Microwave assisted synthesis and magnetic properties of octanuclear and enneanuclear Ni(ii) complexes: an unprecedented coordination mode for the NO(2)(-) ligand.
Pons-Balagué, Alba; Ioanidis, Nicoleta; Wernsdorfer, Wolfgang; Yamaguchi, Akira; Sañudo, E Carolina; Dalton transactions (Cambridge, England : 2003) 40 (2011) 11765–11769; doi:10.1039/c1dt10993f

data_7017312
_publ_section_title
;
 Microwave assisted synthesis and magnetic properties of octanuclear and
 enneanuclear Ni(ii) complexes: an unprecedented coordination mode for the
 NO(2)(-) ligand.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11765
_journal_page_last               11769
_journal_paper_doi               10.1039/c1dt10993f
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C106 H144 N8 Ni8 O34, 4(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C114 H160 N12 Ni8 O36'
_chemical_formula_weight         2731.99
_chemical_name_systematic
;
?
;
_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                 103.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.345(3)
_cell_length_b                   24.453(5)
_cell_length_c                   17.148(3)
_cell_measurement_reflns_used    1331
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      16.842
_cell_measurement_theta_min      2.443
_cell_volume                     6664(2)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1284
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6940
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.490
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.0833
_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^)+(0.1251P)^2^+33.6741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2594
_reflns_number_gt                3780
_reflns_number_total             6940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10993f.txt
_cod_data_source_block           ap1140new
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7017312