#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:11:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178683 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/94/4079462.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_4079462
loop_
_publ_author_name
'Shi, Xiao-Chao'
'Jin, Guo-Xin'
_publ_section_title
;
 Titanium and Zirconium Catalysts with [N,O] Ligands: Syntheses,
 Characterization, and Their Catalytic Properties for Olefin
 Polymerization
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7198
_journal_paper_doi               10.1021/om3007568
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C42 H46 Cl4 N2 O4 Zr'
_chemical_formula_weight         875.83
_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                 125.335(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.285(4)
_cell_length_b                   17.774(3)
_cell_length_c                   17.224(5)
_cell_measurement_reflns_used    5448
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.29
_cell_volume                     5815(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20226
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        5.98
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.7939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_platon_squeeze_details          ' '
_refine_diff_density_max         0.773
_refine_diff_density_min         -4.311
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1339P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1981
_reflns_number_gt                4476
_reflns_number_total             6356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3007568_si_001.cif
_cod_data_source_block           3d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4079462
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 0.5000 0.64011(2) 0.2500 0.03749(17) Uani 1 2 d S
Cl1 Cl 0.51471(6) 0.72685(6) 0.36809(7) 0.0616(3) Uani 1 1 d .
Cl2 Cl 0.29715(7) 0.41514(9) 0.27644(12) 0.0960(5) Uani 1 1 d .
O1 O 0.60269(12) 0.62630(13) 0.31274(17) 0.0425(5) Uani 1 1 d .
O2 O 0.59654(12) 0.46469(13) 0.48014(18) 0.0520(6) Uani 1 1 d .
N1 N 0.52832(14) 0.53918(14) 0.3540(2) 0.0394(6) Uani 1 1 d .
C1 C 0.66320(17) 0.59913(18) 0.3890(2) 0.0416(7) Uani 1 1 d .
C2 C 0.72895(18) 0.6212(2) 0.4094(3) 0.0509(9) Uani 1 1 d .
C3 C 0.7874(2) 0.5915(2) 0.4906(3) 0.0611(11) Uani 1 1 d .
H3 H 0.8312 0.6064 0.5060 0.073 Uiso 1 1 calc R
C4 C 0.78661(19) 0.5406(2) 0.5521(3) 0.0633(11) Uani 1 1 d .
C5 C 0.72288(18) 0.5188(2) 0.5298(3) 0.0570(10) Uani 1 1 d .
H5 H 0.7202 0.4847 0.5686 0.068 Uiso 1 1 calc R
C6 C 0.66031(17) 0.5480(2) 0.4473(3) 0.0462(8) Uani 1 1 d .
C7 C 0.59315(17) 0.52039(18) 0.4242(2) 0.0421(7) Uani 1 1 d .
C8 C 0.48488(17) 0.49011(18) 0.3628(2) 0.0424(7) Uani 1 1 d .
C9 C 0.41264(18) 0.4820(2) 0.3087(3) 0.0506(9) Uani 1 1 d .
H9 H 0.3827 0.5110 0.2548 0.061 Uiso 1 1 calc R
C10 C 0.3875(2) 0.4271(2) 0.3403(3) 0.0574(10) Uani 1 1 d .
C11 C 0.4312(3) 0.3838(2) 0.4203(4) 0.0654(11) Uani 1 1 d .
H11 H 0.4117 0.3489 0.4391 0.078 Uiso 1 1 calc R
C12 C 0.5029(2) 0.3917(2) 0.4725(3) 0.0597(10) Uani 1 1 d .
H12 H 0.5331 0.3624 0.5260 0.072 Uiso 1 1 calc R
C13 C 0.52759(19) 0.44507(19) 0.4412(3) 0.0474(8) Uani 1 1 d .
C14 C 0.7344(2) 0.6772(3) 0.3464(3) 0.0639(11) Uani 1 1 d .
C15 C 0.6938(3) 0.6497(3) 0.2430(4) 0.0832(15) Uani 1 1 d .
H15A H 0.7088 0.5996 0.2418 0.125 Uiso 1 1 calc R
H15B H 0.7029 0.6827 0.2072 0.125 Uiso 1 1 calc R
H15C H 0.6443 0.6494 0.2155 0.125 Uiso 1 1 calc R
C16 C 0.7045(3) 0.7539(3) 0.3472(5) 0.0861(15) Uani 1 1 d .
H16A H 0.6547 0.7496 0.3160 0.129 Uiso 1 1 calc R
H16B H 0.7137 0.7901 0.3143 0.129 Uiso 1 1 calc R
H16C H 0.7265 0.7699 0.4118 0.129 Uiso 1 1 calc R
C17 C 0.8119(3) 0.6888(4) 0.3818(5) 0.101(2) Uani 1 1 d .
H17A H 0.8379 0.7108 0.4442 0.152 Uiso 1 1 calc R
H17B H 0.8135 0.7217 0.3388 0.152 Uiso 1 1 calc R
H17C H 0.8323 0.6411 0.3843 0.152 Uiso 1 1 calc R
C18 C 0.8571(2) 0.5104(3) 0.6407(4) 0.0827(15) Uani 1 1 d .
C19 C 0.9007(3) 0.5783(4) 0.7030(5) 0.131(3) Uani 1 1 d .
H19A H 0.9412 0.5607 0.7626 0.196 Uiso 1 1 calc R
H19B H 0.8723 0.6090 0.7142 0.196 Uiso 1 1 calc R
H19C H 0.9157 0.6074 0.6708 0.196 Uiso 1 1 calc R
C20 C 0.8428(3) 0.4580(5) 0.6993(6) 0.155(4) Uani 1 1 d .
H20A H 0.8056 0.4237 0.6573 0.232 Uiso 1 1 calc R
H20B H 0.8292 0.4876 0.7328 0.232 Uiso 1 1 calc R
H20C H 0.8848 0.4302 0.7442 0.232 Uiso 1 1 calc R
C21 C 0.8959(3) 0.4695(4) 0.6105(6) 0.134(3) Uani 1 1 d .
H21A H 0.8685 0.4274 0.5718 0.201 Uiso 1 1 calc R
H21B H 0.9398 0.4519 0.6656 0.201 Uiso 1 1 calc R
H21C H 0.9048 0.5025 0.5745 0.201 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'
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 165.83(13) 2_655 .
O1 Zr1 N1 76.81(9) 2_655 2_655
O1 Zr1 N1 92.25(9) . 2_655
O1 Zr1 N1 92.25(9) 2_655 .
O1 Zr1 N1 76.82(9) . .
N1 Zr1 N1 80.13(14) 2_655 .
O1 Zr1 Cl1 94.64(7) 2_655 2_655
O1 Zr1 Cl1 94.40(7) . 2_655
N1 Zr1 Cl1 90.28(8) 2_655 2_655
N1 Zr1 Cl1 166.61(7) . 2_655
O1 Zr1 Cl1 94.40(7) 2_655 .
O1 Zr1 Cl1 94.64(7) . .
N1 Zr1 Cl1 166.61(7) 2_655 .
N1 Zr1 Cl1 90.28(8) . .
Cl1 Zr1 Cl1 100.60(6) 2_655 .
C1 O1 Zr1 145.8(2) . .
C7 O2 C13 105.5(3) . .
C7 N1 C8 104.9(3) . .
C7 N1 Zr1 124.1(2) . .
C8 N1 Zr1 130.8(2) . .
O1 C1 C6 118.8(3) . .
O1 C1 C2 121.1(3) . .
C6 C1 C2 120.1(3) . .
C3 C2 C1 116.1(4) . .
C3 C2 C14 122.1(3) . .
C1 C2 C14 121.8(3) . .
C2 C3 C4 125.4(4) . .
C5 C4 C3 117.5(4) . .
C5 C4 C18 122.7(5) . .
C3 C4 C18 119.8(4) . .
C4 C5 C6 119.9(4) . .
C1 C6 C5 120.9(3) . .
C1 C6 C7 121.2(3) . .
C5 C6 C7 117.8(3) . .
N1 C7 O2 113.8(3) . .
N1 C7 C6 130.0(3) . .
O2 C7 C6 116.2(3) . .
C13 C8 C9 120.5(3) . .
C13 C8 N1 108.0(3) . .
C9 C8 N1 131.5(3) . .
C8 C9 C10 115.5(3) . .
C11 C10 C9 123.0(4) . .
C11 C10 Cl2 119.2(3) . .
C9 C10 Cl2 117.8(3) . .
C12 C11 C10 120.8(4) . .
C13 C12 C11 116.2(4) . .
C12 C13 C8 123.9(4) . .
C12 C13 O2 128.2(3) . .
C8 C13 O2 107.8(3) . .
C2 C14 C16 110.3(4) . .
C2 C14 C15 111.5(3) . .
C16 C14 C15 108.4(4) . .
C2 C14 C17 111.3(4) . .
C16 C14 C17 108.0(4) . .
C15 C14 C17 107.2(4) . .
C21 C18 C19 110.0(5) . .
C21 C18 C20 110.0(6) . .
C19 C18 C20 108.7(7) . .
C21 C18 C4 109.9(5) . .
C19 C18 C4 108.0(4) . .
C20 C18 C4 110.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1 1.989(2) 2_655
Zr1 O1 1.989(2) .
Zr1 N1 2.344(3) 2_655
Zr1 N1 2.344(3) .
Zr1 Cl1 2.4136(11) 2_655
Zr1 Cl1 2.4136(11) .
Cl2 C10 1.733(4) .
O1 C1 1.343(4) .
O2 C7 1.351(4) .
O2 C13 1.380(4) .
N1 C7 1.320(4) .
N1 C8 1.408(4) .
C1 C6 1.384(5) .
C1 C2 1.414(4) .
C2 C3 1.373(6) .
C2 C14 1.531(6) .
C3 C4 1.402(7) .
C4 C5 1.357(5) .
C4 C18 1.554(6) .
C5 C6 1.421(5) .
C6 C7 1.458(5) .
C8 C13 1.379(5) .
C8 C9 1.381(5) .
C9 C10 1.400(5) .
C10 C11 1.380(6) .
C11 C12 1.372(6) .
C12 C13 1.370(5) .
C14 C16 1.534(7) .
C14 C15 1.535(7) .
C14 C17 1.548(5) .
C18 C21 1.468(8) .
C18 C19 1.541(9) .
C18 C20 1.544(10) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.458 0.011 -0.032 2336.8 389.4
