#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:30:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179183 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/30/4313099.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_4313099
loop_
_publ_author_name
'Udo Beckmann'
'Eckhard Bill'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
 Dinuclear Cyano Complexes of Cobalt(III) and Iron(III) Containing
 Noninnocent 1,2,4,5-Tetrakis(2-pyridinecarboxamido)benzene Bridging
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1045
_journal_page_last               1056
_journal_paper_doi               10.1021/ic020518z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural     '[C50 H50 Co2 N12 O4], 4 CH2Cl2'
_chemical_formula_sum            'C54 H58 Cl8 Co2 N12 O4'
_chemical_formula_weight         1340.58
_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
_cell_angle_alpha                113.72(2)
_cell_angle_beta                 103.35(2)
_cell_angle_gamma                102.22(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3351(8)
_cell_length_b                   13.1244(10)
_cell_length_c                   13.3233(11)
_cell_measurement_reflns_used    5659
_cell_measurement_temperature    100(2)
_cell_volume                     1512.8(5)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       'ω, 0.3 deg./frame'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16013
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick 1994'
_exptl_crystal_colour            'red violet'
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.909
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         9710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_obs          0.0519
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0603P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1222
_refine_ls_wR_factor_obs         0.1092
_reflns_number_observed          6003
_reflns_number_total             9718
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020518z_2.cif
_cod_data_source_block           3
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1512.8(2)
_cod_database_code               4313099
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.60925(3) 0.46464(3) 0.77709(3) 0.01174(8) Uani 1 d . .
N1 N 0.7404(2) 0.5900(2) 0.9318(2) 0.0136(4) Uani 1 d . .
C2 C 0.8078(2) 0.5827(2) 1.0267(2) 0.0163(5) Uani 1 d . .
H2 H 0.7871(2) 0.5077(2) 1.0245(2) 0.020 Uiso 1 calc R .
C3 C 0.9065(3) 0.6808(2) 1.1274(2) 0.0167(5) Uani 1 d . .
H3 H 0.9507(3) 0.6715(2) 1.1925(2) 0.020 Uiso 1 calc R .
C4 C 0.9422(2) 0.7932(2) 1.1348(2) 0.0134(4) Uani 1 d . .
C5 C 0.8709(2) 0.7992(2) 1.0354(2) 0.0145(4) Uani 1 d . .
H5 H 0.8894(2) 0.8732(2) 1.0353(2) 0.017 Uiso 1 calc R .
C6 C 0.7739(2) 0.6983(2) 0.9376(2) 0.0134(4) Uani 1 d . .
O7 O 0.7185(2) 0.79177(14) 0.81973(14) 0.0193(4) Uani 1 d . .
C7 C 0.7075(2) 0.7013(2) 0.8265(2) 0.0134(4) Uani 1 d . .
N8 N 0.6350(2) 0.5853(2) 0.7348(2) 0.0119(4) Uani 1 d . .
C9 C 0.5709(2) 0.5539(2) 0.6215(2) 0.0113(4) Uani 1 d . .
C10 C 0.5709(2) 0.6288(2) 0.5707(2) 0.0125(4) Uani 1 d . .
H10 H 0.6156(2) 0.7122(2) 0.6168(2) 0.015 Uiso 1 calc R .
C11 C 0.4968(2) 0.4237(2) 0.5498(2) 0.0118(4) Uani 1 d . .
N12 N 0.5039(2) 0.3690(2) 0.6170(2) 0.0123(4) Uani 1 d . .
C13 C 0.4562(2) 0.2471(2) 0.5763(2) 0.0142(4) Uani 1 d . .
O13 O 0.4041(2) 0.16974(14) 0.47501(14) 0.0200(4) Uani 1 d . .
C14 C 0.4764(2) 0.2219(2) 0.6786(2) 0.0142(4) Uani 1 d . .
C15 C 0.4230(2) 0.1088(2) 0.6631(2) 0.0159(5) Uani 1 d . .
H15 H 0.3783(2) 0.0438(2) 0.5863(2) 0.019 Uiso 1 calc R .
C16 C 0.4345(2) 0.0898(2) 0.7603(2) 0.0162(5) Uani 1 d . .
C17 C 0.4967(3) 0.1916(2) 0.8696(2) 0.0195(5) Uani 1 d . .
H17 H 0.5028(3) 0.1842(2) 0.9385(2) 0.023 Uiso 1 calc R .
C18 C 0.5494(3) 0.3021(2) 0.8796(2) 0.0181(5) Uani 1 d . .
H18 H 0.5910(3) 0.3690(2) 0.9554(2) 0.022 Uiso 1 calc R .
N19 N 0.5438(2) 0.3183(2) 0.7855(2) 0.0142(4) Uani 1 d . .
C20 C 1.0554(3) 0.9000(2) 1.2442(2) 0.0163(5) Uani 1 d . .
C21 C 1.1901(3) 0.8702(2) 1.2762(2) 0.0231(6) Uani 1 d . .
H21A H 1.1693(5) 0.8053(11) 1.2953(15) 0.035 Uiso 1 calc R .
H21B H 1.2640(7) 0.9401(5) 1.3441(10) 0.035 Uiso 1 calc R .
H21C H 1.2228(11) 0.8463(15) 1.2095(6) 0.035 Uiso 1 calc R .
C22 C 0.9990(3) 0.9281(2) 1.3460(2) 0.0251(6) Uani 1 d . .
H22A H 1.0696(8) 0.9975(10) 1.4166(5) 0.038 Uiso 1 calc R .
H22B H 0.9802(19) 0.8600(7) 1.3609(11) 0.038 Uiso 1 calc R .
H22C H 0.9112(11) 0.9445(16) 1.3254(7) 0.038 Uiso 1 calc R .
C23 C 1.0934(3) 1.0087(2) 1.2256(2) 0.0196(5) Uani 1 d . .
H23A H 1.1663(13) 1.0752(5) 1.2972(5) 0.029 Uiso 1 calc R .
H23B H 1.0089(5) 1.0298(9) 1.2067(15) 0.029 Uiso 1 calc R .
H23C H 1.1294(17) 0.9905(5) 1.1608(10) 0.029 Uiso 1 calc R .
C24 C 0.3854(3) -0.0332(2) 0.7508(2) 0.0200(5) Uani 1 d . .
C25 C 0.2893(3) -0.1280(2) 0.6263(3) 0.0315(7) Uani 1 d . .
H25A H 0.2586(17) -0.2047(4) 0.6247(4) 0.047 Uiso 1 calc R .
H25B H 0.3414(7) -0.1328(12) 0.5727(4) 0.047 Uiso 1 calc R .
H25C H 0.2063(10) -0.1070(9) 0.6019(7) 0.047 Uiso 1 calc R .
C26 C 0.5173(3) -0.0650(2) 0.7854(3) 0.0291(6) Uani 1 d . .
H26A H 0.4887(3) -0.1438(8) 0.7797(17) 0.044 Uiso 1 calc R .
H26B H 0.5783(10) -0.0066(10) 0.8661(6) 0.044 Uiso 1 calc R .
H26C H 0.5693(12) -0.0651(17) 0.7325(11) 0.044 Uiso 1 calc R .
C27 C 0.3072(3) -0.0313(3) 0.8362(3) 0.0334(7) Uani 1 d . .
H27A H 0.2693(19) -0.1117(4) 0.8250(13) 0.050 Uiso 1 calc R .
H27B H 0.2293(14) -0.0017(18) 0.8212(12) 0.050 Uiso 1 calc R .
H27C H 0.3731(6) 0.0206(15) 0.9169(3) 0.050 Uiso 1 calc R .
C30 C 0.7696(2) 0.4274(2) 0.7427(2) 0.0150(5) Uani 1 d . .
N30 N 0.8631(2) 0.4037(2) 0.7190(2) 0.0237(5) Uani 1 d . .
C40 C 0.4506(3) 0.5023(2) 0.8152(2) 0.0161(5) Uani 1 d . .
N40 N 0.3572(2) 0.5278(2) 0.8385(2) 0.0232(5) Uani 1 d . .
C50 C 0.1027(3) 0.4062(2) 0.5809(3) 0.0270(6) Uani 1 d . .
H50A H 0.1286(3) 0.4317(2) 0.6658(3) 0.032 Uiso 1 calc R .
H50B H 0.0007(3) 0.3932(2) 0.5488(3) 0.032 Uiso 1 calc R .
Cl1 Cl 0.20176(8) 0.51983(6) 0.56113(7) 0.0302(2) Uani 1 d . .
Cl2 Cl 0.13276(8) 0.27138(6) 0.51113(7) 0.0308(2) Uani 1 d . .
C60 C 1.1087(3) 0.6553(3) 0.8163(3) 0.0300(6) Uani 1 d . .
H60A H 1.0644(3) 0.5684(3) 0.7807(3) 0.036 Uiso 1 calc R 1
H60B H 1.1981(3) 0.6712(3) 0.8009(3) 0.036 Uiso 1 calc R 1
Cl3 Cl 0.99536(8) 0.70828(7) 0.74661(8) 0.0421(2) Uani 1 d . .
Cl4 Cl 1.14834(15) 0.7159(2) 0.96530(10) 0.0576(4) Uani 0.75 d P 1
Cl4X Cl 1.1746(5) 0.7785(4) 0.9702(4) 0.0535(12) Uiso 0.25 d P 2
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'
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'
Cl Cl 0.1484 0.1585 '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
N8 Co1 N12 83.07(8) . . ?
N8 Co1 C30 92.82(9) . . ?
N12 Co1 C30 87.39(9) . . ?
N8 Co1 C40 87.99(9) . . ?
N12 Co1 C40 93.81(9) . . ?
C30 Co1 C40 178.62(10) . . ?
N8 Co1 N19 166.14(8) . . ?
N12 Co1 N19 83.87(8) . . ?
C30 Co1 N19 91.19(9) . . ?
C40 Co1 N19 88.27(9) . . ?
N8 Co1 N1 84.26(8) . . ?
N12 Co1 N1 166.33(8) . . ?
C30 Co1 N1 88.12(9) . . ?
C40 Co1 N1 90.86(9) . . ?
N19 Co1 N1 109.14(8) . . ?
C2 N1 C6 117.1(2) . . ?
C2 N1 Co1 130.0(2) . . ?
C6 N1 Co1 112.60(14) . . ?
N1 C2 C3 122.4(2) . . ?
C2 C3 C4 121.2(2) . . ?
C3 C4 C5 115.7(2) . . ?
C3 C4 C20 120.9(2) . . ?
C5 C4 C20 123.4(2) . . ?
C6 C5 C4 120.3(2) . . ?
N1 C6 C5 123.2(2) . . ?
N1 C6 C7 115.8(2) . . ?
C5 C6 C7 120.8(2) . . ?
O7 C7 N8 126.6(2) . . ?
O7 C7 C6 123.7(2) . . ?
N8 C7 C6 109.7(2) . . ?
C9 N8 C7 126.1(2) . . ?
C9 N8 Co1 116.97(15) . . ?
C7 N8 Co1 116.56(14) . . ?
N8 C9 C10 127.1(2) . . ?
N8 C9 C11 111.6(2) . . ?
C10 C9 C11 121.3(2) . . ?
C11 C10 C9 117.3(2) 2_666 . ?
N12 C11 C10 127.1(2) . 2_666 ?
N12 C11 C9 111.6(2) . . ?
C10 C11 C9 121.4(2) 2_666 . ?
C11 N12 C13 126.0(2) . . ?
C11 N12 Co1 116.65(15) . . ?
C13 N12 Co1 116.77(15) . . ?
O13 C13 N12 127.1(2) . . ?
O13 C13 C14 123.1(2) . . ?
N12 C13 C14 109.8(2) . . ?
N19 C14 C15 123.0(2) . . ?
N19 C14 C13 115.2(2) . . ?
C15 C14 C13 121.7(2) . . ?
C14 C15 C16 120.2(2) . . ?
C15 C16 C17 115.7(2) . . ?
C15 C16 C24 123.4(2) . . ?
C17 C16 C24 120.9(2) . . ?
C18 C17 C16 121.5(2) . . ?
N19 C18 C17 122.1(2) . . ?
C18 N19 C14 117.3(2) . . ?
C18 N19 Co1 129.6(2) . . ?
C14 N19 Co1 112.91(15) . . ?
C4 C20 C23 111.7(2) . . ?
C4 C20 C21 109.7(2) . . ?
C23 C20 C21 108.5(2) . . ?
C4 C20 C22 108.4(2) . . ?
C23 C20 C22 109.7(2) . . ?
C21 C20 C22 108.8(2) . . ?
C25 C24 C16 112.2(2) . . ?
C25 C24 C26 108.6(2) . . ?
C16 C24 C26 107.8(2) . . ?
C25 C24 C27 109.5(2) . . ?
C16 C24 C27 110.0(2) . . ?
C26 C24 C27 108.6(2) . . ?
N30 C30 Co1 178.1(2) . . ?
N40 C40 Co1 178.2(2) . . ?
Cl2 C50 Cl1 112.15(15) . . ?
Cl4 C60 Cl3 114.8(2) . . ?
Cl3 C60 Cl4X 99.6(2) . . ?
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 N8 1.872(2) . ?
Co1 N12 1.873(2) . ?
Co1 C30 1.926(3) . ?
Co1 C40 1.928(3) . ?
Co1 N19 1.953(2) . ?
Co1 N1 1.957(2) . ?
N1 C2 1.345(3) . ?
N1 C6 1.355(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.400(3) . ?
C4 C5 1.400(3) . ?
C4 C20 1.528(3) . ?
C5 C6 1.380(3) . ?
C6 C7 1.501(3) . ?
O7 C7 1.210(3) . ?
C7 N8 1.404(3) . ?
N8 C9 1.346(3) . ?
C9 C10 1.400(3) . ?
C9 C11 1.488(3) . ?
C10 C11 1.388(3) 2_666 ?
C11 N12 1.353(3) . ?
C11 C10 1.388(3) 2_666 ?
N12 C13 1.393(3) . ?
C13 O13 1.214(3) . ?
C13 C14 1.506(3) . ?
C14 N19 1.354(3) . ?
C14 C15 1.380(3) . ?
C15 C16 1.397(3) . ?
C16 C17 1.399(4) . ?
C16 C24 1.530(3) . ?
C17 C18 1.377(3) . ?
C18 N19 1.344(3) . ?
C20 C23 1.530(3) . ?
C20 C21 1.537(3) . ?
C20 C22 1.539(4) . ?
C24 C25 1.530(4) . ?
C24 C26 1.533(4) . ?
C24 C27 1.536(4) . ?
C30 N30 1.149(3) . ?
C40 N40 1.154(3) . ?
C50 Cl2 1.770(3) . ?
C50 Cl1 1.771(3) . ?
C60 Cl4 1.720(3) . ?
C60 Cl3 1.754(3) . ?
C60 Cl4X 1.872(6) . ?
