Synthesis and Characterization of Three-Coordinate and Related β-Diketiminate Derivatives of Manganese, Iron, and Cobalt
Arunashree Panda; Matthias Stender; Robert J. Wright; Marilyn M. Olmstead; Peter Klavins; Philip P. Power; Inorganic Chemistry 41 (2002) 3909–3916; doi:10.1021/ic025552s

data_4318279
_publ_section_title
;
 Synthesis and Characterization of Three-Coordinate and Related
 \b-Diketiminate Derivatives of Manganese, Iron, and Cobalt
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3909
_journal_page_last               3916
_journal_paper_doi               10.1021/ic025552s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C47.5 H67.5 Cl2 Co Li N2 O2'
_chemical_formula_weight         835.31
_chemical_name_common            'NacNacCoCl2Li(thf)2*1.5 toluene'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4549(11)
_cell_length_b                   17.8271(12)
_cell_length_c                   15.8304(11)
_cell_measurement_reflns_used    5074
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.57
_cell_volume                     4642.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43088
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.8738
_exptl_absorpt_correction_T_min  0.7790
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick
using the method described by Blessing, R. H.; Acta Cryst.
A51, 1995, 33.
;
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1786
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.00000(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          3.772
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+1.9347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                6465
_reflns_number_total             8391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025552s_s1_4.cif
_cod_data_source_block           mas45
_cod_original_formula_sum        'C47.50 H67.50 Cl2 Co Li N2 O2'
_cod_database_code               4318279