#------------------------------------------------------------------------------
#$Date: 2016-02-20 17:35:30 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/61/2216108.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_2216108
loop_
_publ_author_name
'Churakov, Andrei V.'
'Howard, Judith A. K.'
_publ_section_title
;
 Thymine hydrogen peroxide 0.55-solvate 0.45-hydrate
;
_journal_coeditor_code           RZ2169
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4483
_journal_page_last               o4483
_journal_paper_doi               10.1107/S1600536807053585
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C5 H6 N2 O2 , 0.55H2 O2 , 0.45H2 O'
_chemical_formula_moiety         'C5 H6 N2 O2 , 0.55H2 O2 , 0.45H2 O'
_chemical_formula_sum            'C5 H8 N2 O3.55'
_chemical_formula_weight         152.93
_chemical_name_systematic
;
Thymine hydrogen peroxide 0.55-solvate 0.45-hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.078(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5047(16)
_cell_length_b                   19.194(5)
_cell_length_c                   5.6190(13)
_cell_measurement_reflns_used    1539
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.445
_cell_measurement_theta_min      3.334
_cell_volume                     658.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL (Bruker, 2003)'
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1K'
_diffrn_measurement_method       ω
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4556
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9869
_exptl_absorpt_correction_T_min  0.9741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             321.6
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1733
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0449
_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)+(0.0537P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                1174
_reflns_number_total             1733
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rz2169.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2216108
_cod_database_fobs_code          2216108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_disorder_assembly
_atom_site_disorder_group
N N1 0.5189(2) 0.43892(7) 0.7551(3) 0.0193(3) Uani d . 1 . .
N N2 0.1954(2) 0.43931(7) 0.4159(2) 0.0201(3) Uani d . 1 . .
O O3 0.22793(17) 0.50240(5) 0.77214(19) 0.0214(3) Uani d . 1 . .
O O4 0.81449(18) 0.37725(6) 0.7577(2) 0.0269(3) Uani d . 1 . .
C C1 0.3077(2) 0.46216(7) 0.6531(3) 0.0180(3) Uani d . 1 . .
C C2 0.2878(3) 0.39447(8) 0.2885(3) 0.0206(3) Uani d . 1 . .
C C3 0.4944(2) 0.37063(7) 0.3883(3) 0.0187(3) Uani d . 1 . .
C C4 0.6227(2) 0.39384(7) 0.6405(3) 0.0192(3) Uani d . 1 . .
C C5 0.5985(3) 0.32256(9) 0.2523(3) 0.0239(4) Uani d . 1 . .
O O1 0.0489(5) 0.26290(15) 0.7488(6) 0.0323(7) Uani d PD 0.55 A 1
O O2 0.2145(5) 0.29347(15) 0.6611(7) 0.0320(7) Uani d PD 0.55 A 1
H H1 -0.040(7) 0.302(2) 0.740(9) 0.057(11) Uiso d PD 0.55 B 1
H H2 0.183(8) 0.269(2) 0.503(8) 0.057(11) Uiso d PD 0.55 C 1
O O12 0.1421(8) 0.2877(2) 0.7417(7) 0.0324(8) Uani d PD 0.45 D 2
H H3 0.041(10) 0.320(2) 0.711(10) 0.049(13) Uiso d PD 0.45 E 2
H H4 0.124(11) 0.269(3) 0.592(10) 0.049(13) Uiso d PD 0.45 F 2
H H22 0.191(3) 0.3837(9) 0.119(3) 0.025(5) Uiso d . 1 . .
H H53 0.501(3) 0.3136(9) 0.082(4) 0.030(5) Uiso d . 1 . .
H H52 0.638(3) 0.2786(10) 0.342(4) 0.032(5) Uiso d . 1 . .
H H11 0.590(3) 0.4559(10) 0.893(4) 0.031(5) Uiso d . 1 . .
H H51 0.738(3) 0.3440(10) 0.241(3) 0.029(5) Uiso d . 1 . .
H H21 0.055(4) 0.4561(11) 0.337(4) 0.043(6) Uiso d . 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.0163(6) 0.0200(6) 0.0183(7) 0.0007(5) 0.0018(5) -0.0030(5)
N2 0.0142(6) 0.0223(6) 0.0207(7) 0.0020(5) 0.0020(5) -0.0018(5)
O3 0.0169(6) 0.0230(6) 0.0224(6) 0.0026(4) 0.0044(5) -0.0034(4)
O4 0.0182(6) 0.0316(6) 0.0263(6) 0.0081(5) 0.0016(5) -0.0019(5)
C1 0.0152(7) 0.0163(7) 0.0205(8) -0.0012(5) 0.0036(6) 0.0014(6)
C2 0.0204(8) 0.0218(7) 0.0190(8) -0.0010(6) 0.0059(6) -0.0007(6)
C3 0.0205(8) 0.0170(7) 0.0196(8) -0.0012(6) 0.0081(6) 0.0001(6)
C4 0.0188(7) 0.0171(7) 0.0223(8) 0.0018(6) 0.0079(6) 0.0034(6)
C5 0.0241(8) 0.0241(8) 0.0237(9) 0.0028(7) 0.0082(7) 0.0000(7)
O1 0.0287(15) 0.0302(15) 0.0441(17) 0.0045(12) 0.0201(14) 0.0113(12)
O2 0.0252(15) 0.0292(14) 0.0436(19) -0.0035(11) 0.0143(14) 0.0008(12)
O12 0.026(2) 0.037(2) 0.032(2) 0.0122(18) 0.0064(18) -0.0006(17)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 N1 C4 126.05(14)
C1 N1 H11 115.0(14)
C4 N1 H11 118.8(14)
C1 N2 C2 121.90(13)
C1 N2 H21 118.0(13)
C2 N2 H21 120.0(13)
O3 C1 N2 123.11(13)
O3 C1 N1 121.37(14)
N2 C1 N1 115.51(14)
C3 C2 N2 123.03(15)
C3 C2 H22 123.9(10)
N2 C2 H22 113.0(10)
C2 C3 C4 117.47(14)
C2 C3 C5 123.88(14)
C4 C3 C5 118.65(14)
O4 C4 N1 118.51(14)
O4 C4 C3 125.46(14)
N1 C4 C3 116.03(13)
C3 C5 H53 111.0(11)
C3 C5 H52 110.7(11)
H53 C5 H52 109.1(15)
C3 C5 H51 110.4(10)
H53 C5 H51 107.8(14)
H52 C5 H51 107.7(16)
O2 O1 H1 100(3)
O1 O2 H2 99(2)
H3 O12 H4 105(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.3689(19)
N1 C4 1.385(2)
N1 H11 0.82(2)
N2 C1 1.3544(19)
N2 C2 1.382(2)
N2 H21 0.93(2)
O3 C1 1.2453(18)
O4 C4 1.2361(18)
C2 C3 1.346(2)
C2 H22 0.968(18)
C3 C4 1.446(2)
C3 C5 1.500(2)
C5 H53 0.965(19)
C5 H52 0.972(19)
C5 H51 1.016(19)
O1 O2 1.453(4)
O1 H1 0.93(4)
O2 H2 0.97(4)
O12 H3 0.87(5)
O12 H4 0.89(5)
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
O1 H1 O4 1_455 0.93(4) 1.75(4) 2.683(3) 173(5)
O12 H3 O4 1_455 0.87(5) 1.93(5) 2.764(4) 160(5)
O2 H2 O1 4_565 0.97(4) 1.52(4) 2.446(5) 159(4)
O12 H4 O1 4_565 0.89(5) 1.92(5) 2.798(5) 172(6)
N1 H11 O3 3_667 0.82(2) 2.01(2) 2.8347(18) 178.1(18)
N2 H21 O3 3_566 0.93(2) 1.90(2) 2.8204(18) 170.3(18)
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
C2 N2 C1 O3 -179.79(14)
C2 N2 C1 N1 1.2(2)
C4 N1 C1 O3 179.41(14)
C4 N1 C1 N2 -1.5(2)
C1 N2 C2 C3 -0.4(2)
N2 C2 C3 C4 -0.1(2)
N2 C2 C3 C5 -179.33(14)
C1 N1 C4 O4 -179.59(14)
C1 N1 C4 C3 1.0(2)
C2 C3 C4 O4 -179.46(15)
C5 C3 C4 O4 -0.2(2)
C2 C3 C4 N1 -0.1(2)
C5 C3 C4 N1 179.10(14)
H1 O1 O2 H2 -113(4)
