Coordination features of ditopic oxa-azamacrocycles toward Ni(II) and Co(II). Dioxygen uptake by their dinuclear Co(II) complexes.
Bazzicalupi, Carla; Bencini, Andrea; Bianchi, Antonio; Duce, Celia; Fornasari, Patrizia; Giorgi, Claudia; Paoletti, Piero; Pardini, Rodolfo; Rosaria Tinè, Maria; Valtancoli, Barbara; Dalton transactions (Cambridge, England : 2003)  (2004) 463–469; doi:10.1039/b312751f

data_7013707
_publ_section_title
;
 Coordination features of ditopic oxa-azamacrocycles toward Ni(II) and
 Co(II). Dioxygen uptake by their dinuclear Co(II) complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              463
_journal_page_last               469
_journal_paper_doi               10.1039/b312751f
_journal_year                    2004
_chemical_formula_moiety
;
(C20 H54 Br2 N6 Ni2 O8 2+), (Br 1-)2, (H2 O)2
;
_chemical_formula_sum            'C20 H58 Br4 N6 Ni2 O10'
_chemical_formula_weight         979.78
_chemical_name_systematic
;
[Ni2L1Br2(H2O)4]Br2.2H2O
(L1=1,4,7,16,19,22-hexaza-10,13,25,28-tetraoxacyclotriacontane)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 100.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.354(3)
_cell_length_b                   18.862(3)
_cell_length_c                   12.057(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    298
_cell_measurement_theta_max      25
_cell_measurement_theta_min      17
_cell_volume                     1865.3(10)
_computing_cell_refinement       'XSCANS BRUKER'
_computing_data_collection       'XSCANS BRUKER'
_computing_data_reduction        'XSCANS BRUKER'
_computing_molecular_graphics    'ORTEP3 Ver. 1.01\b (Farrugia, 1997)'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'siemens P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3535
_diffrn_reflns_theta_full        60.04
_diffrn_reflns_theta_max         60.04
_diffrn_reflns_theta_min         4.41
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.716
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.840
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+7.1138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                2162
_reflns_number_total             2690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312751f.txt
_cod_data_source_block           '[Ni2L1Br2(H2O)4]Br2.2H2O'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7013707