#------------------------------------------------------------------------------
#$Date: 2019-06-08 03:25:03 +0300 (Sat, 08 Jun 2019) $
#$Revision: 215765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551282.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_1551282
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, Chemistry, 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]'
_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     other
_audit_creation_date             2018-10-17
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2019-03-09 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                   15.0884(5)
_cell_length_b                   15.0884(5)
_cell_length_c                   15.0884(5)
_cell_measurement_reflns_used    6439
_cell_measurement_temperature    180
_cell_measurement_theta_max      134
_cell_measurement_theta_min      8
_cell_volume                     3435.0(2)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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  0.059
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6134
_diffrn_reflns_theta_full        66.875
_diffrn_reflns_theta_max         66.875
_diffrn_reflns_theta_min         4.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.721
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.38
_refine_ls_abs_structure_details 'Flack (1983), 262 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         597
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.0113563
_refine_ls_shift/su_mean         0.0010846
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 1.28P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1193
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1193
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              1
_reflns_number_gt                534
_reflns_number_total             601
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   3.82
_oxford_diffrn_Wilson_scale      340.25
_oxford_refine_ls_r_factor_ref   0.0473
_oxford_refine_ls_scale          0.07349(6)
_oxford_reflns_number_all        597
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_B1_0096 in I-43m'
_iucr_refine_instructions_details
;
#
# Punched on 17/10/18 at 17:34:35
#
#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 17/10/18 at 17:34:35
#
#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           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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.

'_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        3435.02(11)
_cod_original_sg_symbol_Hall     'I -4 2 3 '
_cod_original_sg_symbol_H-M      'I -4 3 m '
_cod_database_code               1551282
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
-z,x,-y
-z+1/2,x+1/2,-y+1/2
z,-x,-y
z+1/2,-x+1/2,-y+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
-x,z,-y
-x+1/2,z+1/2,-y+1/2
-z,y,-x
-z+1/2,y+1/2,-x+1/2
z,-y,-x
z+1/2,-y+1/2,-x+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
x,-y,-z
x+1/2,-y+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,-x,z
-y+1/2,-x+1/2,z+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
z,x,y
z+1/2,x+1/2,y+1/2
y,x,z
y+1/2,x+1/2,z+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
-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,z,y
x+1/2,z+1/2,y+1/2
-y,-z,x
-y+1/2,-z+1/2,x+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 0.5694(3) 0.8251(3) 0.5694(3) 0.0883 1.0000 Uani DS T
C2 C 0.5394(3) 0.9017(3) 0.6054(3) 0.1085 0.5000 Uani D .
C3 C 0.5979(3) 0.9491(3) 0.6604(3) 0.1359 0.5000 Uani D .
C4 C 0.6797(3) 0.9226(4) 0.6797(3) 0.1547 1.0000 Uani DS T
C5 C 0.7057(3) 0.8467(4) 0.6432(3) 0.1541 0.5000 Uani D .
C6 C 0.6526(3) 0.7953(3) 0.5865(3) 0.1221 0.5000 Uani D .
Ti1 Ti 0.43127(5) 0.56873(5) 0.56873(5) 0.0510 1.0000 Uani S T
O2 O 0.43957(17) 0.7024(2) 0.56043(17) 0.0652 1.0000 Uani S T
P3 P 0.5000 0.75596(12) 0.5000 0.0684 1.0000 Uani S T
O5 O 0.56140(18) 0.56140(18) 0.56140(18) 0.0497 1.0000 Uani S T
H21 H 0.4787 0.9221 0.5955 0.1432 0.5000 Uiso R .
H31 H 0.5827 0.9999 0.6954 0.2330 0.5000 Uiso R .
H51 H 0.7675 0.8367 0.6545 0.2760 0.5000 Uiso R .
H61 H 0.6743 0.7394 0.5616 0.1620 0.5000 Uiso R .
H41 H 0.7177 0.9556 0.7177 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 0.103(2) 0.058(3) 0.103(2) -0.013(2) 0.016(4) -0.013(2)
C2 0.167(8) 0.072(4) 0.087(5) -0.026(4) 0.002(5) 0.003(5)
C3 0.196(8) 0.097(6) 0.115(6) -0.036(5) 0.006(7) -0.027(6)
C4 0.172(5) 0.121(7) 0.172(5) -0.049(4) -0.003(7) -0.049(4)
C5 0.149(8) 0.135(7) 0.179(9) -0.032(6) -0.005(8) -0.036(7)
C6 0.114(6) 0.102(6) 0.151(8) -0.031(6) 0.004(6) -0.012(5)
Ti1 0.0510(4) 0.0510(4) 0.0510(4) -0.0013(3) 0.0013(3) 0.0013(3)
O2 0.0724(13) 0.0508(15) 0.0724(13) -0.0054(10) 0.016(2) 0.0054(10)
P3 0.0789(8) 0.0473(9) 0.0789(8) 0.0000 0.0159(10) 0.0000
O5 0.0497(11) 0.0497(11) 0.0497(11) -0.0027(13) -0.0027(13) -0.0027(13)
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
C6 31_555 C1 C2 31_555 120.95(4) yes
C6 31_555 C1 C2 . 88.54(3) yes
C2 31_555 C1 C2 . 62.62(5) yes
C6 31_555 C1 C6 . 62.59(5) yes
C2 31_555 C1 C6 . 88.54(3) yes
C2 . C1 C6 . 120.95(4) yes
C6 31_555 C1 P3 . 117.0(3) yes
C2 31_555 C1 P3 . 122.0(3) yes
C2 . C1 P3 . 122.0(3) yes
C6 . C1 P3 . 117.0(3) yes
C2 31_555 C2 C1 . 58.69(3) yes
C2 31_555 C2 C3 . 88.48(3) yes
C1 . C2 C3 . 117.44(5) yes
C2 31_555 C2 H21 . 123.7 no
C1 . C2 H21 . 121.2 no
C3 . C2 H21 . 121.3 no
C2 . C3 C3 31_555 91.52(3) yes
C2 . C3 C5 31_555 91.47(4) yes
C3 31_555 C3 C5 31_555 90.00(3) yes
C2 . C3 C4 . 124.00(4) yes
C3 31_555 C3 C4 . 59.90(2) yes
C5 31_555 C3 C4 . 46.78(4) yes
C2 . C3 H31 . 125.6 no
C3 31_555 C3 H31 . 123.9 no
C5 31_555 C3 H31 . 124.1 no
C4 . C3 H31 . 109.9 no
C5 31_555 C4 C3 . 86.44(3) yes
C5 31_555 C4 C3 31_555 116.17(3) yes
C3 . C4 C3 31_555 60.20(5) yes
C5 31_555 C4 C5 . 60.21(5) yes
C3 . C4 C5 . 116.17(3) yes
C3 31_555 C4 C5 . 86.44(3) yes
C5 31_555 C4 H41 . 121.5 no
C3 . C4 H41 . 122.3 no
C3 31_555 C4 H41 . 122.3 no
C5 . C4 H41 . 121.5 no
C5 31_555 C5 C4 . 59.90(2) yes
C5 31_555 C5 C3 31_555 90.00(3) yes
C4 . C5 C3 31_555 46.78(4) yes
C5 31_555 C5 C6 . 91.55(3) yes
C4 . C5 C6 . 124.00(4) yes
C3 31_555 C5 C6 . 91.46(4) yes
C5 31_555 C5 H51 . 124.1 no
C4 . C5 H51 . 110.3 no
C3 31_555 C5 H51 . 124.4 no
C6 . C5 H51 . 125.2 no
C6 31_555 C6 C5 . 88.45(3) yes
C6 31_555 C6 C1 . 58.71(3) yes
C5 . C6 C1 . 117.43(5) yes
C6 31_555 C6 H61 . 120.5 no
C5 . C6 H61 . 121.2 no
C1 . C6 H61 . 121.4 no
Ti1 9_665 Ti1 Ti1 13_656 60.000 yes
Ti1 9_665 Ti1 Ti1 7_665 60.000 yes
Ti1 13_656 Ti1 Ti1 7_665 60.000 yes
Ti1 9_665 Ti1 O2 . 131.35(8) yes
Ti1 13_656 Ti1 O2 . 84.98(11) yes
Ti1 7_665 Ti1 O2 . 131.35(8) yes
Ti1 9_665 Ti1 P3 . 113.40(2) yes
Ti1 13_656 Ti1 P3 . 62.56(3) yes
Ti1 7_665 Ti1 P3 . 113.40(2) yes
O2 . Ti1 P3 . 22.42(10) yes
Ti1 9_665 Ti1 O5 . 41.88(8) yes
Ti1 13_656 Ti1 O5 . 41.88(8) yes
Ti1 7_665 Ti1 O5 . 85.45(12) yes
O2 . Ti1 O5 . 89.47(12) yes
P3 . Ti1 O5 . 72.95(5) yes
Ti1 . O2 P3 . 127.1(2) yes
C1 15_656 P3 C1 . 109.7(3) yes
C1 15_656 P3 O2 41_656 107.80(9) yes
C1 . P3 O2 41_656 107.80(9) yes
C1 15_656 P3 O2 . 107.80(9) yes
C1 . P3 O2 . 107.80(9) yes
O2 41_656 P3 O2 . 115.9(3) yes
C1 15_656 P3 Ti1 21_566 120.73(14) yes
C1 . P3 Ti1 21_566 120.73(14) yes
O2 . P3 Ti1 21_566 85.38(15) yes
C1 15_656 P3 Ti1 . 120.73(14) yes
C1 . P3 Ti1 . 120.73(14) yes
O2 41_656 P3 Ti1 . 85.38(15) yes
Ti1 21_566 P3 Ti1 . 54.87(6) yes
Ti1 . O5 Ti1 35_555 96.25(16) yes
Ti1 . O5 Ti1 31_555 96.25(16) yes
Ti1 35_555 O5 Ti1 31_555 96.25(16) 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 C6 31_555 1.358(2) yes
C1 C2 31_555 1.356(2) yes
C1 C2 . 1.356(2) yes
C1 C6 . 1.358(2) yes
C1 P3 . 1.811(5) yes
C2 C2 31_555 1.409(2) yes
C2 C3 . 1.406(4) yes
C2 H21 . 0.978 no
C3 C3 31_555 1.335(2) yes
C3 C5 31_555 1.823(2) yes
C3 C4 . 1.3307(19) yes
C3 H31 . 0.959 no
C4 C5 31_555 1.3308(19) yes
C4 C5 . 1.3308(19) yes
C4 H41 . 0.950 no
C5 C5 31_555 1.335(2) yes
C5 C6 . 1.405(4) yes
C5 H51 . 0.959 no
C6 C6 31_555 1.411(2) yes
C6 H61 . 0.980 no
Ti1 Ti1 9_665 2.933(2) yes
Ti1 Ti1 13_656 2.933(2) yes
Ti1 Ti1 7_665 2.933(2) yes
Ti1 O2 . 2.025(3) yes
Ti1 P3 . 3.1830(16) yes
Ti1 O5 . 1.970(2) yes
O2 P3 . 1.522(4) 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 15_656 125.53(7) 0.978 2.418 3.091(6) yes
C2 H21 C3 25_675 128.72(16) 0.978 2.464 3.169(6) yes
C5 H51 C5 35_555 128.47(6) 0.959 2.316 3.008(6) yes
C6 H61 C6 35_555 134.40(5) 0.980 2.278 3.045(6) yes
