#------------------------------------------------------------------------------
#$Date: 2021-03-05 04:05:22 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262645 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/63/7706388.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_7706388
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 K4 N6 O3 Os'
_chemical_formula_sum            'C6 H6 K4 N6 O3 Os'
_chemical_formula_weight         556.77
_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             2019-08-09T12:58:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-08-09 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4865(3)
_cell_length_b                   17.0659(6)
_cell_length_c                   9.4952(3)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      3.21
_cell_volume                     1537.23(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0091
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            40475
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.39
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'numerical from crystal shape'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.018
_refine_ls_R_factor_gt           0.0172
_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)+(0.0343P)²+4.2596P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0
_reflns_number_gt                1525
_reflns_number_total             1576
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt04155f2.cif
_cod_data_source_block           k4[os(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               7706388
_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
Os Os 0 0.17800(2) 0.25 0.01483(9) Uani 1 2 d S T P . .
K1 K 0.59987(9) 0.14386(6) 0.43888(9) 0.0275(2) Uani 1 1 d . . . . .
K2 K 0.31486(9) 0.35802(6) 0.34625(9) 0.0282(2) Uani 1 1 d . . . . .
C1 C 0 0.0581(3) 0.25 0.0232(11) Uani 1 2 d S T P . .
N1 N 0 -0.0094(4) 0.25 0.0455(16) Uani 1 2 d S T P . .
C2 C 0 0.2995(3) 0.25 0.0137(10) Uani 1 2 d S T P . .
N2 N 0 0.3640(3) 0.25 0.0294(11) Uani 1 2 d S T P . .
C3 C 0.0723(4) 0.17812(18) 0.0475(4) 0.0144(7) Uani 1 1 d . . . . .
N3 N 0.1136(4) 0.1787(2) -0.0669(4) 0.0258(8) Uani 1 1 d . . . . .
C4 C 0.2021(4) 0.17730(19) 0.3241(4) 0.0152(7) Uani 1 1 d . . . . .
N4 N 0.3165(4) 0.1762(2) 0.3663(4) 0.0284(9) Uani 1 1 d . . . . .
O1 O 0.2416(6) -0.0026(3) 0.4857(6) 0.0773(16) Uani 1 1 d . . . . .
H1A H 0.173905 -0.036128 0.440688 0.116 Uiso 1 1 d R U . . .
H1B H 0.229149 0.047354 0.440817 0.116 Uiso 1 1 d R U . . .
O2 O 0.4609(9) 0.0293(4) 0.2777(11) 0.055(2) Uani 0.50(1) 1 d . . P . .
H2A H 0.499999 -0.020267 0.25 0.083 Uiso 1 2 d R U P . .
H2B H 0.362217 0.024722 0.256696 0.083 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
Os Os -1.2165 7.603 '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
C4 Os C4 179.33(18) 2 . ?
C4 Os C3 89.56(15) 2 . ?
C4 Os C3 90.44(15) . . ?
C4 Os C3 90.44(15) 2 2 ?
C4 Os C3 89.56(15) . 2 ?
C3 Os C3 179.89(18) . 2 ?
C4 Os C1 89.66(9) 2 . ?
C4 Os C1 89.66(9) . . ?
C3 Os C1 90.06(9) . . ?
C3 Os C1 90.06(9) 2 . ?
C4 Os C2 90.34(9) 2 . ?
C4 Os C2 90.34(9) . . ?
C3 Os C2 89.94(9) . . ?
C3 Os C2 89.94(9) 2 . ?
C1 Os C2 180 . . ?
O2 K1 N4 63.77(18) . . ?
O2 K1 O2 18.3(3) . 2_655 ?
N4 K1 O2 76.73(19) . 2_655 ?
O2 K1 O1 78.5(2) . 5_656 ?
N4 K1 O1 135.02(13) . 5_656 ?
O2 K1 O1 73.7(2) 2_655 5_656 ?
O2 K1 N3 134.9(2) . 8_556 ?
N4 K1 N3 80.89(11) . 8_556 ?
O2 K1 N3 132.09(19) 2_655 8_556 ?
O1 K1 N3 143.54(12) 5_656 8_556 ?
O2 K1 N3 140.68(18) . 2_655 ?
N4 K1 N3 155.47(11) . 2_655 ?
O2 K1 N3 126.45(18) 2_655 2_655 ?
O1 K1 N3 66.68(12) 5_656 2_655 ?
N3 K1 N3 76.88(11) 8_556 2_655 ?
O2 K1 N4 74.43(19) . 2_655 ?
N4 K1 N4 88.95(12) . 2_655 ?
O2 K1 N4 60.00(18) 2_655 2_655 ?
O1 K1 N4 104.27(14) 5_656 2_655 ?
N3 K1 N4 77.95(10) 8_556 2_655 ?
N3 K1 N4 96.37(11) 2_655 2_655 ?
O2 K1 N2 110.1(2) . 7_556 ?
N4 K1 N2 87.08(9) . 7_556 ?
O2 K1 N2 125.85(19) 2_655 7_556 ?
O1 K1 N2 83.64(15) 5_656 7_556 ?
N3 K1 N2 94.22(13) 8_556 7_556 ?
N3 K1 N2 84.36(8) 2_655 7_556 ?
N4 K1 N2 171.70(13) 2_655 7_556 ?
N3 K2 O1 137.09(13) 7 7_556 ?
N3 K2 N1 74.87(10) 7 3 ?
O1 K2 N1 69.28(13) 7_556 3 ?
N3 K2 N3 89.05(12) 7 8_556 ?
O1 K2 N3 101.23(12) 7_556 8_556 ?
N1 K2 N3 71.97(9) 3 8_556 ?
N3 K2 N4 154.06(11) 7 7_556 ?
O1 K2 N4 66.87(13) 7_556 7_556 ?
N1 K2 N4 130.82(9) 3 7_556 ?
N3 K2 N4 95.77(11) 8_556 7_556 ?
N3 K2 N4 80.44(11) 7 . ?
O1 K2 N4 142.43(13) 7_556 . ?
N1 K2 N4 140.05(11) 3 . ?
N3 K2 N4 76.78(10) 8_556 . ?
N4 K2 N4 75.94(12) 7_556 . ?
N3 K2 N2 87.90(9) 7 . ?
O1 K2 N2 87.55(13) 7_556 . ?
N1 K2 N2 116.43(10) 3 . ?
N3 K2 N2 169.84(13) 8_556 . ?
N4 K2 N2 82.91(8) 7_556 . ?
N4 K2 N2 93.16(13) . . ?
N1 C1 Os 180 . . ?
C1 N1 K2 138.80(8) . 3_445 ?
C1 N1 K2 138.80(8) . 4_545 ?
K2 N1 K2 82.41(16) 3_445 4_545 ?
N2 C2 Os 180 . . ?
C2 N2 K1 87.53(11) . 8_455 ?
C2 N2 K1 87.53(11) . 7_556 ?
K1 N2 K1 175.1(2) 8_455 7_556 ?
C2 N2 K2 88.14(11) . 2 ?
K1 N2 K2 90.76(2) 8_455 2 ?
K1 N2 K2 89.08(2) 7_556 2 ?
C2 N2 K2 88.13(11) . . ?
K1 N2 K2 89.08(2) 8_455 . ?
K1 N2 K2 90.76(2) 7_556 . ?
K2 N2 K2 176.3(2) 2 . ?
N3 C3 Os 179.5(3) . . ?
C3 N3 K2 165.6(3) . 7 ?
C3 N3 K2 86.3(3) . 8_455 ?
K2 N3 K2 85.64(10) 7 8_455 ?
C3 N3 K1 88.7(2) . 8_455 ?
K2 N3 K1 104.51(12) 7 8_455 ?
K2 N3 K1 99.91(11) 8_455 8_455 ?
C3 N3 K1 85.8(3) . 2_655 ?
K2 N3 K1 96.73(12) 7 2_655 ?
K2 N3 K1 155.43(13) 8_455 2_655 ?
K1 N3 K1 103.12(11) 8_455 2_655 ?
N4 C4 Os 179.4(3) . . ?
C4 N4 K1 168.2(3) . . ?
C4 N4 K1 85.4(3) . 2_655 ?
K1 N4 K1 87.02(11) . 2_655 ?
C4 N4 K2 85.9(3) . 7_556 ?
K1 N4 K2 97.69(12) . 7_556 ?
K1 N4 K2 156.72(14) 2_655 7_556 ?
C4 N4 K2 87.6(3) . . ?
K1 N4 K2 102.37(12) . . ?
K1 N4 K2 97.09(11) 2_655 . ?
K2 N4 K2 104.06(12) 7_556 . ?
K1 O1 K2 129.89(17) 5_656 7_556 ?
K1 O2 K1 90.5(2) . 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
Os C4 2.041(4) 2 ?
Os C4 2.041(4) . ?
Os C3 2.043(4) . ?
Os C3 2.043(4) 2 ?
Os C1 2.046(6) . ?
Os C2 2.073(6) . ?
K1 O2 2.810(9) . ?
K1 N4 2.828(4) . ?
K1 O2 2.895(9) 2_655 ?
K1 O1 2.930(5) 5_656 ?
K1 N3 3.032(4) 8_556 ?
K1 N3 3.035(4) 2_655 ?
K1 N4 3.056(4) 2_655 ?
K1 N2 3.1067(9) 7_556 ?
K2 N3 2.809(4) 7 ?
K2 O1 2.987(5) 7_556 ?
K2 N1 3.008(5) 3 ?
K2 N3 3.016(4) 8_556 ?
K2 N4 3.059(4) 7_556 ?
K2 N4 3.109(4) . ?
K2 N2 3.1239(9) . ?
C1 N1 1.152(9) . ?
C2 N2 1.101(8) . ?
C3 N3 1.155(6) . ?
C4 N4 1.157(6) . ?
