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#$Date: 2016-03-24 02:50:32 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179599 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/63/4506337.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_4506337
loop_
_publ_author_name
'Pérez-Yáñez, Sonia'
'Beobide, Garikoitz'
'Castillo, Oscar'
'Cepeda, Javier'
'Luque, Antonio'
'Román, Pascual'
_publ_contact_author
;
 Oscar Castillo. Departamento de Quimica Inorganica. 
 Facultad de Ciencia y Tecnologia
 Universidad del Pais Vasco,  Apdo. 644,
 E-48080 Bilbao, Spain
;
_publ_section_title
;
 Directing the Formation of Adenine Coordination Polymers from Tunable
 Copper(II)/Dicarboxylato/Adenine Paddle-Wheel Building Units
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3324
_journal_paper_doi               10.1021/cg300446d
_journal_volume                  12
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H26 Cu2 N10 O8'
_chemical_formula_structural     'C22 H26 Cu2 N10 O8'
_chemical_formula_sum            'C22 H26 Cu2 N10 O8'
_chemical_formula_weight         685.62
_chemical_name_systematic
;
poly-[(mu-adipato-K2-O,O')(mu3-adeninato-k3-N3:N7:N9)copper(II)]
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.688(1)
_cell_length_b                   14.688(1)
_cell_length_c                   24.331(3)
_cell_measurement_reflns_used    9502
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.17
_cell_measurement_theta_min      2.58
_cell_volume                     5249.1(8)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'IPDS IT'
_diffrn_measurement_method       ω
_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  0.1155
_diffrn_reflns_av_sigmaI/netI    0.1663
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7184
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
X-RED; Stoe & Cie, 2001
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      1.66(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0606
_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)+(0.0210P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                1256
_reflns_number_total             2577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300446d_si_002.cif
_cod_data_source_block           "'compound2'"
_cod_original_cell_volume        5248.9(9)
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               4506337
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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 0.04537(6) 0.01966(6) 0.55097(3) 0.0347(2) Uani 1 1 d . . .
N1 N -0.3082(4) 0.0911(5) 0.4925(3) 0.0543(18) Uani 1 1 d . . .
C2 C -0.2380(6) 0.0555(5) 0.4654(4) 0.055(2) Uani 1 1 d . B .
H2 H -0.2490 0.0355 0.4297 0.066 Uiso 1 1 calc R A 2
N3 N -0.1520(4) 0.0456(4) 0.4846(3) 0.0429(15) Uani 1 1 d . . .
C4 C -0.1450(5) 0.0775(5) 0.5375(4) 0.047(2) Uani 1 1 d . B .
C5 C -0.2139(8) 0.1182(7) 0.5719(4) 0.036(2) Uani 0.71 1 d P B 1
C6 C -0.2996(7) 0.1261(7) 0.5481(5) 0.034(2) Uani 0.71 1 d P B 1
N6 N -0.3723(8) 0.1579(7) 0.5755(4) 0.045(3) Uiso 0.71 1 d P B 1
H6A H -0.3669 0.1744 0.6093 0.054 Uiso 0.71 1 calc PR B 1
H6B H -0.4242 0.1618 0.5593 0.054 Uiso 0.71 1 calc PR B 1
C5B C -0.2487(19) 0.1032(18) 0.5287(11) 0.037(6) Uani 0.29 1 d P B 2
C6B C -0.270(2) 0.1404(18) 0.5783(12) 0.034(6) Uani 0.29 1 d P B 2
N6B N -0.3561(19) 0.1900(19) 0.5799(11) 0.051(8) Uiso 0.29 1 d P B 2
H6B1 H -0.3892 0.1938 0.5509 0.061 Uiso 0.29 1 calc PR B 2
H6B2 H -0.3738 0.2154 0.6099 0.061 Uiso 0.29 1 calc PR B 2
N7 N -0.1873(5) 0.1394(5) 0.6229(2) 0.0530(18) Uani 1 1 d . . .
C8 C -0.1000(7) 0.1119(6) 0.6185(4) 0.061(2) Uani 1 1 d . B .
H8 H -0.0599 0.1173 0.6479 0.074 Uiso 1 1 calc R C 1
N9 N -0.0728(5) 0.0763(4) 0.5701(3) 0.0457(17) Uani 1 1 d . . .
O11 O 0.0838(3) 0.1294(3) 0.50933(19) 0.0417(12) Uani 1 1 d . . .
O12 O 0.0117(4) 0.0982(4) 0.4303(2) 0.0455(13) Uani 1 1 d . . .
C11 C 0.0686(5) 0.1441(5) 0.4594(3) 0.0377(16) Uani 1 1 d . B .
C12 C 0.1245(5) 0.2156(5) 0.4303(3) 0.049(2) Uani 1 1 d . . .
H12A H 0.0908 0.2380 0.3988 0.059 Uiso 1 1 calc R B .
H12B H 0.1348 0.2664 0.4550 0.059 Uiso 1 1 calc R . .
C13 C 0.2138(5) 0.1789(7) 0.4116(3) 0.060(2) Uani 1 1 d . B .
H13A H 0.2385 0.2210 0.3847 0.072 Uiso 1 1 calc R . .
H13B H 0.2024 0.1219 0.3927 0.072 Uiso 1 1 calc R . .
C14 C 0.2870(6) 0.1619(5) 0.4549(3) 0.054(2) Uani 1 1 d . . .
H14A H 0.2985 0.2184 0.4743 0.065 Uiso 1 1 calc R B .
H14B H 0.2638 0.1183 0.4814 0.065 Uiso 1 1 calc R . .
C15 C 0.3749(5) 0.1271(7) 0.4325(3) 0.063(2) Uani 1 1 d . B .
H15A H 0.3648 0.0653 0.4198 0.076 Uiso 1 1 calc R . .
H15B H 0.3901 0.1634 0.4005 0.076 Uiso 1 1 calc R . .
C16 C 0.4551(5) 0.1261(6) 0.4689(3) 0.0500(19) Uani 1 1 d . . .
O21 O 0.4558(5) 0.1453(6) 0.5169(3) 0.099(3) Uani 1 1 d . B .
O22 O 0.5297(4) 0.1006(7) 0.4429(3) 0.094(2) Uani 1 1 d . B .
H22 H 0.5743 0.1114 0.4622 0.141 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'
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
O12 Cu1 N9 86.7(3) 9_556 .
O12 Cu1 O11 161.6(2) 9_556 .
N9 Cu1 O11 91.6(2) . .
O12 Cu1 N3 90.7(2) 9_556 9_556
N9 Cu1 N3 167.1(2) . 9_556
O11 Cu1 N3 87.0(2) . 9_556
O12 Cu1 N7 104.2(2) 9_556 16_556
N9 Cu1 N7 93.7(3) . 16_556
O11 Cu1 N7 94.2(2) . 16_556
N3 Cu1 N7 99.2(3) 9_556 16_556
O12 Cu1 Cu1 79.99(15) 9_556 9_556
N9 Cu1 Cu1 83.15(19) . 9_556
O11 Cu1 Cu1 81.63(14) . 9_556
N3 Cu1 Cu1 83.97(17) 9_556 9_556
N7 Cu1 Cu1 174.6(2) 16_556 9_556
C5B N1 C2 82.2(15) . .
C2 N1 C6 122.2(7) . .
N1 C2 N3 126.4(8) . .
N1 C2 H2 116.8 . .
N3 C2 H2 116.8 . .
C5B C2 H2 163.6 . .
C2 N3 C4 111.0(7) . .
C2 N3 Cu1 128.5(6) . 9_556
C4 N3 Cu1 120.1(5) . 9_556
C5B N3 Cu1 172.2(8) . 9_556
N9 C4 N3 128.1(6) . .
N9 C4 C5 102.7(8) . .
N3 C4 C5 129.2(8) . .
N9 C4 C5B 148.7(12) . .
N3 C4 C5B 83.2(12) . .
N7 C5 C6 129.2(12) . .
N7 C5 C4 115.5(10) . .
C6 C5 C4 115.3(10) . .
C6 C5 C8 170.4(10) . .
N6 C6 C5 122.8(12) . .
N6 C6 N1 121.1(10) . .
C5 C6 N1 115.9(10) . .
C6 N6 H6A 120.0 . .
C6 N6 H6B 120.0 . .
H6A N6 H6B 120.0 . .
N1 C5B C6B 122(3) . .
N1 C5B C4 137(2) . .
C6B C5B C4 101(2) . .
C6B C5B C2 172(3) . .
C6B C5B N3 145(2) . .
N6B C6B C5B 115(3) . .
N6B C6B N7 129(2) . .
C5B C6B N7 115(3) . .
C6B N6B H6B1 120.0 . .
C6B N6B H6B2 120.0 . .
H6B1 N6B H6B2 120.0 . .
C5 N7 C8 97.7(8) . .
C8 N7 C6B 131.1(12) . .
C5 N7 Cu1 143.7(7) . 15_556
C8 N7 Cu1 118.4(5) . 15_556
C6B N7 Cu1 110.3(11) . 15_556
N7 C8 N9 117.9(8) . .
N7 C8 H8 121.1 . .
N9 C8 H8 121.1 . .
C5 C8 H8 162.0 . .
C4 N9 C8 106.3(7) . .
C4 N9 Cu1 124.5(5) . .
C8 N9 Cu1 128.9(6) . .
C11 O11 Cu1 125.7(5) . .
C11 O12 Cu1 127.4(4) . 9_556
O11 C11 O12 124.0(6) . .
O11 C11 C12 118.6(7) . .
O12 C11 C12 117.3(6) . .
C13 C12 C11 111.8(6) . .
C13 C12 H12A 109.3 . .
C11 C12 H12A 109.3 . .
C13 C12 H12B 109.3 . .
C11 C12 H12B 109.3 . .
H12A C12 H12B 107.9 . .
C12 C13 C14 117.9(7) . .
C12 C13 H13A 107.8 . .
C14 C13 H13A 107.8 . .
C12 C13 H13B 107.8 . .
C14 C13 H13B 107.8 . .
H13A C13 H13B 107.2 . .
C15 C14 C13 114.4(7) . .
C15 C14 H14A 108.7 . .
C13 C14 H14A 108.7 . .
C15 C14 H14B 108.7 . .
C13 C14 H14B 108.7 . .
H14A C14 H14B 107.6 . .
C16 C15 C14 118.4(7) . .
C16 C15 H15A 107.7 . .
C14 C15 H15A 107.7 . .
C16 C15 H15B 107.7 . .
C14 C15 H15B 107.7 . .
H15A C15 H15B 107.1 . .
O21 C16 O22 121.8(8) . .
O21 C16 C15 126.0(8) . .
O22 C16 C15 112.2(7) . .
C16 O22 H22 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O12 1.977(5) 9_556
Cu1 N9 1.980(7) .
Cu1 O11 1.986(5) .
Cu1 N3 2.030(6) 9_556
Cu1 N7 2.179(6) 16_556
Cu1 Cu1 2.875(2) 9_556
N1 C5B 1.25(2) .
N1 C2 1.331(10) .
N1 C6 1.453(14) .
C2 N3 1.354(9) .
C2 C5B 1.70(3) .
C2 H2 0.9300 .
N3 C4 1.374(10) .
N3 C5B 1.97(3) .
C4 N9 1.324(10) .
C4 C5 1.443(13) .
C4 C5B 1.58(3) .
C5 N7 1.337(11) .
C5 C6 1.391(14) .
C5 C8 2.022(16) .
C6 N6 1.343(15) .
N6 H6A 0.8600 .
N6 H6B 0.8600 .
C5B C6B 1.36(4) .
C6B N6B 1.47(4) .
C6B N7 1.63(3) .
N6B H6B1 0.8600 .
N6B H6B2 0.8600 .
N7 C8 1.348(11) .
C8 N9 1.349(9) .
C8 H8 0.9300 .
O11 C11 1.253(7) .
O12 C11 1.286(8) .
C11 C12 1.510(10) .
C12 C13 1.489(11) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.526(11) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.492(11) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.475(11) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 O21 1.200(9) .
C16 O22 1.320(9) .
O22 H22 0.8200 .
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
N6 H6A O12 0.86 2.17 2.99(2) 159.8 3_455
N6 H6B O21 0.86 2.06 2.91(2) 169.0 1_455
N6B H6B2 O12 0.86 1.88 2.66(3) 150.4 3_455
N6B H6B1 O21 0.86 2.52 3.23(3) 139.5 1_455
O22 H22 N1 0.82 1.90 2.673(8) 156.4 1_655
