Mimic uracil–uracil base pairing: self-assembly and single crystal structure
Zhang, Menglei; Li, Zhongkui; Zhu, Yanhong; Yan, Li; Zhong, Xue; Zhang, Yijie; Li, Ziyao; Bai, Yixiang; Li, Hui; CrystEngComm 26 (2024) 261–267; doi:10.1039/D3CE01056B

data_7247824
_publ_section_title
;
 Mimic uracil--uracil base pairing: self-assembly and single crystal
 structure
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              261
_journal_page_last               267
_journal_paper_doi               10.1039/D3CE01056B
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H36 Co N8 O20 P2, Co H12 O6, H2 O'
_chemical_formula_sum            'C30 H50 Co2 N8 O27 P2'
_chemical_formula_weight         1134.58
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-16 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                115.138(4)
_cell_angle_beta                 93.184(4)
_cell_angle_gamma                96.631(5)
_cell_formula_units_Z            1
_cell_length_a                   6.9314(10)
_cell_length_b                   13.624(2)
_cell_length_c                   15.739(2)
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.63
_cell_volume                     1327.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.1724
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9661
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.671
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.6681.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         8522
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0821
_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/[\s^2^(Fo^2^)+(0.0816P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.853
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                5080
_reflns_number_total             8522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01056b2.cif
_cod_data_source_block           1_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7247822--7247826.cif.'
_cod_original_cell_volume        1327.5(3)
_cod_database_code               7247824
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(5)
 0.11(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H,H) groups
3. Restrained distances
 H4b-O4
 0.85 with sigma of 0.02
 O2-H2b
 0.85 with sigma of 0.02
 H24b-O24
 0.85 with sigma of 0.02
 O24-H24a
 0.85 with sigma of 0.02
 O27-H27a
 0.85 with sigma of 0.02
 O27-H27b
 0.85 with sigma of 0.02
 O19-C25
 1.4 with sigma of 0.02
 H2b-H4b_$4
 2.12 with sigma of 0.02
 H2a-O13_$4
 1.9 with sigma of 0.02
 O13-H4b
 2.08 with sigma of 0.02
 O5_$1-H4a
 2.07 with sigma of 0.02
 O5-H2b
 1.9 with sigma of 0.02
 H4b-O13
 1.9 with sigma of 0.02
 H4a-O5_$1
 1.9 with sigma of 0.02
 O1-H27a
 1.85 with sigma of 0.02
 H9-H19_$7
 2.12 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3.8A
Uanis(C12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(Co2)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C19) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(O20) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O18) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(O19)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed X: Co2(0.08473)
 Fixed Y: Co2(-0.02316)
 Fixed Z: Co1(0.65621)
6.a Free rotating group:
 O27(H24a,H24b,H27a,H27b)
6.b Rotating group:
 O2(H2a,H2b), O4(H4a,H4b), O21(H21a,H21b), O22(H22c,H22d), O23(H23a,H23b),
 O25(H25a,H25b), O26(H26a,H26b)
6.c Ternary CH refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C23(H23), C24(H24), C25(H25), C26(H26)
6.d Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C22(H22a,H22b)
6.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C1(H1), C6(H6), C7(H7), C8(H8), C12(H12), C11(H11),
 C9(H9a), N6(H6a), C19(H19a), C18(H18), C28(H28), C27(H27), N8(H8a)
6.f Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,N1,C1), C8(N4,C12,C11,C10,C9), N6(C20,C19,C18,N5,C21), C28(C27,N7,
 C30,N8,C29)
6.g Tetrahedral OH refined with riding coordinates:
 O19(H19), O20(H20)
6.h Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22416
_shelx_fab_checksum              71964
_olex2_submission_special_instructions 'No special instructions were received'