#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:29:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178567 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/76/4067625.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_4067625
loop_
_publ_author_name
'Zhu, Di'
'Janssen, Femke F. B. J.'
'Budzelaar, Peter H. M.'
_publ_contact_author
;
        Peter H.M. Budzelaar
        Department of Chemistry
        University of Manitoba
        Winnipeg, MB R3T 2N2
        Canada
;
_publ_section_title
;
 (Py)2Co(CH2SiMe3)2As an Easily Accessible Source of “CoR2”
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1897
_journal_paper_doi               10.1021/om901045s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C29 H38 Co N3 Si'
_chemical_formula_sum            'C29 H38 Co N3 Si'
_chemical_formula_weight         515.64
_chemical_name_systematic
;
{2,6-bis[1-(2,6-dimethylphenylimino)ethyl]pyridine}
(trimethylsilylmethyl) cobalt(I)
;
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 99.1876(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6802(3)
_cell_length_b                   21.2770(10)
_cell_length_c                   8.5207(4)
_cell_measurement_reflns_used    7851
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.574
_cell_measurement_theta_min      2.4215
_cell_volume                     1374.52(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker 4-circle, APEX detector'
_diffrn_measurement_method       'area detector phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9173
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'deep purple'
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_recrystallization_method hexance/toluene
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0675P)²+0.2183P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                2459
_reflns_number_total             2634
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om901045s_si_002.cif
_cod_data_source_block           2dm0m
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4067625
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
Co1 Co 0.68935(4) 0.7500 0.91742(4) 0.03573(14) Uani 1 2 d S
N1 N 0.5865(3) 0.7500 1.0974(2) 0.0376(4) Uani 1 2 d S
N2 N 0.67877(18) 0.66118(7) 0.95193(18) 0.0401(3) Uani 1 1 d .
C1 C 0.6009(2) 0.64302(9) 1.0730(2) 0.0436(4) Uani 1 1 d .
C2 C 0.5384(2) 0.69433(9) 1.1578(2) 0.0414(4) Uani 1 1 d .
C3 C 0.4441(3) 0.69342(10) 1.2835(2) 0.0520(5) Uani 1 1 d .
H1 H 0.4126 0.6555 1.3252 0.062 Uiso 1 1 calc R
C4 C 0.3975(4) 0.7500 1.3464(4) 0.0569(7) Uani 1 2 d S
H2 H 0.3347 0.7500 1.4311 0.068 Uiso 1 2 calc SR
C5 C 0.7523(2) 0.61314(8) 0.8641(2) 0.0441(4) Uani 1 1 d .
C6 C 0.6465(3) 0.58481(10) 0.7344(3) 0.0552(5) Uani 1 1 d .
C7 C 0.9278(3) 0.59555(10) 0.9126(3) 0.0538(5) Uani 1 1 d .
C8 C 0.9971(3) 0.54878(12) 0.8267(4) 0.0729(7) Uani 1 1 d .
H3 H 1.1136 0.5362 0.8569 0.088 Uiso 1 1 calc R
C9 C 0.8958(4) 0.52076(11) 0.6975(4) 0.0789(8) Uani 1 1 d .
H4 H 0.9443 0.4897 0.6410 0.095 Uiso 1 1 calc R
C10 C 0.7226(4) 0.53870(11) 0.6521(3) 0.0734(7) Uani 1 1 d .
H5 H 0.6555 0.5195 0.5646 0.088 Uiso 1 1 calc R
C11 C 0.4562(3) 0.60262(13) 0.6882(3) 0.0714(7) Uani 1 1 d .
H6 H 0.4086 0.5823 0.5902 0.107 Uiso 1 1 calc R
H7 H 0.4467 0.6474 0.6749 0.107 Uiso 1 1 calc R
H8 H 0.3913 0.5896 0.7701 0.107 Uiso 1 1 calc R
C12 C 1.0367(3) 0.62505(13) 1.0554(3) 0.0719(7) Uani 1 1 d .
H9 H 1.0225 0.6699 1.0501 0.108 Uiso 1 1 calc R
H10 H 1.1586 0.6146 1.0573 0.108 Uiso 1 1 calc R
H11 H 0.9987 0.6095 1.1502 0.108 Uiso 1 1 calc R
C13 C 0.5825(3) 0.57631(10) 1.1228(3) 0.0626(6) Uani 1 1 d .
H12 H 0.5911 0.5489 1.0349 0.094 Uiso 1 1 calc R
H13 H 0.4699 0.5707 1.1562 0.094 Uiso 1 1 calc R
H14 H 0.6746 0.5665 1.2094 0.094 Uiso 1 1 calc R
C14 C 0.7354(3) 0.7500 0.6972(3) 0.0443(6) Uani 1 2 d S
H15 H 0.6730 0.7136 0.6479 0.053 Uiso 0.50 1 calc PR
H16 H 0.6730 0.7864 0.6479 0.053 Uiso 0.50 1 calc PR
Si Si 0.95224(10) 0.7500 0.62445(9) 0.0470(2) Uani 1 2 d S
C15 C 0.9678(3) 0.67919(13) 0.4969(3) 0.0724(7) Uani 1 1 d .
H17 H 0.9627 0.6418 0.5592 0.109 Uiso 1 1 calc R
H18 H 1.0772 0.6802 0.4561 0.109 Uiso 1 1 calc R
H19 H 0.8713 0.6793 0.4100 0.109 Uiso 1 1 calc R
C16 C 1.1531(4) 0.7500 0.7794(5) 0.0766(10) Uani 1 2 d S
H20 H 1.1687 0.7091 0.8271 0.115 Uiso 0.50 1 calc PR
H21 H 1.1398 0.7806 0.8595 0.115 Uiso 0.50 1 calc PR
H22 H 1.2544 0.7603 0.7314 0.115 Uiso 0.50 1 calc PR
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'
Si Si 0.0817 0.0704 '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 N2 80.63(5) . .
N1 Co1 N2 80.63(5) . 4_575
N2 Co1 N2 160.94(9) . 4_575
N1 Co1 C14 165.07(10) . .
N2 Co1 C14 99.50(5) . .
N2 Co1 C14 99.50(5) 4_575 .
C2 N1 C2 120.3(2) . 4_575
C2 N1 Co1 119.56(11) . .
C2 N1 Co1 119.56(11) 4_575 .
C1 N2 C5 117.45(15) . .
C1 N2 Co1 116.17(12) . .
C5 N2 Co1 126.33(12) . .
N2 C1 C2 113.45(16) . .
N2 C1 C13 124.82(18) . .
C2 C1 C13 121.70(17) . .
N1 C2 C3 120.62(18) . .
N1 C2 C1 109.78(16) . .
C3 C2 C1 129.60(18) . .
C2 C3 C4 119.0(2) . .
C3 C4 C3 120.4(3) . 4_575
C7 C5 C6 122.00(19) . .
C7 C5 N2 118.56(17) . .
C6 C5 N2 119.44(17) . .
C10 C6 C5 117.7(2) . .
C10 C6 C11 121.2(2) . .
C5 C6 C11 121.12(19) . .
C8 C7 C5 117.9(2) . .
C8 C7 C12 121.0(2) . .
C5 C7 C12 121.01(19) . .
C9 C8 C7 121.0(2) . .
C8 C9 C10 120.1(2) . .
C9 C10 C6 121.3(2) . .
Si C14 Co1 128.55(15) . .
C16 Si C14 116.51(15) . .
C16 Si C15 106.79(11) . .
C14 Si C15 109.60(9) . .
C16 Si C15 106.79(11) . 4_575
C14 Si C15 109.60(9) . 4_575
C15 Si C15 107.13(18) . 4_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.834(2) .
Co1 N2 1.9164(15) .
Co1 N2 1.9165(15) 4_575
Co1 C14 1.964(3) .
N1 C2 1.365(2) .
N1 C2 1.366(2) 4_575
N2 C1 1.330(2) .
N2 C5 1.435(2) .
C1 C2 1.434(3) .
C1 C13 1.495(3) .
C2 C3 1.386(3) .
C3 C4 1.387(3) .
C4 C3 1.387(3) 4_575
C5 C7 1.396(3) .
C5 C6 1.399(3) .
C6 C10 1.388(3) .
C6 C11 1.500(3) .
C7 C8 1.391(3) .
C7 C12 1.500(3) .
C8 C9 1.378(4) .
C9 C10 1.378(4) .
C14 Si 1.867(3) .
Si C16 1.863(4) .
Si C15 1.873(2) .
Si C15 1.873(2) 4_575
