#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:31:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180185 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/81/7108161.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_7108161
loop_
_publ_author_name
'Dawid Pinkowicz'
'Michal Rams'
'Wojciech Nitek'
'Bernard Czarnecki'
'Barbara Sieklucka'
_publ_section_title
;
 Evidence for magnetic anisotropy of [NbIV(CN)8]\4- in a
 pillared-layered Mn2Nb framework showing spin-flop transition
;
_journal_name_full               Chem.Commun.
_journal_page_first              8323
_journal_paper_doi               10.1039/c2cc32234j
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H28 Mn2 N10 Nb1 O12'
_chemical_formula_sum            'C18 H28 Mn2 N10 Nb O12'
_chemical_formula_weight         779.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-04-17T10:30:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.49250(10)
_cell_length_b                   11.47820(10)
_cell_length_c                   12.3333(2)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     1485.36(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19735
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.29
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(13)
_refine_ls_extinction_coef       0.0079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         6512
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0316P)²+0.1160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                5824
_reflns_number_total             6512
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2cc32234j.txt
_cod_data_source_block           bpdo
_cod_database_code               7108161
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -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 -0.5 -0.720170(12) 0.01792(4) Uani 1 2 d S
Mn2 Mn -0.33830(2) -0.45260(2) -0.380199(17) 0.02087(5) Uani 1 1 d .
O5 O -0.5 -0.5 -0.27311(10) 0.0256(3) Uani 1 2 d S
N4 N -0.5 -0.5 -0.16380(12) 0.0214(3) Uani 1 2 d S
C1 C -0.5 -0.5 0.06016(15) 0.0225(3) Uani 1 2 d S
O10 O -0.5 -0.5 0.51360(11) 0.0275(3) Uani 1 2 d S
N9 N -0.5 -0.5 0.40426(13) 0.0237(3) Uani 1 2 d S
C11 C -0.12916(16) -0.45883(14) -0.57883(13) 0.0244(3) Uani 1 1 d .
C12 C -0.15554(18) -0.38176(14) -0.77831(14) 0.0284(3) Uani 1 1 d .
O2H O -0.28865(16) -0.64114(13) -0.39495(14) 0.0416(3) Uani 1 1 d D
O1H O -0.20365(15) -0.44721(16) -0.25018(12) 0.0441(4) Uani 1 1 d D
N11 N -0.19850(15) -0.43637(14) -0.51027(12) 0.0313(3) Uani 1 1 d .
N13 N 0.11120(16) -0.23294(13) -0.64253(14) 0.0323(3) Uani 1 1 d .
C3 C -0.53446(19) -0.40365(15) -0.11017(14) 0.0330(4) Uani 1 1 d .
H3 H -0.5585 -0.3375 -0.1485 0.04 Uiso 1 1 calc R
C7 C -0.57811(18) -0.42486(15) 0.23937(13) 0.0285(3) Uani 1 1 d .
H7 H -0.6314 -0.3732 0.203 0.034 Uiso 1 1 calc R
C8 C -0.57708(17) -0.42641(15) 0.35150(13) 0.0279(3) Uani 1 1 d .
H8 H -0.6299 -0.3764 0.3902 0.034 Uiso 1 1 calc R
C2 C -0.5345(2) -0.40192(15) 0.00141(13) 0.0333(4) Uani 1 1 d .
H2 H -0.5579 -0.3343 0.0378 0.04 Uiso 1 1 calc R
C13 C 0.07508(17) -0.32365(14) -0.66581(13) 0.0254(3) Uani 1 1 d .
N12 N -0.23385(19) -0.32056(17) -0.80896(15) 0.0433(4) Uani 1 1 d .
C6 C -0.5 -0.5 0.18040(15) 0.0236(3) Uani 1 2 d S
C14 C 0.0861(2) -0.41265(17) -0.86451(15) 0.0351(4) Uani 1 1 d .
O3H O -0.0341(2) -0.6842(2) -0.38673(17) 0.0662(5) Uani 1 1 d D
O5H O -0.2135(3) -0.3361(2) -0.05927(16) 0.0675(6) Uani 1 1 d D
O4H O -0.08475(19) -0.64107(17) -0.17040(15) 0.0530(4) Uani 1 1 d D
N15 N 0.1295(3) -0.3670(2) -0.93831(18) 0.0610(6) Uani 1 1 d .
H1A H -0.167(3) -0.5150(19) -0.232(2) 0.073(10) Uiso 1 1 d D
H5A H -0.201(4) -0.389(3) -0.007(3) 0.112(16) Uiso 1 1 d D
H1B H -0.223(3) -0.408(2) -0.1913(17) 0.054(8) Uiso 1 1 d D
H4B H -0.148(3) -0.691(2) -0.174(3) 0.073(10) Uiso 1 1 d D
H3A H -0.014(4) -0.660(3) -0.3166(17) 0.092(12) Uiso 1 1 d D
H5B H -0.272(5) -0.281(4) -0.046(4) 0.16(3) Uiso 1 1 d D
H2A H -0.2079(18) -0.661(3) -0.395(3) 0.076(11) Uiso 1 1 d D
H2B H -0.337(3) -0.695(3) -0.365(3) 0.108(14) Uiso 1 1 d D
H4A H -0.052(4) -0.630(5) -0.102(2) 0.15(2) Uiso 1 1 d D
H3B H 0.013(6) -0.632(4) -0.429(3) 0.17(2) Uiso 1 1 d 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 0 '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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.006 '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
C14 Nb1 C14 74.32(11) 2_545 .
C14 Nb1 C12 76.56(7) 2_545 2_545
C14 Nb1 C12 73.88(7) . 2_545
C14 Nb1 C12 73.88(7) 2_545 .
C14 Nb1 C12 76.56(7) . .
C12 Nb1 C12 142.67(9) 2_545 .
C14 Nb1 C11 139.81(6) 2_545 2_545
C14 Nb1 C11 117.81(7) . 2_545
C12 Nb1 C11 71.53(6) 2_545 2_545
C12 Nb1 C11 144.20(6) . 2_545
C14 Nb1 C11 117.81(7) 2_545 .
C14 Nb1 C11 139.81(6) . .
C12 Nb1 C11 144.20(6) 2_545 .
C12 Nb1 C11 71.53(6) . .
C11 Nb1 C11 78.93(8) 2_545 .
C14 Nb1 C13 140.79(6) 2_545 .
C14 Nb1 C13 72.26(7) . .
C12 Nb1 C13 112.42(6) 2_545 .
C12 Nb1 C13 78.90(6) . .
C11 Nb1 C13 75.56(6) 2_545 .
C11 Nb1 C13 78.11(6) . .
C14 Nb1 C13 72.26(7) 2_545 2_545
C14 Nb1 C13 140.79(6) . 2_545
C12 Nb1 C13 78.90(6) 2_545 2_545
C12 Nb1 C13 112.42(6) . 2_545
C11 Nb1 C13 78.11(6) 2_545 2_545
C11 Nb1 C13 75.56(6) . 2_545
C13 Nb1 C13 145.69(8) . 2_545
O1H Mn2 N11 96.01(6) . .
O1H Mn2 O10 163.41(6) . 1_554
N11 Mn2 O10 95.81(5) . 1_554
O1H Mn2 N13 92.03(7) . 3_444
N11 Mn2 N13 99.90(6) . 3_444
O10 Mn2 N13 97.36(5) 1_554 3_444
O1H Mn2 O5 93.78(5) . .
N11 Mn2 O5 166.69(5) . .
O10 Mn2 O5 72.87(4) 1_554 .
N13 Mn2 O5 88.71(4) 3_444 .
O1H Mn2 O2H 86.28(7) . .
N11 Mn2 O2H 82.30(6) . .
O10 Mn2 O2H 83.82(5) 1_554 .
N13 Mn2 O2H 177.36(6) 3_444 .
O5 Mn2 O2H 89.39(5) . .
N4 O5 Mn2 126.55(3) . 2_445
N4 O5 Mn2 126.55(3) . .
Mn2 O5 Mn2 106.90(5) 2_445 .
C3 N4 C3 120.76(18) 2_445 .
C3 N4 O5 119.62(9) 2_445 .
C3 N4 O5 119.62(9) . .
C2 C1 C2 117.01(18) 2_445 .
C2 C1 C6 121.50(9) 2_445 .
C2 C1 C6 121.50(9) . .
N9 O10 Mn2 126.32(3) . 1_556
N9 O10 Mn2 126.32(3) . 2_446
Mn2 O10 Mn2 107.36(6) 1_556 2_446
C8 N9 C8 121.82(18) . 2_445
C8 N9 O10 119.09(9) . .
C8 N9 O10 119.09(9) 2_445 .
N11 C11 Nb1 177.06(15) . .
N12 C12 Nb1 179.04(18) . .
C11 N11 Mn2 162.00(15) . .
C13 N13 Mn2 170.65(16) . 3_544
N4 C3 C2 120.41(15) . .
C8 C7 C6 120.59(16) . .
N9 C8 C7 119.93(16) . .
C3 C2 C1 120.70(16) . .
N13 C13 Nb1 177.10(16) . .
C7 C6 C7 117.13(19) . 2_445
C7 C6 C1 121.44(9) . .
C7 C6 C1 121.44(9) 2_445 .
N15 C14 Nb1 179.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 C14 2.2338(18) 2_545
Nb1 C14 2.2338(18) .
Nb1 C12 2.2405(17) 2_545
Nb1 C12 2.2405(17) .
Nb1 C11 2.2580(17) 2_545
Nb1 C11 2.2580(17) .
Nb1 C13 2.2732(16) .
Nb1 C13 2.2732(17) 2_545
Mn2 O1H 2.1380(14) .
Mn2 N11 2.1817(15) .
Mn2 O10 2.2114(8) 1_554
Mn2 N13 2.2125(15) 3_444
Mn2 O5 2.2179(8) .
Mn2 O2H 2.2333(14) .
O5 N4 1.3481(19) .
O5 Mn2 2.2179(8) 2_445
N4 C3 1.3384(19) 2_445
N4 C3 1.3384(19) .
C1 C2 1.3869(19) 2_445
C1 C2 1.3869(19) .
C1 C6 1.483(2) .
O10 N9 1.349(2) .
O10 Mn2 2.2114(8) 1_556
O10 Mn2 2.2114(8) 2_446
N9 C8 1.3383(19) .
N9 C8 1.3383(19) 2_445
C11 N11 1.145(2) .
C12 N12 1.145(2) .
N13 C13 1.145(2) .
N13 Mn2 2.2125(15) 3_544
C3 C2 1.376(2) .
C7 C8 1.383(2) .
C7 C6 1.394(2) .
C6 C7 1.394(2) 2_445
C14 N15 1.145(3) .
