Self-Assembled Dinuclear, Trinuclear, Tetranuclear, Pentanuclear, and Octanuclear Ni(II) Complexes of a Series of Polytopic Diazine Based Ligands: Structural and Magnetic Properties
Zhiqiang Xu; Laurence K. Thompson; Victoria A. Milway; Liang Zhao; Timothy Kelly; David O. Miller; Inorganic Chemistry 42 (2003) 2950–2959; doi:10.1021/ic0206950

data_4313544
_publ_section_title
;
 Self-Assembled Dinuclear, Trinuclear, Tetranuclear, Pentanuclear, and
 Octanuclear Ni(II) Complexes of a Series of Polytopic Diazine Based
 Ligands: Structural and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2950
_journal_page_last               2959
_journal_paper_doi               10.1021/ic0206950
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C44 H71.5 N31 Ni5 O44'
_chemical_formula_weight         2032.37
_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                100.3950(10)
_cell_angle_beta                 109.5140(10)
_cell_angle_gamma                109.6860(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6677(8)
_cell_length_b                   18.1101(11)
_cell_length_c                   19.9980(12)
_cell_measurement_temperature    193(2)
_cell_volume                     3843.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26029
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  0.86169
_exptl_absorpt_correction_T_min  0.72387
_exptl_absorpt_process_details   'Gaussian integration (face indexed)'
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2089
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         15519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+0.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                10422
_reflns_number_total             15519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206950_4.cif
_cod_data_source_block           shelxl(4)
_cod_original_formula_sum        'C44 H71.50 N31 Ni5 O44'
_cod_database_code               4313544