#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308579.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_4308579
loop_
_publ_author_name
'Heather K. Izumi'
'Janet E. Kirsch'
'Charlotte L. Stern'
'Kenneth R. Poeppelmeier'
_publ_section_title
;
Examining the Out-of-Center Distortion in the [NbOF5]2- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              884
_journal_page_last               895
_journal_paper_doi               10.1021/ic048766d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C30 H38 Cu F10 N12 Nb2 O2'
_chemical_formula_weight         1038.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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            8
_cell_length_a                   20.8745(8)
_cell_length_b                   20.8745(8)
_cell_length_c                   17.2929(9)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.48
_cell_volume                     7535.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33069
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.9397
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   'face indexed'
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      1.83(7)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.438
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.165
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0436P)²+20.4668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                1913
_reflns_number_total             2436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048766dsi20040903_031408_1.cif
_cod_data_source_block           '[4-apyH][Cu(4-apy)4(NbOF5)2]'
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4308579
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
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 0.360039(10) 0.889961(10) 0.1250 0.01715(10) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.7500 0.1250 0.01675(14) Uani 1 4 d S . .
F1 F 0.28830(7) 0.96170(7) 0.1250 0.0282(5) Uani 1 2 d S . .
F2 F 0.40968(8) 0.95489(8) 0.17897(10) 0.0352(4) Uani 1 1 d . . .
F3 F 0.32001(8) 0.86443(8) 0.22211(9) 0.0327(4) Uani 1 1 d . . .
O1 O 0.41864(9) 0.83136(9) 0.1250 0.0266(6) Uani 1 2 d S . .
N1 N 0.44875(9) 0.70389(9) 0.20775(12) 0.0188(4) Uani 1 1 d . . .
N2 N 0.33880(12) 0.63334(12) 0.38999(14) 0.0311(5) Uani 1 1 d . . .
H2A H 0.3579 0.6174 0.4311 0.035(10) Uiso 1 1 calc R . .
H2B H 0.2967 0.6353 0.3881 0.042(10) Uiso 1 1 calc R . .
N3 N 0.2500 0.72983(15) 1.0000 0.0292(7) Uani 1 2 d S . .
H3A H 0.2500 0.7720 1.0000 0.035 Uiso 1 2 calc SR . .
N4 N 0.2500 0.53375(15) 1.0000 0.0310(7) Uani 1 2 d S . .
H4A H 0.2523 0.5127 1.0440 0.037 Uiso 0.50 1 calc PR . .
H4B H 0.2477 0.5127 0.9560 0.037 Uiso 0.50 1 calc PR . .
C1 C 0.47561(11) 0.67671(11) 0.27020(13) 0.0204(5) Uani 1 1 d . . .
H1A H 0.5210 0.6741 0.2723 0.034(9) Uiso 1 1 calc R . .
C2 C 0.44125(12) 0.65236(12) 0.33140(14) 0.0219(5) Uani 1 1 d . . .
H2C H 0.4629 0.6340 0.3743 0.027(8) Uiso 1 1 calc R . .
C3 C 0.37397(12) 0.65480(12) 0.33008(14) 0.0217(5) Uani 1 1 d . . .
C4 C 0.34571(12) 0.68141(12) 0.26352(15) 0.0242(5) Uani 1 1 d . . .
H4C H 0.3004 0.6828 0.2585 0.028(8) Uiso 1 1 calc R . .
C5 C 0.38413(12) 0.70524(12) 0.20601(15) 0.0226(5) Uani 1 1 d . . .
H5A H 0.3640 0.7239 0.1622 0.031(8) Uiso 1 1 calc R . .
C7 C 0.2500 0.59708(17) 1.0000 0.0245(7) Uani 1 2 d S . .
C8 C 0.24630(12) 0.63300(12) 0.93029(16) 0.0262(5) Uani 1 1 d . . .
H8A H 0.2437 0.6115 0.8820 0.031 Uiso 1 1 calc R . .
C9 C 0.24650(13) 0.69796(13) 0.93254(16) 0.0287(5) Uani 1 1 d . . .
H9A H 0.2441 0.7214 0.8855 0.034 Uiso 1 1 calc R . .
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'
F F 0.0171 0.0103 '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'
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
O1 Nb1 F2 96.66(5) . 8_665 ?
O1 Nb1 F2 96.66(5) . . ?
F2 Nb1 F2 166.68(10) 8_665 . ?
O1 Nb1 F3 96.30(5) . . ?
F2 Nb1 F3 88.22(7) 8_665 . ?
F2 Nb1 F3 90.32(7) . . ?
O1 Nb1 F3 96.30(5) . 8_665 ?
F2 Nb1 F3 90.32(7) 8_665 8_665 ?
F2 Nb1 F3 88.22(7) . 8_665 ?
F3 Nb1 F3 167.40(10) . 8_665 ?
O1 Nb1 F1 180.000(1) . . ?
F2 Nb1 F1 83.34(5) 8_665 . ?
F2 Nb1 F1 83.34(5) . . ?
F3 Nb1 F1 83.70(5) . . ?
F3 Nb1 F1 83.70(5) 8_665 . ?
N1 Cu1 N1 175.71(11) 10_564 15_444 ?
N1 Cu1 N1 89.83(11) 10_564 8_665 ?
N1 Cu1 N1 90.33(11) 15_444 8_665 ?
N1 Cu1 N1 90.33(11) 10_564 . ?
N1 Cu1 N1 89.83(11) 15_444 . ?
N1 Cu1 N1 175.71(11) 8_665 . ?
N1 Cu1 O1 87.86(6) 10_564 10_564 ?
N1 Cu1 O1 87.86(6) 15_444 10_564 ?
N1 Cu1 O1 92.14(6) 8_665 10_564 ?
N1 Cu1 O1 92.14(5) . 10_564 ?
N1 Cu1 O1 92.14(6) 10_564 . ?
N1 Cu1 O1 92.14(6) 15_444 . ?
N1 Cu1 O1 87.86(6) 8_665 . ?
N1 Cu1 O1 87.86(6) . . ?
O1 Cu1 O1 180.000(1) 10_564 . ?
Nb1 O1 Cu1 180.00(15) . . ?
C1 N1 C5 116.4(2) . . ?
C1 N1 Cu1 123.19(16) . . ?
C5 N1 Cu1 120.09(16) . . ?
C3 N2 H2A 120.0 . . ?
C3 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C9 N3 C9 120.7(3) . 5_557 ?
C9 N3 H3A 119.7 . . ?
C9 N3 H3A 119.7 5_557 . ?
C7 N4 H4A 120.0 . . ?
C7 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
N1 C1 C2 123.9(2) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
C1 C2 C3 119.7(2) . . ?
C1 C2 H2C 120.2 . . ?
C3 C2 H2C 120.2 . . ?
N2 C3 C2 121.3(2) . . ?
N2 C3 C4 122.1(2) . . ?
C2 C3 C4 116.5(2) . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4C 120.3 . . ?
C3 C4 H4C 120.3 . . ?
N1 C5 C4 124.1(2) . . ?
N1 C5 H5A 117.9 . . ?
C4 C5 H5A 117.9 . . ?
N4 C7 C8 121.83(16) . 5_557 ?
N4 C7 C8 121.83(16) . . ?
C8 C7 C8 116.3(3) 5_557 . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
N3 C9 C8 121.3(3) . . ?
N3 C9 H9A 119.3 . . ?
C8 C9 H9A 119.3 . . ?
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 O1 1.730(3) . ?
Nb1 F2 1.9447(15) 8_665 ?
Nb1 F2 1.9447(15) . ?
Nb1 F3 1.9499(15) . ?
Nb1 F3 1.9499(15) 8_665 ?
Nb1 F1 2.118(2) . ?
Cu1 N1 2.029(2) 10_564 ?
Cu1 N1 2.029(2) 15_444 ?
Cu1 N1 2.029(2) 8_665 ?
Cu1 N1 2.029(2) . ?
Cu1 O1 2.402(3) 10_564 ?
Cu1 O1 2.402(3) . ?
N1 C1 1.343(3) . ?
N1 C5 1.349(3) . ?
N2 C3 1.346(3) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N3 C9 1.345(3) . ?
N3 C9 1.345(3) 5_557 ?
N3 H3A 0.8800 . ?
N4 C7 1.322(5) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
C1 C2 1.376(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.405(4) . ?
C2 H2C 0.9500 . ?
C3 C4 1.408(3) . ?
C4 C5 1.371(3) . ?
C4 H4C 0.9500 . ?
C5 H5A 0.9500 . ?
C7 C8 1.422(3) 5_557 ?
C7 C8 1.422(3) . ?
C8 C9 1.356(4) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
