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_4517219
_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         'C32 H36 Fe2 N8 O13, 4.4(H2 O)'
_chemical_formula_sum            'C32 H44.8 Fe2 N8 O17.4'
_chemical_formula_weight         931.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0203(18)
_cell_length_b                   18.028(2)
_cell_length_c                   22.855(3)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.68
_cell_volume                     7424.9(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.163
_diffrn_reflns_theta_min         1.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0607 before and 0.0353 after correction.
The Ratio of minimum to maximum transmission is 0.8687.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8231
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0258P)^2^+9.7507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7674
_reflns_number_total             8231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03164_si_004.cif
_cod_data_source_block           '[Fe(edtaod)]'
_cod_depositor_comments
'Adding full bibliography for 4517219--4517221.cif.'
_cod_original_cell_volume        7424.9(14)
_cod_original_formula_sum        'C32 H44.80 Fe2 N8 O17.40'
_cod_database_code               4517219
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.690
_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
 O2A-H4WB
 1.9 with sigma of 0.02
3. Others
 Fixed Sof: O5W(0.7) H5WA(0.7) H5WB(0.7) O4W(0.7) H4WA(0.7) H4WB(0.7)
4.a Free rotating group:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB), O1W(H1WA,H1WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB)
4.b Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C6A(H6AA,H6AB), C2B(H2BA,H2BB), C9A(H9AA,H9AB), C5A(H5AA,
 H5AB), C9B(H9BA,H9BB), C2A(H2AA,H2AB), C5B(H5BA,H5BB), C6B(H6BA,H6BB),
 C3A(H3AA,H3AB), C3B(H3BA,H3BB), C7B(H7BA,H7BB)
4.c Aromatic/amide H refined with riding coordinates:
 N4A(H4A), N4B(H4B), N1B(H1B), N1A(H1A), C16A(H16A), C16B(H16B), C13A(H13A),
 C14B(H14B), C13B(H13B), C15A(H15A), C15B(H15B), C14A(H14A)
;
_shelx_res_checksum              67292
_shelx_hkl_checksum              70076
_olex2_submission_special_instructions 'No special instructions were received'