Induction of Λ-helicity in a zinc complex with an alanine-appended aminopyridine ligand
Perić, Berislav; Kokan, Zoran; Kirin, Srećko I.; Acta Crystallographica Section C 77 (2021) –; doi:10.1107/S2053229621006471

data_2022399
_publ_section_title
;
 Induction of \L-helicity in a zinc complex with an alanine-appended
 aminopyridine ligand
;
_journal_coeditor_code           EF3020
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229621006471
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_iupac          '[Zn (C19 H19 N3 O6)3] (N O3)2, 3C2 H3 N'
_chemical_formula_moiety         'C57 H57 N9 O18 Zn 2+, 2(N O3 -), 3(C2 H3 N)'
_chemical_formula_sum            'C63 H66 N14 O24 Zn'
_chemical_formula_weight         1468.66
_chemical_name_systematic
;Tris[dimethyl
5-({1-[(pyridin-2-yl-\k<i>N</i>)carbamoyl-\k<i>O</i>]ethyl}carbamoyl)benzene-1,3-dicarboxylate]zinc(II) dinitrate acetonitrile trisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.524(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5897(2)
_cell_length_b                   22.8595(5)
_cell_length_c                   14.3102(3)
_cell_measurement_reflns_used    8319
_cell_measurement_temperature    136(2)
_cell_measurement_theta_max      74.4630
_cell_measurement_theta_min      3.6400
_cell_volume                     3460.78(12)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      136(2)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Agilent Xcalibur Nova diffractometer with a Ruby detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19332
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.536
_diffrn_reflns_theta_min         3.091
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.661
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3017 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         10880
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0770P)^2^+1.8689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                10178
_reflns_number_total             10880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3020sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2022399
_shelx_hkl_checksum              21018
_shelx_res_checksum              36304
_cod_database_fobs_code 2022399