#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:50:02 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179766 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/62/7006229.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_7006229
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            'C74 H98 N4 O2 Ti2'
_chemical_formula_weight         1171.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 110.296(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.7080(17)
_cell_length_b                   20.4316(18)
_cell_length_c                   9.0082(8)
_cell_measurement_reflns_used    7150
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.32
_cell_volume                     3229.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.1551
_diffrn_reflns_av_sigmaI/netI    0.1021
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20806
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1051P)²+10.0013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2132
_reflns_number_gt                2283
_reflns_number_total             3406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710470g.txt
_cod_data_source_block           goega
_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_sg_symbol_H-M      'C 2/m'
_cod_database_code               7006229
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.43348(5) 0.0000 0.53427(11) 0.0108(3) Uani 1 2 d S . .
O O 0.5000 0.05967(16) 0.5000 0.0144(8) Uani 1 2 d S . .
N N 0.34287(17) 0.07074(14) 0.4689(3) 0.0135(7) Uani 1 1 d U . .
C1 C 0.4595(3) 0.0000 0.7797(6) 0.0192(12) Uani 1 2 d S . .
H1A H 0.4748 -0.0441 0.8212 0.023 Uiso 0.50 1 calc PR . .
H1B H 0.4146 0.0136 0.8041 0.023 Uiso 0.50 1 calc PR . .
H1C H 0.5015 0.0306 0.8288 0.023 Uiso 0.50 1 calc PR . .
C2 C 0.2797(2) 0.06116(18) 0.5039(4) 0.0157(8) Uani 1 1 d U . .
C3 C 0.2557(3) 0.0000 0.5357(6) 0.0166(11) Uani 1 2 d SU . .
H3 H 0.2183 0.0000 0.5852 0.020 Uiso 1 2 calc SR . .
C4 C 0.2283(2) 0.1179(2) 0.5065(5) 0.0251(9) Uani 1 1 d U . .
H4A H 0.2556 0.1481 0.5919 0.030 Uiso 1 1 calc R . .
H4B H 0.1827 0.1014 0.5242 0.030 Uiso 1 1 calc R . .
H4C H 0.2132 0.1410 0.4049 0.030 Uiso 1 1 calc R . .
C11 C 0.3503(2) 0.13594(18) 0.4110(4) 0.0157(8) Uani 1 1 d U . .
C12 C 0.3789(2) 0.18761(18) 0.5169(5) 0.0173(8) Uani 1 1 d U . .
C13 C 0.3815(2) 0.24987(18) 0.4548(5) 0.0221(9) Uani 1 1 d U . .
H13 H 0.4025 0.2852 0.5250 0.027 Uiso 1 1 calc R . .
C14 C 0.3544(2) 0.2612(2) 0.2943(5) 0.0242(9) Uani 1 1 d U . .
H14 H 0.3557 0.3041 0.2547 0.029 Uiso 1 1 calc R . .
C15 C 0.3251(2) 0.20984(19) 0.1903(5) 0.0223(9) Uani 1 1 d U . .
H15 H 0.3059 0.2180 0.0797 0.027 Uiso 1 1 calc R . .
C16 C 0.3232(2) 0.14650(19) 0.2455(5) 0.0206(9) Uani 1 1 d U . .
C17 C 0.4061(2) 0.17898(19) 0.6945(5) 0.0195(8) Uani 1 1 d U . .
H17 H 0.3879 0.1354 0.7174 0.023 Uiso 1 1 calc R . .
C18 C 0.3742(3) 0.2317(2) 0.7765(5) 0.0256(9) Uani 1 1 d U . .
H18A H 0.3935 0.2242 0.8911 0.038 Uiso 1 1 calc R . .
H18B H 0.3184 0.2295 0.7368 0.038 Uiso 1 1 calc R . .
H18C H 0.3904 0.2750 0.7539 0.038 Uiso 1 1 calc R . .
C19 C 0.4926(2) 0.1792(2) 0.7629(5) 0.0247(9) Uani 1 1 d U . .
H19A H 0.5093 0.1736 0.8779 0.037 Uiso 1 1 calc R . .
H19B H 0.5118 0.2209 0.7382 0.037 Uiso 1 1 calc R . .
H19C H 0.5124 0.1432 0.7166 0.037 Uiso 1 1 calc R . .
C20 C 0.2887(3) 0.0922(2) 0.1287(5) 0.0344(11) Uani 1 1 d U . .
H20 H 0.3063 0.0497 0.1844 0.041 Uiso 1 1 calc R . .
C21 C 0.2033(4) 0.0937(4) 0.0774(7) 0.082(3) Uani 1 1 d U . .
H21A H 0.1819 0.0582 0.0017 0.123 Uiso 1 1 calc R . .
H21B H 0.1845 0.1358 0.0270 0.123 Uiso 1 1 calc R . .
H21C H 0.1878 0.0880 0.1699 0.123 Uiso 1 1 calc R . .
C22 C 0.3133(3) 0.0939(3) -0.0146(6) 0.0479(14) Uani 1 1 d U . .
H22A H 0.2891 0.0578 -0.0859 0.072 Uiso 1 1 calc R . .
H22B H 0.3689 0.0893 0.0196 0.072 Uiso 1 1 calc R . .
H22C H 0.2980 0.1356 -0.0701 0.072 Uiso 1 1 calc R . .
C91 C -0.0051(7) 0.0335(5) 0.2502(13) 0.081(4) Uiso 0.50 1 d PGU A -1
C92 C 0.0427(6) -0.0076(7) 0.2042(12) 0.124(5) Uiso 0.50 1 d PGU A -1
H92 H 0.0791 0.0104 0.1639 0.149 Uiso 0.50 1 calc PR A -1
C93 C 0.0372(7) -0.0751(6) 0.2173(15) 0.143(9) Uiso 0.50 1 d PGU A -1
H93 H 0.0699 -0.1032 0.1859 0.172 Uiso 0.50 1 calc PR A -1
C94 C -0.0160(8) -0.1014(4) 0.2763(16) 0.086(5) Uiso 0.50 1 d PGU A -1
H94 H -0.0197 -0.1475 0.2853 0.103 Uiso 0.50 1 calc PR A -1
C95 C -0.0638(6) -0.0603(6) 0.3223(13) 0.129(7) Uiso 0.50 1 d PGU A -1
H95 H -0.1002 -0.0784 0.3626 0.155 Uiso 0.50 1 calc PR A -1
C96 C -0.0584(6) 0.0071(6) 0.3092(13) 0.129(5) Uiso 0.50 1 d PGU A -1
H96 H -0.0910 0.0352 0.3406 0.155 Uiso 0.50 1 calc PR A -1
C97 C 0.0033(14) 0.1076(12) 0.205(3) 0.124(7) Uiso 0.50 1 d PU A -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'
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 82.83(16) 5_656 . ?
O Ti C1 104.69(12) 5_656 . ?
O Ti C1 104.69(12) . . ?
O Ti N 155.98(9) 5_656 . ?
O Ti N 91.35(11) . . ?
C1 Ti N 99.33(14) . . ?
O Ti N 91.35(11) 5_656 6 ?
O Ti N 155.98(9) . 6 ?
C1 Ti N 99.33(14) . 6 ?
N Ti N 84.54(16) . 6 ?
O Ti Ti 41.42(8) 5_656 5_656 ?
O Ti Ti 41.41(8) . 5_656 ?
C1 Ti Ti 109.76(16) . 5_656 ?
N Ti Ti 128.66(8) . 5_656 ?
N Ti Ti 128.66(8) 6 5_656 ?
Ti O Ti 97.17(16) 5_656 . ?
C2 N C11 114.8(3) . . ?
C2 N Ti 120.9(2) . . ?
C11 N Ti 123.4(2) . . ?
N C2 C3 123.7(4) . . ?
N C2 C4 120.6(3) . . ?
C3 C2 C4 115.7(3) . . ?
C2 C3 C2 127.9(5) 6 . ?
C12 C11 C16 121.1(3) . . ?
C12 C11 N 120.5(3) . . ?
C16 C11 N 118.3(3) . . ?
C13 C12 C11 118.2(4) . . ?
C13 C12 C17 119.0(3) . . ?
C11 C12 C17 122.9(3) . . ?
C14 C13 C12 121.5(4) . . ?
C13 C14 C15 119.9(4) . . ?
C14 C15 C16 121.0(4) . . ?
C15 C16 C11 118.3(4) . . ?
C15 C16 C20 119.5(4) . . ?
C11 C16 C20 122.1(3) . . ?
C12 C17 C19 110.4(3) . . ?
C12 C17 C18 112.5(3) . . ?
C19 C17 C18 109.8(3) . . ?
C21 C20 C16 110.6(4) . . ?
C21 C20 C22 110.0(4) . . ?
C16 C20 C22 113.2(4) . . ?
C92 C91 C96 120.0 . . ?
C92 C91 C97 111.7(14) . . ?
C96 C91 C97 127.9(14) . . ?
C93 C92 C91 120.0 . . ?
C92 C93 C94 120.0 . . ?
C95 C94 C93 120.0 . . ?
C96 C95 C94 120.0 . . ?
C95 C96 C91 120.0 . . ?
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 1.843(2) 5_656 ?
Ti O 1.843(2) . ?
Ti C1 2.092(5) . ?
Ti N 2.149(3) . ?
Ti N 2.149(3) 6 ?
Ti Ti 2.7643(18) 5_656 ?
O Ti 1.843(2) 5_656 ?
N C2 1.339(5) . ?
N C11 1.455(5) . ?
C2 C3 1.391(4) . ?
C2 C4 1.512(5) . ?
C3 C2 1.391(4) 6 ?
C11 C12 1.399(5) . ?
C11 C16 1.415(5) . ?
C12 C13 1.397(5) . ?
C12 C17 1.511(5) . ?
C13 C14 1.376(6) . ?
C14 C15 1.386(6) . ?
C15 C16 1.391(5) . ?
C16 C20 1.511(6) . ?
C17 C19 1.519(6) . ?
C17 C18 1.539(5) . ?
C20 C21 1.502(8) . ?
C20 C22 1.514(7) . ?
C91 C92 1.3900 . ?
C91 C96 1.3900 . ?
C91 C97 1.59(2) . ?
C92 C93 1.3900 . ?
C93 C94 1.3900 . ?
C94 C95 1.3900 . ?
C95 C96 1.3900 . ?
