Further Study of the Reaction of Fe2+ with CN-: Synthesis and Characterization of cis and trans[FeII,III(CN)4L2]n- Complexes
Gina M. Chiarella; Doris Y. Melgarejo; Stephen A. Koch; Journal of the American Chemical Society 128 (2006) 1416–1417; doi:10.1021/ja0571951

data_4110389
_publ_contact_author_address
;Department of Chemistry
SUNY at Stony Brook
Stony Brook, NY 11794-3400
;
_publ_contact_author_email       stephen.koch@sunysb.edu
_publ_contact_author_fax         631-632-7960
_publ_contact_author_name        'Stephen Koch'
_publ_contact_author_phone       631-632-7944
_publ_section_title
;
 Further Study of the Reaction of Fe2+ with CN-: Synthesis and
 Characterization of cis and trans[FeII,III(CN)4L2]n- Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1416
_journal_page_last               1417
_journal_paper_doi               10.1021/ja0571951
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source
'From reaction of cis-[Fe(II)(CN)4(py)2]2-  with CO'
_chemical_formula_moiety         '2(C16N1H36 1-), Fe1O1C10N5H5 2-'
_chemical_formula_sum            'C42 H77 Fe N7 O'
_chemical_formula_weight         751.96
_chemical_name_common            trans-[(n-Bu)4N]2[Fe(II)(CN)4(CO)py]
_chemical_name_systematic
'bis-tetrabutylammonium trans-iron(II)tetracyanidecarbonylpyradine'
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.631(4)
_cell_length_b                   21.874(4)
_cell_length_c                   19.345(3)
_cell_measurement_reflns_used    3659
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.94
_cell_measurement_theta_min      2.47
_cell_volume                     9576(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25958
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.9374
_exptl_absorpt_correction_T_min  0.8022
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1863
_reflns_number_gt                2457
_reflns_number_total             5548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0571951si20051021_042151_6.cif
_cod_data_source_block           Fe(II)(CN)4(CO)py
_cod_original_cell_volume        9577(3)
_cod_database_code               4110389