#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:50:32 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179599 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/63/4506338.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_4506338
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         'C24 H30 Cu2 N10 O8'
_chemical_formula_structural     'C24 H30 Cu2 N10 O8'
_chemical_formula_sum            'C24 H30 Cu2 N10 O8'
_chemical_formula_weight         713.66
_chemical_name_systematic
;
poly-[(mu-pimelato-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                   15.6854(5)
_cell_length_b                   15.6854(5)
_cell_length_c                   23.2536(9)
_cell_measurement_reflns_used    17962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.93
_cell_volume                     5721.1(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17962
_diffrn_reflns_theta_full        26.77
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.554
_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    1.657
_exptl_crystal_density_meas      1.66(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3048
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0601
_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)+(0.0557P)²+19.4945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                2294
_reflns_number_total             3048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300446d_si_002.cif
_cod_data_source_block           "'compound3'"
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               4506338
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 0.04027(3) 0.02577(4) 0.55249(2) 0.03964(19) Uani 1 1 d . . .
N1 N -0.2870(3) 0.0811(3) 0.4849(2) 0.0548(11) Uani 1 1 d . . .
C2 C -0.2215(3) 0.0440(4) 0.4592(3) 0.0630(16) Uani 1 1 d . B .
H2 H -0.2315 0.0193 0.4235 0.076 Uiso 1 1 calc R A 2
N3 N -0.1416(2) 0.0390(3) 0.4800(2) 0.0510(11) Uani 1 1 d . . .
C4 C -0.1387(3) 0.0768(3) 0.5329(3) 0.0541(14) Uani 1 1 d . B .
C5 C -0.2016(5) 0.1209(4) 0.5672(3) 0.0346(14) Uani 0.671(4) 1 d P B 1
C6 C -0.2811(5) 0.1233(5) 0.5416(4) 0.0387(15) Uani 0.671(4) 1 d P B 1
N6 N -0.3509(8) 0.1601(9) 0.5657(6) 0.045(2) Uani 0.671(4) 1 d P B 1
H6A H -0.3472 0.1837 0.5990 0.054 Uiso 0.671(4) 1 calc PR B 1
H6B H -0.3988 0.1596 0.5478 0.054 Uiso 0.671(4) 1 calc PR B 1
C5B C -0.2330(8) 0.0946(8) 0.5244(5) 0.028(3) Uani 0.329(4) 1 d P B 2
C6B C -0.2585(9) 0.1404(8) 0.5735(6) 0.029(3) Uani 0.329(4) 1 d P B 2
N6B N -0.3330(17) 0.172(2) 0.5801(13) 0.056(6) Uani 0.329(4) 1 d P B 2
H6B1 H -0.3708 0.1652 0.5536 0.067 Uiso 0.329(4) 1 calc PR B 2
H6B2 H -0.3455 0.1992 0.6109 0.067 Uiso 0.329(4) 1 calc PR B 2
N7 N -0.1792(3) 0.1484(3) 0.61867(18) 0.0600(12) Uani 1 1 d . . .
C8 C -0.0988(4) 0.1222(4) 0.6158(3) 0.0693(17) Uani 1 1 d . B .
H8 H -0.0616 0.1314 0.6462 0.083 Uiso 1 1 calc R C 1
N9 N -0.0719(3) 0.0815(3) 0.56714(18) 0.0505(10) Uani 1 1 d . . .
O11 O 0.0758(2) 0.1238(2) 0.50437(15) 0.0502(8) Uani 1 1 d . . .
O12 O 0.0133(2) 0.0843(2) 0.42290(14) 0.0473(8) Uani 1 1 d . . .
C11 C 0.0616(3) 0.1315(3) 0.4515(2) 0.0426(10) Uani 1 1 d . B .
C12 C 0.1068(3) 0.2031(3) 0.4203(3) 0.0565(14) Uani 1 1 d . . .
H12A H 0.1090 0.1897 0.3796 0.068 Uiso 1 1 calc R B .
H12B H 0.0740 0.2551 0.4248 0.068 Uiso 1 1 calc R . .
C13 C 0.1963(3) 0.2185(3) 0.4417(3) 0.0554(13) Uani 1 1 d . B .
H13A H 0.1940 0.2327 0.4823 0.066 Uiso 1 1 calc R . .
H13B H 0.2201 0.2670 0.4215 0.066 Uiso 1 1 calc R . .
C14 C 0.2548(3) 0.1424(3) 0.4336(2) 0.0479(12) Uani 1 1 d . . .
H14A H 0.2581 0.1285 0.3930 0.057 Uiso 1 1 calc R B .
H14B H 0.2312 0.0935 0.4535 0.057 Uiso 1 1 calc R . .
C15 C 0.3442(3) 0.1603(4) 0.4564(3) 0.0551(13) Uani 1 1 d . B .
H15A H 0.3636 0.2148 0.4416 0.066 Uiso 1 1 calc R . .
H15B H 0.3420 0.1644 0.4980 0.066 Uiso 1 1 calc R . .
C16 C 0.4069(3) 0.0925(4) 0.4398(3) 0.0558(13) Uani 1 1 d . . .
H16A H 0.4130 0.0922 0.3983 0.067 Uiso 1 1 calc R B .
H16B H 0.3846 0.0374 0.4513 0.067 Uiso 1 1 calc R . .
C17 C 0.4941(3) 0.1050(4) 0.4669(3) 0.0573(14) Uani 1 1 d . B .
O22 O 0.5551(3) 0.0733(5) 0.4405(2) 0.115(2) Uani 1 1 d . . .
O21 O 0.5038(4) 0.1366(7) 0.5106(4) 0.207(5) Uani 1 1 d . . .
H22 H 0.6180 0.0827 0.4555 0.050 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 0.0033 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
O11 Cu1 N9 90.27(16) . .
O11 Cu1 O12 161.41(14) . 9_556
N9 Cu1 O12 87.65(16) . 9_556
O11 Cu1 N3 87.57(15) . 9_556
N9 Cu1 N3 166.61(18) . 9_556
O12 Cu1 N3 90.20(15) 9_556 9_556
O11 Cu1 N7 95.68(17) . 16_556
N9 Cu1 N7 95.93(18) . 16_556
O12 Cu1 N7 102.91(17) 9_556 16_556
N3 Cu1 N7 97.43(18) 9_556 16_556
O11 Cu1 Cu1 82.06(11) . 9_556
N9 Cu1 Cu1 83.12(13) . 9_556
O12 Cu1 Cu1 79.35(10) 9_556 9_556
N3 Cu1 Cu1 83.50(13) 9_556 9_556
N7 Cu1 Cu1 177.53(14) 16_556 9_556
C5B N1 C2 83.2(7) . .
C2 N1 C6 123.4(5) . .
N1 C2 N3 125.9(6) . .
N1 C2 H2 117.0 . .
N3 C2 H2 117.0 . .
C5B C2 H2 164.0 . .
C2 N3 C4 109.2(5) . .
C2 N3 Cu1 128.6(5) . 9_556
C4 N3 Cu1 121.7(3) . 9_556
C5B N3 Cu1 170.2(4) . 9_556
N9 C4 N3 126.5(4) . .
N9 C4 C5 100.5(5) . .
N3 C4 C5 133.0(6) . .
N9 C4 C5B 147.4(7) . .
N3 C4 C5B 86.0(6) . .
N7 C5 C6 128.5(7) . .
N7 C5 C4 118.3(6) . .
C6 C5 C4 113.0(6) . .
C6 C5 C8 170.3(6) . .
N6 C6 C5 124.1(9) . .
N6 C6 N1 120.5(7) . .
C5 C6 N1 115.4(6) . .
C6 N6 H6A 120.0 . .
C6 N6 H6B 120.0 . .
H6A N6 H6B 120.0 . .
N1 C5B C6B 118.9(13) . .
N1 C5B C4 135.6(10) . .
C6B C5B C4 105.4(11) . .
C6B C5B C2 168.6(12) . .
C6B C5B N3 149.0(11) . .
N6B C6B C5B 123.6(18) . .
N6B C6B N7 126.3(15) . .
C5B C6B N7 110.2(11) . .
C6B N6B H6B1 120.0 . .
C6B N6B H6B2 120.0 . .
H6B1 N6B H6B2 120.0 . .
C5 N7 C8 96.1(5) . .
C5 N7 C6B 35.8(5) . .
C8 N7 C6B 131.8(6) . .
C5 N7 Cu1 144.8(5) . 15_556
C8 N7 Cu1 119.0(4) . 15_556
C6B N7 Cu1 109.1(5) . 15_556
N7 C8 N9 118.7(6) . .
N7 C8 H8 120.6 . .
N9 C8 H8 120.6 . .
C5 C8 H8 162.5 . .
C4 N9 C8 106.3(5) . .
C4 N9 Cu1 125.0(3) . .
C8 N9 Cu1 128.3(4) . .
C11 O11 Cu1 125.4(3) . .
C11 O12 Cu1 127.7(3) . 9_556
O12 C11 O11 124.8(4) . .
O12 C11 C12 117.9(5) . .
O11 C11 C12 117.3(5) . .
C13 C12 C11 113.3(4) . .
C13 C12 H12A 108.9 . .
C11 C12 H12A 108.9 . .
C13 C12 H12B 108.9 . .
C11 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
C12 C13 C14 113.3(4) . .
C12 C13 H13A 108.9 . .
C14 C13 H13A 108.9 . .
C12 C13 H13B 108.9 . .
C14 C13 H13B 108.9 . .
H13A C13 H13B 107.7 . .
C13 C14 C15 111.6(4) . .
C13 C14 H14A 109.3 . .
C15 C14 H14A 109.3 . .
C13 C14 H14B 109.3 . .
C15 C14 H14B 109.3 . .
H14A C14 H14B 108.0 . .
C16 C15 C14 112.5(5) . .
C16 C15 H15A 109.1 . .
C14 C15 H15A 109.1 . .
C16 C15 H15B 109.1 . .
C14 C15 H15B 109.1 . .
H15A C15 H15B 107.8 . .
C15 C16 C17 113.1(5) . .
C15 C16 H16A 109.0 . .
C17 C16 H16A 109.0 . .
C15 C16 H16B 109.0 . .
C17 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
O21 C17 O22 120.8(6) . .
O21 C17 C16 123.1(6) . .
O22 C17 C16 115.9(5) . .
C17 O22 H22 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O11 1.981(3) .
Cu1 N9 1.994(4) .
Cu1 O12 2.004(3) 9_556
Cu1 N3 2.032(4) 9_556
Cu1 N7 2.188(4) 16_556
Cu1 Cu1 2.8651(11) 9_556
N1 C5B 1.267(13) .
N1 C2 1.324(8) .
N1 C6 1.479(10) .
C2 N3 1.346(6) .
C2 C5B 1.720(14) .
C2 H2 0.9300 .
N3 C4 1.365(8) .
N3 C5B 1.970(14) .
C4 N9 1.319(8) .
C4 C5 1.446(8) .
C4 C5B 1.518(14) .
C5 N7 1.320(8) .
C5 C6 1.381(10) .
C5 C8 1.969(10) .
C6 N6 1.358(16) .
N6 H6A 0.8600 .
N6 H6B 0.8600 .
C5B C6B 1.408(18) .
C6B N6B 1.28(3) .
C6B N7 1.633(17) .
N6B H6B1 0.8600 .
N6B H6B2 0.8600 .
N7 C8 1.327(8) .
C8 N9 1.365(6) .
C8 H8 0.9300 .
O11 C11 1.255(6) .
O12 C11 1.252(6) .
C11 C12 1.513(7) .
C12 C13 1.508(8) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.517(7) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.525(7) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.500(7) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C17 1.519(8) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 O21 1.142(8) .
C17 O22 1.241(7) .
O22 H22 1.0570 .
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 2.13 2.98(1) 169.6 3_455
N6 H6B O21 0.86 1.79 2.64(1) 168.8 1_455
N6B H6B2 O12 0.86 1.77 2.59(3) 160.8 3_455
N6B H6B1 O21 0.86 2.25 3.076(19) 160.5 1_455
O22 H22 N1 1.06 1.64 2.686(6) 169.7 1_655
