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_7056325
_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_moiety         'C20 H12 N10 Ni O4, H2 O'
_chemical_formula_sum            'C20 H14 N10 Ni O5'
_chemical_formula_weight         533.10
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-05-18 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                74.233(3)
_cell_angle_beta                 83.559(3)
_cell_angle_gamma                64.292(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8015(15)
_cell_length_b                   10.0257(17)
_cell_length_c                   13.876(2)
_cell_measurement_reflns_used    3371
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      53.837
_cell_measurement_theta_min      4.656
_cell_volume                     1061.7(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker smart1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12287
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.9175
_exptl_absorpt_correction_T_min  0.6576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.2245 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.7008. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3468
_reflns_number_total             4765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00526a2.cif
_cod_data_source_block           rich1m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7056325
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.658
_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.a Free rotating group:
 O1W(H1WA,H1WB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              40429
_olex2_submission_special_instructions 'No special instructions were received'