#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:14:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179318 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/15/4321541.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_4321541
loop_
_publ_author_name
'Paul V. Bernhardt'
'Brendan P. Macpherson'
'Manuel Martinez'
_publ_section_title
;
 Discrete Dinuclear Cyano-Bridged Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5203
_journal_page_last               5208
_journal_paper_doi               10.1021/ic000379q
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C11 H27 Cl3 Co N5 O8'
_chemical_formula_weight         522.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.833(3)
_cell_length_b                   13.363(2)
_cell_length_c                   26.015(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     4113.6(13)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        XTAL3.2
_computing_molecular_graphics    PLATON
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.820
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_device_type  CAD4
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5412
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.57
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.8833
_exptl_absorpt_correction_T_min  0.5686
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0726P)²+4.8759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                3659
_reflns_number_total             5412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000379q_1.cif
_cod_data_source_block           bm14039
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+4.8759P] 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^)+(0.0726P)^2^+4.8759P] 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               4321541
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.00379(3) 0.14271(3) 0.095565(14) 0.03003(12) Uani 1 d . . .
N1 N 0.1021(2) 0.2522(2) 0.11660(12) 0.0457(7) Uani 1 d . . .
H1 H 0.1744 0.2356 0.1083 0.055 Uiso 1 calc R . .
N2 N 0.1045(2) 0.0523(2) 0.13191(10) 0.0405(6) Uani 1 d . . .
H2 H 0.1763 0.0646 0.1211 0.049 Uiso 1 calc R . .
N3 N -0.0870(2) 0.0255(2) 0.07855(10) 0.0392(6) Uani 1 d . . .
H3 H -0.0662 0.0082 0.0461 0.047 Uiso 1 calc R . .
N4 N -0.0902(2) 0.2414(2) 0.06051(10) 0.0442(6) Uani 1 d . . .
H4 H -0.0691 0.2390 0.0269 0.053 Uiso 1 calc R . .
N5 N -0.0673(2) 0.1619(2) 0.16291(9) 0.0365(5) Uani 1 d . . .
H5A H -0.1111 0.2169 0.1635 0.044 Uiso 1 calc R . .
H5B H -0.1086 0.1083 0.1722 0.044 Uiso 1 calc R . .
C1 C 0.0952(3) 0.2633(3) 0.17358(15) 0.0557(9) Uani 1 d . . .
H1C H 0.0544 0.3240 0.1822 0.067 Uiso 1 calc R . .
H1D H 0.1706 0.2682 0.1880 0.067 Uiso 1 calc R . .
C2 C 0.0349(3) 0.1737(3) 0.19594(13) 0.0453(8) Uani 1 d . . .
C11 C 0.0072(4) 0.1881(3) 0.25254(15) 0.0640(11) Uani 1 d . . .
H11A H -0.0336 0.2496 0.2570 0.096 Uiso 1 calc R . .
H11B H 0.0760 0.1906 0.2720 0.096 Uiso 1 calc R . .
H11C H -0.0382 0.1332 0.2643 0.096 Uiso 1 calc R . .
C3 C 0.0985(3) 0.0752(3) 0.18809(13) 0.0506(9) Uani 1 d . . .
H3A H 0.1742 0.0806 0.2021 0.061 Uiso 1 calc R . .
H3B H 0.0596 0.0215 0.2059 0.061 Uiso 1 calc R . .
C4 C 0.0753(4) -0.0528(3) 0.11767(15) 0.0527(9) Uani 1 d . . .
H4A H 0.1003 -0.0984 0.1443 0.063 Uiso 1 calc R . .
H4B H 0.1124 -0.0710 0.0858 0.063 Uiso 1 calc R . .
C5 C -0.0499(4) -0.0587(3) 0.11158(14) 0.0542(9) Uani 1 d . . .
H5A H -0.0706 -0.1219 0.0959 0.065 Uiso 1 calc R . .
H5B H -0.0862 -0.0544 0.1449 0.065 Uiso 1 calc R . .
C6 C -0.2119(3) 0.0383(4) 0.07651(16) 0.0577(10) Uani 1 d . . .
H6A H -0.2401 0.0510 0.1109 0.069 Uiso 1 calc R . .
H6B H -0.2461 -0.0232 0.0643 0.069 Uiso 1 calc R . .
C7 C -0.2462(3) 0.1229(4) 0.04192(15) 0.0622(11) Uani 1 d . . .
H7A H -0.3275 0.1205 0.0374 0.075 Uiso 1 calc R . .
H7B H -0.2120 0.1125 0.0085 0.075 Uiso 1 calc R . .
C8 C -0.2146(3) 0.2258(3) 0.06062(15) 0.0577(10) Uani 1 d . . .
H8A H -0.2499 0.2755 0.0387 0.069 Uiso 1 calc R . .
H8B H -0.2431 0.2350 0.0952 0.069 Uiso 1 calc R . .
C9 C -0.0558(4) 0.3422(3) 0.07918(16) 0.0590(10) Uani 1 d . . .
H9A H -0.0932 0.3570 0.1115 0.071 Uiso 1 calc R . .
H9B H -0.0774 0.3928 0.0543 0.071 Uiso 1 calc R . .
C10 C 0.0701(4) 0.3431(3) 0.08653(18) 0.0627(11) Uani 1 d . . .
H10A H 0.1078 0.3426 0.0534 0.075 Uiso 1 calc R . .
H10B H 0.0928 0.4030 0.1049 0.075 Uiso 1 calc R . .
Cl1 Cl 0.10204(7) 0.12026(6) 0.02257(3) 0.0441(2) Uani 1 d . . .
Cl2 Cl -0.28002(9) -0.09046(7) 0.21827(3) 0.0529(2) Uani 1 d . . .
Cl3 Cl 0.08778(7) 0.65711(7) 0.08562(4) 0.0486(2) Uani 1 d . . .
O1 O -0.3001(3) -0.1232(2) 0.26867(12) 0.0731(9) Uani 1 d . . .
O2 O -0.2523(3) -0.1708(2) 0.18461(12) 0.0762(9) Uani 1 d . . .
O3 O -0.3832(4) -0.0481(4) 0.19880(17) 0.1233(18) Uani 1 d . . .
O4 O -0.1999(4) -0.0153(4) 0.21818(17) 0.137(2) Uani 1 d . . .
O5 O 0.0693(5) 0.5885(4) 0.0460(2) 0.142(2) Uani 1 d . . .
O6 O 0.1408(4) 0.7423(3) 0.0631(2) 0.1195(17) Uani 1 d . . .
O7 O 0.1621(3) 0.6173(5) 0.12119(17) 0.138(2) Uani 1 d . . .
O8 O -0.0137(3) 0.6840(4) 0.11058(18) 0.1045(14) Uani 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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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 Co N1 87.96(13) . . ?
N2 Co N3 87.05(12) . . ?
N1 Co N3 174.94(12) . . ?
N2 Co N4 175.90(13) . . ?
N1 Co N4 87.95(13) . . ?
N3 Co N4 97.05(13) . . ?
N2 Co N5 84.81(11) . . ?
N1 Co N5 84.67(12) . . ?
N3 Co N5 94.08(11) . . ?
N4 Co N5 94.86(11) . . ?
N2 Co Cl1 90.63(9) . . ?
N1 Co Cl1 91.65(9) . . ?
N3 Co Cl1 89.20(8) . . ?
N4 Co Cl1 89.44(8) . . ?
N5 Co Cl1 174.23(8) . . ?
C1 N1 C10 115.2(3) . . ?
C1 N1 Co 108.7(2) . . ?
C10 N1 Co 108.2(2) . . ?
C4 N2 C3 115.1(3) . . ?
C4 N2 Co 108.8(2) . . ?
C3 N2 Co 108.6(2) . . ?
C5 N3 C6 113.8(3) . . ?
C5 N3 Co 108.3(2) . . ?
C6 N3 Co 117.5(2) . . ?
C8 N4 C9 113.4(3) . . ?
C8 N4 Co 117.9(2) . . ?
C9 N4 Co 107.6(2) . . ?
C2 N5 Co 100.39(19) . . ?
N1 C1 C2 109.2(3) . . ?
N5 C2 C1 104.2(3) . . ?
N5 C2 C11 113.3(3) . . ?
C1 C2 C11 112.0(3) . . ?
N5 C2 C3 103.3(3) . . ?
C1 C2 C3 113.5(3) . . ?
C11 C2 C3 110.1(3) . . ?
N2 C3 C2 109.3(3) . . ?
N2 C4 C5 107.8(3) . . ?
N3 C5 C4 108.4(3) . . ?
N3 C6 C7 112.1(3) . . ?
C6 C7 C8 115.2(3) . . ?
N4 C8 C7 112.0(3) . . ?
N4 C9 C10 108.7(3) . . ?
N1 C10 C9 108.1(3) . . ?
O4 Cl2 O1 110.2(3) . . ?
O4 Cl2 O2 112.9(2) . . ?
O1 Cl2 O2 112.3(2) . . ?
O4 Cl2 O3 107.3(4) . . ?
O1 Cl2 O3 108.0(3) . . ?
O2 Cl2 O3 106.0(2) . . ?
O7 Cl3 O5 109.9(4) . . ?
O7 Cl3 O8 109.3(3) . . ?
O5 Cl3 O8 111.9(3) . . ?
O7 Cl3 O6 107.6(3) . . ?
O5 Cl3 O6 106.8(3) . . ?
O8 Cl3 O6 111.1(3) . . ?
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
Co N2 1.943(3) . ?
Co N1 1.947(3) . ?
Co N3 1.951(3) . ?
Co N4 1.951(3) . ?
Co N5 1.960(2) . ?
Co Cl1 2.2467(8) . ?
N1 C1 1.492(5) . ?
N1 C10 1.494(5) . ?
N2 C4 1.492(4) . ?
N2 C3 1.495(4) . ?
N3 C5 1.482(5) . ?
N3 C6 1.488(4) . ?
N4 C8 1.486(5) . ?
N4 C9 1.489(5) . ?
N5 C2 1.493(4) . ?
C1 C2 1.510(6) . ?
C2 C11 1.521(5) . ?
C2 C3 1.530(5) . ?
C4 C5 1.492(6) . ?
C6 C7 1.501(6) . ?
C7 C8 1.505(6) . ?
C9 C10 1.502(7) . ?
Cl2 O4 1.381(4) . ?
Cl2 O1 1.403(3) . ?
Cl2 O2 1.424(3) . ?
Cl2 O3 1.438(4) . ?
Cl3 O7 1.383(4) . ?
Cl3 O5 1.397(4) . ?
Cl3 O8 1.411(4) . ?
Cl3 O6 1.426(4) . ?
