#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:02:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024379.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_7024379
loop_
_publ_author_name
'Yu, Sze-Man'
'Tritschler, Ulrich'
'Göttker-Schnetmann, Inigo'
'Mecking, Stefan'
_publ_section_title
;
 Zirconium enolatoimine complexes in olefin polymerization.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4612
_journal_page_last               4618
_journal_paper_doi               10.1039/b916289e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C22 H14 Cl2 F10 N2 O2 Zr'
_chemical_formula_sum            'C22 H14 Cl2 F10 N2 O2 Zr'
_chemical_formula_weight         690.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 95.468(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3139(13)
_cell_length_b                   13.3171(14)
_cell_length_c                   19.161(2)
_cell_measurement_reflns_used    30247
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      1.46
_cell_volume                     2619.8(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP32 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17115
_diffrn_reflns_theta_full        26.84
_diffrn_reflns_theta_max         26.84
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_correction_T_min  0.6981
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0328P)²+2.3521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                2428
_reflns_number_total             2789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b916289e.txt
_cod_data_source_block           g:\x_ray\sy\sy194\sy194
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7024379
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
Zr1 Zr 0.0000 0.00659(2) 0.2500 0.01129(9) Uani 1 2 d S
Cl1 Cl 0.10700(5) 0.12761(4) 0.32843(3) 0.01932(13) Uani 1 1 d .
F4 F -0.06328(13) -0.27945(10) 0.31111(6) 0.0225(3) Uani 1 1 d .
O1 O 0.15017(13) -0.01645(11) 0.19125(7) 0.0160(3) Uani 1 1 d .
F5 F 0.18008(14) -0.03872(10) 0.44438(7) 0.0273(3) Uani 1 1 d .
C6 C 0.0556(2) -0.15467(16) 0.37490(11) 0.0160(4) Uani 1 1 d .
F3 F 0.44420(14) -0.10472(12) 0.13529(8) 0.0351(4) Uani 1 1 d .
F2 F 0.27484(15) -0.05263(17) 0.07394(8) 0.0485(5) Uani 1 1 d .
C5 C 0.2877(2) -0.24125(18) 0.35122(13) 0.0261(5) Uani 1 1 d .
H5A H 0.2283 -0.2983 0.3537 0.031 Uiso 1 1 calc R
H5B H 0.3071 -0.2125 0.3981 0.031 Uiso 1 1 calc R
H5C H 0.3687 -0.2641 0.3335 0.031 Uiso 1 1 calc R
N1 N 0.11389(16) -0.12167(13) 0.31319(9) 0.0146(3) Uani 1 1 d .
F1 F 0.38751(18) 0.04790(12) 0.14174(10) 0.0511(5) Uani 1 1 d .
C10 C 0.0313(2) -0.13875(18) 0.49950(11) 0.0240(5) Uani 1 1 d .
H10A H 0.0542 -0.1061 0.5430 0.029 Uiso 1 1 calc R
C4 C 0.2249(2) -0.16287(15) 0.30277(11) 0.0159(4) Uani 1 1 d .
C3 C 0.2965(2) -0.13637(16) 0.24420(11) 0.0182(4) Uani 1 1 d .
H3A H 0.3771 -0.1695 0.2404 0.022 Uiso 1 1 calc R
C2 C 0.25803(19) -0.06881(15) 0.19484(10) 0.0148(4) Uani 1 1 d .
C11 C 0.0872(2) -0.11037(17) 0.44008(11) 0.0204(4) Uani 1 1 d .
C1 C 0.3415(2) -0.04479(17) 0.13593(12) 0.0203(4) Uani 1 1 d .
C7 C -0.0340(2) -0.23252(16) 0.37287(11) 0.0179(4) Uani 1 1 d .
C9 C -0.0593(2) -0.21616(19) 0.49423(12) 0.0256(5) Uani 1 1 d .
H9A H -0.0994 -0.2364 0.5346 0.031 Uiso 1 1 calc R
C8 C -0.0919(2) -0.26418(18) 0.43110(12) 0.0236(5) Uani 1 1 d .
H8A H -0.1529 -0.3178 0.4278 0.028 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 162.55(8) . 2
O1 Zr1 N1 88.55(6) . 2
O1 Zr1 N1 78.71(6) 2 2
O1 Zr1 N1 78.71(6) . .
O1 Zr1 N1 88.55(6) 2 .
N1 Zr1 N1 86.42(8) 2 .
O1 Zr1 Cl1 94.83(4) . 2
O1 Zr1 Cl1 96.86(4) 2 2
N1 Zr1 Cl1 89.31(4) 2 2
N1 Zr1 Cl1 172.34(4) . 2
O1 Zr1 Cl1 96.86(4) . .
O1 Zr1 Cl1 94.83(4) 2 .
N1 Zr1 Cl1 172.34(4) 2 .
N1 Zr1 Cl1 89.31(4) . .
Cl1 Zr1 Cl1 95.61(3) 2 .
C2 O1 Zr1 138.02(13) . .
C7 C6 C11 116.14(19) . .
C7 C6 N1 122.17(18) . .
C11 C6 N1 121.68(19) . .
C4 N1 C6 115.96(17) . .
C4 N1 Zr1 129.25(14) . .
C6 N1 Zr1 114.66(13) . .
C11 C10 C9 118.4(2) . .
N1 C4 C3 122.56(19) . .
N1 C4 C5 122.13(19) . .
C3 C4 C5 115.31(18) . .
C2 C3 C4 125.06(19) . .
O1 C2 C3 126.05(19) . .
O1 C2 C1 112.84(18) . .
C3 C2 C1 121.11(19) . .
F5 C11 C10 119.6(2) . .
F5 C11 C6 117.34(19) . .
C10 C11 C6 123.0(2) . .
F2 C1 F1 107.6(2) . .
F2 C1 F3 106.99(19) . .
F1 C1 F3 106.36(18) . .
F2 C1 C2 111.67(18) . .
F1 C1 C2 110.99(18) . .
F3 C1 C2 112.96(18) . .
F4 C7 C8 119.4(2) . .
F4 C7 C6 117.66(18) . .
C8 C7 C6 123.0(2) . .
C8 C9 C10 120.9(2) . .
C7 C8 C9 118.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1 2.0230(14) .
Zr1 O1 2.0230(14) 2
Zr1 N1 2.3435(17) 2
Zr1 N1 2.3435(17) .
Zr1 Cl1 2.3994(6) 2
Zr1 Cl1 2.3995(6) .
F4 C7 1.347(2) .
O1 C2 1.309(2) .
F5 C11 1.349(3) .
C6 C7 1.387(3) .
C6 C11 1.391(3) .
C6 N1 1.445(3) .
F3 C1 1.327(2) .
F2 C1 1.319(3) .
C5 C4 1.502(3) .
N1 C4 1.302(3) .
F1 C1 1.323(3) .
C10 C11 1.377(3) .
C10 C9 1.389(3) .
C4 C3 1.445(3) .
C3 C2 1.338(3) .
C2 C1 1.518(3) .
C7 C8 1.381(3) .
C9 C8 1.381(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O1 Zr1 O1 C2 -50.58(19) 2
N1 Zr1 O1 C2 -93.38(19) 2
N1 Zr1 O1 C2 -6.74(19) .
Cl1 Zr1 O1 C2 177.43(19) 2
Cl1 Zr1 O1 C2 81.18(19) .
C7 C6 N1 C4 -93.1(2) .
C11 C6 N1 C4 86.4(2) .
C7 C6 N1 Zr1 90.6(2) .
C11 C6 N1 Zr1 -89.9(2) .
O1 Zr1 N1 C4 5.07(17) .
O1 Zr1 N1 C4 173.07(18) 2
N1 Zr1 N1 C4 94.30(18) 2
Cl1 Zr1 N1 C4 38.0(4) 2
Cl1 Zr1 N1 C4 -92.07(17) .
O1 Zr1 N1 C6 -179.23(14) .
O1 Zr1 N1 C6 -11.23(14) 2
N1 Zr1 N1 C6 -90.00(14) 2
Cl1 Zr1 N1 C6 -146.3(3) 2
Cl1 Zr1 N1 C6 83.63(13) .
C6 N1 C4 C3 -178.77(18) .
Zr1 N1 C4 C3 -3.1(3) .
C6 N1 C4 C5 1.0(3) .
Zr1 N1 C4 C5 176.65(15) .
N1 C4 C3 C2 -0.5(3) .
C5 C4 C3 C2 179.8(2) .
Zr1 O1 C2 C3 6.1(3) .
Zr1 O1 C2 C1 -173.20(14) .
C4 C3 C2 O1 -0.4(3) .
C4 C3 C2 C1 178.9(2) .
C9 C10 C11 F5 -176.8(2) .
C9 C10 C11 C6 1.0(3) .
C7 C6 C11 F5 176.01(18) .
N1 C6 C11 F5 -3.5(3) .
C7 C6 C11 C10 -1.9(3) .
N1 C6 C11 C10 178.6(2) .
O1 C2 C1 F2 -52.9(3) .
C3 C2 C1 F2 127.7(2) .
O1 C2 C1 F1 67.1(2) .
C3 C2 C1 F1 -112.3(2) .
O1 C2 C1 F3 -173.59(18) .
C3 C2 C1 F3 7.1(3) .
C11 C6 C7 F4 -177.65(18) .
N1 C6 C7 F4 1.9(3) .
C11 C6 C7 C8 1.3(3) .
N1 C6 C7 C8 -179.2(2) .
C11 C10 C9 C8 0.5(3) .
F4 C7 C8 C9 179.04(19) .
C6 C7 C8 C9 0.1(3) .
C10 C9 C8 C7 -1.0(3) .
