#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/10/7001090.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_7001090
loop_
_publ_author_name
'Mahenthirarajah, Thushitha'
'Li, Yang'
'Lightfoot, Philip'
_publ_section_title
;
 Organic--inorganic hybrid chains and layers constructed from
 copper-amine cations and early transition metal (Nb, Mo) oxyfluoride
 anions
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3280
_journal_page_last               3285
_journal_paper_doi               10.1039/b900356h
_journal_year                    2009
_chemical_formula_moiety         'C20 H18 Cu2 F7 N6 Nb O '
_chemical_formula_sum            'C20 H18 Cu2 F7 N6 Nb O'
_chemical_formula_weight         711.41
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 112.57(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.469(6)
_cell_length_b                   17.173(10)
_cell_length_c                   7.419(5)
_cell_measurement_reflns_used    3853
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     1114.0(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Confocal optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3853
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.38
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.271
_refine_diff_density_min         -1.966
_refine_diff_density_rms         0.627
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1184
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0529
_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)+(0.1144P)²+2.4201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1843
_reflns_number_gt                974
_reflns_number_total             1184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b900356h.txt
_cod_data_source_block           6
_cod_original_sg_symbol_Hall     '-C 2y '
_cod_original_sg_symbol_H-M      'C 2/m '
_cod_original_formula_sum        'C20 H18 Cu2 F7 N6 Nb O '
_cod_database_code               7001090
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.0000 0.0000 0.5000 0.0245(4) Uani 1 4 d S . .
Cu1 Cu -0.17213(9) 0.0000 -0.07811(12) 0.0177(4) Uani 1 2 d S . .
F2 F -0.1613(5) 0.0000 0.2414(6) 0.0263(11) Uani 0.75 2 d SP . .
O2 O -0.1613(5) 0.0000 0.2414(6) 0.0263(11) Uani 0.25 2 d SP . .
F3 F 0.1591(5) 0.0000 0.3983(6) 0.0292(12) Uani 0.75 2 d SP . .
O3 O 0.1591(5) 0.0000 0.3983(6) 0.0292(12) Uani 0.25 2 d SP . .
F1 F 0.0000 0.1119(3) 0.5000 0.0410(13) Uani 1 2 d S . .
F4 F 0.0000 0.0719(3) 0.0000 0.0235(10) Uani 1 2 d S . .
N1 N -0.3296(5) 0.0837(3) -0.1679(6) 0.0185(10) Uani 1 1 d . . .
N2 N -0.5416(9) 0.0000 -0.2322(14) 0.042(2) Uani 1 2 d SD . .
H2A H -0.632(6) 0.0000 -0.320(13) 0.063 Uiso 1 2 d SD . .
C4 C -0.5839(5) 0.1364(4) -0.2906(8) 0.0267(15) Uani 1 1 d . . .
H41 H -0.6885 0.1276 -0.3319 0.032 Uiso 1 1 calc R . .
C1 C -0.2797(6) 0.1580(3) -0.1680(8) 0.0256(13) Uani 1 1 d . . .
H11 H -0.1748 0.1663 -0.1249 0.031 Uiso 1 1 calc R . .
C5 C -0.4818(6) 0.0732(3) -0.2289(8) 0.0224(12) Uani 1 1 d . . .
C3 C -0.5315(6) 0.2095(3) -0.2905(8) 0.0261(12) Uani 1 1 d . . .
H31 H -0.5989 0.2512 -0.3317 0.031 Uiso 1 1 calc R . .
C2 C -0.3738(6) 0.2211(3) -0.2271(8) 0.0265(12) Uani 1 1 d . . .
H21 H -0.3339 0.2707 -0.2253 0.032 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'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 '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'
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
F1 Nb1 F1 180.0 . 5_556 ?
F1 Nb1 F3 90.000(1) . . ?
F1 Nb1 F3 90.0 5_556 . ?
F1 Nb1 O3 90.0 . 5_556 ?
F1 Nb1 O3 90.000(1) 5_556 5_556 ?
F3 Nb1 O3 180.0 . 5_556 ?
F1 Nb1 F3 90.0 . 5_556 ?
F1 Nb1 F3 90.000(1) 5_556 5_556 ?
F3 Nb1 F3 180.0 . 5_556 ?
O3 Nb1 F3 0.00(10) 5_556 5_556 ?
F1 Nb1 F2 90.000(1) . 5_556 ?
F1 Nb1 F2 90.0 5_556 5_556 ?
F3 Nb1 F2 87.14(18) . 5_556 ?
O3 Nb1 F2 92.86(18) 5_556 5_556 ?
F3 Nb1 F2 92.86(18) 5_556 5_556 ?
F1 Nb1 O2 90.000(1) . 5_556 ?
F1 Nb1 O2 90.0 5_556 5_556 ?
F3 Nb1 O2 87.14(18) . 5_556 ?
O3 Nb1 O2 92.86(18) 5_556 5_556 ?
F3 Nb1 O2 92.86(18) 5_556 5_556 ?
F2 Nb1 O2 0.0(2) 5_556 5_556 ?
F1 Nb1 F2 90.0 . . ?
F1 Nb1 F2 90.000(1) 5_556 . ?
F3 Nb1 F2 92.86(18) . . ?
O3 Nb1 F2 87.14(18) 5_556 . ?
F3 Nb1 F2 87.14(18) 5_556 . ?
F2 Nb1 F2 180.0 5_556 . ?
O2 Nb1 F2 180.0 5_556 . ?
F4 Cu1 F4 78.7(2) . 5 ?
F4 Cu1 N1 172.06(16) . 6 ?
F4 Cu1 N1 94.34(17) 5 6 ?
F4 Cu1 N1 94.34(17) . . ?
F4 Cu1 N1 172.06(16) 5 . ?
N1 Cu1 N1 92.3(3) 6 . ?
F4 Cu1 F2 89.56(9) . . ?
F4 Cu1 F2 89.56(9) 5 . ?
N1 Cu1 F2 94.31(14) 6 . ?
N1 Cu1 F2 94.31(14) . . ?
F4 Cu1 O3 86.57(8) . 5 ?
F4 Cu1 O3 86.57(8) 5 5 ?
N1 Cu1 O3 89.16(14) 6 5 ?
N1 Cu1 O3 89.16(14) . 5 ?
F2 Cu1 O3 174.98(15) . 5 ?
F4 Cu1 Cu1 39.36(10) . 5 ?
F4 Cu1 Cu1 39.36(10) 5 5 ?
N1 Cu1 Cu1 133.59(13) 6 5 ?
N1 Cu1 Cu1 133.59(13) . 5 ?
F2 Cu1 Cu1 89.42(11) . 5 ?
O3 Cu1 Cu1 85.56(11) 5 5 ?
Nb1 F2 Cu1 135.7(2) . . ?
Cu1 F4 Cu1 101.3(2) . 5 ?
C5 N1 C1 116.8(4) . . ?
C5 N1 Cu1 125.7(3) . . ?
C1 N1 Cu1 117.4(3) . . ?
C5 N2 C5 132.3(8) . 6 ?
C5 N2 H2A 107(3) . . ?
C5 N2 H2A 107(3) 6 . ?
C3 C4 C5 120.7(5) . . ?
C3 C4 H41 119.6 . . ?
C5 C4 H41 119.6 . . ?
N1 C1 C2 124.1(5) . . ?
N1 C1 H11 117.9 . . ?
C2 C1 H11 117.9 . . ?
N1 C5 N2 120.5(5) . . ?
N1 C5 C4 121.3(5) . . ?
N2 C5 C4 118.2(6) . . ?
C4 C3 C2 118.5(5) . . ?
C4 C3 H31 120.7 . . ?
C2 C3 H31 120.7 . . ?
C1 C2 C3 118.5(5) . . ?
C1 C2 H21 120.7 . . ?
C3 C2 H21 120.7 . . ?
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 F1 1.921(5) . ?
Nb1 F1 1.921(5) 5_556 ?
Nb1 F3 1.926(4) . ?
Nb1 O3 1.926(4) 5_556 ?
Nb1 F3 1.926(4) 5_556 ?
Nb1 F2 1.940(4) 5_556 ?
Nb1 O2 1.940(4) 5_556 ?
Nb1 F2 1.940(4) . ?
Cu1 F4 1.948(3) . ?
Cu1 F4 1.948(3) 5 ?
Cu1 N1 1.992(5) 6 ?
Cu1 N1 1.992(5) . ?
Cu1 F2 2.333(5) . ?
Cu1 O3 2.426(5) 5 ?
Cu1 Cu1 3.011(2) 5 ?
F4 Cu1 1.948(3) 5 ?
N1 C5 1.347(7) . ?
N1 C1 1.362(7) . ?
N2 C5 1.375(7) . ?
N2 C5 1.375(7) 6 ?
N2 H2A 0.86(2) . ?
C4 C3 1.350(9) . ?
C4 C5 1.406(8) . ?
C4 H41 0.9300 . ?
C1 C2 1.363(8) . ?
C1 H11 0.9300 . ?
C3 C2 1.397(7) . ?
C3 H31 0.9300 . ?
C2 H21 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A F2 0.86(2) 2.24(11) 2.788(9) 122(10) 5_455
N2 H2A F3 0.86(2) 2.26(4) 3.096(10) 166(12) 1_454
