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_7059688
_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, 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  t~exp~   \w     \q     \k     \f   Frames
  1  \w      6.00  42.00   0.80   30.00    --  -15.89  77.00 -60.00   45
  2  \w    -41.00  44.60   0.80   30.00    --  -15.89  77.00-180.00  107
  3  \w     18.00  45.20   0.80   30.00    --  -15.89  77.00-150.00   34
  4  \w    -11.00  39.40   0.80   30.00    --   16.05  77.00  60.00   63
  5  \w    -11.00  67.40   0.80   30.00    --   16.05  77.00 -60.00   98
  6  \w      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       '\w 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/[\s^2^(Fo^2^)+(0.0844P)^2^+0.1939P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              81498
_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