Cubane-Type CuII4 and MnII2MnIII2 Complexes Based on Pyridoxine: A Versatile Ligand for Metal Assembling
Nadia Marino; Donatella Armentano; Teresa F. Mastropietro; Miguel Julve; Giovanni De Munno; José Martínez-Lillo; Inorganic Chemistry 52 (2013) 11934–11943; doi:10.1021/ic4016355

data_4336433
_publ_section_title
;
 Cubane-Type CuII4 and MnII2MnIII2 Complexes Based on Pyridoxine: A
 Versatile Ligand for Metal Assembling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11934
_journal_page_last               11943
_journal_paper_doi               10.1021/ic4016355
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C32 H44 Cl4 Cu4 N4 O14'
_chemical_formula_weight         1104.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            8
_cell_length_a                   31.315(2)
_cell_length_b                   13.7554(8)
_cell_length_c                   17.9847(8)
_cell_measurement_reflns_used    8967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.60
_cell_volume                     7746.9(8)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36901
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    2.516
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.7522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.311(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3728
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0502P)^2^+3.8363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                3198
_reflns_number_total             3728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4016355_si_002.cif
_cod_data_source_block           cub61
_cod_original_cell_volume        7747.0(8)
_cod_database_code               4336433