DOTA analogue with phosphinate-iminodiacetate pendant arm: modification of complex formation rate with a strongly chelating pendant
Prochazkova, Sona; Kubicek, Vojtech; Bohmova, Zuzana; Holà, Katerina; Kotek, Jan; Hermann, Petr; Dalton Trans.  (2017) –; doi:10.1039/C7DT01797A

data_7043659
_publ_section_title
;
 DOTA analogue with phosphinate-iminodiacetate pendant arm: modification
 of complex formation rate with a strongly chelating pendant
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01797A
_journal_year                    2017
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C20 H39 Cu4 N5 O17 P, 7.5 (H2 O), Cl'
_chemical_formula_sum            'C20 H54 Cl Cu4 N5 O24.5 P'
_chemical_formula_weight         1077.26
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-10 deposited with the CCDC.
2017-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                85.606(2)
_cell_angle_beta                 78.603(2)
_cell_angle_gamma                86.931(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0847(5)
_cell_length_b                   12.4493(5)
_cell_length_c                   12.9847(5)
_cell_measurement_reflns_used    9660
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.425
_cell_volume                     1907.87(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            86722
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    2.407
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       prism
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.209
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0327P)^2^+8.9320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7764
_reflns_number_total             8790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01797a2.cif
_cod_data_source_block           do3aidpcu
_cod_original_formula_sum        'C20 H54 Cl Cu4 N5 O24.50 P'
_cod_database_code               7043659
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.633
_shelx_res_checksum              44104