Isotypic Mn^II^ and Fe^II^ binuclear complexes of the ligand 5,6-bis(pyridin-2-yl)-pyrazine-2,3-dicarboxylic acid
Alfonso, Monserrat; Stoeckli-Evans, Helen; Acta Crystallographica Section E 72 (2016) 1412–1416; doi:10.1107/S2056989016014055

data_2241845
_publ_section_title
;
 Isotypic Mn^II^ and Fe^II^ binuclear complexes of the ligand
 5,6-bis(pyridin-2-yl)-pyrazine-2,3-dicarboxylic acid
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1412
_journal_page_last               1416
_journal_paper_doi               10.1107/S2056989016014055
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Fe2 (C16 H8 N4 O4)2 (H2 O)4], 4H2 O'
_chemical_formula_moiety         'C32 H24 Fe2 N8 O12, 4(H2 O)'
_chemical_formula_sum            'C32 H32 Fe2 N8 O16'
_chemical_formula_weight         896.35
_chemical_name_systematic
'Bis[\m-5,6-bis(pyridin-2-yl)pyrazine-2,3-dicarboxylato]-\k^4^<i>N</i>^1^,<i>O</i>^2^,<i>N</i>^6^:<i>O</i>^3^;\k^4^<i>O</i>^3^:<i>N</i>^1^,<i>O</i>^2^,<i>N</i>^6^-bis[diaquairon(II)] tetrahydrate'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                69.500(12)
_cell_angle_beta                 83.593(13)
_cell_angle_gamma                84.238(13)
_cell_formula_units_Z            1
_cell_length_a                   8.0933(9)
_cell_length_b                   10.3403(11)
_cell_length_c                   11.5679(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     899.16(18)
_computing_cell_refinement
;
CELL in IPDS-I (Stoe & Cie, 2004)
;
_computing_data_collection
;
EXPOSE in IPDS-I (Stoe & Cie, 2004)
;
_computing_data_reduction
;
INTEGRATE in IPDS-I (Stoe & Cie, 2004)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       '1 circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 1 image plate'
_diffrn_measurement_method       '\f rotation'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.735
_diffrn_reflns_theta_min         2.107
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2009)
;
_exptl_crystal_colour            dark-violet
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.685
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0720P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                2475
_reflns_number_total             3202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pj2034sup1.cif
_cod_data_source_block           II
_cod_database_code               2241845
_cod_database_fobs_code          2241845
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.916
_shelx_hkl_checksum              20171
_shelx_res_checksum              64516
_shelxl_version_number           2014/6