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_4331057
_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            'C25 H33 F6 N4 Ni O9 P'
_chemical_formula_weight         737.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_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
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.861(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6877(16)
_cell_length_b                   14.3209(14)
_cell_length_c                   19.184(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      61.1
_cell_measurement_theta_min      5.5
_cell_volume                     3103.6(8)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0941
_diffrn_reflns_av_sigmaI/netI    0.1352
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36710
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.74
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       shiver
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.770
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         9355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.770
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                4101
_reflns_number_total             9355
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3016047_si_001_3.cif
_cod_data_source_block           sh36
_cod_original_cell_volume        3103.6(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4331057