#------------------------------------------------------------------------------
#$Date: 2017-07-01 11:43:35 +0300 (Sat, 01 Jul 2017) $
#$Revision: 198310 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/26/4032607.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_4032607
loop_
_publ_author_name
'N.N. Golovnev'
'M.S. Molokeev'
'M.K. Lesnikov'
'S.N. Vereshchagin'
_publ_section_title
;
 Polymeric Lithium(I) Diaquabarbiturate: Crystal Structure
;
_journal_issue                   6
_journal_name_full               'Russian Journal of Inorganic Chemistry'
_journal_page_first              746
_journal_page_last               750
_journal_paper_doi               10.1134/S0036023617060092
_journal_volume                  62
_journal_year                    2017
_chemical_formula_moiety         'C4 H7 Li N2 O5'
_chemical_formula_sum            'C4 H7 Li N2 O5'
_chemical_formula_weight         170.06
_chemical_name_systematic
;
Catena-diaquabarbiturate lithium(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.253(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4306(7)
_cell_length_b                   16.7199(14)
_cell_length_c                   7.1732(8)
_cell_measurement_reflns_used    6236
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.563
_cell_measurement_theta_min      2.436
_cell_volume                     732.45(13)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6236
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.563
_diffrn_reflns_theta_min         2.436
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         6236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0363
_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)+(0.0496P)²+0.1448P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5492
_reflns_number_total             6236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            LiHbarH2O2.cif
_cod_data_source_block           z
_cod_database_code               4032607
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Li Li 0.7381(4) 0.41581(16) 0.5103(4) 0.0200(6) Uani 1 1 d . . . . .
N1 N -0.0531(2) 0.25764(7) 0.10011(18) 0.0160(3) Uani 1 1 d . . . . .
H1 H -0.1845 0.2442 0.0335 0.019 Uiso 1 1 calc R U . . .
O1 O -0.14878(18) 0.38880(6) 0.05965(16) 0.0215(3) Uani 1 1 d . . . . .
C2 C -0.0067(2) 0.33645(9) 0.1266(2) 0.0154(3) Uani 1 1 d . . . . .
N3 N 0.2028(2) 0.35516(8) 0.23122(18) 0.0166(3) Uani 1 1 d . . . . .
H3 H 0.2360 0.4050 0.2497 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3682(2) 0.29949(9) 0.3110(2) 0.0157(3) Uani 1 1 d . . . . .
O2 O 0.55557(17) 0.32604(6) 0.40300(16) 0.0216(3) Uani 1 1 d . . . . .
C5 C 0.3099(2) 0.21895(9) 0.2809(2) 0.0160(3) Uani 1 1 d . . . . .
H5 H 0.4143 0.1797 0.3335 0.019 Uiso 1 1 calc R U . . .
C6 C 0.0983(2) 0.19654(9) 0.1737(2) 0.0150(3) Uani 1 1 d . . . . .
O3 O 0.02722(17) 0.12584(6) 0.13568(16) 0.0207(3) Uani 1 1 d . . . . .
O1W O 0.68490(19) 0.47542(7) 0.72439(17) 0.0195(3) Uani 1 1 d . . . . .
H11 H 0.547(3) 0.4824(11) 0.723(3) 0.029 Uiso 1 1 d . U . . .
H12 H 0.755(3) 0.4463(11) 0.831(3) 0.029 Uiso 1 1 d . U . . .
O2W O 0.73598(18) 0.49248(7) 0.30371(17) 0.0188(3) Uani 1 1 d . . . . .
H21 H 0.773(3) 0.4646(11) 0.222(3) 0.028 Uiso 1 1 d . U . . .
H22 H 0.813(3) 0.5392(12) 0.316(3) 0.028 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'
Li Li -0.0003 0.0001 '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
O2 Li O3 106.58(13) . 4_666
O2 Li O1W 118.78(15) . .
O3 Li O1W 101.48(13) 4_666 .
O2 Li O2W 110.60(14) . .
O3 Li O2W 111.57(14) 4_666 .
O1W Li O2W 107.49(14) . .
O2 Li H12 113.7(5) . .
O3 Li H12 83.0(5) 4_666 .
O1W Li H12 22.1(5) . .
O2W Li H12 126.4(5) . .
O2 Li H21 97.9(5) . .
O3 Li H21 101.3(5) 4_666 .
O1W Li H21 128.2(5) . .
O2W Li H21 20.9(5) . .
H12 Li H21 145.6(7) . .
C2 N1 C6 124.30(13) . .
C2 N1 H1 117.9 . .
C6 N1 H1 117.9 . .
O1 C2 N1 121.82(14) . .
O1 C2 N3 122.10(14) . .
N1 C2 N3 116.08(13) . .
C2 N3 C4 124.77(13) . .
C2 N3 H3 117.6 . .
C4 N3 H3 117.6 . .
O2 C4 N3 117.47(14) . .
O2 C4 C5 125.97(14) . .
N3 C4 C5 116.56(13) . .
C4 O2 Li 148.57(14) . .
C6 C5 C4 121.00(14) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
O3 C6 C5 126.62(14) . .
O3 C6 N1 116.10(13) . .
C5 C6 N1 117.28(13) . .
C6 O3 Li 132.02(12) . 4_465
Li O1W H11 118.5(12) . .
Li O1W H12 103.3(12) . .
H11 O1W H12 108.2(17) . .
Li O2W H21 103.4(13) . .
Li O2W H22 127.6(11) . .
H21 O2W H22 106.1(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Li O2 1.912(3) .
Li O3 1.925(3) 4_666
Li O1W 1.949(3) .
Li O2W 1.956(3) .
Li H12 2.328(19) .
Li H21 2.302(19) .
N1 C2 1.3513(19) .
N1 C6 1.3956(19) .
N1 H1 0.8600 .
O1 C2 1.2479(18) .
C2 N3 1.3575(19) .
N3 C4 1.394(2) .
N3 H3 0.8600 .
C4 O2 1.2595(18) .
C4 C5 1.396(2) .
C5 C6 1.388(2) .
C5 H5 0.9300 .
C6 O3 1.2660(18) .
O3 Li 1.925(3) 4_465
O1W H11 0.89(2) .
O1W H12 0.90(2) .
O2W H21 0.842(19) .
O2W H22 0.91(2) .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C6 N1 C2 O1 -179.11(13) . . . .
C6 N1 C2 N3 0.4(2) . . . .
O1 C2 N3 C4 179.46(13) . . . .
N1 C2 N3 C4 -0.1(2) . . . .
C2 N3 C4 O2 179.31(14) . . . .
C2 N3 C4 C5 -0.7(2) . . . .
N3 C4 O2 Li 6.6(3) . . . .
C5 C4 O2 Li -173.4(2) . . . .
O2 C4 C5 C6 -178.84(15) . . . .
N3 C4 C5 C6 1.1(2) . . . .
C4 C5 C6 O3 179.38(14) . . . .
C4 C5 C6 N1 -0.8(2) . . . .
C2 N1 C6 O3 179.81(14) . . . .
C2 N1 C6 C5 0.0(2) . . . .
C5 C6 O3 Li 174.01(16) . . . 4_465
N1 C6 O3 Li -5.8(2) . . . 4_465
