#------------------------------------------------------------------------------
#$Date: 2016-06-17 01:56:20 +0300 (Fri, 17 Jun 2016) $
#$Revision: 183606 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/64/4086430.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_4086430
loop_
_publ_author_name
'Wright, Luka A.'
'Hope, Eric G.'
'Solan, Gregory A.'
'Cross, Warren B.'
'Singh, Kuldip'
_publ_section_title
;
 Active O,Npy,N-Titanium(IV) Fluoride Precatalysts for Ethylene
 Polymerization: Exploring “Fluoride Effects” on Polymer
 Properties and Catalytic Performance
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1183
_journal_paper_doi               10.1021/acs.organomet.5b00900
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C13 H13 F3 N2 O Ti, H2 O'
_chemical_formula_sum            'C13 H15 F3 N2 O2 Ti'
_chemical_formula_weight         336.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   9.502(4)
_cell_length_b                   7.282(3)
_cell_length_c                   20.079(8)
_cell_measurement_reflns_used    965
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.413
_cell_measurement_theta_min      2.372
_cell_volume                     1389.3(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1251
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10407
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 2397 reflections(SADABS);Rint 0.1245 before
correction and 0.0631 after.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1478
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0539
_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)+(0.0562P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                1031
_reflns_number_total             1478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00900_si_002.cif
_cod_data_source_block           14062
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086427--4086430.cif.
;
_cod_original_cell_volume        1389.4(9)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4086430
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Ti1 Ti 0.30694(9) 0.2500 0.40217(4) 0.0216(3) Uani 1 2 d S
F1 F 0.4953(3) 0.2500 0.38903(13) 0.0395(8) Uani 1 2 d S
F2 F 0.3082(2) -0.0009(3) 0.41615(9) 0.0351(5) Uani 1 1 d .
O1 O 0.2261(3) 0.2500 0.32058(15) 0.0270(8) Uani 1 2 d S
N1 N 0.2757(4) 0.2500 0.51153(18) 0.0232(10) Uani 1 2 d S
N2 N 0.0856(4) 0.2500 0.42180(18) 0.0212(9) Uani 1 2 d S
C1 C 0.3825(5) 0.2500 0.5550(2) 0.0307(12) Uani 1 2 d S
H1 H 0.4758 0.2500 0.5381 0.037 Uiso 1 2 calc SR
C2 C 0.3643(6) 0.2500 0.6229(3) 0.0359(13) Uani 1 2 d S
H2 H 0.4428 0.2500 0.6522 0.043 Uiso 1 2 calc SR
C3 C 0.2276(5) 0.2500 0.6474(3) 0.0333(13) Uani 1 2 d S
H3 H 0.2110 0.2500 0.6940 0.040 Uiso 1 2 calc SR
C4 C 0.1167(5) 0.2500 0.6036(2) 0.0286(12) Uani 1 2 d S
H4 H 0.0226 0.2500 0.6196 0.034 Uiso 1 2 calc SR
C5 C 0.1435(5) 0.2500 0.5361(2) 0.0215(11) Uani 1 2 d S
C6 C 0.0312(5) 0.2500 0.4845(2) 0.0207(10) Uani 1 2 d S
C7 C -0.1111(5) 0.2500 0.4951(2) 0.0251(11) Uani 1 2 d S
H7 H -0.1484 0.2500 0.5390 0.030 Uiso 1 2 calc SR
C8 C -0.1998(5) 0.2500 0.4398(3) 0.0306(12) Uani 1 2 d S
H8 H -0.2990 0.2500 0.4460 0.037 Uiso 1 2 calc SR
C9 C -0.1449(5) 0.2500 0.3765(2) 0.0275(12) Uani 1 2 d S
H9 H -0.2048 0.2500 0.3386 0.033 Uiso 1 2 calc SR
C10 C 0.0013(5) 0.2500 0.3692(2) 0.0221(11) Uani 1 2 d S
C11 C 0.0799(5) 0.2500 0.3032(2) 0.0244(11) Uani 1 2 d S
C12 C 0.0465(4) 0.0772(5) 0.26339(16) 0.0306(9) Uani 1 1 d .
H12A H 0.0953 0.0821 0.2204 0.046 Uiso 1 1 calc R
H12B H -0.0552 0.0695 0.2559 0.046 Uiso 1 1 calc R
H12C H 0.0780 -0.0310 0.2883 0.046 Uiso 1 1 calc R
O2 O 0.2916(5) 0.7500 0.3133(2) 0.0560(13) Uani 1 2 d SD
H2B H 0.289(4) 0.846(4) 0.3408(18) 0.067 Uiso 1 1 d D
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'
Ti Ti 0.2776 0.4457 '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 Ti1 F1 106.74(13) . .
O1 Ti1 F2 98.06(6) . 7_565
F1 Ti1 F2 90.91(7) . 7_565
O1 Ti1 F2 98.06(6) . .
F1 Ti1 F2 90.91(7) . .
F2 Ti1 F2 162.51(13) 7_565 .
O1 Ti1 N2 75.50(14) . .
F1 Ti1 N2 177.77(13) . .
F2 Ti1 N2 88.75(7) 7_565 .
F2 Ti1 N2 88.75(7) . .
O1 Ti1 N1 147.19(15) . .
F1 Ti1 N1 106.08(13) . .
F2 Ti1 N1 81.39(6) 7_565 .
F2 Ti1 N1 81.39(6) . .
N2 Ti1 N1 71.69(14) . .
C11 O1 Ti1 129.2(3) . .
C1 N1 C5 117.8(4) . .
C1 N1 Ti1 123.0(3) . .
C5 N1 Ti1 119.1(3) . .
C10 N2 C6 120.5(4) . .
C10 N2 Ti1 116.6(3) . .
C6 N2 Ti1 122.9(3) . .
N1 C1 C2 123.5(5) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C1 C2 C3 117.9(5) . .
C1 C2 H2 121.0 . .
C3 C2 H2 121.0 . .
C4 C3 C2 119.5(5) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.2(5) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
N1 C5 C4 122.1(4) . .
N1 C5 C6 114.4(4) . .
C4 C5 C6 123.5(4) . .
N2 C6 C7 121.2(4) . .
N2 C6 C5 111.8(4) . .
C7 C6 C5 127.0(4) . .
C6 C7 C8 118.3(5) . .
C6 C7 H7 120.8 . .
C8 C7 H7 120.8 . .
C9 C8 C7 120.5(5) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 118.3(4) . .
C8 C9 H9 120.9 . .
C10 C9 H9 120.9 . .
N2 C10 C9 121.2(4) . .
N2 C10 C11 113.4(4) . .
C9 C10 C11 125.4(4) . .
O1 C11 C10 105.3(4) . .
O1 C11 C12 109.3(2) . .
C10 C11 C12 110.8(2) . .
O1 C11 C12 109.3(2) . 7_565
C10 C11 C12 110.8(2) . 7_565
C12 C11 C12 111.3(4) . 7_565
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.809(3) .
Ti1 F1 1.809(3) .
Ti1 F2 1.849(2) 7_565
Ti1 F2 1.849(2) .
Ti1 N2 2.140(4) .
Ti1 N1 2.216(4) .
O1 C11 1.432(5) .
N1 C1 1.339(6) .
N1 C5 1.350(6) .
N2 C10 1.325(6) .
N2 C6 1.362(5) .
C1 C2 1.374(7) .
C1 H1 0.9500 .
C2 C3 1.388(7) .
C2 H2 0.9500 .
C3 C4 1.372(7) .
C3 H3 0.9500 .
C4 C5 1.379(6) .
C4 H4 0.9500 .
C5 C6 1.487(6) .
C6 C7 1.368(6) .
C7 C8 1.393(7) .
C7 H7 0.9500 .
C8 C9 1.376(7) .
C8 H8 0.9500 .
C9 C10 1.397(6) .
C9 H9 0.9500 .
C10 C11 1.522(6) .
C11 C12 1.524(4) .
C11 C12 1.524(4) 7_565
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
O2 H2B 0.894(19) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2B F2 0.894(19) 1.89(2) 2.753(4) 163(4) 1_565
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
_geom_torsion_site_symmetry_4
F1 Ti1 O1 C11 180.0 . .
F2 Ti1 O1 C11 -86.60(7) 7_565 .
F2 Ti1 O1 C11 86.60(7) . .
N2 Ti1 O1 C11 0.0 . .
N1 Ti1 O1 C11 0.0 . .
O1 Ti1 N1 C1 180.000(1) . .
F1 Ti1 N1 C1 0.000(1) . .
F2 Ti1 N1 C1 -88.46(7) 7_565 .
F2 Ti1 N1 C1 88.46(7) . .
N2 Ti1 N1 C1 180.000(1) . .
O1 Ti1 N1 C5 0.000(1) . .
F1 Ti1 N1 C5 180.0 . .
F2 Ti1 N1 C5 91.54(7) 7_565 .
F2 Ti1 N1 C5 -91.54(7) . .
N2 Ti1 N1 C5 0.0 . .
O1 Ti1 N2 C10 0.0 . .
F2 Ti1 N2 C10 98.65(6) 7_565 .
F2 Ti1 N2 C10 -98.65(6) . .
N1 Ti1 N2 C10 180.0 . .
O1 Ti1 N2 C6 180.0 . .
F2 Ti1 N2 C6 -81.35(6) 7_565 .
F2 Ti1 N2 C6 81.35(6) . .
N1 Ti1 N2 C6 0.0 . .
C5 N1 C1 C2 0.000(2) . .
Ti1 N1 C1 C2 180.000(1) . .
N1 C1 C2 C3 0.000(2) . .
C1 C2 C3 C4 0.000(2) . .
C2 C3 C4 C5 0.000(2) . .
C1 N1 C5 C4 0.000(2) . .
Ti1 N1 C5 C4 180.000(1) . .
C1 N1 C5 C6 180.000(1) . .
Ti1 N1 C5 C6 0.000(1) . .
C3 C4 C5 N1 0.000(2) . .
C3 C4 C5 C6 180.000(2) . .
C10 N2 C6 C7 0.000(1) . .
Ti1 N2 C6 C7 180.0 . .
C10 N2 C6 C5 180.0 . .
Ti1 N2 C6 C5 0.000(1) . .
N1 C5 C6 N2 0.000(1) . .
C4 C5 C6 N2 180.000(1) . .
N1 C5 C6 C7 180.000(1) . .
C4 C5 C6 C7 0.000(2) . .
N2 C6 C7 C8 0.000(2) . .
C5 C6 C7 C8 180.000(1) . .
C6 C7 C8 C9 0.000(1) . .
C7 C8 C9 C10 0.000(1) . .
C6 N2 C10 C9 0.000(1) . .
Ti1 N2 C10 C9 180.0 . .
C6 N2 C10 C11 180.0 . .
Ti1 N2 C10 C11 0.0 . .
C8 C9 C10 N2 0.000(1) . .
C8 C9 C10 C11 180.0 . .
Ti1 O1 C11 C10 0.0 . .
Ti1 O1 C11 C12 -119.0(3) . .
Ti1 O1 C11 C12 119.0(3) . 7_565
N2 C10 C11 O1 0.0 . .
C9 C10 C11 O1 180.0 . .
N2 C10 C11 C12 118.0(3) . .
C9 C10 C11 C12 -62.0(3) . .
N2 C10 C11 C12 -118.0(3) . 7_565
C9 C10 C11 C12 62.0(3) . 7_565
