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

data_v 
_database_code_CSD                  179863

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Voskoboynikov, Alexander Z.'
'Borisenko, Anatoly A.'
'Canich, Jo Ann M.'
'Howard, Judith A. K.'
'Izmer, Vyacheslav V.'
'Kuzmina, Lyudmila G.'
'Ryabov, Alexey N.'

_publ_contact_author_name     	'Prof Alexander Z Voskoboynikov'  
_publ_contact_author_address 
;
Department of Chemistry
Moscow State University
Leninskie Gory, GSP-3
Moscow
119899
RUSSIAN FEDERATION
;

_publ_contact_author_email       'VOSKOBOY@ORG.CHEM.MSU.SU'

_publ_section_title		
;
Zirconium Complexes of Cyclopenta[b]pyridine: Synthesis, Structure,
and Olefin Polymerization Catalysis
;

_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C18 H21 Cl2 N Zr' 
_chemical_formula_weight          413.48 
_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' 
'Cl'  'Cl'   0.1484   0.1585 
'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            '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                    13.546(2) 
_cell_length_b                    8.7659(11) 
_cell_length_c                    14.989(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  97.552(7) 
_cell_angle_gamma                 90.00 
_cell_volume                      1764.4(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     120.0(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.557 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              840 
_exptl_absorpt_coefficient_mu     0.922 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       120(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        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11395 
_diffrn_reflns_av_R_equivalents   0.3251 
_diffrn_reflns_av_sigmaI/netI     0.2329 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.52 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              3479 
_reflns_number_observed           1816 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 531 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^)+(0.1122P)^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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0056(18) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          2948 
_refine_ls_number_parameters      206 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1745 
_refine_ls_R_factor_obs           0.0933 
_refine_ls_wR_factor_all          0.2837 
_refine_ls_wR_factor_obs          0.2161 
_refine_ls_goodness_of_fit_all    1.001 
_refine_ls_goodness_of_fit_obs    1.128 
_refine_ls_restrained_S_all       1.059 
_refine_ls_restrained_S_obs       1.128 
_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 
Zr1 Zr 0.75576(8) 0.21736(10) 0.92744(8) 0.0248(4) Uani 1 d . . 
Cl2 Cl 0.8062(2) 0.0899(3) 0.7959(2) 0.0344(8) Uani 1 d . . 
Cl1 Cl 0.6681(2) 0.4330(3) 0.8497(2) 0.0318(8) Uani 1 d . . 
C11 C 0.8481(8) 0.4279(10) 1.0142(8) 0.026(3) Uani 1 d . . 
H11A H 0.8079(8) 0.5131(10) 1.0248(8) 0.031 Uiso 1 calc R . 
C12 C 0.8646(8) 0.2986(10) 1.0686(8) 0.025(3) Uani 1 d . . 
H12A H 0.8412(8) 0.2845(10) 1.1250(8) 0.030 Uiso 1 calc R . 
C13 C 0.9211(8) 0.1926(10) 1.0266(9) 0.030(3) Uani 1 d . . 
H13A H 0.9356(8) 0.0906(10) 1.0455(9) 0.036 Uiso 1 calc R . 
C14 C 0.9514(8) 0.2634(10) 0.9534(9) 0.028(3) Uani 1 d . . 
N1 N 1.0168(6) 0.2084(9) 0.8923(7) 0.029(2) Uani 1 d . . 
C16 C 1.0304(8) 0.2941(11) 0.8277(9) 0.032(3) Uani 1 d . . 
H16A H 1.0771(8) 0.2615(11) 0.7897(9) 0.039 Uiso 1 calc R . 
C17 C 0.9803(8) 0.4396(11) 0.8063(9) 0.036(3) Uani 1 d . . 
H17A H 0.9912(8) 0.4947(11) 0.7539(9) 0.043 Uiso 1 calc R . 
C18 C 0.9171(8) 0.4957(11) 0.8633(8) 0.026(4) Uani 0.99(4) d P . 
H18A H 0.8838(8) 0.5904(11) 0.8518(8) 0.031 Uiso 1 calc R . 
C19 C 0.9037(8) 0.4078(10) 0.9388(9) 0.032(3) Uani 1 d . . 
C1 C 0.6310(8) 0.1725(11) 1.0351(8) 0.025(3) Uani 1 d . . 
C2 C 0.7001(8) 0.0456(10) 1.0463(8) 0.026(3) Uani 1 d . . 
C3 C 0.6889(9) -0.0367(10) 0.9651(8) 0.030(3) Uani 1 d . . 
C4 C 0.6119(8) 0.0322(11) 0.9012(8) 0.031(3) Uani 1 d . . 
C5 C 0.5766(8) 0.1607(12) 0.9476(10) 0.041(4) Uani 1 d . . 
C6 C 0.6125(9) 0.2896(12) 1.1039(10) 0.040(3) Uani 1 d . . 
H6A H 0.5420(15) 0.2878(65) 1.1126(41) 0.060 Uiso 1 calc R . 
H6B H 0.6297(60) 0.3910(17) 1.0831(28) 0.060 Uiso 1 calc R . 
H6C H 0.6536(46) 0.2666(56) 1.1611(19) 0.060 Uiso 1 calc R . 
C7 C 0.7596(8) -0.0019(11) 1.1324(7) 0.028(3) Uani 1 d . . 
H7A H 0.7245(24) -0.0832(54) 1.1601(23) 0.043 Uiso 1 calc R . 
H7B H 0.7689(43) 0.0857(22) 1.1733(18) 0.043 Uiso 1 calc R . 
H7C H 0.8248(20) -0.0394(70) 1.1204(9) 0.043 Uiso 1 calc R . 
C8 C 0.7440(10) -0.1830(10) 0.9502(9) 0.036(3) Uani 1 d . . 
H8A H 0.7043(29) -0.2705(11) 0.9652(52) 0.054 Uiso 1 calc R . 
H8B H 0.8082(28) -0.1835(42) 0.9889(40) 0.054 Uiso 1 calc R . 
H8C H 0.7552(53) -0.1896(45) 0.8871(15) 0.054 Uiso 1 calc R . 
C9 C 0.5709(11) -0.0249(14) 0.8102(11) 0.062(5) Uani 1 d . . 
H9A H 0.5167(50) -0.0969(88) 0.8156(13) 0.092 Uiso 1 calc R . 
H9B H 0.6237(21) -0.0764(97) 0.7829(29) 0.092 Uiso 1 calc R . 
H9C H 0.5454(67) 0.0612(20) 0.7723(24) 0.092 Uiso 1 calc R . 
C10 C 0.4882(9) 0.2567(15) 0.9136(13) 0.065(5) Uani 1 d . . 
H10A H 0.4278(13) 0.2100(66) 0.9309(63) 0.098 Uiso 1 calc R . 
H10B H 0.4824(46) 0.2639(99) 0.8479(15) 0.098 Uiso 1 calc R . 
H10C H 0.4966(38) 0.3591(40) 0.9398(57) 0.098 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 
Zr1 0.0199(6) 0.0085(5) 0.0479(9) -0.0008(5) 0.0112(5) -0.0020(4) 
Cl2 0.030(2) 0.0270(13) 0.049(2) -0.0088(12) 0.0165(14) -0.0046(11) 
Cl1 0.0249(15) 0.0159(12) 0.055(2) 0.0100(12) 0.0075(14) 0.0009(10) 
C11 0.027(6) 0.017(5) 0.035(8) -0.010(5) 0.009(5) -0.005(4) 
C12 0.024(6) 0.011(5) 0.039(8) -0.002(4) 0.005(5) -0.002(4) 
C13 0.019(6) 0.009(5) 0.064(9) 0.002(5) 0.015(6) -0.005(4) 
C14 0.020(6) 0.009(4) 0.056(9) -0.004(5) 0.006(5) 0.002(4) 
N1 0.018(5) 0.018(4) 0.054(7) 0.008(4) 0.016(4) -0.002(4) 
C16 0.018(6) 0.022(5) 0.056(9) -0.006(5) 0.000(5) -0.004(5) 
C17 0.026(6) 0.015(5) 0.070(10) 0.008(5) 0.019(6) -0.008(4) 
C18 0.013(6) 0.019(6) 0.044(9) 0.001(5) -0.005(5) -0.007(4) 
C19 0.016(6) 0.006(4) 0.073(10) -0.004(5) 0.004(6) 0.000(4) 
C1 0.014(5) 0.021(5) 0.041(8) 0.005(5) 0.006(5) 0.003(4) 
C2 0.022(6) 0.006(4) 0.051(8) 0.002(5) 0.011(5) -0.001(4) 
C3 0.033(7) 0.012(5) 0.046(8) -0.008(5) 0.011(6) -0.009(4) 
C4 0.029(6) 0.021(5) 0.046(8) -0.004(5) 0.018(6) -0.015(5) 
C5 0.020(6) 0.017(5) 0.092(12) 0.014(6) 0.028(7) -0.003(5) 
C6 0.032(7) 0.023(5) 0.068(10) 0.007(6) 0.019(6) 0.007(5) 
C7 0.022(6) 0.028(5) 0.036(8) 0.008(5) 0.004(5) 0.003(5) 
C8 0.054(8) 0.010(5) 0.048(9) -0.005(4) 0.023(7) 0.002(5) 
C9 0.047(9) 0.032(7) 0.105(14) 0.002(8) 0.010(9) -0.031(6) 
C10 0.009(6) 0.052(8) 0.135(16) 0.029(9) 0.008(8) 0.004(5) 

_geom_special_details 
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
; 

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
Zr1 Cl2 2.440(3) . ? 
Zr1 Cl1 2.444(3) . ? 
Zr1 C3 2.497(9) . ? 
Zr1 C11 2.497(10) . ? 
Zr1 C12 2.517(12) . ? 
Zr1 C1 2.517(11) . ? 
Zr1 C2 2.522(10) . ? 
Zr1 C13 2.529(12) . ? 
Zr1 C4 2.527(10) . ? 
Zr1 C5 2.533(11) . ? 
Zr1 C19 2.597(10) . ? 
Zr1 C14 2.659(11) . ? 
C11 C12 1.396(15) . ? 
C11 C19 1.45(2) . ? 
C12 C13 1.404(14) . ? 
C13 C14 1.37(2) . ? 
C14 C19 1.425(13) . ? 
C14 N1 1.438(14) . ? 
N1 C16 1.257(15) . ? 
C16 C17 1.460(14) . ? 
C17 C18 1.38(2) . ? 
C18 C19 1.40(2) . ? 
C1 C5 1.42(2) . ? 
C1 C2 1.450(13) . ? 
C1 C6 1.50(2) . ? 
C2 C3 1.41(2) . ? 
C2 C7 1.49(2) . ? 
C3 C4 1.45(2) . ? 
C3 C8 1.514(13) . ? 
C4 C5 1.44(2) . ? 
C4 C9 1.49(2) . ? 
C5 C10 1.50(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 
Cl2 Zr1 Cl1 98.00(11) . . ? 
Cl2 Zr1 C3 85.5(3) . . ? 
Cl1 Zr1 C3 129.0(3) . . ? 
Cl2 Zr1 C11 125.8(3) . . ? 
Cl1 Zr1 C11 81.7(3) . . ? 
C3 Zr1 C11 135.5(4) . . ? 
Cl2 Zr1 C12 127.8(3) . . ? 
Cl1 Zr1 C12 112.1(2) . . ? 
C3 Zr1 C12 104.6(4) . . ? 
C11 Zr1 C12 32.3(3) . . ? 
Cl2 Zr1 C1 136.8(3) . . ? 
Cl1 Zr1 C1 95.8(2) . . ? 
C3 Zr1 C1 54.7(3) . . ? 
C11 Zr1 C1 96.6(4) . . ? 
C12 Zr1 C1 82.8(4) . . ? 
Cl2 Zr1 C2 116.0(2) . . ? 
Cl1 Zr1 C2 128.8(2) . . ? 
C3 Zr1 C2 32.5(4) . . ? 
C11 Zr1 C2 104.4(4) . . ? 
C12 Zr1 C2 76.8(4) . . ? 
C1 Zr1 C2 33.4(3) . . ? 
Cl2 Zr1 C13 96.6(3) . . ? 
Cl1 Zr1 C13 133.1(2) . . ? 
C3 Zr1 C13 96.3(4) . . ? 
C11 Zr1 C13 54.1(3) . . ? 
C12 Zr1 C13 32.3(3) . . ? 
C1 Zr1 C13 103.1(4) . . ? 
C2 Zr1 C13 81.8(4) . . ? 
Cl2 Zr1 C4 82.7(3) . . ? 
Cl1 Zr1 C4 96.1(3) . . ? 
C3 Zr1 C4 33.6(4) . . ? 
C11 Zr1 C4 151.5(4) . . ? 
C12 Zr1 C4 131.8(4) . . ? 
C1 Zr1 C4 55.2(4) . . ? 
C2 Zr1 C4 55.3(4) . . ? 
C13 Zr1 C4 129.9(3) . . ? 
Cl2 Zr1 C5 112.4(3) . . ? 
Cl1 Zr1 C5 78.2(3) . . ? 
C3 Zr1 C5 54.3(4) . . ? 
C11 Zr1 C5 120.3(4) . . ? 
C12 Zr1 C5 114.8(4) . . ? 
C1 Zr1 C5 32.7(4) . . ? 
C2 Zr1 C5 54.5(4) . . ? 
C13 Zr1 C5 134.5(4) . . ? 
C4 Zr1 C5 33.0(4) . . ? 
Cl2 Zr1 C19 93.0(3) . . ? 
Cl1 Zr1 C19 81.8(2) . . ? 
C3 Zr1 C19 149.1(4) . . ? 
C11 Zr1 C19 33.0(4) . . ? 
C12 Zr1 C19 53.2(4) . . ? 
C1 Zr1 C19 129.5(4) . . ? 
C2 Zr1 C19 129.6(4) . . ? 
C13 Zr1 C19 53.2(3) . . ? 
C4 Zr1 C19 174.9(4) . . ? 
C5 Zr1 C19 149.4(3) . . ? 
Cl2 Zr1 C14 78.9(3) . . ? 
Cl1 Zr1 C14 111.4(2) . . ? 
C3 Zr1 C14 119.1(3) . . ? 
C11 Zr1 C14 52.4(3) . . ? 
C12 Zr1 C14 51.1(4) . . ? 
C1 Zr1 C14 132.1(4) . . ? 
C2 Zr1 C14 111.8(4) . . ? 
C13 Zr1 C14 30.5(4) . . ? 
C4 Zr1 C14 148.6(3) . . ? 
C5 Zr1 C14 164.7(5) . . ? 
C19 Zr1 C14 31.4(3) . . ? 
C12 C11 C19 107.3(9) . . ? 
C12 C11 Zr1 74.6(6) . . ? 
C19 C11 Zr1 77.3(6) . . ? 
C11 C12 C13 109.3(10) . . ? 
C11 C12 Zr1 73.1(6) . . ? 
C13 C12 Zr1 74.3(7) . . ? 
C14 C13 C12 107.3(8) . . ? 
C14 C13 Zr1 80.0(7) . . ? 
C12 C13 Zr1 73.3(7) . . ? 
C13 C14 C19 110.3(10) . . ? 
C13 C14 N1 129.3(9) . . ? 
C19 C14 N1 120.3(11) . . ? 
C13 C14 Zr1 69.5(6) . . ? 
C19 C14 Zr1 71.9(6) . . ? 
N1 C14 Zr1 122.8(8) . . ? 
C16 N1 C14 117.0(9) . . ? 
N1 C16 C17 125.5(11) . . ? 
C18 C17 C16 118.9(11) . . ? 
C17 C18 C19 117.5(10) . . ? 
C18 C19 C14 120.5(11) . . ? 
C18 C19 C11 134.4(9) . . ? 
C14 C19 C11 105.1(10) . . ? 
C18 C19 Zr1 118.7(8) . . ? 
C14 C19 Zr1 76.7(6) . . ? 
C11 C19 Zr1 69.7(6) . . ? 
C5 C1 C2 107.4(10) . . ? 
C5 C1 C6 124.9(10) . . ? 
C2 C1 C6 127.6(11) . . ? 
C5 C1 Zr1 74.3(6) . . ? 
C2 C1 Zr1 73.5(6) . . ? 
C6 C1 Zr1 121.4(7) . . ? 
C3 C2 C1 107.4(10) . . ? 
C3 C2 C7 126.3(9) . . ? 
C1 C2 C7 125.7(10) . . ? 
C3 C2 Zr1 72.7(6) . . ? 
C1 C2 Zr1 73.1(6) . . ? 
C7 C2 Zr1 127.0(7) . . ? 
C2 C3 C4 110.1(9) . . ? 
C2 C3 C8 124.2(11) . . ? 
C4 C3 C8 125.5(10) . . ? 
C2 C3 Zr1 74.7(5) . . ? 
C4 C3 Zr1 74.4(5) . . ? 
C8 C3 Zr1 121.4(7) . . ? 
C5 C4 C3 105.3(11) . . ? 
C5 C4 C9 126.8(12) . . ? 
C3 C4 C9 127.8(10) . . ? 
C5 C4 Zr1 73.7(6) . . ? 
C3 C4 Zr1 72.0(6) . . ? 
C9 C4 Zr1 123.0(8) . . ? 
C1 C5 C4 109.8(10) . . ? 
C1 C5 C10 124.6(12) . . ? 
C4 C5 C10 125.2(14) . . ? 
C1 C5 Zr1 73.0(6) . . ? 
C4 C5 Zr1 73.3(6) . . ? 
C10 C5 Zr1 125.8(7) . . ? 

_refine_diff_density_max    1.276 
_refine_diff_density_min   -1.478 
_refine_diff_density_rms    0.212