#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:24:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179410 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/07/4330759.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_4330759
loop_
_publ_author_name
'Michael P. Marshak'
'Matthew B. Chambers'
'Daniel G. Nocera'
_publ_section_title
;
 Cobalt in a Bis-β-diketiminate Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11190
_journal_page_last               11197
_journal_paper_doi               10.1021/ic301970w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C26 H34 Co N4, 2(C2 H3 N)'
_chemical_formula_sum            'C30 H40 Co N6'
_chemical_formula_weight         543.61
_chemical_name_common            (MesNacNac)2Co(NCCH3)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                110.2470(10)
_cell_angle_beta                 97.5450(10)
_cell_angle_gamma                96.6970(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5629(5)
_cell_length_b                   8.6093(5)
_cell_length_c                   10.7283(6)
_cell_measurement_temperature    100(2)
_cell_volume                     724.35(7)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16251
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             289
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0425P)²+0.3062P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                3725
_reflns_number_total             4026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301970w_si_002_2.cif
_cod_data_source_block           NacNac2CoACN2_1a
_cod_database_code               4330759
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
C15 C 0.3191(2) 0.2942(2) 0.97031(18) 0.0373(4) Uani 1 1 d .
H15A H 0.3073 0.4086 0.9771 0.056 Uiso 1 1 calc R
H15B H 0.2467 0.2559 1.0214 0.056 Uiso 1 1 calc R
H15C H 0.2927 0.2188 0.8752 0.056 Uiso 1 1 calc R
C10 C 0.37033(19) 0.43324(19) 0.60763(16) 0.0286(3) Uani 1 1 d .
H10A H 0.4211 0.5427 0.6103 0.043 Uiso 1 1 calc R
H10B H 0.2924 0.4497 0.6682 0.043 Uiso 1 1 calc R
H10C H 0.3157 0.3645 0.5152 0.043 Uiso 1 1 calc R
N2 N 0.87251(13) 0.10218(13) 0.90913(11) 0.0175(2) Uani 1 1 d .
H2 H 0.8203 0.1738 0.9600 0.021 Uiso 1 1 calc R
C4 C 0.84745(15) 0.08443(15) 0.77939(13) 0.0173(2) Uani 1 1 d .
C3 C 0.92191(16) -0.02171(16) 0.68402(13) 0.0194(2) Uani 1 1 d .
H3 H 0.9019 -0.0250 0.5938 0.023 Uiso 1 1 calc R
Co1 Co 1.0000 0.0000 1.0000 0.01490(8) Uani 1 2 d S
N1 N 1.06507(13) -0.12042(13) 0.83989(11) 0.0170(2) Uani 1 1 d .
H1 H 1.1339 -0.1860 0.8486 0.020 Uiso 1 1 calc R
C2 C 1.02467(15) -0.12348(15) 0.71498(12) 0.0173(2) Uani 1 1 d .
C5 C 0.72711(15) 0.17632(15) 0.73425(12) 0.0169(2) Uani 1 1 d .
C6 C 0.77395(15) 0.33792(16) 0.73421(12) 0.0183(2) Uani 1 1 d .
C12 C 0.56521(16) 0.09908(16) 0.69512(13) 0.0201(2) Uani 1 1 d .
C9 C 0.49625(17) 0.34521(17) 0.65259(13) 0.0216(3) Uani 1 1 d .
C7 C 0.94651(17) 0.42429(17) 0.78001(15) 0.0252(3) Uani 1 1 d .
H7A H 0.9606 0.5237 0.7551 0.038 Uiso 1 1 calc R
H7B H 1.0152 0.3466 0.7363 0.038 Uiso 1 1 calc R
H7C H 0.9757 0.4587 0.8783 0.038 Uiso 1 1 calc R
C11 C 0.45300(16) 0.18497(17) 0.65424(13) 0.0221(3) Uani 1 1 d .
H11 H 0.3437 0.1327 0.6267 0.027 Uiso 1 1 calc R
C13 C 0.51113(18) -0.07230(18) 0.69874(16) 0.0275(3) Uani 1 1 d .
H13A H 0.4579 -0.0602 0.7762 0.041 Uiso 1 1 calc R
H13B H 0.6041 -0.1268 0.7073 0.041 Uiso 1 1 calc R
H13C H 0.4362 -0.1412 0.6151 0.041 Uiso 1 1 calc R
C8 C 0.65701(17) 0.41981(16) 0.69309(13) 0.0207(2) Uani 1 1 d .
H8 H 0.6881 0.5292 0.6928 0.025 Uiso 1 1 calc R
C1 C 1.08536(16) -0.24659(17) 0.60075(13) 0.0219(3) Uani 1 1 d .
H1A H 1.1749 -0.2882 0.6381 0.033 Uiso 1 1 calc R
H1B H 1.1214 -0.1900 0.5419 0.033 Uiso 1 1 calc R
H1C H 0.9990 -0.3412 0.5483 0.033 Uiso 1 1 calc R
N3 N 0.6138(2) 0.2936(2) 1.06919(16) 0.0433(4) Uani 1 1 d .
C14 C 0.4841(2) 0.29343(19) 1.02582(16) 0.0319(3) Uani 1 1 d .
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
C4 N2 Co1 130.42(9) . .
N2 C4 C3 122.86(11) . .
N2 C4 C5 117.75(11) . .
C3 C4 C5 119.31(11) . .
C4 C3 C2 123.09(12) . .
N2 Co1 N2 180.00(6) 2_757 .
N2 Co1 N1 90.60(5) 2_757 2_757
N2 Co1 N1 89.40(5) . 2_757
N2 Co1 N1 89.40(5) 2_757 .
N2 Co1 N1 90.60(5) . .
N1 Co1 N1 180.0 2_757 .
C2 N1 Co1 130.71(9) . .
N1 C2 C3 122.25(11) . .
N1 C2 C1 119.21(11) . .
C3 C2 C1 118.48(11) . .
C6 C5 C12 120.48(11) . .
C6 C5 C4 120.80(11) . .
C12 C5 C4 118.69(11) . .
C8 C6 C5 118.77(12) . .
C8 C6 C7 120.22(12) . .
C5 C6 C7 121.00(11) . .
C11 C12 C5 118.76(12) . .
C11 C12 C13 119.77(12) . .
C5 C12 C13 121.47(12) . .
C8 C9 C11 118.23(12) . .
C8 C9 C10 121.75(13) . .
C11 C9 C10 120.02(13) . .
C9 C11 C12 121.97(12) . .
C9 C8 C6 121.78(12) . .
N3 C14 C15 179.60(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C15 C14 1.461(2) .
C10 C9 1.5089(18) .
N2 C4 1.3317(16) .
N2 Co1 1.8585(10) .
C4 C3 1.3959(17) .
C4 C5 1.4987(17) .
C3 C2 1.3988(17) .
Co1 N2 1.8585(10) 2_757
Co1 N1 1.8679(11) 2_757
Co1 N1 1.8679(11) .
N1 C2 1.3296(16) .
C2 C1 1.5139(17) .
C5 C6 1.4025(17) .
C5 C12 1.4068(18) .
C6 C8 1.3994(17) .
C6 C7 1.5092(19) .
C12 C11 1.3936(18) .
C12 C13 1.5093(19) .
C9 C8 1.3928(19) .
C9 C11 1.3928(19) .
N3 C14 1.147(2) .
