# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef 'web_deposit_cif_file_0_BrianSkelton_1302590078.cif' # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Chemistry, School of Biomedical, Biomolecular and Chemical Science, M313, University of Western Australia, Perth, WA 6009, Australia ; _publ_contact_author_email brian.skelton@uwa.edu.au _publ_contact_author_fax (+61)_08_6488_1118 _publ_contact_author_phone (+61)_08_6488_7107 loop_ _publ_author_name _publ_author_footnote _publ_author_address R.O.Fuller . ; Chemistry, School of Biomedical, Biomolecular and Chemical Science, M313, University of Western Australia, Perth, WA 6009, Australia ; C.S.Griffith '' '' G.A.Koutsantonis '' '' K.M.Lapere '' '' B.W.Skelton '' '' M.A.Spackman '' '' A.H.White '' '' D.A.Wild '' '' _publ_section_references ; Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_gk54 _database_code_depnum_ccdc_archive 'CCDC 821463' #TrackingRef 'web_deposit_cif_file_0_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-04T13:25:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C7 H5 Cl O2 Ru' _chemical_formula_moiety 'C7 H5 Cl O2 Ru' _chemical_formula_weight 257.63 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc 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 6.6793(10) _cell_length_b 10.676(2) _cell_length_c 12.150(2) _cell_angle_alpha 90 _cell_angle_beta 99.859(3) _cell_angle_gamma 90 _cell_volume 853.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5015 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.9 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.86 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_unetI/netI 0.0079 _diffrn_reflns_number 8391 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 29.02 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.939 _reflns_number_total 2131 _reflns_number_gt 1923 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.7146P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2131 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.065 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.52 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.43557(3) 0.743300(16) 0.583491(14) 0.04127(8) Uani 1 1 d . . . Cl1 Cl 0.32293(13) 0.59099(7) 0.70610(6) 0.0696(2) Uani 1 1 d . . . C11 C 0.2163(5) 0.7031(4) 0.4697(2) 0.0699(8) Uani 1 1 d . . . O11 O 0.0924(4) 0.6788(4) 0.3975(2) 0.1157(11) Uani 1 1 d . . . C12 C 0.2796(4) 0.8683(3) 0.6395(3) 0.0617(6) Uani 1 1 d . . . O12 O 0.1868(4) 0.9466(2) 0.6686(2) 0.0915(8) Uani 1 1 d . . . C101 C 0.7562(5) 0.6682(4) 0.6189(3) 0.0808(10) Uani 1 1 d . . . H101 H 0.7965 0.5983 0.6629 0.097 Uiso 1 1 calc R . . C102 C 0.6852(5) 0.6674(3) 0.5018(3) 0.0725(8) Uani 1 1 d . . . H102 H 0.6689 0.5977 0.4552 0.087 Uiso 1 1 calc R . . C103 C 0.6441(4) 0.7940(3) 0.4698(2) 0.0644(7) Uani 1 1 d . . . H103 H 0.596 0.8221 0.3976 0.077 Uiso 1 1 calc R . . C104 C 0.6881(4) 0.8691(3) 0.5649(3) 0.0640(7) Uani 1 1 d . . . H104 H 0.6748 0.9558 0.5667 0.077 Uiso 1 1 calc R . . C105 C 0.7553(4) 0.7924(4) 0.6572(3) 0.0720(8) Uani 1 1 d . . . H105 H 0.7927 0.8189 0.7307 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03993(12) 0.05054(13) 0.03245(11) -0.00028(6) 0.00362(8) -0.00339(6) Cl1 0.0802(5) 0.0708(4) 0.0587(4) 0.0101(3) 0.0149(3) -0.0139(4) C11 0.0542(15) 0.108(2) 0.0465(14) -0.0049(16) 0.0062(12) -0.0100(16) O11 0.0689(15) 0.207(4) 0.0626(14) -0.022(2) -0.0119(12) -0.0257(19) C12 0.0547(14) 0.0628(15) 0.0706(17) -0.0047(13) 0.0192(13) -0.0103(12) O12 0.0783(15) 0.0782(15) 0.126(2) -0.0287(15) 0.0410(15) -0.0043(12) C101 0.0519(16) 0.094(2) 0.099(3) 0.039(2) 0.0204(16) 0.0176(15) C102 0.0631(17) 0.0746(19) 0.087(2) -0.0181(17) 0.0324(16) -0.0031(15) C103 0.0557(15) 0.090(2) 0.0502(14) 0.0100(15) 0.0154(12) -0.0049(15) C104 0.0555(15) 0.0640(16) 0.0744(18) 0.0000(14) 0.0163(13) -0.0115(12) C105 0.0447(14) 0.112(3) 0.0563(16) -0.0029(17) 0.0000(12) -0.0078(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C11 1.883(3) . ? Ru1 C12 1.890(3) . ? Ru1 C103 2.191(3) . ? Ru1 C104 2.198(3) . ? Ru1 C102 2.234(3) . ? Ru1 C105 2.232(3) . ? Ru1 C101 2.258(3) . ? Ru1 Cl1 2.4110(8) . ? C11 O11 1.128(3) . ? C12 O12 1.132(3) . ? C101 C105 1.406(6) . ? C101 C102 1.421(5) . ? C101 H101 0.93 . ? C102 C103 1.420(5) . ? C102 H102 0.93 . ? C103 C104 1.396(4) . ? C103 H103 0.93 . ? C104 C105 1.399(5) . ? C104 H104 0.93 . ? C105 H105 0.93 . ? 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 Ru1 C12 91.01(14) . . ? C11 Ru1 C103 95.28(12) . . ? C12 Ru1 C103 120.12(13) . . ? C11 Ru1 C104 125.31(13) . . ? C12 Ru1 C104 94.90(12) . . ? C103 Ru1 C104 37.11(12) . . ? C11 Ru1 C102 97.89(14) . . ? C12 Ru1 C102 156.29(12) . . ? C103 Ru1 C102 37.42(13) . . ? C104 Ru1 C102 62.08(12) . . ? C11 Ru1 C105 156.69(13) . . ? C12 Ru1 C105 103.79(14) . . ? C103 Ru1 C105 61.77(12) . . ? C104 Ru1 C105 36.80(12) . . ? C102 Ru1 C105 61.81(13) . . ? C11 Ru1 C101 130.70(16) . . ? C12 Ru1 C101 138.19(15) . . ? C103 Ru1 C101 61.53(12) . . ? C104 Ru1 C101 61.13(12) . . ? C102 Ru1 C101 36.87(14) . . ? C105 Ru1 C101 36.48(14) . . ? C11 Ru1 Cl1 90.81(11) . . ? C12 Ru1 Cl1 90.24(9) . . ? C103 Ru1 Cl1 148.81(10) . . ? C104 Ru1 Cl1 143.30(9) . . ? C102 Ru1 Cl1 111.44(10) . . ? C105 Ru1 Cl1 106.80(10) . . ? C101 Ru1 Cl1 91.65(9) . . ? O11 C11 Ru1 176.1(3) . . ? O12 C12 Ru1 176.7(3) . . ? C105 C101 C102 108.5(3) . . ? C105 C101 Ru1 70.75(17) . . ? C102 C101 Ru1 70.63(17) . . ? C105 C101 H101 125.8 . . ? C102 C101 H101 125.8 . . ? Ru1 C101 H101 124.5 . . ? C103 C102 C101 106.5(3) . . ? C103 C102 Ru1 69.65(16) . . ? C101 C102 Ru1 72.49(18) . . ? C103 C102 H102 126.7 . . ? C101 C102 H102 126.7 . . ? Ru1 C102 H102 122.8 . . ? C104 C103 C102 108.5(3) . . ? C104 C103 Ru1 71.71(16) . . ? C102 C103 Ru1 72.93(16) . . ? C104 C103 H103 125.8 . . ? C102 C103 H103 125.8 . . ? Ru1 C103 H103 121.3 . . ? C103 C104 C105 108.7(3) . . ? C103 C104 Ru1 71.18(16) . . ? C105 C104 Ru1 72.93(17) . . ? C103 C104 H104 125.7 . . ? C105 C104 H104 125.7 . . ? Ru1 C104 H104 121.9 . . ? C101 C105 C104 107.8(3) . . ? C101 C105 Ru1 72.77(17) . . ? C104 C105 Ru1 70.26(16) . . ? C101 C105 H105 126.1 . . ? C104 C105 H105 126.1 . . ? Ru1 C105 H105 122.6 . . ? #===END # Attachment 'web_deposit_cif_file_1_BrianSkelton_1302590078.cif' data_gk97l _database_code_depnum_ccdc_archive 'CCDC 821464' #TrackingRef 'web_deposit_cif_file_1_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-04T14:16:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C7 H5 Cl O2 Os' _chemical_formula_moiety 'C7 H5 Cl O2 Os' _chemical_formula_weight 346.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall '-p 2ybc' 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 6.5729(12) _cell_length_b 10.455(2) _cell_length_c 12.066(2) _cell_angle_alpha 90 _cell_angle_beta 98.710(2) _cell_angle_gamma 90 _cell_volume 819.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4644 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 28 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rhomboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.81 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 15.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .40 _exptl_absorpt_correction_T_max .77 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_unetI/netI 0.0157 _diffrn_reflns_number 8949 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.64 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 2008 _reflns_number_gt 1768 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+4.4762P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2008 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.908 _refine_diff_density_min -2.392 _refine_diff_density_rms 0.254 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.603 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.43996(3) 0.742973(18) 0.583055(16) 0.01174(9) Uani 1 1 d . . . Cl1 Cl 0.3296(2) 0.58897(14) 0.71080(12) 0.0211(3) Uani 1 1 d . . . C11 C 0.2258(9) 0.6984(6) 0.4674(5) 0.0211(12) Uani 1 1 d . . . O11 O 0.1063(7) 0.6684(6) 0.3930(4) 0.0352(12) Uani 1 1 d . . . C12 C 0.2721(9) 0.8714(6) 0.6335(5) 0.0190(11) Uani 1 1 d . . . O12 O 0.1771(7) 0.9539(4) 0.6597(4) 0.0252(9) Uani 1 1 d . . . C101 C 0.7701(9) 0.6651(6) 0.6222(6) 0.0232(13) Uani 1 1 d . . . H101 H 0.8114 0.593 0.6681 0.028 Uiso 1 1 calc R . . C102 C 0.7058(9) 0.6614(6) 0.5050(5) 0.0218(12) Uani 1 1 d . . . H102 H 0.6952 0.5874 0.4588 0.026 Uiso 1 1 calc R . . C103 C 0.6588(9) 0.7924(6) 0.4685(5) 0.0200(12) Uani 1 1 d . . . H103 H 0.6107 0.8193 0.3939 0.024 Uiso 1 1 calc R . . C104 C 0.6974(9) 0.8724(6) 0.5640(5) 0.0193(12) Uani 1 1 d . . . H104 H 0.6821 0.9628 0.5639 0.023 Uiso 1 1 calc R . . C105 C 0.7635(9) 0.7948(6) 0.6611(5) 0.0210(12) Uani 1 1 d . . . H105 H 0.7964 0.8236 0.7364 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.01063(13) 0.01346(13) 0.01060(14) -0.00005(7) -0.00016(8) -0.00184(7) Cl1 0.0255(7) 0.0191(6) 0.0186(7) 0.0042(5) 0.0030(5) -0.0063(5) C11 0.014(3) 0.030(3) 0.021(3) -0.003(2) 0.006(2) -0.003(2) O11 0.025(2) 0.058(4) 0.020(2) -0.006(2) -0.0062(19) -0.005(2) C12 0.016(3) 0.025(3) 0.016(3) -0.001(2) 0.003(2) -0.008(2) O12 0.021(2) 0.022(2) 0.034(3) -0.0048(19) 0.0095(19) 0.0019(17) C101 0.014(3) 0.024(3) 0.032(3) 0.006(3) 0.006(2) 0.006(2) C102 0.020(3) 0.018(3) 0.030(3) -0.001(2) 0.011(2) 0.000(2) C103 0.018(3) 0.024(3) 0.019(3) 0.004(2) 0.006(2) -0.003(2) C104 0.014(3) 0.018(3) 0.026(3) 0.001(2) 0.005(2) -0.006(2) C105 0.009(3) 0.028(3) 0.025(3) 0.000(3) 0.000(2) -0.004(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C11 1.884(6) . ? Os1 C12 1.896(6) . ? Os1 C103 2.202(6) . ? Os1 C104 2.206(5) . ? Os1 C105 2.257(6) . ? Os1 C102 2.273(6) . ? Os1 C101 2.299(6) . ? Os1 Cl1 2.4153(14) . ? C11 O11 1.144(7) . ? C12 O12 1.137(7) . ? C101 C102 1.413(9) . ? C101 C105 1.438(9) . ? C101 H101 0.95 . ? C102 C103 1.458(8) . ? C102 H102 0.95 . ? C103 C104 1.415(9) . ? C103 H103 0.95 . ? C104 C105 1.437(9) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? 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 Os1 C12 90.4(3) . . ? C11 Os1 C103 94.5(2) . . ? C12 Os1 C103 120.2(2) . . ? C11 Os1 C104 125.0(2) . . ? C12 Os1 C104 95.3(2) . . ? C103 Os1 C104 37.5(2) . . ? C11 Os1 C105 156.8(2) . . ? C12 Os1 C105 104.7(2) . . ? C103 Os1 C105 62.7(2) . . ? C104 Os1 C105 37.6(2) . . ? C11 Os1 C102 97.8(2) . . ? C12 Os1 C102 157.0(2) . . ? C103 Os1 C102 38.0(2) . . ? C104 Os1 C102 62.4(2) . . ? C105 Os1 C102 61.8(2) . . ? C11 Os1 C101 129.8(3) . . ? C12 Os1 C101 139.6(2) . . ? C103 Os1 C101 61.7(2) . . ? C104 Os1 C101 61.5(2) . . ? C105 Os1 C101 36.8(2) . . ? C102 Os1 C101 36.0(2) . . ? C11 Os1 Cl1 92.56(19) . . ? C12 Os1 Cl1 91.23(18) . . ? C103 Os1 Cl1 147.67(17) . . ? C104 Os1 Cl1 141.71(16) . . ? C105 Os1 Cl1 104.40(17) . . ? C102 Os1 Cl1 109.76(16) . . ? C101 Os1 Cl1 89.90(16) . . ? O11 C11 Os1 175.1(5) . . ? O12 C12 Os1 175.6(5) . . ? C102 C101 C105 109.5(5) . . ? C102 C101 Os1 71.0(3) . . ? C105 C101 Os1 70.0(3) . . ? C102 C101 H101 125.3 . . ? C105 C101 H101 125.3 . . ? Os1 C101 H101 125.3 . . ? C101 C102 C103 107.1(5) . . ? C101 C102 Os1 73.0(3) . . ? C103 C102 Os1 68.4(3) . . ? C101 C102 H102 126.4 . . ? C103 C102 H102 126.4 . . ? Os1 C102 H102 123.8 . . ? C104 C103 C102 107.8(5) . . ? C104 C103 Os1 71.4(3) . . ? C102 C103 Os1 73.6(3) . . ? C104 C103 H103 126.1 . . ? C102 C103 H103 126.1 . . ? Os1 C103 H103 120.6 . . ? C103 C104 C105 108.9(5) . . ? C103 C104 Os1 71.1(3) . . ? C105 C104 Os1 73.2(3) . . ? C103 C104 H104 125.5 . . ? C105 C104 H104 125.5 . . ? Os1 C104 H104 121.8 . . ? C101 C105 C104 106.7(5) . . ? C101 C105 Os1 73.2(3) . . ? C104 C105 Os1 69.3(3) . . ? C101 C105 H105 126.7 . . ? C104 C105 H105 126.7 . . ? Os1 C105 H105 122.6 . . ? #===END # Attachment 'web_deposit_cif_file_2_BrianSkelton_1302590078.cif' data_gk132 _database_code_depnum_ccdc_archive 'CCDC 821465' #TrackingRef 'web_deposit_cif_file_2_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-04T21:47:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C12 H15 Cl O2 Ru' _chemical_formula_moiety 'C12 H15 Cl O2 Ru' _chemical_formula_weight 327.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7919(8) _cell_length_b 7.8225(10) _cell_length_c 12.819(2) _cell_angle_alpha 84.500(3) _cell_angle_beta 87.327(3) _cell_angle_gamma 72.547(3) _cell_volume 646.61(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5946 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 25.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour off_white _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .77 _exptl_absorpt_correction_T_max .89 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_unetI/netI 0.0317 _diffrn_reflns_number 13382 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 37.74 _diffrn_reflns_theta_full 35 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 6634 _reflns_number_gt 5533 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule is rotationally disordered about the cp*(centroid)-Ru1 bond by approximately 120 degrees. The site occupancies of the two components refined to 0.651(6) and its complement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6634 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.458 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.483278(17) 0.178098(15) 0.246096(9) 0.02045(4) Uani 1 1 d . . . Cl1 Cl 0.79385(15) -0.06891(14) 0.28999(7) 0.0351(3) Uani 0.651(6) 1 d P A 1 C11 C 0.5558(2) 0.3360(2) 0.33168(13) 0.0276(3) Uani 1 1 d . A . O11 O 0.5848(2) 0.4312(2) 0.38321(12) 0.0398(3) Uani 1 1 d . . . C21 C 0.6114(5) 0.2633(5) 0.1307(3) 0.0293(6) Uani 0.651(6) 1 d P A 1 O21 O 0.6819(7) 0.3231(4) 0.0547(3) 0.0499(8) Uani 0.651(6) 1 d P A 1 Cl2 Cl 0.6136(3) 0.3149(3) 0.08848(17) 0.0390(8) Uani 0.349(6) 1 d P A 2 C31 C 0.7335(12) -0.0002(12) 0.2715(6) 0.0339(12) Uani 0.349(6) 1 d P A 2 O31 O 0.8777(15) -0.1188(9) 0.2932(5) 0.0528(15) Uani 0.349(6) 1 d P A 2 C101 C 0.2708(2) 0.0387(2) 0.32915(12) 0.0267(3) Uani 1 1 d . A . C102 C 0.1721(2) 0.2283(3) 0.32326(13) 0.0285(3) Uani 1 1 d . A . C103 C 0.1500(2) 0.2945(2) 0.21451(13) 0.0248(3) Uani 1 1 d . A . C104 C 0.2254(2) 0.1410(2) 0.15353(12) 0.0225(2) Uani 1 1 d . A . C105 C 0.3015(2) -0.0148(2) 0.22320(12) 0.0227(2) Uani 1 1 d . A . C106 C 0.3131(4) -0.0907(3) 0.42540(15) 0.0403(4) Uani 1 1 d . . . H10A H 0.3097 -0.0245 0.487 0.06 Uiso 1 1 calc R A . H10B H 0.4496 -0.1784 0.4185 0.06 Uiso 1 1 calc R . . H10C H 0.2077 -0.1536 0.4337 0.06 Uiso 1 1 calc R . . C107 C 0.1002(3) 0.3384(3) 0.41501(16) 0.0410(5) Uani 1 1 d . . . H10D H -0.0371 0.3321 0.4382 0.062 Uiso 1 1 calc R A . H10E H 0.0936 0.4638 0.3942 0.062 Uiso 1 1 calc R . . H10F H 0.1972 0.2912 0.4725 0.062 Uiso 1 1 calc R . . C108 C 0.0398(3) 0.4816(2) 0.17136(19) 0.0375(4) Uani 1 1 d . . . H10G H -0.1014 0.4887 0.1537 0.056 Uiso 1 1 calc R A . H10H H 0.1128 0.5132 0.1082 0.056 Uiso 1 1 calc R . . H10I H 0.0356 0.5658 0.2239 0.056 Uiso 1 1 calc R . . C109 C 0.2116(3) 0.1484(3) 0.03674(13) 0.0314(3) Uani 1 1 d . . . H10J H 0.3076 0.0392 0.0113 0.047 Uiso 1 1 calc R A . H10K H 0.2478 0.254 0.0045 0.047 Uiso 1 1 calc R . . H10L H 0.0705 0.1568 0.0181 0.047 Uiso 1 1 calc R . . C100 C 0.3875(3) -0.2051(2) 0.19565(15) 0.0327(3) Uani 1 1 d . . . H10M H 0.2848 -0.2692 0.2128 0.049 Uiso 1 1 calc R A . H10N H 0.5127 -0.2645 0.2357 0.049 Uiso 1 1 calc R . . H10O H 0.4211 -0.206 0.1205 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01867(5) 0.02056(6) 0.02271(6) -0.00395(4) -0.00024(3) -0.00607(4) Cl1 0.0225(6) 0.0289(6) 0.0502(5) -0.0081(4) -0.0045(3) 0.0002(5) C11 0.0213(6) 0.0283(7) 0.0297(7) 0.0038(6) -0.0016(5) -0.0037(5) O11 0.0453(8) 0.0326(7) 0.0415(7) -0.0051(6) -0.0086(6) -0.0099(6) C21 0.0300(13) 0.0406(16) 0.0225(13) -0.0028(12) 0.0001(10) -0.0184(12) O21 0.0526(17) 0.084(2) 0.0275(12) -0.0056(12) 0.0136(12) -0.0437(16) Cl2 0.0413(9) 0.0489(11) 0.0346(15) -0.0102(8) 0.0041(8) -0.0237(7) C31 0.024(3) 0.024(3) 0.056(4) -0.008(3) -0.004(2) -0.008(2) O31 0.031(3) 0.033(3) 0.088(4) -0.012(3) -0.008(3) 0.003(2) C101 0.0253(7) 0.0334(8) 0.0233(6) -0.0013(6) -0.0004(5) -0.0122(6) C102 0.0207(6) 0.0379(9) 0.0292(7) -0.0123(6) 0.0037(5) -0.0101(6) C103 0.0193(6) 0.0238(7) 0.0317(7) -0.0061(5) -0.0012(5) -0.0057(5) C104 0.0202(6) 0.0236(6) 0.0244(6) -0.0029(5) -0.0028(5) -0.0069(5) C105 0.0231(6) 0.0222(6) 0.0250(6) -0.0020(5) -0.0016(5) -0.0101(5) C106 0.0470(11) 0.0510(12) 0.0273(8) 0.0069(8) -0.0035(7) -0.0242(9) C107 0.0314(8) 0.0570(13) 0.0373(9) -0.0248(9) 0.0092(7) -0.0121(8) C108 0.0278(8) 0.0239(8) 0.0582(12) -0.0061(7) -0.0091(8) -0.0019(6) C109 0.0338(8) 0.0351(9) 0.0245(7) -0.0027(6) -0.0058(6) -0.0080(7) C100 0.0408(9) 0.0221(7) 0.0366(9) -0.0035(6) -0.0049(7) -0.0107(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C21 1.852(4) . ? Ru1 C31 1.866(9) . ? Ru1 C11 1.9098(19) . ? Ru1 C103 2.2123(15) . ? Ru1 C102 2.2318(16) . ? Ru1 C101 2.2327(16) . ? Ru1 C105 2.2632(15) . ? Ru1 C104 2.2642(15) . ? Ru1 Cl1 2.4407(11) . ? Ru1 Cl2 2.449(2) . ? C11 O11 1.106(2) . ? C21 O21 1.183(7) . ? C31 O31 1.152(15) . ? C101 C102 1.429(3) . ? C101 C105 1.447(2) . ? C101 C106 1.499(2) . ? C102 C103 1.438(2) . ? C102 C107 1.501(2) . ? C103 C104 1.446(2) . ? C103 C108 1.495(2) . ? C104 C105 1.416(2) . ? C104 C109 1.499(2) . ? C105 C100 1.497(2) . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? C107 H10D 0.98 . ? C107 H10E 0.98 . ? C107 H10F 0.98 . ? C108 H10G 0.98 . ? C108 H10H 0.98 . ? C108 H10I 0.98 . ? C109 H10J 0.98 . ? C109 H10K 0.98 . ? C109 H10L 0.98 . ? C100 H10M 0.98 . ? C100 H10N 0.98 . ? C100 H10O 0.98 . ? 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 Ru1 C11 90.73(10) . . ? C31 Ru1 C11 91.90(19) . . ? C21 Ru1 C103 104.04(12) . . ? C31 Ru1 C103 157.77(19) . . ? C11 Ru1 C103 106.71(6) . . ? C21 Ru1 C102 140.03(13) . . ? C31 Ru1 C102 132.4(2) . . ? C11 Ru1 C102 91.64(6) . . ? C103 Ru1 C102 37.76(6) . . ? C21 Ru1 C101 155.62(10) . . ? C31 Ru1 C101 99.0(2) . . ? C11 Ru1 C101 112.39(7) . . ? C103 Ru1 C101 63.05(6) . . ? C102 Ru1 C101 37.34(7) . . ? C21 Ru1 C105 118.77(10) . . ? C31 Ru1 C105 95.33(18) . . ? C11 Ru1 C105 149.84(6) . . ? C103 Ru1 C105 62.48(6) . . ? C102 Ru1 C105 62.21(6) . . ? C101 Ru1 C105 37.53(6) . . ? C21 Ru1 C104 94.79(10) . . ? C31 Ru1 C104 123.71(19) . . ? C11 Ru1 C104 144.11(6) . . ? C103 Ru1 C104 37.66(6) . . ? C102 Ru1 C104 62.21(6) . . ? C101 Ru1 C104 62.06(6) . . ? C105 Ru1 C104 36.45(5) . . ? C21 Ru1 Cl1 92.28(12) . . ? C11 Ru1 Cl1 93.08(5) . . ? C103 Ru1 Cl1 153.90(5) . . ? C102 Ru1 Cl1 127.38(6) . . ? C101 Ru1 Cl1 94.01(5) . . ? C105 Ru1 Cl1 91.89(5) . . ? C104 Ru1 Cl1 122.00(4) . . ? C31 Ru1 Cl2 93.9(2) . . ? C11 Ru1 Cl2 91.23(6) . . ? C103 Ru1 Cl2 97.60(6) . . ? C102 Ru1 Cl2 133.43(7) . . ? C101 Ru1 Cl2 152.46(6) . . ? C105 Ru1 Cl2 117.34(5) . . ? C104 Ru1 Cl2 90.55(6) . . ? O11 C11 Ru1 175.46(16) . . ? O21 C21 Ru1 176.1(3) . . ? O31 C31 Ru1 173.6(6) . . ? C102 C101 C105 107.71(14) . . ? C102 C101 C106 127.76(16) . . ? C105 C101 C106 124.12(17) . . ? C102 C101 Ru1 71.30(9) . . ? C105 C101 Ru1 72.38(9) . . ? C106 C101 Ru1 127.66(13) . . ? C101 C102 C103 108.29(14) . . ? C101 C102 C107 125.71(18) . . ? C103 C102 C107 125.98(18) . . ? C101 C102 Ru1 71.36(9) . . ? C103 C102 Ru1 70.38(9) . . ? C107 C102 Ru1 124.93(12) . . ? C102 C103 C104 107.30(14) . . ? C102 C103 C108 126.82(16) . . ? C104 C103 C108 125.22(15) . . ? C102 C103 Ru1 71.85(9) . . ? C104 C103 Ru1 73.12(8) . . ? C108 C103 Ru1 127.67(12) . . ? C105 C104 C103 108.43(13) . . ? C105 C104 C109 126.86(14) . . ? C103 C104 C109 124.62(14) . . ? C105 C104 Ru1 71.74(8) . . ? C103 C104 Ru1 69.23(8) . . ? C109 C104 Ru1 127.44(11) . . ? C104 C105 C101 108.16(14) . . ? C104 C105 C100 127.31(14) . . ? C101 C105 C100 124.43(15) . . ? C104 C105 Ru1 71.81(8) . . ? C101 C105 Ru1 70.09(9) . . ? C100 C105 Ru1 126.61(11) . . ? C101 C106 H10A 109.5 . . ? C101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? C102 C107 H10D 109.5 . . ? C102 C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C102 C107 H10F 109.5 . . ? H10D C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C103 C108 H10G 109.5 . . ? C103 C108 H10H 109.5 . . ? H10G C108 H10H 109.5 . . ? C103 C108 H10I 109.5 . . ? H10G C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? C104 C109 H10J 109.5 . . ? C104 C109 H10K 109.5 . . ? H10J C109 H10K 109.5 . . ? C104 C109 H10L 109.5 . . ? H10J C109 H10L 109.5 . . ? H10K C109 H10L 109.5 . . ? C105 C100 H10M 109.5 . . ? C105 C100 H10N 109.5 . . ? H10M C100 H10N 109.5 . . ? C105 C100 H10O 109.5 . . ? H10M C100 H10O 109.5 . . ? H10N C100 H10O 109.5 . . ? #===END # Attachment 'web_deposit_cif_file_3_BrianSkelton_1302590078.cif' data_cprucl _database_code_depnum_ccdc_archive 'CCDC 821466' #TrackingRef 'web_deposit_cif_file_3_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-05T14:52:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C12 H15 Cl O2 Ru' _chemical_formula_moiety 'C12 H15 Cl O2 Ru' _chemical_formula_weight 327.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_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 12.0242(10) _cell_length_b 7.9991(7) _cell_length_c 14.1805(12) _cell_angle_alpha 90 _cell_angle_beta 106.583(2) _cell_angle_gamma 90 _cell_volume 1307.19(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7791 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .57 _exptl_absorpt_correction_T_max .80 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_unetI/netI 0.034 _diffrn_reflns_number 27344 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 37.5 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 6866 _reflns_number_gt 5145 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6866 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.681 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.756849(9) 0.682157(14) 0.532048(8) 0.01684(3) Uani 1 1 d . . . C11 C 0.71393(13) 0.5326(2) 0.42488(11) 0.0240(3) Uani 1 1 d . . . O11 O 0.69163(11) 0.45058(18) 0.35635(10) 0.0369(3) Uani 1 1 d . . . C21 C 0.61121(14) 0.66250(19) 0.55718(12) 0.0246(3) Uani 1 1 d . . . O21 O 0.52213(11) 0.66313(17) 0.57077(11) 0.0376(3) Uani 1 1 d . . . Cl1 Cl 0.84664(3) 0.46085(5) 0.64593(3) 0.02409(7) Uani 1 1 d . . . C101 C 0.92841(12) 0.81262(18) 0.55745(11) 0.0194(2) Uani 1 1 d . . . C102 C 0.86211(12) 0.84028(17) 0.45865(10) 0.0196(3) Uani 1 1 d . . . C103 C 0.75646(12) 0.92580(18) 0.46002(10) 0.0191(2) Uani 1 1 d . . . C104 C 0.76238(11) 0.95854(17) 0.55981(11) 0.0192(2) Uani 1 1 d . . . C105 C 0.86586(12) 0.88432(19) 0.62216(10) 0.0202(2) Uani 1 1 d . . . C106 C 1.04513(13) 0.7298(2) 0.59074(13) 0.0279(3) Uani 1 1 d . . . H10A H 1.0639 0.6805 0.5339 0.042 Uiso 1 1 calc R . . H10B H 1.0436 0.6419 0.6385 0.042 Uiso 1 1 calc R . . H10C H 1.1041 0.813 0.6216 0.042 Uiso 1 1 calc R . . C107 C 0.89578(15) 0.7949(2) 0.36832(12) 0.0271(3) Uani 1 1 d . . . H10D H 0.932 0.8915 0.3464 0.041 Uiso 1 1 calc R . . H10E H 0.8265 0.7617 0.3161 0.041 Uiso 1 1 calc R . . H10F H 0.9509 0.7016 0.3831 0.041 Uiso 1 1 calc R . . C108 C 0.66628(14) 0.9933(2) 0.37187(12) 0.0288(3) Uani 1 1 d . . . H10G H 0.5895 0.9841 0.3825 0.043 Uiso 1 1 calc R . . H10H H 0.6676 0.929 0.3134 0.043 Uiso 1 1 calc R . . H10I H 0.683 1.111 0.3622 0.043 Uiso 1 1 calc R . . C109 C 0.67700(14) 1.0594(2) 0.59623(13) 0.0276(3) Uani 1 1 d . . . H10J H 0.7005 1.1772 0.6018 0.041 Uiso 1 1 calc R . . H10K H 0.6756 1.0178 0.6609 0.041 Uiso 1 1 calc R . . H10L H 0.5995 1.0489 0.5497 0.041 Uiso 1 1 calc R . . C100 C 0.90804(14) 0.8882(2) 0.73176(11) 0.0292(3) Uani 1 1 d . . . H10M H 0.9631 0.9805 0.7529 0.044 Uiso 1 1 calc R . . H10N H 0.9466 0.7822 0.756 0.044 Uiso 1 1 calc R . . H10O H 0.8421 0.9043 0.7585 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01594(5) 0.01750(5) 0.01725(5) -0.00045(4) 0.00502(3) -0.00169(4) C11 0.0216(6) 0.0249(7) 0.0245(7) -0.0013(6) 0.0049(5) -0.0017(5) O11 0.0343(6) 0.0416(7) 0.0317(6) -0.0149(6) 0.0044(5) -0.0043(6) C21 0.0223(6) 0.0214(7) 0.0307(7) 0.0025(6) 0.0085(6) -0.0020(5) O21 0.0242(6) 0.0397(8) 0.0536(9) 0.0061(6) 0.0187(6) -0.0006(5) Cl1 0.02570(16) 0.02189(16) 0.02577(16) 0.00581(13) 0.00912(13) 0.00234(13) C101 0.0163(5) 0.0215(6) 0.0210(6) 0.0006(5) 0.0063(4) -0.0026(5) C102 0.0207(6) 0.0204(6) 0.0196(6) 0.0001(5) 0.0086(5) -0.0018(5) C103 0.0188(6) 0.0176(6) 0.0204(6) 0.0007(5) 0.0046(5) -0.0014(5) C104 0.0158(5) 0.0140(5) 0.0284(6) -0.0009(5) 0.0074(5) -0.0019(4) C105 0.0194(6) 0.0220(6) 0.0190(6) -0.0020(5) 0.0051(5) -0.0055(5) C106 0.0177(6) 0.0322(8) 0.0330(8) 0.0042(7) 0.0061(6) 0.0021(6) C107 0.0343(8) 0.0285(8) 0.0237(7) -0.0006(6) 0.0166(6) -0.0007(6) C108 0.0286(7) 0.0292(8) 0.0258(7) 0.0061(6) 0.0030(6) 0.0024(6) C109 0.0273(7) 0.0248(7) 0.0337(8) -0.0057(6) 0.0138(6) 0.0012(6) C100 0.0259(7) 0.0415(9) 0.0190(6) -0.0038(6) 0.0046(5) -0.0071(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C11 1.8867(16) . ? Ru1 C21 1.8906(16) . ? Ru1 C103 2.1997(14) . ? Ru1 C105 2.2383(14) . ? Ru1 C104 2.2433(14) . ? Ru1 C102 2.2443(14) . ? Ru1 C101 2.2472(14) . ? Ru1 Cl1 2.4315(4) . ? C11 O11 1.1392(19) . ? C21 O21 1.141(2) . ? C101 C102 1.418(2) . ? C101 C105 1.460(2) . ? C101 C106 1.501(2) . ? C102 C103 1.4479(19) . ? C102 C107 1.494(2) . ? C103 C104 1.421(2) . ? C103 C108 1.502(2) . ? C104 C105 1.433(2) . ? C104 C109 1.508(2) . ? C105 C100 1.491(2) . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? C107 H10D 0.98 . ? C107 H10E 0.98 . ? C107 H10F 0.98 . ? C108 H10G 0.98 . ? C108 H10H 0.98 . ? C108 H10I 0.98 . ? C109 H10J 0.98 . ? C109 H10K 0.98 . ? C109 H10L 0.98 . ? C100 H10M 0.98 . ? C100 H10N 0.98 . ? C100 H10O 0.98 . ? 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 Ru1 C21 92.52(7) . . ? C11 Ru1 C103 102.94(6) . . ? C21 Ru1 C103 106.37(6) . . ? C11 Ru1 C105 154.02(6) . . ? C21 Ru1 C105 112.05(6) . . ? C103 Ru1 C105 63.14(5) . . ? C11 Ru1 C104 138.93(6) . . ? C21 Ru1 C104 91.81(6) . . ? C103 Ru1 C104 37.28(5) . . ? C105 Ru1 C104 37.30(5) . . ? C11 Ru1 C102 92.56(6) . . ? C21 Ru1 C102 144.05(6) . . ? C103 Ru1 C102 38.01(5) . . ? C105 Ru1 C102 62.72(5) . . ? C104 Ru1 C102 62.20(5) . . ? C11 Ru1 C101 116.82(6) . . ? C21 Ru1 C101 149.96(6) . . ? C103 Ru1 C101 62.82(5) . . ? C105 Ru1 C101 37.98(5) . . ? C104 Ru1 C101 62.24(5) . . ? C102 Ru1 C101 36.80(5) . . ? C11 Ru1 Cl1 92.34(5) . . ? C21 Ru1 Cl1 94.24(5) . . ? C103 Ru1 Cl1 153.52(4) . . ? C105 Ru1 Cl1 94.02(4) . . ? C104 Ru1 Cl1 128.00(4) . . ? C102 Ru1 Cl1 121.06(4) . . ? C101 Ru1 Cl1 91.05(4) . . ? O11 C11 Ru1 174.83(15) . . ? O21 C21 Ru1 174.85(14) . . ? C102 C101 C105 108.34(12) . . ? C102 C101 C106 126.24(13) . . ? C105 C101 C106 125.38(13) . . ? C102 C101 Ru1 71.49(8) . . ? C105 C101 Ru1 70.68(8) . . ? C106 C101 Ru1 125.35(11) . . ? C101 C102 C103 107.97(12) . . ? C101 C102 C107 126.57(13) . . ? C103 C102 C107 125.44(13) . . ? C101 C102 Ru1 71.71(8) . . ? C103 C102 Ru1 69.32(8) . . ? C107 C102 Ru1 125.96(10) . . ? C104 C103 C102 107.80(12) . . ? C104 C103 C108 125.57(14) . . ? C102 C103 C108 125.91(13) . . ? C104 C103 Ru1 73.02(8) . . ? C102 C103 Ru1 72.66(8) . . ? C108 C103 Ru1 127.62(11) . . ? C103 C104 C105 109.02(12) . . ? C103 C104 C109 126.45(13) . . ? C105 C104 C109 124.50(14) . . ? C103 C104 Ru1 69.70(8) . . ? C105 C104 Ru1 71.16(8) . . ? C109 C104 Ru1 126.76(10) . . ? C104 C105 C101 106.70(12) . . ? C104 C105 C100 127.70(14) . . ? C101 C105 C100 125.47(13) . . ? C104 C105 Ru1 71.54(8) . . ? C101 C105 Ru1 71.34(8) . . ? C100 C105 Ru1 125.41(11) . . ? C101 C106 H10A 109.5 . . ? C101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? C102 C107 H10D 109.5 . . ? C102 C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C102 C107 H10F 109.5 . . ? H10D C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C103 C108 H10G 109.5 . . ? C103 C108 H10H 109.5 . . ? H10G C108 H10H 109.5 . . ? C103 C108 H10I 109.5 . . ? H10G C108 H10I 109.5 . . ? H10H C108 H10I 109.5 . . ? C104 C109 H10J 109.5 . . ? C104 C109 H10K 109.5 . . ? H10J C109 H10K 109.5 . . ? C104 C109 H10L 109.5 . . ? H10J C109 H10L 109.5 . . ? H10K C109 H10L 109.5 . . ? C105 C100 H10M 109.5 . . ? C105 C100 H10N 109.5 . . ? H10M C100 H10N 109.5 . . ? C105 C100 H10O 109.5 . . ? H10M C100 H10O 109.5 . . ? H10N C100 H10O 109.5 . . ? #===END # Attachment 'web_deposit_cif_file_4_BrianSkelton_1302590078.cif' data_gk99 _database_code_depnum_ccdc_archive 'CCDC 821467' #TrackingRef 'web_deposit_cif_file_4_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-06T09:09:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H7 Cl O2 Ru' _chemical_formula_sum 'C8 H7 Cl O2 Ru' _chemical_formula_weight 271.66 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_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 8.4488(13) _cell_length_b 9.9193(15) _cell_length_c 11.619(2) _cell_angle_alpha 90 _cell_angle_beta 107.559(2) _cell_angle_gamma 90 _cell_volume 928.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6791 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.89 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_unetI/netI 0.012 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_number 10334 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.89 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.947 _reflns_number_total 2325 _reflns_number_gt 2177 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.3994P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2325 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.511 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.261229(16) 0.292332(13) 0.491045(11) 0.01866(6) Uani 1 1 d . . . C11 C 0.2482(2) 0.39497(18) 0.35110(16) 0.0260(4) Uani 1 1 d . . . O11 O 0.2325(2) 0.45307(16) 0.26365(12) 0.0401(4) Uani 1 1 d . . . C12 C 0.4874(3) 0.2516(2) 0.51405(18) 0.0304(4) Uani 1 1 d . . . O12 O 0.6208(2) 0.21849(17) 0.52855(18) 0.0500(5) Uani 1 1 d . . . Cl1 Cl 0.33445(6) 0.49011(4) 0.61573(4) 0.02686(10) Uani 1 1 d . . . C101 C 0.0766(2) 0.23011(18) 0.59195(17) 0.0253(4) Uani 1 1 d . . . C102 C -0.0083(2) 0.2519(2) 0.46787(19) 0.0308(4) Uani 1 1 d . . . H102 H -0.0927 0.317 0.4361 0.037 Uiso 1 1 calc R . . C103 C 0.0559(3) 0.1580(2) 0.39890(19) 0.0377(5) Uani 1 1 d . . . H103 H 0.0205 0.1492 0.3135 0.045 Uiso 1 1 calc R . . C104 C 0.1808(3) 0.08144(19) 0.4806(2) 0.0362(5) Uani 1 1 d . . . H104 H 0.2446 0.0119 0.4598 0.043 Uiso 1 1 calc R . . C105 C 0.1951(2) 0.12645(18) 0.60039(18) 0.0291(4) Uani 1 1 d . . . H105 H 0.2707 0.0928 0.6728 0.035 Uiso 1 1 calc R . . C106 C 0.0462(3) 0.3040(2) 0.6950(2) 0.0365(5) Uani 1 1 d . . . H10A H 0.018 0.398 0.6718 0.055 Uiso 1 1 calc R . . H10B H 0.1465 0.301 0.7647 0.055 Uiso 1 1 calc R . . H10C H -0.0459 0.2614 0.7163 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02043(8) 0.01749(8) 0.01929(8) 0.00077(4) 0.00783(6) 0.00111(5) C11 0.0262(9) 0.0283(9) 0.0248(9) -0.0003(7) 0.0096(7) 0.0025(7) O11 0.0461(9) 0.0482(9) 0.0282(7) 0.0131(7) 0.0146(7) 0.0083(7) C12 0.0322(10) 0.0272(9) 0.0356(10) 0.0108(8) 0.0159(8) 0.0065(8) O12 0.0328(8) 0.0528(10) 0.0722(12) 0.0297(8) 0.0276(8) 0.0194(7) Cl1 0.0324(2) 0.0226(2) 0.0255(2) -0.00330(15) 0.00860(17) -0.00402(16) C101 0.0249(9) 0.0241(8) 0.0315(9) 0.0000(7) 0.0157(8) -0.0050(7) C102 0.0209(9) 0.0358(10) 0.0350(11) 0.0022(8) 0.0072(8) -0.0059(8) C103 0.0412(12) 0.0402(11) 0.0324(10) -0.0110(9) 0.0121(9) -0.0186(9) C104 0.0496(12) 0.0195(9) 0.0493(12) -0.0074(8) 0.0295(10) -0.0070(8) C105 0.0346(10) 0.0212(8) 0.0359(10) 0.0063(7) 0.0172(8) -0.0002(7) C106 0.0416(12) 0.0377(11) 0.0402(12) -0.0031(8) 0.0277(10) -0.0010(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C12 1.892(2) . ? Ru1 C11 1.8933(18) . ? Ru1 C104 2.1914(19) . ? Ru1 C103 2.193(2) . ? Ru1 C102 2.2472(19) . ? Ru1 C105 2.2499(17) . ? Ru1 C101 2.3004(18) . ? Ru1 Cl1 2.4062(5) . ? C11 O11 1.141(2) . ? C12 O12 1.137(3) . ? C101 C105 1.418(3) . ? C101 C102 1.420(3) . ? C101 C106 1.491(3) . ? C102 C103 1.437(3) . ? C102 H102 0.95 . ? C103 C104 1.410(3) . ? C103 H103 0.95 . ? C104 C105 1.431(3) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? 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 C12 Ru1 C11 91.77(8) . . ? C12 Ru1 C104 94.99(9) . . ? C11 Ru1 C104 121.95(8) . . ? C12 Ru1 C103 123.77(9) . . ? C11 Ru1 C103 94.29(8) . . ? C104 Ru1 C103 37.52(9) . . ? C12 Ru1 C102 157.36(10) . . ? C11 Ru1 C102 101.46(8) . . ? C104 Ru1 C102 62.42(8) . . ? C103 Ru1 C102 37.75(8) . . ? C12 Ru1 C105 100.16(8) . . ? C11 Ru1 C105 156.67(8) . . ? C104 Ru1 C105 37.57(7) . . ? C103 Ru1 C105 62.41(8) . . ? C102 Ru1 C105 61.44(8) . . ? C12 Ru1 C101 133.01(8) . . ? C11 Ru1 C101 135.17(7) . . ? C104 Ru1 C101 61.67(7) . . ? C103 Ru1 C101 61.82(7) . . ? C102 Ru1 C101 36.36(7) . . ? C105 Ru1 C101 36.28(7) . . ? C12 Ru1 Cl1 91.36(7) . . ? C11 Ru1 Cl1 90.94(6) . . ? C104 Ru1 Cl1 146.16(6) . . ? C103 Ru1 Cl1 144.20(6) . . ? C102 Ru1 Cl1 106.55(6) . . ? C105 Ru1 Cl1 108.59(5) . . ? C101 Ru1 Cl1 90.15(5) . . ? O11 C11 Ru1 176.23(17) . . ? O12 C12 Ru1 175.51(19) . . ? C105 C101 C102 108.11(17) . . ? C105 C101 C106 126.16(18) . . ? C102 C101 C106 125.73(19) . . ? C105 C101 Ru1 69.92(10) . . ? C102 C101 Ru1 69.78(10) . . ? C106 C101 Ru1 125.82(13) . . ? C101 C102 C103 107.89(19) . . ? C101 C102 Ru1 73.86(10) . . ? C103 C102 Ru1 69.08(11) . . ? C101 C102 H102 126.1 . . ? C103 C102 H102 126.1 . . ? Ru1 C102 H102 122.7 . . ? C104 C103 C102 107.78(18) . . ? C104 C103 Ru1 71.18(12) . . ? C102 C103 Ru1 73.17(11) . . ? C104 C103 H103 126.1 . . ? C102 C103 H103 126.1 . . ? Ru1 C103 H103 121.3 . . ? C103 C104 C105 108.24(18) . . ? C103 C104 Ru1 71.30(11) . . ? C105 C104 Ru1 73.43(10) . . ? C103 C104 H104 125.9 . . ? C105 C104 H104 125.9 . . ? Ru1 C104 H104 121.1 . . ? C101 C105 C104 107.96(18) . . ? C101 C105 Ru1 73.80(10) . . ? C104 C105 Ru1 69.00(10) . . ? C101 C105 H105 126 . . ? C104 C105 H105 126 . . ? Ru1 C105 H105 122.8 . . ? C101 C106 H10A 109.5 . . ? C101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? #===END # Attachment 'web_deposit_cif_file_5_BrianSkelton_1302590078.cif' data_gk102 _database_code_depnum_ccdc_archive 'CCDC 821468' #TrackingRef 'web_deposit_cif_file_5_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-06T10:48:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H7 Br O2 Ru' _chemical_formula_sum 'C8 H7 Br O2 Ru' _chemical_formula_weight 316.12 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1076(11) _cell_length_b 6.8545(12) _cell_length_c 11.658(2) _cell_angle_alpha 80.201(2) _cell_angle_beta 82.342(3) _cell_angle_gamma 79.028(2) _cell_volume 469.57(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3685 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 2.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.77 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_unetI/netI 0.017 _diffrn_reflns_number 3685 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.98 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.903 _reflns_number_total 2252 _reflns_number_gt 2088 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule, except for the cp' ring, is rotationally disordered about the cp'(centroid)-Ru1 bond by approximately 120 degrees with occupancies of the major and minor components refined to 0.756(2) and its complement. Displacement parameters and geometries of the minor component were refined with restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.0638P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2252 _refine_ls_number_parameters 139 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.372 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.87963(3) 0.43460(2) 0.278017(15) 0.01854(9) Uani 1 1 d D . . C1 C 1.0896(4) 0.1928(4) 0.2753(2) 0.0282(5) Uani 1 1 d . . . O1 O 1.2211(3) 0.0505(3) 0.2727(2) 0.0478(6) Uani 1 1 d . . . C2 C 0.7060(9) 0.3144(8) 0.4066(5) 0.0303(11) Uani 0.7562(16) 1 d P . . O2 O 0.6004(10) 0.2384(9) 0.4836(4) 0.0501(16) Uani 0.7562(16) 1 d P . . Br1 Br 0.65157(9) 0.32732(8) 0.14470(5) 0.02467(16) Uani 0.7562(16) 1 d P . . C3 C 0.715(3) 0.348(3) 0.1741(15) 0.041(4) Uani 0.2438(16) 1 d PDU . . O3 O 0.605(2) 0.301(2) 0.1144(12) 0.038(3) Uani 0.2438(16) 1 d PDU . . Br2 Br 0.6421(3) 0.2680(3) 0.44503(17) 0.0287(5) Uani 0.2438(16) 1 d P . . C101 C 0.8677(4) 0.7435(3) 0.1654(2) 0.0223(4) Uani 1 1 d . . . C102 C 0.7568(4) 0.7656(3) 0.2791(2) 0.0243(5) Uani 1 1 d . . . H102 H 0.6034 0.8202 0.297 0.029 Uiso 1 1 calc R . . C103 C 0.9183(4) 0.6904(3) 0.3615(2) 0.0268(5) Uani 1 1 d . . . H103 H 0.8911 0.6887 0.4438 0.032 Uiso 1 1 calc R . . C104 C 1.1258(4) 0.6188(3) 0.2993(2) 0.0263(5) Uani 1 1 d . . . H104 H 1.2617 0.5607 0.3323 0.032 Uiso 1 1 calc R . . C105 C 1.0932(4) 0.6501(3) 0.1778(2) 0.0235(5) Uani 1 1 d . . . H105 H 1.2038 0.6145 0.116 0.028 Uiso 1 1 calc R . . C106 C 0.7649(5) 0.8102(4) 0.0524(2) 0.0315(5) Uani 1 1 d . . . H10A H 0.7894 0.9471 0.0206 0.047 Uiso 1 1 calc R . . H10B H 0.6035 0.8079 0.0663 0.047 Uiso 1 1 calc R . . H10C H 0.8345 0.7193 -0.0037 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01717(11) 0.01817(11) 0.01912(12) -0.00090(7) -0.00183(7) -0.00186(7) C1 0.0232(11) 0.0227(11) 0.0383(14) 0.0019(9) -0.0054(10) -0.0075(9) O1 0.0276(10) 0.0222(9) 0.0892(17) 0.0003(9) -0.0090(10) 0.0010(8) C2 0.034(3) 0.033(2) 0.024(3) 0.0006(19) -0.0025(19) -0.0096(18) O2 0.054(3) 0.067(3) 0.029(3) 0.006(2) 0.007(2) -0.0272(18) Br1 0.0238(4) 0.0271(2) 0.0255(4) -0.0069(2) -0.0041(2) -0.0067(2) C3 0.032(9) 0.034(7) 0.046(10) 0.008(7) 0.002(7) 0.003(6) O3 0.036(7) 0.037(6) 0.042(8) -0.012(5) -0.008(5) -0.004(4) Br2 0.0319(11) 0.0338(10) 0.0209(14) 0.0007(9) -0.0014(9) -0.0120(7) C101 0.0261(11) 0.0168(10) 0.0234(11) -0.0011(8) -0.0041(9) -0.0028(8) C102 0.0237(11) 0.0202(10) 0.0272(12) -0.0055(9) -0.0015(9) 0.0016(9) C103 0.0365(13) 0.0253(11) 0.0204(11) -0.0056(9) -0.0052(9) -0.0061(10) C104 0.0250(11) 0.0217(11) 0.0347(13) -0.0033(9) -0.0092(10) -0.0067(9) C105 0.0223(10) 0.0208(10) 0.0280(12) -0.0041(9) -0.0004(9) -0.0061(8) C106 0.0406(14) 0.0274(12) 0.0257(12) 0.0011(9) -0.0092(10) -0.0044(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 1.881(6) . ? Ru1 C1 1.895(2) . ? Ru1 C3 1.905(9) . ? Ru1 C104 2.201(2) . ? Ru1 C103 2.208(2) . ? Ru1 C105 2.234(2) . ? Ru1 C102 2.251(2) . ? Ru1 C101 2.288(2) . ? Ru1 Br1 2.5005(6) . ? Ru1 Br2 2.514(2) . ? C1 O1 1.142(3) . ? C2 O2 1.144(7) . ? C3 O3 1.149(12) . ? C101 C105 1.419(3) . ? C101 C102 1.424(3) . ? C101 C106 1.499(3) . ? C102 C103 1.433(3) . ? C102 H102 0.95 . ? C103 C104 1.419(3) . ? C103 H103 0.95 . ? C104 C105 1.430(3) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru1 C1 91.05(17) . . ? C2 Ru1 C3 89.9(6) . . ? C2 Ru1 C104 122.12(18) . . ? C1 Ru1 C104 95.23(9) . . ? C3 Ru1 C104 147.5(6) . . ? C2 Ru1 C103 95.61(17) . . ? C1 Ru1 C103 124.98(10) . . ? C3 Ru1 C103 145.1(6) . . ? C104 Ru1 C103 37.54(9) . . ? C2 Ru1 C105 157.71(17) . . ? C1 Ru1 C105 99.17(9) . . ? C3 Ru1 C105 109.9(6) . . ? C104 Ru1 C105 37.61(9) . . ? C103 Ru1 C105 62.32(9) . . ? C2 Ru1 C102 103.24(16) . . ? C1 Ru1 C102 157.56(9) . . ? C3 Ru1 C102 107.8(6) . . ? C104 Ru1 C102 62.55(9) . . ? C103 Ru1 C102 37.47(9) . . ? C105 Ru1 C102 61.73(8) . . ? C2 Ru1 C101 137.17(17) . . ? C1 Ru1 C101 131.76(9) . . ? C3 Ru1 C101 91.4(6) . . ? C104 Ru1 C101 61.94(8) . . ? C103 Ru1 C101 61.69(8) . . ? C105 Ru1 C101 36.56(8) . . ? C102 Ru1 C101 36.56(8) . . ? C2 Ru1 Br1 88.88(16) . . ? C1 Ru1 Br1 90.92(8) . . ? C104 Ru1 Br1 148.16(7) . . ? C103 Ru1 Br1 143.59(7) . . ? C105 Ru1 Br1 110.55(6) . . ? C102 Ru1 Br1 106.37(6) . . ? C101 Ru1 Br1 91.03(6) . . ? C1 Ru1 Br2 90.65(8) . . ? C3 Ru1 Br2 87.9(6) . . ? C104 Ru1 Br2 124.12(8) . . ? C103 Ru1 Br2 97.45(8) . . ? C105 Ru1 Br2 159.63(7) . . ? C102 Ru1 Br2 104.21(7) . . ? C101 Ru1 Br2 137.58(7) . . ? O1 C1 Ru1 177.9(2) . . ? O2 C2 Ru1 178.7(6) . . ? O3 C3 Ru1 176(2) . . ? C105 C101 C102 108.0(2) . . ? C105 C101 C106 126.1(2) . . ? C102 C101 C106 125.9(2) . . ? C105 C101 Ru1 69.64(12) . . ? C102 C101 Ru1 70.34(13) . . ? C106 C101 Ru1 126.32(16) . . ? C101 C102 C103 107.6(2) . . ? C101 C102 Ru1 73.11(12) . . ? C103 C102 Ru1 69.63(12) . . ? C101 C102 H102 126.2 . . ? C103 C102 H102 126.2 . . ? Ru1 C102 H102 122.7 . . ? C104 C103 C102 108.3(2) . . ? C104 C103 Ru1 70.95(12) . . ? C102 C103 Ru1 72.89(12) . . ? C104 C103 H103 125.8 . . ? C102 C103 H103 125.8 . . ? Ru1 C103 H103 122 . . ? C103 C104 C105 107.6(2) . . ? C103 C104 Ru1 71.51(13) . . ? C105 C104 Ru1 72.42(12) . . ? C103 C104 H104 126.2 . . ? C105 C104 H104 126.2 . . ? Ru1 C104 H104 121.6 . . ? C101 C105 C104 108.4(2) . . ? C101 C105 Ru1 73.79(13) . . ? C104 C105 Ru1 69.96(13) . . ? C101 C105 H105 125.8 . . ? C104 C105 H105 125.8 . . ? Ru1 C105 H105 122.1 . . ? C101 C106 H10A 109.5 . . ? C101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? #===END # Attachment 'web_deposit_cif_file_6_BrianSkelton_1302590078.cif' data_gk103 _database_code_depnum_ccdc_archive 'CCDC 821469' #TrackingRef 'web_deposit_cif_file_6_BrianSkelton_1302590078.cif' _audit_creation_date 2010-10-06T15:06:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H7 I O2 Ru' _chemical_formula_sum 'C8 H7 I O2 Ru' _chemical_formula_weight 363.11 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9642(13) _cell_length_b 7.4745(14) _cell_length_c 10.068(2) _cell_angle_alpha 92.968(3) _cell_angle_beta 95.936(3) _cell_angle_gamma 108.783(3) _cell_volume 491.49(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1968 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.4 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.89 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_av_unetI/netI 0.015 _diffrn_reflns_number 2679 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.86 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.879 _reflns_number_total 2270 _reflns_number_gt 1912 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.4204P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2270 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.1 _refine_ls_restrained_S_all 1.1 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.045 _refine_diff_density_min -1.445 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.47051(5) 0.27382(4) 0.26794(3) 0.01848(11) Uani 1 1 d . . . C11 C 0.6308(6) 0.1650(6) 0.1712(4) 0.0278(9) Uani 1 1 d . . . O11 O 0.7158(5) 0.0919(5) 0.1086(3) 0.0386(8) Uani 1 1 d . . . C12 C 0.5974(7) 0.2283(6) 0.4322(4) 0.0289(9) Uani 1 1 d . . . O12 O 0.6723(5) 0.1960(5) 0.5303(3) 0.0413(9) Uani 1 1 d . . . I1 I 0.75978(4) 0.62186(3) 0.29078(2) 0.02609(11) Uani 1 1 d . . . C101 C 0.2226(6) 0.3910(6) 0.1778(4) 0.0230(8) Uani 1 1 d . . . C102 C 0.2140(6) 0.2253(6) 0.0997(4) 0.0241(8) Uani 1 1 d . . . H102 H 0.2322 0.2173 0.0076 0.029 Uiso 1 1 calc R . . C103 C 0.1731(6) 0.0710(6) 0.1837(4) 0.0273(8) Uani 1 1 d . . . H103 H 0.1608 -0.0565 0.1573 0.033 Uiso 1 1 calc R . . C104 C 0.1541(6) 0.1431(6) 0.3134(4) 0.0277(9) Uani 1 1 d . . . H104 H 0.1239 0.0716 0.3884 0.033 Uiso 1 1 calc R . . C105 C 0.1882(6) 0.3409(6) 0.3110(4) 0.0240(8) Uani 1 1 d . . . H105 H 0.1881 0.4253 0.3849 0.029 Uiso 1 1 calc R . . C106 C 0.2554(7) 0.5824(6) 0.1274(5) 0.0315(9) Uani 1 1 d . . . H10A H 0.3223 0.5899 0.0459 0.047 Uiso 1 1 calc R . . H10B H 0.3421 0.6808 0.1963 0.047 Uiso 1 1 calc R . . H10C H 0.1232 0.6018 0.1072 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0183(2) 0.01581(17) 0.02009(17) 0.00218(12) 0.00065(13) 0.00432(15) C11 0.023(2) 0.026(2) 0.032(2) 0.0018(16) -0.0028(18) 0.0068(19) O11 0.0335(19) 0.0401(18) 0.0462(19) -0.0077(15) 0.0038(15) 0.0196(16) C12 0.029(2) 0.0213(19) 0.033(2) 0.0050(16) 0.0013(18) 0.0031(18) O12 0.044(2) 0.0346(17) 0.0382(18) 0.0097(14) -0.0126(16) 0.0080(17) I1 0.02391(19) 0.02215(16) 0.02643(17) 0.00356(11) 0.00271(12) -0.00045(13) C101 0.020(2) 0.0245(19) 0.0266(18) 0.0058(15) 0.0031(16) 0.0102(17) C102 0.020(2) 0.0273(19) 0.0230(18) -0.0009(15) -0.0015(16) 0.0069(18) C103 0.019(2) 0.0196(18) 0.039(2) -0.0021(16) -0.0002(17) 0.0025(17) C104 0.021(2) 0.025(2) 0.036(2) 0.0117(17) 0.0069(18) 0.0019(18) C105 0.023(2) 0.0243(19) 0.0249(19) 0.0019(15) 0.0044(16) 0.0070(17) C106 0.036(3) 0.023(2) 0.038(2) 0.0074(17) 0.003(2) 0.013(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C12 1.892(4) . ? Ru1 C11 1.893(4) . ? Ru1 C103 2.189(4) . ? Ru1 C104 2.211(4) . ? Ru1 C102 2.255(4) . ? Ru1 C105 2.257(4) . ? Ru1 C101 2.303(4) . ? Ru1 I1 2.7104(6) . ? C11 O11 1.138(5) . ? C12 O12 1.143(5) . ? C101 C102 1.413(5) . ? C101 C105 1.434(5) . ? C101 C106 1.499(5) . ? C102 C103 1.438(6) . ? C102 H102 0.95 . ? C103 C104 1.421(6) . ? C103 H103 0.95 . ? C104 C105 1.422(5) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? 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 C12 Ru1 C11 90.69(18) . . ? C12 Ru1 C103 118.34(17) . . ? C11 Ru1 C103 96.58(17) . . ? C12 Ru1 C104 95.42(18) . . ? C11 Ru1 C104 129.13(18) . . ? C103 Ru1 C104 37.69(16) . . ? C12 Ru1 C102 155.65(17) . . ? C11 Ru1 C102 96.20(16) . . ? C103 Ru1 C102 37.72(15) . . ? C104 Ru1 C102 62.30(15) . . ? C12 Ru1 C105 107.55(16) . . ? C11 Ru1 C105 156.73(17) . . ? C103 Ru1 C105 62.30(15) . . ? C104 Ru1 C105 37.11(14) . . ? C102 Ru1 C105 61.33(14) . . ? C12 Ru1 C101 142.89(17) . . ? C11 Ru1 C101 126.38(16) . . ? C103 Ru1 C101 61.81(14) . . ? C104 Ru1 C101 61.62(14) . . ? C102 Ru1 C101 36.11(14) . . ? C105 Ru1 C101 36.64(13) . . ? C12 Ru1 I1 88.08(13) . . ? C11 Ru1 I1 92.02(13) . . ? C103 Ru1 I1 151.95(11) . . ? C104 Ru1 I1 138.52(11) . . ? C102 Ru1 I1 114.88(10) . . ? C105 Ru1 I1 102.68(11) . . ? C101 Ru1 I1 91.73(10) . . ? O11 C11 Ru1 175.6(4) . . ? O12 C12 Ru1 178.2(4) . . ? C102 C101 C105 107.8(3) . . ? C102 C101 C106 125.4(4) . . ? C105 C101 C106 126.7(4) . . ? C102 C101 Ru1 70.1(2) . . ? C105 C101 Ru1 69.9(2) . . ? C106 C101 Ru1 126.9(3) . . ? C101 C102 C103 108.1(4) . . ? C101 C102 Ru1 73.8(2) . . ? C103 C102 Ru1 68.6(2) . . ? C101 C102 H102 125.9 . . ? C103 C102 H102 125.9 . . ? Ru1 C102 H102 123.3 . . ? C104 C103 C102 107.8(3) . . ? C104 C103 Ru1 72.0(2) . . ? C102 C103 Ru1 73.7(2) . . ? C104 C103 H103 126.1 . . ? C102 C103 H103 126.1 . . ? Ru1 C103 H103 120.1 . . ? C103 C104 C105 108.0(3) . . ? C103 C104 Ru1 70.3(2) . . ? C105 C104 Ru1 73.2(2) . . ? C103 C104 H104 126 . . ? C105 C104 H104 126 . . ? Ru1 C104 H104 122.2 . . ? C104 C105 C101 108.2(3) . . ? C104 C105 Ru1 69.7(2) . . ? C101 C105 Ru1 73.4(2) . . ? C104 C105 H105 125.9 . . ? C101 C105 H105 125.9 . . ? Ru1 C105 H105 122.6 . . ? C101 C106 H10A 109.5 . . ? C101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? C101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? #===END