Zero-Field Splitting in a Series of Structurally Related Mononuclear NiII-Bispidine Complexes
Mihail Atanasov; Peter Comba; Stefan Helmle; Dennis Müller; Frank Neese; Inorganic Chemistry 51 (2012) 12324–12335; doi:10.1021/ic3016047

data_4331055
_publ_contact_author_address
;Universit\"at Heidelberg, Anorganisch-Chemisches Institut,
INF 270, D-69120 Heidelberg, Germany
;
_publ_contact_author_email       peter.comba@aci.uni-heidelberg.de
_publ_contact_author_fax         49-6226-546617
_publ_contact_author_name        'Professor Peter Comba'
_publ_section_title
;
 Zero-Field Splitting in a Series of Structurally Related Mononuclear
 NiII-Bispidine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12324
_journal_page_last               12335
_journal_paper_doi               10.1021/ic3016047
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H38 F12 N6 Ni O6 P2'
_chemical_formula_weight         951.33
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P -2bc -2c'
_symmetry_space_group_name_H-M   'P c 21 b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                chb345
_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                   9.2105(9)
_cell_length_b                   13.5475(10)
_cell_length_c                   31.361(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      60.9
_cell_measurement_theta_min      5.3
_cell_volume                     3913.2(5)
_computing_cell_refinement       'STOE XCELL'
_computing_data_collection       'STOE EXPOSE'
_computing_data_reduction        XRED
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       'image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            31016
_diffrn_reflns_theta_full        30.46
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         2.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.8798
_exptl_absorpt_correction_T_min  0.7862
_exptl_absorpt_correction_type   numerically
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.188
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9899
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                7172
_reflns_number_total             9899
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3016047_si_001_1.cif
_cod_data_source_block           chb345
_cod_database_code               4331055