Synthesis, Structural, and Magnetic Characterization of Linear and Bent Geometry Cobalt(II) and Nickel(II) Amido Complexes: Evidence of Very Large Spin-Orbit Coupling Effects in Rigorously Linear Coordinated Co2+
Aimee M. Bryan; W. Alexander Merrill; William M. Reiff; James C. Fettinger; Philip P. Power; Inorganic Chemistry 51 (2012) 3366–3373; doi:10.1021/ic2012414

data_4328602
_publ_section_title
;
 Synthesis, Structural, and Magnetic Characterization of Linear and Bent
 Geometry Cobalt(II) and Nickel(II) Amido Complexes: Evidence of Very
 Large Spin-Orbit Coupling Effects in Rigorously Linear Coordinated Co2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3366
_journal_page_last               3373
_journal_paper_doi               10.1021/ic2012414
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C72 H100 N2 Ni'
_chemical_formula_sum            'C72 H100 N2 Ni'
_chemical_formula_weight         1049.85
_chemical_melting_point          550
_chemical_name_common            Ni(NHArPri6)2_compound2
_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                66.827(2)
_cell_angle_beta                 73.513(2)
_cell_angle_gamma                75.750(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7334(18)
_cell_length_b                   11.5751(19)
_cell_length_c                   14.771(3)
_cell_measurement_reflns_used    7668
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.77
_cell_volume                     1598.8(5)
_computing_cell_refinement       'SAINT (7.60A) (Bruker, 2008)'
_computing_data_collection       'Apex2 (2009-3) (Bruker, 2009)'
_computing_data_reduction        'SAINT (7.60A) (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13639
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.8573
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       Needle
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7299
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                5714
_reflns_number_total             7299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012414_si_001_2.cif
_cod_data_source_block           alx502fmi
_cod_database_code               4328602