Comparative Studies of Structures and Peroxidase-like Activities of Copper(II) and Iron(III) Complexes with an EDTA-Based Phenylene-Macrocycle and Its Acyclic Analogue
Beltran-Torres, Melissa; Sugich-Miranda, Rocío; Santacruz-Ortega, Hisila; Machi, Lorena; Inoue, Motomichi; Velázquez-Contreras, Enrique F.; Soberanes, Yedith; Höpfl, Herbert; Pérez-González, Refugio; Navarro, Rosa Elena; Salazar-Medina, Alex J.; Sotelo Mundo, Rogerio R.; ACS Omega 4 (2019) 22487–; doi:10.1021/acsomega.9b03164

data_4517220
_publ_section_title
;
 Comparative Studies of Structures and Peroxidase-like Activities of
 Copper(II) and Iron(III) Complexes with an EDTA-Based
 Phenylene-Macrocycle and Its Acyclic Analogue
;
_journal_issue                   27
_journal_name_full               'ACS Omega'
_journal_page_first              22487
_journal_paper_doi               10.1021/acsomega.9b03164
_journal_volume                  4
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H26 N4 O6, 2(H2 O)'
_chemical_formula_sum            'C22 H30 N4 O8'
_chemical_formula_weight         478.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3272(5)
_cell_length_b                   13.6323(10)
_cell_length_c                   23.8535(18)
_cell_measurement_reflns_used    6933
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      23.57
_cell_measurement_theta_min      2.27
_cell_volume                     2382.6(3)
_computing_cell_refinement       'Bruker SAINT version 6.01 and 6.04'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT version 6.01 and 6.04'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_min         1.707
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS was used for absorption correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1212 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0778
_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^)+(0.0471P)^2^+0.6912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4009
_reflns_number_total             4439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03164_si_003.cif
_cod_data_source_block           udlafunm
_cod_depositor_comments
'Adding full bibliography for 4517219--4517221.cif.'
_cod_database_code               4517220
_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.a Free rotating group:
 O31(H31A,H31B), O32(H32A,H32B)
2.b Ternary CH refined with riding coordinates:
 N2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4B,H4C), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B)
2.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_shelx_res_checksum              81900
_shelx_hkl_checksum              35909
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'