#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:01:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179274 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319401.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_4319401
loop_
_publ_author_name
'Rodolphe Clérac'
'F. Albert Cotton'
'Lee M. Daniels'
'Kim R. Dunbar'
'Carlos A. Murillo'
'Xiaoping Wang'
_publ_section_title
;
 Tuning the Metal-Metal Bonds in the Linear Tricobalt Compound
 Co3(dpa)4Cl2: Bond-Stretch and Spin-State Isomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1256
_journal_page_last               1264
_journal_paper_doi               10.1021/ic001068i
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesis
_chemical_formula_sum            'C42 H36 Cl2 Co3 N12 O'
_chemical_formula_weight         972.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7906(6)
_cell_length_b                   14.1355(9)
_cell_length_c                   23.6060(10)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      9.05
_cell_volume                     4268.0(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21289
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.167
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_obs          0.0418
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0652P)²+6.1922P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1278
_refine_ls_wR_factor_obs         0.1212
_reflns_number_observed          3319
_reflns_number_total             3734
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001068i_04.cif
_cod_data_source_block           1.THFat213K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+6.1922P] 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^)+(0.0652P)^2^+6.1922P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319401
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.08831(3) 0.17579(3) 0.14819(2) 0.0191(2) Uani 1 d . .
Co2 Co 0.2500 0.2500 0.15012(2) 0.0158(2) Uani 1 d S .
Cl1 Cl -0.08184(6) 0.09826(6) 0.14477(3) 0.0300(2) Uani 1 d . .
N1 N 0.1648(2) 0.0648(2) 0.17926(10) 0.0223(5) Uani 1 d . .
N2 N 0.2975(2) 0.1653(2) 0.20725(10) 0.0188(5) Uani 1 d . .
N3 N 0.4219(2) 0.2777(2) 0.22787(10) 0.0201(5) Uani 1 d . .
N4 N 0.1275(2) 0.1392(2) 0.06934(10) 0.0238(5) Uani 1 d . .
N5 N 0.2988(2) 0.1650(2) 0.09366(10) 0.0224(5) Uani 1 d . .
N6 N 0.4669(2) 0.2009(2) 0.12158(10) 0.0242(5) Uani 1 d . .
C1 C 0.1245(3) -0.0229(2) 0.17506(15) 0.0327(7) Uani 1 d . .
H1A H 0.0643(3) -0.0314(2) 0.15285(15) 0.039 Uiso 1 calc R .
C2 C 0.1664(3) -0.1005(3) 0.2013(2) 0.0454(10) Uani 1 d . .
H2A H 0.1347(3) -0.1603(3) 0.1981(2) 0.054 Uiso 1 calc R .
C3 C 0.2573(3) -0.0886(2) 0.2330(2) 0.0415(9) Uani 1 d . .
H3A H 0.2873(3) -0.1402(2) 0.2522(2) 0.050 Uiso 1 calc R .
C4 C 0.3026(3) -0.0011(2) 0.23595(15) 0.0319(7) Uani 1 d . .
H4A H 0.3652(3) 0.0072(2) 0.25617(15) 0.038 Uiso 1 calc R .
C5 C 0.2557(2) 0.0767(2) 0.20881(12) 0.0212(6) Uani 1 d . .
C6 C 0.3638(2) 0.2030(2) 0.24662(12) 0.0214(6) Uani 1 d . .
C7 C 0.3679(3) 0.1768(2) 0.30410(14) 0.0301(7) Uani 1 d . .
H7A H 0.3293(3) 0.1244(2) 0.31694(14) 0.036 Uiso 1 calc R .
C8 C 0.4281(3) 0.2275(3) 0.34146(14) 0.0362(8) Uani 1 d . .
H8A H 0.4307(3) 0.2103(3) 0.37989(14) 0.043 Uiso 1 calc R .
C9 C 0.4852(3) 0.3047(2) 0.32188(14) 0.0345(8) Uani 1 d . .
H9A H 0.5270(3) 0.3403(2) 0.34672(14) 0.041 Uiso 1 calc R .
C10 C 0.4790(2) 0.3276(2) 0.26558(13) 0.0262(7) Uani 1 d . .
H10A H 0.5163(2) 0.3806(2) 0.25259(13) 0.031 Uiso 1 calc R .
C11 C 0.0542(3) 0.1194(2) 0.02975(14) 0.0325(7) Uani 1 d . .
H11A H -0.0166(3) 0.1260(2) 0.03967(14) 0.039 Uiso 1 calc R .
C12 C 0.0781(3) 0.0901(3) -0.02429(14) 0.0395(9) Uani 1 d . .
H12A H 0.0248(3) 0.0758(3) -0.05033(14) 0.047 Uiso 1 calc R .
C13 C 0.1818(3) 0.0824(3) -0.03947(14) 0.0437(9) Uani 1 d . .
H13A H 0.2002(3) 0.0614(3) -0.07592(14) 0.052 Uiso 1 calc R .
C14 C 0.2580(3) 0.1055(3) -0.00094(14) 0.0391(8) Uani 1 d . .
H14A H 0.3288(3) 0.1025(3) -0.01133(14) 0.047 Uiso 1 calc R .
C15 C 0.2297(2) 0.1337(2) 0.05429(13) 0.0259(7) Uani 1 d . .
C16 C 0.4016(2) 0.1378(2) 0.09609(12) 0.0252(7) Uani 1 d . .
C17 C 0.4394(3) 0.0477(3) 0.0801(2) 0.0386(8) Uani 1 d . .
H17A H 0.3946(3) 0.0043(3) 0.0622(2) 0.046 Uiso 1 calc R .
C18 C 0.5405(3) 0.0239(3) 0.0905(2) 0.0461(10) Uani 1 d . .
H18A H 0.5657(3) -0.0359(3) 0.0797(2) 0.055 Uiso 1 calc R .
C19 C 0.6067(3) 0.0883(3) 0.1173(2) 0.0465(10) Uani 1 d . .
H19A H 0.6770(3) 0.0730(3) 0.1246(2) 0.056 Uiso 1 calc R .
C20 C 0.5667(3) 0.1746(3) 0.1327(2) 0.0342(8) Uani 1 d . .
H20A H 0.6105(3) 0.2175(3) 0.1518(2) 0.041 Uiso 1 calc R .
O1S O -0.1588(13) 0.2824(12) -0.0237(8) 0.102(5) Uiso 0.30 d P 1
O2S O -0.1571(21) 0.2321(20) -0.0548(12) 0.110(8) Uiso 0.20 d P 2
C1S C -0.1828(16) 0.3255(14) -0.0576(9) 0.099(5) Uiso 0.38 d P .
C2S C -0.2500 0.2500 0.0135(16) 0.167(12) Uiso 0.50 d SP .
C3S C -0.2192(18) 0.1701(17) -0.0329(10) 0.115(7) Uiso 0.38 d P .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N6 Co1 N1 170.17(10) 2 . ?
N6 Co1 N4 91.26(10) 2 . ?
N1 Co1 N4 90.90(10) . . ?
N6 Co1 N3 89.19(10) 2 2 ?
N1 Co1 N3 86.82(10) . 2 ?
N4 Co1 N3 168.62(10) . 2 ?
N6 Co1 Co2 85.76(7) 2 . ?
N1 Co1 Co2 84.87(7) . . ?
N4 Co1 Co2 84.94(7) . . ?
N3 Co1 Co2 83.75(7) 2 . ?
N6 Co1 Cl1 93.84(7) 2 . ?
N1 Co1 Cl1 95.56(7) . . ?
N4 Co1 Cl1 94.38(7) . . ?
N3 Co1 Cl1 96.93(7) 2 . ?
Co2 Co1 Cl1 179.21(3) . . ?
N5 Co2 N5 90.9(2) 2 . ?
N5 Co2 N2 179.29(10) 2 . ?
N5 Co2 N2 89.68(11) . . ?
N5 Co2 N2 89.69(11) 2 2 ?
N5 Co2 N2 179.29(10) . 2 ?
N2 Co2 N2 89.73(14) . 2 ?
N5 Co2 Co1 88.80(7) 2 . ?
N5 Co2 Co1 89.62(7) . . ?
N2 Co2 Co1 90.80(7) . . ?
N2 Co2 Co1 90.79(7) 2 . ?
N5 Co2 Co1 89.62(7) 2 2 ?
N5 Co2 Co1 88.81(7) . 2 ?
N2 Co2 Co1 90.79(7) . 2 ?
N2 Co2 Co1 90.80(7) 2 2 ?
Co1 Co2 Co1 177.75(3) . 2 ?
C1 N1 C5 118.5(3) . . ?
C1 N1 Co1 120.7(2) . . ?
C5 N1 Co1 120.6(2) . . ?
C5 N2 C6 125.7(2) . . ?
C5 N2 Co2 118.2(2) . . ?
C6 N2 Co2 115.8(2) . . ?
C10 N3 C6 119.0(3) . . ?
C10 N3 Co1 119.0(2) . 2 ?
C6 N3 Co1 121.6(2) . 2 ?
C11 N4 C15 118.4(3) . . ?
C11 N4 Co1 121.6(2) . . ?
C15 N4 Co1 120.0(2) . . ?
C15 N5 C16 124.2(3) . . ?
C15 N5 Co2 118.2(2) . . ?
C16 N5 Co2 117.6(2) . . ?
C20 N6 C16 118.9(3) . . ?
C20 N6 Co1 121.0(2) . 2 ?
C16 N6 Co1 119.8(2) . 2 ?
N1 C1 C2 123.7(3) . . ?
C1 C2 C3 118.3(3) . . ?
C4 C3 C2 119.3(3) . . ?
C3 C4 C5 120.3(3) . . ?
N2 C5 N1 115.7(2) . . ?
N2 C5 C4 124.3(3) . . ?
N1 C5 C4 119.9(3) . . ?
N3 C6 N2 114.8(2) . . ?
N3 C6 C7 119.7(3) . . ?
N2 C6 C7 125.2(3) . . ?
C8 C7 C6 120.2(3) . . ?
C7 C8 C9 119.4(3) . . ?
C10 C9 C8 118.5(3) . . ?
N3 C10 C9 123.2(3) . . ?
N4 C11 C12 123.3(3) . . ?
C11 C12 C13 118.6(3) . . ?
C14 C13 C12 119.5(3) . . ?
C13 C14 C15 119.9(3) . . ?
N5 C15 N4 115.5(3) . . ?
N5 C15 C14 124.0(3) . . ?
N4 C15 C14 120.3(3) . . ?
N6 C16 N5 115.0(3) . . ?
N6 C16 C17 119.9(3) . . ?
N5 C16 C17 124.7(3) . . ?
C18 C17 C16 120.0(3) . . ?
C17 C18 C19 119.9(3) . . ?
C20 C19 C18 118.3(3) . . ?
N6 C20 C19 122.9(3) . . ?
C1S O1S C3S 53.9(15) . 2_455 ?
C1S O1S C3S 107.4(19) . . ?
C3S O1S C3S 86.5(14) 2_455 . ?
C3S O2S C1S 121.9(26) . . ?
O1S C1S C3S 88.2(20) . 2_455 ?
O2S C1S C3S 104.0(20) . 2_455 ?
C3S C2S C3S 95.0(26) . 2_455 ?
O2S C3S C1S 111.0(23) . 2_455 ?
O2S C3S C2S 87.0(20) . . ?
C1S C3S C2S 91.9(17) 2_455 . ?
C1S C3S O1S 37.9(11) 2_455 2_455 ?
C2S C3S O1S 54.5(10) . 2_455 ?
C1S C3S O1S 113.9(17) 2_455 . ?
C2S C3S O1S 53.2(10) . . ?
O1S C3S O1S 91.7(13) 2_455 . ?
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 N6 1.983(3) 2 ?
Co1 N1 1.990(2) . ?
Co1 N4 1.996(3) . ?
Co1 N3 1.997(2) 2 ?
Co1 Co2 2.3194(4) . ?
Co1 Cl1 2.4380(8) . ?
Co2 N5 1.900(2) 2 ?
Co2 N5 1.900(2) . ?
Co2 N2 1.903(2) . ?
Co2 N2 1.903(2) 2 ?
Co2 Co1 2.3194(4) 2 ?
N1 C1 1.346(4) . ?
N1 C5 1.366(4) . ?
N2 C5 1.362(4) . ?
N2 C6 1.367(4) . ?
N3 C10 1.350(4) . ?
N3 C6 1.366(4) . ?
N3 Co1 1.996(2) 2 ?
N4 C11 1.353(4) . ?
N4 C15 1.358(4) . ?
N5 C15 1.357(4) . ?
N5 C16 1.371(4) . ?
N6 C20 1.355(4) . ?
N6 C16 1.361(4) . ?
N6 Co1 1.983(3) 2 ?
C1 C2 1.370(5) . ?
C2 C3 1.392(5) . ?
C3 C4 1.368(5) . ?
C4 C5 1.407(4) . ?
C6 C7 1.407(4) . ?
C7 C8 1.373(5) . ?
C8 C9 1.392(5) . ?
C9 C10 1.370(5) . ?
C11 C12 1.375(5) . ?
C12 C13 1.379(6) . ?
C13 C14 1.372(5) . ?
C14 C15 1.410(4) . ?
C16 C17 1.414(5) . ?
C17 C18 1.359(5) . ?
C18 C19 1.395(6) . ?
C19 C20 1.372(5) . ?
O1S C1S 1.05(2) . ?
O1S C3S 1.71(3) 2_455 ?
O1S C3S 1.78(3) . ?
O2S C3S 1.29(3) . ?
O2S C1S 1.36(3) . ?
C1S C3S 1.38(3) 2_455 ?
C2S C3S 1.62(3) . ?
C2S C3S 1.62(3) 2_455 ?
C3S C1S 1.38(3) 2_455 ?
C3S O1S 1.71(3) 2_455 ?
