G-quadruplex DNA binding properties of novel nickel Schiff base complexes with four pendant groups
Ralph, Stephen; Assadawi, Nawal; Richardson, Christopher; Dalton Transactions  (2023) –; doi:10.1039/D3DT02040A

data_7713750
_publ_section_title
;
 G-quadruplex DNA binding properties of novel nickel Schiff base complexes
 with four pendant groups
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02040A
_journal_year                    2023
_chemical_formula_moiety         'C44 H58 N6 Ni O10, 1.6(H2 O)'
_chemical_formula_sum            'C44 H61.2 N6 Ni O11.6'
_chemical_formula_weight         918.50
_chemical_name_common            'compound (9) in manuscript'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-04 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.209(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.6127(5)
_cell_length_b                   15.8401(3)
_cell_length_c                   9.8494(2)
_cell_measurement_reflns_used    21460
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.3850
_cell_measurement_theta_min      2.3730
_cell_volume                     4748.04(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -74.00 110.00   0.50   20.00    --   20.00  54.00 120.00  368
  2  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00-120.00  368
  3  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00 -60.00  368
  4  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00-180.00  368
  5  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00  30.00  368
  6  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00  90.00  368
  7  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00-150.00  368
  8  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00 -30.00  368
  9  \w    -74.00 110.00   0.50   20.00    --   20.00  54.00  60.00  368
 10  \w    -74.00 -41.50   0.50   20.00    --   20.00  54.00 -90.00   65
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0230724000
_diffrn_orient_matrix_UB_12      0.0061373000
_diffrn_orient_matrix_UB_13      -0.0093862000
_diffrn_orient_matrix_UB_21      -0.0014339000
_diffrn_orient_matrix_UB_22      -0.0128468000
_diffrn_orient_matrix_UB_23      0.0683758000
_diffrn_orient_matrix_UB_31      0.0028975000
_diffrn_orient_matrix_UB_32      0.0424664000
_diffrn_orient_matrix_UB_33      0.0220346000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            64511
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.384
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_recrystallization_method 'Chloroform / Pet. spirit'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0387P)^2^+3.0887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5665
_reflns_number_total             6653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02040a3.cif
_cod_data_source_block           exp_218_na
_cod_original_formula_sum        'C44 H61.20 N6 Ni O11.60'
_cod_database_code               7713750
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C44H48N6Ni1O10
_chemical_oxdiff_usercomment     Ni34
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O1W(0.8) H1WA(0.8) H1WB(0.8)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9)
;
_shelx_res_checksum              40226
_shelx_fab_checksum              69356
_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 1.105
_oxdiff_exptl_absorpt_empirical_full_min 0.927