#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/36/2103664.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2103664
loop_
_publ_author_name
'Low, John N.'
'Moreno Sánchez, Jose M.'
'Arranz Mascarós, Paloma'
'Godino Salido, M. Luz'
'López Garzon, Rafael'
'Cobo Domingo, Justo'
'Glidewell, Christopher'
_publ_section_title
;Hydrated metal complexes of
 N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl)glycinate:
 interplay of molecular, molecular--electronic and supramolecular structures
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              317
_journal_page_last               328
_journal_paper_doi               10.1107/S0108768100020280
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C14 H24 Mn N10 O12, 6(H2 O)'
_chemical_formula_sum            'C14 H36 Mn N10 O18'
_chemical_formula_weight         687.46
_chemical_name_systematic
;
Tetraaqua-bis[N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-
oxopyrimidin-2-yl)glycinato]manganese(II) hexahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                105.258(2)
_cell_angle_beta                 92.153(3)
_cell_angle_gamma                108.94(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4476(3)
_cell_length_b                   8.2351(4)
_cell_length_c                   12.6372(5)
_cell_measurement_reflns_used    3131
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.69
_cell_volume                     700.80(11)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976), PLATON (Spek, 2000)'
_computing_publication_material
'SHELXL-97  and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full .974
_diffrn_measured_fraction_theta_max .974
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .068
_diffrn_reflns_av_sigmaI/netI    .0456
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7489
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .569
_exptl_absorpt_correction_T_max  .9586
_exptl_absorpt_correction_T_min  .7840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995 & 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             359
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .08
_refine_diff_density_max         .499
_refine_diff_density_min         -.570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3131
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          .0457
_refine_ls_R_factor_gt           .0400
_refine_ls_shift/su_max          .006
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0452P)²+0.4451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1066
_reflns_number_gt                2814
_reflns_number_total             3131
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            na0116.cif
_cod_data_source_block           MnL2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        700.81(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2103664
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Mn1 .5000 .0000 .5000 .01698(13) Uani d S 1 Mn
N1 .1453(2) .1486(2) .91956(13) .0187(3) Uani d . 1 N
C2 -.0347(3) .0625(2) .87141(15) .0173(4) Uani d . 1 C
N2 -.0704(2) -.0790(2) .78329(13) .0197(3) Uani d . 1 N
C21 .0819(3) -.1344(3) .73489(16) .0206(4) Uani d . 1 C
C22 .1847(2) -.0280(2) .65941(14) .0171(4) Uani d . 1 C
O21 .32251(18) -.07366(18) .62267(11) .0211(3) Uani d . 1 O
O22 .13010(19) .08985(18) .63825(11) .0219(3) Uani d . 1 O
C3 -.3836(3) .0089(3) .84736(17) .0247(4) Uani d . 1 C
N3 -.1892(2) .1080(2) .90783(13) .0184(3) Uani d . 1 N
C4 -.1650(3) .2478(3) 1.00356(15) .0187(4) Uani d . 1 C
O4 -.3040(2) .2836(2) 1.03735(12) .0269(3) Uani d . 1 O
C5 .0298(3) .3443(3) 1.05824(15) .0179(4) Uani d . 1 C
N5 .0466(2) .4789(2) 1.14923(13) .0217(3) Uani d . 1 N
O5 .2152(2) .5711(2) 1.20237(12) .0270(3) Uani d . 1 O
C6 .1810(3) .2877(3) 1.01120(15) .0178(4) Uani d . 1 C
N6 .3591(2) .3701(2) 1.05951(14) .0226(3) Uani d . 1 N
O1W .4172(2) .23277(18) .52434(12) .0241(3) Uani d D 1 O
O2W .2367(2) -.1481(2) .37756(12) .0276(3) Uani d D 1 O
O3W .3797(2) .36643(19) .35193(13) .0294(3) Uani d D 1 O
O4W .1927(3) .5302(3) .5202(2) .0554(6) Uani d D 1 O
O5W .6924(3) .5341(2) .25271(16) .0458(5) Uani d D 1 O
H2 -.1899 -.1411 .7533 .024 Uiso calc R 1 H
H21A .0271 -.2627 .6919 .025 Uiso calc R 1 H
H21B .1774 -.1232 .7955 .025 Uiso calc R 1 H
H3A -.3815 .0022 .7689 .037 Uiso calc R 1 H
H3B -.4704 .0712 .8779 .037 Uiso calc R 1 H
H3C -.4282 -.1127 .8551 .037 Uiso calc R 1 H
H6A .4508 .3338 1.0317 .027 Uiso calc R 1 H
H6B .3867 .4617 1.1197 .027 Uiso calc R 1 H
H1W1 .2982(17) .206(3) .5541(16) .029 Uiso d D 1 H
H2W1 .402(3) .275(3) .4621(13) .029 Uiso d D 1 H
H1W2 .121(2) -.121(3) .377(2) .043(7) Uiso d D 1 H
H2W2 .210(4) -.266(2) .328(2) .084(12) Uiso d D 1 H
H1W3 .494(3) .434(3) .329(3) .087(12) Uiso d D 1 H
H2W3 .323(4) .449(3) .392(3) .077(11) Uiso d D 1 H
H1W4 .067(3) .511(5) .488(4) .135(19) Uiso d D 1 H
H2W4 .258(5) .6570(12) .550(3) .104(15) Uiso d D 1 H
H1W5 .762(3) .480(3) .2016(19) .055 Uiso d D 1 H
H2W5 .769(3) .6574(13) .286(2) .055 Uiso d D 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn .3368 .7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1W Mn1 O1W . 2_656 180.0 no
O1W Mn1 O21 . 2_656 91.84(5) no
O1W Mn1 O21 2_656 2_656 88.16(5) no
O1W Mn1 O21 . . 88.16(5) no
O1W Mn1 O21 2_656 . 91.84(5) no
O21 Mn1 O21 2_656 . 180.0 no
O1W Mn1 O2W . . 87.15(6) no
O1W Mn1 O2W 2_656 . 92.85(6) no
O21 Mn1 O2W 2_656 . 93.72(5) no
O21 Mn1 O2W . . 86.28(5) no
O1W Mn1 O2W . 2_656 92.85(6) no
O1W Mn1 O2W 2_656 2_656 87.15(6) no
O21 Mn1 O2W 2_656 2_656 86.28(5) no
O21 Mn1 O2W . 2_656 93.72(5) no
O2W Mn1 O2W . 2_656 180.0 no
C2 N1 C6 . . 118.46(15) no
N2 C2 N1 . . 118.28(16) no
N2 C2 N3 . . 117.25(16) no
N1 C2 N3 . . 124.45(17) no
C2 N2 C21 . . 121.97(16) no
C2 N2 H2 . . 119.0 no
C21 N2 H2 . . 119.0 no
N2 C21 C22 . . 114.76(15) no
N2 C21 H21A . . 108.6 no
C22 C21 H21A . . 108.6 no
N2 C21 H21B . . 108.6 no
C22 C21 H21B . . 108.6 no
H21A C21 H21B . . 107.6 no
O22 C22 O21 . . 126.21(16) no
O22 C22 C21 . . 120.52(15) no
O21 C22 C21 . . 113.27(16) no
C22 O21 Mn1 . . 131.54(12) no
N3 C3 H3A . . 109.5 no
N3 C3 H3B . . 109.5 no
H3A C3 H3B . . 109.5 no
N3 C3 H3C . . 109.5 no
H3A C3 H3C . . 109.5 no
H3B C3 H3C . . 109.5 no
C2 N3 C4 . . 120.64(16) no
C2 N3 C3 . . 120.96(16) no
C4 N3 C3 . . 118.39(15) no
O4 C4 N3 . . 120.23(17) no
O4 C4 C5 . . 123.57(17) no
N3 C4 C5 . . 116.20(15) no
N5 C5 C6 . . 127.45(17) no
N5 C5 C4 . . 114.18(15) no
C6 C5 C4 . . 118.37(16) no
O5 N5 C5 . . 117.91(15) no
N6 C6 N1 . . 118.07(16) no
N6 C6 C5 . . 120.10(17) no
N1 C6 C5 . . 121.81(17) no
C6 N6 H6A . . 120.0 no
C6 N6 H6B . . 120.0 no
H6A N6 H6B . . 120.0 no
Mn1 O1W H1W1 . . 106.8(13) no
Mn1 O1W H2W1 . . 118.6(14) no
H1W1 O1W H2W1 . . 108(2) no
Mn1 O2W H1W2 . . 126.6(14) no
Mn1 O2W H2W2 . . 124.1(15) no
H1W2 O2W H2W2 . . 108(2) no
H1W3 O3W H2W3 . . 108(2) no
H1W4 O4W H2W4 . . 108(3) no
H1W5 O5W H2W5 . . 109(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1W . 2.1498(13) no
Mn1 O1W 2_656 2.1498(13) no
Mn1 O21 2_656 2.1555(12) no
Mn1 O21 . 2.1556(12) no
Mn1 O2W . 2.2254(14) no
Mn1 O2W 2_656 2.2254(15) no
N1 C2 . 1.328(2) no
N1 C6 . 1.344(2) no
C2 N2 . 1.327(3) no
C2 N3 . 1.381(2) no
N2 C21 . 1.452(2) no
N2 H2 . .8800 no
C21 C22 . 1.524(2) no
C21 H21A . .9900 no
C21 H21B . .9900 no
C22 O22 . 1.250(2) no
C22 O21 . 1.267(2) no
C3 N3 . 1.472(2) no
C3 H3A . .9800 no
C3 H3B . .9800 no
C3 H3C . .9800 no
N3 C4 . 1.392(2) no
C4 O4 . 1.227(2) no
C4 C5 . 1.449(3) no
C5 N5 . 1.340(3) no
C5 C6 . 1.444(2) no
N5 O5 . 1.286(2) no
C6 N6 . 1.315(2) no
N6 H6A . .8800 no
N6 H6B . .8800 no
O1W H1W1 . .96(2) no
O1W H2W1 . .96(2) no
O2W H1W2 . .96(2) no
O2W H2W2 . .96(2) no
O3W H1W3 . .96(3) no
O3W H2W3 . .96(3) no
O4W H1W4 . .95(3) no
O4W H2W4 . .96(2) no
O5W H1W5 . .95(2) no
O5W H2W5 . .96(2) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2 O3W 2_556 .88 2.02 2.804(2) 148 y
N6 H6A O4 1_655 .88 2.00 2.828(2) 156 y
N6 H6B O5 . .88 1.97 2.620(2) 130 y
O1W H1W1 O22 . .96(2) 1.86(2) 2.742(2) 151(2) y
O1W H2W1 O3W . .96(2) 1.77(2) 2.731(2) 177(2) y
O2W H1W2 O22 2_556 .96(2) 1.98(2) 2.933(2) 174(2) y
O2W H2W2 O5 1_544 .96(2) 1.80(2) 2.705(2) 156(2) y
O3W H1W3 O5W . .96(3) 1.88(3) 2.817(3) 167(3) y
O3W H2W3 O4W . .96(3) 2.00(3) 2.865(3) 150(3) y
O4W H1W4 O4W 2_566 .95(3) 1.85(3) 2.754(3) 158(4) y
O4W H2W4 O21 1_565 .96(2) 2.05(2) 2.981(3) 164(3) y
O5W H1W5 O4 1_654 .95(2) 2.19(2) 2.958(2) 137(2) y
O5W H1W5 N5 1_654 .95(2) 2.24(2) 3.100(3) 148(2) y
O5W H2W5 O22 2_666 .96(2) 1.92(2) 2.864(2) 167(2) y
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_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C2 N2 . -177.54(16) no
C6 N1 C2 N3 . 1.3(3) no
N1 C2 N2 C21 . -3.8(3) no
N3 C2 N2 C21 . 177.24(15) no
C2 N2 C21 C22 . -80.4(2) no
N2 C21 C22 O22 . -3.8(3) no
N2 C21 C22 O21 . 176.85(15) no
O22 C22 O21 Mn1 . -7.5(3) no
C21 C22 O21 Mn1 . 171.83(12) no
O1W Mn1 O21 C22 . 20.30(16) no
O1W Mn1 O21 C22 2_656 -159.70(16) no
O2W Mn1 O21 C22 . -66.96(16) no
O2W Mn1 O21 C22 2_656 113.04(16) no
N2 C2 N3 C4 . 176.06(15) no
N1 C2 N3 C4 . -2.8(3) no
N2 C2 N3 C3 . -3.2(2) no
N1 C2 N3 C3 . 177.98(17) no
C2 N3 C4 O4 . -177.60(16) no
C3 N3 C4 O4 . 1.7(3) no
C2 N3 C4 C5 . 2.4(2) no
C3 N3 C4 C5 . -178.33(16) no
O4 C4 C5 N5 . -.7(3) no
N3 C4 C5 N5 . 179.25(15) no
O4 C4 C5 C6 . 179.13(17) no
N3 C4 C5 C6 . -.9(2) no
C6 C5 N5 O5 . .2(3) no
C4 C5 N5 O5 . -179.93(15) no
C2 N1 C6 N6 . 178.78(16) no
C2 N1 C6 C5 . .3(3) no
N5 C5 C6 N6 . .9(3) no
C4 C5 C6 N6 . -178.90(16) no
N5 C5 C6 N1 . 179.34(17) no
C4 C5 C6 N1 . -.5(3) no
