#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:06:14 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224413 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048783.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_7048783
loop_
_publ_author_name
'Liu, Pai-Heng'
'Tsai, Fu-Te'
'Chen, Bo-Hao'
'Hsu, I-Jui'
'Hsieh, Hung-Hsi'
'Liaw, Wen-Feng'
_publ_section_title
;
 Insight into chalcogenolate-bound {Fe(NO)₂}⁹
 dinitrosyl iron complexes (DNICs): covalent character versus ionic
 character.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6040
_journal_page_last               6050
_journal_paper_doi               10.1039/c8dt04670k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C13 H27 Fe K N2 O9'
_chemical_formula_weight         450.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-09-05 deposited with the CCDC.
2019-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.071(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8963(15)
_cell_length_b                   8.4665(9)
_cell_length_c                   20.035(2)
_cell_measurement_reflns_used    4352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3899
_cell_measurement_theta_min      2.9532
_cell_volume                     2017.6(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_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  0.0979
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4085
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         1.712
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_correction_T_min  0.5852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Lump
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0667P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3246
_reflns_number_total             4085
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04670k2.cif
_cod_data_source_block           twin5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048782--7048783.cif.
;
_cod_original_cell_volume        2017.5(4)
_cod_database_code               7048783
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.61424(3) 0.45557(5) 0.53685(2) 0.01883(16) Uani 1 1 d . .
K1 K 0.78480(5) 0.70324(7) 0.71122(3) 0.01971(19) Uani 1 1 d . .
N1 N 0.62590(18) 0.4667(3) 0.61886(10) 0.0220(6) Uani 1 1 d . .
N2 N 0.72206(18) 0.3840(3) 0.49576(10) 0.0212(5) Uani 1 1 d . .
O1 O 0.64736(16) 0.4651(3) 0.67887(9) 0.0298(5) Uani 1 1 d . .
O2 O 0.80736(15) 0.3170(2) 0.47813(9) 0.0287(5) Uani 1 1 d . .
O3 O 0.47182(14) 0.3601(2) 0.50041(9) 0.0200(4) Uani 1 1 d . .
O4 O 0.95053(15) 0.6694(2) 0.61041(8) 0.0187(4) Uani 1 1 d . .
O5 O 0.80427(15) 0.9252(2) 0.61203(9) 0.0224(5) Uani 1 1 d . .
O6 O 0.70327(15) 1.0154(2) 0.73121(9) 0.0249(5) Uani 1 1 d . .
O7 O 0.68256(16) 0.7834(2) 0.82869(9) 0.0264(5) Uani 1 1 d . .
O8 O 0.82001(15) 0.5153(2) 0.82876(9) 0.0238(5) Uani 1 1 d . .
O9 O 0.91984(14) 0.4352(2) 0.70631(8) 0.0188(4) Uani 1 1 d . .
C1 C 0.4747(2) 0.2161(4) 0.46572(15) 0.0320(7) Uani 1 1 d . .
H1A H 0.5129 0.2311 0.4233 0.048 Uiso 1 1 calc R U
H1B H 0.3977 0.1793 0.4570 0.048 Uiso 1 1 calc R U
H1C H 0.5154 0.1374 0.4927 0.048 Uiso 1 1 calc R U
C2 C 0.9161(2) 0.7487(4) 0.55033(12) 0.0226(7) Uani 1 1 d . .
H2A H 0.8472 0.6987 0.5316 0.027 Uiso 1 1 calc R U
H2B H 0.9760 0.7407 0.5168 0.027 Uiso 1 1 calc R U
C3 C 0.8937(2) 0.9183(3) 0.56580(13) 0.0242(7) Uani 1 1 d . .
H3A H 0.9620 0.9681 0.5853 0.029 Uiso 1 1 calc R U
H3B H 0.8725 0.9758 0.5244 0.029 Uiso 1 1 calc R U
C4 C 0.7643(3) 1.0820(4) 0.62237(15) 0.0357(8) Uani 1 1 d . .
H4A H 0.7420 1.1306 0.5792 0.043 Uiso 1 1 calc R U
H4B H 0.8242 1.1476 0.6433 0.043 Uiso 1 1 calc R U
C5 C 0.6646(3) 1.0730(4) 0.66737(14) 0.0351(8) Uani 1 1 d . .
H5A H 0.6304 1.1789 0.6723 0.042 Uiso 1 1 calc R U
H5B H 0.6072 1.0008 0.6481 0.042 Uiso 1 1 calc R U
C6 C 0.6150(2) 1.0176(4) 0.77865(14) 0.0292(7) Uani 1 1 d . .
H6A H 0.5494 0.9580 0.7609 0.035 Uiso 1 1 calc R U
H6B H 0.5911 1.1279 0.7868 0.035 Uiso 1 1 calc R U
C7 C 0.6557(2) 0.9454(4) 0.84175(14) 0.0284(7) Uani 1 1 d . .
H7A H 0.7233 1.0020 0.8587 0.034 Uiso 1 1 calc R U
H7B H 0.5968 0.9520 0.8759 0.034 Uiso 1 1 calc R U
C8 C 0.7076(3) 0.6980(4) 0.88836(13) 0.0334(8) Uani 1 1 d . .
H8A H 0.6452 0.7086 0.9200 0.040 Uiso 1 1 calc R U
H8B H 0.7769 0.7401 0.9100 0.040 Uiso 1 1 calc R U
C9 C 0.7236(2) 0.5286(4) 0.87006(14) 0.0322(8) Uani 1 1 d . .
H9A H 0.7345 0.4643 0.9109 0.039 Uiso 1 1 calc R U
H9B H 0.6561 0.4890 0.8457 0.039 Uiso 1 1 calc R U
C10 C 0.8386(2) 0.3557(4) 0.80847(13) 0.0238(7) Uani 1 1 d . .
H10A H 0.7731 0.3167 0.7821 0.029 Uiso 1 1 calc R U
H10B H 0.8487 0.2872 0.8482 0.029 Uiso 1 1 calc R U
C11 C 0.9423(2) 0.3510(3) 0.76691(12) 0.0207(6) Uani 1 1 d . .
H11A H 1.0061 0.4004 0.7915 0.025 Uiso 1 1 calc R U
H11B H 0.9624 0.2402 0.7569 0.025 Uiso 1 1 calc R U
C12 C 1.0126(2) 0.4307(3) 0.66236(12) 0.0201(6) Uani 1 1 d . .
H12A H 1.0352 0.3199 0.6543 0.024 Uiso 1 1 calc R U
H12B H 1.0775 0.4875 0.6825 0.024 Uiso 1 1 calc R U
C13 C 0.9778(2) 0.5074(3) 0.59799(12) 0.0216(6) Uani 1 1 d . .
H13A H 1.0399 0.5010 0.5658 0.026 Uiso 1 1 calc R U
H13B H 0.9117 0.4521 0.5785 0.026 Uiso 1 1 calc R U
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'
K K 0.2009 0.2494 '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
N1 Fe1 N2 117.77(11) . .
N1 Fe1 O3 116.18(9) . .
N2 Fe1 O3 109.25(9) . .
N1 Fe1 O3 111.07(10) . 3_666
N2 Fe1 O3 119.75(9) . 3_666
O3 Fe1 O3 75.87(9) . 3_666
O1 K1 O5 113.61(6) . .
O1 K1 O7 96.62(6) . .
O5 K1 O7 119.60(6) . .
O1 K1 O9 74.14(6) . .
O5 K1 O9 118.39(5) . .
O7 K1 O9 119.70(6) . .
O1 K1 O6 121.80(6) . .
O5 K1 O6 60.02(5) . .
O7 K1 O6 59.59(6) . .
O9 K1 O6 163.86(6) . .
O1 K1 O4 100.37(6) . .
O5 K1 O4 59.32(5) . .
O7 K1 O4 161.51(6) . .
O9 K1 O4 59.20(5) . .
O6 K1 O4 115.67(6) . .
O1 K1 O8 81.93(6) . .
O5 K1 O8 163.90(6) . .
O7 K1 O8 59.66(6) . .
O9 K1 O8 60.05(5) . .
O6 K1 O8 116.41(6) . .
O4 K1 O8 115.59(5) . .
O1 K1 C11 149.72(7) . 2_756
O5 K1 C11 75.85(6) . 2_756
O7 K1 C11 103.20(6) . 2_756
O9 K1 C11 76.19(6) . 2_756
O6 K1 C11 88.18(6) . 2_756
O4 K1 C11 58.30(5) . 2_756
O8 K1 C11 88.55(6) . 2_756
O1 N1 Fe1 171.8(2) . .
O2 N2 Fe1 166.43(19) . .
N1 O1 K1 110.23(16) . .
C1 O3 Fe1 120.19(16) . .
C1 O3 Fe1 120.59(17) . 3_666
Fe1 O3 Fe1 104.13(9) . 3_666
C2 O4 C13 111.43(19) . .
C2 O4 K1 110.87(14) . .
C13 O4 K1 112.33(14) . .
C3 O5 C4 112.8(2) . .
C3 O5 K1 121.09(15) . .
C4 O5 K1 119.91(15) . .
C6 O6 C5 111.1(2) . .
C6 O6 K1 111.24(17) . .
C5 O6 K1 107.12(16) . .
C8 O7 C7 112.1(2) . .
C8 O7 K1 120.23(16) . .
C7 O7 K1 119.69(15) . .
C10 O8 C9 111.7(2) . .
C10 O8 K1 108.19(14) . .
C9 O8 K1 108.95(15) . .
C12 O9 C11 112.17(19) . .
C12 O9 K1 119.84(15) . .
C11 O9 K1 118.38(14) . .
O3 C1 H1A 109.5 . .
O3 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O3 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O4 C2 C3 109.0(2) . .
O4 C2 H2A 109.9 . .
C3 C2 H2A 109.9 . .
O4 C2 H2B 109.9 . .
C3 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
O5 C3 C2 108.2(2) . .
O5 C3 H3A 110.1 . .
C2 C3 H3A 110.1 . .
O5 C3 H3B 110.1 . .
C2 C3 H3B 110.1 . .
H3A C3 H3B 108.4 . .
O5 C4 C5 108.0(2) . .
O5 C4 H4A 110.1 . .
C5 C4 H4A 110.1 . .
O5 C4 H4B 110.1 . .
C5 C4 H4B 110.1 . .
H4A C4 H4B 108.4 . .
O6 C5 C4 108.0(2) . .
O6 C5 H5A 110.1 . .
C4 C5 H5A 110.1 . .
O6 C5 H5B 110.1 . .
C4 C5 H5B 110.1 . .
H5A C5 H5B 108.4 . .
O6 C6 C7 109.3(2) . .
O6 C6 H6A 109.8 . .
C7 C6 H6A 109.8 . .
O6 C6 H6B 109.8 . .
C7 C6 H6B 109.8 . .
H6A C6 H6B 108.3 . .
O7 C7 C6 108.1(2) . .
O7 C7 H7A 110.1 . .
C6 C7 H7A 110.1 . .
O7 C7 H7B 110.1 . .
C6 C7 H7B 110.1 . .
H7A C7 H7B 108.4 . .
O7 C8 C9 107.9(2) . .
O7 C8 H8A 110.1 . .
C9 C8 H8A 110.1 . .
O7 C8 H8B 110.1 . .
C9 C8 H8B 110.1 . .
H8A C8 H8B 108.4 . .
O8 C9 C8 108.9(3) . .
O8 C9 H9A 109.9 . .
C8 C9 H9A 109.9 . .
O8 C9 H9B 109.9 . .
C8 C9 H9B 109.9 . .
H9A C9 H9B 108.3 . .
O8 C10 C11 108.4(2) . .
O8 C10 H10A 110.0 . .
C11 C10 H10A 110.0 . .
O8 C10 H10B 110.0 . .
C11 C10 H10B 110.0 . .
H10A C10 H10B 108.4 . .
O9 C11 C10 108.4(2) . .
O9 C11 K1 116.29(14) . 2_746
C10 C11 K1 135.22(16) . 2_746
O9 C11 H11A 110.0 . .
C10 C11 H11A 110.0 . .
K1 C11 H11A 52.3 2_746 .
O9 C11 H11B 110.0 . .
C10 C11 H11B 110.0 . .
K1 C11 H11B 57.2 2_746 .
H11A C11 H11B 108.4 . .
O9 C12 C13 108.5(2) . .
O9 C12 H12A 110.0 . .
C13 C12 H12A 110.0 . .
O9 C12 H12B 110.0 . .
C13 C12 H12B 110.0 . .
H12A C12 H12B 108.4 . .
O4 C13 C12 109.0(2) . .
O4 C13 H13A 109.9 . .
C12 C13 H13A 109.9 . .
O4 C13 H13B 109.9 . .
C12 C13 H13B 109.9 . .
H13A C13 H13B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.649(2) .
Fe1 N2 1.652(2) .
Fe1 O3 2.0028(18) .
Fe1 O3 2.0034(19) 3_666
K1 O1 2.668(2) .
K1 O5 2.7477(19) .
K1 O7 2.7543(18) .
K1 O9 2.7835(19) .
K1 O6 2.846(2) .
K1 O4 2.8630(18) .
K1 O8 2.8663(19) .
K1 C11 3.499(3) 2_756
N1 O1 1.225(3) .
N2 O2 1.221(3) .
O3 C1 1.404(3) .
O3 Fe1 2.0034(19) 3_666
O4 C2 1.432(3) .
O4 C13 1.432(3) .
O5 C3 1.425(3) .
O5 C4 1.427(3) .
O6 C6 1.430(3) .
O6 C5 1.436(3) .
O7 C8 1.424(3) .
O7 C7 1.433(3) .
O8 C10 1.429(4) .
O8 C9 1.432(3) .
O9 C12 1.425(3) .
O9 C11 1.428(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.494(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.505(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.478(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.493(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.501(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 K1 3.499(3) 2_746
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.495(3) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
