#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:39:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179856 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/52/7015272.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_7015272
loop_
_publ_author_name
'Caballero, Ana B.'
'Rodríguez-Diéguez, Antonio'
'Lezama, Luis'
'Barea, Elisa'
'Salas, Juan M.'
_publ_section_title
;
 Structural and magnetic properties of three novel complexes with the
 versatile ligand 5-methyl-1,2,4-triazolo[1,5-a]pyrimidin-7(4H)-one.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5180
_journal_page_last               5187
_journal_paper_doi               10.1039/c0dt01416h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C6 H15 Cl2 Co N4 O14'
_chemical_formula_weight         497.05
_chemical_name_systematic
;
?
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.923(5)
_cell_length_b                   6.542(5)
_cell_length_c                   10.446(5)
_cell_measurement_reflns_used    3102
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.40
_cell_measurement_theta_min      2.51
_cell_volume                     883.1(9)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9737
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.98(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2149
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0536
_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)+(0.0926P)²+0.8821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                1948
_reflns_number_total             2149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01416h.txt
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      Pmn21
_cod_database_code               7015272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, 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
Co1 Co 0.0000 0.65650(11) 0.31211(6) 0.0280(2) Uani 1 2 d S . .
O1W O 0.1577(3) 0.6617(5) 0.3105(7) 0.0527(10) Uani 1 1 d D . .
O2W O 0.0000 0.5886(11) 0.1172(6) 0.0434(14) Uani 1 2 d S . .
071A O 0.0000 0.7189(8) 0.5145(5) 0.0387(11) Uani 1 2 d S . .
N1A N 0.0000 0.9917(7) 0.3219(7) 0.0304(10) Uani 1 2 d S . .
N8A N 0.0000 1.0420(8) 0.4488(5) 0.0270(10) Uani 1 2 d S . .
C2A C 0.0000 1.1745(9) 0.2662(7) 0.0307(13) Uani 1 2 d S . .
H2A H 0.0000 1.1908 0.1778 0.037 Uiso 1 2 calc SR . .
C7A C 0.0000 0.9037(9) 0.5475(6) 0.0299(13) Uani 1 2 d S . .
C6A C 0.0000 0.9905(9) 0.6682(6) 0.0331(14) Uani 1 2 d S . .
H6A H 0.0000 0.9060 0.7398 0.040 Uiso 1 2 calc SR . .
C5A C 0.0000 1.1992(10) 0.6846(7) 0.0364(15) Uani 1 2 d S . .
C51A C 0.0000 1.3039(10) 0.8113(10) 0.0490(18) Uani 1 2 d S . .
H51A H -0.0450 1.4205 0.8080 0.073 Uiso 0.50 1 calc PR . .
H51B H 0.0690 1.3478 0.8316 0.073 Uiso 0.50 1 calc PR . .
H51C H -0.0239 1.2110 0.8760 0.073 Uiso 0.50 1 calc PR . .
Cl1B Cl 0.29272(10) 1.1081(3) 0.46473(16) 0.0483(4) Uani 1 1 d . . .
O2B O 0.3632(13) 0.987(2) 0.5179(11) 0.203(7) Uani 1 1 d . . .
O5B O 0.2562(7) 1.0435(11) 0.3450(6) 0.103(2) Uani 1 1 d . . .
O4B O 0.3493(12) 1.285(2) 0.4489(11) 0.204(8) Uani 1 1 d . . .
O3W O 0.2731(7) 1.3993(11) 0.1697(7) 0.094(2) Uani 1 1 d . . .
O3B O 0.2191(8) 1.127(3) 0.5504(13) 0.208(10) Uani 1 1 d . . .
N3A N 0.0000 1.3351(8) 0.3481(5) 0.0316(13) Uani 1 2 d S . .
N4A N 0.0000 1.3225(7) 0.5808(6) 0.0307(12) Uani 1 2 d S . .
C3AA C 0.0000 1.2462(9) 0.4625(6) 0.0256(11) Uani 1 2 d S . .
H11W H 0.200(5) 0.765(9) 0.293(10) 0.08(2) Uiso 1 1 d D . .
H31W H 0.227(8) 1.449(12) 0.099(11) 0.09(3) Uiso 1 1 d D . .
H32W H 0.240(5) 1.278(11) 0.138(7) 0.046(17) Uiso 1 1 d D . .
H12W H 0.198(5) 0.582(11) 0.263(7) 0.07(3) Uiso 1 1 d D . .
H22W H 0.034(7) 0.635(13) 0.085(9) 0.08(4) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
H H 0.0000 0.0000 '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
O1W Co1 O1W 177.9(3) . 3 ?
O1W Co1 O2W 89.8(2) . . ?
O1W Co1 O2W 89.8(2) 3 . ?
O1W Co1 N3A 91.02(10) . 1_545 ?
O1W Co1 N3A 91.02(10) 3 1_545 ?
O2W Co1 N3A 87.8(3) . 1_545 ?
O1W Co1 071A 90.3(2) . . ?
O1W Co1 071A 90.3(2) 3 . ?
O2W Co1 071A 178.6(3) . . ?
N3A Co1 071A 90.79(19) 1_545 . ?
O1W Co1 N1A 89.06(10) . . ?
O1W Co1 N1A 89.06(10) 3 . ?
O2W Co1 N1A 105.0(3) . . ?
N3A Co1 N1A 167.2(2) 1_545 . ?
071A Co1 N1A 76.4(2) . . ?
Co1 O1W H11W 129(5) . . ?
Co1 O1W H12W 126(5) . . ?
H11W O1W H12W 88(8) . . ?
Co1 O2W H22W 115(9) . . ?
C7A 071A Co1 116.8(4) . . ?
C2A N1A N8A 102.0(5) . . ?
C2A N1A Co1 151.4(5) . . ?
N8A N1A Co1 106.6(4) . . ?
C3AA N8A N1A 110.1(5) . . ?
C3AA N8A C7A 125.1(6) . . ?
N1A N8A C7A 124.8(5) . . ?
N1A C2A N3A 114.9(6) . . ?
N1A C2A H2A 122.5 . . ?
N3A C2A H2A 122.5 . . ?
071A C7A N8A 115.4(6) . . ?
071A C7A C6A 130.1(6) . . ?
N8A C7A C6A 114.5(6) . . ?
C5A C6A C7A 121.4(6) . . ?
C5A C6A H6A 119.3 . . ?
C7A C6A H6A 119.3 . . ?
N4A C5A C6A 119.5(6) . . ?
N4A C5A C51A 116.0(6) . . ?
C6A C5A C51A 124.6(6) . . ?
C5A C51A H51A 109.5 . . ?
C5A C51A H51B 109.5 . . ?
H51A C51A H51B 109.5 . . ?
C5A C51A H51C 109.5 . . ?
H51A C51A H51C 109.5 . . ?
H51B C51A H51C 109.5 . . ?
O3B Cl1B O2B 105.6(11) . . ?
O3B Cl1B O4B 112.8(10) . . ?
O2B Cl1B O4B 100.8(11) . . ?
O3B Cl1B O5B 113.1(7) . . ?
O2B Cl1B O5B 115.1(6) . . ?
O4B Cl1B O5B 108.9(5) . . ?
H31W O3W H32W 76(5) . . ?
C3AA N3A C2A 103.2(5) . . ?
C3AA N3A Co1 126.1(4) . 1_565 ?
C2A N3A Co1 130.7(5) . 1_565 ?
C3AA N4A C5A 121.3(5) . . ?
N3A C3AA N4A 132.0(5) . . ?
N3A C3AA N8A 109.8(5) . . ?
N4A C3AA N8A 118.1(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
Co1 O1W 2.038(4) . ?
Co1 O1W 2.038(4) 3 ?
Co1 O2W 2.084(7) . ?
Co1 N3A 2.136(6) 1_545 ?
Co1 071A 2.154(5) . ?
Co1 N1A 2.195(5) . ?
O1W H11W 0.89(2) . ?
O1W H12W 0.89(2) . ?
O2W H22W 0.63(9) . ?
071A C7A 1.257(8) . ?
N1A C2A 1.330(8) . ?
N1A N8A 1.366(9) . ?
N8A C3AA 1.343(8) . ?
N8A C7A 1.372(8) . ?
C2A N3A 1.355(8) . ?
C2A H2A 0.9300 . ?
C7A C6A 1.382(10) . ?
C6A C5A 1.376(9) . ?
C6A H6A 0.9300 . ?
C5A N4A 1.352(9) . ?
C5A C51A 1.490(12) . ?
C51A H51A 0.9600 . ?
C51A H51B 0.9600 . ?
C51A H51C 0.9600 . ?
Cl1B O3B 1.312(10) . ?
Cl1B O2B 1.330(9) . ?
Cl1B O4B 1.377(9) . ?
Cl1B O5B 1.402(6) . ?
O3W H31W 1.00(11) . ?
O3W H32W 0.96(7) . ?
N3A C3AA 1.329(8) . ?
N3A Co1 2.136(6) 1_565 ?
N4A C3AA 1.333(8) . ?
