#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:01:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179274 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319412.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_4319412
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_structural     Co3(dpa)4Cl2.C6H12
_chemical_formula_sum            'C46 H44 Cl2 Co3 N12'
_chemical_formula_weight         1012.62
_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                   12.9685(8)
_cell_length_b                   14.2468(9)
_cell_length_c                   23.7039(14)
_cell_measurement_reflns_used    5977
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.506
_cell_measurement_theta_min      2.236
_cell_volume                     4379.5(5)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26390
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_T_max  0.7244
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.206
_refine_ls_goodness_of_fit_obs   1.273
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5020
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.206
_refine_ls_restrained_S_obs      1.273
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_obs          0.0545
_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)+(0.0489P)²+13.9878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1536
_refine_ls_wR_factor_obs         0.1493
_reflns_number_observed          4291
_reflns_number_total             5020
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001068i_15.cif
_cod_data_source_block           s1.C6H12at213K
_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^)+(0.0489P)^2^+13.9878P] 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^)+(0.0489P)^2^+13.9878P] 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               4319412
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 -0.09161(4) 0.82728(4) 0.14833(2) 0.0261(2) Uani 1 d . .
Co2 Co -0.2500 0.7500 0.15043(3) 0.0224(2) Uani 1 d S .
Cl1 Cl 0.07470(8) 0.90654(8) 0.14454(4) 0.0364(2) Uani 1 d . .
N1 N -0.0802(3) 0.7803(2) 0.22773(13) 0.0278(7) Uani 1 d . .
N2 N -0.2989(3) 0.8334(2) 0.20715(13) 0.0264(6) Uani 1 d . .
N3 N -0.1698(3) 0.9357(2) 0.18023(13) 0.0282(7) Uani 1 d . .
N4 N -0.1325(3) 0.8637(2) 0.06941(13) 0.0281(7) Uani 1 d . .
N5 N -0.3009(3) 0.8329(2) 0.09401(13) 0.0275(7) Uani 1 d . .
N6 N -0.0346(3) 0.7050(2) 0.12220(14) 0.0301(7) Uani 1 d . .
C1 C -0.1358(3) 0.7046(3) 0.2463(2) 0.0284(8) Uani 1 d . .
C2 C -0.1313(4) 0.6782(3) 0.3036(2) 0.0384(10) Uani 1 d . .
H2A H -0.1691(4) 0.6261(3) 0.3165(2) 0.046 Uiso 1 calc R .
C3 C -0.0717(4) 0.7287(3) 0.3404(2) 0.0475(12) Uani 1 d . .
H3A H -0.0677(4) 0.7108(3) 0.3785(2) 0.057 Uiso 1 calc R .
C4 C -0.0169(4) 0.8065(3) 0.3214(2) 0.0460(11) Uani 1 d . .
H4A H 0.0239(4) 0.8421(3) 0.3462(2) 0.055 Uiso 1 calc R .
C5 C -0.0244(3) 0.8298(3) 0.2652(2) 0.0359(9) Uani 1 d . .
H5A H 0.0113(3) 0.8831(3) 0.2523(2) 0.043 Uiso 1 calc R .
C6 C -0.2595(3) 0.9225(3) 0.2093(2) 0.0273(7) Uani 1 d . .
C7 C -0.3067(4) 0.9983(3) 0.2369(2) 0.0395(10) Uani 1 d . .
H7A H -0.3692(4) 0.9893(3) 0.2563(2) 0.047 Uiso 1 calc R .
C8 C -0.2621(4) 1.0852(3) 0.2358(2) 0.0490(12) Uani 1 d . .
H8A H -0.2926(4) 1.1354(3) 0.2553(2) 0.059 Uiso 1 calc R .
C9 C -0.1717(4) 1.0990(3) 0.2056(2) 0.0492(12) Uani 1 d . .
H9A H -0.1399(4) 1.1583(3) 0.2042(2) 0.059 Uiso 1 calc R .
C10 C -0.1303(4) 1.0234(3) 0.1780(2) 0.0385(10) Uani 1 d . .
H10A H -0.0708(4) 1.0332(3) 0.1561(2) 0.046 Uiso 1 calc R .
C11 C -0.0613(3) 0.8853(3) 0.0302(2) 0.0348(9) Uani 1 d . .
H11A H 0.0087(3) 0.8817(3) 0.0403(2) 0.042 Uiso 1 calc R .
C12 C -0.0860(4) 0.9123(3) -0.0240(2) 0.0435(11) Uani 1 d . .
H12A H -0.0341(4) 0.9289(3) -0.0498(2) 0.052 Uiso 1 calc R .
C13 C -0.1882(4) 0.9147(4) -0.0396(2) 0.0466(11) Uani 1 d . .
H13A H -0.2070(4) 0.9333(4) -0.0762(2) 0.056 Uiso 1 calc R .
C14 C -0.2628(4) 0.8895(3) -0.0012(2) 0.0417(10) Uani 1 d . .
H14A H -0.3327(4) 0.8889(3) -0.0117(2) 0.050 Uiso 1 calc R .
C15 C -0.2334(3) 0.8648(3) 0.0541(2) 0.0296(8) Uani 1 d . .
C16 C -0.0978(3) 0.6422(3) 0.0963(2) 0.0297(8) Uani 1 d . .
C17 C -0.0576(4) 0.5543(3) 0.0791(2) 0.0425(10) Uani 1 d . .
H17A H -0.0997(4) 0.5115(3) 0.0597(2) 0.051 Uiso 1 calc R .
C18 C 0.0424(4) 0.5320(4) 0.0909(2) 0.0535(13) Uani 1 d . .
H18A H 0.0689(4) 0.4735(4) 0.0798(2) 0.064 Uiso 1 calc R .
C19 C 0.1056(4) 0.5955(4) 0.1192(2) 0.0523(13) Uani 1 d . .
H19A H 0.1743(4) 0.5804(4) 0.1280(2) 0.063 Uiso 1 calc R .
C20 C 0.0642(3) 0.6803(3) 0.1336(2) 0.0404(10) Uani 1 d . .
H20A H 0.1065(3) 0.7239(3) 0.1525(2) 0.049 Uiso 1 calc R .
C1S C 0.2270(25) 0.8270(19) 0.4250(9) 0.185(12) Uiso 0.50 d PD .
C2S C 0.1575(20) 0.7299(14) 0.4229(10) 0.162(10) Uiso 0.50 d PD .
C3S C 0.2181(12) 0.6486(12) 0.4596(8) 0.097(5) Uiso 0.50 d PD .
C4S C 0.3377(12) 0.6873(14) 0.4660(9) 0.108(6) Uiso 0.50 d PD .
C5S C 0.3108(18) 0.7701(15) 0.5124(11) 0.188(12) Uiso 0.50 d PD .
C6S C 0.2173(17) 0.8424(14) 0.4937(8) 0.113(6) Uiso 0.50 d PD .
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'
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
Co1 Co2 Co1 177.56(4) 2_465 . y
Co2 Co1 Cl1 178.95(4) . . y
N1 Co1 N3 86.60(13) . . y
N1 Co1 N4 168.26(14) . . y
N1 Co1 N6 88.41(13) . . y
N3 Co1 N4 91.09(13) . . y
N3 Co1 N6 169.51(14) . . y
N4 Co1 N6 91.94(13) . . y
N2 Co2 N2 90.1(2) . 2_465 y
N5 Co2 N2 89.63(14) . . y
N5 Co2 N2 179.14(14) 2_465 . y
N5 Co2 N5 90.7(2) . 2_465 y
N1 Co1 Cl1 97.13(10) . . y
N3 Co1 Cl1 96.02(10) . . y
N4 Co1 Cl1 94.55(10) . . y
N6 Co1 Cl1 93.76(10) . . y
N5 Co2 N2 179.14(14) . 2_465 ?
N5 Co2 N2 89.63(14) 2_465 2_465 ?
N6 Co1 Co2 85.44(10) . . ?
N3 Co1 Co2 84.83(10) . . ?
N1 Co1 Co2 83.53(10) . . ?
N4 Co1 Co2 84.80(10) . . ?
N5 Co2 Co1 88.42(10) . 2_465 ?
N5 Co2 Co1 89.87(10) 2_465 2_465 ?
N2 Co2 Co1 90.94(10) . 2_465 ?
N2 Co2 Co1 90.78(10) 2_465 2_465 ?
N5 Co2 Co1 89.87(10) . . ?
N5 Co2 Co1 88.42(10) 2_465 . ?
N2 Co2 Co1 90.78(10) . . ?
N2 Co2 Co1 90.95(10) 2_465 . ?
C5 N1 C1 118.9(3) . . ?
C5 N1 Co1 119.0(3) . . ?
C1 N1 Co1 121.8(3) . . ?
C1 N2 C6 124.9(3) 2_465 . ?
C1 N2 Co2 116.0(3) 2_465 . ?
C6 N2 Co2 118.7(2) . . ?
C10 N3 C6 118.1(3) . . ?
C10 N3 Co1 120.5(3) . . ?
C6 N3 Co1 121.1(3) . . ?
C11 N4 C15 118.3(3) . . ?
C11 N4 Co1 121.3(3) . . ?
C15 N4 Co1 120.3(3) . . ?
C16 N5 C15 124.0(3) 2_465 . ?
C16 N5 Co2 118.0(3) 2_465 . ?
C15 N5 Co2 118.1(3) . . ?
C20 N6 C16 119.2(4) . . ?
C20 N6 Co1 121.0(3) . . ?
C16 N6 Co1 119.5(3) . . ?
N2 C1 N1 114.8(3) 2_465 . ?
N2 C1 C2 124.9(4) 2_465 . ?
N1 C1 C2 119.9(4) . . ?
C3 C2 C1 119.7(4) . . ?
C2 C3 C4 120.0(4) . . ?
C5 C4 C3 118.0(4) . . ?
N1 C5 C4 123.4(4) . . ?
N3 C6 N2 115.3(3) . . ?
N3 C6 C7 120.1(4) . . ?
N2 C6 C7 124.6(4) . . ?
C8 C7 C6 120.2(4) . . ?
C7 C8 C9 119.8(4) . . ?
C10 C9 C8 117.7(4) . . ?
N3 C10 C9 124.0(4) . . ?
N4 C11 C12 123.2(4) . . ?
C13 C12 C11 118.7(4) . . ?
C14 C13 C12 119.6(4) . . ?
C13 C14 C15 119.3(4) . . ?
N4 C15 N5 115.4(3) . . ?
N4 C15 C14 120.8(4) . . ?
N5 C15 C14 123.5(4) . . ?
N6 C16 N5 115.3(3) . 2_465 ?
N6 C16 C17 119.3(4) . . ?
N5 C16 C17 125.1(4) 2_465 . ?
C18 C17 C16 119.8(4) . . ?
C17 C18 C19 120.4(5) . . ?
C20 C19 C18 117.7(4) . . ?
N6 C20 C19 123.4(4) . . ?
C3S C1S C4S 85.0(13) 2_565 2_565 ?
C3S C1S C6S 45.3(11) 2_565 . ?
C4S C1S C6S 39.9(10) 2_565 . ?
C3S C1S C2S 128.2(21) 2_565 . ?
C4S C1S C2S 62.5(16) 2_565 . ?
C6S C1S C2S 95.7(14) . . ?
C3S C1S C2S 67.5(19) 2_565 2_565 ?
C4S C1S C2S 120.9(22) 2_565 2_565 ?
C6S C1S C2S 99.1(18) . 2_565 ?
C2S C1S C2S 94.6(23) . 2_565 ?
C4S C2S C3S 99.6(15) 2_565 . ?
C4S C2S C1S 47.6(11) 2_565 . ?
C3S C2S C1S 108.2(17) . . ?
C4S C2S C1S 107.8(18) 2_565 2_565 ?
C3S C2S C1S 39.7(9) . 2_565 ?
C1S C2S C1S 85.3(23) . 2_565 ?
C1S C3S C6S 90.9(14) 2_565 2_565 ?
C1S C3S C2S 72.8(21) 2_565 . ?
C6S C3S C2S 128.9(16) 2_565 . ?
C1S C3S C4S 51.6(14) 2_565 . ?
C6S C3S C4S 39.6(11) 2_565 . ?
C2S C3S C4S 105.1(15) . . ?
C1S C3S C5S 116.5(21) 2_565 2_565 ?
C6S C3S C5S 65.5(12) 2_565 2_565 ?
C2S C3S C5S 79.0(13) . 2_565 ?
C4S C3S C5S 85.0(13) . 2_565 ?
C6S C4S C1S 88.1(14) 2_565 2_565 ?
C6S C4S C2S 137.3(20) 2_565 2_565 ?
C1S C4S C2S 69.8(12) 2_565 2_565 ?
C6S C4S C5S 74.3(19) 2_565 . ?
C1S C4S C5S 118.3(20) 2_565 . ?
C2S C4S C5S 84.5(16) 2_565 . ?
C6S C4S C3S 44.9(12) 2_565 . ?
C1S C4S C3S 43.4(12) 2_565 . ?
C2S C4S C3S 103.3(14) 2_565 . ?
C5S C4S C3S 95.8(13) . . ?
C4S C5S C6S 115.0(15) . . ?
C4S C5S C5S 87.4(15) . 2_565 ?
C6S C5S C5S 61.5(14) . 2_565 ?
C4S C5S C6S 36.8(9) . 2_565 ?
C6S C5S C6S 111.1(17) . 2_565 ?
C5S C5S C6S 58.5(13) 2_565 2_565 ?
C4S C5S C3S 92.4(15) . 2_565 ?
C6S C5S C3S 40.3(9) . 2_565 ?
C5S C5S C3S 91.4(12) 2_565 2_565 ?
C6S C5S C3S 113.1(15) 2_565 2_565 ?
C4S C6S C3S 95.6(16) 2_565 2_565 ?
C4S C6S C1S 52.0(14) 2_565 . ?
C3S C6S C1S 43.8(13) 2_565 . ?
C4S C6S C5S 114.4(19) 2_565 . ?
C3S C6S C5S 74.3(18) 2_565 . ?
C1S C6S C5S 97.2(18) . . ?
C4S C6S C5S 69.0(15) 2_565 2_565 ?
C3S C6S C5S 115.9(21) 2_565 2_565 ?
C1S C6S C5S 98.5(16) . 2_565 ?
C5S C6S C5S 60.0(19) . 2_565 ?
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 Co2 2.3311(5) . y
Co2 Co1 2.3311(5) 2_465 y
Co1 Cl1 2.4362(11) . y
Co1 N1 2.003(3) . y
Co1 N3 1.997(3) . y
Co1 N4 2.012(3) . y
Co1 N6 1.990(3) . y
Co2 N2 1.903(3) . y
Co2 N5 1.902(3) . y
Co2 N5 1.902(3) 2_465 ?
Co2 N2 1.903(3) 2_465 ?
N1 C5 1.345(5) . ?
N1 C1 1.369(5) . ?
N2 C1 1.369(5) 2_465 ?
N2 C6 1.370(5) . ?
N3 C10 1.351(5) . ?
N3 C6 1.364(5) . ?
N4 C11 1.345(5) . ?
N4 C15 1.358(5) . ?
N5 C16 1.362(5) 2_465 ?
N5 C15 1.367(5) . ?
N6 C20 1.357(5) . ?
N6 C16 1.360(5) . ?
C1 N2 1.369(5) 2_465 ?
C1 C2 1.411(6) . ?
C2 C3 1.370(6) . ?
C3 C4 1.391(7) . ?
C4 C5 1.377(6) . ?
C6 C7 1.404(5) . ?
C7 C8 1.366(6) . ?
C8 C9 1.388(7) . ?
C9 C10 1.370(6) . ?
C11 C12 1.380(6) . ?
C12 C13 1.376(7) . ?
C13 C14 1.376(6) . ?
C14 C15 1.410(5) . ?
C16 N5 1.362(5) 2_465 ?
C16 C17 1.416(6) . ?
C17 C18 1.364(7) . ?
C18 C19 1.392(7) . ?
C19 C20 1.366(7) . ?
C1S C3S 1.14(3) 2_565 ?
C1S C4S 1.30(3) 2_565 ?
C1S C6S 1.649(11) . ?
C1S C2S 1.652(12) . ?
C1S C2S 1.70(4) 2_565 ?
C2S C4S 1.56(3) 2_565 ?
C2S C3S 1.648(12) . ?
C2S C1S 1.70(4) 2_565 ?
C3S C1S 1.14(3) 2_565 ?
C3S C6S 1.17(2) 2_565 ?
C3S C4S 1.654(11) . ?
C3S C5S 1.75(3) 2_565 ?
C4S C6S 1.06(2) 2_565 ?
C4S C1S 1.30(3) 2_565 ?
C4S C2S 1.56(3) 2_565 ?
C4S C5S 1.650(11) . ?
C5S C6S 1.651(12) . ?
C5S C5S 1.68(5) 2_565 ?
C5S C6S 1.70(3) 2_565 ?
C5S C3S 1.75(3) 2_565 ?
C6S C4S 1.06(2) 2_565 ?
C6S C3S 1.17(2) 2_565 ?
C6S C5S 1.70(3) 2_565 ?
