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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/99/4309933.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_4309933
loop_
_publ_author_name
'Urko García-Couceiro'
'David Olea'
'Oscar Castillo'
'Antonio Luque'
'Pascual Román'
'Pedro J. de Pablo'
'Julio Gómez-Herrero'
'Félix Zamora'
_publ_contact_author
;
 Oscar Castillo. Departamento de Quimica Inorganica. Facultad de Ciencias
 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
;
Scanning Probe Microscopy Characterization of Single Chains Based on a
One-Dimensional Oxalato-Bridged Manganese(II) Complex with 4-Aminotriazole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8343
_journal_page_last               8348
_journal_paper_doi               10.1021/ic0505302
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C6 H8 Mn1 N8 O4'
_chemical_formula_structural     'C6 H8 Mn1 N8 O4'
_chemical_formula_sum            'C6 H8 Mn N8 O4'
_chemical_formula_weight         311.12
_chemical_name_systematic
;
catena-[(mu-oxalato)bis(4-amine-1,2,4-triazole)manganese(II)]
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      58
_symmetry_space_group_name_Hall  '-P 2n 2n'
_symmetry_space_group_name_H-M   'P n m n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.599(1)
_cell_length_b                   7.401(2)
_cell_length_c                   14.232(4)
_cell_measurement_reflns_used    4971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.91
_cell_volume                     589.7(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4971
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.91901
_exptl_absorpt_correction_T_min  0.79598
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_meas      1.74(1)
_exptl_crystal_density_method    'flotation method'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0400
_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)+(0.0372P)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                518
_reflns_number_total             924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505302si20050712_120224.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        589.8(3)
_cod_original_formula_sum        'C6 H8 Mn1 N8 O4'
_cod_database_code               4309933
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'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 0.5000 0.0000 0.5000 0.0435(3) Uani 1 4 d S . .
C1 C 1.0000 0.1035(4) 0.5000 0.0346(7) Uani 1 2 d S . .
O1 O 0.8029(2) 0.1821(2) 0.4929(1) 0.0418(4) Uani 1 1 d . . .
N11 N 0.4843(4) 0.0000 0.34358(19) 0.0527(8) Uani 1 2 d S . .
N12 N 0.2786(5) 0.0000 0.2897(2) 0.0663(10) Uani 1 2 d S . .
C13 C 0.3469(7) 0.0000 0.2037(3) 0.0649(12) Uani 1 2 d S . .
H13 H 0.253(5) 0.0000 0.153(2) 0.043(9) Uiso 1 2 d S . .
N14 N 0.5889(5) 0.0000 0.1968(2) 0.0455(7) Uani 1 2 d S . .
C15 C 0.6627(7) 0.0000 0.2856(3) 0.0501(10) Uani 1 2 d S . .
H15 H 0.815(6) 0.0000 0.300(2) 0.061(11) Uiso 1 2 d S . .
N16 N 0.7420(6) 0.0000 0.1190(2) 0.0520(8) Uani 1 2 d S . .
H16 H 0.710(4) 0.096(3) 0.085(2) 0.081(10) Uiso 1 1 d . . .
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
Mn1 0.0237(3) 0.0645(6) 0.0425(5) 0.000 -0.0025(3) 0.000
C1 0.029(1) 0.048(2) 0.028(2) 0.000 -0.002(2) 0.000
O1 0.030(1) 0.043(1) 0.052(1) -0.002(1) -0.006(1) 0.005(1)
N11 0.037(1) 0.083(2) 0.038(2) 0.000 -0.005(1) 0.000
N12 0.037(2) 0.116(3) 0.046(2) 0.000 -0.008(2) 0.000
C13 0.050(2) 0.104(4) 0.041(3) 0.000 -0.018(2) 0.000
N14 0.049(2) 0.051(2) 0.036(2) 0.000 -0.003(1) 0.000
C15 0.036(2) 0.076(3) 0.038(2) 0.000 -0.006(2) 0.000
N16 0.065(2) 0.055(2) 0.036(2) 0.000 0.006(2) 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'
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 Mn1 O1 180.0 5_656 . ?
O1 Mn1 O1 76.83(9) 5_656 4_656 ?
O1 Mn1 O1 103.17(9) . 4_656 ?
O1 Mn1 O1 103.17(9) 5_656 8 ?
O1 Mn1 O1 76.83(9) . 8 ?
O1 Mn1 O1 180.0 4_656 8 ?
O1 Mn1 N11 89.09(6) 5_656 5_656 ?
O1 Mn1 N11 90.91(6) . 5_656 ?
O1 Mn1 N11 89.09(6) 4_656 5_656 ?
O1 Mn1 N11 90.91(6) 8 5_656 ?
O1 Mn1 N11 90.91(6) 5_656 . ?
O1 Mn1 N11 89.09(6) . . ?
O1 Mn1 N11 90.91(6) 4_656 . ?
O1 Mn1 N11 89.09(6) 8 . ?
N11 Mn1 N11 180.0 5_656 . ?
O1 C1 O1 124.7(3) 4_756 . ?
O1 C1 C1 117.7(2) 4_756 5_756 ?
O1 C1 C1 117.7(2) . 5_756 ?
C1 O1 Mn1 113.4(2) . . ?
C15 N11 N12 106.8(3) . . ?
C15 N11 Mn1 127.3(2) . . ?
N12 N11 Mn1 125.9(2) . . ?
C13 N12 N11 106.3(3) . . ?
N12 C13 N14 111.5(3) . . ?
N12 C13 H13 127(2) . . ?
N14 C13 H13 122(2) . . ?
C15 N14 C13 104.0(3) . . ?
C15 N14 N16 124.1(3) . . ?
C13 N14 N16 131.9(3) . . ?
N11 C15 N14 111.5(3) . . ?
N11 C15 H15 127(2) . . ?
N14 C15 H15 122(2) . . ?
N14 N16 H16 108(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 O1 2.169(2) 5_656 ?
Mn1 O1 2.169(2) . ?
Mn1 O1 2.169(2) 4_656 ?
Mn1 O1 2.169(2) 8 ?
Mn1 N11 2.228(3) 5_656 ?
Mn1 N11 2.228(3) . ?
C1 O1 1.251(2) 4_756 ?
C1 O1 1.251(2) . ?
C1 C1 1.533(7) 5_756 ?
N11 C15 1.295(4) . ?
N11 N12 1.384(4) . ?
N12 C13 1.282(4) . ?
C13 N14 1.359(5) . ?
C13 H13 0.89(3) . ?
N14 C15 1.329(4) . ?
N14 N16 1.401(4) . ?
C15 H15 0.87(3) . ?
N16 H16 0.88(2) . ?
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
N16 H16 O1 0.88(2) 2.10(2) 2.970(3) 169(2) 2_654
C15 H15 N12 0.87(3) 2.60(3) 3.449(6) 163(3) 1_655
