Structure of the first dinuclear Ni(II) complex with an azapurine derivative (the anionic form of 4,6-dimethyl-1,2,3-triazolo[4,5-d]pyrimidin-5,7-dione)
Carmen R. Maldonado; Miguel Quirós; Juan M. Salas; Duane Choquesillo-Lazarte; Inorganic Chemistry Communications 13 (2010) 1081–1084; doi:10.1016/j.inoche.2010.06.020

data_4331393
_publ_contact_author_address
;
Departamento de Qu\'imica Inorg\'anica, Facultad de Ciencias,
c/ Severo Ochoa s/n, 18071 Granada, Spain
;
_publ_contact_author_email       jsalas@ugr.es
_publ_contact_author_fax         '34 958 248526'
_publ_contact_author_name        'Miguel Quir\'os'
_publ_contact_author_phone       '34 958 248525'
_publ_section_title
;
 Structure of the first dinuclear Ni(II) complex with an azapurine
 derivative (the anionic form of
 4,6-dimethyl-1,2,3-triazolo[4,5-d]pyrimidin-5,7-dione)
;
_journal_name_full               'Inorganic Chemistry Communications'
_journal_page_first              1081
_journal_page_last               1084
_journal_paper_doi               10.1016/j.inoche.2010.06.020
_journal_volume                  13
_journal_year                    2010
_chemical_formula_moiety
'C50 H62 N19 Ni2 O8 1+, C6 H6 N5 O2 1-, C H4 O, 2 (H2 O)'
_chemical_formula_sum            'C57 H76 N24 Ni2 O13'
_chemical_formula_weight         1422.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.462(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1449(6)
_cell_length_b                   23.9300(12)
_cell_length_c                   22.4250(11)
_cell_measurement_reflns_used    9145
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      66.19
_cell_measurement_theta_min      4.21
_cell_volume                     6363.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graded multi-layer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            93406
_diffrn_reflns_theta_full        66.55
_diffrn_reflns_theta_max         66.55
_diffrn_reflns_theta_min         2.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         11015
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2317
_refine_ls_wR_factor_ref         0.2340
_reflns_number_gt                10768
_reflns_number_total             11015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            niaxbfly.cif
_cod_data_source_block           niaxbfly
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4331393
_cod_database_fobs_code          4331393