#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305069.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_4305069
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         'C6 H8 Mn N2 O7, 2(H2 O)'
_chemical_formula_structural     'C6 H8 Mn N2 O7, 2(H2 O)'
_chemical_formula_sum            'C6 H12 Mn N2 O9'
_chemical_formula_weight         311.12
_chemical_name_systematic
;
catena-[(mu-pyrimidine-4,6-dicarboxylato-N,O:N,O)-
triacuamanganese(II)-water (1/2)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.000
_cell_angle_beta                 121.96(2)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   12.204(5)
_cell_length_b                   7.093(5)
_cell_length_c                   14.846(4)
_cell_measurement_reflns_used    10524
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.8
_cell_volume                     1090.3(10)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.1338
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10524
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.758
_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 yellow'
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_meas      1.89(1)
_exptl_crystal_density_method    'flotation method'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0598
_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)+(0.0771P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                2562
_reflns_number_total             3226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8002788-file003_1.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4305069
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.26749(3) -0.52452(4) -0.68709(3) 0.01825(13) Uani 1 1 d . . .
O81 O 0.25634(16) -0.4781(2) -0.83800(16) 0.0273(4) Uani 1 1 d . . .
O71 O -0.31337(15) 0.0118(2) -0.97559(15) 0.0247(4) Uani 1 1 d . . .
O72 O -0.27966(15) -0.0328(3) -1.10744(15) 0.0295(4) Uani 1 1 d . . .
C4 C -0.11724(16) -0.1280(3) -0.93477(16) 0.0161(4) Uani 1 1 d . . .
C8 C 0.16645(17) -0.3859(3) -0.91272(17) 0.0181(4) Uani 1 1 d . . .
N3 N -0.08785(15) -0.1356(2) -0.83467(14) 0.0182(3) Uani 1 1 d . . .
O82 O 0.14452(15) -0.3662(2) -1.00306(14) 0.0299(4) Uani 1 1 d . . .
C6 C 0.07365(16) -0.2916(2) -0.88733(16) 0.0159(4) Uani 1 1 d . . .
C5 C -0.03654(17) -0.2005(3) -0.96504(16) 0.0175(4) Uani 1 1 d . . .
H5 H -0.0553 -0.1888 -1.0342 0.021 Uiso 1 1 calc R . .
C7 C -0.24741(18) -0.0423(3) -1.01385(18) 0.0182(4) Uani 1 1 d . . .
N1 N 0.10197(15) -0.3056(2) -0.78757(14) 0.0190(3) Uani 1 1 d . . .
C2 C 0.02125(18) -0.2229(3) -0.76500(17) 0.0196(4) Uani 1 1 d . . .
H2 H 0.0430 -0.2265 -0.6948 0.024 Uiso 1 1 calc R . .
O1W O 0.40658(19) -0.2728(2) -0.62514(17) 0.0403(4) Uani 1 1 d . . .
H11 H 0.4394 -0.2117 -0.6537 0.050 Uiso 1 1 d . . .
H12 H 0.4155 -0.2287 -0.5721 0.050 Uiso 1 1 d . . .
O2W O 0.45323(13) -0.6706(2) -0.61890(16) 0.0318(4) Uani 1 1 d . . .
H21 H 0.5182 -0.6060 -0.6066 0.050 Uiso 1 1 d . . .
H22 H 0.4272 -0.7729 -0.6547 0.050 Uiso 1 1 d . . .
O3W O 0.20107(14) -0.8169(2) -0.76202(14) 0.0271(3) Uani 1 1 d . . .
H31 H 0.2196 -0.8795 -0.7076 0.050 Uiso 1 1 d . . .
H32 H 0.2374 -0.8806 -0.7775 0.050 Uiso 1 1 d . . .
O4W O 0.3006(2) -0.5151(3) -1.0640(2) 0.0430(5) Uani 1 1 d . . .
H41 H 0.2634 -0.4657 -1.0393 0.061 Uiso 1 1 d . . .
H42 H 0.3122 -0.6112 -1.0230 0.050 Uiso 1 1 d . . .
O5W O -0.49726(15) -0.0013(2) -1.30230(16) 0.0283(4) Uani 1 1 d . . .
H51 H -0.4415 -0.0377 -1.2449 0.050 Uiso 1 1 d . . .
H52 H -0.5569 0.0000 -1.3003 0.050 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'
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
O71 Mn1 O2W 87.02(7) 2_543 . ?
O71 Mn1 O81 161.88(7) 2_543 . ?
O2W Mn1 O81 91.87(7) . . ?
O71 Mn1 O3W 117.47(6) 2_543 . ?
O2W Mn1 O3W 79.03(6) . . ?
O81 Mn1 O3W 79.95(7) . . ?
O71 Mn1 O1W 76.29(7) 2_543 . ?
O2W Mn1 O1W 79.52(8) . . ?
O81 Mn1 O1W 85.72(7) . . ?
O3W Mn1 O1W 153.70(7) . . ?
O71 Mn1 N1 104.76(7) 2_543 . ?
O2W Mn1 N1 159.42(7) . . ?
O81 Mn1 N1 71.64(6) . . ?
O3W Mn1 N1 109.01(7) . . ?
O1W Mn1 N1 86.85(8) . . ?
O71 Mn1 N3 67.96(6) 2_543 2_543 ?
O2W Mn1 N3 123.58(7) . 2_543 ?
O81 Mn1 N3 126.33(7) . 2_543 ?
O3W Mn1 N3 70.67(6) . 2_543 ?
O1W Mn1 N3 134.84(7) . 2_543 ?
N1 Mn1 N3 76.88(7) . 2_543 ?
C8 O81 Mn1 122.24(13) . . ?
C7 O71 Mn1 127.45(14) . 2_553 ?
N3 C4 C5 122.06(17) . . ?
N3 C4 C7 115.67(16) . . ?
C5 C4 C7 122.22(18) . . ?
O82 C8 O81 127.45(18) . . ?
O82 C8 C6 117.30(17) . . ?
O81 C8 C6 115.24(18) . . ?
C2 N3 C4 116.99(17) . . ?
C2 N3 Mn1 129.07(14) . 2_553 ?
C4 N3 Mn1 113.18(12) . 2_553 ?
N1 C6 C5 121.77(17) . . ?
N1 C6 C8 116.87(16) . . ?
C5 C6 C8 121.34(18) . . ?
C4 C5 C6 116.66(18) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
O72 C7 O71 126.25(19) . . ?
O72 C7 C4 118.36(17) . . ?
O71 C7 C4 115.39(19) . . ?
C2 N1 C6 117.04(16) . . ?
C2 N1 Mn1 129.23(14) . . ?
C6 N1 Mn1 112.58(12) . . ?
N3 C2 N1 125.35(19) . . ?
N3 C2 H2 117.3 . . ?
N1 C2 H2 117.3 . . ?
Mn1 O1W H11 130.4 . . ?
Mn1 O1W H12 112.7 . . ?
H11 O1W H12 116.2 . . ?
Mn1 O2W H21 117.6 . . ?
Mn1 O2W H22 99.3 . . ?
H21 O2W H22 126.2 . . ?
Mn1 O3W H31 99.5 . . ?
Mn1 O3W H32 125.5 . . ?
H31 O3W H32 94.3 . . ?
H41 O4W H42 86.9 . . ?
H51 O5W H52 105.0 . . ?
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 O71 2.186(2) 2_543 ?
Mn1 O2W 2.1928(17) . ?
Mn1 O81 2.196(2) . ?
Mn1 O3W 2.290(2) . ?
Mn1 O1W 2.294(2) . ?
Mn1 N1 2.3512(18) . ?
Mn1 N3 2.5060(18) 2_543 ?
O81 C8 1.254(3) . ?
O71 C7 1.266(3) . ?
O71 Mn1 2.186(2) 2_553 ?
O72 C7 1.229(3) . ?
C4 N3 1.333(3) . ?
C4 C5 1.380(3) . ?
C4 C7 1.516(3) . ?
C8 O82 1.229(3) . ?
C8 C6 1.525(3) . ?
N3 C2 1.330(3) . ?
N3 Mn1 2.5060(18) 2_553 ?
C6 N1 1.334(3) . ?
C6 C5 1.384(3) . ?
C5 H5 0.9300 . ?
N1 C2 1.333(3) . ?
C2 H2 0.9300 . ?
O1W H11 0.8411 . ?
O1W H12 0.7987 . ?
O2W H21 0.8474 . ?
O2W H22 0.8547 . ?
O3W H31 0.8410 . ?
O3W H32 0.7494 . ?
O4W H41 0.7988 . ?
O4W H42 0.8735 . ?
O5W H51 0.8009 . ?
O5W H52 0.7441 . ?
