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_4324191
_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         'C54 H60 B2 N16 Ni2 O16 P2'
_chemical_formula_sum            'C54 H60 B2 N16 Ni2 O16 P2'
_chemical_formula_weight         1390.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.990(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6445(8)
_cell_length_b                   14.7369(18)
_cell_length_c                   21.543(2)
_cell_measurement_temperature    100(2)
_cell_volume                     3057.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.857
_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  0.0902
_diffrn_reflns_av_sigmaI/netI    0.2691
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21851
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.8464
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.656
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.656
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                2667
_reflns_number_total             7078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100980x_si_001_3.cif
_cod_data_source_block           3
_cod_database_code               4324191