Bis(2,3,5,6-tetra-2-pyridylpyrazine-κ^3^<i>N</i>^2^,<i>N</i>^1^,<i>N</i>^6^)iron(II) bis(dicyanamidate) 4.5-hydrate
Callejo, L.; De la Pinta, N.; Madariaga, G.; Fidalgo, M.L.; Cortés, R.; Acta Crystallographica Section E 66 (2010) m249–m250; doi:10.1107/S1600536810003363

data_2225412
_publ_section_title
;Bis(2,3,5,6-tetra-2-pyridylpyrazine-\k^3^<i>N</i>^2^,<i>N</i>^1^,<i>N</i>^6^)iron(II)
 bis(dicyanamidate) 4.5-hydrate
;
_journal_coeditor_code           ZL2260
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m249
_journal_page_last               m250
_journal_paper_doi               10.1107/S1600536810003363
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Fe (C24 H16 N6)2] (C2 N3)2, 4.5H2 O'
_chemical_formula_moiety         'C48 H32 Fe N12 2+, 2(C2 N3 -), 4.5(H2 O)'
_chemical_formula_sum            'C52 H41 Fe N18 O4.5'
_chemical_formula_weight         1045.88
_chemical_name_systematic
;
Bis(2,3,5,6-tetra-2-pyridylpyrazine-
\k^3^<i>N</i>^2^,<i>N</i>^1^,<i>N</i>^6^)iron(II) bis(dicyanamidate)
4.5-hydrate
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.017(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9216(7)
_cell_length_b                   18.9271(9)
_cell_length_c                   19.1425(9)
_cell_measurement_reflns_used    8676
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.94
_cell_measurement_theta_min      3.2
_cell_volume                     5006.2(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.7
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 2'
_diffrn_measurement_method
;
656 images at 0.7^o^ stepwise rotation in omega and 90^o^ phi, 30 sec./frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51234
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         31.94
_diffrn_reflns_theta_min         3.2
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      1.39(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.344
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     779
_refine_ls_number_reflns         15912
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1444
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                8433
_reflns_number_total             15912
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2260.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C52 H41 Fe1 N18 O4.5'
_cod_database_code               2225412
_cod_database_fobs_code          2225412