The self-assembly and magnetic properties of a Ni(II)8(micro4-hydroxo)6 cube with micro2-pyrazolate as an exogeneous ancillary ligand.
Xu, Jing-Yuan; Qiao, Xin; Song, Hai-Bin; Yan, Shi-Ping; Liao, Dai-Zheng; Gao, Song; Journaux, Yves; Cano, Joan; Chemical communications (Cambridge, England)  (2008) 6414–6416; doi:10.1039/b813705f

data_7103592
_publ_section_title
;
 The self-assembly and magnetic properties of a
 Ni(II)8(micro4-hydroxo)6 cube with micro2-pyrazolate as an exogeneous
 ancillary ligand.
;
_journal_issue                   47
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6414
_journal_page_last               6416
_journal_paper_doi               10.1039/b813705f
_journal_year                    2008
_chemical_formula_moiety
'C36 H42 N24 Ni8 O6, C16 H21 N5 Ni O3, 6(C2 H6 O S)'
_chemical_formula_sum            'C64 H99 N29 Ni9 O15 S6'
_chemical_formula_weight         2235.47
_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                81.716(9)
_cell_angle_beta                 79.430(8)
_cell_angle_gamma                77.472(10)
_cell_formula_units_Z            1
_cell_length_a                   13.118(2)
_cell_length_b                   13.782(2)
_cell_length_c                   15.595(3)
_cell_measurement_reflns_used    8422
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.1
_cell_volume                     2689.6(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22203
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  0.8471
_exptl_absorpt_correction_T_min  0.7708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.0174(11)
_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   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10475
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+15.9711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                8891
_reflns_number_total             10475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813705f.txt
_cod_data_source_block           shelxl
_cod_database_code               7103592