#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:07:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178636 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/47/4074761.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4074761
loop_
_publ_author_name
'Chan, Michael C. W.'
'Tam, Ka-Ho'
'Zhu, Nianyong'
'Chiu, Pauline'
'Matsui, Shigekazu'
_publ_section_title
;
 Synthesis, Structures, and Olefin Polymerization Characteristics of Group
 4 Catalysts [Zr{(OAr)2py}Cl2(D)] (D = O-Donors, Cl[HPR3]) Supported by
 Tridentate Pyridine-2,6-bis(aryloxide) Ligands
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              785
_journal_paper_doi               10.1021/om050864z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C54 H62 N2 O4 Zr'
_chemical_formula_sum            'C54 H62 N2 O4 Zr'
_chemical_formula_weight         894.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.376(3)
_cell_length_b                   18.376(3)
_cell_length_c                   29.187(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     9856(3)
_computing_cell_refinement       Scalepack
_computing_data_collection       MarControl
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Marresearch imaging plate mar300'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31226
_diffrn_reflns_theta_full        25.62
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0614P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                1438
_reflns_number_total             2305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050864zsi20051006_095758.cif
_cod_data_source_block           Zr(L1)2_mar610
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4074761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z'
'y+1/4, x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, -y+1/2, z+1'
'-x+1, y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'-x, y, z-1/2'
'x-1/2, y, -z-1/2'
'x-1/2, -y, z'
'-y-1/4, -x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x, y+1/2, -z'
'x, -y+1/2, z+1/2'
'-y+1/4, -x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'y+1/4, x+1/4, z+1/4'
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
Zr1 Zr 0.5000 0.2500 0.1250 0.04349(15) Uani 1 4 d S
O1 O 0.46520(7) 0.35074(7) 0.11014(4) 0.0539(3) Uani 1 1 d .
N1 N 0.5000 0.2500 0.04421(8) 0.0467(5) Uani 1 2 d S
C1 C 0.50399(9) 0.40083(11) 0.08651(7) 0.0528(5) Uani 1 1 d .
C2 C 0.51418(11) 0.47112(11) 0.10485(9) 0.0652(6) Uani 1 1 d .
C3 C 0.55999(12) 0.51710(12) 0.08029(9) 0.0791(7) Uani 1 1 d .
H3 H 0.5685 0.5634 0.0920 0.095 Uiso 1 1 calc R
C4 C 0.59376(12) 0.49831(13) 0.03952(9) 0.0794(7) Uani 1 1 d .
C5 C 0.57947(11) 0.43079(12) 0.02163(8) 0.0710(6) Uani 1 1 d .
H5 H 0.6007 0.4176 -0.0061 0.085 Uiso 1 1 calc R
C6 C 0.53356(10) 0.38106(11) 0.04408(7) 0.0552(5) Uani 1 1 d .
C7 C 0.51499(9) 0.31245(11) 0.02062(7) 0.0520(5) Uani 1 1 d .
C8 C 0.51256(10) 0.31263(13) -0.02716(7) 0.0658(6) Uani 1 1 d .
H8 H 0.5196 0.3559 -0.0431 0.079 Uiso 1 1 calc R
C9 C 0.5000 0.2500 -0.05064(12) 0.0684(10) Uani 1 2 d S
H9 H 0.5000 0.2500 -0.0825 0.082 Uiso 1 2 calc SR
C10 C 0.47739(17) 0.49415(12) 0.14903(9) 0.0889(7) Uani 1 1 d .
C11 C 0.39422(18) 0.48360(15) 0.14556(11) 0.1237(11) Uani 1 1 d .
H11A H 0.3756 0.5124 0.1208 0.186 Uiso 1 1 calc R
H11B H 0.3718 0.4986 0.1737 0.186 Uiso 1 1 calc R
H11C H 0.3836 0.4332 0.1400 0.186 Uiso 1 1 calc R
C12 C 0.50785(18) 0.44943(14) 0.18941(10) 0.1284(13) Uani 1 1 d .
H12A H 0.5596 0.4563 0.1913 0.193 Uiso 1 1 calc R
H12B H 0.4974 0.3988 0.1846 0.193 Uiso 1 1 calc R
H12C H 0.4855 0.4653 0.2174 0.193 Uiso 1 1 calc R
C13 C 0.49085(18) 0.57544(15) 0.16064(11) 0.1387(14) Uani 1 1 d .
H13A H 0.5422 0.5840 0.1635 0.208 Uiso 1 1 calc R
H13B H 0.4672 0.5872 0.1890 0.208 Uiso 1 1 calc R
H13C H 0.4715 0.6054 0.1366 0.208 Uiso 1 1 calc R
C14 C 0.64467(14) 0.55073(13) 0.01497(11) 0.1188(10) Uani 1 1 d .
H14A H 0.6631 0.5281 -0.0123 0.178 Uiso 1 1 calc R
H14B H 0.6845 0.5630 0.0348 0.178 Uiso 1 1 calc R
H14C H 0.6185 0.5941 0.0069 0.178 Uiso 1 1 calc R
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'
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'
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
O1 Zr1 O1 155.03(7) 22_656 31_565
O1 Zr1 O1 92.679(14) 22_656 .
O1 Zr1 O1 92.679(15) 31_565 .
O1 Zr1 O1 92.679(15) 22_656 11_554
O1 Zr1 O1 92.679(15) 31_565 11_554
O1 Zr1 O1 155.03(7) . 11_554
O1 Zr1 N1 77.51(3) 22_656 22_656
O1 Zr1 N1 77.51(3) 31_565 22_656
O1 Zr1 N1 102.49(3) . 22_656
O1 Zr1 N1 102.49(3) 11_554 22_656
O1 Zr1 N1 102.49(3) 22_656 .
O1 Zr1 N1 102.49(3) 31_565 .
O1 Zr1 N1 77.51(3) . .
O1 Zr1 N1 77.51(3) 11_554 .
N1 Zr1 N1 180.0 22_656 .
C1 O1 Zr1 124.75(11) . .
C7 N1 C7 119.5(2) . 11_554
C7 N1 Zr1 120.26(12) . .
C7 N1 Zr1 120.26(12) 11_554 .
O1 C1 C6 118.61(17) . .
O1 C1 C2 119.96(18) . .
C6 C1 C2 121.44(19) . .
C3 C2 C1 116.2(2) . .
C3 C2 C10 122.6(2) . .
C1 C2 C10 121.3(2) . .
C4 C3 C2 124.2(2) . .
C5 C4 C3 117.8(2) . .
C5 C4 C14 120.7(2) . .
C3 C4 C14 121.5(2) . .
C4 C5 C6 121.7(2) . .
C1 C6 C5 118.5(2) . .
C1 C6 C7 122.85(17) . .
C5 C6 C7 118.56(19) . .
N1 C7 C8 119.9(2) . .
N1 C7 C6 122.06(18) . .
C8 C7 C6 118.00(19) . .
C9 C8 C7 120.5(2) . .
C8 C9 C8 119.4(3) 11_554 .
C2 C10 C12 109.8(2) . .
C2 C10 C11 110.5(2) . .
C12 C10 C11 110.0(2) . .
C2 C10 C13 112.5(2) . .
C12 C10 C13 106.8(2) . .
C11 C10 C13 107.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1 2.0060(13) 22_656
Zr1 O1 2.0060(13) 31_565
Zr1 O1 2.0060(13) .
Zr1 O1 2.0060(12) 11_554
Zr1 N1 2.358(2) 22_656
Zr1 N1 2.358(2) .
O1 C1 1.353(2) .
N1 C7 1.366(2) .
N1 C7 1.366(2) 11_554
C1 C6 1.400(3) .
C1 C2 1.411(3) .
C2 C3 1.391(3) .
C2 C10 1.516(4) .
C3 C4 1.386(3) .
C4 C5 1.372(3) .
C4 C14 1.522(3) .
C5 C6 1.406(3) .
C6 C7 1.475(3) .
C7 C8 1.395(3) .
C8 C9 1.359(3) .
C9 C8 1.359(3) 11_554
C10 C12 1.542(4) .
C10 C11 1.544(4) .
C10 C13 1.552(4) .
