#------------------------------------------------------------------------------
#$Date: 2016-02-18 13:25:00 +0100 (jue 18 de feb de 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/20/8102029.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_8102029
loop_
_publ_author_name
'Xu, S.-P.'
'Liu, C.-H.'
'Zhu, Y.'
_publ_section_title
;
Crystal structure of tetra(2-aminopyrimidine)di-methanolato-dicobalt
(II) diperchlorate, [Co₂(CH₃O)₂(C₄H₅N₃)₄][ClO₄]₂
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              401
_journal_page_last               402
_journal_volume                  221
_journal_year                    2006
_chemical_formula_moiety         '(C18H26CoN6O2), 2(ClO4)'
_chemical_formula_structural     '[Co2(CH3O)2(C4H5N3)4][ClO4]2'
_chemical_formula_sum            'C18 H26 Cl2 Co2 N12 O10'
_chemical_formula_weight         759.26
_chemical_name_systematic
; 
tetra(2-aminopyrimidine)dimethanolato-dicobalt(II) diperchlorate 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 132.400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.466(5)
_cell_length_b                   14.969(5)
_cell_length_c                   12.003(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2184.7(13)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4544
_diffrn_reflns_theta_full        26.54
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS [8]'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0532
_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)+(0.1200P)²+0.2251P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                1864
_reflns_number_total             2359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1847.cff
_cod_data_source_block           co6
_cod_original_cell_volume        2184.7(12)
_cod_original_sg_symbol_H-M      C12/m1
_cod_database_code               8102029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.09856(4) 0.0000 0.0432(3) Uani 1 4 g d S . .
O1 O 0.0254(3) 0.0000 0.1238(4) 0.0507(8) Uani 1 4 i d S . .
O2 O 0.2792(3) 0.4222(2) 0.8604(4) 0.0789(9) Uani 1 8 j d . . .
O3 O 0.1871(5) 0.5000 0.6380(7) 0.1016(17) Uani 1 4 i d S . .
O4 O 0.1211(5) 0.5000 0.7646(9) 0.110(2) Uani 1 4 i d S . .
N1 N 0.0090(3) 0.1942(2) 0.1266(4) 0.0616(9) Uani 1 8 j d . . .
N2 N 0.1883(3) 0.1658(3) 0.3397(4) 0.0880(14) Uani 1 8 j d . . .
H3A H 0.2488 0.1793 0.4354 0.080 Uiso 1 8 j d R . .
H3B H 0.1893 0.1194 0.2929 0.080 Uiso 1 8 j d R . .
N3 N 0.1047(3) 0.2836(3) 0.3472(4) 0.0807(12) Uani 1 8 j d . . .
C1 C 0.0996(3) 0.2146(3) 0.2688(5) 0.0633(11) Uani 1 8 j d . . .
C2 C 0.0152(4) 0.3306(4) 0.2802(6) 0.0887(17) Uani 1 8 j d . . .
H2A H 0.0170 0.3786 0.3349 0.080 Uiso 1 8 j d R . .
C3 C -0.0826(5) 0.3128(4) 0.1353(7) 0.0945(18) Uani 1 8 j d . . .
H3C H -0.1484 0.3463 0.0893 0.080 Uiso 1 8 j d R . .
C4 C -0.0815(4) 0.2447(3) 0.0599(6) 0.0778(13) Uani 1 8 j d . . .
H4A H -0.1466 0.2330 -0.0432 0.080 Uiso 1 8 j d R . .
C5 C -0.0055(7) 0.0000 0.2083(8) 0.0788(19) Uani 1 4 i d S . .
H5A H 0.0152 -0.0557 0.2612 0.080 Uiso 0.50 8 j d PR . .
H5B H 0.0303 0.0483 0.2796 0.080 Uiso 0.50 8 j d PR . .
H5C H -0.0838 0.0074 0.1409 0.080 Uiso 0.50 8 j d PR . .
Cl1 Cl 0.21447(12) 0.5000 0.78045(19) 0.0640(4) Uani 1 4 i d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0543(5) 0.0309(4) 0.0359(4) 0.000 0.0271(3) 0.000
O1 0.060(2) 0.0445(19) 0.0476(18) 0.000 0.0361(17) 0.000
O2 0.080(2) 0.0531(17) 0.101(2) 0.0072(16) 0.060(2) 0.0081(15)
O3 0.118(4) 0.089(4) 0.081(3) 0.000 0.060(3) 0.000
O4 0.091(4) 0.070(3) 0.197(6) 0.000 0.110(4) 0.000
N1 0.069(2) 0.0470(18) 0.0534(18) -0.0040(14) 0.0351(16) 0.0070(15)
N2 0.072(2) 0.087(3) 0.062(2) -0.027(2) 0.0276(19) 0.020(2)
N3 0.075(2) 0.071(3) 0.069(2) -0.0219(19) 0.038(2) 0.012(2)
C1 0.065(2) 0.055(2) 0.055(2) -0.0128(18) 0.0346(19) 0.0036(19)
C2 0.083(3) 0.075(3) 0.084(3) -0.027(3) 0.047(3) 0.013(3)
C3 0.079(3) 0.075(3) 0.094(4) -0.013(3) 0.044(3) 0.019(3)
C4 0.071(3) 0.056(3) 0.072(3) -0.009(2) 0.035(2) 0.010(2)
C5 0.105(5) 0.080(5) 0.072(4) 0.000 0.068(4) 0.000
Cl1 0.0606(8) 0.0461(7) 0.0876(10) 0.000 0.0509(8) 0.000
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'
Co Co 0.3494 0.9721 '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
O1 Co1 O1 80.23(16) 5 . ?
O1 Co1 N1 171.77(14) 5 . ?
O1 Co1 N1 95.44(13) . . ?
O1 Co1 N1 95.44(13) 5 2 ?
O1 Co1 N1 171.77(14) . 2 ?
N1 Co1 N1 89.7(2) . 2 ?
O1 Co1 Co1 40.11(8) 5 5 ?
O1 Co1 Co1 40.11(8) . 5 ?
N1 Co1 Co1 135.16(10) . 5 ?
N1 Co1 Co1 135.16(10) 2 5 ?
C5 O1 Co1 123.96(18) . 5 ?
C5 O1 Co1 123.96(18) . . ?
Co1 O1 Co1 99.77(16) 5 . ?
C1 N1 C4 117.6(4) . . ?
C1 N1 Co1 125.0(3) . . ?
C4 N1 Co1 117.3(3) . . ?
C1 N2 H3A 119.6 . . ?
C1 N2 H3B 120.4 . . ?
H3A N2 H3B 120.0 . . ?
C2 N3 C1 117.6(4) . . ?
N2 C1 N1 119.7(4) . . ?
N2 C1 N3 116.9(4) . . ?
N1 C1 N3 123.4(4) . . ?
N3 C2 C3 122.9(4) . . ?
N3 C2 H2A 118.6 . . ?
C3 C2 H2A 118.4 . . ?
C4 C3 C2 116.8(5) . . ?
C4 C3 H3C 121.3 . . ?
C2 C3 H3C 122.0 . . ?
N1 C4 C3 121.7(4) . . ?
N1 C4 H4A 119.2 . . ?
C3 C4 H4A 119.1 . . ?
O1 C5 H5A 109.7 . . ?
O1 C5 H5B 109.8 . . ?
H5A C5 H5B 109.5 . . ?
O1 C5 H5C 108.9 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 Cl1 O2 110.0(2) . 6_565 ?
O4 Cl1 O2 110.0(2) . . ?
O2 Cl1 O2 109.5(3) 6_565 . ?
O4 Cl1 O3 113.4(4) . . ?
O2 Cl1 O3 107.0(2) 6_565 . ?
O2 Cl1 O3 107.0(2) . . ?
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 O1 1.929(2) 5 ?
Co1 O1 1.929(2) . ?
Co1 N1 2.020(3) . ?
Co1 N1 2.020(3) 2 ?
Co1 Co1 2.9508(15) 5 ?
O1 C5 1.409(7) . ?
O1 Co1 1.929(2) 5 ?
O2 Cl1 1.427(3) . ?
O3 Cl1 1.444(6) . ?
O4 Cl1 1.416(5) . ?
N1 C1 1.341(5) . ?
N1 C4 1.351(5) . ?
N2 C1 1.310(5) . ?
N2 H3A 0.9000 . ?
N2 H3B 0.8999 . ?
N3 C2 1.309(6) . ?
N3 C1 1.361(5) . ?
C2 C3 1.383(7) . ?
C2 H2A 0.9599 . ?
C3 C4 1.372(7) . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9601 . ?
C5 H5C 0.9600 . ?
Cl1 O2 1.427(3) 6_565 ?
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 H3B O3 0.90 2.40 3.115(6) 136.7 7_556
N2 H3B O2 0.90 2.31 3.085(5) 144.4 7_556
N2 H3A N3 0.90 2.11 3.006(5) 175.4 7_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Co1 O1 C5 -143.1(5) 5 . . . ?
N1 Co1 O1 C5 29.9(5) . . . . ?
N1 Co1 O1 C5 158.1(8) 2 . . . ?
Co1 Co1 O1 C5 -143.1(5) 5 . . . ?
O1 Co1 O1 Co1 0.0 5 . . 5 ?
N1 Co1 O1 Co1 172.93(14) . . . 5 ?
N1 Co1 O1 Co1 -58.8(9) 2 . . 5 ?
O1 Co1 N1 C1 123.4(8) 5 . . . ?
O1 Co1 N1 C1 65.5(4) . . . . ?
N1 Co1 N1 C1 -108.1(4) 2 . . . ?
Co1 Co1 N1 C1 71.9(4) 5 . . . ?
O1 Co1 N1 C4 -60.5(10) 5 . . . ?
O1 Co1 N1 C4 -118.4(4) . . . . ?
N1 Co1 N1 C4 68.1(4) 2 . . . ?
Co1 Co1 N1 C4 -111.9(4) 5 . . . ?
C4 N1 C1 N2 178.0(5) . . . . ?
Co1 N1 C1 N2 -5.9(7) . . . . ?
C4 N1 C1 N3 -0.9(7) . . . . ?
Co1 N1 C1 N3 175.2(4) . . . . ?
C2 N3 C1 N2 -177.1(6) . . . . ?
C2 N3 C1 N1 1.8(8) . . . . ?
C1 N3 C2 C3 0.1(9) . . . . ?
N3 C2 C3 C4 -2.6(10) . . . . ?
C1 N1 C4 C3 -1.9(8) . . . . ?
Co1 N1 C4 C3 -178.3(4) . . . . ?
C2 C3 C4 N1 3.5(9) . . . . ?
