#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:44:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179762 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/58/7005827.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_7005827
loop_
_publ_author_name
'Boudalis, Athanassios K.'
'Raptopoulou, Catherine P.'
'Psycharis, Vassilis'
'Sanakis, Yiannis'
'Abarca, Belén'
'Ballesteros, Rafael'
'Chadlaoui, Mimoun'
_publ_section_title
;
 An "S"-shaped pentanuclear CuII cluster derived from the
 metal-assisted hydrolysis of pyCOpyCOpy: structural, magnetic and
 spectroscopic studies.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3582
_journal_page_last               3589
_journal_paper_doi               10.1039/b705962k
_journal_year                    2007
_chemical_formula_sum            'C46 H52 Cu5 N6 O24'
_chemical_formula_weight         1390.64
_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                100.09(4)
_cell_angle_beta                 110.70(3)
_cell_angle_gamma                95.96(3)
_cell_formula_units_Z            1
_cell_length_a                   13.108(12)
_cell_length_b                   10.539(9)
_cell_length_c                   10.636(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      11
_cell_volume                     1331(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'P21 Nicolet upgraded by Crystal Logic'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3850
_diffrn_reflns_theta_full        59.12
_diffrn_reflns_theta_max         59.12
_diffrn_reflns_theta_min         3.66
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.994
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             707
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.740
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         3850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0737
_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)+(0.1179P)²+4.3757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                3305
_reflns_number_total             3850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b705962k.txt
_cod_data_source_block           tb515b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005827
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.5000 0.5000 0.0401(4) Uani 1 2 d S . .
Cu2 Cu 0.09398(9) 0.37245(9) 0.24495(11) 0.0383(4) Uani 1 1 d . . .
Cu3 Cu 0.24882(9) 0.17781(11) 0.25058(13) 0.0465(4) Uani 1 1 d . . .
O1 O 0.0129(4) 0.4986(4) 0.3182(5) 0.0391(12) Uani 1 1 d . . .
O3 O 0.1711(4) 0.2858(4) 0.1293(5) 0.0379(12) Uani 1 1 d . . .
N1 N 0.1192(5) 0.6539(6) 0.5585(7) 0.0412(15) Uani 1 1 d . . .
N2 N 0.1443(5) 0.5220(6) 0.1896(7) 0.0383(14) Uani 1 1 d . . .
N3 N 0.3806(5) 0.3054(6) 0.2725(7) 0.0458(16) Uani 1 1 d . . .
O11 O -0.0009(4) 0.2126(5) 0.2272(6) 0.0452(13) Uani 1 1 d . . .
O12 O 0.1085(5) 0.0632(5) 0.2151(7) 0.0577(16) Uani 1 1 d . . .
O13 O 0.1388(6) 0.3621(6) 0.5669(7) 0.0640(17) Uani 1 1 d . . .
O14 O 0.2247(4) 0.3296(5) 0.4247(6) 0.0495(14) Uani 1 1 d . . .
O15 O 0.3321(5) 0.0563(6) 0.3444(7) 0.0622(17) Uani 1 1 d . . .
O16 O 0.3459(7) -0.0225(7) 0.1463(9) 0.085(2) Uani 1 1 d . . .
C1 C 0.1873(7) 0.7071(8) 0.6870(10) 0.051(2) Uani 1 1 d . . .
H1 H 0.1807 0.6703 0.7578 0.067 Uiso 1 1 calc R . .
C2 C 0.2687(8) 0.8170(9) 0.7193(10) 0.061(2) Uani 1 1 d . . .
H2 H 0.3193 0.8504 0.8094 0.079 Uiso 1 1 calc R . .
C3 C 0.2720(8) 0.8738(8) 0.6155(11) 0.061(2) Uani 1 1 d . . .
H3 H 0.3221 0.9508 0.6354 0.080 Uiso 1 1 calc R . .
C4 C 0.2023(7) 0.8188(8) 0.4817(10) 0.054(2) Uani 1 1 d . . .
H4 H 0.2057 0.8566 0.4102 0.070 Uiso 1 1 calc R . .
C5 C 0.1260(6) 0.7050(7) 0.4548(9) 0.0416(18) Uani 1 1 d . . .
C6 C 0.0453(6) 0.6298(7) 0.3117(8) 0.0401(18) Uani 1 1 d . . .
O2 O -0.0480(4) 0.6913(5) 0.2661(6) 0.0425(13) Uani 1 1 d . . .
HO2 H -0.069(8) 0.695(10) 0.321(10) 0.055 Uiso 1 1 d . . .
C7 C 0.0995(6) 0.6277(7) 0.2076(8) 0.0387(17) Uani 1 1 d . . .
C8 C 0.1072(7) 0.7244(8) 0.1333(9) 0.0470(19) Uani 1 1 d . . .
H8 H 0.0759 0.7987 0.1446 0.061 Uiso 1 1 calc R . .
C9 C 0.1611(7) 0.7075(7) 0.0450(9) 0.048(2) Uani 1 1 d . . .
H9 H 0.1679 0.7719 -0.0026 0.063 Uiso 1 1 calc R . .
C10 C 0.2065(7) 0.5946(8) 0.0243(9) 0.0471(19) Uani 1 1 d . . .
H10 H 0.2423 0.5813 -0.0372 0.061 Uiso 1 1 calc R . .
C11 C 0.1949(6) 0.5023(7) 0.1024(8) 0.0419(18) Uani 1 1 d . . .
C12 C 0.2364(6) 0.3711(7) 0.0918(9) 0.0440(19) Uani 1 1 d . . .
O4 O 0.2342(5) 0.3238(5) -0.0399(6) 0.0471(13) Uani 1 1 d . . .
HO4 H 0.160(8) 0.321(9) -0.106(10) 0.061 Uiso 1 1 d . . .
C13 C 0.3581(7) 0.3892(7) 0.1907(9) 0.048(2) Uani 1 1 d . . .
C14 C 0.4414(7) 0.4842(10) 0.1910(12) 0.067(3) Uani 1 1 d . . .
H14 H 0.4258 0.5407 0.1313 0.087 Uiso 1 1 calc R . .
C15 C 0.5468(8) 0.4901(11) 0.2830(15) 0.094(4) Uani 1 1 d . . .
H15 H 0.6035 0.5534 0.2868 0.123 Uiso 1 1 calc R . .
C16 C 0.5712(8) 0.4069(10) 0.3687(13) 0.076(3) Uani 1 1 d . . .
H16 H 0.6433 0.4113 0.4299 0.098 Uiso 1 1 calc R . .
C17 C 0.4839(7) 0.3144(9) 0.3613(11) 0.064(3) Uani 1 1 d . . .
H17 H 0.4982 0.2571 0.4202 0.083 Uiso 1 1 calc R . .
C21 C 0.0203(8) 0.0981(8) 0.2096(10) 0.056(2) Uani 1 1 d . . .
C22 C -0.0787(8) -0.0106(8) 0.1726(16) 0.088(4) Uani 1 1 d . . .
H22A H -0.1451 0.0158 0.1180 0.114 Uiso 1 1 calc R . .
H22B H -0.0852 -0.0271 0.2557 0.114 Uiso 1 1 calc R . .
H22C H -0.0681 -0.0889 0.1209 0.114 Uiso 1 1 calc R . .
C23 C 0.1975(8) 0.3046(8) 0.5221(9) 0.050(2) Uani 1 1 d . . .
C24 C 0.2429(12) 0.1945(12) 0.5865(13) 0.087(4) Uani 1 1 d . . .
H24A H 0.2948 0.1636 0.5488 0.113 Uiso 1 1 calc R . .
H24B H 0.1831 0.1239 0.5669 0.113 Uiso 1 1 calc R . .
H24C H 0.2797 0.2263 0.6846 0.113 Uiso 1 1 calc R . .
C25 C 0.3630(7) -0.0243(8) 0.2692(11) 0.056(2) Uani 1 1 d . . .
C26 C 0.4219(9) -0.1245(10) 0.3352(14) 0.082(3) Uani 1 1 d . . .
H26A H 0.4630 -0.0875 0.4317 0.106 Uiso 1 1 calc R . .
H26B H 0.4719 -0.1507 0.2920 0.106 Uiso 1 1 calc R . .
H26C H 0.3686 -0.1996 0.3240 0.106 Uiso 1 1 calc R . .
OW1 O 0.3712(7) 0.1251(8) 0.9563(10) 0.092(2) Uani 1 1 d . . .
OW2 O 0.5769(9) 0.2416(11) 0.9767(12) 0.125(3) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
N1 Cu1 N1 180.0(3) . 2_566 ?
N1 Cu1 O1 81.3(2) . . ?
N1 Cu1 O1 98.7(2) 2_566 . ?
N1 Cu1 O1 98.7(2) . 2_566 ?
N1 Cu1 O1 81.3(2) 2_566 2_566 ?
O1 Cu1 O1 180.000(1) . 2_566 ?
N1 Cu1 O13 90.2(3) . 2_566 ?
N1 Cu1 O13 89.8(3) 2_566 2_566 ?
O1 Cu1 O13 86.4(2) . 2_566 ?
O1 Cu1 O13 93.6(2) 2_566 2_566 ?
N1 Cu1 O13 89.8(3) . . ?
N1 Cu1 O13 90.2(3) 2_566 . ?
O1 Cu1 O13 93.6(2) . . ?
O1 Cu1 O13 86.4(2) 2_566 . ?
O13 Cu1 O13 180.000(1) 2_566 . ?
N2 Cu2 O11 156.8(3) . . ?
N2 Cu2 O1 81.9(2) . . ?
O11 Cu2 O1 98.0(2) . . ?
N2 Cu2 O3 81.2(2) . . ?
O11 Cu2 O3 94.3(2) . . ?
O1 Cu2 O3 161.1(2) . . ?
N2 Cu2 O14 112.4(2) . . ?
O11 Cu2 O14 89.8(2) . . ?
O1 Cu2 O14 107.7(2) . . ?
O3 Cu2 O14 86.5(2) . . ?
N2 Cu2 Cu3 109.63(19) . . ?
O11 Cu2 Cu3 78.89(17) . . ?
O1 Cu2 Cu3 157.76(16) . . ?
O3 Cu2 Cu3 39.62(14) . . ?
O14 Cu2 Cu3 50.66(16) . . ?
O15 Cu3 O3 170.1(3) . . ?
O15 Cu3 O12 90.4(3) . . ?
O3 Cu3 O12 91.4(2) . . ?
O15 Cu3 N3 96.1(3) . . ?
O3 Cu3 N3 82.1(2) . . ?
O12 Cu3 N3 173.5(2) . . ?
O15 Cu3 O14 105.6(3) . . ?
O3 Cu3 O14 84.1(2) . . ?
O12 Cu3 O14 91.5(2) . . ?
N3 Cu3 O14 87.7(2) . . ?
O15 Cu3 Cu2 148.7(2) . . ?
O3 Cu3 Cu2 40.99(16) . . ?
O12 Cu3 Cu2 78.09(17) . . ?
N3 Cu3 Cu2 96.77(19) . . ?
O14 Cu3 Cu2 46.77(14) . . ?
C6 O1 Cu1 108.9(4) . . ?
C6 O1 Cu2 112.9(5) . . ?
Cu1 O1 Cu2 120.8(2) . . ?
C12 O3 Cu3 116.1(4) . . ?
C12 O3 Cu2 114.8(4) . . ?
Cu3 O3 Cu2 99.4(2) . . ?
C1 N1 C5 120.5(7) . . ?
C1 N1 Cu1 125.5(6) . . ?
C5 N1 Cu1 113.9(5) . . ?
C11 N2 C7 122.3(6) . . ?
C11 N2 Cu2 117.2(5) . . ?
C7 N2 Cu2 117.5(5) . . ?
C13 N3 C17 119.7(8) . . ?
C13 N3 Cu3 114.2(5) . . ?
C17 N3 Cu3 126.1(6) . . ?
C21 O11 Cu2 126.8(6) . . ?
C21 O12 Cu3 126.6(5) . . ?
C23 O13 Cu1 140.0(6) . . ?
C23 O14 Cu2 117.5(5) . . ?
C23 O14 Cu3 127.1(5) . . ?
Cu2 O14 Cu3 82.6(2) . . ?
C25 O15 Cu3 114.4(6) . . ?
N1 C1 C2 121.7(9) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 118.0(9) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 120.7(8) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 118.6(9) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 120.2(8) . . ?
N1 C5 C6 114.7(6) . . ?
C4 C5 C6 125.1(8) . . ?
O2 C6 O1 111.1(6) . . ?
O2 C6 C7 107.1(6) . . ?
O1 C6 C7 108.9(6) . . ?
O2 C6 C5 110.5(6) . . ?
O1 C6 C5 108.5(6) . . ?
C7 C6 C5 110.8(6) . . ?
C6 O2 HO2 104(8) . . ?
N2 C7 C8 119.6(7) . . ?
N2 C7 C6 113.5(6) . . ?
C8 C7 C6 126.9(6) . . ?
C9 C8 C7 119.1(7) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 121.2(7) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C10 C11 116.1(8) . . ?
C9 C10 H10 122.0 . . ?
C11 C10 H10 122.0 . . ?
N2 C11 C10 121.6(7) . . ?
N2 C11 C12 114.3(6) . . ?
C10 C11 C12 124.0(7) . . ?
O3 C12 O4 112.6(6) . . ?
O3 C12 C11 107.2(6) . . ?
O4 C12 C11 111.2(6) . . ?
O3 C12 C13 109.4(6) . . ?
O4 C12 C13 106.1(7) . . ?
C11 C12 C13 110.4(6) . . ?
C12 O4 HO4 109(6) . . ?
N3 C13 C14 121.8(8) . . ?
N3 C13 C12 115.8(7) . . ?
C14 C13 C12 122.4(8) . . ?
C15 C14 C13 117.0(10) . . ?
C15 C14 H14 121.5 . . ?
C13 C14 H14 121.5 . . ?
C16 C15 C14 122.2(10) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C15 C16 C17 117.3(9) . . ?
C15 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
N3 C17 C16 122.0(9) . . ?
N3 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
O12 C21 O11 129.0(8) . . ?
O12 C21 C22 116.5(7) . . ?
O11 C21 C22 114.5(8) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O13 C23 O14 124.6(8) . . ?
O13 C23 C24 118.0(9) . . ?
O14 C23 C24 117.5(8) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O16 C25 O15 122.7(8) . . ?
O16 C25 C26 121.1(10) . . ?
O15 C25 C26 116.2(10) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
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 N1 1.972(7) . ?
Cu1 N1 1.972(7) 2_566 ?
Cu1 O1 1.997(6) . ?
Cu1 O1 1.997(6) 2_566 ?
Cu1 O13 2.435(6) 2_566 ?
Cu1 O13 2.435(6) . ?
Cu2 N2 1.910(6) . ?
Cu2 O11 1.926(5) . ?
Cu2 O1 2.005(5) . ?
Cu2 O3 2.011(5) . ?
Cu2 O14 2.223(6) . ?
Cu2 Cu3 3.025(2) . ?
Cu3 O15 1.949(6) . ?
Cu3 O3 1.956(5) . ?
Cu3 O12 1.968(6) . ?
Cu3 N3 1.993(7) . ?
Cu3 O14 2.360(6) . ?
O1 C6 1.425(8) . ?
O3 C12 1.381(9) . ?
N1 C1 1.321(11) . ?
N1 C5 1.335(10) . ?
N2 C11 1.319(10) . ?
N2 C7 1.327(9) . ?
N3 C13 1.328(11) . ?
N3 C17 1.331(11) . ?
O11 C21 1.263(9) . ?
O12 C21 1.235(10) . ?
O13 C23 1.200(10) . ?
O14 C23 1.267(11) . ?
O15 C25 1.260(12) . ?
O16 C25 1.250(12) . ?
C1 C2 1.394(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.356(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.397(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.525(11) . ?
C6 O2 1.416(9) . ?
C6 C7 1.511(11) . ?
O2 HO2 0.73(9) . ?
C7 C8 1.411(11) . ?
C8 C9 1.359(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.402(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.415(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.538(10) . ?
C12 O4 1.392(10) . ?
C12 C13 1.539(11) . ?
O4 HO4 0.97(10) . ?
C13 C14 1.402(12) . ?
C14 C15 1.370(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.354(16) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(14) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C21 C22 1.524(12) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.518(13) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.501(13) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
