Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Chan, Michael C. W.'
'Pui, Yung-Lin'
'Tam, Ka-Ho'
'Zhu, Nianyong'

_publ_contact_author_name     	'Dr Michael C. W. Chan'  
_publ_contact_author_address 
;
Chemistry
The University of Hong Kong
Pokfulam Road
Hong Kong
HONG KONG
;

_publ_contact_author_email       'MCWCHAN@HKU.HK'

_publ_section_title		
;
Surprising Activity for Group 4 Polyolefin Catalysts
[M{(OAr)2py}Cl2(thf)] (M = Zr, Ti) Bearing Tridentate
Pyridine-2,6-Bis(aryloxide) Ligands
;

data_mar441                       185372
_database_code_CSD 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C45 H55 Cl2 N O3 Zr'
_chemical_formula_sum
'C45 H55 Cl2 N O3 Zr'
_chemical_formula_weight          820.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'Zr'  'Zr'  -2.9673   0.5597
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'   0.1484   0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0106   0.0060
'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'
'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'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P 1 21/n 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                    14.466(3)
_cell_length_b                    16.874(3)
_cell_length_c                    18.241(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.36(3)
_cell_angle_gamma                 90.00
_cell_volume                      4451.4(16)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     0
_cell_measurement_theta_min       0
_cell_measurement_theta_max       0

_exptl_crystal_description        prism
_exptl_crystal_colour             'pale yellow'
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.4
_exptl_crystal_size_min           0.25
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.224
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1720
_exptl_absorpt_coefficient_mu     0.404
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Marresearch Imaging Plate mar300'
_diffrn_measurement_method        Oscillation
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             21781
_diffrn_reflns_av_R_equivalents   0.0404
_diffrn_reflns_av_sigmaI/netI     0.0776
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          1.64
_diffrn_reflns_theta_max          25.33
_reflns_number_total              6330
_reflns_number_gt                 3673
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        Marcontrol
_computing_cell_refinement        Scalepack
_computing_data_reduction         Denzo
_computing_structure_solution     'SIR-97'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0827P)^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          6330
_refine_ls_number_parameters      440
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0765
_refine_ls_R_factor_gt            0.0423
_refine_ls_wR_factor_ref          0.1375
_refine_ls_wR_factor_gt           0.1136
_refine_ls_goodness_of_fit_ref    0.904
_refine_ls_restrained_S_all       0.904
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.26199(3) 0.54249(2) 0.25998(2) 0.06269(19) Uani 1 1 d . . .
Cl1 Cl 0.22638(10) 0.60434(7) 0.37562(7) 0.0952(4) Uani 1 1 d . . .
Cl2 Cl 0.22213(10) 0.64940(7) 0.17813(8) 0.1051(5) Uani 1 1 d . . .
O1 O 0.14434(19) 0.48780(15) 0.24159(15) 0.0675(7) Uani 1 1 d . . .
O2 O 0.3948(2) 0.56489(14) 0.25625(15) 0.0673(8) Uani 1 1 d . . .
O3 O 0.3044(2) 0.43547(15) 0.32591(16) 0.0727(8) Uani 1 1 d . . .
N1 N 0.3056(2) 0.45495(17) 0.16138(18) 0.0601(8) Uiso 1 1 d . . .
C1 C 0.0954(3) 0.4587(2) 0.1826(2) 0.0656(11) Uani 1 1 d . . .
C2 C -0.0001(3) 0.4723(2) 0.1750(3) 0.0720(12) Uani 1 1 d . . .
C3 C -0.0418(3) 0.4415(3) 0.1117(3) 0.0833(14) Uani 1 1 d . . .
H3 H -0.1050 0.4497 0.1045 0.100 Uiso 1 1 calc R . .
C4 C 0.0041(4) 0.3999(3) 0.0591(3) 0.0824(14) Uani 1 1 d . . .
C5 C 0.0968(3) 0.3865(2) 0.0704(3) 0.0765(13) Uani 1 1 d . . .
H5 H 0.1288 0.3573 0.0360 0.092 Uiso 1 1 calc R . .
C6 C 0.1441(3) 0.4155(2) 0.1322(2) 0.0651(11) Uani 1 1 d . . .
C7 C 0.2443(3) 0.3967(2) 0.1413(2) 0.0644(11) Uani 1 1 d . . .
C8 C 0.2730(3) 0.3202(3) 0.1264(2) 0.0755(13) Uani 1 1 d . . .
H8 H 0.2295 0.2808 0.1164 0.091 Uiso 1 1 calc R . .
C9 C 0.3652(4) 0.3027(2) 0.1262(3) 0.0849(14) Uani 1 1 d . . .
H9 H 0.3851 0.2509 0.1193 0.102 Uiso 1 1 calc R . .
C10 C 0.4285(3) 0.3637(3) 0.1366(3) 0.0780(13) Uani 1 1 d . . .
H10 H 0.4915 0.3540 0.1326 0.094 Uiso 1 1 calc R . .
C11 C 0.3972(3) 0.4394(2) 0.1530(2) 0.0626(11) Uani 1 1 d . . .
C12 C 0.4673(3) 0.5043(2) 0.1575(2) 0.0613(11) Uani 1 1 d . . .
C13 C 0.4652(3) 0.5644(2) 0.2094(2) 0.0623(11) Uani 1 1 d . . .
C14 C 0.5355(3) 0.6229(2) 0.2140(2) 0.0670(12) Uani 1 1 d . . .
C15 C 0.6040(3) 0.6184(3) 0.1618(3) 0.0727(12) Uani 1 1 d . . .
H15 H 0.6513 0.6557 0.1637 0.087 Uiso 1 1 calc R . .
C16 C 0.6055(3) 0.5614(3) 0.1070(3) 0.0722(12) Uani 1 1 d . . .
C17 C 0.5369(3) 0.5042(3) 0.1061(2) 0.0691(12) Uani 1 1 d . . .
H17 H 0.5373 0.4649 0.0704 0.083 Uiso 1 1 calc R . .
C18 C -0.0538(3) 0.5172(3) 0.2332(3) 0.0915(15) Uani 1 1 d . . .
C19 C -0.1571(4) 0.5244(4) 0.2110(4) 0.150(3) Uani 1 1 d . . .
H19A H -0.1890 0.5531 0.2481 0.226 Uiso 1 1 calc R . .
H19B H -0.1834 0.4724 0.2058 0.226 Uiso 1 1 calc R . .
H19C H -0.1630 0.5521 0.1651 0.226 Uiso 1 1 calc R . .
C20 C -0.0462(4) 0.4734(3) 0.3069(3) 0.1099(18) Uani 1 1 d . . .
H20A H -0.0791 0.5024 0.3433 0.165 Uiso 1 1 calc R . .
H20B H 0.0177 0.4691 0.3218 0.165 Uiso 1 1 calc R . .
H20C H -0.0723 0.4214 0.3017 0.165 Uiso 1 1 calc R . .
C21 C -0.0158(4) 0.6022(3) 0.2428(3) 0.120(2) Uani 1 1 d . . .
H21A H -0.0499 0.6292 0.2798 0.180 Uiso 1 1 calc R . .
H21B H -0.0221 0.6303 0.1972 0.180 Uiso 1 1 calc R . .
H21C H 0.0484 0.5999 0.2575 0.180 Uiso 1 1 calc R . .
C22 C -0.0476(4) 0.3698(3) -0.0094(3) 0.1183(19) Uani 1 1 d . . .
H22A H -0.0055 0.3417 -0.0399 0.177 Uiso 1 1 calc R . .
H22B H -0.0734 0.4139 -0.0361 0.177 Uiso 1 1 calc R . .
H22C H -0.0964 0.3348 0.0047 0.177 Uiso 1 1 calc R . .
C23 C 0.5335(3) 0.6888(3) 0.2708(3) 0.0852(14) Uani 1 1 d . . .
C24 C 0.4490(3) 0.7435(3) 0.2547(3) 0.1034(17) Uani 1 1 d . . .
H24A H 0.4478 0.7852 0.2904 0.155 Uiso 1 1 calc R . .
H24B H 0.3931 0.7130 0.2570 0.155 Uiso 1 1 calc R . .
H24C H 0.4539 0.7660 0.2066 0.155 Uiso 1 1 calc R . .
C25 C 0.5289(5) 0.6568(3) 0.3489(3) 0.129(2) Uani 1 1 d . . .
H25A H 0.5276 0.7003 0.3828 0.194 Uiso 1 1 calc R . .
H25B H 0.5823 0.6246 0.3594 0.194 Uiso 1 1 calc R . .
H25C H 0.4740 0.6255 0.3537 0.194 Uiso 1 1 calc R . .
C26 C 0.6209(3) 0.7422(3) 0.2677(3) 0.117(2) Uani 1 1 d . . .
H26A H 0.6171 0.7833 0.3040 0.175 Uiso 1 1 calc R . .
H26B H 0.6244 0.7657 0.2199 0.175 Uiso 1 1 calc R . .
H26C H 0.6750 0.7107 0.2773 0.175 Uiso 1 1 calc R . .
C27 C 0.6785(3) 0.5626(3) 0.0487(3) 0.0958(15) Uani 1 1 d . . .
H27A H 0.7200 0.6062 0.0577 0.144 Uiso 1 1 calc R . .
H27B H 0.6492 0.5687 0.0013 0.144 Uiso 1 1 calc R . .
H27C H 0.7126 0.5138 0.0503 0.144 Uiso 1 1 calc R . .
C28 C 0.2421(4) 0.3783(3) 0.3570(3) 0.115(2) Uani 1 1 d . . .
H28A H 0.2231 0.3394 0.3205 0.139 Uiso 1 1 calc R . .
H28B H 0.1874 0.4044 0.3751 0.139 Uiso 1 1 calc R . .
C29 C 0.2938(5) 0.3402(3) 0.4174(3) 0.127(2) Uani 1 1 d . . .
H29A H 0.2811 0.3660 0.4636 0.153 Uiso 1 1 calc R . .
H29B H 0.2773 0.2847 0.4210 0.153 Uiso 1 1 calc R . .
C30 C 0.3913(5) 0.3490(4) 0.3994(5) 0.174(4) Uani 1 1 d . . .
H30A H 0.4292 0.3546 0.4436 0.209 Uiso 1 1 calc R . .
H30B H 0.4125 0.3033 0.3723 0.209 Uiso 1 1 calc R . .
C31 C 0.3965(4) 0.4204(4) 0.3546(4) 0.132(2) Uani 1 1 d . . .
H31A H 0.4181 0.4648 0.3841 0.159 Uiso 1 1 calc R . .
H31B H 0.4389 0.4126 0.3148 0.159 Uiso 1 1 calc R . .
C32 C 0.6744(5) 0.4201(6) 0.3992(6) 0.199(4) Uani 1 1 d G . .
C33 C 0.6576(5) 0.4344(5) 0.3251(7) 0.178(3) Uani 1 1 d G . .
H33 H 0.6567 0.4861 0.3075 0.214 Uiso 1 1 calc R . .
C34 C 0.6423(4) 0.3714(9) 0.2772(3) 0.186(4) Uani 1 1 d G . .
H34 H 0.6311 0.3810 0.2276 0.223 Uiso 1 1 calc R . .
C35 C 0.6437(4) 0.2941(7) 0.3035(7) 0.234(7) Uani 1 1 d G . .
H35 H 0.6334 0.2520 0.2715 0.281 Uiso 1 1 calc R . .
C36 C 0.6605(5) 0.2798(4) 0.3777(8) 0.279(9) Uani 1 1 d G . .
H36 H 0.6614 0.2281 0.3953 0.335 Uiso 1 1 calc R . .
C37 C 0.6758(5) 0.3428(8) 0.4256(4) 0.243(6) Uani 1 1 d G . .
H37 H 0.6870 0.3332 0.4752 0.291 Uiso 1 1 calc R . .
C38 C 0.7062(17) 0.4881(10) 0.4354(11) 0.498(16) Uani 1 1 d . . .
H38A H 0.7183 0.4761 0.4861 0.747 Uiso 1 1 calc R . .
H38B H 0.6600 0.5288 0.4314 0.747 Uiso 1 1 calc R . .
H38C H 0.7620 0.5060 0.4133 0.747 Uiso 1 1 calc R . .
C39 C 0.0369(4) 0.2814(6) 0.4912(5) 0.194(5) Uani 1 1 d G . .
C40 C 0.0751(5) 0.2103(5) 0.4681(3) 0.144(3) Uani 1 1 d G . .
H40 H 0.0506 0.1847 0.4269 0.173 Uiso 1 1 calc R . .
C41 C 0.1499(6) 0.1775(3) 0.5066(5) 0.164(3) Uani 1 1 d G . .
H41 H 0.1754 0.1300 0.4911 0.197 Uiso 1 1 calc R . .
C42 C 0.1864(4) 0.2158(6) 0.5682(4) 0.192(5) Uani 1 1 d G . .
H42 H 0.2364 0.1939 0.5940 0.231 Uiso 1 1 calc R . .
C43 C 0.1483(7) 0.2869(6) 0.5913(3) 0.273(9) Uani 1 1 d G . .
H43 H 0.1727 0.3125 0.6325 0.327 Uiso 1 1 calc R . .
C44 C 0.0735(7) 0.3197(3) 0.5528(6) 0.268(8) Uani 1 1 d G . .
H44 H 0.0480 0.3672 0.5683 0.322 Uiso 1 1 calc R . .
C45 C -0.0334(9) 0.3340(11) 0.4719(8) 0.430(14) Uani 1 1 d . . .
H45A H -0.0315 0.3786 0.5045 0.645 Uiso 1 1 calc R . .
H45B H -0.0921 0.3079 0.4752 0.645 Uiso 1 1 calc R . .
H45C H -0.0252 0.3519 0.4225 0.645 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
Zr1 0.0710(3) 0.0629(3) 0.0544(3) 0.00022(19) 0.0067(2) 0.0029(2)
Cl1 0.1224(11) 0.0939(9) 0.0699(9) -0.0168(6) 0.0156(8) 0.0111(7)
Cl2 0.1186(11) 0.0954(9) 0.1008(11) 0.0369(7) -0.0035(8) 0.0059(7)
O1 0.0635(18) 0.0780(17) 0.061(2) -0.0023(14) 0.0056(15) 0.0059(14)
O2 0.071(2) 0.0703(17) 0.0603(19) -0.0051(13) 0.0063(16) -0.0057(13)
O3 0.071(2) 0.0731(18) 0.075(2) 0.0148(14) 0.0046(17) 0.0033(15)
C1 0.068(3) 0.067(3) 0.061(3) 0.003(2) 0.002(3) -0.003(2)
C2 0.061(3) 0.085(3) 0.069(3) 0.004(2) 0.001(3) 0.005(2)
C3 0.065(3) 0.107(4) 0.078(4) 0.012(3) -0.004(3) -0.002(3)
C4 0.081(4) 0.098(3) 0.068(4) 0.000(3) 0.000(3) -0.016(3)
C5 0.074(4) 0.089(3) 0.067(3) -0.006(2) 0.010(3) -0.011(3)
C6 0.067(3) 0.067(2) 0.061(3) -0.002(2) 0.003(3) -0.008(2)
C7 0.067(3) 0.070(3) 0.056(3) -0.001(2) 0.013(2) -0.003(2)
C8 0.075(4) 0.067(3) 0.086(4) -0.013(2) 0.013(3) -0.005(2)
C9 0.084(4) 0.060(3) 0.111(4) -0.012(2) 0.012(3) 0.001(3)
C10 0.069(3) 0.078(3) 0.088(4) -0.008(2) 0.013(3) 0.012(3)
C11 0.064(3) 0.066(3) 0.058(3) 0.0003(19) 0.005(2) 0.003(2)
C12 0.053(3) 0.068(3) 0.064(3) 0.002(2) 0.007(2) 0.002(2)
C13 0.059(3) 0.069(3) 0.059(3) 0.009(2) 0.003(2) 0.001(2)
C14 0.067(3) 0.070(3) 0.064(3) 0.000(2) -0.008(3) 0.000(2)
C15 0.061(3) 0.081(3) 0.076(4) 0.006(3) -0.002(3) -0.004(2)
C16 0.059(3) 0.087(3) 0.070(3) 0.007(3) 0.004(3) 0.001(2)
C17 0.062(3) 0.084(3) 0.061(3) -0.004(2) -0.001(2) 0.004(2)
C18 0.067(3) 0.115(4) 0.093(4) -0.006(3) 0.003(3) 0.019(3)
C19 0.077(4) 0.231(7) 0.143(6) -0.041(5) 0.001(4) 0.044(4)
C20 0.113(5) 0.127(4) 0.091(4) 0.009(3) 0.031(3) 0.018(3)
C21 0.122(5) 0.109(4) 0.128(5) -0.013(4) 0.012(4) 0.038(4)
C22 0.097(4) 0.168(5) 0.089(4) -0.008(4) -0.019(3) -0.031(4)
C23 0.081(4) 0.091(3) 0.083(4) -0.012(3) -0.001(3) -0.017(3)
C24 0.097(4) 0.081(3) 0.133(5) -0.029(3) 0.014(3) -0.004(3)
C25 0.173(6) 0.133(5) 0.081(4) -0.018(4) -0.021(4) -0.021(4)
C26 0.096(4) 0.114(4) 0.141(6) -0.038(4) -0.004(4) -0.030(3)
C27 0.074(3) 0.133(4) 0.081(4) 0.001(3) 0.014(3) -0.010(3)
C28 0.105(4) 0.107(4) 0.134(5) 0.050(4) -0.011(4) -0.028(3)
C29 0.184(7) 0.095(4) 0.103(5) 0.034(3) 0.005(5) -0.017(4)
C30 0.115(6) 0.180(7) 0.225(9) 0.132(7) -0.013(6) 0.005(5)
C31 0.090(4) 0.163(5) 0.143(6) 0.080(5) -0.008(4) 0.000(4)
C32 0.246(11) 0.186(11) 0.164(11) -0.040(8) -0.027(8) 0.013(8)
C33 0.123(7) 0.239(11) 0.172(11) -0.015(9) -0.004(7) 0.002(6)
C34 0.093(5) 0.247(11) 0.218(11) -0.033(12) 0.000(6) -0.011(7)
C35 0.170(10) 0.206(15) 0.33(2) -0.044(11) 0.075(11) -0.044(9)
C36 0.236(14) 0.219(14) 0.39(3) -0.028(15) 0.125(16) 0.003(10)
C37 0.261(13) 0.185(10) 0.282(15) 0.013(12) -0.008(10) 0.075(10)
C38 0.72(4) 0.327(18) 0.45(3) -0.21(2) -0.10(3) 0.06(2)
C39 0.180(10) 0.157(7) 0.251(14) 0.057(8) 0.119(10) 0.004(7)
C40 0.131(7) 0.206(10) 0.094(5) 0.020(6) -0.017(5) -0.079(6)
C41 0.199(11) 0.156(6) 0.141(8) -0.004(6) 0.095(7) -0.064(7)
C42 0.122(6) 0.361(16) 0.095(7) 0.038(7) 0.015(6) -0.050(9)
C43 0.200(13) 0.39(2) 0.233(14) -0.187(14) 0.096(11) -0.104(12)
C44 0.256(15) 0.350(16) 0.203(13) -0.120(12) 0.079(11) -0.181(13)
C45 0.227(13) 0.72(3) 0.353(19) 0.37(2) 0.117(12) 0.216(17)

_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
Zr1 O1 1.958(3) . ?
Zr1 O2 1.960(3) . ?
Zr1 O3 2.247(3) . ?
Zr1 Cl2 2.4033(12) . ?
Zr1 Cl1 2.4199(13) . ?
Zr1 N1 2.422(3) . ?
O1 C1 1.365(5) . ?
O2 C13 1.345(5) . ?
O3 C31 1.442(6) . ?
O3 C28 1.446(5) . ?
N1 C11 1.363(5) . ?
N1 C7 1.368(5) . ?
C1 C6 1.380(6) . ?
C1 C2 1.402(6) . ?
C2 C3 1.391(6) . ?
C2 C18 1.532(7) . ?
C3 C4 1.373(6) . ?
C4 C5 1.370(6) . ?
C4 C22 1.529(6) . ?
C5 C6 1.394(6) . ?
C6 C7 1.490(6) . ?
C7 C8 1.384(5) . ?
C8 C9 1.366(6) . ?
C9 C10 1.387(6) . ?
C10 C11 1.390(5) . ?
C11 C12 1.494(5) . ?
C12 C13 1.388(6) . ?
C12 C17 1.392(6) . ?
C13 C14 1.418(5) . ?
C14 C15 1.392(6) . ?
C14 C23 1.522(6) . ?
C15 C16 1.388(6) . ?
C16 C17 1.384(6) . ?
C16 C27 1.516(6) . ?
C18 C20 1.535(7) . ?
C18 C19 1.543(7) . ?
C18 C21 1.545(7) . ?
C23 C25 1.527(7) . ?
C23 C24 1.554(6) . ?
C23 C26 1.555(6) . ?
C28 C29 1.464(7) . ?
C29 C30 1.463(8) . ?
C30 C31 1.458(7) . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C32 C38 1.395(15) . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C39 C45 1.390(11) . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C40 C41 1.3900 . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O2 158.96(11) . . ?
O1 Zr1 O3 86.46(11) . . ?
O2 Zr1 O3 85.30(11) . . ?
O1 Zr1 Cl2 93.01(9) . . ?
O2 Zr1 Cl2 93.13(9) . . ?
O3 Zr1 Cl2 173.87(8) . . ?
O1 Zr1 Cl1 98.66(9) . . ?
O2 Zr1 Cl1 100.14(9) . . ?
O3 Zr1 Cl1 86.62(8) . . ?
Cl2 Zr1 Cl1 99.49(5) . . ?
O1 Zr1 N1 79.98(11) . . ?
O2 Zr1 N1 79.58(11) . . ?
O3 Zr1 N1 80.49(10) . . ?
Cl2 Zr1 N1 93.40(8) . . ?
Cl1 Zr1 N1 167.10(8) . . ?
C1 O1 Zr1 137.5(3) . . ?
C13 O2 Zr1 141.1(3) . . ?
C31 O3 C28 108.6(3) . . ?
C31 O3 Zr1 125.0(3) . . ?
C28 O3 Zr1 125.6(3) . . ?
C11 N1 C7 117.2(3) . . ?
C11 N1 Zr1 118.2(2) . . ?
C7 N1 Zr1 117.3(3) . . ?
O1 C1 C6 116.8(4) . . ?
O1 C1 C2 120.7(4) . . ?
C6 C1 C2 122.5(4) . . ?
C3 C2 C1 115.4(4) . . ?
C3 C2 C18 122.8(4) . . ?
C1 C2 C18 121.8(4) . . ?
C4 C3 C2 124.3(5) . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C22 121.7(5) . . ?
C3 C4 C22 120.4(5) . . ?
C4 C5 C6 121.5(5) . . ?
C1 C6 C5 118.4(4) . . ?
C1 C6 C7 123.3(4) . . ?
C5 C6 C7 118.3(4) . . ?
N1 C7 C8 121.8(4) . . ?
N1 C7 C6 120.0(3) . . ?
C8 C7 C6 118.2(4) . . ?
C9 C8 C7 120.0(4) . . ?
C8 C9 C10 118.7(4) . . ?
C9 C10 C11 119.5(4) . . ?
N1 C11 C10 121.6(4) . . ?
N1 C11 C12 120.8(3) . . ?
C10 C11 C12 117.5(4) . . ?
C13 C12 C17 119.2(4) . . ?
C13 C12 C11 123.2(4) . . ?
C17 C12 C11 117.6(4) . . ?
O2 C13 C12 117.8(4) . . ?
O2 C13 C14 120.7(4) . . ?
C12 C13 C14 121.4(4) . . ?
C15 C14 C13 116.3(4) . . ?
C15 C14 C23 122.1(4) . . ?
C13 C14 C23 121.6(4) . . ?
C16 C15 C14 123.6(4) . . ?
C17 C16 C15 117.9(4) . . ?
C17 C16 C27 120.9(4) . . ?
C15 C16 C27 121.2(4) . . ?
C16 C17 C12 121.4(4) . . ?
C2 C18 C20 110.0(4) . . ?
C2 C18 C19 111.1(4) . . ?
C20 C18 C19 108.5(5) . . ?
C2 C18 C21 110.6(4) . . ?
C20 C18 C21 109.2(5) . . ?
C19 C18 C21 107.3(4) . . ?
C14 C23 C25 112.3(4) . . ?
C14 C23 C24 109.4(4) . . ?
C25 C23 C24 109.6(5) . . ?
C14 C23 C26 111.7(4) . . ?
C25 C23 C26 107.0(4) . . ?
C24 C23 C26 106.6(4) . . ?
O3 C28 C29 106.0(4) . . ?
C30 C29 C28 105.4(5) . . ?
C31 C30 C29 105.8(5) . . ?
O3 C31 C30 106.9(5) . . ?
C33 C32 C37 120.0 . . ?
C33 C32 C38 111.4(13) . . ?
C37 C32 C38 127.3(13) . . ?
C34 C33 C32 120.0 . . ?
C35 C34 C33 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C37 120.0 . . ?
C36 C37 C32 120.0 . . ?
C45 C39 C40 140.2(11) . . ?
C45 C39 C44 99.8(11) . . ?
C40 C39 C44 120.0 . . ?
C41 C40 C39 120.0 . . ?
C42 C41 C40 120.0 . . ?
C43 C42 C41 120.0 . . ?
C44 C43 C42 120.0 . . ?
C43 C44 C39 120.0 . . ?

_diffrn_measured_fraction_theta_max    0.778
_diffrn_reflns_theta_full              25.33
_diffrn_measured_fraction_theta_full   0.778
_refine_diff_density_max    0.531
_refine_diff_density_min   -0.366
_refine_diff_density_rms    0.096

data_mar544
_database_code_CSD                185373
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C37 H41 Cl2 D6 N O3 Zr'
_chemical_formula_sum
'C37 H41 Cl2 D6 N O3 Zr'
_chemical_formula_weight          721.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'Zr'  'Zr'  -2.9673   0.5597
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'   0.1484   0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0106   0.0060
'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'
'C'  'C'   0.0033   0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'D'  'D'   0.0000   0.0000
'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'

_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    'P b c a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                    15.485(3)
_cell_length_b                    18.357(4)
_cell_length_c                    26.266(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      7466(3)
_cell_formula_units_Z             8
_cell_measurement_temperature     301(2)
_cell_measurement_reflns_used     0
_cell_measurement_theta_min       0
_cell_measurement_theta_max       0

_exptl_crystal_description        prism
_exptl_crystal_colour             'pale yellow'
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.284
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2992
_exptl_absorpt_coefficient_mu     0.471
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       301(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Marresearch Imaging Plate mar300'
_diffrn_measurement_method        Oscillation
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             31515
_diffrn_reflns_av_R_equivalents   0.0397
_diffrn_reflns_av_sigmaI/netI     0.0554
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -31
_diffrn_reflns_limit_l_max        31
_diffrn_reflns_theta_min          1.89
_diffrn_reflns_theta_max          25.35
_reflns_number_total              6225
_reflns_number_gt                 3982
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        MarControl
_computing_cell_refinement        Scalepack
_computing_data_reduction         Denzo
_computing_structure_solution     'SIR-97'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0571P)^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          6225
_refine_ls_number_parameters      397
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0613
_refine_ls_R_factor_gt            0.0336
_refine_ls_wR_factor_ref          0.1017
_refine_ls_wR_factor_gt           0.0877
_refine_ls_goodness_of_fit_ref    0.948
_refine_ls_restrained_S_all       0.948
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.246185(18) 0.188430(13) 0.637655(9) 0.04225(11) Uani 1 1 d . . .
Cl1 Cl 0.33263(6) 0.09906(4) 0.68248(3) 0.0763(3) Uani 1 1 d . . .
Cl2 Cl 0.22354(6) 0.11970(4) 0.56092(3) 0.0707(3) Uani 1 1 d . . .
O1 O 0.33664(12) 0.24884(9) 0.60784(7) 0.0496(5) Uani 1 1 d . . .
O2 O 0.13193(13) 0.16253(9) 0.66472(7) 0.0494(5) Uani 1 1 d . . .
O3 O 0.26165(13) 0.25744(10) 0.70996(7) 0.0562(5) Uani 1 1 d . . .
N1 N 0.16259(15) 0.29373(10) 0.61064(8) 0.0413(5) Uani 1 1 d . . .
C1 C 0.35134(19) 0.30396(13) 0.57429(10) 0.0445(7) Uani 1 1 d . . .
C2 C 0.42917(19) 0.30710(13) 0.54672(10) 0.0475(7) Uani 1 1 d . . .
C3 C 0.4384(2) 0.36614(15) 0.51367(11) 0.0563(8) Uani 1 1 d . . .
H3 H 0.4891 0.3701 0.4949 0.068 Uiso 1 1 calc R . .
C4 C 0.3754(2) 0.41927(15) 0.50754(11) 0.0541(8) Uani 1 1 d . . .
C5 C 0.3018(2) 0.41384(14) 0.53567(11) 0.0533(8) Uani 1 1 d . . .
H5 H 0.2595 0.4494 0.5318 0.064 Uiso 1 1 calc R . .
C6 C 0.2873(2) 0.35698(13) 0.57014(10) 0.0463(7) Uani 1 1 d . . .
C7 C 0.20619(19) 0.35671(13) 0.59931(10) 0.0468(7) Uani 1 1 d . . .
C8 C 0.1712(2) 0.42468(14) 0.61302(13) 0.0586(8) Uani 1 1 d . . .
H8 H 0.2034 0.4669 0.6082 0.070 Uiso 1 1 calc R . .
C9 C 0.0904(2) 0.42899(15) 0.63331(13) 0.0676(10) Uani 1 1 d . . .
H9 H 0.0682 0.4736 0.6437 0.081 Uiso 1 1 calc R . .
C10 C 0.0424(2) 0.36678(15) 0.63814(12) 0.0613(9) Uani 1 1 d . . .
H10 H -0.0146 0.3695 0.6491 0.074 Uiso 1 1 calc R . .
C11 C 0.0789(2) 0.29963(13) 0.62668(10) 0.0460(7) Uani 1 1 d . . .
C12 C 0.02121(19) 0.23495(13) 0.63046(10) 0.0446(7) Uani 1 1 d . . .
C13 C 0.0480(2) 0.16870(14) 0.65147(10) 0.0453(7) Uani 1 1 d . . .
C14 C -0.0109(2) 0.11132(14) 0.65888(11) 0.0505(7) Uani 1 1 d . . .
C15 C -0.0947(2) 0.12220(15) 0.64213(11) 0.0554(8) Uani 1 1 d . . .
H15 H -0.1345 0.0850 0.6470 0.066 Uiso 1 1 calc R . .
C16 C -0.1225(2) 0.18571(15) 0.61845(12) 0.0556(8) Uani 1 1 d . . .
C17 C -0.0635(2) 0.24194(14) 0.61395(11) 0.0520(7) Uani 1 1 d . . .
H17 H -0.0811 0.2857 0.5994 0.062 Uiso 1 1 calc R . .
C18 C 0.4997(2) 0.24939(16) 0.55191(11) 0.0582(8) Uani 1 1 d . . .
C19 C 0.5799(2) 0.2673(2) 0.51986(14) 0.0850(11) Uani 1 1 d . . .
H19A H 0.6224 0.2298 0.5243 0.128 Uiso 1 1 calc R . .
H19B H 0.6035 0.3132 0.5306 0.128 Uiso 1 1 calc R . .
H19C H 0.5641 0.2702 0.4846 0.128 Uiso 1 1 calc R . .
C20 C 0.5293(3) 0.2417(2) 0.60727(13) 0.0894(12) Uani 1 1 d . . .
H20A H 0.5734 0.2051 0.6094 0.134 Uiso 1 1 calc R . .
H20B H 0.4811 0.2277 0.6281 0.134 Uiso 1 1 calc R . .
H20C H 0.5518 0.2874 0.6190 0.134 Uiso 1 1 calc R . .
C21 C 0.4638(2) 0.17578(17) 0.53260(15) 0.0831(11) Uani 1 1 d . . .
H21A H 0.5075 0.1390 0.5358 0.125 Uiso 1 1 calc R . .
H21B H 0.4474 0.1804 0.4975 0.125 Uiso 1 1 calc R . .
H21C H 0.4143 0.1623 0.5525 0.125 Uiso 1 1 calc R . .
C22 C 0.3895(2) 0.48217(16) 0.47086(13) 0.0744(10) Uani 1 1 d . . .
H22A H 0.4442 0.4765 0.4542 0.112 Uiso 1 1 calc R . .
H22B H 0.3888 0.5273 0.4893 0.112 Uiso 1 1 calc R . .
H22C H 0.3442 0.4825 0.4459 0.112 Uiso 1 1 calc R . .
C23 C 0.0174(2) 0.03885(15) 0.68359(12) 0.0631(9) Uani 1 1 d . . .
C24 C 0.0546(3) 0.05336(18) 0.73674(14) 0.0921(13) Uani 1 1 d . . .
H24A H 0.0717 0.0081 0.7520 0.138 Uiso 1 1 calc R . .
H24B H 0.0114 0.0762 0.7576 0.138 Uiso 1 1 calc R . .
H24C H 0.1038 0.0849 0.7340 0.138 Uiso 1 1 calc R . .
C25 C 0.0834(3) 0.00017(18) 0.64940(16) 0.0898(13) Uani 1 1 d . . .
H25A H 0.1004 -0.0449 0.6649 0.135 Uiso 1 1 calc R . .
H25B H 0.1331 0.0307 0.6450 0.135 Uiso 1 1 calc R . .
H25C H 0.0578 -0.0095 0.6168 0.135 Uiso 1 1 calc R . .
C26 C -0.0605(2) -0.01278(17) 0.69050(16) 0.0935(13) Uani 1 1 d . . .
H26A H -0.0415 -0.0574 0.7059 0.140 Uiso 1 1 calc R . .
H26B H -0.0857 -0.0231 0.6579 0.140 Uiso 1 1 calc R . .
H26C H -0.1027 0.0100 0.7120 0.140 Uiso 1 1 calc R . .
C27 C -0.2133(2) 0.19221(16) 0.59761(14) 0.0749(10) Uani 1 1 d . . .
H27A H -0.2444 0.1480 0.6043 0.112 Uiso 1 1 calc R . .
H27B H -0.2109 0.2005 0.5615 0.112 Uiso 1 1 calc R . .
H27C H -0.2422 0.2323 0.6138 0.112 Uiso 1 1 calc R . .
C28 C 0.3237(3) 0.31614(18) 0.71629(15) 0.0874(12) Uani 1 1 d . . .
H28A H 0.3375 0.3361 0.6831 0.105 Uiso 1 1 calc R . .
H28B H 0.2973 0.3546 0.7362 0.105 Uiso 1 1 calc R . .
C29 C 0.4027(3) 0.2941(3) 0.7409(2) 0.138(2) Uani 1 1 d . . .
H29A H 0.4407 0.3352 0.7437 0.207 Uiso 1 1 calc R . .
H29B H 0.4301 0.2567 0.7211 0.207 Uiso 1 1 calc R . .
H29C H 0.3899 0.2757 0.7742 0.207 Uiso 1 1 calc R . .
C30 C 0.2198(3) 0.2361(2) 0.75704(14) 0.0972(14) Uani 1 1 d . . .
H30A H 0.2598 0.2425 0.7851 0.117 Uiso 1 1 calc R . .
H30B H 0.2045 0.1849 0.7553 0.117 Uiso 1 1 calc R . .
C31 C 0.1425(4) 0.2792(4) 0.7663(2) 0.175(3) Uani 1 1 d . . .
H31A H 0.1157 0.2633 0.7974 0.262 Uiso 1 1 calc R . .
H31B H 0.1029 0.2729 0.7386 0.262 Uiso 1 1 calc R . .
H31C H 0.1579 0.3297 0.7692 0.262 Uiso 1 1 calc R . .
C32 C 0.2977(4) 0.0908(3) 0.4248(3) 0.1131(17) Uani 1 1 d . . .
D32 H 0.2761 0.1278 0.4454 0.136 Uiso 1 1 calc R . .
C33 C 0.3516(5) 0.0441(4) 0.4440(2) 0.1243(19) Uani 1 1 d . . .
D33 H 0.3686 0.0483 0.4778 0.149 Uiso 1 1 calc R . .
C34 C 0.3834(4) -0.0108(4) 0.4149(4) 0.145(2) Uani 1 1 d . . .
D34 H 0.4223 -0.0439 0.4287 0.174 Uiso 1 1 calc R . .
C35 C 0.3583(5) -0.0175(3) 0.3654(3) 0.136(2) Uani 1 1 d . . .
D35 H 0.3795 -0.0552 0.3453 0.163 Uiso 1 1 calc R . .
C36 C 0.3023(5) 0.0315(5) 0.3459(2) 0.130(2) Uani 1 1 d . . .
D36 H 0.2840 0.0279 0.3123 0.155 Uiso 1 1 calc R . .
C37 C 0.2726(3) 0.0868(4) 0.3765(3) 0.1203(17) Uani 1 1 d . . .
D37 H 0.2350 0.1215 0.3634 0.144 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
Zr1 0.0375(2) 0.04545(17) 0.04383(16) 0.00122(10) -0.00299(13) 0.00407(11)
Cl1 0.0755(7) 0.0719(5) 0.0815(6) 0.0098(4) -0.0222(5) 0.0248(4)
Cl2 0.0830(7) 0.0722(5) 0.0569(5) -0.0156(4) -0.0085(4) 0.0004(4)
O1 0.0371(13) 0.0572(11) 0.0545(12) 0.0048(9) 0.0014(10) 0.0060(9)
O2 0.0383(14) 0.0511(10) 0.0587(12) 0.0090(8) -0.0043(10) 0.0002(9)
O3 0.0541(16) 0.0688(12) 0.0456(11) -0.0096(9) 0.0019(10) -0.0107(10)
N1 0.0332(16) 0.0421(12) 0.0485(14) 0.0004(9) -0.0025(11) 0.0010(9)
C1 0.0398(19) 0.0484(15) 0.0454(16) -0.0003(11) -0.0006(13) -0.0036(12)
C2 0.039(2) 0.0573(16) 0.0466(16) -0.0034(12) 0.0001(14) -0.0016(13)
C3 0.049(2) 0.0674(18) 0.0526(18) -0.0022(14) 0.0081(15) -0.0092(16)
C4 0.055(2) 0.0525(16) 0.0552(18) 0.0046(13) 0.0036(16) -0.0035(15)
C5 0.048(2) 0.0484(15) 0.0631(19) 0.0030(13) 0.0041(17) 0.0032(14)
C6 0.0407(19) 0.0458(15) 0.0525(17) -0.0033(12) 0.0005(15) -0.0041(13)
C7 0.039(2) 0.0483(15) 0.0529(17) 0.0034(12) 0.0002(15) 0.0021(13)
C8 0.049(2) 0.0410(15) 0.085(2) -0.0043(13) 0.0132(19) -0.0026(13)
C9 0.056(3) 0.0442(17) 0.103(3) -0.0072(14) 0.018(2) 0.0054(15)
C10 0.042(2) 0.0548(17) 0.087(2) -0.0045(14) 0.0150(17) 0.0077(14)
C11 0.039(2) 0.0491(15) 0.0498(17) 0.0010(11) -0.0002(14) 0.0032(12)
C12 0.035(2) 0.0491(15) 0.0498(17) 0.0000(11) 0.0018(14) 0.0017(12)
C13 0.039(2) 0.0548(16) 0.0422(16) -0.0001(11) -0.0020(13) 0.0002(14)
C14 0.045(2) 0.0530(16) 0.0540(17) 0.0039(12) 0.0029(15) -0.0037(14)
C15 0.043(2) 0.0525(16) 0.071(2) 0.0032(13) 0.0007(17) -0.0051(14)
C16 0.037(2) 0.0634(18) 0.0662(19) -0.0032(14) -0.0012(16) 0.0001(15)
C17 0.041(2) 0.0555(16) 0.0594(18) 0.0023(13) 0.0003(16) 0.0057(14)
C18 0.042(2) 0.0797(19) 0.0535(19) 0.0030(15) 0.0045(16) 0.0093(16)
C19 0.051(3) 0.117(3) 0.087(3) 0.011(2) 0.020(2) 0.016(2)
C20 0.057(3) 0.138(3) 0.074(3) 0.012(2) -0.006(2) 0.025(2)
C21 0.068(3) 0.076(2) 0.105(3) -0.0081(19) 0.007(2) 0.0204(19)
C22 0.079(3) 0.0669(19) 0.077(2) 0.0160(16) 0.018(2) -0.0026(17)
C23 0.053(2) 0.0559(17) 0.081(2) 0.0200(15) -0.0020(18) -0.0021(15)
C24 0.102(4) 0.090(2) 0.084(3) 0.038(2) -0.018(2) -0.010(2)
C25 0.089(3) 0.056(2) 0.124(3) 0.0180(18) 0.011(3) 0.0135(19)
C26 0.074(3) 0.064(2) 0.143(4) 0.036(2) -0.006(3) -0.0160(19)
C27 0.044(2) 0.079(2) 0.101(3) 0.0022(18) -0.011(2) -0.0013(17)
C28 0.101(4) 0.091(2) 0.071(2) -0.0129(18) -0.001(2) -0.028(2)
C29 0.095(4) 0.196(5) 0.123(4) 0.014(3) -0.038(3) -0.053(4)
C30 0.090(4) 0.145(3) 0.056(2) -0.021(2) 0.008(2) -0.034(3)
C31 0.088(4) 0.311(8) 0.124(5) -0.074(5) 0.032(4) 0.025(5)
C32 0.122(5) 0.096(3) 0.122(5) -0.009(3) 0.032(4) -0.019(3)
C33 0.149(6) 0.117(4) 0.107(4) 0.007(4) -0.003(4) -0.041(4)
C34 0.135(6) 0.116(5) 0.183(7) 0.051(5) 0.013(5) 0.010(4)
C35 0.172(7) 0.092(4) 0.143(6) -0.010(4) 0.064(5) -0.020(4)
C36 0.136(6) 0.155(5) 0.098(4) -0.001(4) 0.016(4) -0.067(5)
C37 0.083(4) 0.131(5) 0.147(6) 0.029(4) 0.010(4) -0.007(3)

_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
Zr1 O1 1.9507(18) . ?
Zr1 O2 1.965(2) . ?
Zr1 O3 2.2954(19) . ?
Zr1 Cl2 2.4035(8) . ?
Zr1 Cl1 2.4227(8) . ?
Zr1 N1 2.432(2) . ?
O1 C1 1.361(3) . ?
O2 C13 1.350(3) . ?
O3 C30 1.450(4) . ?
O3 C28 1.454(4) . ?
N1 C11 1.367(3) . ?
N1 C7 1.372(3) . ?
C1 C6 1.394(4) . ?
C1 C2 1.407(4) . ?
C2 C3 1.396(4) . ?
C2 C18 1.527(4) . ?
C3 C4 1.388(4) . ?
C4 C5 1.362(4) . ?
C4 C22 1.519(4) . ?
C5 C6 1.400(4) . ?
C6 C7 1.470(4) . ?
C7 C8 1.407(4) . ?
C8 C9 1.362(4) . ?
C9 C10 1.369(4) . ?
C10 C11 1.389(4) . ?
C11 C12 1.489(4) . ?
C12 C17 1.387(4) . ?
C12 C13 1.399(4) . ?
C13 C14 1.407(4) . ?
C14 C15 1.384(4) . ?
C14 C23 1.544(4) . ?
C15 C16 1.390(4) . ?
C16 C17 1.383(4) . ?
C16 C27 1.514(4) . ?
C18 C20 1.531(4) . ?
C18 C19 1.537(4) . ?
C18 C21 1.546(4) . ?
C23 C24 1.533(4) . ?
C23 C25 1.534(5) . ?
C23 C26 1.545(4) . ?
C28 C29 1.440(6) . ?
C30 C31 1.455(6) . ?
C32 C33 1.298(7) . ?
C32 C37 1.329(7) . ?
C33 C34 1.358(8) . ?
C34 C35 1.363(8) . ?
C35 C36 1.350(8) . ?
C36 C37 1.374(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O2 158.32(7) . . ?
O1 Zr1 O3 86.77(7) . . ?
O2 Zr1 O3 85.88(7) . . ?
O1 Zr1 Cl2 93.81(6) . . ?
O2 Zr1 Cl2 92.58(6) . . ?
O3 Zr1 Cl2 177.09(6) . . ?
O1 Zr1 Cl1 100.56(6) . . ?
O2 Zr1 Cl1 99.08(6) . . ?
O3 Zr1 Cl1 85.06(6) . . ?
Cl2 Zr1 Cl1 97.63(3) . . ?
O1 Zr1 N1 79.24(7) . . ?
O2 Zr1 N1 79.55(7) . . ?
O3 Zr1 N1 81.86(7) . . ?
Cl2 Zr1 N1 95.45(6) . . ?
Cl1 Zr1 N1 166.91(5) . . ?
C1 O1 Zr1 143.39(18) . . ?
C13 O2 Zr1 138.85(16) . . ?
C30 O3 C28 113.5(3) . . ?
C30 O3 Zr1 120.68(19) . . ?
C28 O3 Zr1 124.94(19) . . ?
C11 N1 C7 117.8(2) . . ?
C11 N1 Zr1 118.53(15) . . ?
C7 N1 Zr1 118.11(18) . . ?
O1 C1 C6 116.8(2) . . ?
O1 C1 C2 120.5(2) . . ?
C6 C1 C2 122.7(2) . . ?
C3 C2 C1 116.1(3) . . ?
C3 C2 C18 121.4(3) . . ?
C1 C2 C18 122.5(2) . . ?
C4 C3 C2 123.1(3) . . ?
C5 C4 C3 118.3(3) . . ?
C5 C4 C22 121.3(3) . . ?
C3 C4 C22 120.4(3) . . ?
C4 C5 C6 122.7(3) . . ?
C1 C6 C5 117.1(3) . . ?
C1 C6 C7 124.4(2) . . ?
C5 C6 C7 118.5(3) . . ?
N1 C7 C8 120.1(3) . . ?
N1 C7 C6 122.4(2) . . ?
C8 C7 C6 117.3(2) . . ?
C9 C8 C7 120.4(3) . . ?
C8 C9 C10 119.1(3) . . ?
C9 C10 C11 120.0(3) . . ?
N1 C11 C10 121.5(3) . . ?
N1 C11 C12 121.7(2) . . ?
C10 C11 C12 116.7(3) . . ?
C17 C12 C13 119.0(3) . . ?
C17 C12 C11 118.2(2) . . ?
C13 C12 C11 122.8(3) . . ?
O2 C13 C12 117.4(2) . . ?
O2 C13 C14 121.7(2) . . ?
C12 C13 C14 120.9(3) . . ?
C15 C14 C13 117.1(3) . . ?
C15 C14 C23 121.6(3) . . ?
C13 C14 C23 121.3(3) . . ?
C14 C15 C16 123.6(3) . . ?
C17 C16 C15 117.4(3) . . ?
C17 C16 C27 121.6(3) . . ?
C15 C16 C27 121.0(3) . . ?
C16 C17 C12 121.9(3) . . ?
C2 C18 C20 111.3(2) . . ?
C2 C18 C19 112.4(2) . . ?
C20 C18 C19 107.3(3) . . ?
C2 C18 C21 108.7(3) . . ?
C20 C18 C21 109.8(3) . . ?
C19 C18 C21 107.3(3) . . ?
C24 C23 C25 111.4(3) . . ?
C24 C23 C14 109.9(2) . . ?
C25 C23 C14 110.0(3) . . ?
C24 C23 C26 107.0(3) . . ?
C25 C23 C26 107.7(3) . . ?
C14 C23 C26 110.9(3) . . ?
C29 C28 O3 113.8(3) . . ?
O3 C30 C31 111.3(4) . . ?
C33 C32 C37 121.5(6) . . ?
C32 C33 C34 120.3(6) . . ?
C33 C34 C35 120.1(6) . . ?
C36 C35 C34 119.0(6) . . ?
C35 C36 C37 119.0(6) . . ?
C32 C37 C36 120.1(6) . . ?

_diffrn_measured_fraction_theta_max    0.911
_diffrn_reflns_theta_full              25.35
_diffrn_measured_fraction_theta_full   0.911
_refine_diff_density_max    0.279
_refine_diff_density_min   -0.351
_refine_diff_density_rms    0.053

data_mar470
_database_code_CSD                185374
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C38 H47 Cl2 N O3 Ti'
_chemical_formula_sum
'C38 H47 Cl2 N O3 Ti'
_chemical_formula_weight          684.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'Ti'  'Ti'   0.2776   0.4457
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'   0.1484   0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0106   0.0060
'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'
'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'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P 1 21/n 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                    15.904(3)
_cell_length_b                    15.026(3)
_cell_length_c                    16.426(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  110.49(3)
_cell_angle_gamma                 90.00
_cell_volume                      3677.0(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     0
_cell_measurement_theta_min       0
_cell_measurement_theta_max       0

_exptl_crystal_description        prism
_exptl_crystal_colour             brown
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.237
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1448
_exptl_absorpt_coefficient_mu     0.413
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Marresearch Imaging Plate mar300'
_diffrn_measurement_method        Oscillation
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             15780
_diffrn_reflns_av_R_equivalents   0.0530
_diffrn_reflns_av_sigmaI/netI     0.0918
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.89
_diffrn_reflns_theta_max          25.34
_reflns_number_total              4771
_reflns_number_gt                 2808
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        MarControl
_computing_cell_refinement        Scalepack
_computing_data_reduction         Denzo
_computing_structure_solution     'SIR-97'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX publication routines (Farrugia, 1999)'

_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          4771
_refine_ls_number_parameters      405
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0923
_refine_ls_R_factor_gt            0.0477
_refine_ls_wR_factor_ref          0.1462
_refine_ls_wR_factor_gt           0.1193
_refine_ls_goodness_of_fit_ref    0.910
_refine_ls_restrained_S_all       0.910
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.06693(5) 0.22370(5) 0.85113(5) 0.0409(3) Uani 1 1 d . A .
Cl1 Cl -0.06917(7) 0.15120(8) 0.81148(8) 0.0625(4) Uani 1 1 d . . .
Cl2 Cl 0.06068(8) 0.27668(8) 0.71842(7) 0.0578(4) Uani 1 1 d . . .
O1 O 0.13206(18) 0.12627(17) 0.84459(17) 0.0436(7) Uani 1 1 d . . .
O2 O 0.02915(17) 0.33078(17) 0.87926(17) 0.0429(7) Uani 1 1 d . . .
O3 O 0.08768(19) 0.18702(18) 0.98314(17) 0.0507(8) Uani 1 1 d . . .
N1 N 0.2066(2) 0.2842(2) 0.91756(19) 0.0398(8) Uani 1 1 d . . .
C1 C 0.2145(3) 0.0983(3) 0.8505(3) 0.0408(11) Uani 1 1 d . A .
C2 C 0.2253(3) 0.0218(3) 0.8059(3) 0.0425(11) Uani 1 1 d . . .
C3 C 0.3125(3) -0.0027(3) 0.8162(3) 0.0494(12) Uani 1 1 d . . .
H3 H 0.3214 -0.0530 0.7872 0.059 Uiso 1 1 calc R . .
C4 C 0.3876(3) 0.0448(3) 0.8680(3) 0.0539(12) Uani 1 1 d . . .
C5 C 0.3742(3) 0.1192(3) 0.9110(3) 0.0536(12) Uani 1 1 d . A .
H5 H 0.4237 0.1516 0.9454 0.064 Uiso 1 1 calc R . .
C6 C 0.2879(3) 0.1473(3) 0.9041(3) 0.0423(11) Uani 1 1 d . . .
C7 C 0.2791(3) 0.2293(3) 0.9512(3) 0.0415(11) Uani 1 1 d . A .
C8 C 0.3491(3) 0.2518(3) 1.0273(3) 0.0554(13) Uani 1 1 d . . .
H8 H 0.3955 0.2116 1.0521 0.066 Uiso 1 1 calc R A .
C9 C 0.3503(3) 0.3325(3) 1.0658(3) 0.0627(14) Uani 1 1 d . A .
H9 H 0.3950 0.3465 1.1183 0.075 Uiso 1 1 calc R . .
C10 C 0.2839(3) 0.3927(3) 1.0250(3) 0.0541(13) Uani 1 1 d . . .
H10 H 0.2867 0.4502 1.0469 0.065 Uiso 1 1 calc R A .
C11 C 0.2120(3) 0.3679(3) 0.9506(3) 0.0425(11) Uani 1 1 d . A .
C12 C 0.1448(3) 0.4365(3) 0.9085(2) 0.0419(11) Uani 1 1 d . . .
C13 C 0.0527(3) 0.4167(3) 0.8776(3) 0.0415(11) Uani 1 1 d . A .
C14 C -0.0123(3) 0.4839(3) 0.8468(3) 0.0452(11) Uani 1 1 d . . .
C15 C 0.0202(3) 0.5683(3) 0.8408(3) 0.0552(13) Uani 1 1 d . A .
H15 H -0.0213 0.6138 0.8195 0.066 Uiso 1 1 calc R . .
C16 C 0.1104(3) 0.5894(3) 0.8646(3) 0.0567(13) Uani 1 1 d . . .
C17 C 0.1718(3) 0.5229(3) 0.9011(3) 0.0505(12) Uani 1 1 d . A .
H17 H 0.2327 0.5363 0.9212 0.061 Uiso 1 1 calc R . .
C18 C 0.1441(3) -0.0303(3) 0.7458(3) 0.0498(12) Uani 1 1 d . . .
C19 C 0.0827(3) -0.0604(3) 0.7945(3) 0.0703(15) Uani 1 1 d . . .
H19A H 0.0327 -0.0929 0.7557 0.106 Uiso 1 1 calc R . .
H19B H 0.0611 -0.0092 0.8162 0.106 Uiso 1 1 calc R . .
H19C H 0.1157 -0.0980 0.8423 0.106 Uiso 1 1 calc R . .
C20 C 0.1729(3) -0.1143(3) 0.7094(3) 0.0711(15) Uani 1 1 d . . .
H20A H 0.1206 -0.1453 0.6726 0.107 Uiso 1 1 calc R . .
H20B H 0.2064 -0.1524 0.7565 0.107 Uiso 1 1 calc R . .
H20C H 0.2097 -0.0979 0.6764 0.107 Uiso 1 1 calc R . .
C21 C 0.0907(3) 0.0291(3) 0.6688(3) 0.0704(15) Uani 1 1 d . . .
H21A H 0.0398 -0.0033 0.6312 0.106 Uiso 1 1 calc R . .
H21B H 0.1285 0.0462 0.6369 0.106 Uiso 1 1 calc R . .
H21C H 0.0704 0.0813 0.6901 0.106 Uiso 1 1 calc R . .
C22 C 0.4808(3) 0.0157(3) 0.8760(3) 0.0696(15) Uani 1 1 d . . .
H22A H 0.4772 -0.0370 0.8418 0.104 Uiso 1 1 calc R . .
H22B H 0.5151 0.0033 0.9357 0.104 Uiso 1 1 calc R . .
H22C H 0.5096 0.0622 0.8553 0.104 Uiso 1 1 calc R . .
C23 C 0.1407(4) 0.6819(3) 0.8511(4) 0.0911(19) Uani 1 1 d . A .
H23A H 0.2051 0.6839 0.8712 0.137 Uiso 1 1 calc R . .
H23B H 0.1191 0.7241 0.8830 0.137 Uiso 1 1 calc R . .
H23C H 0.1171 0.6965 0.7903 0.137 Uiso 1 1 calc R . .
C24 C -0.1130(3) 0.4638(3) 0.8208(3) 0.0554(13) Uani 1 1 d . A .
C25 C -0.1704(3) 0.5492(3) 0.7979(4) 0.0828(18) Uani 1 1 d . . .
H25A H -0.2327 0.5340 0.7821 0.124 Uiso 1 1 calc R A .
H25B H -0.1608 0.5787 0.7500 0.124 Uiso 1 1 calc R . .
H25C H -0.1534 0.5882 0.8473 0.124 Uiso 1 1 calc R . .
C26 C -0.1308(3) 0.4201(4) 0.8974(4) 0.0876(18) Uani 1 1 d . . .
H26A H -0.1937 0.4070 0.8812 0.131 Uiso 1 1 calc R A .
H26B H -0.1130 0.4599 0.9462 0.131 Uiso 1 1 calc R . .
H26C H -0.0970 0.3659 0.9129 0.131 Uiso 1 1 calc R . .
C27 C -0.1439(3) 0.4025(3) 0.7413(3) 0.0784(17) Uani 1 1 d . . .
H27A H -0.2068 0.3902 0.7261 0.118 Uiso 1 1 calc R A .
H27B H -0.1107 0.3479 0.7546 0.118 Uiso 1 1 calc R . .
H27C H -0.1337 0.4312 0.6934 0.118 Uiso 1 1 calc R . .
C28 C 0.0825(8) 0.2441(7) 1.0515(7) 0.064(3) Uiso 0.50 1 d P A 1
H28A H 0.0265 0.2770 1.0320 0.076 Uiso 0.50 1 calc PR A 1
H28B H 0.1317 0.2864 1.0677 0.076 Uiso 0.50 1 calc PR A 1
C28' C 0.0402(8) 0.2312(7) 1.0350(6) 0.057(3) Uiso 0.50 1 d P A 2
H28C H -0.0235 0.2179 1.0127 0.068 Uiso 0.50 1 calc PR A 2
H28D H 0.0487 0.2952 1.0366 0.068 Uiso 0.50 1 calc PR A 2
C29 C 0.0875(5) 0.1884(4) 1.1257(3) 0.094(2) Uani 1 1 d . . .
H29A H 0.0355 0.1983 1.1425 0.113 Uiso 0.50 1 calc PR A 1
H29B H 0.1410 0.2025 1.1749 0.113 Uiso 0.50 1 calc PR A 1
H29C H 0.1472 0.2124 1.1543 0.113 Uiso 0.50 1 d PR A 2
H29D H 0.0525 0.1953 1.1633 0.113 Uiso 0.50 1 d PR A 2
C30 C 0.0902(4) 0.0942(4) 1.0988(3) 0.0851(17) Uani 1 1 d . A .
H30A H 0.1352 0.0608 1.1438 0.102 Uiso 1 1 calc R . .
H30B H 0.0323 0.0658 1.0866 0.102 Uiso 1 1 calc R . .
C31 C 0.1136(4) 0.0999(3) 1.0189(3) 0.0809(17) Uani 1 1 d . A .
H31A H 0.1775 0.0912 1.0330 0.097 Uiso 1 1 calc R . .
H31B H 0.0817 0.0546 0.9775 0.097 Uiso 1 1 calc R . .
C32 C 0.1949(6) 0.3209(6) 1.4552(7) 0.133(3) Uani 1 1 d . . .
C33 C 0.1527(6) 0.3118(7) 1.5146(5) 0.118(3) Uani 1 1 d . . .
H33 H 0.1564 0.3545 1.5567 0.141 Uiso 1 1 calc R . .
C34 C 0.1023(7) 0.2306(8) 1.5067(7) 0.151(4) Uani 1 1 d . . .
H34 H 0.0727 0.2237 1.5462 0.181 Uiso 1 1 calc R . .
C35 C 0.0929(6) 0.1684(7) 1.4544(8) 0.146(3) Uani 1 1 d . . .
H35 H 0.0594 0.1175 1.4539 0.175 Uiso 1 1 calc R . .
C36 C 0.1416(8) 0.1846(8) 1.3917(6) 0.154(4) Uani 1 1 d . . .
H36 H 0.1378 0.1422 1.3493 0.185 Uiso 1 1 calc R . .
C37 C 0.1895(6) 0.2570(7) 1.3952(5) 0.122(3) Uani 1 1 d . . .
H37 H 0.2197 0.2644 1.3564 0.147 Uiso 1 1 calc R . .
C38 C 0.2500(6) 0.3970(6) 1.4582(6) 0.204(6) Uani 1 1 d . . .
H38A H 0.2494 0.4356 1.5046 0.306 Uiso 1 1 calc R . .
H38B H 0.2272 0.4285 1.4040 0.306 Uiso 1 1 calc R . .
H38C H 0.3104 0.3780 1.4680 0.306 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
Ti1 0.0412(5) 0.0370(5) 0.0431(4) -0.0013(4) 0.0129(4) -0.0021(4)
Cl1 0.0492(7) 0.0569(8) 0.0781(8) -0.0061(6) 0.0179(6) -0.0144(6)
Cl2 0.0685(8) 0.0569(8) 0.0453(6) 0.0039(5) 0.0165(6) -0.0027(6)
O1 0.0433(17) 0.0407(18) 0.0466(16) -0.0054(13) 0.0155(14) 0.0007(13)
O2 0.0437(16) 0.0344(18) 0.0505(16) -0.0016(13) 0.0164(14) -0.0005(13)
O3 0.068(2) 0.0406(19) 0.0489(17) 0.0017(14) 0.0269(16) 0.0056(15)
N1 0.041(2) 0.042(2) 0.0323(18) -0.0016(16) 0.0085(16) -0.0012(17)
C1 0.045(3) 0.037(3) 0.042(2) 0.007(2) 0.017(2) 0.007(2)
C2 0.054(3) 0.035(3) 0.043(2) 0.003(2) 0.023(2) 0.003(2)
C3 0.058(3) 0.044(3) 0.047(3) -0.001(2) 0.019(2) 0.006(2)
C4 0.055(3) 0.052(3) 0.056(3) 0.003(2) 0.021(3) 0.013(2)
C5 0.050(3) 0.053(3) 0.053(3) -0.001(2) 0.013(2) 0.001(2)
C6 0.040(3) 0.042(3) 0.043(2) 0.002(2) 0.011(2) 0.007(2)
C7 0.034(2) 0.049(3) 0.039(2) 0.001(2) 0.010(2) 0.005(2)
C8 0.048(3) 0.059(3) 0.051(3) -0.006(2) 0.006(3) 0.011(2)
C9 0.051(3) 0.073(4) 0.049(3) -0.017(3) -0.001(2) 0.002(3)
C10 0.050(3) 0.048(3) 0.059(3) -0.019(2) 0.013(3) -0.002(2)
C11 0.041(3) 0.041(3) 0.045(3) -0.007(2) 0.014(2) -0.003(2)
C12 0.046(3) 0.035(3) 0.044(3) -0.005(2) 0.015(2) -0.003(2)
C13 0.051(3) 0.031(3) 0.043(2) -0.0017(19) 0.017(2) -0.002(2)
C14 0.050(3) 0.041(3) 0.043(2) -0.004(2) 0.014(2) 0.003(2)
C15 0.066(3) 0.040(3) 0.057(3) 0.003(2) 0.019(3) 0.010(2)
C16 0.065(3) 0.038(3) 0.068(3) -0.001(2) 0.025(3) -0.003(2)
C17 0.049(3) 0.043(3) 0.061(3) -0.008(2) 0.020(2) -0.008(2)
C18 0.064(3) 0.040(3) 0.052(3) -0.010(2) 0.028(3) -0.006(2)
C19 0.081(4) 0.056(3) 0.082(4) -0.017(3) 0.039(3) -0.022(3)
C20 0.081(4) 0.053(3) 0.084(4) -0.022(3) 0.036(3) -0.008(3)
C21 0.081(4) 0.061(3) 0.059(3) -0.006(3) 0.012(3) -0.004(3)
C22 0.058(3) 0.076(4) 0.075(3) -0.008(3) 0.024(3) 0.015(3)
C23 0.102(4) 0.039(3) 0.133(5) 0.010(3) 0.042(4) -0.007(3)
C24 0.048(3) 0.049(3) 0.061(3) -0.008(2) 0.009(2) 0.007(2)
C25 0.061(3) 0.064(4) 0.109(4) -0.009(3) 0.011(3) 0.021(3)
C26 0.067(4) 0.094(5) 0.115(5) 0.007(4) 0.047(4) 0.005(3)
C27 0.056(3) 0.075(4) 0.085(4) -0.014(3) 0.000(3) 0.007(3)
C29 0.151(6) 0.080(5) 0.067(3) 0.018(3) 0.056(4) 0.021(4)
C30 0.108(5) 0.078(5) 0.076(4) 0.021(3) 0.041(4) -0.007(3)
C31 0.127(5) 0.050(4) 0.073(4) 0.019(3) 0.044(4) 0.017(3)
C32 0.135(7) 0.108(7) 0.105(7) 0.020(6) -0.023(6) 0.020(6)
C33 0.143(7) 0.126(8) 0.064(5) -0.006(5) 0.010(5) 0.055(6)
C34 0.135(8) 0.134(9) 0.144(9) -0.020(7) -0.001(6) 0.052(7)
C35 0.123(7) 0.139(9) 0.139(8) 0.005(7) 0.002(6) -0.025(6)
C36 0.178(10) 0.150(10) 0.116(7) -0.027(7) 0.027(7) 0.042(8)
C37 0.140(8) 0.115(7) 0.081(5) -0.030(5) -0.001(5) 0.037(6)
C38 0.194(9) 0.129(7) 0.177(9) 0.055(6) -0.076(8) -0.065(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
Ti1 O1 1.818(3) . ?
Ti1 O2 1.832(3) . ?
Ti1 O3 2.148(3) . ?
Ti1 Cl2 2.2899(14) . ?
Ti1 N1 2.292(3) . ?
Ti1 Cl1 2.3042(14) . ?
O1 C1 1.348(5) . ?
O2 C13 1.347(4) . ?
O3 C31 1.435(5) . ?
O3 C28 1.438(11) . ?
O3 C28' 1.478(11) . ?
N1 C11 1.361(5) . ?
N1 C7 1.368(5) . ?
C1 C6 1.399(6) . ?
C1 C2 1.406(6) . ?
C2 C3 1.386(6) . ?
C2 C18 1.536(6) . ?
C3 C4 1.397(6) . ?
C4 C5 1.377(6) . ?
C4 C22 1.507(6) . ?
C5 C6 1.403(6) . ?
C6 C7 1.487(6) . ?
C7 C8 1.394(6) . ?
C8 C9 1.364(6) . ?
C9 C10 1.373(6) . ?
C10 C11 1.400(5) . ?
C11 C12 1.471(5) . ?
C12 C17 1.387(6) . ?
C12 C13 1.404(5) . ?
C13 C14 1.406(5) . ?
C14 C15 1.386(6) . ?
C14 C24 1.536(6) . ?
C15 C16 1.385(6) . ?
C16 C17 1.380(6) . ?
C16 C23 1.513(6) . ?
C18 C19 1.532(6) . ?
C18 C20 1.534(6) . ?
C18 C21 1.539(6) . ?
C24 C27 1.531(6) . ?
C24 C26 1.532(7) . ?
C24 C25 1.544(6) . ?
C28 C29 1.457(11) . ?
C28' C29 1.555(11) . ?
C29 C30 1.487(7) . ?
C30 C31 1.486(7) . ?
C32 C37 1.356(11) . ?
C32 C33 1.372(11) . ?
C32 C38 1.432(10) . ?
C33 C34 1.441(12) . ?
C34 C35 1.242(11) . ?
C35 C36 1.510(13) . ?
C36 C37 1.317(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O2 164.98(12) . . ?
O1 Ti1 O3 87.92(11) . . ?
O2 Ti1 O3 85.35(12) . . ?
O1 Ti1 Cl2 93.41(10) . . ?
O2 Ti1 Cl2 91.49(9) . . ?
O3 Ti1 Cl2 172.03(9) . . ?
O1 Ti1 N1 82.54(12) . . ?
O2 Ti1 N1 83.13(12) . . ?
O3 Ti1 N1 80.81(11) . . ?
Cl2 Ti1 N1 91.56(9) . . ?
O1 Ti1 Cl1 95.79(9) . . ?
O2 Ti1 Cl1 97.35(9) . . ?
O3 Ti1 Cl1 87.78(9) . . ?
Cl2 Ti1 Cl1 99.90(6) . . ?
N1 Ti1 Cl1 168.51(9) . . ?
C1 O1 Ti1 143.8(3) . . ?
C13 O2 Ti1 135.9(3) . . ?
C31 O3 C28 108.1(5) . . ?
C31 O3 C28' 107.7(5) . . ?
C28 O3 C28' 26.1(5) . . ?
C31 O3 Ti1 124.6(3) . . ?
C28 O3 Ti1 127.2(5) . . ?
C28' O3 Ti1 122.5(4) . . ?
C11 N1 C7 118.0(3) . . ?
C11 N1 Ti1 118.2(3) . . ?
C7 N1 Ti1 119.5(3) . . ?
O1 C1 C6 117.2(4) . . ?
O1 C1 C2 120.7(4) . . ?
C6 C1 C2 122.1(4) . . ?
C3 C2 C1 116.9(4) . . ?
C3 C2 C18 121.6(4) . . ?
C1 C2 C18 121.5(4) . . ?
C2 C3 C4 123.0(4) . . ?
C5 C4 C3 118.3(4) . . ?
C5 C4 C22 121.0(4) . . ?
C3 C4 C22 120.6(4) . . ?
C4 C5 C6 121.7(4) . . ?
C1 C6 C5 118.0(4) . . ?
C1 C6 C7 123.6(4) . . ?
C5 C6 C7 118.3(4) . . ?
N1 C7 C8 120.8(4) . . ?
N1 C7 C6 120.6(3) . . ?
C8 C7 C6 118.5(4) . . ?
C9 C8 C7 120.6(4) . . ?
C8 C9 C10 118.4(4) . . ?
C9 C10 C11 120.3(4) . . ?
N1 C11 C10 120.8(4) . . ?
N1 C11 C12 121.7(3) . . ?
C10 C11 C12 117.5(4) . . ?
C17 C12 C13 118.9(4) . . ?
C17 C12 C11 120.0(4) . . ?
C13 C12 C11 121.1(4) . . ?
O2 C13 C12 117.2(4) . . ?
O2 C13 C14 121.4(4) . . ?
C12 C13 C14 121.4(4) . . ?
C15 C14 C13 116.0(4) . . ?
C15 C14 C24 122.6(4) . . ?
C13 C14 C24 121.5(4) . . ?
C16 C15 C14 124.4(4) . . ?
C17 C16 C15 117.5(4) . . ?
C17 C16 C23 121.1(5) . . ?
C15 C16 C23 121.4(4) . . ?
C16 C17 C12 121.5(4) . . ?
C19 C18 C20 107.0(4) . . ?
C19 C18 C2 111.2(3) . . ?
C20 C18 C2 111.8(4) . . ?
C19 C18 C21 109.4(4) . . ?
C20 C18 C21 108.1(4) . . ?
C2 C18 C21 109.3(4) . . ?
C27 C24 C26 110.2(4) . . ?
C27 C24 C14 110.3(4) . . ?
C26 C24 C14 109.4(4) . . ?
C27 C24 C25 107.8(4) . . ?
C26 C24 C25 107.0(4) . . ?
C14 C24 C25 112.0(4) . . ?
O3 C28 C29 108.0(7) . . ?
O3 C28' C29 101.1(6) . . ?
C28 C29 C30 107.2(6) . . ?
C28 C29 C28' 25.0(5) . . ?
C30 C29 C28' 99.4(5) . . ?
C31 C30 C29 104.5(5) . . ?
O3 C31 C30 106.8(4) . . ?
C37 C32 C33 121.6(9) . . ?
C37 C32 C38 118.2(13) . . ?
C33 C32 C38 120.1(11) . . ?
C32 C33 C34 114.5(8) . . ?
C35 C34 C33 128.9(12) . . ?
C34 C35 C36 112.6(11) . . ?
C37 C36 C35 122.0(10) . . ?
C36 C37 C32 120.3(11) . . ?

_diffrn_measured_fraction_theta_max    0.710
_diffrn_reflns_theta_full              25.34
_diffrn_measured_fraction_theta_full   0.710
_refine_diff_density_max    0.564
_refine_diff_density_min   -0.487
_refine_diff_density_rms    0.128