? C3A C4A O1A C5A 163(2) . . . . ? C4A O1A C5A C6A 167(2) . . . . ? O1A C5A C6A Sb2 58(2) . . . . ? Sb1 C3B C4B O1B -52.6(18) . . . . ? C3B C4B O1B C5B -74(2) . . . . ? C4B O1B C5B C6B 160.3(19) . . . . ? O1B C5B C6B Sb2 -46(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cr1 O1A 3.647(19) . . ? Cr1 O1B 4.390(13) . . ? Sb1 O1A 3.060(18) . . ? SB2 O1A 2.859(16) . . ? Sb1 O1B 3.159(13) . . ? Sb2 O1B 3.418(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.179 _refine_diff_density_min -2.372 _refine_diff_density_rms 0.187 #===END OF CIF ============================================================== # 10slb098x2.cif data_10slb098x _database_code_depnum_ccdc_archive 'CCDC 817773' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-01-05 _audit_author_name 'Benjamin, Sophie L.' _audit_update_record ; 2011-01-08 Changed labels on Sb1 & Sb2, reordered atoms list. ; _chemical_name_systematic ; fac-tricarbonyl(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine)manganese(I) trifluoromethanesulfonate ; # C19H27NSb2 = MeN{CH2(o-C6H4(SbMe2))}2 # N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]- # -N-methylmethanamine (iLab IUPAC (defaults)) # bis(N-(2-(dimethylstibanyl)benzyl))-methanamine (mw) # [F3CSO3]- = triflate anion # trifluoromethanesulphonate (from CSD search - very few hits(2?)) # trifluoromethanesulfonate (from CSD search - many hits with 'f' spelling) # trifluoromethanesulfonate (iLab defaults & selected options) # (sodium) trifluoromethanesulfonate (chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H27 Mn N O3 Sb2 1+, C F3 O3 S 1-' _chemical_formula_sum 'C23 H27 F3 Mn N O6 S Sb2' _chemical_formula_weight 800.96 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 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _space_group_name_Hall '-P 2yn' _space_group_IT_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 11.2440(15) _cell_length_b 14.737(2) _cell_length_c 17.721(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.168(10) _cell_angle_gamma 90.00 _cell_volume 2805.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6375 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rhombus _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 2.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8942 # Exptl Tmin _exptl_absorpt_correction_T_max 1.0000 # and Tmax _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27167 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5493 _reflns_number_gt 4205 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+40.5500P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5493 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.87656(10) 0.22256(8) 0.18208(6) 0.0226(3) Uani 1 1 d . . . Sb1 Sb 0.76067(5) 0.09134(4) 0.09622(3) 0.02859(16) Uani 1 1 d . . . Sb2 Sb 0.76508(5) 0.34899(4) 0.08846(3) 0.02740(15) Uani 1 1 d . . . O1 O 0.9995(6) 0.0836(5) 0.2997(4) 0.054(2) Uani 1 1 d . . . O2 O 1.0120(6) 0.3614(5) 0.2953(4) 0.0471(18) Uani 1 1 d . . . O3 O 0.6748(6) 0.2272(6) 0.2570(4) 0.060(2) Uani 1 1 d . . . N1 N 1.0262(5) 0.2180(4) 0.1225(3) 0.0195(13) Uani 1 1 d . . . C1 C 0.6407(10) 0.0131(8) 0.1424(8) 0.070(4) Uani 1 1 d . . . H1A H 0.5641 0.0473 0.1379 0.104 Uiso 1 1 calc R . . H1B H 0.6822 -0.0006 0.1981 0.104 Uiso 1 1 calc R . . H1C H 0.6201 -0.0437 0.1127 0.104 Uiso 1 1 calc R . . C2 C 0.6680(9) 0.0872(7) -0.0270(5) 0.048(3) Uani 1 1 d . . . H2A H 0.5944 0.1263 -0.0390 0.073 Uiso 1 1 calc R . . H2B H 0.6424 0.0247 -0.0427 0.073 Uiso 1 1 calc R . . H2C H 0.7245 0.1085 -0.0560 0.073 Uiso 1 1 calc R . . C3 C 0.9168(8) 0.0040(6) 0.1128(6) 0.037(2) Uani 1 1 d . . . C4 C 0.9223(9) -0.0821(6) 0.1464(7) 0.059(3) Uani 1 1 d . . . H4 H 0.8484 -0.1100 0.1508 0.070 Uiso 1 1 calc R . . C5 C 1.0370(10) -0.1281(7) 0.1737(8) 0.063(4) Uani 1 1 d . . . H5 H 1.0407 -0.1865 0.1969 0.075 Uiso 1 1 calc R . . C6 C 1.1418(9) -0.0885(6) 0.1668(6) 0.048(3) Uani 1 1 d . . . H6 H 1.2190 -0.1197 0.1849 0.058 Uiso 1 1 calc R . . C7 C 1.1380(8) -0.0023(6) 0.1335(5) 0.034(2) Uani 1 1 d . . . H7 H 1.2123 0.0245 0.1287 0.041 Uiso 1 1 calc R . . C8 C 1.0260(7) 0.0445(5) 0.1073(5) 0.0280(18) Uani 1 1 d . . . C9 C 1.0237(8) 0.1367(5) 0.0690(5) 0.0269(18) Uani 1 1 d . . . H9A H 0.9477 0.1406 0.0234 0.032 Uiso 1 1 calc R . . H9B H 1.0962 0.1409 0.0483 0.032 Uiso 1 1 calc R . . C10 C 1.1507(6) 0.2176(6) 0.1839(4) 0.0238(16) Uani 1 1 d . . . H10A H 1.1557 0.2687 0.2202 0.036 Uiso 1 1 calc R . . H10B H 1.2165 0.2234 0.1582 0.036 Uiso 1 1 calc R . . H10C H 1.1614 0.1606 0.2136 0.036 Uiso 1 1 calc R . . C11 C 1.0295(7) 0.2973(5) 0.0674(5) 0.0246(17) Uani 1 1 d . . . H11A H 1.1039 0.2899 0.0489 0.029 Uiso 1 1 calc R . . H11B H 0.9555 0.2925 0.0205 0.029 Uiso 1 1 calc R . . C12 C 1.0322(7) 0.3915(5) 0.1009(5) 0.0252(17) Uani 1 1 d . . . C13 C 1.1448(8) 0.4388(6) 0.1261(5) 0.035(2) Uani 1 1 d . . . H13 H 1.2196 0.4105 0.1239 0.042 Uiso 1 1 calc R . . C14 C 1.1480(9) 0.5270(6) 0.1543(6) 0.044(2) Uani 1 1 d . . . H14 H 1.2255 0.5576 0.1730 0.053 Uiso 1 1 calc R . . C15 C 1.0407(9) 0.5704(7) 0.1555(7) 0.055(3) Uani 1 1 d . . . H15 H 1.0431 0.6314 0.1731 0.067 Uiso 1 1 calc R . . C16 C 0.9275(9) 0.5235(6) 0.1305(7) 0.049(3) Uani 1 1 d . . . H16 H 0.8529 0.5526 0.1320 0.059 Uiso 1 1 calc R . . C17 C 0.9236(8) 0.4356(6) 0.1038(5) 0.0314(19) Uani 1 1 d . . . C18 C 0.6387(9) 0.4340(7) 0.1236(7) 0.055(3) Uani 1 1 d . . . H18A H 0.5615 0.4007 0.1191 0.082 Uiso 1 1 calc R . . H18B H 0.6203 0.4877 0.0895 0.082 Uiso 1 1 calc R . . H18C H 0.6760 0.4529 0.1786 0.082 Uiso 1 1 calc R . . C19 C 0.6878(8) 0.3417(7) -0.0363(5) 0.044(2) Uani 1 1 d . . . H19A H 0.7406 0.3034 -0.0583 0.066 Uiso 1 1 calc R . . H19B H 0.6831 0.4028 -0.0588 0.066 Uiso 1 1 calc R . . H19C H 0.6040 0.3156 -0.0492 0.066 Uiso 1 1 calc R . . C20 C 0.9527(8) 0.1371(6) 0.2520(5) 0.036(2) Uani 1 1 d . . . C21 C 0.9602(8) 0.3093(7) 0.2500(5) 0.036(2) Uani 1 1 d . . . C22 C 0.7515(8) 0.2258(7) 0.2266(5) 0.042(2) Uani 1 1 d . . . S1 S 0.40830(17) 0.22851(15) 0.06065(12) 0.0282(4) Uani 1 1 d . . . O4 O 0.3505(6) 0.1427(5) 0.0605(5) 0.0518(19) Uani 1 1 d . . . O5 O 0.5394(5) 0.2251(4) 0.0662(3) 0.0325(13) Uani 1 1 d . . . O6 O 0.3760(6) 0.2963(5) 0.1084(4) 0.054(2) Uani 1 1 d . . . F1 F 0.3680(5) 0.2162(6) -0.0909(3) 0.071(2) Uani 1 1 d . . . F2 F 0.2140(4) 0.2731(4) -0.0572(3) 0.0469(14) Uani 1 1 d . . . F3 F 0.3784(6) 0.3529(5) -0.0484(5) 0.083(3) Uani 1 1 d . . . C23 C 0.3390(8) 0.2695(7) -0.0395(5) 0.038(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 Mn1 0.0180(5) 0.0322(6) 0.0188(5) -0.0024(5) 0.0072(4) -0.0058(5) Sb1 0.0201(3) 0.0233(3) 0.0359(3) 0.0028(2) -0.0017(2) -0.0055(2) Sb2 0.0178(3) 0.0239(3) 0.0399(3) -0.0020(2) 0.0077(2) 0.0001(2) O1 0.041(4) 0.066(5) 0.042(4) 0.024(4) -0.006(3) -0.020(4) O2 0.027(3) 0.070(5) 0.045(4) -0.033(4) 0.012(3) -0.013(3) O3 0.029(3) 0.121(7) 0.036(4) -0.009(4) 0.021(3) -0.017(4) N1 0.019(3) 0.020(3) 0.020(3) 0.005(3) 0.006(2) 0.002(3) C1 0.043(6) 0.055(7) 0.095(9) 0.049(7) -0.004(6) -0.018(5) C2 0.039(5) 0.048(6) 0.040(5) -0.028(5) -0.017(4) 0.019(5) C3 0.023(4) 0.020(4) 0.054(6) 0.000(4) -0.010(4) -0.001(3) C4 0.032(5) 0.027(5) 0.099(9) 0.015(5) -0.008(6) -0.007(4) C5 0.041(6) 0.027(5) 0.104(10) 0.016(6) -0.004(6) -0.001(4) C6 0.034(5) 0.032(5) 0.059(6) -0.005(5) -0.015(5) 0.006(4) C7 0.038(5) 0.026(4) 0.034(5) -0.006(4) 0.003(4) -0.001(4) C8 0.025(4) 0.022(4) 0.028(4) -0.001(3) -0.006(3) 0.005(3) C9 0.028(4) 0.029(4) 0.022(4) -0.007(3) 0.004(3) 0.003(3) C10 0.014(3) 0.028(4) 0.028(4) -0.002(3) 0.005(3) 0.001(3) C11 0.016(4) 0.029(4) 0.026(4) 0.007(3) 0.001(3) -0.002(3) C12 0.019(4) 0.025(4) 0.031(4) 0.003(3) 0.007(3) -0.006(3) C13 0.025(4) 0.036(5) 0.041(5) 0.004(4) 0.005(4) -0.006(4) C14 0.032(5) 0.029(5) 0.068(7) 0.009(5) 0.007(5) -0.014(4) C15 0.038(6) 0.028(5) 0.092(9) -0.005(5) 0.006(6) 0.002(4) C16 0.034(5) 0.026(5) 0.084(8) 0.001(5) 0.012(5) 0.003(4) C17 0.024(4) 0.029(5) 0.041(5) 0.007(4) 0.009(4) -0.001(3) C18 0.025(5) 0.041(6) 0.097(9) -0.018(6) 0.016(5) 0.002(4) C19 0.026(5) 0.057(6) 0.042(5) 0.019(5) -0.002(4) 0.001(4) C20 0.024(4) 0.049(6) 0.030(5) 0.008(4) 0.003(4) -0.016(4) C21 0.022(4) 0.059(6) 0.032(5) -0.011(4) 0.015(4) -0.004(4) C22 0.026(4) 0.074(7) 0.022(4) -0.009(5) 0.002(4) -0.016(5) S1 0.0191(9) 0.0384(12) 0.0287(10) -0.0011(9) 0.0097(8) -0.0011(9) O4 0.029(3) 0.044(4) 0.085(5) 0.022(4) 0.019(4) -0.003(3) O5 0.017(3) 0.043(3) 0.038(3) -0.002(3) 0.010(2) 0.001(3) O6 0.029(3) 0.077(5) 0.058(4) -0.035(4) 0.018(3) -0.005(3) F1 0.042(3) 0.138(6) 0.033(3) -0.008(4) 0.012(3) 0.033(4) F2 0.024(3) 0.070(4) 0.045(3) 0.016(3) 0.008(2) 0.013(3) F3 0.047(4) 0.073(5) 0.138(7) 0.070(5) 0.040(4) 0.014(3) C23 0.026(4) 0.051(6) 0.038(5) 0.011(4) 0.010(4) 0.003(4) _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 Mn1 C20 1.797(9) . ? Mn1 C22 1.806(9) . ? Mn1 C21 1.817(9) . ? Mn1 N1 2.236(6) . ? Mn1 Sb2 2.5628(14) . ? Mn1 Sb1 2.5656(13) . ? Sb1 C1 2.115(10) . ? Sb1 C2 2.124(9) . ? Sb1 C3 2.126(8) . ? Sb2 C18 2.121(9) . ? Sb2 C19 2.126(9) . ? Sb2 C17 2.144(8) . ? O1 C20 1.162(10) . ? O2 C21 1.139(10) . ? O3 C22 1.144(10) . ? N1 C10 1.498(9) . ? N1 C9 1.524(9) . ? N1 C11 1.530(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C8 1.395(12) . ? C3 C4 1.395(12) . ? C4 C5 1.410(14) . ? C4 H4 0.9500 . ? C5 C6 1.352(15) . ? C5 H5 0.9500 . ? C6 C7 1.396(13) . ? C6 H6 0.9500 . ? C7 C8 1.391(11) . ? C7 H7 0.9500 . ? C8 C9 1.515(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.507(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.397(11) . ? C12 C17 1.397(11) . ? C13 C14 1.389(13) . ? C13 H13 0.9500 . ? C14 C15 1.371(14) . ? C14 H14 0.9500 . ? C15 C16 1.400(13) . ? C15 H15 0.9500 . ? C16 C17 1.375(13) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? S1 O4 1.421(7) . ? S1 O6 1.423(7) . ? S1 O5 1.449(5) . ? S1 C23 1.818(9) . ? F1 C23 1.315(11) . ? F2 C23 1.347(10) . ? F3 C23 1.332(11) . ? 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 C20 Mn1 C22 89.5(4) . . ? C20 Mn1 C21 89.3(4) . . ? C22 Mn1 C21 90.5(4) . . ? C20 Mn1 N1 91.9(3) . . ? C22 Mn1 N1 177.9(3) . . ? C21 Mn1 N1 91.1(3) . . ? C20 Mn1 Sb2 176.9(3) . . ? C22 Mn1 Sb2 88.2(3) . . ? C21 Mn1 Sb2 88.6(3) . . ? N1 Mn1 Sb2 90.50(15) . . ? C20 Mn1 Sb1 86.3(3) . . ? C22 Mn1 Sb1 87.4(3) . . ? C21 Mn1 Sb1 175.2(3) . . ? N1 Mn1 Sb1 91.08(16) . . ? Sb2 Mn1 Sb1 95.64(4) . . ? C1 Sb1 C2 101.9(5) . . ? C1 Sb1 C3 102.2(4) . . ? C2 Sb1 C3 105.0(4) . . ? C1 Sb1 Mn1 116.9(4) . . ? C2 Sb1 Mn1 129.8(3) . . ? C3 Sb1 Mn1 96.9(2) . . ? C18 Sb2 C19 103.4(4) . . ? C18 Sb2 C17 102.4(4) . . ? C19 Sb2 C17 103.4(3) . . ? C18 Sb2 Mn1 118.8(3) . . ? C19 Sb2 Mn1 127.5(3) . . ? C17 Sb2 Mn1 97.0(2) . . ? C10 N1 C9 106.9(6) . . ? C10 N1 C11 105.9(6) . . ? C9 N1 C11 101.7(5) . . ? C10 N1 Mn1 109.2(4) . . ? C9 N1 Mn1 116.0(5) . . ? C11 N1 Mn1 116.2(4) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C3 C4 119.4(8) . . ? C8 C3 Sb1 116.0(6) . . ? C4 C3 Sb1 122.7(8) . . ? C3 C4 C5 120.3(10) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.7(9) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.8(9) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 120.3(9) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C3 119.6(8) . . ? C7 C8 C9 119.2(8) . . ? C3 C8 C9 121.1(7) . . ? C8 C9 N1 115.6(6) . . ? C8 C9 H9A 108.4 . . ? N1 C9 H9A 108.4 . . ? C8 C9 H9B 108.4 . . ? N1 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 117.0(6) . . ? C12 C11 H11A 108.1 . . ? N1 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? N1 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C13 C12 C17 118.4(8) . . ? C13 C12 C11 119.8(7) . . ? C17 C12 C11 121.8(7) . . ? C14 C13 C12 120.4(9) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.8(9) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.1(9) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 120.5(9) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 120.7(8) . . ? C16 C17 Sb2 123.0(7) . . ? C12 C17 Sb2 114.9(6) . . ? Sb2 C18 H18A 109.5 . . ? Sb2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Sb2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C20 Mn1 176.8(9) . . ? O2 C21 Mn1 176.9(9) . . ? O3 C22 Mn1 177.9(8) . . ? O4 S1 O6 115.4(4) . . ? O4 S1 O5 115.1(4) . . ? O6 S1 O5 114.6(4) . . ? O4 S1 C23 103.3(4) . . ? O6 S1 C23 103.6(5) . . ? O5 S1 C23 102.3(4) . . ? F1 C23 F3 108.0(8) . . ? F1 C23 F2 108.4(8) . . ? F3 C23 F2 107.3(8) . . ? F1 C23 S1 110.8(6) . . ? F3 C23 S1 111.2(7) . . ? F2 C23 S1 111.0(6) . . ? 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 C8 C9 N1 C11 177.3(6) . . . . ? C9 N1 C11 C12 179.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.186 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.171 #===END OF CIF ============================================================== # 10mr328a.cif data_10mr328 _database_code_depnum_ccdc_archive 'CCDC 817774' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-01-14 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetracarbonyl-(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine)-tungsten(0) ; # MeN{CH2(o-C6H4(SbMe2))}2 = C19H27NSb2 # N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]- # N-methylmethanamine (iLab IUPAC (defaults)) # bis(N-(2-(dimethylstibanyl)benzyl))-methanamine (mw) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H27 N O4 Sb2 W' _chemical_formula_sum 'C23 H27 N O4 Sb2 W' _chemical_formula_structural '(C19 H27 N Sb2) (C O)4 W' _chemical_formula_weight 808.81 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 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' 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 8.9364(15) _cell_length_b 18.427(3) _cell_length_c 16.230(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.494(7) _cell_angle_gamma 90.00 _cell_volume 2627.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5305 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rhomb _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 6.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7791 # 0.5809 # Exptl Tmin & Tmax _exptl_absorpt_correction_T_max 1.0000 # 0.7456 # scaled to Tmax=1. _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17567 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5975 _reflns_number_gt 5576 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.3614P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5975 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 W1 W 0.351274(13) 0.213255(6) 0.254141(7) 0.01407(5) Uani 1 1 d . . . Sb1 Sb 0.33046(2) 0.111998(11) 0.128918(12) 0.01710(6) Uani 1 1 d . . . Sb2 Sb 0.32378(2) 0.330893(11) 0.145725(13) 0.01703(6) Uani 1 1 d . . . O1 O -0.0101(3) 0.21334(13) 0.21623(18) 0.0384(7) Uani 1 1 d . . . O2 O 0.3718(3) 0.32495(13) 0.40189(16) 0.0361(6) Uani 1 1 d . . . O3 O 0.3580(3) 0.08891(12) 0.38616(15) 0.0317(6) Uani 1 1 d . . . O4 O 0.7106(2) 0.19386(12) 0.28882(15) 0.0279(5) Uani 1 1 d . . . N1 N 0.5472(3) 0.28050(12) 0.04085(16) 0.0163(6) Uani 1 1 d . . . C1 C 0.5013(4) 0.02993(17) 0.1482(2) 0.0330(8) Uani 1 1 d . . . H1A H 0.4819 -0.0052 0.1022 0.049 Uiso 1 1 calc R . . H1B H 0.4991 0.0050 0.2014 0.049 Uiso 1 1 calc R . . H1C H 0.6014 0.0522 0.1501 0.049 Uiso 1 1 calc R . . C2 C 0.1325(4) 0.04515(19) 0.1174(2) 0.0354(9) Uani 1 1 d . . . H2A H 0.0436 0.0725 0.0893 0.053 Uiso 1 1 calc R . . H2B H 0.1170 0.0304 0.1732 0.053 Uiso 1 1 calc R . . H2C H 0.1461 0.0020 0.0843 0.053 Uiso 1 1 calc R . . C3 C 0.3308(3) 0.13009(16) -0.00133(18) 0.0183(6) Uani 1 1 d . . . C4 C 0.2132(3) 0.10194(16) -0.0604(2) 0.0232(7) Uani 1 1 d . . . H4 H 0.1293 0.0794 -0.0421 0.028 Uiso 1 1 calc R . . C5 C 0.2156(4) 0.10599(17) -0.1451(2) 0.0267(8) Uani 1 1 d . . . H5 H 0.1328 0.0874 -0.1846 0.032 Uiso 1 1 calc R . . C6 C 0.3383(4) 0.13708(17) -0.1722(2) 0.0260(7) Uani 1 1 d . . . H6 H 0.3418 0.1389 -0.2303 0.031 Uiso 1 1 calc R . . C7 C 0.4566(3) 0.16562(16) -0.1141(2) 0.0224(7) Uani 1 1 d . . . H7 H 0.5414 0.1866 -0.1330 0.027 Uiso 1 1 calc R . . C8 C 0.4539(3) 0.16414(15) -0.02851(19) 0.0170(6) Uani 1 1 d . . . C9 C 0.5801(3) 0.20224(16) 0.03052(19) 0.0179(6) Uani 1 1 d . . . H9A H 0.5947 0.1782 0.0860 0.021 Uiso 1 1 calc R . . H9B H 0.6761 0.1975 0.0087 0.021 Uiso 1 1 calc R . . C10 C 0.5306(4) 0.31973(17) -0.03943(19) 0.0242(7) Uani 1 1 d . . . H10A H 0.5147 0.3715 -0.0300 0.036 Uiso 1 1 calc R . . H10B H 0.4430 0.3004 -0.0785 0.036 Uiso 1 1 calc R . . H10C H 0.6230 0.3134 -0.0632 0.036 Uiso 1 1 calc R . . C11 C 0.6723(3) 0.31274(16) 0.10022(19) 0.0181(6) Uani 1 1 d . . . H11A H 0.7665 0.3109 0.0763 0.022 Uiso 1 1 calc R . . H11B H 0.6897 0.2840 0.1526 0.022 Uiso 1 1 calc R . . C12 C 0.6394(3) 0.39031(16) 0.12008(19) 0.0193(7) Uani 1 1 d . . . C13 C 0.7480(3) 0.44374(18) 0.1193(2) 0.0249(7) Uani 1 1 d . . . H13 H 0.8412 0.4315 0.1024 0.030 Uiso 1 1 calc R . . C14 C 0.7242(4) 0.51407(18) 0.1423(2) 0.0323(8) Uani 1 1 d . . . H14 H 0.8019 0.5494 0.1428 0.039 Uiso 1 1 calc R . . C15 C 0.5891(4) 0.53330(17) 0.1644(2) 0.0296(8) Uani 1 1 d . . . H15 H 0.5731 0.5816 0.1811 0.036 Uiso 1 1 calc R . . C16 C 0.4750(4) 0.48128(16) 0.16205(19) 0.0246(7) Uani 1 1 d . . . H16 H 0.3798 0.4949 0.1755 0.029 Uiso 1 1 calc R . . C17 C 0.4985(3) 0.40991(16) 0.14032(18) 0.0175(6) Uani 1 1 d . . . C18 C 0.1885(3) 0.32559(19) 0.0234(2) 0.0294(8) Uani 1 1 d . . . H18A H 0.0816 0.3184 0.0279 0.044 Uiso 1 1 calc R . . H18B H 0.2228 0.2850 -0.0074 0.044 Uiso 1 1 calc R . . H18C H 0.1988 0.3710 -0.0065 0.044 Uiso 1 1 calc R . . C19 C 0.1701(4) 0.40197(18) 0.1946(2) 0.0320(8) Uani 1 1 d . . . H19A H 0.1469 0.4440 0.1575 0.048 Uiso 1 1 calc R . . H19B H 0.2176 0.4184 0.2507 0.048 Uiso 1 1 calc R . . H19C H 0.0758 0.3758 0.1978 0.048 Uiso 1 1 calc R . . C20 C 0.1197(4) 0.21423(16) 0.2311(2) 0.0216(7) Uani 1 1 d . . . C21 C 0.3650(3) 0.28423(16) 0.3467(2) 0.0213(7) Uani 1 1 d . . . C22 C 0.3535(3) 0.13393(17) 0.3363(2) 0.0204(7) Uani 1 1 d . . . C23 C 0.5815(4) 0.20354(16) 0.27402(19) 0.0188(7) 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 W1 0.01440(7) 0.01530(8) 0.01303(8) 0.00045(4) 0.00383(5) -0.00088(4) Sb1 0.02050(11) 0.01579(12) 0.01508(11) -0.00069(8) 0.00342(8) -0.00162(8) Sb2 0.01628(10) 0.01610(12) 0.01864(12) 0.00363(8) 0.00294(8) 0.00203(8) O1 0.0186(13) 0.0522(18) 0.0451(18) -0.0052(12) 0.0080(11) -0.0013(11) O2 0.0337(13) 0.0416(15) 0.0360(16) -0.0222(13) 0.0140(11) -0.0091(12) O3 0.0386(13) 0.0268(13) 0.0298(14) 0.0102(11) 0.0066(11) -0.0058(11) O4 0.0167(11) 0.0338(13) 0.0326(14) 0.0074(11) 0.0028(10) 0.0008(10) N1 0.0181(13) 0.0166(14) 0.0130(14) 0.0031(10) -0.0002(10) -0.0015(10) C1 0.049(2) 0.0219(18) 0.028(2) 0.0013(15) 0.0075(16) 0.0115(17) C2 0.042(2) 0.035(2) 0.030(2) -0.0028(16) 0.0090(16) -0.0227(17) C3 0.0242(15) 0.0171(16) 0.0132(16) -0.0029(12) 0.0025(12) 0.0064(13) C4 0.0242(16) 0.0215(17) 0.0220(18) -0.0005(14) -0.0006(13) 0.0029(13) C5 0.0362(18) 0.0228(18) 0.0163(17) -0.0047(14) -0.0080(14) 0.0044(15) C6 0.0397(19) 0.0225(18) 0.0155(17) -0.0005(14) 0.0046(14) 0.0091(15) C7 0.0274(16) 0.0203(17) 0.0201(18) -0.0002(13) 0.0057(13) 0.0050(14) C8 0.0193(14) 0.0137(15) 0.0177(17) 0.0002(12) 0.0025(12) 0.0070(12) C9 0.0182(15) 0.0213(16) 0.0157(16) 0.0024(13) 0.0075(12) 0.0030(13) C10 0.0315(17) 0.0240(18) 0.0171(17) 0.0078(14) 0.0045(13) -0.0003(14) C11 0.0140(14) 0.0242(17) 0.0158(16) 0.0031(13) 0.0022(11) -0.0035(13) C12 0.0207(15) 0.0205(16) 0.0141(16) 0.0071(12) -0.0037(12) -0.0037(13) C13 0.0224(16) 0.0299(19) 0.0201(18) 0.0074(14) -0.0027(13) -0.0067(14) C14 0.040(2) 0.0239(19) 0.028(2) 0.0080(15) -0.0063(15) -0.0132(16) C15 0.046(2) 0.0157(17) 0.0238(19) 0.0041(14) -0.0031(15) -0.0017(16) C16 0.0364(18) 0.0175(17) 0.0183(17) 0.0056(13) 0.0010(14) 0.0002(14) C17 0.0229(15) 0.0169(16) 0.0111(15) 0.0047(12) -0.0009(12) -0.0012(13) C18 0.0258(17) 0.035(2) 0.0240(19) 0.0061(15) -0.0039(14) 0.0011(15) C19 0.0304(18) 0.0257(19) 0.043(2) 0.0036(16) 0.0147(16) 0.0116(15) C20 0.0214(17) 0.0209(19) 0.0232(19) -0.0007(13) 0.0057(13) -0.0032(13) C21 0.0174(16) 0.0233(19) 0.025(2) 0.0013(14) 0.0096(13) -0.0052(12) C22 0.0187(15) 0.0186(16) 0.0238(18) -0.0025(14) 0.0034(13) -0.0025(13) C23 0.0269(18) 0.0144(15) 0.0154(17) 0.0014(12) 0.0051(13) -0.0040(13) _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 W1 C22 1.976(3) . ? W1 C21 1.978(3) . ? W1 C23 2.032(3) . ? W1 C20 2.035(3) . ? W1 Sb1 2.7402(4) . ? W1 Sb2 2.7745(4) . ? Sb1 C1 2.131(3) . ? Sb1 C2 2.136(3) . ? Sb1 C3 2.141(3) . ? Sb2 C18 2.130(3) . ? Sb2 C17 2.149(3) . ? Sb2 C19 2.151(3) . ? O1 C20 1.141(4) . ? O2 C21 1.162(4) . ? O3 C22 1.155(4) . ? O4 C23 1.148(3) . ? N1 C11 1.463(3) . ? N1 C10 1.474(4) . ? N1 C9 1.487(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.388(4) . ? C3 C8 1.405(4) . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.386(4) . ? C6 H6 0.9500 . ? C7 C8 1.394(4) . ? C7 H7 0.9500 . ? C8 C9 1.513(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.506(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.384(4) . ? C12 C17 1.405(4) . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C15 1.367(5) . ? C14 H14 0.9500 . ? C15 C16 1.395(4) . ? C15 H15 0.9500 . ? C16 C17 1.387(4) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C22 W1 C21 89.15(13) . . ? C22 W1 C23 86.68(12) . . ? C21 W1 C23 90.95(12) . . ? C22 W1 C20 90.88(12) . . ? C21 W1 C20 93.09(12) . . ? C23 W1 C20 175.25(12) . . ? C22 W1 Sb1 89.30(9) . . ? C21 W1 Sb1 178.41(9) . . ? C23 W1 Sb1 89.30(9) . . ? C20 W1 Sb1 86.59(9) . . ? C22 W1 Sb2 174.07(9) . . ? C21 W1 Sb2 87.20(9) . . ? C23 W1 Sb2 98.03(8) . . ? C20 W1 Sb2 84.67(9) . . ? Sb1 W1 Sb2 94.325(14) . . ? C1 Sb1 C2 99.41(14) . . ? C1 Sb1 C3 97.23(12) . . ? C2 Sb1 C3 98.83(13) . . ? C1 Sb1 W1 115.09(10) . . ? C2 Sb1 W1 113.64(10) . . ? C3 Sb1 W1 127.90(8) . . ? C18 Sb2 C17 106.65(12) . . ? C18 Sb2 C19 94.55(14) . . ? C17 Sb2 C19 96.89(12) . . ? C18 Sb2 W1 121.66(9) . . ? C17 Sb2 W1 125.05(7) . . ? C19 Sb2 W1 103.33(10) . . ? C11 N1 C10 109.0(2) . . ? C11 N1 C9 109.0(2) . . ? C10 N1 C9 111.5(2) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 119.2(3) . . ? C4 C3 Sb1 119.1(2) . . ? C8 C3 Sb1 121.4(2) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 121.4(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 118.6(3) . . ? C7 C8 C9 118.4(3) . . ? C3 C8 C9 123.0(3) . . ? N1 C9 C8 112.4(2) . . ? N1 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 111.8(2) . . ? N1 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C11 120.6(3) . . ? C17 C12 C11 120.8(3) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C12 119.1(3) . . ? C16 C17 Sb2 119.2(2) . . ? C12 C17 Sb2 121.6(2) . . ? Sb2 C18 H18A 109.5 . . ? Sb2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Sb2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C20 W1 177.9(3) . . ? O2 C21 W1 178.7(3) . . ? O3 C22 W1 177.8(3) . . ? O4 C23 W1 175.1(3) . . ? 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 C8 C9 N1 C11 178.6(2) . . . . ? C9 N1 C11 C12 -174.5(2) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Sb1 N1 4.055(2) . . ? Sb2 N1 2.997(3) . . ? Sb1 Sb2 4.0439(6) . . ? W1 N1 4.335(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.669 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.120 #===END OF CIF ============================================================== # 11slbcrsb2nxa.cif data_11slbcrsb2nx _database_code_depnum_ccdc_archive 'CCDC 817775' #TrackingRef '- all7a.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-02-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetracarbonyl-(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine)-chromium(0) ; # MeN{CH2(o-C6H4(SbMe2))}2 = C19H27NSb2 # N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]- # N-methylmethanamine (iLab IUPAC (defaults)) # bis(N-(2-(dimethylstibanyl)benzyl))-methanamine (mw) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H27 Cr N O4 Sb2' _chemical_formula_sum 'C23 H27 Cr N O4 Sb2' _chemical_formula_structural '(C19 H27 N Sb2) Cr (C O)4' _chemical_formula_weight 676.96 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 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_name_Hall '-P 2yn ' _space_group_IT_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 9.6141(15) _cell_length_b 26.060(4) _cell_length_c 10.2948(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.699(10) _cell_angle_gamma 90.00 _cell_volume 2556.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17643 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7803 # Exptl Tmin _exptl_absorpt_correction_T_max 1.0000 # and Tmax _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20852 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5710 _reflns_number_gt 4740 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+27.9000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5710 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.50201(12) 0.15977(4) 0.59201(11) 0.0259(2) Uani 1 1 d . . . Sb1 Sb 0.24407(5) 0.144382(17) 0.63016(5) 0.02751(13) Uani 1 1 d . . . Sb2 Sb 0.60771(5) 0.095789(17) 0.77126(4) 0.02493(12) Uani 1 1 d . . . O1 O 0.5387(6) 0.2432(2) 0.8019(5) 0.0428(13) Uani 1 1 d . . . O2 O 0.7937(6) 0.1787(2) 0.5306(6) 0.0483(14) Uani 1 1 d . . . O3 O 0.4014(7) 0.2347(2) 0.3771(6) 0.0506(15) Uani 1 1 d . . . O4 O 0.4615(9) 0.0694(2) 0.4070(6) 0.069(2) Uani 1 1 d . . . N1 N 0.3466(6) 0.1443(2) 0.9661(6) 0.0273(12) Uani 1 1 d . . . C1 C 0.1135(8) 0.1295(3) 0.4495(8) 0.045(2) Uani 1 1 d . . . H1A H 0.1524 0.1008 0.4045 0.068 Uiso 1 1 calc R . . H1B H 0.1093 0.1602 0.3940 0.068 Uiso 1 1 calc R . . H1C H 0.0187 0.1207 0.4673 0.068 Uiso 1 1 calc R . . C2 C 0.1229(8) 0.2063(3) 0.6881(9) 0.045(2) Uani 1 1 d . . . H2A H 0.1459 0.2376 0.6430 0.067 Uiso 1 1 calc R . . H2B H 0.1440 0.2113 0.7831 0.067 Uiso 1 1 calc R . . H2C H 0.0229 0.1985 0.6651 0.067 Uiso 1 1 calc R . . C3 C 0.1864(7) 0.0778(3) 0.7349(7) 0.0296(15) Uani 1 1 d . . . C4 C 0.1664(8) 0.0325(3) 0.6629(8) 0.0364(17) Uani 1 1 d . . . H4 H 0.1700 0.0336 0.5712 0.044 Uiso 1 1 calc R . . C5 C 0.1418(8) -0.0136(3) 0.7198(9) 0.044(2) Uani 1 1 d . . . H5 H 0.1288 -0.0438 0.6682 0.053 Uiso 1 1 calc R . . C6 C 0.1361(8) -0.0155(3) 0.8528(10) 0.046(2) Uani 1 1 d . . . H6 H 0.1189 -0.0471 0.8934 0.055 Uiso 1 1 calc R . . C7 C 0.1556(7) 0.0292(3) 0.9276(9) 0.0401(19) Uani 1 1 d . . . H7 H 0.1508 0.0275 1.0191 0.048 Uiso 1 1 calc R . . C8 C 0.1823(7) 0.0765(3) 0.8705(8) 0.0309(16) Uani 1 1 d . . . C9 C 0.2040(7) 0.1235(3) 0.9561(7) 0.0308(15) Uani 1 1 d . . . H9A H 0.1366 0.1503 0.9202 0.037 Uiso 1 1 calc R . . H9B H 0.1831 0.1148 1.0450 0.037 Uiso 1 1 calc R . . C10 C 0.3479(9) 0.1955(3) 1.0285(9) 0.045(2) Uani 1 1 d . . . H10A H 0.4427 0.2100 1.0359 0.067 Uiso 1 1 calc R . . H10B H 0.3195 0.1922 1.1161 0.067 Uiso 1 1 calc R . . H10C H 0.2823 0.2183 0.9749 0.067 Uiso 1 1 calc R . . C11 C 0.4443(7) 0.1105(3) 1.0486(7) 0.0286(15) Uani 1 1 d . . . H11A H 0.4385 0.0756 1.0100 0.034 Uiso 1 1 calc R . . H11B H 0.4139 0.1082 1.1365 0.034 Uiso 1 1 calc R . . C12 C 0.5952(7) 0.1280(2) 1.0638(7) 0.0246(14) Uani 1 1 d . . . C13 C 0.6567(8) 0.1472(3) 1.1849(7) 0.0323(16) Uani 1 1 d . . . H13 H 0.6034 0.1477 1.2562 0.039 Uiso 1 1 calc R . . C14 C 0.7931(8) 0.1655(3) 1.2037(7) 0.0327(16) Uani 1 1 d . . . H14 H 0.8323 0.1786 1.2868 0.039 Uiso 1 1 calc R . . C15 C 0.8709(8) 0.1646(3) 1.1022(7) 0.0340(16) Uani 1 1 d . . . H15 H 0.9641 0.1776 1.1140 0.041 Uiso 1 1 calc R . . C16 C 0.8143(7) 0.1449(3) 0.9821(7) 0.0296(15) Uani 1 1 d . . . H16 H 0.8692 0.1444 0.9120 0.036 Uiso 1 1 calc R . . C17 C 0.6783(7) 0.1258(2) 0.9623(6) 0.0244(14) Uani 1 1 d . . . C18 C 0.5271(8) 0.0227(3) 0.8170(8) 0.0369(17) Uani 1 1 d . . . H18A H 0.4907 0.0048 0.7357 0.055 Uiso 1 1 calc R . . H18B H 0.4512 0.0273 0.8707 0.055 Uiso 1 1 calc R . . H18C H 0.6023 0.0022 0.8656 0.055 Uiso 1 1 calc R . . C19 C 0.8029(8) 0.0661(3) 0.7257(8) 0.0389(18) Uani 1 1 d . . . H19A H 0.7887 0.0505 0.6383 0.058 Uiso 1 1 calc R . . H19B H 0.8382 0.0401 0.7908 0.058 Uiso 1 1 calc R . . H19C H 0.8712 0.0940 0.7271 0.058 Uiso 1 1 calc R . . C20 C 0.5225(7) 0.2119(3) 0.7226(8) 0.0324(16) Uani 1 1 d . . . C21 C 0.6809(9) 0.1712(3) 0.5550(7) 0.0363(17) Uani 1 1 d . . . C22 C 0.4366(8) 0.2061(3) 0.4607(7) 0.0347(16) Uani 1 1 d . . . C23 C 0.4775(9) 0.1043(3) 0.4773(7) 0.0390(18) 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 Cr1 0.0292(6) 0.0233(5) 0.0249(5) 0.0004(4) 0.0028(5) -0.0013(4) Sb1 0.0247(2) 0.0227(2) 0.0335(3) 0.00265(19) -0.00190(19) -0.00027(18) Sb2 0.0248(2) 0.0233(2) 0.0262(2) -0.00067(18) 0.00178(18) 0.00278(18) O1 0.052(3) 0.028(3) 0.045(3) -0.010(2) -0.006(3) 0.001(2) O2 0.042(3) 0.055(4) 0.049(4) 0.007(3) 0.014(3) -0.006(3) O3 0.069(4) 0.042(3) 0.039(3) 0.011(3) 0.001(3) 0.007(3) O4 0.114(6) 0.046(4) 0.050(4) -0.022(3) 0.021(4) -0.011(4) N1 0.029(3) 0.021(3) 0.031(3) -0.006(2) 0.000(2) 0.003(2) C1 0.036(4) 0.053(5) 0.043(5) 0.005(4) -0.012(4) -0.004(4) C2 0.039(4) 0.026(4) 0.068(6) 0.000(4) 0.001(4) 0.013(3) C3 0.022(3) 0.025(3) 0.042(4) -0.002(3) 0.002(3) -0.002(3) C4 0.030(4) 0.028(4) 0.050(5) -0.003(3) 0.000(3) 0.000(3) C5 0.038(4) 0.027(4) 0.064(6) 0.004(4) -0.006(4) -0.008(3) C6 0.032(4) 0.024(4) 0.077(6) 0.018(4) -0.005(4) -0.007(3) C7 0.023(4) 0.043(4) 0.052(5) 0.013(4) -0.003(3) -0.006(3) C8 0.020(3) 0.027(3) 0.045(4) 0.000(3) 0.000(3) -0.002(3) C9 0.019(3) 0.034(4) 0.039(4) -0.006(3) 0.005(3) 0.002(3) C10 0.046(5) 0.032(4) 0.053(5) -0.016(4) -0.005(4) 0.004(4) C11 0.024(3) 0.031(3) 0.032(4) 0.000(3) 0.006(3) -0.002(3) C12 0.021(3) 0.017(3) 0.036(4) 0.003(3) 0.000(3) 0.001(2) C13 0.034(4) 0.030(4) 0.033(4) -0.001(3) 0.003(3) 0.001(3) C14 0.033(4) 0.031(4) 0.032(4) -0.003(3) -0.003(3) -0.002(3) C15 0.026(4) 0.030(4) 0.043(4) -0.001(3) -0.009(3) -0.001(3) C16 0.026(3) 0.025(3) 0.037(4) -0.002(3) 0.003(3) 0.005(3) C17 0.024(3) 0.021(3) 0.027(3) 0.000(3) 0.001(3) 0.003(3) C18 0.038(4) 0.022(3) 0.049(5) -0.003(3) 0.004(4) 0.002(3) C19 0.031(4) 0.048(5) 0.038(4) 0.000(4) 0.003(3) 0.014(3) C20 0.026(4) 0.027(3) 0.042(4) 0.006(3) -0.004(3) 0.004(3) C21 0.043(5) 0.030(4) 0.035(4) 0.000(3) 0.004(4) -0.004(3) C22 0.043(4) 0.032(4) 0.030(4) 0.001(3) 0.009(3) 0.000(3) C23 0.051(5) 0.037(4) 0.030(4) 0.006(3) 0.009(4) -0.004(4) _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 Cr1 C21 1.835(8) . ? Cr1 C22 1.859(8) . ? Cr1 C23 1.862(8) . ? Cr1 C20 1.902(8) . ? Cr1 Sb2 2.5914(12) . ? Cr1 Sb1 2.5934(12) . ? Sb1 C2 2.122(7) . ? Sb1 C1 2.135(8) . ? Sb1 C3 2.155(7) . ? Sb2 C18 2.134(7) . ? Sb2 C17 2.141(7) . ? Sb2 C19 2.139(7) . ? O1 C20 1.150(9) . ? O2 C21 1.162(9) . ? O3 C22 1.153(9) . ? O4 C23 1.160(9) . ? N1 C9 1.466(8) . ? N1 C11 1.472(9) . ? N1 C10 1.480(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.392(10) . ? C3 C8 1.403(10) . ? C4 C5 1.371(10) . ? C4 H4 0.9500 . ? C5 C6 1.379(12) . ? C5 H5 0.9500 . ? C6 C7 1.393(12) . ? C6 H6 0.9500 . ? C7 C8 1.404(10) . ? C7 H7 0.9500 . ? C8 C9 1.508(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.509(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.399(9) . ? C12 C13 1.398(10) . ? C13 C14 1.385(10) . ? C13 H13 0.9500 . ? C14 C15 1.365(10) . ? C14 H14 0.9500 . ? C15 C16 1.381(10) . ? C15 H15 0.9500 . ? C16 C17 1.388(9) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C21 Cr1 C22 88.7(3) . . ? C21 Cr1 C23 92.1(3) . . ? C22 Cr1 C23 92.4(3) . . ? C21 Cr1 C20 91.1(3) . . ? C22 Cr1 C20 92.5(3) . . ? C23 Cr1 C20 174.2(3) . . ? C21 Cr1 Sb2 87.9(2) . . ? C22 Cr1 Sb2 176.6(2) . . ? C23 Cr1 Sb2 87.5(2) . . ? C20 Cr1 Sb2 87.8(2) . . ? C21 Cr1 Sb1 176.7(2) . . ? C22 Cr1 Sb1 88.5(2) . . ? C23 Cr1 Sb1 86.2(3) . . ? C20 Cr1 Sb1 90.8(2) . . ? Sb2 Cr1 Sb1 94.84(4) . . ? C2 Sb1 C1 95.8(3) . . ? C2 Sb1 C3 106.5(3) . . ? C1 Sb1 C3 97.4(3) . . ? C2 Sb1 Cr1 119.8(2) . . ? C1 Sb1 Cr1 111.0(2) . . ? C3 Sb1 Cr1 121.04(18) . . ? C18 Sb2 C17 101.7(3) . . ? C18 Sb2 C19 94.6(3) . . ? C17 Sb2 C19 98.9(3) . . ? C18 Sb2 Cr1 127.8(2) . . ? C17 Sb2 Cr1 117.72(17) . . ? C19 Sb2 Cr1 110.4(2) . . ? C9 N1 C11 109.7(5) . . ? C9 N1 C10 108.5(6) . . ? C11 N1 C10 108.8(6) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 119.3(7) . . ? C4 C3 Sb1 116.2(6) . . ? C8 C3 Sb1 124.1(5) . . ? C5 C4 C3 122.3(8) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 119.2(8) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C7 119.9(7) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C8 121.3(8) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 118.0(7) . . ? C7 C8 C9 119.2(7) . . ? C3 C8 C9 122.8(6) . . ? N1 C9 C8 113.4(5) . . ? N1 C9 H9A 108.9 . . ? C8 C9 H9A 108.9 . . ? N1 C9 H9B 108.9 . . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 114.1(6) . . ? N1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C17 C12 C13 117.7(6) . . ? C17 C12 C11 123.2(6) . . ? C13 C12 C11 119.1(6) . . ? C14 C13 C12 121.8(7) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C15 C14 C13 119.5(7) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.1(7) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.0(7) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C12 119.8(6) . . ? C16 C17 Sb2 116.2(5) . . ? C12 C17 Sb2 123.9(5) . . ? Sb2 C18 H18A 109.5 . . ? Sb2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Sb2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C20 Cr1 178.2(6) . . ? O2 C21 Cr1 179.4(8) . . ? O3 C22 Cr1 177.1(7) . . ? O4 C23 Cr1 179.2(7) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.347 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.169 #===END OF CIF ============================================================== # # 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 FILE =============================================================