Complex self-assembly of pyrimido[4,5-d]pyrimidine nucleoside supramolecular structures.
Zhao, Hang; Guo, Xiurong; He, Shiliang; Zeng, Xin; Zhou, Xinglong; Zhang, Chaoliang; Hu, Jing; Wu, Xiaohua; Xing, Zhihua; Chu, Liangyin; He, Yang; Chen, Qianming; Nature communications 5 (2014) 3108–; doi:10.1038/ncomms4108

data_1513798
_publ_section_title
;
 Complex self-assembly of pyrimido[4,5-d]pyrimidine nucleoside
 supramolecular structures.
;
_journal_name_full               'Nature communications'
_journal_page_first              3108
_journal_paper_doi               10.1038/ncomms4108
_journal_volume                  5
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C11 H13 N5 O6, H2 O'
_chemical_formula_sum            'C11 H15 N5 O7'
_chemical_formula_weight         329.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.291(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6548(14)
_cell_length_b                   27.587(7)
_cell_length_c                   8.526(2)
_cell_measurement_reflns_used    4743
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.40
_cell_volume                     1324.4(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2012 (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9399
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.476
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 2052 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.1278P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.915
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                4694
_reflns_number_total             5127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms4108-s2.cif
_cod_data_source_block           luo21
_cod_database_code               1513798
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O15-H15B
 0.98 with sigma of 0.001
 O16-H16A
 0.98 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uiso(H8D) = Uiso(H7D)
Uiso(H16B) = Uiso(H16A)
4.a Ternary CH refined with riding coordinates:
 C1C(H1C), C1D(H1D), C2C(H2C), C2D(H2D), C3C(H3C), C3D(H3D), C4C(H4C), C4D(H4D)
4.b Secondary CH2 refined with riding coordinates:
 C5C(H5CA,H5CB), C5D(H5DA,H5DB)
4.c Aromatic/amide H refined with riding coordinates:
 N3A(H3A), N3B(H3B), C7A(H7A), C7B(H7B)
4.d X=CH2 refined with riding coordinates:
 N11A(H11A,H11B), N11B(H11C,H11D)
4.e Idealised tetrahedral OH refined as rotating group:
 O7C(H7C), O8C(H8C), O8D(H8D), O9D(H9D)
;
_shelx_res_checksum              64674
_shelx_hkl_checksum              1739