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_4115350
_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            'C39 H61 N2 Ni O'
_chemical_formula_weight         632.61
_chemical_name_common            LNiCl
_chemical_name_systematic
; 
 2,2,6,6-tetramethyl-3,5-bis(2,6-diisopropylphenylimido)heptyl nickel(I)
 tetrahydrofuran
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.543(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5620(7)
_cell_length_b                   17.7515(14)
_cell_length_c                   21.7048(17)
_cell_measurement_temperature    293(2)
_cell_volume                     3666.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_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  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22418
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   'empirical; SADABS'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+1.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                7273
_reflns_number_total             8524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025583m-3_s1_5.cif
_cod_data_source_block           LNiTHF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'na' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4115350