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#$Date: 2016-03-22 10:32:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178874 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/03/4110389.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4110389
loop_
_publ_author_name
'Gina M. Chiarella'
'Doris Y. Melgarejo'
'Stephen A. Koch'
_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/[σ²(Fo²)+(0.1012P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x-1/2, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.50084(2) 0.28478(3) 0.0480(2) Uani 1 2 d S . .
C1 C 0.5000 0.4641(2) 0.2060(3) 0.0771(15) Uani 1 2 d S . .
C2 C 0.43959(14) 0.44613(13) 0.31861(16) 0.0546(7) Uani 1 1 d . . .
C3 C 0.55991(14) 0.55720(14) 0.25300(16) 0.0563(7) Uani 1 1 d . . .
N4 N 0.5000 0.23002(15) 0.34644(18) 0.0623(10) Uani 1 2 d S . .
N1 N 0.5000 0.54365(14) 0.37998(16) 0.0505(8) Uani 1 2 d S . .
N2 N 0.40318(13) 0.41442(13) 0.33803(15) 0.0813(9) Uani 1 1 d . . .
N3 N 0.59509(12) 0.59070(13) 0.23431(16) 0.0808(9) Uani 1 1 d . . .
O1 O 0.5000 0.4395(2) 0.1533(2) 0.1313(17) Uani 1 2 d S . .
C4 C 0.44999(15) 0.55623(14) 0.41291(17) 0.0669(9) Uani 1 1 d . . .
H4 H 0.4142 0.5492 0.3906 0.080 Uiso 1 1 calc R . .
C5 C 0.4494(2) 0.57970(16) 0.4803(2) 0.0859(12) Uani 1 1 d . . .
H5 H 0.4135 0.5876 0.5020 0.103 Uiso 1 1 calc R . .
C6 C 0.5000 0.5909(2) 0.5136(3) 0.0870(17) Uani 1 2 d S . .
H6 H 0.5000 0.6059 0.5586 0.104 Uiso 1 2 calc SR . .
C7 C 0.5000 0.16588(18) 0.3752(2) 0.0670(13) Uani 1 2 d S . .
H7A H 0.5345 0.1447 0.3576 0.080 Uiso 0.50 1 calc PR . .
H7B H 0.4655 0.1447 0.3576 0.080 Uiso 0.50 1 calc PR . .
C8 C 0.5000 0.1606(2) 0.4533(2) 0.105(2) Uani 1 2 d S A .
H8A H 0.4653 0.1806 0.4721 0.126 Uiso 0.50 1 calc PR . .
H8B H 0.5347 0.1806 0.4721 0.126 Uiso 0.50 1 calc PR . .
C9 C 0.5000 0.0929(3) 0.4736(4) 0.163(4) Uani 1 2 d S . .
H9A H 0.4707 0.0706 0.4470 0.195 Uiso 0.50 1 calc PR A .
H9B H 0.4910 0.0882 0.5223 0.195 Uiso 0.50 1 calc PR . .
C10 C 0.5713(8) 0.0655(5) 0.4556(6) 0.193(7) Uani 0.50 1 d P A -1
H10A H 0.6000 0.0953 0.4697 0.289 Uiso 0.50 1 calc PR A -1
H10B H 0.5750 0.0581 0.4068 0.289 Uiso 0.50 1 calc PR A -1
H10C H 0.5778 0.0280 0.4803 0.289 Uiso 0.50 1 calc PR A -1
C11 C 0.55369(16) 0.26554(15) 0.36997(18) 0.0794(10) Uani 1 1 d . . .
H11A H 0.5515 0.3063 0.3505 0.095 Uiso 1 1 calc R . .
H11B H 0.5520 0.2696 0.4199 0.095 Uiso 1 1 calc R . .
C12 C 0.61245(18) 0.23827(19) 0.3510(3) 0.1121(14) Uani 1 1 d . . .
H12A H 0.6141 0.1965 0.3677 0.134 Uiso 1 1 calc R . .
H12B H 0.6160 0.2372 0.3010 0.134 Uiso 1 1 calc R . .
C13 C 0.6635(2) 0.2735(2) 0.3804(4) 0.167(3) Uani 1 1 d . . .
H13A H 0.6997 0.2573 0.3609 0.200 Uiso 1 1 calc R . .
H13B H 0.6600 0.3157 0.3656 0.200 Uiso 1 1 calc R . .
C14 C 0.6684(4) 0.2726(5) 0.4525(5) 0.275(6) Uani 1 1 d . . .
H14A H 0.6375 0.2970 0.4724 0.412 Uiso 1 1 calc R . .
H14B H 0.7061 0.2889 0.4659 0.412 Uiso 1 1 calc R . .
H14C H 0.6649 0.2313 0.4688 0.412 Uiso 1 1 calc R . .
C15 C 0.5000 0.22227(19) 0.2691(2) 0.0663(12) Uani 1 2 d S . .
H15A H 0.5346 0.1986 0.2562 0.080 Uiso 0.50 1 calc PR . .
H15B H 0.4654 0.1986 0.2562 0.080 Uiso 0.50 1 calc PR . .
C16 C 0.5000 0.2803(2) 0.2279(3) 0.0873(16) Uani 1 2 d S . .
H16A H 0.5347 0.3043 0.2396 0.105 Uiso 0.50 1 calc PR . .
H16B H 0.4653 0.3043 0.2396 0.105 Uiso 0.50 1 calc PR . .
C17 C 0.5000 0.2670(4) 0.1505(4) 0.209(6) Uani 1 2 d S . .
H17A H 0.4659 0.2894 0.1337 0.251 Uiso 0.50 1 calc PR . .
H17B H 0.5341 0.2894 0.1337 0.251 Uiso 0.50 1 calc PR . .
C18 C 0.5000 0.2256(4) 0.1187(4) 0.381(14) Uani 1 2 d S . .
H18A H 0.4849 0.2353 0.0737 0.572 Uiso 0.50 1 d PR . .
H18B H 0.4755 0.1950 0.1398 0.572 Uiso 0.50 1 d PR . .
H18C H 0.5396 0.2104 0.1146 0.572 Uiso 0.50 1 d PR . .
C19 C 0.70106(16) -0.0430(2) 0.2806(2) 0.0943(13) Uani 1 1 d . . .
H19A H 0.6712 -0.0159 0.2992 0.113 Uiso 1 1 calc R . .
H19B H 0.6829 -0.0667 0.2439 0.113 Uiso 1 1 calc R . .
C20 C 0.7205(2) -0.0862(3) 0.3369(3) 0.172(3) Uani 1 1 d . . .
H20A H 0.7353 -0.0636 0.3764 0.207 Uiso 1 1 calc R . .
H20B H 0.7515 -0.1131 0.3202 0.207 Uiso 1 1 calc R . .
C21 C 0.6627(6) -0.1252(6) 0.3579(6) 0.291(8) Uani 1 1 d . . .
H21A H 0.6278 -0.1041 0.3411 0.350 Uiso 1 1 calc R . .
H21B H 0.6644 -0.1647 0.3353 0.350 Uiso 1 1 calc R . .
C22 C 0.6590(8) -0.1312(12) 0.4068(9) 0.531(17) Uani 1 1 d . . .
H22A H 0.6612 -0.0924 0.4299 0.797 Uiso 1 1 calc R . .
H22B H 0.6905 -0.1570 0.4227 0.797 Uiso 1 1 calc R . .
H22C H 0.6217 -0.1502 0.4167 0.797 Uiso 1 1 calc R . .
C23 C 0.77956(16) 0.0329(2) 0.3053(2) 0.0913(12) Uani 1 1 d . . .
H23A H 0.8096 0.0581 0.2837 0.110 Uiso 1 1 calc R . .
H23B H 0.7993 0.0056 0.3373 0.110 Uiso 1 1 calc R . .
C24 C 0.7382(2) 0.0742(3) 0.3462(3) 0.145(2) Uani 1 1 d . . .
H24A H 0.7011 0.0537 0.3559 0.174 Uiso 1 1 calc R . .
H24B H 0.7302 0.1118 0.3213 0.174 Uiso 1 1 calc R . .
C25 C 0.7765(5) 0.0883(8) 0.4206(10) 0.52(2) Uani 1 1 d . . .
H25A H 0.7524 0.0979 0.4607 0.626 Uiso 1 1 calc R . .
H25B H 0.8077 0.0594 0.4312 0.626 Uiso 1 1 calc R . .
C26 C 0.7964(7) 0.1472(6) 0.3736(8) 0.477(17) Uani 1 1 d . . .
H26A H 0.7812 0.1425 0.3276 0.715 Uiso 1 1 d R . .
H26B H 0.8387 0.1495 0.3720 0.715 Uiso 1 1 d R . .
H26C H 0.7809 0.1841 0.3936 0.715 Uiso 1 1 d R . .
N5 N 0.7500 -0.00490(17) 0.2500 0.0730(11) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Fe1 C2 90.62(15) . .
C1 Fe1 C2 90.62(15) . 11_655
C2 Fe1 C2 90.13(17) . 11_655
C1 Fe1 C3 90.92(15) . .
C2 Fe1 C3 178.38(13) . .
C2 Fe1 C3 90.37(12) 11_655 .
C1 Fe1 C3 90.92(15) . 11_655
C2 Fe1 C3 90.37(12) . 11_655
C2 Fe1 C3 178.38(13) 11_655 11_655
C3 Fe1 C3 89.08(16) . 11_655
C1 Fe1 N1 179.16(18) . .
C2 Fe1 N1 88.79(11) . .
C2 Fe1 N1 88.79(11) 11_655 .
C3 Fe1 N1 89.68(11) . .
C3 Fe1 N1 89.68(11) 11_655 .
O1 C1 Fe1 179.9(5) . .
N2 C2 Fe1 178.8(3) . .
N3 C3 Fe1 179.7(3) . .
C15 N4 C7 105.2(3) . .
C15 N4 C11 110.9(2) . 11_655
C7 N4 C11 111.5(2) . 11_655
C15 N4 C11 110.9(2) . .
C7 N4 C11 111.5(2) . .
C11 N4 C11 106.9(3) 11_655 .
C4 N1 C4 117.0(4) 11_655 .
C4 N1 Fe1 121.45(19) 11_655 .
C4 N1 Fe1 121.45(19) . .
N1 C4 C5 122.1(4) . .
C6 C5 C4 120.5(4) . .
C5 C6 C5 117.9(5) . 11_655
N4 C7 C8 116.0(4) . .
C7 C8 C9 109.2(4) . .
C8 C9 C10 106.2(5) . 11_655
C8 C9 C10 106.2(5) . .
C10 C9 C10 133.5(11) 11_655 .
C12 C11 N4 115.7(3) . .
C13 C12 C11 112.6(4) . .
C14 C13 C12 115.6(7) . .
C16 C15 N4 115.6(4) . .
C15 C16 C17 111.0(5) . .
C18 C17 C16 135.3(8) . .
C20 C19 N5 114.6(3) . .
C19 C20 C21 106.0(5) . .
C22 C21 C20 113(2) . .
N5 C23 C24 114.9(3) . .
C23 C24 C25 103.5(5) . .
C26 C25 C24 79.3(12) . .
C19 N5 C19 112.8(4) . 4_655
C19 N5 C23 104.8(2) . 4_655
C19 N5 C23 110.6(2) 4_655 4_655
C19 N5 C23 110.6(2) . .
C19 N5 C23 104.8(2) 4_655 .
C23 N5 C23 113.5(4) 4_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C1 1.722(6) .
Fe1 C2 1.931(3) .
Fe1 C2 1.931(3) 11_655
Fe1 C3 1.933(3) .
Fe1 C3 1.933(3) 11_655
Fe1 N1 2.066(3) .
C1 O1 1.153(5) .
C2 N2 1.141(3) .
C3 N3 1.141(3) .
N4 C15 1.506(5) .
N4 C7 1.509(5) .
N4 C11 1.512(4) 11_655
N4 C11 1.512(4) .
N1 C4 1.328(3) 11_655
N1 C4 1.328(3) .
C4 C5 1.401(5) .
C5 C6 1.337(5) .
C6 C5 1.337(5) 11_655
C7 C8 1.516(6) .
C8 C9 1.533(9) .
C9 C10 1.756(15) 11_655
C9 C10 1.756(15) .
C11 C12 1.503(5) .
C12 C13 1.500(6) .
C13 C14 1.399(9) .
C15 C16 1.500(6) .
C16 C17 1.525(8) .
C17 C18 1.093(9) .
C19 C20 1.507(6) .
C19 N5 1.508(4) .
C20 C21 1.613(12) .
C21 C22 0.959(18) .
C23 N5 1.509(4) .
C23 C24 1.522(5) .
C24 C25 1.710(17) .
C25 C26 1.64(3) .
N5 C19 1.508(4) 4_655
N5 C23 1.509(4) 4_655
