#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:07:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179776 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007201.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_7007201
loop_
_publ_author_name
'Fandos, Rosa'
'Gallego, Beatriz'
'Otero, Antonio'
'Rodríguez, Ana'
'Ruiz, María José'
'Terreros, Pilar'
'Pastor, Cesar'
_publ_section_title
;
 A new titanium building block for early-late heterometallic complexes;
 preparation of a new tetrameric metallomacrocycle by self assembly.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2683
_journal_page_last               2690
_journal_paper_doi               10.1039/b601544a
_journal_year                    2006
_chemical_formula_moiety         'C34 H36 N2 O9 Ti2, H2 O'
_chemical_formula_sum            'C34 H38 N2 O10 Ti2'
_chemical_formula_weight         730.40
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.210(2)
_cell_length_b                   14.420(3)
_cell_length_c                   14.711(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3323.5(13)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2θ 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  0.0077
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4141
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.19
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.233
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0851P)²+1.7950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                3361
_reflns_number_total             3988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601544a.txt
_cod_data_source_block           3
_cod_original_cell_volume        3323.5(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7007201
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.41196(2) 0.31360(2) 0.28457(2) 0.03211(13) Uani 1 1 d . . .
O1 O 0.5000 0.36691(15) 0.2500 0.0486(5) Uani 1 2 d S . .
O2 O 0.40124(11) 0.21668(11) 0.18108(10) 0.0456(4) Uani 1 1 d . . .
O3 O 0.45919(11) 0.32744(11) 0.42510(11) 0.0490(4) Uani 1 1 d . . .
O4 O 0.37900(15) 0.07021(13) 0.13032(13) 0.0702(6) Uani 1 1 d . . .
O5 O 0.47735(18) 0.2725(2) 0.57160(13) 0.0880(8) Uani 1 1 d . . .
N1 N 0.40688(11) 0.17983(11) 0.34631(12) 0.0368(4) Uani 1 1 d . . .
C1 C 0.39086(13) 0.10484(15) 0.29153(16) 0.0418(4) Uani 1 1 d . . .
C2 C 0.38403(16) 0.01841(17) 0.3293(2) 0.0585(7) Uani 1 1 d . . .
H2 H 0.3726 -0.0340 0.2913 0.070 Uiso 1 1 calc . . .
C3 C 0.39478(17) 0.0123(2) 0.4254(2) 0.0638(8) Uani 1 1 d . . .
H3 H 0.3872 -0.0445 0.4520 0.077 Uiso 1 1 calc . . .
C4 C 0.41646(16) 0.0888(2) 0.48210(18) 0.0577(7) Uani 1 1 d . . .
H4 H 0.4260 0.0841 0.5470 0.069 Uiso 1 1 calc . . .
C5 C 0.42379(14) 0.17314(17) 0.43993(16) 0.0442(5) Uani 1 1 d . . .
C6 C 0.38862(15) 0.12900(15) 0.19127(16) 0.0451(5) Uani 1 1 d . . .
C7 C 0.45577(16) 0.26404(19) 0.48614(15) 0.0523(6) Uani 1 1 d . . .
C10 C 0.26069(15) 0.32289(17) 0.22664(19) 0.0500(5) Uani 1 1 d . . .
C11 C 0.28226(16) 0.3641(2) 0.31671(17) 0.0545(6) Uani 1 1 d . . .
C12 C 0.33284(16) 0.44340(17) 0.31334(15) 0.0488(5) Uani 1 1 d . . .
C13 C 0.34057(14) 0.45214(15) 0.22011(15) 0.0429(5) Uani 1 1 d . . .
C14 C 0.29752(14) 0.37696(16) 0.16769(14) 0.0433(5) Uani 1 1 d . . .
C15 C 0.20520(19) 0.2395(2) 0.1963(3) 0.0830(10) Uani 1 1 d . . .
H15A H 0.1464 0.2582 0.1783 0.125 Uiso 1 1 calc R . .
H15B H 0.2138 0.1962 0.2474 0.125 Uiso 1 1 calc R . .
H15C H 0.2199 0.2107 0.1437 0.125 Uiso 1 1 calc R . .
C16 C 0.2523(3) 0.3321(3) 0.3995(3) 0.0980(14) Uani 1 1 d . . .
H16A H 0.2956 0.3443 0.4563 0.147 Uiso 1 1 calc R . .
H16B H 0.2409 0.2667 0.3943 0.147 Uiso 1 1 calc R . .
H16C H 0.2010 0.3647 0.4011 0.147 Uiso 1 1 calc R . .
C17 C 0.3678(3) 0.5092(2) 0.3930(2) 0.0878(12) Uani 1 1 d . . .
H17A H 0.3247 0.5537 0.3968 0.132 Uiso 1 1 calc R . .
H17B H 0.4165 0.5408 0.3823 0.132 Uiso 1 1 calc R . .
H17C H 0.3844 0.4751 0.4509 0.132 Uiso 1 1 calc R . .
C18 C 0.3840(2) 0.52898(19) 0.1822(2) 0.0683(8) Uani 1 1 d . . .
H18A H 0.4230 0.5033 0.1496 0.103 Uiso 1 1 calc R . .
H18B H 0.4149 0.5671 0.2331 0.103 Uiso 1 1 calc R . .
H18C H 0.3421 0.5659 0.1394 0.103 Uiso 1 1 calc R . .
C19 C 0.2907(2) 0.3617(2) 0.06511(17) 0.0696(8) Uani 1 1 d . . .
H19A H 0.2524 0.4065 0.0286 0.104 Uiso 1 1 calc R . .
H19B H 0.2694 0.3004 0.0476 0.104 Uiso 1 1 calc R . .
H19C H 0.3461 0.3683 0.0535 0.104 Uiso 1 1 calc R . .
O6 O 0.0000 0.6731(4) 0.7500 0.1302(19) Uani 1 2 d S . .
H1 H 0.017(8) 0.721(9) 0.814(7) 0.39(7) Uiso 1 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
O1 Ti1 O3 97.28(6) . . ?
O1 Ti1 O2 90.20(7) . . ?
O3 Ti1 O2 140.15(7) . . ?
O1 Ti1 N1 128.46(8) . . ?
O3 Ti1 N1 72.61(7) . . ?
O2 Ti1 N1 72.21(7) . . ?
O1 Ti1 C14 99.21(7) . . ?
O3 Ti1 C14 136.53(7) . . ?
O2 Ti1 C14 79.72(7) . . ?
N1 Ti1 C14 123.20(8) . . ?
O1 Ti1 C12 102.56(9) . . ?
O3 Ti1 C12 79.61(7) . . ?
O2 Ti1 C12 136.75(8) . . ?
N1 Ti1 C12 123.67(8) . . ?
C14 Ti1 C12 57.64(8) . . ?
O1 Ti1 C13 82.48(8) . . ?
O3 Ti1 C13 110.02(7) . . ?
O2 Ti1 C13 109.75(7) . . ?
N1 Ti1 C13 148.95(7) . . ?
C14 Ti1 C13 34.50(8) . . ?
C12 Ti1 C13 34.66(7) . . ?
O1 Ti1 C11 136.63(10) . . ?
O3 Ti1 C11 83.62(9) . . ?
O2 Ti1 C11 116.52(9) . . ?
N1 Ti1 C11 93.39(8) . . ?
C14 Ti1 C11 57.26(8) . . ?
C12 Ti1 C11 34.65(10) . . ?
C13 Ti1 C11 57.27(8) . . ?
O1 Ti1 C10 133.65(7) . . ?
O3 Ti1 C10 116.41(9) . . ?
O2 Ti1 C10 83.62(8) . . ?
N1 Ti1 C10 93.11(8) . . ?
C14 Ti1 C10 34.48(8) . . ?
C12 Ti1 C10 57.65(9) . . ?
C13 Ti1 C10 57.33(8) . . ?
C11 Ti1 C10 34.45(9) . . ?
O1 Ti1 Ti1 25.20(6) . 2_655 ?
O3 Ti1 Ti1 100.75(6) . 2_655 ?
O2 Ti1 Ti1 71.44(5) . 2_655 ?
N1 Ti1 Ti1 105.29(5) . 2_655 ?
C14 Ti1 Ti1 111.01(6) . 2_655 ?
C12 Ti1 Ti1 127.76(7) . 2_655 ?
C13 Ti1 Ti1 104.49(6) . 2_655 ?
C11 Ti1 Ti1 161.29(7) . 2_655 ?
C10 Ti1 Ti1 142.12(7) . 2_655 ?
Ti1 O1 Ti1 129.60(13) . 2_655 ?
C6 O2 Ti1 124.59(14) . . ?
C7 O3 Ti1 124.62(15) . . ?
C1 N1 C5 121.37(19) . . ?
C1 N1 Ti1 119.77(14) . . ?
C5 N1 Ti1 118.79(15) . . ?
N1 C1 C2 120.8(2) . . ?
N1 C1 C6 110.85(18) . . ?
C2 C1 C6 128.2(2) . . ?
C1 C2 C3 117.9(3) . . ?
C4 C3 C2 121.0(2) . . ?
C3 C4 C5 118.1(2) . . ?
N1 C5 C4 120.4(2) . . ?
N1 C5 C7 110.98(19) . . ?
C4 C5 C7 128.4(2) . . ?
O4 C6 O2 126.1(2) . . ?
O4 C6 C1 121.8(2) . . ?
O2 C6 C1 111.97(18) . . ?
O5 C7 O3 126.3(3) . . ?
O5 C7 C5 121.8(3) . . ?
O3 C7 C5 111.91(19) . . ?
C14 C10 C11 107.6(2) . . ?
C14 C10 C15 125.3(3) . . ?
C11 C10 C15 127.0(3) . . ?
C14 C10 Ti1 72.03(13) . . ?
C11 C10 Ti1 72.78(14) . . ?
C15 C10 Ti1 123.00(19) . . ?
C10 C11 C12 108.3(2) . . ?
C10 C11 C16 125.5(3) . . ?
C12 C11 C16 126.2(3) . . ?
C10 C11 Ti1 72.78(13) . . ?
C12 C11 Ti1 72.03(13) . . ?
C16 C11 Ti1 123.69(19) . . ?
C13 C12 C11 107.6(2) . . ?
C13 C12 C17 126.3(3) . . ?
C11 C12 C17 126.1(3) . . ?
C13 C12 Ti1 73.16(12) . . ?
C11 C12 Ti1 73.31(13) . . ?
C17 C12 Ti1 121.73(18) . . ?
C14 C13 C12 107.9(2) . . ?
C14 C13 C18 125.5(2) . . ?
C12 C13 C18 126.5(2) . . ?
C14 C13 Ti1 72.17(12) . . ?
C12 C13 Ti1 72.18(12) . . ?
C18 C13 Ti1 122.88(17) . . ?
C13 C14 C10 108.5(2) . . ?
C13 C14 C19 124.2(2) . . ?
C10 C14 C19 127.2(2) . . ?
C13 C14 Ti1 73.33(12) . . ?
C10 C14 Ti1 73.49(13) . . ?
C19 C14 Ti1 121.02(17) . . ?
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 O1 1.8051(10) . ?
Ti1 O3 2.0217(17) . ?
Ti1 O2 2.0410(16) . ?
Ti1 N1 2.1427(17) . ?
Ti1 C14 2.366(2) . ?
Ti1 C12 2.368(2) . ?
Ti1 C13 2.380(2) . ?
Ti1 C11 2.384(2) . ?
Ti1 C10 2.384(2) . ?
Ti1 Ti1 3.2666(9) 2_655 ?
O1 Ti1 1.8051(10) 2_655 ?
O2 C6 1.296(3) . ?
O3 C7 1.293(3) . ?
O4 C6 1.215(3) . ?
O5 C7 1.222(3) . ?
N1 C1 1.334(3) . ?
N1 C5 1.337(3) . ?
C1 C2 1.380(3) . ?
C1 C6 1.507(3) . ?
C2 C3 1.382(4) . ?
C3 C4 1.374(4) . ?
C4 C5 1.384(3) . ?
C5 C7 1.506(4) . ?
C10 C14 1.408(3) . ?
C10 C11 1.412(4) . ?
C10 C15 1.500(4) . ?
C11 C12 1.415(4) . ?
C11 C16 1.496(4) . ?
C12 C13 1.414(3) . ?
C12 C17 1.501(4) . ?
C13 C14 1.407(3) . ?
C13 C18 1.496(3) . ?
C14 C19 1.501(3) . ?
