Synthesis and crystal structure of a nickel(II) 2'-deoxy-6-thioguanosine nitrate complex.
Hribesh, Samira O.; Clegg, William; Harrington, Ross W.; Houlton, Andrew; Pike, Andrew R.; Acta crystallographica. Section C, Structural chemistry 81 (2025) 165–169; doi:10.1107/S2053229625001500

data_2312762
_publ_section_title
;
 Synthesis and crystal structure of a nickel(II) 2'-deoxy-6-thioguanosine
 nitrate complex.
;
_journal_coeditor_code           ZO3062
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              165
_journal_page_last               169
_journal_paper_doi               10.1107/S2053229625001500
_journal_volume                  81
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Ni (C10 H13 N5 O3 S1)3] (N O3)2, 2H2 O'
_chemical_formula_moiety         'C30 H39 N15 Ni O9 S3 2+, 2(N O3 -), 2(H2 O)'
_chemical_formula_sum            'C30 H43 N17 Ni O17 S3'
_chemical_formula_weight         1068.70
_chemical_name_systematic
;
Tris(2'-deoxy-6-thioguanosine)nickel(II) dinitrate dihydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   24.185(4)
_cell_length_b                   24.185(4)
_cell_length_c                   6.6341(10)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.49
_cell_volume                     3360.5(9)
_computing_cell_refinement
;
APEX2 (Bruker, 2012)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2015)
;
_computing_data_reduction
;
APEX2 (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2012)
;
_computing_publication_material
;
SHELXL2019 (Sheldrick, 2015<i>b</i>) and local programs
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn 724+ CCD on kappa'
_diffrn_measurement_method       'wide-frame \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            28605
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.379
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'Diamond beamline I19'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1662
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.553
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3360 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.031(8)
_refine_ls_extinction_coef       0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019/2 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10450
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1065P)^2^+0.2709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                8773
_reflns_number_total             10450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3062sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2312762.cif.'
_cod_original_cell_volume        3360.4(12)
_cod_database_code               2312762
_cod_database_fobs_code          2312762
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              70758
_shelx_res_checksum              57609