Investigating Magnetostructural Correlations in the Pseudooctahedral trans-[NiII{(OPPh2)(EPPh2)N}2(sol)2] Complexes (E = S, Se; sol = DMF, THF) by Magnetometry, HFEPR, and ab Initio Quantum Chemistry
Dimitrios Maganas; J. Krzystek; Eleftherios Ferentinos; Alexander M. Whyte; Neil Robertson; Vassilis Psycharis; Aris Terzis; Frank Neese; Panayotis Kyritsis; Inorganic Chemistry 51 (2012) 7218–7231; doi:10.1021/ic300453y

data_4329616
_publ_section_title
;
 Investigating Magnetostructural Correlations in the Pseudooctahedral
 trans-[NiII{(OPPh2)(EPPh2)N}2(sol)2] Complexes (E = S, Se; sol = DMF,
 THF) by Magnetometry, HFEPR, and ab Initio Quantum Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7218
_journal_page_last               7231
_journal_paper_doi               10.1021/ic300453y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C14 H14 N0.5 Ni0.25 O P S0.5'
_chemical_formula_weight         266.93
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.4250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.7934(2)
_cell_length_b                   9.49580(10)
_cell_length_c                   20.7500(3)
_cell_measurement_reflns_used    15174
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      133.90
_cell_measurement_theta_min      13.10
_cell_volume                     2619.92(6)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15977
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.45
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       parallelepide
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+2.4573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3759
_reflns_number_total             4294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300453y_si_002_1.cif
_cod_data_source_block           kyniosthf
_cod_original_formula_sum        'C14 H14 N0.50 Ni0.25 O P S0.50'
_cod_database_code               4329616