#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:37:25 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233307 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348744.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_4348744
loop_
_publ_author_name
'Narayanam, Nagaraju'
'Chintakrinda, Kalpana'
'Fang, Wei-Hui'
'Kang, Yao'
'Zhang, Lei'
'Zhang, Jian'
_publ_section_title
;
 Azole Functionalized Polyoxo-Titanium Clusters with Sunlight-Driven Dye
 Degradation Applications: Synthesis, Structure, and Photocatalytic
 Studies.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10294
_journal_page_last               10301
_journal_paper_doi               10.1021/acs.inorgchem.6b01551
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C54 H88 N6 O22 P2 Ti6'
_chemical_formula_weight         1522.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                110.1390(10)
_cell_angle_beta                 101.778(4)
_cell_angle_gamma                108.014(3)
_cell_formula_units_Z            1
_cell_length_a                   12.076(5)
_cell_length_b                   12.451(5)
_cell_length_c                   14.470(6)
_cell_measurement_reflns_used    5523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5243
_cell_measurement_theta_min      2.4968
_cell_volume                     1821.2(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18648
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.717
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       Prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0850P)²+0.2572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6879
_reflns_number_total             8103
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01551_si_002.cif
_cod_data_source_block           PTC-37
_cod_database_code               4348744
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ti1 Ti 0.18241(3) 0.97643(3) 0.57696(2) 0.03293(10) Uani 1 1 d . .
Ti2 Ti -0.00561(3) 1.14458(3) 0.68071(2) 0.03313(10) Uani 1 1 d . .
Ti3 Ti 0.24209(3) 1.25892(3) 0.64012(2) 0.03581(11) Uani 1 1 d . .
P4 P -0.07128(5) 0.84703(4) 0.61202(3) 0.03293(12) Uani 1 1 d . .
O5 O 0.11194(13) 1.30523(12) 0.68881(10) 0.0397(3) Uani 1 1 d . .
O6 O 0.11638(12) 1.09825(11) 0.62181(9) 0.0338(3) Uani 1 1 d . .
O7 O 0.36446(14) 1.40362(13) 0.67485(11) 0.0523(4) Uani 1 1 d . .
O8 O 0.32402(13) 1.28623(14) 0.78768(11) 0.0492(4) Uani 1 1 d . .
O9 O 0.30839(13) 1.13325(13) 0.58443(11) 0.0424(3) Uani 1 1 d . .
O10 O -0.16699(13) 0.76427(12) 0.50214(10) 0.0414(3) Uani 1 1 d . .
O11 O 0.12299(13) 0.88562(12) 0.43891(10) 0.0388(3) Uani 1 1 d . .
O12 O -0.06904(14) 1.21073(13) 0.77432(10) 0.0444(3) Uani 1 1 d . .
O13 O 0.30304(14) 0.94553(15) 0.64384(12) 0.0498(4) Uani 1 1 d . .
O14 O -0.07953(12) 0.97174(12) 0.66556(10) 0.0370(3) Uani 1 1 d . .
N15 N 0.15510(16) 1.18389(17) 0.82858(12) 0.0446(4) Uani 1 1 d . .
C16 C 0.3385(2) 1.1925(2) 0.90634(15) 0.0480(5) Uani 1 1 d . .
O17 O 0.05926(13) 0.86698(12) 0.61052(11) 0.0408(3) Uani 1 1 d . .
N18 N 0.27454(16) 1.22109(16) 0.83627(12) 0.0436(4) Uani 1 1 d . .
C19 C 0.2495(2) 1.1355(2) 0.94164(15) 0.0494(5) Uani 1 1 d . .
N20 N 0.13744(18) 1.13157(18) 0.89274(13) 0.0493(4) Uani 1 1 d . .
C21 C -0.10096(18) 0.76231(18) 0.68924(15) 0.0383(4) Uani 1 1 d . .
C22 C -0.1487(2) 0.6325(2) 0.64341(19) 0.0553(6) Uani 1 1 d . .
H22 H -0.1716 0.5881 0.5711 0.066 Uiso 1 1 calc R U
C23 C -0.0850(3) 0.7616(3) 0.8575(2) 0.0712(8) Uani 1 1 d . .
H23 H -0.0642 0.8052 0.9296 0.085 Uiso 1 1 calc R U
C24 C -0.1308(3) 0.6331(3) 0.8110(2) 0.0709(8) Uani 1 1 d . .
H24 H -0.1404 0.5897 0.8518 0.085 Uiso 1 1 calc R U
C25 C -0.1626(3) 0.5682(2) 0.7046(2) 0.0706(8) Uani 1 1 d . .
H25 H -0.1936 0.4810 0.6735 0.085 Uiso 1 1 calc R U
C26 C -0.0697(3) 0.8264(2) 0.79624(17) 0.0583(6) Uani 1 1 d . .
H26 H -0.0381 0.9137 0.8277 0.070 Uiso 1 1 calc R U
C27 C -0.0959(3) 1.2441(3) 0.8670(2) 0.0697(7) Uani 1 1 d . .
H27 H -0.0206 1.2736 0.9266 0.084 Uiso 1 1 calc R U
C28 C 0.4922(3) 1.1666(3) 1.0126(2) 0.0757(8) Uani 1 1 d . .
H28 H 0.5734 1.1758 1.0381 0.091 Uiso 1 1 calc R U
C29 C 0.4024(3) 1.1076(3) 1.0492(2) 0.0779(9) Uani 1 1 d . .
H29 H 0.4265 1.0787 1.0978 0.094 Uiso 1 1 calc R U
C30 C 0.2834(3) 1.0918(3) 1.01619(19) 0.0647(7) Uani 1 1 d . .
H30 H 0.2258 1.0536 1.0416 0.078 Uiso 1 1 calc R U
C31 C 0.3273(2) 0.8506(2) 0.66487(19) 0.0567(6) Uani 1 1 d . .
H31 H 0.4172 0.8753 0.6857 0.068 Uiso 1 1 calc R U
C32 C 0.5053(4) 1.5705(4) 0.6606(4) 0.1368(19) Uani 1 1 d . .
H32A H 0.5784 1.5593 0.6524 0.205 Uiso 1 1 calc R U
H32B H 0.5235 1.6585 0.6904 0.205 Uiso 1 1 calc R U
H32C H 0.4403 1.5285 0.5932 0.205 Uiso 1 1 calc R U
C33 C 0.2658(3) 0.7285(3) 0.5647(2) 0.0799(8) Uani 1 1 d . .
H33A H 0.1772 0.6992 0.5449 0.120 Uiso 1 1 calc R U
H33B H 0.2903 0.6666 0.5764 0.120 Uiso 1 1 calc R U
H33C H 0.2910 0.7425 0.5096 0.120 Uiso 1 1 calc R U
C34 C 0.4141(2) 1.1374(3) 0.5513(2) 0.0706(8) Uani 1 1 d . .
H34 H 0.3989 1.0484 0.5203 0.085 Uiso 1 1 calc R U
C35 C 0.2893(3) 0.8401(3) 0.7547(2) 0.0760(8) Uani 1 1 d . .
H35A H 0.3335 0.9193 0.8159 0.114 Uiso 1 1 calc R U
H35B H 0.3084 0.7767 0.7687 0.114 Uiso 1 1 calc R U
H35C H 0.2016 0.8176 0.7370 0.114 Uiso 1 1 calc R U
C37 C 0.5288(3) 1.1915(4) 0.6435(3) 0.0916(10) Uani 1 1 d . .
H37A H 0.5499 1.2790 0.6838 0.137 Uiso 1 1 calc R U
H37B H 0.5956 1.1824 0.6200 0.137 Uiso 1 1 calc R U
H37C H 0.5152 1.1482 0.6865 0.137 Uiso 1 1 calc R U
C42 C 0.4620(2) 1.2104(3) 0.94058(19) 0.0619(6) Uani 1 1 d . .
H42 H 0.5202 1.2495 0.9162 0.074 Uiso 1 1 calc R U
C55 C -0.1392(4) 1.3475(4) 0.8811(3) 0.1050(12) Uani 1 1 d . .
H55A H -0.0728 1.4214 0.8905 0.158 Uiso 1 1 calc R U
H55B H -0.1639 1.3655 0.9418 0.158 Uiso 1 1 calc R U
H55C H -0.2086 1.3216 0.8201 0.158 Uiso 1 1 calc R U
C1AA C 0.0909(3) 1.4192(2) 0.7197(2) 0.0593(6) Uani 1 1 d . .
H1AA H 0.0062 1.3977 0.7210 0.071 Uiso 1 1 calc R U
C2 C 0.1805(3) 1.5090(3) 0.8303(2) 0.0920(11) Uani 1 1 d . .
H2A H 0.1722 1.4675 0.8751 0.138 Uiso 1 1 calc R U
H2B H 0.1620 1.5811 0.8558 0.138 Uiso 1 1 calc R U
H2C H 0.2640 1.5352 0.8301 0.138 Uiso 1 1 calc R U
C3 C 0.1012(3) 1.4702(3) 0.6404(3) 0.0797(9) Uani 1 1 d . .
H3A H 0.1852 1.4972 0.6413 0.120 Uiso 1 1 calc R U
H3B H 0.0787 1.5403 0.6574 0.120 Uiso 1 1 calc R U
H3C H 0.0464 1.4059 0.5718 0.120 Uiso 1 1 calc R U
C4 C -0.1934(5) 1.1305(4) 0.8607(4) 0.140(2) Uani 1 1 d . .
H4A H -0.2658 1.0988 0.8002 0.210 Uiso 1 1 calc R U
H4B H -0.2148 1.1527 0.9229 0.210 Uiso 1 1 calc R U
H4C H -0.1623 1.0672 0.8548 0.210 Uiso 1 1 calc R U
C0AA C 0.4103(4) 1.1645(7) 0.4655(4) 0.186(3) Uani 1 1 d . .
H0AA H 0.3899 1.0894 0.4040 0.279 Uiso 1 1 calc R U
H0AB H 0.4899 1.2263 0.4785 0.279 Uiso 1 1 calc R U
H0AC H 0.3483 1.1965 0.4546 0.279 Uiso 1 1 calc R U
C1 C 0.4676(4) 1.5210(3) 0.7257(3) 0.1214(17) Uani 1 1 d . .
C10 C 0.5491(3) 1.5391(3) 0.8243(3) 0.0965(11) Uani 1 1 d . .
H10A H 0.5024 1.5296 0.8695 0.145 Uiso 1 1 calc R U
H10B H 0.6150 1.6219 0.8579 0.145 Uiso 1 1 calc R U
H10C H 0.5836 1.4779 0.8106 0.145 Uiso 1 1 calc R U
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'
P P 0.1023 0.0942 '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
O11 Ti1 O13 113.51(7) . .
O11 Ti1 O6 112.90(6) . .
O13 Ti1 O6 133.24(7) . .
O11 Ti1 O17 97.78(7) . .
O13 Ti1 O17 91.10(7) . .
O6 Ti1 O17 88.11(6) . .
O11 Ti1 O9 98.49(6) . .
O13 Ti1 O9 91.54(7) . .
O6 Ti1 O9 76.36(7) . .
O17 Ti1 O9 160.89(6) . .
O12 Ti2 O11 99.00(7) . 2_576
O12 Ti2 O14 96.40(6) . .
O11 Ti2 O14 94.48(6) 2_576 .
O12 Ti2 O6 159.82(6) . .
O11 Ti2 O6 100.42(6) 2_576 .
O14 Ti2 O6 87.51(6) . .
O12 Ti2 O5 98.21(7) . .
O11 Ti2 O5 92.84(6) 2_576 .
O14 Ti2 O5 162.42(6) . .
O6 Ti2 O5 75.45(6) . .
O12 Ti2 N15 84.53(7) . .
O11 Ti2 N15 176.13(6) 2_576 .
O14 Ti2 N15 86.66(6) . .
O6 Ti2 N15 75.92(7) . .
O5 Ti2 N15 85.05(6) . .
O7 Ti3 O10 93.62(6) . 2_576
O7 Ti3 O9 103.95(8) . .
O10 Ti3 O9 89.77(6) 2_576 .
O7 Ti3 O6 171.53(6) . .
O10 Ti3 O6 94.83(6) 2_576 .
O9 Ti3 O6 75.52(6) . .
O7 Ti3 O5 104.82(8) . .
O10 Ti3 O5 93.24(6) 2_576 .
O9 Ti3 O5 150.81(6) . .
O6 Ti3 O5 75.29(6) . .
O7 Ti3 O8 84.97(6) . .
O10 Ti3 O8 178.51(6) 2_576 .
O9 Ti3 O8 90.11(7) . .
O6 Ti3 O8 86.58(6) . .
O5 Ti3 O8 87.59(7) . .
O10 P4 O14 113.36(8) . .
O10 P4 O17 110.67(8) . .
O14 P4 O17 111.26(8) . .
O10 P4 C21 107.03(9) . .
O14 P4 C21 107.73(9) . .
O17 P4 C21 106.41(8) . .
C1AA O5 Ti3 133.65(13) . .
C1AA O5 Ti2 122.66(14) . .
Ti3 O5 Ti2 103.62(6) . .
Ti1 O6 Ti2 147.69(7) . .
Ti1 O6 Ti3 105.78(7) . .
Ti2 O6 Ti3 105.27(6) . .
C1 O7 Ti3 166.99(19) . .
N18 O8 Ti3 125.89(11) . .
C34 O9 Ti3 133.80(16) . .
C34 O9 Ti1 124.05(16) . .
Ti3 O9 Ti1 102.11(7) . .
P4 O10 Ti3 149.57(9) . 2_576
Ti1 O11 Ti2 141.83(8) . 2_576
C27 O12 Ti2 158.94(16) . .
C31 O13 Ti1 142.91(15) . .
P4 O14 Ti2 138.05(8) . .
N20 N15 N18 109.03(17) . .
N20 N15 Ti2 123.60(14) . .
N18 N15 Ti2 123.23(12) . .
N18 C16 C19 103.6(2) . .
N18 C16 C42 132.6(2) . .
C19 C16 C42 123.7(2) . .
P4 O17 Ti1 135.77(8) . .
O8 N18 N15 123.59(16) . .
O8 N18 C16 125.42(18) . .
N15 N18 C16 110.77(17) . .
N20 C19 C16 109.53(19) . .
N20 C19 C30 131.1(2) . .
C16 C19 C30 119.4(2) . .
N15 N20 C19 107.04(18) . .
C26 C21 C22 119.06(19) . .
C26 C21 P4 120.19(16) . .
C22 C21 P4 120.65(16) . .
C21 C22 C25 120.4(2) . .
C24 C23 C26 119.6(2) . .
C23 C24 C25 120.5(2) . .
C24 C25 C22 120.0(2) . .
C21 C26 C23 120.5(2) . .
O12 C27 C4 108.5(3) . .
O12 C27 C55 109.7(2) . .
C4 C27 C55 111.0(3) . .
C42 C28 C29 121.4(3) . .
C30 C29 C28 122.5(2) . .
C29 C30 C19 117.4(3) . .
O13 C31 C35 110.8(2) . .
O13 C31 C33 109.2(2) . .
C35 C31 C33 113.7(3) . .
C0AA C34 O9 114.0(3) . .
C0AA C34 C37 123.3(3) . .
O9 C34 C37 110.5(2) . .
C28 C42 C16 115.6(3) . .
O5 C1AA C3 110.0(2) . .
O5 C1AA C2 107.7(2) . .
C3 C1AA C2 114.5(3) . .
C32 C1 O7 115.1(3) . .
C32 C1 C10 125.2(3) . .
O7 C1 C10 112.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O11 1.7723(15) .
Ti1 O13 1.7984(15) .
Ti1 O6 1.9077(14) .
Ti1 O17 1.9498(14) .
Ti1 O9 2.0221(15) .
Ti2 O12 1.7736(14) .
Ti2 O11 1.8351(15) 2_576
Ti2 O14 1.9707(15) .
Ti2 O6 1.9821(14) .
Ti2 O5 2.0110(15) .
Ti2 N15 2.3623(19) .
Ti3 O7 1.7632(15) .
Ti3 O10 1.9518(15) 2_576
Ti3 O9 1.9770(16) .
Ti3 O6 1.9923(14) .
Ti3 O5 2.0081(16) .
Ti3 O8 2.0206(16) .
P4 O10 1.5201(14) .
P4 O14 1.5231(15) .
P4 O17 1.5241(16) .
P4 C21 1.7975(19) .
O5 C1AA 1.453(3) .
O7 C1 1.410(3) .
O8 N18 1.332(2) .
O9 C34 1.445(3) .
O10 Ti3 1.9519(15) 2_576
O11 Ti2 1.8351(14) 2_576
O12 C27 1.398(3) .
O13 C31 1.415(3) .
N15 N20 1.320(2) .
N15 N18 1.339(3) .
C16 N18 1.360(3) .
C16 C19 1.387(3) .
C16 C42 1.392(3) .
C19 N20 1.370(3) .
C19 C30 1.410(3) .
C21 C26 1.379(3) .
C21 C22 1.384(3) .
C22 C25 1.385(3) .
C23 C24 1.370(4) .
C23 C26 1.393(3) .
C24 C25 1.371(4) .
C27 C4 1.494(5) .
C27 C55 1.501(4) .
C28 C42 1.370(4) .
C28 C29 1.415(4) .
C29 C30 1.346(4) .
C31 C35 1.496(4) .
C31 C33 1.519(4) .
C32 C1 1.371(5) .
C34 C0AA 1.390(5) .
C34 C37 1.485(4) .
C1AA C3 1.499(4) .
C1AA C2 1.515(4) .
C1 C10 1.456(5) .
