#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:02:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024376.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_7024376
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 H18 Cl2 F6 N2 O2 Zr'
_chemical_formula_sum            'C22 H18 Cl2 F6 N2 O2 Zr'
_chemical_formula_weight         618.50
_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                 95.011(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7961(6)
_cell_length_b                   14.0461(8)
_cell_length_c                   18.3236(12)
_cell_measurement_reflns_used    30223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.23
_cell_volume                     2511.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP32 '
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1265
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18366
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.8723
_exptl_absorpt_correction_T_min  0.6480
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cubic fragment'
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+6.2439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                2643
_reflns_number_total             3015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b916289e.txt
_cod_data_source_block           d:\x_ray\gs08_035\gs08_035
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7024376
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 -0.00237(2) 0.2500 0.01270(8) Uani 1 2 d S
Cl1 Cl 0.12943(6) -0.11413(4) 0.32955(3) 0.01766(12) Uani 1 1 d .
O1 O 0.15128(15) 0.01397(11) 0.18198(8) 0.0173(3) Uani 1 1 d .
F2 F 0.45969(15) 0.08759(12) 0.11437(8) 0.0321(4) Uani 1 1 d .
F1 F 0.27311(17) 0.04867(14) 0.05168(8) 0.0385(4) Uani 1 1 d .
C4 C 0.2358(2) 0.16324(16) 0.28924(11) 0.0171(4) Uani 1 1 d .
N1 N 0.12352(19) 0.12195(13) 0.30568(9) 0.0157(4) Uani 1 1 d .
F3 F 0.3811(2) -0.05415(12) 0.12099(11) 0.0449(5) Uani 1 1 d .
C3 C 0.3053(2) 0.13521(17) 0.22574(12) 0.0184(4) Uani 1 1 d .
H3A H 0.3864 0.1685 0.2165 0.022 Uiso 1 1 calc R
C10 C -0.0751(2) 0.26479(18) 0.43234(12) 0.0215(5) Uani 1 1 d .
H10A H -0.1324 0.3194 0.4311 0.026 Uiso 1 1 calc R
C6 C 0.0657(2) 0.15493(16) 0.37173(11) 0.0163(4) Uani 1 1 d .
C9 C -0.0466(3) 0.21510(18) 0.49743(12) 0.0237(5) Uani 1 1 d .
H9A H -0.0853 0.2354 0.5406 0.028 Uiso 1 1 calc R
C11 C -0.0194(2) 0.23440(16) 0.36887(12) 0.0185(4) Uani 1 1 d .
H11A H -0.0394 0.2676 0.3241 0.022 Uiso 1 1 calc R
C5 C 0.3018(2) 0.24252(18) 0.33473(13) 0.0233(5) Uani 1 1 d .
H5C H 0.3971 0.2500 0.3234 0.028 Uiso 1 1 calc R
H5B H 0.2994 0.2273 0.3868 0.028 Uiso 1 1 calc R
H5A H 0.2518 0.3019 0.3236 0.028 Uiso 1 1 calc R
C8 C 0.0383(3) 0.13576(18) 0.49962(12) 0.0229(5) Uani 1 1 d .
H8A H 0.0579 0.1023 0.5444 0.027 Uiso 1 1 calc R
C2 C 0.2622(2) 0.06500(16) 0.17899(11) 0.0164(4) Uani 1 1 d .
C1 C 0.3443(2) 0.03681(17) 0.11616(13) 0.0206(5) Uani 1 1 d .
C7 C 0.0944(2) 0.10522(17) 0.43693(12) 0.0200(5) Uani 1 1 d .
H7A H 0.1522 0.0508 0.4384 0.024 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'
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'
F F 0.0171 0.0103 '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'
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 167.02(9) 2 .
O1 Zr1 N1 91.47(6) 2 .
O1 Zr1 N1 78.67(6) . .
O1 Zr1 N1 78.67(6) 2 2
O1 Zr1 N1 91.47(6) . 2
N1 Zr1 N1 81.81(9) . 2
O1 Zr1 Cl1 94.33(4) 2 .
O1 Zr1 Cl1 94.06(5) . .
N1 Zr1 Cl1 89.87(5) . .
N1 Zr1 Cl1 168.92(4) 2 .
O1 Zr1 Cl1 94.06(5) 2 2
O1 Zr1 Cl1 94.33(4) . 2
N1 Zr1 Cl1 168.92(4) . 2
N1 Zr1 Cl1 89.87(5) 2 2
Cl1 Zr1 Cl1 99.26(3) . 2
C2 O1 Zr1 137.86(14) . .
N1 C4 C3 121.9(2) . .
N1 C4 C5 122.2(2) . .
C3 C4 C5 115.9(2) . .
C4 N1 C6 116.65(19) . .
C4 N1 Zr1 130.92(15) . .
C6 N1 Zr1 112.37(13) . .
C2 C3 C4 124.3(2) . .
C9 C10 C11 119.9(2) . .
C7 C6 C11 120.7(2) . .
C7 C6 N1 119.3(2) . .
C11 C6 N1 119.95(19) . .
C10 C9 C8 120.2(2) . .
C6 C11 C10 119.4(2) . .
C7 C8 C9 120.3(2) . .
O1 C2 C3 126.1(2) . .
O1 C2 C1 112.80(19) . .
C3 C2 C1 121.1(2) . .
F3 C1 F1 107.3(2) . .
F3 C1 F2 106.8(2) . .
F1 C1 F2 106.86(19) . .
F3 C1 C2 111.09(19) . .
F1 C1 C2 111.75(19) . .
F2 C1 C2 112.65(19) . .
C8 C7 C6 119.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1 2.0310(15) 2
Zr1 O1 2.0310(15) .
Zr1 N1 2.3105(19) .
Zr1 N1 2.3105(19) 2
Zr1 Cl1 2.4235(5) .
Zr1 Cl1 2.4235(5) 2
O1 C2 1.307(3) .
F2 C1 1.339(3) .
F1 C1 1.329(3) .
C4 N1 1.302(3) .
C4 C3 1.452(3) .
C4 C5 1.503(3) .
N1 C6 1.456(3) .
F3 C1 1.328(3) .
C3 C2 1.350(3) .
C10 C9 1.389(3) .
C10 C11 1.394(3) .
C6 C7 1.391(3) .
C6 C11 1.391(3) .
C9 C8 1.389(4) .
C8 C7 1.385(3) .
C2 C1 1.514(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 45.8(2) 2
N1 Zr1 O1 C2 4.6(2) .
N1 Zr1 O1 C2 86.0(2) 2
Cl1 Zr1 O1 C2 -84.4(2) .
Cl1 Zr1 O1 C2 176.0(2) 2
C3 C4 N1 C6 178.53(19) .
C5 C4 N1 C6 -1.3(3) .
C3 C4 N1 Zr1 1.5(3) .
C5 C4 N1 Zr1 -178.37(16) .
O1 Zr1 N1 C4 -174.08(19) 2
O1 Zr1 N1 C4 -2.58(19) .
N1 Zr1 N1 C4 -95.8(2) 2
Cl1 Zr1 N1 C4 91.59(19) .
Cl1 Zr1 N1 C4 -54.1(4) 2
O1 Zr1 N1 C6 8.78(14) 2
O1 Zr1 N1 C6 -179.72(15) .
N1 Zr1 N1 C6 87.11(14) 2
Cl1 Zr1 N1 C6 -85.55(13) .
Cl1 Zr1 N1 C6 128.8(2) 2
N1 C4 C3 C2 -0.5(4) .
C5 C4 C3 C2 179.3(2) .
C4 N1 C6 C7 -96.7(3) .
Zr1 N1 C6 C7 80.9(2) .
C4 N1 C6 C11 84.5(3) .
Zr1 N1 C6 C11 -97.9(2) .
C11 C10 C9 C8 0.6(4) .
C7 C6 C11 C10 0.6(3) .
N1 C6 C11 C10 179.5(2) .
C9 C10 C11 C6 -0.8(3) .
C10 C9 C8 C7 -0.4(4) .
Zr1 O1 C2 C3 -5.5(4) .
Zr1 O1 C2 C1 173.63(15) .
C4 C3 C2 O1 2.1(4) .
C4 C3 C2 C1 -176.9(2) .
O1 C2 C1 F3 -58.6(3) .
C3 C2 C1 F3 120.6(2) .
O1 C2 C1 F1 61.3(3) .
C3 C2 C1 F1 -119.5(2) .
O1 C2 C1 F2 -178.39(19) .
C3 C2 C1 F2 0.8(3) .
C9 C8 C7 C6 0.3(4) .
C11 C6 C7 C8 -0.4(3) .
N1 C6 C7 C8 -179.2(2) .
