Synthesis, structural and electrochemical properties of a new family of amino-acid-based coordination complexes
Rey, Juan Manuel; Movilla, Federico; Suárez, Sebastián Angel; Di Salvo, Florencia; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520622003912

data_2108984
_publ_section_title
;
 Synthesis, structural and electrochemical properties of a new family of
 amino-acid-based coordination complexes
;
_journal_coeditor_code           LO5107
_journal_issue                   '3 Part 2'
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622003912
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C34 H33 N2 O9 Zn, C34 H34 N2 O9 Zn'
_chemical_formula_sum            'C68 H67 N4 O18 Zn2'
_chemical_formula_weight         1358.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-18 deposited with the CCDC. 2021-09-02 downloaded from the CCDC.

2022-04-27 # Formatted by IUCr publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 92.48(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.050(8)
_cell_length_b                   8.110(3)
_cell_length_c                   31.470(18)
_cell_measurement_reflns_used    5621
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      1
_cell_measurement_theta_min      0.8324
_cell_volume                     3073(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'MXCuBE (Gabadinho et al., 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'custom air-bearing with MK3 mini-kappa'
_diffrn_measurement_method       'shuterless \f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82612
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            56923
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.506
_diffrn_source                   LNLS-MX2
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       prism
_exptl_crystal_F_000             1414
_exptl_crystal_recrystallization_method 'Gel crystallization'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.603
_refine_diff_density_min         -2.107
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 1605 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0912
_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^)+(0.1340P)^2^+32.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3886
_reflns_number_total             4431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5107sup1.cif
_cod_data_source_block           zn_phepip
_cod_database_code               2108984
_publcif_datablock.id            {9fab5d5e-c9a8-4ca6-846e-d0f89e5e36cf}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.904
_exptl_absorpt_special_details
;
_exptl_absorpt_correction_T_min and _exptl_absorpt_correction_T_max
from ABSORP.cbf, the absorption factors used by XDS.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained planarity
 C69, C72, C75, C77, C83, C84
 with sigma of 0.1
 C78, C79, C80, C81, C82, C85
 with sigma of 0.1
 C4, C20, C28, C40, C44, C56
 with sigma of 0.1
 C12, C32, C48, C52, C64, C68
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C20 \\sim C56: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C20 \\sim C40 \\sim C56: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O18: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Zn1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O24(0.5) H24(0.5) H18A(0.5) H18B(0.5)
5.a Rotating group:
 O24(H24), O18(H18A,H18B)
5.b Ternary CH refined with riding coordinates:
 N4(H4), C16(H16), N5(H5), C73(H73)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C36(H36A,H36B), C60(H60A,H60B), C70(H70A,H70B), C71(H71A,H71B),
 C76(H76A,H76B)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4A), C12(H12), C20(H20), C32(H32), C44(H44), C52(H52), C64(H64), C68(H68),
  C69(H69), C72(H72), C75(H75), C77(H77), C78(H78), C81(H81), C84(H84), C85(H85)
;
_shelx_res_checksum              54003
_shelx_hkl_checksum              54358
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108984