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_7703750
_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 O6, 4(C H4 O)'
_chemical_formula_sum            'C32 H38 N2 Ni O10'
_chemical_formula_weight         669.35
_chemical_name_systematic
N,N'-Bis-(4,4'(dihydroxybenzophenylidene))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   mixed
_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                 97.9782(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9739(3)
_cell_length_b                   18.8657(3)
_cell_length_c                   13.1912(2)
_cell_measurement_reflns_used    17483
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.4310
_cell_measurement_theta_min      1.9550
_cell_volume                     3197.45(10)
_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 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    -16.00 110.00   0.50   12.00    --   20.00  54.00 150.00  252
  2  \w    -19.50 110.00   0.50   12.00    --   20.00  54.00 -60.00  259
  3  \w    -74.00 110.00   0.50   12.00    --   20.00  54.00  90.00  368
  4  \w     -5.00  33.00   0.50   12.00    --   20.00  54.00  90.00   76
  5  \w     83.00 109.00   0.50   12.00    --   20.00  54.00  90.00   52
  6  \w    -21.00  42.00   0.50   12.00    --   20.00  54.00-180.00  126
  7  \w    -71.00 -38.00   0.50   12.00    --   20.00  54.00  30.00   66
  8  \w     -9.00 110.00   0.50   12.00    --   20.00  54.00  30.00  238
  9  \w    -58.00 -28.00   0.50   12.00    --   20.00  54.00 120.00   60
 10  \w     22.00  56.00   0.50   12.00    --   20.00  54.00 120.00   68
 11  \w    -74.00   9.00   0.50   12.00    --   20.00  54.00 150.00  166
;
_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      -0.0181857000
_diffrn_orient_matrix_UB_12      -0.0354327000
_diffrn_orient_matrix_UB_13      0.0005196000
_diffrn_orient_matrix_UB_21      0.0082418000
_diffrn_orient_matrix_UB_22      0.0001966000
_diffrn_orient_matrix_UB_23      0.0542856000
_diffrn_orient_matrix_UB_31      -0.0514766000
_diffrn_orient_matrix_UB_32      0.0125747000
_diffrn_orient_matrix_UB_33      0.0004078000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0231
_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       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44690
_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         29.129
_diffrn_reflns_theta_min         1.896
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85218
_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    1.390
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method 'from methanol/DMSO'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0508
_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^)+(0.0617P)^2^+2.4358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7326
_reflns_number_total             8605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00319k2.cif
_cod_data_source_block           cmpd13_exp_136_tsb
_cod_depositor_comments
'Adding full bibliography for 7703742--7703750.cif.'
_cod_original_cell_volume        3197.46(10)
_cod_database_code               7703750
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C32H38N2NiO10
_chemical_oxdiff_usercomment     'TSB 9_P from DMSO/acetone/methanol'
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.732
_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, H1M of O1M, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H5 of O5, H4 of O4, H6 of O6, H3 of O3, H1E of O1E,
  H1H of O1H, H1O of O1O
2.a Rotating group:
 O1M(H1M)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5A), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C16(H16),
 C18(H18), C19(H19), C23(H23), C24(H24), C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C1E(H1EA,H1EB,H1EC), C1O(H1OA,H1OB,H1OC), C1M(H1MA,H1MB,H1MC), C1H(H1HA,H1HB,
 H1HC)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O5(H5), O6(H6), O1E(H1E), O1O(H1O), O1H(H1H)
;
_shelx_res_checksum              526
_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 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.914