Azulene tethered N-aryl nucleobases: synthesis, morphology and biochemical evaluations
Meher, Sagarika; Sharma, Nagendra K.; New Journal of Chemistry 47 (2023) 5593–5597; doi:10.1039/D2NJ06272K

data_7062336
_publ_section_title
;
 Azulene tethered N-aryl nucleobases: synthesis, morphology and
 biochemical evaluations
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5593
_journal_page_last               5597
_journal_paper_doi               10.1039/D2NJ06272K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C2 H6 O S, C21 H21 N3 O6'
_chemical_formula_sum            'C23 H27 N3 O7 S'
_chemical_formula_weight         489.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-05
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                108.665(1)
_cell_angle_beta                 99.074(1)
_cell_angle_gamma                101.146(1)
_cell_formula_units_Z            2
_cell_length_a                   8.7670(1)
_cell_length_b                   10.6359(2)
_cell_length_c                   14.1150(2)
_cell_measurement_reflns_used    13338
_cell_measurement_temperature    256(40)
_cell_measurement_theta_max      75.1510
_cell_measurement_theta_min      3.4340
_cell_volume                     1188.79(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      256(40)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9771
_diffrn_measured_fraction_theta_max 0.9771
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -79.00   9.00   0.50    1.24    --  -38.50 107.00-126.00  176
  2  \w     13.00  90.00   0.50    1.24    --   49.56-107.00 135.00  154
  3  \w     34.00 108.00   0.50    4.82    --  102.63-107.00 135.00  148
  4  \w    104.00 171.00   0.50    4.82    --  102.63 107.00-126.00  134
  5  \w    -50.00  24.00   0.50    1.24    --  -38.50  57.00  60.00  148
  6  \w    -42.00  28.00   0.50    1.24    --  -38.50  38.00  60.00  140
  7  \w   -101.00 -28.00   0.50    1.24    --  -38.50 -55.00 101.03  146
  8  \w    -42.00  28.00   0.50    1.24    --  -38.50  38.00 150.00  140
  9  \w    -13.00  61.00   0.50    1.24    --   49.56 -57.00-150.00  148
 10  \w     38.00 113.00   0.50    1.24    --   49.56  57.00 -90.00  150
 11  \w     38.00 113.00   0.50    1.24    --   49.56  57.00   0.00  150
 12  \w     38.00 107.00   0.50    4.82    --  102.63 -45.00  30.00  138
 13  \w     40.00 116.00   0.50    4.82    --  102.63 -61.00 150.00  152
 14  \w     38.00 126.00   0.50    4.82    --  102.63 -77.00 -30.00  176
 15  \w     34.00 107.00   0.50    4.82    --  102.63 -94.00  90.00  146
 16  \w     99.00 171.00   0.50    4.82    --  102.63  30.00-120.00  144
 17  \w     34.00 107.00   0.50    4.82    --  102.63 -94.00 -30.00  146
 18  \w     35.00 106.00   0.50    4.82    --  102.63 -30.00 -60.00  142
 19  \w     98.00 167.00   0.50    4.82    --  102.63  45.00 -60.00  138
 20  \w     38.00 126.00   0.50    4.82    --  102.63 -77.00  60.00  176
 21  \w     38.00 126.00   0.50    4.82    --  102.63 -77.00 120.00  176
 22  \w     38.00 107.00   0.50    4.82    --  102.63 -45.00 120.00  138
 23  \w    103.00 167.00   0.50    4.82    --  102.63  77.00 -60.00  128
 24  \w     34.00 107.00   0.50    4.82    --  102.63 -94.00 -90.00  146
 25  \w     90.00 165.00   0.50    4.82    --  102.63  61.00   0.00  150
 26  \w     34.00 107.00   0.50    4.82    --  102.63 -94.00-150.00  146
 27  \w    103.00 167.00   0.50    4.82    --  102.63  77.00-150.00  128
 28  \w     98.00 167.00   0.50    4.82    --  102.63  45.00 -90.00  138
 29  \w     40.00 116.00   0.50    4.82    --  102.63 -61.00-150.00  152
 30  \w     95.00 171.00   0.50    4.82    --  102.63  15.00-180.00  152
 31  \w     38.00 113.00   0.50    1.24    --   49.56  57.00  90.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0021219000
_diffrn_orient_matrix_UB_12      -0.0398423000
_diffrn_orient_matrix_UB_13      -0.1146728000
_diffrn_orient_matrix_UB_21      -0.0150103000
_diffrn_orient_matrix_UB_22      -0.1503823000
_diffrn_orient_matrix_UB_23      -0.0091463000
_diffrn_orient_matrix_UB_31      -0.1836938000
_diffrn_orient_matrix_UB_32      -0.0295782000
_diffrn_orient_matrix_UB_33      -0.0286796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18490
_diffrn_reflns_theta_full        75.4595
_diffrn_reflns_theta_max         75.46
_diffrn_reflns_theta_min         3.40
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3675
_exptl_crystal_description       needle
_exptl_crystal_F_000             518.4068
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.4984
_refine_diff_density_min         -0.3743
_refine_diff_density_rms         0.0456
_refine_ls_d_res_high            0.7964
_refine_ls_d_res_low             12.9942
_refine_ls_goodness_of_fit_ref   1.0268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0268
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.2140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4444
_reflns_number_total             4820
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj06272k2.cif
_cod_data_source_block           SNM-TAZ
_cod_depositor_comments
'Adding full bibliography for 7062335--7062336.cif.'
_cod_database_code               7062336
_chemical_oxdiff_formula         'C H N O'
_diffrn_oxdiff_digest_frames
;
01048985ad56b663ae3b4c3da7a327cd0000030b685
;
_diffrn_oxdiff_digest_hkl
;
015c519f591701a66efe5164f4d53d794ae6f2
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C17(H17a,H17b)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C8(H8), C5(H5), C11(H11), C12(H12)
2.c X=CH2 refined with riding coordinates:
 N3(H3a,H3b)
2.d Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C21(H21a,H21b,H21c), C18(H18a,H18b,H18c), C00V(H00a,H00b,
 H00c), C00Y(H00d,H00e,H00f)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.026
_oxdiff_exptl_absorpt_empirical_full_min 0.680