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_4332122
_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            'C68 H140 Ni7 O34.5'
_chemical_formula_weight         1920.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1272(8)
_cell_length_b                   26.9340(15)
_cell_length_c                   27.2743(16)
_cell_measurement_reflns_used    6391
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.08
_cell_measurement_theta_min      2.15
_cell_volume                     11112.5(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48730
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4080
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(16)
_refine_ls_extinction_coef       0.00038(5)
_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   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         16038
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          9.453
_refine_ls_shift/su_mean         0.164
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                12476
_reflns_number_total             16038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0522028sup1.cif
_cod_data_source_block           Ni7_RT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C68 H140 Ni7 O34.50'
_cod_database_code               4332122