#------------------------------------------------------------------------------
#$Date: 2015-08-05 23:52:45 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152926 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/93/1529357.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_1529357
loop_
_publ_author_name
'Liu, Bing'
'Fernandes, José A'
'Tomé, João P C'
'Paz, Filipe A Almeida'
'Cunha-Silva, Luís'
_publ_section_title
;
 Multidimensional Transition Metal Complexes Based on
 3-Amino-1H-1,2,4-triazole-5-carboxylic Acid: From Discrete Mononuclear
 Complexes to Layered Materials.
;
_journal_issue                   7
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              12341
_journal_page_last               12363
_journal_paper_doi               10.3390/molecules200712341
_journal_volume                  20
_journal_year                    2015
_chemical_formula_moiety         'C6 H10 Mn N8 O6, 2(H2 O)'
_chemical_formula_sum            'C6 H14 Mn N8 O8'
_chemical_formula_weight         381.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             '22 June 2015'
_audit_creation_method           'SHELXL-2014/7, manual editing plus enCIFer'
_cell_angle_alpha                90.532(10)
_cell_angle_beta                 102.774(11)
_cell_angle_gamma                109.139(10)
_cell_formula_units_Z            1
_cell_length_a                   5.2482(9)
_cell_length_b                   6.5330(11)
_cell_length_c                   10.6128(18)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      3.31
_cell_volume                     333.93(10)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 2012.4 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'ω / φ scans'
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_laue_measured_fraction_full 0.993
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4790
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.953
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS V2012/1 (Bruker AXS Inc.) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       Block
_exptl_crystal_F_000             195
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.971
_exptl_transmission_factor_min   0.951
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1519
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0133P)²+0.4447P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1372
_reflns_number_total             1519
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            comp_2.cif
_cod_data_source_block           comp_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Triclinic' changed to
'triclinic' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/MDPI/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/MDPI/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               1529357
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.969
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.5000 0.5000 0.5000 0.00853(18) Uani 1 2 d S . P
N11 N 0.0251(5) 0.2462(4) 0.0981(2) 0.0135(6) Uani 1 1 d . . .
H11A H -0.106(9) 0.217(7) 0.022(4) 0.020 Uiso 0.75 1 d . U P
N12 N 0.1988(5) 0.1277(4) 0.1338(2) 0.0133(5) Uani 1 1 d D . .
H12A H 0.18(3) 0.005(11) 0.093(11) 0.020 Uiso 0.25 1 d D U P
C13 C 0.3279(6) 0.2114(5) 0.2532(3) 0.0121(6) Uani 1 1 d . . .
N14 N 0.2506(5) 0.3740(4) 0.2978(2) 0.0121(5) Uani 1 1 d . . .
C15 C 0.0565(6) 0.3904(5) 0.1968(3) 0.0124(6) Uani 1 1 d . . .
N1 N -0.0826(6) 0.5312(5) 0.1900(3) 0.0182(6) Uani 1 1 d . . .
H1A H -0.095(7) 0.589(6) 0.263(4) 0.022 Uiso 1 1 d . U .
H1B H -0.216(8) 0.509(6) 0.128(4) 0.022 Uiso 1 1 d . U .
C1 C 0.5488(6) 0.1425(5) 0.3370(3) 0.0111(6) Uani 1 1 d . . .
O1 O 0.6487(4) 0.2410(3) 0.45041(19) 0.0135(5) Uani 1 1 d . . .
O2 O 0.6236(4) -0.0004(3) 0.2932(2) 0.0169(5) Uani 1 1 d . . .
O1W O 0.8334(4) 0.7265(3) 0.4234(2) 0.0147(5) Uani 1 1 d D . .
H1WA H 1.019(3) 0.772(4) 0.471(3) 0.022 Uiso 1 1 d D U .
H1WB H 0.792(5) 0.846(3) 0.387(3) 0.022 Uiso 1 1 d D U .
O2W O 0.4732(5) 0.7414(4) 0.0638(2) 0.0191(5) Uani 1 1 d D . .
H2WA H 0.596(6) 0.828(5) 0.018(3) 0.029 Uiso 1 1 d D U .
H3WB H 0.516(8) 0.824(6) 0.129(4) 0.029 Uiso 1 1 d . U .
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'
Mn Mn 0.3368 0.7283 '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'
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
O1 Mn1 O1 180.0 2_666 .
O1 Mn1 O1W 87.38(8) 2_666 2_666
O1 Mn1 O1W 92.62(8) . 2_666
O1 Mn1 O1W 92.62(8) 2_666 .
O1 Mn1 O1W 87.38(8) . .
O1W Mn1 O1W 180.0 2_666 .
O1 Mn1 N14 76.23(8) 2_666 2_666
O1 Mn1 N14 103.77(8) . 2_666
O1W Mn1 N14 90.45(9) 2_666 2_666
O1W Mn1 N14 89.56(9) . 2_666
O1 Mn1 N14 103.77(8) 2_666 .
O1 Mn1 N14 76.23(8) . .
O1W Mn1 N14 89.55(9) 2_666 .
O1W Mn1 N14 90.44(8) . .
N14 Mn1 N14 180.0 2_666 .
C15 N11 N12 110.3(2) . .
C15 N11 H11A 126(3) . .
N12 N11 H11A 123(3) . .
C13 N12 N11 102.1(2) . .
C13 N12 H12A 131(9) . .
N11 N12 H12A 125(9) . .
N12 C13 N14 115.3(3) . .
N12 C13 C1 124.1(3) . .
N14 C13 C1 120.5(3) . .
C15 N14 C13 102.9(2) . .
C15 N14 Mn1 147.2(2) . .
C13 N14 Mn1 109.89(19) . .
N14 C15 N1 126.7(3) . .
N14 C15 N11 109.4(3) . .
N1 C15 N11 123.9(3) . .
C15 N1 H1A 118(2) . .
C15 N1 H1B 116(2) . .
H1A N1 H1B 117(3) . .
O2 C1 O1 125.1(3) . .
O2 C1 C13 119.7(3) . .
O1 C1 C13 115.2(3) . .
C1 O1 Mn1 118.08(19) . .
Mn1 O1W H1WA 121.1(18) . .
Mn1 O1W H1WB 114.5(18) . .
H1WA O1W H1WB 109.7(15) . .
H2WA O2W H3WB 99(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.186(2) 2_666
Mn1 O1 2.186(2) .
Mn1 O1W 2.206(2) 2_666
Mn1 O1W 2.206(2) .
Mn1 N14 2.239(3) 2_666
Mn1 N14 2.239(3) .
N11 C15 1.348(4) .
N11 N12 1.375(3) .
N11 H11A 0.91(5) .
N12 C13 1.315(4) .
N12 H12A 0.880(10) .
C13 N14 1.370(4) .
C13 C1 1.493(4) .
N14 C15 1.337(4) .
C15 N1 1.343(4) .
N1 H1A 0.88(4) .
N1 H1B 0.82(4) .
C1 O2 1.247(3) .
C1 O1 1.274(3) .
O1W H1WA 0.939(10) .
O1W H1WB 0.942(10) .
O2W H2WA 0.939(10) .
O2W H3WB 0.82(4) .
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
N11 H11A O2W 0.91(5) 2.05(5) 2.820(3) 142(4) 2_565
N11 H11A N12 0.91(5) 2.63(4) 3.183(3) 120(3) 2
N1 H1A O1W 0.88(4) 2.08(4) 2.957(4) 173(3) 1_455
N1 H1B O2W 0.82(4) 2.43(4) 3.115(4) 142(3) 2_565
N1 H1B O2W 0.82(4) 2.57(4) 3.141(4) 128(3) 1_455
O1W H1WA O1 0.939(10) 1.789(12) 2.689(3) 160(3) 2_766
O1W H1WB O2 0.942(10) 1.729(12) 2.639(3) 162(3) 1_565
O2W H2WA N12 0.939(10) 2.098(19) 2.959(3) 152(3) 2_665
O2W H3WB O2 0.82(4) 1.94(4) 2.757(3) 175(4) 1_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C15 N11 N12 C13 -0.7(3)
N11 N12 C13 N14 0.3(3)
N11 N12 C13 C1 -178.5(3)
N12 C13 N14 C15 0.2(4)
C1 C13 N14 C15 179.0(3)
N12 C13 N14 Mn1 -178.6(2)
C1 C13 N14 Mn1 0.2(3)
C13 N14 C15 N1 -178.6(3)
Mn1 N14 C15 N1 -0.7(6)
C13 N14 C15 N11 -0.6(3)
Mn1 N14 C15 N11 177.3(3)
N12 N11 C15 N14 0.9(3)
N12 N11 C15 N1 178.9(3)
N12 C13 C1 O2 1.3(5)
N14 C13 C1 O2 -177.4(3)
N12 C13 C1 O1 -179.5(3)
N14 C13 C1 O1 1.8(4)
O2 C1 O1 Mn1 176.3(2)
C13 C1 O1 Mn1 -2.9(3)
