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_7704587
_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         'C42 H47.67 N4 Ni O4, C H Cl3, 0.15(H2 O)'
_chemical_formula_sum            'C43 H48.96 Cl3 N4 Ni O4.15'
_chemical_formula_weight         853.28
_chemical_name_systematic
N,N'-Bis-(4'-((1-(2-ethyl)piperidine)oxy)benzophenylidene)ethylenediaminenickel(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   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                84.318(3)
_cell_angle_beta                 76.970(3)
_cell_angle_gamma                73.292(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9317(3)
_cell_length_b                   14.6642(6)
_cell_length_c                   14.9018(5)
_cell_measurement_reflns_used    12865
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5970
_cell_measurement_theta_min      1.9750
_cell_volume                     2023.80(13)
_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'
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_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    -74.00 109.00   0.50   20.00    --   20.00  54.00  30.00  366
  2  \w    -56.00 -29.00   0.50   20.00    --   20.00  54.00 120.00   54
  3  \w     18.00  72.00   0.50   20.00    --   20.00  54.00 120.00  108
  4  \w    -71.00 110.00   0.50   20.00    --   20.00  54.00 -90.00  362
  5  \w    -41.00 -16.00   0.50   20.00    --   20.00  54.00-150.00   50
  6  \w      4.00  30.00   0.50   20.00    --   20.00  54.00-150.00   52
  7  \w     36.00  61.00   0.50   20.00    --   20.00  54.00-150.00   50
  8  \w    -73.00  32.00   0.50   20.00    --   20.00  54.00 150.00  210
  9  \w     39.00  64.00   0.50   20.00    --   20.00  54.00 150.00   50
 10  \w     85.00 110.00   0.50   20.00    --   20.00  54.00 150.00   50
 11  \w    -65.00   2.00   0.50   20.00    --   20.00  54.00  60.00  134
 12  \w      7.00  33.00   0.50   20.00    --   20.00  54.00  60.00   52
 13  \w    -73.00 -26.00   0.50   20.00    --   20.00  54.00-120.00   94
 14  \w    -61.00 -35.00   0.50   20.00    --   20.00  54.00-180.00   52
 15  \w     -8.00  17.00   0.50   20.00    --   20.00  54.00-180.00   50
 16  \w    -69.00 -42.00   0.50   20.00    --   20.00  54.00 -60.00   54
 17  \w    -63.00  67.00   0.50   20.00    --   20.00  54.00  90.00  260
 18  \w    -70.00  72.00   0.50   20.00    --   20.00  54.00 -13.07  284
;
_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      0.0446175000
_diffrn_orient_matrix_UB_12      -0.0166580000
_diffrn_orient_matrix_UB_13      -0.0427475000
_diffrn_orient_matrix_UB_21      -0.0562303000
_diffrn_orient_matrix_UB_22      0.0242317000
_diffrn_orient_matrix_UB_23      -0.0229533000
_diffrn_orient_matrix_UB_31      0.0256055000
_diffrn_orient_matrix_UB_32      0.0410992000
_diffrn_orient_matrix_UB_33      -0.0059955000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38950
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.981
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89264
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       rod
_exptl_crystal_F_000             894
_exptl_crystal_recrystallization_method 'from chloroform'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         10295
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0386P)^2^+0.7952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8551
_reflns_number_total             10295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01370f2.cif
_cod_data_source_block           cmpd4_exp_104_sp
_cod_depositor_comments
;Adding full bibliography for 7704580--7704587.cif.

 Adding full bibliography for 7704580--7704587.cif.
;
_cod_database_code               7704587
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C43 H49 Cl3 N4 Ni O4.15'
_chemical_oxdiff_usercomment     'TSB 19'
_reflns_odcompleteness_completeness 98.30
_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,H) groups
2. Restrained distances
 C4DA-Cl1A = C4DA-Cl1B
 1.76 with sigma of 0.005
 N2-C1 \\sim N2-C1A
 with sigma of 0.02
 N2P-C1P \\sim N2P-C1AP
 with sigma of 0.02
 C1-C1P \\sim C1A-C1AP
 with sigma of 0.02
 C19P-N20P \\sim C19-N20
 with sigma of 0.02
 C19P-N20P \\sim C19-N20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C22A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C1) = Uanis(C1A)
Uanis(C21) = Uanis(C25A)
Uanis(C23) = Uanis(C23A)
4. Rigid body (RIGU) restrains
 C19, N20, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, N20A, C21A, C22A, C23A, C24A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N20P, C21P, C22P, C23P, C24P, C25P} sigma for 1-2: 0.01, 1-3: 0.02
as
{N20, C21, C22, C23, C24, C25}
{N20P, C21P, C22P, C23P, C24P, C25P} sigma for 1-2: 0.01, 1-3: 0.02
as
{N20A, C21A, C22A, C23A, C24A, C25A}
6. Others
 Sof(H4DB)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(H4DA)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1AP)=Sof(H1AC)=Sof(H1AD)=1-FVAR(2)
 Sof(C1P)=Sof(H1PA)=Sof(H1PB)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(N20A)=Sof(C21A)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22E)=Sof(H22F)=
 Sof(C23A)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25E)=Sof(H25F)=1-FVAR(3)
 Sof(H19C)=Sof(H19D)=Sof(N20)=Sof(C21)=Sof(H21C)=Sof(H21D)=Sof(C22)=Sof(H22C)=
 Sof(H22D)=Sof(C23)=Sof(H23C)=Sof(H23D)=Sof(C24)=Sof(H24C)=Sof(H24D)=Sof(C25)=
 Sof(H25C)=Sof(H25D)=FVAR(3)
 Fixed Sof: O1W(0.15) H1WA(0.15) H1WB(0.15)
 Fixed X: O1W(-0.14243)
 Fixed Y: O1W(0.89371)
 Fixed Z: O1W(0.88236)
7.a Free rotating group:
 O1W(H1WA,H1WB)
7.b Ternary CH refined with riding coordinates:
 C4DA(H4DA), C4DA(H4DB)
7.c Secondary CH2 refined with riding coordinates:
 C1P(H1PA,H1PB), C18P(H18A,H18B), C19P(H19A,H19B), C21P(H21A,H21B), C22P(H22A,
 H22B), C23P(H23A,H23B), C24P(H24A,H24B), C25P(H25A,H25B), C1(H1A,H1B),
 C18(H18C,H18D), C19(H19C,H19D), C21(H21C,H21D), C22(H22C,H22D), C23(H23C,H23D),
  C24(H24C,H24D), C25(H25C,H25D), C21A(H21E,H21F), C22A(H22E,H22F), C23A(H23E,
 H23F), C24A(H24E,H24F), C25A(H25E,H25F), C1A(H1AA,H1AB), C1AP(H1AC,H1AD)
7.d Aromatic/amide H refined with riding coordinates:
 C5P(H5P), C6P(H6P), C8P(H8P), C9P(H9P), C11P(H11P), C12P(H12P), C13P(H13P),
 C14P(H14P), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14)
;
_shelx_res_checksum              26083
_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 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.895