Structural Diversity due to Amino Alcohol Ligands Leading to Rare μ4-Hydroxo-Bridged Tetranuclear and "Bicapped Cubane" Cores in Copper(II) Complexes: A Theoretical and Experimental Magnetostructural Study
Petri Seppälä; Enrique Colacio; Antonio J. Mota; Reijo Sillanpää; Inorganic Chemistry 52 (2013) 11096–11109; doi:10.1021/ic401325b

data_4336178
_publ_contact_author_address
;
Department of Chemistry
University of Jyv\"askyl\"a
P.O.Box 35
FI-40014 University of Jyv\"askyl\"a
Finland
;
_publ_contact_author_email       resillan@jyu.fi
_publ_contact_author_fax         '+358 14 260 1021'
_publ_contact_author_name        'Sillanp\"a\"a, Reijo'
_publ_section_title
;
 Structural Diversity due to Amino Alcohol Ligands Leading to Rare
 \m4-Hydroxo-Bridged Tetranuclear and "Bicapped Cubane" Cores in
 Copper(II) Complexes: A Theoretical and Experimental Magnetostructural
 Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11096
_journal_page_last               11109
_journal_paper_doi               10.1021/ic401325b
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H41 Cu4 N8 Na1 O17'
_chemical_formula_sum            'C16 H41 Cu4 N8 Na O17'
_chemical_formula_weight         894.72
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2012-06-21T14:44:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1240(5)
_cell_length_b                   13.1240(5)
_cell_length_c                   9.4257(2)
_cell_measurement_reflns_used    2132
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     1623.48(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.16874E-1
_diffrn_orient_matrix_UB_12      0.246746E-1
_diffrn_orient_matrix_UB_13      0.975877E-1
_diffrn_orient_matrix_UB_21      -0.742411E-1
_diffrn_orient_matrix_UB_22      -0.26332E-2
_diffrn_orient_matrix_UB_23      -0.235963E-1
_diffrn_orient_matrix_UB_31      -0.30658E-2
_diffrn_orient_matrix_UB_32      -0.720424E-1
_diffrn_orient_matrix_UB_33      0.342864E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16294
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.68
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker (2001). SADABS-2008/1. Bruker AXS Inc., Madison, Wisconsin, USA.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.83
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.72
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1593
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.0160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                1419
_reflns_number_total             1593
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic401325b_si_002_3.cif
_cod_data_source_block           import_Complex2
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4336178