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_4517221
_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_formula_moiety         '2(C22 H26 Fe N4 O7), 2(N O3), 8(O), 3(H2 O)'
_chemical_formula_sum            'C44 H58 Fe2 N10 O31'
_chemical_formula_weight         1334.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 105.176(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1188(8)
_cell_length_b                   18.1908(12)
_cell_length_c                   14.0536(9)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      74.6
_cell_measurement_theta_min      4.1
_cell_volume                     2990.1(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      125.68
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.567
_diffrn_reflns_theta_min         4.065
_exptl_absorpt_coefficient_mu    4.759
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.3689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1460 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.4894.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.398
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6110
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0601P)^2^+2.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5727
_reflns_number_total             6110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03164_si_002.cif
_cod_data_source_block           '[Fe(edtabz)]'
_cod_depositor_comments
'Adding full bibliography for 4517219--4517221.cif.'
_cod_database_code               4517221
_shelx_estimated_absorpt_t_max   0.410
_shelx_estimated_absorpt_t_min   0.221
_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,H) groups
2. Restrained distances
 OW1-HW1A = OW1-HW1B = OW3-HW3A = OW3-HW3B = OW6-HW6A = OW6-HW6B
 0.85 with sigma of 0.001
3. Restrained planarity
 N5A, ON1A, ON2A, ON3A
 with sigma of 0.001
 N5B, ON1B, ON2B, ON3B
 with sigma of 0.001
4. Rigid bond restraints
 N5A, ON1A, ON2A, ON3A, N5B, ON1B, ON2B, ON3B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
OW7A \\sim OW7B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
6. Others
 Sof(N5B)=Sof(ON1B)=Sof(ON2B)=Sof(ON3B)=1-FVAR(1)
 Sof(N5A)=Sof(ON1A)=Sof(ON2A)=Sof(ON3A)=FVAR(1)
 Sof(OW2B)=1-FVAR(2)
 Sof(OW2A)=FVAR(2)
 Sof(OW4B)=1-FVAR(3)
 Sof(OW4A)=FVAR(3)
 Sof(OW5B)=1-FVAR(4)
 Sof(OW5A)=FVAR(4)
 Sof(OW7B)=1-FVAR(5)
 Sof(OW7A)=FVAR(5)
 Fixed Sof: OW3(0.5) HW3A(0.5) HW3B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B)
7.b 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)
;
_shelx_res_checksum              41221
_shelx_hkl_checksum              66565
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'