Metal(II)-assisted hydrolysis of 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine (tpymt): synthesis, crystal structure and magnetic properties of [Co(bpcam)2]ClO4 . dmso . H2O, [Co(bpcam)2]2[Co(NCS)4] . dmso . H2O and [Ni(bpcam)2] . H2O [Hbpcam = bis(2-pyrimidylcarbonyl)amide]
Rabelo, Renato; Valdo, Ana Karoline Silva Medanha; Robertson, Craig C.; Thomas, Jim; Stumpf, Humberto Osório; Martins, Felipe Terra; Pedroso, Emerson F.; Julve, Miguel; Lloret, Francesc; Cangussu, Danielle; New J. Chem. 41 (2017) 6911–6921; doi:10.1039/C7NJ00526A

data_7056327
_publ_section_title
;
 Metal(II)-assisted hydrolysis of 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine
 (tpymt): synthesis, crystal structure and magnetic properties of
 [Co(bpcam)2]ClO4 . dmso . H2O, [Co(bpcam)2]2[Co(NCS)4] . dmso . H2O and
 [Ni(bpcam)2] . H2O [Hbpcam = bis(2-pyrimidylcarbonyl)amide]
;
_journal_issue                   14
_journal_name_full               'New J. Chem.'
_journal_page_first              6911
_journal_page_last               6921
_journal_paper_doi               10.1039/C7NJ00526A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C92 H61 Co6 N48 O20 S10'
_chemical_formula_weight         2833.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-07 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.8860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.5807(5)
_cell_length_b                   24.4918(6)
_cell_length_c                   14.4619(4)
_cell_measurement_reflns_used    8826
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.90
_cell_volume                     6130.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2008)'
_computing_publication_material
'SHELXL-2014/7 (Sheldrick, 2015), WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR 2004 (Burla, 2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22885
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         1.663
_exptl_absorpt_coefficient_mu    1.046
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       plate
_exptl_crystal_F_000             2862
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.677
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         10478
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.677
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+13.0950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                8975
_reflns_number_total             10478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00526a2.cif
_cod_data_source_block           shelx
_cod_database_code               7056327
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              89246
_shelx_fab_checksum              28627