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_7713749
_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         'C48 H67 N6 Ni O6, H2 O, 0.5[CH2Cl2]'
_chemical_formula_sum            'C48.5 H69 Cl N6 Ni O7'
_chemical_formula_weight         942.25
_chemical_name_common            'compound (5) in manuscript'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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             2023-01-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-23 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                101.829(6)
_cell_angle_beta                 96.030(5)
_cell_angle_gamma                97.639(6)
_cell_formula_units_Z            2
_cell_length_a                   11.7197(8)
_cell_length_b                   12.5847(8)
_cell_length_c                   16.6523(10)
_cell_measurement_reflns_used    13180
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.7620
_cell_measurement_theta_min      2.0000
_cell_volume                     2360.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_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    -11.00  53.50   0.50   20.00    --   20.00  54.00   0.00  129
  2  \w     83.00 109.00   0.50   20.00    --   20.00  54.00 -30.00   52
  3  \w     77.00 103.00   0.50   20.00    --   20.00  54.00-180.00   52
  4  \w     41.00  67.00   0.50   20.00    --   20.00  54.00-120.00   52
  5  \w     18.00  43.00   0.50   20.00    --   20.00  54.00 -30.00   50
  6  \w     27.00  79.50   0.50   20.00    --   20.00  54.00  30.00  105
  7  \w     55.00  81.00   0.50   20.00    --   20.00  54.00 150.00   52
  8  \w     -3.00  42.50   0.50   20.00    --   20.00  54.00  90.00   91
  9  \w    -23.00  11.00   0.50   20.00    --   20.00  54.00 -60.00   68
 10  \w    -16.00  10.00   0.50   20.00    --   20.00  54.00-180.00   52
 11  \w    -64.00  -3.50   0.50   20.00    --   20.00  54.00  30.00  121
 12  \w    -72.00 -12.50   0.50   20.00    --   20.00  54.00  90.00  119
 13  \w    -70.00   8.50   0.50   20.00    --   20.00  54.00 -30.00  157
 14  \w    -73.00 -20.50   0.50   20.00    --   20.00  54.00-120.00  105
 15  \w    -73.00 -33.50   0.50   20.00    --   20.00  54.00 -60.00   79
 16  \w    -74.00  55.50   0.50   20.00    --   20.00  54.00-150.00  259
 17  \w    -70.00  75.50   0.50   20.00    --   20.00  54.00 120.00  291
 18  \w    -72.00 108.50   0.50   20.00    --   20.00  54.00  60.00  361
 19  \w    -66.00 -33.00   0.50   20.00    --   20.00  54.00 150.00   66
 20  \w    -63.00  65.50   0.50   20.00    --   20.00  54.00 165.66  257
 21  \w    -66.00  55.50   0.50   20.00    --   20.00  54.00 -90.00  243
 22  \w    -68.00 -41.00   0.50   20.00    --   20.00  54.00   0.00   54
 23  \w    -59.00 -32.00   0.50   20.00    --   20.00  54.00-180.00   54
;
_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      0.0073092000
_diffrn_orient_matrix_UB_12      -0.0389433000
_diffrn_orient_matrix_UB_13      0.0247002000
_diffrn_orient_matrix_UB_21      0.0611993000
_diffrn_orient_matrix_UB_22      0.0145372000
_diffrn_orient_matrix_UB_23      0.0035827000
_diffrn_orient_matrix_UB_31      -0.0008436000
_diffrn_orient_matrix_UB_32      0.0409116000
_diffrn_orient_matrix_UB_33      0.0361503000
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55431
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         1.859
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plate
_exptl_crystal_F_000             1006
_exptl_crystal_recrystallization_method dichloromethane
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         11983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0449P)^2^+0.5545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8992
_reflns_number_total             11983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02040a3.cif
_cod_data_source_block           exp_44
_cod_original_formula_sum        'C48.50 H69 Cl N6 Ni O7'
_cod_database_code               7713749
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C48 H69 N6 Ni O8'
_chemical_oxdiff_usercomment     'Nawal Assadouwi 150 K'
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.776
_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. Uiso/Uaniso restraints and constraints
Uanis(C48) = Uanis(C52A)
Uanis(C52) = Uanis(C48A)
Uanis(C49) = Uanis(C51A)
Uanis(C50) = Uanis(C50A)
Uanis(C51) = Uanis(C49A)
3. Others
 Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=
 Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=
 Sof(H52B)=1-FVAR(1)
 Sof(C48)=Sof(H48C)=Sof(H48D)=Sof(C49)=Sof(H49C)=Sof(H49D)=Sof(C50)=Sof(H50C)=
 Sof(H50D)=Sof(C51)=Sof(H51C)=Sof(H51D)=Sof(C52)=Sof(H52C)=Sof(H52D)=FVAR(1)
 Fixed X: O1W(0.45516) H1WA(0.47536) H1WB(0.384589)
 Fixed Y: O1W(0.76146) H1WA(0.756129) H1WB(0.77199)
 Fixed Z: O1W(0.7143) H1WA(0.66604) H1WB(0.71272)
4.a Free rotating group:
 N47(C48A,C49A,C50A,C51A,C52A)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C45(H45A,H45B), C46(H46A,H46B), C48A(H48A,H48B), C49A(H49A,H49B), C50A(H50A,
 H50B), C51A(H51A,H51B), C52A(H52A,H52B), C48(H48C,H48D), C49(H49C,H49D),
 C50(H50C,H50D), C51(H51C,H51D), C52(H52C,H52D), C54(H54A,H54B), C55(H55A,H55B),
  C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C21(H21), C23(H23)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 41 electrons were 
found in a volume of 156\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 0.5[CH2Cl2] per Asymmetric Unit 
which account for 42 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2319
_shelx_fab_checksum              92617
_olex2_exptl_crystal_mounting_method 'MiTeGen mount + Paratone-N'
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.879