Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_trcr _database_code_CSD 181231 _audit_creation_method Xtal3.6 _audit_creation_date 01-02-13 _audit_update_record ? _journal_coden_Cambridge 186 loop_ _publ_author_name 'Thomas Ruether' 'Nathalie C. Braussaud' 'Kingsley Cavell' 'Brian W. Skelton' 'Allan H. White' _publ_contact_author_name 'Dr Thomas Ruether' _publ_contact_author_address ; Centre for Green Chemistry Monash University Box 23 Melbourne 3800 AUSTRALIA ; _publ_contact_author_email 'THOMAS.RUETHER@SCI.MONASH.EDU.AU' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, characterisation and catalytic behaviour of a novel class of chromium(III) and vanadium(III) complexes containing bi- and tri-dentate imidazole chelating ligands: a comparative study ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C13 H16 Cl3 Cr1 N6 O1' _chemical_formula_moiety ? _chemical_formula_weight 430.67 _chemical_melting_point ? _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 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 6.9757(2) _cell_length_b 14.6946(5) _cell_length_c 17.5803(6) _cell_angle_alpha 90.00000 _cell_angle_beta 94.4190(10) _cell_angle_gamma 90.00000 _cell_volume 1796.71(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 26.6 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.096 _exptl_crystal_description bar _exptl_crystal_size_max .5 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour green _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .72 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 37346 _reflns_number_total 9433 _reflns_Friedel_coverage 0 _reflns_number_gt 6992 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.61 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .03 _refine_ls_wR_factor_ref .035 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_number_reflns 6992 _refine_ls_number_parameters 281 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .022 _refine_diff_density_min -.373 _refine_diff_density_max .547 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 52 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 64 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 12 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cr ? 0 4 .284 .624 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cr .72277(2) .745190(11) .050928(9) .01385(7) Uani ? ? 1.00000 ? ? Cl1 .87174(4) .793591(18) -.056055(15) .01997(11) Uani ? ? 1.00000 ? ? Cl2 .53935(4) .638728(18) -.019714(15) .01817(11) Uani ? ? 1.00000 ? ? Cl3 .89998(5) .84631(2) .128404(17) .02453(13) Uani ? ? 1.00000 ? ? N11 .58213(13) .70568(6) .14453(5) .0171(4) Uani ? ? 1.00000 ? ? C12 .58655(15) .62238(7) .17538(6) .0161(4) Uani ? ? 1.00000 ? ? N13 .46729(14) .61854(7) .23269(5) .0191(4) Uani ? ? 1.00000 ? ? C14 .38439(18) .70257(9) .23799(7) .0246(5) Uani ? ? 1.00000 ? ? C15 .45545(19) .75569(8) .18293(7) .0232(5) Uani ? ? 1.00000 ? ? C16 .4399(2) .54234(9) .28504(7) .0258(6) Uani ? ? 1.00000 ? ? C0 .70584(15) .54505(7) .15408(6) .0166(4) Uani ? ? 1.00000 ? ? O0 .66796(13) .46757(6) .17223(5) .0247(4) Uani ? ? 1.00000 ? ? N21 .91627(13) .64434(6) .07901(5) .0152(4) Uani ? ? 1.00000 ? ? C22 .87957(15) .56644(7) .11493(6) .0154(4) Uani ? ? 1.00000 ? ? N23 1.03057(13) .50863(6) .11259(5) .0174(4) Uani ? ? 1.00000 ? ? C24 1.16747(16) .55135(8) .07390(7) .0194(5) Uani ? ? 1.00000 ? ? C25 1.09581(15) .63514(8) .05325(6) .0181(4) Uani ? ? 1.00000 ? ? C26 1.0518(2) .41760(8) .14647(8) .0268(6) Uani ? ? 1.00000 ? ? N101 .50873(14) .84106(6) .02770(6) .0198(4) Uani ? ? 1.00000 ? ? C101 .38891(16) .89290(7) .01770(7) .0198(5) Uani ? ? 1.00000 ? ? C102 .23451(19) .95930(9) .00617(9) .0276(6) Uani ? ? 1.00000 ? ? N201 .9699(2) .55825(12) .31958(9) .0490(8) Uani ? ? 1.00000 ? ? C201 .9280(2) .63345(12) .32054(8) .0362(7) Uani ? ? 1.00000 ? ? C202 .8740(3) .72886(14) .32181(11) .0467(10) Uani ? ? 1.00000 ? ? H14 .297(2) .7154(10) .2758(9) .024(4) Uiso ? ? 1.00000 ? ? H15 .429(2) .8176(10) .1697(8) .022(4) Uiso ? ? 1.00000 ? ? H16a .564(2) .5158(10) .3011(9) .024(4) Uiso ? ? 1.00000 ? ? H16b .366(3) .5000(13) .2608(11) .044(5) Uiso ? ? 1.00000 ? ? H16c .378(2) .5665(12) .3278(10) .040(5) Uiso ? ? 1.00000 ? ? H24 1.278(2) .5243(11) .0683(9) .031(4) Uiso ? ? 1.00000 ? ? H25 1.153(2) .6785(10) .0255(9) .022(4) Uiso ? ? 1.00000 ? ? H26a 1.031(2) .4221(11) .1970(9) .032(4) Uiso ? ? 1.00000 ? ? H26b 1.179(2) .3983(11) .1412(9) .034(4) Uiso ? ? 1.00000 ? ? H26c .968(2) .3782(12) .1185(10) .037(5) Uiso ? ? 1.00000 ? ? H102a .233(3) .9846(13) -.0407(11) .047(5) Uiso ? ? 1.00000 ? ? H102b .253(2) 1.0045(12) .0442(10) .036(5) Uiso ? ? 1.00000 ? ? H102c .120(3) .9277(13) .0119(11) .053(6) Uiso ? ? 1.00000 ? ? H202a .749(4) .7340(15) .3327(13) .073(8) Uiso ? ? 1.00000 ? ? H202b .869(3) .7539(15) .2699(15) .074(7) Uiso ? ? 1.00000 ? ? H202c .958(3) .7616(13) .3541(12) .053(6) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr .01632(7) .01207(7) .01340(7) .00210(5) .00274(5) .00071(5) Cl1 .02486(12) .01752(11) .01836(11) .00023(9) .00695(9) .00288(9) Cl2 .01819(11) .01844(11) .01790(11) -.00047(9) .00156(8) -.00141(8) Cl3 .03237(15) .01798(12) .02286(13) -.00387(10) -.00040(11) -.00377(9) N11 .0194(4) .0174(4) .0149(4) .0030(3) .0036(3) .0005(3) C12 .0164(4) .0185(4) .0136(4) -.0000(3) .0023(3) .0001(3) N13 .0206(4) .0217(4) .0156(4) .0013(3) .0052(3) .0021(3) C14 .0272(6) .0282(6) .0195(5) .0077(5) .0090(4) .0017(4) C15 .0293(6) .0223(5) .0190(5) .0089(4) .0080(4) .0008(4) C16 .0316(6) .0268(6) .0202(5) -.0015(5) .0097(5) .0049(4) C0 .0191(5) .0160(4) .0147(4) -.0008(3) .0019(3) -.0004(3) O0 .0304(4) .0162(4) .0284(4) -.0032(3) .0081(3) .0002(3) N21 .0151(4) .0144(4) .0163(4) .0008(3) .0018(3) .0007(3) C22 .0175(4) .0139(4) .0150(4) .0020(3) .0014(3) -.0003(3) N23 .0213(4) .0137(4) .0173(4) .0039(3) .0021(3) -.0004(3) C24 .0172(5) .0203(5) .0211(5) .0041(4) .0031(4) -.0005(4) C25 .0156(4) .0182(5) .0206(5) .0007(4) .0030(4) .0006(4) C26 .0354(7) .0169(5) .0289(6) .0087(5) .0075(5) .0052(4) N101 .0234(4) .0168(4) .0197(4) .0032(3) .0046(3) .0016(3) C101 .0216(5) .0166(4) .0215(5) .0004(4) .0035(4) .0022(4) C102 .0208(5) .0187(5) .0435(8) .0052(4) .0037(5) .0061(5) N201 .0347(7) .0575(10) .0549(9) -.0072(6) .0037(6) -.0115(8) C201 .0277(7) .0528(10) .0279(6) -.0083(6) .0004(5) -.0092(6) C202 .0492(11) .0526(10) .0359(9) .0014(8) -.0115(8) -.0116(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cr Cl1 . . 2.3290(3) ? Cr Cl2 . . 2.3199(3) ? Cr Cl3 . . 2.3090(3) ? Cr N11 . . 2.0630(10) ? Cr N21 . . 2.0394(9) ? Cr N101 . . 2.0704(10) ? N11 C12 . . 1.3382(14) ? N11 C15 . . 1.3670(16) ? C12 N13 . . 1.3563(15) ? C12 C0 . . 1.4738(15) ? N13 C14 . . 1.3697(16) ? N13 C16 . . 1.4713(17) ? C14 C15 . . 1.3660(18) ? C14 H14 . . .954(16) ? C15 H15 . . .954(14) ? C16 H16a . . .972(15) ? C16 H16b . . .894(18) ? C16 H16c . . .963(18) ? C0 O0 . . 1.2169(13) ? C0 C22 . . 1.4730(15) ? N21 C22 . . 1.3414(13) ? N21 C25 . . 1.3709(14) ? C22 N23 . . 1.3563(14) ? N23 C24 . . 1.3671(15) ? N23 C26 . . 1.4672(16) ? C24 C25 . . 1.3673(16) ? C24 H24 . . .882(16) ? C25 H25 . . .912(15) ? C26 H26a . . .913(17) ? C26 H26b . . .942(17) ? C26 H26c . . .936(17) ? N101 C101 . . 1.1346(15) ? C101 C102 . . 1.4558(17) ? C102 H102a . . .90(2) ? C102 H102b . . .944(17) ? C102 H102c . . .94(2) ? N201 C201 . . 1.143(2) ? C201 C202 . . 1.453(3) ? C202 H202a . . .91(3) ? C202 H202b . . .98(3) ? C202 H202c . . .92(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl1 Cr Cl2 . . . 92.041(11) ? Cl1 Cr Cl3 . . . 91.601(12) ? Cl1 Cr N11 . . . 177.79(4) ? Cl1 Cr N21 . . . 95.12(3) ? Cl1 Cr N101 . . . 89.59(3) ? Cl2 Cr Cl3 . . . 176.232(17) ? Cl2 Cr N11 . . . 87.75(3) ? Cl2 Cr N21 . . . 88.11(3) ? Cl2 Cr N101 . . . 89.64(3) ? Cl3 Cr N11 . . . 88.65(3) ? Cl3 Cr N21 . . . 90.60(3) ? Cl3 Cr N101 . . . 91.35(3) ? N11 Cr N21 . . . 87.07(4) ? N11 Cr N101 . . . 88.21(4) ? N21 Cr N101 . . . 174.85(4) ? Cr N11 C12 . . . 125.67(7) ? Cr N11 C15 . . . 127.44(8) ? C12 N11 C15 . . . 106.69(9) ? N11 C12 N13 . . . 110.05(9) ? N11 C12 C0 . . . 126.74(10) ? N13 C12 C0 . . . 123.18(10) ? C12 N13 C14 . . . 107.42(10) ? C12 N13 C16 . . . 127.82(10) ? C14 N13 C16 . . . 124.59(10) ? N13 C14 C15 . . . 106.79(11) ? N13 C14 H14 . . . 121.4(9) ? C15 C14 H14 . . . 131.8(9) ? N11 C15 C14 . . . 109.05(11) ? N11 C15 H15 . . . 120.9(9) ? C14 C15 H15 . . . 130.0(9) ? N13 C16 H16a . . . 109.3(9) ? N13 C16 H16b . . . 109.2(12) ? N13 C16 H16c . . . 107.2(10) ? H16a C16 H16b . . . 109.0(15) ? H16a C16 H16c . . . 111.4(14) ? H16b C16 H16c . . . 110.6(16) ? C12 C0 O0 . . . 121.10(10) ? C12 C0 C22 . . . 117.07(9) ? O0 C0 C22 . . . 121.69(10) ? Cr N21 C22 . . . 125.96(7) ? Cr N21 C25 . . . 126.59(7) ? C22 N21 C25 . . . 106.48(9) ? C0 C22 N21 . . . 126.57(9) ? C0 C22 N23 . . . 123.32(9) ? N21 C22 N23 . . . 110.08(9) ? C22 N23 C24 . . . 107.54(9) ? C22 N23 C26 . . . 127.81(10) ? C24 N23 C26 . . . 124.63(10) ? N23 C24 C25 . . . 106.88(10) ? N23 C24 H24 . . . 120.1(10) ? C25 C24 H24 . . . 133.0(10) ? N21 C25 C24 . . . 109.01(10) ? N21 C25 H25 . . . 123.7(9) ? C24 C25 H25 . . . 127.2(9) ? N23 C26 H26a . . . 108.0(11) ? N23 C26 H26b . . . 107.5(10) ? N23 C26 H26c . . . 108.2(11) ? H26a C26 H26b . . . 109.7(14) ? H26a C26 H26c . . . 114.7(15) ? H26b C26 H26c . . . 108.5(15) ? Cr N101 C101 . . . 177.31(10) ? N101 C101 C102 . . . 179.06(15) ? C101 C102 H102a . . . 110.9(12) ? C101 C102 H102b . . . 108.1(10) ? C101 C102 H102c . . . 106.4(12) ? H102a C102 H102b . . . 110.3(16) ? H102a C102 H102c . . . 110.8(16) ? H102b C102 H102c . . . 110.2(16) ? N201 C201 C202 . . . 179.7(2) ? C201 C202 H202a . . . 109.7(14) ? C201 C202 H202b . . . 109.8(13) ? C201 C202 H202c . . . 111.1(12) ? H202a C202 H202b . . . 102(2) ? H202a C202 H202c . . . 114(2) ? H202b C202 H202c . . . 110.5(19) ? _exptl_crystal_F_000 876 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -30 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .582 _reflns_d_resolution_low 11.236 _diffrn_reflns_av_sigmaI/netI .071 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .051 _refine_ls_wR_factor_all .038 _refine_ls_goodness_of_fit_all .983 _refine_ls_shift/su_mean .001 #===END