#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:34:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180227 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/13/7111388.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111388
loop_
_publ_author_name
'Yan, Bangbo'
'Day, Cynthia S.'
'Lachgar, Abdessadek'
_publ_section_title
;
 Octahedral metal clusters as building units in a neutral layered
 honeycomb network, [Zn(en)]2[Nb6Cl12(CN)6]
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2390
_journal_page_last               2391
_journal_paper_doi               10.1039/b408000a
_journal_year                    2004
_chemical_formula_sum            'C10 H16 Cl12 N10 Nb6 Zn2'
_chemical_formula_weight         1389.93
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   10.8914(10)
_cell_length_b                   10.8914(10)
_cell_length_c                   8.6850(17)
_cell_measurement_temperature    193(2)
_cell_volume                     892.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9092
_diffrn_reflns_theta_full        30.46
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         4.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.097
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       retangular
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0568
_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)+(0.0550P)²+3.7808P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                1278
_reflns_number_total             1770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b408000asup1.cif
_cod_data_source_block           a24c2f
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7111388
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb1 Nb 0.0885(2) 0.17857(6) 0.13735(6) 0.0223(2) Uani 1 1 d .
Zn1 Zn 0.3333 0.6667 0.47109(17) 0.0372(4) Uani 1 3 d S
Cl1 Cl -0.0043(10) 0.3141(5) -0.0075(6) 0.0329(5) Uani 1 1 d .
Cl2 Cl 0.2100(2) 0.1076(7) 0.32313(19) 0.0338(5) Uani 1 1 d .
C1 C 0.195(3) 0.3733(9) 0.2886(9) 0.029(3) Uani 1 1 d .
N1 N 0.237(2) 0.4741(8) 0.3614(9) 0.051(2) Uani 1 1 d .
N2 N 0.289(11) 0.551(4) 0.674(3) 0.10(2) Uani 0.33 1 d P
C2 C 0.386(6) 0.639(5) 0.803(2) 0.096(16) Uani 0.67 1 d P
N2' N 0.409(5) 0.567(5) 0.666(3) 0.044(7) Uiso 0.33 1 d P
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'
Zn Zn 0.2839 1.4301 '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
C1 Nb1 Cl1 78.3(6) . 5
C1 Nb1 Cl2 78.9(6) . .
Cl1 Nb1 Cl2 88.1(2) 5 .
C1 Nb1 Cl2 83.5(5) . 2
Cl1 Nb1 Cl2 161.8(2) 5 2
Cl2 Nb1 Cl2 88.67(9) . 2
C1 Nb1 Cl1 84.8(6) . .
Cl1 Nb1 Cl1 88.68(2) 5 .
Cl2 Nb1 Cl1 163.6(2) . .
Cl2 Nb1 Cl1 89.4(2) 2 .
C1 Nb1 Nb1 136.7(6) . 2
Cl1 Nb1 Nb1 144.94(15) 5 2
Cl2 Nb1 Nb1 96.25(13) . 2
Cl2 Nb1 Nb1 53.22(15) 2 2
Cl1 Nb1 Nb1 95.6(2) . 2
C1 Nb1 Nb1 132.8(6) . 3
Cl1 Nb1 Nb1 96.7(2) 5 3
Cl2 Nb1 Nb1 53.90(16) . 3
Cl2 Nb1 Nb1 95.77(11) 2 3
Cl1 Nb1 Nb1 142.45(13) . 3
Nb1 Nb1 Nb1 60.0 2 3
C1 Nb1 Nb1 137.2(6) . 6
Cl1 Nb1 Nb1 97.27(14) 5 6
Cl2 Nb1 Nb1 143.90(17) . 6
Cl2 Nb1 Nb1 95.87(12) 2 6
Cl1 Nb1 Nb1 52.45(14) . 6
Nb1 Nb1 Nb1 60.035(14) 2 6
Nb1 Nb1 Nb1 90.0 3 6
C1 Nb1 Nb1 133.2(6) . 5
Cl1 Nb1 Nb1 54.94(15) 5 5
Cl2 Nb1 Nb1 96.34(11) . 5
Cl2 Nb1 Nb1 143.22(15) 2 5
Cl1 Nb1 Nb1 94.89(13) . 5
Nb1 Nb1 Nb1 90.0 2 5
Nb1 Nb1 Nb1 60.035(14) 3 5
Nb1 Nb1 Nb1 59.93(3) 6 5
N1 Zn1 N1 100.2(3) 3_565 .
N1 Zn1 N1 100.2(3) 3_565 2_665
N1 Zn1 N1 100.2(3) . 2_665
N1 Zn1 N2 86.0(11) 3_565 3_565
N1 Zn1 N2 125(4) . 3_565
N1 Zn1 N2 133(4) 2_665 3_565
N1 Zn1 N2 125(3) 3_565 2_665
N1 Zn1 N2 133(4) . 2_665
N1 Zn1 N2 86.0(11) 2_665 2_665
N2 Zn1 N2 55(2) 3_565 2_665
N1 Zn1 N2 133(4) 3_565 .
N1 Zn1 N2 86.0(11) . .
N1 Zn1 N2 125(3) 2_665 .
N2 Zn1 N2 55(2) 3_565 .
N2 Zn1 N2 55(2) 2_665 .
N1 Zn1 N2' 93.8(12) 3_565 2_665
N1 Zn1 N2' 161.7(7) . 2_665
N1 Zn1 N2' 88.7(12) 2_665 2_665
N2 Zn1 N2' 44(3) 3_565 2_665
N2 Zn1 N2' 31(3) 2_665 2_665
N2 Zn1 N2' 75.9(11) . 2_665
N1 Zn1 N2' 88.7(12) 3_565 3_565
N1 Zn1 N2' 93.8(12) . 3_565
N1 Zn1 N2' 161.7(7) 2_665 3_565
N2 Zn1 N2' 31(3) 3_565 3_565
N2 Zn1 N2' 75.9(11) 2_665 3_565
N2 Zn1 N2' 44(3) . 3_565
N2' Zn1 N2' 74.7(9) 2_665 3_565
N1 Zn1 N2' 161.7(7) 3_565 .
N1 Zn1 N2' 88.7(12) . .
N1 Zn1 N2' 93.8(12) 2_665 .
N2 Zn1 N2' 75.9(11) 3_565 .
N2 Zn1 N2' 44(3) 2_665 .
N2 Zn1 N2' 31(3) . .
N2' Zn1 N2' 74.7(9) 2_665 .
N2' Zn1 N2' 74.7(9) 3_565 .
Nb1 Cl1 Nb1 72.61(6) 6 .
Nb1 Cl2 Nb1 72.89(5) . 3
N1 C1 Nb1 173(3) . .
C1 N1 Zn1 172.6(16) . .
N2' N2 C2 120(4) . 3_565
N2' N2 C2 66(4) . .
C2 N2 C2 53(2) 3_565 .
N2' N2 N2' 159(3) . 3_565
C2 N2 N2' 57(4) 3_565 3_565
C2 N2 N2' 106(5) . 3_565
N2' N2 Zn1 87(3) . .
C2 N2 Zn1 114(5) 3_565 .
C2 N2 Zn1 111(2) . .
N2' N2 Zn1 77(3) 3_565 .
C2 C2 C2 60.000(3) 3_565 2_665
C2 C2 N2 102(2) 3_565 2_665
C2 C2 N2 65(4) 2_665 2_665
C2 C2 N2 61(5) 3_565 .
C2 C2 N2 100(5) 2_665 .
N2 C2 N2 80(3) 2_665 .
C2 C2 N2' 109(4) 3_565 .
C2 C2 N2' 128.2(13) 2_665 .
N2 C2 N2' 69(4) 2_665 .
N2 C2 N2' 48(5) . .
N2 N2' C2 66(3) . .
N2 N2' N2 80(4) . 2_665
C2 N2' N2 54(2) . 2_665
N2 N2' Zn1 61.3(19) . .
C2 N2' Zn1 97.9(14) . .
N2 N2' Zn1 58.9(12) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 C1 2.260(8) .
Nb1 Cl1 2.426(5) 5
Nb1 Cl2 2.445(5) .
Nb1 Cl2 2.466(6) 2
Nb1 Cl1 2.505(5) .
Nb1 Nb1 2.9173(11) 2
Nb1 Nb1 2.9173(11) 3
Nb1 Nb1 2.9203(10) 6
Nb1 Nb1 2.9203(10) 5
Zn1 N1 2.051(8) 3_565
Zn1 N1 2.051(8) .
Zn1 N1 2.051(8) 2_665
Zn1 N2 2.08(3) 3_565
Zn1 N2 2.08(3) 2_665
Zn1 N2 2.08(3) .
Zn1 N2' 2.37(2) 2_665
Zn1 N2' 2.37(2) 3_565
Zn1 N2' 2.37(2) .
Cl1 Nb1 2.426(5) 6
Cl2 Nb1 2.466(6) 3
C1 N1 1.145(11) .
N2 N2' 1.23(12) .
N2 C2 1.46(8) 3_565
N2 C2 1.51(6) .
N2 N2' 1.69(12) 3_565
C2 C2 1.33(5) 3_565
C2 C2 1.33(5) 2_665
C2 N2 1.46(8) 2_665
C2 N2' 1.51(3) .
N2' N2 1.69(12) 2_665
