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_4336480
_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         'C24 H72 Co2 N4 Si8'
_chemical_formula_sum            'C24 H72 Co2 N4 Si8'
_chemical_formula_weight         759.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 117.794(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.966(3)
_cell_length_b                   14.634(2)
_cell_length_c                   18.133(4)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    90
_cell_measurement_theta_max      33.09
_cell_measurement_theta_min      2.54
_cell_volume                     4217.4(13)
_computing_cell_refinement       'SAINT V8.32B (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker, 2013)'
_computing_molecular_graphics    'OLEX2 (Dolomanov, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.307
_diffrn_reflns_theta_min         2.539
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            'red green dichroic'
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         7764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+2.6877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6778
_reflns_number_total             7764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402019w_si_002.cif
_cod_data_source_block           amb71c_a
_cod_original_cell_volume        4217.4(14)
_cod_database_code               4336480
_shelxl_version_number           2013-3
_shelx_res_checksum              96654