#------------------------------------------------------------------------------
#$Date: 2016-02-18 09:40:55 +0100 (jue 18 de feb de 2016) $
#$Revision: 176722 $
#$URL: svn://www.crystallography.net/cod/cif/3/00/00/3000004.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_3000004
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quiros'
'Juan M. Salas'
_publ_section_title
;
 H-bond superstructures built by aquacomplexes and an azapurine
 derivative: A case of molecular recognition
;
_journal_name_full               'Dalton Transactions'
_journal_page_first              10390
_journal_page_last               10395
_journal_paper_doi               10.1039/c2dt30992k
_journal_year                    2012
_chemical_formula_moiety         'C10 H8 N2, H12 Mn O6 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum            'C22 H32 Mn N12 O10'
_chemical_formula_weight         679.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.647(2)
_cell_angle_beta                 108.125(2)
_cell_angle_gamma                101.431(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5570(12)
_cell_length_b                   9.1663(13)
_cell_length_c                   10.9500(15)
_cell_measurement_reflns_used    4227
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.5
_cell_volume                     729.94(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'φ and ω 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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8537
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        -0.1
_diffrn_standards_number         176
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             353
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3306
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0386
_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)+(0.0600P)²+0.1500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                2984
_reflns_number_total             3306
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mnax44.cif
_cod_data_source_block           mnax44
_cod_depositor_comments
;Extending hold period by 9 months (from 2011-12-03 to 2012-09-03)
 Also
 changing journal name to Dalton Transactions

 Releasing structure 3000004 into public domain as published material.
;
_cod_original_cell_volume        729.93(18)
_cod_database_code               3000004
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
Mn Mn 0.5000 0.5000 0.5000 0.03291(13) Uani 1 2 d S
O1W O 0.38415(17) 0.24176(16) 0.34578(14) 0.0437(3) Uani 1 1 d D
H11W H 0.315(2) 0.230(3) 0.2675(14) 0.053(6) Uiso 1 1 d D
H12W H 0.460(3) 0.205(3) 0.327(3) 0.087(9) Uiso 1 1 d D
O2W O 0.58027(17) 0.42212(19) 0.67057(15) 0.0484(3) Uani 1 1 d D
H21W H 0.533(3) 0.405(3) 0.723(2) 0.072(8) Uiso 1 1 d D
H22W H 0.6796(19) 0.413(3) 0.702(3) 0.074(8) Uiso 1 1 d D
O3W O 0.25331(16) 0.48602(19) 0.51155(15) 0.0465(3) Uani 1 1 d D
H31W H 0.174(2) 0.511(3) 0.463(2) 0.056(6) Uiso 1 1 d D
H32W H 0.220(3) 0.472(3) 0.572(2) 0.065(7) Uiso 1 1 d D
N1 N 0.13923(19) 0.4375(2) 0.71109(16) 0.0412(3) Uani 1 1 d .
N2 N -0.01977(19) 0.4426(2) 0.68268(16) 0.0453(4) Uani 1 1 d .
N3 N -0.09668(19) 0.3791(2) 0.75466(16) 0.0411(3) Uani 1 1 d .
C3A C 0.0236(2) 0.3338(2) 0.83089(17) 0.0335(3) Uani 1 1 d .
N4 N 0.01147(17) 0.26468(18) 0.92315(15) 0.0356(3) Uani 1 1 d .
C4 C -0.1471(2) 0.2294(3) 0.9486(2) 0.0476(4) Uani 1 1 d .
H41 H -0.1921 0.1099 0.9276 0.057 Uiso 1 1 d R
H42 H -0.2360 0.2577 0.8869 0.057 Uiso 1 1 d R
H43 H -0.1212 0.2972 1.0480 0.057 Uiso 1 1 d R
C5 C 0.1524(2) 0.23112(19) 0.99522(17) 0.0338(3) Uani 1 1 d .
O5 O 0.14973(16) 0.17507(17) 1.08119(14) 0.0452(3) Uani 1 1 d .
N6 N 0.29924(17) 0.26195(17) 0.96334(14) 0.0343(3) Uani 1 1 d .
C6 C 0.4448(2) 0.2179(3) 1.0371(2) 0.0471(4) Uani 1 1 d .
H61 H 0.5147 0.1937 0.9804 0.057 Uiso 1 1 d R
H62 H 0.3967 0.1182 1.0508 0.057 Uiso 1 1 d R
H63 H 0.5201 0.3117 1.1299 0.057 Uiso 1 1 d R
C7 C 0.3211(2) 0.3330(2) 0.87202(17) 0.0331(3) Uani 1 1 d .
O7 O 0.45824(15) 0.35773(17) 0.85600(13) 0.0437(3) Uani 1 1 d .
C7A C 0.1708(2) 0.3689(2) 0.80528(17) 0.0333(3) Uani 1 1 d .
N1P N 0.6319(2) 0.0869(2) 0.3182(2) 0.0594(5) Uani 1 1 d .
C2P C 0.6219(3) -0.0061(3) 0.3895(3) 0.0592(5) Uani 1 1 d .
H2P H 0.5100 -0.0490 0.3906 0.071 Uiso 1 1 d R
C3P C 0.7617(3) -0.0416(3) 0.4620(2) 0.0520(5) Uani 1 1 d .
H3P H 0.7452 -0.1060 0.5140 0.062 Uiso 1 1 d R
C4P C 0.9226(2) 0.0166(2) 0.46071(19) 0.0402(4) Uani 1 1 d .
C5P C 0.9315(3) 0.1081(3) 0.3824(2) 0.0537(5) Uani 1 1 d .
H5P H 1.0400 0.1476 0.3749 0.064 Uiso 1 1 d R
C6P C 0.7862(3) 0.1408(3) 0.3152(3) 0.0613(6) Uani 1 1 d .
H6P H 0.7988 0.2058 0.2631 0.074 Uiso 1 1 d R
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
O3W Mn O3W 179.999(2) . 2_666
O3W Mn O2W 88.78(5) . 2_666
O3W Mn O2W 91.22(5) 2_666 2_666
O3W Mn O2W 91.22(5) . .
O3W Mn O2W 88.78(5) 2_666 .
O2W Mn O2W 180.00(7) 2_666 .
O3W Mn O1W 91.50(5) . 2_666
O3W Mn O1W 88.50(5) 2_666 2_666
O2W Mn O1W 89.98(6) 2_666 2_666
O2W Mn O1W 90.02(6) . 2_666
O3W Mn O1W 88.50(5) . .
O3W Mn O1W 91.50(5) 2_666 .
O2W Mn O1W 90.02(6) 2_666 .
O2W Mn O1W 89.98(6) . .
O1W Mn O1W 179.999(1) 2_666 .
Mn O1W H11W 112.6(16) . .
Mn O1W H12W 111(2) . .
H11W O1W H12W 103(3) . .
Mn O2W H21W 131.5(19) . .
Mn O2W H22W 122.2(19) . .
H21W O2W H22W 106(3) . .
Mn O3W H31W 126.6(16) . .
Mn O3W H32W 129.0(17) . .
H31W O3W H32W 104(2) . .
N2 N1 C7A 106.49(13) . .
N1 N2 N3 112.10(13) . .
C3A N3 N2 104.79(13) . .
N3 C3A N4 127.92(15) . .
N3 C3A C7A 109.30(14) . .
N4 C3A C7A 122.77(14) . .
C3A N4 C5 119.17(13) . .
C3A N4 C4 121.42(14) . .
C5 N4 C4 119.39(14) . .
N4 C4 H41 110.0 . .
N4 C4 H42 109.0 . .
H41 C4 H42 109.6 . .
N4 C4 H43 109.4 . .
H41 C4 H43 110.3 . .
H42 C4 H43 108.6 . .
O5 C5 N4 121.51(15) . .
O5 C5 N6 121.37(15) . .
N4 C5 N6 117.12(14) . .
C7 N6 C5 126.67(13) . .
C7 N6 C6 117.36(13) . .
C5 N6 C6 115.95(14) . .
N6 C6 H61 110.2 . .
N6 C6 H62 108.7 . .
H61 C6 H62 109.1 . .
N6 C6 H63 108.7 . .
H61 C6 H63 109.5 . .
H62 C6 H63 110.7 . .
O7 C7 N6 120.47(14) . .
O7 C7 C7A 127.13(15) . .
N6 C7 C7A 112.40(13) . .
N1 C7A C3A 107.32(14) . .
N1 C7A C7 130.94(14) . .
C3A C7A C7 121.74(14) . .
C6P N1P C2P 116.14(18) . .
N1P C2P C3P 123.7(2) . .
N1P C2P H2P 117.4 . .
C3P C2P H2P 118.9 . .
C2P C3P C4P 120.0(2) . .
C2P C3P H3P 118.9 . .
C4P C3P H3P 121.1 . .
C3P C4P C5P 116.28(17) . .
C3P C4P C4P 121.8(2) . 2_756
C5P C4P C4P 121.9(2) . 2_756
C6P C5P C4P 120.0(2) . .
C6P C5P H5P 120.6 . .
C4P C5P H5P 119.4 . .
N1P C6P C5P 123.8(2) . .
N1P C6P H6P 119.1 . .
C5P C6P H6P 117.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn O3W 2.1349(12) .
Mn O3W 2.1349(12) 2_666
Mn O2W 2.1722(12) 2_666
Mn O2W 2.1722(12) .
Mn O1W 2.2158(14) 2_666
Mn O1W 2.2158(14) .
O1W H11W 0.835(10) .
O1W H12W 0.835(10) .
O2W H21W 0.830(10) .
O2W H22W 0.845(10) .
O3W H31W 0.840(10) .
O3W H32W 0.831(10) .
N1 N2 1.312(2) .
N1 C7A 1.356(2) .
N2 N3 1.363(2) .
N3 C3A 1.336(2) .
C3A N4 1.372(2) .
C3A C7A 1.373(2) .
N4 C5 1.372(2) .
N4 C4 1.463(2) .
C4 H41 1.0093 .
C4 H42 0.9860 .
C4 H43 0.9912 .
C5 O5 1.2120(19) .
C5 N6 1.405(2) .
N6 C7 1.394(2) .
N6 C6 1.466(2) .
C6 H61 0.9937 .
C6 H62 1.0019 .
C6 H63 1.0010 .
C7 O7 1.2274(19) .
C7 C7A 1.426(2) .
N1P C6P 1.329(3) .
N1P C2P 1.335(3) .
C2P C3P 1.378(3) .
C2P H2P 0.9656 .
C3P C4P 1.381(3) .
C3P H3P 0.9610 .
C4P C5P 1.386(3) .
C4P C4P 1.485(3) 2_756
C5P C6P 1.378(3) .
C5P H5P 0.9653 .
C6P H6P 0.9608 .
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
O1W H12W N1P 0.835(10) 2.003(13) 2.814(2) 164(3) .
O1W H11W O5 0.835(10) 1.918(10) 2.7489(18) 173(2) 1_554
O2W H21W O7 0.830(10) 1.899(11) 2.7207(17) 170(3) .
O2W H22W N3 0.845(10) 1.937(10) 2.7795(19) 174(3) 1_655
O3W H32W N1 0.831(10) 1.944(10) 2.7752(19) 179(3) .
O3W H31W N2 0.840(10) 1.957(11) 2.7767(19) 165(2) 2_566
