#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317277.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_4317277
loop_
_publ_author_name
'Urko García-Couceiro'
'Oscar Castillo'
'Javier Cepeda'
'Mónica Lanchas'
'Antonio Luque'
'Sonia Pérez-Yáñez'
'Pascual Román'
'Daniel Vallejo-Sánchez'
_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       oscar.castillo@ehu.es
_publ_contact_author_fax         '+34-946 013 500'
_publ_contact_author_phone       '+34-946 015 991'
_publ_section_title
;
 Influence of the Synthetic Conditions on the Structural Diversity of
 Extended Manganese-Oxalato-1,2-bis(4-pyridyl)ethylene Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11346
_journal_page_last               11361
_journal_paper_doi               10.1021/ic100928t
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H10 Mn N2 O4, 0.25(H2 O)'
_chemical_formula_structural     'C14 H10 Mn N2 O4, 0.25(H2 O)'
_chemical_formula_sum            'C14 H10.5 Mn N2 O4.25'
_chemical_formula_weight         329.68
_chemical_name_systematic
;
catena-[(mu-oxalato)(mu-1,2-bis(4-pyridyl)ethylene)manganese(II)] water (1/0.25)
;
_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           SHELXL97
_cell_angle_alpha                106.00(1)
_cell_angle_beta                 116.48(1)
_cell_angle_gamma                90.66(1)
_cell_formula_units_Z            2
_cell_length_a                   9.243(1)
_cell_length_b                   9.727(1)
_cell_length_c                   9.732(1)
_cell_measurement_reflns_used    4273
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      2.74
_cell_volume                     743.60(16)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7422
_diffrn_reflns_theta_full        30.12
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             335
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0439
_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)+(0.0588P)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                3020
_reflns_number_total             4273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100928t_si_002_2.cif
_cod_data_source_block           compound-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4317277
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
Mn01 Mn 0.17011(3) 0.25939(3) 0.02756(3) 0.02590(10) Uani 1 1 d . . .
C1 C 0.0689(2) 0.0018(2) 0.0849(2) 0.0263(4) Uani 1 1 d . . .
O1 O 0.18810(16) 0.10289(15) 0.15324(17) 0.0352(3) Uani 1 1 d . . .
O2 O 0.05090(17) -0.09584(15) 0.13905(17) 0.0369(3) Uani 1 1 d . . .
C2 C 0.0220(2) 0.5076(2) -0.0661(2) 0.0281(4) Uani 1 1 d . . .
O3 O 0.10841(18) 0.41995(16) -0.10053(18) 0.0381(3) Uani 1 1 d . . .
O4 O -0.03224(19) 0.60458(16) -0.12778(18) 0.0413(4) Uani 1 1 d . . .
N11 N 0.4257(2) 0.36801(19) 0.2255(2) 0.0355(4) Uani 1 1 d . . .
C12 C 0.5169(3) 0.4522(3) 0.1951(3) 0.0464(6) Uani 1 1 d . . .
H12 H 0.4638 0.4874 0.1083 0.056 Uiso 1 1 calc R . .
C13 C 0.6842(3) 0.4893(3) 0.2847(3) 0.0485(6) Uani 1 1 d . . .
H13 H 0.7413 0.5450 0.2554 0.058 Uiso 1 1 calc R . .
C14 C 0.7682(2) 0.4433(3) 0.4193(2) 0.0399(5) Uani 1 1 d . . .
C15 C 0.6727(3) 0.3627(3) 0.4560(3) 0.0465(6) Uani 1 1 d . . .
H15 H 0.7218 0.3321 0.5467 0.056 Uiso 1 1 calc R . .
C16 C 0.5057(3) 0.3279(3) 0.3582(3) 0.0413(5) Uani 1 1 d . . .
H16 H 0.4453 0.2738 0.3857 0.050 Uiso 1 1 calc R . .
C17 C 0.9476(3) 0.4719(3) 0.5182(3) 0.0450(6) Uani 1 1 d . . .
H17 H 0.9909 0.4485 0.6138 0.054 Uiso 1 1 calc R . .
N21 N 0.2753(2) 0.16382(19) -0.1457(2) 0.0358(4) Uani 1 1 d . . .
C22 C 0.1777(3) 0.1416(3) -0.3034(3) 0.0452(6) Uani 1 1 d . . .
H22 H 0.0712 0.1608 -0.3346 0.054 Uiso 1 1 calc R . .
C23 C 0.2235(3) 0.0928(3) -0.4220(3) 0.0488(6) Uani 1 1 d . . .
H23 H 0.1495 0.0795 -0.5295 0.059 Uiso 1 1 calc R . .
C24 C 0.3807(3) 0.0635(3) -0.3804(3) 0.0439(5) Uani 1 1 d . . .
C25 C 0.4845(3) 0.0853(3) -0.2172(3) 0.0594(7) Uani 1 1 d . . .
H25 H 0.5912 0.0663 -0.1836 0.071 Uiso 1 1 calc R . .
C26 C 0.4279(3) 0.1355(3) -0.1046(3) 0.0510(6) Uani 1 1 d . . .
H26 H 0.4992 0.1499 0.0039 0.061 Uiso 1 1 calc R . .
C27 C 0.4269(3) 0.0094(3) -0.5119(3) 0.0491(6) Uani 1 1 d . . .
H27 H 0.3450 -0.0121 -0.6181 0.059 Uiso 1 1 calc R . .
O1W O 0.8346(13) 0.1818(10) 0.1713(14) 0.100(3) Uani 0.25 1 d P . .
H1W H 0.7579 0.2207 0.1880 0.050 Uiso 0.25 1 d P . .
H2W H 0.8915 0.2522 0.1687 0.050 Uiso 0.25 1 d P . .
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
O1 Mn01 O4 95.73(6) . 2_565 ?
O1 Mn01 O3 169.54(5) . . ?
O4 Mn01 O3 75.63(5) 2_565 . ?
O1 Mn01 O2 76.02(5) . 2 ?
O4 Mn01 O2 91.06(6) 2_565 2 ?
O3 Mn01 O2 97.95(6) . 2 ?
O1 Mn01 N11 87.65(6) . . ?
O4 Mn01 N11 97.79(7) 2_565 . ?
O3 Mn01 N11 99.24(6) . . ?
O2 Mn01 N11 162.15(6) 2 . ?
O1 Mn01 N21 104.75(6) . . ?
O4 Mn01 N21 158.39(6) 2_565 . ?
O3 Mn01 N21 83.24(6) . . ?
O2 Mn01 N21 87.35(6) 2 . ?
N11 Mn01 N21 89.95(6) . . ?
O2 C1 O1 126.32(16) . . ?
O2 C1 C1 117.18(19) . 2 ?
O1 C1 C1 116.5(2) . 2 ?
C1 O1 Mn01 115.76(11) . . ?
C1 O2 Mn01 114.34(11) . 2 ?
O4 C2 O3 126.54(17) . . ?
O4 C2 C2 117.1(2) . 2_565 ?
O3 C2 C2 116.3(2) . 2_565 ?
C2 O3 Mn01 115.45(12) . . ?
C2 O4 Mn01 115.34(12) . 2_565 ?
C16 N11 C12 116.04(17) . . ?
C16 N11 Mn01 122.99(14) . . ?
C12 N11 Mn01 119.21(14) . . ?
N11 C12 C13 123.9(2) . . ?
N11 C12 H12 118.1 . . ?
C13 C12 H12 118.1 . . ?
C12 C13 C14 119.9(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 116.14(19) . . ?
C15 C14 C17 119.9(2) . . ?
C13 C14 C17 123.89(19) . . ?
C16 C15 C14 120.3(2) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
N11 C16 C15 123.53(19) . . ?
N11 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C17 C17 C14 125.4(3) 2_766 . ?
C17 C17 H17 117.3 2_766 . ?
C14 C17 H17 117.3 . . ?
C22 N21 C26 116.27(19) . . ?
C22 N21 Mn01 117.02(14) . . ?
C26 N21 Mn01 126.60(15) . . ?
N21 C22 C23 124.7(2) . . ?
N21 C22 H22 117.7 . . ?
C23 C22 H22 117.7 . . ?
C22 C23 C24 119.4(2) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 117.0(2) . . ?
C23 C24 C27 118.3(2) . . ?
C25 C24 C27 124.7(2) . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
N21 C26 C25 122.8(2) . . ?
N21 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C27 C27 C24 124.3(3) 2_654 . ?
C27 C27 H27 117.9 2_654 . ?
C24 C27 H27 117.9 . . ?
H1W O1W H2W 104.6 . . ?
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
Mn01 O1 2.1661(14) . ?
Mn01 O4 2.1821(14) 2_565 ?
Mn01 O3 2.1859(14) . ?
Mn01 O2 2.2095(14) 2 ?
Mn01 N11 2.2738(17) . ?
Mn01 N21 2.2962(17) . ?
C1 O2 1.248(2) . ?
C1 O1 1.259(2) . ?
C1 C1 1.563(3) 2 ?
O2 Mn01 2.2095(14) 2 ?
C2 O4 1.248(2) . ?
C2 O3 1.254(2) . ?
C2 C2 1.553(4) 2_565 ?
O4 Mn01 2.1821(14) 2_565 ?
N11 C16 1.341(3) . ?
N11 C12 1.346(3) . ?
C12 C13 1.376(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.394(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(3) . ?
C14 C17 1.474(3) . ?
C15 C16 1.380(3) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C17 1.328(4) 2_766 ?
C17 H17 0.9300 . ?
N21 C22 1.339(3) . ?
N21 C26 1.339(3) . ?
C22 C23 1.370(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.380(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.393(3) . ?
C24 C27 1.489(3) . ?
C25 C26 1.390(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C27 1.290(5) 2_654 ?
C27 H27 0.9300 . ?
O1W H1W 0.8647 . ?
O1W H2W 0.8707 . ?
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
C13 H13 O3 0.93 2.54 3.400(3) 153.7 2_665
C17 H17 O3 0.93 2.59 3.517(3) 172.0 1_656
C17 H17 O4 0.93 2.66 3.247(3) 122.1 1_656
C23 H23 O2 0.93 2.91 3.701(3) 144.0 1_554
C25 H25 O1 0.93 2.60 3.460(3) 153.9 2_655
C27 H27 O1 0.93 2.61 3.403(3) 142.9 1_554
C27 H27 O2 0.93 2.61 3.484(3) 157.5 1_554
O1W H2W O4 0.87 2.13 2.986(10) 169.7 2_665
