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_7701405
_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_moiety         'C11 H15 N2 O10 Ti, H4 N, H2 O'
_chemical_formula_sum            'C11 H21 N3 O11 Ti'
_chemical_formula_weight         419.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-10-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-17 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                83.398(4)
_cell_angle_beta                 85.937(4)
_cell_angle_gamma                77.802(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6948(3)
_cell_length_b                   7.5422(4)
_cell_length_c                   16.7297(8)
_cell_measurement_reflns_used    1953
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.78
_cell_volume                     819.25(7)
_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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  ShelXL
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Oxford Gemini Diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.1485
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10186
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.627
_diffrn_reflns_theta_min         2.778
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_correction_T_min  0.7983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2819
_reflns_number_total             5294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03589c2.cif
_cod_data_source_block           sad
_cod_database_code               7701405
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3A = N3-H3B = N3-H3C = N3-H3D = O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.01
 H3A-H3B = H3A-H3C = H3A-H3D = H3B-H3C = H3B-H3D = H3C-H3D = H1WA-H1WB
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C3 \\sim O4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B)
5.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              92369
_olex2_submission_special_instructions 'No special instructions were received'