Novel Polynuclear Nickel(II) Complex: Hydrazine, Sulfato, and Hydroxo Bridging in an Unusual Metal Hexamer. Crystal Structure and Magnetic Properties of [Ni6(N2H4)6(SO4)4(OH)2(H2O)8](SO4)(H2O)10
Magnus Gustafsson; Andreas Fischer; Andrey Ilyukhin; Mikhail Maliarik; Per Nordblad; Inorganic Chemistry 49 (2010) 5359–5361; doi:10.1021/ic100648c

data_4315832
_publ_contact_author_address
;Department of Chemistry, 
Link\"oping University,
SE-581 83 Link\"oping,
Sweden
;
_publ_contact_author_email       mikhail.maliarik@hotmail.com
_publ_contact_author_name        'Mikhail Maliarik '
_publ_section_title
;
 Novel Polynuclear Nickel(II) Complex: Hydrazine, Sulfato, and Hydroxo
 Bridging in an Unusual Metal Hexamer. Crystal Structure and Magnetic
 Properties of [Ni6(N2H4)6(SO4)4(OH)2(H2O)8](SO4)(H2O)10
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5359
_journal_page_last               5361
_journal_paper_doi               10.1021/ic100648c
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'H62 N12 Ni6 O40 S5'
_chemical_formula_sum            'H62 N12 Ni6 O40 S5'
_chemical_formula_weight         1383.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2006-07-20T17:13:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                60.19(2)
_cell_angle_beta                 71.96(2)
_cell_angle_gamma                69.23(2)
_cell_formula_units_Z            1
_cell_length_a                   10.965(2)
_cell_length_b                   11.214(3)
_cell_length_c                   11.306(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      25.4
_cell_measurement_wavelength     1.54184
_cell_volume                     1112.5(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.067196
_diffrn_orient_matrix_UB_12      0.024421
_diffrn_orient_matrix_UB_13      0.072489
_diffrn_orient_matrix_UB_21      -0.006445
_diffrn_orient_matrix_UB_22      0.103204
_diffrn_orient_matrix_UB_23      -0.062176
_diffrn_orient_matrix_UB_31      -0.072106
_diffrn_orient_matrix_UB_32      0.003475
_diffrn_orient_matrix_UB_33      -0.039107
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.074
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7537
_diffrn_reflns_theta_full        70.11
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         4.37
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.084
_exptl_absorpt_correction_T_max  0.7651
_exptl_absorpt_correction_T_min  0.3427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                3514
_reflns_number_total             4206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100648c_si_002.cif
_cod_data_source_block           ni01
_cod_database_code               4315832