#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305072.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_4305072
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 Fe Mn N4 O13, 2(H2 O)'
_chemical_formula_structural     'C12 H14 Fe Mn N4 O13, 2(H2 O)'
_chemical_formula_sum            'C12 H18 Fe Mn N4 O15'
_chemical_formula_weight         569.09
_chemical_name_systematic
; 
catena-[di(mu-pyrimidine-4,6-dicarboxylato-N,O:N,O)-
pentaacua-iron(II)manganese(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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.388(1)
_cell_angle_beta                 103.293(1)
_cell_angle_gamma                103.764(1)
_cell_formula_units_Z            2
_cell_length_a                   7.7854(6)
_cell_length_b                   10.2442(8)
_cell_length_c                   13.3952(11)
_cell_measurement_reflns_used    11435
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.61
_cell_volume                     978.15(13)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Nonius'
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       10
_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       -17
_diffrn_reflns_number            11435
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS
Bruker Nonius area detector scaling and absorption correction
v2.05
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_meas      1.93(1)
_exptl_crystal_density_method    'flotation method'
_exptl_crystal_description       tabullar
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4727
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.4648P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                4060
_reflns_number_total             4727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8002788-file003_4.cif
_cod_data_source_block           compound5
_cod_database_code               4305072
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
Fe1 Fe 0.21766(4) 1.00332(3) 0.80260(2) 0.02460(10) Uani 1 1 d . . .
Mn1 Mn 0.81024(5) 1.49165(4) 0.70101(3) 0.02622(11) Uani 1 1 d . . .
O2W O 0.3433(3) 0.8364(2) 0.79337(15) 0.0388(4) Uani 1 1 d D . .
H2WB H 0.392(4) 0.828(4) 0.7410(17) 0.059(10) Uiso 1 1 d D . .
H2WA H 0.389(4) 0.794(3) 0.839(2) 0.053(10) Uiso 1 1 d D . .
O1W O 0.0086(3) 0.9081(2) 0.86097(17) 0.0406(5) Uani 1 1 d D . .
H1WB H -0.073(3) 0.949(3) 0.873(2) 0.041(8) Uiso 1 1 d D . .
H1WA H -0.019(5) 0.8192(7) 0.856(3) 0.069(11) Uiso 1 1 d D . .
O4W O 0.7628(3) 1.6807(2) 0.64943(18) 0.0434(5) Uani 1 1 d D . .
H4WB H 0.849(3) 1.753(2) 0.650(3) 0.062(11) Uiso 1 1 d D . .
H4WA H 0.674(3) 1.715(4) 0.658(3) 0.072(12) Uiso 1 1 d D . .
O3W O 0.5600(3) 1.5019(2) 0.75623(16) 0.0423(5) Uani 1 1 d D . .
H3WB H 0.564(5) 1.571(2) 0.8059(18) 0.056(10) Uiso 1 1 d D . .
H3WA H 0.454(2) 1.468(3) 0.7084(19) 0.056(10) Uiso 1 1 d D . .
O5W O 1.0639(3) 1.5789(2) 0.65867(18) 0.0461(5) Uani 1 1 d D . .
H5WA H 1.109(4) 1.517(3) 0.629(2) 0.059(11) Uiso 1 1 d D . .
H5WB H 1.141(4) 1.6606(18) 0.690(3) 0.082(13) Uiso 1 1 d D . .
O6W O -0.2396(3) 0.6085(2) 0.41211(16) 0.0421(5) Uani 1 1 d D . .
H6WB H -0.149(3) 0.685(2) 0.430(3) 0.072(12) Uiso 1 1 d D . .
H6WA H -0.260(6) 0.573(4) 0.464(2) 0.081(14) Uiso 1 1 d D . .
O7W O -0.2431(3) 1.0411(2) 0.8876(2) 0.0508(6) Uani 1 1 d D . .
H7WB H -0.210(5) 1.119(4) 0.927(3) 0.050(10) Uiso 1 1 d . . .
H7WA H -0.337(4) 1.015(6) 0.911(4) 0.13(2) Uiso 1 1 d D . .
N11 N 0.1484(3) 1.20720(19) 0.83303(14) 0.0234(4) Uani 1 1 d . . .
C12 C 0.0295(3) 1.2568(2) 0.77314(17) 0.0253(5) Uani 1 1 d . . .
H12 H -0.0445 1.1987 0.7081 0.030 Uiso 1 1 calc R . .
N13 N 0.0083(3) 1.38274(19) 0.79911(15) 0.0246(4) Uani 1 1 d . . .
C14 C 0.1150(3) 1.4660(2) 0.89254(17) 0.0226(4) Uani 1 1 d . . .
C15 C 0.2439(3) 1.4244(2) 0.95975(17) 0.0241(4) Uani 1 1 d . . .
H15 H 0.3190 1.4831 1.0243 0.029 Uiso 1 1 calc R . .
C16 C 0.2558(3) 1.2923(2) 0.92671(17) 0.0230(4) Uani 1 1 d . . .
C17 C 0.0834(3) 1.6070(2) 0.92449(18) 0.0243(4) Uani 1 1 d . . .
C18 C 0.3878(3) 1.2319(2) 0.99314(18) 0.0255(5) Uani 1 1 d . . .
N23 N 0.6085(3) 1.2560(2) 0.66159(15) 0.0248(4) Uani 1 1 d . . .
C22 C 0.5345(3) 1.1970(2) 0.72877(18) 0.0261(5) Uani 1 1 d . . .
H22 H 0.5953 1.2319 0.8007 0.031 Uiso 1 1 calc R . .
N21 N 0.3798(2) 1.09182(19) 0.70094(14) 0.0232(4) Uani 1 1 d . . .
C26 C 0.2958(3) 1.0393(2) 0.59706(17) 0.0221(4) Uani 1 1 d . . .
C25 C 0.3652(3) 1.0911(2) 0.52181(17) 0.0232(4) Uani 1 1 d . . .
H25 H 0.3088 1.0524 0.4498 0.028 Uiso 1 1 calc R . .
C24 C 0.5227(3) 1.2033(2) 0.55810(17) 0.0227(4) Uani 1 1 d . . .
C27 C 0.1181(3) 0.9208(2) 0.56893(17) 0.0239(4) Uani 1 1 d . . .
C28 C 0.6050(3) 1.2796(2) 0.48494(18) 0.0265(5) Uani 1 1 d . . .
O172 O 0.1759(2) 1.68135(17) 1.01212(14) 0.0357(4) Uani 1 1 d . . .
O171 O -0.0413(2) 1.63228(17) 0.85804(13) 0.0301(4) Uani 1 1 d . . .
O181 O 0.4019(2) 1.11751(17) 0.94830(13) 0.0315(4) Uani 1 1 d . . .
O182 O 0.4708(3) 1.29763(19) 1.08608(13) 0.0365(4) Uani 1 1 d . . .
O281 O 0.0532(2) 0.90314(17) 0.64590(13) 0.0299(4) Uani 1 1 d . . .
O282 O 0.0521(2) 0.85314(18) 0.47585(13) 0.0336(4) Uani 1 1 d . . .
O271 O 0.7157(3) 1.39750(19) 0.52953(14) 0.0407(5) Uani 1 1 d . . .
O272 O 0.5517(2) 1.22085(19) 0.38906(13) 0.0333(4) 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'
Fe Fe 0.3463 0.8444 '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 Fe1 O181 96.82(8) . . ?
O1W Fe1 O281 90.39(8) . . ?
O181 Fe1 O281 172.63(7) . . ?
O1W Fe1 O2W 95.85(8) . . ?
O181 Fe1 O2W 93.80(7) . . ?
O281 Fe1 O2W 86.92(7) . . ?
O1W Fe1 N21 164.70(8) . . ?
O181 Fe1 N21 97.39(7) . . ?
O281 Fe1 N21 75.28(6) . . ?
O2W Fe1 N21 88.83(7) . . ?
O1W Fe1 N11 91.60(7) . . ?
O181 Fe1 N11 75.40(6) . . ?
O281 Fe1 N11 103.00(7) . . ?
O2W Fe1 N11 167.57(8) . . ?
N21 Fe1 N11 86.53(7) . . ?
O171 Mn1 O271 163.14(7) 1_655 . ?
O171 Mn1 O5W 84.58(8) 1_655 . ?
O271 Mn1 O5W 80.34(8) . . ?
O171 Mn1 O4W 86.40(7) 1_655 . ?
O271 Mn1 O4W 82.85(8) . . ?
O5W Mn1 O4W 76.78(8) . . ?
O171 Mn1 O3W 82.95(7) 1_655 . ?
O271 Mn1 O3W 107.93(8) . . ?
O5W Mn1 O3W 154.77(8) . . ?
O4W Mn1 O3W 80.62(8) . . ?
O171 Mn1 N13 71.17(6) 1_655 1_655 ?
O271 Mn1 N13 113.63(7) . 1_655 ?
O5W Mn1 N13 81.57(8) . 1_655 ?
O4W Mn1 N13 150.13(7) . 1_655 ?
O3W Mn1 N13 114.62(7) . 1_655 ?
O171 Mn1 N23 127.37(7) 1_655 . ?
O271 Mn1 N23 69.17(6) . . ?
O5W Mn1 N23 132.29(7) . . ?
O4W Mn1 N23 131.46(7) . . ?
O3W Mn1 N23 71.99(7) . . ?
N13 Mn1 N23 78.41(6) 1_655 . ?
C12 N11 C16 116.90(18) . . ?
C12 N11 Fe1 131.50(15) . . ?
C16 N11 Fe1 111.51(14) . . ?
N13 C12 N11 125.3(2) . . ?
C12 N13 C14 117.18(19) . . ?
C12 N13 Mn1 130.11(15) . 1_455 ?
C14 N13 Mn1 112.68(14) . 1_455 ?
N13 C14 C15 121.7(2) . . ?
N13 C14 C17 117.02(19) . . ?
C15 C14 C17 121.2(2) . . ?
C16 C15 C14 117.1(2) . . ?
N11 C16 C15 121.7(2) . . ?
N11 C16 C18 115.41(19) . . ?
C15 C16 C18 122.9(2) . . ?
O172 C17 O171 127.1(2) . . ?
O172 C17 C14 117.2(2) . . ?
O171 C17 C14 115.70(19) . . ?
O182 C18 O181 125.6(2) . . ?
O182 C18 C16 118.1(2) . . ?
O181 C18 C16 116.27(19) . . ?
C22 N23 C24 117.18(19) . . ?
C22 N23 Mn1 126.30(15) . . ?
C24 N23 Mn1 112.80(14) . . ?
N23 C22 N21 125.1(2) . . ?
C22 N21 C26 117.16(19) . . ?
C22 N21 Fe1 129.19(15) . . ?
C26 N21 Fe1 113.23(14) . . ?
N21 C26 C25 121.7(2) . . ?
N21 C26 C27 115.38(19) . . ?
C25 C26 C27 122.87(19) . . ?
C26 C25 C24 117.0(2) . . ?
N23 C24 C25 121.7(2) . . ?
N23 C24 C28 115.26(19) . . ?
C25 C24 C28 123.0(2) . . ?
O282 C27 O281 126.9(2) . . ?
O282 C27 C26 118.0(2) . . ?
O281 C27 C26 115.11(19) . . ?
O272 C28 O271 127.9(2) . . ?
O272 C28 C24 117.2(2) . . ?
O271 C28 C24 115.0(2) . . ?
C17 O171 Mn1 123.04(14) . 1_455 ?
C18 O181 Fe1 120.51(14) . . ?
C27 O281 Fe1 119.67(14) . . ?
C28 O271 Mn1 125.61(16) . . ?
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
Fe1 O1W 2.0779(19) . ?
Fe1 O181 2.0798(17) . ?
Fe1 O281 2.1120(16) . ?
Fe1 O2W 2.1617(18) . ?
Fe1 N21 2.2276(19) . ?
Fe1 N11 2.2690(19) . ?
Mn1 O171 2.1984(17) 1_655 ?
Mn1 O271 2.1987(18) . ?
Mn1 O5W 2.209(2) . ?
Mn1 O4W 2.2514(19) . ?
Mn1 O3W 2.255(2) . ?
Mn1 N13 2.4012(18) 1_655 ?
Mn1 N23 2.4348(19) . ?
N11 C12 1.337(3) . ?
N11 C16 1.345(3) . ?
C12 N13 1.334(3) . ?
N13 C14 1.335(3) . ?
N13 Mn1 2.4012(18) 1_455 ?
C14 C15 1.388(3) . ?
C14 C17 1.524(3) . ?
C15 C16 1.377(3) . ?
C16 C18 1.521(3) . ?
C17 O172 1.226(3) . ?
C17 O171 1.268(3) . ?
C18 O182 1.242(3) . ?
C18 O181 1.258(3) . ?
N23 C22 1.333(3) . ?
N23 C24 1.339(3) . ?
C22 N21 1.335(3) . ?
N21 C26 1.341(3) . ?
C26 C25 1.377(3) . ?
C26 C27 1.525(3) . ?
C25 C24 1.383(3) . ?
C24 C28 1.520(3) . ?
C27 O282 1.234(3) . ?
C27 O281 1.271(3) . ?
C28 O272 1.241(3) . ?
C28 O271 1.251(3) . ?
O171 Mn1 2.1984(17) 1_455 ?
