#------------------------------------------------------------------------------
#$Date: 2019-06-08 02:25:03 +0200 (Sat 08 de Jun de 2019) $
#$Revision: 215765 $
#$URL: svn://www.crystallography.net/cod/cif/1/55/12/1551283.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_1551283
loop_
_publ_author_name
'Kraemer, Tobias'
'Tuna, Floriana'
'Pike, Sebastian D.'
_publ_section_title
;
 Photo-redox reactivity of titanium-oxo clusters: mechanistic insight into
 a two-electron intramolecular process, and structural characterisation of
 mixed-valent Ti(III)/Ti(IV) products
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01241A
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        'Lab 301, Dept Chem, Uni Cambridge'
_chemical_formula_moiety         'C72 H60 O16 P6 Ti4'
_chemical_formula_sum            'C72 H60 O16 P6 Ti4'
_chemical_formula_weight         1558.70
_chemical_name_systematic        '[Ti4O4(O2PPh2)6][O2}2'
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-04
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2019-04-24 deposited with the CCDC.    2019-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.069(9)
_cell_length_b                   15.069(9)
_cell_length_c                   15.069(9)
_cell_measurement_reflns_used    4136
_cell_measurement_temperature    180
_cell_measurement_theta_max      117
_cell_measurement_theta_min      8
_cell_volume                     3422(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.214
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4136
_diffrn_reflns_theta_full        58.538
_diffrn_reflns_theta_max         58.538
_diffrn_reflns_theta_min         4.149
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.743
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method
'single crystal to single crystal transformation'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.68
_refine_diff_density_min         -0.85
_refine_ls_abs_structure_details 'Flack (1983), 215 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.07(8)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         489
_refine_ls_number_restraints     272
_refine_ls_R_factor_all          0.2717
_refine_ls_R_factor_gt           0.1390
_refine_ls_shift/su_max          0.0003973
_refine_ls_shift/su_mean         0.0000617
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² +93.43P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2587
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2587
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              1
_reflns_number_gt                180
_reflns_number_total             494
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   3.36
_oxford_diffrn_Wilson_scale      945.63
_oxford_refine_ls_r_factor_ref   0.2717
_oxford_refine_ls_scale          0.0929(2)
_oxford_reflns_number_all        489
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_B1_0068 in I-43m'
_iucr_refine_instructions_details
;
#
# Punched on 04/03/19 at 11: 1:37
#
#LIST     12                                                                    
BLOCK SCALE X'S  U'S 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
END                                                                             
#
# Punched on 04/03/19 at 11: 1:37
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
PLANAR 0.010000  C(4) C(1) C(2) C(3) C(5) C(6) 
SAME C(1) C(2) C(3) C(4) C(5) C(6) AND 
CONT C(1) C(6) C(5) C(4) C(3) C(2) 
SIMU 0.03 C(1) C(2) C(3) C(4) C(5) C(6) AND 
CONT C(1) C(6) C(5) C(4) C(3) C(2) 
DELU 0.03 C(1) C(2) C(3) C(4) C(5) C(6) AND 
CONT C(1) C(6) C(5) C(4) C(3) C(2) 
END                                                                             
;
_cod_data_source_file            c9sc01241a2.cif
_cod_data_source_block           7ox
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3421.5176(13)
_cod_original_sg_symbol_Hall     'I -4 2 3 '
_cod_original_sg_symbol_H-M      'I -4 3 m '
_cod_database_code               1551283
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,z,x
y+1/2,z+1/2,x+1/2
z,x,y
z+1/2,x+1/2,y+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
z,-y,-x
z+1/2,-y+1/2,-x+1/2
x,-z,-y
x+1/2,-z+1/2,-y+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-z,x,-y
-z+1/2,x+1/2,-y+1/2
-x,y,-z
-x+1/2,y+1/2,-z+1/2
-y,-z,x
-y+1/2,-z+1/2,x+1/2
-z,-x,y
-z+1/2,-x+1/2,y+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-z,y,-x
-z+1/2,y+1/2,-x+1/2
-x,z,-y
-x+1/2,z+1/2,-y+1/2
-y,z,-x
-y+1/2,z+1/2,-x+1/2
z,y,x
z+1/2,y+1/2,x+1/2
x,z,y
x+1/2,z+1/2,y+1/2
y,x,z
y+1/2,x+1/2,z+1/2
y,-z,-x
y+1/2,-z+1/2,-x+1/2
-y,-x,z
-y+1/2,-x+1/2,z+1/2
-z,-y,x
-z+1/2,-y+1/2,x+1/2
-x,-z,y
-x+1/2,-z+1/2,y+1/2
x,-y,-z
x+1/2,-y+1/2,-z+1/2
z,-x,-y
z+1/2,-x+1/2,-y+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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C -0.568(1) -0.8216(10) -0.568(1) 0.1931 1.0000 Uani DS T
C2 C -0.5377(9) -0.8949(10) -0.6004(9) 0.1982 0.5000 Uani D .
C3 C -0.5939(10) -0.9456(9) -0.6541(10) 0.2055 0.5000 Uani D .
C4 C -0.6731(9) -0.9232(10) -0.6731(9) 0.2073 1.0000 Uani DS T
C5 C -0.7001(9) -0.8504(10) -0.6400(9) 0.2044 0.5000 Uani D .
C6 C -0.6481(10) -0.7963(9) -0.5854(10) 0.1975 0.5000 Uani D .
Ti1 Ti -0.4292(4) -0.5708(4) -0.5708(4) 0.1420 1.0000 Uani S T
O2 O -0.4386(7) -0.6989(12) -0.5614(7) 0.1486 1.0000 Uani S T
P3 P -0.5000 -0.7535(10) -0.5000 0.1738 1.0000 Uani S T
O5 O -0.5582(11) -0.5582(11) -0.5582(11) 0.1391 1.0000 Uani S T
H21 H -0.4769 -0.9153 -0.5904 0.1432 0.5000 Uiso R .
H31 H -0.5788 -0.9964 -0.6891 0.2330 0.5000 Uiso R .
H51 H -0.7619 -0.8405 -0.6513 0.2760 0.5000 Uiso R .
H61 H -0.6698 -0.7404 -0.5605 0.1620 0.5000 Uiso R .
H41 H -0.7110 -0.9562 -0.7110 0.1975 1.0000 Uiso RS .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.220(15) 0.140(19) 0.220(15) 0.004(13) 0.023(16) 0.004(13)
C2 0.222(16) 0.15(2) 0.222(16) 0.001(14) 0.022(16) 0.005(14)
C3 0.229(16) 0.159(19) 0.228(16) -0.007(14) 0.017(16) 0.003(15)
C4 0.230(15) 0.16(2) 0.230(15) -0.003(13) 0.014(16) -0.003(13)
C5 0.229(16) 0.16(2) 0.228(16) 0.003(14) 0.020(16) -0.003(15)
C6 0.222(16) 0.148(19) 0.222(16) 0.006(14) 0.021(17) 0.000(15)
Ti1 0.142(4) 0.142(4) 0.142(4) 0.009(4) -0.009(4) -0.009(4)
O2 0.134(10) 0.178(15) 0.134(10) 0.001(9) 0.060(13) -0.001(9)
P3 0.170(8) 0.181(14) 0.170(8) 0.0000 0.041(12) 0.0000
O5 0.139(11) 0.139(11) 0.139(11) 0.026(14) 0.026(14) 0.026(14)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ti 0.2191 1.8069 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 31_555 C1 C6 31_555 120.63(3) yes
C2 31_555 C1 C2 . 62.33(4) yes
C6 31_555 C1 C2 . 88.50(3) yes
C2 31_555 C1 C6 . 88.50(6) yes
C6 31_555 C1 C6 . 62.33(4) yes
C2 . C1 C6 . 120.63(4) yes
C2 31_555 C1 P3 . 120.4(6) yes
C6 31_555 C1 P3 . 119.0(6) yes
C2 . C1 P3 . 120.4(6) yes
C6 . C1 P3 . 119.0(6) yes
C2 31_555 C2 C1 . 58.83(2) yes
C2 31_555 C2 C6 31_555 90.00(2) yes
C1 . C2 C6 31_555 45.75(3) yes
C2 31_555 C2 C3 . 88.88(3) yes
C1 . C2 C3 . 117.96(4) yes
C6 31_555 C2 C3 . 88.68(4) yes
C2 31_555 C2 H21 . 123.7 no
C1 . C2 H21 . 122.9 no
C6 31_555 C2 H21 . 134.0 no
C3 . C2 H21 . 119.1 no
C2 . C3 C5 31_555 91.32(4) yes
C2 . C3 C3 31_555 91.12(4) yes
C5 31_555 C3 C3 31_555 90.00(4) yes
C2 . C3 C4 . 123.70(5) yes
C5 31_555 C3 C4 . 46.95(3) yes
C3 31_555 C3 C4 . 59.76(4) yes
C2 . C3 H31 . 127.7 no
C5 31_555 C3 H31 . 122.3 no
C3 31_555 C3 H31 . 123.9 no
C4 . C3 H31 . 108.1 no
C3 . C4 C3 31_555 60.48(4) yes
C3 . C4 C5 31_555 86.10(3) yes
C3 31_555 C4 C5 31_555 116.06(3) yes
C3 . C4 C5 . 116.06(3) yes
C3 31_555 C4 C5 . 86.10(3) yes
C5 31_555 C4 C5 . 60.48(4) yes
C3 . C4 H41 . 124.2 no
C3 31_555 C4 H41 . 124.2 no
C5 31_555 C4 H41 . 119.7 no
C5 . C4 H41 . 119.7 no
C3 31_555 C5 C5 31_555 90.00(2) yes
C3 31_555 C5 C4 . 46.95(3) yes
C5 31_555 C5 C4 . 59.76(2) yes
C3 31_555 C5 C6 . 91.32(4) yes
C5 31_555 C5 C6 . 91.12(4) yes
C4 . C5 C6 . 123.70(4) yes
C3 31_555 C5 H51 . 126.1 no
C5 31_555 C5 H51 . 124.1 no
C4 . C5 H51 . 112.1 no
C6 . C5 H51 . 123.9 no
C5 . C6 C6 31_555 88.88(3) yes
C5 . C6 C1 . 117.96(5) yes
C6 31_555 C6 C1 . 58.84(4) yes
C5 . C6 C2 31_555 88.68(4) yes
C6 31_555 C6 C2 31_555 90.00(4) yes
C1 . C6 C2 31_555 45.75(3) yes
C5 . C6 H61 . 122.7 no
C6 31_555 C6 H61 . 120.5 no
C1 . C6 H61 . 119.3 no
C2 31_555 C6 H61 . 133.7 no
Ti1 35_555 Ti1 Ti1 41_445 60.00(2) yes
Ti1 35_555 Ti1 O2 . 130.6(4) yes
Ti1 41_445 Ti1 O2 . 130.6(4) yes
Ti1 35_555 Ti1 P3 . 112.32(18) yes
Ti1 41_445 Ti1 P3 . 112.32(18) yes
O2 . Ti1 P3 . 22.8(5) yes
Ti1 35_555 Ti1 O5 . 39.8(5) yes
Ti1 41_445 Ti1 O5 . 82.1(8) yes
O2 . Ti1 O5 . 90.9(6) yes
P3 . Ti1 O5 . 73.5(3) yes
Ti1 . O2 P3 . 128.1(11) yes
C1 17_454 P3 C1 . 109.4(10) yes
C1 17_454 P3 O2 31_555 107.9(3) yes
C1 . P3 O2 31_555 107.9(3) yes
C1 17_454 P3 O2 . 107.9(3) yes
C1 . P3 O2 . 107.9(3) yes
O2 31_555 P3 O2 . 115.7(15) yes
C1 17_454 P3 Ti1 . 120.4(4) yes
C1 . P3 Ti1 . 120.4(4) yes
O2 31_555 P3 Ti1 . 86.6(9) yes
O2 . P3 Ti1 . 29.1(7) yes
C1 17_454 P3 Ti1 3_555 120.4(4) yes
C1 . P3 Ti1 3_555 120.4(4) yes
O2 31_555 P3 Ti1 3_555 29.1(7) yes
O2 . P3 Ti1 3_555 86.6(9) yes
Ti1 . P3 Ti1 3_555 57.5(4) yes
Ti1 . O5 Ti1 3_555 100.5(10) yes
Ti1 . O5 Ti1 5_555 100.5(10) yes
Ti1 3_555 O5 Ti1 5_555 100.5(10) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 31_555 1.2909(16) yes
C1 C6 31_555 1.2909(16) yes
C1 C2 . 1.2909(16) yes
C1 C6 . 1.2909(17) yes
C1 P3 . 1.78(2) yes
C2 C2 31_555 1.3361(17) yes
C2 C6 31_555 1.801(2) yes
C2 C3 . 1.398(4) yes
C2 H21 . 0.977 no
C3 C5 31_555 1.737(2) yes
C3 C3 31_555 1.2815(17) yes
C3 C4 . 1.2722(17) yes
C3 H31 . 0.958 no
C4 C5 31_555 1.2722(16) yes
C4 C5 . 1.2722(16) yes
C4 H41 . 0.949 no
C5 C5 31_555 1.2814(17) yes
C5 C6 . 1.398(4) yes
C5 H51 . 0.958 no
C6 C6 31_555 1.3360(17) yes
C6 H61 . 0.979 no
Ti1 Ti1 35_555 3.018(17) yes
Ti1 Ti1 41_445 3.018(17) yes
Ti1 O2 . 1.941(19) yes
Ti1 P3 . 3.139(13) yes
Ti1 O5 . 1.963(13) yes
O2 P3 . 1.545(17) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C2 H21 C2 25_454 124.6(3) 0.977 2.275 2.94(2) yes
C2 H21 C3 13_435 126.5(7) 0.977 2.541 3.22(2) yes
C5 H51 C5 35_555 129.61(6) 0.958 2.507 3.20(2) yes
C6 H61 C6 35_555 135.05(6) 0.979 2.389 3.16(2) yes
