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_7247823
_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 O18 P2, 4(H2 O), Co H12 O6, 3(O), C3 H7 N O'
_chemical_formula_sum            'C33 H63 Co2 N9 O32 P2'
_chemical_formula_weight         1277.72
_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                68.453(3)
_cell_angle_beta                 89.860(3)
_cell_angle_gamma                80.963(3)
_cell_formula_units_Z            1
_cell_length_a                   6.7824(6)
_cell_length_b                   13.8721(12)
_cell_length_c                   15.7504(14)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.203
_cell_measurement_theta_min      2.482
_cell_volume                     1358.8(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.959
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18386
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.359
_diffrn_reflns_theta_min         1.601
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0743 before and 0.0524 after correction.
The Ratio of minimum to maximum transmission is 0.7542.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.457
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         14757
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+1.1318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1780
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                10276
_reflns_number_total             14757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01056b2.cif
_cod_data_source_block           1_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7247822--7247826.cif.'
_cod_database_code               7247823
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(2)
 0.03(2)
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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 H3B-O13
 2 with sigma of 0.02
 H1B-O1
 0.86 with sigma of 0.02
 H3A_$1-O5
 1.8 with sigma of 0.02
 H3A-H28A
 2.12 with sigma of 0.02
 O3_$1-H3A_$1
 0.86 with sigma of 0.02
 O1-H1A
 0.86 with sigma of 0.02
 O3_$1-H3B_$1
 0.86 with sigma of 0.02
 H3A_$1-H1B
 2.12 with sigma of 0.02
 O5-H1B
 1.8 with sigma of 0.02
 O5-H28A_$1
 2.077 with sigma of 0.02
 O32-H19B
 1.95 with sigma of 0.02
 H1A-O13_$1
 1.6 with sigma of 0.02
 Co2-H21A \\sim Co2-H21B
 with sigma of 0.02
 Co2-H24A \\sim Co2-H24B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Free rotating group:
 O28(H28A,H28B), O21(H21A,H21B), O24(H24A,H24B), O25(H25C,H25D), O26(H26A,
 H26B), O27(H27A,H27B)
5.b Rotating group:
 O1(H1A,H1B), O3(H3A,H3B), O19(H19A,H19B), O20(H20A,H20B), O22(H22C,H22D),
 O23(H23A,H23B)
5.c Ternary CH refined with riding coordinates:
 C14(H14), C15(H15A), C17(H17), C23(H23), C24(H24), C26(H26)
5.d Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C22(H22A,H22B), C25(H25A,H25B)
5.e Aromatic/amide H refined with riding coordinates:
 N6(H6), N8(H8A), C1(H1), C2(H2), C4(H4), C5(H5), C6(H6A), C7(H7), C8(H8B),
 C10(H10), C11(H11), C12(H12), C20(H20), C21(H21), C27(H27), C28(H28), C33(H33)
5.f Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
5.g Idealised tetrahedral OH refined as rotating group:
 O8(H8), O15(H15)
;
_shelx_res_checksum              52059
_olex2_submission_special_instructions 'No special instructions were received'