#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:01:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178545 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/52/4065215.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_4065215
loop_
_publ_author_name
'Knisley, Thomas J.'
'Saly, Mark J.'
'Heeg, Mary Jane'
'Roberts, John L.'
'Winter, Charles H.'
_publ_section_title
;
 Volatility and High Thermal Stability in Mid- to Late-First-Row
 Transition-Metal Diazadienyl Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5010
_journal_paper_doi               10.1021/om200626w
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C20 H40 Co N4'
_chemical_formula_weight         395.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2363(8)
_cell_length_b                   13.3810(6)
_cell_length_c                   9.2410(4)
_cell_measurement_reflns_used    8086
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.7
_cell_volume                     2254.99(17)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       'Bruker APEX2'
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            56591
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.8052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0262
_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)+(0.0303P)²+1.3188P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2603
_reflns_number_total             2911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200626w_si_002.cif
_cod_data_source_block           ucot
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

 Adding full bibliography for 4065213--4065216.cif.
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4065215
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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 0.827932(12) 0.2500 0.79589(2) 0.01196(7) Uani 1 2 d S
N1 N 0.81255(8) 0.2500 1.00245(15) 0.0144(3) Uani 1 2 d S
N2 N 0.72192(8) 0.2500 0.78490(15) 0.0142(3) Uani 1 2 d S
C1 C 0.74113(9) 0.2500 1.03345(19) 0.0171(3) Uani 1 2 d S
H1 H 0.7241 0.2500 1.1306 0.020 Uiso 1 2 calc SR
C2 C 0.69266(9) 0.2500 0.91693(19) 0.0166(3) Uani 1 2 d S
H2 H 0.6411 0.2500 0.9310 0.020 Uiso 1 2 calc SR
C3 C 0.86651(9) 0.2500 1.12238(18) 0.0165(3) Uani 1 2 d S
C4 C 0.94299(10) 0.2500 1.0559(2) 0.0246(4) Uani 1 2 d S
H4A H 0.9492 0.1905 0.9956 0.029 Uiso 1 1 d .
H4B H 0.9798 0.2500 1.1336 0.029 Uiso 1 2 d S
C5 C 0.85745(8) 0.15641(11) 1.21553(15) 0.0267(3) Uani 1 1 d .
H5A H 0.8080 0.1553 1.2572 0.032 Uiso 1 1 calc R
H5B H 0.8938 0.1571 1.2936 0.032 Uiso 1 1 calc R
H5C H 0.8647 0.0968 1.1555 0.032 Uiso 1 1 calc R
C6 C 0.67232(9) 0.2500 0.65745(19) 0.0169(3) Uani 1 2 d S
C7 C 0.72030(11) 0.2500 0.5230(2) 0.0262(4) Uani 1 2 d S
H7A H 0.7464 0.1862 0.5160 0.031 Uiso 1 1 d .
H7B H 0.6894 0.2589 0.4370 0.031 Uiso 0.50 1 d P
C8 C 0.62417(8) 0.15652(11) 0.65849(16) 0.0273(3) Uani 1 1 d .
H8A H 0.6553 0.0969 0.6624 0.033 Uiso 1 1 calc R
H8B H 0.5943 0.1548 0.5703 0.033 Uiso 1 1 calc R
H8C H 0.5920 0.1579 0.7434 0.033 Uiso 1 1 calc R
N3 N 0.88869(5) 0.15270(7) 0.69868(10) 0.01300(19) Uani 1 1 d .
C9 C 0.93967(6) 0.19759(8) 0.61790(12) 0.0152(2) Uani 1 1 d .
H9 H 0.9743 0.1604 0.5631 0.018 Uiso 1 1 calc R
C10 C 0.88555(7) 0.04190(9) 0.70299(13) 0.0161(2) Uani 1 1 d .
C11 C 0.82154(8) 0.01231(10) 0.79900(16) 0.0267(3) Uani 1 1 d .
H11A H 0.8290 0.0394 0.8964 0.032 Uiso 1 1 calc R
H11B H 0.8183 -0.0607 0.8040 0.032 Uiso 1 1 calc R
H11C H 0.7760 0.0392 0.7585 0.032 Uiso 1 1 calc R
C12 C 0.95616(8) -0.00028(10) 0.76812(19) 0.0323(3) Uani 1 1 d .
H12A H 0.9979 0.0185 0.7072 0.039 Uiso 1 1 calc R
H12B H 0.9527 -0.0733 0.7733 0.039 Uiso 1 1 calc R
H12C H 0.9631 0.0269 0.8657 0.039 Uiso 1 1 calc R
C13 C 0.87363(11) 0.00012(11) 0.55140(16) 0.0361(4) Uani 1 1 d .
H13A H 0.8282 0.0277 0.5109 0.043 Uiso 1 1 calc R
H13B H 0.8699 -0.0729 0.5563 0.043 Uiso 1 1 calc R
H13C H 0.9151 0.0187 0.4895 0.043 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
N1 Co1 N3 122.93(4) . 7_565
N1 Co1 N3 122.93(4) . .
N3 Co1 N3 84.77(6) 7_565 .
N1 Co1 N2 84.65(6) . .
N3 Co1 N2 123.26(4) 7_565 .
N3 Co1 N2 123.26(4) . .
C1 N1 C3 119.20(14) . .
C1 N1 Co1 110.76(11) . .
C3 N1 Co1 130.04(11) . .
C2 N2 C6 118.85(14) . .
C2 N2 Co1 110.61(11) . .
C6 N2 Co1 130.53(11) . .
N1 C1 C2 116.97(15) . .
N2 C2 C1 117.00(15) . .
N1 C3 C4 107.83(14) . .
N1 C3 C5 110.44(10) . 7_565
C4 C3 C5 109.02(10) . 7_565
N1 C3 C5 110.44(10) . .
C4 C3 C5 109.02(10) . .
C5 C3 C5 110.02(15) 7_565 .
N2 C6 C7 107.31(13) . .
N2 C6 C8 110.18(10) . 7_565
C7 C6 C8 109.64(10) . 7_565
N2 C6 C8 110.18(10) . .
C7 C6 C8 109.64(10) . .
C8 C6 C8 109.85(15) 7_565 .
C9 N3 C10 119.43(10) . .
C9 N3 Co1 110.87(8) . .
C10 N3 Co1 129.70(8) . .
N3 C9 C9 116.74(6) . 7_565
N3 C10 C11 107.80(10) . .
N3 C10 C13 110.32(10) . .
C11 C10 C13 109.38(12) . .
N3 C10 C12 110.29(10) . .
C11 C10 C12 108.73(11) . .
C13 C10 C12 110.28(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.9292(14) .
Co1 N3 1.9313(10) 7_565
Co1 N3 1.9313(10) .
Co1 N2 1.9359(14) .
N1 C1 1.334(2) .
N1 C3 1.482(2) .
N2 C2 1.332(2) .
N2 C6 1.485(2) .
C1 C2 1.393(2) .
C3 C4 1.524(2) .
C3 C5 1.5286(16) 7_565
C3 C5 1.5286(16) .
C6 C7 1.519(3) .
C6 C8 1.5285(16) 7_565
C6 C8 1.5285(16) .
N3 C9 1.3350(15) .
N3 C10 1.4843(14) .
C9 C9 1.403(2) 7_565
C10 C11 1.5188(17) .
C10 C13 1.5239(18) .
C10 C12 1.5292(18) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N3 Co1 N1 C1 126.56(4) 7_565 .
N3 Co1 N1 C1 -126.56(4) . .
N2 Co1 N1 C1 0.0 . .
N3 Co1 N1 C3 -53.44(4) 7_565 .
N3 Co1 N1 C3 53.44(4) . .
N2 Co1 N1 C3 180.0 . .
N1 Co1 N2 C2 0.0 . .
N3 Co1 N2 C2 -126.27(4) 7_565 .
N3 Co1 N2 C2 126.27(4) . .
N1 Co1 N2 C6 180.0 . .
N3 Co1 N2 C6 53.73(4) 7_565 .
N3 Co1 N2 C6 -53.73(4) . .
C3 N1 C1 C2 180.0 . .
Co1 N1 C1 C2 0.0 . .
C6 N2 C2 C1 180.0 . .
Co1 N2 C2 C1 0.0 . .
N1 C1 C2 N2 0.0 . .
C1 N1 C3 C4 180.0 . .
Co1 N1 C3 C4 0.0 . .
C1 N1 C3 C5 -60.97(11) . 7_565
Co1 N1 C3 C5 119.03(11) . 7_565
C1 N1 C3 C5 60.97(10) . .
Co1 N1 C3 C5 -119.03(10) . .
C2 N2 C6 C7 180.0 . .
Co1 N2 C6 C7 0.0 . .
C2 N2 C6 C8 60.69(11) . 7_565
Co1 N2 C6 C8 -119.31(11) . 7_565
C2 N2 C6 C8 -60.69(11) . .
Co1 N2 C6 C8 119.31(11) . .
N1 Co1 N3 C9 -125.98(8) . .
N3 Co1 N3 C9 0.26(10) 7_565 .
N2 Co1 N3 C9 127.04(8) . .
N1 Co1 N3 C10 54.02(11) . .
N3 Co1 N3 C10 -179.74(8) 7_565 .
N2 Co1 N3 C10 -52.97(11) . .
C10 N3 C9 C9 179.79(7) . 7_565
Co1 N3 C9 C9 -0.22(8) . 7_565
C9 N3 C10 C11 -178.41(11) . .
Co1 N3 C10 C11 1.60(15) . .
C9 N3 C10 C13 -59.04(15) . .
Co1 N3 C10 C13 120.97(11) . .
C9 N3 C10 C12 63.03(14) . .
Co1 N3 C10 C12 -116.97(11) . .
