Two Cu(II) and Zn(II) complexes derived from 5-(Pyrazol-1-yl)nicotinic acid: Crystal structure, DNA binding and anticancer studies
Ji, Xiaoxi; Zhu, Xiaopeng; Chen, Shiyu; Song, Dongxue; Wu, Shuangyan; Zhang, Ying; Gao, Enjun; Xu, Jin; Zhu, Mingchang; Journal of Solid State Chemistry 305 (2022) 122707–; doi:10.1016/j.jssc.2021.122707

data_1566062
_publ_section_title
;
 Two Cu(II) and Zn(II) complexes derived from 5-(Pyrazol-1-yl)nicotinic
 acid: Crystal structure, DNA binding and anticancer studies
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              122707
_journal_paper_doi               10.1016/j.jssc.2021.122707
_journal_volume                  305
_journal_year                    2022
_chemical_formula_moiety         'C18 H12 N6 O4 Zn, 2(H2 O)'
_chemical_formula_sum            'C18 H17 N6 O6 Zn'
_chemical_formula_weight         478.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 95.807(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9796(12)
_cell_length_b                   10.0261(10)
_cell_length_c                   16.1223(18)
_cell_measurement_reflns_used    5517
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.419
_cell_measurement_theta_min      2.540
_cell_volume                     1926.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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_temperature      150.02
_diffrn_measured_fraction_theta_full 0.998
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25632
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.426
_diffrn_reflns_theta_min         2.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0851 before and 0.0684 after correction. The Ratio of minimum to maximum transmission is 0.3913. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       needle
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0327P)^2^+1.8271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2861
_reflns_number_total             3955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2022-305-122707.cif
_cod_data_source_block           mo_0912_7_0m
_cod_database_code               1566062
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-H5B
 0.89 with sigma of 0.01
3.a Free rotating group:
 O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C10(H10), C6(H6), C15(H15), C0AA(H0AA), C9(H9), C18(H18),
 C17(H17), C16(H16), C8(H8), C7(H7)
;
_shelx_res_checksum              28585
_shelx_hkl_checksum              27362