Magnetic Ordering in Two Molecule-Based (10,3)-a Nets Prepared from a Copper(II) Trinuclear Secondary Building Unit
Beatriz Gil-Hernández; Pedro Gili; Jana K. Vieth; Christoph Janiak; Joaquín Sanchiz; Inorganic Chemistry 49 (2010) 7478–7490; doi:10.1021/ic100796e

data_4316269
_publ_section_title
;
 Magnetic Ordering in Two Molecule-Based (10,3)-a Nets Prepared from a
 Copper(II) Trinuclear Secondary Building Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7478
_journal_page_last               7490
_journal_paper_doi               10.1021/ic100796e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'2(C18 H6 Cu6 K Mn2 O36), K O14.04, K O9, 12(C2 O), 12(O0.50), O4.08'
_chemical_formula_sum            'C60 H12 Cu12 K4 Mn4 O117.12'
_chemical_formula_weight         3745.38
_chemical_name_systematic
; 
catena-{hemi(hexaaquapotassium)-hemi[(18-crown-6)potassium]-
[(\m-mesoxalato-\kO,O'':O':O'':O''',O'''':O''''')tricopper-
manganese]}.5.25hydrate,
with H2 on crystal water and 18-c-6 included for calculation:
C15 H31.50 Cu3 K Mn O29.25, M = 964.56, 
Z = 8, F(000) = 3892, Dx = 2.075 g/cm-3, kmin -20, lmin -19 
hmax 19, kmax 15 lmax5
C36 H12 Cu12 Mn4 O72, 12(C2 O), K O3, 12(O1.17), 16.08(O), 3(K) 
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.346(2)
_cell_length_b                   18.346(2)
_cell_length_c                   18.346(2)
_cell_measurement_reflns_used    1989
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      4.1
_cell_volume                     6174.8(12)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_sigmaI/netI    0.1374
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7060
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.686
_exptl_absorpt_correction_T_max  0.8138
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             3665.6
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+5.0478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                1167
_reflns_number_total             1981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100796e_si_002_1.cif
_cod_data_source_block           C60H12Cu12K4Mn4O117.12
_cod_original_sg_symbol_Hall     '-P 2ac 2ab'
_cod_database_code               4316269