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_4336432
_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            'C40 H61 Cl3 Mn4 N4 O22'
_chemical_formula_weight         1276.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.992(2)
_cell_angle_beta                 102.438(2)
_cell_angle_gamma                90.994(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6914(5)
_cell_length_b                   11.8134(5)
_cell_length_c                   20.2545(8)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.89
_cell_measurement_theta_min      2.26
_cell_volume                     2702.0(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58864
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details
; 
 The residual agreement factors were 
 R_factor_gt = 0.0899 and wR2_factor_gt = 0.2748 before SQUEEZE 
 whereas they were R_factor_gt = 0.0459 and wR2_factor_gt = 0.1305 
 after SQUEEZE. The final formulation of the compound is in agreement 
 with the residual electron density and volume.  
;
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         10193
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+2.6314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                7851
_reflns_number_total             10193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4016355_si_001.cif
_cod_data_source_block           mnb6p
_cod_original_cell_volume        2702.03(19)
_cod_database_code               4336432