Effect of substituents on the ability of nickel Schiff base complexes with four pendant groups to bind to G-quadruplexes.
Assadawi, Nawal; Ferderer, Myles; Kusi-Appauh, Nicholas; Yu, Haibo; Dillon, Carolyn T.; Sluyter, Ronald; Richardson, Christopher; Ralph, Stephen F.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12720–12739; doi:10.1039/d4dt00448e

data_7716650
_publ_section_title
;
 Effect of substituents on the ability of nickel Schiff base complexes
 with four pendant groups to bind to G-quadruplexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12720
_journal_page_last               12739
_journal_paper_doi               10.1039/d4dt00448e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C56 H74 N6 Ni O6, 0.205(H2 O)'
_chemical_formula_sum            'C56 H74.41 N6 Ni O6.2'
_chemical_formula_weight         989.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.678(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7829(3)
_cell_length_b                   21.9025(5)
_cell_length_c                   22.2389(5)
_cell_measurement_reflns_used    11105
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.3760
_cell_measurement_theta_min      2.0810
_cell_volume                     5177.5(2)
_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      149.99(10)
_diffrn_detector                 'HyPix Bantam HPC3000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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     59.00  91.00   0.50   25.00    --   20.00  54.00   0.00   64
  2  \w    -48.00 110.00   0.50   25.00    --   20.00  54.00 120.00  316
  3  \w    -69.00 106.50   0.50   25.00    --   20.00  54.00-150.00  351
  4  \w    -53.00 -18.00   0.50   25.00    --   20.00  54.00-180.00   70
  5  \w     -9.00  33.00   0.50   25.00    --   20.00  54.00-180.00   84
  6  \w     46.00  83.50   0.50   25.00    --   20.00  54.00-180.00   75
;
_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      0.0471731000
_diffrn_orient_matrix_UB_12      -0.0183467000
_diffrn_orient_matrix_UB_13      0.0173492000
_diffrn_orient_matrix_UB_21      -0.0052586000
_diffrn_orient_matrix_UB_22      -0.0213014000
_diffrn_orient_matrix_UB_23      -0.0243413000
_diffrn_orient_matrix_UB_31      0.0469265000
_diffrn_orient_matrix_UB_32      0.0160676000
_diffrn_orient_matrix_UB_33      -0.0123868000
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39931
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74131
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             2120
_exptl_crystal_recrystallization_method
'Slow evaporation DCM/petroleum spirit (1:3)'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         12745
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0745P)^2^+3.5286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8427
_reflns_number_total             12745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00448e27.cif
_cod_data_source_block           exp_84ni20
_cod_depositor_comments
'Adding full bibliography for 7716650--7716651.cif.'
_cod_original_cell_volume        5177.4(2)
_cod_original_formula_sum        'C56 H74.41 N6 Ni O6.20'
_cod_database_code               7716650
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C56 H74.5 N6 Ni O6.25'
_chemical_oxdiff_usercomment     'Ni20 from Nawal'
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N23A-C23A \\sim N1-C23A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim N1 \\sim C1F
\\sim C1E \\sim C1D \\sim C1C \\sim C1B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O1W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=Sof(N1)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1E)=
 Sof(H1EA)=Sof(H1EB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(N23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=
 Sof(H28A)=Sof(H28B)=Sof(H23C)=Sof(H23D)=FVAR(1)
 Fixed X: O1W(1.15277) H1WA(1.0946) H1WB(1.13385)
 Fixed Y: O1W(0.18079) H1WA(0.15751) H1WB(0.19295)
 Fixed Z: O1W(0.62665) H1WA(0.60867) H1WB(0.66046)
5.a Free rotating group:
 N23A(C24A,C25A,C26A,C27A,C28A), N1(C1F,C1E,C1D,C1C,C1B)
5.b Ternary CH refined with riding coordinates:
 C7(H7), C7A(H7A)
5.c Secondary CH2 refined with riding coordinates:
 C24A(H24A,H24B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,H27B), C28A(H28A,
 H28B), C15(H15A,H15B), C15A(H15C,H15D), C16(H16A,H16B), C16A(H16C,H16D),
 C17(H17A,H17B), C17A(H17C,H17D), C18(H18A,H18B), C18A(H18C,H18D), C19(H19A,
 H19B), C19A(H19C,H19D), C20(H20A,H20B), C20A(H20C,H20D), C21(H21A,H21B),
 C21A(H21C,H21D), C22(H22A,H22B), C22A(H22C,H22D), C23(H23A,H23B), C24(H24C,
 H24D), C25(H25C,H25D), C26(H26C,H26D), C27(H27C,H27D), C28(H28C,H28D),
 C1F(H1FA,H1FB), C1E(H1EA,H1EB), C1D(H1DA,H1DB), C1C(H1CA,H1CB), C1B(H1BA,H1BB),
  C23A(H23C,H23D), C23A(H23E,H23F)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3), C3A(H3A), C4(H4), C4A(H4A),
 C5(H5), C5A(H5A), C8(H8), C8A(H8A), C11(H11), C11A(H11A), C13(H13), C13A(H13A)
;
_shelx_res_checksum              22061
_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 1.153
_oxdiff_exptl_absorpt_empirical_full_min 0.855