Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'W Levason' _publ_contact_author_email WXL@SOTON.AC.UK _publ_section_title ; Synthesis, Chemistry and Structures of Complexes of the Dioxovanadium(V) Halides VO2F and VO2Cl ; loop_ _publ_author_name 'W Levason' 'Martin F. Davis' 'Marek Jura' 'Alethea Leung' 'Benjamin Littlefield' 'Gillian Reid' ; M.Webster ; # Attachment 'V_all5_2.cif' data_07mj002 _database_code_depnum_ccdc_archive 'CCDC 687015' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-05-15 _audit_author_name 'Webster, M.' _audit_update_record ; 2007-10-24 Added second lit. reference and CSD name. 2007-10-25 Set Z=2 and re-ran shelxl. New cif. ; _chemical_name_systematic ; bis((mu!2$-Oxo)-(2,2'-bipyridyl-N,N')-fluoro-oxo-vanadium(v)) ; # bis((mu!2$-Oxo)-(bipyridyl-N,N')-fluoro-oxo-vanadium(v)) CSD name. # Fluorodioxo(2,2'-bipyridyl)vanadium(V) # Treated as dimer (Z=2). # # See: # 1. A.J. Edwards, D.R. Slim, J.E. Guerchais & J. Sala-Pala, # J. Chem. Soc., Dalton, 1977, 984-986. (Refcode: OXFPYV10) for # report of same structure. [The unit cell used is different # but can be transformed into the cell in this cif. The CSD uses Z=2 (mw)]. # # 2. V.S. Sergienko, V.K. Borzunov, Kristallografiya(Russ.) # (Crystallogr.Rep.), 39, 1123, 1994. (Refcode: OXFPYV11). # # For both structure determinations data were recorded at room temperature. _chemical_name_common bis((mu!2$-Oxo)-(2,2'-bipyridyl-N,N')-fluoro-oxo-vanadium(v)) _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 F2 N4 O4 V2' _chemical_formula_sum 'C20 H16 F2 N4 O4 V2' _chemical_formula_weight 516.25 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2'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 6.3764(15) _cell_length_b 15.828(3) _cell_length_c 10.287(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.869(10) _cell_angle_gamma 90.00 _cell_volume 988.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2314 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8718 # 0.9152 _exptl_absorpt_correction_T_max 1.0000 # 0.9516 _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_% 0 _diffrn_reflns_number 11803 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2270 _reflns_number_gt 1852 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _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^+4.2460P] 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 2270 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 V1 V 0.38199(10) 0.47255(4) 0.84866(6) 0.01747(17) Uani 1 1 d . . . F1 F 0.5923(4) 0.39647(13) 0.8433(2) 0.0269(5) Uani 1 1 d . . . O1 O 0.1715(4) 0.43850(16) 0.7271(3) 0.0235(6) Uani 1 1 d . . . O2 O 0.3323(4) 0.45183(15) 0.9967(2) 0.0202(5) Uani 1 1 d . . . N1 N 0.2311(5) 0.59431(17) 0.8361(3) 0.0164(6) Uani 1 1 d . . . N2 N 0.5212(5) 0.55115(18) 0.7191(3) 0.0178(6) Uani 1 1 d . . . C1 C 0.0803(6) 0.6102(2) 0.9000(4) 0.0194(7) Uani 1 1 d . . . H1 H 0.0430 0.5666 0.9524 0.023 Uiso 1 1 calc R . . C2 C -0.0225(6) 0.6876(2) 0.8923(4) 0.0218(7) Uani 1 1 d . . . H2 H -0.1304 0.6966 0.9372 0.026 Uiso 1 1 calc R . . C3 C 0.0339(6) 0.7519(2) 0.8185(4) 0.0247(8) Uani 1 1 d . . . H3 H -0.0318 0.8061 0.8139 0.030 Uiso 1 1 calc R . . C4 C 0.1882(6) 0.7360(2) 0.7509(4) 0.0232(8) Uani 1 1 d . . . H4 H 0.2289 0.7791 0.6991 0.028 Uiso 1 1 calc R . . C5 C 0.2818(5) 0.6562(2) 0.7601(3) 0.0176(7) Uani 1 1 d . . . C6 C 0.4413(6) 0.6302(2) 0.6892(3) 0.0191(7) Uani 1 1 d . . . C7 C 0.5023(6) 0.6812(3) 0.5970(4) 0.0259(8) Uani 1 1 d . . . H7 H 0.4433 0.7365 0.5765 0.031 Uiso 1 1 calc R . . C8 C 0.6512(6) 0.6496(3) 0.5354(4) 0.0293(9) Uani 1 1 d . . . H8 H 0.6910 0.6822 0.4691 0.035 Uiso 1 1 calc R . . C9 C 0.7416(6) 0.5703(3) 0.5711(4) 0.0287(9) Uani 1 1 d . . . H9 H 0.8487 0.5487 0.5328 0.034 Uiso 1 1 calc R . . C10 C 0.6728(6) 0.5230(2) 0.6636(3) 0.0217(7) Uani 1 1 d . . . H10 H 0.7353 0.4687 0.6887 0.026 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 V1 0.0222(3) 0.0134(3) 0.0174(3) 0.0010(2) 0.0069(2) 0.0022(2) F1 0.0333(12) 0.0224(11) 0.0262(11) -0.0001(9) 0.0107(10) 0.0095(9) O1 0.0242(13) 0.0167(12) 0.0295(14) -0.0029(10) 0.0082(11) -0.0035(10) O2 0.0229(13) 0.0166(12) 0.0218(12) 0.0027(10) 0.0081(10) 0.0020(10) N1 0.0183(14) 0.0146(14) 0.0151(13) 0.0024(11) 0.0035(11) 0.0020(11) N2 0.0173(14) 0.0194(15) 0.0151(14) -0.0006(11) 0.0024(11) -0.0016(11) C1 0.0182(17) 0.0179(17) 0.0214(17) -0.0004(14) 0.0049(14) 0.0008(13) C2 0.0196(18) 0.0177(17) 0.0270(19) -0.0051(14) 0.0054(15) 0.0029(14) C3 0.0244(19) 0.0167(17) 0.0278(19) -0.0009(15) 0.0002(15) 0.0058(14) C4 0.0265(19) 0.0161(17) 0.0245(18) 0.0034(14) 0.0041(15) -0.0025(14) C5 0.0160(16) 0.0173(16) 0.0156(15) 0.0015(13) -0.0009(13) -0.0023(13) C6 0.0163(17) 0.0216(18) 0.0171(16) 0.0004(13) 0.0017(13) -0.0047(13) C7 0.0219(19) 0.0265(19) 0.0270(19) 0.0062(16) 0.0042(15) -0.0056(15) C8 0.025(2) 0.041(2) 0.0235(19) 0.0030(17) 0.0089(16) -0.0115(17) C9 0.0225(19) 0.043(2) 0.0226(19) -0.0065(17) 0.0097(16) -0.0071(17) C10 0.0190(17) 0.0262(19) 0.0201(17) -0.0064(15) 0.0061(14) -0.0037(14) _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 V1 O1 1.621(3) . ? V1 O2 1.680(2) . ? V1 F1 1.816(2) . ? V1 N1 2.140(3) . ? V1 N2 2.200(3) . ? V1 O2 2.346(3) 3_667 ? O2 V1 2.346(3) 3_667 ? N1 C1 1.345(4) . ? N1 C5 1.353(4) . ? N2 C10 1.341(4) . ? N2 C6 1.351(5) . ? C1 C2 1.380(5) . ? C1 H1 0.9500 . ? C2 C3 1.382(5) . ? C2 H2 0.9500 . ? C3 C4 1.391(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.480(5) . ? C6 C7 1.388(5) . ? C7 C8 1.387(6) . ? C7 H7 0.9500 . ? C8 C9 1.383(6) . ? C8 H8 0.9500 . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 O1 V1 O2 107.02(13) . . ? O1 V1 F1 101.56(12) . . ? O2 V1 F1 104.15(11) . . ? O1 V1 N1 90.13(12) . . ? O2 V1 N1 91.40(11) . . ? F1 V1 N1 156.62(11) . . ? O1 V1 N2 96.49(12) . . ? O2 V1 N2 152.01(12) . . ? F1 V1 N2 85.27(11) . . ? N1 V1 N2 73.23(11) . . ? O1 V1 O2 168.51(11) . 3_667 ? O2 V1 O2 78.94(11) . 3_667 ? F1 V1 O2 86.10(10) . 3_667 ? N1 V1 O2 79.79(10) . 3_667 ? N2 V1 O2 75.43(9) . 3_667 ? V1 O2 V1 101.06(11) . 3_667 ? C1 N1 C5 118.7(3) . . ? C1 N1 V1 121.0(2) . . ? C5 N1 V1 120.3(2) . . ? C10 N2 C6 118.8(3) . . ? C10 N2 V1 123.3(2) . . ? C6 N2 V1 117.9(2) . . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.1(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 114.0(3) . . ? C4 C5 C6 124.4(3) . . ? N2 C6 C7 121.9(3) . . ? N2 C6 C5 114.4(3) . . ? C7 C6 C5 123.7(3) . . ? C8 C7 C6 118.5(4) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 118.6(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C9 122.4(4) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.724 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.102 #===END OF CIF ============================================================== # 07mfd024 CCDC refcode: 687016 data_07mfd024 _database_code_depnum_ccdc_archive 'CCDC 687016' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-10-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dioxidofluoridobis(pyridine)vanadium(V) ; _chemical_name_common Dioxidofluoridobis(pyridine)vanadium(V) _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 F N2 O2 V' _chemical_formula_sum 'C10 H10 F N2 O2 V' _chemical_formula_weight 260.14 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.991(3) _cell_length_b 10.844(3) _cell_length_c 8.186(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.703(10) _cell_angle_gamma 90.00 _cell_volume 1054.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6526 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8993 # 0.8060 _exptl_absorpt_correction_T_max 1.0000 # 0.9724 _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_% 0 _diffrn_reflns_number 5449 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.59 _reflns_number_total 1205 _reflns_number_gt 1163 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _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^)+(0.0247P)^2^+1.3934P] 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 1205 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 V1 V 0.0000 0.64311(3) 0.2500 0.01344(11) Uani 1 2 d S . . F1 F 0.0000 0.47299(10) 0.2500 0.0225(3) Uani 1 2 d S . . O1 O -0.04554(8) 0.72824(10) 0.09144(13) 0.0228(2) Uani 1 1 d . . . N1 N 0.16643(9) 0.62256(10) 0.18463(13) 0.0141(2) Uani 1 1 d . . . C1 C 0.19798(11) 0.52330(12) 0.10370(16) 0.0157(3) Uani 1 1 d . . . H1 H 0.1457 0.4580 0.0778 0.019 Uiso 1 1 calc R . . C2 C 0.30481(11) 0.51340(12) 0.05680(16) 0.0185(3) Uani 1 1 d . . . H2 H 0.3253 0.4421 0.0003 0.022 Uiso 1 1 calc R . . C3 C 0.38112(11) 0.60864(13) 0.09333(16) 0.0186(3) Uani 1 1 d . . . H3 H 0.4544 0.6037 0.0618 0.022 Uiso 1 1 calc R . . C4 C 0.34878(11) 0.71149(12) 0.17680(17) 0.0182(3) Uani 1 1 d . . . H4 H 0.3994 0.7782 0.2034 0.022 Uiso 1 1 calc R . . C5 C 0.24114(11) 0.71448(12) 0.22020(16) 0.0166(3) Uani 1 1 d . . . H5 H 0.2190 0.7846 0.2777 0.020 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 V1 0.01193(17) 0.01161(17) 0.01712(17) 0.000 0.00322(11) 0.000 F1 0.0178(5) 0.0126(5) 0.0392(7) 0.000 0.0118(5) 0.000 O1 0.0168(5) 0.0264(5) 0.0262(5) 0.0101(4) 0.0067(4) 0.0039(4) N1 0.0126(5) 0.0142(5) 0.0157(5) 0.0005(4) 0.0021(4) -0.0001(4) C1 0.0159(6) 0.0135(6) 0.0178(6) -0.0003(5) 0.0025(5) -0.0012(5) C2 0.0189(6) 0.0173(6) 0.0201(6) -0.0003(5) 0.0057(5) 0.0025(5) C3 0.0136(6) 0.0223(7) 0.0203(6) 0.0037(5) 0.0042(5) 0.0014(5) C4 0.0144(6) 0.0174(6) 0.0221(6) 0.0014(5) 0.0007(5) -0.0031(5) C5 0.0164(6) 0.0136(6) 0.0197(6) -0.0013(5) 0.0019(5) -0.0006(5) _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 V1 O1 1.6264(10) 2 ? V1 O1 1.6264(10) . ? V1 F1 1.8448(12) . ? V1 N1 2.1460(11) 2 ? V1 N1 2.1460(11) . ? N1 C1 1.3446(17) . ? N1 C5 1.3457(17) . ? C1 C2 1.3898(18) . ? C1 H1 0.9500 . ? C2 C3 1.386(2) . ? C2 H2 0.9500 . ? C3 C4 1.3900(19) . ? C3 H3 0.9500 . ? C4 C5 1.3843(19) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? 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 O1 V1 O1 110.83(8) 2 . ? O1 V1 F1 124.58(4) 2 . ? O1 V1 F1 124.58(4) . . ? O1 V1 N1 94.81(5) 2 2 ? O1 V1 N1 91.95(5) . 2 ? F1 V1 N1 84.04(3) . 2 ? O1 V1 N1 91.95(5) 2 . ? O1 V1 N1 94.81(5) . . ? F1 V1 N1 84.04(3) . . ? N1 V1 N1 168.08(6) 2 . ? C1 N1 C5 118.46(11) . . ? C1 N1 V1 122.58(9) . . ? C5 N1 V1 118.91(9) . . ? N1 C1 C2 121.91(12) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.29(12) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.98(12) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.43(12) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 122.93(12) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.308 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.050 #===END OF CIF ============================================================== # 08mj21 CCDC refcode: 687017 data_08mj21 _database_code_depnum_ccdc_archive 'CCDC 687017' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-04-19 _audit_author_name 'Webster, M.' _chemical_name_systematic ; chlorodioxobis(pyridine)vanadium(V) ; # chlorido-dioxidobis(pyridine)vanadium(V) # See: M. Motovalli, D. Shah, S.A.A. Shah, A.C. Sullivan, Polyhedron, # 15, 1996, 2387-2395. CDS refcode: TIMJUU01. This is described # as green crystals and the structure was determined at room temp. # There is also a polymorph (TIMJUU). _chemical_name_common chlorodioxobis(pyridine)vanadium(V) _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Cl N2 O2 V' _chemical_formula_sum 'C10 H10 Cl N2 O2 V' _chemical_formula_weight 276.59 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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 5.9806(10) _cell_length_b 7.3517(10) _cell_length_c 25.960(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.454(10) _cell_angle_gamma 90.00 _cell_volume 1139.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11795 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8045 # 0.5998 # _exptl_absorpt_correction_T_max 1.0000 # 0.7456 # _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 ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15379 _diffrn_reflns_av_R_equivalents 0.1084 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2615 _reflns_number_gt 1770 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _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^)+(0.0250P)^2^+1.1901P] 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 2615 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 V1 V 0.77180(10) 0.15702(8) 0.12554(2) 0.02104(18) Uani 1 1 d . . . Cl1 Cl 0.94730(16) 0.43757(11) 0.11880(3) 0.0279(2) Uani 1 1 d . . . O1 O 0.8957(4) -0.0302(3) 0.11065(9) 0.0294(6) Uani 1 1 d . . . O2 O 0.5253(4) 0.1145(4) 0.14492(9) 0.0328(6) Uani 1 1 d . . . N1 N 0.6377(5) 0.2112(4) 0.04899(10) 0.0217(6) Uani 1 1 d . . . N2 N 0.9130(4) 0.1556(4) 0.20335(10) 0.0205(6) Uani 1 1 d . . . C1 C 0.4290(6) 0.2753(5) 0.03980(13) 0.0251(8) Uani 1 1 d . . . H1 H 0.3394 0.2983 0.0681 0.030 Uiso 1 1 calc R . . C2 C 0.3410(6) 0.3089(5) -0.00975(13) 0.0274(8) Uani 1 1 d . . . H2 H 0.1935 0.3558 -0.0153 0.033 Uiso 1 1 calc R . . C3 C 0.4688(6) 0.2737(5) -0.05110(14) 0.0290(9) Uani 1 1 d . . . H3 H 0.4098 0.2942 -0.0854 0.035 Uiso 1 1 calc R . . C4 C 0.6829(7) 0.2086(5) -0.04189(13) 0.0309(9) Uani 1 1 d . . . H4 H 0.7747 0.1844 -0.0697 0.037 Uiso 1 1 calc R . . C5 C 0.7620(6) 0.1791(5) 0.00843(12) 0.0258(8) Uani 1 1 d . . . H5 H 0.9102 0.1343 0.0147 0.031 Uiso 1 1 calc R . . C6 C 0.7972(6) 0.2217(5) 0.24199(12) 0.0237(8) Uani 1 1 d . . . H6 H 0.6542 0.2742 0.2340 0.028 Uiso 1 1 calc R . . C7 C 0.8787(6) 0.2162(5) 0.29297(13) 0.0260(8) Uani 1 1 d . . . H7 H 0.7932 0.2644 0.3195 0.031 Uiso 1 1 calc R . . C8 C 1.0869(6) 0.1394(5) 0.30477(13) 0.0280(8) Uani 1 1 d . . . H8 H 1.1462 0.1335 0.3395 0.034 Uiso 1 1 calc R . . C9 C 1.2068(6) 0.0716(5) 0.26525(13) 0.0266(8) Uani 1 1 d . . . H9 H 1.3499 0.0182 0.2724 0.032 Uiso 1 1 calc R . . C10 C 1.1155(6) 0.0827(5) 0.21506(13) 0.0244(8) Uani 1 1 d . . . H10 H 1.1992 0.0369 0.1879 0.029 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 V1 0.0204(3) 0.0249(3) 0.0176(3) 0.0015(2) -0.0003(2) -0.0014(3) Cl1 0.0342(5) 0.0253(4) 0.0235(4) 0.0011(4) -0.0059(4) -0.0054(4) O1 0.0367(15) 0.0231(13) 0.0274(13) -0.0014(11) -0.0063(11) 0.0028(11) O2 0.0208(14) 0.0536(17) 0.0238(13) 0.0079(12) 0.0006(11) -0.0068(12) N1 0.0193(15) 0.0242(15) 0.0212(14) 0.0007(12) -0.0026(12) -0.0018(12) N2 0.0189(15) 0.0232(14) 0.0196(14) 0.0029(12) 0.0014(11) -0.0024(13) C1 0.0204(19) 0.0274(18) 0.0279(18) -0.0004(15) 0.0031(15) -0.0039(15) C2 0.023(2) 0.031(2) 0.0277(19) 0.0041(16) -0.0075(16) -0.0049(16) C3 0.035(2) 0.0276(19) 0.0232(18) 0.0021(15) -0.0060(16) -0.0080(17) C4 0.042(2) 0.029(2) 0.0223(18) -0.0041(16) 0.0058(17) -0.0010(18) C5 0.027(2) 0.028(2) 0.0223(18) -0.0028(15) 0.0021(15) 0.0020(16) C6 0.0191(18) 0.0273(18) 0.0249(18) -0.0011(15) 0.0018(14) 0.0033(15) C7 0.034(2) 0.0243(18) 0.0198(17) -0.0029(15) 0.0043(15) 0.0003(16) C8 0.033(2) 0.0295(19) 0.0211(17) -0.0003(16) -0.0033(15) 0.0030(17) C9 0.0230(19) 0.032(2) 0.0239(18) 0.0021(15) -0.0014(15) 0.0004(16) C10 0.023(2) 0.0275(18) 0.0228(17) -0.0002(15) 0.0022(14) -0.0011(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 V1 O2 1.617(2) . ? V1 O1 1.621(2) . ? V1 N1 2.135(3) . ? V1 N2 2.142(3) . ? V1 Cl1 2.3256(10) . ? N1 C1 1.342(4) . ? N1 C5 1.346(4) . ? N2 C10 1.342(4) . ? N2 C6 1.344(4) . ? C1 C2 1.382(5) . ? C1 H1 0.9500 . ? C2 C3 1.379(5) . ? C2 H2 0.9500 . ? C3 C4 1.374(5) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.383(5) . ? C6 H6 0.9500 . ? C7 C8 1.385(5) . ? C7 H7 0.9500 . ? C8 C9 1.380(5) . ? C8 H8 0.9500 . ? C9 C10 1.384(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 O2 V1 O1 110.40(14) . . ? O2 V1 N1 91.56(12) . . ? O1 V1 N1 95.06(11) . . ? O2 V1 N2 91.18(11) . . ? O1 V1 N2 93.48(11) . . ? N1 V1 N2 169.50(11) . . ? O2 V1 Cl1 128.26(11) . . ? O1 V1 Cl1 121.34(10) . . ? N1 V1 Cl1 84.86(8) . . ? N2 V1 Cl1 85.48(8) . . ? C1 N1 C5 118.3(3) . . ? C1 N1 V1 121.6(2) . . ? C5 N1 V1 120.0(2) . . ? C10 N2 C6 118.3(3) . . ? C10 N2 V1 121.0(2) . . ? C6 N2 V1 120.7(2) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 118.9(3) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.6(3) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? N2 C6 C7 122.4(3) . . ? N2 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C6 C7 C8 118.9(3) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 118.9(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 119.0(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 122.4(3) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? 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 O2 V1 N1 C1 28.7(3) . . . . ? O1 V1 N1 C1 139.3(3) . . . . ? N2 V1 N1 C1 -76.4(7) . . . . ? Cl1 V1 N1 C1 -99.6(3) . . . . ? O2 V1 N1 C5 -150.5(3) . . . . ? O1 V1 N1 C5 -39.9(3) . . . . ? N2 V1 N1 C5 104.4(6) . . . . ? Cl1 V1 N1 C5 81.2(2) . . . . ? O2 V1 N2 C10 141.3(3) . . . . ? O1 V1 N2 C10 30.7(3) . . . . ? N1 V1 N2 C10 -113.6(6) . . . . ? Cl1 V1 N2 C10 -90.5(2) . . . . ? O2 V1 N2 C6 -36.2(3) . . . . ? O1 V1 N2 C6 -146.8(3) . . . . ? N1 V1 N2 C6 68.9(7) . . . . ? Cl1 V1 N2 C6 92.0(3) . . . . ? C5 N1 C1 C2 -0.2(5) . . . . ? V1 N1 C1 C2 -179.4(3) . . . . ? N1 C1 C2 C3 0.8(5) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C1 N1 C5 C4 -0.3(5) . . . . ? V1 N1 C5 C4 178.9(3) . . . . ? C3 C4 C5 N1 0.1(5) . . . . ? C10 N2 C6 C7 -0.4(5) . . . . ? V1 N2 C6 C7 177.2(3) . . . . ? N2 C6 C7 C8 -0.2(5) . . . . ? C6 C7 C8 C9 0.3(5) . . . . ? C7 C8 C9 C10 0.1(5) . . . . ? C6 N2 C10 C9 0.8(5) . . . . ? V1 N2 C10 C9 -176.8(3) . . . . ? C8 C9 C10 N2 -0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.371 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.099 #===END OF CIF ============================================================== # 08mj023 CCDC refcode: 687018 data_08mj23 _database_code_depnum_ccdc_archive 'CCDC 687018' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-04-27 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Chloridodioxidobis(pyridine N-oxide)vanadium(V) ; _chemical_name_common 'Chloridodioxidobis(pyridine N-oxide)vanadium(V)' _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Cl N2 O4 V' _chemical_formula_sum 'C10 H10 Cl N2 O4 V' _chemical_formula_weight 308.59 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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 8.0165(15) _cell_length_b 5.8756(10) _cell_length_c 25.701(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.897(10) _cell_angle_gamma 90.00 _cell_volume 1209.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23019 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8411 # 0.8503 _exptl_absorpt_correction_T_max 1.0000 # 0.9398 _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 11672 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.52 _reflns_number_total 2774 _reflns_number_gt 2224 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _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^)+(0.0222P)^2^+3.8931P] 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 2774 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 V1 V 0.09644(6) 0.85895(10) 0.13812(2) 0.01563(15) Uani 1 1 d . . . Cl1 Cl 0.37132(9) 0.95029(15) 0.11448(3) 0.02034(19) Uani 1 1 d . . . O1 O 0.0568(3) 0.8154(4) 0.06070(8) 0.0206(5) Uani 1 1 d . . . O2 O 0.1828(3) 0.9894(4) 0.20629(8) 0.0187(5) Uani 1 1 d . . . O3 O -0.0782(3) 1.0005(4) 0.13893(8) 0.0213(5) Uani 1 1 d . . . O4 O 0.0622(3) 0.6010(4) 0.15741(9) 0.0241(5) Uani 1 1 d . . . N1 N 0.1480(3) 0.6819(5) 0.02968(10) 0.0172(6) Uani 1 1 d . . . N2 N 0.0672(3) 1.0288(5) 0.24282(9) 0.0160(5) Uani 1 1 d . . . C1 C 0.1568(4) 0.7480(6) -0.02055(12) 0.0207(7) Uani 1 1 d . . . H1 H 0.1078 0.8876 -0.0317 0.025 Uiso 1 1 calc R . . C2 C 0.2369(4) 0.6126(6) -0.05531(13) 0.0247(8) Uani 1 1 d . . . H2 H 0.2422 0.6578 -0.0907 0.030 Uiso 1 1 calc R . . C3 C 0.3103(4) 0.4094(6) -0.03890(13) 0.0245(8) Uani 1 1 d . . . H3 H 0.3662 0.3146 -0.0627 0.029 Uiso 1 1 calc R . . C4 C 0.3002(4) 0.3488(6) 0.01256(13) 0.0229(7) Uani 1 1 d . . . H4 H 0.3504 0.2112 0.0246 0.027 Uiso 1 1 calc R . . C5 C 0.2177(4) 0.4861(6) 0.04697(13) 0.0215(7) Uani 1 1 d . . . H5 H 0.2102 0.4430 0.0824 0.026 Uiso 1 1 calc R . . C6 C -0.0169(4) 1.2272(6) 0.24144(12) 0.0188(7) Uani 1 1 d . . . H6 H 0.0021 1.3357 0.2149 0.023 Uiso 1 1 calc R . . C7 C -0.1310(4) 1.2703(6) 0.27912(12) 0.0185(7) Uani 1 1 d . . . H7 H -0.1912 1.4096 0.2787 0.022 Uiso 1 1 calc R . . C8 C -0.1581(4) 1.1111(6) 0.31770(12) 0.0193(7) Uani 1 1 d . . . H8 H -0.2374 1.1394 0.3436 0.023 Uiso 1 1 calc R . . C9 C -0.0678(4) 0.9099(6) 0.31794(12) 0.0208(7) Uani 1 1 d . . . H9 H -0.0850 0.7988 0.3441 0.025 Uiso 1 1 calc R . . C10 C 0.0472(4) 0.8714(6) 0.28013(12) 0.0185(7) Uani 1 1 d . . . H10 H 0.1114 0.7355 0.2804 0.022 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 V1 0.0165(3) 0.0179(3) 0.0125(3) 0.0008(2) 0.00118(19) -0.0013(2) Cl1 0.0177(4) 0.0258(4) 0.0177(4) -0.0004(3) 0.0021(3) -0.0025(3) O1 0.0215(11) 0.0264(14) 0.0137(11) -0.0033(10) 0.0005(9) 0.0061(10) O2 0.0176(11) 0.0244(13) 0.0143(11) -0.0032(9) 0.0031(8) 0.0002(10) O3 0.0190(11) 0.0280(14) 0.0169(11) -0.0023(10) -0.0002(9) 0.0026(10) O4 0.0307(13) 0.0214(13) 0.0203(12) 0.0025(10) 0.0025(10) -0.0051(10) N1 0.0172(13) 0.0194(15) 0.0149(12) -0.0029(11) -0.0007(10) 0.0013(11) N2 0.0154(12) 0.0225(15) 0.0102(12) -0.0010(11) 0.0005(9) -0.0014(11) C1 0.0210(16) 0.0229(18) 0.0183(15) 0.0033(14) 0.0020(12) 0.0002(14) C2 0.0267(17) 0.032(2) 0.0161(16) 0.0001(14) 0.0028(13) 0.0017(15) C3 0.0236(17) 0.028(2) 0.0217(17) -0.0059(14) 0.0011(13) 0.0023(15) C4 0.0265(17) 0.0191(18) 0.0227(17) -0.0006(14) -0.0031(13) 0.0036(15) C5 0.0233(16) 0.0232(18) 0.0178(16) 0.0006(13) -0.0026(12) -0.0009(14) C6 0.0211(15) 0.0192(17) 0.0162(15) 0.0009(13) -0.0012(12) -0.0033(13) C7 0.0187(15) 0.0167(17) 0.0198(15) -0.0026(13) -0.0036(12) 0.0052(13) C8 0.0179(15) 0.0283(19) 0.0117(14) -0.0008(13) -0.0010(11) 0.0021(14) C9 0.0219(16) 0.0250(19) 0.0158(15) 0.0051(13) 0.0041(12) 0.0018(14) C10 0.0191(15) 0.0198(17) 0.0164(15) 0.0012(13) -0.0015(12) 0.0022(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 V1 O4 1.621(2) . ? V1 O3 1.629(2) . ? V1 O2 2.014(2) . ? V1 O1 2.021(2) . ? V1 Cl1 2.3668(10) . ? O1 N1 1.351(3) . ? O2 N2 1.361(3) . ? N1 C5 1.348(4) . ? N1 C1 1.352(4) . ? N2 C10 1.346(4) . ? N2 C6 1.346(4) . ? C1 C2 1.371(5) . ? C1 H1 0.9500 . ? C2 C3 1.391(5) . ? C2 H2 0.9500 . ? C3 C4 1.375(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.377(4) . ? C6 H6 0.9500 . ? C7 C8 1.386(5) . ? C7 H7 0.9500 . ? C8 C9 1.386(5) . ? C8 H8 0.9500 . ? C9 C10 1.379(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 O4 V1 O3 108.60(13) . . ? O4 V1 O2 98.43(11) . . ? O3 V1 O2 93.76(10) . . ? O4 V1 O1 99.21(11) . . ? O3 V1 O1 88.28(10) . . ? O2 V1 O1 160.57(10) . . ? O4 V1 Cl1 117.33(9) . . ? O3 V1 Cl1 134.06(9) . . ? O2 V1 Cl1 80.83(7) . . ? O1 V1 Cl1 83.89(7) . . ? N1 O1 V1 125.73(18) . . ? N2 O2 V1 116.25(17) . . ? C5 N1 C1 121.7(3) . . ? C5 N1 O1 121.8(3) . . ? C1 N1 O1 116.3(3) . . ? C10 N2 C6 122.8(3) . . ? C10 N2 O2 118.3(3) . . ? C6 N2 O2 118.8(3) . . ? N1 C1 C2 119.7(3) . . ? N1 C1 H1 120.1 . . ? C2 C1 H1 120.1 . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 118.4(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 119.3(3) . . ? N1 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N2 C6 C7 119.0(3) . . ? N2 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C8 120.2(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 119.2(3) . . ? N2 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? 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 N1 O1 V1 Cl1 53.1(2) . . . . ? N2 O2 V1 Cl1 169.4(2) . . . . ? V1 O1 N1 C1 -150.5(2) . . . . ? V1 O2 N2 C6 -85.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.466 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.101 #===END OF CIF ============================================================== # 08mj025 CCDC refcode: 687019 data_08mj25 _database_code_depnum_ccdc_archive 'CCDC 687019' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-04-29 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dioxotris(triphenylphosphine oxide-O)vanadium(V) dichlorodioxovanadate ; _chemical_name_common ;Dioxotris(triphenylphosphine oxide-O)vanadium(V) dichlorodioxovanadate ; _chemical_melting_point ? _chemical_formula_moiety 'C54 H45 O5 P3 V 1+, Cl2 O2 V 1-' _chemical_formula_sum 'C54 H45 Cl2 O7 P3 V2' _chemical_formula_structural '((C18 H15 O P)3 O2 V) (Cl2 O2 V)' _chemical_formula_weight 1071.59 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' P P 0.1023 0.0942 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.431(4) _cell_length_b 14.080(4) _cell_length_c 14.558(4) _cell_angle_alpha 94.45(2) _cell_angle_beta 94.367(15) _cell_angle_gamma 97.27(2) _cell_volume 2510.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 80284 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8208 # 0.6120 scaled to Tmax=1.0 _exptl_absorpt_correction_T_max 1.0000 # 0.7456 " " _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 ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29767 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 27.61 _reflns_number_total 11001 _reflns_number_gt 8449 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _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^)+(0.1038P)^2^+5.7632P] 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 11001 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2089 _refine_ls_wR_factor_gt 0.1919 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 V1 V 0.55179(5) 0.38377(5) 0.23305(4) 0.01679(17) Uani 1 1 d . . . V2 V 0.97902(6) 0.84860(6) 0.25070(5) 0.0283(2) Uani 1 1 d . . . P1 P 0.75588(8) 0.25370(7) 0.27318(7) 0.0185(2) Uani 1 1 d . . . P2 P 0.38741(8) 0.53717(7) 0.17985(7) 0.0174(2) Uani 1 1 d . . . P3 P 0.36007(8) 0.18934(7) 0.25358(7) 0.0181(2) Uani 1 1 d . . . Cl1 Cl 0.97421(10) 0.98846(9) 0.33170(8) 0.0359(3) Uani 1 1 d . . . Cl2 Cl 1.15156(11) 0.83143(9) 0.22675(9) 0.0401(3) Uani 1 1 d . . . O1 O 0.6477(2) 0.2907(2) 0.28289(19) 0.0213(6) Uani 1 1 d . . . O2 O 0.4187(2) 0.43599(19) 0.17849(19) 0.0203(6) Uani 1 1 d . . . O3 O 0.4410(2) 0.2650(2) 0.22036(19) 0.0216(6) Uani 1 1 d . . . O4 O 0.5765(2) 0.4610(2) 0.32309(19) 0.0235(6) Uani 1 1 d . . . O5 O 0.6287(2) 0.4195(2) 0.15530(19) 0.0244(6) Uani 1 1 d . . . O6 O 0.9244(3) 0.7623(3) 0.3057(2) 0.0397(8) Uani 1 1 d . . . O7 O 0.9085(3) 0.8478(3) 0.1529(2) 0.0438(9) Uani 1 1 d . . . C1 C 0.8671(3) 0.3494(3) 0.2794(3) 0.0209(8) Uani 1 1 d . . . C2 C 0.9694(3) 0.3302(3) 0.2572(3) 0.0271(9) Uani 1 1 d . . . H2 H 0.9802 0.2671 0.2350 0.033 Uiso 1 1 calc R . . C3 C 1.0570(4) 0.4052(4) 0.2678(3) 0.0334(10) Uani 1 1 d . . . H3 H 1.1276 0.3925 0.2542 0.040 Uiso 1 1 calc R . . C4 C 1.0403(4) 0.4969(4) 0.2979(3) 0.0331(10) Uani 1 1 d . . . H4 H 1.0997 0.5472 0.3050 0.040 Uiso 1 1 calc R . . C5 C 0.9373(4) 0.5165(3) 0.3180(3) 0.0339(10) Uani 1 1 d . . . H5 H 0.9263 0.5803 0.3374 0.041 Uiso 1 1 calc R . . C6 C 0.8510(4) 0.4434(3) 0.3096(3) 0.0266(9) Uani 1 1 d . . . H6 H 0.7809 0.4566 0.3243 0.032 Uiso 1 1 calc R . . C7 C 0.7795(3) 0.1807(3) 0.3661(3) 0.0207(8) Uani 1 1 d . . . C8 C 0.8700(3) 0.2025(3) 0.4305(3) 0.0260(9) Uani 1 1 d . . . H8 H 0.9229 0.2563 0.4253 0.031 Uiso 1 1 calc R . . C9 C 0.8816(4) 0.1436(4) 0.5028(3) 0.0340(10) Uani 1 1 d . . . H9 H 0.9422 0.1587 0.5476 0.041 Uiso 1 1 calc R . . C10 C 0.8073(4) 0.0647(4) 0.5101(3) 0.0320(10) Uani 1 1 d . . . H10 H 0.8173 0.0249 0.5590 0.038 Uiso 1 1 calc R . . C11 C 0.7173(4) 0.0429(4) 0.4461(3) 0.0313(10) Uani 1 1 d . . . H11 H 0.6658 -0.0120 0.4509 0.038 Uiso 1 1 calc R . . C12 C 0.7027(3) 0.1016(3) 0.3745(3) 0.0266(9) Uani 1 1 d . . . H12 H 0.6402 0.0877 0.3314 0.032 Uiso 1 1 calc R . . C13 C 0.7551(3) 0.1805(3) 0.1664(3) 0.0201(8) Uani 1 1 d . . . C14 C 0.7856(3) 0.0884(3) 0.1617(3) 0.0241(8) Uani 1 1 d . . . H14 H 0.8112 0.0626 0.2164 0.029 Uiso 1 1 calc R . . C15 C 0.7787(4) 0.0343(3) 0.0766(3) 0.0278(9) Uani 1 1 d . . . H15 H 0.7996 -0.0284 0.0732 0.033 Uiso 1 1 calc R . . C16 C 0.7413(4) 0.0719(3) -0.0030(3) 0.0297(9) Uani 1 1 d . . . H16 H 0.7351 0.0342 -0.0607 0.036 Uiso 1 1 calc R . . C17 C 0.7129(4) 0.1636(4) 0.0007(3) 0.0348(11) Uani 1 1 d . . . H17 H 0.6885 0.1893 -0.0544 0.042 Uiso 1 1 calc R . . C18 C 0.7198(4) 0.2184(3) 0.0852(3) 0.0298(10) Uani 1 1 d . . . H18 H 0.7005 0.2817 0.0877 0.036 Uiso 1 1 calc R . . C19 C 0.2725(3) 0.5373(3) 0.0977(3) 0.0199(8) Uani 1 1 d . . . C20 C 0.2645(3) 0.4769(3) 0.0160(3) 0.0251(8) Uani 1 1 d . . . H20 H 0.3143 0.4316 0.0080 0.030 Uiso 1 1 calc R . . C21 C 0.1836(4) 0.4832(3) -0.0535(3) 0.0289(9) Uani 1 1 d . . . H21 H 0.1782 0.4421 -0.1090 0.035 Uiso 1 1 calc R . . C22 C 0.1106(4) 0.5489(4) -0.0425(3) 0.0316(10) Uani 1 1 d . . . H22 H 0.0555 0.5528 -0.0904 0.038 Uiso 1 1 calc R . . C23 C 0.1180(4) 0.6093(4) 0.0389(3) 0.0351(11) Uani 1 1 d . . . H23 H 0.0682 0.6546 0.0461 0.042 Uiso 1 1 calc R . . C24 C 0.1981(3) 0.6033(3) 0.1096(3) 0.0273(9) Uani 1 1 d . . . H24 H 0.2023 0.6437 0.1655 0.033 Uiso 1 1 calc R . . C25 C 0.3549(3) 0.5759(3) 0.2942(3) 0.0196(8) Uani 1 1 d . . . C26 C 0.3422(4) 0.6710(3) 0.3195(3) 0.0252(8) Uani 1 1 d . . . H26 H 0.3522 0.7178 0.2762 0.030 Uiso 1 1 calc R . . C27 C 0.3147(4) 0.6977(3) 0.4079(3) 0.0330(10) Uani 1 1 d . . . H27 H 0.3026 0.7619 0.4244 0.040 Uiso 1 1 calc R . . C28 C 0.3051(4) 0.6286(4) 0.4723(3) 0.0362(11) Uani 1 1 d . . . H28 H 0.2901 0.6467 0.5338 0.043 Uiso 1 1 calc R . . C29 C 0.3173(4) 0.5348(4) 0.4470(3) 0.0331(10) Uani 1 1 d . . . H29 H 0.3087 0.4882 0.4907 0.040 Uiso 1 1 calc R . . C30 C 0.3420(3) 0.5073(3) 0.3579(3) 0.0245(8) Uani 1 1 d . . . H30 H 0.3500 0.4423 0.3407 0.029 Uiso 1 1 calc R . . C31 C 0.4933(3) 0.6241(3) 0.1469(3) 0.0192(7) Uani 1 1 d . . . C32 C 0.4814(3) 0.6643(3) 0.0625(3) 0.0237(8) Uani 1 1 d . . . H32 H 0.4158 0.6480 0.0234 0.028 Uiso 1 1 calc R . . C33 C 0.5655(4) 0.7279(3) 0.0361(3) 0.0274(9) Uani 1 1 d . . . H33 H 0.5570 0.7552 -0.0213 0.033 Uiso 1 1 calc R . . C34 C 0.6619(4) 0.7522(3) 0.0921(3) 0.0258(9) Uani 1 1 d . . . H34 H 0.7188 0.7963 0.0736 0.031 Uiso 1 1 calc R . . C35 C 0.6745(4) 0.7114(3) 0.1760(3) 0.0255(9) Uani 1 1 d . . . H35 H 0.7406 0.7270 0.2144 0.031 Uiso 1 1 calc R . . C36 C 0.5899(3) 0.6475(3) 0.2035(3) 0.0219(8) Uani 1 1 d . . . H36 H 0.5984 0.6201 0.2608 0.026 Uiso 1 1 calc R . . C37 C 0.4132(3) 0.0765(3) 0.2520(3) 0.0218(8) Uani 1 1 d . . . C38 C 0.4027(4) 0.0175(3) 0.3241(3) 0.0292(9) Uani 1 1 d . . . H38 H 0.3659 0.0361 0.3761 0.035 Uiso 1 1 calc R . . C39 C 0.4464(4) -0.0690(4) 0.3198(4) 0.0382(11) Uani 1 1 d . . . H39 H 0.4390 -0.1094 0.3689 0.046 Uiso 1 1 calc R . . C40 C 0.5001(4) -0.0963(3) 0.2449(4) 0.0372(11) Uani 1 1 d . . . H40 H 0.5302 -0.1551 0.2429 0.045 Uiso 1 1 calc R . . C41 C 0.5106(4) -0.0388(3) 0.1724(4) 0.0356(11) Uani 1 1 d . . . H41 H 0.5468 -0.0584 0.1204 0.043 Uiso 1 1 calc R . . C42 C 0.4678(4) 0.0480(3) 0.1761(3) 0.0272(9) Uani 1 1 d . . . H42 H 0.4757 0.0881 0.1268 0.033 Uiso 1 1 calc R . . C43 C 0.3277(3) 0.2207(3) 0.3694(3) 0.0219(8) Uani 1 1 d . . . C44 C 0.4112(4) 0.2680(4) 0.4326(3) 0.0301(10) Uani 1 1 d . . . H44 H 0.4826 0.2829 0.4140 0.036 Uiso 1 1 calc R . . C45 C 0.3894(4) 0.2933(4) 0.5234(3) 0.0410(12) Uani 1 1 d . . . H45 H 0.4448 0.3273 0.5665 0.049 Uiso 1 1 calc R . . C46 C 0.2842(4) 0.2677(5) 0.5499(3) 0.0445(13) Uani 1 1 d . . . H46 H 0.2686 0.2837 0.6116 0.053 Uiso 1 1 calc R . . C47 C 0.2037(4) 0.2196(5) 0.4871(3) 0.0439(13) Uani 1 1 d . . . H47 H 0.1333 0.2011 0.5063 0.053 Uiso 1 1 calc R . . C48 C 0.2239(4) 0.1979(4) 0.3970(3) 0.0344(10) Uani 1 1 d . . . H48 H 0.1668 0.1672 0.3536 0.041 Uiso 1 1 calc R . . C49 C 0.2374(3) 0.1743(3) 0.1782(3) 0.0208(8) Uani 1 1 d . . . C50 C 0.1641(3) 0.0901(3) 0.1719(3) 0.0252(9) Uani 1 1 d . . . H50 H 0.1790 0.0385 0.2072 0.030 Uiso 1 1 calc R . . C51 C 0.0677(3) 0.0822(3) 0.1130(3) 0.0250(8) Uani 1 1 d . . . H51 H 0.0162 0.0258 0.1094 0.030 Uiso 1 1 calc R . . C52 C 0.0483(4) 0.1569(3) 0.0604(3) 0.0273(9) Uani 1 1 d . . . H52 H -0.0159 0.1508 0.0194 0.033 Uiso 1 1 calc R . . C53 C 0.1209(4) 0.2401(3) 0.0667(3) 0.0272(9) Uani 1 1 d . . . H53 H 0.1057 0.2913 0.0310 0.033 Uiso 1 1 calc R . . C54 C 0.2170(3) 0.2497(3) 0.1254(3) 0.0216(8) Uani 1 1 d . . . H54 H 0.2676 0.3067 0.1293 0.026 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 V1 0.0173(3) 0.0168(3) 0.0161(3) 0.0022(2) 0.0017(2) 0.0011(2) V2 0.0278(4) 0.0320(4) 0.0234(4) 0.0053(3) -0.0003(3) -0.0021(3) P1 0.0184(5) 0.0201(5) 0.0173(5) 0.0040(4) 0.0001(4) 0.0028(4) P2 0.0185(5) 0.0165(5) 0.0170(4) 0.0023(4) -0.0001(4) 0.0023(4) P3 0.0179(5) 0.0168(5) 0.0193(5) 0.0030(4) 0.0008(4) 0.0004(4) Cl1 0.0389(6) 0.0384(6) 0.0327(6) 0.0025(5) 0.0019(5) 0.0151(5) Cl2 0.0408(7) 0.0333(6) 0.0500(7) 0.0047(5) 0.0153(5) 0.0122(5) O1 0.0187(13) 0.0230(14) 0.0221(13) 0.0037(11) 0.0008(11) 0.0024(11) O2 0.0224(14) 0.0169(13) 0.0207(13) 0.0019(11) -0.0023(11) 0.0014(11) O3 0.0222(14) 0.0187(14) 0.0230(14) 0.0052(11) 0.0015(11) -0.0021(11) O4 0.0268(15) 0.0234(15) 0.0202(13) -0.0020(11) -0.0007(11) 0.0065(12) O5 0.0230(14) 0.0287(15) 0.0225(14) 0.0066(12) 0.0058(11) 0.0027(12) O6 0.042(2) 0.040(2) 0.0358(18) 0.0111(15) 0.0027(15) -0.0065(15) O7 0.045(2) 0.053(2) 0.0281(17) 0.0051(16) -0.0079(15) -0.0061(17) C1 0.0216(19) 0.023(2) 0.0184(18) 0.0049(15) 0.0011(15) 0.0020(15) C2 0.024(2) 0.031(2) 0.027(2) 0.0021(17) 0.0053(17) 0.0035(17) C3 0.024(2) 0.043(3) 0.032(2) 0.000(2) 0.0052(18) -0.0009(19) C4 0.023(2) 0.038(3) 0.036(2) 0.003(2) 0.0036(18) -0.0058(18) C5 0.034(2) 0.024(2) 0.041(3) 0.0009(19) -0.001(2) -0.0015(19) C6 0.025(2) 0.025(2) 0.029(2) 0.0014(17) -0.0006(17) 0.0011(17) C7 0.0223(19) 0.023(2) 0.0182(18) 0.0057(15) 0.0017(15) 0.0067(16) C8 0.024(2) 0.029(2) 0.026(2) 0.0036(17) 0.0000(16) 0.0028(17) C9 0.028(2) 0.047(3) 0.027(2) 0.012(2) -0.0040(18) 0.002(2) C10 0.032(2) 0.041(3) 0.025(2) 0.0135(19) 0.0027(18) 0.007(2) C11 0.030(2) 0.036(2) 0.028(2) 0.0136(19) 0.0004(18) 0.0000(19) C12 0.023(2) 0.030(2) 0.025(2) 0.0086(17) -0.0023(16) -0.0041(17) C13 0.0194(18) 0.0194(19) 0.0213(18) 0.0030(15) 0.0024(15) 0.0006(15) C14 0.022(2) 0.026(2) 0.024(2) 0.0033(16) 0.0003(16) 0.0027(16) C15 0.028(2) 0.023(2) 0.032(2) 0.0000(17) 0.0061(18) 0.0034(17) C16 0.031(2) 0.033(2) 0.024(2) -0.0055(18) -0.0010(17) 0.0049(18) C17 0.047(3) 0.038(3) 0.020(2) -0.0011(18) -0.0044(19) 0.013(2) C18 0.041(3) 0.030(2) 0.021(2) 0.0035(17) 0.0002(18) 0.0156(19) C19 0.0173(18) 0.0227(19) 0.0200(18) 0.0073(15) 0.0000(14) 0.0021(15) C20 0.024(2) 0.030(2) 0.0200(19) 0.0013(16) -0.0007(16) 0.0004(17) C21 0.026(2) 0.037(2) 0.022(2) 0.0071(18) 0.0010(16) -0.0063(18) C22 0.023(2) 0.040(3) 0.030(2) 0.016(2) -0.0056(17) -0.0027(18) C23 0.028(2) 0.037(3) 0.042(3) 0.012(2) -0.005(2) 0.0091(19) C24 0.022(2) 0.029(2) 0.031(2) 0.0020(18) -0.0013(17) 0.0065(17) C25 0.0199(18) 0.0226(19) 0.0159(17) -0.0009(15) 0.0013(14) 0.0032(15) C26 0.029(2) 0.025(2) 0.0219(19) 0.0030(16) 0.0025(16) 0.0025(17) C27 0.039(3) 0.026(2) 0.034(2) -0.0068(18) 0.010(2) 0.0029(19) C28 0.040(3) 0.043(3) 0.027(2) 0.002(2) 0.012(2) 0.006(2) C29 0.043(3) 0.037(3) 0.022(2) 0.0079(19) 0.0088(19) 0.009(2) C30 0.026(2) 0.025(2) 0.025(2) 0.0056(16) 0.0058(16) 0.0064(16) C31 0.0212(18) 0.0160(18) 0.0202(18) 0.0013(14) 0.0046(15) 0.0006(14) C32 0.025(2) 0.026(2) 0.0198(19) 0.0039(16) -0.0004(15) 0.0013(16) C33 0.033(2) 0.030(2) 0.0201(19) 0.0053(17) 0.0050(17) 0.0028(18) C34 0.029(2) 0.020(2) 0.028(2) -0.0006(16) 0.0093(17) -0.0033(16) C35 0.024(2) 0.025(2) 0.025(2) 0.0010(17) 0.0011(16) -0.0015(16) C36 0.024(2) 0.022(2) 0.0197(18) 0.0025(15) -0.0005(15) 0.0010(16) C37 0.0191(18) 0.0192(19) 0.026(2) 0.0015(15) -0.0004(15) -0.0013(15) C38 0.024(2) 0.026(2) 0.039(2) 0.0107(19) 0.0057(18) 0.0025(17) C39 0.038(3) 0.028(2) 0.052(3) 0.019(2) 0.005(2) 0.005(2) C40 0.026(2) 0.021(2) 0.065(3) 0.004(2) 0.005(2) 0.0042(18) C41 0.026(2) 0.029(2) 0.050(3) -0.007(2) 0.007(2) 0.0011(19) C42 0.025(2) 0.027(2) 0.029(2) 0.0004(17) 0.0013(17) 0.0020(17) C43 0.024(2) 0.0185(19) 0.0229(19) 0.0024(15) 0.0013(15) 0.0019(15) C44 0.026(2) 0.041(3) 0.021(2) 0.0023(18) 0.0010(17) -0.0023(19) C45 0.036(3) 0.059(3) 0.023(2) -0.006(2) -0.0007(19) -0.005(2) C46 0.038(3) 0.072(4) 0.022(2) -0.004(2) 0.006(2) 0.006(3) C47 0.030(2) 0.070(4) 0.028(2) -0.003(2) 0.0088(19) -0.004(2) C48 0.023(2) 0.050(3) 0.027(2) -0.005(2) 0.0036(17) -0.004(2) C49 0.0209(19) 0.0208(19) 0.0195(18) 0.0010(15) 0.0038(15) -0.0021(15) C50 0.025(2) 0.022(2) 0.027(2) 0.0002(16) 0.0005(16) -0.0015(16) C51 0.0192(19) 0.024(2) 0.029(2) -0.0020(17) -0.0012(16) -0.0039(16) C52 0.023(2) 0.034(2) 0.023(2) -0.0006(17) -0.0025(16) 0.0017(17) C53 0.029(2) 0.032(2) 0.022(2) 0.0098(17) 0.0019(16) 0.0047(18) C54 0.0181(18) 0.024(2) 0.0226(19) 0.0036(16) 0.0028(15) 0.0018(15) _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 V1 O5 1.606(3) . ? V1 O4 1.621(3) . ? V1 O3 2.015(3) . ? V1 O1 2.019(3) . ? V1 O2 2.027(3) . ? V2 O7 1.612(3) . ? V2 O6 1.614(3) . ? V2 Cl1 2.2253(16) . ? V2 Cl2 2.2389(16) . ? P1 O1 1.515(3) . ? P1 C7 1.790(4) . ? P1 C1 1.796(4) . ? P1 C13 1.796(4) . ? P2 O2 1.522(3) . ? P2 C19 1.793(4) . ? P2 C31 1.800(4) . ? P2 C25 1.802(4) . ? P3 O3 1.504(3) . ? P3 C49 1.789(4) . ? P3 C37 1.796(4) . ? P3 C43 1.797(4) . ? C1 C2 1.391(6) . ? C1 C6 1.405(6) . ? C2 C3 1.408(6) . ? C2 H2 0.9500 . ? C3 C4 1.377(7) . ? C3 H3 0.9500 . ? C4 C5 1.391(7) . ? C4 H4 0.9500 . ? C5 C6 1.381(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.392(6) . ? C7 C8 1.395(6) . ? C8 C9 1.399(6) . ? C8 H8 0.9500 . ? C9 C10 1.369(7) . ? C9 H9 0.9500 . ? C10 C11 1.387(7) . ? C10 H10 0.9500 . ? C11 C12 1.396(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.393(6) . ? C13 C18 1.398(6) . ? C14 C15 1.395(6) . ? C14 H14 0.9500 . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 C17 1.379(7) . ? C16 H16 0.9500 . ? C17 C18 1.391(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.397(6) . ? C19 C24 1.402(6) . ? C20 C21 1.387(6) . ? C20 H20 0.9500 . ? C21 C22 1.384(7) . ? C21 H21 0.9500 . ? C22 C23 1.394(7) . ? C22 H22 0.9500 . ? C23 C24 1.391(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.394(5) . ? C25 C26 1.392(6) . ? C26 C27 1.393(6) . ? C26 H26 0.9500 . ? C27 C28 1.404(7) . ? C27 H27 0.9500 . ? C28 C29 1.373(7) . ? C28 H28 0.9500 . ? C29 C30 1.393(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.391(6) . ? C31 C32 1.398(5) . ? C32 C33 1.387(6) . ? C32 H32 0.9500 . ? C33 C34 1.387(6) . ? C33 H33 0.9500 . ? C34 C35 1.396(6) . ? C34 H34 0.9500 . ? C35 C36 1.398(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.392(6) . ? C37 C42 1.399(6) . ? C38 C39 1.393(7) . ? C38 H38 0.9500 . ? C39 C40 1.376(8) . ? C39 H39 0.9500 . ? C40 C41 1.384(7) . ? C40 H40 0.9500 . ? C41 C42 1.392(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.387(6) . ? C43 C44 1.398(6) . ? C44 C45 1.398(6) . ? C44 H44 0.9500 . ? C45 C46 1.402(7) . ? C45 H45 0.9500 . ? C46 C47 1.374(7) . ? C46 H46 0.9500 . ? C47 C48 1.373(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.394(6) . ? C49 C54 1.395(6) . ? C50 C51 1.407(6) . ? C50 H50 0.9500 . ? C51 C52 1.383(6) . ? C51 H51 0.9500 . ? C52 C53 1.378(6) . ? C52 H52 0.9500 . ? C53 C54 1.400(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 V1 O4 108.32(16) . . ? O5 V1 O3 126.05(14) . . ? O4 V1 O3 125.61(14) . . ? O5 V1 O1 96.24(13) . . ? O4 V1 O1 94.98(13) . . ? O3 V1 O1 81.41(12) . . ? O5 V1 O2 95.02(13) . . ? O4 V1 O2 96.56(13) . . ? O3 V1 O2 79.06(11) . . ? O1 V1 O2 160.47(12) . . ? O7 V2 O6 108.39(19) . . ? O7 V2 Cl1 108.52(16) . . ? O6 V2 Cl1 109.42(15) . . ? O7 V2 Cl2 109.79(15) . . ? O6 V2 Cl2 111.08(15) . . ? Cl1 V2 Cl2 109.59(6) . . ? O1 P1 C7 108.07(17) . . ? O1 P1 C1 112.24(18) . . ? C7 P1 C1 108.21(19) . . ? O1 P1 C13 111.65(17) . . ? C7 P1 C13 107.92(19) . . ? C1 P1 C13 108.61(19) . . ? O2 P2 C19 109.05(17) . . ? O2 P2 C31 113.20(17) . . ? C19 P2 C31 106.26(18) . . ? O2 P2 C25 109.86(17) . . ? C19 P2 C25 110.28(19) . . ? C31 P2 C25 108.12(18) . . ? O3 P3 C49 109.20(17) . . ? O3 P3 C37 110.26(18) . . ? C49 P3 C37 108.50(19) . . ? O3 P3 C43 112.14(18) . . ? C49 P3 C43 108.61(19) . . ? C37 P3 C43 108.05(19) . . ? P1 O1 V1 142.88(17) . . ? P2 O2 V1 132.26(17) . . ? P3 O3 V1 155.74(19) . . ? C2 C1 C6 120.1(4) . . ? C2 C1 P1 120.2(3) . . ? C6 C1 P1 119.7(3) . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.1(5) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C7 C8 120.0(4) . . ? C12 C7 P1 118.0(3) . . ? C8 C7 P1 122.1(3) . . ? C7 C8 C9 118.9(4) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 121.3(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.9(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.0(4) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C18 119.5(4) . . ? C14 C13 P1 123.2(3) . . ? C18 C13 P1 117.3(3) . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.5(4) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.0(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0(4) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 120.0(4) . . ? C20 C19 P2 118.4(3) . . ? C24 C19 P2 121.3(3) . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 119.5(4) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? C30 C25 C26 120.0(4) . . ? C30 C25 P2 118.0(3) . . ? C26 C25 P2 122.0(3) . . ? C27 C26 C25 120.3(4) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 119.1(4) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 120.6(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 119.5(4) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? C36 C31 C32 119.8(4) . . ? C36 C31 P2 119.8(3) . . ? C32 C31 P2 120.3(3) . . ? C33 C32 C31 119.8(4) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.9(4) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C35 119.4(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 120.0(4) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C42 119.4(4) . . ? C38 C37 P3 122.1(3) . . ? C42 C37 P3 118.5(3) . . ? C37 C38 C39 119.8(4) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C41 120.5(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C40 C41 C42 119.6(5) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C41 C42 C37 120.3(4) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? C48 C43 C44 120.0(4) . . ? C48 C43 P3 121.9(3) . . ? C44 C43 P3 118.0(3) . . ? C43 C44 C45 119.7(4) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 118.9(5) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? C47 C46 C45 120.4(5) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C46 120.7(5) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C43 120.1(4) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C50 C49 C54 120.6(4) . . ? C50 C49 P3 121.4(3) . . ? C54 C49 P3 118.0(3) . . ? C49 C50 C51 119.4(4) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C52 C51 C50 119.7(4) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C53 C52 C51 120.8(4) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 120.4(4) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C49 C54 C53 119.1(4) . . ? C49 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.953 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.144 #===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 =============================================================