Crystal Structures and Magnetic Properties of Nickel Complexes with Hydrotris(pyrazolyl)borate Ligand and Double Bridged by Phosphate Esters
Luisa López-Banet; M. Dolores Santana; Gabriel García; Luis García; José Pérez; Teófilo Rojo; Luis Lezama; Jean-Pierre Costes; Inorganic Chemistry 50 (2011) 437–443; doi:10.1021/ic100980x

data_4324190
_publ_section_title
;
 Crystal Structures and Magnetic Properties of Nickel Complexes with
 Hydrotris(pyrazolyl)borate Ligand and Double Bridged by Phosphate Esters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              437
_journal_page_last               443
_journal_paper_doi               10.1021/ic100980x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C46 H80 B2 N12 Ni2 O8 P2'
_chemical_formula_sum            'C46 H80 B2 N12 Ni2 O8 P2'
_chemical_formula_weight         1130.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           135
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2ab'
_symmetry_space_group_name_H-M   'P 42/m b c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.533
_cell_length_b                   16.533
_cell_length_c                   20.512
_cell_measurement_temperature    100(2)
_cell_volume                     5606.752
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.976
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61075
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.303
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0845P)^2^+11.3775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                3171
_reflns_number_total             3478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100980x_si_001_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        5606.6
_cod_database_code               4324190