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_7704586
_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_absolute_configuration ad
_chemical_formula_moiety         'C33 H33 N3 Ni O3'
_chemical_formula_sum            'C33 H33 N3 Ni O3'
_chemical_formula_weight         578.33
_chemical_name_systematic
N-(4-((1-(2-ethyl)piperidine)oxy)benzophenylidene)-N'-(naphthalidine)ethylenediaminenickel(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                 99.5135(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9200(4)
_cell_length_b                   7.61382(12)
_cell_length_c                   19.7486(3)
_cell_measurement_reflns_used    29870
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5700
_cell_measurement_theta_min      1.7240
_cell_volume                     2805.73(9)
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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    8.50    --   20.00  54.00 -97.68  368
  2  \w    -74.00 110.00   0.50    8.50    --   20.00  54.00 -62.93  368
  3  \w    -74.00 110.00   0.50    8.50    --   20.00  54.00 -55.68  368
  4  \w    -74.00 110.00   0.50    8.50    --   20.00  54.00 -55.68  368
  5  \w    -74.00 109.50   0.50    8.50    --   20.00  54.00-133.48  367
  6  \w    -74.00 109.50   0.50    8.50    --   20.00  54.00 164.70  367
  7  \w    -74.00 110.00   0.50    8.50    --   20.00  54.00-120.00  368
  8  \w     60.00 110.00   0.50    8.50    --   20.00  54.00-120.00  100
  9  \w    -69.00  48.00   0.50    8.50    --   20.00  54.00 -80.48  234
 10  \w     85.00 110.00   0.50    8.50    --   20.00  54.00 -80.48   50
 11  \w    -63.00  45.00   0.50    8.50    --   20.00  54.00  30.00  216
 12  \w     51.00  77.00   0.50    8.50    --   20.00  54.00  30.00   52
;
_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      0.0363243000
_diffrn_orient_matrix_UB_12      -0.0194346000
_diffrn_orient_matrix_UB_13      -0.0017386000
_diffrn_orient_matrix_UB_21      -0.0072291000
_diffrn_orient_matrix_UB_22      0.0097036000
_diffrn_orient_matrix_UB_23      -0.0361806000
_diffrn_orient_matrix_UB_31      0.0085794000
_diffrn_orient_matrix_UB_32      0.0906426000
_diffrn_orient_matrix_UB_33      0.0035141000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73796
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         2.091
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88653
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method 'from DCM/MeOH'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 5621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(5)
_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     721
_refine_ls_number_reflns         14383
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.7377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                13184
_reflns_number_total             14383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01370f2.cif
_cod_data_source_block           cmpd16_exp_134_tsb
_cod_depositor_comments
;Adding full bibliography for 7704580--7704587.cif.

 Adding full bibliography for 7704580--7704587.cif.
;
_cod_original_cell_volume        2805.73(8)
_cod_database_code               7704586
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C33H33N3Ni1O3
_chemical_oxdiff_usercomment     'TSB 27 from DCM/MeOH'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.759
_reflns_odcompleteness_completeness 99.53
_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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C1A(H1AA,H1AB),
  C26A(H26C,H26D), C27A(H27C,H27D), C28A(H28C,H28D), C29A(H29C,H29D), C30A(H30C,
 H30D), C31A(H31C,H31D), C32A(H32C,H32D), C33A(H33C,H33D)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C2A(H2A),
  C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A), C14A(H14A),
 C16A(H16A), C17A(H17A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C25A(H25A)
;
_shelx_res_checksum              21310
_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 1.097
_oxdiff_exptl_absorpt_empirical_full_min 0.943