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_7247825
_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
'C20 H24 Co N8 O4, C29 H33 Co N10 O11 P, C9 H11 N2 O8 P, 7(H2 O)'
_chemical_formula_sum            'C58 H82 Co2 N20 O30 P2'
_chemical_formula_weight         1719.23
_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'
_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                90
_cell_angle_beta                 106.376(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.700(2)
_cell_length_b                   31.930(6)
_cell_length_c                   11.774(2)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.288
_cell_measurement_theta_min      2.205
_cell_volume                     4220.1(13)
_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_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41264
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.331
_diffrn_reflns_theta_min         1.803
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1598 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.8639.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.082(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         15105
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+2.0978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                12944
_reflns_number_total             15105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01056b2.cif
_cod_data_source_block           3_a
_cod_depositor_comments
'Adding full bibliography for 7247822--7247826.cif.'
_cod_database_code               7247825
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.918(19)
 0.082(19)
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
3. Restrained distances
 H3a-H35a
 2.12 with sigma of 0.02
 O3-H3b
 0.85 with sigma of 0.02
 O16-H28a
 1.962 with sigma of 0.02
 O9-H25b
 1.916 with sigma of 0.02
 N5-H26a
 2.01 with sigma of 0.02
 H24c-H25b
 2.12 with sigma of 0.02
 H3b-O3
 0.85 with sigma of 0.02
 H8a-H26b_$5
 2.12 with sigma of 0.02
 H27a-O28
 1.938 with sigma of 0.02
 H3b_$2-H27a
 2.12 with sigma of 0.02
 O2-H33a
 2.05 with sigma of 0.02
 H33b-N7_$5
 2.05 with sigma of 0.02
 H24d-O33
 2.07 with sigma of 0.02
 H6b_$9-H33a
 2.12 with sigma of 0.02
 H33b-H24d
 2.12 with sigma of 0.02
 H33a-H24d
 2.09 with sigma of 0.02
 H24d-H33a
 2.12 with sigma of 0.02
 Co2-H7a \\sim Co2-H7b
 with sigma of 0.02
4. Restrained planarity
 N18, C29, N17, C26, C27, C28
 with sigma of 0.1
 C57, C56, C55, N20, C58, N19
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6.a Free rotating group:
 O7(H7a,H7b), O24(H24c,H24d), O25(H25a,H25b), O26(H26a,H26b), O27(H27a,H27b),
 O28(H28a,H28b), O33(H33a,H33b), O35(H35a,H35b)
6.b Rotating group:
 O1(H1a,H1b), O2(H2a,H2b), O3(H3a,H3b), O4(H4a,H4b), O6(H6a,H6b), O8(H8a,H8b)
6.c Ternary CH refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C51(H51), C52(H52), C54(H54)
6.d Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C24(H24a,H24b), C50(H50a,H50b), C53(H53a,H53b)
6.e Aromatic/amide H refined with riding coordinates:
 N18(H18), C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10),
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C26(H26), C27(H27), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C46(H46), C48(H48), C49(H49), N20(H20a), C56(H56), C57(H57)
6.f Idealised tetrahedral OH refined as rotating group:
 O13(H13), O21(H21)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7126
_shelx_fab_checksum              78417
_olex2_submission_special_instructions 'No special instructions were received'