Unprecedented tetranuclear complexes "weighing balance shaped" topology: Single crystal structures, unusual EPR spectra, magnetic properties and antioxidant activity
Singh, Yogendra; Patel, Ram Niwas; Singh, Yogendra Pratap; Patel, Abhay Kumar; Patel, N.; Singh, Rita; Jasinski, Jerry P.; Butcher, R. J.; Colacio, Enrique; Palacios, Maria A.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02595E

data_7043950
_publ_section_title
;
 Unprecedented tetranuclear complexes "weighing balance shaped" topology:
 Single crystal structures, unusual EPR spectra, magnetic properties and
 antioxidant activity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02595E
_journal_year                    2017
_chemical_formula_moiety         '2(C79 H60 Cu4 N12 O15), 4(N O3), 7(H2 O)'
_chemical_formula_sum            'C79 H67 Cu4 N14 O24.5'
_chemical_formula_weight         1858.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-07 deposited with the CCDC.
2017-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                110.553(2)
_cell_angle_beta                 105.564(2)
_cell_angle_gamma                95.942(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7802(3)
_cell_length_b                   18.3127(4)
_cell_length_c                   20.1463(6)
_cell_measurement_reflns_used    12212
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.2910
_cell_measurement_theta_min      3.5290
_cell_volume                     4149.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    Shelxt
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27533
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         32.822
_diffrn_reflns_theta_min         3.002
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale blue-green'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description
'The symmetry employed for this shelxl refinement is uniquely definedby the following loop, which should always be used as a source ofsymmetry information in preference to the above space-group names.They are only intended as comments.'
_exptl_crystal_F_000             1902
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         27533
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+2.2089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15545
_reflns_number_total             27533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02595e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        4149.59(19)
_cod_original_formula_sum        'C79 H67 Cu4 N14 O24.50'
_cod_database_code               7043950
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              67192