Terminal Titanyl Complexes of Tri- and Tetrametaphosphate: Synthesis, Structures, and Reactivity with Hydrogen Peroxide.
Stauber, Julia M.; Cummins, Christopher C.; Inorganic chemistry 56 (2017) 3022–3029; doi:10.1021/acs.inorgchem.6b03149

data_4345225
_publ_section_title
;
 Terminal Titanyl Complexes of Tri- and Tetrametaphosphate: Synthesis,
 Structures, and Reactivity with Hydrogen Peroxide.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3022
_journal_page_last               3029
_journal_paper_doi               10.1021/acs.inorgchem.6b03149
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C77 H67 N2 O12 P7 Ti'
_chemical_formula_weight         1477.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.945(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.714(2)
_cell_length_b                   12.719(2)
_cell_length_c                   27.457(5)
_cell_measurement_reflns_used    9005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      2.51
_cell_volume                     3673.5(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            135224
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.081
_diffrn_reflns_theta_min         1.511
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   0.7462
_exptl_transmission_factor_min   0.6805
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 8004 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         22707
_refine_ls_number_restraints     1489
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.8064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                19472
_reflns_number_total             22707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03149_si_004.cif
_cod_data_source_block           OTiP3O9acac
_cod_depositor_comments          'Adding full bibliography for 4345225.cif.'
_cod_original_cell_volume        3673.7(12)
_cod_database_code               4345225
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              46056
_shelx_hkl_checksum              78244
_shelx_fab_checksum              29090