#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/91/1509141.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_1509141
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         'C18 H30 N12 Ni O2'
_chemical_formula_sum            'C18 H30 N12 Ni O2'
_chemical_formula_weight         505.25
_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                 110.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.841(5)
_cell_length_b                   8.667(5)
_cell_length_c                   16.086(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1158.3(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Axs APEX automatic diffractometer'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5971
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0467P)²+0.2774P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                1850
_reflns_number_total             2042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Compound2a.cif
_cod_data_source_block           compound_2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Wrong last page number
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1509141
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
Ni1 Ni 0.0000 0.0000 -0.5000 0.02820(13) Uani 1 2 d S
O71A O 0.32056(18) -0.4403(2) -0.14647(9) 0.0509(4) Uani 1 1 d .
N1A N 0.0782(2) -0.2377(2) -0.24911(10) 0.0429(4) Uani 1 1 d .
N1B N 0.0775(2) -0.18510(17) -0.55870(10) 0.0372(4) Uani 1 1 d .
H11B H 0.1831 -0.1991 -0.5288 0.045 Uiso 1 1 d R
H12B H 0.0681 -0.1566 -0.6141 0.045 Uiso 1 1 d R
N3A N 0.08550(19) -0.12478(18) -0.37486(9) 0.0340(4) Uani 1 1 d .
N4A N 0.33415(19) -0.23595(18) -0.37548(10) 0.0363(4) Uani 1 1 d .
N5B N -0.2349(2) -0.09333(19) -0.52478(10) 0.0401(4) Uani 1 1 d .
H52B H -0.3029 -0.0414 -0.5710 0.048 Uiso 1 1 d R
H51B H -0.2634 -0.0713 -0.4775 0.048 Uiso 1 1 d R
N8A N 0.21367(18) -0.28177(18) -0.26626(9) 0.0330(4) Uani 1 1 d .
C3AA C 0.2174(2) -0.2142(2) -0.34226(11) 0.0307(4) Uani 1 1 d .
C2A C 0.0089(2) -0.1451(2) -0.31568(12) 0.0399(5) Uani 1 1 d .
H2A H -0.0879 -0.0958 -0.3220 0.048 Uiso 1 1 calc R
C2B C -0.0017(3) -0.3338(2) -0.56426(14) 0.0495(6) Uani 1 1 d .
H21B H 0.0267 -0.3774 -0.5054 0.059 Uiso 1 1 calc R
H22B H 0.0374 -0.4034 -0.5996 0.059 Uiso 1 1 calc R
C3B C -0.1802(3) -0.3223(3) -0.60402(16) 0.0623(7) Uani 1 1 d .
H32B H -0.2229 -0.4243 -0.6236 0.075 Uiso 1 1 calc R
H31B H -0.2066 -0.2569 -0.6560 0.075 Uiso 1 1 calc R
C4B C -0.2645(3) -0.2591(3) -0.54343(16) 0.0557(6) Uani 1 1 d .
H42B H -0.3794 -0.2761 -0.5706 0.067 Uiso 1 1 calc R
H41B H -0.2280 -0.3156 -0.4880 0.067 Uiso 1 1 calc R
C5A C 0.4517(2) -0.3317(2) -0.32773(13) 0.0384(5) Uani 1 1 d .
C6A C 0.4551(2) -0.4033(2) -0.25094(13) 0.0400(5) Uani 1 1 d .
H6A H 0.5413 -0.4675 -0.2221 0.048 Uiso 1 1 calc R
C7A C 0.3327(2) -0.3830(2) -0.21410(12) 0.0366(4) Uani 1 1 d .
C51A C 0.5843(3) -0.3578(3) -0.36473(17) 0.0621(7) Uani 1 1 d .
H51A H 0.6324 -0.2606 -0.3701 0.093 Uiso 1 1 calc R
H52A H 0.5409 -0.4052 -0.4219 0.093 Uiso 1 1 calc R
H53A H 0.6645 -0.4241 -0.3258 0.093 Uiso 1 1 calc R
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'
Ni Ni 0.3393 1.1124 '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'
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
N1B Ni1 N1B 180.0 . 3_554
N1B Ni1 N5B 94.19(7) . .
N1B Ni1 N5B 85.81(7) 3_554 .
N1B Ni1 N5B 85.81(7) . 3_554
N1B Ni1 N5B 94.19(7) 3_554 3_554
N5B Ni1 N5B 180.0 . 3_554
N1B Ni1 N3A 91.56(6) . 3_554
N1B Ni1 N3A 88.44(6) 3_554 3_554
N5B Ni1 N3A 90.44(6) . 3_554
N5B Ni1 N3A 89.56(6) 3_554 3_554
N1B Ni1 N3A 88.44(6) . .
N1B Ni1 N3A 91.56(6) 3_554 .
N5B Ni1 N3A 89.56(6) . .
N5B Ni1 N3A 90.44(6) 3_554 .
N3A Ni1 N3A 180.00(5) 3_554 .
C2A N1A N8A 101.69(15) . .
C2B N1B Ni1 118.83(13) . .
C2B N1B H11B 107.6 . .
Ni1 N1B H11B 107.6 . .
C2B N1B H12B 107.6 . .
Ni1 N1B H12B 107.6 . .
H11B N1B H12B 107.0 . .
C3AA N3A C2A 103.05(15) . .
C3AA N3A Ni1 128.70(12) . .
C2A N3A Ni1 127.89(13) . .
C3AA N4A C5A 114.35(16) . .
C4B N5B Ni1 120.09(14) . .
C4B N5B H52B 107.3 . .
Ni1 N5B H52B 107.3 . .
C4B N5B H51B 107.3 . .
Ni1 N5B H51B 107.3 . .
H52B N5B H51B 106.9 . .
C3AA N8A N1A 110.50(15) . .
C3AA N8A C7A 124.02(16) . .
N1A N8A C7A 125.48(15) . .
N4A C3AA N3A 127.79(16) . .
N4A C3AA N8A 123.99(17) . .
N3A C3AA N8A 108.21(16) . .
N1A C2A N3A 116.55(18) . .
N1A C2A H2A 121.7 . .
N3A C2A H2A 121.7 . .
N1B C2B C3B 112.58(19) . .
N1B C2B H21B 109.1 . .
C3B C2B H21B 109.1 . .
N1B C2B H22B 109.1 . .
C3B C2B H22B 109.1 . .
H21B C2B H22B 107.8 . .
C2B C3B C4B 115.4(2) . .
C2B C3B H32B 108.4 . .
C4B C3B H32B 108.4 . .
C2B C3B H31B 108.4 . .
C4B C3B H31B 108.4 . .
H32B C3B H31B 107.5 . .
N5B C4B C3B 113.01(19) . .
N5B C4B H42B 109.0 . .
C3B C4B H42B 109.0 . .
N5B C4B H41B 109.0 . .
C3B C4B H41B 109.0 . .
H42B C4B H41B 107.8 . .
N4A C5A C6A 124.51(18) . .
N4A C5A C51A 114.91(18) . .
C6A C5A C51A 120.58(19) . .
C5A C6A C7A 122.53(18) . .
C5A C6A H6A 118.7 . .
C7A C6A H6A 118.7 . .
O71A C7A N8A 120.28(18) . .
O71A C7A C6A 129.12(19) . .
N8A C7A C6A 110.60(16) . .
C5A C51A H51A 109.5 . .
C5A C51A H52A 109.5 . .
H51A C51A H52A 109.5 . .
C5A C51A H53A 109.5 . .
H51A C51A H53A 109.5 . .
H52A C51A H53A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1B 2.0922(17) .
Ni1 N1B 2.0922(17) 3_554
Ni1 N5B 2.1353(19) .
Ni1 N5B 2.1353(19) 3_554
Ni1 N3A 2.1800(15) 3_554
Ni1 N3A 2.1800(15) .
O71A C7A 1.233(2) .
N1A C2A 1.311(3) .
N1A N8A 1.372(2) .
N1B C2B 1.455(3) .
N1B H11B 0.9000 .
N1B H12B 0.9001 .
N3A C3AA 1.348(2) .
N3A C2A 1.355(2) .
N4A C3AA 1.328(2) .
N4A C5A 1.347(3) .
N5B C4B 1.473(3) .
N5B H52B 0.9000 .
N5B H51B 0.9000 .
N8A C3AA 1.366(2) .
N8A C7A 1.406(2) .
C2A H2A 0.9300 .
C2B C3B 1.490(4) .
C2B H21B 0.9700 .
C2B H22B 0.9700 .
C3B C4B 1.517(4) .
C3B H32B 0.9700 .
C3B H31B 0.9700 .
C4B H42B 0.9700 .
C4B H41B 0.9700 .
C5A C6A 1.373(3) .
C5A C51A 1.503(3) .
C6A C7A 1.411(3) .
C6A H6A 0.9300 .
C51A H51A 0.9600 .
C51A H52A 0.9600 .
C51A H53A 0.9600 .
