#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:05:22 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262645 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/63/7706386.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_7706386
loop_
_publ_author_name
'Fujii, Susumu'
'Ohtani, Ryo'
'Kuwabara, Akihide'
_publ_section_title
;
 Theoretical investigation of tetrahedral distortion of four-coordinate
 iron(II) centres in FePd(CN)₄.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1990
_journal_page_last               1994
_journal_paper_doi               10.1039/d0dt04155f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C6 H6 Fe K4 N6 O3'
_chemical_formula_sum            'C6 H6 Fe K4 N6 O3'
_chemical_formula_weight         422.42
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-01T15:53:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-07-01 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3940(4)
_cell_length_b                   16.8754(8)
_cell_length_c                   9.3975(4)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      3.24
_cell_volume                     1489.76(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25859
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'numerical from crystal shape'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0896P)²+0.5254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0
_reflns_number_gt                966
_reflns_number_total             1524
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04155f2.cif
_cod_data_source_block           k4[fe(cn)6]3h2o
_cod_depositor_comments
'Adding full bibliography for 7706383--7706389.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7706386
_shelx_shelxl_version_number     2018/3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0 0.17730(4) 0.25 0.0167(3) Uani 1 2 d S T P . .
K1 K 0.59677(10) 0.14402(5) 0.43894(10) 0.0328(3) Uani 1 1 d . . . . .
K2 K 0.31405(10) 0.35847(6) 0.34362(10) 0.0340(3) Uani 1 1 d . . . . .
C1 C 0 0.0637(3) 0.25 0.0285(12) Uani 1 2 d S T P . .
N1 N 0 -0.0055(3) 0.25 0.0435(14) Uani 1 2 d S T P . .
C2 C 0 0.2920(3) 0.25 0.0203(10) Uani 1 2 d S T P . .
N2 N 0 0.3580(3) 0.25 0.0318(12) Uani 1 2 d S T P . .
C3 C 0.0680(4) 0.17748(18) 0.0576(4) 0.0217(8) Uani 1 1 d . . . . .
N3 N 0.1093(4) 0.1775(2) -0.0603(4) 0.0337(9) Uani 1 1 d . . . . .
C4 C 0.1927(4) 0.17690(18) 0.3187(4) 0.0215(7) Uani 1 1 d . . . . .
N4 N 0.3086(4) 0.1752(2) 0.3612(4) 0.0360(10) Uani 1 1 d . . . . .
O1 O 0.2430(5) -0.0021(2) 0.4849(7) 0.0827(18) Uani 1 1 d . . . . .
H1A H 0.261923 -0.03382 0.402306 0.124 Uiso 1 1 d R U . . .
H1B H 0.148848 0.018457 0.469909 0.124 Uiso 1 1 d R U . . .
O2 O 0.4661(10) 0.0282(3) 0.2803(11) 0.056(3) Uani 0.50(1) 1 d . . P . .
H2A H 0.500001 -0.022765 0.250003 0.084 Uiso 1 2 d R U P . .
H2B H 0.366943 0.028549 0.255488 0.084 Uiso 0.50(1) 1 d R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
C1 Fe C3 90.09(9) . 2 ?
C1 Fe C3 90.10(9) . . ?
C3 Fe C3 179.81(18) 2 . ?
C1 Fe C4 89.80(9) . . ?
C3 Fe C4 89.83(16) 2 . ?
C3 Fe C4 90.17(16) . . ?
C1 Fe C4 89.80(9) . 2 ?
C3 Fe C4 90.17(16) 2 2 ?
C3 Fe C4 89.83(16) . 2 ?
C4 Fe C4 179.60(19) . 2 ?
C1 Fe C2 180 . . ?
C3 Fe C2 89.91(9) 2 . ?
C3 Fe C2 89.90(9) . . ?
C4 Fe C2 90.20(9) . . ?
C4 Fe C2 90.20(9) 2 . ?
O2 K1 N4 64.4(2) . . ?
O2 K1 O2 17.1(3) . 2_655 ?
N4 K1 O2 75.5(2) . 2_655 ?
O2 K1 O1 77.3(2) . 5_656 ?
N4 K1 O1 134.74(13) . 5_656 ?
O2 K1 O1 74.1(2) 2_655 5_656 ?
O2 K1 N4 75.4(2) . 2_655 ?
N4 K1 N4 90.47(12) . 2_655 ?
O2 K1 N4 60.76(17) 2_655 2_655 ?
O1 K1 N4 102.79(16) 5_656 2_655 ?
O2 K1 N3 136.9(2) . 8_556 ?
N4 K1 N3 81.55(11) . 8_556 ?
O2 K1 N3 133.08(17) 2_655 8_556 ?
O1 K1 N3 143.08(10) 5_656 8_556 ?
N4 K1 N3 79.37(11) 2_655 8_556 ?
O2 K1 N3 137.9(2) . 2_655 ?
N4 K1 N3 157.43(13) . 2_655 ?
O2 K1 N3 125.2(2) 2_655 2_655 ?
O1 K1 N3 65.93(11) 5_656 2_655 ?
N4 K1 N3 92.89(11) 2_655 2_655 ?
N3 K1 N3 77.17(11) 8_556 2_655 ?
O2 K1 N2 112.18(19) . 7_556 ?
N4 K1 N2 87.98(9) . 7_556 ?
O2 K1 N2 127.62(17) 2_655 7_556 ?
O1 K1 N2 84.85(16) 5_656 7_556 ?
N4 K1 N2 170.52(11) 2_655 7_556 ?
N3 K1 N2 91.16(12) 8_556 7_556 ?
N3 K1 N2 85.05(8) 2_655 7_556 ?
N3 K2 O1 137.36(14) 7 7_556 ?
N3 K2 N3 90.24(10) 7 8_556 ?
O1 K2 N3 99.82(11) 7_556 8_556 ?
N3 K2 N1 74.99(10) 7 3 ?
O1 K2 N1 68.92(13) 7_556 3 ?
N3 K2 N1 72.81(9) 8_556 3 ?
N3 K2 N4 155.72(13) 7 7_556 ?
O1 K2 N4 65.80(14) 7_556 7_556 ?
N3 K2 N4 92.17(10) 8_556 7_556 ?
N1 K2 N4 128.65(9) 3 7_556 ?
N3 K2 N2 88.55(8) 7 . ?
O1 K2 N2 89.10(12) 7_556 . ?
N3 K2 N2 167.99(12) 8_556 . ?
N1 K2 N2 118.28(9) 3 . ?
N4 K2 N2 84.13(7) 7_556 . ?
N3 K2 N4 80.78(11) 7 . ?
O1 K2 N4 141.79(13) 7_556 . ?
N3 K2 N4 78.21(10) 8_556 . ?
N1 K2 N4 141.74(10) 3 . ?
N4 K2 N4 76.09(13) 7_556 . ?
N2 K2 N4 89.80(11) . . ?
N1 C1 Fe 180 . . ?
C1 N1 K2 139.57(6) . 3_445 ?
C1 N1 K2 139.57(6) . 4_545 ?
K2 N1 K2 80.86(13) 3_445 4_545 ?
N2 C2 Fe 180 . . ?
C2 N2 K1 89.37(9) . 8_455 ?
C2 N2 K1 89.37(9) . 7_556 ?
K1 N2 K1 178.74(18) 8_455 7_556 ?
C2 N2 K2 90.16(9) . . ?
K1 N2 K2 89.33(2) 8_455 . ?
K1 N2 K2 90.68(2) 7_556 . ?
C2 N2 K2 90.16(9) . 2 ?
K1 N2 K2 90.68(2) 8_455 2 ?
K1 N2 K2 89.33(2) 7_556 2 ?
K2 N2 K2 179.69(19) . 2 ?
N3 C3 Fe 179.8(4) . . ?
C3 N3 K2 166.9(3) . 7 ?
C3 N3 K2 88.8(3) . 8_455 ?
K2 N3 K2 84.72(9) 7 8_455 ?
C3 N3 K1 89.4(3) . 8_455 ?
K2 N3 K1 102.86(12) 7 8_455 ?
K2 N3 K1 99.61(11) 8_455 8_455 ?
C3 N3 K1 86.9(2) . 2_655 ?
K2 N3 K1 94.69(13) 7 2_655 ?
K2 N3 K1 157.09(15) 8_455 2_655 ?
K1 N3 K1 102.84(11) 8_455 2_655 ?
N4 C4 Fe 178.7(3) . . ?
C4 N4 K1 169.5(3) . . ?
C4 N4 K1 87.7(3) . 2_655 ?
K1 N4 K1 85.81(12) . 2_655 ?
C4 N4 K2 87.9(3) . 7_556 ?
K1 N4 K2 95.21(10) . 7_556 ?
K1 N4 K2 158.58(16) 2_655 7_556 ?
C4 N4 K2 88.5(3) . . ?
K1 N4 K2 100.50(12) . . ?
K1 N4 K2 96.90(12) 2_655 . ?
K2 N4 K2 103.91(13) 7_556 . ?
K1 O1 K2 129.21(19) 5_656 7_556 ?
K1 O2 K1 89.81(17) . 2_655 ?
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 C1 1.917(5) . ?
Fe C3 1.918(4) 2 ?
Fe C3 1.918(4) . ?
Fe C4 1.922(4) . ?
Fe C4 1.922(4) 2 ?
Fe C2 1.936(5) . ?
K1 O2 2.748(9) . ?
K1 N4 2.853(3) . ?
K1 O2 2.901(9) 2_655 ?
K1 O1 2.918(4) 5_656 ?
K1 N4 3.004(4) 2_655 ?
K1 N3 3.014(4) 8_556 ?
K1 N3 3.041(4) 2_655 ?
K1 N2 3.0616(10) 7_556 ?
K2 N3 2.825(4) 7 ?
K2 O1 2.959(5) 7_556 ?
K2 N3 2.979(4) 8_556 ?
K2 N1 3.016(4) 3 ?
K2 N4 3.057(5) 7_556 ?
K2 N2 3.0784(9) . ?
K2 N4 3.097(4) . ?
C1 N1 1.168(7) . ?
C2 N2 1.113(8) . ?
C3 N3 1.174(6) . ?
C4 N4 1.159(5) . ?
