#------------------------------------------------------------------------------
#$Date: 2020-10-06 13:51:43 +0200 (mar 06 de oct de 2020) $
#$Revision: 258143 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/99/7239944.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_7239944
loop_
_publ_author_name
'Svensson, Fredric G.'
'Daniel, Geoffrey'
'Tai, Cheuk-Wai'
'Seisenbaeva, Gulaim A.'
'Kessler, Vadim G.'
_publ_section_title
;
 Titanium phosphonate oxo-alkoxide “clusters”: solution
 stability and facile hydrolytic transformation into nano titania
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              6873
_journal_page_last               6883
_journal_paper_doi               10.1039/C9RA10691J
_journal_volume                  10
_journal_year                    2020
_chemical_formula_sum            'C48 H92 O24 P4 Ti4'
_chemical_formula_weight         1368.70
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.010(5)
_cell_length_b                   13.950(3)
_cell_length_c                   22.820(5)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9173
_cell_measurement_theta_min      2.3170
_cell_volume                     7190(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28268
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.8924
_exptl_absorpt_correction_T_min  0.8446
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00089(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6291
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0704P)²+22.7266P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2398
_refine_ls_wR_factor_ref         0.2584
_reflns_number_gt                4068
_reflns_number_total             6291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ra10691j2.cif
_cod_data_source_block           tiacopbu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7239942--7239948.cif.
;
_cod_original_cell_volume        7190(2)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               7239944
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 0.09217(4) 0.74250(7) 0.23473(5) 0.0464(3) Uani 1 1 d U . .
Ti2 Ti 0.06754(6) 0.47847(9) 0.37273(6) 0.0657(4) Uani 1 1 d U . .
P3 P 0.04948(6) 0.71453(11) 0.35748(7) 0.0467(4) Uani 1 1 d U . .
P4 P 0.07640(7) 0.50221(10) 0.22817(8) 0.0514(4) Uani 1 1 d U . .
O6 O 0.06656(17) 0.7249(3) 0.30081(17) 0.0504(9) Uani 1 1 d U . .
O4 O 0.01472(17) 0.7413(3) 0.16427(19) 0.0526(9) Uani 1 1 d U . .
O7 O 0.07232(18) 0.4919(3) 0.29304(19) 0.0591(10) Uani 1 1 d U . .
O5 O 0.17524(19) 0.7282(3) 0.3022(2) 0.0679(12) Uani 1 1 d U . .
O2 O 0.09729(19) 0.6017(3) 0.2220(2) 0.0587(10) Uani 1 1 d U . .
O11 O 0.12954(19) 0.7494(3) 0.1717(2) 0.0592(10) Uani 1 1 d U . .
O9 O 0.05603(19) 0.4504(3) 0.4534(2) 0.0617(11) Uani 1 1 d U . .
O3 O 0.0986(2) 0.8703(3) 0.2402(2) 0.0688(12) Uani 1 1 d U . .
O10 O 0.1460(2) 0.4751(3) 0.4239(2) 0.0748(12) Uani 1 1 d U . .
O12 O 0.0653(2) 0.3374(3) 0.3630(2) 0.0764(13) Uani 1 1 d U . .
O1 O 0.0629(2) 0.6153(3) 0.3873(2) 0.0630(11) Uani 1 1 d U . .
O8 O -0.0201(2) 0.4759(3) 0.3289(2) 0.0683(11) Uani 1 1 d U . .
C4 C 0.1819(3) 0.7286(5) 0.1796(4) 0.0681(17) Uani 1 1 d U . .
C9 C 0.0473(4) 0.3767(6) 0.4778(4) 0.081(2) Uani 1 1 d U . .
C3 C 0.2266(3) 0.7047(5) 0.2402(4) 0.0763(18) Uani 1 1 d U . .
H3A H 0.2623 0.6840 0.2410 0.092 Uiso 1 1 calc R . .
C6 C 0.1327(3) 0.4175(5) 0.2309(4) 0.0726(18) Uani 1 1 d U . .
C15 C 0.0924(3) 0.8007(5) 0.4203(3) 0.0697(17) Uani 1 1 d U . .
C5 C 0.1912(4) 0.7342(8) 0.1198(4) 0.111(3) Uani 1 1 d U . .
H5A H 0.1547 0.7514 0.0838 0.167 Uiso 1 1 calc R . .
H5B H 0.2043 0.6731 0.1117 0.167 Uiso 1 1 calc R . .
H5C H 0.2207 0.7819 0.1253 0.167 Uiso 1 1 calc R . .
C2 C 0.2234(3) 0.7086(5) 0.2979(4) 0.0665(16) Uani 1 1 d U . .
C8 C 0.0453(5) 0.2861(6) 0.4485(5) 0.104(3) Uani 1 1 d U . .
H8B H 0.0347 0.2338 0.4665 0.124 Uiso 1 1 calc R . .
C10 C 0.1257(7) 0.9533(8) 0.2320(6) 0.147(5) Uani 1 1 d U . .
H10 H 0.1549 0.9198 0.2216 0.177 Uiso 1 1 calc R . .
C6A C 0.1122(4) 0.3164(5) 0.2351(5) 0.107(3) Uani 1 1 d U . .
H6AA H 0.1419 0.2715 0.2368 0.160 Uiso 1 1 calc R . .
H6AB H 0.0759 0.3035 0.1977 0.160 Uiso 1 1 calc R . .
H6AC H 0.1059 0.3103 0.2736 0.160 Uiso 1 1 calc R . .
C1 C 0.2744(4) 0.6894(6) 0.3590(4) 0.097(3) Uani 1 1 d U . .
H1A H 0.2630 0.6946 0.3941 0.146 Uiso 1 1 calc R . .
H1B H 0.3050 0.7351 0.3651 0.146 Uiso 1 1 calc R . .
H1C H 0.2888 0.6259 0.3582 0.146 Uiso 1 1 calc R . .
C15A C 0.0772(4) 0.7950(7) 0.4766(4) 0.105(3) Uani 1 1 d U . .
H15A H 0.1005 0.8405 0.5090 0.157 Uiso 1 1 calc R . .
H15B H 0.0852 0.7316 0.4946 0.157 Uiso 1 1 calc R . .
H15C H 0.0359 0.8093 0.4624 0.157 Uiso 1 1 calc R . .
C6B C 0.1886(4) 0.4392(6) 0.2889(5) 0.098(2) Uani 1 1 d U . .
H6BA H 0.2189 0.3954 0.2909 0.147 Uiso 1 1 calc R . .
H6BB H 0.1822 0.4327 0.3274 0.147 Uiso 1 1 calc R . .
H6BC H 0.2007 0.5036 0.2860 0.147 Uiso 1 1 calc R . .
C7 C 0.0577(4) 0.2674(6) 0.3956(5) 0.094(2) Uani 1 1 d U . .
C14A C 0.2383(7) 0.4041(11) 0.4785(8) 0.197(5) Uani 1 1 d DU . .
H14A H 0.2210 0.3536 0.4475 0.295 Uiso 1 1 calc R . .
H14B H 0.2627 0.3768 0.5201 0.295 Uiso 1 1 calc R . .
H14C H 0.2620 0.4443 0.4648 0.295 Uiso 1 1 calc R . .
C13 C 0.0406(4) 0.3886(7) 0.5402(4) 0.108(3) Uani 1 1 d U . .
H13A H 0.0437 0.4553 0.5516 0.161 Uiso 1 1 calc R . .
H13B H 0.0713 0.3534 0.5743 0.161 Uiso 1 1 calc R . .
H13C H 0.0027 0.3648 0.5344 0.161 Uiso 1 1 calc R . .
C14 C 0.1913(7) 0.4613(12) 0.4833(5) 0.181(5) Uani 1 1 d U . .
H14D H 0.1734 0.4121 0.5000 0.217 Uiso 1 1 calc R . .
C6C C 0.1400(5) 0.4275(7) 0.1677(5) 0.109(3) Uani 1 1 d U . .
H6CA H 0.1700 0.3839 0.1684 0.164 Uiso 1 1 calc R . .
H6CB H 0.1514 0.4920 0.1637 0.164 Uiso 1 1 calc R . .
H6CC H 0.1031 0.4128 0.1314 0.164 Uiso 1 1 calc R . .
C14B C 0.2073(7) 0.5316(10) 0.5356(7) 0.185(4) Uani 1 1 d DU . .
H14E H 0.1721 0.5621 0.5335 0.278 Uiso 1 1 calc R . .
H14F H 0.2331 0.5790 0.5309 0.278 Uiso 1 1 calc R . .
H14G H 0.2273 0.4999 0.5767 0.278 Uiso 1 1 calc R . .
C15C C 0.0802(5) 0.9003(6) 0.3907(5) 0.113(3) Uani 1 1 d U . .
H15D H 0.1030 0.9464 0.4230 0.170 Uiso 1 1 calc R . .
H15E H 0.0388 0.9146 0.3753 0.170 Uiso 1 1 calc R . .
H15F H 0.0911 0.9028 0.3552 0.170 Uiso 1 1 calc R . .
C15B C 0.1580(4) 0.7765(7) 0.4424(4) 0.111(3) Uani 1 1 d U . .
H15G H 0.1819 0.8210 0.4754 0.167 Uiso 1 1 calc R . .
H15H H 0.1677 0.7808 0.4061 0.167 Uiso 1 1 calc R . .
H15I H 0.1656 0.7126 0.4597 0.167 Uiso 1 1 calc R . .
C10A C 0.1648(9) 0.9947(11) 0.2850(8) 0.265(11) Uani 1 1 d U . .
H10A H 0.1810 1.0500 0.2734 0.397 Uiso 1 1 calc R . .
H10B H 0.1961 0.9503 0.3084 0.397 Uiso 1 1 calc R . .
H10C H 0.1459 1.0141 0.3118 0.397 Uiso 1 1 calc R . .
C11 C 0.0543(7) 0.1729(7) 0.3675(6) 0.177(6) Uani 1 1 d U . .
H11A H 0.0645 0.1773 0.3316 0.265 Uiso 1 1 calc R . .
H11B H 0.0147 0.1486 0.3527 0.265 Uiso 1 1 calc R . .
H11C H 0.0814 0.1305 0.3997 0.265 Uiso 1 1 calc R . .
C10B C 0.0978(6) 0.9998(11) 0.1720(7) 0.173(4) Uani 1 1 d U . .
H10D H 0.1205 1.0549 0.1716 0.259 Uiso 1 1 calc R . .
H10E H 0.0588 1.0197 0.1655 0.259 Uiso 1 1 calc R . .
H10F H 0.0947 0.9566 0.1380 0.259 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'
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
_geom_angle_publ_flag
O3 Ti1 O6 97.15(19) . . ?
O3 Ti1 O4 95.44(19) . . ?
O6 Ti1 O4 95.83(17) . . ?
O3 Ti1 O5 90.8(2) . . ?
O6 Ti1 O5 88.22(18) . . ?
O4 Ti1 O5 172.07(19) . . ?
O3 Ti1 O2 168.6(2) . . ?
O6 Ti1 O2 93.03(17) . . ?
O4 Ti1 O2 88.54(17) . . ?
O5 Ti1 O2 84.43(18) . . ?
O3 Ti1 O11 86.98(19) . . ?
O6 Ti1 O11 171.84(18) . . ?
O4 Ti1 O11 90.75(17) . . ?
O5 Ti1 O11 84.68(19) . . ?
O2 Ti1 O11 82.29(17) . . ?
O10 Ti2 O7 97.2(2) . . ?
O10 Ti2 O1 92.5(2) . . ?
O7 Ti2 O1 95.79(17) . . ?
O10 Ti2 O12 91.0(2) . . ?
O7 Ti2 O12 90.08(19) . . ?
O1 Ti2 O12 172.7(2) . . ?
O10 Ti2 O8 170.9(2) . . ?
O7 Ti2 O8 91.72(19) . . ?
O1 Ti2 O8 88.25(19) . . ?
O12 Ti2 O8 87.3(2) . . ?
O10 Ti2 O9 86.9(2) . . ?
O7 Ti2 O9 173.1(2) . . ?
O1 Ti2 O9 89.55(18) . . ?
O12 Ti2 O9 84.28(18) . . ?
O8 Ti2 O9 84.04(18) . . ?
O4 P3 O1 111.9(2) 2 . ?
O4 P3 O6 110.0(2) 2 . ?
O1 P3 O6 112.2(2) . . ?
O4 P3 C15 106.2(3) 2 . ?
O1 P3 C15 107.9(3) . . ?
O6 P3 C15 108.5(3) . . ?
O8 P4 O2 112.2(3) 2 . ?
O8 P4 O7 112.9(3) 2 . ?
O2 P4 O7 110.2(2) . . ?
O8 P4 C6 107.2(3) 2 . ?
O2 P4 C6 107.9(3) . . ?
O7 P4 C6 106.1(3) . . ?
P3 O6 Ti1 176.1(3) . . ?
P3 O4 Ti1 145.9(3) 2 . ?
P4 O7 Ti2 179.7(3) . . ?
C2 O5 Ti1 131.7(5) . . ?
P4 O2 Ti1 147.5(3) . . ?
C4 O11 Ti1 130.3(4) . . ?
C9 O9 Ti2 134.1(5) . . ?
C10 O3 Ti1 148.4(7) . . ?
C14 O10 Ti2 149.4(8) . . ?
C7 O12 Ti2 133.9(5) . . ?
P3 O1 Ti2 146.7(3) . . ?
P4 O8 Ti2 149.1(3) 2 . ?
O11 C4 C3 122.2(6) . . ?
O11 C4 C5 114.6(7) . . ?
C3 C4 C5 123.2(7) . . ?
O9 C9 C8 120.4(7) . . ?
O9 C9 C13 116.5(7) . . ?
C8 C9 C13 123.0(7) . . ?
C2 C3 C4 126.5(7) . . ?
C6B C6 C6C 111.9(7) . . ?
C6B C6 C6A 110.3(7) . . ?
C6C C6 C6A 108.9(7) . . ?
C6B C6 P4 108.4(5) . . ?
C6C C6 P4 108.1(5) . . ?
C6A C6 P4 109.2(5) . . ?
C15A C15 C15C 110.8(7) . . ?
C15A C15 C15B 109.8(7) . . ?
C15C C15 C15B 109.3(8) . . ?
C15A C15 P3 111.1(6) . . ?
C15C C15 P3 108.4(5) . . ?
C15B C15 P3 107.4(5) . . ?
O5 C2 C3 122.3(6) . . ?
O5 C2 C1 115.7(7) . . ?
C3 C2 C1 122.0(7) . . ?
C7 C8 C9 126.7(8) . . ?
C10A C10 C10B 123.7(12) . . ?
C10A C10 O3 116.9(10) . . ?
C10B C10 O3 116.7(11) . . ?
O12 C7 C8 120.0(7) . . ?
O12 C7 C11 115.4(9) . . ?
C8 C7 C11 124.0(9) . . ?
C14 C14A C14B 30.7(7) . . ?
O10 C14 C14A 110.9(12) . . ?
O10 C14 C14B 122.6(12) . . ?
C14A C14 C14B 118.6(12) . . ?
C14 C14B C14A 30.7(7) . . ?
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 O3 1.790(4) . ?
Ti1 O6 1.890(4) . ?
Ti1 O4 1.914(4) . ?
Ti1 O5 1.995(4) . ?
Ti1 O2 1.997(4) . ?
Ti1 O11 2.026(4) . ?
Ti2 O10 1.801(5) . ?
Ti2 O7 1.882(4) . ?
Ti2 O1 1.949(4) . ?
Ti2 O12 1.978(4) . ?
Ti2 O8 1.981(5) . ?
Ti2 O9 2.020(4) . ?
P3 O4 1.510(4) 2 ?
P3 O1 1.516(4) . ?
P3 O6 1.533(4) . ?
P3 C15 1.825(6) . ?
P4 O8 1.496(5) 2 ?
P4 O2 1.511(4) . ?
P4 O7 1.534(4) . ?
P4 C6 1.818(6) . ?
O4 P3 1.510(4) 2 ?
O5 C2 1.278(8) . ?
O11 C4 1.275(8) . ?
O9 C9 1.231(8) . ?
O3 C10 1.393(10) . ?
O10 C14 1.356(11) . ?
O12 C7 1.290(9) . ?
O8 P4 1.496(5) 2 ?
C4 C3 1.395(10) . ?
C4 C5 1.482(10) . ?
C9 C8 1.422(11) . ?
C9 C13 1.513(10) . ?
C3 C2 1.356(10) . ?
C6 C6B 1.486(11) . ?
C6 C6C 1.537(11) . ?
C6 C6A 1.518(10) . ?
C15 C15A 1.490(11) . ?
C15 C15C 1.516(11) . ?
C15 C15B 1.534(11) . ?
C2 C1 1.454(10) . ?
C8 C7 1.393(12) . ?
C10 C10A 1.319(15) . ?
C10 C10B 1.400(15) . ?
C7 C11 1.451(12) . ?
C14A C14 1.463(17) . ?
C14A C14B 2.516(10) . ?
C14 C14B 1.462(16) . ?
