New binuclear Ni(ii) metallates containing ONS chelators: synthesis, characterisation, DNA binding, DNA cleavage, protein binding, antioxidant activity, antimicrobial and in vitro cytotoxicity
Kalaiarasi, G.; Jain, Ruchi; Puschman, H.; Poorna Chandrika, S.; Preethi, K.; Prabhakaran, R.; New J. Chem. 41 (2017) 2543–; doi:10.1039/C6NJ03516G

data_7056014
_publ_section_title
;
 New binuclear Ni(ii) metallates containing ONS chelators: synthesis,
 characterisation, DNA binding, DNA cleavage, protein binding, antioxidant
 activity, antimicrobial and in vitro cytotoxicity
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              2543
_journal_paper_doi               10.1039/C6NJ03516G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C44 H42 N6 Ni2 O4 P2 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C50 H56 N8 Ni2 O6 P2 S2'
_chemical_formula_weight         1108.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-09-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-10-20 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                93.080(4)
_cell_angle_beta                 108.522(3)
_cell_angle_gamma                98.363(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5619(11)
_cell_length_b                   11.0171(12)
_cell_length_c                   11.3222(12)
_cell_measurement_reflns_used    4581
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.304
_cell_volume                     1228.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0980
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16394
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.304
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1338 before and 0.1036 after correction.
The Ratio of minimum to maximum transmission is 0.7395.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             578
_exptl_crystal_recrystallization_method
'The material was recrystallised from DMF by slow evaporation'
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3848
_reflns_number_total             5617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03516g2.cif
_cod_data_source_block           rpn14de
_cod_depositor_comments
'Adding full bibliography for 7056013--7056014.cif.'
_cod_database_code               7056014
_shelxl_version_number           2014/6
_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
 N3-H3B \\sim N3-H3A
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C1S(H1S)
3.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              8767
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700 Series'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id NiPL14DE
_olex2_submission_special_instructions 'No special instructions were received'