#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:33:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179188 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/32/4313296.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_4313296
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)4(H2O)12Ni4Co4(CN)12]Br8-22(H2O)
;
_chemical_formula_sum            'C36 H128 Br8 Co4 N24 Ni4 O34'
_chemical_formula_weight         2551.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           111
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      111
_symmetry_space_group_name_Hall  'P -4 2'
_symmetry_space_group_name_H-M   'P -4 2 m'
_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            1
_cell_length_a                   13.9193(4)
_cell_length_b                   13.9193(4)
_cell_length_c                   12.8152(4)
_cell_measurement_temperature    159(2)
_cell_volume                     2482.91(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      159(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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11067
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    4.688
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.464338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.140
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0460
_refine_ls_shift/esd_max         0.041
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0692P)²+7.0831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1371
_refine_ls_wR_factor_obs         0.1330
_reflns_number_observed          2021
_reflns_number_total             2235
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic026065f-2_s2_07.cif
_cod_data_source_block           8-4H2O
_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^)+(0.0692P)^2^+7.0831P] 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^)+(0.0692P)^2^+7.0831P] 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               4313296
#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, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, 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 0.31051(6) 0.68949(6) 0.69592(11) 0.0173(3) Uani 1 d S .
C1 C 0.3162(4) 0.6838(4) 0.5480(9) 0.018(2) Uani 1 d S .
N1 N 0.3176(4) 0.6824(4) 0.4600(8) 0.024(2) Uani 1 d S .
C2 C 0.4464(5) 0.6855(5) 0.6984(6) 0.0199(15) Uani 1 d . .
N2 N 0.5290(4) 0.6818(4) 0.6983(5) 0.0215(13) Uani 1 d . .
N3 N 0.3135(4) 0.8328(4) 0.6896(5) 0.0234(13) Uani 1 d . .
H3A H 0.3730(4) 0.8520(4) 0.7072(5) 0.028 Uiso 1 calc R .
H3B H 0.3039(4) 0.8502(4) 0.6227(5) 0.028 Uiso 1 calc R .
N4 N 0.3052(4) 0.6948(4) 0.8507(7) 0.021(2) Uani 1 d S .
H4A H 0.2910(4) 0.6354(4) 0.8739(7) 0.025 Uiso 0.50 calc PR .
H4B H 0.3646(4) 0.7090(4) 0.8739(7) 0.025 Uiso 0.50 calc PR .
C4 C 0.2432(6) 0.8876(5) 0.7560(6) 0.029(2) Uani 1 d . .
H4 H 0.2524(6) 0.9565(5) 0.7437(6) 0.034 Uiso 1 calc R .
C5 C 0.2602(6) 0.8669(5) 0.8712(5) 0.026(2) Uani 1 d . .
H5A H 0.3272(6) 0.8787(5) 0.8874(5) 0.032 Uiso 1 calc R .
H5B H 0.2219(6) 0.9110(5) 0.9126(5) 0.032 Uiso 1 calc R .
C6 C 0.2352(5) 0.7648(5) 0.9018(9) 0.030(3) Uani 1 d S .
H6 H 0.2412(5) 0.7588(5) 0.9778(9) 0.036 Uiso 1 calc SR .
C7 C 0.1395(5) 0.8605(5) 0.7256(8) 0.027(2) Uiso 1 d S .
H7A H 0.0954(5) 0.9046(5) 0.7594(8) 0.032 Uiso 1 calc SR .
H7B H 0.1319(5) 0.8681(5) 0.6508(8) 0.032 Uiso 1 calc SR .
Ni1 Ni 0.32593(6) 0.67407(6) 0.30188(10) 0.0182(3) Uani 1 d S .
O1 O 0.1741(3) 0.6787(4) 0.2900(4) 0.0287(12) Uani 1 d . .
O2 O 0.3263(4) 0.6737(4) 0.1395(6) 0.035(2) Uani 1 d S .
Br1 Br 0.5000 0.77134(9) 0.0000 0.0398(3) Uani 1 d S .
Br2 Br 0.12732(8) 0.87268(8) 0.15395(12) 0.0287(5) Uani 0.683(4) d SP .
Br2A Br 0.2754(3) 1.0000 0.5000 0.052(2) Uani 0.317(4) d SP .
O3 O 0.2532(11) 1.0896(11) 0.5280(11) 0.041(4) Uiso 0.410(2) d P .
O3A O 0.3375(18) 1.0846(17) 0.5230(18) 0.049(6) Uiso 0.273(2) d P .
O4 O 0.0954(5) 0.5073(5) 0.2160(5) 0.050(2) Uani 1 d . .
O5 O 0.0741(5) 0.9259(5) 0.3955(7) 0.049(2) Uani 1 d S .
O6 O 0.5000 0.5000 0.1185(26) 0.088(10) Uiso 0.50 d SP .
O7 O 0.5000 1.1450(21) 0.5000 0.093(7) Uiso 0.50 d SP .
O8 O 0.0000 0.5000 0.2466(24) 0.042(7) Uiso 0.25 d SP .
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C2 Co1 C2 86.6(4) . 7_665 ?
C2 Co1 C1 88.5(3) . . ?
C2 Co1 C1 88.5(3) 7_665 . ?
C2 Co1 N4 91.2(3) . . ?
C2 Co1 N4 91.2(3) 7_665 . ?
C1 Co1 N4 179.6(3) . . ?
C2 Co1 N3 90.5(3) . . ?
C2 Co1 N3 176.8(3) 7_665 . ?
C1 Co1 N3 90.0(3) . . ?
N4 Co1 N3 90.3(2) . . ?
C2 Co1 N3 176.8(3) . 7_665 ?
C2 Co1 N3 90.5(3) 7_665 7_665 ?
C1 Co1 N3 90.0(3) . 7_665 ?
N4 Co1 N3 90.3(2) . 7_665 ?
N3 Co1 N3 92.3(3) . 7_665 ?
N1 C1 Co1 178.1(9) . . ?
C1 N1 Ni1 176.9(9) . . ?
N2 C2 Co1 178.6(7) . . ?
C2 N2 Ni1 179.5(6) . 3_566 ?
C4 N3 Co1 118.1(5) . . ?
C6 N4 Co1 118.4(6) . . ?
N3 C4 C5 110.6(6) . . ?
N3 C4 C7 109.9(6) . . ?
C5 C4 C7 110.1(7) . . ?
C6 C5 C4 113.2(7) . . ?
C5 C6 C5 111.4(9) 7_665 . ?
C5 C6 N4 109.9(5) 7_665 . ?
C5 C6 N4 109.9(5) . . ?
C4 C7 C4 113.2(8) 7_665 . ?
N2 Ni1 N2 96.1(3) 5_656 4_656 ?
N2 Ni1 N1 93.1(2) 5_656 . ?
N2 Ni1 N1 93.1(2) 4_656 . ?
N2 Ni1 O2 89.8(2) 5_656 . ?
N2 Ni1 O2 89.8(2) 4_656 . ?
N1 Ni1 O2 175.6(3) . . ?
N2 Ni1 O1 88.7(2) 5_656 7_665 ?
N2 Ni1 O1 173.7(2) 4_656 7_665 ?
N1 Ni1 O1 90.8(2) . 7_665 ?
O2 Ni1 O1 86.0(2) . 7_665 ?
N2 Ni1 O1 173.7(2) 5_656 . ?
N2 Ni1 O1 88.7(2) 4_656 . ?
N1 Ni1 O1 90.8(2) . . ?
O2 Ni1 O1 86.0(2) . . ?
O1 Ni1 O1 86.3(3) 7_665 . ?
O3 Br2A O3 153.2(14) 6_576 . ?
O3 Br2A O3A 157.9(12) 6_576 . ?
O3 Br2A O3A 48.9(10) . . ?
O3 Br2A O3A 48.9(10) 6_576 6_576 ?
O3 Br2A O3A 157.8(13) . 6_576 ?
O3A Br2A O3A 109.1(18) . 6_576 ?
O3A O3 Br2A 72.5(14) . . ?
O3 O3A Br2A 58.6(13) . . ?
O4 O8 O4 147.2(24) . 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 C2 1.893(7) . ?
Co1 C2 1.893(7) 7_665 ?
Co1 C1 1.899(11) . ?
Co1 N4 1.986(9) . ?
Co1 N3 1.996(6) . ?
Co1 N3 1.996(6) 7_665 ?
C1 N1 1.129(12) . ?
N1 Ni1 2.033(10) . ?
C2 N2 1.151(8) . ?
N2 Ni1 2.022(6) 3_566 ?
N3 C4 1.505(9) . ?
N4 C6 1.527(12) . ?
C4 C5 1.523(10) . ?
C4 C7 1.543(10) . ?
C5 C6 1.515(10) . ?
C6 C5 1.515(10) 7_665 ?
C7 C4 1.543(10) 7_665 ?
Ni1 N2 2.022(6) 5_656 ?
Ni1 N2 2.022(6) 4_656 ?
Ni1 O2 2.081(7) . ?
Ni1 O1 2.120(5) 7_665 ?
Ni1 O1 2.120(5) . ?
Br2A O3 1.33(2) 6_576 ?
Br2A O3 1.33(2) . ?
Br2A O3A 1.49(2) . ?
Br2A O3A 1.49(2) 6_576 ?
O3 O3A 1.18(3) . ?
O4 O8 1.388(10) . ?
O8 O4 1.388(10) 2_565 ?
