A hexacarboxylic open-shell building block: synthesis, structure and magnetism of a three-dimensional metal‒radical framework
Roques, Nans; Maspoch, Daniel; Luis, Fernando; Camón, Agustín; Wurst, Klaus; Datcu, Angela; Rovira, Concepció; Ruiz-Molina, Daniel; Veciana, Jaume; Journal of Materials Chemistry 18 (2008) 98–; doi:10.1039/b713705b

data_7201721
_publ_section_title
;
 A hexacarboxylic open-shell building block: synthesis, structure and
 magnetism of a three-dimensional metal--radical framework
;
_journal_issue                   1
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              98
_journal_paper_doi               10.1039/b713705b
_journal_volume                  18
_journal_year                    2008
_chemical_formula_sum            'C89.6 H76.4 Cl18 Cu6 N6 O43'
_chemical_formula_weight         2944.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.3534(4)
_cell_length_b                   22.3534(3)
_cell_length_c                   41.1462(3)
_cell_measurement_reflns_used    61114
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     17805.2(4)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            33151
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    'constr, omitted at water and THF molecules'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1194P)^2^+138.0242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.1973
_reflns_number_gt                2907
_reflns_number_total             3483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713705b.txt
_cod_data_source_block           rn59
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        'C89.60 H76.40 Cl18 Cu6 N6 O43'
_cod_database_code               7201721