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_7711592
_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
'C60 H68 N8 Ni O10 2+, 2(Cl O4 -), 4.35(C H3 N O2)'
_chemical_formula_sum            'C64.35 H81.05 Cl2 N12.35 Ni O26.7'
_chemical_formula_weight         1584.37
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_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                114.840(3)
_cell_angle_beta                 110.408(3)
_cell_angle_gamma                95.136(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8136(3)
_cell_length_b                   14.3149(4)
_cell_length_c                   14.8173(5)
_cell_measurement_reflns_used    12235
_cell_measurement_temperature    136(11)
_cell_measurement_theta_max      75.4700
_cell_measurement_theta_min      4.4410
_cell_volume                     1874.20(13)
_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      136(11)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.979
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18687
_diffrn_reflns_point_group_measured_fraction_full 0.604
_diffrn_reflns_point_group_measured_fraction_max 0.589
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.861
_diffrn_reflns_theta_min         4.442
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85781
_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            purple
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       prism
_exptl_crystal_F_000             829
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.008(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         9207
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1095P)^2^+0.7810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.204
_reflns_Friedel_fraction_full    0.218
_reflns_Friedel_fraction_max     0.200
_reflns_number_gt                9000
_reflns_number_total             9207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02895f3.cif
_cod_data_source_block           i3BNi
_cod_original_cell_volume        1874.20(11)
_cod_original_formula_sum        'C64.35 H81.05 Cl2 N12.35 Ni O26.70'
_cod_database_code               7711592
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              82893
_shelx_hkl_checksum              12373