Ni(ii)-polypyridyl complexes as potential DNA binders
Sahni, Priya; Gupta, Rahat; Tripathy, Debakanta; Rath, Soumya Lipsa; Pal, Amlan K.; New Journal of Chemistry 47 (2023) 14717–14725; doi:10.1039/D3NJ00961K

data_7062562
_publ_section_title
;
 Ni(ii)-polypyridyl complexes as potential DNA binders
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14717
_journal_page_last               14725
_journal_paper_doi               10.1039/D3NJ00961K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C38 H54 N14 Ni, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C40 H57 F12 N15 Ni P2'
_chemical_formula_weight         1096.65
_chemical_melting_point          ?
_chemical_name_systematic
'[Bis(di(1,3,4,6,7,8-Hexahydro-2H-pyrimido[1,2-a]pyrimidino)pyridine]Nickel(II) hexafluorophosphate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7720(14)
_cell_length_b                   14.0221(8)
_cell_length_c                   13.8462(9)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.24
_cell_volume                     4615.4(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59351
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.324
_diffrn_reflns_theta_min         2.067
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.8579.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_preparation       'Synthesized in laboratory'
_exptl_crystal_recrystallization_method
'The title compound was crystallized by vapour diffusion of diethylether into a concentrated solution of the title compound in acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 4727 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.112(4)
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         11414
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0563P)^2^+4.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                10897
_reflns_number_total             11414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00961k2.cif
_cod_data_source_block           mo_rg07_0ma_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'Not determined' was
changed to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7062562--7062564.cif.
;
_cod_database_code               7062562
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.891
_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
2. Restrained distances
 C17-H17B
 0.95 with sigma of 0.005
 C19-H19A
 0.95 with sigma of 0.005
 H19A-H19B
 1.3 with sigma of 0.04
3. Others
 Fixed Sof: C18A(0.5) C18B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C18A(H18A), C18B(H18B), C19(H19B), C21(H21), C22(H22),
  C23(H23)
4.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              76530
_olex2_exptl_crystal_mounting_method 'On a fiber loop'
_olex2_submission_original_sample_id NiDGPY
_olex2_submission_special_instructions 'No special instructions were received'