#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:54:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179735 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/31/7003199.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_7003199
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            'C7 H13 Cu F6 N5 O11 S2'
_chemical_formula_weight         584.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.107(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3167(14)
_cell_length_b                   18.549(3)
_cell_length_c                   12.895(2)
_cell_measurement_temperature    273(2)
_cell_volume                     1986.3(6)
_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      273(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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17163
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3875
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.313
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0573
_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)+(0.0.1104P)²+1.9613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                3174
_reflns_number_total             3875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713960h.txt
_cod_data_source_block           cutfgua
_cod_original_sg_symbol_H-M      P(2)1/c
_cod_database_code               7003199
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.15914(5) 0.66804(2) 0.18628(3) 0.0325(2) Uani 1 1 d . . .
S2 S 0.29760(13) 0.39640(6) 0.59736(8) 0.0465(3) Uani 1 1 d . . .
O2W O -0.0620(3) 0.70249(16) 0.1899(2) 0.0416(6) Uani 1 1 d D . .
O1W O 0.0856(5) 0.55259(16) 0.1397(3) 0.0585(8) Uani 1 1 d D . .
O3W O 0.3885(4) 0.6495(3) 0.1890(2) 0.0767(12) Uani 1 1 d D . .
O6 O 0.1810(4) 0.65733(15) 0.6648(2) 0.0474(7) Uani 1 1 d . . .
N1 N 0.1771(4) 0.60317(17) 0.5064(2) 0.0382(7) Uani 1 1 d . . .
H1A H 0.1822 0.5621 0.5374 0.046 Uiso 1 1 calc R . .
C4 C 0.1627(4) 0.72363(19) 0.4029(2) 0.0311(7) Uani 1 1 d . . .
C2 C 0.1725(5) 0.6017(2) 0.4003(3) 0.0374(8) Uani 1 1 d . . .
C6 C 0.1744(4) 0.66372(19) 0.5699(3) 0.0346(8) Uani 1 1 d . . .
N2 N 0.1747(5) 0.53747(19) 0.3561(3) 0.0517(9) Uani 1 1 d . . .
H2A H 0.1729 0.5339 0.2895 0.062 Uiso 1 1 calc R . .
H2B H 0.1780 0.4992 0.3938 0.062 Uiso 1 1 calc R . .
N3 N 0.1674(4) 0.66194(15) 0.3434(2) 0.0335(7) Uani 1 1 d . . .
N9 N 0.1585(4) 0.79275(17) 0.3679(2) 0.0390(7) Uani 1 1 d . . .
H9A H 0.1563 0.8063 0.3040 0.047 Uiso 1 1 calc R . .
C5 C 0.1642(4) 0.72715(19) 0.5090(3) 0.0311(7) Uani 1 1 d . . .
C8 C 0.1583(5) 0.8363(2) 0.4518(3) 0.0407(9) Uani 1 1 d . . .
H8A H 0.1555 0.8863 0.4486 0.049 Uiso 1 1 calc R . .
N7 N 0.1626(4) 0.79893(17) 0.5390(2) 0.0351(7) Uani 1 1 d . . .
O7 O 0.2089(5) 0.33916(19) 0.6404(3) 0.0760(11) Uani 1 1 d . . .
O5 O 0.1973(4) 0.45434(18) 0.5566(3) 0.0672(9) Uani 1 1 d . . .
O4 O 0.4423(5) 0.4178(2) 0.6544(3) 0.0848(12) Uani 1 1 d . . .
C3 C 0.3699(6) 0.3563(3) 0.4796(4) 0.0659(13) Uani 1 1 d . . .
F6 F 0.2493(5) 0.3322(2) 0.4191(3) 0.0998(13) Uani 1 1 d . . .
F5 F 0.4498(4) 0.4048(2) 0.4280(3) 0.0993(12) Uani 1 1 d . . .
F4 F 0.4693(4) 0.3021(2) 0.5025(3) 0.0990(13) Uani 1 1 d . . .
O4W O 0.1932(9) 0.9789(4) 0.3114(5) 0.150(2) Uani 1 1 d . . .
H5W H 0.447(4) 0.639(3) 0.1291(19) 0.060 Uiso 1 1 d D . .
H1W H 0.155(4) 0.521(2) 0.105(4) 0.060 Uiso 1 1 d D . .
H3W H -0.137(4) 0.697(2) 0.131(2) 0.060 Uiso 1 1 d D . .
H2W H -0.021(2) 0.536(2) 0.123(4) 0.060 Uiso 1 1 d D . .
H4W H -0.122(5) 0.681(2) 0.243(2) 0.060 Uiso 1 1 d D . .
H6W H 0.465(4) 0.641(3) 0.246(2) 0.060 Uiso 1 1 d D . .
S1 S 0.32329(16) 0.39290(8) 0.02100(9) 0.0627(4) Uani 1 1 d . . .
C1 C 0.3512(8) 0.3793(4) 0.1593(4) 0.0843(17) Uani 1 1 d . . .
F3 F 0.4303(8) 0.3215(3) 0.1830(4) 0.139(2) Uani 1 1 d . . .
F2 F 0.2132(6) 0.3792(4) 0.2039(3) 0.143(2) Uani 1 1 d . . .
F1 F 0.4257(8) 0.4343(3) 0.2029(3) 0.147(2) Uani 1 1 d . . .
O3 O 0.2319(6) 0.3302(3) -0.0120(4) 0.1041(17) Uani 1 1 d . . .
O2 O 0.2326(6) 0.4585(3) 0.0097(4) 0.1028(15) Uani 1 1 d . . .
O1 O 0.4817(6) 0.3963(3) -0.0132(4) 0.1135(19) Uani 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O3W Cu1 O2W 170.79(16) . . ?
O3W Cu1 N7 90.39(13) . 4_575 ?
O2W Cu1 N7 89.09(12) . 4_575 ?
O3W Cu1 N3 89.54(13) . . ?
O2W Cu1 N3 88.60(12) . . ?
N7 Cu1 N3 165.07(12) 4_575 . ?
O3W Cu1 O1W 94.99(17) . . ?
O2W Cu1 O1W 94.22(13) . . ?
N7 Cu1 O1W 93.15(12) 4_575 . ?
N3 Cu1 O1W 101.72(12) . . ?
O7 S2 O4 116.5(3) . . ?
O7 S2 O5 113.3(2) . . ?
O4 S2 O5 115.7(2) . . ?
O7 S2 C3 102.8(3) . . ?
O4 S2 C3 103.6(3) . . ?
O5 S2 C3 102.2(2) . . ?
C2 N1 C6 127.2(3) . . ?
N9 C4 C5 106.6(3) . . ?
N9 C4 N3 126.7(3) . . ?
C5 C4 N3 126.6(3) . . ?
N2 C2 N3 121.2(3) . . ?
N2 C2 N1 116.7(3) . . ?
N3 C2 N1 122.1(3) . . ?
O6 C6 N1 120.5(3) . . ?
O6 C6 C5 129.2(3) . . ?
N1 C6 C5 110.3(3) . . ?
C2 N3 C4 112.9(3) . . ?
C2 N3 Cu1 126.4(2) . . ?
C4 N3 Cu1 120.6(2) . . ?
C8 N9 C4 107.3(3) . . ?
C4 C5 N7 109.0(3) . . ?
C4 C5 C6 120.8(3) . . ?
N7 C5 C6 130.1(3) . . ?
N7 C8 N9 111.6(3) . . ?
C8 N7 C5 105.4(3) . . ?
C8 N7 Cu1 130.4(3) . 4_576 ?
C5 N7 Cu1 124.1(2) . 4_576 ?
F6 C3 F5 108.7(5) . . ?
F6 C3 F4 108.8(5) . . ?
F5 C3 F4 107.7(4) . . ?
F6 C3 S2 110.9(4) . . ?
F5 C3 S2 109.9(4) . . ?
F4 C3 S2 110.7(4) . . ?
O1 S1 O2 115.1(4) . . ?
O1 S1 O3 115.4(3) . . ?
O2 S1 O3 112.9(3) . . ?
O1 S1 C1 104.0(3) . . ?
O2 S1 C1 104.9(3) . . ?
O3 S1 C1 102.5(3) . . ?
F3 C1 F1 108.9(6) . . ?
F3 C1 F2 110.1(7) . . ?
F1 C1 F2 102.7(6) . . ?
F3 C1 S1 112.8(5) . . ?
F1 C1 S1 110.5(5) . . ?
F2 C1 S1 111.4(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 O3W 1.937(3) . ?
Cu1 O2W 1.950(3) . ?
Cu1 N7 1.997(3) 4_575 ?
Cu1 N3 2.027(3) . ?
Cu1 O1W 2.298(3) . ?
S2 O7 1.423(3) . ?
S2 O4 1.432(4) . ?
S2 O5 1.442(3) . ?
S2 C3 1.822(6) . ?
O6 C6 1.227(5) . ?
N1 C2 1.367(4) . ?
N1 C6 1.391(5) . ?
C4 N9 1.359(5) . ?
C4 C5 1.369(5) . ?
C4 N3 1.379(4) . ?
C2 N2 1.322(5) . ?
C2 N3 1.336(5) . ?
C6 C5 1.414(5) . ?
N9 C8 1.350(5) . ?
C5 N7 1.387(5) . ?
C8 N7 1.320(5) . ?
N7 Cu1 1.997(3) 4_576 ?
C3 F6 1.316(6) . ?
C3 F5 1.320(6) . ?
C3 F4 1.324(7) . ?
S1 O1 1.413(4) . ?
S1 O2 1.436(5) . ?
S1 O3 1.441(5) . ?
S1 C1 1.804(6) . ?
C1 F3 1.286(8) . ?
C1 F1 1.304(7) . ?
C1 F2 1.310(7) . ?
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
N2 H2A O1W 0.86 2.06 2.861(5) 155.6 .
N1 H1A O5 0.86 2.02 2.838(5) 159.4 .
N2 H2B O5 0.86 2.26 3.008(5) 146.1 .
O1W H1W O2 0.956(10) 1.825(19) 2.751(5) 162(4) .
N9 H9A O6 0.86 1.94 2.794(4) 171.9 4_575
O1W H2W O4W 0.951(10) 2.01(4) 2.794(8) 139(4) 2_545
O3W H5W O1 0.951(10) 1.767(16) 2.699(5) 166(4) 3_665
O1W H2W O2 0.951(10) 2.39(3) 3.195(6) 142(4) 3_565
O2W H3W O3 0.957(10) 1.764(17) 2.696(5) 164(4) 3_565
O3W H6W O4 0.954(10) 1.83(3) 2.703(5) 150(4) 3_666
O2W H4W O7 0.961(10) 1.740(16) 2.677(4) 164(4) 3_566
