Synthesis, Spectroscopic Characterization, and Determination of the Solution Association Energy of the Dimer [Co{N(SiMe3)2}2]2: Magnetic Studies of Low-Coordinate Co(II) Silylamides [Co{N(SiMe3)2}2L] (L = PMe3, Pyridine, and THF) and Related Species That Reveal Evidence of Very Large Zero-Field Splittings
Aimee M. Bryan; Gary J. Long; Fernande Grandjean; Philip P. Power; Inorganic Chemistry 52 (2013) 12152–12160; doi:10.1021/ic402019w

data_4336482
_publ_section_title
;
 Synthesis, Spectroscopic Characterization, and Determination of the
 Solution Association Energy of the Dimer [Co{N(SiMe3)2}2]2: Magnetic
 Studies of Low-Coordinate Co(II) Silylamides [Co{N(SiMe3)2}2L] (L = PMe3,
 Pyridine, and THF) and Related Species That Reveal Evidence of Very Large
 Zero-Field Splittings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12152
_journal_page_last               12160
_journal_paper_doi               10.1021/ic402019w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C16 H44 Co N2 O Si4'
_chemical_formula_sum            'C16 H44 Co N2 O Si4'
_chemical_formula_weight         451.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5395(3)
_cell_length_b                   11.1656(3)
_cell_length_c                   17.7402(4)
_cell_measurement_reflns_used    7398
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.869
_cell_measurement_theta_min      4.728
_cell_volume                     2681.90(11)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2011)'
_computing_data_collection       'Apex2 (Bruker, 2011)'
_computing_data_reduction        'SAINT V7.68A (Bruker, 2011)'
_computing_molecular_graphics    'OLEX2 (Dolomanov, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex DUO'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            91070
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       needle
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3080
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.4067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2601
_reflns_number_total             3080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402019w_si_004.cif
_cod_data_source_block           amb44x
_cod_database_code               4336482
_shelx_estimated_absorpt_t_min   0.734
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-4
_shelx_res_checksum              59198