Synthesis and structural characterization of a dumbbell-like phenylphosphonate-stabilized Ti~7~‒oxide cluster
Gao, Mei-Yan; Liu, Xiao-Xue; Fang, Wei-Hui; Zhang, Lei; Zhang, Jian; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618010707

data_2021247
_publ_section_title
;
 Synthesis and structural characterization of a dumbbell-like
 phenylphosphonate-stabilized Ti~7~--oxide cluster
;
_journal_coeditor_code           JR3016
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618010707
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Ti7 O2 (C6 H5 O3 P1)6 (C3 H7 O)12], 4H2 O'
_chemical_formula_moiety         'C72 H114 O32 P6 Ti7, 4(H2 O1)'
_chemical_formula_sum            'C72 H122 O36 P6 Ti7'
_chemical_formula_weight         2010.73
_chemical_name_systematic
;
Hexa-\m-isopropanolato-hexaisopropanolatodi-\m~3~-oxido-hexa-\m~3~-\
phenylphosphonato-heptatitanium tetrahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.158(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.073(4)
_cell_length_b                   12.9877(19)
_cell_length_c                   34.994(5)
_cell_measurement_reflns_used    13036
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.0427
_cell_volume                     10122(3)
_computing_data_collection
;
<b>Please provide references for software used for data collection, cell
refinement, data reduction, structure solution and molecular graphics</b>
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            37753
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.043
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (REFERENCE?)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       strip
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.949
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         11330
_refine_ls_number_restraints     452
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1774P)^2^+10.8217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2347
_reflns_number_gt                9545
_reflns_number_total             11330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3016sup1.cif
_cod_data_source_block           I
_cod_database_code               2021247
_shelx_hkl_checksum              64741
_shelx_res_checksum              10408
_shelx_fab_checksum              75635
_cod_database_fobs_code 2021247