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#$Date: 2016-03-21 18:45:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178822 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/76/4107662.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_4107662
loop_
_publ_author_name
'Wei Gao'
'Dongmei Cui'
_publ_section_title
;
 Highlycis-1,4 Selective Polymerization of Dienes with Homogeneous
 Ziegler-Natta Catalysts Based on NCN-Pincer Rare Earth Metal Dichloride
 Precursors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4984
_journal_page_last               4991
_journal_paper_doi               10.1021/ja711146t
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C36 H47 Cl2 N2 O2 Y'
_chemical_formula_weight         699.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 100.859(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3444(12)
_cell_length_b                   14.4914(16)
_cell_length_c                   21.450(2)
_cell_measurement_temperature    187(2)
_cell_volume                     3463.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      187(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Phi and omega scan'
_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  0.1137
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9558
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.872
_exptl_absorpt_correction_T_max  0.9122
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0420
_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)+(0.0485P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2667
_reflns_number_total             3404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711146t-file003_02.cif
_cod_data_source_block           complex_2
_cod_database_code               4107662
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'
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
C18A C 0.2388(8) -0.1977(6) 0.3394(4) 0.053(2) Uani 0.79(2) 1 d P A 1
H18A H 0.2543 -0.2629 0.3296 0.063 Uiso 0.79(2) 1 calc PR A 1
H18B H 0.3165 -0.1657 0.3527 0.063 Uiso 0.79(2) 1 calc PR A 1
C18B C 0.188(3) -0.2274(16) 0.3207(12) 0.040(6) Uani 0.21(2) 1 d P A 2
H18C H 0.2724 -0.2478 0.3231 0.048 Uiso 0.21(2) 1 calc PR A 2
H18D H 0.1338 -0.2790 0.3047 0.048 Uiso 0.21(2) 1 calc PR A 2
Y1 Y 0.0000 0.05297(3) 0.2500 0.02609(14) Uani 1 2 d S . .
Cl1 Cl -0.17253(7) 0.04272(5) 0.31463(3) 0.03143(19) Uani 1 1 d . . .
O1 O 0.09447(18) -0.08150(13) 0.30895(8) 0.0312(5) Uani 1 1 d . A .
N1 N 0.1321(2) 0.13054(16) 0.35282(10) 0.0277(5) Uani 1 1 d . . .
C1 C 0.0000 0.2194(3) 0.2500 0.0270(9) Uani 1 2 d S . .
C2 C 0.0697(3) 0.27152(19) 0.29848(12) 0.0274(6) Uani 1 1 d . . .
C3 C 0.0712(3) 0.3682(2) 0.29859(13) 0.0352(7) Uani 1 1 d . . .
H3 H 0.1212 0.4006 0.3320 0.042 Uiso 1 1 calc R . .
C4 C 0.0000 0.4163(3) 0.2500 0.0396(11) Uani 1 2 d S . .
H4 H 0.0000 0.4818 0.2500 0.047 Uiso 1 2 calc SR . .
C5 C 0.1371(3) 0.2192(2) 0.35121(13) 0.0297(7) Uani 1 1 d . . .
H5 H 0.1859 0.2511 0.3853 0.036 Uiso 1 1 calc R . .
C6 C 0.1886(3) 0.0891(2) 0.41185(12) 0.0289(7) Uani 1 1 d . . .
C11 C 0.2948(3) 0.0393(2) 0.41439(14) 0.0329(7) Uani 1 1 d . . .
C10 C 0.3432(3) -0.0044(2) 0.47099(15) 0.0430(8) Uani 1 1 d . . .
H10 H 0.4151 -0.0390 0.4738 0.052 Uiso 1 1 calc R . .
C9 C 0.2894(3) 0.0013(2) 0.52308(15) 0.0485(9) Uani 1 1 d . . .
H9 H 0.3241 -0.0296 0.5612 0.058 Uiso 1 1 calc R . .
C8 C 0.1859(3) 0.0513(2) 0.52033(14) 0.0423(8) Uani 1 1 d . . .
H8 H 0.1499 0.0552 0.5568 0.051 Uiso 1 1 calc R . .
C7 C 0.1328(3) 0.0967(2) 0.46453(12) 0.0325(7) Uani 1 1 d . . .
C14 C 0.0173(3) 0.1494(2) 0.46323(14) 0.0397(8) Uani 1 1 d . . .
H14A H -0.0349 0.1136 0.4865 0.048 Uiso 1 1 calc R . .
H14B H -0.0251 0.1555 0.4187 0.048 Uiso 1 1 calc R . .
C15 C 0.0370(3) 0.2454(3) 0.49263(17) 0.0564(10) Uani 1 1 d . . .
H15A H 0.0844 0.2404 0.5357 0.085 Uiso 1 1 calc R . .
H15B H -0.0408 0.2737 0.4944 0.085 Uiso 1 1 calc R . .
H15C H 0.0801 0.2838 0.4667 0.085 Uiso 1 1 calc R . .
C12 C 0.3577(3) 0.0357(2) 0.35856(15) 0.0422(8) Uani 1 1 d . . .
H12A H 0.2969 0.0287 0.3192 0.051 Uiso 1 1 calc R . .
H12B H 0.4102 -0.0194 0.3627 0.051 Uiso 1 1 calc R . .
C13 C 0.4337(3) 0.1216(3) 0.35259(17) 0.0558(10) Uani 1 1 d . . .
H13A H 0.3816 0.1759 0.3454 0.084 Uiso 1 1 calc R . .
H13B H 0.4751 0.1139 0.3167 0.084 Uiso 1 1 calc R . .
H13C H 0.4931 0.1298 0.3918 0.084 Uiso 1 1 calc R . .
C17 C 0.1659(3) -0.1920(3) 0.38938(16) 0.0508(9) Uani 1 1 d . . .
H17A H 0.2163 -0.1725 0.4301 0.061 Uiso 1 1 calc R A 1
H17B H 0.1300 -0.2528 0.3956 0.061 Uiso 1 1 calc R A 1
C19 C 0.1633(3) -0.1503(2) 0.28230(15) 0.0462(9) Uani 1 1 d . . .
H19A H 0.2151 -0.1209 0.2557 0.055 Uiso 1 1 calc R A 1
H19B H 0.1096 -0.1951 0.2561 0.055 Uiso 1 1 calc R A 1
C16 C 0.0684(3) -0.1212(2) 0.36733(13) 0.0378(8) Uani 1 1 d . A .
H16A H -0.0115 -0.1511 0.3593 0.045 Uiso 1 1 calc R . .
H16B H 0.0693 -0.0728 0.3999 0.045 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
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'
Y Y -2.7962 3.5667 '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
C17 C18A C19 104.7(4) . .
C17 C18A H18A 110.8 . .
C19 C18A H18A 110.8 . .
C17 C18A H18B 110.8 . .
C19 C18A H18B 110.8 . .
H18A C18A H18B 108.9 . .
C19 C18B C17 103.6(12) . .
C19 C18B H18C 111.0 . .
C17 C18B H18C 111.0 . .
C19 C18B H18D 111.0 . .
C17 C18B H18D 111.0 . .
H18C C18B H18D 109.0 . .
C1 Y1 O1 142.49(5) . 2
C1 Y1 O1 142.49(5) . .
O1 Y1 O1 75.01(9) 2 .
C1 Y1 Cl1 93.267(17) . 2
O1 Y1 Cl1 88.83(5) 2 2
O1 Y1 Cl1 85.99(5) . 2
C1 Y1 Cl1 93.267(17) . .
O1 Y1 Cl1 85.99(5) 2 .
O1 Y1 Cl1 88.83(5) . .
Cl1 Y1 Cl1 173.47(3) 2 .
C1 Y1 N1 65.10(5) . .
O1 Y1 N1 151.86(7) 2 .
O1 Y1 N1 77.66(7) . .
Cl1 Y1 N1 95.88(5) 2 .
Cl1 Y1 N1 86.88(5) . .
C1 Y1 N1 65.10(5) . 2
O1 Y1 N1 77.66(7) 2 2
O1 Y1 N1 151.86(7) . 2
Cl1 Y1 N1 86.88(5) 2 2
Cl1 Y1 N1 95.88(5) . 2
N1 Y1 N1 130.20(10) . 2
C19 O1 C16 106.2(2) . .
C19 O1 Y1 123.93(16) . .
C16 O1 Y1 128.03(17) . .
C5 N1 C6 115.2(2) . .
C5 N1 Y1 114.76(18) . .
C6 N1 Y1 129.71(17) . .
C2 C1 C2 114.9(4) . 2
C2 C1 Y1 122.57(18) . .
C2 C1 Y1 122.57(18) 2 .
C3 C2 C1 123.0(3) . .
C3 C2 C5 121.1(3) . .
C1 C2 C5 115.9(3) . .
C4 C3 C2 119.9(3) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C3 119.4(4) 2 .
C3 C4 H4 120.3 2 .
C3 C4 H4 120.3 . .
N1 C5 C2 121.5(3) . .
N1 C5 H5 119.2 . .
C2 C5 H5 119.2 . .
C11 C6 C7 121.8(3) . .
C11 C6 N1 119.2(3) . .
C7 C6 N1 118.9(3) . .
C10 C11 C6 117.8(3) . .
C10 C11 C12 120.8(3) . .
C6 C11 C12 121.4(3) . .
C9 C10 C11 121.5(3) . .
C9 C10 H10 119.3 . .
C11 C10 H10 119.3 . .
C8 C9 C10 120.3(3) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
C9 C8 C7 120.8(3) . .
C9 C8 H8 119.6 . .
C7 C8 H8 119.6 . .
C8 C7 C6 117.8(3) . .
C8 C7 C14 119.0(3) . .
C6 C7 C14 123.1(3) . .
C7 C14 C15 113.2(3) . .
C7 C14 H14A 108.9 . .
C15 C14 H14A 108.9 . .
C7 C14 H14B 108.9 . .
C15 C14 H14B 108.9 . .
H14A C14 H14B 107.8 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C11 C12 C13 113.4(3) . .
C11 C12 H12A 108.9 . .
C13 C12 H12A 108.9 . .
C11 C12 H12B 108.9 . .
C13 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C18A C17 C16 106.7(3) . .
C18A C17 C18B 28.1(9) . .
C16 C17 C18B 99.2(8) . .
C18A C17 H17A 110.4 . .
C16 C17 H17A 110.4 . .
C18B C17 H17A 136.6 . .
C18A C17 H17B 110.4 . .
C16 C17 H17B 110.4 . .
C18B C17 H17B 88.8 . .
H17A C17 H17B 108.6 . .
C18B C19 O1 112.7(9) . .
C18B C19 C18A 30.1(12) . .
O1 C19 C18A 104.9(4) . .
C18B C19 H19A 127.8 . .
O1 C19 H19A 110.8 . .
C18A C19 H19A 110.8 . .
C18B C19 H19B 81.0 . .
O1 C19 H19B 110.8 . .
C18A C19 H19B 110.8 . .
H19A C19 H19B 108.8 . .
O1 C16 C17 106.3(3) . .
O1 C16 H16A 110.5 . .
C17 C16 H16A 110.5 . .
O1 C16 H16B 110.5 . .
C17 C16 H16B 110.5 . .
H16A C16 H16B 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C18A C17 1.474(7) .
C18A C19 1.520(7) .
C18A H18A 0.9900 .
C18A H18B 0.9900 .
C18B C19 1.385(19) .
C18B C17 1.63(2) .
C18B H18C 0.9900 .
C18B H18D 0.9900 .
Y1 C1 2.412(4) .
Y1 O1 2.4564(19) 2
Y1 O1 2.4564(19) .
Y1 Cl1 2.6072(7) 2
Y1 Cl1 2.6072(7) .
Y1 N1 2.670(2) .
Y1 N1 2.670(2) 2
O1 C19 1.449(4) .
O1 C16 1.458(3) .
N1 C5 1.286(4) .
N1 C6 1.438(3) .
C1 C2 1.402(3) .
C1 C2 1.402(3) 2
C2 C3 1.401(4) .
C2 C5 1.454(4) .
C3 C4 1.381(4) .
C3 H3 0.9500 .
C4 C3 1.381(4) 2
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C11 1.397(4) .
C6 C7 1.399(4) .
C11 C10 1.387(4) .
C11 C12 1.506(5) .
C10 C9 1.372(5) .
C10 H10 0.9500 .
C9 C8 1.372(5) .
C9 H9 0.9500 .
C8 C7 1.398(4) .
C8 H8 0.9500 .
C7 C14 1.513(4) .
C14 C15 1.526(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C12 C13 1.533(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C17 C16 1.517(5) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
