A new class of quadruplex DNA-binding nickel Schiff base complexes.
Pham, Son Q. T.; Assadawi, Nawal; Wells, Jadon; Sophocleous, Reece A.; Davis, Kimberley J.; Yu, Haibo; Sluyter, Ronald; Dillon, Carolyn T.; Kelso, Celine; Beck, Jennifer L.; Willis, Anthony C.; Richardson, Christopher; Ralph, Stephen F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4843–4860; doi:10.1039/d0dt00319k

data_7703749
_publ_section_title
;
 A new class of quadruplex DNA-binding nickel Schiff base complexes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4843
_journal_page_last               4860
_journal_paper_doi               10.1039/d0dt00319k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C28 H22 N2 Ni O4, 2(C2 D6 O S)'
_chemical_formula_sum            'C32 H22 D12 N2 Ni O6 S2'
_chemical_formula_weight         677.51
_chemical_name_systematic
N,N'-Bis-(4-(hydroxybenzophenylidene))ethylenediaminenickel(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-11 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1632(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4100(2)
_cell_length_b                   9.8299(2)
_cell_length_c                   21.9572(5)
_cell_measurement_reflns_used    20757
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5510
_cell_measurement_theta_min      1.8050
_cell_volume                     3486.31(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  79.50   0.50   10.00    --   20.00  54.00 135.93  307
  2  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00   0.00  368
  3  \w    -34.50 110.00   0.50   10.00    --   20.00  54.00 -60.63  289
  4  \w    -34.50 110.00   0.50   10.00    --   20.00  54.00 -60.63  289
  5  \w    -34.50 110.00   0.50   10.00    --   20.00  54.00-120.00  289
  6  \w    -34.50 110.00   0.50   10.00    --   20.00  54.00-120.00  289
  7  \w    -34.50 110.00   0.50   10.00    --   20.00  54.00 -80.64  289
  8  \w    -74.00  23.00   0.50   10.00    --   20.00  54.00  60.00  194
;
_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      -0.0071937000
_diffrn_orient_matrix_UB_12      -0.0697101000
_diffrn_orient_matrix_UB_13      -0.0072592000
_diffrn_orient_matrix_UB_21      0.0384213000
_diffrn_orient_matrix_UB_22      -0.0035465000
_diffrn_orient_matrix_UB_23      -0.0105614000
_diffrn_orient_matrix_UB_31      0.0200961000
_diffrn_orient_matrix_UB_32      -0.0180594000
_diffrn_orient_matrix_UB_33      0.0302055000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64412
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.702
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_recrystallization_method 'From a solution of d6-DMSO'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0433P)^2^+2.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7826
_reflns_number_total             8956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00319k2.cif
_cod_data_source_block           cmpd3_exp_131_tsb
_cod_depositor_comments
'Adding full bibliography for 7703742--7703750.cif.'
_cod_original_cell_volume        3486.30(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7703749
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C32 H22 D12 N2 Ni O6 S2'
_chemical_oxdiff_usercomment     'TSB 3_P from DMSO'
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.715
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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 C(H,H,H) groups, All O(H) groups
2. Shared sites
{C1AA, C501}
3. Restrained distances
 S400-O400 \\sim S500-O500
 with sigma of 0.01
 S400-C400 \\sim S500-C401
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1AA) = Uanis(C501)
Uanis(C400) = Uanis(C401)
5. Others
 Sof(S500)=Sof(O500)=Sof(C501)=Sof(D50A)=Sof(D50B)=Sof(D50C)=Sof(C401)=
 Sof(D40D)=Sof(D40E)=Sof(D40F)=1-FVAR(1)
 Sof(S400)=Sof(O400)=Sof(C400)=Sof(D40A)=Sof(D40B)=Sof(D40C)=Sof(C1AA)=
 Sof(D1AA)=Sof(D1AB)=Sof(D1AC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1P(H1PA,H1PB)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C5P(H5P), C6(H6), C6P(H6P), C7(H7), C7P(H7P), C8(H8), C8P(H8P),
 C9(H9), C9P(H9P), C11(H11), C11P(H11P), C12(H12), C12P(H12P), C14(H14),
 C14P(H14P)
6.c Idealised Me refined as rotating group:
 C400(D40A,D40B,D40C), C1AA(D1AA,D1AB,D1AC), C501(D50A,D50B,D50C), C100(D10A,
 D10B,D10C), C101(D10D,D10E,D10F), C401(D40D,D40E,D40F)
6.d Idealised tetrahedral OH refined as rotating group:
 O17(H17), O17P(H17P)
;
_shelx_res_checksum              73463
_shelx_fab_checksum              9024
_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_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 0.903