#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318517.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_4318517
loop_
_publ_author_name
'Christine E. Plečnik'
'Shengming Liu'
'Jianping Liu'
'Xuenian Chen'
'Edward A. Meyers'
'Sheldon G. Shore'
_publ_section_title
;
 Lanthanide-Transition-Metal Carbonyl Complexes. 1. Syntheses and
 Structures of Ytterbium(II) Solvent-Separated Ion Pairs and Isocarbonyl
 Polymeric Arrays of Tetracarbonylcobaltate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4936
_journal_page_last               4943
_journal_paper_doi               10.1021/ic020254g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C28 H20 Co2 N4 O8 Yb'
_chemical_formula_weight         831.38
_chemical_name_common            '[(Pyr)4Yb{(u-CO)2Co(CO)2}2]inf'
_chemical_name_systematic
;
 bis[u-(carbonyl-C,O)](dicarbonylcobalt)(tetrapyridine)ytterbium
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0467(10)
_cell_length_b                   13.4232(10)
_cell_length_c                   21.9334(10)
_cell_measurement_reflns_used    '10 frames'
_cell_measurement_temperature    150(2)
_cell_volume                     3162.6(4)
_computing_cell_refinement       'DENZO (Otwinowsky & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowsky & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       'omega at 55/-55'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10572
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_T_max  0.4098
_exptl_absorpt_correction_T_min  0.3103
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0158
_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)+(0.0142P)²+2.3747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0366
_reflns_number_gt                2649
_reflns_number_total             2794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020254g_2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4318517
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.0000 0.182846(9) 0.2500 0.01650(5) Uani 1 2 d S . .
N1 N 0.20416(17) 0.11748(13) 0.32236(9) 0.0275(4) Uani 1 1 d . . .
C11 C 0.2966(2) 0.07678(19) 0.30072(12) 0.0375(6) Uani 1 1 d . . .
H11 H 0.2875 0.0724 0.2567 0.045 Uiso 1 1 calc . . .
C12 C 0.4041(3) 0.0410(2) 0.33950(17) 0.0619(9) Uani 1 1 d . . .
H12 H 0.4676 0.0127 0.3223 0.074 Uiso 1 1 calc . . .
C13 C 0.4187(3) 0.0466(3) 0.40314(18) 0.0668(10) Uani 1 1 d . . .
H13 H 0.4922 0.0223 0.4307 0.080 Uiso 1 1 calc . . .
C14 C 0.3247(3) 0.0883(2) 0.42654(13) 0.0494(7) Uani 1 1 d . . .
H14 H 0.3319 0.0933 0.4704 0.059 Uiso 1 1 calc . . .
C15 C 0.2210(2) 0.12204(18) 0.38467(12) 0.0355(6) Uani 1 1 d . . .
H15 H 0.1565 0.1507 0.4010 0.043 Uiso 1 1 calc . . .
N2 N 0.15687(16) 0.25042(13) 0.18939(8) 0.0227(4) Uani 1 1 d . . .
C21 C 0.2673(2) 0.29015(18) 0.21565(11) 0.0296(5) Uani 1 1 d . . .
H21 H 0.2951 0.2884 0.2600 0.036 Uiso 1 1 calc . . .
C22 C 0.3432(2) 0.3338(2) 0.18116(13) 0.0407(7) Uani 1 1 d . . .
H22 H 0.4209 0.3620 0.2017 0.049 Uiso 1 1 calc . . .
C23 C 0.3054(3) 0.3360(2) 0.11708(12) 0.0400(7) Uani 1 1 d . . .
H23 H 0.3562 0.3653 0.0925 0.048 Uiso 1 1 calc . . .
C24 C 0.1922(2) 0.29486(19) 0.08928(11) 0.0339(6) Uani 1 1 d . . .
H24 H 0.1629 0.2951 0.0450 0.041 Uiso 1 1 calc . . .
C25 C 0.1219(2) 0.25323(17) 0.12694(10) 0.0285(5) Uani 1 1 d . . .
H25 H 0.0438 0.2248 0.1073 0.034 Uiso 1 1 calc . . .
Co1 Co 0.19144(3) -0.06137(2) 0.108090(13) 0.02254(8) Uani 1 1 d . . .
C1 C 0.3186(2) -0.12570(16) 0.15321(10) 0.0224(5) Uani 1 1 d . . .
O1 O 0.40188(15) -0.16852(11) 0.18477(8) 0.0292(4) Uani 1 1 d . . .
C2 C 0.1016(2) -0.1434(2) 0.05194(13) 0.0407(6) Uani 1 1 d . . .
O2 O 0.0448(2) -0.19564(17) 0.01474(11) 0.0693(7) Uani 1 1 d . . .
C3 C 0.2391(3) 0.0336(2) 0.06293(12) 0.0392(7) Uani 1 1 d . . .
O3 O 0.2707(2) 0.09484(16) 0.03353(10) 0.0679(7) Uani 1 1 d . . .
C4 C 0.1049(2) -0.00554(16) 0.15583(10) 0.0231(5) Uani 1 1 d . . .
O4 O 0.05012(15) 0.03431(11) 0.18847(7) 0.0294(4) 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'
O O 0.0106 0.0060 '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'
Yb Yb -0.3850 5.5486 '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'
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
O4 Yb1 O4 76.56(7) . 2 ?
O4 Yb1 O1 142.84(5) . 4 ?
O4 Yb1 O1 115.70(5) 2 4 ?
O4 Yb1 O1 115.70(5) . 3_455 ?
O4 Yb1 O1 142.84(5) 2 3_455 ?
O1 Yb1 O1 76.78(7) 4 3_455 ?
O4 Yb1 N2 143.60(5) . 2 ?
O4 Yb1 N2 75.32(5) 2 2 ?
O1 Yb1 N2 71.59(5) 4 2 ?
O1 Yb1 N2 76.42(5) 3_455 2 ?
O4 Yb1 N2 75.32(5) . . ?
O4 Yb1 N2 143.60(5) 2 . ?
O1 Yb1 N2 76.42(5) 4 . ?
O1 Yb1 N2 71.59(5) 3_455 . ?
N2 Yb1 N2 138.87(8) 2 . ?
O4 Yb1 N1 71.03(5) . 2 ?
O4 Yb1 N1 78.06(6) 2 2 ?
O1 Yb1 N1 143.70(5) 4 2 ?
O1 Yb1 N1 74.05(5) 3_455 2 ?
N2 Yb1 N1 80.88(6) 2 2 ?
N2 Yb1 N1 113.37(6) . 2 ?
O4 Yb1 N1 78.06(6) . . ?
O4 Yb1 N1 71.03(5) 2 . ?
O1 Yb1 N1 74.05(5) 4 . ?
O1 Yb1 N1 143.70(6) 3_455 . ?
N2 Yb1 N1 113.37(6) 2 . ?
N2 Yb1 N1 80.88(6) . . ?
N1 Yb1 N1 140.39(8) 2 . ?
C15 N1 C11 116.5(2) . . ?
C15 N1 Yb1 120.30(15) . . ?
C11 N1 Yb1 123.24(16) . . ?
N1 C11 C12 122.9(3) . . ?
N1 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C13 C12 C11 119.3(3) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 118.8(3) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C15 C14 C13 118.0(3) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
N1 C15 C14 124.5(2) . . ?
N1 C15 H15 117.8 . . ?
C14 C15 H15 117.8 . . ?
C21 N2 C25 116.67(19) . . ?
C21 N2 Yb1 125.06(14) . . ?
C25 N2 Yb1 118.06(14) . . ?
N2 C21 C22 122.9(2) . . ?
N2 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 118.4(2) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 H23 120.8 . . ?
C23 C24 C25 118.6(2) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N2 C25 C24 124.0(2) . . ?
N2 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
C4 Co1 C1 110.69(10) . . ?
C4 Co1 C3 107.64(10) . . ?
C1 Co1 C3 111.66(11) . . ?
C4 Co1 C2 112.80(11) . . ?
C1 Co1 C2 109.42(11) . . ?
C3 Co1 C2 104.49(13) . . ?
O1 C1 Co1 178.08(19) . . ?
C1 O1 Yb1 153.35(15) . 3_545 ?
O2 C2 Co1 178.6(3) . . ?
O3 C3 Co1 179.5(2) . . ?
O4 C4 Co1 177.7(2) . . ?
C4 O4 Yb1 153.19(15) . . ?
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
Yb1 O4 2.5401(15) . ?
Yb1 O4 2.5401(15) 2 ?
Yb1 O1 2.5454(15) 4 ?
Yb1 O1 2.5454(15) 3_455 ?
Yb1 N2 2.5822(17) 2 ?
Yb1 N2 2.5822(17) . ?
Yb1 N1 2.5894(19) 2 ?
Yb1 N1 2.5894(19) . ?
N1 C15 1.337(3) . ?
N1 C11 1.339(3) . ?
C11 C12 1.376(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.370(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.368(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N2 C21 1.333(3) . ?
N2 C25 1.334(3) . ?
C21 C22 1.384(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.370(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
Co1 C4 1.743(2) . ?
Co1 C1 1.746(2) . ?
Co1 C3 1.768(3) . ?
Co1 C2 1.773(3) . ?
C1 O1 1.166(3) . ?
O1 Yb1 2.5454(15) 3_545 ?
C2 O2 1.146(3) . ?
C3 O3 1.148(3) . ?
C4 O4 1.169(3) . ?
