Electronically Unsaturated Three-Coordinate Chloride and Methyl Complexes of Iron, Cobalt, and Nickel
Patrick L. Holland; Thomas R. Cundari; Lanyn L. Perez; Nathan A. Eckert; Rene J. Lachicotte; Journal of the American Chemical Society 124 (2002) 14416–14424; doi:10.1021/ja025583m

data_4115349
_publ_section_title
;
 Electronically Unsaturated Three-Coordinate Chloride and Methyl Complexes
 of Iron, Cobalt, and Nickel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14416
_journal_page_last               14424
_journal_paper_doi               10.1021/ja025583m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C36 H56 Co N2'
_chemical_formula_weight         575.76
_chemical_name_common            LCoCH3
_chemical_name_systematic
; 
2,2,6,6-tetramethyl-3,5-bis(2,6-diisopropylphenylimido)heptyl cobalt(II) methyl 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.2190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8841(12)
_cell_length_b                   9.3872(7)
_cell_length_c                   22.7802(16)
_cell_measurement_reflns_used    4183
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.6
_cell_volume                     3448.7(4)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        XPREP
_computing_molecular_graphics    ORTEP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10660
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0422P)^2^+2.6300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                3799
_reflns_number_total             4167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025583m-3_s1_4.cif
_cod_data_source_block           LCoCH3
_cod_database_code               4115349