#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:14:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180067 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/13/7051327.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_7051327
loop_
_publ_author_name
'Iwayan Dasna'
'Stéphane Golhen'
'Lahcène Ouahab'
'Octavio Peña'
'Nathalie Daro'
_publ_section_title
;
 A dimeric Cu(II) acetate complex containing axially coordinated
 p-pyridyl nitronyl nitroxide radicals: [CuII(CH3COO)2(NITpPy)]2
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              903
_journal_page_last               906
_journal_paper_doi               10.1039/b004491l
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C16 H22 Cu N3 O6'
_chemical_formula_weight         415.91
_chemical_name_common            '[Cu(CH3COO)2(NITpPy)]2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.79(2)
_cell_angle_beta                 97.75(2)
_cell_angle_gamma                103.75(3)
_cell_formula_units_Z            2
_cell_length_a                   7.307(3)
_cell_length_b                   9.337(2)
_cell_length_c                   14.654(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.085
_cell_measurement_theta_min      8.312
_cell_volume                     932.8(5)
_computing_cell_refinement       MolEN
_computing_data_collection       'Enraf Nonius CAD4'
_computing_data_reduction        molEN
_computing_molecular_graphics    'ORTEP III'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       θ-2θ
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4844
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        -2.0
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  0.999635
_exptl_absorpt_correction_T_min  0.930035
_exptl_absorpt_correction_type   '\y scan'
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             432
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0451P)²+0.4340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3165
_reflns_number_total             4500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004491l.txt
_cod_data_source_block           calcul
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.4340P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.4340P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        932.7(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051327
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.62690(5) 0.54730(4) 0.57968(2) 0.03518(11) Uani 1 d . . .
N1 N 0.8395(3) 0.6238(2) 0.71077(14) 0.0319(5) Uani 1 d . . .
O6 O 1.5042(3) 0.7697(2) 0.93962(13) 0.0445(5) Uani 1 d . . .
N4 N 1.1381(3) 0.7221(2) 1.06315(13) 0.0309(4) Uani 1 d . . .
O2 O 0.7831(3) 0.6611(3) 0.50548(14) 0.0552(6) Uani 1 d . . .
C16 C 0.2710(4) 0.3421(3) 0.57997(19) 0.0422(6) Uani 1 d . . .
O4 O 0.4290(3) 0.4204(3) 0.63051(14) 0.0535(5) Uani 1 d . . .
O5 O 0.9652(3) 0.6759(3) 1.07309(14) 0.0517(5) Uani 1 d . . .
N3 N 1.3944(3) 0.7592(2) 0.99928(13) 0.0280(4) Uani 1 d . . .
O1 O 0.5034(3) 0.7123(2) 0.60707(14) 0.0543(6) Uani 1 d . . .
O3 O 0.7071(3) 0.3649(2) 0.52945(14) 0.0544(6) Uani 1 d . . .
C6 C 1.2015(3) 0.7176(3) 0.98050(15) 0.0277(5) Uani 1 d . . .
C8 C 1.4725(3) 0.7813(3) 1.10329(15) 0.0286(5) Uani 1 d . . .
C4 C 0.8964(3) 0.7043(3) 0.87986(17) 0.0316(5) Uani 1 d . . .
H4 H 0.8510 0.7385 0.9343 0.038 Uiso 1 calc R . .
C12 C 1.6525(4) 0.9148(3) 1.1344(2) 0.0430(7) Uani 1 d . . .
H12A H 1.7512 0.8902 1.1021 0.064 Uiso 1 calc R . .
H12B H 1.6960 0.9351 1.2017 0.064 Uiso 1 calc R . .
H12C H 1.6239 1.0031 1.1188 0.064 Uiso 1 calc R . .
C10 C 1.2677(4) 0.7405(3) 1.23194(18) 0.0437(7) Uani 1 d . . .
H10A H 1.1556 0.7604 1.2534 0.066 Uiso 1 calc R . .
H10B H 1.3779 0.7871 1.2821 0.066 Uiso 1 calc R . .
H10C H 1.2509 0.6327 1.2143 0.066 Uiso 1 calc R . .
C2 C 1.1404(4) 0.6329(3) 0.80283(17) 0.0348(6) Uani 1 d . . .
H2 H 1.2623 0.6185 0.8043 0.042 Uiso 1 calc R . .
C7 C 1.2973(3) 0.8062(3) 1.14623(16) 0.0294(5) Uani 1 d . . .
C1 C 1.0156(4) 0.6050(3) 0.71748(17) 0.0357(6) Uani 1 d . . .
H1 H 1.0567 0.5713 0.6617 0.043 Uiso 1 calc R . .
C5 C 0.7833(3) 0.6738(3) 0.79121(17) 0.0320(5) Uani 1 d . . .
H5 H 0.6615 0.6890 0.7874 0.038 Uiso 1 calc R . .
C11 C 1.5196(4) 0.6343(3) 1.11325(19) 0.0404(6) Uani 1 d . . .
H11A H 1.4061 0.5507 1.0896 0.061 Uiso 1 calc R . .
H11B H 1.5655 0.6413 1.1790 0.061 Uiso 1 calc R . .
H11C H 1.6168 0.6181 1.0775 0.061 Uiso 1 calc R . .
C9 C 1.2858(4) 0.9700(3) 1.1672(2) 0.0444(7) Uani 1 d . . .
H9A H 1.3076 1.0111 1.1134 0.067 Uiso 1 calc R . .
H9B H 1.3817 1.0294 1.2218 0.067 Uiso 1 calc R . .
H9C H 1.1609 0.9729 1.1796 0.067 Uiso 1 calc R . .
C3 C 1.0790(3) 0.6832(3) 0.88674(16) 0.0277(5) Uani 1 d . . .
C13 C 0.6310(4) 0.2749(3) 0.4506(2) 0.0438(7) Uani 1 d . . .
C14 C 0.7074(5) 0.1394(4) 0.4231(3) 0.0705(11) Uani 1 d . . .
H14A H 0.6428 0.0815 0.3603 0.106 Uiso 1 calc R . .
H14B H 0.6855 0.0768 0.4672 0.106 Uiso 1 calc R . .
H14C H 0.8427 0.1734 0.4244 0.106 Uiso 1 calc R . .
C15 C 0.1340(5) 0.2435(4) 0.6240(2) 0.0602(9) Uani 1 d . . .
H15A H 0.1338 0.1393 0.6019 0.090 Uiso 1 calc R . .
H15B H 0.0071 0.2536 0.6065 0.090 Uiso 1 calc R . .
H15C H 0.1733 0.2743 0.6919 0.090 Uiso 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'
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
O2 Cu1 O1 89.38(10) . . ?
O2 Cu1 O3 90.68(10) . . ?
O1 Cu1 O3 168.20(8) . . ?
O2 Cu1 O4 168.25(8) . . ?
O1 Cu1 O4 88.74(10) . . ?
O3 Cu1 O4 88.81(10) . . ?
O2 Cu1 N1 96.33(9) . . ?
O1 Cu1 N1 96.19(8) . . ?
O3 Cu1 N1 95.54(8) . . ?
O4 Cu1 N1 95.41(9) . . ?
O2 Cu1 Cu1 83.41(7) . 2_666 ?
O1 Cu1 Cu1 84.56(6) . 2_666 ?
O3 Cu1 Cu1 83.72(6) . 2_666 ?
O4 Cu1 Cu1 84.87(7) . 2_666 ?
N1 Cu1 Cu1 179.21(6) . 2_666 ?
C5 N1 C1 117.5(2) . . ?
C5 N1 Cu1 118.07(16) . . ?
C1 N1 Cu1 123.77(17) . . ?
O5 N4 C6 126.8(2) . . ?
O5 N4 C7 121.89(19) . . ?
C6 N4 C7 110.96(19) . . ?
C16 O2 Cu1 124.3(2) 2_666 . ?
O4 C16 O2 125.2(3) . 2_666 ?
O4 C16 C15 118.1(3) . . ?
O2 C16 C15 116.7(3) 2_666 . ?
C16 O4 Cu1 122.14(18) . . ?
O6 N3 C6 126.88(19) . . ?
O6 N3 C8 121.54(18) . . ?
C6 N3 C8 111.39(19) . . ?
C13 O1 Cu1 122.58(19) 2_666 . ?
C13 O3 Cu1 123.52(18) . . ?
N3 C6 N4 108.87(19) . . ?
N3 C6 C3 125.9(2) . . ?
N4 C6 C3 125.1(2) . . ?
N3 C8 C11 106.30(19) . . ?
N3 C8 C12 109.2(2) . . ?
C11 C8 C12 110.7(2) . . ?
N3 C8 C7 100.49(17) . . ?
C11 C8 C7 113.5(2) . . ?
C12 C8 C7 115.6(2) . . ?
C5 C4 C3 119.0(2) . . ?
C1 C2 C3 118.3(2) . . ?
N4 C7 C9 105.4(2) . . ?
N4 C7 C10 110.4(2) . . ?
C9 C7 C10 110.1(2) . . ?
N4 C7 C8 100.28(18) . . ?
C9 C7 C8 114.5(2) . . ?
C10 C7 C8 115.2(2) . . ?
N1 C1 C2 123.6(2) . . ?
N1 C5 C4 123.4(2) . . ?
C4 C3 C2 118.1(2) . . ?
C4 C3 C6 119.5(2) . . ?
C2 C3 C6 122.4(2) . . ?
O3 C13 O1 125.6(3) . 2_666 ?
O3 C13 C14 116.9(3) . . ?
O1 C13 C14 117.5(3) 2_666 . ?
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 O2 1.960(2) . ?
Cu1 O1 1.964(2) . ?
Cu1 O3 1.966(2) . ?
Cu1 O4 1.971(2) . ?
Cu1 N1 2.173(2) . ?
Cu1 Cu1 2.6236(12) 2_666 ?
N1 C5 1.332(3) . ?
N1 C1 1.333(3) . ?
O6 N3 1.266(3) . ?
N4 O5 1.272(3) . ?
N4 C6 1.351(3) . ?
N4 C7 1.499(3) . ?
O2 C16 1.253(3) 2_666 ?
C16 O4 1.250(3) . ?
C16 O2 1.253(3) 2_666 ?
C16 C15 1.499(4) . ?
N3 C6 1.343(3) . ?
N3 C8 1.507(3) . ?
O1 C13 1.251(3) 2_666 ?
O3 C13 1.249(3) . ?
C6 C3 1.464(3) . ?
C8 C11 1.522(3) . ?
C8 C12 1.523(4) . ?
C8 C7 1.545(3) . ?
C4 C5 1.378(3) . ?
C4 C3 1.388(3) . ?
C10 C7 1.525(3) . ?
C2 C1 1.382(3) . ?
C2 C3 1.395(3) . ?
C7 C9 1.522(4) . ?
C13 O1 1.251(3) 2_666 ?
C13 C14 1.504(4) . ?
