The effect of isomerism and other structural variations on the G-quadruplex DNA-binding properties of some nickel Schiff base complexes.
Pham, Son Q. T.; Richardson, Christopher; Kelso, Celine; Willis, Anthony C.; Ralph, Stephen F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10360–10379; doi:10.1039/d0dt01370f

data_7704580
_publ_section_title
;
 The effect of isomerism and other structural variations on the
 G-quadruplex DNA-binding properties of some nickel Schiff base complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10360
_journal_page_last               10379
_journal_paper_doi               10.1039/d0dt01370f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C28 H22 N2 Ni O4, C3 H7 N O'
_chemical_formula_sum            'C31 H29 N3 Ni O5'
_chemical_formula_weight         582.28
_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             2020-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.082(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5896(2)
_cell_length_b                   17.1222(3)
_cell_length_c                   13.0803(3)
_cell_measurement_reflns_used    16667
_cell_measurement_temperature    294
_cell_measurement_theta_max      28.9920
_cell_measurement_theta_min      1.9730
_cell_volume                     2709.27(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_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_temperature      294
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.0000
_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   10.00    --   20.00  54.00   0.00  368
  2  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-180.00  368
  3  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00  90.00  368
  4  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 150.00  368
  5  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 -60.00  368
  6  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 -30.00  368
  7  \w    -74.00  -4.00   0.50   10.00    --   20.00  54.00  60.00  140
  8  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-120.00  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      -0.0004505000
_diffrn_orient_matrix_UB_12      -0.0008972000
_diffrn_orient_matrix_UB_13      -0.0543756000
_diffrn_orient_matrix_UB_21      0.0504146000
_diffrn_orient_matrix_UB_22      0.0211800000
_diffrn_orient_matrix_UB_23      0.0125123000
_diffrn_orient_matrix_UB_31      0.0299630000
_diffrn_orient_matrix_UB_32      -0.0355418000
_diffrn_orient_matrix_UB_33      0.0087663000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60527
_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         29.130
_diffrn_reflns_theta_min         1.987
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.48a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       cubeoctahedron
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method 'from DMF solvent'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+1.0442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5190
_reflns_number_total             7293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01370f2.cif
_cod_data_source_block           cmpd3_exp_140_tsb19_p
_cod_depositor_comments
;Adding full bibliography for 7704580--7704587.cif.

 Adding full bibliography for 7704580--7704587.cif.
;
_cod_original_cell_volume        2709.28(9)
_cod_database_code               7704580
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C31H29N3NiO5
_chemical_oxdiff_usercomment     'TSB 19_P from DMF'
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.750
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07
_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. Restrained distances
 N2P-C1PA = N2P-C1PB
 1.48 with sigma of 0.02
 N2-C1A = N2-C1B
 1.48 with sigma of 0.02
 C1A-C1PA = C1B-C1PB
 1.51 with sigma of 0.02
 N2-C1PA = N2-C1PB
 2.4 with sigma of 0.04
 N2P-C1A = N2P-C1B
 2.4 with sigma of 0.04
 N3D-C4D \\sim N3D-C5D
 with sigma of 0.02
 N3M-C4M \\sim N3M-C5M
 with sigma of 0.02
3. Restrained planarity
 C2D, O3AA, N3D, C4D, C5D
 with sigma of 0.1
 C2M, O4AA, N3M, C4M, C5M
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2D \\sim O3AA \\sim N3D \\sim C4D \\sim C5D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C2M \\sim O4AA \\sim N3M \\sim C4M \\sim C5M: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C2D, O3AA, N3D, C4D, C5D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2M, O4AA, N3M, C4M, C5M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1PA)=Sof(H1PA)=Sof(H1PB)=1-FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1PB)=Sof(H1PC)=Sof(H1PD)=FVAR(1)
 Sof(C2D)=Sof(H2D)=Sof(O3AA)=Sof(N3D)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(H4DC)=
 Sof(C5D)=Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=1-FVAR(2)
 Sof(C2M)=Sof(H2M)=Sof(O4AA)=Sof(N3M)=Sof(C4M)=Sof(H4MA)=Sof(H4MB)=Sof(H4MC)=
 Sof(C5M)=Sof(H5MA)=Sof(H5MB)=Sof(H5MC)=FVAR(2)
7.a Free rotating group:
 C2D(O3AA,N3D,C4D,C5D), C2M(O4AA,N3M,C4M,C5M)
7.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1PA(H1PA,H1PB), C1PB(H1PC,H1PD)
7.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C5(H5), C5P(H5P), C6(H6), C6P(H6P), C8(H8), C8P(H8P), C9(H9),
 C9P(H9P), C11P(H11P), C12(H12), C12P(H12P), C13(H13), C13P(H13P), C14(H14),
 C14P(H14P), C2D(H2D), C2M(H2M)
7.d Idealised Me refined as rotating group:
 C4D(H4DA,H4DB,H4DC), C5D(H5DA,H5DB,H5DC), C4M(H4MA,H4MB,H4MC), C5M(H5MA,H5MB,
 H5MC)
7.e Idealised tetrahedral OH refined as rotating group:
 O17(H17), O17P(H17P)
;
_shelx_res_checksum              88457
_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.846