#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:00:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179166 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/27/4312768.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_4312768
loop_
_publ_author_name
'Bangbo Yan'
'Huajun Zhou'
'Abdessadek Lachgar'
_publ_contact_author_address
;
    Department of Chemistry, 
    Wake Forest University, 
    Winston-Salem, NC 27109
;
_publ_contact_author_email       lachgar@wfu.edu
_publ_contact_author_fax         '(336) 758-4656'
_publ_contact_author_name        'Abdessadek Lachgar'
_publ_contact_author_phone       '(336) 758-4676'
_publ_section_title
;
 Octahedral Niobium Chloride Clusters as Building Blocks of Templated
 Prussian Blue Framework Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8818
_journal_page_last               8822
_journal_paper_doi               10.1021/ic034514l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C14 H24 Cl12 Mn N8 Nb6'
_chemical_formula_weight         1342.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_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            4
_cell_length_a                   15.513(4)
_cell_length_b                   15.513(4)
_cell_length_c                   15.513(4)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7.91
_cell_measurement_theta_min      2.27
_cell_volume                     3733.3(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω scans'
_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  0.1305
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1168
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         2.27
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.986
_exptl_absorpt_correction_T_max  0.8635
_exptl_absorpt_correction_T_min  0.7771
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.008
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0218P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                155
_reflns_number_total             212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034514lsi20030514_053953_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3733.2(16)
_cod_database_code               4312768
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.13396(13) 0.5000 0.0000 0.0150(5) Uani 1 8 d S . .
Mn2 Mn 0.5000 0.5000 0.0000 0.0117(18) Uani 1 48 d S . .
Cl3 Cl 0.15736(15) 0.5000 -0.15736(15) 0.0220(10) Uani 1 4 d S . .
C1 C 0.2804(15) 0.5000 0.0000 0.033(7) Uani 1 8 d S . .
N1 N 0.3553(14) 0.5000 0.0000 0.038(5) Uani 1 8 d S . .
C2 C 0.1958(6) 0.1958(6) 0.1958(6) 0.034(5) Uani 1 6 d S . .
H1 H 0.1519 0.2110 0.1519 0.041 Uiso 1 2 d SR . .
N2 N 0.2500 0.2500 0.2500 0.031(9) Uani 1 24 d S . .
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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 Nb1 Cl3 81.54(6) . 126_554 ?
C1 Nb1 Cl3 81.54(6) . 98 ?
Cl3 Nb1 Cl3 88.761(18) 126_554 98 ?
C1 Nb1 Cl3 81.54(6) . . ?
Cl3 Nb1 Cl3 88.761(18) 126_554 . ?
Cl3 Nb1 Cl3 163.09(13) 98 . ?
C1 Nb1 Cl3 81.54(6) . 125 ?
Cl3 Nb1 Cl3 163.09(13) 126_554 125 ?
Cl3 Nb1 Cl3 88.761(18) 98 125 ?
Cl3 Nb1 Cl3 88.761(18) . 125 ?
C1 Nb1 Nb1 135.0 . 125 ?
Cl3 Nb1 Nb1 143.46(6) 126_554 125 ?
Cl3 Nb1 Nb1 95.97(4) 98 125 ?
Cl3 Nb1 Nb1 95.97(4) . 125 ?
Cl3 Nb1 Nb1 53.46(6) 125 125 ?
C1 Nb1 Nb1 135.0 . 177 ?
Cl3 Nb1 Nb1 95.97(4) 126_554 177 ?
Cl3 Nb1 Nb1 143.46(6) 98 177 ?
Cl3 Nb1 Nb1 53.46(6) . 177 ?
Cl3 Nb1 Nb1 95.97(4) 125 177 ?
Nb1 Nb1 Nb1 60.0 125 177 ?
C1 Nb1 Nb1 135.0 . 29_554 ?
Cl3 Nb1 Nb1 53.46(6) 126_554 29_554 ?
Cl3 Nb1 Nb1 95.97(4) 98 29_554 ?
Cl3 Nb1 Nb1 95.97(4) . 29_554 ?
Cl3 Nb1 Nb1 143.46(6) 125 29_554 ?
Nb1 Nb1 Nb1 90.0 125 29_554 ?
Nb1 Nb1 Nb1 60.0 177 29_554 ?
C1 Nb1 Nb1 135.0 . 81_455 ?
Cl3 Nb1 Nb1 95.97(4) 126_554 81_455 ?
Cl3 Nb1 Nb1 53.46(6) 98 81_455 ?
Cl3 Nb1 Nb1 143.46(6) . 81_455 ?
Cl3 Nb1 Nb1 95.97(4) 125 81_455 ?
Nb1 Nb1 Nb1 60.0 125 81_455 ?
Nb1 Nb1 Nb1 90.0 177 81_455 ?
Nb1 Nb1 Nb1 60.0 29_554 81_455 ?
N1 Mn2 N1 90.0 33_554 149_565 ?
N1 Mn2 N1 180.000(1) 33_554 129_655 ?
N1 Mn2 N1 90.0 149_565 129_655 ?
N1 Mn2 N1 90.000(2) 33_554 . ?
N1 Mn2 N1 90.0 149_565 . ?
N1 Mn2 N1 90.0 129_655 . ?
N1 Mn2 N1 90.0 33_554 53_554 ?
N1 Mn2 N1 180.000(1) 149_565 53_554 ?
N1 Mn2 N1 90.0 129_655 53_554 ?
N1 Mn2 N1 90.000(1) . 53_554 ?
N1 Mn2 N1 90.0 33_554 97_665 ?
N1 Mn2 N1 90.000(2) 149_565 97_665 ?
N1 Mn2 N1 90.000(2) 129_655 97_665 ?
N1 Mn2 N1 180.0 . 97_665 ?
N1 Mn2 N1 90.0 53_554 97_665 ?
Nb1 Cl3 Nb1 73.09(13) 177 . ?
N1 C1 Nb1 180.0 . . ?
C1 N1 Mn2 180.0 . . ?
C2 N2 C2 109.471(1) . 28 ?
C2 N2 C2 109.471(1) . 74 ?
C2 N2 C2 109.471(3) 28 74 ?
C2 N2 C2 109.5 . 51 ?
C2 N2 C2 109.471(1) 28 51 ?
C2 N2 C2 109.471(3) 74 51 ?
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
Nb1 C1 2.27(2) . ?
Nb1 Cl3 2.468(3) 126_554 ?
Nb1 Cl3 2.468(3) 98 ?
Nb1 Cl3 2.468(3) . ?
Nb1 Cl3 2.468(3) 125 ?
Nb1 Nb1 2.939(3) 125 ?
Nb1 Nb1 2.939(3) 177 ?
Nb1 Nb1 2.939(3) 29_554 ?
Nb1 Nb1 2.939(3) 81_455 ?
Mn2 N1 2.24(2) 33_554 ?
Mn2 N1 2.24(2) 149_565 ?
Mn2 N1 2.24(2) 129_655 ?
Mn2 N1 2.24(2) . ?
Mn2 N1 2.24(2) 53_554 ?
Mn2 N1 2.24(2) 97_665 ?
Cl3 Nb1 2.468(3) 177 ?
C1 N1 1.16(3) . ?
C2 N2 1.458(17) . ?
N2 C2 1.458(17) 28 ?
N2 C2 1.458(17) 74 ?
N2 C2 1.458(17) 51 ?
