Spin Density Distribution in Iron(II) and Cobalt(II) Alkyl Complexes Containing 1,3-Bis(2-pyridylimino)isoindolate Ligands
Sauer, Désirée C.; Kruck, Matthias; Wadepohl, Hubert; Enders, Markus; Gade, Lutz H.; Organometallics 32 (2013) 885–; doi:10.1021/om301198b

data_4080022
_publ_section_title
;
 Spin Density Distribution in Iron(II) and Cobalt(II) Alkyl Complexes
 Containing 1,3-Bis(2-pyridylimino)isoindolate Ligands
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              885
_journal_paper_doi               10.1021/om301198b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C30 H35 Fe N5 Si'
_chemical_formula_weight         549.57
_chemical_properties_physical    air-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_mkr33
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.176(10)
_cell_angle_beta                 113.954(11)
_cell_angle_gamma                102.384(10)
_cell_formula_units_Z            2
_cell_length_a                   10.528(5)
_cell_length_b                   11.752(6)
_cell_length_c                   12.215(6)
_cell_measurement_reflns_used    8134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.89
_cell_measurement_theta_min      2.18
_cell_volume                     1331.7(11)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction
'SAINT (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al., 2004)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33191
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.07
_diffrn_reflns_theta_min         2.18
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8755
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.5113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                7288
_reflns_number_total             8755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301198b_si_002.cif
_cod_data_source_block           ga_mkr33
_cod_database_code               4080022
_audit_block_refno               1271