#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:20:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178895 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/24/4112448.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4112448
loop_
_publ_author_name
'Xuliang Dai'
'Pooja Kapoor'
'Timothy H. Warren'
_publ_contact_author             'Timothy H. Warren'
_publ_contact_author_email       thw@georgetown.edu
_publ_section_title
;
 [Me2NN]Co(η6-toluene): OO, NN, and ON Bond Cleavage Provides
 β-Diketiminato Cobalt μ-Oxo and Imido Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4798
_journal_page_last               4799
_journal_paper_doi               10.1021/ja036308i
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C29 H34 Co N3'
_chemical_formula_weight         483.52
_chemical_name_common            {[Me2NN]Co}2(m-NAr)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.587(4)
_cell_angle_beta                 103.088(4)
_cell_angle_gamma                111.907(4)
_cell_formula_units_Z            2
_cell_length_a                   11.081(3)
_cell_length_b                   11.487(3)
_cell_length_c                   11.586(3)
_cell_measurement_reflns_used    2264
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      2.33
_cell_volume                     1280.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics
'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12938
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  XXXX
_exptl_absorpt_correction_T_min  XXXX
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5035
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0577
_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/[σ²(Fo²)+(0.0764P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                2801
_reflns_number_total             5035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036308isi20030523_032743.cif
_cod_data_source_block           c:\papers\co-imide\conar\01079s
_cod_original_cell_volume        1280.2(5)
_cod_database_code               4112448
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.57131(6) 0.52808(5) 0.63804(5) 0.02463(19) Uani 1 1 d .
N1 N 0.7199(3) 0.6819(3) 0.7653(3) 0.0286(8) Uani 1 1 d .
N2 N 0.5540(3) 0.4119(3) 0.7450(3) 0.0278(8) Uani 1 1 d .
C6 C 0.7445(4) 0.8132(4) 0.7643(4) 0.0285(10) Uani 1 1 d .
C22 C 0.6713(4) 0.4048(4) 0.4576(4) 0.0276(10) Uani 1 1 d .
C12 C 0.4279(4) 0.2965(4) 0.7205(4) 0.0274(10) Uani 1 1 d .
C7 C 0.7103(4) 0.8883(4) 0.8497(4) 0.0335(11) Uani 1 1 d .
C19 C 0.8326(5) 0.7828(4) 0.5850(4) 0.0402(12) Uani 1 1 d .
H19A H 0.8788 0.8361 0.5367 0.060 Uiso 1 1 calc R
H19B H 0.7483 0.7090 0.5296 0.060 Uiso 1 1 calc R
H19C H 0.8934 0.7501 0.6298 0.060 Uiso 1 1 calc R
C25 C 0.8462(5) 0.2906(4) 0.4240(4) 0.0373(11) Uani 1 1 d .
H25 H 0.9059 0.2512 0.4126 0.045 Uiso 1 1 calc R
C23 C 0.7865(4) 0.4299(4) 0.5540(4) 0.0320(10) Uani 1 1 d .
H23 H 0.8052 0.4877 0.6314 0.038 Uiso 1 1 calc R
C11 C 0.7977(4) 0.8647(4) 0.6755(4) 0.0304(10) Uani 1 1 d .
C3 C 0.6608(4) 0.4318(4) 0.8393(4) 0.0293(10) Uani 1 1 d .
C10 C 0.8202(5) 0.9917(4) 0.6760(4) 0.0384(11) Uani 1 1 d .
H10 H 0.8590 1.0284 0.6180 0.046 Uiso 1 1 calc R
C13 C 0.4093(5) 0.1743(4) 0.6524(4) 0.0334(11) Uani 1 1 d .
C2 C 0.7839(4) 0.5464(4) 0.8802(4) 0.0290(10) Uani 1 1 d .
H2 H 0.8602 0.5423 0.9334 0.035 Uiso 1 1 calc R
C4 C 0.9435(5) 0.7800(4) 0.9287(4) 0.0443(12) Uani 1 1 d .
H4A H 0.9860 0.8249 0.8735 0.066 Uiso 1 1 calc R
H4B H 1.0049 0.7488 0.9751 0.066 Uiso 1 1 calc R
H4C H 0.9270 0.8407 0.9862 0.066 Uiso 1 1 calc R
C1 C 0.8086(4) 0.6649(4) 0.8531(4) 0.0317(10) Uani 1 1 d .
C5 C 0.6533(5) 0.3299(4) 0.9086(4) 0.0424(12) Uani 1 1 d .
H5A H 0.5780 0.3145 0.9436 0.064 Uiso 1 1 calc R
H5B H 0.7399 0.3610 0.9751 0.064 Uiso 1 1 calc R
H5C H 0.6372 0.2483 0.8518 0.064 Uiso 1 1 calc R
C27 C 0.6463(4) 0.3223(4) 0.3440(4) 0.0306(10) Uani 1 1 d .
H27 H 0.5681 0.3043 0.2772 0.037 Uiso 1 1 calc R
C17 C 0.3260(4) 0.3086(4) 0.7679(4) 0.0298(10) Uani 1 1 d .
C24 C 0.8750(4) 0.3730(4) 0.5404(4) 0.0323(10) Uani 1 1 d .
C18 C 0.6576(5) 0.8365(5) 0.9473(4) 0.0442(13) Uani 1 1 d .
H18A H 0.7339 0.8420 1.0137 0.066 Uiso 1 1 calc R
H18B H 0.5903 0.7451 0.9115 0.066 Uiso 1 1 calc R
H18C H 0.6140 0.8883 0.9807 0.066 Uiso 1 1 calc R
C16 C 0.2085(5) 0.1982(5) 0.7483(4) 0.0387(11) Uani 1 1 d .
H16 H 0.1380 0.2055 0.7784 0.046 Uiso 1 1 calc R
C21 C 0.3458(5) 0.4401(4) 0.8393(4) 0.0395(12) Uani 1 1 d .
H21A H 0.3375 0.4933 0.7827 0.059 Uiso 1 1 calc R
H21B H 0.4370 0.4841 0.9011 0.059 Uiso 1 1 calc R
H21C H 0.2758 0.4285 0.8806 0.059 Uiso 1 1 calc R
C8 C 0.7317(5) 1.0131(4) 0.8440(4) 0.0404(12) Uani 1 1 d .
H8 H 0.7076 1.0640 0.8999 0.049 Uiso 1 1 calc R
C9 C 0.7872(5) 1.0664(4) 0.7592(4) 0.0421(12) Uani 1 1 d .
H9 H 0.8026 1.1532 0.7581 0.051 Uiso 1 1 calc R
C14 C 0.2906(5) 0.0661(4) 0.6383(4) 0.0434(12) Uani 1 1 d .
H14 H 0.2777 -0.0175 0.5947 0.052 Uiso 1 1 calc R
C20 C 0.5133(5) 0.1602(4) 0.5944(4) 0.0457(13) Uani 1 1 d .
H20A H 0.5262 0.0828 0.6068 0.068 Uiso 1 1 calc R
H20B H 0.6006 0.2380 0.6326 0.068 Uiso 1 1 calc R
H20C H 0.4807 0.1506 0.5058 0.068 Uiso 1 1 calc R
C15 C 0.1912(5) 0.0764(5) 0.6855(4) 0.0445(12) Uani 1 1 d .
H15 H 0.1110 0.0006 0.6752 0.053 Uiso 1 1 calc R
N3 N 0.5832(3) 0.4575(3) 0.4742(2) 0.0102(6) Uani 1 1 d U
C26 C 0.7353(5) 0.2655(4) 0.3268(4) 0.0365(11) Uani 1 1 d .
C28 C 0.9972(5) 0.3987(5) 0.6457(5) 0.0463(13) Uani 1 1 d .
H28A H 0.9914 0.4442 0.7223 0.069 Uiso 1 1 calc R
H28B H 1.0810 0.4531 0.6306 0.069 Uiso 1 1 calc R
H28C H 0.9991 0.3156 0.6532 0.069 Uiso 1 1 calc R
C29 C 0.7046(6) 0.1770(5) 0.2006(4) 0.0579(15) Uani 1 1 d .
H29A H 0.7820 0.1555 0.1992 0.087 Uiso 1 1 calc R
H29B H 0.6902 0.2219 0.1375 0.087 Uiso 1 1 calc R
H29C H 0.6218 0.0965 0.1836 0.087 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Co1 N1 95.03(14) . .
N2 Co1 N3 125.40(13) . 2_666
N1 Co1 N3 121.17(13) . 2_666
N2 Co1 N3 115.28(12) . .
N1 Co1 N3 123.88(13) . .
N3 Co1 N3 78.88(11) 2_666 .
C1 N1 C6 117.6(3) . .
C1 N1 Co1 119.2(3) . .
C6 N1 Co1 123.1(3) . .
C3 N2 C12 117.4(3) . .
C3 N2 Co1 120.9(3) . .
C12 N2 Co1 121.6(3) . .
C11 C6 C7 120.5(4) . .
C11 C6 N1 119.7(3) . .
C7 C6 N1 119.7(4) . .
N3 C22 C27 120.4(4) . .
N3 C22 C23 120.9(4) . .
C27 C22 C23 118.6(4) . .
C17 C12 C13 120.7(4) . .
C17 C12 N2 118.9(3) . .
C13 C12 N2 120.5(4) . .
C8 C7 C6 118.2(4) . .
C8 C7 C18 120.6(4) . .
C6 C7 C18 121.2(4) . .
C26 C25 C24 122.1(4) . .
C24 C23 C22 121.9(4) . .
C10 C11 C6 118.7(4) . .
C10 C11 C19 121.6(4) . .
C6 C11 C19 119.7(4) . .
N2 C3 C2 122.7(4) . .
N2 C3 C5 120.5(4) . .
C2 C3 C5 116.8(4) . .
C9 C10 C11 121.3(4) . .
C14 C13 C12 118.0(4) . .
C14 C13 C20 120.3(4) . .
C12 C13 C20 121.6(4) . .
C1 C2 C3 128.6(4) . .
N1 C1 C2 123.6(4) . .
N1 C1 C4 119.2(4) . .
C2 C1 C4 117.2(4) . .
C22 C27 C26 120.8(4) . .
C16 C17 C12 118.7(4) . .
C16 C17 C21 120.9(4) . .
C12 C17 C21 120.4(4) . .
C23 C24 C25 117.6(4) . .
C23 C24 C28 121.4(4) . .
C25 C24 C28 121.0(4) . .
C17 C16 C15 121.2(4) . .
C7 C8 C9 122.0(4) . .
C8 C9 C10 119.2(4) . .
C15 C14 C13 121.8(4) . .
C14 C15 C16 119.5(4) . .
C22 N3 Co1 134.4(2) . 2_666
C22 N3 Co1 124.2(2) . .
Co1 N3 Co1 101.12(11) 2_666 .
C25 C26 C27 119.0(4) . .
C25 C26 C29 122.1(4) . .
C27 C26 C29 118.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.955(3) .
Co1 N1 1.967(3) .
Co1 N3 1.981(3) 2_666
Co1 N3 1.990(3) .
N1 C1 1.341(5) .
N1 C6 1.431(5) .
N2 C3 1.333(5) .
N2 C12 1.450(5) .
C6 C11 1.404(6) .
C6 C7 1.414(5) .
C22 N3 1.357(5) .
C22 C27 1.390(5) .
C22 C23 1.391(6) .
C12 C17 1.402(6) .
C12 C13 1.406(5) .
C7 C8 1.379(6) .
C7 C18 1.496(6) .
C19 C11 1.502(5) .
C25 C26 1.365(6) .
C25 C24 1.404(6) .
C23 C24 1.388(5) .
C11 C10 1.385(6) .
C3 C2 1.406(6) .
C3 C5 1.514(6) .
C10 C9 1.384(6) .
C13 C14 1.384(6) .
C13 C20 1.503(6) .
C2 C1 1.389(6) .
C4 C1 1.515(6) .
C27 C26 1.402(6) .
C17 C16 1.377(6) .
C17 C21 1.507(6) .
C24 C28 1.498(6) .
C16 C15 1.386(6) .
C8 C9 1.382(6) .
C14 C15 1.368(6) .
N3 Co1 1.981(3) 2_666
C26 C29 1.519(6) .
