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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/91/1509140.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_1509140
loop_
_publ_author_name
'Caballero, Ana B.'
'Rodríquez-Diéguez, Antonio'
'Quirós, Miguel'
'Lezama, Luis'
'Salas, Juan M.'
_publ_contact_author_address
;
Departamento de Química Inorgánica, Facultad de Ciencias,
c/ Severo Ochoa s/n, 18071 Granada, Spain
;
_publ_contact_author_email       acaballero@ugr.es
_publ_contact_author_fax         '34 958 248526'
_publ_contact_author_name        'Ana B. Caballero'
_publ_contact_author_phone       '34 958 240442'
_publ_section_title
;
 New Metal Complexes with 1,2,4-Triazolo[1,5-a]Pyrimidines and the
 Chelating Ligand 1,3-Propanediamine
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              194
_journal_page_last               201
_journal_paper_doi               10.1016/j.ica.2011.08.060
_journal_volume                  378
_journal_year                    2011
_chemical_formula_moiety         'C20 H36 Cu N12 2+, 2 (Cl O4 1-)'
_chemical_formula_sum            'C20 H36 Cl2 Cu N12 O8'
_chemical_formula_weight         707.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.457(1)
_cell_angle_beta                 99.007(1)
_cell_angle_gamma                111.190(1)
_cell_formula_units_Z            1
_cell_length_a                   8.0816(5)
_cell_length_b                   8.2729(5)
_cell_length_c                   12.4711(8)
_cell_measurement_reflns_used    5309
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.7
_cell_volume                     759.63(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'φ and ω 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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8820
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        -0.1
_diffrn_standards_number         190
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             367
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0700P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                3146
_reflns_number_total             3411
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            Compound1.cif
_cod_data_source_block           compound_1
_cod_depositor_comments          'Wrong last page number'
_cod_original_cell_volume        759.62(8)
_cod_database_code               1509140
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cu Cu 0.5000 0.5000 0.5000 0.04069(13) Uani 1 2 d S
N1 N 0.2528(3) -0.1371(2) 0.34563(14) 0.0465(4) Uani 1 1 d .
C2 C 0.3078(3) -0.0009(3) 0.42471(18) 0.0490(5) Uani 1 1 d .
H2 H 0.3140 -0.0160 0.4981 0.059 Uiso 1 1 d R
N3 N 0.3537(3) 0.1592(2) 0.39456(14) 0.0454(4) Uani 1 1 d .
C3A C 0.3253(3) 0.1239(2) 0.28569(16) 0.0385(4) Uani 1 1 d .
N4 N 0.3489(3) 0.2362(2) 0.21272(15) 0.0485(4) Uani 1 1 d .
C5 C 0.3092(4) 0.1666(3) 0.10867(19) 0.0562(6) Uani 1 1 d .
C51 C 0.3397(7) 0.2905(4) 0.0253(3) 0.0973(13) Uani 1 1 d .
H51 H 0.3111 0.3889 0.0488 0.117 Uiso 1 1 d R
H52 H 0.2630 0.2310 -0.0442 0.117 Uiso 1 1 d R
H53 H 0.4641 0.3307 0.0180 0.117 Uiso 1 1 d R
C6 C 0.2430(4) -0.0154(3) 0.07403(18) 0.0565(6) Uani 1 1 d .
H6 H 0.2169 -0.0578 -0.0005 0.068 Uiso 1 1 d R
C7 C 0.2180(3) -0.1291(3) 0.14791(17) 0.0457(5) Uani 1 1 d .
C71 C 0.1468(4) -0.3234(3) 0.1223(2) 0.0635(7) Uani 1 1 d .
H71 H 0.2321 -0.3659 0.1603 0.076 Uiso 1 1 d R
H72 H 0.1293 -0.3572 0.0447 0.076 Uiso 1 1 d R
H73 H 0.0333 -0.3727 0.1455 0.076 Uiso 1 1 d R
N8 N 0.2640(2) -0.0535(2) 0.25526(13) 0.0378(3) Uani 1 1 d .
N1P N 0.5513(2) 0.4150(2) 0.64601(13) 0.0382(3) Uani 1 1 d .
H11P H 0.6099 0.5111 0.6965 0.046 Uiso 1 1 d R
H12P H 0.6303 0.3628 0.6396 0.046 Uiso 1 1 d R
C1P C 0.4051(3) 0.2944(3) 0.69303(18) 0.0476(5) Uani 1 1 d .
H13P H 0.4544 0.2865 0.7676 0.057 Uiso 1 1 d R
H14P H 0.3610 0.1784 0.6508 0.057 Uiso 1 1 d R
C2P C 0.2495(3) 0.3531(3) 0.69413(19) 0.0528(5) Uani 1 1 d .
H21P H 0.1659 0.2775 0.7339 0.063 Uiso 1 1 d R
H22P H 0.2950 0.4713 0.7334 0.063 Uiso 1 1 d R
C3P C 0.1483(3) 0.3499(3) 0.5815(2) 0.0524(5) Uani 1 1 d .
H33P H 0.1176 0.2367 0.5382 0.063 Uiso 1 1 d R
H34P H 0.0362 0.3644 0.5878 0.063 Uiso 1 1 d R
N3P N 0.2554(2) 0.4891(2) 0.52466(15) 0.0450(4) Uani 1 1 d .
H31P H 0.2719 0.5926 0.5626 0.054 Uiso 1 1 d R
H32P H 0.1869 0.4802 0.4586 0.054 Uiso 1 1 d R
Cl Cl 0.86126(8) 0.20597(7) 0.25472(4) 0.05145(16) Uani 1 1 d .
O1P O 0.9029(4) 0.0588(3) 0.2245(2) 0.0910(7) Uani 1 1 d .
O2P O 1.0214(3) 0.3566(3) 0.2945(2) 0.0942(7) Uani 1 1 d .
O3P O 0.7527(4) 0.1774(3) 0.3360(2) 0.1024(9) Uani 1 1 d .
O4P O 0.7673(5) 0.2488(5) 0.1605(2) 0.1162(11) 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'
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
N3P Cu N3P 179.998(1) 2_666 .
N3P Cu N1P 91.56(7) 2_666 2_666
N3P Cu N1P 88.44(7) . 2_666
N3P Cu N1P 88.44(7) 2_666 .
N3P Cu N1P 91.56(7) . .
N1P Cu N1P 180.0 2_666 .
C2 N1 N8 100.48(17) . .
N1 C2 N3 117.5(2) . .
N1 C2 H2 121.3 . .
N3 C2 H2 121.2 . .
C3A N3 C2 102.43(17) . .
N3 C3A N4 128.31(18) . .
N3 C3A N8 109.25(18) . .
N4 C3A N8 122.44(17) . .
C5 N4 C3A 116.20(18) . .
N4 C5 C6 123.0(2) . .
N4 C5 C51 117.2(2) . .
C6 C5 C51 119.8(2) . .
C5 C51 H51 109.4 . .
C5 C51 H52 109.4 . .
H51 C51 H52 109.5 . .
C5 C51 H53 109.6 . .
H51 C51 H53 109.5 . .
H52 C51 H53 109.5 . .
C7 C6 C5 120.7(2) . .
C7 C6 H6 119.7 . .
C5 C6 H6 119.6 . .
C6 C7 N8 115.10(18) . .
C6 C7 C71 126.1(2) . .
N8 C7 C71 118.8(2) . .
C7 C71 H71 109.3 . .
C7 C71 H72 109.5 . .
H71 C71 H72 109.5 . .
C7 C71 H73 109.6 . .
H71 C71 H73 109.5 . .
H72 C71 H73 109.5 . .
N1 N8 C7 127.13(17) . .
N1 N8 C3A 110.37(16) . .
C7 N8 C3A 122.48(17) . .
C1P N1P Cu 122.03(14) . .
C1P N1P H11P 106.9 . .
Cu N1P H11P 106.8 . .
C1P N1P H12P 106.8 . .
Cu N1P H12P 106.8 . .
H11P N1P H12P 106.7 . .
N1P C1P C2P 112.74(17) . .
N1P C1P H13P 108.9 . .
C2P C1P H13P 108.9 . .
N1P C1P H14P 109.1 . .
C2P C1P H14P 109.2 . .
H13P C1P H14P 107.8 . .
C3P C2P C1P 113.60(19) . .
C3P C2P H21P 108.8 . .
C1P C2P H21P 108.7 . .
C3P C2P H22P 108.8 . .
C1P C2P H22P 109.0 . .
H21P C2P H22P 107.7 . .
N3P C3P C2P 111.97(19) . .
N3P C3P H33P 109.2 . .
C2P C3P H33P 109.2 . .
N3P C3P H34P 109.3 . .
C2P C3P H34P 109.1 . .
H33P C3P H34P 107.9 . .
C3P N3P Cu 119.68(14) . .
C3P N3P H31P 107.4 . .
Cu N3P H31P 107.4 . .
C3P N3P H32P 107.2 . .
Cu N3P H32P 107.5 . .
H31P N3P H32P 106.9 . .
O1P Cl O2P 110.95(16) . .
O1P Cl O3P 112.33(16) . .
O2P Cl O3P 108.71(18) . .
O1P Cl O4P 110.29(17) . .
O2P Cl O4P 105.7(2) . .
O3P Cl O4P 108.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N3P 2.0186(17) 2_666
Cu N3P 2.0186(17) .
Cu N1P 2.0384(16) 2_666
Cu N1P 2.0384(16) .
N1 C2 1.329(3) .
N1 N8 1.366(2) .
C2 N3 1.341(3) .
C2 H2 0.9300 .
N3 C3A 1.332(3) .
C3A N4 1.336(3) .
C3A N8 1.368(2) .
N4 C5 1.318(3) .
C5 C6 1.409(3) .
C5 C51 1.502(4) .
C51 H51 0.9600 .
C51 H52 0.9600 .
C51 H53 0.9600 .
C6 C7 1.353(3) .
C6 H6 0.9300 .
C7 N8 1.367(2) .
C7 C71 1.487(3) .
C71 H71 0.9601 .
C71 H72 0.9601 .
C71 H73 0.9601 .
N1P C1P 1.480(3) .
N1P H11P 0.9000 .
N1P H12P 0.9000 .
C1P C2P 1.504(3) .
C1P H13P 0.9700 .
C1P H14P 0.9700 .
C2P C3P 1.503(3) .
C2P H21P 0.9700 .
C2P H22P 0.9700 .
C3P N3P 1.476(3) .
C3P H33P 0.9700 .
C3P H34P 0.9700 .
N3P H31P 0.9000 .
N3P H32P 0.9000 .
Cl O1P 1.415(2) .
Cl O2P 1.418(2) .
Cl O3P 1.421(2) .
Cl O4P 1.437(3) .
