#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:22:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179243 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/63/4316322.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_4316322
loop_
_publ_author_name
'Chhatra B. Khadka'
'Daniel G. Macdonald'
'Yanhua Lan'
'Annie K. Powell'
'Dieter Fenske'
'John F. Corrigan'
_publ_contact_author_address
;Dept of Chemistry
The University of Western Ontario
London ON
N6A 5B7 Canada    
;
_publ_contact_author_email       corrigan@uwo.ca
_publ_contact_author_name        'John F Corrigan'
_publ_section_title
;
 Trimethylsilylchalcogenolates of Co(II) and Mn(II): From Mononuclear
 Coordination Complexes to Clusters Containing -ESiMe3 Moieties (E = S,
 Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7289
_journal_page_last               7297
_journal_paper_doi               10.1021/ic902346u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C20 H36 Co N2 Se2 Si2'
_chemical_formula_sum            'C20 H36 Co N2 Se2 Si2'
_chemical_formula_weight         577.54
_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                95.734(2)
_cell_angle_beta                 91.369(2)
_cell_angle_gamma                115.881(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0799(4)
_cell_length_b                   9.9145(5)
_cell_length_c                   16.6353(6)
_cell_measurement_reflns_used    10364
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     1336.80(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_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  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14442
_diffrn_reflns_theta_full        27.68
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         2.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0461
_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)+(0.0621P)²+2.1258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                4984
_reflns_number_total             6176
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic902346u_si_002_5.cif
_cod_data_source_block           07063
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1336.79(10)
_cod_database_code               4316322
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 1.19903(6) 0.50021(5) -0.24979(3) 0.02028(13) Uani 1 1 d . . .
Se1 Se 1.23010(5) 0.30523(5) -0.18746(2) 0.02694(12) Uani 1 1 d . . .
Se2 Se 1.41065(5) 0.70776(4) -0.30488(2) 0.02537(12) Uani 1 1 d . . .
Si1 Si 1.31982(14) 0.18611(13) -0.28278(7) 0.0274(2) Uani 1 1 d . . .
Si2 Si 1.62623(13) 0.76752(12) -0.21442(6) 0.0237(2) Uani 1 1 d . . .
N2 N 1.0090(4) 0.4092(4) -0.33873(18) 0.0225(6) Uani 1 1 d . . .
N1 N 1.0943(4) 0.5856(4) -0.16245(18) 0.0219(6) Uani 1 1 d . . .
C1 C 1.1623(6) -0.0148(5) -0.3104(3) 0.0414(11) Uani 1 1 d . . .
H1A H 1.2104 -0.0703 -0.3437 0.062 Uiso 1 1 calc R . .
H1B H 1.0677 -0.0168 -0.3410 0.062 Uiso 1 1 calc R . .
H1C H 1.1267 -0.0622 -0.2610 0.062 Uiso 1 1 calc R . .
C2 C 1.3654(6) 0.2820(5) -0.3765(3) 0.0360(10) Uani 1 1 d . . .
H2A H 1.4237 0.2398 -0.4119 0.054 Uiso 1 1 calc R . .
H2B H 1.4341 0.3905 -0.3618 0.054 Uiso 1 1 calc R . .
H2C H 1.2624 0.2661 -0.4051 0.054 Uiso 1 1 calc R . .
C3 C 1.5102(7) 0.1819(6) -0.2413(3) 0.0505(13) Uani 1 1 d . . .
H3A H 1.5417 0.1197 -0.2800 0.076 Uiso 1 1 calc R . .
H3B H 1.4899 0.1389 -0.1899 0.076 Uiso 1 1 calc R . .
H3C H 1.5990 0.2849 -0.2323 0.076 Uiso 1 1 calc R . .
C4 C 1.7618(6) 0.9753(5) -0.2061(3) 0.0428(11) Uani 1 1 d . . .
H4A H 1.8682 0.9978 -0.1788 0.064 Uiso 1 1 calc R . .
H4B H 1.7102 1.0298 -0.1748 0.064 Uiso 1 1 calc R . .
H4C H 1.7780 1.0070 -0.2605 0.064 Uiso 1 1 calc R . .
C5 C 1.7453(6) 0.6637(6) -0.2506(3) 0.0439(12) Uani 1 1 d . . .
H5A H 1.8391 0.6894 -0.2118 0.066 Uiso 1 1 calc R . .
H5B H 1.7848 0.6923 -0.3036 0.066 Uiso 1 1 calc R . .
H5C H 1.6745 0.5547 -0.2557 0.066 Uiso 1 1 calc R . .
C6 C 1.5639(5) 0.7196(5) -0.1112(2) 0.0349(10) Uani 1 1 d . . .
H6A H 1.6615 0.7429 -0.0755 0.052 Uiso 1 1 calc R . .
H6B H 1.4893 0.6117 -0.1143 0.052 Uiso 1 1 calc R . .
H6C H 1.5080 0.7789 -0.0896 0.052 Uiso 1 1 calc R . .
C7 C 0.9323(5) 0.2602(5) -0.3629(2) 0.0265(8) Uani 1 1 d . . .
H7A H 0.9649 0.1956 -0.3367 0.032 Uiso 1 1 calc R . .
C8 C 0.8074(5) 0.1962(5) -0.4245(2) 0.0308(9) Uani 1 1 d . . .
C9 C 0.7606(5) 0.2920(5) -0.4611(2) 0.0330(9) Uani 1 1 d . . .
H9A H 0.6760 0.2517 -0.5038 0.040 Uiso 1 1 calc R . .
C10 C 0.8358(5) 0.4465(5) -0.4363(2) 0.0283(9) Uani 1 1 d . . .
C11 C 0.9597(5) 0.5001(5) -0.3748(2) 0.0249(8) Uani 1 1 d . . .
H11A H 1.0125 0.6055 -0.3572 0.030 Uiso 1 1 calc R . .
C12 C 0.7268(7) 0.0277(6) -0.4490(3) 0.0502(13) Uani 1 1 d . . .
H12A H 0.6421 0.0019 -0.4932 0.075 Uiso 1 1 calc R . .
H12B H 0.6764 -0.0238 -0.4025 0.075 Uiso 1 1 calc R . .
H12C H 0.8095 -0.0046 -0.4673 0.075 Uiso 1 1 calc R . .
C13 C 0.7836(6) 0.5532(6) -0.4738(3) 0.0390(11) Uani 1 1 d . . .
H13A H 0.7515 0.5180 -0.5315 0.058 Uiso 1 1 calc R . .
H13B H 0.8753 0.6548 -0.4675 0.058 Uiso 1 1 calc R . .
H13C H 0.6903 0.5562 -0.4466 0.058 Uiso 1 1 calc R . .
C14 C 0.9583(5) 0.4927(5) -0.1304(2) 0.0257(8) Uani 1 1 d . . .
H14A H 0.9097 0.3881 -0.1499 0.031 Uiso 1 1 calc R . .
C15 C 0.8854(5) 0.5438(5) -0.0695(2) 0.0295(9) Uani 1 1 d . . .
C16 C 0.9613(5) 0.6965(5) -0.0412(2) 0.0308(9) Uani 1 1 d . . .
H16A H 0.9165 0.7345 0.0014 0.037 Uiso 1 1 calc R . .
C17 C 1.1011(5) 0.7948(5) -0.0740(2) 0.0304(9) Uani 1 1 d . . .
C18 C 1.1627(5) 0.7339(5) -0.1352(2) 0.0257(8) Uani 1 1 d . . .
H18A H 1.2576 0.7998 -0.1591 0.031 Uiso 1 1 calc R . .
C19 C 0.7300(6) 0.4360(6) -0.0371(3) 0.0398(11) Uani 1 1 d . . .
H19A H 0.7293 0.4690 0.0204 0.060 Uiso 1 1 calc R . .
H19B H 0.7241 0.3344 -0.0432 0.060 Uiso 1 1 calc R . .
H19C H 0.6351 0.4345 -0.0673 0.060 Uiso 1 1 calc R . .
C20 C 1.1845(7) 0.9614(6) -0.0455(3) 0.0482(12) Uani 1 1 d . . .
H20A H 1.1584 0.9794 0.0102 0.072 Uiso 1 1 calc R . .
H20B H 1.1459 1.0145 -0.0809 0.072 Uiso 1 1 calc R . .
H20C H 1.3035 0.9988 -0.0472 0.072 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'
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'
Se Se -0.0929 2.2259 '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
N2 Co1 N1 99.86(12) . . ?
N2 Co1 Se1 110.91(9) . . ?
N1 Co1 Se1 102.83(9) . . ?
N2 Co1 Se2 104.73(9) . . ?
N1 Co1 Se2 108.60(9) . . ?
Se1 Co1 Se2 126.75(2) . . ?
Si1 Se1 Co1 106.17(3) . . ?
Si2 Se2 Co1 101.30(3) . . ?
C3 Si1 C2 108.8(2) . . ?
C3 Si1 C1 107.5(2) . . ?
C2 Si1 C1 108.8(2) . . ?
C3 Si1 Se1 109.38(18) . . ?
C2 Si1 Se1 111.91(14) . . ?
C1 Si1 Se1 110.33(16) . . ?
C6 Si2 C5 108.3(2) . . ?
C6 Si2 C4 107.9(2) . . ?
C5 Si2 C4 109.1(2) . . ?
C6 Si2 Se2 113.14(14) . . ?
C5 Si2 Se2 109.10(16) . . ?
C4 Si2 Se2 109.19(15) . . ?
C7 N2 C11 118.4(3) . . ?
C7 N2 Co1 121.6(2) . . ?
C11 N2 Co1 120.0(3) . . ?
C14 N1 C18 118.8(3) . . ?
C14 N1 Co1 120.1(3) . . ?
C18 N1 Co1 121.0(3) . . ?
N2 C7 C8 122.9(4) . . ?
C9 C8 C7 117.6(4) . . ?
C9 C8 C12 122.2(4) . . ?
C7 C8 C12 120.2(4) . . ?
C8 C9 C10 120.8(4) . . ?
C11 C10 C9 117.5(4) . . ?
C11 C10 C13 120.6(4) . . ?
C9 C10 C13 121.8(4) . . ?
N2 C11 C10 122.8(4) . . ?
N1 C14 C15 122.5(4) . . ?
C16 C15 C14 117.3(4) . . ?
C16 C15 C19 122.1(4) . . ?
C14 C15 C19 120.6(4) . . ?
C17 C16 C15 121.1(4) . . ?
C18 C17 C16 117.3(4) . . ?
C18 C17 C20 120.3(4) . . ?
C16 C17 C20 122.3(4) . . ?
N1 C18 C17 122.9(4) . . ?
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 N2 2.057(3) . ?
Co1 N1 2.063(3) . ?
Co1 Se1 2.3988(6) . ?
Co1 Se2 2.4033(6) . ?
Se1 Si1 2.2584(11) . ?
Se2 Si2 2.2618(11) . ?
Si1 C3 1.865(5) . ?
Si1 C2 1.868(4) . ?
Si1 C1 1.877(5) . ?
Si2 C6 1.862(4) . ?
Si2 C5 1.863(5) . ?
Si2 C4 1.870(5) . ?
N2 C7 1.342(5) . ?
N2 C11 1.349(5) . ?
N1 C14 1.339(5) . ?
N1 C18 1.345(5) . ?
C7 C8 1.387(5) . ?
C8 C9 1.382(6) . ?
C8 C12 1.509(6) . ?
C9 C10 1.390(6) . ?
C10 C11 1.382(5) . ?
C10 C13 1.513(6) . ?
C14 C15 1.394(5) . ?
C15 C16 1.386(6) . ?
C15 C19 1.503(6) . ?
C16 C17 1.385(6) . ?
C17 C18 1.384(5) . ?
C17 C20 1.504(6) . ?
