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_7704581
_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         'C22 H18 N2 Ni O3, 0.5(H2 O)'
_chemical_formula_sum            'C22 H19 N2 Ni O3.5'
_chemical_formula_weight         426.10
_chemical_name_systematic
N-(4-(hydroxybenzophenylidene))-N'-salicylidineethylenediaminenickel(II)
_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             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                 106.606(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3061(3)
_cell_length_b                   20.2032(5)
_cell_length_c                   9.6204(3)
_cell_measurement_reflns_used    11958
_cell_measurement_temperature    294.0
_cell_measurement_theta_max      27.5640
_cell_measurement_theta_min      2.0400
_cell_volume                     1919.58(10)
_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      294.0
_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    5.00    --   20.00  54.00 -60.00  368
  2  \w    -74.00 110.00   0.50    5.00    --   20.00  54.00 -60.00  368
  3  \w    -74.00 110.00   0.50    5.00    --   20.00  54.00 -90.00  368
  4  \w    -74.00 110.00   0.50    5.00    --   20.00  54.00  30.00  368
  5  \w    -74.00 110.00   0.50    5.00    --   20.00  54.00-180.00  368
  6  \w    -74.00 110.00   0.50    5.00    --   20.00  54.00  90.00  368
  7  \w    -74.00  71.00   0.50    5.00    --   20.00  54.00   0.00  290
  8  \w    -74.00 110.00   0.50    5.00    --   20.00  54.00 150.00  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      0.0035215000
_diffrn_orient_matrix_UB_12      -0.0097179000
_diffrn_orient_matrix_UB_13      0.0719000000
_diffrn_orient_matrix_UB_21      -0.0713477000
_diffrn_orient_matrix_UB_22      0.0031213000
_diffrn_orient_matrix_UB_23      -0.0162383000
_diffrn_orient_matrix_UB_31      -0.0076427000
_diffrn_orient_matrix_UB_32      -0.0335665000
_diffrn_orient_matrix_UB_33      -0.0221580000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            40482
_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         28.279
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69253
_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    1.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_recrystallization_method 'From DMSO-water'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4762
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0392P)^2^+0.5205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3718
_reflns_number_total             4762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01370f2.cif
_cod_data_source_block           cmpd13_exp_139_tsb5_p
_cod_depositor_comments
;Adding full bibliography for 7704580--7704587.cif.

 Adding full bibliography for 7704580--7704587.cif.
;
_cod_original_formula_sum        'C22 H19 N2 Ni O3.50'
_cod_database_code               7704581
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C22H19N2NiO3.5
_chemical_oxdiff_usercomment     'TSB 5_P from DMSO/water'
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.625
_reflns_odcompleteness_completeness 99.94
_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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.34 with sigma of 0.04
3. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
4.c Idealised tetrahedral OH refined as rotating group:
 O2AA(H2AA)
;
_shelx_res_checksum              43234
_olex2_exptl_crystal_mounting_method 'Mitegen mount with 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 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.860