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_7703748
_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         'C43 H50 N4 Ni O4'
_chemical_formula_sum            'C43 H50 N4 Ni O4'
_chemical_formula_weight         745.58
_chemical_name_systematic
N,N'-Bis-(4-((1-(2-ethyl)piperidine)oxy)benzophenylidene)-1,2-propylenediaminenickel(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                67.3813(17)
_cell_angle_beta                 74.2421(15)
_cell_angle_gamma                79.8434(15)
_cell_formula_units_Z            2
_cell_length_a                   11.83480(19)
_cell_length_b                   12.9908(2)
_cell_length_c                   16.1427(3)
_cell_measurement_reflns_used    23700
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.0920
_cell_measurement_theta_min      1.7280
_cell_volume                     2197.61(7)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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   23.00    --   20.00  54.00 -15.23  368
  2  \w    -74.00 110.00   0.50   23.00    --   20.00  54.00-150.00  368
  3  \w    -74.00 109.50   0.50   23.00    --   20.00  54.00 106.96  367
  4  \w    -62.00  76.50   0.50   23.00    --   20.00  54.00 -91.64  277
  5  \w    -74.00  57.00   0.50   23.00    --   20.00  54.00 150.00  262
  6  \w     66.00 108.00   0.50   23.00    --   20.00  54.00 150.00   84
  7  \w    -67.00 -14.00   0.50   23.00    --   20.00  54.00  30.00  106
  8  \w      7.00  33.00   0.50   23.00    --   20.00  54.00  30.00   52
  9  \w     54.00  79.50   0.50   23.00    --   20.00  54.00  30.00   51
 10  \w    -71.00  86.00   0.50   23.00    --   20.00  54.00-101.07  314
 11  \w    -73.00  74.00   0.50   23.00    --   20.00  54.00-180.00  294
 12  \w    -73.00 -18.00   0.50   23.00    --   20.00  54.00   0.00  110
 13  \w     58.00 101.00   0.50   23.00    --   20.00  54.00   0.00   86
 14  \w    -74.00  25.00   0.50   23.00    --   20.00  54.00 -30.00  198
;
_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      -0.0171994000
_diffrn_orient_matrix_UB_12      0.0348682000
_diffrn_orient_matrix_UB_13      0.0267407000
_diffrn_orient_matrix_UB_21      0.0510173000
_diffrn_orient_matrix_UB_22      0.0294452000
_diffrn_orient_matrix_UB_23      -0.0246565000
_diffrn_orient_matrix_UB_31      -0.0317019000
_diffrn_orient_matrix_UB_32      0.0379331000
_diffrn_orient_matrix_UB_33      -0.0326004000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48728
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        27.102
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.704
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90860
_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    1.127
_exptl_crystal_description       irregular
_exptl_crystal_F_000             792
_exptl_crystal_recrystallization_method dichloromethane/hexane
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9563
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0542P)^2^+0.4620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8124
_reflns_number_total             9563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00319k2.cif
_cod_data_source_block           cmpd6_exp_118_tsb18
_cod_depositor_comments
'Adding full bibliography for 7703742--7703750.cif.'
_cod_original_cell_volume        2197.62(7)
_cod_database_code               7703748
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C49H64N4NiO4
_chemical_oxdiff_usercomment     'TSB18 from Sean Pham'
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.827
_reflns_odcompleteness_completeness 98.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N18B, N18}
3. Restrained distances
 N1-C2P = C2P-C1P = C1P-N3 = C1P-C1MP
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(N18B) = Uanis(N18)
5. Rigid body (RIGU) restrains
 N18, C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23B, C22B, C21B, C20B, C19B, N18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1MP)=Sof(H1MD)=Sof(H1ME)=Sof(H1MF)=Sof(C1P)=Sof(H1P)=Sof(C2P)=Sof(H2PA)=
 Sof(H2PB)=1-FVAR(1)
 Sof(C1ME)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
 Sof(H18C)=Sof(H18D)=Sof(C23B)=Sof(H23E)=Sof(H23F)=Sof(C22B)=Sof(H22E)=
 Sof(H22F)=Sof(C21B)=Sof(H21E)=Sof(H21F)=Sof(C20B)=Sof(H20E)=Sof(H20F)=
 Sof(C19B)=Sof(H19E)=Sof(H19F)=Sof(N18B)=1-FVAR(2)
 Sof(H18A)=Sof(H18B)=Sof(N18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=FVAR(2)
7.a Free rotating group:
 C23B(C22B,C21B,C20B,C19B,N18B)
7.b Ternary CH refined with riding coordinates:
 C1(H1), C1P(H1P)
7.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2P(H2PA,H2PB), C17(H17A,H17B), C18(H18A,H18B), C18(H18C,H18D),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
  C17P(H17C,H17D), C18P(H18E,H18F), C19P(H19C,H19D), C20P(H20C,H20D), C21P(H21C,
 H21D), C22P(H22C,H22D), C23P(H23C,H23D), C23B(H23E,H23F), C22B(H22E,H22F),
 C21B(H21E,H21F), C20B(H20E,H20F), C19B(H19E,H19F)
7.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15),
 C6P(H6P), C7P(H7P), C8P(H8P), C9P(H9P), C10P(H10P), C12P(H12P), C13P(H13P),
 C15P(H15P)
7.e Idealised Me refined as rotating group:
 C1ME(H1MA,H1MB,H1MC), C1MP(H1MD,H1ME,H1MF)
;
_shelx_res_checksum              56246
_shelx_fab_checksum              1312
_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 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.941