A new route for the synthesis of 2,4-bis(2-pyridyl)-6-(pyridyl)pyrimidines: Synthesis and characterization of Co(II), Ni(II) complexes of 2,4,6-tris(2-pyridyl)pyrimidine
Bori, Jugal; Mahata, Satyajit; Manivannan, Vadivelu; Inorganica Chimica Acta 506 (2020) 119506–; doi:10.1016/j.ica.2020.119506

data_1564973
_publ_section_title
;
 A new route for the synthesis of
 2,4-bis(2-pyridyl)-6-(pyridyl)pyrimidines: Synthesis and characterization
 of Co(II), Ni(II) complexes of 2,4,6-tris(2-pyridyl)pyrimidine
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119506
_journal_paper_doi               10.1016/j.ica.2020.119506
_journal_volume                  506
_journal_year                    2020
_chemical_formula_sum            'C76 H52 N24 Ni2 O13'
_chemical_formula_weight         1626.80
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.758(4)
_cell_angle_beta                 103.528(5)
_cell_angle_gamma                90.351(5)
_cell_formula_units_Z            1
_cell_length_a                   8.7983(6)
_cell_length_b                   13.6714(7)
_cell_length_c                   15.8434(8)
_cell_measurement_reflns_used    6085
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3120
_cell_measurement_theta_min      3.4360
_cell_volume                     1834.49(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15524
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76875
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836.0
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+2.8230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                6009
_reflns_number_total             7594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-506-119506.cif
_cod_data_source_block           compound-2
_cod_original_cell_volume        1834.48(18)
_cod_database_code               1564973