#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:13:21 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267002 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/83/7128398.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_7128398
loop_
_publ_author_name
'Hung, Ling-I'
'Hsieh, Tsung-Hsiu'
'Syu, Jhao-Yang'
'Chen, Pei-Lin'
'Lin, Chia-Her'
'Wang, Sue-Lein'
_publ_section_title
;
 A titanium(iii) phosphite exhibits polymorph-distinct redox activity
 involving proton-coupled electron transfer.
;
_journal_issue                   53
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6542
_journal_page_last               6545
_journal_paper_doi               10.1039/d1cc01190a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'H4 O7 P2 Ti'
_chemical_formula_weight         225.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2021-02-17 deposited with the CCDC.	2021-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.341(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0671(10)
_cell_length_b                   7.3832(10)
_cell_length_c                   12.0992(16)
_cell_measurement_reflns_used    2602
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2641
_cell_measurement_theta_min      3.0827
_cell_volume                     616.72(15)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5412
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         3.083
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.433
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0405P)²+1.9371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1351
_reflns_number_total             1518
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01190a2.cif
_cod_data_source_block           beta-IV
_cod_depositor_comments
;
The following automatic conversions were performed:

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 7128397--7128400.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7128398
_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.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.48703(8) 0.23252(7) 0.33802(4) 0.00883(16) Uani 1 1 d . . . . .
P1 P 0.75069(11) 0.13802(11) 0.59117(6) 0.00942(19) Uani 1 1 d . . . . .
P2 P 0.69062(13) 0.63718(11) 0.30405(7) 0.0151(2) Uani 1 1 d . . . . .
O1 O 0.6399(4) 0.2408(3) 0.48916(19) 0.0175(5) Uani 1 1 d . . . . .
O2 O 0.6318(4) -0.0131(3) 0.6273(2) 0.0173(5) Uani 1 1 d . . . . .
O3 O 0.8130(3) 0.2749(3) 0.68592(18) 0.0119(4) Uani 1 1 d . . . . .
O4 O 0.5737(4) 0.4617(3) 0.3030(2) 0.0187(5) Uani 1 1 d . . . . .
O5 O 0.8215(4) 0.6097(3) 0.2181(2) 0.0187(5) Uani 1 1 d . . . . .
O6 O 0.7990(5) 0.6922(5) 0.4170(2) 0.0374(8) Uani 1 1 d . . . . .
O7 O 0.2679(4) 0.3650(3) 0.3901(2) 0.0181(5) Uani 1 1 d . . . . .
H1 H 0.9114 0.0611 0.5644 0.050 Uiso 1 1 d . U . . .
H2 H 0.5579 0.7606 0.2524 0.050 Uiso 1 1 d . U . . .
H7A H 0.2543 0.3507 0.4579 0.050 Uiso 1 1 d . U . . .
H7B H 0.2286 0.4903 0.3642 0.050 Uiso 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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
O5 Ti1 O4 93.36(11) 2_645 . ?
O5 Ti1 O2 93.12(11) 2_645 3_656 ?
O4 Ti1 O2 172.89(11) . 3_656 ?
O5 Ti1 O1 93.31(11) 2_645 . ?
O4 Ti1 O1 92.43(10) . . ?
O2 Ti1 O1 90.12(10) 3_656 . ?
O5 Ti1 O3 90.18(10) 2_645 4_565 ?
O4 Ti1 O3 89.02(10) . 4_565 ?
O2 Ti1 O3 88.04(10) 3_656 4_565 ?
O1 Ti1 O3 176.14(10) . 4_565 ?
O5 Ti1 O7 176.66(11) 2_645 . ?
O4 Ti1 O7 86.76(11) . . ?
O2 Ti1 O7 86.60(11) 3_656 . ?
O1 Ti1 O7 90.01(11) . . ?
O3 Ti1 O7 86.49(10) 4_565 . ?
O2 P1 O1 112.41(14) . . ?
O2 P1 O3 111.13(13) . . ?
O1 P1 O3 107.27(13) . . ?
O2 P1 H1 107.6 . . ?
O1 P1 H1 109.0 . . ?
O3 P1 H1 109.5 . . ?
O6 P2 O4 114.39(16) . . ?
O6 P2 O5 113.14(16) . . ?
O4 P2 O5 106.38(14) . . ?
O6 P2 H2 114.3 . . ?
O4 P2 H2 104.1 . . ?
O5 P2 H2 103.4 . . ?
P1 O1 Ti1 148.08(16) . . ?
P1 O2 Ti1 169.45(17) . 3_656 ?
P1 O3 Ti1 134.66(14) . 4_666 ?
P2 O4 Ti1 163.54(17) . . ?
P2 O5 Ti1 139.73(16) . 2_655 ?
Ti1 O7 H7A 119.1 . . ?
Ti1 O7 H7B 121.7 . . ?
H7A O7 H7B 109.7 . . ?
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 O5 1.872(2) 2_645 ?
Ti1 O4 1.879(2) . ?
Ti1 O2 1.912(2) 3_656 ?
Ti1 O1 1.916(2) . ?
Ti1 O3 1.984(2) 4_565 ?
Ti1 O7 2.042(2) . ?
P1 O2 1.516(2) . ?
P1 O1 1.516(2) . ?
P1 O3 1.521(2) . ?
P1 H1 1.3691 . ?
P2 O6 1.473(3) . ?
P2 O4 1.535(2) . ?
P2 O5 1.546(2) . ?
P2 H2 1.3601 . ?
O2 Ti1 1.912(2) 3_656 ?
O3 Ti1 1.984(2) 4_666 ?
O5 Ti1 1.872(2) 2_655 ?
O7 H7A 0.8525 . ?
O7 H7B 0.9969 . ?
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
O7 H7A O6 0.85 1.67 2.514(4) 172.4 3_666
O7 H7B O3 1.00 1.84 2.831(3) 172.9 3_666
