#------------------------------------------------------------------------------
#$Date: 2016-10-14 09:19:16 +0300 (Fri, 14 Oct 2016) $
#$Revision: 187336 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/68/7226803.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_7226803
loop_
_publ_author_name
'Kim, Hyejin'
'Choi, Sung Ho'
'Ahn, Duseong'
'Kim, Yoseph'
'Ryu, Ji Yeon'
'Lee, Junseong'
'Kim, Youngjo'
_publ_section_title
;
 Facile synthesis of a dimeric titanium(iv) complex with terminal
 TiO moieties and its application as a catalyst for the
 cycloaddition reaction of CO2to epoxides
;
_journal_issue                   100
_journal_name_full               'RSC Adv.'
_journal_page_first              97800
_journal_paper_doi               10.1039/C6RA23255H
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C28 H42 Cl6 N4 O6 Ti2'
_chemical_formula_weight         839.15
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-08-06 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.588(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5970(3)
_cell_length_b                   19.6755(6)
_cell_length_c                   9.9008(3)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.37
_cell_volume                     1800.76(10)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.573
_diffrn_reflns_theta_min         2.070
_exptl_absorpt_coefficient_mu    0.934
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0436P)²+3.6450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3145
_reflns_number_total             3738
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra23255h2.cif
_cod_data_source_block           kyj35-2
_cod_database_code               7226803
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ti1 Ti 0.95809(4) 0.08047(2) 0.49266(4) 0.01006(12) Uani 1 1 d . .
N1 N 0.8292(2) 0.20578(10) 0.2189(2) 0.0139(4) Uani 1 1 d . .
N2 N 1.0176(2) 0.13131(10) 0.3238(2) 0.0118(4) Uani 1 1 d . .
O1 O 0.77350(17) 0.11537(8) 0.42886(18) 0.0132(4) Uani 1 1 d . .
O2 O 1.08900(17) 0.00992(8) 0.43469(17) 0.0114(3) Uani 1 1 d . .
O3 O 1.04836(18) 0.12707(8) 0.62825(18) 0.0162(4) Uani 1 1 d . .
C1 C 0.7407(3) 0.23712(13) 0.1032(3) 0.0186(5) Uani 1 1 d . .
H1 H 0.6701 0.2671 0.1154 0.022 Uiso 1 1 calc R U
C2 C 0.7531(3) 0.22558(13) -0.0276(3) 0.0214(6) Uani 1 1 d . .
H2 H 0.6920 0.2470 -0.1048 0.026 Uiso 1 1 calc R U
C3 C 0.8603(3) 0.18061(13) -0.0441(3) 0.0201(5) Uani 1 1 d . .
H3 H 0.8703 0.1716 -0.1333 0.024 Uiso 1 1 calc R U
C4 C 0.9499(3) 0.14995(12) 0.0696(3) 0.0167(5) Uani 1 1 d . .
H4 H 1.0224 0.1213 0.0567 0.020 Uiso 1 1 calc R U
C5 C 0.9361(2) 0.16042(11) 0.2083(3) 0.0125(5) Uani 1 1 d . .
C6 C 0.8144(3) 0.22746(12) 0.3573(3) 0.0145(5) Uani 1 1 d . .
H6A H 0.7762 0.2734 0.3492 0.017 Uiso 1 1 calc R U
H6B H 0.9097 0.2286 0.4231 0.017 Uiso 1 1 calc R U
C7 C 0.7164(3) 0.18180(12) 0.4173(3) 0.0143(5) Uani 1 1 d . .
C8 C 0.5622(3) 0.17913(14) 0.3219(3) 0.0219(6) Uani 1 1 d . .
H8A H 0.5635 0.1608 0.2323 0.033 Uiso 1 1 calc R U
H8B H 0.5223 0.2242 0.3097 0.033 Uiso 1 1 calc R U
H8C H 0.5039 0.1507 0.3636 0.033 Uiso 1 1 calc R U
C9 C 0.7177(3) 0.20945(13) 0.5615(3) 0.0208(6) Uani 1 1 d . .
H9A H 0.6568 0.1818 0.6017 0.031 Uiso 1 1 calc R U
H9B H 0.6824 0.2553 0.5523 0.031 Uiso 1 1 calc R U
H9C H 0.8148 0.2087 0.6212 0.031 Uiso 1 1 calc R U
C10 C 1.1593(2) 0.10401(12) 0.3208(3) 0.0132(5) Uani 1 1 d . .
H10A H 1.2333 0.1225 0.3990 0.016 Uiso 1 1 calc R U
H10B H 1.1810 0.1182 0.2349 0.016 Uiso 1 1 calc R U
C11 C 1.1625(3) 0.02613(12) 0.3294(3) 0.0139(5) Uani 1 1 d . .
C12 C 1.0814(3) -0.00719(13) 0.1921(3) 0.0223(6) Uani 1 1 d . .
H12A H 1.0777 -0.0554 0.2053 0.033 Uiso 1 1 calc R U
H12B H 1.1306 0.0022 0.1216 0.033 Uiso 1 1 calc R U
H12C H 0.9848 0.0106 0.1629 0.033 Uiso 1 1 calc R U
C13 C 1.3186(3) 0.00238(14) 0.3774(3) 0.0237(6) Uani 1 1 d . .
H13A H 1.3632 0.0205 0.4688 0.036 Uiso 1 1 calc R U
H13B H 1.3700 0.0180 0.3125 0.036 Uiso 1 1 calc R U
H13C H 1.3212 -0.0464 0.3813 0.036 Uiso 1 1 calc R U
C14 C 0.3243(3) 0.07708(14) 0.8296(3) 0.0233(6) Uani 1 1 d . .
H14 H 0.2364 0.0972 0.7684 0.028 Uiso 1 1 calc R U
Cl1 Cl 0.47398(11) 0.11608(5) 0.79143(13) 0.0582(3) Uani 1 1 d . .
Cl2 Cl 0.32483(10) 0.09339(5) 1.00375(8) 0.0409(2) Uani 1 1 d . .
Cl3 Cl 0.32334(9) -0.00929(4) 0.79257(11) 0.0433(2) Uani 1 1 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'
Ti Ti 0.2776 0.4457 '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
O3 Ti1 O1 108.35(8) . .
O3 Ti1 O2 108.45(8) . 3_756
O1 Ti1 O2 99.43(7) . 3_756
O3 Ti1 O2 111.88(8) . .
O1 Ti1 O2 139.32(7) . .
O2 Ti1 O2 73.50(7) 3_756 .
O3 Ti1 N2 100.45(8) . .
O1 Ti1 N2 89.54(7) . .
O2 Ti1 N2 144.99(7) 3_756 .
O2 Ti1 N2 77.71(7) . .
O3 Ti1 Ti1 115.49(6) . 3_756
O1 Ti1 Ti1 125.39(5) . 3_756
O2 Ti1 Ti1 37.17(4) 3_756 3_756
O2 Ti1 Ti1 36.33(4) . 3_756
N2 Ti1 Ti1 111.84(6) . 3_756
C1 N1 C5 122.0(2) . .
C1 N1 C6 116.8(2) . .
C5 N1 C6 120.9(2) . .
C5 N2 C10 118.3(2) . .
C5 N2 Ti1 130.60(16) . .
C10 N2 Ti1 106.60(14) . .
C7 O1 Ti1 133.55(15) . .
C11 O2 Ti1 130.79(14) . 3_756
C11 O2 Ti1 120.45(13) . .
Ti1 O2 Ti1 106.50(7) 3_756 .
C2 C1 N1 121.9(2) . .
C1 C2 C3 118.4(2) . .
C4 C3 C2 120.3(2) . .
C3 C4 C5 122.0(2) . .
N2 C5 N1 119.3(2) . .
N2 C5 C4 125.4(2) . .
N1 C5 C4 115.3(2) . .
N1 C6 C7 114.3(2) . .
O1 C7 C9 110.4(2) . .
O1 C7 C8 108.0(2) . .
C9 C7 C8 110.7(2) . .
O1 C7 C6 108.04(19) . .
C9 C7 C6 107.6(2) . .
C8 C7 C6 112.0(2) . .
N2 C10 C11 111.63(19) . .
O2 C11 C13 109.8(2) . .
O2 C11 C12 108.6(2) . .
C13 C11 C12 111.8(2) . .
O2 C11 C10 104.74(18) . .
C13 C11 C10 109.1(2) . .
C12 C11 C10 112.5(2) . .
Cl3 C14 Cl2 112.64(17) . .
Cl3 C14 Cl1 109.88(15) . .
Cl2 C14 Cl1 110.19(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O3 1.6638(17) .
Ti1 O1 1.8459(17) .
Ti1 O2 2.0147(16) 3_756
Ti1 O2 2.0549(16) .
Ti1 N2 2.153(2) .
Ti1 Ti1 3.2609(8) 3_756
N1 C1 1.375(3) .
N1 C5 1.385(3) .
N1 C6 1.478(3) .
N2 C5 1.329(3) .
N2 C10 1.470(3) .
O1 C7 1.410(3) .
O2 C11 1.443(3) .
O2 Ti1 2.0148(16) 3_756
C1 C2 1.352(4) .
C2 C3 1.399(4) .
C3 C4 1.360(4) .
C4 C5 1.430(3) .
C6 C7 1.531(3) .
C7 C9 1.525(4) .
C7 C8 1.528(3) .
C10 C11 1.535(3) .
C11 C13 1.518(3) .
C11 C12 1.521(4) .
C14 Cl3 1.738(3) .
C14 Cl2 1.753(3) .
C14 Cl1 1.757(3) .
