#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:06:50 +0100 (vie 25 de mar de 2016) $
#$Revision: 179952 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/47/7024752.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_7024752
loop_
_publ_author_name
'Deng, Yuanfu'
'Lv, Qiying'
'Wu, Songping'
'Zhan, Shuzhong'
_publ_section_title
;
 Heterobimetallic peroxo-titanium(IV) nitrilotriacetate complexes as
 single source precursors for preparation of MTiO3 (M = Co, Ni and Zn).
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2497
_journal_page_last               2503
_journal_paper_doi               10.1039/b920987e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C12 H46 N2 Ni2 O34 Ti2'
_chemical_formula_weight         975.73
_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                 100.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.043(3)
_cell_length_b                   13.250(3)
_cell_length_c                   17.368(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.07
_cell_volume                     3399.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15938
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            gree
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3884
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0549P)²+3.7381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                3352
_reflns_number_total             3884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920987e.txt
_cod_data_source_block           2
_cod_original_cell_volume        3399.0(12)
_cod_original_sg_symbol_H-M      C2/C
_cod_database_code               7024752
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
Ni1 Ni 0.13279(2) 0.38547(2) 0.467622(17) 0.02249(11) Uani 1 1 d .
Ti1 Ti 0.42326(3) 0.36081(3) 0.31894(2) 0.01732(11) Uani 1 1 d .
C1 C 0.21895(16) 0.34116(18) 0.24551(13) 0.0222(5) Uani 1 1 d .
H1A H 0.1898 0.2773 0.2293 0.027 Uiso 1 1 calc R
H1B H 0.1790 0.3947 0.2217 0.027 Uiso 1 1 calc R
C2 C 0.23165(16) 0.35001(16) 0.33359(13) 0.0197(4) Uani 1 1 d .
C3 C 0.32164(16) 0.25436(17) 0.17399(13) 0.0226(5) Uani 1 1 d .
H3A H 0.3626 0.2689 0.1385 0.027 Uiso 1 1 calc R
H3B H 0.2651 0.2300 0.1432 0.027 Uiso 1 1 calc R
C4 C 0.36240(16) 0.17433(17) 0.23215(14) 0.0223(5) Uani 1 1 d .
C5 C 0.30834(17) 0.43865(17) 0.16827(13) 0.0241(5) Uani 1 1 d .
H5A H 0.2490 0.4514 0.1366 0.029 Uiso 1 1 calc R
H5B H 0.3507 0.4285 0.1333 0.029 Uiso 1 1 calc R
C6 C 0.33764(16) 0.52864(17) 0.22092(14) 0.0239(5) Uani 1 1 d .
N1 N 0.30505(13) 0.34731(13) 0.21615(10) 0.0174(4) Uani 1 1 d .
O1 O 0.31115(11) 0.35841(14) 0.37243(10) 0.0263(4) Uani 1 1 d .
O2 O 0.16186(11) 0.34870(13) 0.36177(10) 0.0258(4) Uani 1 1 d .
O3 O 0.39829(12) 0.20482(12) 0.30064(9) 0.0240(3) Uani 1 1 d .
O4 O 0.36124(14) 0.08520(13) 0.20998(11) 0.0341(4) Uani 1 1 d .
O5 O 0.38352(12) 0.50906(12) 0.28956(10) 0.0260(4) Uani 1 1 d .
O6 O 0.32087(16) 0.61470(13) 0.19536(12) 0.0397(5) Uani 1 1 d .
O7 O 0.5000 0.35963(18) 0.2500 0.0234(5) Uani 1 2 d S
O8 O 0.49874(11) 0.31305(13) 0.41168(10) 0.0264(4) Uani 1 1 d .
O9 O 0.49304(12) 0.42409(14) 0.40780(10) 0.0291(4) Uani 1 1 d .
O1W O 0.08926(17) 0.41898(16) 0.56907(11) 0.0422(5) Uani 1 1 d D
O2W O 0.25569(14) 0.36747(16) 0.53436(11) 0.0361(4) Uani 1 1 d D
O3W O 0.17185(13) 0.53616(14) 0.44898(11) 0.0317(4) Uani 1 1 d D
O4W O 0.09295(12) 0.23775(13) 0.47601(10) 0.0273(4) Uani 1 1 d D
O5W O 0.00389(12) 0.41498(14) 0.40427(10) 0.0285(4) Uani 1 1 d D
O6W O 0.0000 0.4535(2) 0.2500 0.0320(6) Uani 1 2 d SD
O7W O 0.12707(16) 0.30502(18) 0.05071(14) 0.0466(5) Uani 1 1 d D
O8W O 0.35762(16) 0.5775(2) 0.46113(15) 0.0529(6) Uani 1 1 d D
O9W O 0.49562(19) 0.6858(2) 0.33713(15) 0.0574(6) Uani 1 1 d D
H1W1 H 0.060(2) 0.4711(16) 0.576(2) 0.069 Uiso 1 1 d D
H1W2 H 0.085(3) 0.3735(19) 0.6019(19) 0.069 Uiso 1 1 d D
H2W1 H 0.2994(19) 0.338(3) 0.5199(19) 0.069 Uiso 1 1 d D
H2W2 H 0.262(3) 0.368(3) 0.5834(7) 0.069 Uiso 1 1 d D
H3W1 H 0.2282(9) 0.544(3) 0.4650(19) 0.069 Uiso 1 1 d D
H3W2 H 0.158(2) 0.554(3) 0.4009(9) 0.069 Uiso 1 1 d D
H4W1 H 0.069(2) 0.218(3) 0.5147(14) 0.069 Uiso 1 1 d D
H4W2 H 0.059(2) 0.217(3) 0.4337(12) 0.069 Uiso 1 1 d D
H5W1 H -0.031(2) 0.368(2) 0.415(2) 0.069 Uiso 1 1 d D
H5W2 H 0.010(3) 0.409(3) 0.3571(10) 0.069 Uiso 1 1 d D
H6W1 H 0.0428(18) 0.495(2) 0.262(3) 0.069 Uiso 1 1 d D
H7W1 H 0.128(3) 0.333(2) 0.0081(16) 0.069 Uiso 1 1 d D
H7W2 H 0.122(3) 0.2419(13) 0.046(2) 0.069 Uiso 1 1 d D
H8W1 H 0.391(2) 0.555(3) 0.5016(13) 0.069 Uiso 1 1 d D
H8W2 H 0.373(3) 0.558(3) 0.4201(13) 0.069 Uiso 1 1 d D
H9W1 H 0.460(2) 0.637(2) 0.325(2) 0.069 Uiso 1 1 d D
H9W2 H 0.522(2) 0.701(3) 0.2996(15) 0.069 Uiso 1 1 d 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'
Ni Ni 0.3393 1.1124 '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
O2W Ni1 O2 99.33(8) . .
O2W Ni1 O1W 86.46(9) . .
O2 Ni1 O1W 173.79(9) . .
O2W Ni1 O4W 95.45(8) . .
O2 Ni1 O4W 87.22(7) . .
O1W Ni1 O4W 90.03(8) . .
O2W Ni1 O5W 175.04(8) . .
O2 Ni1 O5W 84.55(7) . .
O1W Ni1 O5W 89.79(9) . .
O4W Ni1 O5W 87.79(7) . .
O2W Ni1 O3W 87.04(8) . .
O2 Ni1 O3W 88.52(7) . .
O1W Ni1 O3W 94.04(8) . .
O4W Ni1 O3W 175.36(7) . .
O5W Ni1 O3W 89.98(8) . .
O7 Ti1 O9 102.62(7) . .
O7 Ti1 O8 101.80(6) . .
O9 Ti1 O8 45.85(8) . .
O7 Ti1 O1 165.62(5) . .
O9 Ti1 O1 90.80(8) . .
O8 Ti1 O1 91.22(7) . .
O7 Ti1 O5 92.03(9) . 1
O9 Ti1 O5 82.60(8) . 1
O8 Ti1 O5 128.28(7) . 1
O1 Ti1 O5 84.52(7) . 1
O7 Ti1 O5 92.03(9) . .
O9 Ti1 O5 82.60(8) . .
O8 Ti1 O5 128.28(7) . .
O1 Ti1 O5 84.52(7) . .
O5 Ti1 O5 0.00(14) 1 .
O7 Ti1 O3 90.54(9) . .
O9 Ti1 O3 127.72(7) . .
O8 Ti1 O3 82.07(7) . .
O1 Ti1 O3 85.18(7) . .
O5 Ti1 O3 148.04(7) 1 .
O5 Ti1 O3 148.04(7) . .
O7 Ti1 N1 88.96(5) . .
O9 Ti1 N1 154.95(8) . .
O8 Ti1 N1 153.36(7) . .
O1 Ti1 N1 76.66(7) . .
O5 Ti1 N1 74.77(7) 1 .
O5 Ti1 N1 74.77(7) . .
O3 Ti1 N1 73.44(6) . .
N1 C1 C2 113.18(19) . .
O2 C2 O1 125.3(2) . .
O2 C2 C1 116.4(2) . .
O1 C2 C1 118.3(2) . .
N1 C3 C4 109.79(18) . .
O4 C4 O3 124.7(2) . .
O4 C4 C3 118.7(2) . .
O3 C4 C3 116.57(19) . .
N1 C5 C6 110.01(18) . .
O6 C6 O5 123.9(2) . 1
O6 C6 O5 123.9(2) . .
O5 C6 O5 0.00(16) 1 .
O6 C6 C5 119.6(2) . .
O5 C6 C5 116.4(2) 1 .
O5 C6 C5 116.4(2) . .
C5 N1 C3 112.19(17) . .
C5 N1 C1 111.37(18) . .
C3 N1 C1 111.44(18) . .
C5 N1 Ti1 105.85(14) . .
C3 N1 Ti1 105.90(13) . .
C1 N1 Ti1 109.78(13) . .
C2 O1 Ti1 122.06(15) . .
C2 O2 Ni1 134.32(16) . .
C4 O3 Ti1 118.80(14) . .
O5 O5 C6 0(10) 1 .
O5 O5 Ti1 0(10) 1 .
C6 O5 Ti1 119.66(14) . .
Ti1 O7 Ti1 179.01(15) 2_655 .
O9 O8 Ti1 66.90(9) . .
O8 O9 Ti1 67.25(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2W 2.002(2) .
Ni1 O2 2.0282(17) .
Ni1 O1W 2.0414(19) .
Ni1 O4W 2.0602(18) .
Ni1 O5W 2.0772(19) .
Ni1 O3W 2.1234(19) .
Ti1 O7 1.8138(6) .
Ti1 O9 1.8901(18) .
Ti1 O8 1.8951(18) .
Ti1 O1 2.0741(17) .
Ti1 O5 2.0882(17) 1
Ti1 O5 2.0882(17) .
Ti1 O3 2.1140(17) .
Ti1 N1 2.276(2) .
C1 N1 1.481(3) .
C1 C2 1.510(3) .
C2 O2 1.239(3) .
C2 O1 1.262(3) .
C3 N1 1.478(3) .
C3 C4 1.512(3) .
C4 O4 1.241(3) .
C4 O3 1.275(3) .
C5 N1 1.475(3) .
C5 C6 1.516(3) .
C6 O6 1.232(3) .
C6 O5 1.286(3) 1
C6 O5 1.286(3) .
O5 O5 0.000(6) 1
O7 Ti1 1.8138(6) 2_655
O8 O9 1.475(3) .
O6W O6W 0.000(5) 1
O8W O8W 0.000(9) 1
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W2 O3 0.840(10) 1.961(17) 2.772(2) 162(4) 7_556
O1W H1W1 O5W 0.836(10) 1.860(11) 2.695(3) 177(3) 5_566
O2W H2W2 O6 0.839(10) 1.993(19) 2.792(3) 159(4) 6_566
O2W H2W1 O4W 0.846(10) 1.891(16) 2.705(3) 161(3) 7_556
O3W H3W2 O4 0.854(10) 1.937(11) 2.788(3) 174(4) 4
O3W H3W1 O8W 0.847(10) 2.010(17) 2.816(3) 159(3) 1
O4W H4W1 O8 0.855(18) 1.83(2) 2.679(3) 170(4) 7_556
O4W H4W2 O9W 0.860(18) 1.811(17) 2.664(3) 172(4) 3_445
O5W H5W2 O6W 0.847(10) 1.93(2) 2.7172(19) 154(4) 1
O5W H5W1 O7W 0.853(10) 1.865(16) 2.683(3) 160(4) 2
O6W H6W1 O4 0.839(10) 1.870(11) 2.709(3) 178(5) 4
O7W H7W1 O3W 0.832(18) 2.18(2) 2.908(3) 146(4) 6_565
O7W H7W2 O8W 0.843(18) 2.21(2) 3.034(4) 167(4) 4_545
O8W H8W1 O9 0.837(18) 2.13(3) 2.880(3) 148(4) 5_666
O9W H9W1 O5 0.842(10) 2.075(12) 2.912(3) 173(4) 1
