Synthesis, Structure, and Magnetic Properties of (6−9)-Nuclear Ni(II) Trimethylacetates and Their Heterospin Complexes with Nitroxides
Ovcharenko, Victor; Fursova, Elena; Romanenko, Galina; Eremenko, Igor; Tretyakov, Evgeny; Ikorskii, Vladimir; Inorganic Chemistry 45 (2006) 5338–5350; doi:10.1021/ic0522028

data_4332114
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of (6&#x2212;9)-Nuclear
 Ni(II) Trimethylacetates and Their Heterospin Complexes with Nitroxides
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5338
_journal_page_last               5350
_journal_paper_doi               10.1021/ic0522028
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C66.5 H117 N4 Ni4 O23'
_chemical_formula_weight         1575.48
_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                95.948(5)
_cell_angle_beta                 95.077(5)
_cell_angle_gamma                102.827(6)
_cell_formula_units_Z            2
_cell_length_a                   14.719(4)
_cell_length_b                   16.350(4)
_cell_length_c                   19.068(5)
_cell_measurement_reflns_used    2008
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.21
_cell_measurement_theta_min      2.37
_cell_volume                     4421(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.1268
_diffrn_reflns_av_sigmaI/netI    0.2142
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19267
_diffrn_reflns_theta_full        23.44
_diffrn_reflns_theta_max         23.44
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     996
_refine_ls_number_reflns         12758
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1876
_refine_ls_R_factor_gt           0.1141
_refine_ls_shift/su_max          1.879
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2569
_reflns_number_gt                6938
_reflns_number_total             12758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0522028sup1.cif
_cod_data_source_block           Ni4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4421.0(19)
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C66.50 H117 N4 Ni4 O23'
_cod_database_code               4332114