The monoiron anion fac-[Fe(CO)3I3]− and its organic aminium salts: their preparation, CO-release, and cytotoxicity
Yang, Xiuqin; Jin, Jing; Guo, Zhuming; Xiao, Zhiyin; Chen, Naiwen; Jiang, Xiujuan; He, Yi; Liu, Xiaoming; New Journal of Chemistry 44 (2020) 10300–10308; doi:10.1039/D0NJ01182G

data_7059689
_publ_section_title
;
 The monoiron anion fac-[Fe(CO)3I3]&#x2212; 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, C5 H14 N'
_chemical_formula_sum            'C8 H14 Fe I3 N O3'
_chemical_formula_weight         608.75
_chemical_name_systematic        'salt 4'
_chemical_properties_physical
Air-sensitive,Heat-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                100.214(9)
_cell_angle_beta                 94.639(16)
_cell_angle_gamma                92.457(16)
_cell_formula_units_Z            2
_cell_length_a                   8.092(2)
_cell_length_b                   8.2197(8)
_cell_length_c                   13.3496(16)
_cell_measurement_reflns_used    1582
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.7780
_cell_measurement_theta_min      3.5000
_cell_volume                     869.5(3)
_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)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  23.00   1.00    6.00    --  -15.89 -99.00-150.00   26
  2  \w     -9.00  23.00   1.00    6.00    --  -15.89 -99.00  60.00   32
  3  \w     16.00  72.00   1.00    6.00    --   16.05  38.00  30.00   56
  4  \w     35.00  60.00   1.00    6.00    --   16.05 178.00-150.00   25
  5  \w      0.00  84.00   1.00    6.00    --   16.05  38.00  90.00   84
  6  \w     20.00  89.00   1.00    6.00    --   16.05-159.00 -89.00   69
  7  \w    -53.00  25.00   1.00    6.00    --   16.05 -38.00 -90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0075689000
_diffrn_orient_matrix_UB_12      -0.0779599000
_diffrn_orient_matrix_UB_13      0.0152097000
_diffrn_orient_matrix_UB_21      0.0069549000
_diffrn_orient_matrix_UB_22      -0.0376152000
_diffrn_orient_matrix_UB_23      -0.0514599000
_diffrn_orient_matrix_UB_31      0.0874935000
_diffrn_orient_matrix_UB_32      0.0148929000
_diffrn_orient_matrix_UB_33      0.0076864000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_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       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3010
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33145
_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            dark-red
_exptl_crystal_colour_primary    dark-red
_exptl_crystal_density_diffrn    2.325
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.715
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3010
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.1170
_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/[\s^2^(Fo^2^)+(0.1780P)^2^+7.1201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2920
_refine_ls_wR_factor_ref         0.3462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1765
_reflns_number_total             3010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01182g2.cif
_cod_data_source_block           180624-yxq-fec5ni_tw
_cod_depositor_comments
;Adding full bibliography for 7059687--7059690.cif.

 Adding full bibliography for 7059687--7059690.cif.
;
_cod_database_code               7059689
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'H C N O Fe I'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.634(9)
 0.366(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C8-C7 = C6-C5
 1.5 with sigma of 0.001
 C4-C5 = C6-C7
 1.5 with sigma of 0.001
 C4-N1
 1.4 with sigma of 0.001
4. Rigid body (RIGU) restrains
 N1, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              1443
_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 1.803
_oxdiff_exptl_absorpt_empirical_full_min 0.576