#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/32/7003200.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_7003200
loop_
_publ_author_name
'Mastropietro, Teresa F.'
'Armentano, Donatella'
'Grisolia, Ettore'
'Zanchini, Claudia'
'Lloret, Francesc'
'Julve, Miguel'
'De Munno, Giovanni'
_publ_section_title
;
 Guanine-containing copper(ii) complexes: synthesis, X-ray structures
 and magnetic properties
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              514
_journal_page_last               520
_journal_paper_doi               10.1039/b713960h
_journal_year                    2008
_chemical_formula_sum            'C11.5 H16 Cl Cu N10 O11'
_chemical_formula_weight         569.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.2450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.6576(9)
_cell_length_b                   13.4180(4)
_cell_length_c                   12.8429(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3932.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'X8APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27302
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4188
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0380
_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)+(0.0665P)²+5.0887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                3404
_reflns_number_total             4188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713960h.txt
_cod_data_source_block           cuclog3
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C11.50 H16 Cl Cu N10 O11'
_cod_database_code               7003200
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.327017(14) 0.08330(2) 0.69063(3) 0.02837(13) Uani 1 1 d . . .
Cl1 Cl -0.05919(3) -0.21831(5) 0.48303(7) 0.0400(2) Uani 1 1 d . . .
O61 O 0.35235(9) 0.57398(12) 0.69329(19) 0.0353(5) Uani 1 1 d . . .
O6 O 0.19433(9) -0.35202(14) 0.5665(2) 0.0400(5) Uani 1 1 d . . .
N9 N 0.30050(10) -0.06030(15) 0.6714(2) 0.0275(5) Uani 1 1 d . . .
N91 N 0.34914(10) 0.22856(15) 0.69646(19) 0.0272(5) Uani 1 1 d . . .
O1W O 0.24657(9) 0.12430(14) 0.6576(2) 0.0433(6) Uani 1 1 d D . .
N3 N 0.19441(10) -0.04697(16) 0.59277(19) 0.0274(5) Uani 1 1 d . . .
N1 N 0.14740(10) -0.20320(15) 0.5430(2) 0.0294(5) Uani 1 1 d . . .
H1A H 0.1143 -0.2333 0.5126 0.035 Uiso 1 1 calc R . .
C4 C 0.24892(12) -0.20229(17) 0.6275(2) 0.0263(6) Uani 1 1 d . . .
N7 N 0.30754(10) -0.22507(15) 0.6720(2) 0.0297(5) Uani 1 1 d . . .
H7A H 0.3227 -0.2838 0.6824 0.036 Uiso 1 1 calc R . .
N71 N 0.40674(10) 0.36116(16) 0.7383(2) 0.0333(5) Uani 1 1 d . . .
H71A H 0.4381 0.3967 0.7633 0.040 Uiso 1 1 calc R . .
N21 N 0.17480(11) 0.41623(17) 0.5338(2) 0.0377(6) Uani 1 1 d . . .
H21A H 0.1524 0.3650 0.5115 0.045 Uiso 1 1 calc R . .
H21B H 0.1602 0.4752 0.5193 0.045 Uiso 1 1 calc R . .
N11 N 0.26587(10) 0.48941(15) 0.62048(19) 0.0277(5) Uani 1 1 d . . .
H11A H 0.2474 0.5453 0.6063 0.033 Uiso 1 1 calc R . .
N31 N 0.25553(10) 0.31411(15) 0.61399(19) 0.0264(5) Uani 1 1 d . . .
C81 C 0.40379(12) 0.26192(19) 0.7398(3) 0.0325(6) Uani 1 1 d . . .
H81A H 0.4364 0.2207 0.7680 0.039 Uiso 1 1 calc R . .
C2 C 0.14663(12) -0.10156(18) 0.5517(2) 0.0263(5) Uani 1 1 d . . .
C5 C 0.24479(12) -0.09968(17) 0.6278(2) 0.0237(5) Uani 1 1 d . . .
C61 C 0.32597(12) 0.49308(19) 0.6703(2) 0.0270(6) Uani 1 1 d . . .
C41 C 0.35037(12) 0.39591(18) 0.6894(2) 0.0268(6) Uani 1 1 d . . .
N2 N 0.09383(11) -0.05785(18) 0.5154(2) 0.0379(6) Uani 1 1 d . . .
H2A H 0.0912 0.0059 0.5190 0.045 Uiso 1 1 calc R . .
H2B H 0.0626 -0.0935 0.4886 0.045 Uiso 1 1 calc R . .
C6 C 0.19806(12) -0.26145(19) 0.5800(2) 0.0275(6) Uani 1 1 d . . .
C8 C 0.33662(12) -0.13885(19) 0.6961(2) 0.0316(6) Uani 1 1 d . . .
H8A H 0.3773 -0.1339 0.7266 0.038 Uiso 1 1 calc R . .
C21 C 0.23281(12) 0.40419(17) 0.5915(2) 0.0255(5) Uani 1 1 d . . .
C51 C 0.31472(12) 0.31294(18) 0.6635(2) 0.0244(5) Uani 1 1 d . . .
O9 O -0.11644(12) -0.1875(2) 0.4720(3) 0.0717(8) Uani 1 1 d . . .
O3 O -0.06110(14) -0.2650(3) 0.3826(3) 0.0849(10) Uani 1 1 d . . .
O1 O -0.02323(14) -0.1334(2) 0.5020(4) 0.0919(12) Uani 1 1 d . . .
O2 O -0.03639(18) -0.2857(3) 0.5737(3) 0.1098(15) Uani 1 1 d . . .
O2W O 0.05803(12) -0.3218(2) 0.4084(3) 0.0621(7) Uani 1 1 d D . .
C10 C 0.43548(15) 0.0327(2) 0.8453(4) 0.0493(9) Uani 1 1 d . . .
O4 O 0.41295(14) 0.0412(2) 0.9148(3) 0.0712(8) Uani 1 1 d . . .
O5 O 0.40850(9) 0.04362(15) 0.7397(2) 0.0447(6) Uani 1 1 d . . .
C11 C 0.5000 0.5752(3) 0.7500 0.0588(15) Uani 1 2 d S . .
O7 O 0.5000 0.4855(2) 0.7500 0.0467(8) Uani 1 2 d S . .
O8 O 0.4659(2) 0.6378(3) 0.7338(4) 0.0467(11) Uani 0.50 1 d P . .
H1W H 0.2325(15) 0.1872(14) 0.623(3) 0.060 Uiso 1 1 d D . .
H2W H 0.2140(11) 0.082(2) 0.621(3) 0.060 Uiso 1 1 d D . .
H3W H 0.0184(7) -0.301(3) 0.377(3) 0.060 Uiso 1 1 d D . .
H4W H 0.0585(16) -0.367(2) 0.466(2) 0.060 Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O5 Cu1 O1W 174.14(11) . . ?
O5 Cu1 N91 91.20(9) . . ?
O1W Cu1 N91 88.51(9) . . ?
O5 Cu1 N9 91.46(9) . . ?
O1W Cu1 N9 89.25(9) . . ?
N91 Cu1 N9 175.28(10) . . ?
O1 Cl1 O2 110.3(3) . . ?
O1 Cl1 O3 108.5(2) . . ?
O2 Cl1 O3 109.5(2) . . ?
O1 Cl1 O9 108.51(19) . . ?
O2 Cl1 O9 109.8(2) . . ?
O3 Cl1 O9 110.3(2) . . ?
C8 N9 C5 105.4(2) . . ?
C8 N9 Cu1 124.53(19) . . ?
C5 N9 Cu1 129.98(17) . . ?
C81 N91 C51 105.1(2) . . ?
C81 N91 Cu1 124.00(17) . . ?
C51 N91 Cu1 130.85(18) . . ?
C2 N3 C5 114.4(2) . . ?
C2 N1 C6 124.6(2) . . ?
N7 C4 C5 106.7(2) . . ?
N7 C4 C6 132.6(2) . . ?
C5 C4 C6 120.5(2) . . ?
C8 N7 C4 107.0(2) . . ?
C81 N71 C41 107.1(2) . . ?
C21 N11 C61 125.6(2) . . ?
C21 N31 C51 114.0(2) . . ?
N91 C81 N71 112.5(2) . . ?
N3 C2 N2 120.0(2) . . ?
N3 C2 N1 123.3(2) . . ?
N2 C2 N1 116.7(2) . . ?
N3 C5 N9 125.8(2) . . ?
N3 C5 C4 125.5(2) . . ?
N9 C5 C4 108.7(2) . . ?
O61 C61 N11 121.1(2) . . ?
O61 C61 C41 127.8(3) . . ?
N11 C61 C41 111.1(2) . . ?
N71 C41 C51 106.2(2) . . ?
N71 C41 C61 133.0(2) . . ?
C51 C41 C61 120.7(2) . . ?
O6 C6 N1 119.8(2) . . ?
O6 C6 C4 128.7(3) . . ?
N1 C6 C4 111.5(2) . . ?
N7 C8 N9 112.1(2) . . ?
N31 C21 N21 120.3(2) . . ?
N31 C21 N11 123.1(2) . . ?
N21 C21 N11 116.6(2) . . ?
N31 C51 C41 125.4(2) . . ?
N31 C51 N91 125.5(2) . . ?
C41 C51 N91 109.0(2) . . ?
O4 C10 O5 124.6(3) . . ?
C10 O5 Cu1 115.9(2) . . ?
O8 C11 O8 86.2(5) 2_656 . ?
O8 C11 O7 136.9(3) 2_656 . ?
O8 C11 O7 136.9(3) . . ?
C11 O8 O8 46.9(3) . 2_656 ?
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 O5 1.939(2) . ?
Cu1 O1W 1.944(2) . ?
Cu1 N91 2.018(2) . ?
Cu1 N9 2.020(2) . ?
Cl1 O1 1.407(3) . ?
Cl1 O2 1.412(3) . ?
Cl1 O3 1.419(3) . ?
Cl1 O9 1.426(3) . ?
O61 C61 1.242(3) . ?
O6 C6 1.226(3) . ?
N9 C8 1.338(3) . ?
N9 C5 1.377(3) . ?
N91 C81 1.326(4) . ?
N91 C51 1.382(3) . ?
N3 C2 1.316(3) . ?
N3 C5 1.350(3) . ?
N1 C2 1.369(3) . ?
N1 C6 1.396(3) . ?
C4 N7 1.373(3) . ?
C4 C5 1.381(3) . ?
C4 C6 1.413(4) . ?
N7 C8 1.334(3) . ?
N71 C81 1.334(3) . ?
N71 C41 1.372(4) . ?
N21 C21 1.348(4) . ?
N11 C21 1.371(3) . ?
N11 C61 1.375(4) . ?
N31 C21 1.318(3) . ?
N31 C51 1.354(4) . ?
C2 N2 1.340(4) . ?
C61 C41 1.418(3) . ?
C41 C51 1.379(4) . ?
C10 O4 1.221(5) . ?
C10 O5 1.273(5) . ?
C11 O8 1.151(5) 2_656 ?
C11 O8 1.151(5) . ?
C11 O7 1.204(6) . ?
O8 O8 1.572(9) 2_656 ?
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 H1W N31 0.954(10) 1.81(2) 2.635(3) 142(3) .
O1W H2W N3 0.951(10) 1.79(2) 2.611(3) 142(3) .
N1 H1A O2W 0.86 1.93 2.738(3) 156.0 .
N71 H71A O7 0.86 1.99 2.798(3) 155.2 .
N7 H7A O61 0.86 2.03 2.887(3) 174.7 1_545
N11 H11A O6 0.86 1.84 2.682(3) 167.9 1_565
O2W H4W O4 0.954(10) 1.882(15) 2.796(5) 160(3) 4_546
N21 H21B O4 0.86 2.43 3.002(4) 124.4 4_556
N21 H21B O6 0.86 2.46 3.150(3) 137.4 1_565
N2 H2B O1 0.86 2.25 3.002(4) 145.7 .
N2 H2A O1 0.86 2.34 3.061(4) 141.9 5_556
O2W H3W O3 0.946(10) 2.05(2) 2.930(4) 154(3) .
