#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:11:03 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243923 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702611.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_7702611
loop_
_publ_author_name
'Weymann-Schildknetch, Sandrine'
'Henry, Marc'
_publ_section_title
;
 Mechanistic aspects of the hydrolysis and condensation of titanium
 alkoxides complexed by tripodal ligands†
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2425
_journal_paper_doi               10.1039/b103398k
_journal_year                    2001
_chemical_formula_moiety         C28H62N2O20Ti4
_chemical_formula_sum            'C28 H62 N2 O20 Ti4'
_chemical_formula_weight         938.4
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 102.44(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.351(5)
_cell_length_b                   13.158(4)
_cell_length_c                   13.182(5)
_cell_measurement_temperature    173
_cell_volume                     2261.3(14)
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Philips PW1100/16'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_theta_max         52
_diffrn_reflns_theta_min         3
_exptl_absorpt_coefficient_mu    68.101
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.17
_refine_diff_density_min         0.82
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.439
_refine_ls_hydrogen_treatment    included_not_refined
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6263
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.048
_refine_ls_shift/esd_max         0.08
_refine_ls_shift/esd_mean        0.03
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo²/(σ²(Fo²) + 0.0064 Fo⁴)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.070
_reflns_number_observed          1763
_reflns_number_total             2634
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            b103398k.txt
_cod_data_source_block           ST854
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) +
0.0064 Fo^4^)' was changed to 'calc'. A new data item
'_refine_ls_weighting_details' was created with the value set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4287(1)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        C28H62N2O20Ti4
_cod_database_code               7702611
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
-x,y,1/2-z
1/2+x,1/2+y,z
x,-y,1/2+z
1/2-x,1/2-y,-z
loop_
_atom_site_label
_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_type_symbol
TI1 0.60998(6) 0.27999(9) 0.53987(6) 4.95(3) Biso Ti
TI2 0.73303(5) 0.11918(8) 0.49251(5) 4.23(2) Biso Ti
O1 0.5180(2) 0.3036(4) 0.4851(2) 7.2(1) Biso O
C1 0.4547(4) 0.3605(7) 0.4693(5) 9.8(3) Biso C
C2 0.4101(4) 0.3603(7) 0.5263(5) 11.5(3) Biso C
O2 0.5911(2) 0.1729(3) 0.5945(2) 5.9(1) Biso O
C3 0.5385(4) 0.0951(6) 0.5764(5) 9.3(2) Biso C
C4 0.5097(5) 0.0602(9) 0.6394(6) 16.2(3) Biso C
O3 0.6217(2) 0.3732(3) 0.6135(2) 6.7(1) Biso O
C5 0.6043(6) 0.3962(9) 0.6808(5) 14.5(3) Biso C
C6 0.6000(9) 0.359(1) 0.7317(6) 24.2(6) Biso C
O4 0.6325(2) 0.1750(3) 0.4577(2) 4.12(8) Biso O
C7 0.6052(3) 0.1915(5) 0.3804(3) 5.2(2) Biso C
C8 0.6443(3) 0.2809(5) 0.3522(3) 5.1(1) Biso C
C9 0.7278(3) 0.2626(4) 0.3579(3) 4.4(1) Biso C
O5 0.7669(2) 0.2508(2) 0.4341(2) 3.80(8) Biso O
N1 0.6125(3) 0.2975(5) 0.2694(3) 7.4(2) Biso N
O6 0.5592(6) 0.3640(8) 0.2512(6) 10.1(3) Biso O
O7 0.5926(5) 0.2255(5) 0.2337(3) 15.0(3) Biso O
O6' 0.3609(5) 0.3467(8) 0.2701(4) 9.0(3) Biso O
C10 0.6275(3) 0.3783(5) 0.3897(3) 5.5(2) Biso C
O8 0.6579(2) 0.3752(3) 0.4688(2) 4.61(9) Biso O
O9 0.7175(2) 0.0325(3) 0.5619(2) 5.8(1) Biso O
C11 0.7085(6) -0.0522(8) 0.5979(8) 23.2(4) Biso C
C12 0.7032(9) -0.1283(8) 0.600(1) 21.2(6) Biso C
O10 0.7299(2) 0.0396(3) 0.4140(2) 5.7(1) Biso O
C13 0.7363(6) -0.0404(8) 0.3684(6) 16.1(3) Biso C
C14 0.6950(7) -0.0951(9) 0.3292(7) 19.3(4) Biso C
H1 0.4244 0.3354 0.4237 12 Biso H
H2 0.4686 0.4287 0.4622 12 Biso H
H3 0.3673 0.4019 0.5101 14 Biso H
H4 0.3947 0.2928 0.5338 14 Biso H
H5 0.4389 0.3860 0.5722 14 Biso H
H6 0.5613 0.0392 0.5570 12 Biso H
H7 0.4980 0.1194 0.5387 12 Biso H
H8 0.4743 0.0075 0.6235 21 Biso H
H9 0.5494 0.0349 0.6773 21 Biso H
H10 0.4861 0.1150 0.6591 21 Biso H
H11 0.5559 0.4247 0.6650 18 Biso H
H12 0.6391 0.4486 0.6989 18 Biso H
H13 0.5855 0.4067 0.7649 31 Biso H
H14 0.5636 0.3065 0.7207 31 Biso H
H15 0.6469 0.3304 0.7546 31 Biso H
H16 0.5532 0.2053 0.3717 6 Biso H
H17 0.6132 0.1320 0.3536 6 Biso H
H18 0.7480 0.3189 0.3365 5 Biso H
H19 0.7339 0.2027 0.3307 5 Biso H
H20 0.5750 0.3869 0.3812 7 Biso H
H21 0.6487 0.4338 0.3683 7 Biso H
H22 0.6636 -0.0341 0.6127 30 Biso H
H23 0.7494 -0.0443 0.6394 30 Biso H
H24 0.6972 -0.1470 0.6492 27 Biso H
H25 0.6608 -0.1496 0.5639 27 Biso H
H26 0.7467 -0.1598 0.5906 27 Biso H
H27 0.7670 -0.0861 0.4017 20 Biso H
H28 0.7640 -0.0120 0.3348 20 Biso H
H29 0.7224 -0.1422 0.3063 25 Biso H
H30 0.6660 -0.1307 0.3582 25 Biso H
H31 0.6629 -0.0566 0.2912 25 Biso H
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 TI1 O2 99.9(2)
O5 TI2 O8 76.8(1)
O1 TI1 O3 104.1(2)
O5 TI2 O9 164.1(1)
O1 TI1 O4 91.4(1)
O5 TI2 O10 92.3(1)
O1 TI1 O5 159.0(1)
O5 TI2 O8 83.4(1)
O1 TI1 O8 91.3(1)
O5 TI2 O9 92.8(1)
O2 TI1 O3 97.4(2)
O5 TI2 O10 164.4(1)
O2 TI1 O4 88.2(1)
O8 TI2 O9 94.4(1)
O2 TI1 O5 92.7(1)
O8 TI2 O10 99.4(1)
O2 TI1 O8 162.3(1)
O9 TI2 O10 102.3(1)
O3 TI1 O4 162.2(1)
O1 C1 C2 115.8(6)
O3 TI1 O5 90.7(1)
O2 C3 C4 113.6(6)
O3 TI1 O8 93.0(1)
O3 C5 C6 139.(2)
O4 TI1 O5 72.17(9)
O4 C7 C8 111.4(3)
O4 TI1 O8 77.8(1)
C7 C8 C9 113.1(4)
O5 TI1 O8 72.8(1)
C7 C8 N1 109.8(4)
O4 TI2 O5 83.8(1)
C7 C8 C10 110.2(4)
O4 TI2 O5 77.2(1)
C9 C8 N1 104.9(4)
O4 TI2 O8 155.9(1)
C9 C8 C10 113.6(4)
O4 TI2 O9 100.8(1)
N1 C8 C10 104.8(4)
O4 TI2 O10 95.6(1)
C8 C9 O5 111.8(3)
O5 TI2 O5 73.3(1)
C8 N1 O6 117.3(6)
C8 N1 O7 116.6(6)
N1 O7 O6' 38.0(4)
C8 N1 O6' 125.4(6)
O6 O7 O6' 50.2(5)
O6 N1 O7 106.1(6)
N1 O6' O6 53.1(5)
O6 N1 O6' 81.9(8)
N1 O6' O7 38.4(4)
O7 N1 O6' 103.6(7)
O6 O6' O7 69.8(5)
N1 O6 O7 34.5(4)
C8 C10 O8 110.9(3)
N1 O6 O6' 45.0(5)
O9 C11 C12 152.(2)
O7 O6 O6' 60.0(5)
O10 C13 C14 136.(1)
N1 O7 O6 39.4(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
TI1 O1 1.792(3)
O4 C7 1.402(5)
TI1 O2 1.800(3)
C7 C8 1.525(6)
TI1 O3 1.794(3)
C8 C9 1.531(6)
TI1 O4 2.140(3)
C8 N1 1.508(6)
TI1 O5 2.243(3)
C8 C10 1.513(6)
TI1 O8 2.122(3)
C9 O5 1.424(5)
TI2 O4 1.960(3)
N1 O6 1.302(9)
TI2 O5 2.191(2)
N1 O7 1.161(7)
TI2 O5 2.170(3)
N1 O6' 1.151(7)
TI2 O8 1.974(3)
O6 O7 1.97(1)
TI2 O9 1.768(3)
O6 O6' 1.61(1)
TI2 O10 1.761(3)
O7 O6' 1.82(1)
O1 C1 1.359(6)
C10 O8 1.428(5)
C1 C2 1.454(9)
O9 C11 1.321(9)
O2 C3 1.397(7)
C11 C12 1.01(1)
C3 C4 1.438(9)
O10 C13 1.361(8)
O3 C5 1.362(8)
C13 C14 1.17(1)
C5 C6 1.07(1)
