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_4324189
_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_sum            'C38 H70 B2 N12 Ni2 O8 P2'
_chemical_formula_weight         1024.04
_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                90.6430(10)
_cell_angle_beta                 100.9280(10)
_cell_angle_gamma                97.5660(10)
_cell_formula_units_Z            1
_cell_length_a                   8.1475(6)
_cell_length_b                   11.5772(9)
_cell_length_c                   13.3096(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1221.09(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.903
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14217
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.7503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0723P)^2^+4.3426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                4390
_reflns_number_total             5478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100980x_si_001_1.cif
_cod_data_source_block           1
_cod_database_code               4324189