#------------------------------------------------------------------------------
#$Date: 2020-10-06 13:18:58 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257793 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/96/7059688.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_7059688
loop_
_publ_author_name
'Yang, Xiuqin'
'Jin, Jing'
'Guo, Zhuming'
'Xiao, Zhiyin'
'Chen, Naiwen'
'Jiang, Xiujuan'
'He, Yi'
'Liu, Xiaoming'
_publ_section_title
;
 The monoiron anion fac-[Fe(CO)3I3]− and its organic aminium salts:
 their preparation, CO-release, and cytotoxicity
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10300
_journal_page_last               10308
_journal_paper_doi               10.1039/D0NJ01182G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C3 Fe I3 O3, 0.5(C8 H24 N2)'
_chemical_formula_sum            'C7 H12 Fe I3 N O3'
_chemical_formula_weight         594.73
_chemical_name_systematic        'salt 3'
_chemical_properties_physical
Air-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-02 deposited with the CCDC.	2020-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2405(9)
_cell_length_b                   8.0958(9)
_cell_length_c                   12.6129(12)
_cell_measurement_reflns_used    1448
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2230
_cell_measurement_theta_min      3.6650
_cell_volume                     806.50(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00  42.00   0.80   30.00    --  -15.89  77.00 -60.00   45
  2  ω    -41.00  44.60   0.80   30.00    --  -15.89  77.00-180.00  107
  3  ω     18.00  45.20   0.80   30.00    --  -15.89  77.00-150.00   34
  4  ω    -11.00  39.40   0.80   30.00    --   16.05  77.00  60.00   63
  5  ω    -11.00  67.40   0.80   30.00    --   16.05  77.00 -60.00   98
  6  ω      9.00  83.40   0.80   30.00    --   16.05  77.00  90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0553024000
_diffrn_orient_matrix_UB_12      0.0008933000
_diffrn_orient_matrix_UB_13      -0.0545739000
_diffrn_orient_matrix_UB_21      0.0705299000
_diffrn_orient_matrix_UB_22      -0.0061079000
_diffrn_orient_matrix_UB_23      -0.0214287000
_diffrn_orient_matrix_UB_31      -0.0054624000
_diffrn_orient_matrix_UB_32      -0.0874598000
_diffrn_orient_matrix_UB_33      0.0009563000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4931
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.449
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1515
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0844P)²+0.1939P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                935
_reflns_number_total             1515
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj01182g2.cif
_cod_data_source_block           180624-yxq-feic4ni
_cod_depositor_comments
;Adding full bibliography for 7059687--7059690.cif.

 Adding full bibliography for 7059687--7059690.cif.
;
_cod_database_code               7059688
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'H C N O Fe I'
_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.
;
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.204
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 = C4-C3
 1.55 with sigma of 0.001
 C5-C4
 1.55 with sigma of 0.001
 C3-N1
 1.45 with sigma of 0.001
3. Rigid body (RIGU) restrains
 C6, C5, C4, C3, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(I2A)=1-FVAR(1)
 Sof(I2)=FVAR(1)
 Fixed Sof: H5A(0.5) H5B(0.5) H4A(0.5) H4B(0.5) H3A(0.5) H3B(0.5) H1A(0.5)
 H1B(0.5) H1C(0.5) H6A(0.5) H6B(0.5) H6C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.695
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
C1 C 0.268(2) 0.250000 0.6895(16) 0.125(6) Uani 1 2 d S T P B .
C2 C -0.0099(14) 0.0883(18) 0.6554(10) 0.119(4) Uani 1 1 d . . . . .
C5 C 0.537(3) 0.250000 0.3651(17) 0.282(18) Uani 1 2 d DS TU P . .
H5A H 0.591552 0.345948 0.344257 0.338 Uiso 0.5 1 calc R . . . .
H5B H 0.591552 0.154052 0.344257 0.338 Uiso 0.5 1 calc R . . . .
C4 C 0.353(3) 0.250000 0.2890(16) 0.234(13) Uani 1 2 d DS TU P . .
H4A H 0.296112 0.153631 0.307461 0.281 Uiso 0.5 1 calc R . . . .
H4B H 0.296112 0.346369 0.307461 0.281 Uiso 0.5 1 calc R . . . .
C3 C 0.323(2) 0.250000 0.1620(16) 0.233(12) Uani 1 2 d DS TU P . .
H3A H 0.376808 0.346784 0.141640 0.279 Uiso 0.5 1 calc R . . . .
H3B H 0.376808 0.153216 0.141640 0.279 Uiso 0.5 1 calc R . . . .
N1 N 0.1453(18) 0.250000 0.1001(13) 0.176(7) Uani 1 2 d DS TU P . .
H1A H 0.118907 0.148220 0.074231 0.211 Uiso 0.5 1 d R . . A -1
H1B H 0.142927 0.317860 0.044141 0.211 Uiso 0.5 1 d R . . A -1
H1C H 0.070857 0.283920 0.134461 0.211 Uiso 0.5 1 d R . . A -1
Fe1 Fe 0.0926(2) 0.250000 0.74248(14) 0.0800(6) Uani 1 2 d S T P . .
I1 I -0.16813(11) 0.250000 0.82591(8) 0.1015(5) Uani 1 2 d S T P B .
I2 I 0.2710(19) 0.0433(18) 0.8864(6) 0.141(3) Uani 0.45(2) 1 d . . . B 1
C6 C 0.586(5) 0.250000 0.4932(18) 0.42(4) Uani 1 2 d DS TU P . .
H6A H 0.642325 0.352430 0.518124 0.632 Uiso 0.5 1 d R . . C -1
H6B H 0.663115 0.159980 0.517394 0.632 Uiso 0.5 1 d R . . C -1
H6C H 0.491605 0.237590 0.523344 0.632 Uiso 0.5 1 d R . . C -1
O2 O -0.0745(19) -0.0158(14) 0.5980(12) 0.196(6) Uani 1 1 d . . . . .
O1 O 0.3715(18) 0.250000 0.6494(14) 0.172(6) Uani 1 2 d S T P . .
I2A I 0.2280(10) -0.0104(13) 0.8672(9) 0.135(2) Uani 0.55(2) 1 d . . . B 2
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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
O1 C1 Fe1 175.4(19) . . ?
O2 C2 Fe1 178.8(11) . . ?
H5A C5 H5B 106.4 . . ?
C4 C5 H5A 106.3 . . ?
C4 C5 H5B 106.3 . . ?
C4 C5 C6 124(2) . . ?
C6 C5 H5A 106.3 . . ?
C6 C5 H5B 106.3 . . ?
C5 C4 H4A 107.7 . . ?
C5 C4 H4B 107.7 . . ?
H4A C4 H4B 107.1 . . ?
C3 C4 C5 118.5(16) . . ?
C3 C4 H4A 107.7 . . ?
C3 C4 H4B 107.7 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N1 C3 C4 113.1(15) . . ?
N1 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C3 N1 H1A 107.5 . . ?
C3 N1 H1B 102.6 . . ?
C3 N1 H1C 117.9 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 Fe1 C2 93.6(6) . 4_565 ?
C1 Fe1 C2 93.6(6) . . ?
C1 Fe1 I1 179.0(6) . . ?
C1 Fe1 I2 84.4(6) . . ?
C1 Fe1 I2 84.4(6) . 4_565 ?
C1 Fe1 I2A 88.4(4) . 4_565 ?
C1 Fe1 I2A 88.4(4) . . ?
C2 Fe1 C2 96.0(9) . 4_565 ?
C2 Fe1 I1 87.0(4) 4_565 . ?
C2 Fe1 I1 87.0(4) . . ?
C2 Fe1 I2 91.8(6) . . ?
C2 Fe1 I2 172.0(6) 4_565 . ?
C2 Fe1 I2 172.0(6) . 4_565 ?
C2 Fe1 I2 91.8(6) 4_565 4_565 ?
C2 Fe1 I2A 80.0(5) 4_565 4_565 ?
C2 Fe1 I2A 175.6(5) . 4_565 ?
C2 Fe1 I2A 175.6(5) 4_565 . ?
C2 Fe1 I2A 80.0(5) . . ?
I1 Fe1 I2A 90.92(15) . 4_565 ?
I1 Fe1 I2A 90.92(15) . . ?
I2 Fe1 I1 94.8(3) . . ?
I2 Fe1 I1 94.8(3) 4_565 . ?
I2 Fe1 I2 80.3(7) 4_565 . ?
I2 Fe1 I2A 12.3(3) 4_565 4_565 ?
I2 Fe1 I2A 92.2(6) . 4_565 ?
I2A Fe1 I2A 103.9(6) . 4_565 ?
C5 C6 H6A 107.4 . . ?
C5 C6 H6B 106.4 . . ?
C5 C6 H6C 114.6 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
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
C1 Fe1 1.758(18) . ?
C1 O1 1.108(17) . ?
C2 Fe1 1.762(14) . ?
C2 O2 1.139(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.5498(10) . ?
C5 C6 1.5499(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.5498(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 N1 1.4500(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8898 . ?
Fe1 I1 2.6482(19) . ?
Fe1 I2 2.595(8) . ?
Fe1 I2 2.595(8) 4_565 ?
Fe1 I2A 2.676(7) . ?
Fe1 I2A 2.676(7) 4_565 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9601 . ?
C6 H6C 0.9602 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C4 C3 N1 180.000(3) . . . . ?
C6 C5 C4 C3 180.000(5) . . . . ?
