#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322624.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_4322624
loop_
_publ_author_name
'Alain Diebold'
'Karl S. Hagen'
_publ_section_title
;
 Iron(II) Polyamine Chemistry: Variation of Spin State and Coordination
 Number in Solid State and Solution with Iron(II)
 Tris(2-pyridylmethyl)amine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              215
_journal_page_last               223
_journal_paper_doi               10.1021/ic971105e
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         '[Fe(TPA)2](BPh4)2'
_chemical_formula_sum            'C84 H76 B2 Fe N8'
_chemical_formula_weight         1275.00
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4890(10)
_cell_length_b                   14.1890(10)
_cell_length_c                   19.8430(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      4.57
_cell_volume                     3428.4(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5786
_diffrn_reflns_theta_max         56.73
_diffrn_reflns_theta_min         3.84
_diffrn_standards_decay_%        5.30
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  0.3110
_exptl_absorpt_correction_T_min  0.2324
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0032(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_obs          0.0494
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0495P)²+0.6403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1257
_refine_ls_wR_factor_obs         0.1090
_reflns_number_observed          3146
_reflns_number_total             4553
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971105e_5.cif
_cod_data_source_block           4-BPh4(AD1234c)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.6403P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.6403P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322624
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.0000 0.0000 0.0000 0.0602(3) Uani 1 d S .
N1 N 0.0599(2) -0.1367(2) 0.06826(13) 0.0509(7) Uani 1 d . .
N2 N -0.1471(2) -0.1133(2) -0.00530(13) 0.0552(7) Uani 1 d . .
N3 N 0.0634(2) 0.0368(2) 0.12479(14) 0.0591(8) Uani 1 d . .
N4 N 0.1575(2) -0.0862(2) -0.03493(13) 0.0593(8) Uani 1 d . .
C1 C -0.2441(3) -0.1146(3) -0.0514(2) 0.0650(10) Uani 1 d . .
H1A H -0.2538(3) -0.0727(3) -0.0883(2) 0.078 Uiso 1 calc R .
C2 C -0.3290(3) -0.1731(3) -0.0477(2) 0.0698(11) Uani 1 d . .
H2A H -0.3950(3) -0.1699(3) -0.0804(2) 0.084 Uiso 1 calc R .
C3 C -0.3146(3) -0.2369(3) 0.0054(2) 0.0710(11) Uani 1 d . .
H3A H -0.3704(3) -0.2786(3) 0.0091(2) 0.085 Uiso 1 calc R .
C4 C -0.2158(3) -0.2381(3) 0.0532(2) 0.0621(10) Uani 1 d . .
H4A H -0.2041(3) -0.2811(3) 0.0895(2) 0.075 Uiso 1 calc R .
C5 C -0.1349(3) -0.1756(2) 0.0468(2) 0.0500(8) Uani 1 d . .
C6 C -0.0301(3) -0.1696(2) 0.0994(2) 0.0577(9) Uani 1 d . .
H6A H -0.0388(3) -0.1265(2) 0.1358(2) 0.069 Uiso 1 calc R .
H6B H -0.0119(3) -0.2312(2) 0.1200(2) 0.069 Uiso 1 calc R .
C7 C 0.0440(3) 0.1156(3) 0.1578(2) 0.0690(11) Uani 1 d . .
H7A H -0.0025(3) 0.1608(3) 0.1329(2) 0.083 Uiso 1 calc R .
C8 C 0.0892(3) 0.1333(3) 0.2264(2) 0.0696(11) Uani 1 d . .
H8A H 0.0726(3) 0.1885(3) 0.2472(2) 0.084 Uiso 1 calc R .
C9 C 0.1593(3) 0.0679(3) 0.2638(2) 0.0672(11) Uani 1 d . .
H9A H 0.1910(3) 0.0781(3) 0.3102(2) 0.081 Uiso 1 calc R .
C10 C 0.1815(3) -0.0127(3) 0.2313(2) 0.0568(9) Uani 1 d . .
H10A H 0.2288(3) -0.0579(3) 0.2555(2) 0.068 Uiso 1 calc R .
C11 C 0.1327(3) -0.0262(2) 0.1622(2) 0.0503(9) Uani 1 d . .
C12 C 0.1549(3) -0.1122(2) 0.1244(2) 0.0586(9) Uani 1 d . .
H12A H 0.2187(3) -0.1015(2) 0.1050(2) 0.070 Uiso 1 calc R .
H12B H 0.1713(3) -0.1646(2) 0.1565(2) 0.070 Uiso 1 calc R .
C13 C 0.2226(3) -0.0549(3) -0.0761(2) 0.0725(11) Uani 1 d . .
H13A H 0.2189(3) 0.0087(3) -0.0879(2) 0.087 Uiso 1 calc R .
C14 C 0.2934(3) -0.1101(4) -0.1014(2) 0.0784(12) Uani 1 d . .
H14A H 0.3373(3) -0.0847(4) -0.1290(2) 0.094 Uiso 1 calc R .
C15 C 0.2985(4) -0.2048(4) -0.0851(2) 0.0893(14) Uani 1 d . .
H15A H 0.3449(4) -0.2449(4) -0.1024(2) 0.107 Uiso 1 calc R .
C16 C 0.2338(3) -0.2386(3) -0.0431(2) 0.0768(12) Uani 1 d . .
H16A H 0.2362(3) -0.3021(3) -0.0310(2) 0.092 Uiso 1 calc R .
C17 C 0.1652(3) -0.1777(2) -0.0189(2) 0.0543(9) Uani 1 d . .
C18 C 0.0904(3) -0.2118(2) 0.0256(2) 0.0621(10) Uani 1 d . .
H18A H 0.0243(3) -0.2378(2) -0.0037(2) 0.075 Uiso 1 calc R .
H18B H 0.1266(3) -0.2620(2) 0.0553(2) 0.075 Uiso 1 calc R .
B B -0.0664(3) 0.5087(3) 0.2103(2) 0.0450(9) Uani 1 d . .
C19 C -0.1950(3) 0.5040(2) 0.1696(2) 0.0486(8) Uani 1 d . .
C20 C -0.2290(3) 0.4990(3) 0.0976(2) 0.0734(11) Uani 1 d . .
H20A H -0.1760(3) 0.4947(3) 0.0713(2) 0.088 Uiso 1 calc R .
C21 C -0.3377(4) 0.5002(4) 0.0644(2) 0.108(2) Uani 1 d . .
H21A H -0.3566(4) 0.4964(4) 0.0164(2) 0.129 Uiso 1 calc R .
C22 C -0.4183(4) 0.5068(3) 0.1002(3) 0.097(2) Uani 1 d . .
H22A H -0.4917(4) 0.5083(3) 0.0769(3) 0.117 Uiso 1 calc R .
C23 C -0.3905(3) 0.5114(3) 0.1712(2) 0.0745(11) Uani 1 d . .
H23A H -0.4445(3) 0.5159(3) 0.1966(2) 0.089 Uiso 1 calc R .
C24 C -0.2804(3) 0.5091(2) 0.2041(2) 0.0591(9) Uani 1 d . .
H24A H -0.2625(3) 0.5112(2) 0.2521(2) 0.071 Uiso 1 calc R .
C25 C 0.0143(3) 0.4764(2) 0.15913(15) 0.0458(8) Uani 1 d . .
C26 C 0.0448(3) 0.5379(3) 0.1121(2) 0.0702(11) Uani 1 d . .
H26A H 0.0177(3) 0.5992(3) 0.1097(2) 0.084 Uiso 1 calc R .
C27 C 0.1128(4) 0.5134(3) 0.0688(2) 0.0850(13) Uani 1 d . .
H27A H 0.1310(4) 0.5580(3) 0.0389(2) 0.102 Uiso 1 calc R .
C28 C 0.1534(3) 0.4241(3) 0.0698(2) 0.0733(11) Uani 1 d . .
H28A H 0.1999(3) 0.4073(3) 0.0411(2) 0.088 Uiso 1 calc R .
C29 C 0.1242(3) 0.3598(3) 0.1139(2) 0.0646(10) Uani 1 d . .
H29A H 0.1500(3) 0.2982(3) 0.1147(2) 0.078 Uiso 1 calc R .
C30 C 0.0566(3) 0.3857(2) 0.1571(2) 0.0562(9) Uani 1 d . .
H30A H 0.0382(3) 0.3403(2) 0.1863(2) 0.067 Uiso 1 calc R .
C31 C -0.0350(3) 0.6176(2) 0.23617(14) 0.0425(8) Uani 1 d . .
C32 C 0.0751(3) 0.6470(2) 0.2549(2) 0.0530(9) Uani 1 d . .
H32A H 0.1295(3) 0.6041(2) 0.2507(2) 0.064 Uiso 1 calc R .
C33 C 0.1067(3) 0.7362(3) 0.2792(2) 0.0588(9) Uani 1 d . .
H33A H 0.1807(3) 0.7524(3) 0.2901(2) 0.071 Uiso 1 calc R .
C34 C 0.0289(3) 0.8010(2) 0.2875(2) 0.0612(10) Uani 1 d . .
H34A H 0.0495(3) 0.8606(2) 0.3052(2) 0.073 Uiso 1 calc R .
C35 C -0.0796(3) 0.7761(2) 0.2690(2) 0.0599(10) Uani 1 d . .
H35A H -0.1332(3) 0.8197(2) 0.2735(2) 0.072 Uiso 1 calc R .
C36 C -0.1107(3) 0.6868(2) 0.2436(2) 0.0503(8) Uani 1 d . .
H36A H -0.1851(3) 0.6725(2) 0.2311(2) 0.060 Uiso 1 calc R .
C37 C -0.0463(2) 0.4374(2) 0.2773(2) 0.0465(8) Uani 1 d . .
C38 C 0.0243(3) 0.4573(3) 0.3409(2) 0.0646(10) Uani 1 d . .
H38A H 0.0579(3) 0.5161(3) 0.3472(2) 0.078 Uiso 1 calc R .
C39 C 0.0463(3) 0.3933(4) 0.3950(2) 0.0853(13) Uani 1 d . .
H39A H 0.0929(3) 0.4100(4) 0.4367(2) 0.102 Uiso 1 calc R .
C40 C -0.0002(3) 0.3056(3) 0.3871(2) 0.0874(14) Uani 1 d . .
H40A H 0.0169(3) 0.2616(3) 0.4226(2) 0.105 Uiso 1 calc R .
C41 C -0.0723(3) 0.2830(3) 0.3266(2) 0.0783(12) Uani 1 d . .
H41A H -0.1061(3) 0.2242(3) 0.3213(2) 0.094 Uiso 1 calc R .
C42 C -0.0947(3) 0.3483(3) 0.2731(2) 0.0619(10) Uani 1 d . .
H42A H -0.1443(3) 0.3318(3) 0.2326(2) 0.074 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
_geom_angle_publ_flag
N1 Fe N1 180.0 3 . ?
N1 Fe N2 67.98(9) 3 3 ?
N1 Fe N2 112.02(9) . 3 ?
N1 Fe N2 112.02(9) 3 . ?
N1 Fe N2 67.98(9) . . ?
N2 Fe N2 180.0 3 . ?
N1 Fe N3 67.32(9) 3 3 ?
N1 Fe N3 112.68(9) . 3 ?
N2 Fe N3 104.67(9) 3 3 ?
N2 Fe N3 75.33(9) . 3 ?
N1 Fe N3 112.68(9) 3 . ?
N1 Fe N3 67.32(9) . . ?
N2 Fe N3 75.33(9) 3 . ?
N2 Fe N3 104.67(9) . . ?
N3 Fe N3 180.0 3 . ?
N1 Fe N4 113.59(9) 3 . ?
N1 Fe N4 66.41(9) . . ?
N2 Fe N4 72.91(9) 3 . ?
N2 Fe N4 107.09(9) . . ?
N3 Fe N4 73.83(9) 3 . ?
N3 Fe N4 106.17(9) . . ?
N1 Fe N4 66.41(9) 3 3 ?
N1 Fe N4 113.59(9) . 3 ?
N2 Fe N4 107.09(9) 3 3 ?
N2 Fe N4 72.91(9) . 3 ?
N3 Fe N4 106.17(9) 3 3 ?
N3 Fe N4 73.83(9) . 3 ?
N4 Fe N4 180.0 . 3 ?
C18 N1 C12 109.8(3) . . ?
C18 N1 C6 109.4(3) . . ?
C12 N1 C6 108.6(2) . . ?
C18 N1 Fe 110.6(2) . . ?
C12 N1 Fe 109.6(2) . . ?
C6 N1 Fe 108.9(2) . . ?
C5 N2 C1 116.4(3) . . ?
C5 N2 Fe 116.6(2) . . ?
C1 N2 Fe 126.7(2) . . ?
C11 N3 C7 116.5(3) . . ?
C11 N3 Fe 115.7(2) . . ?
C7 N3 Fe 127.5(2) . . ?
C17 N4 C13 116.3(3) . . ?
C17 N4 Fe 115.0(2) . . ?
C13 N4 Fe 127.9(3) . . ?
N2 C1 C2 124.5(3) . . ?
C1 C2 C3 118.2(4) . . ?
C2 C3 C4 118.8(4) . . ?
C5 C4 C3 119.5(3) . . ?
N2 C5 C4 122.5(3) . . ?
N2 C5 C6 115.8(3) . . ?
C4 C5 C6 121.6(3) . . ?
N1 C6 C5 111.0(3) . . ?
N3 C7 C8 123.7(4) . . ?
C9 C8 C7 118.9(4) . . ?
C10 C9 C8 118.8(3) . . ?
C9 C10 C11 119.4(3) . . ?
N3 C11 C10 122.8(3) . . ?
N3 C11 C12 115.8(3) . . ?
C10 C11 C12 121.5(3) . . ?
N1 C12 C11 111.3(3) . . ?
N4 C13 C14 124.3(4) . . ?
C13 C14 C15 118.4(4) . . ?
C16 C15 C14 118.7(4) . . ?
C15 C16 C17 119.3(4) . . ?
N4 C17 C16 123.1(3) . . ?
N4 C17 C18 115.6(3) . . ?
C16 C17 C18 121.3(3) . . ?
N1 C18 C17 112.4(3) . . ?
C19 B C37 109.4(3) . . ?
C19 B C31 109.4(3) . . ?
C37 B C31 110.0(2) . . ?
C19 B C25 110.7(2) . . ?
C37 B C25 108.9(3) . . ?
C31 B C25 108.5(3) . . ?
C24 C19 C20 114.4(3) . . ?
C24 C19 B 122.1(3) . . ?
C20 C19 B 123.4(3) . . ?
C21 C20 C19 122.2(4) . . ?
C22 C21 C20 121.4(4) . . ?
C21 C22 C23 119.4(4) . . ?
C22 C23 C24 118.7(4) . . ?
C23 C24 C19 123.9(4) . . ?
C26 C25 C30 113.4(3) . . ?
C26 C25 B 122.4(3) . . ?
C30 C25 B 124.2(3) . . ?
C27 C26 C25 123.9(4) . . ?
C28 C27 C26 120.3(4) . . ?
C27 C28 C29 118.6(4) . . ?
C28 C29 C30 120.4(4) . . ?
C29 C30 C25 123.5(3) . . ?
C36 C31 C32 114.2(3) . . ?
C36 C31 B 125.0(3) . . ?
C32 C31 B 120.7(3) . . ?
C33 C32 C31 123.5(3) . . ?
C34 C33 C32 120.0(3) . . ?
C35 C34 C33 118.7(3) . . ?
C34 C35 C36 120.9(3) . . ?
C35 C36 C31 122.7(3) . . ?
C42 C37 C38 114.4(3) . . ?
C42 C37 B 121.6(3) . . ?
C38 C37 B 123.9(3) . . ?
C39 C38 C37 123.0(4) . . ?
C40 C39 C38 120.1(4) . . ?
C41 C40 C39 119.6(4) . . ?
C40 C41 C42 119.7(4) . . ?
C41 C42 C37 123.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe N1 2.389(3) 3 ?
Fe N1 2.389(3) . ?
Fe N2 2.426(3) 3 ?
Fe N2 2.426(3) . ?
Fe N3 2.482(3) 3 ?
Fe N3 2.482(3) . ?
Fe N4 2.540(3) . ?
Fe N4 2.540(3) 3 ?
N1 C18 1.464(4) . ?
N1 C12 1.477(4) . ?
N1 C6 1.475(4) . ?
N2 C5 1.342(4) . ?
N2 C1 1.347(4) . ?
N3 C11 1.346(4) . ?
N3 C7 1.346(4) . ?
N4 C17 1.336(4) . ?
N4 C13 1.349(4) . ?
C1 C2 1.361(5) . ?
C2 C3 1.371(5) . ?
C3 C4 1.379(5) . ?
C4 C5 1.372(4) . ?
C5 C6 1.484(4) . ?
C7 C8 1.376(5) . ?
C8 C9 1.374(5) . ?
C9 C10 1.370(5) . ?
C10 C11 1.385(4) . ?
C11 C12 1.491(4) . ?
C13 C14 1.358(5) . ?
C14 C15 1.381(6) . ?
C15 C16 1.371(5) . ?
C16 C17 1.376(5) . ?
C17 C18 1.501(4) . ?
B C19 1.631(5) . ?
B C37 1.644(5) . ?
B C31 1.649(5) . ?
B C25 1.646(5) . ?
C19 C24 1.392(4) . ?
C19 C20 1.399(5) . ?
C20 C21 1.371(6) . ?
C21 C22 1.359(6) . ?
C22 C23 1.376(6) . ?
C23 C24 1.385(5) . ?
C25 C26 1.391(4) . ?
C25 C30 1.396(4) . ?
C26 C27 1.379(5) . ?
C27 C28 1.363(5) . ?
C28 C29 1.369(5) . ?
C29 C30 1.380(4) . ?
C31 C36 1.393(4) . ?
C31 C32 1.406(4) . ?
C32 C33 1.380(4) . ?
C33 C34 1.374(5) . ?
C34 C35 1.369(5) . ?
C35 C36 1.387(4) . ?
C37 C42 1.396(4) . ?
C37 C38 1.399(4) . ?
C38 C39 1.386(5) . ?
C39 C40 1.368(6) . ?
C40 C41 1.370(5) . ?
C41 C42 1.389(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139134673
