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_7017311
_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_sum            'C40 H102 Ni9 O40'
_chemical_formula_weight         1751.61
_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                85.585(2)
_cell_angle_beta                 80.224(2)
_cell_angle_gamma                71.235(3)
_cell_formula_units_Z            1
_cell_length_a                   11.0288(5)
_cell_length_b                   12.1147(5)
_cell_length_c                   14.1046(5)
_cell_measurement_reflns_used    1856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.257
_cell_measurement_theta_min      2.27
_cell_volume                     1757.94(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52676
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.443
_exptl_absorpt_correction_T_max  0.8476
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2004
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0347P)^2^+2.8641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                5493
_reflns_number_total             7174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10993f.txt
_cod_data_source_block           newni9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1757.94(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7017311