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_1564974
_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            'C38 H26 Co N12 O6.5'
_chemical_formula_weight         1627.28
_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                98.402(3)
_cell_angle_beta                 103.957(3)
_cell_angle_gamma                90.379(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8536(9)
_cell_length_b                   13.6966(14)
_cell_length_c                   15.8989(16)
_cell_measurement_reflns_used    9345
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      2.37
_cell_volume                     1849.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            72778
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         7649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1400P)^2^+2.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2441
_reflns_number_gt                5398
_reflns_number_total             7649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-506-119506.cif
_cod_data_source_block           compound-3
_cod_depositor_comments
;

2022-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H52 Co2 N24 O13'
_cod_original_formula_weight         1627.28
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1564974