Metal-Metal Interactions in Trinuclear Copper(II) Complexes [Cu3(RCOO)4(H2TEA)2] and Binuclear [Cu2(RCOO)2(H2TEA)2]. Syntheses and Combined Structural, Magnetic, High-Field Electron Paramagnetic Resonance, and Theoretical Studies.
Ozarowski, Andrew; Calzado, Carmen J.; Sharma, Raj Pal; Kumar, Santosh; Jezierska, Julia; Angeli, Celestino; Spizzo, Federico; Ferretti, Valeria; Inorganic chemistry 54 (2015) 11916–11934; doi:10.1021/acs.inorgchem.5b02199

data_4346821
_publ_section_title
;
 Metal-Metal Interactions in Trinuclear Copper(II) Complexes
 [Cu3(RCOO)4(H2TEA)2] and Binuclear [Cu2(RCOO)2(H2TEA)2]. Syntheses and
 Combined Structural, Magnetic, High-Field Electron Paramagnetic
 Resonance, and Theoretical Studies.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11916
_journal_page_last               11934
_journal_paper_doi               10.1021/acs.inorgchem.5b02199
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C44 H56 Cu3 N2 O18'
_chemical_formula_sum            'C44 H56 Cu3 N2 O18'
_chemical_formula_weight         1091.52
_chemical_name_systematic
;
[Cu3(m-methoxy-carboxylato)4(H2-triethanolamine)2]
;
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.1420(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4231(1)
_cell_length_b                   13.4250(1)
_cell_length_c                   26.0803(3)
_cell_measurement_reflns_used    40773
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.
_cell_measurement_theta_min      2.0
_cell_volume                     4652.43(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
;
 SHELXL-2014/7 (Sheldrick, 2014); WINGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al.,1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            40773
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.350
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         11114
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8061
_reflns_number_total             11114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02199_si_004.cif
_cod_data_source_block           CuTEA3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4346821
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              22616
_shelx_hkl_checksum              13059