# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1777 data_mvbcrc _audit_creation_date 98-02-04 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C18 H27 Cl3 Cr N3' #ActaC _chemical_formula_weight 443.8 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf Nonius software' #ActaC _computing_cell_refinement 'Enraf Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 15.530(5) #ActaC _cell_length_b 13.770(7) #ActaC _cell_length_c 12.697(5) #ActaC _cell_angle_alpha 115.93(3) #ActaC _cell_angle_beta 101.53(3) #ActaC _cell_angle_gamma 105.48(3) #ActaC _cell_volume 2191(2) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 8 #ActaC _cell_measurement_theta_min 18.6 #ActaC _cell_measurement_theta_max 20.7 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour colourless #ActaC _exptl_crystal_size_max .50 #ActaC _exptl_crystal_size_mid .30 #ActaC _exptl_crystal_size_min .08 #ActaC _exptl_crystal_density_diffrn 1.346 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 924 #ActaC _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_coefficient_mu .89 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min .78 #ActaC _exptl_absorpt_correction_T_max .94 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength .71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'rotating anode' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method '2\Q-\w scans' #ActaC _diffrn_standards_number 8 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 7 4 4 -7 -4 -4 -7 7 7 7 -7 -7 9 -6 7 -9 6 -7 -9 -7 7 9 7 -7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number .139000+05 #ActaC _diffrn_reflns_av_R_equivalents .033 #ActaC _diffrn_reflns_av_sigmaI/netI .047 #ActaC _diffrn_reflns_limit_h_min -18 #ActaC _diffrn_reflns_limit_h_max 18 #ActaC _diffrn_reflns_limit_k_min -16 #ActaC _diffrn_reflns_limit_k_max 16 #ActaC _diffrn_reflns_limit_l_min -15 #ActaC _diffrn_reflns_limit_l_max 9 #ActaC _diffrn_reflns_theta_min 1.46 #ActaC _diffrn_reflns_theta_max 24.98 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 72 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 0 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 12 .004 .003 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 Cl ? 0 12 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 108 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Cr1 .74446(6) 1.20528(7) 1.09699(7) .0309(3) Uani ? ? Cr2 .75200(6) .69918(7) .61875(7) .0326(3) Uani ? ? Cl11 .61906(11) 1.18995(13) 1.16689(14) .0534(7) Uani ? ? Cl12 .74230(11) 1.34970(12) 1.05655(14) .0502(6) Uani ? ? Cl13 .87234(11) 1.31839(13) 1.28448(13) .0533(6) Uani ? ? Cl21 .62213(11) .68113(13) .67888(14) .0527(6) Uani ? ? Cl22 .75742(11) .85071(12) .58677(14) .0487(6) Uani ? ? Cl23 .87360(11) .80432(13) .81145(13) .0520(6) Uani ? ? N11 .8255(3) 1.1459(3) .9893(4) .0318(16) Uani ? ? C111 .9157(4) 1.2178(5) .9896(5) .043(2) Uani ? ? C112 .9469(4) 1.1474(5) .8846(6) .053(3) Uani ? ? C113 1.0400(4) 1.2252(6) .8903(6) .060(3) Uani ? ? C114 1.0353(4) 1.3282(6) .8849(6) .061(3) Uani ? ? C115 1.0324(5) 1.4103(6) .8816(7) .071(3) Uani ? ? C12 .8326(4) 1.0621(5) 1.0302(5) .039(2) Uani ? ? N13 .7459(3) 1.0425(3) 1.0643(4) .0343(17) Uani ? ? C131 .7459(4) 1.0007(5) 1.1534(5) .052(3) Uani ? ? C132 .7448(4) .8804(5) 1.1069(6) .056(3) Uani ? ? C133 .7400(5) .8463(6) 1.2062(6) .071(3) Uani ? ? C134 .7437(4) .7319(5) 1.1689(6) .048(3) Uani ? ? C135 .7471(5) .6406(6) 1.1365(6) .058(3) Uani ? ? C14 .6592(4) .9750(4) .9498(5) .036(2) Uani ? ? N15 .6617(3) 1.0635(3) .9127(4) .0313(16) Uani ? ? C151 .5691(4) 1.0417(5) .8272(5) .040(2) Uani ? ? C152 .5373(4) .9382(5) .6941(5) .051(2) Uani ? ? C153 .4372(4) .9107(6) .6129(6) .064(3) Uani ? ? C154 .4268(5) 1.0102(7) .6069(6) .065(3) Uani ? ? C155 .4166(6) 1.0873(7) .5993(7) .093(4) Uani ? ? C16 .7422(4) 1.0858(4) .8697(5) .036(2) Uani ? ? N21 .8376(3) .6458(4) .5160(4) .0339(17) Uani ? ? C211 .9324(4) .7209(5) .5302(5) .044(2) Uani ? ? C212 .9714(4) .6587(5) .4304(6) .054(3) Uani ? ? C213 1.0715(4) .7390(6) .4560(6) .060(3) Uani ? ? C214 1.0791(5) .8477(7) .4610(7) .070(3) Uani ? ? C215 1.0846(6) .9343(7) .4632(9) .097(4) Uani ? ? C22 .8356(4) .5525(5) .5449(5) .042(2) Uani ? ? N23 .7460(3) .5281(4) .5707(4) .0386(18) Uani ? ? C231 .7310(5) .4545(6) .6290(6) .067(3) Uani ? ? C232 .8000(6) .5028(6) .7510(7) .088(4) Uani ? ? C233 .7685(6) .4269(7) .8094(7) .078(4) Uani ? ? C234 .7572(5) .3053(7) .7335(6) .056(3) Uani ? ? C235 .7478(5) .2067(7) .6705(7) .067(3) Uani ? ? C24 .6635(4) .4721(5) .4519(5) .040(2) Uani ? ? N25 .6744(3) .5685(4) .4276(4) .0336(17) Uani ? ? C251 .5864(4) .5576(5) .3440(5) .044(2) Uani ? ? C252 .5524(4) .4587(5) .2081(5) .051(2) Uani ? ? C253 .4572(4) .4460(6) .1303(6) .059(3) Uani ? ? C254 .4604(4) .5545(6) .1323(6) .064(3) Uani ? ? C255 .4606(6) .6383(7) .1331(8) .093(4) Uani ? ? C26 .7600(4) .5950(5) .3940(5) .037(2) Uani ? ? H111a .96745 1.25360 1.06899 .05300 Uiso ? ? H111b .90809 1.28290 .98214 .05300 Uiso ? ? H112a .89612 1.11531 .80303 .07300 Uiso ? ? H112b .95140 1.08113 .88793 .07300 Uiso ? ? H113a 1.05851 1.18032 .82206 .07900 Uiso ? ? H113b 1.09057 1.25177 .96744 .07900 Uiso ? ? H115 1.03028 1.47944 .87732 .10400 Uiso ? ? H12a .82933 .99081 .96443 .04700 Uiso ? ? H12b .89009 1.09519 1.10095 .04700 Uiso ? ? H131a .69082 1.00439 1.18026 .07100 Uiso ? ? H131b .80217 1.05791 1.23219 .07100 Uiso ? ? H132a .80181 .87736 1.08761 .06800 Uiso ? ? H132b .69062 .82361 1.02855 .06800 Uiso ? ? H133a .67981 .84320 1.22161 .09000 Uiso ? ? H133b .79068 .90554 1.28656 .09000 Uiso ? ? H135 .74914 .56291 1.10717 .08400 Uiso ? ? H14a .60202 .95070 .96666 .04400 Uiso ? ? H14b .66207 .90678 .88677 .04400 Uiso ? ? H151a .57650 1.11320 .82420 .04700 Uiso ? ? H151b .52040 1.02981 .86144 .04700 Uiso ? ? H152a .53998 .87017 .69885 .06500 Uiso ? ? H152b .58329 .95528 .65593 .06500 Uiso ? ? H153a .39100 .88396 .64652 .08500 Uiso ? ? H153b .41868 .84649 .52818 .08500 Uiso ? ? H155 .40770 1.15085 .58956 .13500 Uiso ? ? H16a .74194 1.01182 .80559 .04700 Uiso ? ? H16b .74012 1.13214 .83140 .04700 Uiso ? ? H211a .97938 .75197 .61257 .05600 Uiso ? ? H211b .92896 .78999 .52817 .05600 Uiso ? ? H212a .92794 .63520 .34896 .06700 Uiso ? ? H212b .97023 .58769 .42810 .06700 Uiso ? ? H213a 1.09586 .69791 .39217 .07500 Uiso ? ? H213b 1.11599 .75832 .53536 .07500 Uiso ? ? H215 1.09123 1.00792 .46471 .14200 Uiso ? ? H22a .89131 .57932 .61638 .05300 Uiso ? ? H22b .83431 .48393 .47532 .05300 Uiso ? ? H231a .72657 .37921 .57452 .08500 Uiso ? ? H231b .66856 .44556 .63968 .08500 Uiso ? ? H232a .81306 .58532 .80830 .11300 Uiso ? ? H232b .86272 .50429 .74514 .11300 Uiso ? ? H233a .70751 .42774 .81892 .10000 Uiso ? ? H233b .81318 .46200 .89537 .10000 Uiso ? ? H235 .74081 .12641 .61711 .09700 Uiso ? ? H24a .60294 .44355 .46014 .05300 Uiso ? ? H24b .66686 .40515 .38440 .05300 Uiso ? ? H251a .59915 .63230 .34739 .05400 Uiso ? ? H251b .53623 .54577 .37604 .05400 Uiso ? ? H252a .54754 .38766 .20554 .06500 Uiso ? ? H252b .59968 .47732 .17263 .06500 Uiso ? ? H253a .40800 .42266 .16190 .07400 Uiso ? ? H253b .43592 .38286 .04374 .07400 Uiso ? ? H26a .76406 .64932 .36516 .04100 Uiso ? ? H26b .76043 .52460 .32828 .04100 Uiso ? ? H255 .46000 .70732 .13016 .12700 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Cr1 .0374(5) .0243(5) .0309(5) .0135(4) .0137(4) .0132(4) Cr2 .0385(5) .0283(5) .0296(5) .0148(4) .0126(4) .0129(4) Cl11 .0576(10) .0448(9) .0607(10) .0211(8) .0366(8) .0232(8) Cl12 .0641(10) .0375(8) .0624(10) .0268(8) .0255(8) .0319(8) Cl13 .0592(10) .0428(9) .0364(8) .0198(8) .0053(7) .0091(7) Cl21 .0567(10) .0489(9) .0575(10) .0245(8) .0347(8) .0239(8) Cl22 .0628(10) .0342(8) .0513(9) .0223(7) .0201(8) .0227(7) Cl23 .0595(10) .0444(9) .0335(8) .0208(8) .0046(7) .0109(7) N11 .036(2) .027(2) .033(2) .014(2) .015(2) .014(2) C111 .033(3) .033(3) .055(4) .006(3) .016(3) .020(3) C112 .046(4) .044(4) .066(4) .015(3) .033(3) .023(3) C113 .045(4) .056(4) .077(5) .018(3) .033(3) .029(4) C114 .052(4) .064(5) .067(5) .019(4) .032(4) .033(4) C115 .071(5) .060(5) .080(5) .020(4) .032(4) .038(4) C12 .041(3) .037(3) .039(3) .021(3) .010(3) .017(3) N13 .047(3) .027(2) .030(2) .013(2) .013(2) .017(2) C131 .071(4) .041(4) .046(4) .020(3) .017(3) .028(3) C132 .070(4) .048(4) .061(4) .028(3) .026(3) .033(3) C133 .111(6) .055(4) .066(5) .039(4) .035(4) .042(4) C134 .058(4) .044(4) .050(4) .017(3) .019(3) .032(3) C135 .063(4) .053(4) .065(4) .023(4) .026(3) .035(4) C14 .046(3) .025(3) .032(3) .012(3) .012(3) .013(3) N15 .034(2) .027(2) .029(2) .011(2) .009(2) .013(2) C151 .034(3) .043(3) .040(3) .019(3) .009(3) .019(3) C152 .053(4) .047(4) .038(3) .024(3) .006(3) .012(3) C153 .055(4) .055(4) .048(4) .008(3) -.006(3) .018(3) C154 .062(5) .079(5) .044(4) .033(4) .004(3) .028(4) C155 .124(7) .090(6) .061(5) .063(6) .009(5) .035(5) C16 .039(3) .032(3) .030(3) .011(3) .012(2) .013(3) N21 .033(2) .038(3) .030(2) .013(2) .011(2) .017(2) C211 .040(3) .042(3) .037(3) .014(3) .011(3) .013(3) C212 .053(4) .053(4) .058(4) .021(3) .030(3) .026(3) C213 .057(4) .067(5) .066(4) .025(4) .035(4) .038(4) C214 .057(4) .076(6) .072(5) .012(4) .029(4) .041(5) C215 .102(7) .071(6) .109(7) .017(5) .045(6) .049(6) C22 .054(4) .041(3) .038(3) .029(3) .017(3) .020(3) N23 .055(3) .033(3) .040(3) .023(2) .021(2) .024(2) C231 .095(5) .058(5) .057(4) .030(4) .024(4) .040(4) C232 .124(7) .061(5) .064(5) .025(5) .014(5) .036(4) C233 .120(7) .083(6) .065(5) .049(5) .043(5) .056(5) C234 .056(4) .075(5) .052(4) .021(4) .017(3) .049(4) C235 .075(5) .067(5) .063(5) .024(4) .018(4) .044(4) C24 .040(3) .033(3) .040(3) .011(3) .014(3) .016(3) N25 .034(3) .034(3) .033(2) .014(2) .012(2) .019(2) C251 .040(3) .045(4) .039(3) .017(3) .008(3) .018(3) C252 .054(4) .043(4) .041(3) .017(3) .006(3) .017(3) C253 .048(4) .056(4) .049(4) .009(3) .000(3) .022(3) C254 .050(4) .069(5) .059(4) .021(4) -.002(3) .032(4) C255 .091(6) .075(6) .110(7) .040(5) .006(5) .055(6) C26 .043(3) .043(3) .028(3) .019(3) .014(2) .019(3) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme calc #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 4519 #ActaC _refine_ls_number_parameters 451 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .101 #ActaC _refine_ls_R_factor_gt .048 #ActaC _refine_ls_wR_factor_all .067 #ActaC _refine_ls_wR_factor_ref .056 #ActaC _refine_ls_goodness_of_fit_all 1.284 #ActaC _refine_ls_goodness_of_fit_ref 1.421 #ActaC _refine_ls_shift/su_max .068 #ActaC _refine_ls_shift/su_mean .004 #ActaC _refine_diff_density_min -.371 #ActaC _refine_diff_density_max .486 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Cr2 Cl21 2.286(2) . . ? Cr2 Cl22 2.277(2) . . ? Cr2 Cl23 2.2900(16) . . ? Cr2 N21 2.094(5) . . ? Cr2 N23 2.130(5) . . ? Cr2 N25 2.106(3) . . ? N21 C211 1.479(7) . . ? N21 C22 1.477(9) . . ? N21 C26 1.482(6) . . ? C211 C212 1.530(9) . . ? C211 H211a .972(5) . . ? C211 H211b .978(7) . . ? C212 C213 1.520(9) . . ? C212 H212a .970(7) . . ? C212 H212b .961(8) . . ? C213 C214 1.441(14) . . ? C213 H213a .978(8) . . ? C213 H213b .976(7) . . ? C214 C215 1.160(15) . . ? C215 H215 .983(11) . . ? C22 N23 1.477(8) . . ? C22 H22a .965(6) . . ? C22 H22b .962(6) . . ? N23 C231 1.492(11) . . ? N23 C24 1.481(6) . . ? C231 C232 1.430(10) . . ? C231 H231a .935(7) . . ? C231 H231b .989(8) . . ? C232 C233 1.559(15) . . ? C232 H232a .978(8) . . ? C232 H232b .987(10) . . ? C233 C234 1.458(12) . . ? C233 H233a .982(9) . . ? C233 H233b .982(7) . . ? C234 C235 1.185(11) . . ? C235 H235 .972(8) . . ? C24 N25 1.466(9) . . ? C24 H24a .963(6) . . ? C24 H24b .969(6) . . ? N25 C251 1.479(8) . . ? N25 C26 1.478(8) . . ? C251 C252 1.519(7) . . ? C251 H251a .974(7) . . ? C251 H251b .957(7) . . ? C252 C253 1.523(10) . . ? C252 H252a .946(8) . . ? C252 H252b .969(7) . . ? C253 C254 1.470(13) . . ? C253 H253a .976(8) . . ? C253 H253b .969(6) . . ? C254 C255 1.150(15) . . ? C255 H255 .970(11) . . ? C26 H26a .959(7) . . ? C26 H26b .967(5) . . ? Cr1 Cl11 2.293(2) . . ? Cr1 Cl12 2.267(3) . . ? Cr1 Cl13 2.2919(16) . . ? Cr1 N11 2.094(5) . . ? Cr1 N13 2.101(5) . . ? Cr1 N15 2.099(3) . . ? N11 C111 1.482(8) . . ? N11 C12 1.478(9) . . ? N11 C16 1.486(6) . . ? C111 C112 1.527(9) . . ? C111 H111a .967(5) . . ? C111 H111b .976(7) . . ? C112 C113 1.519(10) . . ? C112 H112a .989(6) . . ? C112 H112b .952(8) . . ? C113 C114 1.470(13) . . ? C113 H113a .970(7) . . ? C113 H113b .968(7) . . ? C114 C115 1.161(14) . . ? C115 H115 .986(10) . . ? C12 N13 1.487(8) . . ? C12 H12a .950(5) . . ? C12 H12b .956(5) . . ? N13 C131 1.478(10) . . ? N13 C14 1.469(6) . . ? C131 C132 1.489(10) . . ? C131 H131a .987(7) . . ? C131 H131b .989(5) . . ? C132 C133 1.534(13) . . ? C132 H132a .971(8) . . ? C132 H132b .971(5) . . ? C133 C134 1.455(11) . . ? C133 H133a .986(9) . . ? C133 H133b .967(5) . . ? C134 C135 1.159(11) . . ? C135 H135 .979(8) . . ? C14 N15 1.480(9) . . ? C14 H14a .963(6) . . ? C14 H14b .951(5) . . ? N15 C151 1.482(7) . . ? N15 C16 1.473(8) . . ? C151 C152 1.521(7) . . ? C151 H151a .979(7) . . ? C151 H151b .957(6) . . ? C152 C153 1.525(9) . . ? C152 H152a .975(8) . . ? C152 H152b .975(7) . . ? C153 C154 1.454(13) . . ? C153 H153a .975(8) . . ? C153 H153b .965(6) . . ? C154 C155 1.155(15) . . ? C155 H155 .976(11) . . ? C16 H16a .986(5) . . ? C16 H16b .959(7) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Cr1 C111 3.221(7) . . ? Cr1 C12 2.632(7) . . ? Cr1 C131 3.200(8) . . ? Cr1 C14 2.624(5) . . ? Cr1 C151 3.236(5) . . ? Cr1 C16 2.611(5) . . ? Cr1 H111b 3.3348(13) . . ? Cr1 H12b 3.0442(13) . . ? Cr1 H131a 3.3383(17) . . ? Cr1 H131b 3.3572(16) . . ? Cr1 H14a 3.0406(16) . . ? Cr1 H151a 3.3452(14) . . ? Cr1 H16b 3.0485(16) . . ? Cr2 C211 3.211(7) . . ? Cr2 C22 2.621(7) . . ? Cr2 C231 3.359(9) . . ? Cr2 C24 2.628(5) . . ? Cr2 C251 3.221(5) . . ? Cr2 C26 2.622(6) . . ? Cr2 H211b 3.3356(13) . . ? Cr2 H22a 3.0487(14) . . ? Cr2 H24a 3.0646(15) . . ? Cr2 H251a 3.3381(15) . . ? Cr2 H26a 3.0415(16) . . ? Cl11 N13 3.248(5) . . ? Cl11 N15 3.232(5) . . ? Cl11 H24b 2.7944(17) . 1_566 ? Cl12 N11 3.249(5) . . ? Cl12 N15 3.255(5) . . ? Cl12 H135 2.683(2) . 1_565 ? Cl13 N11 3.228(4) . . ? Cl13 N13 3.262(4) . . ? Cl21 N23 3.275(6) . . ? Cl21 N25 3.260(5) . . ? Cl22 N21 3.229(6) . . ? Cl22 N25 3.203(5) . . ? Cl23 N21 3.240(4) . . ? Cl23 N23 3.336(4) . . ? N11 C112 2.516(9) . . ? N11 N13 2.275(8) . . ? N11 C131 3.636(10) . . ? N11 C14 2.768(7) . . ? N11 N15 2.283(6) . . ? N11 C151 3.639(7) . . ? N11 H111a 2.033(4) . . ? N11 H111b 2.029(5) . . ? N11 H112a 2.717(5) . . ? N11 H112b 2.684(5) . . ? N11 H12a 2.037(5) . . ? N11 H12b 2.043(5) . . ? N11 H14b 3.074(4) . . ? N11 H16a 2.068(3) . . ? N11 H16b 2.070(5) . . ? C111 C113 2.512(10) . . ? C111 C114 2.963(11) . . ? C111 C12 2.507(10) . . ? C111 N13 3.644(9) . . ? C111 N15 3.633(7) . . ? C111 C16 2.491(6) . . ? C111 H112a 2.062(6) . . ? C111 H112b 2.057(6) . . ? C111 H12b 2.638(8) . . ? C111 H16b 2.623(5) . . ? C112 C114 2.500(12) . . ? C112 H111a 2.045(6) . . ? C112 H111b 2.063(7) . . ? C112 H113a 2.070(7) . . ? C112 H113b 2.044(5) . . ? C113 C115 2.631(13) . . ? C113 H111a 2.656(8) . . ? C113 H111b 2.684(8) . . ? C113 H112a 2.062(5) . . ? C113 H112b 2.075(8) . . ? C114 H111b 2.609(8) . . ? C114 H113a 2.000(9) . . ? C114 H113b 2.008(10) . . ? C114 H115 2.147(10) . . ? C12 C131 2.523(10) . . ? C12 C14 2.417(7) . . ? C12 N15 2.783(8) . . ? C12 C16 2.433(9) . . ? C12 H111a 2.662(6) . . ? C12 H14b 2.559(4) . . ? C12 H16a 2.597(6) . . ? N13 C132 2.513(10) . . ? N13 N15 2.276(7) . . ? N13 C151 3.640(8) . . ? N13 C16 2.777(9) . . ? N13 H12a 2.037(5) . . ? N13 H12b 2.043(5) . . ? N13 H131a 2.029(5) . . ? N13 H131b 2.029(5) . . ? N13 H132a 2.748(6) . . ? N13 H132b 2.701(5) . . ? N13 H14a 2.036(4) . . ? N13 H14b 2.028(3) . . ? N13 H16a 3.108(5) . . ? C131 C133 2.479(12) . . ? C131 C14 2.486(9) . . ? C131 N15 3.622(10) . . ? C131 H12b 2.636(7) . . ? C131 H132a 2.043(7) . . ? C131 H132b 2.039(5) . . ? C131 H133b 2.648(8) . . ? C131 H14a 2.593(6) . . ? C132 C134 2.489(12) . . ? C132 H131a 2.042(8) . . ? C132 H131b 2.042(6) . . ? C132 H133a 2.090(8) . . ? C132 H133b 2.088(8) . . ? C133 C135 2.614(12) . . ? C133 H131a 2.616(10) . . ? C133 H131b 2.657(8) . . ? C133 H132a 2.072(9) . . ? C133 H132b 2.082(8) . . ? C134 H132a 2.666(8) . . ? C134 H133a 1.991(8) . . ? C134 H133b 1.998(6) . . ? C134 H135 2.138(8) . . ? C14 C151 2.508(10) . . ? C14 C16 2.420(9) . . ? C14 H12a 2.554(6) . . ? C14 H131a 2.693(6) . . ? C14 H151b 2.667(7) . . ? C14 H16a 2.581(7) . . ? N15 C152 2.510(6) . . ? N15 H12a 3.081(5) . . ? N15 H14a 2.039(5) . . ? N15 H14b 2.037(5) . . ? N15 H151a 2.011(5) . . ? N15 H151b 2.019(4) . . ? N15 H152a 2.640(3) . . ? N15 H152b 2.743(4) . . ? N15 H16a 2.052(5) . . ? N15 H16b 2.045(5) . . ? C151 C153 2.522(7) . . ? C151 C154 2.975(10) . . ? C151 C16 2.480(8) . . ? C151 H14a 2.625(8) . . ? C151 H152a 2.051(5) . . ? C151 H152b 2.064(6) . . ? C151 H16b 2.594(6) . . ? C152 C154 2.502(12) . . ? C152 C16 2.997(7) . . ? C152 H151a 2.059(6) . . ? C152 H151b 2.057(6) . . ? C152 H153a 2.058(6) . . ? C152 H153b 2.075(5) . . ? C153 C155 2.609(14) . . ? C153 H151b 2.651(6) . . ? C153 H152a 2.088(8) . . ? C153 H152b 2.071(7) . . ? C154 H151a 2.699(6) . . ? C154 H153a 1.986(10) . . ? C154 H153b 1.981(9) . . ? C154 H155 2.131(10) . . ? C16 H112a 2.680(6) . . ? C16 H12a 2.581(7) . . ? C16 H14b 2.571(6) . . ? C16 H151a 2.686(6) . . ? N21 C212 2.531(9) . . ? N21 N23 2.298(8) . . ? N21 C24 2.768(7) . . ? N21 N25 2.278(6) . . ? N21 C251 3.634(7) . . ? N21 H211a 2.031(4) . . ? N21 H211b 2.030(5) . . ? N21 H212a 2.742(5) . . ? N21 H212b 2.673(5) . . ? N21 H22a 2.040(6) . . ? N21 H22b 2.040(5) . . ? N21 H24b 3.082(4) . . ? N21 H26a 2.052(5) . . ? N21 H26b 2.053(3) . . ? C211 C213 2.519(10) . . ? C211 C22 2.510(10) . . ? C211 N23 3.657(8) . . ? C211 N25 3.631(7) . . ? C211 C26 2.493(6) . . ? C211 H212a 2.052(6) . . ? C211 H212b 2.047(6) . . ? C211 H22a 2.624(8) . . ? C211 H26a 2.613(5) . . ? C212 C214 2.500(12) . . ? C212 H211a 2.054(7) . . ? C212 H211b 2.060(7) . . ? C212 H213a 2.076(7) . . ? C212 H213b 2.065(5) . . ? C213 C215 2.601(15) . . ? C213 H211a 2.645(8) . . ? C213 H212a 2.061(6) . . ? C213 H212b 2.079(8) . . ? C214 H211b 2.682(9) . . ? C214 H213a 1.971(9) . . ? C214 H213b 1.977(11) . . ? C214 H215 2.143(11) . . ? C22 C231 2.526(11) . . ? C22 C24 2.404(8) . . ? C22 N25 2.761(8) . . ? C22 C26 2.416(10) . . ? C22 H211a 2.676(6) . . ? C22 H24b 2.559(5) . . ? C22 H26b 2.574(7) . . ? N23 C232 2.480(11) . . ? N23 N25 2.292(8) . . ? N23 C251 3.647(9) . . ? N23 C26 2.797(9) . . ? N23 H22a 2.048(5) . . ? N23 H22b 2.044(5) . . ? N23 H231a 2.014(6) . . ? N23 H231b 2.017(6) . . ? N23 H232a 2.653(5) . . ? N23 H232b 2.765(6) . . ? N23 H24a 2.051(4) . . ? N23 H24b 2.048(4) . . ? N23 H26b 3.110(6) . . ? C231 C233 2.465(13) . . ? C231 C234 2.960(14) . . ? C231 C24 2.425(11) . . ? C231 N25 3.623(11) . . ? C231 H232a 2.020(5) . . ? C231 H232b 1.997(7) . . ? C231 H233a 2.673(9) . . ? C231 H24a 2.535(8) . . ? C232 C234 2.517(14) . . ? C232 H231a 1.956(6) . . ? C232 H231b 1.949(8) . . ? C232 H233a 2.088(10) . . ? C232 H233b 2.129(10) . . ? C233 C235 2.643(12) . . ? C233 H231a 2.651(9) . . ? C233 H231b 2.545(10) . . ? C233 H232a 2.112(10) . . ? C233 H232b 2.084(10) . . ? C234 H231a 2.647(10) . . ? C234 H233a 2.010(8) . . ? C234 H233b 2.010(6) . . ? C234 H235 2.156(8) . . ? C24 C251 2.490(11) . . ? C24 C26 2.414(10) . . ? C24 H22b 2.562(6) . . ? C24 H231a 2.611(7) . . ? C24 H231b 2.555(7) . . ? C24 H251b 2.651(7) . . ? C24 H26b 2.571(7) . . ? N25 C252 2.513(6) . . ? N25 H22b 3.074(5) . . ? N25 H24a 2.038(5) . . ? N25 H24b 2.032(5) . . ? N25 H251a 2.007(6) . . ? N25 H251b 2.008(5) . . ? N25 H252a 2.656(3) . . ? N25 H252b 2.751(4) . . ? N25 H26a 2.047(5) . . ? N25 H26b 2.044(5) . . ? C251 C253 2.506(7) . . ? C251 C254 2.967(11) . . ? C251 C26 2.495(8) . . ? C251 H24a 2.606(8) . . ? C251 H252a 2.038(5) . . ? C251 H252b 2.048(6) . . ? C251 H26a 2.612(6) . . ? C252 C254 2.505(12) . . ? C252 H251a 2.058(5) . . ? C252 H251b 2.046(6) . . ? C252 H253a 2.061(6) . . ? C252 H253b 2.073(6) . . ? C253 C255 2.619(14) . . ? C253 H251b 2.636(6) . . ? C253 H252a 2.064(8) . . ? C253 H252b 2.045(7) . . ? C254 H251a 2.665(7) . . ? C254 H253a 2.007(10) . . ? C254 H253b 2.005(8) . . ? C254 H255 2.119(10) . . ? C26 H22b 2.566(7) . . ? C26 H24b 2.564(7) . . ? C26 H251a 2.686(6) . . ? H111a H111b 1.5524(4) . . ? H111a H112b 2.3806(8) . . ? H111b H112a 2.3546(8) . . ? H112a H112b 1.5524(4) . . ? H112a H113a 2.3626(8) . . ? H112b H113a 2.3821(6) . . ? H112b H113b 2.3567(9) . . ? H113a H113b 1.5511(6) . . ? H12a H12b 1.5506(5) . . ? H12a H14b 2.3307(8) . . ? H12a H16a 2.3704(7) . . ? H131a H131b 1.5515(5) . . ? H131a H132b 2.3890(9) . . ? H131b H132a 2.3555(9) . . ? H132a H132b 1.5513(5) . . ? H132b H133a 2.3917(10) . . ? H133a H133b 1.5511(5) . . ? H14a H14b 1.5515(4) . . ? H14b H16a 2.3560(6) . . ? H151a H151b 1.5513(5) . . ? H151a H152b 2.3354(7) . . ? H152a H152b 1.5515(5) . . ? H152a H153a 2.3581(7) . . ? H152b H153b 2.3629(7) . . ? H153a H153b 1.5515(5) . . ? H16a H16b 1.5515(8) . . ? H211a H211b 1.5524(4) . . ? H211a H212b 2.3843(8) . . ? H211b H212a 2.3339(7) . . ? H212a H212b 1.5522(4) . . ? H212a H213a 2.3789(8) . . ? H212b H213a 2.3872(6) . . ? H212b H213b 2.3726(8) . . ? H213a H213b 1.5513(6) . . ? H22a H22b 1.5508(5) . . ? H22a H232b 2.3367(7) . . ? H22b H24b 2.3390(8) . . ? H22b H26b 2.3487(7) . . ? H231a H231b 1.5514(4) . . ? H231a H232b 2.2566(6) . . ? H231b H232a 2.3439(6) . . ? H231b H233a 2.3711(9) . . ? H231b H24a 2.2885(8) . . ? H232a H232b 1.5514(4) . . ? H232a H233b 2.3976(9) . . ? H233a H233b 1.5515(5) . . ? H24a H24b 1.5514(4) . . ? H24b H26b 2.3426(7) . . ? H251a H251b 1.5513(5) . . ? H251a H252b 2.3137(7) . . ? H251b H252a 2.3857(7) . . ? H252a H252b 1.5516(5) . . ? H252a H253a 2.3551(7) . . ? H252a H253b 2.3720(7) . . ? H252b H253b 2.3551(7) . . ? H253a H253b 1.5515(5) . . ? H26a H26b 1.5513(8) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Cl21 Cr2 Cl22 98.69(8) . . . ? Cl21 Cr2 Cl23 100.07(7) . . . ? Cl21 Cr2 N21 157.62(11) . . . ? Cl21 Cr2 N23 95.66(16) . . . ? Cl21 Cr2 N25 95.76(14) . . . ? Cl22 Cr2 Cl23 98.39(7) . . . ? Cl22 Cr2 N21 95.12(17) . . . ? Cl22 Cr2 N23 155.97(15) . . . ? Cl22 Cr2 N25 93.82(17) . . . ? Cl23 Cr2 N21 95.20(12) . . . ? Cl23 Cr2 N23 97.94(13) . . . ? Cl23 Cr2 N25 158.25(16) . . . ? N21 Cr2 N23 65.9(2) . . . ? N21 Cr2 N25 65.70(16) . . . ? N23 Cr2 N25 65.5(2) . . . ? Cr2 N21 C211 127.1(3) . . . ? Cr2 N21 C22 92.8(4) . . . ? Cr2 N21 C26 92.7(3) . . . ? C211 N21 C22 116.2(5) . . . ? C211 N21 C26 114.7(5) . . . ? C22 N21 C26 109.5(4) . . . ? N21 C211 C212 114.5(4) . . . ? N21 C211 H211a 110.1(6) . . . ? N21 C211 H211b 109.7(6) . . . ? C212 C211 H211a 108.3(6) . . . ? C212 C211 H211b 108.4(7) . . . ? H211a C211 H211b 105.5(4) . . . ? C211 C212 C213 111.4(4) . . . ? C211 C212 H212a 108.3(6) . . . ? C211 C212 H212b 108.4(7) . . . ? C213 C212 H212a 109.8(7) . . . ? C213 C212 H212b 111.9(7) . . . ? H212a C212 H212b 107.0(5) . . . ? C212 C213 C214 115.2(7) . . . ? C212 C213 H213a 110.6(5) . . . ? C212 C213 H213b 109.6(8) . . . ? C214 C213 H213a 107.6(8) . . . ? C214 C213 H213b 108.2(5) . . . ? H213a C213 H213b 105.1(8) . . . ? C213 C214 C215 179.0(8) . . . ? C214 C215 H215 178.2(12) . . . ? N21 C22 N23 102.1(5) . . . ? N21 C22 H22a 111.6(4) . . . ? N21 C22 H22b 111.7(6) . . . ? N23 C22 H22a 112.2(6) . . . ? N23 C22 H22b 112.1(4) . . . ? H22a C22 H22b 107.1(7) . . . ? Cr2 N23 C22 91.4(4) . . . ? Cr2 N23 C231 135.3(4) . . . ? Cr2 N23 C24 91.6(4) . . . ? C22 N23 C231 116.6(6) . . . ? C22 N23 C24 108.7(5) . . . ? C231 N23 C24 109.3(4) . . . ? N23 C231 C232 116.1(6) . . . ? N23 C231 H231a 110.0(7) . . . ? N23 C231 H231b 107.0(8) . . . ? C232 C231 H231a 109.8(9) . . . ? C232 C231 H231b 105.9(7) . . . ? H231a C231 H231b 107.4(6) . . . ? C231 C232 C233 111.0(6) . . . ? C231 C232 H232a 112.7(9) . . . ? C231 C232 H232b 110.1(8) . . . ? C233 C232 H232a 110.6(8) . . . ? C233 C232 H232b 107.7(9) . . . ? H232a C232 H232b 104.3(7) . . . ? C232 C233 C234 113.0(7) . . . ? C232 C233 H233a 108.4(9) . . . ? C232 C233 H233b 111.8(6) . . . ? C234 C233 H233a 109.4(6) . . . ? C234 C233 H233b 109.4(9) . . . ? H233a C233 H233b 104.4(8) . . . ? C233 C234 C235 179.1(10) . . . ? C234 C235 H235 178.3(11) . . . ? N23 C24 N25 102.1(4) . . . ? N23 C24 H24a 112.3(6) . . . ? N23 C24 H24b 111.7(6) . . . ? N25 C24 H24a 112.4(6) . . . ? N25 C24 H24b 111.5(6) . . . ? H24a C24 H24b 106.8(4) . . . ? Cr2 N25 C24 93.0(3) . . . ? Cr2 N25 C251 127.0(4) . . . ? Cr2 N25 C26 92.4(2) . . . ? C24 N25 C251 115.5(4) . . . ? C24 N25 C26 110.2(5) . . . ? C251 N25 C26 115.1(5) . . . ? N25 C251 C252 113.9(5) . . . ? N25 C251 H251a 108.0(4) . . . ? N25 C251 H251b 109.2(6) . . . ? C252 C251 H251a 109.3(6) . . . ? C252 C251 H251b 109.3(4) . . . ? H251a C251 H251b 106.8(6) . . . ? C251 C252 C253 110.9(6) . . . ? C251 C252 H252a 109.3(7) . . . ? C251 C252 H252b 108.8(4) . . . ? C253 C252 H252a 111.3(5) . . . ? C253 C252 H252b 108.2(7) . . . ? H252a C252 H252b 108.2(7) . . . ? C252 C253 C254 113.6(5) . . . ? C252 C253 H253a 109.2(7) . . . ? C252 C253 H253b 110.6(7) . . . ? C254 C253 H253a 108.6(7) . . . ? C254 C253 H253b 108.8(8) . . . ? H253a C253 H253b 105.8(5) . . . ? C253 C254 C255 178.3(7) . . . ? C254 C255 H255 177.8(10) . . . ? N21 C26 N25 100.6(5) . . . ? N21 C26 H26a 112.6(4) . . . ? N21 C26 H26b 112.2(6) . . . ? N25 C26 H26a 112.4(6) . . . ? N25 C26 H26b 111.7(4) . . . ? H26a C26 H26b 107.3(6) . . . ? Cl11 Cr1 Cl12 98.75(8) . . . ? Cl11 Cr1 Cl13 100.66(7) . . . ? Cl11 Cr1 N11 156.72(11) . . . ? Cl11 Cr1 N13 95.22(15) . . . ? Cl11 Cr1 N15 94.65(14) . . . ? Cl12 Cr1 Cl13 98.10(8) . . . ? Cl12 Cr1 N11 96.25(17) . . . ? Cl12 Cr1 N13 158.08(15) . . . ? Cl12 Cr1 N15 96.33(17) . . . ? Cl13 Cr1 N11 94.70(12) . . . ? Cl13 Cr1 N13 95.79(13) . . . ? Cl13 Cr1 N15 157.05(16) . . . ? N11 Cr1 N13 65.7(2) . . . ? N11 Cr1 N15 65.98(16) . . . ? N13 Cr1 N15 65.64(19) . . . ? Cr1 N11 C111 127.7(3) . . . ? Cr1 N11 C12 93.3(4) . . . ? Cr1 N11 C16 92.1(3) . . . ? C111 N11 C12 115.8(5) . . . ? C111 N11 C16 114.1(5) . . . ? C12 N11 C16 110.3(4) . . . ? N11 C111 C112 113.5(4) . . . ? N11 C111 H111a 110.5(6) . . . ? N11 C111 H111b 109.5(5) . . . ? C112 C111 H111a 108.0(6) . . . ? C112 C111 H111b 109.1(7) . . . ? H111a C111 H111b 106.0(4) . . . ? C111 C112 C113 111.1(4) . . . ? C111 C112 H112a 108.2(6) . . . ? C111 C112 H112b 110.0(7) . . . ? C113 C112 H112a 108.8(7) . . . ? C113 C112 H112b 112.2(7) . . . ? H112a C112 H112b 106.3(5) . . . ? C112 C113 C114 113.5(6) . . . ? C112 C113 H113a 110.6(5) . . . ? C112 C113 H113b 108.5(8) . . . ? C114 C113 H113a 108.4(8) . . . ? C114 C113 H113b 109.2(5) . . . ? H113a C113 H113b 106.4(7) . . . ? C113 C114 C115 179.3(6) . . . ? C114 C115 H115 178.9(10) . . . ? N11 C12 N13 100.2(5) . . . ? N11 C12 H12a 112.2(6) . . . ? N11 C12 H12b 112.4(5) . . . ? N13 C12 H12a 111.5(4) . . . ? N13 C12 H12b 111.6(6) . . . ? H12a C12 H12b 108.8(7) . . . ? Cr1 N13 C12 92.7(4) . . . ? Cr1 N13 C131 125.9(3) . . . ? Cr1 N13 C14 92.9(4) . . . ? C12 N13 C131 116.6(5) . . . ? C12 N13 C14 109.6(4) . . . ? C131 N13 C14 115.0(4) . . . ? N13 C131 C132 115.8(5) . . . ? N13 C131 H131a 109.2(7) . . . ? N13 C131 H131b 109.0(6) . . . ? C132 C131 H131a 109.4(6) . . . ? C132 C131 H131b 109.2(7) . . . ? H131a C131 H131b 103.5(6) . . . ? C131 C132 C133 110.1(6) . . . ? C131 C132 H132a 110.5(6) . . . ? C131 C132 H132b 110.1(7) . . . ? C133 C132 H132a 109.6(7) . . . ? C133 C132 H132b 110.4(6) . . . ? H132a C132 H132b 106.0(6) . . . ? C132 C133 C134 112.8(6) . . . ? C132 C133 H133a 110.2(8) . . . ? C132 C133 H133b 111.2(7) . . . ? C134 C133 H133a 107.7(7) . . . ? C134 C133 H133b 109.5(8) . . . ? H133a C133 H133b 105.2(7) . . . ? C133 C134 C135 178.3(9) . . . ? C134 C135 H135 178.7(8) . . . ? N13 C14 N15 101.0(4) . . . ? N13 C14 H14a 112.0(5) . . . ? N13 C14 H14b 112.1(6) . . . ? N15 C14 H14a 111.4(6) . . . ? N15 C14 H14b 112.0(6) . . . ? H14a C14 H14b 108.3(5) . . . ? Cr1 N15 C14 92.7(3) . . . ? Cr1 N15 C151 128.5(4) . . . ? Cr1 N15 C16 92.2(2) . . . ? C14 N15 C151 115.7(4) . . . ? C14 N15 C16 110.0(5) . . . ? C151 N15 C16 114.1(5) . . . ? N15 C151 C152 113.4(5) . . . ? N15 C151 H151a 107.8(4) . . . ? N15 C151 H151b 109.8(6) . . . ? C152 C151 H151a 109.0(6) . . . ? C152 C151 H151b 110.1(4) . . . ? H151a C151 H151b 106.5(6) . . . ? C151 C152 C153 111.7(6) . . . ? C151 C152 H152a 108.5(6) . . . ? C151 C152 H152b 109.6(5) . . . ? C153 C152 H152a 111.4(5) . . . ? C153 C152 H152b 110.0(7) . . . ? H152a C152 H152b 105.4(7) . . . ? C152 C153 C154 114.3(5) . . . ? C152 C153 H153a 108.8(7) . . . ? C152 C153 H153b 110.9(7) . . . ? C154 C153 H153a 108.0(7) . . . ? C154 C153 H153b 108.3(7) . . . ? H153a C153 H153b 106.2(5) . . . ? C153 C154 C155 178.3(6) . . . ? C154 C155 H155 177.9(9) . . . ? N11 C16 N15 100.9(4) . . . ? N11 C16 H16a 112.0(6) . . . ? N11 C16 H16b 113.9(4) . . . ? N15 C16 H16a 111.6(4) . . . ? N15 C16 H16b 112.7(6) . . . ? H16a C16 H16b 105.8(5) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min -16 _reflns_limit_k_max 15 _reflns_limit_l_min -15 _reflns_limit_l_max 14 _reflns_number_total 7710 #ActaC _reflns_number_gt 4519 #ActaC _reflns_threshold_expression refl_observed_if_I____>2.000_sigma(I___) _reflns_d_resolution_high .841 _reflns_d_resolution_low 13.932 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 2.6841 #======================================================================= # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? ; _publ_requested_journal 'J.Chem.Soc., Dalton' _publ_requested_category ? _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Baker, Murray V.' . ; Department of Chemistry University of Western Australia, Nedlands, WA 6907 Australia. ; 'Brown, David H.' . ; Department of Chemistry University of Western Australia, Nedlands, WA 6907 Australia. ; 'Skelton, Brian W.' . ; Department of Chemistry University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Department of Chemistry University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; 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 ; ? ; #==END data_dbcrb # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C6 H15 Br3 Cr1 N3' _chemical_formula_moiety ? _chemical_formula_weight 420.92 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p_n_m_a _symmetry_space_group_name_Hall -p_2ac_2n loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,1/2+z +x,1/2-y,+z _cell_length_a 15.476(2) _cell_length_b 12.1587(10) _cell_length_c 7.0261(8) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 1322.1(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.115 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5613 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 9.90 _exptl_crystal_description bar _exptl_crystal_size_max .35 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .20 _exptl_crystal_size_rad ? _exptl_crystal_colour purple #<< use NfA code _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 .398 _exptl_absorpt_correction_T_max .695 _diffrn_reflns_number 14359 _reflns_number_total 1745 _reflns_Friedel_coverage ? _reflns_number_gt 1449 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.07 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .031 _refine_ls_wR_factor_ref .044 _refine_ls_goodness_of_fit_ref 1.585 _refine_ls_number_reflns 1449 _refine_ls_number_parameters 68 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .044 _refine_diff_density_min -1.27 _refine_diff_density_max 1.132 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1462(213) _refine_ls_abs_structure_details none _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 24 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 60 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 12 -.374 2.456 '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 12 .004 .003 '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 .63407(5) .25000 -.01184(10) .0256(4) Uani ? ? 1.00000 ? ? Br1 .58893(3) .40336(3) -.21229(5) .0476(3) Uani ? ? 1.00000 ? ? Br2 .78741(3) .25000 -.08983(9) .0510(4) Uani ? ? 1.00000 ? ? N1 .5211(2) .25000 .1550(6) .033(2) Uani ? ? 1.00000 ? ? C1 .4306(4) .25000 .0970(10) .065(4) Uani ? ? 1.00000 ? ? C2 .5489(2) .3490(3) .2610(5) .0377(19) Uani ? ? 1.00000 ? ? N3 .64251(19) .3440(2) .2395(4) .0325(15) Uani ? ? 1.00000 ? ? C3 .6865(4) .4496(4) .2756(6) .062(3) Uani ? ? 1.00000 ? ? C4 .6769(3) .25000 .3487(7) .036(3) Uani ? ? 1.00000 ? ? H1a .39404 .25000 .19772 .10200 Uiso ? ? 1.00000 ? ? H1b .42126 .18561 .01796 .10200 Uiso ? ? 1.00000 ? ? H2a .52589 .41380 .20650 .04700 Uiso ? ? 1.00000 ? ? H2b .53219 .34471 .39168 .04700 Uiso ? ? 1.00000 ? ? H3a .67676 .47408 .40395 .08800 Uiso ? ? 1.00000 ? ? H3b .66242 .50645 .19261 .08800 Uiso ? ? 1.00000 ? ? H3c .74612 .44520 .25240 .08800 Uiso ? ? 1.00000 ? ? H4a .65445 .25000 .47663 .05800 Uiso ? ? 1.00000 ? ? H4b .73720 .25000 .35184 .05800 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 .0267(4) .0245(3) .0256(4) .00000 .0020(3) .00000 Br1 .0683(3) .0379(2) .0367(3) .01452(17) .00167(18) .00685(14) Br2 .0335(3) .0579(4) .0614(4) .00000 .0146(3) .00000 N1 .024(2) .043(2) .032(2) .00000 -.0004(17) .00000 C1 .025(3) .106(5) .064(4) .00000 -.002(3) .00000 C2 .041(2) .0390(18) .0333(18) .0115(16) .0059(16) -.0018(14) N3 .0375(16) .0271(14) .0329(14) -.0057(12) -.0005(12) -.0045(11) C3 .089(3) .044(2) .052(2) -.031(2) .002(2) -.012(2) C4 .034(3) .044(3) .032(2) .00000 -.008(2) .00000 # 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 Br1 . . 2.4390(6) ? Cr Br2 . . 2.4355(9) ? Cr N1 . . 2.104(4) ? Cr N3 . . 2.108(3) ? Cr Br1 . 8 2.4390(6) ? Cr N3 . 8 2.108(3) ? N1 C1 . . 1.459(7) ? N1 C2 . . 1.479(4) ? N1 C2 . 8 1.479(4) ? C1 H1a . . .906(7) ? C1 H1b . . .971(4) ? C1 H1b . 8 .971(4) ? C2 N3 . . 1.458(5) ? C2 H2a . . .945(4) ? C2 H2b . . .955(3) ? N3 C3 . . 1.475(6) ? N3 C4 . . 1.476(4) ? C3 H3a . . .962(4) ? C3 H3b . . .979(5) ? C3 H3c . . .938(6) ? C4 H4a . . .964(5) ? C4 H4b . . .934(5) ? 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 Br1 Cr Br2 . . . 98.58(2) ? Br1 Cr N1 . . . 94.80(7) ? Br1 Cr N3 . . . 94.98(7) ? Br1 Cr Br1 . . 8 99.73(3) ? Br1 Cr N3 . . 8 156.39(8) ? Br2 Cr N1 . . . 159.16(11) ? Br2 Cr N3 . . . 97.36(9) ? Br2 Cr Br1 . . 8 98.58(2) ? Br2 Cr N3 . . 8 97.36(9) ? N1 Cr N3 . . . 65.47(12) ? N1 Cr Br1 . . 8 94.80(7) ? N1 Cr N3 . . 8 65.47(12) ? N3 Cr Br1 . . 8 156.39(8) ? N3 Cr N3 . . 8 65.71(11) ? Br1 Cr N3 8 . 8 94.98(7) ? Cr N1 C1 . . . 130.0(4) ? Cr N1 C2 . . . 92.3(2) ? Cr N1 C2 . . 8 92.3(2) ? C1 N1 C2 . . . 114.8(3) ? C1 N1 C2 . . 8 114.8(3) ? C2 N1 C2 . . 8 108.9(3) ? N1 C1 H1a . . . 112.5(6) ? N1 C1 H1b . . . 107.6(4) ? N1 C1 H1b . . 8 107.6(4) ? H1a C1 H1b . . . 110.7(4) ? H1a C1 H1b . . 8 110.7(4) ? H1b C1 H1b . . 8 107.5(7) ? N1 C2 N3 . . . 101.7(3) ? N1 C2 H2a . . . 111.4(3) ? N1 C2 H2b . . . 111.2(3) ? N3 C2 H2a . . . 111.5(3) ? N3 C2 H2b . . . 111.5(3) ? H2a C2 H2b . . . 109.5(3) ? Cr N3 C2 . . . 92.74(19) ? Cr N3 C3 . . . 130.2(2) ? Cr N3 C4 . . . 92.1(2) ? C2 N3 C3 . . . 113.9(3) ? C2 N3 C4 . . . 109.6(3) ? C3 N3 C4 . . . 114.7(3) ? N3 C3 H3a . . . 111.0(4) ? N3 C3 H3b . . . 109.6(4) ? N3 C3 H3c . . . 112.0(4) ? H3a C3 H3b . . . 106.2(5) ? H3a C3 H3c . . . 109.6(5) ? H3b C3 H3c . . . 108.1(5) ? N3 C4 H4a . . . 110.8(3) ? N3 C4 H4b . . . 111.9(3) ? N3 C4 N3 . . 8 101.6(3) ? H4a C4 H4b . . . 109.7(5) ? H4a C4 N3 . . 8 110.8(3) ? H4b C4 N3 . . 8 111.9(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #----------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cr C2 2.620(4) . . ? Cr C2 2.620(4) . 8 ? Cr C4 2.618(5) . . ? Br1 Br1 3.7294(6) . 8 ? Br1 Br2 3.6949(7) . . ? Br1 N1 3.352(3) . . ? Br1 C2 3.447(3) . . ? Br1 N3 3.359(3) . . ? Br1 H2a 2.8463(5) . '5 665' ? Br1 H2a 3.1026(5) . . ? Br1 H2b 3.0037(5) . '1 554' ? Br1 H3a 3.1396(5) . '1 554' ? Br1 H3c 3.1572(5) . '2 664' ? Br1 H4a 3.0467(4) . '1 554' ? Br2 N3 3.419(3) . 8 ? Br2 N3 3.419(3) . . ? Br2 H4b 3.1991(7) . . ? N1 N3 2.278(4) . . ? N1 N3 2.278(4) . 8 ? N1 C4 2.768(6) . . ? N1 H1a 1.990(4) . . ? N1 H1b 1.982(4) . . ? N1 H1b 1.982(4) . 8 ? N1 H2a 2.0256(8) . . ? N1 H2a 2.0256(8) . 8 ? N1 H2b 2.030(3) . 8 ? N1 H2b 2.030(3) . . ? C1 C2 2.475(7) . 8 ? C1 C2 2.475(7) . . ? C1 H2a 2.595(4) . . ? C1 H2a 2.595(4) . 8 ? C2 C2 2.408(5) . 8 ? C2 N3 2.763(5) . 8 ? C2 C3 2.459(7) . . ? C2 C4 2.398(6) . . ? C2 H1b 2.644(4) . 8 ? C2 H2b 2.541(4) . 8 ? C2 H3a 2.691(4) . . ? C2 H3b 2.643(4) . . ? C2 H4a 2.533(4) . . ? N3 N3 2.287(4) . 8 ? N3 H2a 2.008(3) . . ? N3 H2b 2.015(3) . . ? N3 H3a 2.029(3) . . ? N3 H3b 2.026(3) . . ? N3 H3c 2.023(3) . . ? N3 H4a 2.029(3) . . ? N3 H4b 2.019(3) . . ? C3 C4 2.485(5) . . ? C3 H2a 2.570(6) . . ? C3 H4b 2.606(5) . . ? C4 H2b 2.536(5) . 8 ? C4 H2b 2.536(5) . . ? C4 H3c 2.691(2) . . ? C4 H3c 2.691(2) . 8 ? H1a H1b 1.54453(12) . 8 ? H1a H1b 1.54453(12) . . ? H1b H1b 1.56580(13) . 8 ? H2a H2b 1.55178(13) . . ? H2a H3b 2.3964(2) . . ? H2b H2b 2.30310(19) . 8 ? H2b H4a 2.2940(2) . . ? H3a H3b 1.55212(16) . . ? H3a H3c 1.55219(13) . . ? H3b H3c 1.55208(14) . . ? H4a H4b 1.55202(15) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 804 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 20 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 9 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 7.726 _diffrn_reflns_av_sigmaI/netI .033 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .04 _refine_ls_wR_factor_all .045 _refine_ls_goodness_of_fit_all 1.489 _refine_ls_shift/su_mean .004