#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305070.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_4305070
loop_
_publ_author_name
'Garikoitz Beobide'
'Wen-guo Wang'
'Oscar Castillo'
'Antonio Luque'
'Pascual Román'
'Giulia Tagliabue'
'Simona Galli'
'Jorge A. R. Navarro'
_publ_contact_author
;
 Oscar Castillo. Departamento de Quimica Inorganica. 
 Facultad de Ciencia y Tecnologia
 Universidad del Pais Vasco,  Apdo. 644, E-48080 Bilbao, Spain
;
_publ_contact_author_email       qipcacao@lg.ehu.es
_publ_contact_author_fax         '+34-946 013 500'
_publ_contact_author_phone       '+34-946 015 991'
_publ_section_title
;
Manganese(II) Pyrimidine-4,6-dicarboxylates: Synthetic, Structural,
Magnetic, and Adsorption Insights
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5267
_journal_page_last               5277
_journal_paper_doi               10.1021/ic8002788
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C12 H14 Mn2 N4 O13, 2(H2 O)'
_chemical_formula_structural     'C12 H14 Mn2 N4 O13, 2(H2 O)'
_chemical_formula_sum            'C12 H18 Mn2 N4 O15'
_chemical_formula_weight         568.18
_chemical_name_systematic
;
catena-[di(mu-pyrimidine-4,6-dicarboxylato-N,O:N,O)-
pentaacua-dimanganese(II)-water (1/2)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                100.18(1)
_cell_angle_beta                 103.52(1)
_cell_angle_gamma                103.82(1)
_cell_formula_units_Z            2
_cell_length_a                   7.767(1)
_cell_length_b                   10.281(2)
_cell_length_c                   13.451(2)
_cell_measurement_reflns_used    4729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      3.21
_cell_volume                     982.8(3)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altamore et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ω
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8240
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_density_meas      1.91(1)
_exptl_crystal_density_method    'flotation method'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.800
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.800
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0412
_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)+(0.0225P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                2723
_reflns_number_total             4729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8002788-file003_2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        982.9(3)
_cod_database_code               4305070
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.21733(6) 0.99845(5) 0.80428(4) 0.02304(12) Uani 1 1 d . . .
Mn2 Mn 0.81023(6) 1.49167(5) 0.70035(4) 0.02509(13) Uani 1 1 d . . .
O2W O 0.3474(3) 0.8340(2) 0.79261(17) 0.0376(6) Uani 1 1 d . . .
H2WB H 0.4099 0.8242 0.7492 0.056 Uiso 1 1 d . . .
H2WA H 0.3902 0.7980 0.8428 0.056 Uiso 1 1 d . . .
O1W O 0.0002(3) 0.9059(2) 0.86155(19) 0.0420(6) Uani 1 1 d . . .
H1WB H -0.0891 0.9336 0.8765 0.063 Uiso 1 1 d . . .
H1WA H -0.0141 0.8237 0.8713 0.063 Uiso 1 1 d . . .
O4W O 0.7636(3) 1.6792(2) 0.64799(18) 0.0414(6) Uani 1 1 d . . .
H4WB H 0.8527 1.7508 0.6528 0.062 Uiso 1 1 d . . .
H4WA H 0.6704 1.7087 0.6558 0.062 Uiso 1 1 d . . .
O3W O 0.5606(3) 1.5015(2) 0.75428(17) 0.0406(6) Uani 1 1 d . . .
H3WB H 0.5603 1.5689 0.8027 0.061 Uiso 1 1 d . . .
H3WA H 0.4583 1.4782 0.7050 0.061 Uiso 1 1 d . . .
O5W O 1.0638(3) 1.5762(2) 0.65841(18) 0.0434(6) Uani 1 1 d . . .
H5WA H 1.1224 1.5261 0.6305 0.065 Uiso 1 1 d . . .
H5WB H 1.1125 1.6573 0.6767 0.065 Uiso 1 1 d . . .
O6W O -0.2376(3) 0.6100(2) 0.41226(17) 0.0394(6) Uani 1 1 d . . .
H6WB H -0.1360 0.6779 0.4316 0.059 Uiso 1 1 d . . .
H6WA H -0.2519 0.5880 0.4701 0.059 Uiso 1 1 d . . .
O7W O -0.2436(3) 1.0441(2) 0.88888(19) 0.0503(7) Uani 1 1 d . . .
H7WB H -0.2091 1.1256 0.9303 0.075 Uiso 1 1 d . . .
H7WA H -0.3340 0.9966 0.9080 0.075 Uiso 1 1 d . . .
N11 N 0.1498(3) 1.2091(2) 0.83439(18) 0.0211(5) Uani 1 1 d . . .
C12 C 0.0319(4) 1.2593(3) 0.7746(2) 0.0249(7) Uani 1 1 d . . .
H12 H -0.0408 1.2021 0.7092 0.030 Uiso 1 1 calc R . .
N13 N 0.0089(3) 1.3838(2) 0.79997(18) 0.0224(6) Uani 1 1 d . . .
C14 C 0.1156(4) 1.4665(3) 0.8930(2) 0.0198(6) Uani 1 1 d . . .
C15 C 0.2435(4) 1.4243(3) 0.9599(2) 0.0229(7) Uani 1 1 d . . .
H15 H 0.3185 1.4826 1.0245 0.027 Uiso 1 1 calc R . .
C16 C 0.2560(4) 1.2941(3) 0.9278(2) 0.0208(7) Uani 1 1 d . . .
C17 C 0.0831(4) 1.6060(3) 0.9245(2) 0.0223(7) Uani 1 1 d . . .
C18 C 0.3870(4) 1.2332(3) 0.9963(2) 0.0234(7) Uani 1 1 d . . .
N23 N 0.6077(3) 1.2570(2) 0.66093(18) 0.0223(6) Uani 1 1 d . . .
C22 C 0.5340(4) 1.1975(3) 0.7267(2) 0.0243(7) Uani 1 1 d . . .
H22 H 0.5950 1.2322 0.7984 0.029 Uiso 1 1 calc R . .
N21 N 0.3792(3) 1.0917(2) 0.69912(18) 0.0218(6) Uani 1 1 d . . .
C26 C 0.2960(4) 1.0391(3) 0.5956(2) 0.0197(6) Uani 1 1 d . . .
C25 C 0.3653(4) 1.0914(3) 0.5217(2) 0.0217(7) Uani 1 1 d . . .
H25 H 0.3088 1.0528 0.4500 0.026 Uiso 1 1 calc R . .
C24 C 0.5224(4) 1.2038(3) 0.5576(2) 0.0200(6) Uani 1 1 d . . .
C27 C 0.1197(4) 0.9198(3) 0.5673(2) 0.0220(7) Uani 1 1 d . . .
C28 C 0.6045(4) 1.2797(3) 0.4852(2) 0.0242(7) Uani 1 1 d . . .
O172 O 0.1764(3) 1.6812(2) 1.01211(16) 0.0327(5) Uani 1 1 d . . .
O171 O -0.0420(3) 1.6318(2) 0.85746(16) 0.0278(5) Uani 1 1 d . . .
O181 O 0.4009(3) 1.1191(2) 0.95337(15) 0.0300(5) Uani 1 1 d . . .
O182 O 0.4687(3) 1.3004(2) 1.08792(16) 0.0340(6) Uani 1 1 d . . .
O281 O 0.0540(3) 0.8983(2) 0.64324(15) 0.0275(5) Uani 1 1 d . . .
O282 O 0.0543(3) 0.8535(2) 0.47440(15) 0.0313(5) Uani 1 1 d . . .
O271 O 0.7156(3) 1.3978(2) 0.52927(16) 0.0386(6) Uani 1 1 d . . .
O272 O 0.5527(3) 1.2210(2) 0.39009(16) 0.0319(5) 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'
Mn Mn 0.3368 0.7283 '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 Mn1 O181 96.57(9) . . ?
O1W Mn1 O281 91.29(9) . . ?
O181 Mn1 O281 171.45(8) . . ?
O1W Mn1 O2W 98.89(8) . . ?
O181 Mn1 O2W 96.00(8) . . ?
O281 Mn1 O2W 86.04(8) . . ?
O1W Mn1 N21 162.62(9) . . ?
O181 Mn1 N21 98.29(9) . . ?
O281 Mn1 N21 73.43(8) . . ?
O2W Mn1 N21 88.48(8) . . ?
O1W Mn1 N11 90.99(8) . . ?
O181 Mn1 N11 73.38(8) . . ?
O281 Mn1 N11 103.24(8) . . ?
O2W Mn1 N11 166.34(9) . . ?
N21 Mn1 N11 84.70(8) . . ?
O5W Mn2 O271 80.02(9) . . ?
O5W Mn2 O171 85.24(8) . 1_655 ?
O271 Mn2 O171 163.38(8) . 1_655 ?
O5W Mn2 O3W 155.40(8) . . ?
O271 Mn2 O3W 108.00(9) . . ?
O171 Mn2 O3W 82.64(8) 1_655 . ?
O5W Mn2 O4W 77.06(8) . . ?
O271 Mn2 O4W 82.70(9) . . ?
O171 Mn2 O4W 86.56(8) 1_655 . ?
O3W Mn2 O4W 80.91(8) . . ?
O5W Mn2 N13 81.38(8) . 1_655 ?
O271 Mn2 N13 113.91(8) . 1_655 ?
O171 Mn2 N13 70.96(8) 1_655 1_655 ?
O3W Mn2 N13 114.32(8) . 1_655 ?
O4W Mn2 N13 150.00(9) . 1_655 ?
O5W Mn2 N23 131.69(8) . . ?
O271 Mn2 N23 69.12(8) . . ?
O171 Mn2 N23 127.21(8) 1_655 . ?
O3W Mn2 N23 71.97(8) . . ?
O4W Mn2 N23 131.46(8) . . ?
N13 Mn2 N23 78.54(8) 1_655 . ?
Mn1 O2W H2WB 121.1 . . ?
Mn1 O2W H2WA 126.9 . . ?
H2WB O2W H2WA 105.9 . . ?
Mn1 O1W H1WB 131.8 . . ?
Mn1 O1W H1WA 121.0 . . ?
H1WB O1W H1WA 107.2 . . ?
Mn2 O4W H4WB 123.1 . . ?
Mn2 O4W H4WA 121.7 . . ?
H4WB O4W H4WA 106.8 . . ?
Mn2 O3W H3WB 123.3 . . ?
Mn2 O3W H3WA 115.3 . . ?
H3WB O3W H3WA 108.5 . . ?
Mn2 O5W H5WA 123.8 . . ?
Mn2 O5W H5WB 118.8 . . ?
H5WA O5W H5WB 116.9 . . ?
H6WB O6W H6WA 105.7 . . ?
H7WB O7W H7WA 105.2 . . ?
C12 N11 C16 116.2(2) . . ?
C12 N11 Mn1 131.6(2) . . ?
C16 N11 Mn1 112.14(18) . . ?
N13 C12 N11 126.0(3) . . ?
N13 C12 H12 117.0 . . ?
N11 C12 H12 117.0 . . ?
C12 N13 C14 116.9(2) . . ?
C12 N13 Mn2 130.10(18) . 1_455 ?
C14 N13 Mn2 112.95(18) . 1_455 ?
N13 C14 C15 121.4(3) . . ?
N13 C14 C17 117.0(2) . . ?
C15 C14 C17 121.6(3) . . ?
C16 C15 C14 117.7(3) . . ?
C16 C15 H15 121.2 . . ?
C14 C15 H15 121.2 . . ?
N11 C16 C15 121.9(3) . . ?
N11 C16 C18 115.4(3) . . ?
C15 C16 C18 122.7(3) . . ?
O172 C17 O171 126.7(3) . . ?
O172 C17 C14 117.5(3) . . ?
O171 C17 C14 115.9(3) . . ?
O182 C18 O181 126.2(3) . . ?
O182 C18 C16 117.4(3) . . ?
O181 C18 C16 116.5(3) . . ?
C22 N23 C24 116.9(3) . . ?
C22 N23 Mn2 126.71(19) . . ?
C24 N23 Mn2 112.99(18) . . ?
N23 C22 N21 125.6(3) . . ?
N23 C22 H22 117.2 . . ?
N21 C22 H22 117.2 . . ?
C22 N21 C26 116.7(2) . . ?
C22 N21 Mn1 128.96(19) . . ?
C26 N21 Mn1 114.02(18) . . ?
N21 C26 C25 121.7(3) . . ?
N21 C26 C27 115.2(2) . . ?
C25 C26 C27 123.1(3) . . ?
C26 C25 C24 117.5(3) . . ?
C26 C25 H25 121.2 . . ?
C24 C25 H25 121.2 . . ?
N23 C24 C25 121.4(3) . . ?
N23 C24 C28 115.3(3) . . ?
C25 C24 C28 123.2(3) . . ?
O282 C27 O281 126.3(3) . . ?
O282 C27 C26 117.8(3) . . ?
O281 C27 C26 115.9(3) . . ?
O272 C28 O271 127.5(3) . . ?
O272 C28 C24 117.2(3) . . ?
O271 C28 C24 115.3(3) . . ?
C17 O171 Mn2 122.85(18) . 1_455 ?
C18 O181 Mn1 121.82(18) . . ?
C27 O281 Mn1 120.23(19) . . ?
C28 O271 Mn2 125.3(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
Mn1 O1W 2.108(2) . ?
Mn1 O181 2.129(2) . ?
Mn1 O281 2.160(2) . ?
Mn1 O2W 2.167(2) . ?
Mn1 N21 2.288(2) . ?
Mn1 N11 2.337(2) . ?
Mn2 O5W 2.197(2) . ?
Mn2 O271 2.203(2) . ?
Mn2 O171 2.204(2) 1_655 ?
Mn2 O3W 2.241(2) . ?
Mn2 O4W 2.245(2) . ?
Mn2 N13 2.405(2) 1_655 ?
Mn2 N23 2.433(2) . ?
O2W H2WB 0.8501 . ?
O2W H2WA 0.8639 . ?
O1W H1WB 0.8619 . ?
O1W H1WA 0.8625 . ?
O4W H4WB 0.8620 . ?
O4W H4WA 0.8700 . ?
O3W H3WB 0.8639 . ?
O3W H3WA 0.8574 . ?
O5W H5WA 0.8585 . ?
O5W H5WB 0.7948 . ?
O6W H6WB 0.8681 . ?
O6W H6WA 0.8712 . ?
O7W H7WB 0.8621 . ?
O7W H7WA 0.8729 . ?
N11 C12 1.334(3) . ?
N11 C16 1.344(4) . ?
C12 N13 1.330(3) . ?
C12 H12 0.9300 . ?
N13 C14 1.334(4) . ?
N13 Mn2 2.405(2) 1_455 ?
C14 C15 1.382(4) . ?
C14 C17 1.519(4) . ?
C15 C16 1.366(4) . ?
C15 H15 0.9300 . ?
C16 C18 1.531(4) . ?
C17 O172 1.234(3) . ?
C17 O171 1.275(3) . ?
C18 O182 1.234(3) . ?
C18 O181 1.254(3) . ?
N23 C22 1.321(3) . ?
N23 C24 1.341(3) . ?
C22 N21 1.339(3) . ?
C22 H22 0.9300 . ?
N21 C26 1.340(3) . ?
C26 C25 1.366(4) . ?
C26 C27 1.522(4) . ?
C25 C24 1.383(4) . ?
C25 H25 0.9300 . ?
C24 C28 1.512(4) . ?
C27 O282 1.233(3) . ?
C27 O281 1.274(3) . ?
C28 O272 1.238(3) . ?
C28 O271 1.255(3) . ?
O171 Mn2 2.204(2) 1_455 ?
