#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:14:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179318 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/15/4321555.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_4321555
loop_
_publ_author_name
'Chuan He'
'Stephen J. Lippard'
_publ_section_title
;
 Synthesis and Characterization of Several Dicopper(I) Complexes and a
 Spin-Delocalized Dicopper(I,II) Mixed-Valence Complex Using a
 1,8-Naphthyridine-Based Dinucleating Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5225
_journal_page_last               5231
_journal_paper_doi               10.1021/ic0005339
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C50 H46 Cu2 F6 N6 O6 S2'
_chemical_formula_weight         1132.13
_chemical_name_common            '[Cu2(TBAN)(py)2](OTf)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 101.369(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   15.490(5)
_cell_length_b                   15.846(5)
_cell_length_c                   21.070(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5070(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15767
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.998
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.798
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.798
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                4448
_reflns_number_total             5856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0005339_2.cif
_cod_data_source_block           Compound2
_cod_database_code               4321555
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Cu1 Cu 0.559010(16) 0.073856(14) 0.711992(13) 0.03092(10) Uani 1 1 d . . .
N1 N 0.56370(10) -0.04751(10) 0.72876(7) 0.0240(3) Uani 1 1 d . . .
N2 N 0.65382(10) 0.03364(10) 0.64240(8) 0.0267(3) Uani 1 1 d . . .
C1 C 0.62786(13) -0.08946(12) 0.70843(9) 0.0273(4) Uani 1 1 d . . .
C2 C 0.63435(14) -0.17788(13) 0.71044(10) 0.0352(5) Uani 1 1 d . . .
H2A H 0.6820 -0.2047 0.6983 0.042 Uiso 1 1 calc R . .
C3 C 0.57071(16) -0.22387(13) 0.73016(11) 0.0389(5) Uani 1 1 d . . .
H3A H 0.5735 -0.2825 0.7306 0.047 Uiso 1 1 calc R . .
C4 C 0.5000 -0.18187(17) 0.7500 0.0312(6) Uani 1 2 d S . .
C5 C 0.5000 -0.09298(16) 0.7500 0.0239(5) Uani 1 2 d S . .
C6 C 0.69482(12) -0.03737(13) 0.68200(10) 0.0290(4) Uani 1 1 d . . .
H6A H 0.7385 -0.0158 0.7178 0.035 Uiso 1 1 calc R . .
H6B H 0.7249 -0.0732 0.6559 0.035 Uiso 1 1 calc R . .
C7 C 0.71562(13) 0.10562(13) 0.64212(10) 0.0315(4) Uani 1 1 d . . .
H7A H 0.7316 0.1271 0.6860 0.038 Uiso 1 1 calc R . .
H7B H 0.6841 0.1502 0.6157 0.038 Uiso 1 1 calc R . .
C8 C 0.79996(14) 0.08827(12) 0.61793(11) 0.0313(4) Uani 1 1 d . . .
C9 C 0.87858(15) 0.07551(14) 0.66210(12) 0.0399(5) Uani 1 1 d . . .
H9A H 0.8787 0.0753 0.7063 0.048 Uiso 1 1 calc R . .
C10 C 0.95675(16) 0.06315(17) 0.64049(14) 0.0512(6) Uani 1 1 d . . .
H10A H 1.0091 0.0560 0.6703 0.061 Uiso 1 1 calc R . .
C11 C 0.95741(17) 0.06140(16) 0.57583(14) 0.0494(6) Uani 1 1 d . . .
H11A H 1.0100 0.0525 0.5618 0.059 Uiso 1 1 calc R . .
C12 C 0.88065(17) 0.07275(16) 0.53146(13) 0.0481(6) Uani 1 1 d . . .
H12A H 0.8811 0.0705 0.4874 0.058 Uiso 1 1 calc R . .
C13 C 0.80186(16) 0.08762(15) 0.55235(12) 0.0411(5) Uani 1 1 d . . .
H13A H 0.7503 0.0972 0.5221 0.049 Uiso 1 1 calc R . .
C14 C 0.61371(13) 0.00766(13) 0.57529(9) 0.0320(4) Uani 1 1 d . . .
H14A H 0.6594 -0.0157 0.5549 0.038 Uiso 1 1 calc R . .
H14B H 0.5904 0.0573 0.5509 0.038 Uiso 1 1 calc R . .
C15 C 0.54053(13) -0.05682(13) 0.57155(9) 0.0290(4) Uani 1 1 d . . .
C16 C 0.46045(13) -0.03602(14) 0.58814(9) 0.0316(4) Uani 1 1 d . . .
H16A H 0.4506 0.0190 0.6003 0.038 Uiso 1 1 calc R . .
C17 C 0.39482(14) -0.09653(16) 0.58681(10) 0.0380(5) Uani 1 1 d . . .
H17A H 0.3423 -0.0823 0.5993 0.046 Uiso 1 1 calc R . .
C18 C 0.40795(16) -0.17768(16) 0.56695(12) 0.0451(6) Uani 1 1 d . . .
H18A H 0.3644 -0.2183 0.5661 0.054 Uiso 1 1 calc R . .
C19 C 0.48624(17) -0.19874(15) 0.54824(13) 0.0472(6) Uani 1 1 d . . .
H19A H 0.4947 -0.2532 0.5342 0.057 Uiso 1 1 calc R . .
C20 C 0.55177(15) -0.13871(14) 0.55053(11) 0.0382(5) Uani 1 1 d . . .
H20A H 0.6040 -0.1533 0.5379 0.046 Uiso 1 1 calc R . .
N3 N 0.54717(11) 0.19227(10) 0.69042(8) 0.0294(3) Uani 1 1 d . . .
C21 C 0.48817(15) 0.21995(15) 0.63924(12) 0.0421(5) Uani 1 1 d . . .
H21A H 0.4450 0.1828 0.6187 0.050 Uiso 1 1 calc R . .
C22 C 0.4889(2) 0.30099(18) 0.61589(14) 0.0590(7) Uani 1 1 d . . .
H22A H 0.4462 0.3185 0.5810 0.071 Uiso 1 1 calc R . .
C23 C 0.5537(2) 0.35590(16) 0.64487(15) 0.0621(8) Uani 1 1 d . . .
H23A H 0.5571 0.4102 0.6287 0.074 Uiso 1 1 calc R . .
C24 C 0.61280(19) 0.32902(16) 0.69767(15) 0.0586(7) Uani 1 1 d . . .
H24A H 0.6565 0.3652 0.7187 0.070 Uiso 1 1 calc R . .
C25 C 0.60722(16) 0.24750(14) 0.71963(12) 0.0432(5) Uani 1 1 d . . .
H25A H 0.6470 0.2303 0.7564 0.052 Uiso 1 1 calc R . .
S1 S 0.76242(3) -0.08502(3) 0.34965(2) 0.03004(13) Uani 1 1 d . . .
O1 O 0.79645(12) -0.00382(11) 0.37082(9) 0.0555(5) Uani 1 1 d . . .
O2 O 0.81455(12) -0.13153(12) 0.31278(8) 0.0548(5) Uani 1 1 d . . .
O3 O 0.66918(11) -0.08815(11) 0.32456(9) 0.0501(4) Uani 1 1 d . . .
C26 C 0.77243(15) -0.14575(16) 0.42426(11) 0.0436(5) Uani 1 1 d . . .
F1 F 0.72309(12) -0.11283(14) 0.46284(8) 0.0758(5) Uani 1 1 d . . .
F2 F 0.85428(10) -0.14937(13) 0.45717(8) 0.0740(6) Uani 1 1 d . . .
F3 F 0.74473(12) -0.22479(10) 0.41219(9) 0.0702(5) Uani 1 1 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 0.0000 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'
S S 0.1246 0.1234 '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'
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
N3 Cu1 N1 175.85(7) . . ?
N3 Cu1 N2 99.09(6) . . ?
N1 Cu1 N2 80.85(6) . . ?
N3 Cu1 Cu1 95.58(5) . 2_656 ?
N1 Cu1 Cu1 84.06(5) . 2_656 ?
N2 Cu1 Cu1 164.04(4) . 2_656 ?
C1 N1 C5 118.30(17) . . ?
C1 N1 Cu1 115.83(13) . . ?
C5 N1 Cu1 125.08(13) . . ?
C6 N2 C14 112.40(16) . . ?
C6 N2 C7 112.49(16) . . ?
C14 N2 C7 110.90(15) . . ?
C6 N2 Cu1 96.11(11) . . ?
C14 N2 Cu1 118.15(11) . . ?
C7 N2 Cu1 105.96(12) . . ?
N1 C1 C2 122.72(18) . . ?
N1 C1 C6 116.99(17) . . ?
C2 C1 C6 120.29(18) . . ?
C3 C2 C1 119.57(19) . . ?
C2 C3 C4 119.4(2) . . ?
C5 C4 C3 118.09(13) . 2_656 ?
C5 C4 C3 118.09(13) . . ?
C3 C4 C3 123.8(3) 2_656 . ?
N1 C5 N1 116.4(2) 2_656 . ?
N1 C5 C4 121.83(11) 2_656 . ?
N1 C5 C4 121.82(11) . . ?
N2 C6 C1 112.06(15) . . ?
N2 C7 C8 117.32(17) . . ?
C13 C8 C9 118.5(2) . . ?
C13 C8 C7 121.6(2) . . ?
C9 C8 C7 119.9(2) . . ?
C10 C9 C8 120.3(2) . . ?
C11 C10 C9 120.6(2) . . ?
C10 C11 C12 120.1(2) . . ?
C11 C12 C13 120.1(2) . . ?
C8 C13 C12 120.4(2) . . ?
N2 C14 C15 113.83(15) . . ?
C20 C15 C16 118.26(19) . . ?
C20 C15 C14 120.33(18) . . ?
C16 C15 C14 121.40(19) . . ?
C15 C16 C17 120.9(2) . . ?
C18 C17 C16 119.8(2) . . ?
C17 C18 C19 120.0(2) . . ?
C20 C19 C18 120.0(2) . . ?
C19 C20 C15 120.9(2) . . ?
C25 N3 C21 117.26(19) . . ?
C25 N3 Cu1 120.20(15) . . ?
C21 N3 Cu1 121.65(15) . . ?
N3 C21 C22 122.7(2) . . ?
C21 C22 C23 119.2(2) . . ?
C24 C23 C22 118.6(2) . . ?
C23 C24 C25 119.3(2) . . ?
N3 C25 C24 122.9(2) . . ?
O1 S1 O2 114.88(12) . . ?
O1 S1 O3 115.35(11) . . ?
O2 S1 O3 114.59(12) . . ?
O1 S1 C26 104.05(12) . . ?
O2 S1 C26 103.60(11) . . ?
O3 S1 C26 101.97(11) . . ?
F2 C26 F1 107.7(2) . . ?
F2 C26 F3 107.4(2) . . ?
F1 C26 F3 106.5(2) . . ?
F2 C26 S1 112.65(17) . . ?
F1 C26 S1 111.04(17) . . ?
F3 C26 S1 111.23(17) . . ?
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
Cu1 N3 1.9308(17) . ?
Cu1 N1 1.9542(17) . ?
Cu1 N2 2.3583(16) . ?
Cu1 Cu1 2.6574(7) 2_656 ?
N1 C1 1.335(2) . ?
N1 C5 1.366(2) . ?
N2 C6 1.469(3) . ?
N2 C14 1.486(2) . ?
N2 C7 1.490(3) . ?
C1 C2 1.405(3) . ?
C1 C6 1.515(3) . ?
C2 C3 1.355(3) . ?
C3 C4 1.413(2) . ?
C4 C5 1.409(4) . ?
C4 C3 1.413(2) 2_656 ?
C5 N1 1.366(2) 2_656 ?
C7 C8 1.518(3) . ?
C8 C13 1.388(3) . ?
C8 C9 1.394(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.365(4) . ?
C11 C12 1.372(4) . ?
C12 C13 1.397(3) . ?
C14 C15 1.517(3) . ?
C15 C20 1.393(3) . ?
C15 C16 1.393(3) . ?
C16 C17 1.394(3) . ?
C17 C18 1.380(3) . ?
C18 C19 1.388(3) . ?
C19 C20 1.385(3) . ?
N3 C25 1.336(3) . ?
N3 C21 1.342(3) . ?
C21 C22 1.376(3) . ?
C22 C23 1.377(4) . ?
C23 C24 1.362(4) . ?
C24 C25 1.381(3) . ?
S1 O1 1.4282(18) . ?
S1 O2 1.4304(17) . ?
S1 O3 1.4377(18) . ?
S1 C26 1.824(2) . ?
C26 F2 1.321(3) . ?
C26 F1 1.327(3) . ?
C26 F3 1.332(3) . ?
