#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:33:46 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179188 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/32/4313294.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_4313294
loop_
_publ_author_name
'Jenny Y. Yang'
'Matthew P. Shores'
'Jennifer J. Sokol'
'Jeffrey R. Long'
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 High-Nuclearity Metal-Cyanide Clusters: Synthesis, Magnetic Properties,
 and Inclusion Behavior of Open-Cage Species Incorporating [(tach)M(CN)3]
 (M = Cr, Fe, Co) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1403
_journal_page_last               1419
_journal_paper_doi               10.1021/ic026065f
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        synthetic
_chemical_formula_structural     '[(C6H15N3)Co(CN)3]'
_chemical_formula_sum            'C9 H15 Co N6'
_chemical_formula_weight         266.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   16.230(11)
_cell_length_b                   9.237(6)
_cell_length_c                   7.609(5)
_cell_measurement_temperature    166(2)
_cell_volume                     1140.7(13)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      166(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans with profile analysis'
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4377
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.712794
_exptl_absorpt_correction_T_min  0.894338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_obs          0.0266
_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)+(0.0309P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0581
_refine_ls_wR_factor_obs         0.0545
_reflns_number_observed          832
_reflns_number_total             1042
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic026065f-2_s2_05.cif
_cod_data_source_block           7
_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^)+(0.0309P)^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^)+(0.0309P)^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_database_code               4313294
#BEGIN Tags that were not found in dictionaries:
_diffrn_measurement_detector     'CCD area detector'
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0167(2) 0.0110(2) 0.0150(2) 0.000 -0.0011(2) 0.000
C1 0.0188(12) 0.0162(12) 0.0153(12) -0.0022(9) -0.0029(10) 0.0045(10)
N1 0.0242(11) 0.0238(11) 0.0258(11) 0.0030(9) -0.0010(9) -0.0026(9)
C2 0.026(2) 0.008(2) 0.027(2) 0.000 0.000(2) 0.000
N2 0.048(2) 0.019(2) 0.033(2) 0.000 -0.016(2) 0.000
N3 0.0253(11) 0.0139(10) 0.0172(10) -0.0010(8) 0.0005(8) 0.0005(8)
N4 0.0169(15) 0.0141(13) 0.0152(14) 0.000 0.0017(11) 0.000
C3 0.0186(13) 0.0217(13) 0.0219(12) -0.0028(10) 0.0016(10) 0.0059(9)
C4 0.0165(13) 0.0246(13) 0.0235(13) 0.0054(11) -0.0005(10) 0.0052(9)
C5 0.017(2) 0.027(2) 0.014(2) 0.000 -0.0038(14) 0.000
C6 0.020(2) 0.031(2) 0.017(2) 0.000 0.0035(14) 0.000
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 0.01825(3) 0.2500 0.19376(5) 0.01420(15) Uani 1 d S .
C1 C -0.05213(14) 0.1042(2) 0.2799(3) 0.0168(5) Uani 1 d . .
N1 N -0.09268(12) 0.0080(2) 0.3230(2) 0.0246(5) Uani 1 d . .
C2 C -0.0451(2) 0.2500 -0.0149(4) 0.0206(8) Uani 1 d S .
N2 N -0.0843(2) 0.2500 -0.1415(4) 0.0334(8) Uani 1 d S .
N3 N 0.09243(11) 0.0978(2) 0.0951(2) 0.0188(4) Uani 1 d . .
H3A H 0.07728(11) 0.0124(2) 0.1418(2) 0.023 Uiso 1 calc R .
H3B H 0.08287(11) 0.0925(2) -0.0212(2) 0.023 Uiso 1 calc R .
N4 N 0.08135(15) 0.2500 0.4190(3) 0.0154(6) Uani 1 d S .
H4A H 0.06588(15) 0.3284 0.4809(3) 0.018 Uiso 0.50 calc PR .
H4B H 0.06588(15) 0.1716 0.4809(3) 0.018 Uiso 0.50 calc PR .
C3 C 0.18259(13) 0.1136(2) 0.1206(3) 0.0207(5) Uani 1 d . .
H3 H 0.20987(13) 0.0299(2) 0.0668(3) 0.025 Uiso 1 calc R .
C4 C 0.20301(14) 0.1147(2) 0.3146(3) 0.0215(5) Uani 1 d . .
H4C H 0.26225(14) 0.1071(2) 0.3287(3) 0.026 Uiso 1 calc R .
H4D H 0.17825(14) 0.0305(2) 0.3696(3) 0.026 Uiso 1 calc R .
C5 C 0.1731(2) 0.2500 0.4085(4) 0.0195(7) Uani 1 d S .
H5 H 0.1953(2) 0.2500 0.5282(4) 0.023 Uiso 1 calc SR .
C6 C 0.2131(2) 0.2500 0.0285(4) 0.0230(8) Uani 1 d S .
H6A H 0.1939(2) 0.2500 -0.0922(4) 0.028 Uiso 1 calc SR .
H6B H 0.2728(2) 0.2500 0.0268(4) 0.028 Uiso 1 calc SR .
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'
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
C1 Co1 C1 91.27(14) 7_565 . ?
C1 Co1 C2 87.83(10) 7_565 . ?
C1 Co1 C2 87.83(10) . . ?
C1 Co1 N4 90.72(9) 7_565 . ?
C1 Co1 N4 90.72(9) . . ?
C2 Co1 N4 177.92(12) . . ?
C1 Co1 N3 178.26(8) 7_565 . ?
C1 Co1 N3 89.61(9) . . ?
C2 Co1 N3 90.71(9) . . ?
N4 Co1 N3 90.77(8) . . ?
C1 Co1 N3 89.61(9) 7_565 7_565 ?
C1 Co1 N3 178.26(8) . 7_565 ?
C2 Co1 N3 90.71(9) . 7_565 ?
N4 Co1 N3 90.77(8) . 7_565 ?
N3 Co1 N3 89.47(11) . 7_565 ?
N1 C1 Co1 174.7(2) . . ?
N2 C2 Co1 179.5(3) . . ?
C3 N3 Co1 118.44(13) . . ?
C5 N4 Co1 117.8(2) . . ?
N3 C3 C4 110.1(2) . . ?
N3 C3 C6 110.0(2) . . ?
C4 C3 C6 111.8(2) . . ?
C3 C4 C5 113.2(2) . . ?
N4 C5 C4 110.2(2) . . ?
N4 C5 C4 110.2(2) . 7_565 ?
C4 C5 C4 110.7(3) . 7_565 ?
C3 C6 C3 111.5(3) . 7_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 C1 1.883(2) 7_565 ?
Co1 C1 1.883(2) . ?
Co1 C2 1.892(4) . ?
Co1 N4 1.996(3) . ?
Co1 N3 1.997(2) . ?
Co1 N3 1.997(2) 7_565 ?
C1 N1 1.154(3) . ?
C2 N2 1.153(4) . ?
N3 C3 1.483(3) . ?
N4 C5 1.490(4) . ?
C3 C4 1.513(3) . ?
C3 C6 1.524(3) . ?
C4 C5 1.520(3) . ?
C5 C4 1.520(3) 7_565 ?
C6 C3 1.524(3) 7_565 ?
