#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:26:17 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179060 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/22/4302202.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_4302202
loop_
_publ_author_name
'Theocharis C. Stamatatos'
'Gina C. Vlahopoulou'
'Catherine P. Raptopoulou'
'Aris Terzis'
'Albert Escuer'
'Spyros P. Perlepes'
_publ_section_title
;
Interpretation of the Magnetic Properties of a Compound Consisting of
Cocrystallized CuII3 and CuII4 Clusters through the Targeted Synthesis and
Study of Its Discrete CuII4 Component
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4610
_journal_page_last               4612
_journal_paper_doi               10.1021/ic900188k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C26 H32 Cu5 N2 O16'
_chemical_formula_weight         946.24
_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                72.00(3)
_cell_angle_beta                 75.60(3)
_cell_angle_gamma                70.83(3)
_cell_formula_units_Z            1
_cell_length_a                   9.577(6)
_cell_length_b                   11.739(8)
_cell_length_c                   7.765(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      5.5
_cell_volume                     773.6(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'θ/2θ scans'
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2388
_diffrn_reflns_theta_full        59.04
_diffrn_reflns_theta_max         59.04
_diffrn_reflns_theta_min         4.12
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.514
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             475
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0771P)²+1.5227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                2170
_reflns_number_total             2198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900188k_si_001_3.cif
_cod_data_source_block           pexs1123
_cod_database_code               4302202
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 0.5000 0.5000 0.5000 0.0204(3) Uani 1 2 d S . .
Cu2 Cu 0.32877(6) 1.02289(5) 0.55089(7) 0.0174(2) Uani 1 1 d . . .
Cu3 Cu 0.51456(6) 0.74333(5) 0.63304(8) 0.0179(2) Uani 1 1 d . . .
O1 O 0.4371(3) 0.4353(3) 0.3437(4) 0.0248(7) Uani 1 1 d . . .
O2 O 0.4862(3) 0.0820(2) 0.3482(3) 0.0165(6) Uani 1 1 d . . .
N1 N 0.3924(3) 0.3094(3) 0.1560(4) 0.0171(7) Uani 1 1 d . . .
O11 O 0.3465(3) 0.6571(3) 0.4288(4) 0.0307(7) Uani 1 1 d . . .
O12 O 0.4158(3) 0.8221(2) 0.4230(4) 0.0230(7) Uani 1 1 d . . .
O21 O 0.1824(3) 0.9687(3) 0.7529(4) 0.0311(7) Uani 1 1 d . . .
O22 O 0.2821(4) 0.7638(3) 0.8103(5) 0.0387(8) Uani 1 1 d . . .
O31 O 0.1689(3) 1.1378(3) 0.4198(4) 0.0258(7) Uani 1 1 d . . .
C1 C 0.3443(5) 0.5094(4) 0.2107(6) 0.0252(10) Uani 1 1 d . . .
C2 C 0.3340(4) 0.4315(4) 0.0926(6) 0.0203(9) Uani 1 1 d . . .
C3 C 0.2700(5) 0.4744(4) -0.0644(6) 0.0293(10) Uani 1 1 d . . .
C4 C 0.2654(5) 0.3889(4) -0.1495(6) 0.0297(10) Uani 1 1 d . . .
C5 C 0.3257(5) 0.2621(4) -0.0799(6) 0.0239(9) Uani 1 1 d . . .
C6 C 0.3921(4) 0.2243(4) 0.0743(5) 0.0186(8) Uani 1 1 d . . .
C7 C 0.4709(5) 0.0927(4) 0.1650(5) 0.0200(9) Uani 1 1 d . . .
C11 C 0.3313(4) 0.7718(4) 0.3884(5) 0.0189(9) Uani 1 1 d . . .
C12 C 0.2021(6) 0.8572(5) 0.2947(8) 0.0396(12) Uani 1 1 d . . .
H12A H 0.1361 0.9094 0.3722 0.051 Uiso 1 1 calc R . .
H12B H 0.1486 0.8087 0.2712 0.051 Uiso 1 1 calc R . .
H12C H 0.2389 0.9081 0.1807 0.051 Uiso 1 1 calc R . .
C21 C 0.1773(5) 0.8562(4) 0.8268(5) 0.0227(9) Uani 1 1 d . . .
C22 C 0.0288(5) 0.8393(4) 0.9369(6) 0.0307(10) Uani 1 1 d . . .
H22A H -0.0362 0.8464 0.8555 0.040 Uiso 1 1 calc R . .
H22B H -0.0161 0.9022 1.0042 0.040 Uiso 1 1 calc R . .
H22C H 0.0440 0.7585 1.0210 0.040 Uiso 1 1 calc R . .
O32 O 0.2189(4) 1.2511(3) 0.5633(5) 0.0388(8) Uani 1 1 d . . .
C31 C 0.1446(4) 1.2395(4) 0.4649(6) 0.0234(9) Uani 1 1 d . . .
C32 C 0.0204(6) 1.3472(5) 0.3871(8) 0.0447(13) Uani 1 1 d . . .
H32A H 0.0389 1.3629 0.2557 0.058 Uiso 1 1 calc R . .
H32B H 0.0167 1.4200 0.4216 0.058 Uiso 1 1 calc R . .
H32C H -0.0736 1.3271 0.4345 0.058 Uiso 1 1 calc R . .
H1A H 0.250(5) 0.548(4) 0.271(6) 0.019(11) Uiso 1 1 d . . .
H1B H 0.385(5) 0.573(5) 0.132(7) 0.030(13) Uiso 1 1 d . . .
H3 H 0.233(6) 0.560(6) -0.105(7) 0.041(14) Uiso 1 1 d . . .
H4 H 0.235(5) 0.415(5) -0.272(7) 0.028(12) Uiso 1 1 d . . .
H5 H 0.321(6) 0.200(5) -0.138(7) 0.041(14) Uiso 1 1 d . . .
H7A H 0.415(5) 0.043(5) 0.178(6) 0.025(12) Uiso 1 1 d . . .
H7B H 0.572(6) 0.074(4) 0.088(6) 0.024(12) Uiso 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
O1 Cu1 O1 180.00(13) 2_666 . ?
O1 Cu1 O11 88.12(12) 2_666 2_666 ?
O1 Cu1 O11 91.88(12) . 2_666 ?
O1 Cu1 O11 91.88(12) 2_666 . ?
O1 Cu1 O11 88.12(12) . . ?
O11 Cu1 O11 180.0(2) 2_666 . ?
O21 Cu2 O31 89.98(14) . . ?
O21 Cu2 O2 99.16(13) . 2_666 ?
O31 Cu2 O2 170.81(12) . 2_666 ?
O21 Cu2 O2 177.10(12) . 1_565 ?
O31 Cu2 O2 91.59(13) . 1_565 ?
O2 Cu2 O2 79.24(12) 2_666 1_565 ?
N1 Cu3 O12 171.17(12) 2_666 . ?
N1 Cu3 O1 83.31(13) 2_666 2_666 ?
O12 Cu3 O1 105.52(12) . 2_666 ?
N1 Cu3 O2 81.29(12) 2_666 2_666 ?
O12 Cu3 O2 89.95(11) . 2_666 ?
O1 Cu3 O2 163.30(11) 2_666 2_666 ?
N1 Cu3 O22 91.30(14) 2_666 . ?
O12 Cu3 O22 87.60(14) . . ?
O1 Cu3 O22 96.89(12) 2_666 . ?
O2 Cu3 O22 89.89(11) 2_666 . ?
C1 O1 Cu1 124.1(2) . . ?
C1 O1 Cu3 113.8(2) . 2_666 ?
Cu1 O1 Cu3 121.91(15) . 2_666 ?
C7 O2 Cu2 121.5(2) . 2_666 ?
C7 O2 Cu2 116.7(2) . 1_545 ?
Cu2 O2 Cu2 100.76(12) 2_666 1_545 ?
C7 O2 Cu3 108.4(2) . 2_666 ?
Cu2 O2 Cu3 100.02(11) 2_666 2_666 ?
Cu2 O2 Cu3 107.73(12) 1_545 2_666 ?
C2 N1 C6 123.1(3) . . ?
C2 N1 Cu3 117.7(3) . 2_666 ?
C6 N1 Cu3 119.2(3) . 2_666 ?
C11 O11 Cu1 139.1(3) . . ?
C11 O12 Cu3 119.9(3) . . ?
C21 O21 Cu2 126.2(3) . . ?
C21 O22 Cu3 131.3(3) . . ?
C31 O31 Cu2 104.0(3) . . ?
O1 C1 C2 110.4(3) . . ?
O1 C1 H1A 109(3) . . ?
C2 C1 H1A 113(3) . . ?
O1 C1 H1B 110(3) . . ?
C2 C1 H1B 107(3) . . ?
H1A C1 H1B 107(4) . . ?
N1 C2 C3 119.6(4) . . ?
N1 C2 C1 113.5(3) . . ?
C3 C2 C1 126.8(4) . . ?
C4 C3 C2 118.6(4) . . ?
C4 C3 H3 125(3) . . ?
C2 C3 H3 117(3) . . ?
C3 C4 C5 120.7(4) . . ?
C3 C4 H4 121(3) . . ?
C5 C4 H4 117(3) . . ?
C6 C5 C4 118.4(4) . . ?
C6 C5 H5 120(3) . . ?
C4 C5 H5 121(3) . . ?
N1 C6 C5 119.5(4) . . ?
N1 C6 C7 113.7(3) . . ?
C5 C6 C7 126.8(4) . . ?
O2 C7 C6 111.4(3) . . ?
O2 C7 H7A 104(3) . . ?
C6 C7 H7A 109(3) . . ?
O2 C7 H7B 110(3) . . ?
C6 C7 H7B 105(3) . . ?
H7A C7 H7B 117(4) . . ?
O11 C11 O12 124.9(4) . . ?
O11 C11 C12 118.2(4) . . ?
O12 C11 C12 116.9(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O22 C21 O21 124.8(4) . . ?
O22 C21 C22 119.2(4) . . ?
O21 C21 C22 116.0(4) . . ?
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 . . ?
O32 C31 O31 122.6(4) . . ?
O32 C31 C32 121.0(4) . . ?
O31 C31 C32 116.3(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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 O1 1.909(3) 2_666 ?
Cu1 O1 1.909(3) . ?
Cu1 O11 1.965(3) 2_666 ?
Cu1 O11 1.965(3) . ?
Cu2 O21 1.925(3) . ?
Cu2 O31 1.942(3) . ?
Cu2 O2 1.983(3) 2_666 ?
Cu2 O2 2.016(3) 1_565 ?
Cu3 N1 1.897(3) 2_666 ?
Cu3 O12 1.916(3) . ?
Cu3 O1 1.953(3) 2_666 ?
Cu3 O2 2.098(3) 2_666 ?
Cu3 O22 2.289(3) . ?
O1 C1 1.417(5) . ?
O1 Cu3 1.953(3) 2_666 ?
O2 C7 1.429(5) . ?
O2 Cu2 1.983(3) 2_666 ?
O2 Cu2 2.016(3) 1_545 ?
O2 Cu3 2.098(3) 2_666 ?
N1 C2 1.335(5) . ?
N1 C6 1.340(5) . ?
N1 Cu3 1.897(3) 2_666 ?
O11 C11 1.252(5) . ?
O12 C11 1.263(5) . ?
O21 C21 1.279(5) . ?
O22 C21 1.228(5) . ?
O31 C31 1.280(5) . ?
C1 C2 1.519(6) . ?
C1 H1A 0.94(5) . ?
C1 H1B 0.94(5) . ?
C2 C3 1.381(6) . ?
C3 C4 1.377(7) . ?
C3 H3 0.93(6) . ?
C4 C5 1.391(7) . ?
C4 H4 0.99(5) . ?
C5 C6 1.379(6) . ?
C5 H5 0.99(6) . ?
C6 C7 1.509(6) . ?
C7 H7A 0.88(5) . ?
C7 H7B 1.00(5) . ?
C11 C12 1.499(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C21 C22 1.506(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O32 C31 1.227(5) . ?
C31 C32 1.509(6) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
