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_7716651
_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         'C41 H60 N6 Ni O10, 6(H2 O), 0.15(O)'
_chemical_formula_sum            'C41 H72 N6 Ni O16.15'
_chemical_formula_weight         966.15
_chemical_name_systematic
N,N-Bis-(4,6-((1-(2-ethyl)morpholine)oxy)salicylidine)-1,2-propylenediaminenickel(II)
_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             2024-01-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-22 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                78.2060(10)
_cell_angle_beta                 83.1790(10)
_cell_angle_gamma                89.109(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7651(2)
_cell_length_b                   14.6637(3)
_cell_length_c                   16.8916(3)
_cell_measurement_reflns_used    34096
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      30.5660
_cell_measurement_theta_min      2.1500
_cell_volume                     2350.83(8)
_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      150.01(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_measured_fraction_theta_full 0.993
_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    -74.00 110.00   0.50   15.00    --   20.00  54.00  94.57  368
  2  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00-147.64  368
  3  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 -16.09  368
  4  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 -16.09  368
  5  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 -54.22  368
  6  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 178.63  368
  7  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 178.63  368
  8  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00   0.00  368
  9  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00  79.89  368
 10  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 120.00  368
 11  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 150.00  368
 12  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00 -97.88  368
 13  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00-124.10  368
 14  \w    -74.00  76.00   0.50   15.00    --   20.00  54.00  30.00  300
 15  \w    -74.00 110.00   0.50   15.00    --   20.00  54.00  40.56  368
;
_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      -0.0298337000
_diffrn_orient_matrix_UB_12      -0.0317006000
_diffrn_orient_matrix_UB_13      -0.0197603000
_diffrn_orient_matrix_UB_21      0.0248735000
_diffrn_orient_matrix_UB_22      0.0277225000
_diffrn_orient_matrix_UB_23      -0.0384148000
_diffrn_orient_matrix_UB_31      0.0619933000
_diffrn_orient_matrix_UB_32      -0.0258554000
_diffrn_orient_matrix_UB_33      -0.0001168000
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            104375
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89664
_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    1.365
_exptl_crystal_description       needle
_exptl_crystal_F_000             1034
_exptl_crystal_recrystallization_method 'dichloromethane / Pet. Spirit'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         12431
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0603P)^2^+0.9798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10597
_reflns_number_total             12431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00448e27.cif
_cod_data_source_block           exp_219_na
_cod_depositor_comments
'Adding full bibliography for 7716650--7716651.cif.'
_cod_database_code               7716651
_chemical_oxdiff_formula         'C41 H60 N6 Ni O10'
_chemical_oxdiff_usercomment     Ni38
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.727
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N2-C17B \\sim N2-C17 \\sim N1-C2B \\sim N1-C2
 with sigma of 0.02
 C2B-C17B \\sim C2-C17
 with sigma of 0.02
 C37-N7 \\sim C37-N7A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C40A) = Uanis(C40B)
4. Rigid body (RIGU) restrains
 N7, O11, C38A, C39A, C40A, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7A, O11A, C38B, C39B, C40B, C41B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2B)=Sof(H2BA)=Sof(C17B)=Sof(H17A)=
 Sof(H17B)=1-FVAR(1)
 Sof(C1Z)=Sof(H1ZA)=Sof(H1ZB)=Sof(H1ZC)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C17)=
 Sof(H17)=FVAR(1)
 Sof(N7A)=Sof(O11A)=Sof(C38B)=Sof(H38A)=Sof(H38B)=Sof(C39B)=Sof(H39A)=
 Sof(H39B)=Sof(C40B)=Sof(H40A)=Sof(H40B)=Sof(C41B)=Sof(H41A)=Sof(H41B)=
 Sof(H37C)=Sof(H37D)=1-FVAR(2)
 Sof(N7)=Sof(O11)=Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=
 Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41C)=
 Sof(H41D)=FVAR(2)
 Fixed Sof: O7W(0.15)
6.a Free rotating group:
 N7(O11), N7A(O11A,C38B,C39B,C40B,C41B), O1W(H1WA,H1WB), O2W(H2WA,H2WB),
 O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB)
6.b Ternary CH refined with riding coordinates:
 C2B(H2BA), C17(H17)
6.c Secondary CH2 refined with riding coordinates:
 C38B(H38A,H38B), C39B(H39A,H39B), C40B(H40A,H40B), C41B(H41A,H41B), C2(H2A,
 H2B), C17B(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C37(H37C,H37D), C39A(H39C,
 H39D), C40A(H40C,H40D), C41A(H41C,H41D)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C11(H11), C13(H13), C16(H16)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1Z(H1ZA,H1ZB,H1ZC)
;
_shelx_res_checksum              71085
_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 1.099
_oxdiff_exptl_absorpt_empirical_full_min 0.942