Regioselective conversions of H4pdta (1,2-propanediaminetetraacetic acid) and H4eed3a to their triacetates on peroxotitanates
Yang, Yu-chen; Liu, Qiong-Xin; Zhou, Zhao-Hui; Wan, Huilin; Dalton Transactions  (2019) –; doi:10.1039/C9DT03589C

data_7701408
_publ_section_title
;
 Regioselective conversions of H4pdta (1,2-propanediaminetetraacetic acid)
 and H4eed3a to their triacetates on peroxotitanates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03589C
_journal_year                    2019
_chemical_formula_sum            'C22 H55 N7 O27 Ti2'
_chemical_formula_weight         945.53
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-17 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.99(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.998(14)
_cell_length_b                   12.0774(13)
_cell_length_c                   16.442(9)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9777
_cell_measurement_theta_min      2.8534
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_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.1679
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8458
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       flaky
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2419
_reflns_number_total             4114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03589c2.cif
_cod_data_source_block           sad_CCDC3
_cod_original_cell_volume        3741(3)
_cod_database_code               7701408
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              20652