#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:21:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179839 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/35/7013561.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_7013561
loop_
_publ_author_name
'Boyle, Timothy J.'
'Rodriguez, Mark A.'
'Alam, Todd M.'
_publ_section_title
;
 4,6-Dihydroxypyrimidine: a selective bridging ligand for controlled
 Group IV metal alkoxide structures
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4598
_journal_paper_doi               10.1039/b310087a
_journal_year                    2003
_chemical_formula_sum            'C44 H86 N4 O16 Ti4'
_chemical_formula_weight         1118.77
_chemical_name_common            Ti4(DHP)2(u-OPri)4(OPri)8
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.721(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.361(3)
_cell_length_b                   9.3285(18)
_cell_length_c                   21.262(4)
_cell_measurement_temperature    168(2)
_cell_volume                     3107.9(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '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  0.1168
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19025
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9351
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS ver 2.03, Sheldrick (1999).'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          .123
_exptl_crystal_size_mid          .075
_exptl_crystal_size_min          .033
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4489
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.423
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1794P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.2750
_reflns_number_gt                2544
_reflns_number_total             4489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310087a.txt
_cod_data_source_block           tjb149s
_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      P2(1)/n
_cod_database_code               7013561
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.20673(8) 0.80247(15) 1.02730(7) 0.0317(5) Uani 1 1 d . . .
Ti2 Ti 0.16510(9) 1.02978(16) 0.90804(7) 0.0333(5) Uani 1 1 d . . .
N1 N 0.0845(4) 0.8591(7) 1.0488(3) 0.0305(15) Uani 1 1 d . . .
N2 N 0.0426(4) 1.0840(6) 0.9285(3) 0.0299(15) Uani 1 1 d . . .
O1 O 0.2206(3) 1.0046(5) 1.0088(2) 0.0312(13) Uani 1 1 d . . .
O2 O 0.1473(3) 0.8293(5) 0.9272(2) 0.0299(12) Uani 1 1 d . . .
O3 O 0.1175(3) 0.6436(5) 1.0222(3) 0.0365(14) Uani 1 1 d . . .
O4 O 0.2536(3) 0.7936(6) 1.1139(2) 0.0405(14) Uani 1 1 d . . .
O5 O 0.2882(3) 0.7046(6) 1.0053(3) 0.0417(14) Uani 1 1 d . . .
O6 O 0.1454(3) 1.2378(5) 0.9316(2) 0.0357(13) Uani 1 1 d . . .
O7 O 0.1089(3) 1.0445(6) 0.8227(2) 0.0428(14) Uani 1 1 d . . .
O8 O 0.2709(3) 1.0521(6) 0.8999(3) 0.0433(15) Uani 1 1 d . . .
C1 C 0.0330(5) 0.9524(9) 1.0659(3) 0.0303(19) Uani 1 1 d . . .
C2 C 0.0587(5) 0.7188(8) 1.0365(4) 0.035(2) Uani 1 1 d . . .
C3 C 0.0708(5) 1.2230(8) 0.9402(4) 0.0328(19) Uani 1 1 d . . .
C4 C 0.0200(5) 1.3251(8) 0.9593(4) 0.0344(19) Uani 1 1 d . . .
H4 H 0.0390 1.4210 0.9691 0.041 Uiso 1 1 calc R . .
C5 C 0.2776(5) 1.1101(9) 1.0480(4) 0.041(2) Uani 1 1 d . . .
H5 H 0.2781 1.1940 1.0188 0.049 Uiso 1 1 calc R . .
C6 C 0.2426(6) 1.1627(9) 1.1027(4) 0.049(2) Uani 1 1 d . . .
H6A H 0.1904 1.2182 1.0838 0.074 Uiso 1 1 calc R . .
H6B H 0.2852 1.2236 1.1328 0.074 Uiso 1 1 calc R . .
H6C H 0.2296 1.0803 1.1268 0.074 Uiso 1 1 calc R . .
C7 C 0.3673(5) 1.0537(10) 1.0708(5) 0.058(3) Uani 1 1 d . . .
H7A H 0.3708 0.9788 1.1038 0.087 Uiso 1 1 calc R . .
H7B H 0.4064 1.1319 1.0902 0.087 Uiso 1 1 calc R . .
H7C H 0.3831 1.0134 1.0334 0.087 Uiso 1 1 calc R . .
C8 C 0.1278(6) 0.7015(10) 0.8855(4) 0.047(2) Uani 1 1 d . . .
H8 H 0.1438 0.6144 0.9138 0.057 Uiso 1 1 calc R . .
C9 C 0.0326(6) 0.6986(10) 0.8521(5) 0.066(3) Uani 1 1 d . . .
H9A H 0.0020 0.6923 0.8854 0.098 Uiso 1 1 calc R . .
H9B H 0.0186 0.6153 0.8229 0.098 Uiso 1 1 calc R . .
H9C H 0.0158 0.7865 0.8264 0.098 Uiso 1 1 calc R . .
C10 C 0.1816(8) 0.7060(11) 0.8373(5) 0.079(3) Uani 1 1 d . . .
H10A H 0.1596 0.7809 0.8045 0.118 Uiso 1 1 calc R . .
H10B H 0.1784 0.6130 0.8153 0.118 Uiso 1 1 calc R . .
H10C H 0.2411 0.7270 0.8613 0.118 Uiso 1 1 calc R . .
C11 C 0.2515(8) 0.7718(14) 1.1798(5) 0.079(4) Uani 1 1 d . . .
H11 H 0.2077 0.8381 1.1882 0.095 Uiso 1 1 calc R . .
C12 C 0.3379(7) 0.8139(15) 1.2257(5) 0.094(4) Uani 1 1 d . . .
H12A H 0.3816 0.7480 1.2196 0.140 Uiso 1 1 calc R . .
H12B H 0.3359 0.8091 1.2712 0.140 Uiso 1 1 calc R . .
H12C H 0.3518 0.9119 1.2157 0.140 Uiso 1 1 calc R . .
C13 C 0.2267(14) 0.629(2) 1.1890(7) 0.235(14) Uani 1 1 d . . .
H13A H 0.1785 0.6007 1.1517 0.353 Uiso 1 1 calc R . .
H13B H 0.2099 0.6232 1.2296 0.353 Uiso 1 1 calc R . .
H13C H 0.2748 0.5638 1.1921 0.353 Uiso 1 1 calc R . .
C14 C 0.3653(7) 0.6265(11) 1.0309(6) 0.076(3) Uani 1 1 d . . .
H14 H 0.3893 0.6562 1.0778 0.091 Uiso 1 1 calc R . .
C15 C 0.3427(9) 0.4749(13) 1.0313(8) 0.130(6) Uani 1 1 d . . .
H15A H 0.2995 0.4629 1.0546 0.196 Uiso 1 1 calc R . .
H15B H 0.3937 0.4193 1.0535 0.196 Uiso 1 1 calc R . .
H15C H 0.3199 0.4408 0.9860 0.196 Uiso 1 1 calc R . .
C16 C 0.4263(9) 0.6698(16) 0.9971(11) 0.186(9) Uani 1 1 d . . .
H16A H 0.4063 0.6389 0.9512 0.279 Uiso 1 1 calc R . .
H16B H 0.4817 0.6254 1.0183 0.279 Uiso 1 1 calc R . .
H16C H 0.4323 0.7743 0.9990 0.279 Uiso 1 1 calc R . .
C17 C 0.0370(12) 1.1007(14) 0.7674(5) 0.134(7) Uani 1 1 d D . .
C18 C 0.0343(16) 1.000(2) 0.7097(10) 0.080(7) Uiso 0.50 1 d PD . .
C18' C 0.0831(19) 1.092(4) 0.7108(13) 0.118(10) Uiso 0.50 1 d PD . .
C19 C 0.0640(19) 1.263(2) 0.7690(13) 0.094(9) Uiso 0.50 1 d PD . .
C19' C 0.019(2) 1.260(2) 0.7734(14) 0.099(9) Uiso 0.50 1 d PD . .
C20 C 0.3097(7) 1.0994(13) 0.8518(6) 0.074(3) Uani 1 1 d . . .
H20 H 0.2710 1.0692 0.8082 0.089 Uiso 1 1 calc R . .
C21 C 0.3125(11) 1.2560(17) 0.8511(7) 0.137(6) Uani 1 1 d . . .
H21A H 0.2547 1.2942 0.8440 0.206 Uiso 1 1 calc R . .
H21B H 0.3351 1.2881 0.8155 0.206 Uiso 1 1 calc R . .
H21C H 0.3494 1.2907 0.8932 0.206 Uiso 1 1 calc R . .
C22 C 0.3898(10) 1.021(2) 0.8609(8) 0.157(8) Uani 1 1 d . . .
H22A H 0.4320 1.0550 0.9008 0.235 Uiso 1 1 calc R . .
H22B H 0.4111 1.0365 0.8229 0.235 Uiso 1 1 calc R . .
H22C H 0.3797 0.9181 0.8653 0.235 Uiso 1 1 calc R . .
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 Ti1 O5 96.6(2) . . ?
O4 Ti1 O1 102.3(2) . . ?
O5 Ti1 O1 107.6(2) . . ?
O4 Ti1 O3 96.2(2) . . ?
O5 Ti1 O3 100.9(2) . . ?
O1 Ti1 O3 143.6(2) . . ?
O4 Ti1 O2 175.1(2) . . ?
O5 Ti1 O2 87.6(2) . . ?
O1 Ti1 O2 74.08(19) . . ?
O3 Ti1 O2 85.3(2) . . ?
O4 Ti1 N1 86.8(2) . . ?
O5 Ti1 N1 162.2(2) . . ?
O1 Ti1 N1 88.6(2) . . ?
O3 Ti1 N1 61.3(2) . . ?
O2 Ti1 N1 89.9(2) . . ?
O4 Ti1 C2 92.3(2) . . ?
O5 Ti1 C2 130.3(2) . . ?
O1 Ti1 C2 117.9(2) . . ?
O3 Ti1 C2 29.4(2) . . ?
O2 Ti1 C2 86.7(2) . . ?
N1 Ti1 C2 31.9(2) . . ?
O4 Ti1 Ti2 140.72(19) . . ?
O5 Ti1 Ti2 97.76(19) . . ?
O1 Ti1 Ti2 38.47(14) . . ?
O3 Ti1 Ti2 116.46(15) . . ?
O2 Ti1 Ti2 35.64(14) . . ?
N1 Ti1 Ti2 90.39(16) . . ?
C2 Ti1 Ti2 105.41(16) . . ?
O7 Ti2 O8 97.0(2) . . ?
O7 Ti2 O2 102.8(2) . . ?
O8 Ti2 O2 109.7(2) . . ?
O7 Ti2 O6 96.0(2) . . ?
O8 Ti2 O6 97.9(2) . . ?
O2 Ti2 O6 144.1(2) . . ?
O7 Ti2 O1 174.8(2) . . ?
O8 Ti2 O1 88.0(2) . . ?
O2 Ti2 O1 74.01(19) . . ?
O6 Ti2 O1 84.7(2) . . ?
O7 Ti2 N2 87.2(2) . . ?
O8 Ti2 N2 159.4(3) . . ?
O2 Ti2 N2 88.8(2) . . ?
O6 Ti2 N2 61.6(2) . . ?
O1 Ti2 N2 88.6(2) . . ?
O7 Ti2 C3 92.5(2) . . ?
O8 Ti2 C3 127.4(3) . . ?
O2 Ti2 C3 118.4(2) . . ?
O6 Ti2 C3 29.5(2) . . ?
O1 Ti2 C3 85.6(2) . . ?
N2 Ti2 C3 32.1(2) . . ?
O7 Ti2 Ti1 141.19(19) . . ?
O8 Ti2 Ti1 99.23(19) . . ?
O2 Ti2 Ti1 38.44(14) . . ?
O6 Ti2 Ti1 116.26(15) . . ?
O1 Ti2 Ti1 35.61(14) . . ?
N2 Ti2 Ti1 89.67(16) . . ?
C3 Ti2 Ti1 104.91(17) . . ?
C1 N1 C2 119.3(7) . . ?
C1 N1 Ti1 151.8(5) . . ?
C2 N1 Ti1 88.9(5) . . ?
C1 N2 C3 120.0(7) 3_577 . ?
C1 N2 Ti2 151.4(5) 3_577 . ?
C3 N2 Ti2 88.6(4) . . ?
C5 O1 Ti1 129.5(5) . . ?
C5 O1 Ti2 122.2(5) . . ?
Ti1 O1 Ti2 105.9(2) . . ?
C8 O2 Ti2 132.2(5) . . ?
C8 O2 Ti1 118.5(5) . . ?
Ti2 O2 Ti1 105.9(2) . . ?
C2 O3 Ti1 99.3(5) . . ?
C11 O4 Ti1 153.9(6) . . ?
C14 O5 Ti1 144.0(6) . . ?
C3 O6 Ti2 98.9(4) . . ?
C17 O7 Ti2 151.8(6) . . ?
C20 O8 Ti2 138.3(6) . . ?
N2 C1 N1 122.6(7) 3_577 . ?
O3 C2 N1 110.5(7) . . ?
O3 C2 C4 128.7(7) . 3_577 ?
N1 C2 C4 120.8(7) . 3_577 ?
O3 C2 Ti1 51.3(4) . . ?
N1 C2 Ti1 59.3(4) . . ?
C4 C2 Ti1 179.3(6) 3_577 . ?
O6 C3 N2 110.9(7) . . ?
O6 C3 C4 129.3(7) . . ?
N2 C3 C4 119.8(7) . . ?
O6 C3 Ti2 51.6(4) . . ?
N2 C3 Ti2 59.3(4) . . ?
C4 C3 Ti2 178.3(6) . . ?
C2 C4 C3 117.4(7) 3_577 . ?
O1 C5 C7 110.9(7) . . ?
O1 C5 C6 109.8(6) . . ?
C7 C5 C6 114.5(7) . . ?
O2 C8 C9 108.3(7) . . ?
O2 C8 C10 108.4(7) . . ?
C9 C8 C10 113.4(9) . . ?
O4 C11 C13 110.9(11) . . ?
O4 C11 C12 108.2(9) . . ?
C13 C11 C12 113.7(11) . . ?
O5 C14 C15 107.5(9) . . ?
O5 C14 C16 109.3(10) . . ?
C15 C14 C16 119.0(11) . . ?
O7 C17 C18 104.5(12) . . ?
O7 C17 C19' 113.7(14) . . ?
C18 C17 C19' 134.4(16) . . ?
O7 C17 C19 99.7(15) . . ?
C18 C17 C19 123.2(17) . . ?
C19' C17 C19 28.8(14) . . ?
O7 C17 C18' 98.1(16) . . ?
C18 C17 C18' 43.8(13) . . ?
C19' C17 C18' 105(2) . . ?
C19 C17 C18' 82.7(19) . . ?
O8 C20 C21 109.9(9) . . ?
O8 C20 C22 108.4(10) . . ?
C21 C20 C22 118.2(12) . . ?
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
Ti1 O4 1.782(5) . ?
Ti1 O5 1.785(5) . ?
Ti1 O1 1.952(5) . ?
Ti1 O3 2.061(5) . ?
Ti1 O2 2.084(5) . ?
Ti1 N1 2.240(6) . ?
Ti1 C2 2.606(8) . ?
Ti1 Ti2 3.224(2) . ?
Ti2 O7 1.788(5) . ?
Ti2 O8 1.802(5) . ?
Ti2 O2 1.954(5) . ?
Ti2 O6 2.053(5) . ?
Ti2 O1 2.086(5) . ?
Ti2 N2 2.228(6) . ?
Ti2 C3 2.589(8) . ?
N1 C1 1.332(9) . ?
N1 C2 1.377(10) . ?
N2 C1 1.321(9) 3_577 ?
N2 C3 1.375(9) . ?
O1 C5 1.445(9) . ?
O2 C8 1.466(9) . ?
O3 C2 1.296(9) . ?
O4 C11 1.425(11) . ?
O5 C14 1.423(11) . ?
O6 C3 1.292(9) . ?
O7 C17 1.498(14) . ?
O8 C20 1.419(10) . ?
C1 N2 1.321(9) 3_577 ?
C2 C4 1.378(11) 3_577 ?
C3 C4 1.399(10) . ?
C4 C2 1.378(11) 3_577 ?
C5 C7 1.502(11) . ?
C5 C6 1.518(11) . ?
C8 C9 1.514(12) . ?
C8 C10 1.532(12) . ?
C11 C13 1.425(19) . ?
C11 C12 1.519(14) . ?
C14 C15 1.463(15) . ?
C14 C16 1.444(18) . ?
C17 C18 1.533(16) . ?
C17 C19' 1.533(18) . ?
C17 C19 1.578(17) . ?
C17 C18' 1.594(18) . ?
C20 C21 1.462(17) . ?
C20 C22 1.465(17) . ?
