#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:00:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178764 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/18/4101857.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_4101857
loop_
_publ_author_name
'Amanda C. Bowman'
'Carsten Milsmann'
'Crisita Carmen Hojilla Atienza'
'Emil Lobkovsky'
'Karl Wieghardt'
'Paul J. Chirik'
_publ_section_title
;
 Synthesis and Molecular and Electronic Structures of Reduced
 Bis(imino)pyridine Cobalt Dinitrogen Complexes: Ligand versus Metal
 Reduction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1676
_journal_page_last               1684
_journal_paper_doi               10.1021/ja908955t
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C33 H43 Co N5'
_chemical_formula_sum            'C33 H43 Co N5'
_chemical_formula_weight         568.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.4360(12)
_cell_length_b                   17.851(3)
_cell_length_c                   20.117(3)
_cell_measurement_reflns_used    6485
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.29
_cell_volume                     3029.4(8)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21677
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.8901
_exptl_absorpt_correction_T_min  0.7753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.688(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0307P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                5922
_reflns_number_total             7486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja908955t_si_002.cif
_cod_data_source_block           acb13
_cod_original_cell_volume        3029.5(8)
_cod_database_code               4101857
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.12607(3) 0.401180(12) 0.873681(12) 0.01954(5) Uani 1 1 d . . .
N1 N 0.06138(17) 0.32410(8) 0.81672(7) 0.0212(4) Uani 1 1 d . . .
N2 N 0.01289(17) 0.34658(7) 0.93268(7) 0.0184(3) Uani 1 1 d . . .
N3 N 0.15942(16) 0.46094(7) 0.94918(7) 0.0192(4) Uani 1 1 d . . .
N4 N 0.2383(2) 0.45534(8) 0.81557(8) 0.0307(4) Uani 1 1 d . . .
N5 N 0.3080(2) 0.48838(10) 0.77953(10) 0.0537(6) Uani 1 1 d . . .
C1 C -0.0849(2) 0.20298(10) 0.80527(10) 0.0323(5) Uani 1 1 d . . .
H1A H -0.1418 0.2196 0.7654 0.048 Uiso 1 1 calc R . .
H1B H -0.1562 0.1733 0.8333 0.048 Uiso 1 1 calc R . .
H1C H 0.0062 0.1723 0.7922 0.048 Uiso 1 1 calc R . .
C2 C -0.0283(2) 0.26973(9) 0.84324(9) 0.0223(4) Uani 1 1 d . . .
C3 C -0.0592(2) 0.28138(9) 0.91172(9) 0.0203(4) Uani 1 1 d . . .
C4 C -0.1459(2) 0.23971(9) 0.95738(9) 0.0267(5) Uani 1 1 d . . .
H4A H -0.1986 0.1953 0.9437 0.032 Uiso 1 1 calc R . .
C5 C -0.1551(2) 0.26293(10) 1.02250(9) 0.0277(5) Uani 1 1 d . . .
H5A H -0.2131 0.2339 1.0538 0.033 Uiso 1 1 calc R . .
C6 C -0.0807(2) 0.32828(9) 1.04296(9) 0.0244(5) Uani 1 1 d . . .
H6A H -0.0880 0.3442 1.0879 0.029 Uiso 1 1 calc R . .
C7 C 0.0043(2) 0.37009(9) 0.99726(9) 0.0203(4) Uani 1 1 d . . .
C8 C 0.0912(2) 0.43819(9) 1.00536(9) 0.0199(4) Uani 1 1 d . . .
C9 C 0.1033(3) 0.47811(10) 1.07075(9) 0.0311(5) Uani 1 1 d . . .
H9A H 0.1789 0.5195 1.0669 0.047 Uiso 1 1 calc R . .
H9B H 0.1397 0.4430 1.1049 0.047 Uiso 1 1 calc R . .
H9C H -0.0010 0.4979 1.0831 0.047 Uiso 1 1 calc R . .
C10 C 0.1080(2) 0.31963(9) 0.74786(8) 0.0219(4) Uani 1 1 d . . .
C11 C 0.0153(2) 0.35558(10) 0.69986(9) 0.0260(5) Uani 1 1 d . . .
C12 C 0.0743(2) 0.35859(10) 0.63561(10) 0.0314(5) Uani 1 1 d . . .
H12A H 0.0138 0.3826 0.6020 0.038 Uiso 1 1 calc R . .
C13 C 0.2185(2) 0.32759(10) 0.61941(10) 0.0322(5) Uani 1 1 d . . .
H13A H 0.2580 0.3317 0.5753 0.039 Uiso 1 1 calc R . .
C14 C 0.3055(2) 0.29060(10) 0.66725(9) 0.0306(5) Uani 1 1 d . . .
H14A H 0.4043 0.2687 0.6555 0.037 Uiso 1 1 calc R . .
C15 C 0.2519(2) 0.28473(10) 0.73212(9) 0.0238(5) Uani 1 1 d . . .
C16 C -0.1431(2) 0.39066(10) 0.71657(10) 0.0344(5) Uani 1 1 d . . .
H16A H -0.1797 0.3688 0.7597 0.041 Uiso 1 1 calc R . .
C17 C -0.2686(3) 0.37351(13) 0.66439(11) 0.0489(7) Uani 1 1 d . . .
H17A H -0.2430 0.4001 0.6232 0.073 Uiso 1 1 calc R . .
H17B H -0.3725 0.3899 0.6806 0.073 Uiso 1 1 calc R . .
H17C H -0.2710 0.3195 0.6559 0.073 Uiso 1 1 calc R . .
C18 C -0.1292(3) 0.47491(12) 0.72569(14) 0.0643(8) Uani 1 1 d . . .
H18A H -0.0821 0.4972 0.6858 0.096 Uiso 1 1 calc R . .
H18B H -0.0618 0.4856 0.7642 0.096 Uiso 1 1 calc R . .
H18C H -0.2348 0.4963 0.7330 0.096 Uiso 1 1 calc R . .
C19 C 0.3493(2) 0.24277(10) 0.78358(9) 0.0287(5) Uani 1 1 d . . .
H19A H 0.2793 0.2334 0.8229 0.034 Uiso 1 1 calc R . .
C20 C 0.4068(3) 0.16660(12) 0.75827(11) 0.0574(8) Uani 1 1 d . . .
H20A H 0.3156 0.1366 0.7441 0.086 Uiso 1 1 calc R . .
H20B H 0.4630 0.1404 0.7940 0.086 Uiso 1 1 calc R . .
H20C H 0.4786 0.1740 0.7205 0.086 Uiso 1 1 calc R . .
C21 C 0.4881(3) 0.28893(13) 0.80709(11) 0.0517(7) Uani 1 1 d . . .
H21A H 0.5600 0.2983 0.7697 0.077 Uiso 1 1 calc R . .
H21B H 0.5447 0.2617 0.8421 0.077 Uiso 1 1 calc R . .
H21C H 0.4497 0.3368 0.8247 0.077 Uiso 1 1 calc R . .
C22 C 0.2542(2) 0.52797(9) 0.94843(9) 0.0215(4) Uani 1 1 d . . .
C23 C 0.4189(2) 0.52102(10) 0.95269(10) 0.0294(5) Uani 1 1 d . . .
C24 C 0.5090(2) 0.58593(11) 0.94739(10) 0.0388(6) Uani 1 1 d . . .
H24A H 0.6212 0.5826 0.9499 0.047 Uiso 1 1 calc R . .
C25 C 0.4403(3) 0.65412(12) 0.93876(10) 0.0392(6) Uani 1 1 d . . .
H25A H 0.5047 0.6976 0.9358 0.047 Uiso 1 1 calc R . .
C26 C 0.2781(3) 0.66059(11) 0.93432(10) 0.0340(6) Uani 1 1 d . . .
H26A H 0.2315 0.7084 0.9276 0.041 Uiso 1 1 calc R . .
C27 C 0.1810(2) 0.59701(10) 0.93962(9) 0.0246(4) Uani 1 1 d . . .
C28 C 0.4998(2) 0.44620(11) 0.96339(11) 0.0403(6) Uani 1 1 d . . .
H28A H 0.4200 0.4059 0.9547 0.048 Uiso 1 1 calc R . .
C29 C 0.5539(3) 0.43884(13) 1.03566(13) 0.0542(7) Uani 1 1 d . . .
H29A H 0.5953 0.3883 1.0432 0.081 Uiso 1 1 calc R . .
H29B H 0.4638 0.4479 1.0653 0.081 Uiso 1 1 calc R . .
H29C H 0.6374 0.4756 1.0447 0.081 Uiso 1 1 calc R . .
C30 C 0.6385(3) 0.43391(12) 0.91639(12) 0.0541(7) Uani 1 1 d . . .
H30A H 0.7255 0.4676 0.9285 0.081 Uiso 1 1 calc R . .
H30B H 0.6049 0.4443 0.8707 0.081 Uiso 1 1 calc R . .
H30C H 0.6745 0.3818 0.9197 0.081 Uiso 1 1 calc R . .
C31 C 0.0026(2) 0.60547(11) 0.93356(9) 0.0314(5) Uani 1 1 d . . .
H31A H -0.0465 0.5557 0.9435 0.038 Uiso 1 1 calc R . .
C32 C -0.0635(3) 0.66206(11) 0.98312(10) 0.0386(6) Uani 1 1 d . . .
H32A H -0.0208 0.7119 0.9732 0.058 Uiso 1 1 calc R . .
H32B H -0.0329 0.6474 1.0283 0.058 Uiso 1 1 calc R . .
H32C H -0.1794 0.6632 0.9797 0.058 Uiso 1 1 calc R . .
C33 C -0.0441(3) 0.62724(12) 0.86342(11) 0.0538(7) Uani 1 1 d . . .
H33A H -0.0056 0.6779 0.8539 0.081 Uiso 1 1 calc R . .
H33B H -0.1598 0.6260 0.8592 0.081 Uiso 1 1 calc R . .
H33C H 0.0030 0.5919 0.8318 0.081 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
_geom_angle_publ_flag
N4 Co1 N2 179.80(8) . . ?
N4 Co1 N1 98.73(7) . . ?
N2 Co1 N1 81.47(6) . . ?
N4 Co1 N3 98.18(7) . . ?
N2 Co1 N3 81.63(6) . . ?
N1 Co1 N3 163.07(6) . . ?
C2 N1 C10 119.72(15) . . ?
C2 N1 Co1 116.93(12) . . ?
C10 N1 Co1 123.30(11) . . ?
C7 N2 C3 121.74(14) . . ?
C7 N2 Co1 119.09(11) . . ?
C3 N2 Co1 119.15(11) . . ?
C8 N3 C22 120.18(14) . . ?
C8 N3 Co1 116.65(11) . . ?
C22 N3 Co1 123.17(11) . . ?
N5 N4 Co1 179.55(19) . . ?
N1 C2 C3 112.59(16) . . ?
N1 C2 C1 123.66(16) . . ?
C3 C2 C1 123.72(16) . . ?
N2 C3 C4 118.80(16) . . ?
N2 C3 C2 109.86(15) . . ?
C4 C3 C2 131.35(17) . . ?
C5 C4 C3 119.84(16) . . ?
C4 C5 C6 120.67(17) . . ?
C7 C6 C5 119.40(17) . . ?
N2 C7 C6 119.53(16) . . ?
N2 C7 C8 110.01(15) . . ?
C6 C7 C8 130.45(17) . . ?
N3 C8 C7 112.62(15) . . ?
N3 C8 C9 124.77(15) . . ?
C7 C8 C9 122.62(16) . . ?
C11 C10 C15 122.17(16) . . ?
C11 C10 N1 119.05(16) . . ?
C15 C10 N1 118.56(16) . . ?
C12 C11 C10 117.44(18) . . ?
C12 C11 C16 120.55(17) . . ?
C10 C11 C16 122.00(17) . . ?
C13 C12 C11 121.54(19) . . ?
C12 C13 C14 119.89(19) . . ?
C13 C14 C15 121.30(19) . . ?
C14 C15 C10 117.55(17) . . ?
C14 C15 C19 120.16(17) . . ?
C10 C15 C19 122.28(16) . . ?
C11 C16 C18 111.62(18) . . ?
C11 C16 C17 112.19(16) . . ?
C18 C16 C17 109.62(18) . . ?
C21 C19 C15 111.36(16) . . ?
C21 C19 C20 110.10(18) . . ?
C15 C19 C20 112.50(16) . . ?
C27 C22 C23 121.91(17) . . ?
C27 C22 N3 119.42(17) . . ?
C23 C22 N3 118.56(15) . . ?
C24 C23 C22 117.70(17) . . ?
C24 C23 C28 119.97(18) . . ?
C22 C23 C28 122.33(17) . . ?
C25 C24 C23 121.6(2) . . ?
C24 C25 C26 120.5(2) . . ?
C25 C26 C27 120.50(19) . . ?
C22 C27 C26 117.83(18) . . ?
C22 C27 C31 122.65(17) . . ?
C26 C27 C31 119.49(18) . . ?
C23 C28 C30 112.67(18) . . ?
C23 C28 C29 110.20(18) . . ?
C30 C28 C29 110.43(19) . . ?
C33 C31 C27 110.97(18) . . ?
C33 C31 C32 110.12(17) . . ?
C27 C31 C32 112.09(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N4 1.7884(16) . ?
Co1 N2 1.8084(14) . ?
Co1 N1 1.8719(15) . ?
Co1 N3 1.8773(14) . ?
N1 C2 1.341(2) . ?
N1 C10 1.442(2) . ?
N2 C7 1.367(2) . ?
N2 C3 1.379(2) . ?
N3 C8 1.331(2) . ?
N3 C22 1.439(2) . ?
N4 N5 1.104(2) . ?
C1 C2 1.494(2) . ?
C2 C3 1.418(2) . ?
C3 C4 1.390(2) . ?
C4 C5 1.376(2) . ?
C5 C6 1.387(2) . ?
C6 C7 1.384(2) . ?
C7 C8 1.429(2) . ?
C8 C9 1.500(2) . ?
C10 C11 1.399(3) . ?
C10 C15 1.401(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.513(3) . ?
C12 C13 1.375(3) . ?
C13 C14 1.379(3) . ?
C14 C15 1.385(3) . ?
C15 C19 1.519(3) . ?
C16 C18 1.520(3) . ?
C16 C17 1.522(3) . ?
C19 C21 1.508(3) . ?
C19 C20 1.531(3) . ?
C22 C27 1.390(2) . ?
C22 C23 1.397(3) . ?
C23 C24 1.390(3) . ?
C23 C28 1.515(3) . ?
C24 C25 1.359(3) . ?
C25 C26 1.376(3) . ?
C26 C27 1.404(3) . ?
C27 C31 1.517(3) . ?
C28 C30 1.520(3) . ?
C28 C29 1.529(3) . ?
C31 C33 1.516(3) . ?
C31 C32 1.525(3) . ?
