#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:33:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179188 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/32/4313298.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_4313298
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)2(C10H24N4)3Cu3Cr2(CN)6](NO3)6
;
_chemical_formula_sum            'C48 H102 Cr2 Cu3 N30 O18'
_chemical_formula_weight         1682.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.8616(2)
_cell_length_b                   15.8616(2)
_cell_length_c                   25.0846(5)
_cell_measurement_temperature    160(2)
_cell_volume                     5465.52(15)
_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      160(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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8116
_diffrn_reflns_theta_max         24.68
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.927928
_exptl_absorpt_correction_T_min  0.554534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             2637
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_obs          0.0302
_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)+(0.0462P)²+11.3783P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0828
_refine_ls_wR_factor_obs         0.0771
_reflns_number_observed          1847
_reflns_number_total             2032
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic026065f-2_s2_09.cif
_cod_data_source_block           18
_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^)+(0.0462P)^2^+11.3783P] 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^)+(0.0462P)^2^+11.3783P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4313298
#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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Cr1 Cr 0.6667 0.3333 0.04255(2) 0.0121(2) Uani 1 d S .
C1 C 0.73555(15) 0.28336(15) 0.09309(8) 0.0176(5) Uani 1 d . .
N1 N 0.77270(14) 0.25864(14) 0.12364(8) 0.0249(4) Uani 1 d . .
N2 N 0.78896(13) 0.40194(13) -0.00581(7) 0.0170(4) Uani 1 d . .
H2A H 0.82105(13) 0.46561(13) 0.00265(7) 0.020 Uiso 1 calc R .
H2B H 0.82824(13) 0.37810(13) 0.00248(7) 0.020 Uiso 1 calc R .
C2 C 0.7741(2) 0.3939(2) -0.06473(8) 0.0202(5) Uani 1 d . .
H2 H 0.8379(2) 0.4298(2) -0.08205(8) 0.024 Uiso 1 calc R .
C3 C 0.7262(2) 0.2871(2) -0.08177(9) 0.0221(5) Uani 1 d . .
H3A H 0.7299(2) 0.2842(2) -0.12027(9) 0.027 Uiso 1 calc R .
H3B H 0.7627(2) 0.2588(2) -0.06665(9) 0.027 Uiso 1 calc R .
Cu1 Cu 0.8333 0.1667 0.1667 0.01614(14) Uani 1 d S .
N3 N 0.94569(13) 0.21988(14) 0.11414(7) 0.0200(4) Uani 1 d . .
H3 H 0.93293(13) 0.25289(14) 0.08870(7) 0.024 Uiso 1 calc R .
N4 N 0.74322(13) 0.05078(13) 0.12039(7) 0.0204(4) Uani 1 d . .
H4 H 0.71662(13) 0.07264(13) 0.09570(7) 0.024 Uiso 1 calc R .
C4 C 0.9625(2) 0.1476(2) 0.08622(9) 0.0245(5) Uani 1 d . .
H4A H 0.9805(2) 0.1138(2) 0.11204(9) 0.029 Uiso 1 calc R .
H4B H 1.0162(2) 0.1809(2) 0.06148(9) 0.029 Uiso 1 calc R .
C5 C 0.8723(2) 0.0734(2) 0.05579(9) 0.0268(5) Uani 1 d . .
H5A H 0.8498(2) 0.1082(2) 0.03350(9) 0.032 Uiso 1 calc R .
H5B H 0.8905(2) 0.0364(2) 0.03245(9) 0.032 Uiso 1 calc R .
C6 C 0.7887(2) 0.0029(2) 0.09099(9) 0.0250(5) Uani 1 d . .
H6A H 0.7397(2) -0.0487(2) 0.06903(9) 0.030 Uiso 1 calc R .
H6B H 0.8126(2) -0.0264(2) 0.11633(9) 0.030 Uiso 1 calc R .
C7 C 1.0331(2) 0.2923(2) 0.14335(10) 0.0260(5) Uani 1 d . .
H7A H 1.0833(2) 0.3346(2) 0.11845(10) 0.031 Uiso 1 calc R .
H7B H 1.0585(2) 0.2596(2) 0.16524(10) 0.031 Uiso 1 calc R .
C8 C 1.0033(2) 0.3511(2) 0.17802(10) 0.0263(5) Uani 1 d . .
H8A H 1.0581(2) 0.3973(2) 0.19931(10) 0.032 Uiso 1 calc R .
H8B H 0.9817(2) 0.3869(2) 0.15599(10) 0.032 Uiso 1 calc R .
N5 N 0.62460(13) 0.62251(13) -0.00178(8) 0.0220(4) Uani 1 d . .
O1 O 0.61780(13) 0.69128(13) 0.01759(8) 0.0388(5) Uani 1 d . .
O2 O 0.57619(12) 0.57873(13) -0.04208(7) 0.0329(4) Uani 1 d . .
O3 O 0.68160(13) 0.59850(13) 0.01869(8) 0.0354(4) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cr1 C1 86.48(8) . 3_665 ?
C1 Cr1 C1 86.48(8) . 2_655 ?
C1 Cr1 C1 86.48(8) 3_665 2_655 ?
C1 Cr1 N2 91.43(7) . . ?
C1 Cr1 N2 177.82(7) 3_665 . ?
C1 Cr1 N2 92.78(7) 2_655 . ?
C1 Cr1 N2 92.78(7) . 3_665 ?
C1 Cr1 N2 91.43(7) 3_665 3_665 ?
C1 Cr1 N2 177.82(7) 2_655 3_665 ?
N2 Cr1 N2 89.28(7) . 3_665 ?
C1 Cr1 N2 177.83(7) . 2_655 ?
C1 Cr1 N2 92.78(7) 3_665 2_655 ?
C1 Cr1 N2 91.43(7) 2_655 2_655 ?
N2 Cr1 N2 89.28(7) . 2_655 ?
N2 Cr1 N2 89.28(7) 3_665 2_655 ?
N1 C1 Cr1 175.7(2) . . ?
C1 N1 Cu1 161.6(2) . . ?
C2 N2 Cr1 117.88(13) . . ?
N2 C2 C3 110.3(2) . 2_655 ?
N2 C2 C3 109.9(2) . . ?
C3 C2 C3 111.2(2) 2_655 . ?
C2 C3 C2 113.8(2) 3_665 . ?
N3 Cu1 N3 180.0 13_655 . ?
N3 Cu1 N4 94.55(7) 13_655 13_655 ?
N3 Cu1 N4 85.45(7) . 13_655 ?
N3 Cu1 N4 85.45(7) 13_655 . ?
N3 Cu1 N4 94.55(7) . . ?
N4 Cu1 N4 180.0 13_655 . ?
N3 Cu1 N1 90.54(7) 13_655 . ?
N3 Cu1 N1 89.46(7) . . ?
N4 Cu1 N1 91.24(7) 13_655 . ?
N4 Cu1 N1 88.76(7) . . ?
N3 Cu1 N1 89.46(7) 13_655 13_655 ?
N3 Cu1 N1 90.54(7) . 13_655 ?
N4 Cu1 N1 88.75(7) 13_655 13_655 ?
N4 Cu1 N1 91.25(7) . 13_655 ?
N1 Cu1 N1 180.0 . 13_655 ?
C4 N3 C7 112.0(2) . . ?
C4 N3 Cu1 116.52(14) . . ?
C7 N3 Cu1 106.78(13) . . ?
C8 N4 C6 112.1(2) 13_655 . ?
C8 N4 Cu1 106.46(13) 13_655 . ?
C6 N4 Cu1 116.46(14) . . ?
N3 C4 C5 111.8(2) . . ?
C6 C5 C4 114.4(2) . . ?
N4 C6 C5 112.5(2) . . ?
N3 C7 C8 107.6(2) . . ?
N4 C8 C7 107.7(2) 13_655 . ?
O1 N5 O2 120.2(2) . . ?
O1 N5 O3 119.8(2) . . ?
O2 N5 O3 119.9(2) . . ?
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
Cr1 C1 2.072(2) . ?
Cr1 C1 2.073(2) 3_665 ?
Cr1 C1 2.073(2) 2_655 ?
Cr1 N2 2.076(2) . ?
Cr1 N2 2.076(2) 3_665 ?
Cr1 N2 2.076(2) 2_655 ?
C1 N1 1.149(3) . ?
N1 Cu1 2.371(2) . ?
N2 C2 1.492(3) . ?
C2 C3 1.528(3) 2_655 ?
C2 C3 1.530(3) . ?
C3 C2 1.528(3) 3_665 ?
Cu1 N3 2.030(2) 13_655 ?
Cu1 N3 2.030(2) . ?
Cu1 N4 2.035(2) 13_655 ?
Cu1 N4 2.035(2) . ?
Cu1 N1 2.371(2) 13_655 ?
N3 C4 1.478(3) . ?
N3 C7 1.478(3) . ?
N4 C8 1.476(3) 13_655 ?
N4 C6 1.479(3) . ?
C4 C5 1.526(3) . ?
C5 C6 1.519(3) . ?
C7 C8 1.514(3) . ?
C8 N4 1.476(3) 13_655 ?
N5 O1 1.247(3) . ?
N5 O2 1.249(3) . ?
N5 O3 1.253(2) . ?
