#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:51:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179158 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/19/4311930.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_4311930
loop_
_publ_author_name
'Aaron G. Maestri'
'Seth N. Brown'
_publ_section_title
;
 Titanatranes Derailed: Static and Dynamic Triethanolamine Slippage
 Induced by Polyphenoxide Chelation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6995
_journal_page_last               7004
_journal_paper_doi               10.1021/ic0492901
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         (2-Ph2CH-4,6-tert-Bu2-C6H2O)Ti[(OCH2CH2)3N]
_chemical_formula_sum            'C33 H43 N O4 Ti'
_chemical_formula_weight         565.58
_chemical_name_common
2-(Diphenylmethyl)-4,6-tert-butylphenoxytitanatrane
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.9430(10)
_cell_angle_beta                 102.2840(10)
_cell_angle_gamma                104.3430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4044(7)
_cell_length_b                   10.5516(7)
_cell_length_c                   14.9791(10)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.058
_cell_measurement_theta_min      2.352
_cell_volume                     1552.56(18)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measurement_device       'Bruker SMART APEX'
_diffrn_measurement_method       '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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9696
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.862107
_exptl_absorpt_correction_T_min  0.797962
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       irregular
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0794P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1390
_refine_ls_wR_factor_obs         0.1270
_reflns_number_observed          5252
_reflns_number_total             6831
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0492901si20040531_034943_1.cif
_cod_data_source_block           mono
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1552.6(2)
_cod_database_code               4311930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti Ti 0.94853(4) 0.72508(3) 0.56376(2) 0.02253(12) Uani 1 d . .
O4 O 0.99383(15) 0.72268(14) 0.68807(9) 0.0261(3) Uani 1 d . .
O1 O 0.8388(2) 0.55788(14) 0.53158(10) 0.0312(4) Uani 1 d . .
O2 O 0.8694(2) 0.86235(14) 0.54744(10) 0.0287(3) Uani 1 d . .
O3 O 1.1147(2) 0.75898(15) 0.53283(10) 0.0300(4) Uani 1 d . .
N N 0.8892(2) 0.7233(2) 0.40931(12) 0.0290(4) Uani 1 d . .
C1 C 0.7681(3) 0.5091(2) 0.4405(2) 0.0361(6) Uani 1 d . .
C2 C 0.8433(3) 0.5848(2) 0.3742(2) 0.0451(7) Uani 1 d . .
C3 C 0.8108(3) 0.9020(2) 0.4618(2) 0.0346(5) Uani 1 d . .
C4 C 0.7782(3) 0.7907(3) 0.3904(2) 0.0432(6) Uani 1 d . .
C5 C 1.1347(3) 0.7639(3) 0.4420(2) 0.0362(6) Uani 1 d . .
C6 C 1.0126(3) 0.7980(3) 0.3805(2) 0.0418(6) Uani 1 d . .
C7 C 0.7430(2) 0.6159(2) 0.7321(2) 0.0306(5) Uani 1 d . .
C10 C 0.9953(2) 0.7254(2) 0.77900(13) 0.0224(4) Uani 1 d . .
C11 C 1.1167(2) 0.7784(2) 0.84505(13) 0.0236(4) Uani 1 d . .
C12 C 1.1069(2) 0.7827(2) 0.93613(15) 0.0276(5) Uani 1 d . .
C13 C 0.9866(2) 0.7366(2) 0.96489(14) 0.0295(5) Uani 1 d . .
C14 C 0.8713(2) 0.6805(2) 0.8977(2) 0.0301(5) Uani 1 d . .
C15 C 0.8718(2) 0.6730(2) 0.80545(14) 0.0266(5) Uani 1 d . .
C20 C 0.6421(2) 0.5080(2) 0.7668(2) 0.0323(5) Uani 1 d . .
C21 C 0.5514(3) 0.5358(3) 0.8149(2) 0.0378(6) Uani 1 d . .
C22 C 0.4670(3) 0.4369(3) 0.8514(2) 0.0439(6) Uani 1 d . .
C23 C 0.4705(3) 0.3085(3) 0.8392(2) 0.0513(7) Uani 1 d . .
C24 C 0.5566(3) 0.2791(3) 0.7893(3) 0.0610(9) Uani 1 d . .
C25 C 0.6421(3) 0.3778(3) 0.7531(2) 0.0484(7) Uani 1 d . .
C30 C 0.6761(2) 0.7192(3) 0.6890(2) 0.0355(6) Uani 1 d . .
C31 C 0.6997(3) 0.8426(3) 0.7304(2) 0.0458(7) Uani 1 d . .
C32 C 0.6326(4) 0.9339(4) 0.6899(2) 0.0624(9) Uani 1 d . .
C33 C 0.5414(3) 0.9006(4) 0.6071(3) 0.0662(10) Uani 1 d . .
C34 C 0.5178(3) 0.7792(4) 0.5642(2) 0.0645(10) Uani 1 d . .
C35 C 0.5848(3) 0.6890(3) 0.6039(2) 0.0489(7) Uani 1 d . .
C110 C 1.2539(2) 0.8289(2) 0.81828(14) 0.0283(5) Uani 1 d . .
C111 C 1.2858(3) 0.7193(3) 0.7655(2) 0.0358(6) Uani 1 d . .
C112 C 1.2499(3) 0.9457(3) 0.7589(2) 0.0374(6) Uani 1 d . .
C113 C 1.3723(3) 0.8768(4) 0.9020(2) 0.0471(7) Uani 1 d . .
C130 C 0.9791(3) 0.7441(3) 1.06589(15) 0.0374(6) Uani 1 d . .
C131 C 1.1076(5) 0.8326(6) 1.1251(2) 0.136(2) Uani 1 d . .
H31A H 1.1234(5) 0.9204(6) 1.1024(2) 0.204 Uiso 1 calc R .
H31B H 1.1851(5) 0.7965(6) 1.1228(2) 0.204 Uiso 1 calc R .
H31C H 1.0974(5) 0.8380(6) 1.1885(2) 0.204 Uiso 1 calc R .
C132 C 0.8628(5) 0.8014(5) 1.0766(2) 0.0964(15) Uani 1 d . .
H32C H 0.8776(5) 0.8898(5) 1.0549(2) 0.145 Uiso 1 calc R .
H32B H 0.8588(5) 0.8057(5) 1.1413(2) 0.145 Uiso 1 calc R .
H32A H 0.7770(5) 0.7456(5) 1.0404(2) 0.145 Uiso 1 calc R .
C133 C 0.9539(7) 0.6106(4) 1.0993(2) 0.123(2) Uani 1 d . .
H33C H 1.0281(7) 0.5717(4) 1.0930(2) 0.184 Uiso 1 calc R .
H33B H 0.8675(7) 0.5559(4) 1.0631(2) 0.184 Uiso 1 calc R .
H33A H 0.9494(7) 0.6161(4) 1.1639(2) 0.184 Uiso 1 calc R .
H1A H 0.7559(25) 0.4171(23) 0.4328(15) 0.031(6) Uiso 1 d . .
H1B H 0.6789(34) 0.5288(29) 0.4302(20) 0.062(9) Uiso 1 d . .
H2A H 0.7903(30) 0.5747(26) 0.3144(19) 0.048(8) Uiso 1 d . .
H2B H 0.9453(36) 0.5663(30) 0.3718(21) 0.073(10) Uiso 1 d . .
H3A H 0.7321(32) 0.9369(27) 0.4674(19) 0.055(8) Uiso 1 d . .
H3B H 0.8717(28) 0.9818(25) 0.4463(17) 0.039(7) Uiso 1 d . .
H4A H 0.7802(30) 0.8230(27) 0.3238(19) 0.056(8) Uiso 1 d . .
H4B H 0.6848(29) 0.7188(26) 0.3976(17) 0.046(7) Uiso 1 d . .
H5A H 1.1421(24) 0.6785(23) 0.4222(16) 0.031(6) Uiso 1 d . .
H5B H 1.2148(29) 0.8288(25) 0.4408(17) 0.040(7) Uiso 1 d . .
H6A H 1.0152(30) 0.9037(28) 0.3885(19) 0.058(8) Uiso 1 d . .
H6B H 1.0095(24) 0.7732(22) 0.3159(16) 0.032(6) Uiso 1 d . .
H7 H 0.7673(23) 0.5732(21) 0.6886(15) 0.024(6) Uiso 1 d . .
H12 H 1.1798(28) 0.8128(24) 0.9768(17) 0.038(7) Uiso 1 d . .
H14 H 0.7949(27) 0.6499(23) 0.9116(16) 0.030(6) Uiso 1 d . .
H21 H 0.5496(28) 0.6171(26) 0.8251(17) 0.041(7) Uiso 1 d . .
H22 H 0.4094(33) 0.4593(27) 0.8863(20) 0.059(9) Uiso 1 d . .
H23 H 0.4081(32) 0.2368(29) 0.8635(20) 0.061(9) Uiso 1 d . .
H24 H 0.5620(37) 0.1961(34) 0.7812(23) 0.082(11) Uiso 1 d . .
H25 H 0.6995(31) 0.3618(27) 0.7135(19) 0.054(8) Uiso 1 d . .
H31 H 0.7540(31) 0.8697(27) 0.7830(20) 0.050(8) Uiso 1 d . .
H32 H 0.6548(37) 1.0283(34) 0.7190(23) 0.080(11) Uiso 1 d . .
H33 H 0.4896(37) 0.9596(33) 0.5784(22) 0.075(10) Uiso 1 d . .
H34 H 0.4527(35) 0.7546(29) 0.5122(22) 0.063(9) Uiso 1 d . .
H35 H 0.5684(28) 0.6046(26) 0.5777(18) 0.041(8) Uiso 1 d . .
H11A H 1.2221(33) 0.6910(28) 0.7135(21) 0.057(9) Uiso 1 d . .
H11B H 1.3738(28) 0.7483(23) 0.7513(16) 0.033(6) Uiso 1 d . .
H11C H 1.2916(28) 0.6528(26) 0.8003(18) 0.041(7) Uiso 1 d . .
H12A H 1.1831(30) 0.9289(25) 0.7034(19) 0.045(8) Uiso 1 d . .
H12B H 1.2331(28) 1.0180(26) 0.7927(18) 0.046(8) Uiso 1 d . .
H12C H 1.3400(34) 0.9844(28) 0.7431(20) 0.063(9) Uiso 1 d . .
H13A H 1.3801(30) 0.8131(28) 0.9396(20) 0.050(9) Uiso 1 d . .
H13B H 1.3589(28) 0.9503(26) 0.9389(19) 0.045(8) Uiso 1 d . .
H13C H 1.4553(33) 0.9072(28) 0.8790(20) 0.060(9) Uiso 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'
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
O4 Ti O2 102.95(7) . . ?
O4 Ti O3 102.72(7) . . ?
O2 Ti O3 113.08(7) . . ?
O4 Ti O1 100.96(7) . . ?
O2 Ti O1 118.10(7) . . ?
O3 Ti O1 115.79(7) . . ?
O4 Ti N 178.68(7) . . ?
O2 Ti N 77.69(7) . . ?
O3 Ti N 78.00(7) . . ?
O1 Ti N 77.73(6) . . ?
C10 O4 Ti 165.36(14) . . ?
C1 O1 Ti 124.59(14) . . ?
C3 O2 Ti 125.42(14) . . ?
C5 O3 Ti 125.05(15) . . ?
C2 N C4 112.4(2) . . ?
C2 N C6 113.9(2) . . ?
C4 N C6 112.0(2) . . ?
C2 N Ti 106.64(13) . . ?
C4 N Ti 105.23(14) . . ?
C6 N Ti 105.93(14) . . ?
O1 C1 C2 108.8(2) . . ?
N C2 C1 107.6(2) . . ?
O2 C3 C4 109.1(2) . . ?
N C4 C3 108.2(2) . . ?
O3 C5 C6 108.5(2) . . ?
N C6 C5 107.1(2) . . ?
C30 C7 C15 113.2(2) . . ?
C30 C7 C20 111.5(2) . . ?
C15 C7 C20 112.2(2) . . ?
O4 C10 C11 121.1(2) . . ?
O4 C10 C15 118.0(2) . . ?
C11 C10 C15 120.9(2) . . ?
C12 C11 C10 116.9(2) . . ?
C12 C11 C110 121.2(2) . . ?
C10 C11 C110 121.9(2) . . ?
C13 C12 C11 124.0(2) . . ?
C14 C13 C12 116.8(2) . . ?
C14 C13 C130 120.5(2) . . ?
C12 C13 C130 122.7(2) . . ?
C13 C14 C15 122.9(2) . . ?
C14 C15 C10 118.3(2) . . ?
C14 C15 C7 122.2(2) . . ?
C10 C15 C7 119.4(2) . . ?
C25 C20 C21 117.8(2) . . ?
C25 C20 C7 120.2(2) . . ?
C21 C20 C7 122.0(2) . . ?
C20 C21 C22 121.0(3) . . ?
C23 C22 C21 120.4(3) . . ?
C24 C23 C22 119.1(3) . . ?
C23 C24 C25 120.7(3) . . ?
C20 C25 C24 120.8(3) . . ?
C31 C30 C35 117.6(3) . . ?
C31 C30 C7 123.0(2) . . ?
C35 C30 C7 119.4(2) . . ?
C30 C31 C32 121.4(3) . . ?
C33 C32 C31 119.8(4) . . ?
C34 C33 C32 119.9(3) . . ?
C33 C34 C35 120.4(3) . . ?
C34 C35 C30 120.9(3) . . ?
C111 C110 C11 110.1(2) . . ?
C111 C110 C113 107.5(2) . . ?
C11 C110 C113 112.4(2) . . ?
C111 C110 C112 109.8(2) . . ?
C11 C110 C112 110.0(2) . . ?
C113 C110 C112 107.0(2) . . ?
C133 C130 C132 108.2(3) . . ?
C133 C130 C131 110.1(3) . . ?
C132 C130 C131 106.7(3) . . ?
C133 C130 C13 109.8(2) . . ?
C132 C130 C13 110.0(2) . . ?
C131 C130 C13 111.9(2) . . ?
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 O4 1.8231(14) . y
Ti O2 1.8308(15) . y
Ti O3 1.837(2) . y
Ti O1 1.8406(15) . y
Ti N 2.263(2) . y
O4 C10 1.359(2) . ?
O1 C1 1.424(3) . ?
O2 C3 1.416(3) . ?
O3 C5 1.418(3) . ?
N C2 1.470(3) . ?
N C4 1.480(3) . ?
N C6 1.483(3) . ?
C1 C2 1.512(4) . ?
C3 C4 1.499(4) . ?
C5 C6 1.527(4) . ?
C7 C30 1.516(3) . ?
C7 C15 1.523(3) . ?
C7 C20 1.524(3) . ?
C10 C11 1.410(3) . ?
C10 C15 1.409(3) . ?
C11 C12 1.390(3) . ?
C11 C110 1.535(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.384(3) . ?
C13 C130 1.533(3) . ?
C14 C15 1.384(3) . ?
C20 C25 1.386(4) . ?
C20 C21 1.385(3) . ?
C21 C22 1.389(4) . ?
C22 C23 1.375(4) . ?
C23 C24 1.368(4) . ?
C24 C25 1.391(4) . ?
C30 C31 1.375(4) . ?
C30 C35 1.396(3) . ?
C31 C32 1.398(4) . ?
C32 C33 1.371(5) . ?
C33 C34 1.365(5) . ?
C34 C35 1.385(4) . ?
C110 C111 1.531(3) . ?
C110 C113 1.536(3) . ?
C110 C112 1.536(3) . ?
C130 C133 1.483(4) . ?
C130 C132 1.515(4) . ?
C130 C131 1.515(4) . ?
