Oxamidate-Bridged Dinuclear Five-Coordinate Nickel(II) Complexes: A Magneto-Structural Study
M. Dolores Santana; Gabriel García; Miguel Julve; Francesc Lloret; José Pérez; Malva Liu; Francisco Sanz; Joan Cano; Gregorio López; Inorganic Chemistry 43 (2004) 2132–2140; doi:10.1021/ic030050f

data_4310686
_publ_section_title
;
 Oxamidate-Bridged Dinuclear Five-Coordinate Nickel(II) Complexes: A
 Magneto-Structural Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2132
_journal_page_last               2140
_journal_paper_doi               10.1021/ic030050f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C26 H52 F12 N8 Ni2 O2 P2'
_chemical_formula_sum            'C26 H52 F12 N8 Ni2 O2 P2'
_chemical_formula_weight         916.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.46(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.901(4)
_cell_length_b                   13.597(6)
_cell_length_c                   17.565(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1875.0(17)
_computing_molecular_graphics    'CAMERON(D.J. Watkin and L.J. Pearce)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.955
_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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4313
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                1484
_reflns_number_total             2577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030050f_1.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4310686