Structure and properties of 2,2′-bipyridine-3,3′,6,6′-tetracarboxylic acid and its iron(II) and cobalt(II) complexes
Dawid, Urszula; Pruchnik, Florian P.; Starosta, Radosław; Dalton Transactions  (2009) 3348–3353; doi:10.1039/b820474h

data_7001103
_publ_section_title
;
 Structure and properties of
 2,2&#x2032;-bipyridine-3,3&#x2032;,6,6&#x2032;-tetracarboxylic acid
 and its iron(II) and cobalt(II) complexes
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3348
_journal_page_last               3353
_journal_paper_doi               10.1039/b820474h
_journal_year                    2009
_chemical_formula_moiety         '[Fe2(C10H4N2(COO)2(COOH)2)2(H2O)4]4.74H2O'
_chemical_formula_sum            'C28 H29.47 Fe2 N4 O24.74'
_chemical_formula_weight         929.49
_chemical_name_common
;di-u-(2,2'-bipyridine-3,3',6,6'-tetracarboxylato(2-)-
k4N,N',O6,O6')diiron(ii)
;
_chemical_name_systematic
;
di-u-[2,2'-bipyridine-3,3',6,6'-tetracarboxylato(2-)-k4N,N',O6,O6']diiron(II)
;
_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                 108.06(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.388(5)
_cell_length_b                   11.054(3)
_cell_length_c                   20.139(6)
_cell_measurement_reflns_used    3450
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      2.81
_cell_volume                     3468.5(19)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    "'SHELXTL (Bruker, 1999)'"
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.1532
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23690
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(ABSPACK and analytical correction; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         7950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                3856
_reflns_number_total             7950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820474h.txt
_cod_data_source_block           fp01pac
_cod_original_cell_volume        3468.5(18)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7001103