Polynuclear Nickel(II) Complexes: Preparation, Characterization, Magnetic Properties, and Quantum-Chemical Study of [Ni5(OH)(Rbta)5(acac)4(H2O)4] (RbtaH = Benzotriazole and 5,6-Dimethylbenzotriazole)
Vasilis Tangoulis; Catherine P. Raptopoulou; Aris Terzis; Evangelos G. Bakalbassis; Eleanna Diamantopoulou; Spyros P. Perlepes; Inorganic Chemistry 37 (1998) 3142–3153; doi:10.1021/ic9714091

data_4322854
_publ_section_title
;
 Polynuclear Nickel(II) Complexes: Preparation, Characterization, Magnetic
 Properties, and Quantum-Chemical Study of [Ni5(OH)(Rbta)5(acac)4(H2O)4]
 (RbtaH = Benzotriazole and 5,6-Dimethylbenzotriazole)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3142
_journal_page_last               3153
_journal_paper_doi               10.1021/ic9714091
_journal_volume                  37
_journal_year                    1998
_chemical_formula_analytical     '[Ni(C8H8N3)5(C5H7O2)4(OH)(H2O)4].4(C3H6O)'
_chemical_formula_structural     '[Ni(diMebta)5(acac)4(OH)(H2O)].4(aceton)'
_chemical_formula_sum            'C72 H101 N15 Ni5 O17'
_chemical_formula_weight         1742.23
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.30(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.085(3)
_cell_length_b                   20.142(3)
_cell_length_c                   22.574(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     8445(2)
_computing_cell_refinement       'Program LEAST (UCLA Crystallographic Package)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic Package)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic Package)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Crystal Logic Dual Goniometer Diffractometer'
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5714
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        -2.6
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  1.07
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      1.35
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         5520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_obs          0.0297
_refine_ls_shift/esd_max         -0.082
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+8.5420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0835
_refine_ls_wR_factor_obs         0.0735
_reflns_number_observed          4337
_reflns_number_total             5520
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9714091_2.cif
_cod_data_source_block           shel93
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+8.5420P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+8.5420P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322854