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_4322853
_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
'[Ni5(C6H4N3)5(C5H7O2)2(OH)(H2O)4].4(C3H6O).0.5(C6H14)'
_chemical_formula_structural
'[Ni(bta)5(acac)5(OH)(H2O)4].4(aceton).0.5(hexane)'
_chemical_formula_sum            'C65 H88 N15 Ni5 O17'
_chemical_formula_weight         1645.07
_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
_cell_angle_alpha                89.02(1)
_cell_angle_beta                 104.76(2)
_cell_angle_gamma                111.78(1)
_cell_formula_units_Z            2
_cell_length_a                   13.855(1)
_cell_length_b                   12.013(1)
_cell_length_c                   25.611(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     3813.5(7)
_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
_computing_structure_solution    SHELXS-92
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'P21 Nicolet'
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11263
_diffrn_reflns_theta_max         23.20
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  1.28
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      1.41
_exptl_crystal_density_method    'floating method'
_exptl_crystal_F_000             1718
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.542
_refine_ls_goodness_of_fit_obs   0.888
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         10709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.632
_refine_ls_restrained_S_obs      0.888
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_obs          0.0514
_refine_ls_shift/esd_max         0.098
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2742
_refine_ls_wR_factor_obs         0.1297
_reflns_number_observed          7979
_reflns_number_total             10713
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9714091_1.cif
_cod_data_source_block           peed15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+37.0009P] 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^)+(0.0405P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3813.3(4)
_cod_database_code               4322853