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_7703747
_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         'C29 H24 N2 Ni O5, 2(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C33 H34 N4 Ni O7'
_chemical_formula_weight         657.35
_chemical_name_systematic
N,N'-Bis-(4-(hydroxybenzophenylidene))-2-hydroxy-1,3-propylenediaminenickel(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                 100.144(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3041(4)
_cell_length_b                   8.07129(16)
_cell_length_c                   21.2716(4)
_cell_measurement_reflns_used    15768
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      29.3430
_cell_measurement_theta_min      1.7170
_cell_volume                     3093.49(11)
_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      149.99(10)
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   25.00    --   20.00  54.00  29.95  368
  2  \w    -74.00 110.00   0.50   25.00    --   20.00  54.00 -30.00  368
  3  \w    -74.00 110.00   0.50   25.00    --   20.00  54.00 -30.00  368
  4  \w    -74.00 110.00   0.50   25.00    --   20.00  54.00   1.73  368
  5  \w    -74.00 110.00   0.50   25.00    --   20.00  54.00-150.00  368
  6  \w     12.00  92.00   0.50   25.00    --   20.00  54.00-150.00  160
;
_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      -0.0218037000
_diffrn_orient_matrix_UB_12      0.0488950000
_diffrn_orient_matrix_UB_13      -0.0239592000
_diffrn_orient_matrix_UB_21      0.0060290000
_diffrn_orient_matrix_UB_22      0.0701774000
_diffrn_orient_matrix_UB_23      0.0203063000
_diffrn_orient_matrix_UB_31      0.0322314000
_diffrn_orient_matrix_UB_32      0.0201103000
_diffrn_orient_matrix_UB_33      -0.0126918000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.705
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87203
_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            'translucent green'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method 'from acetonitrile'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7953
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0457P)^2^+2.9016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6297
_reflns_number_total             7953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00319k2.cif
_cod_data_source_block           cmpd9_exp_128_tsb
_cod_depositor_comments
'Adding full bibliography for 7703742--7703750.cif.'
_cod_original_cell_volume        3093.50(11)
_cod_database_code               7703747
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C33 H34 N4 Ni O7'
_chemical_oxdiff_usercomment     TSB22
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.796
_reflns_odcompleteness_completeness 99.47
_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 C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 C2B-N1B = C2C-N1C = N1A-C2A
 1.15 with sigma of 0.01
 C1B-C2B = C1B-C2C = C1A-C2A
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N1B) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1C)
\\sim Ueq, Uanis(C2C) \\sim Ueq: with sigma of 0.05 and sigma for terminal
atoms of 0.1
Uanis(N1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(H16A)=Sof(O18P)=Sof(H18P)=1-FVAR(1)
 Sof(H16)=Sof(O18)=Sof(H18)=FVAR(1)
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(N1C)=Sof(C2C)=1-FVAR(2)
 Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(N1B)=Sof(C2B)=FVAR(2)
5.a Riding coordinates:
 C16(H16), C16(H16A)
5.b Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1P(H1PA,H1PB)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C5P(H5P), C6P(H6P), C7P(H7P), C8P(H8P), C9P(H9P), C11P(H11P), C12P(H12P),
 C14P(H14P)
5.e Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1B(H1BD,H1BE,H1BF)
5.f Idealised tetrahedral OH refined as rotating group:
 O18(H18), O19(H19), O18P(H18P), O19P(H19P)
;
_shelx_res_checksum              90286
_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 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.932