#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/22/2102230.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_2102230
loop_
_publ_author_name
'Godino Salido, M. Luz'
'Arranz Mascarós, Paloma'
'López Garzón, Rafael'
'Gutiérrez Valero, M. Dolores'
'Low, John N.'
'Gallagher, John F.'
'Glidewell, Christopher'
_publ_section_title
;
 Hydrated metal(II) complexes of
 N-(6-amino-3,4-dihydro-3-methyl-5-nitroso-4-oxopyrimidin-2-yl)
 derivatives of glycine, glycylglycine, threonine, serine, valine and
 methionine: a monomeric complex and coordination polymers in one, two
 and three dimensions linked by hydrogen bonding
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              46
_journal_page_last               64
_journal_paper_doi               10.1107/S0108768103029136
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C14 H24 Ca N10 O12, 4(H2 O)'
_chemical_formula_sum            'C14 H32 Ca N10 O16'
_chemical_formula_weight         636.58
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.850(6)
_cell_angle_beta                 97.040(8)
_cell_angle_gamma                110.038(8)
_cell_formula_units_Z            1
_cell_length_a                   7.4540(7)
_cell_length_b                   7.6148(11)
_cell_length_c                   12.5939(17)
_cell_measurement_reflns_used    2833
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.91
_cell_volume                     658.52(15)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997a) and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.945
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.103
_diffrn_reflns_av_sigmaI/netI    0.1774
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5368
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.509
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1647
_refine_ls_R_factor_gt           0.0566
_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)+(0.0574P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                1311
_reflns_number_total             2833
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na5011.cif
_cod_data_source_block           I
_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        658.52(14)
_cod_database_code               2102230
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
Ca1 0.5000 0.5000 0.5000 0.0224(3) Uani d S 1 Ca
N1 0.1464(4) 0.6740(4) 0.9192(3) 0.0207(8) Uani d . 1 N
C2 -0.0348(5) 0.6066(5) 0.8681(3) 0.0190(9) Uani d . 1 C
N2 -0.0766(4) 0.4935(4) 0.7736(3) 0.0225(8) Uani d . 1 N
C121 0.0710(5) 0.4482(5) 0.7239(3) 0.0237(10) Uani d . 1 C
C122 0.1635(5) 0.5834(6) 0.6486(3) 0.0247(10) Uani d . 1 C
O121 0.2939(4) 0.5489(4) 0.6072(2) 0.0311(8) Uani d . 1 O
O122 0.1071(4) 0.7171(4) 0.6330(2) 0.0292(7) Uani d . 1 O
N3 -0.1861(4) 0.6406(4) 0.9076(3) 0.0186(8) Uani d . 1 N
C3 -0.3839(5) 0.5626(6) 0.8454(3) 0.0259(10) Uani d . 1 C
C4 -0.1558(5) 0.7495(5) 1.0078(3) 0.0203(9) Uani d . 1 C
O4 -0.2925(3) 0.7746(4) 1.0436(2) 0.0292(7) Uani d . 1 O
C5 0.0419(5) 0.8280(5) 1.0657(3) 0.0203(9) Uani d . 1 C
N5 0.0640(4) 0.9379(5) 1.1596(3) 0.0246(8) Uani d . 1 N
O5 0.2372(4) 1.0115(4) 1.2156(2) 0.0272(7) Uani d . 1 O
C6 0.1858(5) 0.7826(5) 1.0155(3) 0.0216(10) Uani d . 1 C
N6 0.3677(4) 0.8490(5) 1.0660(3) 0.0256(9) Uani d . 1 N
O1 0.2418(3) 0.2450(4) 0.3919(2) 0.0263(7) Uani d . 1 O
O2 0.4387(4) 0.7072(4) 0.3833(2) 0.0271(7) Uani d . 1 O
O3 0.2328(4) 0.8914(4) 0.4647(2) 0.0381(8) Uani d . 1 O
O4W 0.6811(4) 0.9173(4) 0.2596(2) 0.0357(8) Uani d . 1 O
H2 -0.1976 0.4448 0.7401 0.027 Uiso calc R 1 H
H12A 0.0122 0.3186 0.6825 0.028 Uiso calc R 1 H
H12B 0.1736 0.4484 0.7819 0.028 Uiso calc R 1 H
H3A -0.4304 0.4241 0.8361 0.039 Uiso calc R 1 H
H3B -0.3836 0.6040 0.7742 0.039 Uiso calc R 1 H
H3C -0.4695 0.6078 0.8845 0.039 Uiso calc R 1 H
H6A 0.4571 0.8212 1.0359 0.031 Uiso calc R 1 H
H6B 0.3993 0.9210 1.1297 0.031 Uiso calc R 1 H
H1X 0.1211 0.2598 0.3806 0.032 Uiso d R 1 H
H1Y 0.2507 0.1624 0.3338 0.032 Uiso d R 1 H
H2X 0.5286 0.7725 0.3416 0.033 Uiso d R 1 H
H2Y 0.3700 0.7771 0.4135 0.033 Uiso d R 1 H
H3X 0.1768 0.8379 0.5223 0.046 Uiso d R 1 H
H3Y 0.2269 1.0131 0.4674 0.046 Uiso d R 1 H
H4X 0.7438 0.9011 0.2010 0.043 Uiso d R 1 H
H4Y 0.7418 1.0436 0.2935 0.043 Uiso d R 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 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'
Ca Ca 0.2262 0.3064 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O121 Ca1 O121 . 2_666 180.0000(10) no
O121 Ca1 O1 . 2_666 90.01(9) no
O121 Ca1 O1 2_666 2_666 89.99(9) no
O121 Ca1 O1 . . 89.99(9) no
O121 Ca1 O1 2_666 . 90.01(9) no
O1 Ca1 O1 2_666 . 180.0 no
O121 Ca1 O2 . 2_666 88.20(10) no
O121 Ca1 O2 2_666 2_666 91.80(10) no
O1 Ca1 O2 2_666 2_666 89.41(9) no
O1 Ca1 O2 . 2_666 90.59(9) no
O121 Ca1 O2 . . 91.80(10) no
O121 Ca1 O2 2_666 . 88.20(10) no
O1 Ca1 O2 2_666 . 90.59(9) no
O1 Ca1 O2 . . 89.41(9) no
O2 Ca1 O2 2_666 . 180.00(10) no
C2 N1 C6 . . 117.9(3) no
N1 C2 N2 . . 118.3(3) no
N1 C2 N3 . . 124.4(3) no
N2 C2 N3 . . 117.2(3) no
C2 N2 C121 . . 122.1(3) no
C2 N2 H2 . . 119.0 no
C121 N2 H2 . . 119.0 no
N2 C121 C122 . . 114.2(3) no
N2 C121 H12A . . 108.7 no
C122 C121 H12A . . 108.7 no
N2 C121 H12B . . 108.7 no
C122 C121 H12B . . 108.7 no
H12A C121 H12B . . 107.6 no
O121 C122 O122 . . 125.5(4) no
O121 C122 C121 . . 114.9(4) no
O122 C122 C121 . . 119.6(3) no
C122 O121 Ca1 . . 167.9(3) no
C2 N3 C4 . . 120.7(3) no
C2 N3 C3 . . 121.3(3) no
C4 N3 C3 . . 118.0(3) 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
O4 C4 N3 . . 120.1(3) no
O4 C4 C5 . . 123.4(4) no
N3 C4 C5 . . 116.5(3) no
N5 C5 C6 . . 128.8(3) no
N5 C5 C4 . . 113.9(3) no
C6 C5 C4 . . 117.3(4) no
O5 N5 C5 . . 117.0(3) no
N6 C6 N1 . . 117.4(3) no
N6 C6 C5 . . 119.4(4) no
N1 C6 C5 . . 123.2(3) no
C6 N6 H6A . . 120.0 no
C6 N6 H6B . . 120.0 no
H6A N6 H6B . . 120.0 no
Ca1 O1 H1X . . 116.3 no
Ca1 O1 H1Y . . 126.6 no
H1X O1 H1Y . . 110.1 no
Ca1 O2 H2X . . 122.9 no
Ca1 O2 H2Y . . 111.6 no
H2X O2 H2Y . . 114.6 no
H3X O3 H3Y . . 107.8 no
H4X O4W H4Y . . 107.4 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
Ca1 O121 . 2.263(3) no
Ca1 O121 2_666 2.263(3) no
Ca1 O1 2_666 2.363(3) no
Ca1 O1 . 2.363(3) no
Ca1 O2 2_666 2.379(3) no
Ca1 O2 . 2.379(3) no
N1 C2 . 1.321(5) no
N1 C6 . 1.336(5) no
C2 N2 . 1.331(5) no
C2 N3 . 1.377(4) no
N2 C121 . 1.451(4) no
N2 H2 . 0.88 no
C121 C122 . 1.520(5) no
C121 H12A . 0.99 no
C121 H12B . 0.99 no
C122 O121 . 1.247(4) no
C122 O122 . 1.251(5) no
N3 C4 . 1.386(5) no
N3 C3 . 1.471(4) no
C3 H3A . 0.98 no
C3 H3B . 0.98 no
C3 H3C . 0.98 no
C4 O4 . 1.227(4) no
C4 C5 . 1.451(5) no
C5 N5 . 1.335(5) no
C5 C6 . 1.430(5) no
N5 O5 . 1.296(4) no
C6 N6 . 1.323(5) no
N6 H6A . 0.88 no
N6 H6B . 0.88 no
O1 H1X . 0.94 no
O1 H1Y . 0.94 no
O2 H2X . 0.94 no
O2 H2Y . 0.94 no
O3 H3X . 0.94 no
O3 H3Y . 0.94 no
O4W H4X . 0.94 no
O4W H4Y . 0.94 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 O2 2_566 0.88 2.12 2.962(4) 159 y
N6 H6A O4 1_655 0.88 2.01 2.818(4) 152 y
N6 H6B O5 . 0.88 1.96 2.613(4) 130 y
O1 H1X O122 2_566 0.94 1.76 2.698(4) 177 y
O1 H1Y O5 1_544 0.94 1.75 2.688(4) 172 y
O2 H2X O4W . 0.94 1.80 2.733(3) 172 y
O2 H2Y O3 . 0.94 1.70 2.635(4) 176 y
O3 H3X O122 . 0.94 1.78 2.710(4) 169 y
O3 H3Y O1 1_565 0.94 2.07 2.914(4) 149 y
O4W H4X O4 1_654 0.94 2.06 2.880(4) 145 y
O4W H4X N5 1_654 0.94 2.43 3.220(4) 141 y
O4W H4Y O122 2_676 0.94 1.85 2.787(4) 172 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 . -178.0(4) no
C6 N1 C2 N3 . 0.0(6) no
N1 C2 N2 C121 . -2.1(6) no
N3 C2 N2 C121 . 179.8(3) no
C2 N2 C121 C122 . -90.3(5) no
N2 C121 C122 O121 . 178.4(3) no
N2 C121 C122 O122 . -1.3(5) no
O122 C122 O121 Ca1 . -42.6(15) no
C121 C122 O121 Ca1 . 137.7(11) no
O1 Ca1 O121 C122 2_666 116.5(13) no
O1 Ca1 O121 C122 . -63.5(13) no
O2 Ca1 O121 C122 2_666 -154.1(13) no
O2 Ca1 O121 C122 . 25.9(13) no
N1 C2 N3 C4 . -1.0(6) no
N2 C2 N3 C4 . 177.0(4) no
N1 C2 N3 C3 . 179.2(4) no
N2 C2 N3 C3 . -2.8(5) no
C2 N3 C4 O4 . -177.9(3) no
C3 N3 C4 O4 . 1.9(5) no
C2 N3 C4 C5 . 1.7(5) no
C3 N3 C4 C5 . -178.5(3) no
O4 C4 C5 N5 . -3.0(6) no
N3 C4 C5 N5 . 177.4(3) no
O4 C4 C5 C6 . 178.2(4) no
N3 C4 C5 C6 . -1.4(5) no
C6 C5 N5 O5 . -1.7(6) no
C4 C5 N5 O5 . 179.6(3) no
C2 N1 C6 N6 . 179.9(3) no
C2 N1 C6 C5 . 0.2(6) no
N5 C5 C6 N6 . 2.2(6) no
C4 C5 C6 N6 . -179.1(4) no
N5 C5 C6 N1 . -178.2(4) no
C4 C5 C6 N1 . 0.5(6) no
