Tuning the coordination properties of chiral pseudopeptide bis(2-picolyl)amine and iminodiacetamide ligands in Zn(ii) and Cu(ii) complexes
Pantalon Juraj, Natalija; Tandarić, Tana; Tadić, Vanja; Perić, Berislav; Moreth, Dominik; Schatzschneider, Ulrich; Brozovic, Anamaria; Vianello, Robert; Kirin, Srećko I.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02895F

data_7711591
_publ_section_title
;
 Tuning the coordination properties of chiral pseudopeptide
 bis(2-picolyl)amine and iminodiacetamide ligands in Zn(ii) and Cu(ii)
 complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02895F
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C56 H64 Cu N8 O6, 2(C F3 O3 S), 2(O H2)'
_chemical_formula_sum            'C58 H68 Cu F6 N8 O14 S2'
_chemical_formula_weight         1342.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-09 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.758(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.2084(4)
_cell_length_b                   10.2197(3)
_cell_length_c                   19.4085(6)
_cell_measurement_reflns_used    12094
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      75.4780
_cell_measurement_theta_min      3.7600
_cell_volume                     3684.28(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41089
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.654
_diffrn_reflns_theta_min         3.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.2069(1)
_exptl_crystal_description       prism
_exptl_crystal_F_000             1390.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Flack x determined using 3949 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         14307
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0974
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2806
_refine_ls_wR_factor_ref         0.2961
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.874
_reflns_Friedel_fraction_max     0.850
_reflns_number_gt                12262
_reflns_number_total             14307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02895f3.cif
_cod_data_source_block           i3ACu
_cod_original_sg_symbol_H-M      'P 2'
_cod_database_code               7711591
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              87464
_shelx_hkl_checksum              94360
_shelx_fab_checksum              36643