#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:50:02 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179766 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/62/7006228.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_7006228
loop_
_publ_author_name
'Nikiforov, Grigory B.'
'Roesky, Herbert W.'
'Jones, Peter G.'
'Oswald, Rainer B.'
'Noltemeyer, Mathias'
_publ_section_title
;
 A ligand influence on the stability of heterobimetallic complexes
 containing the Ti(µ-O)Al skeleton. Transformation of
 heterometallic systems to the homometallic Ti(iv) and Al(iii)
 complexes
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              4149
_journal_paper_doi               10.1039/b710470g
_journal_year                    2007
_chemical_formula_sum            'C65 H90 Cl2 N4 O2 Ti2'
_chemical_formula_weight         1126.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.761(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4999(18)
_cell_length_b                   12.9944(16)
_cell_length_c                   17.350(2)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.79
_cell_measurement_theta_min      2.35
_cell_volume                     2979.7(6)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_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            157240
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.9761
_exptl_absorpt_correction_T_min  0.8599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         9104
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0373P)²+1.6762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                7490
_reflns_number_total             9104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710470g.txt
_cod_data_source_block           graggo
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2979.6(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7006228
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.500904(15) 0.506360(15) 0.419883(11) 0.00960(5) Uani 1 1 d . . .
Cl Cl 0.50563(2) 0.35292(2) 0.361473(18) 0.01952(7) Uani 1 1 d . . .
O O 0.40882(6) 0.49367(7) 0.48570(5) 0.01401(16) Uani 1 1 d . . .
N1 N 0.60679(7) 0.58878(7) 0.36820(5) 0.01131(17) Uani 1 1 d . . .
N2 N 0.38929(7) 0.58586(7) 0.33851(5) 0.01150(17) Uani 1 1 d . . .
C1 C 0.67386(10) 0.63863(10) 0.24990(7) 0.0191(2) Uani 1 1 d . . .
H1A H 0.6994 0.7063 0.2696 0.029 Uiso 1 1 calc R . .
H1B H 0.6478 0.6425 0.1930 0.029 Uiso 1 1 calc R . .
H1C H 0.7289 0.5882 0.2609 0.029 Uiso 1 1 calc R . .
C2 C 0.58967(9) 0.60612(8) 0.29034(7) 0.0126(2) Uani 1 1 d . . .
C3 C 0.49396(9) 0.60102(9) 0.24153(6) 0.0135(2) Uani 1 1 d . . .
H3 H 0.4920 0.5953 0.1867 0.016 Uiso 1 1 calc R . .
C4 C 0.40088(9) 0.60333(9) 0.26437(6) 0.0127(2) Uani 1 1 d . . .
C5 C 0.31163(10) 0.63237(10) 0.20014(7) 0.0185(2) Uani 1 1 d . . .
H5A H 0.2609 0.5774 0.1939 0.028 Uiso 1 1 calc R . .
H5B H 0.3344 0.6419 0.1505 0.028 Uiso 1 1 calc R . .
H5C H 0.2818 0.6966 0.2144 0.028 Uiso 1 1 calc R . .
C6 C 0.28873(9) 0.61302(9) 0.35028(7) 0.0130(2) Uani 1 1 d . . .
C7 C 0.20778(9) 0.54352(9) 0.32883(7) 0.0150(2) Uani 1 1 d . . .
C8 C 0.11051(10) 0.57842(10) 0.33128(8) 0.0200(2) Uani 1 1 d . . .
H8 H 0.0552 0.5320 0.3190 0.024 Uiso 1 1 calc R . .
C9 C 0.09280(10) 0.67890(11) 0.35116(8) 0.0211(3) Uani 1 1 d . . .
H9 H 0.0257 0.7019 0.3499 0.025 Uiso 1 1 calc R . .
C10 C 0.17341(10) 0.74551(10) 0.37287(8) 0.0188(2) Uani 1 1 d . . .
H10 H 0.1611 0.8143 0.3869 0.023 Uiso 1 1 calc R . .
C11 C 0.27262(9) 0.71382(9) 0.37469(7) 0.0155(2) Uani 1 1 d . . .
C12 C 0.22113(9) 0.43396(9) 0.30223(7) 0.0160(2) Uani 1 1 d . . .
H12 H 0.2905 0.4276 0.2907 0.019 Uiso 1 1 calc R . .
C13 C 0.21289(11) 0.35939(10) 0.36835(8) 0.0228(3) Uani 1 1 d . . .
H13A H 0.2634 0.3772 0.4155 0.034 Uiso 1 1 calc R . .
H13B H 0.2250 0.2891 0.3520 0.034 Uiso 1 1 calc R . .
H13C H 0.1450 0.3639 0.3801 0.034 Uiso 1 1 calc R . .
C14 C 0.14385(11) 0.40362(11) 0.22771(8) 0.0231(3) Uani 1 1 d . . .
H14A H 0.0758 0.4024 0.2394 0.035 Uiso 1 1 calc R . .
H14B H 0.1605 0.3352 0.2102 0.035 Uiso 1 1 calc R . .
H14C H 0.1459 0.4539 0.1860 0.035 Uiso 1 1 calc R . .
C15 C 0.35870(10) 0.78983(10) 0.39969(8) 0.0198(2) Uani 1 1 d . . .
H15 H 0.4229 0.7491 0.4116 0.024 Uiso 1 1 calc R . .
C16 C 0.36765(18) 0.86378(16) 0.33466(11) 0.0535(6) Uani 1 1 d . . .
H16A H 0.3826 0.8255 0.2897 0.080 Uiso 1 1 calc R . .
H16B H 0.4224 0.9128 0.3536 0.080 Uiso 1 1 calc R . .
H16C H 0.3038 0.9012 0.3183 0.080 Uiso 1 1 calc R . .
C17 C 0.35085(13) 0.84813(13) 0.47425(10) 0.0349(4) Uani 1 1 d . . .
H17A H 0.4095 0.8936 0.4892 0.052 Uiso 1 1 calc R . .
H17B H 0.3493 0.7990 0.5169 0.052 Uiso 1 1 calc R . .
H17C H 0.2887 0.8893 0.4647 0.052 Uiso 1 1 calc R . .
C18 C 0.70781(9) 0.61895(9) 0.40866(7) 0.0127(2) Uani 1 1 d . . .
C19 C 0.78971(9) 0.55091(9) 0.41135(7) 0.0147(2) Uani 1 1 d . . .
C20 C 0.88698(9) 0.58637(10) 0.44374(8) 0.0190(2) Uani 1 1 d . . .
H20 H 0.9429 0.5410 0.4471 0.023 Uiso 1 1 calc R . .
C21 C 0.90373(10) 0.68637(10) 0.47105(8) 0.0199(2) Uani 1 1 d . . .
H21 H 0.9705 0.7094 0.4921 0.024 Uiso 1 1 calc R . .
C22 C 0.82269(9) 0.75231(10) 0.46747(7) 0.0176(2) Uani 1 1 d . . .
H22 H 0.8345 0.8209 0.4861 0.021 Uiso 1 1 calc R . .
C23 C 0.72375(9) 0.72013(9) 0.43696(7) 0.0146(2) Uani 1 1 d . A .
C24 C 0.77695(9) 0.44210(9) 0.37893(7) 0.0158(2) Uani 1 1 d . . .
H24 H 0.7081 0.4363 0.3445 0.019 Uiso 1 1 calc R . .
C25 C 0.85569(11) 0.41451(11) 0.32958(8) 0.0233(3) Uani 1 1 d . . .
H25A H 0.8563 0.4679 0.2898 0.035 Uiso 1 1 calc R . .
H25B H 0.8382 0.3482 0.3035 0.035 Uiso 1 1 calc R . .
H25C H 0.9228 0.4099 0.3640 0.035 Uiso 1 1 calc R . .
C26 C 0.78363(10) 0.36565(10) 0.44669(8) 0.0212(3) Uani 1 1 d . . .
H26A H 0.8507 0.3702 0.4812 0.032 Uiso 1 1 calc R . .
H26B H 0.7729 0.2957 0.4255 0.032 Uiso 1 1 calc R . .
H26C H 0.7317 0.3820 0.4768 0.032 Uiso 1 1 calc R . .
C27 C 0.63860(10) 0.79743(9) 0.43344(8) 0.0185(2) Uani 1 1 d DU . .
H27 H 0.5736 0.7636 0.4080 0.022 Uiso 0.841(8) 1 calc PR A 1
H27' H 0.5772 0.7538 0.4317 0.022 Uiso 0.159(8) 1 calc PR A 2
C28 C 0.6298(2) 0.8329(2) 0.51510(11) 0.0242(5) Uani 0.841(8) 1 d PDU A 1
H28A H 0.6125 0.7741 0.5452 0.036 Uiso 0.841(8) 1 calc PR A 1
H28B H 0.5767 0.8853 0.5107 0.036 Uiso 0.841(8) 1 calc PR A 1
H28C H 0.6945 0.8622 0.5421 0.036 Uiso 0.841(8) 1 calc PR A 1
C29 C 0.65534(19) 0.89221(16) 0.38313(12) 0.0284(6) Uani 0.841(8) 1 d PDU A 1
H29A H 0.7200 0.9249 0.4063 0.043 Uiso 0.841(8) 1 calc PR A 1
H29B H 0.6002 0.9416 0.3820 0.043 Uiso 0.841(8) 1 calc PR A 1
H29C H 0.6564 0.8699 0.3293 0.043 Uiso 0.841(8) 1 calc PR A 1
C28' C 0.6502(12) 0.8573(12) 0.5126(8) 0.032(4) Uiso 0.159(8) 1 d PDU A 2
H28D H 0.6698 0.8094 0.5566 0.049 Uiso 0.159(8) 1 calc PR A 2
H28E H 0.5856 0.8898 0.5157 0.049 Uiso 0.159(8) 1 calc PR A 2
H28F H 0.7023 0.9103 0.5151 0.049 Uiso 0.159(8) 1 calc PR A 2
C29' C 0.6134(11) 0.8599(10) 0.3654(6) 0.032(3) Uiso 0.159(8) 1 d PDU A 2
H29D H 0.5580 0.9064 0.3707 0.048 Uiso 0.159(8) 1 calc PR A 2
H29E H 0.5920 0.8161 0.3189 0.048 Uiso 0.159(8) 1 calc PR A 2
H29F H 0.6726 0.9004 0.3594 0.048 Uiso 0.159(8) 1 calc PR A 2
C91 C 1.0059(6) 0.9319(9) 0.5631(8) 0.025(2) Uani 0.50 1 d PDU B -1
C92 C 0.9292(10) 1.0101(11) 0.5448(9) 0.030(2) Uani 0.50 1 d PDU B -1
H92 H 0.8803 1.0166 0.5769 0.036 Uiso 0.50 1 calc PR B -1
C93 C 0.9249(12) 1.0760(10) 0.4816(10) 0.037(3) Uani 0.50 1 d PDU B -1
H93 H 0.8742 1.1278 0.4710 0.045 Uiso 0.50 1 calc PR B -1
C94 C 0.9917(9) 1.0665(12) 0.4359(10) 0.050(3) Uani 0.50 1 d PDU B -1
H94 H 0.9865 1.1117 0.3922 0.059 Uiso 0.50 1 calc PR B -1
C95 C 1.0654(12) 0.9977(12) 0.4474(10) 0.039(3) Uani 0.50 1 d PDU B -1
H95 H 1.1113 0.9946 0.4126 0.047 Uiso 0.50 1 calc PR B -1
C96 C 1.0755(10) 0.9308(11) 0.5098(10) 0.036(2) Uani 0.50 1 d PDU B -1
H96 H 1.1295 0.8825 0.5181 0.043 Uiso 0.50 1 calc PR B -1
C97 C 1.0089(3) 0.8624(3) 0.6275(2) 0.0382(8) Uani 0.50 1 d PDU B -1
H97A H 0.9771 0.8948 0.6674 0.057 Uiso 0.50 1 calc PR B -1
H97B H 1.0793 0.8455 0.6508 0.057 Uiso 0.50 1 calc PR B -1
H97C H 0.9721 0.7993 0.6085 0.057 Uiso 0.50 1 calc PR B -1
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'
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
_geom_angle_publ_flag
O Ti O 81.78(4) 3_666 . ?
O Ti N2 148.39(4) 3_666 . ?
O Ti N2 88.78(4) . . ?
O Ti N1 89.73(4) 3_666 . ?
O Ti N1 153.56(4) . . ?
N2 Ti N1 85.47(4) . . ?
O Ti Cl 109.19(3) 3_666 . ?
O Ti Cl 106.43(3) . . ?
N2 Ti Cl 102.41(3) . . ?
N1 Ti Cl 100.01(3) . . ?
O Ti Ti 41.26(3) 3_666 3_666 ?
O Ti Ti 40.52(3) . 3_666 ?
N2 Ti Ti 123.02(3) . 3_666 ?
N1 Ti Ti 126.41(3) . 3_666 ?
Cl Ti Ti 113.846(14) . 3_666 ?
Ti O Ti 98.22(4) 3_666 . ?
C2 N1 C18 113.12(9) . . ?
C2 N1 Ti 121.10(8) . . ?
C18 N1 Ti 125.25(7) . . ?
C4 N2 C6 112.71(9) . . ?
C4 N2 Ti 120.99(8) . . ?
C6 N2 Ti 125.65(7) . . ?
N1 C2 C3 123.45(10) . . ?
N1 C2 C1 121.48(11) . . ?
C3 C2 C1 114.99(10) . . ?
C4 C3 C2 127.17(10) . . ?
N2 C4 C3 123.74(10) . . ?
N2 C4 C5 121.04(10) . . ?
C3 C4 C5 115.16(10) . . ?
C11 C6 C7 121.16(11) . . ?
C11 C6 N2 118.25(10) . . ?
C7 C6 N2 120.19(10) . . ?
C8 C7 C6 117.85(11) . . ?
C8 C7 C12 118.93(11) . . ?
C6 C7 C12 123.22(11) . . ?
C9 C8 C7 121.65(12) . . ?
C10 C9 C8 119.52(12) . . ?
C9 C10 C11 121.36(12) . . ?
C10 C11 C6 118.32(11) . . ?
C10 C11 C15 119.30(11) . . ?
C6 C11 C15 122.34(11) . . ?
C7 C12 C13 109.64(10) . . ?
C7 C12 C14 113.18(10) . . ?
C13 C12 C14 109.20(11) . . ?
C16 C15 C11 111.99(12) . . ?
C16 C15 C17 110.45(13) . . ?
C11 C15 C17 112.63(11) . . ?
C23 C18 C19 120.83(11) . . ?
C23 C18 N1 118.86(10) . . ?
C19 C18 N1 119.94(10) . . ?
C20 C19 C18 118.25(11) . . ?
C20 C19 C24 118.84(11) . . ?
C18 C19 C24 122.89(11) . . ?
C21 C20 C19 121.41(12) . . ?
C22 C21 C20 119.60(12) . . ?
C21 C22 C23 121.26(12) . . ?
C22 C23 C18 118.64(11) . . ?
C22 C23 C27 118.35(11) . . ?
C18 C23 C27 122.98(11) . . ?
C19 C24 C26 109.64(10) . . ?
C19 C24 C25 112.61(10) . . ?
C26 C24 C25 109.75(10) . . ?
C29' C27 C28 123.6(5) . . ?
C29' C27 C23 117.7(5) . . ?
C28 C27 C23 111.46(12) . . ?
C29' C27 C29 27.7(6) . . ?
C28 C27 C29 109.40(14) . . ?
C23 C27 C29 110.59(12) . . ?
C29' C27 C28' 114.4(7) . . ?
C28 C27 C28' 15.9(6) . . ?
C23 C27 C28' 110.8(6) . . ?
C29 C27 C28' 95.7(6) . . ?
C97 C91 C92 121.5(9) . . ?
C97 C91 C96 125.1(8) . . ?
C92 C91 C96 113.4(14) . . ?
C93 C92 C91 121.6(13) . . ?
C94 C93 C92 119.6(14) . . ?
C95 C94 C93 124(2) . . ?
C94 C95 C96 119.9(16) . . ?
C95 C96 C91 121.6(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti O 1.8316(8) 3_666 ?
Ti O 1.8589(8) . ?
Ti N2 2.1127(10) . ?
Ti N1 2.1253(10) . ?
Ti Cl 2.2434(4) . ?
Ti Ti 2.7900(5) 3_666 ?
O Ti 1.8316(8) 3_666 ?
N1 C2 1.3422(14) . ?
N1 C18 1.4547(15) . ?
N2 C4 1.3464(14) . ?
N2 C6 1.4568(15) . ?
C1 C2 1.5125(16) . ?
C2 C3 1.3946(16) . ?
C3 C4 1.3928(16) . ?
C4 C5 1.5128(16) . ?
C6 C11 1.4070(16) . ?
C6 C7 1.4080(17) . ?
C7 C8 1.3981(17) . ?
C7 C12 1.5187(17) . ?
C8 C9 1.3837(19) . ?
C9 C10 1.3814(19) . ?
C10 C11 1.3954(17) . ?
C11 C15 1.5193(17) . ?
C12 C13 1.5230(17) . ?
C12 C14 1.5380(17) . ?
C15 C16 1.506(2) . ?
C15 C17 1.521(2) . ?
C18 C23 1.4046(16) . ?
C18 C19 1.4090(16) . ?
C19 C20 1.3970(17) . ?
C19 C24 1.5185(17) . ?
C20 C21 1.3858(18) . ?
C21 C22 1.3811(18) . ?
C22 C23 1.3967(17) . ?
C23 C27 1.5184(17) . ?
C24 C26 1.5277(17) . ?
C24 C25 1.5371(17) . ?
C27 C29' 1.416(9) . ?
C27 C28 1.517(2) . ?
C27 C29 1.552(2) . ?
C27 C28' 1.557(12) . ?
C91 C97 1.431(14) . ?
C91 C92 1.439(14) . ?
C91 C96 1.446(15) . ?
C92 C93 1.384(9) . ?
C93 C94 1.322(16) . ?
C94 C95 1.321(16) . ?
C95 C96 1.374(10) . ?
