#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:08:23 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179653 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/06/4510643.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_4510643
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
;
 Structural Diversity in a Copper(II)/Isophthalato/9-Methyladenine System.
 From One- to Three-Dimensional Metal-Biomolecule Frameworks
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3057
_journal_paper_doi               10.1021/cg400458a
_journal_volume                  13
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H15 Cu N5 O6'
_chemical_formula_structural     'C14 H15 Cu N5 O6'
_chemical_formula_sum            'C14 H15 Cu N5 O6'
_chemical_formula_weight         412.85
_chemical_name_systematic
;
catena-Poly[diaqua(mu-isophthalato-k2O,O':kO'')(9-methyladenine-kN7)copper(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.000
_cell_angle_beta                 99.938(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.289(4)
_cell_length_b                   10.210(5)
_cell_length_c                   17.241(7)
_cell_measurement_reflns_used    12192
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.23
_cell_volume                     1610.6(12)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 2006)'
_computing_data_reduction        IPDS
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12192
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
X-RED; Stoe & Cie, 2001
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      1.71(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0395
_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)+(0.0637P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                2571
_reflns_number_total             3408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400458a_si_002.cif
_cod_data_source_block           "'compound1'"
_cod_original_cell_volume        1611(1)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4510643
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Cu1 Cu 0.92970(4) 0.06019(3) 0.83656(2) 0.02182(12) Uani 1 1 d .
N1 N 0.4859(3) -0.1397(2) 0.92443(15) 0.0262(5) Uani 1 1 d .
C2 C 0.4259(3) -0.2358(3) 0.87672(19) 0.0282(7) Uani 1 1 d .
H2 H 0.3398 -0.2707 0.8885 0.034 Uiso 1 1 calc R
N3 N 0.4723(3) -0.2885(2) 0.81458(15) 0.0263(5) Uani 1 1 d .
C4 C 0.5967(3) -0.2304(3) 0.80210(17) 0.0244(6) Uani 1 1 d .
C5 C 0.6708(3) -0.1296(3) 0.84557(17) 0.0235(6) Uani 1 1 d .
C6 C 0.6128(3) -0.0834(3) 0.91135(18) 0.0246(6) Uani 1 1 d .
N6 N 0.6726(3) 0.0116(3) 0.95897(16) 0.0304(6) Uani 1 1 d .
H6A H 0.6313 0.0369 0.9974 0.036 Uiso 1 1 calc R
H6B H 0.7525 0.0479 0.9514 0.036 Uiso 1 1 calc R
N7 N 0.7932(3) -0.0955(2) 0.81328(15) 0.0240(5) Uani 1 1 d .
C8 C 0.7904(3) -0.1746(3) 0.75256(18) 0.0252(6) Uani 1 1 d .
H8 H 0.8606 -0.1740 0.7201 0.030 Uiso 1 1 calc R
N9 N 0.6735(3) -0.2573(2) 0.74249(15) 0.0244(5) Uani 1 1 d .
C9 C 0.6335(4) -0.3530(3) 0.67910(19) 0.0305(7) Uani 1 1 d .
H9A H 0.5468 -0.3242 0.6448 0.046 Uiso 1 1 calc R
H9B H 0.6156 -0.4364 0.7013 0.046 Uiso 1 1 calc R
H9C H 0.7120 -0.3611 0.6497 0.046 Uiso 1 1 calc R
C11 C 1.1411(3) 0.0322(3) 0.62211(17) 0.0231(6) Uani 1 1 d .
C12 C 1.2573(3) -0.0308(3) 0.59701(18) 0.0265(6) Uani 1 1 d .
H12 H 1.3084 -0.0959 0.6280 0.032 Uiso 1 1 calc R
C13 C 1.2975(4) 0.0033(3) 0.52536(19) 0.0294(7) Uani 1 1 d .
H13 H 1.3752 -0.0395 0.5087 0.035 Uiso 1 1 calc R
C14 C 1.2222(3) 0.1009(3) 0.47872(18) 0.0264(6) Uani 1 1 d .
H14 H 1.2491 0.1228 0.4309 0.032 Uiso 1 1 calc R
C15 C 1.1065(3) 0.3342(3) 1.00377(17) 0.0230(6) Uani 1 1 d .
C16 C 1.0662(3) 0.1307(3) 0.57523(17) 0.0231(6) Uani 1 1 d .
H16 H 0.9886 0.1735 0.5919 0.028 Uiso 1 1 calc R
C17 C 1.0942(3) -0.0010(3) 0.69925(17) 0.0221(6) Uani 1 1 d .
O11 O 0.9981(2) 0.0692(2) 0.72134(12) 0.0258(4) Uani 1 1 d .
O12 O 1.1566(2) -0.0977(2) 0.73832(12) 0.0271(5) Uani 1 1 d .
C18 C 1.0231(3) 0.2285(3) 0.95485(17) 0.0240(6) Uani 1 1 d .
O21 O 0.9375(2) 0.1567(2) 0.98449(12) 0.0264(5) Uani 1 1 d .
O22 O 1.0434(2) 0.21555(19) 0.88383(12) 0.0244(4) Uani 1 1 d .
O1W O 0.7610(2) 0.17731(19) 0.80907(12) 0.0261(4) Uani 1 1 d .
O2W O 1.0990(2) -0.05082(19) 0.87952(12) 0.0254(4) Uani 1 1 d .
H11W H 0.7996 0.2550 0.8061 0.038 Uiso 1 1 d .
H12W H 0.6863 0.1795 0.7717 0.038 Uiso 1 1 d .
H21W H 1.0960 -0.1049 0.9189 0.038 Uiso 1 1 d .
H22W H 1.1157 -0.0990 0.8368 0.038 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
O1W Cu1 O2W 172.06(8) . .
O1W Cu1 O22 87.63(9) . .
O2W Cu1 O22 88.40(9) . .
O1W Cu1 N7 89.08(10) . .
O2W Cu1 N7 93.13(10) . .
O22 Cu1 N7 165.88(9) . .
O1W Cu1 O11 95.73(8) . .
O2W Cu1 O11 91.58(8) . .
O22 Cu1 O11 96.94(8) . .
N7 Cu1 O11 97.05(9) . .
O1W Cu1 O21 84.07(8) . .
O2W Cu1 O21 88.04(8) . .
O22 Cu1 O21 53.44(7) . .
N7 Cu1 O21 112.55(8) . .
O11 Cu1 O21 150.39(7) . .
C2 N1 C6 119.1(3) . .
N3 C2 N1 129.1(3) . .
N3 C2 H2 115.4 . .
N1 C2 H2 115.4 . .
C2 N3 C4 110.7(3) . .
N3 C4 N9 126.9(3) . .
N3 C4 C5 126.9(3) . .
N9 C4 C5 106.2(3) . .
C4 C5 N7 109.5(3) . .
C4 C5 C6 117.2(3) . .
N7 C5 C6 133.3(3) . .
N6 C6 N1 119.1(3) . .
N6 C6 C5 124.1(3) . .
N1 C6 C5 116.8(3) . .
C6 N6 H6A 120.0 . .
C6 N6 H6B 120.0 . .
H6A N6 H6B 120.0 . .
C8 N7 C5 105.0(2) . .
C8 N7 Cu1 124.2(2) . .
C5 N7 Cu1 129.9(2) . .
N7 C8 N9 112.8(3) . .
N7 C8 H8 123.6 . .
N9 C8 H8 123.6 . .
C8 N9 C4 106.6(2) . .
C8 N9 C9 127.0(3) . .
C4 N9 C9 126.3(2) . .
N9 C9 H9A 109.5 . .
N9 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N9 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C12 C11 C16 119.3(3) . .
C12 C11 C17 122.0(3) . .
C16 C11 C17 118.7(3) . .
C11 C12 C13 120.1(3) . .
C11 C12 H12 119.9 . .
C13 C12 H12 119.9 . .
C14 C13 C12 120.4(3) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C13 C14 C15 120.0(3) . 4_565
C13 C14 H14 120.0 . .
C15 C14 H14 120.0 4_565 .
C14 C15 C16 119.4(3) 4_566 4_566
C14 C15 C18 121.3(3) 4_566 .
C16 C15 C18 119.3(3) 4_566 .
C15 C16 C11 120.8(3) 4_565 .
C15 C16 H16 119.6 4_565 .
C11 C16 H16 119.6 . .
O11 C17 O12 124.3(3) . .
O11 C17 C11 117.9(3) . .
O12 C17 C11 117.7(3) . .
C17 O11 Cu1 125.77(19) . .
O21 C18 O22 122.6(3) . .
O21 C18 C15 119.6(3) . .
O22 C18 C15 117.8(3) . .
C18 O21 Cu1 75.29(16) . .
C18 O22 Cu1 108.53(18) . .
Cu1 O1W H11W 104.4 . .
Cu1 O1W H12W 134.7 . .
H11W O1W H12W 102.6 . .
Cu1 O2W H21W 121.4 . .
Cu1 O2W H22W 103.9 . .
H21W O2W H22W 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1W 1.963(2) .
Cu1 O2W 1.976(2) .
Cu1 O22 2.000(2) .
Cu1 N7 2.030(3) .
Cu1 O11 2.189(2) .
Cu1 O21 2.724(2) .
N1 C2 1.339(4) .
N1 C6 1.364(4) .
C2 N3 1.335(4) .
C2 H2 0.9300 .
N3 C4 1.349(4) .
C4 N9 1.376(4) .
C4 C5 1.385(4) .
C5 N7 1.393(4) .
C5 C6 1.418(4) .
C6 N6 1.329(4) .
N6 H6A 0.8600 .
N6 H6B 0.8600 .
N7 C8 1.319(4) .
C8 N9 1.363(4) .
C8 H8 0.9300 .
N9 C9 1.465(4) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C11 C12 1.388(4) .
C11 C16 1.398(4) .
C11 C17 1.508(4) .
C12 C13 1.395(4) .
C12 H12 0.9300 .
C13 C14 1.391(4) .
C13 H13 0.9300 .
C14 C15 1.394(4) 4_565
C14 H14 0.9300 .
C15 C14 1.394(4) 4_566
C15 C16 1.394(4) 4_566
C15 C18 1.500(4) .
C16 C15 1.394(4) 4_565
C16 H16 0.9300 .
C17 O11 1.254(4) .
C17 O12 1.276(4) .
C18 O21 1.253(4) .
C18 O22 1.278(4) .
O1W H11W 0.8757 .
O1W H12W 0.8616 .
O2W H21W 0.8798 .
O2W H22W 0.9202 .
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
O1W H11W O12 0.88 1.77 2.598(3) 157.4 2_756
O1W H12W N3 0.86 1.93 2.787(3) 171.3 2_656
O2W H22W O12 0.92 1.80 2.625(3) 147.3 .
O2W H21W O21 0.88 1.82 2.656(3) 157.0 3_757
N6 H6A N1 0.86 2.15 2.990(4) 166.3 3_657
N6 H6B O21 0.86 2.04 2.841(4) 153.9 .
