# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 186/1667
 
data_scotf
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C44 H56 N2 O2' 
_chemical_formula_weight          644.91 
 
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' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
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                    18.817(2) 
_cell_length_b                    11.504(2) 
_cell_length_c                    18.627(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.337(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      3888.6(9) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     9101 
_cell_measurement_theta_min       2.10 
_cell_measurement_theta_max       28.51 
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             Yellow 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.102 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1400 
_exptl_absorpt_coefficient_mu     0.066 
_exptl_absorpt_correction_type    SADABS 
_exptl_absorpt_correction_T_min   0.796 
_exptl_absorpt_correction_T_max   0.962 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       200(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             22684 
_diffrn_reflns_av_R_equivalents   0.0691 
_diffrn_reflns_av_sigmaI/netI     0.1164 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.10 
_diffrn_reflns_theta_max          28.51 
_reflns_number_total              9101 
_reflns_number_gt                 3973 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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^)+(0.0870P)^2^+0.0000P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          9101 
_refine_ls_number_parameters      447 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1829 
_refine_ls_R_factor_gt            0.0698 
_refine_ls_wR_factor_ref          0.1982 
_refine_ls_wR_factor_gt           0.1534 
_refine_ls_goodness_of_fit_ref    0.983 
_refine_ls_restrained_S_all       0.983 
_refine_ls_shift/su_max           0.073 
_refine_ls_shift/su_mean          0.003 
 
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 
N1 N 0.38037(12) 0.04748(18) 0.18283(12) 0.0318(5) Uani 1 1 d . . . 
N2 N 0.26988(12) -0.13556(18) 0.08475(12) 0.0338(5) Uani 1 1 d . . . 
O1 O 0.37401(10) 0.18547(16) 0.07182(10) 0.0413(5) Uani 1 1 d . . . 
H1B H 0.3807 0.2137 0.0325 0.062 Uiso 1 1 calc R . . 
O2 O 0.21690(10) -0.09178(17) 0.19516(10) 0.0458(5) Uani 1 1 d . . . 
H2B H 0.2136 -0.0712 0.2374 0.069 Uiso 1 1 calc R . . 
C1 C 0.44022(17) -0.3700(2) 0.17475(18) 0.0483(8) Uani 1 1 d . . . 
H1C H 0.4604 -0.4329 0.2097 0.072 Uiso 1 1 calc R . . 
H1D H 0.4733 -0.3551 0.1431 0.072 Uiso 1 1 calc R . . 
H1E H 0.3916 -0.3927 0.1436 0.072 Uiso 1 1 calc R . . 
C2 C 0.43304(14) -0.2615(2) 0.21755(16) 0.0350(7) Uani 1 1 d . . . 
C3 C 0.44519(15) -0.2664(3) 0.29396(17) 0.0425(7) Uani 1 1 d . . . 
H3A H 0.4612 -0.3373 0.3192 0.051 Uiso 1 1 calc R . . 
C4 C 0.43462(16) -0.1705(3) 0.33449(15) 0.0438(8) Uani 1 1 d . . . 
H4A H 0.4430 -0.1762 0.3869 0.053 Uiso 1 1 calc R . . 
C5 C 0.41196(15) -0.0667(2) 0.29904(14) 0.0375(7) Uani 1 1 d . . . 
H5A H 0.4040 -0.0009 0.3268 0.045 Uiso 1 1 calc R . . 
C6 C 0.40079(14) -0.0586(2) 0.22247(14) 0.0308(6) Uani 1 1 d . . . 
C7 C 0.41169(14) -0.1559(2) 0.18108(14) 0.0308(6) Uani 1 1 d . . . 
C8 C 0.40053(15) -0.1441(2) 0.09892(15) 0.0313(6) Uani 1 1 d . . . 
C9 C 0.32951(15) -0.1361(2) 0.05091(15) 0.0348(7) Uani 1 1 d . . . 
C10 C 0.31927(16) -0.1208(2) -0.02494(16) 0.0438(7) Uani 1 1 d . . . 
H10A H 0.2710 -0.1119 -0.0568 0.053 Uiso 1 1 calc R . . 
C11 C 0.37974(19) -0.1186(3) -0.05388(17) 0.0508(8) Uani 1 1 d . . . 
H11A H 0.3728 -0.1107 -0.1060 0.061 Uiso 1 1 calc R . . 
C12 C 0.45036(17) -0.1280(2) -0.00732(17) 0.0468(8) Uani 1 1 d . . . 
H12A H 0.4914 -0.1264 -0.0280 0.056 Uiso 1 1 calc R . . 
C13 C 0.46192(15) -0.1395(2) 0.06887(16) 0.0382(7) Uani 1 1 d . . . 
C14 C 0.53926(16) -0.1427(3) 0.11847(18) 0.0521(8) Uani 1 1 d . . . 
H14A H 0.5741 -0.1250 0.0891 0.078 Uiso 1 1 calc R . . 
H14B H 0.5497 -0.2203 0.1405 0.078 Uiso 1 1 calc R . . 
H14C H 0.5444 -0.0849 0.1582 0.078 Uiso 1 1 calc R . . 
C15 C 0.33908(15) 0.1200(2) 0.20463(15) 0.0348(7) Uani 1 1 d . . . 
H15A H 0.3221 0.1007 0.2468 0.042 Uiso 1 1 calc R . . 
C16 C 0.31681(15) 0.2309(2) 0.16788(14) 0.0328(6) Uani 1 1 d . . . 
C17 C 0.27641(15) 0.3076(2) 0.20059(15) 0.0345(7) Uani 1 1 d . . . 
H17A H 0.2644 0.2852 0.2451 0.041 Uiso 1 1 calc R . . 
C18 C 0.25386(14) 0.4142(2) 0.16975(14) 0.0329(6) Uani 1 1 d . . . 
C19 C 0.27236(14) 0.4409(2) 0.10314(15) 0.0350(7) Uani 1 1 d . . . 
H19A H 0.2568 0.5140 0.0807 0.042 Uiso 1 1 calc R . . 
C20 C 0.31163(14) 0.3686(2) 0.06755(14) 0.0323(6) Uani 1 1 d . . . 
C21 C 0.33476(14) 0.2616(2) 0.10188(14) 0.0322(6) Uani 1 1 d . . . 
C22 C 0.21269(16) 0.5029(2) 0.20518(16) 0.0391(7) Uani 1 1 d . . . 
C23 C 0.19671(19) 0.4554(3) 0.27628(18) 0.0570(9) Uani 1 1 d . . . 
H23A H 0.1650 0.3867 0.2641 0.085 Uiso 1 1 calc R . . 
H23B H 0.1718 0.5152 0.2982 0.085 Uiso 1 1 calc R . . 
H23C H 0.2432 0.4339 0.3120 0.085 Uiso 1 1 calc R . . 
C24 C 0.26117(18) 0.6122(2) 0.22600(18) 0.0543(9) Uani 1 1 d . . . 
H24A H 0.2705 0.6456 0.1810 0.082 Uiso 1 1 calc R . . 
H24B H 0.3081 0.5909 0.2610 0.082 Uiso 1 1 calc R . . 
H24C H 0.2357 0.6694 0.2492 0.082 Uiso 1 1 calc R . . 
C25 C 0.13937(17) 0.5368(3) 0.15017(18) 0.0527(8) Uani 1 1 d . . . 
H25A H 0.1488 0.5669 0.1043 0.079 Uiso 1 1 calc R . . 
H25B H 0.1151 0.5969 0.1725 0.079 Uiso 1 1 calc R . . 
H25C H 0.1074 0.4683 0.1386 0.079 Uiso 1 1 calc R . . 
C26 C 0.32869(15) 0.4047(2) -0.00597(15) 0.0379(7) Uani 1 1 d . . . 
C27 C 0.29783(19) 0.5246(3) -0.03263(18) 0.0571(9) Uani 1 1 d . . . 
H27A H 0.2444 0.5249 -0.0391 0.086 Uiso 1 1 calc R . . 
H27B H 0.3083 0.5424 -0.0803 0.086 Uiso 1 1 calc R . . 
H27C H 0.3210 0.5832 0.0043 0.086 Uiso 1 1 calc R . . 
C28 C 0.29325(17) 0.3165(3) -0.06736(15) 0.0504(8) Uani 1 1 d . . . 
H28A H 0.3114 0.2383 -0.0515 0.076 Uiso 1 1 calc R . . 
H28B H 0.3063 0.3367 -0.1134 0.076 Uiso 1 1 calc R . . 
H28C H 0.2396 0.3185 -0.0762 0.076 Uiso 1 1 calc R . . 
C29 C 0.41238(15) 0.4086(3) 0.00467(16) 0.0456(8) Uani 1 1 d . . . 
H29A H 0.4332 0.3310 0.0180 0.068 Uiso 1 1 calc R . . 
H29B H 0.4346 0.4634 0.0446 0.068 Uiso 1 1 calc R . . 
H29C H 0.4228 0.4338 -0.0417 0.068 Uiso 1 1 calc R . . 
C30 C 0.20487(16) -0.1653(2) 0.04770(15) 0.0365(7) Uani 1 1 d . . . 
H30A H 0.1976 -0.1930 -0.0018 0.044 Uiso 1 1 calc R . . 
C31 C 0.14182(15) -0.1580(2) 0.07894(15) 0.0348(7) Uani 1 1 d . . . 
C32 C 0.07185(15) -0.1860(2) 0.03324(15) 0.0383(7) Uani 1 1 d . . . 
H32A H 0.0674 -0.2110 -0.0164 0.046 Uiso 1 1 calc R . . 
C33 C 0.00915(16) -0.1782(2) 0.05836(16) 0.0404(7) Uani 1 1 d . . . 
C34 C 0.01942(16) -0.1427(3) 0.13189(17) 0.0473(8) Uani 1 1 d . . . 
H34A H -0.0229 -0.1386 0.1504 0.057 Uiso 1 1 calc R . . 
C35 C 0.08689(15) -0.1128(3) 0.18038(15) 0.0421(7) Uani 1 1 d . . . 
C36 C 0.14921(15) -0.1207(2) 0.15210(15) 0.0359(7) Uani 1 1 d . . . 
C37 C -0.06743(16) -0.2120(3) 0.00994(17) 0.0471(8) Uani 1 1 d . . . 
C38 C -0.0721(2) -0.2000(4) -0.07306(18) 0.0848(13) Uani 1 1 d . . . 
H38A H -0.0382 -0.2553 -0.0866 0.127 Uiso 1 1 calc R . . 
H38B H -0.0586 -0.1207 -0.0834 0.127 Uiso 1 1 calc R . . 
H38C H -0.1226 -0.2163 -0.1023 0.127 Uiso 1 1 calc R . . 
C39 C -0.12793(18) -0.1356(3) 0.0270(2) 0.0769(11) Uani 1 1 d . . . 
H39A H -0.1752 -0.1527 -0.0087 0.115 Uiso 1 1 calc R . . 
H39B H -0.1156 -0.0535 0.0231 0.115 Uiso 1 1 calc R . . 
H39C H -0.1316 -0.1518 0.0776 0.115 Uiso 1 1 calc R . . 
C40 C -0.08192(19) -0.3386(3) 0.02655(19) 0.0659(10) Uani 1 1 d . . . 
H40A H -0.0450 -0.3886 0.0136 0.099 Uiso 1 1 calc R . . 
H40B H -0.1312 -0.3612 -0.0029 0.099 Uiso 1 1 calc R . . 
H40C H -0.0788 -0.3471 0.0796 0.099 Uiso 1 1 calc R . . 
C41 C 0.09352(17) -0.0737(3) 0.26076(18) 0.0573(9) Uani 1 1 d . . . 
C42 C 0.0178(2) -0.0699(4) 0.2779(2) 0.0953(15) Uani 1 1 d . . . 
H42A H -0.0045 -0.1474 0.2709 0.143 Uiso 1 1 calc R . . 
H42B H -0.0143 -0.0148 0.2442 0.143 Uiso 1 1 calc R . . 
H42C H 0.0241 -0.0449 0.3295 0.143 Uiso 1 1 calc R . . 
C43 C 0.1266(2) 0.0498(3) 0.2728(2) 0.0739(11) Uani 1 1 d . . . 
H43A H 0.0943 0.1038 0.2384 0.111 Uiso 1 1 calc R . . 
H43B H 0.1755 0.0496 0.2635 0.111 Uiso 1 1 calc R . . 
H43C H 0.1309 0.0743 0.3242 0.111 Uiso 1 1 calc R . . 
C44 C 0.1421(2) -0.1589(3) 0.31588(18) 0.0772(12) Uani 1 1 d . . . 
H44A H 0.1213 -0.2373 0.3068 0.116 Uiso 1 1 calc R . . 
H44B H 0.1439 -0.1352 0.3669 0.116 Uiso 1 1 calc R . . 
H44C H 0.1920 -0.1585 0.3092 0.116 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 
N1 0.0347(14) 0.0298(12) 0.0325(13) -0.0020(10) 0.0116(10) -0.0013(10) 
N2 0.0294(13) 0.0395(13) 0.0325(13) 0.0000(11) 0.0081(10) 0.0014(11) 
O1 0.0510(13) 0.0482(12) 0.0311(11) 0.0007(9) 0.0224(10) 0.0072(10) 
O2 0.0342(12) 0.0679(14) 0.0332(11) -0.0170(10) 0.0055(9) -0.0069(10) 
C1 0.0440(19) 0.0347(17) 0.067(2) -0.0005(15) 0.0158(16) 0.0057(14) 
C2 0.0248(15) 0.0362(16) 0.0433(18) 0.0020(14) 0.0079(13) 0.0010(12) 
C3 0.0349(18) 0.0401(17) 0.047(2) 0.0103(15) 0.0021(14) 0.0013(14) 
C4 0.0474(19) 0.052(2) 0.0275(16) 0.0087(15) 0.0017(14) -0.0115(15) 
C5 0.0428(18) 0.0400(17) 0.0280(16) -0.0019(13) 0.0065(13) -0.0042(14) 
C6 0.0273(15) 0.0332(15) 0.0313(16) 0.0040(13) 0.0067(12) -0.0044(12) 
C7 0.0243(15) 0.0335(15) 0.0348(16) 0.0008(13) 0.0081(12) -0.0013(12) 
C8 0.0336(16) 0.0296(15) 0.0334(16) -0.0028(12) 0.0134(13) 0.0013(12) 
C9 0.0380(17) 0.0383(16) 0.0308(16) -0.0022(13) 0.0139(13) 0.0034(13) 
C10 0.0425(19) 0.055(2) 0.0332(17) -0.0021(14) 0.0096(14) 0.0012(15) 
C11 0.061(2) 0.063(2) 0.0320(17) -0.0049(15) 0.0201(16) -0.0015(17) 
C12 0.050(2) 0.054(2) 0.045(2) -0.0067(15) 0.0276(16) -0.0015(16) 
C13 0.0357(17) 0.0368(16) 0.0452(18) -0.0070(14) 0.0163(14) 0.0018(13) 
C14 0.0378(19) 0.060(2) 0.063(2) 0.0003(17) 0.0209(16) 0.0014(16) 
C15 0.0403(17) 0.0360(16) 0.0314(16) -0.0014(13) 0.0151(13) -0.0056(13) 
C16 0.0347(16) 0.0356(16) 0.0295(15) 0.0008(12) 0.0110(12) -0.0017(13) 
C17 0.0378(17) 0.0358(16) 0.0340(16) 0.0012(13) 0.0165(13) -0.0023(13) 
C18 0.0298(15) 0.0343(16) 0.0364(16) -0.0012(13) 0.0118(13) -0.0035(12) 
C19 0.0323(16) 0.0336(15) 0.0381(16) 0.0066(13) 0.0076(13) 0.0012(12) 
C20 0.0295(15) 0.0373(16) 0.0307(15) 0.0009(13) 0.0091(12) -0.0004(12) 
C21 0.0296(16) 0.0358(16) 0.0322(16) -0.0050(13) 0.0100(12) 0.0012(12) 
C22 0.0398(18) 0.0340(16) 0.0466(18) -0.0033(14) 0.0169(14) 0.0018(14) 
C23 0.070(2) 0.055(2) 0.059(2) -0.0008(17) 0.0399(19) 0.0104(17) 
C24 0.057(2) 0.0436(19) 0.065(2) -0.0162(16) 0.0218(18) -0.0060(16) 
C25 0.046(2) 0.051(2) 0.064(2) -0.0029(16) 0.0187(17) 0.0090(16) 
C26 0.0368(17) 0.0470(17) 0.0307(16) 0.0045(13) 0.0105(13) 0.0015(14) 
C27 0.063(2) 0.064(2) 0.048(2) 0.0236(17) 0.0210(17) 0.0149(18) 
C28 0.0449(19) 0.072(2) 0.0330(17) 0.0028(16) 0.0083(14) -0.0004(17) 
C29 0.0437(19) 0.0551(19) 0.0404(18) 0.0075(14) 0.0156(15) 0.0000(15) 
C30 0.0393(18) 0.0421(17) 0.0277(15) -0.0044(13) 0.0081(13) -0.0028(14) 
C31 0.0307(16) 0.0381(16) 0.0351(16) 0.0007(13) 0.0077(13) -0.0002(13) 
C32 0.0406(18) 0.0424(17) 0.0294(16) -0.0014(13) 0.0049(13) -0.0026(14) 
C33 0.0360(18) 0.0431(17) 0.0398(18) 0.0022(14) 0.0060(14) -0.0066(14) 
C34 0.0318(17) 0.062(2) 0.050(2) -0.0035(16) 0.0132(15) -0.0040(15) 
C35 0.0311(17) 0.058(2) 0.0370(17) -0.0077(14) 0.0090(13) -0.0058(14) 
C36 0.0312(16) 0.0411(17) 0.0334(16) -0.0061(13) 0.0052(13) -0.0043(13) 
C37 0.0343(18) 0.057(2) 0.0463(19) 0.0033(15) 0.0038(14) -0.0127(15) 
C38 0.057(3) 0.136(4) 0.047(2) 0.012(2) -0.0121(18) -0.041(2) 
C39 0.037(2) 0.085(3) 0.098(3) -0.006(2) -0.0007(19) -0.0009(19) 
C40 0.056(2) 0.064(2) 0.071(2) -0.0010(19) 0.0046(18) -0.0218(19) 
C41 0.0376(19) 0.091(3) 0.047(2) -0.0221(19) 0.0179(16) -0.0085(18) 
C42 0.054(3) 0.174(4) 0.068(3) -0.044(3) 0.033(2) -0.015(3) 
C43 0.068(3) 0.088(3) 0.069(3) -0.042(2) 0.024(2) -0.009(2) 
C44 0.074(3) 0.118(3) 0.040(2) -0.010(2) 0.0146(19) -0.015(2) 
 
_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 
N1 C15 1.277(3) . y 
N1 C6 1.426(3) . y 
N2 C30 1.282(3) . y 
N2 C9 1.425(3) . y 
O1 C21 1.358(3) . y 
O2 C36 1.355(3) . y 
C1 C2 1.507(4) . ? 
C2 C3 1.382(4) . ? 
C2 C7 1.398(3) . ? 
C3 C4 1.380(4) . ? 
C4 C5 1.377(4) . ? 
C5 C6 1.389(3) . ? 
C6 C7 1.405(3) . ? 
C7 C8 1.495(3) . ? 
C8 C9 1.401(4) . ? 
C8 C13 1.411(3) . ? 
C9 C10 1.386(4) . ? 
C10 C11 1.382(4) . ? 
C11 C12 1.386(4) . ? 
C12 C13 1.384(4) . ? 
C13 C14 1.504(4) . ? 
C15 C16 1.456(4) . ? 
C16 C21 1.403(3) . ? 
C16 C17 1.405(3) . ? 
C17 C18 1.373(3) . ? 
C18 C19 1.408(3) . ? 
C18 C22 1.532(3) . ? 
C19 C20 1.392(3) . ? 
C20 C21 1.402(4) . ? 
C20 C26 1.544(3) . ? 
C22 C23 1.534(4) . ? 
C22 C25 1.535(4) . ? 
C22 C24 1.541(4) . ? 
C26 C27 1.527(4) . ? 
C26 C29 1.535(4) . ? 
C26 C28 1.542(4) . ? 
C30 C31 1.456(4) . ? 
C31 C36 1.400(3) . ? 
C31 C32 1.403(4) . ? 
C32 C33 1.382(4) . ? 
C33 C34 1.393(4) . ? 
C33 C37 1.534(4) . ? 
C34 C35 1.393(4) . ? 
C35 C36 1.410(4) . ? 
C35 C41 1.536(4) . ? 
C37 C40 1.528(4) . ? 
C37 C38 1.531(4) . ? 
C37 C39 1.537(4) . ? 
C41 C44 1.534(5) . ? 
C41 C43 1.543(5) . ? 
C41 C42 1.541(4) . ? 
 
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 
C15 N1 C6 119.9(2) . . y 
C30 N2 C9 120.8(2) . . y 
C3 C2 C7 118.9(3) . . ? 
C3 C2 C1 119.9(3) . . ? 
C7 C2 C1 121.2(3) . . ? 
C2 C3 C4 121.5(3) . . ? 
C5 C4 C3 120.1(3) . . ? 
C4 C5 C6 119.6(3) . . ? 
C5 C6 C7 120.4(2) . . ? 
C5 C6 N1 122.4(2) . . y 
C7 C6 N1 117.2(2) . . y 
C6 C7 C2 119.4(2) . . ? 
C6 C7 C8 119.2(2) . . ? 
C2 C7 C8 121.4(2) . . ? 
C9 C8 C13 119.1(2) . . ? 
C9 C8 C7 120.8(2) . . ? 
C13 C8 C7 120.1(2) . . ? 
C10 C9 C8 120.7(2) . . ? 
C10 C9 N2 122.5(3) . . y 
C8 C9 N2 116.6(2) . . y 
C11 C10 C9 119.6(3) . . ? 
C10 C11 C12 120.4(3) . . ? 
C13 C12 C11 120.9(3) . . ? 
C12 C13 C8 119.2(3) . . ? 
C12 C13 C14 119.8(2) . . ? 
C8 C13 C14 121.1(3) . . ? 
N1 C15 C16 123.1(2) . . y 
C21 C16 C17 120.4(2) . . ? 
C21 C16 C15 121.7(2) . . ? 
C17 C16 C15 117.9(2) . . ? 
C18 C17 C16 121.5(2) . . ? 
C17 C18 C19 116.3(2) . . ? 
C17 C18 C22 123.4(2) . . ? 
C19 C18 C22 120.3(2) . . ? 
C20 C19 C18 125.1(2) . . ? 
C19 C20 C21 116.6(2) . . ? 
C19 C20 C26 121.5(2) . . ? 
C21 C20 C26 121.9(2) . . ? 
O1 C21 C16 118.8(2) . . y 
O1 C21 C20 121.0(2) . . y 
C16 C21 C20 120.2(2) . . ? 
C18 C22 C23 111.8(2) . . ? 
C18 C22 C25 110.4(2) . . ? 
C23 C22 C25 108.7(2) . . ? 
C18 C22 C24 108.6(2) . . ? 
C23 C22 C24 108.2(2) . . ? 
C25 C22 C24 109.2(2) . . ? 
C27 C26 C29 107.7(2) . . ? 
C27 C26 C20 112.4(2) . . ? 
C29 C26 C20 109.9(2) . . ? 
C27 C26 C28 107.5(2) . . ? 
C29 C26 C28 110.0(2) . . ? 
C20 C26 C28 109.3(2) . . ? 
N2 C30 C31 122.1(3) . . y 
C36 C31 C32 119.8(2) . . ? 
C36 C31 C30 121.7(3) . . ? 
C32 C31 C30 118.5(3) . . ? 
C33 C32 C31 121.9(3) . . ? 
C32 C33 C34 116.3(3) . . ? 
C32 C33 C37 122.5(3) . . ? 
C34 C33 C37 121.1(3) . . ? 
C33 C34 C35 125.2(3) . . ? 
C34 C35 C36 116.6(3) . . ? 
C34 C35 C41 122.0(2) . . ? 
C36 C35 C41 121.4(3) . . ? 
O2 C36 C31 119.2(2) . . y 
O2 C36 C35 120.5(2) . . y 
C31 C36 C35 120.3(3) . . ? 
C40 C37 C38 109.0(3) . . ? 
C40 C37 C39 108.8(3) . . ? 
C38 C37 C39 108.0(3) . . ? 
C40 C37 C33 108.2(3) . . ? 
C38 C37 C33 111.4(2) . . ? 
C39 C37 C33 111.4(3) . . ? 
C44 C41 C35 110.2(3) . . ? 
C44 C41 C43 110.2(3) . . ? 
C35 C41 C43 109.7(3) . . ? 
C44 C41 C42 107.4(3) . . ? 
C35 C41 C42 111.7(3) . . ? 
C43 C41 C42 107.6(3) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C7 C2 C3 C4 1.9(4) . . . . ? 
C1 C2 C3 C4 -175.9(3) . . . . ? 
C2 C3 C4 C5 -0.5(4) . . . . ? 
C3 C4 C5 C6 -0.9(4) . . . . ? 
C4 C5 C6 C7 0.7(4) . . . . ? 
C4 C5 C6 N1 -177.3(2) . . . . ? 
C15 N1 C6 C5 -33.6(4) . . . . ? 
C15 N1 C6 C7 148.4(2) . . . . ? 
C5 C6 C7 C2 0.8(4) . . . . ? 
N1 C6 C7 C2 178.9(2) . . . . ? 
C5 C6 C7 C8 -178.9(2) . . . . ? 
N1 C6 C7 C8 -0.8(3) . . . . ? 
C3 C2 C7 C6 -2.1(4) . . . . ? 
C1 C2 C7 C6 175.7(2) . . . . ? 
C3 C2 C7 C8 177.6(2) . . . . ? 
C1 C2 C7 C8 -4.6(4) . . . . ? 
C6 C7 C8 C9 -74.2(3) . . . . ? 
C2 C7 C8 C9 106.1(3) . . . . ? 
C6 C7 C8 C13 105.1(3) . . . . ? 
C2 C7 C8 C13 -74.6(3) . . . . ? 
C13 C8 C9 C10 -1.6(4) . . . . ? 
C7 C8 C9 C10 177.6(2) . . . . ? 
C13 C8 C9 N2 -177.0(2) . . . . ? 
C7 C8 C9 N2 2.2(4) . . . . ? 
C30 N2 C9 C10 27.0(4) . . . . ? 
C30 N2 C9 C8 -157.7(2) . . . . ? 
C8 C9 C10 C11 2.9(4) . . . . ? 
N2 C9 C10 C11 178.0(2) . . . . ? 
C9 C10 C11 C12 -2.0(5) . . . . ? 
C10 C11 C12 C13 -0.1(5) . . . . ? 
C11 C12 C13 C8 1.3(4) . . . . ? 
C11 C12 C13 C14 -176.6(3) . . . . ? 
C9 C8 C13 C12 -0.5(4) . . . . ? 
C7 C8 C13 C12 -179.7(2) . . . . ? 
C9 C8 C13 C14 177.4(2) . . . . ? 
C7 C8 C13 C14 -1.8(4) . . . . ? 
C6 N1 C15 C16 179.0(2) . . . . ? 
N1 C15 C16 C21 5.1(4) . . . . ? 
N1 C15 C16 C17 -174.8(3) . . . . ? 
C21 C16 C17 C18 -0.5(4) . . . . ? 
C15 C16 C17 C18 179.5(3) . . . . ? 
C16 C17 C18 C19 1.1(4) . . . . ? 
C16 C17 C18 C22 -177.2(3) . . . . ? 
C17 C18 C19 C20 -0.6(4) . . . . ? 
C22 C18 C19 C20 177.8(3) . . . . ? 
C18 C19 C20 C21 -0.7(4) . . . . ? 
C18 C19 C20 C26 179.3(2) . . . . ? 
C17 C16 C21 O1 179.9(2) . . . . ? 
C15 C16 C21 O1 -0.1(4) . . . . ? 
C17 C16 C21 C20 -0.8(4) . . . . ? 
C15 C16 C21 C20 179.2(3) . . . . ? 
C19 C20 C21 O1 -179.4(2) . . . . ? 
C26 C20 C21 O1 0.6(4) . . . . ? 
C19 C20 C21 C16 1.3(4) . . . . ? 
C26 C20 C21 C16 -178.7(2) . . . . ? 
C17 C18 C22 C23 -2.9(4) . . . . ? 
C19 C18 C22 C23 178.8(2) . . . . ? 
C17 C18 C22 C25 -124.0(3) . . . . ? 
C19 C18 C22 C25 57.7(3) . . . . ? 
C17 C18 C22 C24 116.3(3) . . . . ? 
C19 C18 C22 C24 -61.9(3) . . . . ? 
C19 C20 C26 C27 -0.1(4) . . . . ? 
C21 C20 C26 C27 179.9(3) . . . . ? 
C19 C20 C26 C29 119.9(3) . . . . ? 
C21 C20 C26 C29 -60.1(3) . . . . ? 
C19 C20 C26 C28 -119.3(3) . . . . ? 
C21 C20 C26 C28 60.7(3) . . . . ? 
C9 N2 C30 C31 -175.6(2) . . . . ? 
N2 C30 C31 C36 -1.7(4) . . . . ? 
N2 C30 C31 C32 176.4(2) . . . . ? 
C36 C31 C32 C33 -0.2(4) . . . . ? 
C30 C31 C32 C33 -178.3(3) . . . . ? 
C31 C32 C33 C34 -0.9(4) . . . . ? 
C31 C32 C33 C37 -178.1(3) . . . . ? 
C32 C33 C34 C35 1.4(5) . . . . ? 
C37 C33 C34 C35 178.6(3) . . . . ? 
C33 C34 C35 C36 -0.7(5) . . . . ? 
C33 C34 C35 C41 179.6(3) . . . . ? 
C32 C31 C36 O2 -178.7(2) . . . . ? 
C30 C31 C36 O2 -0.6(4) . . . . ? 
C32 C31 C36 C35 0.9(4) . . . . ? 
C30 C31 C36 C35 179.0(3) . . . . ? 
C34 C35 C36 O2 179.1(3) . . . . ? 
C41 C35 C36 O2 -1.2(4) . . . . ? 
C34 C35 C36 C31 -0.5(4) . . . . ? 
C41 C35 C36 C31 179.2(3) . . . . ? 
C32 C33 C37 C40 93.8(3) . . . . ? 
C34 C33 C37 C40 -83.2(3) . . . . ? 
C32 C33 C37 C38 -26.0(4) . . . . ? 
C34 C33 C37 C38 157.0(3) . . . . ? 
C32 C33 C37 C39 -146.7(3) . . . . ? 
C34 C33 C37 C39 36.3(4) . . . . ? 
C34 C35 C41 C44 117.9(3) . . . . ? 
C36 C35 C41 C44 -61.8(4) . . . . ? 
C34 C35 C41 C43 -120.6(3) . . . . ? 
C36 C35 C41 C43 59.7(4) . . . . ? 
C34 C35 C41 C42 -1.4(5) . . . . ? 
C36 C35 C41 C42 178.9(3) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.921 
_diffrn_reflns_theta_full              28.51 
_diffrn_measured_fraction_theta_full   0.921 
_refine_diff_density_max    0.394 
_refine_diff_density_min   -0.488 
_refine_diff_density_rms    0.049 

####END

data_mar1796 # [HfL1Cl2] Scott and co-workers Non-Planar Coordination..
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C44 H54 Cl2 Hf N2 O2' 
_chemical_formula_weight          892.28 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'Hf'  'Hf'  -0.5830   6.1852 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    C2/c 
  
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                    25.226(7) 
_cell_length_b                    10.762(10) 
_cell_length_c                    16.134(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  102.13(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      4282.3(43) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       10 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.384 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1816 
_exptl_absorpt_coefficient_mu     2.597 
_exptl_absorpt_correction_type    psiscans 
_exptl_absorpt_correction_T_min   0.55 
_exptl_absorpt_correction_T_max   0.99 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        ' Enraf-Nonius CAD4' 
_diffrn_measurement_method        \w--2\q 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   120 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             3844 
_diffrn_reflns_av_R_equivalents   0.0727 
_diffrn_reflns_av_sigmaI/netI     0.0399 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        29 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.06 
_diffrn_reflns_theta_max          24.97 
_reflns_number_total              3762 
_reflns_number_observed           3267 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Enraf-Nonius CAD4' 
_computing_cell_refinement        'Enraf-Nonius CAD4' 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'CAMERON (Watkin and Pearce,1993)' 
_computing_publication_material   SHELXL-93 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 1 with very negative 
F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-
factors 
 wR and all goodnesses 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 observed 
criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+2.0568P] 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     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3761 
_refine_ls_number_parameters      231 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0542 
_refine_ls_R_factor_obs           0.0474 
_refine_ls_wR_factor_all          0.1302 
_refine_ls_wR_factor_obs          0.1222 
_refine_ls_goodness_of_fit_all    1.049 
_refine_ls_goodness_of_fit_obs    1.062 
_refine_ls_restrained_S_all       1.051 
_refine_ls_restrained_S_obs       1.062 
_refine_ls_shift/esd_max          -0.002 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Hf Hf 0.0000 0.00618(2) 0.2500 0.0314(2) Uani 1 d S . 
Cl Cl 0.03741(7) 0.14447(14) 0.16115(10) 0.0546(4) Uani 1 d . . 
O O 0.0692(2) -0.0070(3) 0.3372(3) 0.0400(10) Uani 1 d . . 
N N 0.0416(2) -0.1616(4) 0.2033(3) 0.0331(9) Uani 1 d . . 
C1 C 0.1208(2) -0.0402(5) 0.3434(3) 0.0343(10) Uani 1 d . . 
C2 C 0.1622(3) 0.0057(4) 0.4088(4) 0.0383(14) Uani 1 d . . 
C3 C 0.2151(2) -0.0313(6) 0.4068(4) 0.0442(13) Uani 1 d . . 
H3 H 0.2435(2) 0.0007(6) 0.4497(4) 0.053 Uiso 1 calc R . 
C4 C 0.2296(2) -0.1105(6) 0.3479(4) 0.0468(13) Uani 1 d . . 
C5 C 0.1883(2) -0.1585(5) 0.2875(3) 0.0449(13) Uani 1 d . . 
H5 H 0.1964(2) -0.2163(5) 0.2474(3) 0.054 Uiso 1 calc R . 
C6 C 0.1337(2) -0.1239(5) 0.2836(3) 0.0389(11) Uani 1 d . . 
C7 C 0.0925(2) -0.1883(5) 0.2233(3) 0.0390(11) Uani 1 d . . 
H7 H 0.1041(2) -0.2577(5) 0.1955(3) 0.047 Uiso 1 calc R . 
C8 C 0.0081(2) -0.2576(4) 0.1554(3) 0.0324(10) Uani 1 d . . 
C9 C -0.0087(2) -0.3531(4) 0.2027(3) 0.0382(11) Uani 1 d . . 
C10 C -0.0431(2) -0.4455(5) 0.1594(4) 0.0477(13) Uani 1 d . . 
C11 C -0.0564(3) -0.4395(6) 0.0706(4) 0.055(2) Uani 1 d . . 
H11 H -0.0789(3) -0.5023(6) 0.0402(4) 0.066 Uiso 1 calc R . 
C12 C -0.0382(2) -0.3474(6) 0.0266(4) 0.0511(14) Uani 1 d . . 
H12 H -0.0475(2) -0.3474(6) -0.0336(4) 0.061 Uiso 1 calc R . 
C13 C -0.0060(2) -0.2531(5) 0.0688(3) 0.0429(12) Uani 1 d . . 
H13 H 0.0060(2) -0.1870(5) 0.0383(3) 0.051 Uiso 1 calc R . 
C14 C -0.0668(4) -0.5462(7) 0.2049(5) 0.071(2) Uani 1 d . . 
H14A H -0.0537(4) -0.5366(7) 0.2662(5) 0.106 Uiso 0.50 calc PR . 
H14B H -0.0557(4) -0.6275(7) 0.1872(5) 0.106 Uiso 0.50 calc PR . 
H14C H -0.1064(4) -0.5402(7) 0.1912(5) 0.106 Uiso 0.50 calc PR . 
H14D H -0.0902(4) -0.5996(7) 0.1635(5) 0.106 Uiso 0.50 calc PR . 
H14E H -0.0882(4) -0.5087(7) 0.2425(5) 0.106 Uiso 0.50 calc PR . 
H14F H -0.0374(4) -0.5960(7) 0.2385(5) 0.106 Uiso 0.50 calc PR . 
C15 C 0.1497(2) 0.0895(5) 0.4783(3) 0.0450(13) Uani 1 d . . 
C16 C 0.1081(3) 0.0266(7) 0.5222(5) 0.059(2) Uani 1 d . . 
H16A H 0.1004(3) 0.0813(7) 0.5667(5) 0.089 Uiso 1 calc R . 
H16B H 0.1229(3) -0.0522(7) 0.5474(5) 0.089 Uiso 1 calc R . 
H16C H 0.0746(3) 0.0107(7) 0.4804(5) 0.089 Uiso 1 calc R . 
C17 C 0.1269(3) 0.2135(6) 0.4396(5) 0.071(2) Uani 1 d . . 
H17A H 0.1188(3) 0.2673(6) 0.4844(5) 0.106 Uiso 1 calc R . 
H17B H 0.0936(3) 0.1983(6) 0.3971(5) 0.106 Uiso 1 calc R . 
H17C H 0.1537(3) 0.2540(6) 0.4126(5) 0.106 Uiso 1 calc R . 
C18 C 0.2003(3) 0.1190(7) 0.5471(4) 0.068(2) Uani 1 d . . 
H18A H 0.1901(3) 0.1730(7) 0.5902(4) 0.102 Uiso 1 calc R . 
H18B H 0.2272(3) 0.1614(7) 0.5213(4) 0.102 Uiso 1 calc R . 
H18C H 0.2158(3) 0.0416(7) 0.5736(4) 0.102 Uiso 1 calc R . 
C19 C 0.2896(2) -0.1448(7) 0.3534(4) 0.063(2) Uani 1 d . . 
C20 C 0.2978(3) -0.2332(11) 0.2848(6) 0.124(4) Uani 1 d . . 
H20A H 0.2835(3) -0.1958(11) 0.2292(6) 0.186 Uiso 1 calc R . 
H20B H 0.2786(3) -0.3110(11) 0.2898(6) 0.186 Uiso 1 calc R . 
H20C H 0.3366(3) -0.2501(11) 0.2908(6) 0.186 Uiso 1 calc R . 
C21 C 0.3116(3) -0.2025(9) 0.4406(5) 0.088(3) Uani 1 d . . 
H21A H 0.3062(3) -0.1446(9) 0.4850(5) 0.133 Uiso 1 calc R . 
H21B H 0.3504(3) -0.2194(9) 0.4470(5) 0.133 Uiso 1 calc R . 
H21C H 0.2924(3) -0.2803(9) 0.4458(5) 0.133 Uiso 1 calc R . 
C22 C 0.3219(4) -0.0242(9) 0.3500(9) 0.094(3) Uani 1 d . . 
H22A H 0.3162(4) 0.0321(9) 0.3950(9) 0.141 Uiso 1 calc R . 
H22B H 0.3095(4) 0.0159(9) 0.2948(9) 0.141 Uiso 1 calc R . 
H22C H 0.3606(4) -0.0438(9) 0.3579(9) 0.141 Uiso 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 
Hf 0.0197(2) 0.0339(2) 0.0396(2) 0.000 0.00383(14) 0.000 
Cl 0.0482(8) 0.0546(8) 0.0642(9) 0.0106(7) 0.0193(7) -0.0066(7) 
O 0.026(2) 0.046(2) 0.046(2) -0.0075(14) 0.005(2) 0.0016(13) 
N 0.019(2) 0.040(2) 0.038(2) 0.001(2) 0.001(2) -0.005(2) 
C1 0.022(2) 0.040(2) 0.040(3) 0.004(2) 0.004(2) 0.000(2) 
C2 0.028(3) 0.046(3) 0.038(3) 0.007(2) 0.001(3) -0.002(2) 
C3 0.021(3) 0.058(3) 0.048(3) 0.007(3) -0.005(2) -0.003(3) 
C4 0.020(3) 0.064(3) 0.056(3) 0.006(3) 0.006(2) 0.007(2) 
C5 0.026(3) 0.059(3) 0.050(3) -0.002(3) 0.009(2) 0.010(2) 
C6 0.020(2) 0.049(3) 0.047(3) 0.001(2) 0.005(2) 0.002(2) 
C7 0.028(3) 0.044(3) 0.046(3) -0.003(2) 0.011(2) 0.001(2) 
C8 0.023(2) 0.033(2) 0.040(3) -0.005(2) 0.005(2) -0.001(2) 
C9 0.030(3) 0.035(2) 0.050(3) -0.003(2) 0.009(2) 0.001(2) 
C10 0.046(3) 0.039(3) 0.056(4) -0.007(3) 0.009(3) -0.008(3) 
C11 0.051(4) 0.055(4) 0.054(4) -0.014(3) -0.001(3) -0.013(3) 
C12 0.047(3) 0.063(4) 0.041(3) -0.008(3) 0.004(3) -0.006(3) 
C13 0.032(3) 0.051(3) 0.044(3) 0.000(2) 0.006(2) -0.009(2) 
C14 0.086(6) 0.055(4) 0.072(5) -0.006(4) 0.018(4) -0.028(4) 
C15 0.033(3) 0.049(3) 0.048(3) -0.005(2) -0.003(2) 0.003(2) 
C16 0.050(4) 0.075(4) 0.053(4) -0.006(3) 0.013(3) 0.003(4) 
C17 0.081(5) 0.042(3) 0.080(5) -0.006(3) -0.004(4) 0.006(3) 
C18 0.054(4) 0.083(5) 0.060(4) -0.017(3) -0.006(3) -0.006(4) 
C19 0.021(3) 0.092(5) 0.075(4) 0.004(4) 0.009(3) 0.008(3) 
C20 0.034(4) 0.202(12) 0.136(8) -0.061(8) 0.018(5) 0.031(6) 
C21 0.038(4) 0.109(6) 0.113(6) 0.029(5) 0.006(4) 0.022(4) 
C22 0.037(5) 0.112(7) 0.138(10) 0.030(6) 0.028(6) -0.005(4) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are 
taken 
 into account individually in the estimation of esds in distances, 
angles 
 and torsion angles; correlations between esds in cell parameters are 
only 
 used when they are defined by crystal symmetry.  An approximate 
(isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. 
planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Hf O 2.003(5) . ? 
Hf O 2.003(5) 6_556 ? 
Hf N 2.294(4) . ? 
Hf N 2.294(4) 6_556 ? 
Hf Cl 2.394(2) 6_556 ? 
Hf Cl 2.394(2) . ? 
O C1 1.333(7) . ? 
N C7 1.289(6) . ? 
N C8 1.451(6) . ? 
C1 C6 1.408(7) . ? 
C1 C2 1.410(8) . ? 
C2 C3 1.399(9) . ? 
C2 C15 1.522(8) . ? 
C3 C4 1.383(9) . ? 
C4 C5 1.369(8) . ? 
C4 C19 1.542(7) . ? 
C5 C6 1.415(7) . ? 
C6 C7 1.442(7) . ? 
C8 C13 1.368(7) . ? 
C8 C9 1.398(7) . ? 
C9 C10 1.407(7) . ? 
C9 C9 1.495(10) 6_556 ? 
C10 C11 1.403(8) . ? 
C10 C14 1.503(9) . ? 
C11 C12 1.354(8) . ? 
C12 C13 1.385(8) . ? 
C15 C17 1.533(8) . ? 
C15 C18 1.538(8) . ? 
C15 C16 1.541(9) . ? 
C19 C20 1.506(11) . ? 
C19 C21 1.531(10) . ? 
C19 C22 1.540(11) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O Hf O 171.9(2) . 6_556 ? 
O Hf N 77.52(14) . . ? 
O Hf N 96.03(15) 6_556 . ? 
O Hf N 96.03(15) . 6_556 ? 
O Hf N 77.52(14) 6_556 6_556 ? 
N Hf N 76.2(2) . 6_556 ? 
O Hf Cl 91.05(12) . 6_556 ? 
O Hf Cl 93.99(13) 6_556 6_556 ? 
N Hf Cl 162.07(11) . 6_556 ? 
N Hf Cl 91.56(12) 6_556 6_556 ? 
O Hf Cl 93.99(13) . . ? 
O Hf Cl 91.05(12) 6_556 . ? 
N Hf Cl 91.56(12) . . ? 
N Hf Cl 162.07(11) 6_556 . ? 
Cl Hf Cl 103.10(10) 6_556 . ? 
C1 O Hf 139.9(4) . . ? 
C7 N C8 114.4(4) . . ? 
C7 N Hf 126.4(4) . . ? 
C8 N Hf 118.7(3) . . ? 
O C1 C6 118.9(5) . . ? 
O C1 C2 121.4(5) . . ? 
C6 C1 C2 119.7(5) . . ? 
C3 C2 C1 116.3(5) . . ? 
C3 C2 C15 122.1(6) . . ? 
C1 C2 C15 121.5(6) . . ? 
C4 C3 C2 125.6(6) . . ? 
C5 C4 C3 116.8(5) . . ? 
C5 C4 C19 122.8(5) . . ? 
C3 C4 C19 120.4(5) . . ? 
C4 C5 C6 121.4(5) . . ? 
C1 C6 C5 120.1(5) . . ? 
C1 C6 C7 122.1(4) . . ? 
C5 C6 C7 117.4(5) . . ? 
N C7 C6 126.9(5) . . ? 
C13 C8 C9 122.7(4) . . ? 
C13 C8 N 121.1(4) . . ? 
C9 C8 N 116.2(4) . . ? 
C8 C9 C10 118.3(5) . . ? 
C8 C9 C9 120.0(4) . 6_556 ? 
C10 C9 C9 121.7(4) . 6_556 ? 
C11 C10 C9 117.8(5) . . ? 
C11 C10 C14 119.9(5) . . ? 
C9 C10 C14 122.3(6) . . ? 
C12 C11 C10 122.3(5) . . ? 
C11 C12 C13 120.5(5) . . ? 
C8 C13 C12 118.4(5) . . ? 
C2 C15 C17 109.5(5) . . ? 
C2 C15 C18 112.6(5) . . ? 
C17 C15 C18 107.3(5) . . ? 
C2 C15 C16 110.2(5) . . ? 
C17 C15 C16 109.6(5) . . ? 
C18 C15 C16 107.5(5) . . ? 
C20 C19 C21 109.9(7) . . ? 
C20 C19 C22 110.5(8) . . ? 
C21 C19 C22 106.4(7) . . ? 
C20 C19 C4 113.1(6) . . ? 
C21 C19 C4 108.2(5) . . ? 
C22 C19 C4 108.4(6) . . ? 
  
_refine_diff_density_max    1.522 
_refine_diff_density_min   -4.636 
_refine_diff_density_rms    0.165

###END
 
data_dec896 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C56 H64 N2 O4 Zr' 
_chemical_formula_weight          920.31 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
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' 
 'Zr'  'Zr'  -2.9673   0.5597 
 '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 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    13.210(10) 
_cell_length_b                    13.557(8) 
_cell_length_c                    15.287(7) 
_cell_angle_alpha                 69.35(5) 
_cell_angle_beta                  74.15(5) 
_cell_angle_gamma                 77.73(5) 
_cell_volume                      2443.8(26) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       10 
  
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.35 
_exptl_crystal_size_min           0.30 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.251 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              972 
_exptl_absorpt_coefficient_mu     0.272 
_exptl_absorpt_correction_type    psiscans 
_exptl_absorpt_correction_T_min   0.82 
_exptl_absorpt_correction_T_max   1.00 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        ' Enraf-Nonius CAD4' 
_diffrn_measurement_method        \w--2\q 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   120 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             4540 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0957 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.05 
_diffrn_reflns_theta_max          19.99 
_reflns_number_total              4540 
_reflns_number_observed           3437 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Enraf-Nonius CAD4' 
_computing_cell_refinement        'Enraf-Nonius CAD4' 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'CAMERON (Watkin and Pearce,1993)' 
_computing_publication_material   SHELXL-93 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 11 with very negative 
F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-
factors 
 wR and all goodnesses 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 observed 
criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+92.5137P] 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     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4529 
_refine_ls_number_parameters      272 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1494 
_refine_ls_R_factor_obs           0.1186 
_refine_ls_wR_factor_all          0.3742 
_refine_ls_wR_factor_obs          0.3364 
_refine_ls_goodness_of_fit_all    1.064 
_refine_ls_goodness_of_fit_obs    1.145 
_refine_ls_restrained_S_all       1.113 
_refine_ls_restrained_S_obs       1.145 
_refine_ls_shift/esd_max          0.000 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Zr Zr 0.24484(13) 0.29205(13) 0.21905(11) 0.0195(7) Uani 1 d . . 
O1 O 0.2508(8) 0.2697(8) 0.0937(7) 0.019(3) Uiso 1 d . . 
O2 O 0.2660(7) 0.2766(7) 0.3511(7) 0.012(2) Uiso 1 d . . 
O3 O 0.2462(9) 0.4448(9) 0.1655(8) 0.033(3) Uiso 1 d . . 
O4 O 0.0931(9) 0.2813(9) 0.2700(8) 0.030(3) Uiso 1 d . . 
N1 N 0.4273(10) 0.2673(10) 0.1541(9) 0.016(3) Uiso 1 d . . 
N2 N 0.2976(10) 0.1068(10) 0.2837(9) 0.022(3) Uiso 1 d . . 
C1 C 0.3107(13) 0.2889(13) 0.0033(12) 0.023(4) Uiso 1 d . . 
C2 C 0.2604(11) 0.2981(11) -0.0704(10) 0.007(3) Uiso 1 d . . 
C3 C 0.3327(12) 0.3243(12) -0.1623(11) 0.017(4) Uiso 1 d . . 
H3 H 0.3034(12) 0.3374(12) -0.2162(11) 0.020 Uiso 1 calc R . 
C4 C 0.4365(12) 0.3327(12) -0.1814(11) 0.017(4) Uiso 1 d . . 
C5 C 0.4816(14) 0.3186(13) -0.1058(11) 0.023(4) Uiso 1 d . . 
H5 H 0.5549(14) 0.3233(13) -0.1164(11) 0.028 Uiso 1 calc R . 
C6 C 0.4165(12) 0.2966(12) -0.0113(11) 0.016(4) Uiso 1 d . . 
C7 C 0.4719(14) 0.2737(13) 0.0664(12) 0.024(4) Uiso 1 d . . 
H7 H 0.5472(14) 0.2627(13) 0.0506(12) 0.029 Uiso 1 calc R . 
C8 C 0.4942(12) 0.2203(12) 0.2240(11) 0.017(4) Uiso 1 d . . 
C9 C 0.5204(12) 0.2816(13) 0.2616(11) 0.021(4) Uiso 1 d . . 
H9 H 0.5019(12) 0.3565(13) 0.2389(11) 0.025 Uiso 1 calc R . 
C10 C 0.5769(14) 0.2353(14) 0.3367(12) 0.031(5) Uiso 1 d . . 
H10 H 0.6020(14) 0.2779(14) 0.3621(12) 0.037 Uiso 1 calc R . 
C11 C 0.5931(13) 0.1283(13) 0.3702(12) 0.023(4) Uiso 1 d . . 
H11 H 0.6265(13) 0.0970(13) 0.4231(12) 0.028 Uiso 1 calc R . 
C12 C 0.5660(13) 0.0626(13) 0.3351(12) 0.024(4) Uiso 1 d . . 
C13 C 0.5120(12) 0.1089(12) 0.2566(11) 0.018(4) Uiso 1 d . . 
C14 C 0.4751(13) 0.0463(13) 0.2129(12) 0.023(4) Uiso 1 d . . 
C15 C 0.5455(13) -0.0120(13) 0.1542(11) 0.020(4) Uiso 1 d . . 
C16 C 0.5047(14) -0.0645(14) 0.1122(13) 0.033(5) Uiso 1 d . . 
H16 H 0.5521(14) -0.1035(14) 0.0733(13) 0.039 Uiso 1 calc R . 
C17 C 0.3967(13) -0.0624(13) 0.1251(12) 0.025(4) Uiso 1 d . . 
H17 H 0.3697(13) -0.0985(13) 0.0949(12) 0.030 Uiso 1 calc R . 
C18 C 0.3284(14) -0.0060(13) 0.1834(12) 0.026(4) Uiso 1 d . . 
H18 H 0.2539(14) -0.0038(13) 0.1930(12) 0.032 Uiso 1 calc R . 
C19 C 0.3657(13) 0.0447(13) 0.2257(11) 0.021(4) Uiso 1 d . . 
C20 C 0.2668(13) 0.0575(14) 0.3759(12) 0.024(4) Uiso 1 d . . 
H20 H 0.2778(13) -0.0180(14) 0.3956(12) 0.029 Uiso 1 calc R . 
C21 C 0.2187(12) 0.1057(12) 0.4495(11) 0.018(4) Uiso 1 d . . 
C22 C 0.1668(12) 0.0379(13) 0.5364(11) 0.019(4) Uiso 1 d . . 
H22 H 0.1620(12) -0.0336(13) 0.5436(11) 0.022 Uiso 1 calc R . 
C23 C 0.1225(13) 0.0810(13) 0.6122(11) 0.021(4) Uiso 1 d . . 
C24 C 0.1322(13) 0.1830(13) 0.5986(12) 0.022(4) Uiso 1 d . . 
H24 H 0.0998(13) 0.2102(13) 0.6505(12) 0.026 Uiso 1 calc R . 
C25 C 0.1861(13) 0.2521(13) 0.5143(12) 0.022(4) Uiso 1 d . . 
C26 C 0.2209(12) 0.2104(12) 0.4374(11) 0.016(4) Uiso 1 d . . 
C27 C 0.6639(14) -0.0142(15) 0.1346(13) 0.036(5) Uiso 1 d . . 
H27A H 0.6950(17) -0.0828(35) 0.1726(60) 0.054 Uiso 1 calc R . 
H27B H 0.6797(14) 0.0431(56) 0.1520(74) 0.054 Uiso 1 calc R . 
H27C H 0.6940(17) -0.0041(88) 0.0663(20) 0.054 Uiso 1 calc R . 
C28 C 0.5831(15) -0.0549(14) 0.3781(13) 0.035(5) Uiso 1 d . . 
H28A H 0.5740(86) -0.0732(14) 0.4475(16) 0.052 Uiso 1 calc R . 
H28B H 0.6551(32) -0.0823(17) 0.3506(58) 0.052 Uiso 1 calc R . 
H28C H 0.5314(56) -0.0866(15) 0.3644(67) 0.052 Uiso 1 calc R . 
C29 C 0.1466(12) 0.2935(12) -0.0536(11) 0.019(4) Uiso 1 d . . 
C30 C 0.0798(14) 0.3835(14) -0.0165(13) 0.034(5) Uiso 1 d . . 
H30A H 0.0921(65) 0.3744(49) 0.0464(36) 0.051 Uiso 1 calc R . 
H30B H 0.0045(15) 0.3816(53) -0.0109(73) 0.051 Uiso 1 calc R . 
H30C H 0.1001(60) 0.4520(15) -0.0614(40) 0.051 Uiso 1 calc R . 
C31 C 0.1141(14) 0.3073(14) -0.1477(12) 0.028(4) Uiso 1 d . . 
H31A H 0.1305(73) 0.3763(36) -0.1942(27) 0.043 Uiso 1 calc R . 
H31B H 0.0378(20) 0.3040(79) -0.1345(17) 0.043 Uiso 1 calc R . 
H31C H 0.1535(59) 0.2503(47) -0.1738(39) 0.043 Uiso 1 calc R . 
C32 C 0.1173(14) 0.1858(13) 0.0150(12) 0.029(4) Uiso 1 d . . 
H32A H 0.0408(18) 0.1852(30) 0.0263(56) 0.043 Uiso 1 calc R . 
H32B H 0.1369(72) 0.1729(37) 0.0759(27) 0.043 Uiso 1 calc R . 
H32C H 0.1556(61) 0.1299(15) -0.0130(33) 0.043 Uiso 1 calc R . 
C33 C 0.5024(14) 0.3615(14) -0.2867(13) 0.031(5) Uiso 1 d . . 
C34 C 0.4574(14) 0.4685(14) -0.3462(13) 0.032(5) Uiso 1 d . . 
H34A H 0.3844(31) 0.4658(27) -0.3478(62) 0.049 Uiso 1 calc R . 
H34B H 0.5008(49) 0.4861(39) -0.4116(23) 0.049 Uiso 1 calc R . 
H34C H 0.4578(77) 0.5229(19) -0.3179(43) 0.049 Uiso 1 calc R . 
C35 C 0.5008(14) 0.2733(13) -0.3280(12) 0.028(4) Uiso 1 d . . 
H35A H 0.4271(14) 0.2657(55) -0.3231(66) 0.042 Uiso 1 calc R . 
H35B H 0.5360(71) 0.2060(21) -0.2918(47) 0.042 Uiso 1 calc R . 
H35C H 0.5382(69) 0.2924(39) -0.3954(23) 0.042 Uiso 1 calc R . 
C36 C 0.6205(14) 0.3651(15) -0.2920(13) 0.036(5) Uiso 1 d . . 
H36A H 0.6584(24) 0.3866(85) -0.3592(14) 0.054 Uiso 1 calc R . 
H36B H 0.6526(27) 0.2945(25) -0.2583(68) 0.054 Uiso 1 calc R . 
H36C H 0.6251(15) 0.4165(65) -0.2619(70) 0.054 Uiso 1 calc R . 
C37 C 0.0590(13) 0.0062(13) 0.7060(12) 0.025(4) Uiso 1 d . . 
C38 C -0.0380(16) -0.0164(16) 0.6836(14) 0.045(5) Uiso 1 d . . 
H38A H -0.0764(55) -0.0659(76) 0.7408(28) 0.067 Uiso 1 calc R . 
H38B H -0.0151(17) -0.0479(89) 0.6316(60) 0.067 Uiso 1 calc R . 
H38C H -0.0849(49) 0.0502(21) 0.6641(84) 0.067 Uiso 1 calc R . 
C39 C 0.0238(18) 0.0604(18) 0.7841(16) 0.060(6) Uiso 1 d . . 
H39A H -0.0275(89) 0.0205(67) 0.8376(48) 0.089 Uiso 1 calc R . 
H39B H -0.0094(105) 0.1332(42) 0.7578(32) 0.089 Uiso 1 calc R . 
H39C H 0.0857(25) 0.0621(104) 0.8070(74) 0.089 Uiso 1 calc R . 
C40 C 0.1269(17) -0.0964(16) 0.7427(15) 0.051(6) Uiso 1 d . . 
H40A H 0.1471(87) -0.1344(51) 0.6953(43) 0.077 Uiso 1 calc R . 
H40B H 0.0870(39) -0.1403(46) 0.8029(50) 0.077 Uiso 1 calc R . 
H40C H 0.1909(51) -0.0815(17) 0.7539(89) 0.077 Uiso 1 calc R . 
C41 C 0.1972(13) 0.3628(13) 0.5050(12) 0.027(4) Uiso 1 d . . 
C42 C 0.1398(14) 0.4467(14) 0.4303(13) 0.032(5) Uiso 1 d . . 
H42A H 0.1474(70) 0.5179(14) 0.4280(53) 0.048 Uiso 1 calc R . 
H42B H 0.0644(20) 0.4380(53) 0.4479(41) 0.048 Uiso 1 calc R . 
H42C H 0.1711(54) 0.4375(53) 0.3672(18) 0.048 Uiso 1 calc R . 
C43 C 0.1472(16) 0.3897(17) 0.6003(14) 0.048(6) Uiso 1 d . . 
H43A H 0.0718(28) 0.3805(96) 0.6198(49) 0.072 Uiso 1 calc R . 
H43B H 0.1546(89) 0.4635(34) 0.5905(28) 0.072 Uiso 1 calc R . 
H43C H 0.1839(66) 0.3420(66) 0.6505(27) 0.072 Uiso 1 calc R . 
C44 C 0.3139(15) 0.3764(16) 0.4782(14) 0.043(5) Uiso 1 d . . 
H44A H 0.3213(15) 0.4477(36) 0.4760(84) 0.065 Uiso 1 calc R . 
H44B H 0.3455(26) 0.3673(94) 0.4151(40) 0.065 Uiso 1 calc R . 
H44C H 0.3503(23) 0.3230(62) 0.5260(47) 0.065 Uiso 1 calc R . 
C45 C 0.2365(13) 0.5489(13) 0.1083(12) 0.025(4) Uiso 1 d . . 
C46 C 0.2569(14) 0.5691(14) 0.0089(13) 0.031(5) Uiso 1 d . . 
H46 H 0.2811(14) 0.5132(14) -0.0186(13) 0.038 Uiso 1 calc R . 
C47 C 0.2403(15) 0.6741(15) -0.0473(15) 0.042(5) Uiso 1 d . . 
H47 H 0.2525(15) 0.6896(15) -0.1147(15) 0.051 Uiso 1 calc R . 
C48 C 0.2070(15) 0.7563(17) -0.0096(15) 0.045(5) Uiso 1 d . . 
H48 H 0.1964(15) 0.8276(17) -0.0499(15) 0.053 Uiso 1 calc R . 
C49 C 0.1892(16) 0.7330(16) 0.0884(14) 0.046(5) Uiso 1 d . . 
H49 H 0.1670(16) 0.7888(16) 0.1161(14) 0.055 Uiso 1 calc R . 
C50 C 0.2035(13) 0.6283(13) 0.1467(13) 0.028(4) Uiso 1 d . . 
H50 H 0.1899(13) 0.6128(13) 0.2142(13) 0.033 Uiso 1 calc R . 
C51 C -0.0092(13) 0.2984(12) 0.3129(11) 0.019(4) Uiso 1 d . . 
C52 C -0.0818(13) 0.3564(13) 0.2621(13) 0.027(4) Uiso 1 d . . 
H52 H -0.0606(13) 0.3846(13) 0.1944(13) 0.033 Uiso 1 calc R . 
C53 C -0.1872(15) 0.3761(15) 0.3065(13) 0.037(5) Uiso 1 d . . 
H53 H -0.2369(15) 0.4200(15) 0.2697(13) 0.044 Uiso 1 calc R . 
C54 C -0.2194(15) 0.3319(14) 0.4036(13) 0.034(5) Uiso 1 d . . 
H54 H -0.2919(15) 0.3425(14) 0.4343(13) 0.041 Uiso 1 calc R . 
C55 C -0.1458(13) 0.2726(14) 0.4556(13) 0.029(5) Uiso 1 d . . 
H55 H -0.1674(13) 0.2442(14) 0.5232(13) 0.035 Uiso 1 calc R . 
C56 C -0.0413(14) 0.2529(14) 0.4123(12) 0.029(5) Uiso 1 d . . 
H56 H 0.0085(14) 0.2092(14) 0.4491(12) 0.035 Uiso 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 
Zr 0.0200(11) 0.0249(11) 0.0026(9) 0.0004(7) 0.0017(7) 0.0068(7) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are 
taken 
 into account individually in the estimation of esds in distances, 
angles 
 and torsion angles; correlations between esds in cell parameters are 
only 
 used when they are defined by crystal symmetry.  An approximate 
(isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. 
planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Zr O3 1.941(12) . ? 
Zr O4 1.959(11) . ? 
Zr O1 2.022(10) . ? 
Zr O2 2.045(9) . ? 
Zr N1 2.343(12) . ? 
Zr N2 2.377(13) . ? 
O1 C1 1.36(2) . ? 
O2 C26 1.37(2) . ? 
O3 C45 1.37(2) . ? 
O4 C51 1.34(2) . ? 
N1 C7 1.29(2) . ? 
N1 C8 1.46(2) . ? 
N2 C20 1.32(2) . ? 
N2 C19 1.44(2) . ? 
C1 C6 1.37(2) . ? 
C1 C2 1.41(2) . ? 
C2 C3 1.44(2) . ? 
C2 C29 1.47(2) . ? 
C3 C4 1.34(2) . ? 
C4 C5 1.38(2) . ? 
C4 C33 1.56(2) . ? 
C5 C6 1.43(2) . ? 
C6 C7 1.47(2) . ? 
C8 C9 1.31(2) . ? 
C8 C13 1.40(2) . ? 
C9 C10 1.43(2) . ? 
C10 C11 1.35(2) . ? 
C11 C12 1.34(2) . ? 
C12 C13 1.45(2) . ? 
C12 C28 1.49(2) . ? 
C13 C14 1.47(2) . ? 
C14 C19 1.41(2) . ? 
C14 C15 1.42(2) . ? 
C15 C16 1.37(2) . ? 
C15 C27 1.51(2) . ? 
C16 C17 1.38(2) . ? 
C17 C18 1.39(2) . ? 
C18 C19 1.33(2) . ? 
C20 C21 1.43(2) . ? 
C21 C26 1.37(2) . ? 
C21 C22 1.41(2) . ? 
C22 C23 1.41(2) . ? 
C23 C24 1.35(2) . ? 
C23 C37 1.57(2) . ? 
C24 C25 1.41(2) . ? 
C25 C26 1.41(2) . ? 
C25 C41 1.49(2) . ? 
C29 C32 1.52(2) . ? 
C29 C30 1.53(2) . ? 
C29 C31 1.55(2) . ? 
C33 C34 1.51(2) . ? 
C33 C35 1.54(2) . ? 
C33 C36 1.55(2) . ? 
C37 C40 1.50(3) . ? 
C37 C38 1.53(3) . ? 
C37 C39 1.53(3) . ? 
C41 C44 1.52(3) . ? 
C41 C42 1.54(2) . ? 
C41 C43 1.56(3) . ? 
C45 C50 1.34(2) . ? 
C45 C46 1.40(2) . ? 
C46 C47 1.39(3) . ? 
C47 C48 1.37(3) . ? 
C48 C49 1.38(3) . ? 
C49 C50 1.39(3) . ? 
C51 C52 1.34(2) . ? 
C51 C56 1.40(2) . ? 
C52 C53 1.39(2) . ? 
C53 C54 1.37(3) . ? 
C54 C55 1.36(2) . ? 
C55 C56 1.37(2) . ? 
  
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 
O3 Zr O4 102.1(5) . . ? 
O3 Zr O1 95.3(4) . . ? 
O4 Zr O1 95.8(4) . . ? 
O3 Zr O2 96.9(4) .. . ? 
O4 Zr O2 91.2(4) . . ? 
O1 Zr O2 164.4(4) . . ? 
O3 Zr N1 89.4(5) . . ? 
O4 Zr N1 167.0(4) . . ? 
O1 Zr N1 76.8(4) . . ? 
O2 Zr N1 93.6(4) . . ? 
O3 Zr N2 162.6(5) . . ? 
O4 Zr N2 94.3(5) . . ? 
O1 Zr N2 89.0(4) . . ? 
O2 Zr N2 76.5(4) . . ? 
N1 Zr N2 75.1(4) . . ? 
C1 O1 Zr 140.4(10) . . ? 
C26 O2 Zr 127.4(9) . . ? 
C45 O3 Zr 163.9(11) . . ? 
C51 O4 Zr 162.9(10) . . ? 
C7 N1 C8 116.9(13) . . ? 
C7 N1 Zr 126.8(11) . . ? 
C8 N1 Zr 115.2(9) . . ? 
C20 N2 C19 117.4(13) . . ? 
C20 N2 Zr 120.4(11) . . ? 
C19 N2 Zr 122.2(10) . . ? 
O1 C1 C6 118.4(14) . . ? 
O1 C1 C2 117.7(14) . . ? 
C6 C1 C2 123.9(15) . . ? 
C1 C2 C3 110.8(13) . . ? 
C1 C2 C29 122.8(13) . . ? 
C3 C2 C29 126.0(13) . . ? 
C4 C3 C2 128.1(15) . . ? 
C3 C4 C5 118.0(15) . . ? 
C3 C4 C33 120.6(14) . . ? 
C5 C4 C33 121.4(14) . . ? 
C4 C5 C6 119.1(15) . . ? 
C1 C6 C5 120.0(15) . . ? 
C1 C6 C7 123.9(14) . . ? 
C5 C6 C7 115.9(14) . . ? 
N1 C7 C6 125.8(15) . . ? 
C9 C8 C13 124.3(15) . . ? 
C9 C8 N1 119.0(14) . . ? 
C13 C8 N1 115.9(13) . . ? 
C8 C9 C10 119.5(16) . . ? 
C11 C10 C9 116.9(16) . . ? 
C12 C11 C10 125.4(17) . . ? 
C11 C12 C13 118.0(15) . . ? 
C11 C12 C28 122.3(16) . . ? 
C13 C12 C28 119.6(14) . . ? 
C8 C13 C12 115.7(14) . . ? 
C8 C13 C14 120.5(14) . . ? 
C12 C13 C14 123.8(14) . . ? 
C19 C14 C15 116.9(15) . . ? 
C19 C14 C13 120.1(14) . . ? 
C15 C14 C13 122.9(15) . . ? 
C16 C15 C14 119.5(15) . . ? 
C16 C15 C27 119.2(15) . . ? 
C14 C15 C27 121.2(14) . . ? 
C15 C16 C17 121.8(16) . . ? 
C16 C17 C18 118.4(16) . . ? 
C19 C18 C17 121.1(16) . . ? 
C18 C19 C14 122.3(15) . . ? 
C18 C19 N2 122.7(15) . . ? 
C14 C19 N2 114.9(14) . . ? 
N2 C20 C21 126.9(15) . . ? 
C26 C21 C22 121.6(14) . . ? 
C26 C21 C20 123.2(15) . . ? 
C22 C21 C20 115.2(14) . . ? 
C23 C22 C21 116.9(14) . . ? 
C24 C23 C22 119.3(15) . . ? 
C24 C23 C37 124.7(14) . . ? 
C22 C23 C37 115.9(14) . . ? 
C23 C24 C25 125.6(15) . . ? 
C26 C25 C24 113.8(14) . . ? 
C26 C25 C41 123.1(14) . . ? 
C24 C25 C41 123.0(14) . . ? 
O2 C26 C21 120.9(13) . . ? 
O2 C26 C25 116.9(13) . . ? 
C21 C26 C25 122.0(14) . . ? 
C2 C29 C32 111.0(13) . . ? 
C2 C29 C30 111.5(13) . . ? 
C32 C29 C30 110.7(14) . . ? 
C2 C29 C31 111.1(13) . . ? 
C32 C29 C31 106.2(13) . . ? 
C30 C29 C31 106.1(13) . . ? 
C34 C33 C35 110.9(15) . . ? 
C34 C33 C36 108.4(15) . . ? 
C35 C33 C36 106.6(14) . . ? 
C34 C33 C4 110.5(14) . . ? 
C35 C33 C4 108.4(14) . . ? 
C36 C33 C4 111.9(14) . . ? 
C40 C37 C38 109.6(15) . . ? 
C40 C37 C39 108.0(16) . . ? 
C38 C37 C39 109.9(16) . . ? 
C40 C37 C23 110.8(14) . . ? 
C38 C37 C23 108.7(14) . . ? 
C39 C37 C23 109.8(14) . . ? 
C25 C41 C44 109.5(14) . . ? 
C25 C41 C42 112.3(14) . . ? 
C44 C41 C42 109.6(15) . . ? 
C25 C41 C43 112.2(15) . . ? 
C44 C41 C43 107.9(15) . . ? 
C42 C41 C43 105.1(14) . . ? 
C50 C45 O3 120.8(15) . . ? 
C50 C45 C46 121.2(16) . . ? 
O3 C45 C46 117.9(15) . . ? 
C47 C46 C45 117.2(17) . . ? 
C48 C47 C46 122.6(19) . . ? 
C47 C48 C49 118.3(20) . . ? 
C48 C49 C50 120.4(19) . . ? 
C45 C50 C49 120.4(17) . . ? 
C52 C51 O4 121.1(15) . . ? 
C52 C51 C56 119.3(16) . . ? 
O4 C51 C56 119.6(14) . . ? 
C51 C52 C53 121.2(17) . . ? 
C54 C53 C52 119.9(18) . . ? 
C55 C54 C53 119.1(18) . . ? 
C54 C55 C56 121.4(17) . . ? 
C55 C56 C51 119.0(16) . . ? 
  
_refine_diff_density_max    1.369 
_refine_diff_density_min   -1.700 
_refine_diff_density_rms    0.179